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

data_global

_publ_contact_author_name        'Dr Darren Bradshaw '
_journal_name_full               Chem.Commun.
_journal_coden_Cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?

loop_
_publ_author_name
_publ_author_address
T.J.Prior
;     Department of Chemistry
University of Liverpool
Liverpool
L69 7ZD
UK
;
D.Bradshaw
;     Department of Chemistry
University of Liverpool
Liverpool
L69 7ZD
UK
;
S.J.Teat
;     Synchrotron Radiation Source
Daresbury Laboratory
Daresbury
Warrington
WA4 4AD
UK
;
M.J.Rosseinsky
;     Department of Chemistry
University of Liverpool
Liverpool
L69 7ZD
UK
;

_publ_contact_author_address     
;
Department of Chemistry 
University of Liverpool 
Robert Robinson Laboratories 
Liverpool 
L69 7ZD 
UNITED KINGDOM 
;

_publ_section_title              
;
Designed layer assembly:  a three-dimensional
framework with 74% extra-framework volume by connection of infinite
two-dimensional sheets
;

data_[Ni6(btc)4(bipy)6(MeOH)3(H2O)9.guests]
_database_code_CSD                  191255
_publ_section_title              
;
Designed layer assembly:  a three-dimensional
framework with 74% extra-framework volume by connection of infinite
two-dimensional sheets
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_structural     
'Ni 6 (C 9 H 3 O 6) 4 (C 10 H 8 N 2) 6 (C H 4 O) 3 (H 2 O) 9 . guests'
_chemical_formula_sum            'C49 H33 N6 Ni3 O18'
_chemical_formula_weight         1169.94

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   33.5211(10)
_cell_length_b                   33.5211(10)
_cell_length_c                   11.3015(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     10997.7(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    34269
_cell_measurement_theta_min      4.41
_cell_measurement_theta_max      50.79

_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    0.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1791
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_T_max  0.9878
_exptl_absorpt_process_details   
;
Sheldrick, G. M., SADABS; Universitat Gottingen, 1997'
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.68670
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'Bruker AXS SMART 1K CCD Diffractomer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            87340
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         25.46
_reflns_number_total             30013
_reflns_number_gt                22377
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and=

goodness 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 threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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.

This 3-D framework exhibits supercell reflections as intense as those
predicted for the subcell which indicate that the observed supercell is th=
e
true cell. There are no systematic absences in the data and thus a large=

number of space groups are possible for this material, the acentric sp grp
P3 (Laue class -3) gives the best refinement for this structure.

Application of the twin law -1 0 0 0 -1 0 0 0 1 -4 is necessary as the
aggregate crystal mimics the higher Laue group 6/mmm and is applied in
conjunction with the inversion operator such that four twin components
are calculated. All aromatic rings are constrained to be approximately pla=
nar
and to have sensible bond lengths. Isotropic thermal parameters of the
non-hydrogen atoms (other than aniso Ni atoms) are also constrained to
be roughly equal within each aromatic ring system.

Solvent within the voids is not crystallographically well defined and
this extra- framework electron density was removed from the structure and =
the
data treated with the SQUEEZE routine within PLATON. This suggests a void=

electron population of 679 per formula unit. This corresponds to 4 ethylen=
e
glycol and 5 methanol molecules per metal centre. Structural refinement of=
the
framework without this electron density, following modification of the
data with the SQUEEZE routine, gives a significant improvement in the
quality of the fit (before SQUEEZE: R1 == 0.1910, wR2 == 0.4882 for 25938 =
data
with (I > 2sI) and R1 == 0.2015, wR2 == 0.4997 for all
data / restraint / parameters 30013 / 161 / 286)

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w==1/[\s^2^(Fo^2^)+(0.2000P)^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    mixed
_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   0.00
_refine_ls_number_reflns         30013
_refine_ls_number_parameters     299
_refine_ls_number_restraints     161
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.1469
_refine_ls_wR_factor_ref         0.3591
_refine_ls_wR_factor_gt          0.3414
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_restrained_S_all      1.334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.83454(3) 0.66984(3) 1.00668(9) 0.0248(2) Uani 1 1 d . . .
Ni2 Ni 0.99847(4) 0.49920(4) 0.90870(11) 0.0380(3) Uani 1 1 d . . .
Ni3 Ni 1.16566(3) 0.83496(3) 0.84811(10) 0.0273(2) Uani 1 1 d . . .
C11 C 0.96954(12) 0.68369(13) 0.9483(2) 0.0269(14) Uiso 1 1 d GDU . .
C12 C 1.01495(13) 0.71519(10) 0.9193(2) 0.0257(13) Uiso 1 1 d GDU . .
H12 H 1.0250 0.7472 0.9169 0.031 Uiso 1 1 calc R . .
C13 C 1.04564(10) 0.69989(13) 0.8938(2) 0.0323(15) Uiso 1 1 d GDU . .
C14 C 1.03092(12) 0.65309(14) 0.8972(2) 0.0407(18) Uiso 1 1 d GDU . .
H14 H 1.0519 0.6426 0.8797 0.049 Uiso 1 1 calc R . .
C15 C 0.98551(14) 0.62159(10) 0.9262(3) 0.0310(15) Uiso 1 1 d GDU . .
C16 C 0.95482(10) 0.63689(11) 0.9517(2) 0.0220(13) Uiso 1 1 d GDU . .
H16 H 0.9238 0.6154 0.9715 0.026 Uiso 1 1 calc R . .
C17 C 0.9324(3) 0.6958(3) 0.9773(5) 0.0443(19) Uiso 1 1 d DU . .
O11 O 0.89592(17) 0.67223(17) 1.0033(4) 0.0287(11) Uiso 1 1 d DU . .
O12 O 0.9487(2) 0.7413(2) 0.9733(5) 0.0509(15) Uiso 1 1 d DU . .
C18 C 1.0923(2) 0.7366(2) 0.8662(5) 0.0274(14) Uiso 1 1 d DU . .
O13 O 1.10406(16) 0.77381(16) 0.8614(4) 0.0209(10) Uiso 1 1 d DU . .
O14 O 1.12501(18) 0.72247(18) 0.8370(4) 0.0380(12) Uiso 1 1 d DU . .
C19 C 0.9705(3) 0.5707(2) 0.9276(5) 0.0417(18) Uiso 1 1 d DU . .
O15 O 0.99668(17) 0.55922(17) 0.9091(4) 0.0273(11) Uiso 1 1 d DU . .
O16 O 0.9283(3) 0.5425(3) 0.9566(6) 0.080(2) Uiso 1 1 d DU . .
C21 C 0.96964(13) 0.28654(10) 0.9479(2) 0.0257(13) Uiso 1 1 d GDU . .
C22 C 0.95487(10) 0.31859(13) 0.9492(2) 0.0256(13) Uiso 1 1 d GDU . .
H22 H 0.9237 0.3091 0.9670 0.031 Uiso 1 1 calc R . .
C23 C 0.98575(14) 0.36460(12) 0.9244(3) 0.0273(14) Uiso 1 1 d GDU . .
C24 C 1.03140(12) 0.37855(10) 0.8982(3) 0.0349(16) Uiso 1 1 d GDU . .
H24 H 1.0525 0.4100 0.8812 0.042 Uiso 1 1 calc R . .
C25 C 1.04617(10) 0.34649(14) 0.8969(2) 0.0395(17) Uiso 1 1 d GDU . .
C26 C 1.01529(14) 0.30049(13) 0.9217(2) 0.0350(16) Uiso 1 1 d GDU . .
H26 H 1.0254 0.2786 0.9208 0.042 Uiso 1 1 calc R . .
C27 C 0.9337(2) 0.2362(2) 0.9751(5) 0.0313(15) Uiso 1 1 d DU . .
O21 O 0.9485(2) 0.2076(2) 0.9738(5) 0.0488(15) Uiso 1 1 d DU . .
O22 O 0.89399(19) 0.22437(19) 0.9998(4) 0.0351(12) Uiso 1 1 d DU . .
C28 C 0.9720(3) 0.4019(2) 0.9231(5) 0.0366(16) Uiso 1 1 d DU . .
O23 O 0.9268(3) 0.3861(3) 0.9502(6) 0.088(3) Uiso 1 1 d DU . .
O24 O 0.99715(18) 0.43880(18) 0.9045(4) 0.0327(12) Uiso 1 1 d DU . .
C29 C 1.0916(2) 0.3583(2) 0.8716(5) 0.0256(13) Uiso 1 1 d DU . .
O25 O 1.1237(2) 0.4024(2) 0.8457(5) 0.0448(13) Uiso 1 1 d DU . .
O26 O 1.10690(15) 0.33353(15) 0.8678(4) 0.0214(10) Uiso 1 1 d DU . .
N30 N 0.83212(17) 0.67046(16) 0.8316(6) 0.0259(13) Uiso 1 1 d DU . .
C30 C 0.7944(3) 0.6438(2) 0.7569(6) 0.0409(18) Uiso 1 1 d DU . .
H30 H 0.7655 0.6235 0.7921 0.049 Uiso 1 1 calc R . .
C31 C 0.7973(3) 0.6454(2) 0.6357(7) 0.0421(18) Uiso 1 1 d DU . .
H31 H 0.7702 0.6260 0.5920 0.050 Uiso 1 1 calc R . .
C32 C 0.83786(18) 0.67392(17) 0.5718(5) 0.0165(12) Uiso 1 1 d DU . .
C33 C 0.8764(3) 0.7009(2) 0.6394(6) 0.0418(18) Uiso 1 1 d DU . .
H33 H 0.9055 0.7213 0.6052 0.050 Uiso 1 1 calc R . .
C34 C 0.8698(3) 0.6963(2) 0.7579(7) 0.0456(19) Uiso 1 1 d DU . .
H34 H 0.8973 0.7152 0.8010 0.055 Uiso 1 1 calc R . .
N35 N 0.83813(15) 0.67265(14) 0.1938(5) 0.0115(11) Uiso 1 1 d DU . .
C35 C 0.8082(2) 0.68256(19) 0.2566(7) 0.0434(18) Uiso 1 1 d DU . .
H35 H 0.7894 0.6911 0.2129 0.052 Uiso 1 1 calc R . .
C36 C 0.8043(3) 0.6806(2) 0.3769(7) 0.048(2) Uiso 1 1 d DU . .
H36 H 0.7833 0.6875 0.4155 0.058 Uiso 1 1 calc R . .
C37 C 0.8313(3) 0.6687(2) 0.4406(7) 0.052(3) Uiso 1 1 d DU . .
C38 C 0.8608(3) 0.6583(2) 0.3791(7) 0.0448(19) Uiso 1 1 d DU . .
H38 H 0.8793 0.6494 0.4230 0.054 Uiso 1 1 calc R . .
C39 C 0.8646(2) 0.6602(2) 0.2597(6) 0.0330(15) Uiso 1 1 d DU . .
H39 H 0.8855 0.6530 0.2216 0.040 Uiso 1 1 calc R . .
N40 N 0.99606(17) 0.49735(16) 0.7180(7) 0.0312(15) Uiso 1 1 d DU . .
C40 C 0.9717(3) 0.5167(3) 0.6639(8) 0.061(2) Uiso 1 1 d DU . .
H40 H 0.9553 0.5292 0.7027 0.074 Uiso 1 1 calc R . .
C41 C 0.9762(3) 0.5137(3) 0.5457(9) 0.070(3) Uiso 1 1 d DU . .
H41 H 0.9603 0.5261 0.5037 0.083 Uiso 1 1 calc R . .
C42 C 0.9968(2) 0.4982(2) 0.4693(7) 0.042(2) Uiso 1 1 d DU . .
C43 C 1.0193(3) 0.4800(3) 0.5290(8) 0.060(2) Uiso 1 1 d DU . .
H43 H 1.0350 0.4674 0.4870 0.072 Uiso 1 1 calc R . .
C44 C 1.0190(3) 0.4800(3) 0.6501(9) 0.068(3) Uiso 1 1 d DU . .
H44 H 1.0352 0.4675 0.6903 0.082 Uiso 1 1 calc R . .
N45 N 0.99807(14) 0.49881(14) 0.0978(5) 0.0147(11) Uiso 1 1 d DU . .
C45 C 0.9757(2) 0.4566(3) 0.1564(6) 0.059(2) Uiso 1 1 d DU . .
H45 H 0.9609 0.4282 0.1149 0.070 Uiso 1 1 calc R . .
C46 C 0.9762(3) 0.4586(3) 0.2772(7) 0.070(3) Uiso 1 1 d DU . .
H46 H 0.9615 0.4305 0.3203 0.084 Uiso 1 1 calc R . .
C47 C 0.99696(19) 0.49880(18) 0.3385(6) 0.0383(19) Uiso 1 1 d DU . .
C48 C 1.0185(3) 0.5394(3) 0.2782(7) 0.071(3) Uiso 1 1 d DU . .
H48 H 1.0327 0.5675 0.3214 0.085 Uiso 1 1 calc R . .
C49 C 1.0203(3) 0.5409(3) 0.1578(7) 0.063(3) Uiso 1 1 d DU . .
H49 H 1.0360 0.5693 0.1163 0.076 Uiso 1 1 calc R . .
N50 N 1.16279(18) 0.8338(2) 0.6651(7) 0.0402(18) Uiso 1 1 d DU . .
C50 C 1.1355(3) 0.7947(3) 0.5961(7) 0.055(2) Uiso 1 1 d DU . .
H50 H 1.1148 0.7669 0.6354 0.066 Uiso 1 1 calc R . .
C51 C 1.1370(2) 0.7945(2) 0.4766(6) 0.0322(15) Uiso 1 1 d DU . .
H51 H 1.1178 0.7672 0.4330 0.039 Uiso 1 1 calc R . .
C52 C 1.16721(19) 0.8351(2) 0.4193(6) 0.0309(17) Uiso 1 1 d DU . .
C53 C 1.1943(2) 0.8736(2) 0.4830(6) 0.0322(15) Uiso 1 1 d DU . .
H53 H 1.2151 0.9012 0.4431 0.039 Uiso 1 1 calc R . .
C54 C 1.1921(2) 0.8733(3) 0.6023(6) 0.0410(18) Uiso 1 1 d DU . .
H54 H 1.2111 0.9010 0.6444 0.049 Uiso 1 1 calc R . .
N55 N 1.17040(13) 0.83209(13) 0.0184(4) 0.0066(9) Uiso 1 1 d DU . .
C55 C 1.1305(3) 0.8202(2) 0.0928(7) 0.0413(18) Uiso 1 1 d DU . .
H55 H 1.1022 0.8108 0.0532 0.050 Uiso 1 1 calc R . .
C56 C 1.1296(3) 0.8213(3) 0.2152(8) 0.066(3) Uiso 1 1 d DU . .
H56 H 1.1010 0.8128 0.2525 0.079 Uiso 1 1 calc R . .
C57 C 1.1684(2) 0.8344(2) 0.2878(7) 0.039(2) Uiso 1 1 d DU . .
C58 C 1.2081(3) 0.8465(2) 0.2245(6) 0.0421(18) Uiso 1 1 d DU . .
H58 H 1.2367 0.8563 0.2630 0.051 Uiso 1 1 calc R . .
C59 C 1.2044(2) 0.8439(2) 0.1050(6) 0.0352(16) Uiso 1 1 d DU . .
H59 H 1.2333 0.8526 0.0697 0.042 Uiso 1 1 calc R . .
O5W O 1.20239(14) 0.79971(14) 0.8543(4) 0.0158(9) Uiso 1 1 d . . .
O1 O 1.12997(16) 0.87236(16) 0.8784(5) 0.0263(10) Uiso 1 1 d . . .
C1M C 1.1317(5) 0.9089(5) 0.8207(13) 0.081(4) Uiso 1 1 d . . .
H1M1 H 1.1096 0.9164 0.8568 0.122 Uiso 1 1 calc R . .
H1M2 H 1.1237 0.9010 0.7372 0.122 Uiso 1 1 calc R . .
H1M3 H 1.1628 0.9356 0.8266 0.122 Uiso 1 1 calc R . .
O3W O 0.9300(3) 0.4676(3) 0.9246(7) 0.0592(19) Uiso 1 1 d . . .
O4W O 1.0729(2) 0.5387(2) 0.9303(5) 0.0390(14) Uiso 1 1 d . . .
O1W O 0.7949(2) 0.5972(2) 0.9907(6) 0.0469(15) Uiso 1 1 d . . .
O2W O 0.86955(15) 0.73961(15) 1.0105(4) 0.0210(9) Uiso 1 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
Ni1 0.0254(5) 0.0303(5) 0.0183(5) -0.0011(3) -0.0013(3) 0.0138(4)
Ni2 0.0420(6) 0.0403(5) 0.0334(8) 0.0009(5) -0.0001(5) 0.0219(4)
Ni3 0.0290(5) 0.0321(5) 0.0204(5) -0.0007(4) -0.0007(4) 0.0149(4)

_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
Ni1 O22 1.973(6) 2_655 ?
Ni1 N30 1.981(7) . ?
Ni1 O11 2.019(5) . ?
Ni1 O2W 2.026(4) . ?
Ni1 N35 2.118(5) 1_556 ?
Ni1 O1W 2.118(7) . ?
Ni2 O3W 1.997(8) . ?
Ni2 O24 2.003(5) . ?
Ni2 O15 2.043(5) . ?
Ni2 N45 2.137(5) 1_556 ?
Ni2 N40 2.156(8) . ?
Ni2 O4W 2.176(6) . ?
Ni3 N55 1.937(5) 1_556 ?
Ni3 O26 2.010(5) 3_775 ?
Ni3 O13 2.063(5) . ?
Ni3 N50 2.070(8) . ?
Ni3 O5W 2.091(4) . ?
Ni3 O1 2.149(5) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C11 C17 1.526(7) . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C13 C18 1.460(7) . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C15 C19 1.517(7) . ?
C17 O11 1.112(9) . ?
C17 O12 1.342(11) . ?
C18 O13 1.107(8) . ?
C18 O14 1.432(9) . ?
C19 O15 1.140(9) . ?
C19 O16 1.292(12) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C21 C27 1.537(6) . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C23 C28 1.534(6) . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C25 C29 1.399(7) . ?
C27 O22 1.217(9) . ?
C27 O21 1.279(9) . ?
O22 Ni1 1.973(6) 3_665 ?
C28 O24 1.113(9) . ?
C28 O23 1.367(12) . ?
C29 O26 1.174(8) . ?
C29 O25 1.355(9) . ?
O26 Ni3 2.010(5) 2_755 ?
N30 C34 1.395(7) . ?
N30 C30 1.407(7) . ?
C30 C31 1.372(8) . ?
C31 C32 1.408(7) . ?
C32 C33 1.380(7) . ?
C32 C37 1.496(8) . ?
C33 C34 1.353(8) . ?
N35 C39 1.373(7) . ?
N35 C35 1.399(7) . ?
N35 Ni1 2.118(5) 1_554 ?
C35 C36 1.364(8) . ?
C36 C37 1.364(8) . ?
C37 C38 1.389(8) . ?
C38 C39 1.354(8) . ?
N40 C44 1.403(8) . ?
N40 C40 1.411(8) . ?
C40 C41 1.353(8) . ?
C41 C42 1.361(8) . ?
C42 C43 1.362(8) . ?
C42 C47 1.478(8) . ?
C43 C44 1.368(9) . ?
N45 C45 1.393(7) . ?
N45 C49 1.398(8) . ?
N45 Ni2 2.137(5) 1_554 ?
C45 C46 1.366(8) . ?
C46 C47 1.359(8) . ?
C47 C48 1.363(8) . ?
C48 C49 1.362(8) . ?
N50 C54 1.387(7) . ?
N50 C50 1.400(8) . ?
C50 C51 1.352(8) . ?
C51 C52 1.385(7) . ?
C52 C53 1.355(7) . ?
C52 C57 1.488(7) . ?
C53 C54 1.350(8) . ?
N55 C59 1.401(7) . ?
N55 C55 1.457(7) . ?
N55 Ni3 1.937(5) 1_554 ?
C55 C56 1.384(8) . ?
C56 C57 1.409(8) . ?
C57 C58 1.381(7) . ?
C58 C59 1.354(8) . ?
O1 C1M 1.364(14) . ?

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
O22 Ni1 N30 85.1(2) 2_655 . ?
O22 Ni1 O11 176.2(2) 2_655 . ?
N30 Ni1 O11 91.56(19) . . ?
O22 Ni1 O2W 90.4(2) 2_655 . ?
N30 Ni1 O2W 90.72(19) . . ?
O11 Ni1 O2W 87.94(19) . . ?
O22 Ni1 N35 94.25(18) 2_655 1_556 ?
N30 Ni1 N35 177.20(16) . 1_556 ?
O11 Ni1 N35 89.01(17) . 1_556 ?
O2W Ni1 N35 86.56(18) . 1_556 ?
O22 Ni1 O1W 86.6(2) 2_655 . ?
N30 Ni1 O1W 85.5(2) . . ?
O11 Ni1 O1W 94.9(2) . . ?
O2W Ni1 O1W 175.3(2) . . ?
N35 Ni1 O1W 97.2(2) 1_556 . ?
O3W Ni2 O24 91.5(3) . . ?
O3W Ni2 O15 86.0(3) . . ?
O24 Ni2 O15 177.2(2) . . ?
O3W Ni2 N45 84.5(3) . 1_556 ?
O24 Ni2 N45 91.19(18) . 1_556 ?
O15 Ni2 N45 90.03(17) . 1_556 ?
O3W Ni2 N40 93.3(3) . . ?
O24 Ni2 N40 88.0(2) . . ?
O15 Ni2 N40 90.64(19) . . ?
N45 Ni2 N40 177.70(18) 1_556 . ?
O3W Ni2 O4W 167.5(3) . . ?
O24 Ni2 O4W 93.3(2) . . ?
O15 Ni2 O4W 89.4(2) . . ?
N45 Ni2 O4W 83.9(2) 1_556 . ?
N40 Ni2 O4W 98.3(2) . . ?
N55 Ni3 O26 82.50(17) 1_556 3_775 ?
N55 Ni3 O13 86.83(17) 1_556 . ?
O26 Ni3 O13 169.30(17) 3_775 . ?
N55 Ni3 N50 174.71(17) 1_556 . ?
O26 Ni3 N50 98.3(2) 3_775 . ?
O13 Ni3 N50 92.3(2) . . ?
N55 Ni3 O5W 81.53(17) 1_556 . ?
O26 Ni3 O5W 86.77(18) 3_775 . ?
O13 Ni3 O5W 90.91(18) . . ?
N50 Ni3 O5W 93.28(18) . . ?
N55 Ni3 O1 87.38(18) 1_556 . ?
O26 Ni3 O1 90.55(19) 3_775 . ?
O13 Ni3 O1 89.74(18) . . ?
N50 Ni3 O1 97.83(19) . . ?
O5W Ni3 O1 168.84(18) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 C17 125.3(4) . . ?
C16 C11 C17 114.7(4) . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 C18 114.4(4) . . ?
C14 C13 C18 125.6(4) . . ?
C13 C14 C15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 C19 121.5(4) . . ?
C14 C15 C19 118.5(4) . . ?
C15 C16 C11 120.0 . . ?
O11 C17 O12 119.7(7) . . ?
O11 C17 C11 128.4(7) . . ?
O12 C17 C11 111.9(6) . . ?
C17 O11 Ni1 140.2(5) . . ?
O13 C18 O14 117.5(6) . . ?
O13 C18 C13 125.9(6) . . ?
O14 C18 C13 116.5(5) . . ?
C18 O13 Ni3 137.7(5) . . ?
O15 C19 O16 123.0(7) . . ?
O15 C19 C15 120.0(7) . . ?
O16 C19 C15 116.8(7) . . ?
C19 O15 Ni2 137.8(5) . . ?
C22 C21 C26 120.0 . . ?
C22 C21 C27 117.5(4) . . ?
C26 C21 C27 122.5(4) . . ?
C23 C22 C21 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 C28 123.1(4) . . ?
C24 C23 C28 116.9(4) . . ?
C25 C24 C23 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 C29 122.8(4) . . ?
C26 C25 C29 117.2(4) . . ?
C25 C26 C21 120.0 . . ?
O22 C27 O21 122.0(6) . . ?
O22 C27 C21 122.1(6) . . ?
O21 C27 C21 115.9(6) . . ?
C27 O22 Ni1 135.7(5) . 3_665 ?
O24 C28 O23 123.3(7) . . ?
O24 C28 C23 122.6(7) . . ?
O23 C28 C23 114.1(7) . . ?
C28 O24 Ni2 137.7(5) . . ?
O26 C29 O25 112.0(6) . . ?
O26 C29 C25 127.3(6) . . ?
O25 C29 C25 120.7(6) . . ?
C29 O26 Ni3 144.4(5) . 2_755 ?
C34 N30 C30 106.4(7) . . ?
C34 N30 Ni1 125.0(5) . . ?
C30 N30 Ni1 128.4(5) . . ?
C31 C30 N30 123.4(7) . . ?
C30 C31 C32 124.3(7) . . ?
C33 C32 C31 115.5(6) . . ?
C33 C32 C37 131.4(6) . . ?
C31 C32 C37 113.1(6) . . ?
C34 C33 C32 115.3(7) . . ?
C33 C34 N30 135.0(8) . . ?
C39 N35 C35 116.5(6) . . ?
C39 N35 Ni1 124.0(4) . 1_554 ?
C35 N35 Ni1 119.0(4) . 1_554 ?
C36 C35 N35 123.8(8) . . ?
C37 C36 C35 118.6(8) . . ?
C36 C37 C38 118.0(8) . . ?
C36 C37 C32 124.6(6) . . ?
C38 C37 C32 116.4(6) . . ?
C39 C38 C37 123.3(8) . . ?
C38 C39 N35 119.7(7) . . ?
C44 N40 C40 121.1(8) . . ?
C44 N40 Ni2 122.6(6) . . ?
C40 N40 Ni2 116.3(6) . . ?
C41 C40 N40 106.4(9) . . ?
C40 C41 C42 138.7(11) . . ?
C41 C42 C43 110.9(9) . . ?
C41 C42 C47 128.9(8) . . ?
C43 C42 C47 120.2(7) . . ?
C42 C43 C44 119.4(9) . . ?
C43 C44 N40 123.5(10) . . ?
C45 N45 C49 122.6(6) . . ?
C45 N45 Ni2 118.7(4) . 1_554 ?
C49 N45 Ni2 118.7(4) . 1_554 ?
C46 C45 N45 116.0(6) . . ?
C47 C46 C45 123.0(7) . . ?
C46 C47 C48 119.3(7) . . ?
C46 C47 C42 120.0(5) . . ?
C48 C47 C42 120.7(5) . . ?
C49 C48 C47 121.8(7) . . ?
C48 C49 N45 117.2(7) . . ?
C54 N50 C50 115.3(8) . . ?
C54 N50 Ni3 119.3(5) . . ?
C50 N50 Ni3 125.2(6) . . ?
C51 C50 N50 123.6(9) . . ?
C50 C51 C52 118.1(7) . . ?
C53 C52 C51 120.1(7) . . ?
C53 C52 C57 122.4(6) . . ?
C51 C52 C57 117.6(6) . . ?
C54 C53 C52 121.0(7) . . ?
C53 C54 N50 121.8(8) . . ?
C59 N55 C55 100.3(6) . . ?
C59 N55 Ni3 139.1(4) . 1_554 ?
C55 N55 Ni3 120.0(4) . 1_554 ?
C56 C55 N55 126.8(8) . . ?
C55 C56 C57 124.1(9) . . ?
C58 C57 C56 113.2(8) . . ?
C58 C57 C52 122.8(6) . . ?
C56 C57 C52 124.0(6) . . ?
C59 C58 C57 117.0(8) . . ?
C58 C59 N55 138.6(7) . . ?
C1M O1 Ni3 131.5(7) . . ?

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
C16 C11 C12 C13 0.0 . . . . ?
C17 C11 C12 C13 -179.6(2) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C11 C12 C13 C18 -179.3(2) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C18 C13 C14 C15 179.2(2) . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C13 C14 C15 C19 179.3(2) . . . . ?
C14 C15 C16 C11 0.0 . . . . ?
C19 C15 C16 C11 -179.3(2) . . . . ?
C12 C11 C16 C15 0.0 . . . . ?
C17 C11 C16 C15 179.6(2) . . . . ?
C12 C11 C17 O11 -178.2(4) . . . . ?
C16 C11 C17 O11 2.3(6) . . . . ?
C12 C11 C17 O12 -0.8(5) . . . . ?
C16 C11 C17 O12 179.6(3) . . . . ?
O12 C17 O11 Ni1 24.1(9) . . . . ?
C11 C17 O11 Ni1 -158.7(4) . . . . ?
O22 Ni1 O11 C17 39(4) 2_655 . . . ?
N30 Ni1 O11 C17 66.3(7) . . . . ?
O2W Ni1 O11 C17 -24.3(7) . . . . ?
N35 Ni1 O11 C17 -110.9(7) 1_556 . . . ?
O1W Ni1 O11 C17 151.9(7) . . . . ?
C12 C13 C18 O13 -2.2(6) . . . . ?
C14 C13 C18 O13 178.5(4) . . . . ?
C12 C13 C18 O14 -178.8(3) . . . . ?
C14 C13 C18 O14 2.0(5) . . . . ?
O14 C18 O13 Ni3 -13.5(8) . . . . ?
C13 C18 O13 Ni3 169.9(3) . . . . ?
N55 Ni3 O13 C18 -83.8(6) 1_556 . . . ?
O26 Ni3 O13 C18 -79.7(12) 3_775 . . . ?
N50 Ni3 O13 C18 91.0(6) . . . . ?
O5W Ni3 O13 C18 -2.4(6) . . . . ?
O1 Ni3 O13 C18 -171.2(6) . . . . ?
C16 C15 C19 O15 -178.1(4) . . . . ?
C14 C15 C19 O15 2.6(6) . . . . ?
C16 C15 C19 O16 -1.7(5) . . . . ?
C14 C15 C19 O16 179.1(4) . . . . ?
O16 C19 O15 Ni2 -1.0(9) . . . . ?
C15 C19 O15 Ni2 175.2(3) . . . . ?
O3W Ni2 O15 C19 10.6(6) . . . . ?
O24 Ni2 O15 C19 41(5) . . . . ?
N45 Ni2 O15 C19 -73.9(6) 1_556 . . . ?
N40 Ni2 O15 C19 103.9(6) . . . . ?
O4W Ni2 O15 C19 -157.8(6) . . . . ?
C26 C21 C22 C23 0.0 . . . . ?
C27 C21 C22 C23 -179.5(2) . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C21 C22 C23 C28 179.5(2) . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C28 C23 C24 C25 -179.6(2) . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C23 C24 C25 C29 -179.8(2) . . . . ?
C24 C25 C26 C21 0.0 . . . . ?
C29 C25 C26 C21 179.8(2) . . . . ?
C22 C21 C26 C25 0.0 . . . . ?
C27 C21 C26 C25 179.5(2) . . . . ?
C22 C21 C27 O22 -1.7(5) . . . . ?
C26 C21 C27 O22 178.8(4) . . . . ?
C22 C21 C27 O21 -179.7(3) . . . . ?
C26 C21 C27 O21 0.8(5) . . . . ?
O21 C27 O22 Ni1 -18.2(8) . . . 3_665 ?
C21 C27 O22 Ni1 164.0(3) . . . 3_665 ?
C22 C23 C28 O24 179.0(4) . . . . ?
C24 C23 C28 O24 -1.4(6) . . . . ?
C22 C23 C28 O23 0.9(5) . . . . ?
C24 C23 C28 O23 -179.6(3) . . . . ?
O23 C28 O24 Ni2 5.9(9) . . . . ?
C23 C28 O24 Ni2 -172.1(3) . . . . ?
O3W Ni2 O24 C28 -12.7(6) . . . . ?
O15 Ni2 O24 C28 -44(5) . . . . ?
N45 Ni2 O24 C28 71.8(6) 1_556 . . . ?
N40 Ni2 O24 C28 -106.0(6) . . . . ?
O4W Ni2 O24 C28 155.7(6) . . . . ?
C24 C25 C29 O26 -179.4(4) . . . . ?
C26 C25 C29 O26 0.8(6) . . . . ?
C24 C25 C29 O25 -0.7(5) . . . . ?
C26 C25 C29 O25 179.5(3) . . . . ?
O25 C29 O26 Ni3 6.5(8) . . . 2_755 ?
C25 C29 O26 Ni3 -174.7(3) . . . 2_755 ?
O22 Ni1 N30 C34 139.6(4) 2_655 . . . ?
O11 Ni1 N30 C34 -38.7(4) . . . . ?
O2W Ni1 N30 C34 49.3(4) . . . . ?
N35 Ni1 N30 C34 63(4) 1_556 . . . ?
O1W Ni1 N30 C34 -133.5(4) . . . . ?
O22 Ni1 N30 C30 -45.0(3) 2_655 . . . ?
O11 Ni1 N30 C30 136.7(3) . . . . ?
O2W Ni1 N30 C30 -135.3(3) . . . . ?
N35 Ni1 N30 C30 -122(4) 1_556 . . . ?
O1W Ni1 N30 C30 41.9(3) . . . . ?
C34 N30 C30 C31 -0.5(2) . . . . ?
Ni1 N30 C30 C31 -176.5(2) . . . . ?
N30 C30 C31 C32 -0.4(2) . . . . ?
C30 C31 C32 C33 0.8(5) . . . . ?
C30 C31 C32 C37 179.8(2) . . . . ?
C31 C32 C33 C34 -0.2(6) . . . . ?
C37 C32 C33 C34 -179.0(5) . . . . ?
C32 C33 C34 N30 -0.9(9) . . . . ?
C30 N30 C34 C33 1.2(7) . . . . ?
Ni1 N30 C34 C33 177.5(5) . . . . ?
C39 N35 C35 C36 0.2(3) . . . . ?
Ni1 N35 C35 C36 173.1(3) 1_554 . . . ?
N35 C35 C36 C37 0.4(3) . . . . ?
C35 C36 C37 C38 -1.0(6) . . . . ?
C35 C36 C37 C32 167.4(6) . . . . ?
C33 C32 C37 C36 -115.3(7) . . . . ?
C31 C32 C37 C36 65.9(7) . . . . ?
C33 C32 C37 C38 53.2(8) . . . . ?
C31 C32 C37 C38 -125.6(5) . . . . ?
C36 C37 C38 C39 1.0(8) . . . . ?
C32 C37 C38 C39 -168.3(6) . . . . ?
C37 C38 C39 N35 -0.4(8) . . . . ?
C35 N35 C39 C38 -0.2(5) . . . . ?
Ni1 N35 C39 C38 -172.7(4) 1_554 . . . ?
O3W Ni2 N40 C44 -128.2(4) . . . . ?
O24 Ni2 N40 C44 -36.8(4) . . . . ?
O15 Ni2 N40 C44 145.7(4) . . . . ?
N45 Ni2 N40 C44 -107(5) 1_556 . . . ?
O4W Ni2 N40 C44 56.2(4) . . . . ?
O3W Ni2 N40 C40 54.6(4) . . . . ?
O24 Ni2 N40 C40 146.0(3) . . . . ?
O15 Ni2 N40 C40 -31.5(3) . . . . ?
N45 Ni2 N40 C40 76(5) 1_556 . . . ?
O4W Ni2 N40 C40 -121.0(4) . . . . ?
C44 N40 C40 C41 0.1(2) . . . . ?
Ni2 N40 C40 C41 177.4(2) . . . . ?
N40 C40 C41 C42 -0.2(3) . . . . ?
C40 C41 C42 C43 0.6(6) . . . . ?
C40 C41 C42 C47 -179.9(3) . . . . ?
C41 C42 C43 C44 -0.8(6) . . . . ?
C47 C42 C43 C44 179.6(4) . . . . ?
C42 C43 C44 N40 0.9(7) . . . . ?
C40 N40 C44 C43 -0.5(6) . . . . ?
Ni2 N40 C44 C43 -177.6(4) . . . . ?
C49 N45 C45 C46 0.7(3) . . . . ?
Ni2 N45 C45 C46 -179.5(3) 1_554 . . . ?
N45 C45 C46 C47 0.3(3) . . . . ?
C45 C46 C47 C48 -0.3(6) . . . . ?
C45 C46 C47 C42 -179.0(5) . . . . ?
C41 C42 C47 C46 -114.9(6) . . . . ?
C43 C42 C47 C46 64.6(7) . . . . ?
C41 C42 C47 C48 66.4(7) . . . . ?
C43 C42 C47 C48 -114.1(7) . . . . ?
C46 C47 C48 C49 -0.7(8) . . . . ?
C42 C47 C48 C49 178.0(6) . . . . ?
C47 C48 C49 N45 1.5(8) . . . . ?
C45 N45 C49 C48 -1.5(6) . . . . ?
Ni2 N45 C49 C48 178.6(4) 1_554 . . . ?
N55 Ni3 N50 C54 -114(2) 1_556 . . . ?
O26 Ni3 N50 C54 -15.7(4) 3_775 . . . ?
O13 Ni3 N50 C54 166.1(3) . . . . ?
O5W Ni3 N50 C54 -102.9(3) . . . . ?
O1 Ni3 N50 C54 76.0(4) . . . . ?
N55 Ni3 N50 C50 61(2) 1_556 . . . ?
O26 Ni3 N50 C50 159.5(3) 3_775 . . . ?
O13 Ni3 N50 C50 -18.8(3) . . . . ?
O5W Ni3 N50 C50 72.3(3) . . . . ?
O1 Ni3 N50 C50 -108.8(3) . . . . ?
C54 N50 C50 C51 0.3(3) . . . . ?
Ni3 N50 C50 C51 -175.0(2) . . . . ?
N50 C50 C51 C52 0.1(2) . . . . ?
C50 C51 C52 C53 0.0(5) . . . . ?
C50 C51 C52 C57 -179.8(3) . . . . ?
C51 C52 C53 C54 -0.6(7) . . . . ?
C57 C52 C53 C54 179.2(5) . . . . ?
C52 C53 C54 N50 1.1(8) . . . . ?
C50 N50 C54 C53 -0.9(6) . . . . ?
Ni3 N50 C54 C53 174.7(4) . . . . ?
C59 N55 C55 C56 0.0(2) . . . . ?
Ni3 N55 C55 C56 -172.9(3) 1_554 . . . ?
N55 C55 C56 C57 -0.2(3) . . . . ?
C55 C56 C57 C58 0.5(5) . . . . ?
C55 C56 C57 C52 -179.3(5) . . . . ?
C53 C52 C57 C58 57.3(7) . . . . ?
C51 C52 C57 C58 -122.9(6) . . . . ?
C53 C52 C57 C56 -122.8(6) . . . . ?
C51 C52 C57 C56 57.0(7) . . . . ?
C56 C57 C58 C59 -0.6(7) . . . . ?
C52 C57 C58 C59 179.2(6) . . . . ?
C57 C58 C59 N55 0.6(9) . . . . ?
C55 N55 C59 C58 -0.2(7) . . . . ?
Ni3 N55 C59 C58 170.4(5) 1_554 . . . ?
N55 Ni3 O1 C1M 141.1(9) 1_556 . . . ?
O26 Ni3 O1 C1M 58.6(9) 3_775 . . . ?
O13 Ni3 O1 C1M -132.1(9) . . . . ?
N50 Ni3 O1 C1M -39.8(9) . . . . ?
O5W Ni3 O1 C1M 134.6(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.46
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         6.370
_refine_diff_density_min         -2.565
_refine_diff_density_rms         0.191