# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2004

data_global

_publ_contact_author_email       YOHISHI@MWU.MUKOGAWA-U.AC.JP

_publ_contact_author_name        'Prof Yoshitaka Ohishi'
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177
_publ_contact_author_address     
;
Faculty of Pharmaceutical Sciences
Mukogawa Women's University
11-68, Koshien Kyuban-cho Nishinomi
Nishinomiya Hyogo Pref.
663-8179
JAPAN
;

_publ_section_title              
;
Syntheses of 3-acetoacetylaminobenzo[b]furan
derivatives having cysteinyl leukotriene 2 receptor antagonistic
activity
;

_publ_section_references         
;
ENTER OTHER REFERENCES
Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan.
Single Crystal Structure Analysis Software. Version 1.11.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.
Rigaku, 3-9-12 Akishima, Tokyo, Japan.
North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968).
Acta Cryst. A24, 351-359.
Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564.
;

loop_
_publ_author_name
'Yoshitaka Ohishi'
'Kumiko Ando'
'Yuko Ando'
'Shigekatsu Kohno'
'Jun-ichi Kunitomo'
'Noriko Kuwata'
'Shunsaku Ohta'
;
E.Tsuji
;
'Masayuki Yamashita'

#------------------------------------------------------------------------------
data_master_file_afc7*.xtl
_database_code_depnum_ccdc_archive 'CCDC 214287'
#------------------------------------------------------------------------------
# CHEMICAL DATA
_chemical_formula_sum            'C29 H26 N4 O5 '
_chemical_formula_moiety         'C29 H26 N4 O5 '
_chemical_formula_weight         510.55
_chemical_melting_point          ?
#------------------------------------------------------------------------------
# CRYSTAL DATA
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
_cell_length_a                   17.709(3)
_cell_length_b                   7.553(2)
_cell_length_c                   19.656(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.926(8)
_cell_angle_gamma                90
_cell_volume                     2581.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      29.1
_cell_measurement_theta_max      29.9
_cell_measurement_temperature    296.2
#------------------------------------------------------------------------------
_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_exptl_crystal_size_rad          ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_absorpt_coefficient_mu    0.765(mm-1)
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  0.999
#------------------------------------------------------------------------------
# EXPERIMENTAL DATA
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_reflns_number            5184
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_theta_max         67.57
_diffrn_measured_fraction_theta_max 0.9955
_diffrn_reflns_theta_full        67.57
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_decay_%        0.51
#------------------------------------------------------------------------------
# REFINEMENT DATA
_refine_special_details          
;
Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted
R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are
based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only
for calculating R-factor (gt).
;
_reflns_number_total             4619
_reflns_number_gt                2515
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1703
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_reflns         4619
_refine_ls_number_parameters     344
_refine_ls_goodness_of_fit_ref   1.491
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_shift/su_max          0.0006
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_extinction_coef       0.016(3)
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.031 0.018
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.049 0.032
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
#------------------------------------------------------------------------------
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O(1) O 0.5113(1) 0.2225(3) 0.42472(9) 0.0544(6) Uani 1.00 d . . .
O(2) O 0.4731(1) 0.3295(3) 0.5911(1) 0.0628(7) Uani 1.00 d . . .
O(3) O 0.2360(1) 0.3684(4) 0.4206(1) 0.0746(8) Uani 1.00 d . . .
O(4) O 0.1150(1) 0.4337(4) 0.4667(1) 0.093(1) Uani 1.00 d . . .
O(5) O 0.1555(2) 0.4230(5) 0.0741(1) 0.101(1) Uani 1.00 d . . .
N(1) N 0.8626(2) -0.0628(6) 0.6955(2) 0.108(1) Uani 1.00 d . . .
N(2) N 0.3524(1) 0.4034(4) 0.4910(1) 0.0510(8) Uani 1.00 d . . .
N(3) N 0.3238(2) 0.5819(5) 0.6454(2) 0.088(1) Uani 1.00 d . . .
N(4) N 0.0865(2) 0.4754(6) 0.1540(2) 0.092(1) Uani 1.00 d . . .
C(1) C 0.4735(2) 0.2760(4) 0.4768(1) 0.0476(9) Uani 1.00 d . . .
C(2) C 0.4012(2) 0.3362(4) 0.4489(1) 0.0448(8) Uani 1.00 d . . .
C(3) C 0.3921(2) 0.3243(4) 0.3747(1) 0.0466(9) Uani 1.00 d . . .
C(4) C 0.3363(2) 0.3703(4) 0.3175(1) 0.0474(9) Uani 1.00 d . . .
C(5) C 0.3498(2) 0.3399(4) 0.2513(1) 0.0501(9) Uani 1.00 d . . .
C(6) C 0.4206(2) 0.2647(5) 0.2434(2) 0.061(1) Uani 1.00 d . . .
C(7) C 0.4768(2) 0.2208(5) 0.2988(1) 0.061(1) Uani 1.00 d . . .
C(8) C 0.4609(2) 0.2536(5) 0.3640(1) 0.0508(9) Uani 1.00 d . . .
C(9) C 0.5098(2) 0.2686(4) 0.5493(1) 0.0481(9) Uani 1.00 d . . .
C(10) C 0.5882(2) 0.1934(4) 0.5756(1) 0.0497(9) Uani 1.00 d . . .
C(11) C 0.6093(2) 0.1787(5) 0.6474(2) 0.062(1) Uani 1.00 d . . .
C(12) C 0.6803(2) 0.1121(5) 0.6772(2) 0.068(1) Uani 1.00 d . . .
C(13) C 0.7313(2) 0.0632(5) 0.6366(2) 0.059(1) Uani 1.00 d . . .
C(14) C 0.7117(2) 0.0776(5) 0.5647(2) 0.064(1) Uani 1.00 d . . .
C(15) C 0.6402(2) 0.1430(5) 0.5347(2) 0.059(1) Uani 1.00 d . . .
C(16) C 0.8049(2) -0.0090(6) 0.6683(2) 0.074(1) Uani 1.00 d . . .
C(17) C 0.2748(2) 0.4147(5) 0.4768(2) 0.0539(10) Uani 1.00 d . . .
C(18) C 0.2388(2) 0.4815(5) 0.5319(2) 0.057(1) Uani 1.00 d . . .
C(19) C 0.2844(2) 0.5376(5) 0.5957(2) 0.063(1) Uani 1.00 d . . .
C(20) C 0.1601(2) 0.4840(6) 0.5245(2) 0.072(1) Uani 1.00 d . . .
C(21) C 0.1191(3) 0.5438(7) 0.5795(2) 0.099(2) Uani 1.00 d . . .
C(22) C 0.2914(2) 0.3893(5) 0.1891(1) 0.0518(9) Uani 1.00 d . . .
C(23) C 0.3217(2) 0.4564(5) 0.1277(2) 0.068(1) Uani 1.00 d . . .
C(24) C 0.2171(2) 0.3750(5) 0.1909(2) 0.061(1) Uani 1.00 d . . .
C(25) C 0.1522(2) 0.4270(6) 0.1348(2) 0.068(1) Uani 1.00 d . . .
C(26) C 0.0192(2) 0.5242(7) 0.1028(2) 0.095(2) Uani 1.00 d . . .
C(27) C -0.0320(3) 0.3717(8) 0.0803(3) 0.112(2) Uani 1.00 d . . .
C(28) C 0.0695(4) 0.460(1) 0.2320(6) 0.209(4) Uani 1.00 d . . .
C(29) C 0.1012(4) 0.611(1) 0.2515(4) 0.171(4) Uani 1.00 d . . .
H(1) H 0.2893 0.4223 0.3239 0.0568 Uiso 1.00 calc . . .
H(2) H 0.4295 0.2436 0.1979 0.0730 Uiso 1.00 calc . . .
H(3) H 0.5243 0.1705 0.2929 0.0733 Uiso 1.00 calc . . .
H(4) H 0.5744 0.2147 0.6760 0.0744 Uiso 1.00 calc . . .
H(5) H 0.6938 0.1004 0.7261 0.0820 Uiso 1.00 calc . . .
H(6) H 0.7472 0.0427 0.5366 0.0764 Uiso 1.00 calc . . .
H(7) H 0.6266 0.1535 0.4858 0.0709 Uiso 1.00 calc . . .
H(8) H 0.3823 0.4189 0.5346 0.0954 Uiso 1.00 calc . . .
H(9) H 0.1555 0.5791 0.6191 0.1185 Uiso 1.00 calc . . .
H(10) H 0.0887 0.4494 0.5916 0.1185 Uiso 1.00 calc . . .
H(11) H 0.0868 0.6411 0.5630 0.1185 Uiso 1.00 calc . . .
H(12) H 0.1517 0.3630 0.4467 0.0380 Uiso 1.00 calc . . .
H(13) H 0.3763 0.4549 0.1379 0.0816 Uiso 1.00 calc . . .
H(14) H 0.3042 0.5740 0.1176 0.0816 Uiso 1.00 calc . . .
H(15) H 0.3038 0.3826 0.0889 0.0816 Uiso 1.00 calc . . .
H(16) H 0.2041 0.3269 0.2319 0.0733 Uiso 1.00 calc . . .
H(17) H 0.0358 0.5723 0.0635 0.1136 Uiso 1.00 calc . . .
H(18) H -0.0090 0.6112 0.1224 0.1136 Uiso 1.00 calc . . .
H(19) H -0.0045 0.2840 0.0603 0.1347 Uiso 1.00 calc . . .
H(20) H -0.0749 0.4101 0.0469 0.1347 Uiso 1.00 calc . . .
H(21) H -0.0494 0.3232 0.1192 0.1347 Uiso 1.00 calc . . .
H(22) H 0.0948 0.3622 0.2571 0.2512 Uiso 1.00 calc . . .
H(23) H 0.0162 0.4556 0.2334 0.2512 Uiso 1.00 calc . . .
H(24) H 0.0770 0.7021 0.2216 0.2048 Uiso 1.00 calc . . .
H(25) H 0.1543 0.6072 0.2495 0.2048 Uiso 1.00 calc . . .
H(26) H 0.0954 0.6358 0.2976 0.2048 Uiso 1.00 calc . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O(1) 0.046(1) 0.083(2) 0.033(1) 0.006(1) 0.0062(8) -0.002(1)
O(2) 0.061(1) 0.092(2) 0.037(1) 0.001(1) 0.0122(10) -0.002(1)
O(3) 0.054(1) 0.120(2) 0.049(1) 0.000(1) 0.007(1) -0.017(1)
O(4) 0.060(2) 0.132(3) 0.087(2) 0.022(2) 0.013(1) -0.008(2)
O(5) 0.081(2) 0.166(3) 0.049(2) 0.023(2) -0.005(1) 0.007(2)
N(1) 0.070(2) 0.118(3) 0.124(3) -0.001(2) -0.014(2) 0.038(3)
N(2) 0.050(2) 0.064(2) 0.039(1) 0.001(1) 0.008(1) -0.004(1)
N(3) 0.109(3) 0.100(3) 0.055(2) -0.001(2) 0.016(2) -0.014(2)
N(4) 0.064(2) 0.152(4) 0.058(2) 0.016(2) 0.008(2) 0.030(2)
C(1) 0.050(2) 0.061(2) 0.032(1) -0.005(2) 0.008(1) -0.001(1)
C(2) 0.049(2) 0.054(2) 0.031(1) -0.006(1) 0.009(1) -0.003(1)
C(3) 0.045(2) 0.059(2) 0.036(1) -0.005(2) 0.007(1) -0.001(1)
C(4) 0.047(2) 0.054(2) 0.041(2) -0.002(2) 0.008(1) -0.002(1)
C(5) 0.051(2) 0.061(2) 0.038(2) -0.002(2) 0.006(1) -0.003(1)
C(6) 0.056(2) 0.088(3) 0.038(2) 0.004(2) 0.010(1) -0.001(2)
C(7) 0.049(2) 0.096(3) 0.039(2) 0.014(2) 0.010(1) -0.006(2)
C(8) 0.046(2) 0.073(2) 0.032(1) 0.000(2) 0.004(1) 0.000(1)
C(9) 0.050(2) 0.056(2) 0.039(2) -0.012(2) 0.010(1) 0.002(1)
C(10) 0.051(2) 0.056(2) 0.040(2) -0.009(2) 0.003(1) 0.002(1)
C(11) 0.064(2) 0.082(3) 0.039(2) -0.005(2) 0.006(2) 0.002(2)
C(12) 0.068(2) 0.089(3) 0.042(2) -0.005(2) -0.005(2) 0.008(2)
C(13) 0.053(2) 0.065(2) 0.056(2) -0.008(2) -0.002(2) 0.011(2)
C(14) 0.058(2) 0.078(3) 0.053(2) 0.004(2) 0.005(2) 0.001(2)
C(15) 0.059(2) 0.078(3) 0.040(2) 0.005(2) 0.008(1) 0.003(2)
C(16) 0.064(2) 0.080(3) 0.072(2) -0.008(2) -0.004(2) 0.016(2)
C(17) 0.054(2) 0.064(2) 0.044(2) 0.001(2) 0.010(1) -0.002(2)
C(18) 0.066(2) 0.064(2) 0.044(2) 0.008(2) 0.017(2) 0.004(2)
C(19) 0.079(2) 0.066(2) 0.048(2) 0.007(2) 0.026(2) -0.002(2)
C(20) 0.068(2) 0.079(3) 0.072(2) 0.015(2) 0.019(2) 0.005(2)
C(21) 0.087(3) 0.117(4) 0.102(3) 0.028(3) 0.041(3) -0.002(3)
C(22) 0.056(2) 0.058(2) 0.039(2) -0.002(2) 0.003(1) 0.000(1)
C(23) 0.066(2) 0.086(3) 0.050(2) 0.000(2) 0.006(2) 0.013(2)
C(24) 0.057(2) 0.081(3) 0.044(2) 0.002(2) 0.005(1) 0.010(2)
C(25) 0.058(2) 0.086(3) 0.053(2) 0.001(2) -0.001(2) 0.008(2)
C(26) 0.061(2) 0.124(4) 0.091(3) 0.002(3) -0.005(2) 0.030(3)
C(27) 0.095(3) 0.134(5) 0.103(4) -0.011(3) 0.007(3) 0.016(3)
C(28) 0.081(4) 0.133(6) 0.37(1) -0.003(4) -0.057(6) 0.077(8)
C(29) 0.125(6) 0.153(7) 0.233(9) 0.036(5) 0.030(6) -0.024(6)
#------------------------------------------------------------------------------
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_structure_solution    SAPI91
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_molecular_graphics    ?
#------------------------------------------------------------------------------
_geom_special_details            
;
?
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O(1) C(1) 1.386(3) . . yes
O(1) C(8) 1.368(3) . . yes
O(2) C(9) 1.230(3) . . yes
O(3) C(17) 1.236(4) . . yes
O(4) C(20) 1.315(4) . . yes
O(4) H(12) 0.980 . . no
O(5) C(25) 1.206(4) . . yes
N(1) C(16) 1.134(4) . . yes
N(2) C(2) 1.400(4) . . yes
N(2) C(17) 1.352(4) . . yes
N(2) H(8) 0.927 . . no
N(3) C(19) 1.139(4) . . yes
N(4) C(25) 1.340(5) . . yes
N(4) C(26) 1.453(5) . . yes
N(4) C(28) 1.62(1) . . yes
C(1) C(2) 1.371(4) . . yes
C(1) C(9) 1.450(4) . . yes
C(2) C(3) 1.440(4) . . yes
C(3) C(4) 1.392(4) . . yes
C(3) C(8) 1.384(4) . . yes
C(4) C(5) 1.387(4) . . yes
C(4) H(1) 0.950 . . no
C(5) C(6) 1.411(4) . . yes
C(5) C(22) 1.492(4) . . yes
C(6) C(7) 1.371(4) . . yes
C(6) H(2) 0.950 . . no
C(7) C(8) 1.384(4) . . yes
C(7) H(3) 0.950 . . no
C(9) C(10) 1.498(4) . . yes
C(10) C(11) 1.394(4) . . yes
C(10) C(15) 1.385(4) . . yes
C(11) C(12) 1.378(5) . . yes
C(11) H(4) 0.950 . . no
C(12) C(13) 1.365(5) . . yes
C(12) H(5) 0.950 . . no
C(13) C(14) 1.394(4) . . yes
C(13) C(16) 1.441(5) . . yes
C(14) C(15) 1.383(4) . . yes
C(14) H(6) 0.950 . . no
C(15) H(7) 0.950 . . no
C(17) C(18) 1.448(4) . . yes
C(18) C(19) 1.421(5) . . yes
C(18) C(20) 1.373(5) . . yes
C(20) C(21) 1.482(5) . . yes
C(21) H(9) 0.950 . . no
C(21) H(10) 0.950 . . no
C(21) H(11) 0.950 . . no
C(22) C(23) 1.499(4) . . yes
C(22) C(24) 1.328(4) . . yes
C(23) H(13) 0.950 . . no
C(23) H(14) 0.950 . . no
C(23) H(15) 0.950 . . no
C(24) C(25) 1.487(4) . . yes
C(24) H(16) 0.950 . . no
C(26) C(27) 1.481(7) . . yes
C(26) H(17) 0.950 . . no
C(26) H(18) 0.950 . . no
C(27) H(19) 0.950 . . no
C(27) H(20) 0.950 . . no
C(27) H(21) 0.950 . . no
C(28) C(29) 1.302(9) . . yes
C(28) H(22) 0.950 . . no
C(28) H(23) 0.950 . . no
C(29) H(24) 0.950 . . no
C(29) H(25) 0.950 . . no
C(29) H(26) 0.950 . . no
#------------------------------------------------------------------------------
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(1) O(1) C(8) 105.5(2) . . . yes
C(20) O(4) H(12) 99.4 . . . no
C(2) N(2) C(17) 128.2(2) . . . yes
C(2) N(2) H(8) 106.5 . . . no
C(17) N(2) H(8) 124.2 . . . no
C(25) N(4) C(26) 121.1(3) . . . yes
C(25) N(4) C(28) 124.9(4) . . . yes
C(26) N(4) C(28) 113.5(4) . . . yes
O(1) C(1) C(2) 110.3(2) . . . yes
O(1) C(1) C(9) 121.9(3) . . . yes
C(2) C(1) C(9) 127.8(3) . . . yes
N(2) C(2) C(1) 121.2(2) . . . yes
N(2) C(2) C(3) 131.1(3) . . . yes
C(1) C(2) C(3) 107.5(2) . . . yes
C(2) C(3) C(4) 136.8(3) . . . yes
C(2) C(3) C(8) 104.2(2) . . . yes
C(4) C(3) C(8) 119.0(3) . . . yes
C(3) C(4) C(5) 119.6(3) . . . yes
C(3) C(4) H(1) 120.2 . . . no
C(5) C(4) H(1) 120.2 . . . no
C(4) C(5) C(6) 119.1(3) . . . yes
C(4) C(5) C(22) 120.8(3) . . . yes
C(6) C(5) C(22) 120.2(3) . . . yes
C(5) C(6) C(7) 122.4(3) . . . yes
C(5) C(6) H(2) 118.8 . . . no
C(7) C(6) H(2) 118.8 . . . no
C(6) C(7) C(8) 116.6(3) . . . yes
C(6) C(7) H(3) 121.7 . . . no
C(8) C(7) H(3) 121.7 . . . no
O(1) C(8) C(3) 112.4(2) . . . yes
O(1) C(8) C(7) 124.3(3) . . . yes
C(3) C(8) C(7) 123.3(3) . . . yes
O(2) C(9) C(1) 116.8(3) . . . yes
O(2) C(9) C(10) 118.9(3) . . . yes
C(1) C(9) C(10) 124.3(3) . . . yes
C(9) C(10) C(11) 115.7(3) . . . yes
C(9) C(10) C(15) 125.3(3) . . . yes
C(11) C(10) C(15) 119.0(3) . . . yes
C(10) C(11) C(12) 120.5(3) . . . yes
C(10) C(11) H(4) 119.7 . . . no
C(12) C(11) H(4) 119.8 . . . no
C(11) C(12) C(13) 120.1(3) . . . yes
C(11) C(12) H(5) 119.9 . . . no
C(13) C(12) H(5) 119.9 . . . no
C(12) C(13) C(14) 120.4(3) . . . yes
C(12) C(13) C(16) 119.6(3) . . . yes
C(14) C(13) C(16) 119.9(3) . . . yes
C(13) C(14) C(15) 119.5(3) . . . yes
C(13) C(14) H(6) 120.3 . . . no
C(15) C(14) H(6) 120.3 . . . no
C(10) C(15) C(14) 120.4(3) . . . yes
C(10) C(15) H(7) 119.8 . . . no
C(14) C(15) H(7) 119.8 . . . no
N(1) C(16) C(13) 177.5(5) . . . yes
O(3) C(17) N(2) 122.5(3) . . . yes
O(3) C(17) C(18) 121.2(3) . . . yes
N(2) C(17) C(18) 116.3(3) . . . yes
C(17) C(18) C(19) 120.4(3) . . . yes
C(17) C(18) C(20) 120.5(3) . . . yes
C(19) C(18) C(20) 119.0(3) . . . yes
N(3) C(19) C(18) 176.9(4) . . . yes
O(4) C(20) C(18) 121.7(3) . . . yes
O(4) C(20) C(21) 114.6(3) . . . yes
C(18) C(20) C(21) 123.7(4) . . . yes
C(20) C(21) H(9) 109.5 . . . no
C(20) C(21) H(10) 109.5 . . . no
C(20) C(21) H(11) 109.5 . . . no
H(9) C(21) H(10) 109.5 . . . no
H(9) C(21) H(11) 109.5 . . . no
H(10) C(21) H(11) 109.5 . . . no
C(5) C(22) C(23) 116.4(3) . . . yes
C(5) C(22) C(24) 119.7(3) . . . yes
C(23) C(22) C(24) 123.9(3) . . . yes
C(22) C(23) H(13) 109.5 . . . no
C(22) C(23) H(14) 109.5 . . . no
C(22) C(23) H(15) 109.5 . . . no
H(13) C(23) H(14) 109.5 . . . no
H(13) C(23) H(15) 109.5 . . . no
H(14) C(23) H(15) 109.5 . . . no
C(22) C(24) C(25) 126.1(3) . . . yes
C(22) C(24) H(16) 117.0 . . . no
C(25) C(24) H(16) 117.0 . . . no
O(5) C(25) N(4) 119.5(3) . . . yes
O(5) C(25) C(24) 123.5(4) . . . yes
N(4) C(25) C(24) 117.0(3) . . . yes
N(4) C(26) C(27) 112.6(4) . . . yes
N(4) C(26) H(17) 108.7 . . . no
N(4) C(26) H(18) 108.7 . . . no
C(27) C(26) H(17) 108.7 . . . no
C(27) C(26) H(18) 108.7 . . . no
H(17) C(26) H(18) 109.5 . . . no
C(26) C(27) H(19) 109.5 . . . no
C(26) C(27) H(20) 109.5 . . . no
C(26) C(27) H(21) 109.5 . . . no
H(19) C(27) H(20) 109.5 . . . no
H(19) C(27) H(21) 109.5 . . . no
H(20) C(27) H(21) 109.5 . . . no
N(4) C(28) C(29) 93.8(7) . . . yes
N(4) C(28) H(22) 113.2 . . . no
N(4) C(28) H(23) 113.2 . . . no
C(29) C(28) H(22) 113.2 . . . no
C(29) C(28) H(23) 113.2 . . . no
H(22) C(28) H(23) 109.5 . . . no
C(28) C(29) H(24) 109.5 . . . no
C(28) C(29) H(25) 109.5 . . . no
C(28) C(29) H(26) 109.5 . . . no
H(24) C(29) H(25) 109.5 . . . no
H(24) C(29) H(26) 109.5 . . . no
H(25) C(29) H(26) 109.5 . . . no
#------------------------------------------------------------------------------
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O(1) C(1) C(2) N(2) -177.8(3) . . . . yes
O(1) C(1) C(2) C(3) -1.2(4) . . . . yes
O(1) C(1) C(9) O(2) 175.6(3) . . . . yes
O(1) C(1) C(9) C(10) -4.1(5) . . . . yes
O(1) C(8) C(3) C(2) -0.4(4) . . . . yes
O(1) C(8) C(3) C(4) 177.2(3) . . . . yes
O(1) C(8) C(7) C(6) -178.1(3) . . . . yes
O(2) C(9) C(1) C(2) -3.1(5) . . . . yes
O(2) C(9) C(10) C(11) 7.8(5) . . . . yes
O(2) C(9) C(10) C(15) -170.6(3) . . . . yes
O(3) C(17) N(2) C(2) -2.3(6) . . . . yes
O(3) C(17) C(18) C(19) -178.7(3) . . . . yes
O(3) C(17) C(18) C(20) 4.3(6) . . . . yes
O(4) C(20) C(18) C(17) -2.9(6) . . . . yes
O(4) C(20) C(18) C(19) -180.0(4) . . . . yes
O(5) C(25) N(4) C(26) -0.3(7) . . . . yes
O(5) C(25) N(4) C(28) 170.6(5) . . . . yes
O(5) C(25) C(24) C(22) 30.0(7) . . . . yes
N(1) C(16) C(13) C(12) -22(10) . . . . yes
N(1) C(16) C(13) C(14) 159(9) . . . . yes
N(2) C(2) C(1) C(9) 1.0(5) . . . . yes
N(2) C(2) C(3) C(4) 0.2(6) . . . . yes
N(2) C(2) C(3) C(8) 177.2(3) . . . . yes
N(2) C(17) C(18) C(19) 2.4(5) . . . . yes
N(2) C(17) C(18) C(20) -174.6(3) . . . . yes
N(3) C(19) C(18) C(17) 10(8) . . . . yes
N(3) C(19) C(18) C(20) -172(7) . . . . yes
N(4) C(25) C(24) C(22) -152.0(4) . . . . yes
C(1) O(1) C(8) C(3) -0.3(4) . . . . yes
C(1) O(1) C(8) C(7) 178.9(3) . . . . yes
C(1) C(2) N(2) C(17) -156.9(3) . . . . yes
C(1) C(2) C(3) C(4) -176.0(4) . . . . yes
C(1) C(2) C(3) C(8) 0.9(4) . . . . yes
C(1) C(9) C(10) C(11) -172.5(3) . . . . yes
C(1) C(9) C(10) C(15) 9.0(5) . . . . yes
C(2) N(2) C(17) C(18) 176.6(3) . . . . yes
C(2) C(1) O(1) C(8) 0.9(4) . . . . yes
C(2) C(1) C(9) C(10) 177.3(3) . . . . yes
C(2) C(3) C(4) C(5) 178.4(3) . . . . yes
C(2) C(3) C(8) C(7) -179.6(3) . . . . yes
C(3) C(2) N(2) C(17) 27.3(6) . . . . yes
C(3) C(2) C(1) C(9) 177.6(3) . . . . yes
C(3) C(4) C(5) C(6) -0.8(5) . . . . yes
C(3) C(4) C(5) C(22) -179.5(3) . . . . yes
C(3) C(8) C(7) C(6) 1.0(6) . . . . yes
C(4) C(3) C(8) C(7) -2.0(5) . . . . yes
C(4) C(5) C(6) C(7) -0.3(6) . . . . yes
C(4) C(5) C(22) C(23) 144.2(3) . . . . yes
C(4) C(5) C(22) C(24) -34.8(5) . . . . yes
C(5) C(4) C(3) C(8) 1.9(5) . . . . yes
C(5) C(6) C(7) C(8) 0.2(6) . . . . yes
C(5) C(22) C(24) C(25) 176.8(3) . . . . yes
C(6) C(5) C(22) C(23) -34.5(5) . . . . yes
C(6) C(5) C(22) C(24) 146.5(4) . . . . yes
C(7) C(6) C(5) C(22) 178.5(3) . . . . yes
C(8) O(1) C(1) C(9) -178.0(3) . . . . yes
C(9) C(10) C(11) C(12) -179.6(3) . . . . yes
C(9) C(10) C(15) C(14) 179.0(3) . . . . yes
C(10) C(11) C(12) C(13) 1.2(6) . . . . yes
C(10) C(15) C(14) C(13) -0.2(6) . . . . yes
C(11) C(10) C(15) C(14) 0.6(5) . . . . yes
C(11) C(12) C(13) C(14) -0.9(6) . . . . yes
C(11) C(12) C(13) C(16) -179.0(4) . . . . yes
C(12) C(11) C(10) C(15) -1.1(5) . . . . yes
C(12) C(13) C(14) C(15) 0.4(6) . . . . yes
C(15) C(14) C(13) C(16) 178.4(4) . . . . yes
C(17) C(18) C(20) C(21) 177.5(4) . . . . yes
C(19) C(18) C(20) C(21) 0.5(6) . . . . yes
C(23) C(22) C(24) C(25) -2.2(6) . . . . yes
C(24) C(25) N(4) C(26) -178.4(4) . . . . yes
C(24) C(25) N(4) C(28) -7.5(8) . . . . yes
C(25) N(4) C(26) C(27) 91.5(5) . . . . yes
C(25) N(4) C(28) C(29) 85.5(7) . . . . yes
C(26) N(4) C(28) C(29) -102.9(6) . . . . yes
C(27) C(26) N(4) C(28) -80.5(6) . . . . yes
C(27) C(26) N(4) C(28) -80.5(6) . . . . yes
#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O(1) O(2) 3.415(3) . 3_666 ?
O(2) C(6) 3.373(4) . 4_555 ?
O(2) C(8) 3.416(4) . 3_666 ?
O(2) C(1) 3.469(4) . 3_666 ?
O(2) C(3) 3.519(4) . 3_666 ?
O(2) C(2) 3.552(4) . 3_666 ?
O(3) C(16) 3.236(5) . 3_656 ?
O(3) N(1) 3.475(5) . 3_656 ?
O(3) C(14) 3.491(5) . 3_656 ?
O(3) C(13) 3.532(5) . 3_656 ?
O(4) O(5) 3.415(5) . 4_555 ?
O(5) C(20) 3.231(5) . 4_554 ?
O(5) C(18) 3.558(5) . 4_554 ?
O(5) C(21) 3.590(6) . 4_554 ?
N(1) C(28) 3.438(8) . 3_656 ?
N(1) C(27) 3.507(7) . 4_655 ?
N(1) C(29) 3.587(10) . 3_666 ?
N(2) C(15) 3.469(5) . 3_666 ?
N(2) C(10) 3.552(4) . 3_666 ?
N(3) C(6) 3.499(5) . 4_555 ?
N(3) C(23) 3.504(6) . 4_565 ?
N(3) C(12) 3.508(4) . 2_656 ?
C(1) C(9) 3.498(5) . 3_666 ?
C(1) C(1) 3.583(7) . 3_666 ?
C(2) C(9) 3.373(4) . 3_666 ?
C(2) C(10) 3.595(4) . 3_666 ?
C(4) C(11) 3.572(5) . 3_666 ?
C(8) C(11) 3.486(5) . 3_656 ?
#------------------------------------------------------------------------------
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_site_distance_dh
_geom_hbond_site_distance_ha
_geom_hbond_site_distance_da
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O(4) H(12) O(3) . . . 0.980 1.667 2.528(3) 144.189 no
N(2) H(8) O(2) . . . 0.927 1.897 2.676(2) 140.287 no
N(2) H(8) N(3) . . . 0.927 2.861 3.446(4) 122.273 no
O(2) N(2) 2.676(2) . . . 0.3571 0.5537 0.4280 122.273 no
O(2) N(3) 3.582(4) . . . 0.3999 0.6063 0.4314 122.273 no
O(3) O(4) 2.528(3) . . . 0.3942 0.4388 0.1881 122.273 no
N(3) O(2) 3.582(4) . . . 0.5114 0.6303 0.3655 122.273 no
N(3) N(2) 3.446(4) . . . 0.5301 0.6006 0.3321 122.273 no
#------------------------------------------------------------------------------

#------------------------------------------------------------------------------

data_compound_2
_database_code_depnum_ccdc_archive 'CCDC 222922'
_audit_creation_date             'Fri Dec 12 09:29:08 2003'
_audit_creation_method           'by teXsan'
_audit_update_record             ?

#------------------------------------------------------------------------------
# CHEMICAL DATA
_chemical_formula_sum            'C15 H11 Br N2 O4 '
_chemical_formula_moiety         ?
_chemical_formula_weight         363.17
_chemical_melting_point          ?
#------------------------------------------------------------------------------
# CRYSTAL DATA
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a                   7.357(2)
_cell_length_b                   9.914(2)
_cell_length_c                   40.665(1)
_cell_angle_alpha                90
_cell_angle_beta                 94.22(1)
_cell_angle_gamma                90
_cell_volume                     2958.0(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      29.8
_cell_measurement_theta_max      30.0
_cell_measurement_temperature    296.2
#------------------------------------------------------------------------------
_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_crystal_size_rad          ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_absorpt_coefficient_mu    3.984
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_T_max  0.999
#------------------------------------------------------------------------------
# EXPERIMENTAL DATA
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_reflns_number            6126
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_theta_max         67.57
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_reflns_theta_full        67.57
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_decay_%        5.17
#------------------------------------------------------------------------------
# REFINEMENT DATA
_refine_special_details          
;
Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted
R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are
based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only
for calculating R-factor (gt).
;
_reflns_number_total             5317
_reflns_number_gt                3980
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1460
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_reflns         5317
_refine_ls_number_parameters     398
_refine_ls_goodness_of_fit_ref   1.776
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_shift/su_max          0.0011
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_extinction_coef       0.028(3)
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Br Br -0.676 1.280
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.031 0.018
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.049 0.032
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
#------------------------------------------------------------------------------
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br(1) Br 0.25296(10) 0.10884(6) 0.74581(1) 0.0960(2) Uani 1.00 d . . .
Br(2) Br 0.03343(7) 0.98200(5) 0.44977(1) 0.0740(2) Uani 1.00 d . . .
O(1) O 0.3800(4) 0.1393(3) 0.60326(6) 0.0581(8) Uani 1.00 d . . .
O(2) O 0.2671(4) 0.4305(3) 0.55592(7) 0.0698(9) Uani 1.00 d . . .
O(3) O 0.1409(5) 0.5144(3) 0.67307(7) 0.0734(10) Uani 1.00 d . . .
O(4) O 0.0137(5) 0.7423(3) 0.68589(8) 0.087(1) Uani 1.00 d . . .
O(5) O 0.3212(4) 0.4224(3) 0.45821(6) 0.0599(8) Uani 1.00 d . . .
O(6) O 0.4662(5) 0.2550(3) 0.38802(7) 0.0769(10) Uani 1.00 d . . .
O(7) O 0.2221(5) 0.7091(3) 0.35514(7) 0.0752(10) Uani 1.00 d . . .
O(8) O 0.2129(5) 0.7658(4) 0.29483(8) 0.094(1) Uani 1.00 d . . .
N(1) N 0.1980(4) 0.4635(3) 0.62013(7) 0.0549(9) Uani 1.00 d . . .
N(2) N 0.0712(6) 0.7288(4) 0.57030(10) 0.084(1) Uani 1.00 d . . .
N(3) N 0.3265(5) 0.5028(3) 0.37246(7) 0.0538(9) Uani 1.00 d . . .
N(4) N 0.4523(7) 0.3235(4) 0.3069(1) 0.095(2) Uani 1.00 d . . .
C(1) C 0.2555(6) 0.2351(4) 0.68384(9) 0.058(1) Uani 1.00 d . . .
C(2) C 0.2997(6) 0.1184(4) 0.70051(9) 0.063(1) Uani 1.00 d . . .
C(3) C 0.3722(6) 0.0050(4) 0.6864(1) 0.067(1) Uani 1.00 d . . .
C(4) C 0.4046(6) 0.0058(4) 0.6532(1) 0.063(1) Uani 1.00 d . . .
C(5) C 0.3591(6) 0.1229(4) 0.63616(9) 0.055(1) Uani 1.00 d . . .
C(6) C 0.3205(5) 0.2679(4) 0.59597(9) 0.054(1) Uani 1.00 d . . .
C(7) C 0.2623(5) 0.3322(4) 0.62314(8) 0.0491(10) Uani 1.00 d . . .
C(8) C 0.2871(5) 0.2374(4) 0.64996(8) 0.0511(10) Uani 1.00 d . . .
C(9) C 0.3167(6) 0.3161(4) 0.56204(9) 0.059(1) Uani 1.00 d . . .
C(10) C 0.3769(6) 0.2230(5) 0.53587(10) 0.070(1) Uani 1.00 d . . .
C(11) C 0.1402(5) 0.5476(4) 0.64362(9) 0.056(1) Uani 1.00 d . . .
C(12) C 0.0740(5) 0.6798(4) 0.63255(9) 0.056(1) Uani 1.00 d . . .
C(13) C 0.0719(6) 0.7103(4) 0.5984(1) 0.064(1) Uani 1.00 d . . .
C(14) C 0.0104(6) 0.7705(4) 0.6541(1) 0.063(1) Uani 1.00 d . . .
C(15) C -0.0669(7) 0.9055(5) 0.6453(1) 0.078(2) Uani 1.00 d . . .
C(16) C 0.1645(5) 0.7390(4) 0.42478(9) 0.055(1) Uani 1.00 d . . .
C(17) C 0.1140(6) 0.8005(4) 0.45309(9) 0.056(1) Uani 1.00 d . . .
C(18) C 0.1270(6) 0.7380(4) 0.48386(9) 0.062(1) Uani 1.00 d . . .
C(19) C 0.1909(6) 0.6093(4) 0.48703(9) 0.062(1) Uani 1.00 d . . .
C(20) C 0.2464(6) 0.5478(4) 0.45895(9) 0.054(1) Uani 1.00 d . . .
C(21) C 0.3566(6) 0.4006(4) 0.42575(9) 0.055(1) Uani 1.00 d . . .
C(22) C 0.3037(6) 0.5084(4) 0.40644(9) 0.053(1) Uani 1.00 d . . .
C(23) C 0.2324(5) 0.6079(4) 0.42761(8) 0.0507(10) Uani 1.00 d . . .
C(24) C 0.4384(6) 0.2747(4) 0.41704(10) 0.062(1) Uani 1.00 d . . .
C(25) C 0.4897(7) 0.1741(4) 0.4433(1) 0.076(1) Uani 1.00 d . . .
C(26) C 0.2847(6) 0.5966(4) 0.34905(9) 0.055(1) Uani 1.00 d . . .
C(27) C 0.3194(5) 0.5580(4) 0.31537(9) 0.057(1) Uani 1.00 d . . .
C(28) C 0.3946(6) 0.4287(5) 0.30964(9) 0.066(1) Uani 1.00 d . . .
C(29) C 0.2777(7) 0.6455(5) 0.2897(1) 0.070(1) Uani 1.00 d . . .
C(30) C 0.3071(9) 0.6146(6) 0.2546(1) 0.098(2) Uani 1.00 d . . .
H(1) H 0.2063 0.3107 0.6944 0.0689 Uiso 1.00 calc . . .
H(2) H 0.3979 -0.0731 0.6994 0.0801 Uiso 1.00 calc . . .
H(3) H 0.4543 -0.0698 0.6428 0.0755 Uiso 1.00 calc . . .
H(4) H 0.4115 0.1383 0.5454 0.0827 Uiso 1.00 calc . . .
H(5) H 0.2801 0.2104 0.5195 0.0827 Uiso 1.00 calc . . .
H(6) H 0.4787 0.2616 0.5262 0.0827 Uiso 1.00 calc . . .
H(7) H 0.2052 0.5189 0.6001 0.1152 Uiso 1.00 calc . . .
H(8) H 0.0385 0.6442 0.6881 0.1152 Uiso 1.00 calc . . .
H(9) H -0.1883 0.9103 0.6515 0.0937 Uiso 1.00 calc . . .
H(10) H 0.0047 0.9733 0.6567 0.0937 Uiso 1.00 calc . . .
H(11) H -0.0649 0.9189 0.6222 0.0937 Uiso 1.00 calc . . .
H(12) H 0.1525 0.7841 0.4041 0.0657 Uiso 1.00 calc . . .
H(13) H 0.0910 0.7850 0.5027 0.0732 Uiso 1.00 calc . . .
H(14) H 0.1974 0.5643 0.5076 0.0745 Uiso 1.00 calc . . .
H(15) H 0.4571 0.2082 0.4639 0.0894 Uiso 1.00 calc . . .
H(16) H 0.6181 0.1599 0.4444 0.0894 Uiso 1.00 calc . . .
H(17) H 0.4285 0.0921 0.4385 0.0894 Uiso 1.00 calc . . .
H(18) H 0.3687 0.4130 0.3665 0.1152 Uiso 1.00 calc . . .
H(19) H 0.2586 0.7667 0.3194 0.1152 Uiso 1.00 calc . . .
H(20) H 0.3908 0.6791 0.2468 0.1168 Uiso 1.00 calc . . .
H(21) H 0.1944 0.6221 0.2418 0.1168 Uiso 1.00 calc . . .
H(22) H 0.3550 0.5273 0.2530 0.1168 Uiso 1.00 calc . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br(1) 0.1395(6) 0.1052(4) 0.0438(3) -0.0128(3) 0.0107(3) 0.0101(2)
Br(2) 0.0920(4) 0.0638(3) 0.0675(3) 0.0125(2) 0.0148(2) 0.0001(2)
O(1) 0.070(2) 0.064(2) 0.041(1) 0.005(1) 0.008(1) -0.002(1)
O(2) 0.093(2) 0.071(2) 0.046(1) 0.004(2) 0.010(1) 0.009(1)
O(3) 0.106(2) 0.072(2) 0.042(1) 0.012(2) 0.007(1) -0.002(1)
O(4) 0.116(3) 0.089(2) 0.058(2) 0.018(2) 0.015(2) -0.008(2)
O(5) 0.086(2) 0.059(2) 0.036(1) 0.004(1) 0.005(1) 0.002(1)
O(6) 0.114(3) 0.068(2) 0.048(2) 0.013(2) 0.007(2) -0.007(1)
O(7) 0.109(3) 0.070(2) 0.047(1) 0.016(2) 0.010(2) 0.009(1)
O(8) 0.130(3) 0.095(2) 0.058(2) 0.027(2) 0.012(2) 0.022(2)
N(1) 0.067(2) 0.056(2) 0.042(2) 0.002(1) 0.007(1) 0.001(1)
N(2) 0.120(4) 0.072(2) 0.060(2) 0.015(2) 0.013(2) 0.011(2)
N(3) 0.071(2) 0.056(2) 0.034(1) -0.006(1) 0.005(1) -0.002(1)
N(4) 0.144(4) 0.082(3) 0.060(2) 0.016(3) 0.022(3) -0.003(2)
C(1) 0.068(3) 0.066(2) 0.041(2) -0.006(2) 0.005(2) -0.002(2)
C(2) 0.075(3) 0.072(3) 0.041(2) -0.011(2) 0.000(2) 0.001(2)
C(3) 0.078(3) 0.068(3) 0.052(2) -0.003(2) -0.002(2) 0.011(2)
C(4) 0.071(3) 0.066(2) 0.053(2) 0.006(2) 0.001(2) 0.000(2)
C(5) 0.063(2) 0.061(2) 0.040(2) -0.003(2) 0.002(2) -0.002(2)
C(6) 0.061(2) 0.060(2) 0.041(2) -0.001(2) 0.007(2) 0.000(2)
C(7) 0.051(2) 0.055(2) 0.041(2) -0.006(2) 0.002(1) 0.000(2)
C(8) 0.056(2) 0.058(2) 0.040(2) -0.003(2) 0.002(1) 0.000(2)
C(9) 0.064(3) 0.072(3) 0.043(2) -0.007(2) 0.008(2) -0.001(2)
C(10) 0.079(3) 0.087(3) 0.045(2) -0.003(2) 0.010(2) -0.002(2)
C(11) 0.059(2) 0.063(2) 0.045(2) -0.008(2) 0.002(2) -0.001(2)
C(12) 0.057(2) 0.059(2) 0.052(2) -0.003(2) 0.005(2) -0.001(2)
C(13) 0.076(3) 0.054(2) 0.063(3) 0.005(2) 0.008(2) 0.004(2)
C(14) 0.063(3) 0.070(3) 0.056(2) 0.001(2) 0.002(2) -0.004(2)
C(15) 0.076(3) 0.079(3) 0.080(3) 0.009(2) 0.003(2) -0.014(3)
C(16) 0.068(2) 0.054(2) 0.042(2) 0.002(2) 0.001(2) 0.002(2)
C(17) 0.062(2) 0.056(2) 0.050(2) 0.005(2) 0.003(2) -0.002(2)
C(18) 0.075(3) 0.066(2) 0.046(2) 0.006(2) 0.012(2) -0.002(2)
C(19) 0.079(3) 0.068(2) 0.039(2) 0.001(2) 0.008(2) 0.003(2)
C(20) 0.070(2) 0.054(2) 0.039(2) 0.001(2) 0.001(2) 0.001(2)
C(21) 0.075(3) 0.053(2) 0.038(2) -0.003(2) 0.005(2) 0.000(2)
C(22) 0.065(2) 0.058(2) 0.036(2) -0.007(2) 0.002(2) -0.004(2)
C(23) 0.059(2) 0.055(2) 0.038(2) -0.005(2) 0.002(2) 0.001(1)
C(24) 0.078(3) 0.059(2) 0.048(2) -0.001(2) 0.003(2) -0.006(2)
C(25) 0.109(4) 0.058(2) 0.060(2) 0.014(2) 0.009(2) 0.005(2)
C(26) 0.062(2) 0.062(2) 0.041(2) -0.008(2) 0.004(2) 0.001(2)
C(27) 0.060(2) 0.069(2) 0.041(2) -0.006(2) 0.005(2) 0.004(2)
C(28) 0.077(3) 0.081(3) 0.040(2) -0.005(2) 0.007(2) -0.004(2)
C(29) 0.077(3) 0.088(3) 0.045(2) 0.002(2) 0.008(2) 0.010(2)
C(30) 0.126(5) 0.123(5) 0.044(2) 0.028(4) 0.009(3) 0.013(3)
#------------------------------------------------------------------------------
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_structure_solution    SIR88
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_molecular_graphics    ?
#------------------------------------------------------------------------------
_geom_special_details            
;
?
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br(1) C(2) 1.901(4) . . yes
Br(2) C(17) 1.897(4) . . yes
O(1) C(5) 1.368(4) . . yes
O(1) C(6) 1.373(4) . . yes
O(2) C(9) 1.212(5) . . yes
O(3) C(11) 1.242(5) . . yes
O(4) C(14) 1.322(5) . . yes
O(4) H(8) 0.993 . . no
O(5) C(20) 1.361(4) . . yes
O(5) C(21) 1.381(4) . . yes
O(6) C(24) 1.228(5) . . yes
O(7) C(26) 1.239(5) . . yes
O(8) C(29) 1.307(5) . . yes
O(8) H(19) 1.030 . . no
N(1) C(7) 1.388(5) . . yes
N(1) C(11) 1.360(5) . . yes
N(1) H(7) 0.988 . . no
N(2) C(13) 1.157(5) . . yes
N(3) C(22) 1.405(4) . . yes
N(3) C(26) 1.350(5) . . yes
N(3) H(18) 0.979 . . no
N(4) C(28) 1.134(6) . . yes
C(1) C(2) 1.368(5) . . yes
C(1) C(8) 1.414(5) . . yes
C(1) H(1) 0.948 . . no
C(2) C(3) 1.387(6) . . yes
C(3) C(4) 1.386(6) . . yes
C(3) H(2) 0.950 . . no
C(4) C(5) 1.381(5) . . yes
C(4) H(3) 0.947 . . no
C(5) C(8) 1.389(5) . . yes
C(6) C(7) 1.371(5) . . yes
C(6) C(9) 1.458(5) . . yes
C(7) C(8) 1.441(5) . . yes
C(9) C(10) 1.500(6) . . yes
C(10) H(4) 0.951 . . no
C(10) H(5) 0.947 . . no
C(10) H(6) 0.952 . . no
C(11) C(12) 1.458(5) . . yes
C(12) C(13) 1.420(5) . . yes
C(12) C(14) 1.362(5) . . yes
C(14) C(15) 1.488(6) . . yes
C(15) H(9) 0.948 . . no
C(15) H(10) 0.953 . . no
C(15) H(11) 0.947 . . no
C(16) C(17) 1.377(5) . . yes
C(16) C(23) 1.394(5) . . yes
C(16) H(12) 0.950 . . no
C(17) C(18) 1.393(5) . . yes
C(18) C(19) 1.362(6) . . yes
C(18) H(13) 0.950 . . no
C(19) C(20) 1.383(5) . . yes
C(19) H(14) 0.947 . . no
C(20) C(23) 1.404(5) . . yes
C(21) C(22) 1.366(5) . . yes
C(21) C(24) 1.440(5) . . yes
C(22) C(23) 1.434(5) . . yes
C(24) C(25) 1.490(6) . . yes
C(25) H(15) 0.952 . . no
C(25) H(16) 0.953 . . no
C(25) H(17) 0.943 . . no
C(26) C(27) 1.462(5) . . yes
C(27) C(28) 1.422(6) . . yes
C(27) C(29) 1.374(6) . . yes
C(29) C(30) 1.490(6) . . yes
C(30) H(20) 0.957 . . no
C(30) H(21) 0.950 . . no
C(30) H(22) 0.939 . . no
#------------------------------------------------------------------------------
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(5) O(1) C(6) 105.4(3) . . . yes
C(14) O(4) H(8) 106.5 . . . no
C(20) O(5) C(21) 105.6(3) . . . yes
C(29) O(8) H(19) 93.8 . . . no
C(7) N(1) C(11) 129.5(3) . . . yes
C(7) N(1) H(7) 123.8 . . . no
C(11) N(1) H(7) 106.1 . . . no
C(22) N(3) C(26) 128.9(3) . . . yes
C(22) N(3) H(18) 110.0 . . . no
C(26) N(3) H(18) 120.8 . . . no
C(2) C(1) C(8) 116.5(4) . . . yes
C(2) C(1) H(1) 122.0 . . . no
C(8) C(1) H(1) 121.5 . . . no
Br(1) C(2) C(1) 118.0(3) . . . yes
Br(1) C(2) C(3) 117.6(3) . . . yes
C(1) C(2) C(3) 124.4(4) . . . yes
C(2) C(3) C(4) 119.9(4) . . . yes
C(2) C(3) H(2) 119.8 . . . no
C(4) C(3) H(2) 120.3 . . . no
C(3) C(4) C(5) 116.1(4) . . . yes
C(3) C(4) H(3) 122.0 . . . no
C(5) C(4) H(3) 121.9 . . . no
O(1) C(5) C(4) 123.4(3) . . . yes
O(1) C(5) C(8) 111.8(3) . . . yes
C(4) C(5) C(8) 124.8(3) . . . yes
O(1) C(6) C(7) 111.8(3) . . . yes
O(1) C(6) C(9) 119.5(3) . . . yes
C(7) C(6) C(9) 128.6(4) . . . yes
N(1) C(7) C(6) 119.3(3) . . . yes
N(1) C(7) C(8) 134.6(3) . . . yes
C(6) C(7) C(8) 106.1(3) . . . yes
C(1) C(8) C(5) 118.4(3) . . . yes
C(1) C(8) C(7) 136.6(4) . . . yes
C(5) C(8) C(7) 105.0(3) . . . yes
O(2) C(9) C(6) 119.1(4) . . . yes
O(2) C(9) C(10) 122.0(4) . . . yes
C(6) C(9) C(10) 118.9(4) . . . yes
C(9) C(10) H(4) 109.7 . . . no
C(9) C(10) H(5) 109.5 . . . no
C(9) C(10) H(6) 109.2 . . . no
H(4) C(10) H(5) 109.6 . . . no
H(4) C(10) H(6) 109.2 . . . no
H(5) C(10) H(6) 109.6 . . . no
O(3) C(11) N(1) 122.4(4) . . . yes
O(3) C(11) C(12) 120.9(4) . . . yes
N(1) C(11) C(12) 116.7(3) . . . yes
C(11) C(12) C(13) 118.2(3) . . . yes
C(11) C(12) C(14) 121.2(4) . . . yes
C(13) C(12) C(14) 120.6(4) . . . yes
N(2) C(13) C(12) 176.8(5) . . . yes
O(4) C(14) C(12) 120.5(4) . . . yes
O(4) C(14) C(15) 113.9(4) . . . yes
C(12) C(14) C(15) 125.6(4) . . . yes
C(14) C(15) H(9) 109.4 . . . no
C(14) C(15) H(10) 109.2 . . . no
C(14) C(15) H(11) 109.4 . . . no
H(9) C(15) H(10) 109.4 . . . no
H(9) C(15) H(11) 110.0 . . . no
H(10) C(15) H(11) 109.5 . . . no
C(17) C(16) C(23) 117.4(3) . . . yes
C(17) C(16) H(12) 121.2 . . . no
C(23) C(16) H(12) 121.4 . . . no
Br(2) C(17) C(16) 117.5(3) . . . yes
Br(2) C(17) C(18) 119.1(3) . . . yes
C(16) C(17) C(18) 123.3(4) . . . yes
C(17) C(18) C(19) 120.1(4) . . . yes
C(17) C(18) H(13) 120.0 . . . no
C(19) C(18) H(13) 119.9 . . . no
C(18) C(19) C(20) 117.1(3) . . . yes
C(18) C(19) H(14) 121.3 . . . no
C(20) C(19) H(14) 121.6 . . . no
O(5) C(20) C(19) 124.5(3) . . . yes
O(5) C(20) C(23) 111.7(3) . . . yes
C(19) C(20) C(23) 123.8(4) . . . yes
O(5) C(21) C(22) 111.2(3) . . . yes
O(5) C(21) C(24) 118.8(3) . . . yes
C(22) C(21) C(24) 130.0(3) . . . yes
N(3) C(22) C(21) 119.0(3) . . . yes
N(3) C(22) C(23) 133.9(3) . . . yes
C(21) C(22) C(23) 107.1(3) . . . yes
C(16) C(23) C(20) 118.2(3) . . . yes
C(16) C(23) C(22) 137.4(3) . . . yes
C(20) C(23) C(22) 104.3(3) . . . yes
O(6) C(24) C(21) 118.5(4) . . . yes
O(6) C(24) C(25) 122.0(4) . . . yes
C(21) C(24) C(25) 119.5(3) . . . yes
C(24) C(25) H(15) 109.1 . . . no
C(24) C(25) H(16) 109.2 . . . no
C(24) C(25) H(17) 109.7 . . . no
H(15) C(25) H(16) 109.1 . . . no
H(15) C(25) H(17) 110.0 . . . no
H(16) C(25) H(17) 109.8 . . . no
O(7) C(26) N(3) 123.2(3) . . . yes
O(7) C(26) C(27) 121.0(3) . . . yes
N(3) C(26) C(27) 115.7(3) . . . yes
C(26) C(27) C(28) 119.1(3) . . . yes
C(26) C(27) C(29) 120.1(4) . . . yes
C(28) C(27) C(29) 120.8(4) . . . yes
N(4) C(28) C(27) 175.9(4) . . . yes
O(8) C(29) C(27) 121.2(4) . . . yes
O(8) C(29) C(30) 114.9(4) . . . yes
C(27) C(29) C(30) 123.9(5) . . . yes
C(29) C(30) H(20) 108.8 . . . no
C(29) C(30) H(21) 109.1 . . . no
C(29) C(30) H(22) 109.8 . . . no
H(20) C(30) H(21) 108.9 . . . no
H(20) C(30) H(22) 109.8 . . . no
H(21) C(30) H(22) 110.5 . . . no
#------------------------------------------------------------------------------
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br(1) C(2) C(1) C(8) -178.2(3) . . . . yes
Br(1) C(2) C(3) C(4) 178.4(3) . . . . yes
Br(2) C(17) C(16) C(23) 176.8(3) . . . . yes
Br(2) C(17) C(18) C(19) -177.6(3) . . . . yes
O(1) C(5) C(4) C(3) -179.1(4) . . . . yes
O(1) C(5) C(8) C(1) 179.2(3) . . . . yes
O(1) C(5) C(8) C(7) -0.1(4) . . . . yes
O(1) C(6) C(7) N(1) 179.8(3) . . . . yes
O(1) C(6) C(7) C(8) 0.2(4) . . . . yes
O(1) C(6) C(9) O(2) -178.6(4) . . . . yes
O(1) C(6) C(9) C(10) 0.4(6) . . . . yes
O(2) C(9) C(6) C(7) 5.0(7) . . . . yes
O(3) C(11) N(1) C(7) 1.1(7) . . . . yes
O(3) C(11) C(12) C(13) -178.2(4) . . . . yes
O(3) C(11) C(12) C(14) -0.3(6) . . . . yes
O(4) C(14) C(12) C(11) 2.6(7) . . . . yes
O(4) C(14) C(12) C(13) -179.5(4) . . . . yes
O(5) C(20) C(19) C(18) 176.8(4) . . . . yes
O(5) C(20) C(23) C(16) -177.6(3) . . . . yes
O(5) C(20) C(23) C(22) 0.6(4) . . . . yes
O(5) C(21) C(22) N(3) -178.9(3) . . . . yes
O(5) C(21) C(22) C(23) 1.1(5) . . . . yes
O(5) C(21) C(24) O(6) 178.6(4) . . . . yes
O(5) C(21) C(24) C(25) -2.5(6) . . . . yes
O(6) C(24) C(21) C(22) -1.0(7) . . . . yes
O(7) C(26) N(3) C(22) 2.7(7) . . . . yes
O(7) C(26) C(27) C(28) 178.8(4) . . . . yes
O(7) C(26) C(27) C(29) -2.0(6) . . . . yes
O(8) C(29) C(27) C(26) 2.5(7) . . . . yes
O(8) C(29) C(27) C(28) -178.3(4) . . . . yes
N(1) C(7) C(6) C(9) -3.6(6) . . . . yes
N(1) C(7) C(8) C(1) 1.2(8) . . . . yes
N(1) C(7) C(8) C(5) -179.6(4) . . . . yes
N(1) C(11) C(12) C(13) 0.9(6) . . . . yes
N(1) C(11) C(12) C(14) 178.9(4) . . . . yes
N(2) C(13) C(12) C(11) 15(9) . . . . yes
N(2) C(13) C(12) C(14) -162(9) . . . . yes
N(3) C(22) C(21) C(24) 0.7(7) . . . . yes
N(3) C(22) C(23) C(16) -3.4(8) . . . . yes
N(3) C(22) C(23) C(20) 178.9(4) . . . . yes
N(3) C(26) C(27) C(28) -0.6(6) . . . . yes
N(3) C(26) C(27) C(29) 178.6(4) . . . . yes
N(4) C(28) C(27) C(26) 12(7) . . . . yes
N(4) C(28) C(27) C(29) -166(7) . . . . yes
C(1) C(2) C(3) C(4) 0.2(7) . . . . yes
C(1) C(8) C(5) C(4) -0.7(6) . . . . yes
C(1) C(8) C(7) C(6) -179.2(4) . . . . yes
C(2) C(1) C(8) C(5) 0.2(6) . . . . yes
C(2) C(1) C(8) C(7) 179.4(4) . . . . yes
C(2) C(3) C(4) C(5) -0.6(7) . . . . yes
C(3) C(2) C(1) C(8) 0.0(7) . . . . yes
C(3) C(4) C(5) C(8) 0.9(7) . . . . yes
C(4) C(5) O(1) C(6) -179.8(4) . . . . yes
C(4) C(5) C(8) C(7) 179.9(4) . . . . yes
C(5) O(1) C(6) C(7) -0.2(4) . . . . yes
C(5) O(1) C(6) C(9) -177.1(4) . . . . yes
C(5) C(8) C(7) C(6) 0.0(4) . . . . yes
C(6) O(1) C(5) C(8) 0.2(4) . . . . yes
C(6) C(7) N(1) C(11) -177.4(4) . . . . yes
C(7) N(1) C(11) C(12) -178.0(3) . . . . yes
C(7) C(6) C(9) C(10) -175.9(4) . . . . yes
C(8) C(7) N(1) C(11) 2.2(7) . . . . yes
C(8) C(7) C(6) C(9) 176.7(4) . . . . yes
C(11) C(12) C(14) C(15) -177.4(4) . . . . yes
C(13) C(12) C(14) C(15) 0.5(7) . . . . yes
C(16) C(17) C(18) C(19) -0.5(7) . . . . yes
C(16) C(23) C(20) C(19) 2.3(6) . . . . yes
C(16) C(23) C(22) C(21) 176.6(5) . . . . yes
C(17) C(16) C(23) C(20) -0.5(6) . . . . yes
C(17) C(16) C(23) C(22) -178.0(4) . . . . yes
C(17) C(18) C(19) C(20) 2.1(6) . . . . yes
C(18) C(17) C(16) C(23) -0.3(6) . . . . yes
C(18) C(19) C(20) C(23) -3.0(7) . . . . yes
C(19) C(20) O(5) C(21) -179.8(4) . . . . yes
C(19) C(20) C(23) C(22) -179.5(4) . . . . yes
C(20) O(5) C(21) C(22) -0.7(4) . . . . yes
C(20) O(5) C(21) C(24) 179.6(4) . . . . yes
C(20) C(23) C(22) C(21) -1.0(4) . . . . yes
C(21) O(5) C(20) C(23) 0.0(4) . . . . yes
C(21) C(22) N(3) C(26) -179.9(4) . . . . yes
C(22) N(3) C(26) C(27) -177.9(4) . . . . yes
C(22) C(21) C(24) C(25) 177.9(4) . . . . yes
C(23) C(22) N(3) C(26) 0.2(7) . . . . yes
C(23) C(22) C(21) C(24) -179.3(4) . . . . yes
C(26) C(27) C(29) C(30) -179.6(5) . . . . yes
C(28) C(27) C(29) C(30) -0.4(7) . . . . yes
C(28) C(27) C(29) C(30) -0.4(7) . . . . yes
#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Br(1) O(4) 3.422(3) . 2_546 ?
Br(1) O(3) 3.462(3) . 2_546 ?
Br(1) N(4) 3.512(5) . 4_455 ?
Br(2) N(2) 3.064(4) . 3_576 ?
O(1) O(7) 3.600(4) . 3_666 ?
O(2) C(21) 3.274(5) . 3_666 ?
O(2) C(19) 3.328(5) . . ?
O(2) O(5) 3.448(4) . 3_666 ?
O(2) C(22) 3.460(5) . 3_666 ?
O(3) C(26) 3.378(5) . 3_566 ?
O(3) N(4) 3.441(6) . 3_666 ?
O(3) C(28) 3.484(6) . 3_666 ?
O(3) C(27) 3.527(5) . 3_566 ?
O(3) O(7) 3.593(5) . 3_566 ?
O(4) C(28) 3.465(6) . 3_566 ?
O(4) N(4) 3.523(7) . 3_566 ?
O(4) C(30) 3.572(6) . 4_465 ?
O(5) N(2) 3.381(6) . 3_566 ?
O(6) C(4) 3.260(5) . 3_656 ?
O(6) C(13) 3.420(6) . 3_666 ?
O(6) C(15) 3.522(6) . 3_566 ?
O(7) C(5) 3.498(5) . 3_666 ?
N(1) N(3) 3.505(5) . 3_666 ?
N(2) C(21) 3.413(6) . 3_566 ?
N(2) C(25) 3.454(7) . 3_666 ?
N(2) C(18) 3.570(5) . . ?
N(3) C(7) 3.432(5) . 3_666 ?
N(3) C(12) 3.452(5) . 3_566 ?
N(3) C(11) 3.484(5) . 3_566 ?
N(4) C(3) 3.507(6) . 3_656 ?
C(4) C(15) 3.600(7) . 1_545 ?
C(6) C(22) 3.552(5) . 3_666 ?
C(7) C(26) 3.512(5) . 3_666 ?
C(8) C(26) 3.552(5) . 3_666 ?
C(9) C(17) 3.386(6) . 3_566 ?
C(9) C(23) 3.398(6) . 3_666 ?
C(9) C(22) 3.456(6) . 3_666 ?
C(10) C(23) 3.557(6) . 3_666 ?
C(10) C(20) 3.579(6) . 3_666 ?
C(11) C(26) 3.470(6) . 3_566 ?
C(13) C(21) 3.414(6) . 3_566 ?
C(13) C(22) 3.507(6) . 3_566 ?
#------------------------------------------------------------------------------
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_site_distance_DH
_geom_hbond_site_distance_HA
_geom_hbond_site_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O(4) H(8) O(3) . . . 0.993 1.632 2.515(4) 145.709 no
N(1) H(7) O(2) . . . 0.988 2.078 2.716(4) 120.469 no
N(1) H(7) N(2) . . . 0.988 2.567 3.408(4) 142.917 no
O(8) H(19) O(7) . . . 1.029 1.603 2.512(4) 144.250 no
N(3) H(18) O(6) . . . 0.979 1.908 2.720(4) 138.525 no
N(3) H(18) N(4) . . . 0.979 2.694 3.388(5) 128.226 no
O(4) H(8) Br(1) . . 2_556 0.993 3.016 3.422(3) 105.768 no
#------------------------------------------------------------------------------