# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003

data_global
_publ_contact_author_email       dk@anorgchemie.univ.kiev.ua
_publ_contact_author_name        'Dr Konstantin V. Domasevitch'
_journal_name_full               Chem.Commun.
_journal_coden_Cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
I.Boldog
E.B.Rusanov
J.Sieler
S.Blaurock
K.V.Domasevitch

data_dpzn
_database_code_CSD               200495

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
3,3',5,5'-tetramethyl-4,4'-bipyrazole Chloroform solvate
;
_chemical_name_common            
"3,3',5,5'-tetramethyl-4,4'-bipyrazole Chloroform solvate"
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C11 H15 Cl3 N4'
_chemical_formula_weight         309.62
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   29.196(2)
_cell_length_b                   29.196(2)
_cell_length_c                   22.406(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     19099.1(25)
_cell_formula_units_Z            48
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             7680
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'IPDS Stoe'
_diffrn_measurement_method       'phi rotation'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16913
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_sigmaI/netI    0.2676
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         26.01
_reflns_number_total             7333
_reflns_number_observed          1408
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 2242 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.1430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0110(20)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5091
_refine_ls_number_parameters     500
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.3327
_refine_ls_R_factor_obs          0.1270
_refine_ls_wR_factor_all         0.4376
_refine_ls_wR_factor_obs         0.2836
_refine_ls_goodness_of_fit_all   0.844
_refine_ls_goodness_of_fit_obs   1.553
_refine_ls_restrained_S_all      1.110
_refine_ls_restrained_S_obs      1.623
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
C1 C 0.5831(5) 0.4512(5) -0.1442(4) 0.061(4) Uani 1 d . .
C2 C 0.6031(4) 0.4938(4) -0.1562(4) 0.058(3) Uani 1 d . .
C3 C 0.6161(5) 0.4908(5) -0.2169(4) 0.081(5) Uani 1 d . .
C4 C 0.5645(6) 0.4321(5) -0.0878(4) 0.092(5) Uani 1 d . .
H4A H 0.5536(6) 0.4016(5) -0.0949(4) 0.080 Uiso 1 d R .
H4B H 0.5877(6) 0.4315(5) -0.0574(4) 0.080 Uiso 1 d R .
H4C H 0.5396(6) 0.4511(5) -0.0750(4) 0.080 Uiso 1 d R .
C5 C 0.6373(7) 0.5262(6) -0.2544(5) 0.109(6) Uani 1 d . .
H5A H 0.6428(7) 0.5150(6) -0.2941(5) 0.080 Uiso 1 d R .
H5B H 0.6164(7) 0.5516(6) -0.2561(5) 0.080 Uiso 1 d R .
H5C H 0.6657(7) 0.5361(6) -0.2371(5) 0.080 Uiso 1 d R .
C6 C 0.5746(5) 0.5579(5) -0.0878(5) 0.068(4) Uani 1 d . .
C7 C 0.6094(5) 0.5325(4) -0.1155(4) 0.060(3) Uani 1 d . .
C8 C 0.6504(5) 0.5525(5) -0.0973(4) 0.063(3) Uani 1 d . .
C9 C 0.5258(7) 0.5537(8) -0.0928(9) 0.139(9) Uani 1 d . .
H9A H 0.5110(7) 0.5757(8) -0.0674(9) 0.080 Uiso 1 d R .
H9B H 0.5176(7) 0.5595(8) -0.1336(9) 0.080 Uiso 1 d R .
H9C H 0.5161(7) 0.5234(8) -0.0819(9) 0.080 Uiso 1 d R .
C10 C 0.6983(6) 0.5427(7) -0.1124(10) 0.129(7) Uani 1 d . .
H10A H 0.7183(6) 0.5634(7) -0.0917(10) 0.080 Uiso 1 d R .
H10B H 0.7052(6) 0.5118(7) -0.1010(10) 0.080 Uiso 1 d R .
H10C H 0.7026(6) 0.5461(7) -0.1547(10) 0.080 Uiso 1 d R .
C11 C 0.7878(5) 0.8948(6) -0.0123(5) 0.080(4) Uani 1 d . .
C12 C 0.7679(5) 0.8548(5) -0.0379(4) 0.071(4) Uani 1 d . .
C13 C 0.7928(5) 0.8184(6) -0.0148(4) 0.079(4) Uani 1 d . .
C14 C 0.7787(7) 0.9435(6) -0.0223(9) 0.118(6) Uani 1 d . .
H14A H 0.7989(7) 0.9616(6) 0.0019(9) 0.080 Uiso 1 d R .
H14B H 0.7835(7) 0.9507(6) -0.0636(9) 0.080 Uiso 1 d R .
H14C H 0.7475(7) 0.9501(6) -0.0117(9) 0.080 Uiso 1 d R .
C15 C 0.7866(7) 0.7687(6) -0.0264(7) 0.103(5) Uani 1 d . .
H15A H 0.8094(7) 0.7513(6) -0.0054(7) 0.080 Uiso 1 d R .
H15B H 0.7567(7) 0.7601(6) -0.0125(7) 0.080 Uiso 1 d R .
H15C H 0.7889(7) 0.7626(6) -0.0684(7) 0.080 Uiso 1 d R .
C16 C 0.6866(6) 0.8341(5) -0.0743(4) 0.077(5) Uani 1 d . .
C17 C 0.7299(5) 0.8548(5) -0.0805(4) 0.069(4) Uani 1 d . .
C18 C 0.7282(5) 0.8765(5) -0.1346(5) 0.075(4) Uani 1 d . .
C19 C 0.6684(6) 0.8093(9) -0.0250(5) 0.128(8) Uani 1 d . .
H19A H 0.6374(6) 0.8011(9) -0.0343(5) 0.080 Uiso 1 d R .
H19B H 0.6867(6) 0.7821(9) -0.0216(5) 0.080 Uiso 1 d R .
H19C H 0.6691(6) 0.8258(9) 0.0121(5) 0.080 Uiso 1 d R .
C20 C 0.7660(6) 0.9025(7) -0.1663(6) 0.111(6) Uani 1 d . .
H20A H 0.7668(6) 0.8955(7) -0.2081(6) 0.080 Uiso 1 d R .
H20B H 0.7949(6) 0.8957(7) -0.1477(6) 0.080 Uiso 1 d R .
H20C H 0.7600(6) 0.9345(7) -0.1598(6) 0.080 Uiso 1 d R .
C21 C 0.5635(4) 0.7355(4) 0.0481(3) 0.043(3) Uani 1 d . .
C22 C 0.5188(4) 0.7321(4) 0.0249(3) 0.043(3) Uani 1 d . .
C23 C 0.5163(4) 0.6884(4) -0.0020(3) 0.041(3) Uani 1 d . .
C24 C 0.5844(4) 0.7729(4) 0.0825(3) 0.049(3) Uani 1 d . .
H24A H 0.6154(4) 0.7652(4) 0.0924(3) 0.080 Uiso 1 d R .
H24B H 0.5841(4) 0.8003(4) 0.0586(3) 0.080 Uiso 1 d R .
H24C H 0.5673(4) 0.7780(4) 0.1184(3) 0.080 Uiso 1 d R .
C25 C 0.4758(4) 0.6669(4) -0.0351(4) 0.055(3) Uani 1 d . .
H25A H 0.4846(4) 0.6369(4) -0.0483(4) 0.080 Uiso 1 d R .
H25B H 0.4500(4) 0.6644(4) -0.0088(4) 0.080 Uiso 1 d R .
H25C H 0.4676(4) 0.6853(4) -0.0690(4) 0.080 Uiso 1 d R .
C26 C 0.5599(4) 0.7696(5) -0.1596(4) 0.060(4) Uani 1 d . .
C27 C 0.5164(4) 0.7689(5) -0.1832(4) 0.062(4) Uani 1 d . .
C28 C 0.5084(5) 0.8122(6) -0.2061(4) 0.080(4) Uani 1 d . .
C29 C 0.5846(5) 0.7307(5) -0.1283(4) 0.081(4) Uani 1 d . .
H29A H 0.6145(5) 0.7414(5) -0.1171(4) 0.080 Uiso 1 d R .
H29B H 0.5679(5) 0.7221(5) -0.0931(4) 0.080 Uiso 1 d R .
H29C H 0.5875(5) 0.7046(5) -0.1541(4) 0.080 Uiso 1 d R .
C30 C 0.4685(5) 0.8328(6) -0.2384(6) 0.096(5) Uani 1 d . .
H30A H 0.4751(5) 0.8644(6) -0.2469(6) 0.080 Uiso 1 d R .
H30B H 0.4639(5) 0.8165(6) -0.2751(6) 0.080 Uiso 1 d R .
H30C H 0.4412(5) 0.8309(6) -0.2145(6) 0.080 Uiso 1 d R .
N1 N 0.5848(4) 0.4254(3) -0.1948(3) 0.064(3) Uani 1 d . .
N2 N 0.6051(4) 0.4510(4) -0.2392(4) 0.081(4) Uani 1 d . .
N3 N 0.5938(4) 0.5905(4) -0.0540(3) 0.073(3) Uani 1 d . .
N4 N 0.6398(4) 0.5881(4) -0.0605(3) 0.063(3) Uani 1 d . .
N5 N 0.8223(4) 0.8785(5) 0.0227(4) 0.081(4) Uani 1 d . .
N6 N 0.8268(5) 0.8344(5) 0.0212(4) 0.089(4) Uani 1 d . .
N7 N 0.6625(4) 0.8432(4) -0.1238(4) 0.079(4) Uani 1 d . .
N8 N 0.6892(5) 0.8675(4) -0.1637(4) 0.086(4) Uani 1 d . .
N9 N 0.5857(3) 0.6966(3) 0.0361(3) 0.048(2) Uani 1 d . .
N10 N 0.5555(3) 0.6682(3) 0.0065(3) 0.047(2) Uani 1 d . .
N11 N 0.5796(4) 0.8108(4) -0.1678(3) 0.065(3) Uani 1 d . .
N12 N 0.5463(4) 0.8389(4) -0.1950(3) 0.076(3) Uani 1 d . .
C31 C 0.6185(6) 0.8285(6) -0.3224(7) 0.285(31) Uani 1 d D .
Cl1 Cl 0.5827(4) 0.8632(4) -0.3631(4) 0.143(4) Uani 0.60 d PD .
Cl2 Cl 0.6757(3) 0.8384(6) -0.3454(4) 0.204(7) Uani 0.60 d PD .
Cl3 Cl 0.6004(7) 0.7733(3) -0.3282(4) 0.252(10) Uani 0.60 d PD .
Cl1B Cl 0.6136(9) 0.8735(13) -0.3751(21) 0.380(18) Uiso 0.40 d PD .
Cl2B Cl 0.6701(8) 0.8000(13) -0.3375(24) 0.380(18) Uiso 0.40 d PD .
Cl3B Cl 0.5721(8) 0.7908(10) -0.3371(24) 0.380(18) Uiso 0.40 d PD .
C32 C 0.7106(7) 0.7001(5) -0.1990(7) 0.485(67) Uani 1 d D .
Cl4 Cl 0.7077(3) 0.7580(3) -0.1906(3) 0.134(3) Uani 0.80 d PD .
Cl5 Cl 0.6704(4) 0.6772(6) -0.2445(7) 0.250(7) Uani 0.80 d PD .
Cl6 Cl 0.7089(3) 0.6795(3) -0.1221(3) 0.144(3) Uani 0.80 d PD .
Cl6B Cl 0.6993(11) 0.6528(6) -0.1636(8) 0.143(6) Uiso 0.20 d PD .
Cl4B Cl 0.7366(8) 0.7442(7) -0.1674(11) 0.143(6) Uiso 0.20 d PD .
Cl5B Cl 0.6699(9) 0.7150(9) -0.2543(10) 0.143(6) Uiso 0.20 d PD .
C33 C 0.6268(5) 1.0201(6) -0.0795(11) 0.456(52) Uiso 1 d D .
Cl7 Cl 0.6649(9) 0.9771(11) -0.0608(18) 0.364(23) Uiso 0.40 d PD .
Cl8 Cl 0.6498(8) 1.0532(8) -0.1391(10) 0.222(8) Uiso 0.40 d PD .
Cl9 Cl 0.5736(7) 0.9994(11) -0.0993(14) 0.298(14) Uiso 0.40 d PD .
Cl7A Cl 0.6321(9) 0.9618(6) -0.0668(7) 0.253(7) Uiso 0.60 d PD .
Cl8A Cl 0.6728(7) 1.0512(10) -0.0986(14) 0.353(13) Uiso 0.60 d PD .
Cl9A Cl 0.5723(5) 1.0386(8) -0.0943(6) 0.237(6) Uiso 0.60 d PD .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.060(9) 0.064(10) 0.059(5) -0.011(5) 0.017(4) 0.003(7)
C2 0.067(9) 0.048(9) 0.059(5) -0.019(4) 0.017(5) -0.023(7)
C3 0.122(13) 0.059(10) 0.063(6) -0.015(6) 0.049(6) -0.020(9)
C4 0.141(15) 0.065(11) 0.071(6) -0.019(5) 0.032(7) -0.038(10)
C5 0.183(18) 0.077(12) 0.068(6) -0.019(6) 0.035(8) -0.058(12)
C6 0.039(10) 0.068(10) 0.096(7) -0.028(6) 0.013(5) -0.007(7)
C7 0.074(10) 0.046(8) 0.059(5) -0.020(4) 0.014(5) -0.010(7)
C8 0.058(10) 0.050(9) 0.082(6) -0.014(5) 0.019(6) -0.010(7)
C9 0.092(17) 0.118(17) 0.205(15) -0.122(14) 0.037(12) -0.048(13)
C10 0.063(14) 0.082(15) 0.243(17) -0.095(13) 0.024(11) -0.007(10)
C11 0.056(11) 0.073(13) 0.112(8) -0.002(7) -0.016(7) 0.005(8)
C12 0.074(11) 0.065(10) 0.075(6) -0.004(6) -0.023(6) -0.002(8)
C13 0.084(11) 0.081(12) 0.072(6) -0.011(6) -0.030(6) 0.008(9)
C14 0.076(14) 0.071(15) 0.206(15) -0.021(10) -0.070(11) 0.029(10)
C15 0.105(15) 0.073(13) 0.131(10) 0.007(8) -0.049(9) -0.014(10)
C16 0.074(12) 0.096(12) 0.062(6) 0.026(6) -0.015(5) -0.011(9)
C17 0.050(10) 0.087(12) 0.071(6) 0.008(5) -0.013(5) -0.010(8)
C18 0.058(11) 0.067(11) 0.099(8) 0.023(6) -0.013(6) 0.001(8)
C19 0.066(12) 0.245(25) 0.071(7) 0.039(9) -0.007(6) -0.028(13)
C20 0.096(14) 0.117(16) 0.120(9) 0.049(9) -0.029(8) -0.059(12)
C21 0.034(7) 0.052(8) 0.042(4) 0.006(4) 0.003(4) -0.002(6)
C22 0.046(8) 0.049(8) 0.035(4) 0.002(3) 0.003(4) 0.002(5)
C23 0.040(8) 0.046(7) 0.038(4) 0.003(4) -0.005(4) -0.004(5)
C24 0.040(7) 0.065(8) 0.041(4) -0.006(4) -0.009(4) 0.004(6)
C25 0.046(8) 0.058(9) 0.061(5) -0.013(4) -0.008(4) 0.008(6)
C26 0.056(9) 0.077(11) 0.048(5) 0.001(5) 0.004(5) -0.026(8)
C27 0.063(11) 0.073(11) 0.050(5) -0.002(5) 0.002(5) -0.018(7)
C28 0.085(12) 0.092(13) 0.062(6) -0.004(6) -0.016(6) -0.038(9)
C29 0.072(11) 0.100(12) 0.071(6) -0.008(6) 0.010(5) -0.009(9)
C30 0.055(11) 0.122(15) 0.109(8) 0.049(8) -0.037(7) -0.029(9)
N1 0.085(9) 0.045(7) 0.061(4) -0.013(4) 0.016(4) -0.021(6)
N2 0.102(10) 0.070(9) 0.072(5) -0.024(5) 0.037(5) -0.031(7)
N3 0.072(9) 0.076(9) 0.072(5) -0.041(5) 0.007(5) -0.006(7)
N4 0.051(8) 0.071(8) 0.067(4) -0.012(4) 0.003(4) -0.005(6)
N5 0.063(9) 0.082(11) 0.097(6) -0.021(5) -0.027(5) 0.025(7)
N6 0.109(12) 0.065(11) 0.092(6) -0.008(5) -0.027(6) 0.010(8)
N7 0.069(9) 0.093(10) 0.074(5) 0.035(5) -0.019(5) -0.020(7)
N8 0.090(11) 0.064(9) 0.105(6) 0.048(5) -0.023(6) -0.026(7)
N9 0.042(6) 0.048(7) 0.053(4) -0.007(3) 0.003(3) 0.012(5)
N10 0.046(7) 0.051(6) 0.044(4) -0.003(3) -0.002(3) 0.010(5)
N11 0.052(7) 0.088(9) 0.055(4) -0.004(4) 0.000(4) -0.020(7)
N12 0.089(9) 0.101(9) 0.039(4) 0.012(4) -0.003(4) -0.005(8)
C31 0.392(61) 0.216(38) 0.247(30) -0.150(30) 0.243(41) -0.145(41)
Cl1 0.128(9) 0.136(10) 0.164(6) -0.017(5) -0.030(5) 0.016(7)
Cl2 0.125(9) 0.362(21) 0.125(5) 0.070(8) 0.051(5) 0.070(10)
Cl3 0.543(30) 0.103(8) 0.108(5) 0.001(5) 0.101(10) -0.055(12)
C32 0.035(17) 0.637(108) 0.785(108) 0.651(106) 0.025(31) 0.018(31)
Cl4 0.142(7) 0.129(6) 0.131(4) -0.006(3) 0.037(3) 0.003(5)
Cl5 0.167(11) 0.238(16) 0.345(13) -0.173(13) -0.049(9) 0.032(10)
Cl6 0.145(7) 0.122(6) 0.165(4) 0.035(4) 0.018(4) -0.017(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.363(13) . ?
C1 C2 1.40(2) . ?
C1 C4 1.48(2) . ?
C2 C3 1.414(12) . ?
C2 C7 1.46(2) . ?
C3 N2 1.31(2) . ?
C3 C5 1.47(2) . ?
C6 N3 1.34(2) . ?
C6 C7 1.40(2) . ?
C6 C9 1.44(2) . ?
C7 C8 1.39(2) . ?
C8 N4 1.361(15) . ?
C8 C10 1.47(2) . ?
C11 N5 1.36(2) . ?
C11 C12 1.42(2) . ?
C11 C14 1.46(2) . ?
C12 C13 1.39(2) . ?
C12 C17 1.46(2) . ?
C13 N6 1.36(2) . ?
C13 C15 1.48(2) . ?
C16 N7 1.342(14) . ?
C16 C17 1.41(2) . ?
C16 C19 1.42(2) . ?
C17 C18 1.37(2) . ?
C18 N8 1.34(2) . ?
C18 C20 1.52(2) . ?
C21 N9 1.335(12) . ?
C21 C22 1.408(14) . ?
C21 C24 1.470(15) . ?
C22 C23 1.413(14) . ?
C22 C22 1.52(2) 6_564 ?
C23 N10 1.301(12) . ?
C23 C25 1.531(15) . ?
C26 N11 1.346(14) . ?
C26 C27 1.37(2) . ?
C26 C29 1.52(2) . ?
C27 C28 1.38(2) . ?
C27 C27 1.46(2) 6_564 ?
C28 N12 1.38(2) . ?
C28 C30 1.50(2) . ?
N1 N2 1.377(13) . ?
N3 N4 1.352(14) . ?
N5 N6 1.30(2) . ?
N7 N8 1.384(15) . ?
N9 N10 1.379(12) . ?
N11 N12 1.410(15) . ?
C31 Cl3 1.70(2) . ?
C31 Cl1 1.72(2) . ?
C31 Cl2B 1.75(2) . ?
C31 Cl2 1.77(2) . ?
C31 Cl1B 1.77(2) . ?
C31 Cl3B 1.78(2) . ?
Cl1 Cl1B 0.99(2) . ?
Cl1 Cl3B 2.22(3) . ?
Cl2 Cl2B 1.15(3) . ?
Cl2 Cl1B 2.19(3) . ?
Cl3 Cl3B 0.99(2) . ?
Cl3 Cl2B 2.19(3) . ?
C32 Cl6B 1.63(2) . ?
C32 Cl4B 1.65(2) . ?
C32 Cl5 1.69(2) . ?
C32 Cl4 1.70(2) . ?
C32 Cl5B 1.77(2) . ?
C32 Cl6 1.825(15) . ?
Cl4 Cl4B 1.07(2) . ?
Cl4 Cl5B 2.20(2) . ?
Cl5 Cl5B 1.12(2) . ?
Cl5 Cl6B 2.12(3) . ?
Cl6 Cl6B 1.24(2) . ?
Cl6 Cl4B 2.29(2) . ?
C33 Cl8A 1.677(10) . ?
C33 Cl9A 1.712(10) . ?
C33 Cl9 1.724(10) . ?
C33 Cl7 1.730(10) . ?
C33 Cl7A 1.734(10) . ?
C33 Cl8 1.779(11) . ?
Cl7 Cl7A 1.07(2) . ?
Cl7 Cl8A 2.33(3) . ?
Cl8 Cl8A 1.13(2) . ?
Cl9 Cl9A 1.15(2) . ?
Cl9 Cl7A 2.16(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 108.4(8) . . ?
N1 C1 C4 121.1(12) . . ?
C2 C1 C4 130.5(9) . . ?
C1 C2 C3 104.0(8) . . ?
C1 C2 C7 128.2(8) . . ?
C3 C2 C7 127.8(11) . . ?
N2 C3 C2 110.9(10) . . ?
N2 C3 C5 120.8(9) . . ?
C2 C3 C5 128.3(11) . . ?
N3 C6 C7 108.8(12) . . ?
N3 C6 C9 121.3(11) . . ?
C7 C6 C9 129.9(11) . . ?
C8 C7 C6 105.7(10) . . ?
C8 C7 C2 128.0(11) . . ?
C6 C7 C2 126.3(12) . . ?
N4 C8 C7 107.7(11) . . ?
N4 C8 C10 120.4(12) . . ?
C7 C8 C10 131.9(11) . . ?
N5 C11 C12 104.4(13) . . ?
N5 C11 C14 124.1(13) . . ?
C12 C11 C14 131.4(12) . . ?
C13 C12 C11 105.4(11) . . ?
C13 C12 C17 129.7(13) . . ?
C11 C12 C17 124.9(12) . . ?
N6 C13 C12 109.8(14) . . ?
N6 C13 C15 121.9(13) . . ?
C12 C13 C15 128.3(12) . . ?
N7 C16 C17 107.8(9) . . ?
N7 C16 C19 123.1(14) . . ?
C17 C16 C19 129.1(11) . . ?
C18 C17 C16 104.7(10) . . ?
C18 C17 C12 127.2(14) . . ?
C16 C17 C12 128.1(10) . . ?
N8 C18 C17 111.8(13) . . ?
N8 C18 C20 119.4(10) . . ?
C17 C18 C20 128.3(13) . . ?
N9 C21 C22 108.3(9) . . ?
N9 C21 C24 122.5(9) . . ?
C22 C21 C24 129.2(9) . . ?
C21 C22 C23 105.6(9) . . ?
C21 C22 C22 128.4(11) . 6_564 ?
C23 C22 C22 125.9(11) . 6_564 ?
N10 C23 C22 107.6(8) . . ?
N10 C23 C25 124.4(9) . . ?
C22 C23 C25 128.0(10) . . ?
N11 C26 C27 110.7(11) . . ?
N11 C26 C29 121.9(11) . . ?
C27 C26 C29 127.4(12) . . ?
C26 C27 C28 106.6(12) . . ?
C26 C27 C27 128.0(15) . 6_564 ?
C28 C27 C27 125.4(15) . 6_564 ?
N12 C28 C27 108.3(13) . . ?
N12 C28 C30 119.0(13) . . ?
C27 C28 C30 132.7(13) . . ?
C1 N1 N2 108.4(10) . . ?
C3 N2 N1 108.3(7) . . ?
C6 N3 N4 108.5(9) . . ?
N3 N4 C8 109.3(9) . . ?
N6 N5 C11 113.9(12) . . ?
N5 N6 C13 106.6(12) . . ?
C16 N7 N8 109.8(11) . . ?
C18 N8 N7 105.5(9) . . ?
C21 N9 N10 107.4(8) . . ?
C23 N10 N9 111.0(8) . . ?
C26 N11 N12 106.5(10) . . ?
C28 N12 N11 107.6(11) . . ?
Cl3 C31 Cl1 109.3(11) . . ?
Cl3 C31 Cl2B 78.6(13) . . ?
Cl1 C31 Cl2B 134.4(18) . . ?
Cl3 C31 Cl2 115.2(10) . . ?
Cl1 C31 Cl2 108.8(10) . . ?
Cl2B C31 Cl2 38.0(12) . . ?
Cl3 C31 Cl1B 128.9(18) . . ?
Cl1 C31 Cl1B 32.8(7) . . ?
Cl2B C31 Cl1B 107.0(14) . . ?
Cl2 C31 Cl1B 76.1(10) . . ?
Cl3 C31 Cl3B 33.1(7) . . ?
Cl1 C31 Cl3B 78.7(12) . . ?
Cl2B C31 Cl3B 109.1(14) . . ?
Cl2 C31 Cl3B 140.2(17) . . ?
Cl1B C31 Cl3B 106.0(14) . . ?
Cl1B Cl1 C31 76.6(14) . . ?
Cl1B Cl1 Cl3B 119.4(20) . . ?
C31 Cl1 Cl3B 51.8(7) . . ?
Cl2B Cl2 C31 70.2(12) . . ?
Cl2B Cl2 Cl1B 112.8(17) . . ?
C31 Cl2 Cl1B 52.0(7) . . ?
Cl3B Cl3 C31 77.7(14) . . ?
Cl3B Cl3 Cl2B 124.9(19) . . ?
C31 Cl3 Cl2B 51.8(9) . . ?
Cl1 Cl1B C31 70.5(13) . . ?
Cl1 Cl1B Cl2 122.1(16) . . ?
C31 Cl1B Cl2 51.9(8) . . ?
Cl2 Cl2B C31 71.8(13) . . ?
Cl2 Cl2B Cl3 119.6(13) . . ?
C31 Cl2B Cl3 49.6(7) . . ?
Cl3 Cl3B C31 69.2(13) . . ?
Cl3 Cl3B Cl1 115.3(16) . . ?
C31 Cl3B Cl1 49.5(8) . . ?
Cl6B C32 Cl4B 123.0(12) . . ?
Cl6B C32 Cl5 79.6(11) . . ?
Cl4B C32 Cl5 152.1(13) . . ?
Cl6B C32 Cl4 141.1(15) . . ?
Cl4B C32 Cl4 37.1(7) . . ?
Cl5 C32 Cl4 115.1(11) . . ?
Cl6B C32 Cl5B 114.5(12) . . ?
Cl4B C32 Cl5B 114.7(12) . . ?
Cl5 C32 Cl5B 37.8(6) . . ?
Cl4 C32 Cl5B 78.5(10) . . ?
Cl6B C32 Cl6 41.8(7) . . ?
Cl4B C32 Cl6 82.2(11) . . ?
Cl5 C32 Cl6 114.8(11) . . ?
Cl4 C32 Cl6 102.7(10) . . ?
Cl5B C32 Cl6 136.3(15) . . ?
Cl4B Cl4 C32 69.0(10) . . ?
Cl4B Cl4 Cl5B 119.8(13) . . ?
C32 Cl4 Cl5B 52.1(7) . . ?
Cl5B Cl5 C32 75.0(10) . . ?
Cl5B Cl5 Cl6B 120.2(12) . . ?
C32 Cl5 Cl6B 48.9(7) . . ?
Cl6B Cl6 C32 60.5(8) . . ?
Cl6B Cl6 Cl4B 105.4(10) . . ?
C32 Cl6 Cl4B 45.7(6) . . ?
Cl6 Cl6B C32 77.7(10) . . ?
Cl6 Cl6B Cl5 121.0(12) . . ?
C32 Cl6B Cl5 51.6(7) . . ?
Cl4 Cl4B C32 73.9(11) . . ?
Cl4 Cl4B Cl6 104.3(15) . . ?
C32 Cl4B Cl6 52.1(7) . . ?
Cl5 Cl5B C32 67.2(10) . . ?
Cl5 Cl5B Cl4 115.2(11) . . ?
C32 Cl5B Cl4 49.4(7) . . ?
Cl8A C33 Cl9A 121.6(11) . . ?
Cl8A C33 Cl9 147.8(12) . . ?
Cl9A C33 Cl9 39.1(8) . . ?
Cl8A C33 Cl7 86.4(11) . . ?
Cl9A C33 Cl7 151.0(10) . . ?
Cl9 C33 Cl7 112.9(9) . . ?
Cl8A C33 Cl7A 120.1(12) . . ?
Cl9A C33 Cl7A 115.1(9) . . ?
Cl9 C33 Cl7A 77.2(10) . . ?
Cl7 C33 Cl7A 35.9(8) . . ?
Cl8A C33 Cl8 38.1(8) . . ?
Cl9A C33 Cl8 91.9(12) . . ?
Cl9 C33 Cl8 109.7(9) . . ?
Cl7 C33 Cl8 109.4(9) . . ?
Cl7A C33 Cl8 128.5(16) . . ?
Cl7A Cl7 C33 72.3(8) . . ?
Cl7A Cl7 Cl8A 115.6(11) . . ?
C33 Cl7 Cl8A 45.8(6) . . ?
Cl8A Cl8 C33 66.1(7) . . ?
Cl9A Cl9 C33 69.8(8) . . ?
Cl9A Cl9 Cl7A 120.0(11) . . ?
C33 Cl9 Cl7A 51.6(5) . . ?
Cl7 Cl7A C33 71.8(8) . . ?
Cl7 Cl7A Cl9 122.6(10) . . ?
C33 Cl7A Cl9 51.2(6) . . ?
Cl8 Cl8A C33 75.9(8) . . ?
Cl8 Cl8A Cl7 106.3(15) . . ?
C33 Cl8A Cl7 47.7(6) . . ?
Cl9 Cl9A C33 71.0(7) . . ?

_refine_diff_density_max         0.330
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.051

#==============================================================================
data_c1214
_database_code_CSD               200496

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
3,3',5,5'-Tetramethyl-4,4'-Bipyrazole, Tetragonal form (#3)
;
_chemical_name_common            
"3,3',5,5'-Tetramethyl-4,4'-Bipyrazole, Tetragonal form ("
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C10 H14 N4'
_chemical_formula_weight         190.25
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)cd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'

_cell_length_a                   27.619(3)
_cell_length_b                   27.619(3)
_cell_length_c                   8.6029(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6562.5(13)
_cell_formula_units_Z            24
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            'slightly yellowish'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2448
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_T_max  0.8890

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'SMART CCD Siemens'
_diffrn_measurement_method       'omega scnans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19799
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         28.27
_reflns_number_total             3706
_reflns_number_observed          2645
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 746 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+1.1537P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3.04(230)
_refine_ls_number_reflns         2960
_refine_ls_number_parameters     208
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_obs          0.0461
_refine_ls_wR_factor_all         0.1256
_refine_ls_wR_factor_obs         0.1034
_refine_ls_goodness_of_fit_all   1.164
_refine_ls_goodness_of_fit_obs   1.189
_refine_ls_restrained_S_all      1.300
_refine_ls_restrained_S_obs      1.189
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N 0.15390(6) 0.14629(6) 0.3100(2) 0.0401(4) Uani 1 d . .
N2 N 0.15735(7) 0.09798(7) 0.2843(2) 0.0409(5) Uani 1 d . .
N3 N 0.28977(6) 0.11255(7) 0.8070(3) 0.0422(4) Uani 1 d . .
N4 N 0.31876(6) 0.09305(7) 0.6980(2) 0.0385(4) Uani 1 d . .
N5 N 0.44697(6) 0.09174(6) 0.8153(2) 0.0313(4) Uani 1 d . .
N6 N 0.41494(7) 0.06138(6) 0.7477(2) 0.0313(4) Uani 1 d . .
C1 C 0.18438(7) 0.15584(7) 0.4252(3) 0.0347(5) Uani 1 d . .
C2 C 0.20741(6) 0.11329(7) 0.4766(2) 0.0323(4) Uani 1 d . .
C3 C 0.18886(7) 0.07708(8) 0.3812(3) 0.0361(5) Uani 1 d . .
C4 C 0.19849(9) 0.02377(8) 0.3806(3) 0.0503(6) Uani 1 d . .
H4A H 0.2204(6) 0.01575(14) 0.4648(16) 0.080 Uiso 1 calc R .
H4B H 0.2130(7) 0.0146(2) 0.2823(10) 0.080 Uiso 1 calc R .
H4C H 0.16827(14) 0.00640(9) 0.3943(24) 0.080 Uiso 1 calc R .
C5 C 0.19110(9) 0.20643(8) 0.4830(3) 0.0471(6) Uani 1 d . .
H5A H 0.2248(2) 0.2115(2) 0.5099(22) 0.080 Uiso 1 calc R .
H5B H 0.1711(6) 0.2115(2) 0.5743(14) 0.080 Uiso 1 calc R .
H5C H 0.1817(7) 0.22914(8) 0.4025(9) 0.080 Uiso 1 calc R .
C6 C 0.24570(7) 0.12222(8) 0.7492(3) 0.0403(5) Uani 1 d . .
C7 C 0.24600(7) 0.10847(7) 0.5942(2) 0.0326(4) Uani 1 d . .
C8 C 0.29276(7) 0.09020(7) 0.5681(2) 0.0322(4) Uani 1 d . .
C9 C 0.31487(8) 0.07067(9) 0.4224(3) 0.0463(6) Uani 1 d . .
H9A H 0.2979(4) 0.0837(5) 0.3330(3) 0.080 Uiso 1 calc R .
H9B H 0.3123(6) 0.03564(10) 0.4220(10) 0.080 Uiso 1 calc R .
H9C H 0.3487(2) 0.0800(6) 0.4176(11) 0.080 Uiso 1 calc R .
C10 C 0.20613(10) 0.14266(13) 0.8478(4) 0.0653(8) Uani 1 d . .
H10A H 0.1763(2) 0.1439(7) 0.7883(8) 0.080 Uiso 1 calc R .
H10B H 0.2149(3) 0.1751(3) 0.8808(19) 0.080 Uiso 1 calc R .
H10C H 0.2015(5) 0.1223(4) 0.9385(12) 0.080 Uiso 1 calc R .
C11 C 0.48839(6) 0.06665(7) 0.8281(2) 0.0287(4) Uani 1 d . .
C12 C 0.48236(6) 0.01992(6) 0.7673(2) 0.0259(4) Uani 1 d . .
C13 C 0.43422(6) 0.01843(6) 0.7156(2) 0.0267(4) Uani 1 d . .
C14 C 0.40698(7) -0.02018(7) 0.6330(2) 0.0339(5) Uani 1 d . .
H14A H 0.4287(2) -0.0466(3) 0.6076(19) 0.080 Uiso 1 calc R .
H14B H 0.3932(6) -0.0071(2) 0.5382(11) 0.080 Uiso 1 calc R .
H14C H 0.3812(4) -0.0321(5) 0.6994(9) 0.080 Uiso 1 calc R .
C15 C 0.53198(8) 0.08860(8) 0.9025(3) 0.0377(5) Uani 1 d . .
H15A H 0.5465(4) 0.1119(5) 0.8320(10) 0.080 Uiso 1 calc R .
H15B H 0.5553(3) 0.06337(12) 0.9261(21) 0.080 Uiso 1 calc R .
H15C H 0.52254(14) 0.1048(6) 0.9978(12) 0.080 Uiso 1 calc R .
H1 H 0.1383(11) 0.0833(11) 0.2285(37) 0.055(8) Uiso 1 d . .
H2 H 0.3037(12) 0.1247(11) 0.8903(44) 0.068(9) Uiso 1 d . .
H3 H 0.3907(11) 0.0675(9) 0.7296(32) 0.041(7) Uiso 1 d . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0359(9) 0.0459(10) 0.0386(10) 0.0028(9) -0.0089(8) 0.0016(7)
N2 0.0367(9) 0.0431(10) 0.0429(11) -0.0026(9) -0.0136(9) -0.0054(8)
N3 0.0330(9) 0.0551(11) 0.0384(11) -0.0121(9) -0.0098(8) 0.0100(8)
N4 0.0307(8) 0.0445(10) 0.0403(10) -0.0057(8) -0.0075(8) 0.0084(7)
N5 0.0318(8) 0.0358(9) 0.0264(9) -0.0021(7) -0.0017(7) 0.0080(7)
N6 0.0260(8) 0.0391(9) 0.0289(9) -0.0009(7) -0.0031(7) 0.0103(7)
C1 0.0266(10) 0.0432(11) 0.0342(11) -0.0008(9) -0.0025(8) 0.0026(8)
C2 0.0231(8) 0.0438(11) 0.0300(11) -0.0030(9) -0.0009(8) -0.0005(7)
C3 0.0276(9) 0.0428(11) 0.0378(12) -0.0020(9) -0.0042(9) -0.0010(8)
C4 0.0488(12) 0.0417(12) 0.061(2) -0.0029(11) -0.0148(12) -0.0042(10)
C5 0.0434(12) 0.0450(12) 0.053(2) -0.0096(11) -0.0064(11) 0.0081(9)
C6 0.0321(10) 0.0535(12) 0.0352(12) -0.0058(10) -0.0063(9) 0.0095(9)
C7 0.0269(9) 0.0380(10) 0.0330(11) -0.0042(9) -0.0041(8) 0.0019(7)
C8 0.0285(9) 0.0337(9) 0.0344(11) -0.0027(8) -0.0042(8) 0.0007(7)
C9 0.0400(11) 0.0547(13) 0.0443(14) -0.0081(11) 0.0014(10) 0.0110(10)
C10 0.0480(14) 0.106(2) 0.0417(15) -0.011(2) -0.0012(12) 0.0290(14)
C11 0.0298(9) 0.0319(9) 0.0243(9) 0.0003(8) -0.0002(8) 0.0056(7)
C12 0.0251(8) 0.0319(9) 0.0207(8) 0.0023(8) 0.0008(7) 0.0031(6)
C13 0.0261(8) 0.0332(9) 0.0209(9) 0.0013(8) 0.0027(7) 0.0048(7)
C14 0.0326(10) 0.0388(10) 0.0305(11) -0.0014(9) -0.0006(9) 0.0004(8)
C15 0.0378(10) 0.0365(11) 0.0387(12) -0.0056(9) -0.0083(9) 0.0041(8)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.326(3) . ?
N1 N2 1.356(3) . ?
N2 C3 1.336(3) . ?
N3 C6 1.342(3) . ?
N3 N4 1.345(3) . ?
N4 C8 1.331(3) . ?
N5 C11 1.342(2) . ?
N5 N6 1.350(3) . ?
N6 C13 1.329(2) . ?
C1 C2 1.407(3) . ?
C1 C5 1.495(3) . ?
C2 C3 1.392(3) . ?
C2 C7 1.476(3) . ?
C3 C4 1.496(3) . ?
C6 C7 1.386(3) . ?
C6 C10 1.495(3) . ?
C7 C8 1.405(3) . ?
C8 C9 1.495(3) . ?
C11 C12 1.403(3) . ?
C11 C15 1.492(3) . ?
C12 C13 1.403(3) . ?
C12 C12 1.470(3) 10_544 ?
C13 C14 1.486(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 N2 105.8(2) . . ?
C3 N2 N1 111.7(2) . . ?
C6 N3 N4 111.2(2) . . ?
C8 N4 N3 106.7(2) . . ?
C11 N5 N6 105.9(2) . . ?
C13 N6 N5 112.4(2) . . ?
N1 C1 C2 110.8(2) . . ?
N1 C1 C5 120.9(2) . . ?
C2 C1 C5 128.3(2) . . ?
C3 C2 C1 104.4(2) . . ?
C3 C2 C7 127.3(2) . . ?
C1 C2 C7 128.1(2) . . ?
N2 C3 C2 107.3(2) . . ?
N2 C3 C4 122.6(2) . . ?
C2 C3 C4 130.1(2) . . ?
N3 C6 C7 107.3(2) . . ?
N3 C6 C10 121.9(2) . . ?
C7 C6 C10 130.8(2) . . ?
C6 C7 C8 104.9(2) . . ?
C6 C7 C2 129.1(2) . . ?
C8 C7 C2 125.9(2) . . ?
N4 C8 C7 109.9(2) . . ?
N4 C8 C9 120.4(2) . . ?
C7 C8 C9 129.7(2) . . ?
N5 C11 C12 110.1(2) . . ?
N5 C11 C15 120.9(2) . . ?
C12 C11 C15 129.0(2) . . ?
C13 C12 C11 104.95(14) . . ?
C13 C12 C12 127.3(2) . 10_544 ?
C11 C12 C12 127.6(2) . 10_544 ?
N6 C13 C12 106.7(2) . . ?
N6 C13 C14 122.5(2) . . ?
C12 C13 C14 130.7(2) . . ?

_refine_diff_density_max         0.161
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.028

#==============================================================================
data_pz
_database_code_CSD               200497

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
3,3',5,5'-Tetramethyl-4,4'-Bipyrazole, Methanol solvate
;
_chemical_name_common            
"3,3',5,5'-Tetramethyl-4,4'-Bipyrazole, Methanol solvate"
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C31 H46 N12 O'
_chemical_formula_weight         602.80
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   26.1826(13)
_cell_length_b                   9.6386(4)
_cell_length_c                   27.420(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6919.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2592
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'IPDS Stoe'
_diffrn_measurement_method       'phi rotation'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32494
_diffrn_reflns_av_R_equivalents  0.1321
_diffrn_reflns_av_sigmaI/netI    0.1588
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.90
_reflns_number_total             6692
_reflns_number_observed          2704
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 922 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00071(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5770
_refine_ls_number_parameters     403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_obs          0.0475
_refine_ls_wR_factor_all         0.1148
_refine_ls_wR_factor_obs         0.0956
_refine_ls_goodness_of_fit_all   0.772
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_restrained_S_all      0.763
_refine_ls_restrained_S_obs      1.041
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
C1 C -0.06061(12) 0.6975(3) 0.05168(10) 0.0370(8) Uani 1 d . .
C2 C -0.05268(11) 0.7782(3) 0.09296(10) 0.0293(7) Uani 1 d . .
C3 C -0.08701(11) 0.7265(3) 0.12772(10) 0.0310(7) Uani 1 d . .
C4 C -0.03550(15) 0.7048(4) 0.00300(11) 0.0640(12) Uani 1 d . .
H4A H -0.00540(15) 0.6479(4) 0.00348(11) 0.077 Uiso 1 d R .
H4B H -0.02598(15) 0.7986(4) -0.00437(11) 0.077 Uiso 1 d R .
H4C H -0.05808(15) 0.6720(4) -0.02206(11) 0.077 Uiso 1 d R .
C5 C -0.09453(13) 0.7693(3) 0.17944(10) 0.0453(9) Uani 1 d . .
H5A H -0.12716(13) 0.7384(3) 0.19113(10) 0.054 Uiso 1 d R .
H5B H -0.09239(13) 0.8686(3) 0.18127(10) 0.054 Uiso 1 d R .
H5C H -0.06769(13) 0.7314(3) 0.19922(10) 0.054 Uiso 1 d R .
C6 C 0.03573(11) 0.8787(3) 0.11454(10) 0.0332(7) Uani 1 d . .
C7 C -0.01562(11) 0.8916(3) 0.10085(9) 0.0298(7) Uani 1 d . .
C8 C -0.02492(11) 1.0332(3) 0.09926(10) 0.0341(8) Uani 1 d . .
C9 C 0.06716(12) 0.7510(4) 0.12009(13) 0.0537(10) Uani 1 d . .
H9A H 0.09271(12) 0.7642(4) 0.14477(13) 0.064 Uiso 1 d R .
H9B H 0.08316(12) 0.7299(4) 0.08947(13) 0.064 Uiso 1 d R .
H9C H 0.04549(12) 0.6745(4) 0.12871(13) 0.064 Uiso 1 d R .
C10 C -0.07217(11) 1.1107(4) 0.08638(13) 0.0542(10) Uani 1 d . .
H10A H -0.06502(11) 1.1724(4) 0.05978(13) 0.065 Uiso 1 d R .
H10B H -0.08395(11) 1.1634(4) 0.11388(13) 0.065 Uiso 1 d R .
H10C H -0.09865(11) 1.0472(4) 0.07694(13) 0.065 Uiso 1 d R .
C11 C 0.18170(11) 0.4910(3) 0.23848(9) 0.0305(7) Uani 1 d . .
C12 C 0.14710(11) 0.5834(3) 0.25910(9) 0.0280(7) Uani 1 d . .
C13 C 0.09966(11) 0.5452(3) 0.23988(9) 0.0317(7) Uani 1 d . .
C14 C 0.23833(11) 0.4805(4) 0.24485(10) 0.0425(9) Uani 1 d . .
H14A H 0.25513(11) 0.5032(4) 0.21477(10) 0.051 Uiso 1 d R .
H14B H 0.24718(11) 0.3878(4) 0.25450(10) 0.051 Uiso 1 d R .
H14C H 0.24932(11) 0.5429(4) 0.27005(10) 0.051 Uiso 1 d R .
C15 C 0.04791(12) 0.6016(4) 0.25236(11) 0.0464(9) Uani 1 d . .
H15A H 0.02168(12) 0.5377(4) 0.24262(11) 0.056 Uiso 1 d R .
H15B H 0.04368(12) 0.6888(4) 0.23597(11) 0.056 Uiso 1 d R .
H15C H 0.04611(12) 0.6187(4) 0.28681(11) 0.056 Uiso 1 d R .
C16 C 0.18004(11) 0.6759(3) 0.34147(9) 0.0309(7) Uani 1 d . .
C17 C 0.15751(11) 0.6926(3) 0.29543(9) 0.0284(7) Uani 1 d . .
C18 C 0.14402(11) 0.8321(3) 0.29319(9) 0.0317(7) Uani 1 d . .
C19 C 0.20163(13) 0.5490(3) 0.36532(10) 0.0424(9) Uani 1 d . .
H19A H 0.18085(13) 0.4703(3) 0.35712(10) 0.051 Uiso 1 d R .
H19B H 0.20240(13) 0.5608(3) 0.40008(10) 0.051 Uiso 1 d R .
H19C H 0.23597(13) 0.5340(3) 0.35425(10) 0.051 Uiso 1 d R .
C20 C 0.12061(13) 0.9132(3) 0.25247(10) 0.0421(8) Uani 1 d . .
H20A H 0.11652(13) 0.8570(3) 0.22382(10) 0.051 Uiso 1 d R .
H20B H 0.14230(13) 0.9912(3) 0.24581(10) 0.051 Uiso 1 d R .
H20C H 0.08822(13) 0.9486(3) 0.26318(10) 0.051 Uiso 1 d R .
C21 C 0.31851(11) 0.5681(3) 0.07454(9) 0.0253(7) Uani 1 d . .
C22 C 0.26939(10) 0.6213(3) 0.07627(9) 0.0254(7) Uani 1 d . .
C23 C 0.26504(10) 0.6845(3) 0.12241(9) 0.0246(6) Uani 1 d . .
C24 C 0.34498(11) 0.4853(3) 0.03593(10) 0.0363(8) Uani 1 d . .
H24A H 0.32167(11) 0.4621(3) 0.01016(10) 0.044 Uiso 1 d R .
H24B H 0.35855(11) 0.4021(3) 0.05017(10) 0.044 Uiso 1 d R .
H24C H 0.37298(11) 0.5383(3) 0.02313(10) 0.044 Uiso 1 d R .
C25 C 0.22064(11) 0.7617(4) 0.14275(10) 0.0387(8) Uani 1 d . .
H25A H 0.19493(11) 0.7757(4) 0.11828(10) 0.046 Uiso 1 d R .
H25B H 0.23262(11) 0.8491(4) 0.15501(10) 0.046 Uiso 1 d R .
H25C H 0.20696(11) 0.7104(4) 0.16978(10) 0.046 Uiso 1 d R .
C26 C 0.23634(11) 0.6737(3) -0.00957(9) 0.0281(7) Uani 1 d . .
C27 C 0.23100(10) 0.6179(3) 0.03701(9) 0.0241(7) Uani 1 d . .
C28 C 0.18271(11) 0.5560(3) 0.03760(9) 0.0258(7) Uani 1 d . .
C29 C 0.27896(12) 0.7561(3) -0.03152(10) 0.0393(8) Uani 1 d . .
H29A H 0.30791(12) 0.7571(3) -0.01004(10) 0.047 Uiso 1 d R .
H29B H 0.26728(12) 0.8490(3) -0.03741(10) 0.047 Uiso 1 d R .
H29C H 0.28817(12) 0.7161(3) -0.06235(10) 0.047 Uiso 1 d R .
C30 C 0.15733(11) 0.4723(3) 0.07663(9) 0.0341(8) Uani 1 d . .
H30A H 0.16073(11) 0.5185(3) 0.10747(9) 0.041 Uiso 1 d R .
H30B H 0.17263(11) 0.3819(3) 0.07831(9) 0.041 Uiso 1 d R .
H30C H 0.12184(11) 0.4608(3) 0.06879(9) 0.041 Uiso 1 d R .
C31 C -0.01225(13) 0.4265(4) 0.14309(13) 0.0547(10) Uani 1 d . .
H31A H -0.02927(13) 0.3625(4) 0.16444(13) 0.066 Uiso 1 d R .
H31B H -0.03152(13) 0.4383(4) 0.11359(13) 0.066 Uiso 1 d R .
H31C H -0.00923(13) 0.5157(4) 0.15843(13) 0.066 Uiso 1 d R .
N1 N -0.09683(10) 0.6031(3) 0.06169(8) 0.0421(7) Uani 1 d . .
H1A H -0.10828(10) 0.5382(3) 0.04078(8) 0.051 Uiso 0.50 d PR .
N2 N -0.11333(9) 0.6213(3) 0.10835(8) 0.0386(7) Uani 1 d . .
H2A H -0.13775(9) 0.5717(3) 0.12348(8) 0.046 Uiso 0.50 d PR .
N3 N 0.05632(9) 1.0048(3) 0.12222(8) 0.0355(6) Uani 1 d . .
N4 N 0.01856(9) 1.0968(3) 0.11248(8) 0.0366(6) Uani 1 d . .
H4D H 0.02217(9) 1.1894(3) 0.11464(8) 0.044 Uiso 1 d R .
N5 N 0.15481(9) 0.4066(3) 0.20891(7) 0.0325(6) Uani 1 d . .
H5D H 0.16872(9) 0.3378(3) 0.19113(7) 0.039 Uiso 1 d R .
N6 N 0.10435(9) 0.4379(3) 0.20907(8) 0.0333(6) Uani 1 d . .
N7 N 0.17979(9) 0.7970(3) 0.36487(8) 0.0321(6) Uani 1 d . .
H7A H 0.19216(9) 0.8122(3) 0.39502(8) 0.038 Uiso 0.50 d PR .
N8 N 0.15761(9) 0.8935(3) 0.33550(8) 0.0338(6) Uani 1 d . .
H8A H 0.15280(9) 0.9835(3) 0.34291(8) 0.041 Uiso 0.50 d PR .
N9 N 0.34114(8) 0.5998(3) 0.11736(7) 0.0268(6) Uani 1 d . .
N10 N 0.30898(9) 0.6711(2) 0.14758(7) 0.0275(6) Uani 1 d . .
N11 N 0.19331(9) 0.6483(3) -0.03448(8) 0.0325(6) Uani 1 d . .
H11A H 0.18736(9) 0.6751(3) -0.06541(8) 0.039 Uiso 0.50 d PR .
N12 N 0.16022(9) 0.5765(3) -0.00582(7) 0.0320(6) Uani 1 d . .
H12A H 0.12881(9) 0.5476(3) -0.01444(7) 0.038 Uiso 0.50 d PR .
O1A O 0.03712(9) 0.3749(3) 0.13201(12) 0.0383(12) Uani 0.904(10) d P .
O1B O 0.0274(9) 0.3379(28) 0.1623(12) 0.044(10) Uiso 0.096(10) d P .
H1 H 0.3770 0.5813 0.1292 0.053 Uiso 1 d . .
H2 H 0.0628 0.4213 0.1577 0.053 Uiso 1 d . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.035(2) 0.043(2) 0.033(2) 0.000(2) -0.0040(14) -0.014(2)
C2 0.026(2) 0.027(2) 0.036(2) 0.0012(14) -0.0005(14) -0.0050(15)
C3 0.030(2) 0.029(2) 0.034(2) -0.0012(14) -0.0031(14) -0.003(2)
C4 0.078(3) 0.073(3) 0.041(2) -0.009(2) 0.010(2) -0.030(2)
C5 0.054(2) 0.037(2) 0.044(2) -0.002(2) 0.012(2) -0.004(2)
C6 0.028(2) 0.029(2) 0.042(2) 0.0039(15) -0.0006(14) -0.006(2)
C7 0.028(2) 0.031(2) 0.0303(15) -0.0013(14) -0.0004(12) -0.004(2)
C8 0.024(2) 0.036(2) 0.042(2) -0.0078(15) 0.0003(14) -0.004(2)
C9 0.036(2) 0.038(2) 0.087(3) 0.005(2) -0.009(2) -0.001(2)
C10 0.032(2) 0.043(2) 0.088(3) -0.010(2) -0.006(2) 0.000(2)
C11 0.034(2) 0.033(2) 0.0243(14) -0.0022(13) 0.0009(13) 0.000(2)
C12 0.036(2) 0.029(2) 0.0196(13) -0.0028(13) 0.0003(13) 0.0029(15)
C13 0.035(2) 0.032(2) 0.0284(15) -0.0021(14) -0.0017(14) 0.005(2)
C14 0.036(2) 0.049(2) 0.043(2) -0.014(2) 0.003(2) 0.003(2)
C15 0.039(2) 0.055(3) 0.045(2) -0.019(2) -0.010(2) 0.012(2)
C16 0.031(2) 0.032(2) 0.0300(14) -0.0061(14) -0.0009(13) 0.003(2)
C17 0.028(2) 0.031(2) 0.0261(14) -0.0035(13) 0.0021(13) 0.005(2)
C18 0.036(2) 0.035(2) 0.0239(15) -0.0041(14) 0.0018(13) 0.002(2)
C19 0.053(2) 0.036(2) 0.038(2) -0.005(2) -0.007(2) 0.010(2)
C20 0.057(2) 0.031(2) 0.038(2) -0.005(2) -0.004(2) 0.005(2)
C21 0.024(2) 0.024(2) 0.0276(15) -0.0003(12) -0.0005(12) -0.0028(14)
C22 0.025(2) 0.026(2) 0.0252(14) 0.0022(12) -0.0013(12) -0.0020(15)
C23 0.023(2) 0.023(2) 0.0280(14) -0.0006(13) -0.0011(13) -0.0011(13)
C24 0.036(2) 0.039(2) 0.034(2) -0.0044(15) 0.0022(14) 0.004(2)
C25 0.032(2) 0.052(2) 0.032(2) -0.012(2) -0.0030(14) 0.005(2)
C26 0.032(2) 0.025(2) 0.0271(14) -0.0013(13) -0.0048(13) -0.0049(15)
C27 0.026(2) 0.022(2) 0.0245(14) -0.0032(13) -0.0022(12) -0.0002(14)
C28 0.033(2) 0.023(2) 0.0215(14) -0.0006(12) -0.0045(13) -0.0012(15)
C29 0.043(2) 0.043(2) 0.032(2) 0.007(2) -0.0029(14) -0.009(2)
C30 0.033(2) 0.034(2) 0.035(2) 0.0036(14) 0.0004(14) -0.001(2)
C31 0.049(2) 0.038(2) 0.077(2) -0.009(2) -0.011(2) 0.002(2)
N1 0.045(2) 0.047(2) 0.0346(14) 0.0025(13) -0.0072(12) -0.020(2)
N2 0.041(2) 0.037(2) 0.0382(14) 0.0065(12) -0.0044(12) -0.0110(14)
N3 0.0262(14) 0.033(2) 0.0476(15) -0.0023(13) 0.0008(12) -0.0035(14)
N4 0.0297(14) 0.030(2) 0.050(2) -0.0080(13) 0.0022(12) -0.0047(14)
N5 0.037(2) 0.033(2) 0.0280(12) -0.0085(11) 0.0022(11) 0.0045(14)
N6 0.033(2) 0.035(2) 0.0319(13) -0.0058(12) 0.0006(11) 0.0068(13)
N7 0.0326(14) 0.034(2) 0.0297(12) -0.0065(12) -0.0054(11) 0.0060(13)
N8 0.0384(15) 0.029(2) 0.0339(13) -0.0052(12) -0.0050(12) 0.0060(14)
N9 0.0237(12) 0.029(2) 0.0275(12) -0.0020(11) -0.0027(10) 0.0032(12)
N10 0.0267(14) 0.028(2) 0.0279(12) -0.0045(11) -0.0002(11) 0.0026(12)
N11 0.036(2) 0.029(2) 0.0329(13) 0.0062(11) -0.0084(11) -0.0077(12)
N12 0.0360(15) 0.027(2) 0.0329(13) 0.0021(11) -0.0077(12) -0.0081(13)
O1A 0.031(2) 0.035(2) 0.048(2) -0.0097(14) -0.0081(12) -0.0004(12)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.342(4) . ?
C1 C2 1.389(4) . ?
C1 C4 1.490(4) . ?
C2 C3 1.402(4) . ?
C2 C7 1.478(4) . ?
C3 N2 1.336(4) . ?
C3 C5 1.490(4) . ?
C6 N3 1.346(4) . ?
C6 C7 1.401(4) . ?
C6 C9 1.489(4) . ?
C7 C8 1.387(4) . ?
C8 N4 1.343(3) . ?
C8 C10 1.487(4) . ?
C11 N5 1.347(3) . ?
C11 C12 1.390(4) . ?
C11 C14 1.496(4) . ?
C12 C13 1.398(4) . ?
C12 C17 1.475(4) . ?
C13 N6 1.342(3) . ?
C13 C15 1.499(4) . ?
C16 N7 1.332(3) . ?
C16 C17 1.403(4) . ?
C16 C19 1.498(4) . ?
C17 C18 1.392(4) . ?
C18 N8 1.350(3) . ?
C18 C20 1.494(4) . ?
C21 N9 1.350(3) . ?
C21 C22 1.385(4) . ?
C21 C24 1.496(4) . ?
C22 C23 1.409(3) . ?
C22 C27 1.473(3) . ?
C23 N10 1.348(3) . ?
C23 C25 1.488(4) . ?
C26 N11 1.340(3) . ?
C26 C27 1.393(3) . ?
C26 C29 1.496(4) . ?
C27 C28 1.398(4) . ?
C28 N12 1.343(3) . ?
C28 C30 1.496(4) . ?
C31 O1A 1.418(4) . ?
C31 O1B 1.44(3) . ?
N1 N2 1.362(3) . ?
N3 N4 1.355(3) . ?
N5 N6 1.355(3) . ?
N7 N8 1.361(3) . ?
N9 N10 1.367(3) . ?
N11 N12 1.359(3) . ?
O1A O1B 0.94(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 108.6(2) . . ?
N1 C1 C4 121.8(3) . . ?
C2 C1 C4 129.6(3) . . ?
C1 C2 C3 105.0(3) . . ?
C1 C2 C7 129.2(3) . . ?
C3 C2 C7 125.8(2) . . ?
N2 C3 C2 109.3(2) . . ?
N2 C3 C5 121.4(3) . . ?
C2 C3 C5 129.3(3) . . ?
N3 C6 C7 110.2(3) . . ?
N3 C6 C9 120.6(3) . . ?
C7 C6 C9 129.1(3) . . ?
C8 C7 C6 105.3(3) . . ?
C8 C7 C2 127.5(3) . . ?
C6 C7 C2 127.1(3) . . ?
N4 C8 C7 107.0(3) . . ?
N4 C8 C10 122.7(3) . . ?
C7 C8 C10 130.3(3) . . ?
N5 C11 C12 106.9(3) . . ?
N5 C11 C14 123.2(3) . . ?
C12 C11 C14 129.9(3) . . ?
C11 C12 C13 104.9(2) . . ?
C11 C12 C17 127.7(3) . . ?
C13 C12 C17 127.3(3) . . ?
N6 C13 C12 111.0(3) . . ?
N6 C13 C15 120.4(3) . . ?
C12 C13 C15 128.4(3) . . ?
N7 C16 C17 109.3(3) . . ?
N7 C16 C19 120.5(2) . . ?
C17 C16 C19 130.2(3) . . ?
C18 C17 C16 104.9(2) . . ?
C18 C17 C12 127.8(3) . . ?
C16 C17 C12 127.1(3) . . ?
N8 C18 C17 108.6(3) . . ?
N8 C18 C20 121.4(3) . . ?
C17 C18 C20 130.0(3) . . ?
N9 C21 C22 107.1(2) . . ?
N9 C21 C24 122.2(2) . . ?
C22 C21 C24 130.7(2) . . ?
C21 C22 C23 105.4(2) . . ?
C21 C22 C27 126.9(2) . . ?
C23 C22 C27 127.6(2) . . ?
N10 C23 C22 110.4(2) . . ?
N10 C23 C25 121.5(2) . . ?
C22 C23 C25 128.0(2) . . ?
N11 C26 C27 108.2(2) . . ?
N11 C26 C29 121.3(2) . . ?
C27 C26 C29 130.4(2) . . ?
C26 C27 C28 105.4(2) . . ?
C26 C27 C22 126.4(2) . . ?
C28 C27 C22 128.2(2) . . ?
N12 C28 C27 108.9(2) . . ?
N12 C28 C30 121.2(2) . . ?
C27 C28 C30 129.8(2) . . ?
O1A C31 O1B 38.3(13) . . ?
C1 N1 N2 109.2(2) . . ?
C3 N2 N1 107.9(2) . . ?
C6 N3 N4 105.5(2) . . ?
C8 N4 N3 111.9(3) . . ?
C11 N5 N6 111.9(2) . . ?
C13 N6 N5 105.3(2) . . ?
C16 N7 N8 108.4(2) . . ?
C18 N8 N7 108.8(2) . . ?
C21 N9 N10 111.8(2) . . ?
C23 N10 N9 105.3(2) . . ?
C26 N11 N12 109.5(2) . . ?
C28 N12 N11 107.9(2) . . ?
O1B O1A C31 72.4(15) . . ?
O1A O1B C31 69.3(18) . . ?

_refine_diff_density_max         0.268
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.043

#==============================================================================