# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-Co
_database_code_depnum_ccdc_archive 'CCDC 1422947'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        1-Co
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C140 H132 Co8 O42 S8, 8(C3 H7 N O)'
_chemical_formula_sum            'C164 H188 Co8 N8 O50 S8'
_chemical_formula_weight         3799.14

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   12.9710(6)
_cell_length_b                   13.7364(6)
_cell_length_c                   26.0130(11)
_cell_angle_alpha                79.6870(10)
_cell_angle_beta                 81.6550(10)
_cell_angle_gamma                67.1060(10)
_cell_volume                     4186.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9174
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      28.41

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1972
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5144
_exptl_absorpt_correction_T_max  0.7887
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41176
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.00
_reflns_number_total             14679
_reflns_number_gt                12290
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The crystal was poorly diffraction, especially at higher Bragg angles. 
The situation did not improve even with very long exposure time.
The large anisotropic Uij values of the DMF indicates a possible
disorder. Use of L.S. restraints for the refinement of the
geometry and the displacement parameters (DFIX, SADI, SIMU, DELU):
DFIX 2.2 0.02 O16 O17 O20 O21 n4 o25 n3 o24 c80 c81 c80 c82
DFIX 1.23 0.02 C56 O16 C56 O17 C70 O20 C70 O21 C80 O25
SADI 0.005 C57 O16 C57 O17
SADI 0.005 C57 C58 C57 C62
simu 0.01 c75 > C82
isor 0.01 O17 C58
simu 0.005 C56 O1 O16 O17 C58
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1102P)²+25.2437P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14679
_refine_ls_number_parameters     1100
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0803
_refine_ls_wR_factor_ref         0.2233
_refine_ls_wR_factor_gt          0.2101
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.069
_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
Co1 Co 1.01097(7) -0.26239(6) 0.29513(3) 0.0310(2) Uani 1 1 d . . .
Co2 Co 1.24629(7) -0.36034(6) 0.32380(3) 0.0293(2) Uani 1 1 d . . .
Co3 Co 1.29379(7) -0.17875(6) 0.26652(3) 0.0297(2) Uani 1 1 d . . .
Co4 Co 1.05713(7) -0.07790(6) 0.23682(3) 0.0320(2) Uani 1 1 d . . .
S1 S 0.94433(11) -0.39158(10) 0.22889(5) 0.0215(3) Uani 1 1 d . . .
S2 S 1.38826(11) -0.57658(10) 0.28556(5) 0.0218(3) Uani 1 1 d . . .
S3 S 1.47818(12) -0.22763(11) 0.17519(5) 0.0245(3) Uani 1 1 d . . .
S4 S 1.03295(11) -0.04102(10) 0.11739(5) 0.0241(3) Uani 1 1 d . . .
O1 O 1.1375(4) -0.1972(3) 0.30100(15) 0.0335(9) Uani 1 1 d . . .
O2 O 0.9128(3) -0.3401(3) 0.27607(14) 0.0279(8) Uani 1 1 d . . .
O3 O 0.8734(3) -0.4438(3) 0.21961(15) 0.0257(8) Uani 1 1 d . . .
O4 O 1.1466(3) -0.3988(3) 0.28315(14) 0.0256(8) Uani 1 1 d . . .
O5 O 1.3488(3) -0.5215(3) 0.33182(14) 0.0275(8) Uani 1 1 d . . .
O6 O 1.4548(3) -0.6877(3) 0.29543(15) 0.0285(8) Uani 1 1 d . . .
O7 O 1.3418(4) -0.3378(3) 0.25402(17) 0.0359(10) Uani 1 1 d . . .
O8 O 1.4392(3) -0.1732(3) 0.22185(15) 0.0290(8) Uani 1 1 d . . .
O9 O 1.5771(3) -0.2175(3) 0.14586(15) 0.0314(9) Uani 1 1 d . . .
O10 O 1.2155(3) -0.1308(3) 0.19820(14) 0.0264(8) Uani 1 1 d . . .
O11 O 1.0001(3) 0.0098(3) 0.16476(16) 0.0292(8) Uani 1 1 d . . .
O12 O 0.9918(3) 0.0261(3) 0.06997(15) 0.0297(8) Uani 1 1 d . . .
O13 O 1.0240(4) -0.2023(3) 0.21610(15) 0.0354(10) Uani 1 1 d . . .
O14 O 0.9875(4) -0.3045(5) 0.37176(18) 0.0514(13) Uani 1 1 d . . .
O15 O 1.1625(5) -0.3691(4) 0.39365(18) 0.0546(13) Uani 1 1 d . . .
O16 O 1.3472(7) -0.3465(6) 0.3746(3) 0.0915(19) Uani 1 1 d DU . .
O17 O 1.3797(7) -0.2078(7) 0.3345(2) 0.100(2) Uani 1 1 d DU . .
O18 O 0.7487(4) 0.0337(4) 0.7155(2) 0.0488(12) Uani 1 1 d . . .
O19 O 0.9237(4) -0.0422(3) 0.73832(18) 0.0448(11) Uani 1 1 d . . .
O20 O 1.0966(7) 0.0158(11) 0.7224(3) 0.173(6) Uani 1 1 d D . .
O21 O 1.1401(7) 0.1406(6) 0.6831(3) 0.094(2) Uani 1 1 d D . .
C1 C 1.1054(4) -0.5703(4) 0.20097(19) 0.0208(10) Uani 1 1 d . . .
H1A H 1.0462 -0.5721 0.1840 0.025 Uiso 1 1 calc R . .
C2 C 1.0833(4) -0.4868(4) 0.22998(19) 0.0210(10) Uani 1 1 d . . .
C3 C 1.1667(4) -0.4780(4) 0.25669(19) 0.0209(10) Uani 1 1 d . . .
C4 C 1.2720(4) -0.5631(4) 0.25269(19) 0.0215(10) Uani 1 1 d . . .
C5 C 1.2934(4) -0.6455(4) 0.22314(19) 0.0215(10) Uani 1 1 d . . .
H5A H 1.3663 -0.6996 0.2214 0.026 Uiso 1 1 calc R . .
C6 C 1.2105(4) -0.6505(4) 0.19605(19) 0.0211(10) Uani 1 1 d . . .
C7 C 1.2361(4) -0.7363(4) 0.1602(2) 0.0232(11) Uani 1 1 d . . .
C8 C 1.3361(5) -0.8365(5) 0.1764(2) 0.0340(13) Uani 1 1 d . . .
H8A H 1.3498 -0.8890 0.1526 0.051 Uiso 1 1 calc R . .
H8B H 1.3201 -0.8664 0.2123 0.051 Uiso 1 1 calc R . .
H8C H 1.4027 -0.8185 0.1745 0.051 Uiso 1 1 calc R . .
C9 C 1.1344(5) -0.7658(5) 0.1598(2) 0.0298(12) Uani 1 1 d . . .
H9A H 1.1530 -0.8204 0.1367 0.045 Uiso 1 1 calc R . .
H9B H 1.0713 -0.7024 0.1470 0.045 Uiso 1 1 calc R . .
H9C H 1.1136 -0.7937 0.1955 0.045 Uiso 1 1 calc R . .
C10 C 1.2639(5) -0.6869(5) 0.1044(2) 0.0347(13) Uani 1 1 d . . .
H10A H 1.2808 -0.7388 0.0799 0.052 Uiso 1 1 calc R . .
H10B H 1.3291 -0.6675 0.1042 0.052 Uiso 1 1 calc R . .
H10C H 1.1993 -0.6229 0.0935 0.052 Uiso 1 1 calc R . .
C11 C 1.5665(4) -0.5832(4) 0.2176(2) 0.0223(10) Uani 1 1 d . . .
H11A H 1.5849 -0.6580 0.2257 0.027 Uiso 1 1 calc R . .
C12 C 1.4688(4) -0.5151(4) 0.24136(19) 0.0213(10) Uani 1 1 d . . .
C13 C 1.4338(4) -0.4015(4) 0.2311(2) 0.0233(11) Uani 1 1 d . . .
C14 C 1.5071(5) -0.3656(4) 0.1939(2) 0.0238(11) Uani 1 1 d . . .
C15 C 1.6056(4) -0.4351(4) 0.1711(2) 0.0224(11) Uani 1 1 d . . .
H15A H 1.6522 -0.4064 0.1469 0.027 Uiso 1 1 calc R . .
C16 C 1.6384(4) -0.5455(4) 0.1822(2) 0.0221(10) Uani 1 1 d . . .
C17 C 1.7470(4) -0.6237(5) 0.1581(2) 0.0271(12) Uani 1 1 d . . .
C18 C 1.8157(5) -0.5671(5) 0.1218(2) 0.0353(13) Uani 1 1 d . . .
H18A H 1.8350 -0.5230 0.1415 0.053 Uiso 1 1 calc R . .
H18B H 1.7716 -0.5219 0.0929 0.053 Uiso 1 1 calc R . .
H18C H 1.8847 -0.6202 0.1077 0.053 Uiso 1 1 calc R . .
C19 C 1.7185(5) -0.6929(5) 0.1261(3) 0.0396(15) Uani 1 1 d . . .
H19A H 1.6747 -0.7304 0.1489 0.059 Uiso 1 1 calc R . .
H19B H 1.7882 -0.7450 0.1119 0.059 Uiso 1 1 calc R . .
H19C H 1.6746 -0.6472 0.0973 0.059 Uiso 1 1 calc R . .
C20 C 1.8184(5) -0.6952(5) 0.2026(2) 0.0378(14) Uani 1 1 d . . .
H20A H 1.8363 -0.6509 0.2229 0.057 Uiso 1 1 calc R . .
H20B H 1.8882 -0.7460 0.1877 0.057 Uiso 1 1 calc R . .
H20C H 1.7764 -0.7342 0.2256 0.057 Uiso 1 1 calc R . .
C21 C 1.4077(5) -0.1822(4) 0.0792(2) 0.0266(11) Uani 1 1 d . . .
H21A H 1.4864 -0.2113 0.0701 0.032 Uiso 1 1 calc R . .
C22 C 1.3700(5) -0.1782(4) 0.1319(2) 0.0245(11) Uani 1 1 d . . .
C23 C 1.2532(5) -0.1351(4) 0.1490(2) 0.0242(11) Uani 1 1 d . . .
C24 C 1.1811(4) -0.0970(4) 0.1071(2) 0.0233(11) Uani 1 1 d . . .
C25 C 1.2220(5) -0.1035(4) 0.0546(2) 0.0251(11) Uani 1 1 d . . .
H25A H 1.1700 -0.0780 0.0285 0.030 Uiso 1 1 calc R . .
C26 C 1.3361(5) -0.1459(4) 0.0392(2) 0.0252(11) Uani 1 1 d . . .
C27 C 1.3826(5) -0.1526(5) -0.0182(2) 0.0300(12) Uani 1 1 d . . .
C28 C 1.2889(5) -0.1069(6) -0.0557(2) 0.0401(15) Uani 1 1 d . . .
H28A H 1.2381 -0.1458 -0.0467 0.060 Uiso 1 1 calc R . .
H28B H 1.3219 -0.1143 -0.0918 0.060 Uiso 1 1 calc R . .
H28C H 1.2468 -0.0313 -0.0525 0.060 Uiso 1 1 calc R . .
C29 C 1.4611(6) -0.0904(6) -0.0327(2) 0.0381(14) Uani 1 1 d . . .
H29A H 1.4903 -0.0941 -0.0695 0.057 Uiso 1 1 calc R . .
H29B H 1.5238 -0.1218 -0.0103 0.057 Uiso 1 1 calc R . .
H29C H 1.4194 -0.0158 -0.0274 0.057 Uiso 1 1 calc R . .
C30 C 1.4488(6) -0.2694(5) -0.0251(2) 0.0379(14) Uani 1 1 d . . .
H30A H 1.3990 -0.3094 -0.0159 0.057 Uiso 1 1 calc R . .
H30B H 1.5105 -0.2993 -0.0022 0.057 Uiso 1 1 calc R . .
H30C H 1.4793 -0.2744 -0.0617 0.057 Uiso 1 1 calc R . .
C31 C 0.9531(4) -0.1662(4) 0.0804(2) 0.0228(11) Uani 1 1 d . . .
H31A H 0.9559 -0.1205 0.0486 0.027 Uiso 1 1 calc R . .
C32 C 0.9875(4) -0.1489(4) 0.1256(2) 0.0235(11) Uani 1 1 d . . .
C33 C 0.9880(4) -0.2147(4) 0.1741(2) 0.0238(11) Uani 1 1 d . . .
C34 C 0.9474(4) -0.2965(4) 0.1734(2) 0.0221(10) Uani 1 1 d . . .
C35 C 0.9122(4) -0.3112(4) 0.1281(2) 0.0213(10) Uani 1 1 d . . .
H35A H 0.8852 -0.3670 0.1300 0.026 Uiso 1 1 calc R . .
C36 C 0.9150(4) -0.2477(4) 0.0806(2) 0.0230(11) Uani 1 1 d . A .
C37 C 0.8765(5) -0.2673(5) 0.0317(2) 0.0267(11) Uani 1 1 d . . .
C38' C 0.9702(16) -0.2794(18) -0.0140(7) 0.042(5) Uani 0.356(11) 1 d P A 2
H38A H 1.0356 -0.3442 -0.0052 0.063 Uiso 0.356(11) 1 calc PR A 2
H38B H 0.9919 -0.2173 -0.0197 0.063 Uiso 0.356(11) 1 calc PR A 2
H38C H 0.9421 -0.2845 -0.0461 0.063 Uiso 0.356(11) 1 calc PR A 2
C38 C 0.8926(11) -0.1955(9) -0.0155(3) 0.043(3) Uani 0.644(11) 1 d P A 1
H38D H 0.9705 -0.2243 -0.0305 0.065 Uiso 0.644(11) 1 calc PR A 1
H38E H 0.8761 -0.1247 -0.0060 0.065 Uiso 0.644(11) 1 calc PR A 1
H38F H 0.8419 -0.1896 -0.0414 0.065 Uiso 0.644(11) 1 calc PR A 1
C39' C 0.7773(14) -0.1581(13) 0.0102(7) 0.035(4) Uani 0.356(11) 1 d P A 2
H39A H 0.7125 -0.1423 0.0363 0.052 Uiso 0.356(11) 1 calc PR A 2
H39B H 0.7550 -0.1667 -0.0226 0.052 Uiso 0.356(11) 1 calc PR A 2
H39C H 0.8044 -0.0993 0.0038 0.052 Uiso 0.356(11) 1 calc PR A 2
C39 C 0.7539(7) -0.2573(7) 0.0446(3) 0.027(2) Uani 0.644(11) 1 d P A 1
H39D H 0.7513 -0.3230 0.0658 0.041 Uiso 0.644(11) 1 calc PR A 1
H39E H 0.7187 -0.2455 0.0120 0.041 Uiso 0.644(11) 1 calc PR A 1
H39F H 0.7132 -0.1969 0.0643 0.041 Uiso 0.644(11) 1 calc PR A 1
C40 C 0.9466(7) -0.3864(7) 0.0230(3) 0.029(2) Uani 0.644(11) 1 d P A 1
H40A H 0.9996 -0.4206 0.0501 0.044 Uiso 0.644(11) 1 calc PR A 1
H40B H 0.9882 -0.3882 -0.0116 0.044 Uiso 0.644(11) 1 calc PR A 1
H40C H 0.8958 -0.4245 0.0251 0.044 Uiso 0.644(11) 1 calc PR A 1
C40' C 0.8326(19) -0.3518(15) 0.0372(7) 0.043(5) Uani 0.356(11) 1 d P A 2
H40D H 0.8893 -0.4197 0.0508 0.065 Uiso 0.356(11) 1 calc PR A 2
H40E H 0.8140 -0.3573 0.0029 0.065 Uiso 0.356(11) 1 calc PR A 2
H40F H 0.7648 -0.3352 0.0616 0.065 Uiso 0.356(11) 1 calc PR A 2
C41 C 1.0580(6) -0.3399(5) 0.4050(3) 0.0422(15) Uani 1 1 d . . .
C42 C 1.0168(7) -0.3522(5) 0.4610(2) 0.0457(17) Uani 1 1 d . . .
C43 C 0.9064(8) -0.3384(9) 0.4759(3) 0.072(3) Uani 1 1 d . . .
H43A H 0.8544 -0.3152 0.4499 0.087 Uiso 1 1 calc R . .
C44 C 0.8694(9) -0.3573(9) 0.5277(3) 0.076(3) Uani 1 1 d . . .
H44A H 0.7923 -0.3458 0.5368 0.092 Uiso 1 1 calc R . .
C45 C 0.9432(8) -0.3931(6) 0.5669(3) 0.056(2) Uani 1 1 d . . .
C46 C 1.0533(10) -0.4039(10) 0.5515(3) 0.089(3) Uani 1 1 d . . .
H46A H 1.1054 -0.4252 0.5774 0.107 Uiso 1 1 calc R . .
C47 C 1.0894(9) -0.3845(9) 0.4995(3) 0.081(3) Uani 1 1 d . . .
H47A H 1.1659 -0.3937 0.4903 0.097 Uiso 1 1 calc R . .
C48 C 0.9036(9) -0.4150(6) 0.6239(3) 0.061(2) Uani 1 1 d . . .
H48A H 0.9603 -0.4801 0.6410 0.074 Uiso 1 1 calc R . .
H48B H 0.8324 -0.4269 0.6263 0.074 Uiso 1 1 calc R . .
C49 C 0.8858(8) -0.3201(6) 0.6514(3) 0.050(2) Uani 1 1 d . . .
C50 C 0.7839(8) -0.2359(6) 0.6518(3) 0.0506(19) Uani 1 1 d . . .
H50A H 0.7231 -0.2401 0.6370 0.061 Uiso 1 1 calc R . .
C51 C 0.7680(7) -0.1452(6) 0.6733(3) 0.0469(17) Uani 1 1 d . . .
H51A H 0.6967 -0.0883 0.6737 0.056 Uiso 1 1 calc R . .
C52 C 0.8561(6) -0.1381(5) 0.6942(2) 0.0355(14) Uani 1 1 d . . .
C53 C 0.9600(7) -0.2240(5) 0.6951(3) 0.0452(16) Uani 1 1 d . . .
H53A H 1.0205 -0.2203 0.7102 0.054 Uiso 1 1 calc R . .
C54 C 0.9735(7) -0.3139(5) 0.6739(3) 0.0504(19) Uani 1 1 d . . .
H54A H 1.0437 -0.3721 0.6746 0.060 Uiso 1 1 calc R . .
C55 C 0.8414(6) -0.0405(5) 0.7179(2) 0.0383(14) Uani 1 1 d . . .
C56 C 1.3666(10) -0.2618(9) 0.3755(4) 0.0799(19) Uani 1 1 d DU . .
C57 C 1.4134(11) -0.2606(6) 0.4205(3) 0.141(8) Uani 1 1 d D . .
C58 C 1.4125(12) -0.3278(11) 0.4691(4) 0.108(4) Uani 1 1 d DU . .
H58A H 1.3856 -0.3835 0.4703 0.130 Uiso 1 1 calc R . .
C59 C 1.4480(13) -0.3171(12) 0.5144(5) 0.113(5) Uani 1 1 d . . .
H59A H 1.4398 -0.3619 0.5458 0.136 Uiso 1 1 calc R . .
C60 C 1.4952(8) -0.2433(10) 0.5156(4) 0.080(3) Uani 1 1 d . . .
C61 C 1.5082(15) -0.1798(13) 0.4688(5) 0.126(5) Uani 1 1 d . . .
H61A H 1.5471 -0.1331 0.4671 0.151 Uiso 1 1 calc R . .
C62 C 1.4633(14) -0.1863(12) 0.4250(5) 0.123(5) Uani 1 1 d D . .
H62A H 1.4658 -0.1364 0.3948 0.148 Uiso 1 1 calc R . .
C63 C 1.5298(7) -0.2280(9) 0.5660(4) 0.077(3) Uani 1 1 d . . .
H63A H 1.5652 -0.2985 0.5868 0.092 Uiso 1 1 calc R . .
H63B H 1.5862 -0.1942 0.5574 0.092 Uiso 1 1 calc R . .
C64 C 1.4326(8) -0.1609(10) 0.5977(4) 0.077(3) Uani 1 1 d . . .
C65 C 1.3662(9) -0.1991(10) 0.6347(4) 0.082(3) Uani 1 1 d . . .
H65A H 1.3835 -0.2738 0.6408 0.099 Uiso 1 1 calc R . .
C66 C 1.2776(9) -0.1364(8) 0.6628(4) 0.078(3) Uani 1 1 d . . .
H66A H 1.2361 -0.1701 0.6875 0.093 Uiso 1 1 calc R . .
C67 C 1.2412(9) -0.0229(8) 0.6586(3) 0.069(2) Uani 1 1 d . . .
C68 C 1.3154(9) 0.0155(10) 0.6198(4) 0.084(3) Uani 1 1 d . . .
H68A H 1.3018 0.0896 0.6146 0.101 Uiso 1 1 calc R . .
C69 C 1.4030(10) -0.0494(10) 0.5907(5) 0.089(3) Uani 1 1 d . . .
H69A H 1.4454 -0.0186 0.5650 0.106 Uiso 1 1 calc R . .
C70 C 1.1543(10) 0.0428(8) 0.6880(4) 0.089(3) Uani 1 1 d D . .
N1 N 1.6198(5) -1.0045(5) 0.2415(3) 0.0558(17) Uani 1 1 d . . .
O22 O 1.5884(7) -0.8322(6) 0.2106(3) 0.088(2) Uani 1 1 d . . .
C71 C 1.590(2) -0.9048(11) 0.2384(9) 0.194(12) Uani 1 1 d . . .
H71A H 1.5581 -0.8839 0.2718 0.233 Uiso 1 1 calc R . .
C72 C 1.6945(10) -1.0651(13) 0.2048(5) 0.113(5) Uani 1 1 d . . .
H72A H 1.7256 -1.0199 0.1793 0.169 Uiso 1 1 calc R . .
H72B H 1.6549 -1.0951 0.1867 0.169 Uiso 1 1 calc R . .
H72C H 1.7555 -1.1232 0.2226 0.169 Uiso 1 1 calc R . .
C73 C 1.5609(16) -1.0457(19) 0.2811(6) 0.180(10) Uani 1 1 d . . .
H79A H 1.5123 -0.9895 0.3020 0.270 Uiso 1 1 calc R . .
H79B H 1.6133 -1.1033 0.3036 0.270 Uiso 1 1 calc R . .
H79C H 1.5147 -1.0739 0.2662 0.270 Uiso 1 1 calc R . .
N2 N 1.3178(4) -0.4409(4) 0.07507(19) 0.0316(11) Uani 1 1 d . . .
O23 O 1.3391(7) -0.4923(7) -0.0033(3) 0.096(2) Uani 1 1 d . . .
C74 C 1.2886(8) -0.4511(8) 0.0307(3) 0.060(2) Uani 1 1 d . . .
H74A H 1.2104 -0.4175 0.0267 0.073 Uiso 1 1 calc R . .
C75 C 1.4309(5) -0.4818(6) 0.0879(3) 0.0450(16) Uani 1 1 d . . .
H75A H 1.4804 -0.5159 0.0587 0.067 Uiso 1 1 calc R . .
H75B H 1.4397 -0.5344 0.1194 0.067 Uiso 1 1 calc R . .
H75C H 1.4507 -0.4234 0.0943 0.067 Uiso 1 1 calc R . .
C76 C 1.2336(7) -0.3886(6) 0.1152(3) 0.058(2) Uani 1 1 d . . .
H76A H 1.1587 -0.3638 0.1026 0.087 Uiso 1 1 calc R . .
H76B H 1.2477 -0.3276 0.1226 0.087 Uiso 1 1 calc R . .
H76C H 1.2377 -0.4393 0.1473 0.087 Uiso 1 1 calc R . .
N3 N 1.0145(11) -0.0739(10) 0.5694(4) 0.130(4) Uani 1 1 d DU . .
O24 O 0.9187(6) 0.0802(5) 0.6109(3) 0.0768(19) Uani 1 1 d DU . .
C77 C 0.9939(14) 0.0146(14) 0.6002(5) 0.120(4) Uani 1 1 d U . .
H77A H 1.0597 0.0130 0.6129 0.144 Uiso 1 1 calc R . .
C78 C 0.8975(13) -0.0368(16) 0.5566(5) 0.149(6) Uani 1 1 d U . .
H78A H 0.8537 0.0303 0.5708 0.223 Uiso 1 1 calc R . .
H78B H 0.8658 -0.0906 0.5722 0.223 Uiso 1 1 calc R . .
H78C H 0.8951 -0.0253 0.5185 0.223 Uiso 1 1 calc R . .
N4 N 0.6789(15) -0.427(2) 0.3485(7) 0.244(8) Uani 1 1 d DU . .
O25 O 0.6551(18) -0.520(2) 0.4238(7) 0.325(11) Uani 1 1 d DU . .
C80 C 0.686(2) -0.523(2) 0.3741(9) 0.276(9) Uani 1 1 d DU . .
H80A H 0.7110 -0.5858 0.3578 0.332 Uiso 1 1 calc R . .
C81 C 0.7113(18) -0.375(2) 0.3812(9) 0.245(10) Uani 1 1 d DU . .
H81A H 0.7084 -0.3050 0.3627 0.367 Uiso 1 1 calc R . .
H81B H 0.7880 -0.4178 0.3905 0.367 Uiso 1 1 calc R . .
H81C H 0.6601 -0.3646 0.4131 0.367 Uiso 1 1 calc R . .
C79 C 1.1158(16) -0.1548(16) 0.5622(7) 0.166(7) Uani 1 1 d U . .
H79D H 1.1727 -0.1434 0.5787 0.249 Uiso 1 1 calc R . .
H79E H 1.1376 -0.1561 0.5245 0.249 Uiso 1 1 calc R . .
H79F H 1.1099 -0.2229 0.5780 0.249 Uiso 1 1 calc R . .
C82 C 0.6451(15) -0.400(2) 0.3087(7) 0.245(9) Uani 1 1 d DU . .
H82A H 0.6476 -0.3293 0.2952 0.368 Uiso 1 1 calc R . .
H82B H 0.5673 -0.3954 0.3117 0.368 Uiso 1 1 calc R . .
H82C H 0.6910 -0.4508 0.2847 0.368 Uiso 1 1 calc R . .


_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
Co1 O14 1.987(5) . ?
Co1 O4 2.046(4) . ?
Co1 O13 2.083(4) . ?
Co1 O21 2.104(8) 2_756 ?
Co1 O2 2.107(4) . ?
Co1 O1 2.187(4) . ?
Co1 Co4 2.9364(11) . ?
Co1 Co2 2.9647(12) . ?
Co2 O15 1.987(5) . ?
Co2 O4 2.048(4) . ?
Co2 O16 2.070(6) . ?
Co2 O5 2.082(4) . ?
Co2 O7 2.091(4) . ?
Co2 O1 2.162(4) . ?
Co2 Co3 2.9018(11) . ?
Co3 O18 1.975(4) 2_756 ?
Co3 O10 2.051(4) . ?
Co3 O17 2.121(7) . ?
Co3 O8 2.087(4) . ?
Co3 O7 2.098(4) . ?
Co3 O1 2.184(4) . ?
Co3 Co4 2.9892(12) . ?
Co4 O19 1.988(4) 2_756 ?
Co4 O20 2.053(8) 2_756 ?
Co4 O10 2.063(4) . ?
Co4 O13 2.088(4) . ?
Co4 O11 2.101(4) . ?
Co4 O1 2.181(4) . ?
S1 O3 1.435(4) . ?
S1 O2 1.454(4) . ?
S1 C2 1.769(5) . ?
S1 C34 1.771(5) . ?
S2 O6 1.428(4) . ?
S2 O5 1.459(4) . ?
S2 C12 1.765(5) . ?
S2 C4 1.772(5) . ?
S3 O9 1.437(4) . ?
S3 O8 1.463(4) . ?
S3 C14 1.772(5) . ?
S3 C22 1.773(5) . ?
S4 O12 1.434(4) . ?
S4 O11 1.453(4) . ?
S4 C32 1.765(5) . ?
S4 C24 1.769(5) . ?
O4 C3 1.312(6) . ?
O7 C13 1.309(7) . ?
O10 C23 1.305(7) . ?
O13 C33 1.311(7) . ?
O14 C41 1.246(9) . ?
O15 C41 1.260(9) . ?
O16 C56 1.287(10) . ?
O17 C56 1.217(10) . ?
O18 C55 1.239(8) . ?
O18 Co3 1.975(4) 2_756 ?
O19 C55 1.250(8) . ?
O19 Co4 1.988(4) 2_756 ?
O20 C70 1.184(11) . ?
O20 Co4 2.053(8) 2_756 ?
O21 C70 1.268(11) . ?
O21 Co1 2.104(8) 2_756 ?
C1 C6 1.385(7) . ?
C1 C2 1.400(7) . ?
C1 H1A 0.9500 . ?
C2 C3 1.420(7) . ?
C3 C4 1.416(7) . ?
C4 C5 1.397(7) . ?
C5 C6 1.397(7) . ?
C5 H5A 0.9500 . ?
C6 C7 1.539(7) . ?
C7 C8 1.522(8) . ?
C7 C9 1.526(7) . ?
C7 C10 1.544(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.386(8) . ?
C11 C16 1.394(7) . ?
C11 H11A 0.9500 . ?
C12 C13 1.430(7) . ?
C13 C14 1.418(7) . ?
C14 C15 1.389(8) . ?
C15 C16 1.392(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.529(7) . ?
C17 C18 1.524(8) . ?
C17 C20 1.536(8) . ?
C17 C19 1.541(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.388(8) . ?
C21 C22 1.390(8) . ?
C21 H21A 0.9500 . ?
C22 C23 1.430(8) . ?
C23 C24 1.432(8) . ?
C24 C25 1.396(8) . ?
C25 C26 1.390(8) . ?
C25 H25A 0.9500 . ?
C26 C27 1.533(8) . ?
C27 C30 1.526(9) . ?
C27 C29 1.536(8) . ?
C27 C28 1.533(8) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C36 1.387(7) . ?
C31 C32 1.404(7) . ?
C31 H31A 0.9500 . ?
C32 C33 1.415(8) . ?
C33 C34 1.417(7) . ?
C34 C35 1.398(7) . ?
C35 C36 1.384(7) . ?
C35 H35A 0.9500 . ?
C36 C37 1.533(7) . ?
C37 C40' 1.457(19) . ?
C37 C38 1.476(10) . ?
C37 C39 1.533(10) . ?
C37 C38' 1.555(18) . ?
C37 C40 1.572(10) . ?
C37 C39' 1.621(17) . ?
C38' H38A 0.9800 . ?
C38' H38B 0.9800 . ?
C38' H38C 0.9800 . ?
C38 H38D 0.9800 . ?
C38 H38E 0.9800 . ?
C38 H38F 0.9800 . ?
C39' H39A 0.9800 . ?
C39' H39B 0.9800 . ?
C39' H39C 0.9800 . ?
C39 H39D 0.9800 . ?
C39 H39E 0.9800 . ?
C39 H39F 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40' H40D 0.9800 . ?
C40' H40E 0.9800 . ?
C40' H40F 0.9800 . ?
C41 C42 1.481(9) . ?
C42 C47 1.371(13) . ?
C42 C43 1.375(12) . ?
C43 C44 1.378(11) . ?
C43 H43A 0.9500 . ?
C44 C45 1.390(14) . ?
C44 H44A 0.9500 . ?
C45 C46 1.383(14) . ?
C45 C48 1.513(9) . ?
C46 C47 1.380(12) . ?
C46 H46A 0.9500 . ?
C47 H47A 0.9500 . ?
C48 C49 1.524(9) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.377(12) . ?
C49 C54 1.389(12) . ?
C50 C51 1.388(10) . ?
C50 H50A 0.9500 . ?
C51 C52 1.378(10) . ?
C51 H51A 0.9500 . ?
C52 C53 1.403(10) . ?
C52 C55 1.509(8) . ?
C53 C54 1.381(9) . ?
C53 H53A 0.9500 . ?
C54 H54A 0.9500 . ?
C56 C57 1.399(14) . ?
C57 C58 1.428(11) . ?
C57 C62 1.433(11) . ?
C58 C59 1.376(16) . ?
C58 H58A 0.9500 . ?
C59 C60 1.379(17) . ?
C59 H59A 0.9500 . ?
C60 C61 1.394(17) . ?
C60 C63 1.520(13) . ?
C61 C62 1.385(16) . ?
C61 H61A 0.9500 . ?
C62 H62A 0.9500 . ?
C63 C64 1.478(13) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.369(15) . ?
C64 C69 1.411(16) . ?
C65 C66 1.345(13) . ?
C65 H65A 0.9500 . ?
C66 C67 1.430(14) . ?
C66 H66A 0.9500 . ?
C67 C70 1.370(12) . ?
C67 C68 1.465(14) . ?
C68 C69 1.365(14) . ?
C68 H68A 0.9500 . ?
C69 H69A 0.9500 . ?
N1 C71 1.260(14) . ?
N1 C73 1.366(16) . ?
N1 C72 1.391(13) . ?
O22 C71 1.117(16) . ?
C71 H71A 0.9500 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H79A 0.9800 . ?
C73 H79B 0.9800 . ?
C73 H79C 0.9800 . ?
N2 C74 1.313(9) . ?
N2 C75 1.418(8) . ?
N2 C76 1.458(9) . ?
O23 C74 1.119(11) . ?
C74 H74A 0.9500 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N3 C79 1.365(19) . ?
N3 C78 1.469(19) . ?
N3 C77 1.492(19) . ?
O24 C77 1.081(16) . ?
C77 H77A 0.9500 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
N4 C82 1.13(2) . ?
N4 C81 1.41(3) . ?
N4 C80 1.34(4) . ?
O25 C80 1.298(17) . ?
C80 C82 2.139(19) . ?
C80 H80A 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C79 H79D 0.9800 . ?
C79 H79E 0.9800 . ?
C79 H79F 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?

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
O14 Co1 O4 95.09(19) . . ?
O14 Co1 O13 174.0(2) . . ?
O4 Co1 O13 90.75(16) . . ?
O14 Co1 O21 76.9(3) . 2_756 ?
O4 Co1 O21 169.7(2) . 2_756 ?
O13 Co1 O21 97.4(3) . 2_756 ?
O14 Co1 O2 93.36(18) . . ?
O4 Co1 O2 86.44(15) . . ?
O13 Co1 O2 88.32(15) . . ?
O21 Co1 O2 87.5(2) 2_756 . ?
O14 Co1 O1 95.51(18) . . ?
O4 Co1 O1 84.32(15) . . ?
O13 Co1 O1 83.73(15) . . ?
O21 Co1 O1 102.8(2) 2_756 . ?
O2 Co1 O1 167.71(15) . . ?
O14 Co1 Co4 130.71(16) . . ?
O4 Co1 Co4 109.14(11) . . ?
O13 Co1 Co4 45.32(11) . . ?
O21 Co1 Co4 81.2(2) 2_756 . ?
O2 Co1 Co4 129.30(11) . . ?
O1 Co1 Co4 47.66(11) . . ?
O14 Co1 Co2 79.23(15) . . ?
O4 Co1 Co2 43.64(10) . . ?
O13 Co1 Co2 104.27(13) . . ?
O21 Co1 Co2 138.5(2) 2_756 . ?
O2 Co1 Co2 127.50(11) . . ?
O1 Co1 Co2 46.66(11) . . ?
Co4 Co1 Co2 89.48(3) . . ?
O15 Co2 O4 96.9(2) . . ?
O15 Co2 O16 76.1(3) . . ?
O4 Co2 O16 169.2(2) . . ?
O15 Co2 O5 94.60(18) . . ?
O4 Co2 O5 86.98(15) . . ?
O16 Co2 O5 85.4(2) . . ?
O15 Co2 O7 172.5(2) . . ?
O4 Co2 O7 89.90(16) . . ?
O16 Co2 O7 97.5(3) . . ?
O5 Co2 O7 88.75(15) . . ?
O15 Co2 O1 93.11(19) . . ?
O4 Co2 O1 84.92(15) . . ?
O16 Co2 O1 103.5(2) . . ?
O5 Co2 O1 169.43(14) . . ?
O7 Co2 O1 84.45(15) . . ?
O15 Co2 Co3 127.64(16) . . ?
O4 Co2 Co3 110.32(11) . . ?
O16 Co2 Co3 80.4(2) . . ?
O5 Co2 Co3 129.43(10) . . ?
O7 Co2 Co3 46.26(11) . . ?
O1 Co2 Co3 48.43(11) . . ?
O15 Co2 Co1 78.83(16) . . ?
O4 Co2 Co1 43.58(11) . . ?
O16 Co2 Co1 140.0(2) . . ?
O5 Co2 Co1 127.51(11) . . ?
O7 Co2 Co1 104.38(13) . . ?
O1 Co2 Co1 47.38(11) . . ?
Co3 Co2 Co1 91.01(3) . . ?
O18 Co3 O10 95.58(19) 2_756 . ?
O18 Co3 O17 77.6(3) 2_756 . ?
O10 Co3 O17 171.7(3) . . ?
O18 Co3 O8 92.40(18) 2_756 . ?
O10 Co3 O8 87.64(15) . . ?
O17 Co3 O8 87.9(2) . . ?
O18 Co3 O7 175.2(2) 2_756 . ?
O10 Co3 O7 89.04(17) . . ?
O17 Co3 O7 97.9(3) . . ?
O8 Co3 O7 89.24(15) . . ?
O18 Co3 O1 95.27(18) 2_756 . ?
O10 Co3 O1 84.16(15) . . ?
O17 Co3 O1 101.1(3) . . ?
O8 Co3 O1 169.27(14) . . ?
O7 Co3 O1 83.73(15) . . ?
O18 Co3 Co2 130.42(16) 2_756 . ?
O10 Co3 Co2 108.92(11) . . ?
O17 Co3 Co2 79.3(2) . . ?
O8 Co3 Co2 129.85(11) . . ?
O7 Co3 Co2 46.05(11) . . ?
O1 Co3 Co2 47.78(11) . . ?
O18 Co3 Co4 79.19(15) 2_756 . ?
O10 Co3 Co4 43.56(11) . . ?
O17 Co3 Co4 137.6(2) . . ?
O8 Co3 Co4 128.14(11) . . ?
O7 Co3 Co4 103.34(13) . . ?
O1 Co3 Co4 46.73(11) . . ?
Co2 Co3 Co4 89.66(3) . . ?
O19 Co4 O20 80.6(3) 2_756 2_756 ?
O19 Co4 O10 94.39(18) 2_756 . ?
O20 Co4 O10 175.0(3) 2_756 . ?
O19 Co4 O13 174.5(2) 2_756 . ?
O20 Co4 O13 94.1(3) 2_756 . ?
O10 Co4 O13 90.85(16) . . ?
O19 Co4 O11 94.36(17) 2_756 . ?
O20 Co4 O11 93.9(3) 2_756 . ?
O10 Co4 O11 86.88(15) . . ?
O13 Co4 O11 87.50(15) . . ?
O19 Co4 O1 95.21(17) 2_756 . ?
O20 Co4 O1 96.0(3) 2_756 . ?
O10 Co4 O1 83.96(15) . . ?
O13 Co4 O1 83.76(15) . . ?
O11 Co4 O1 167.22(15) . . ?
O19 Co4 Co1 130.96(14) 2_756 . ?
O20 Co4 Co1 74.4(4) 2_756 . ?
O10 Co4 Co1 108.98(11) . . ?
O13 Co4 Co1 45.17(11) . . ?
O11 Co4 Co1 128.35(11) . . ?
O1 Co4 Co1 47.85(11) . . ?
O19 Co4 Co3 78.38(14) 2_756 . ?
O20 Co4 Co3 134.3(2) 2_756 . ?
O10 Co4 Co3 43.25(10) . . ?
O13 Co4 Co3 104.54(13) . . ?
O11 Co4 Co3 127.68(11) . . ?
O1 Co4 Co3 46.82(11) . . ?
Co1 Co4 Co3 89.85(3) . . ?
O3 S1 O2 115.6(2) . . ?
O3 S1 C2 107.8(2) . . ?
O2 S1 C2 110.2(2) . . ?
O3 S1 C34 108.0(2) . . ?
O2 S1 C34 109.6(2) . . ?
C2 S1 C34 105.1(2) . . ?
O6 S2 O5 115.3(2) . . ?
O6 S2 C12 107.8(2) . . ?
O5 S2 C12 109.1(2) . . ?
O6 S2 C4 107.6(2) . . ?
O5 S2 C4 109.8(2) . . ?
C12 S2 C4 106.8(2) . . ?
O9 S3 O8 115.8(2) . . ?
O9 S3 C14 107.4(3) . . ?
O8 S3 C14 109.1(2) . . ?
O9 S3 C22 107.4(2) . . ?
O8 S3 C22 109.3(2) . . ?
C14 S3 C22 107.6(2) . . ?
O12 S4 O11 116.1(2) . . ?
O12 S4 C32 107.6(2) . . ?
O11 S4 C32 109.5(2) . . ?
O12 S4 C24 107.3(2) . . ?
O11 S4 C24 110.0(2) . . ?
C32 S4 C24 105.9(2) . . ?
Co2 O1 Co3 83.79(16) . . ?
Co2 O1 Co4 146.12(19) . . ?
Co3 O1 Co4 86.45(14) . . ?
Co2 O1 Co1 85.96(14) . . ?
Co3 O1 Co1 146.43(19) . . ?
Co4 O1 Co1 84.49(16) . . ?
S1 O2 Co1 119.7(2) . . ?
C3 O4 Co2 132.6(3) . . ?
C3 O4 Co1 134.5(3) . . ?
Co2 O4 Co1 92.77(14) . . ?
S2 O5 Co2 119.7(2) . . ?
C13 O7 Co2 132.3(4) . . ?
C13 O7 Co3 130.9(3) . . ?
Co2 O7 Co3 87.69(15) . . ?
S3 O8 Co3 119.3(2) . . ?
C23 O10 Co3 132.7(4) . . ?
C23 O10 Co4 134.1(4) . . ?
Co3 O10 Co4 93.18(15) . . ?
S4 O11 Co4 120.3(2) . . ?
C33 O13 Co1 133.4(3) . . ?
C33 O13 Co4 133.3(3) . . ?
Co1 O13 Co4 89.51(15) . . ?
C41 O14 Co1 128.4(5) . . ?
C41 O15 Co2 128.9(5) . . ?
C56 O16 Co2 124.8(7) . . ?
C56 O17 Co3 126.0(7) . . ?
C55 O18 Co3 127.8(4) . 2_756 ?
C55 O19 Co4 127.9(4) . 2_756 ?
C70 O20 Co4 139.7(11) . 2_756 ?
C70 O21 Co1 124.5(7) . 2_756 ?
C6 C1 C2 122.5(5) . . ?
C6 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C1 C2 C3 122.6(5) . . ?
C1 C2 S1 114.3(4) . . ?
C3 C2 S1 123.1(4) . . ?
O4 C3 C4 123.6(5) . . ?
O4 C3 C2 122.7(5) . . ?
C4 C3 C2 113.7(4) . . ?
C5 C4 C3 123.1(5) . . ?
C5 C4 S2 113.7(4) . . ?
C3 C4 S2 123.2(4) . . ?
C6 C5 C4 121.9(5) . . ?
C6 C5 H5A 119.0 . . ?
C4 C5 H5A 119.0 . . ?
C1 C6 C5 116.2(5) . . ?
C1 C6 C7 121.8(5) . . ?
C5 C6 C7 122.0(5) . . ?
C8 C7 C9 109.2(5) . . ?
C8 C7 C6 111.9(4) . . ?
C9 C7 C6 111.2(4) . . ?
C8 C7 C10 109.2(5) . . ?
C9 C7 C10 108.9(5) . . ?
C6 C7 C10 106.4(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 122.0(5) . . ?
C12 C11 H11A 119.0 . . ?
C16 C11 H11A 119.0 . . ?
C11 C12 C13 122.7(5) . . ?
C11 C12 S2 116.0(4) . . ?
C13 C12 S2 121.3(4) . . ?
O7 C13 C14 123.8(5) . . ?
O7 C13 C12 122.3(5) . . ?
C14 C13 C12 113.9(5) . . ?
C15 C14 C13 122.6(5) . . ?
C15 C14 S3 116.4(4) . . ?
C13 C14 S3 121.0(4) . . ?
C16 C15 C14 122.4(5) . . ?
C16 C15 H15A 118.8 . . ?
C14 C15 H15A 118.8 . . ?
C15 C16 C11 116.3(5) . . ?
C15 C16 C17 123.5(5) . . ?
C11 C16 C17 120.2(5) . . ?
C18 C17 C16 112.3(5) . . ?
C18 C17 C20 108.4(5) . . ?
C16 C17 C20 108.6(5) . . ?
C18 C17 C19 108.2(5) . . ?
C16 C17 C19 109.5(4) . . ?
C20 C17 C19 109.7(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 123.2(5) . . ?
C26 C21 H21A 118.4 . . ?
C22 C21 H21A 118.4 . . ?
C21 C22 C23 122.1(5) . . ?
C21 C22 S3 114.5(4) . . ?
C23 C22 S3 123.4(4) . . ?
O10 C23 C24 122.9(5) . . ?
O10 C23 C22 123.4(5) . . ?
C24 C23 C22 113.7(5) . . ?
C25 C24 C23 122.6(5) . . ?
C25 C24 S4 114.4(4) . . ?
C23 C24 S4 123.0(4) . . ?
C24 C25 C26 122.3(5) . . ?
C24 C25 H25A 118.8 . . ?
C26 C25 H25A 118.8 . . ?
C21 C26 C25 116.1(5) . . ?
C21 C26 C27 120.9(5) . . ?
C25 C26 C27 123.0(5) . . ?
C30 C27 C29 109.2(5) . . ?
C30 C27 C26 108.9(5) . . ?
C29 C27 C26 109.4(5) . . ?
C30 C27 C28 108.4(5) . . ?
C29 C27 C28 108.8(5) . . ?
C26 C27 C28 112.1(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 122.3(5) . . ?
C36 C31 H31A 118.9 . . ?
C32 C31 H31A 118.9 . . ?
C31 C32 C33 122.3(5) . . ?
C31 C32 S4 115.5(4) . . ?
C33 C32 S4 122.2(4) . . ?
O13 C33 C34 122.6(5) . . ?
O13 C33 C32 123.0(5) . . ?
C34 C33 C32 114.3(5) . . ?
C35 C34 C33 122.3(5) . . ?
C35 C34 S1 115.1(4) . . ?
C33 C34 S1 122.6(4) . . ?
C36 C35 C34 122.6(5) . . ?
C36 C35 H35A 118.7 . . ?
C34 C35 H35A 118.7 . . ?
C35 C36 C31 116.2(5) . . ?
C35 C36 C37 120.8(5) . . ?
C31 C36 C37 123.0(5) . . ?
C40' C37 C38 129.4(9) . . ?
C40' C37 C39 52.7(9) . . ?
C38 C37 C39 113.0(7) . . ?
C40' C37 C36 118.2(8) . . ?
C38 C37 C36 112.4(5) . . ?
C39 C37 C36 107.2(5) . . ?
C40' C37 C38' 111.0(12) . . ?
C38 C37 C38' 46.5(9) . . ?
C39 C37 C38' 142.5(8) . . ?
C36 C37 C38' 109.9(8) . . ?
C40' C37 C40 54.1(9) . . ?
C38 C37 C40 109.6(7) . . ?
C39 C37 C40 106.8(6) . . ?
C36 C37 C40 107.6(5) . . ?
C38' C37 C40 66.5(9) . . ?
C40' C37 C39' 106.4(11) . . ?
C38 C37 C39' 56.7(9) . . ?
C39 C37 C39' 60.8(8) . . ?
C36 C37 C39' 107.8(7) . . ?
C38' C37 C39' 102.2(11) . . ?
C40 C37 C39' 144.6(8) . . ?
C37 C38' H38A 109.5 . . ?
C37 C38' H38B 109.5 . . ?
H38A C38' H38B 109.5 . . ?
C37 C38' H38C 109.5 . . ?
H38A C38' H38C 109.5 . . ?
H38B C38' H38C 109.5 . . ?
C37 C38 H38D 109.5 . . ?
C37 C38 H38E 109.5 . . ?
H38D C38 H38E 109.5 . . ?
C37 C38 H38F 109.5 . . ?
H38D C38 H38F 109.5 . . ?
H38E C38 H38F 109.5 . . ?
C37 C39' H39A 109.5 . . ?
C37 C39' H39B 109.5 . . ?
H39A C39' H39B 109.5 . . ?
C37 C39' H39C 109.5 . . ?
H39A C39' H39C 109.5 . . ?
H39B C39' H39C 109.5 . . ?
C37 C39 H39D 109.5 . . ?
C37 C39 H39E 109.5 . . ?
H39D C39 H39E 109.5 . . ?
C37 C39 H39F 109.5 . . ?
H39D C39 H39F 109.5 . . ?
H39E C39 H39F 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C40' H40D 109.5 . . ?
C37 C40' H40E 109.5 . . ?
H40D C40' H40E 109.5 . . ?
C37 C40' H40F 109.5 . . ?
H40D C40' H40F 109.5 . . ?
H40E C40' H40F 109.5 . . ?
O14 C41 O15 123.9(6) . . ?
O14 C41 C42 118.0(7) . . ?
O15 C41 C42 118.1(7) . . ?
C47 C42 C43 117.8(7) . . ?
C47 C42 C41 120.7(7) . . ?
C43 C42 C41 121.4(7) . . ?
C42 C43 C44 121.5(9) . . ?
C42 C43 H43A 119.2 . . ?
C44 C43 H43A 119.2 . . ?
C43 C44 C45 121.1(9) . . ?
C43 C44 H44A 119.5 . . ?
C45 C44 H44A 119.5 . . ?
C46 C45 C44 116.8(7) . . ?
C46 C45 C48 121.7(9) . . ?
C44 C45 C48 121.4(9) . . ?
C45 C46 C47 121.6(10) . . ?
C45 C46 H46A 119.2 . . ?
C47 C46 H46A 119.2 . . ?
C42 C47 C46 121.1(10) . . ?
C42 C47 H47A 119.4 . . ?
C46 C47 H47A 119.4 . . ?
C45 C48 C49 109.2(5) . . ?
C45 C48 H48A 109.8 . . ?
C49 C48 H48A 109.8 . . ?
C45 C48 H48B 109.8 . . ?
C49 C48 H48B 109.8 . . ?
H48A C48 H48B 108.3 . . ?
C50 C49 C54 118.8(6) . . ?
C50 C49 C48 120.3(8) . . ?
C54 C49 C48 120.8(8) . . ?
C49 C50 C51 121.4(8) . . ?
C49 C50 H50A 119.3 . . ?
C51 C50 H50A 119.3 . . ?
C52 C51 C50 119.6(8) . . ?
C52 C51 H51A 120.2 . . ?
C50 C51 H51A 120.2 . . ?
C51 C52 C53 119.8(6) . . ?
C51 C52 C55 120.8(6) . . ?
C53 C52 C55 119.4(6) . . ?
C54 C53 C52 119.6(7) . . ?
C54 C53 H53A 120.2 . . ?
C52 C53 H53A 120.2 . . ?
C53 C54 C49 120.8(8) . . ?
C53 C54 H54A 119.6 . . ?
C49 C54 H54A 119.6 . . ?
O18 C55 O19 126.1(6) . . ?
O18 C55 C52 116.9(6) . . ?
O19 C55 C52 117.0(6) . . ?
O17 C56 O16 119.6(9) . . ?
O17 C56 C57 120.7(8) . . ?
O16 C56 C57 115.1(8) . . ?
C58 C57 C56 125.5(9) . . ?
C58 C57 C62 110.2(11) . . ?
C56 C57 C62 124.2(8) . . ?
C59 C58 C57 124.2(12) . . ?
C59 C58 H58A 117.9 . . ?
C57 C58 H58A 117.9 . . ?
C58 C59 C60 122.0(13) . . ?
C58 C59 H59A 119.0 . . ?
C60 C59 H59A 119.0 . . ?
C61 C60 C59 118.0(11) . . ?
C61 C60 C63 120.0(11) . . ?
C59 C60 C63 122.0(11) . . ?
C62 C61 C60 118.6(14) . . ?
C62 C61 H61A 120.7 . . ?
C60 C61 H61A 120.7 . . ?
C61 C62 C57 126.6(13) . . ?
C61 C62 H62A 116.7 . . ?
C57 C62 H62A 116.7 . . ?
C64 C63 C60 111.6(7) . . ?
C64 C63 H63A 109.3 . . ?
C60 C63 H63A 109.3 . . ?
C64 C63 H63B 109.3 . . ?
C60 C63 H63B 109.3 . . ?
H63A C63 H63B 108.0 . . ?
C65 C64 C69 115.5(10) . . ?
C65 C64 C63 124.5(11) . . ?
C69 C64 C63 120.0(11) . . ?
C66 C65 C64 123.5(12) . . ?
C66 C65 H65A 118.2 . . ?
C64 C65 H65A 118.2 . . ?
C65 C66 C67 125.1(11) . . ?
C65 C66 H66A 117.5 . . ?
C67 C66 H66A 117.5 . . ?
C70 C67 C66 126.6(10) . . ?
C70 C67 C68 123.0(10) . . ?
C66 C67 C68 110.3(9) . . ?
C69 C68 C67 123.5(11) . . ?
C69 C68 H68A 118.3 . . ?
C67 C68 H68A 118.3 . . ?
C68 C69 C64 122.1(11) . . ?
C68 C69 H69A 119.0 . . ?
C64 C69 H69A 119.0 . . ?
O20 C70 O21 114.7(10) . . ?
O20 C70 C67 126.1(11) . . ?
O21 C70 C67 118.7(10) . . ?
C71 N1 C73 113.2(17) . . ?
C71 N1 C72 123.7(16) . . ?
C73 N1 C72 122.6(12) . . ?
O22 C71 N1 143(2) . . ?
O22 C71 H71A 108.6 . . ?
N1 C71 H71A 108.6 . . ?
N1 C72 H72A 109.5 . . ?
N1 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
N1 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N1 C73 H79A 109.5 . . ?
N1 C73 H79B 109.5 . . ?
H79A C73 H79B 109.5 . . ?
N1 C73 H79C 109.5 . . ?
H79A C73 H79C 109.5 . . ?
H79B C73 H79C 109.5 . . ?
C74 N2 C75 123.0(7) . . ?
C74 N2 C76 121.0(7) . . ?
C75 N2 C76 115.9(6) . . ?
O23 C74 N2 131.7(10) . . ?
O23 C74 H74A 114.2 . . ?
N2 C74 H74A 114.2 . . ?
N2 C75 H75A 109.5 . . ?
N2 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
N2 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N2 C76 H76A 109.5 . . ?
N2 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
N2 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C79 N3 C78 140.8(17) . . ?
C79 N3 C77 124.6(16) . . ?
C78 N3 C77 94.6(12) . . ?
O24 C77 N3 132.4(16) . . ?
O24 C77 H77A 113.8 . . ?
N3 C77 H77A 113.8 . . ?
N3 C78 H78A 109.5 . . ?
N3 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
N3 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C82 N4 C81 132(3) . . ?
C82 N4 C80 120(3) . . ?
C81 N4 C80 108.4(15) . . ?
O25 C80 N4 112(3) . . ?
O25 C80 C82 131(2) . . ?
N4 C80 C82 27.1(11) . . ?
O25 C80 H80A 123.9 . . ?
N4 C80 H80A 123.9 . . ?
C82 C80 H80A 102.3 . . ?
N4 C81 H81A 109.5 . . ?
N4 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
N4 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
N3 C79 H79D 109.5 . . ?
N3 C79 H79E 109.5 . . ?
H79D C79 H79E 109.5 . . ?
N3 C79 H79F 109.5 . . ?
H79D C79 H79F 109.5 . . ?
H79E C79 H79F 109.5 . . ?
N4 C82 C80 33(2) . . ?
N4 C82 H82A 109.5 . . ?
C80 C82 H82A 142.4 . . ?
N4 C82 H82B 109.5 . . ?
C80 C82 H82B 92.1 . . ?
H82A C82 H82B 109.5 . . ?
N4 C82 H82C 109.5 . . ?
C80 C82 H82C 90.6 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         4.358
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.138
_exptl_crystal_recrystallization_method 'Solvothermal reaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-Co
_database_code_depnum_ccdc_archive 'CCDC 1422948'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        2-Co
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C140 H136 Co8 N4 O42 S8'
_chemical_formula_sum            'C140 H136 Co8 N4 O42 S8'
_chemical_formula_weight         3274.45

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4/mnc
_symmetry_space_group_name_Hall  '-P 4 2n'

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

_cell_length_a                   17.1548(12)
_cell_length_b                   17.1548(12)
_cell_length_c                   37.599(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11065.0(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7954
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      18.36

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3368
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7883
_exptl_absorpt_correction_T_max  0.8144
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            67562
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.08
_diffrn_reflns_theta_max         20.65
_reflns_number_total             2892
_reflns_number_gt                2143
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1671P)²+9.4938P] where P=(Fo²+2Fc²)/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_number_reflns         2892
_refine_ls_number_parameters     241
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0828
_refine_ls_wR_factor_ref         0.2622
_refine_ls_wR_factor_gt          0.2373
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_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
Co1 Co 0.87783(7) 0.02290(7) 0.34592(3) 0.0786(6) Uani 1 1 d . . .
S1 S 1.04222(14) 0.22667(14) 0.27961(6) 0.0850(9) Uani 1 1 d . . .
O1 O 1.0000 0.0000 0.3649(2) 0.067(3) Uani 1 4 d S . .
C1 C 0.8132(5) 0.1487(6) 0.2322(2) 0.090(3) Uani 1 1 d . . .
H1 H 0.7652 0.1335 0.2217 0.108 Uiso 1 1 calc R . .
O2 O 0.9320(3) 0.0986(3) 0.31068(13) 0.0811(17) Uani 1 1 d . . .
C2 C 0.8360(5) 0.1145(5) 0.2645(2) 0.080(3) Uani 1 1 d . . .
O3 O 1.0420(4) 0.2243(3) 0.31847(15) 0.0963(19) Uani 1 1 d . . .
C3 C 0.9093(5) 0.1336(4) 0.28068(19) 0.067(2) Uani 1 1 d . . .
O4 O 1.0559(3) 0.3006(3) 0.26359(14) 0.0932(18) Uani 1 1 d . . .
C4 C 0.9538(5) 0.1910(5) 0.2634(2) 0.081(3) Uani 1 1 d . . .
O5 O 0.8452(4) 0.1078(4) 0.37963(16) 0.0927(19) Uani 1 1 d . . .
C5 C 0.9270(6) 0.2250(5) 0.2313(2) 0.091(3) Uani 1 1 d . . .
H5 H 0.9580 0.2642 0.2204 0.109 Uiso 1 1 calc R . .
O6 O 0.9531(5) 0.1842(4) 0.37889(15) 0.0932(19) Uani 1 1 d . . .
C6 C 0.8588(7) 0.2038(6) 0.2152(3) 0.098(3) Uani 1 1 d . . .
C7 C 0.8286(8) 0.2393(8) 0.1801(2) 0.118(4) Uani 1 1 d . . .
C8 C 0.8264(7) 0.3272(9) 0.1856(3) 0.152(5) Uani 1 1 d . . .
H8A H 0.8792 0.3463 0.1905 0.228 Uiso 1 1 calc R . .
H8B H 0.7924 0.3395 0.2058 0.228 Uiso 1 1 calc R . .
H8C H 0.8061 0.3524 0.1641 0.228 Uiso 1 1 calc R . .
C9 C 0.8895(10) 0.2228(13) 0.1520(3) 0.254(12) Uani 1 1 d . . .
H9A H 0.9223 0.2690 0.1487 0.381 Uiso 1 1 calc R . .
H9B H 0.8637 0.2099 0.1295 0.381 Uiso 1 1 calc R . .
H9C H 0.9219 0.1788 0.1596 0.381 Uiso 1 1 calc R . .
C10 C 0.7451(8) 0.2154(9) 0.1688(4) 0.178(6) Uani 1 1 d . . .
H10A H 0.7442 0.1598 0.1629 0.267 Uiso 1 1 calc R . .
H10B H 0.7294 0.2458 0.1479 0.267 Uiso 1 1 calc R . .
H10C H 0.7089 0.2256 0.1884 0.267 Uiso 1 1 calc R . .
C11 C 0.8832(8) 0.1679(8) 0.3881(2) 0.096(3) Uani 1 1 d . . .
C12 C 0.8459(8) 0.2231(6) 0.4139(2) 0.101(3) Uani 1 1 d . . .
C13 C 0.8771(8) 0.2881(9) 0.4213(3) 0.135(4) Uani 1 1 d . . .
H13 H 0.9241 0.3016 0.4094 0.163 Uiso 1 1 calc R . .
C14 C 0.8453(11) 0.3427(8) 0.4467(3) 0.165(6) Uani 1 1 d . . .
H14 H 0.8728 0.3884 0.4534 0.198 Uiso 1 1 calc R . .
C15 C 0.7775(11) 0.3262(10) 0.4599(3) 0.160(5) Uani 1 1 d U . .
C16 C 0.7397(11) 0.2582(10) 0.4528(4) 0.182(5) Uani 1 1 d U . .
H16 H 0.6910 0.2453 0.4632 0.218 Uiso 1 1 calc R . .
C17 C 0.7782(10) 0.2085(8) 0.4288(3) 0.174(5) Uani 1 1 d U . .
H17 H 0.7534 0.1607 0.4229 0.209 Uiso 1 1 calc R . .
N1 N 0.7699(15) 0.3969(14) 0.4850(5) 0.159(6) Uani 0.50 1 d PU . .
C18 C 0.7086(19) 0.3728(17) 0.4864(6) 0.159(8) Uani 0.50 1 d PU . .


_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
Co1 O5 2.011(7) . ?
Co1 O6 2.026(7) 2_645 ?
Co1 O3 2.059(6) 2_645 ?
Co1 O2 2.075(5) . ?
Co1 O2 2.086(5) 2_645 ?
Co1 O1 2.249(3) . ?
S1 O4 1.424(6) . ?
S1 O3 1.462(6) . ?
S1 C2 1.736(9) 4_665 ?
S1 C4 1.745(9) . ?
O1 Co1 2.249(3) 2_645 ?
O1 Co1 2.249(3) 3_755 ?
O1 Co1 2.249(3) 4_665 ?
C1 C2 1.406(11) . ?
C1 C6 1.384(12) . ?
C1 H1 0.9500 . ?
O2 C3 1.336(8) . ?
O2 Co1 2.086(5) 4_665 ?
C2 C3 1.434(11) . ?
C2 S1 1.736(9) 2_645 ?
O3 Co1 2.059(6) 4_665 ?
C3 C4 1.405(11) . ?
C4 C5 1.419(11) . ?
O5 C11 1.260(13) . ?
C5 C6 1.367(12) . ?
C5 H5 0.9500 . ?
O6 C11 1.280(12) . ?
O6 Co1 2.026(7) 4_665 ?
C6 C7 1.541(14) . ?
C7 C9 1.512(17) . ?
C7 C8 1.523(16) . ?
C7 C10 1.549(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.497(14) . ?
C12 C13 1.266(15) . ?
C12 C17 1.314(17) . ?
C13 C14 1.446(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.30(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.36(2) . ?
C15 N1 1.54(3) . ?
C15 C18 1.74(3) . ?
C16 C17 1.407(16) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N1 N1 1.13(4) 11_556 ?
N1 C18 1.56(3) 11_556 ?
C18 C18 1.02(5) 11_556 ?
C18 N1 1.56(3) 11_556 ?

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
O5 Co1 O6 84.0(3) . 2_645 ?
O5 Co1 O3 87.9(3) . 2_645 ?
O6 Co1 O3 87.3(2) 2_645 2_645 ?
O5 Co1 O2 94.2(3) . . ?
O6 Co1 O2 174.9(3) 2_645 . ?
O3 Co1 O2 87.8(2) 2_645 . ?
O5 Co1 O2 175.0(3) . 2_645 ?
O6 Co1 O2 92.8(2) 2_645 2_645 ?
O3 Co1 O2 88.0(2) 2_645 2_645 ?
O2 Co1 O2 88.6(3) . 2_645 ?
O5 Co1 O1 100.7(3) . . ?
O6 Co1 O1 101.1(2) 2_645 . ?
O3 Co1 O1 168.4(3) 2_645 . ?
O2 Co1 O1 83.9(2) . . ?
O2 Co1 O1 83.7(2) 2_645 . ?
O4 S1 O3 116.6(4) . . ?
O4 S1 C2 107.2(4) . 4_665 ?
O3 S1 C2 108.1(4) . 4_665 ?
O4 S1 C4 108.0(4) . . ?
O3 S1 C4 109.6(4) . . ?
C2 S1 C4 106.8(4) 4_665 . ?
Co1 O1 Co1 84.22(12) . 2_645 ?
Co1 O1 Co1 143.0(4) . 3_755 ?
Co1 O1 Co1 84.22(12) 2_645 3_755 ?
Co1 O1 Co1 84.22(12) . 4_665 ?
Co1 O1 Co1 143.0(4) 2_645 4_665 ?
Co1 O1 Co1 84.22(12) 3_755 4_665 ?
C2 C1 C6 121.9(9) . . ?
C2 C1 H1 119.1 . . ?
C6 C1 H1 119.1 . . ?
C3 O2 Co1 133.6(5) . . ?
C3 O2 Co1 131.8(5) . 4_665 ?
Co1 O2 Co1 92.9(2) . 4_665 ?
C1 C2 C3 121.0(8) . . ?
C1 C2 S1 114.1(7) . 2_645 ?
C3 C2 S1 124.6(6) . 2_645 ?
S1 O3 Co1 121.7(4) . 4_665 ?
O2 C3 C4 123.1(8) . . ?
O2 C3 C2 120.7(7) . . ?
C4 C3 C2 116.2(7) . . ?
C3 C4 C5 120.3(8) . . ?
C3 C4 S1 123.9(6) . . ?
C5 C4 S1 115.8(7) . . ?
C11 O5 Co1 127.5(7) . . ?
C6 C5 C4 123.1(9) . . ?
C6 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
C11 O6 Co1 127.2(7) . 4_665 ?
C5 C6 C1 117.4(9) . . ?
C5 C6 C7 124.2(10) . . ?
C1 C6 C7 118.4(10) . . ?
C9 C7 C8 107.3(12) . . ?
C9 C7 C10 113.4(12) . . ?
C8 C7 C10 106.0(11) . . ?
C9 C7 C6 106.9(10) . . ?
C8 C7 C6 106.5(9) . . ?
C10 C7 C6 116.2(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 O6 126.5(10) . . ?
O5 C11 C12 117.4(12) . . ?
O6 C11 C12 115.9(13) . . ?
C13 C12 C17 116.6(11) . . ?
C13 C12 C11 121.2(13) . . ?
C17 C12 C11 122.1(13) . . ?
C12 C13 C14 123.8(14) . . ?
C12 C13 H13 118.1 . . ?
C14 C13 H13 118.1 . . ?
C15 C14 C13 116.8(16) . . ?
C15 C14 H14 121.6 . . ?
C13 C14 H14 121.6 . . ?
C14 C15 C16 122.6(16) . . ?
C14 C15 N1 97.9(18) . . ?
C16 C15 N1 139.0(18) . . ?
C14 C15 C18 137(2) . . ?
C16 C15 C18 100.5(19) . . ?
N1 C15 C18 39.8(14) . . ?
C15 C16 C17 115.0(16) . . ?
C15 C16 H16 122.5 . . ?
C17 C16 H16 122.5 . . ?
C12 C17 C16 124.9(16) . . ?
C12 C17 H17 117.5 . . ?
C16 C17 H17 117.5 . . ?
N1 N1 C18 46.5(11) 11_556 11_556 ?
N1 N1 C15 127.7(9) 11_556 . ?
C18 N1 C15 106(2) 11_556 . ?
C18 C18 N1 46.5(11) 11_556 11_556 ?
C18 C18 C15 125.0(9) 11_556 . ?
N1 C18 C15 93.4(18) 11_556 . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.059 -0.004 -0.010 5272 2085 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        20.65
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.084
_exptl_crystal_recrystallization_method 'Solvothermal reaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1422949'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        3-Ni
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C144 H144 N4 Ni8 O42 S8'
_chemical_formula_sum            'C144 H144 N4 Ni8 O42 S8'
_chemical_formula_weight         3328.79

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'
S S 0.1246 0.1234 '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           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'


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

_cell_length_a                   12.968(2)
_cell_length_b                   13.910(3)
_cell_length_c                   27.919(5)
_cell_angle_alpha                79.284(2)
_cell_angle_beta                 83.244(2)
_cell_angle_gamma                67.342(2)
_cell_volume                     4560.6(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9972
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      22.79

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1724
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4772
_exptl_absorpt_correction_T_max  0.8455
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35816
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         0.74
_diffrn_reflns_theta_max         22.81
_reflns_number_total             12326
_reflns_number_gt                9256
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0845P)²+0.0058P] where P=(Fo²+2Fc²)/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_number_reflns         12326
_refine_ls_number_parameters     940
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1410
_refine_ls_wR_factor_gt          0.1341
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.089
_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 0.18936(4) 0.69196(4) 0.750474(18) 0.02467(16) Uani 1 1 d . . .
Ni2 Ni 0.42675(4) 0.59336(4) 0.779434(19) 0.02564(16) Uani 1 1 d . . .
Ni4 Ni 0.23081(5) 0.87889(5) 0.698594(18) 0.02707(17) Uani 1 1 d . . .
Ni3 Ni 0.46891(4) 0.78010(4) 0.726430(18) 0.02491(16) Uani 1 1 d . . .
S3 S 0.53982(8) 0.90120(8) 0.78801(3) 0.0205(3) Uani 1 1 d . . .
S1 S 0.01197(8) 0.73505(9) 0.83419(4) 0.0221(3) Uani 1 1 d . . .
S2 S 0.45880(9) 0.54936(9) 0.88888(4) 0.0238(3) Uani 1 1 d . . .
S4 S 0.09519(9) 1.08595(9) 0.73479(4) 0.0231(3) Uani 1 1 d . . .
O2 O 0.1415(2) 0.8479(2) 0.76084(10) 0.0267(7) Uani 1 1 d . . .
C11 C 0.2373(3) 0.6450(3) 0.85903(13) 0.0172(9) Uani 1 1 d . . .
O7 O 0.5029(2) 0.4801(2) 0.93307(10) 0.0298(7) Uani 1 1 d . . .
O4 O -0.0847(2) 0.7226(2) 0.86067(9) 0.0263(7) Uani 1 1 d . . .
O9 O 0.5667(2) 0.8544(2) 0.74330(9) 0.0250(7) Uani 1 1 d . . .
O3 O 0.0491(2) 0.6839(2) 0.79085(9) 0.0256(7) Uani 1 1 d . . .
O10 O 0.6120(2) 0.9516(2) 0.79676(9) 0.0237(7) Uani 1 1 d . . .
O6 O 0.4882(2) 0.5028(2) 0.84438(10) 0.0260(7) Uani 1 1 d . . .
O13 O 0.0281(2) 1.1961(2) 0.72611(10) 0.0288(7) Uani 1 1 d . . .
O11 O 0.3337(2) 0.9099(2) 0.73802(9) 0.0229(7) Uani 1 1 d . . .
O1 O 0.3418(2) 0.7151(2) 0.71908(10) 0.0308(7) Uani 1 1 d . . .
O12 O 0.1339(2) 1.0360(2) 0.69105(9) 0.0275(7) Uani 1 1 d . . .
O8 O 0.4606(2) 0.7141(2) 0.79799(9) 0.0260(7) Uani 1 1 d . . .
O5 O 0.2723(2) 0.6446(2) 0.81348(9) 0.0240(7) Uani 1 1 d . . .
O14 O 0.2288(3) 0.5459(2) 0.73763(10) 0.0324(7) Uani 1 1 d . . .
O15 O 0.4058(2) 0.4733(2) 0.75896(11) 0.0339(8) Uani 1 1 d . . .
O16 O 0.5772(3) 0.5270(3) 0.74490(12) 0.0445(9) Uani 1 1 d . . .
O17 O 0.6121(3) 0.6666(3) 0.70696(12) 0.0449(9) Uani 1 1 d . . .
C1 C 0.0523(3) 0.9104(3) 0.78257(14) 0.0196(9) Uani 1 1 d . . .
C4 C -0.1473(3) 1.0474(3) 0.82941(14) 0.0204(10) Uani 1 1 d . . .
C6 C 0.0174(3) 1.0210(3) 0.77400(13) 0.0213(10) Uani 1 1 d . . .
C2 C -0.0178(3) 0.8715(3) 0.81704(13) 0.0213(10) Uani 1 1 d . . .
C3 C -0.1143(3) 0.9388(3) 0.83943(14) 0.0226(10) Uani 1 1 d . . .
H3 H -0.1575 0.9096 0.8617 0.027 Uiso 1 1 calc R . .
C7 C -0.2535(3) 1.1233(3) 0.85269(15) 0.0255(10) Uani 1 1 d . . .
C5 C -0.0783(3) 1.0871(3) 0.79707(14) 0.0221(10) Uani 1 1 d . . .
H5 H -0.0962 1.1596 0.7906 0.026 Uiso 1 1 calc R . .
C8 C -0.2220(4) 1.1890(4) 0.88298(17) 0.0382(12) Uani 1 1 d . . .
H8A H -0.1801 1.1434 0.9100 0.057 Uiso 1 1 calc R . .
H8B H -0.2889 1.2407 0.8949 0.057 Uiso 1 1 calc R . .
H8C H -0.1775 1.2238 0.8629 0.057 Uiso 1 1 calc R . .
C10 C -0.3197(4) 1.0653(4) 0.88688(15) 0.0312(11) Uani 1 1 d . . .
H10A H -0.3415 1.0244 0.8688 0.047 Uiso 1 1 calc R . .
H10B H -0.3852 1.1158 0.9004 0.047 Uiso 1 1 calc R . .
H10C H -0.2737 1.0195 0.9128 0.047 Uiso 1 1 calc R . .
C9 C -0.3289(4) 1.1971(4) 0.81227(16) 0.0391(12) Uani 1 1 d . . .
H9A H -0.2893 1.2357 0.7912 0.059 Uiso 1 1 calc R . .
H9B H -0.3949 1.2456 0.8266 0.059 Uiso 1 1 calc R . .
H9C H -0.3498 1.1564 0.7937 0.059 Uiso 1 1 calc R . .
C14 C 0.1612(3) 0.6491(3) 0.96111(14) 0.0227(10) Uani 1 1 d . . .
C12 C 0.3119(3) 0.6048(3) 0.89800(15) 0.0235(10) Uani 1 1 d . . .
C13 C 0.2745(3) 0.6080(3) 0.94653(15) 0.0245(10) Uani 1 1 d . . .
H13 H 0.3271 0.5816 0.9704 0.029 Uiso 1 1 calc R . .
C15 C 0.0872(3) 0.6865(3) 0.92395(14) 0.0236(10) Uani 1 1 d . . .
H15 H 0.0109 0.7136 0.9321 0.028 Uiso 1 1 calc R . .
C17 C 0.1192(3) 0.6530(4) 1.01435(14) 0.0263(10) Uani 1 1 d . . .
C16 C 0.1225(3) 0.6850(3) 0.87494(14) 0.0211(10) Uani 1 1 d . . .
C19 C 0.0443(4) 0.5881(4) 1.02764(16) 0.0416(13) Uani 1 1 d . . .
H19A H -0.0186 0.6178 1.0073 0.062 Uiso 1 1 calc R . .
H19B H 0.0183 0.5894 1.0613 0.062 Uiso 1 1 calc R . .
H19C H 0.0865 0.5166 1.0227 0.062 Uiso 1 1 calc R . .
C18 C 0.0519(4) 0.7663(4) 1.02120(17) 0.0468(14) Uani 1 1 d . . .
H18A H 0.1003 0.8053 1.0161 0.070 Uiso 1 1 calc R . .
H18B H 0.0183 0.7682 1.0537 0.070 Uiso 1 1 calc R . .
H18C H -0.0057 0.7973 0.9981 0.070 Uiso 1 1 calc R . .
C20 C 0.2147(4) 0.6087(5) 1.04913(17) 0.0505(15) Uani 1 1 d . . .
H20A H 0.2542 0.5350 1.0477 0.076 Uiso 1 1 calc R . .
H20B H 0.1848 0.6179 1.0818 0.076 Uiso 1 1 calc R . .
H20C H 0.2651 0.6453 1.0398 0.076 Uiso 1 1 calc R . .
C21 C 0.5000(3) 0.7234(3) 0.83734(14) 0.0197(9) Uani 1 1 d . . .
C24 C 0.5828(3) 0.7481(3) 0.92463(14) 0.0229(10) Uani 1 1 d . . .
C26 C 0.5046(3) 0.6558(3) 0.88175(14) 0.0212(10) Uani 1 1 d . . .
C27 C 0.6270(4) 0.7638(4) 0.96983(15) 0.0281(11) Uani 1 1 d . . .
C23 C 0.5811(3) 0.8141(3) 0.88073(15) 0.0241(10) Uani 1 1 d . . .
H23 H 0.6078 0.8678 0.8794 0.029 Uiso 1 1 calc R . .
C22 C 0.5415(3) 0.8041(3) 0.83853(14) 0.0197(9) Uani 1 1 d . . .
C25 C 0.5446(3) 0.6687(3) 0.92412(14) 0.0226(10) Uani 1 1 d . . .
H25 H 0.5451 0.6218 0.9527 0.027 Uiso 1 1 calc R . .
C28 C 0.7463(5) 0.7588(5) 0.95848(19) 0.0635(17) Uani 1 1 d . . .
H28A H 0.7706 0.7785 0.9850 0.095 Uiso 1 1 calc R . .
H28B H 0.7492 0.8063 0.9291 0.095 Uiso 1 1 calc R . .
H28C H 0.7945 0.6882 0.9541 0.095 Uiso 1 1 calc R . .
C29 C 0.5568(5) 0.8782(5) 0.9808(2) 0.0689(18) Uani 1 1 d . . .
H29A H 0.4795 0.8869 0.9868 0.103 Uiso 1 1 calc R . .
H29B H 0.5640 0.9284 0.9532 0.103 Uiso 1 1 calc R . .
H29C H 0.5839 0.8896 1.0089 0.103 Uiso 1 1 calc R . .
C30 C 0.6171(9) 0.6886(7) 1.0129(2) 0.126(4) Uani 1 1 d . . .
H30A H 0.5404 0.6952 1.0187 0.189 Uiso 1 1 calc R . .
H30B H 0.6419 0.7034 1.0408 0.189 Uiso 1 1 calc R . .
H30C H 0.6625 0.6182 1.0073 0.189 Uiso 1 1 calc R . .
C31 C 0.3168(3) 0.9855(3) 0.76270(12) 0.0147(9) Uani 1 1 d . . .
C34 C 0.2769(3) 1.1546(3) 0.81965(13) 0.0218(10) Uani 1 1 d . . .
C33 C 0.1930(3) 1.1493(3) 0.79420(13) 0.0206(10) Uani 1 1 d . . .
H33 H 0.1215 1.2009 0.7958 0.025 Uiso 1 1 calc R . .
C37 C 0.2556(3) 1.2359(3) 0.85345(13) 0.0212(10) Uani 1 1 d . . .
C36 C 0.4015(3) 0.9941(3) 0.78779(13) 0.0196(9) Uani 1 1 d . . .
C32 C 0.2121(3) 1.0708(3) 0.76689(13) 0.0205(10) Uani 1 1 d . . .
C35 C 0.3822(3) 1.0742(3) 0.81507(13) 0.0191(9) Uani 1 1 d . . .
H35 H 0.4414 1.0744 0.8309 0.023 Uiso 1 1 calc R . .
C40 C 0.1555(4) 1.3371(4) 0.83833(17) 0.0397(12) Uani 1 1 d . . .
H40A H 0.1685 1.3662 0.8053 0.060 Uiso 1 1 calc R . .
H40B H 0.1463 1.3872 0.8595 0.060 Uiso 1 1 calc R . .
H40C H 0.0891 1.3213 0.8408 0.060 Uiso 1 1 calc R . .
C38 C 0.3586(4) 1.2628(4) 0.85410(15) 0.0302(11) Uani 1 1 d . . .
H38A H 0.4201 1.2003 0.8659 0.045 Uiso 1 1 calc R . .
H38B H 0.3431 1.3145 0.8752 0.045 Uiso 1 1 calc R . .
H38C H 0.3775 1.2907 0.8216 0.045 Uiso 1 1 calc R . .
C39 C 0.2290(4) 1.1862(4) 0.90509(15) 0.0401(13) Uani 1 1 d . . .
H39A H 0.1614 1.1731 0.9052 0.060 Uiso 1 1 calc R . .
H39B H 0.2193 1.2336 0.9277 0.060 Uiso 1 1 calc R . .
H39C H 0.2896 1.1209 0.9145 0.060 Uiso 1 1 calc R . .
C42 C 0.3378(4) 0.3754(4) 0.72015(14) 0.0298(11) Uani 1 1 d . . .
C41 C 0.3219(4) 0.4728(4) 0.74092(15) 0.0307(11) Uani 1 1 d . . .
C44 C 0.4569(5) 0.2051(4) 0.69979(17) 0.0477(14) Uani 1 1 d . . .
H44 H 0.5267 0.1506 0.7001 0.057 Uiso 1 1 calc R . .
C46 C 0.2664(5) 0.2771(4) 0.68064(16) 0.0432(14) Uani 1 1 d . . .
H46 H 0.2068 0.2714 0.6674 0.052 Uiso 1 1 calc R . .
C45 C 0.3692(5) 0.1969(4) 0.67966(15) 0.0449(14) Uani 1 1 d . . .
C43 C 0.4416(4) 0.2942(4) 0.71954(16) 0.0408(13) Uani 1 1 d . . .
H43 H 0.5017 0.2996 0.7325 0.049 Uiso 1 1 calc R . .
C47 C 0.2487(4) 0.3664(4) 0.70077(15) 0.0341(12) Uani 1 1 d . . .
H47 H 0.1781 0.4196 0.7013 0.041 Uiso 1 1 calc R . .
C49 C 0.3880(6) 0.1010(5) 0.65672(17) 0.071(2) Uani 1 1 d . . .
H49A H 0.3164 0.0976 0.6523 0.085 Uiso 1 1 calc R . .
H49B H 0.4299 0.0378 0.6782 0.085 Uiso 1 1 calc R . .
C59 C 0.7263(4) 0.5000(4) 0.68670(17) 0.0431(13) Uani 1 1 d . . .
C62 C 0.9040(5) 0.3672(6) 0.6336(2) 0.069(2) Uani 1 1 d . . .
C64 C 0.7937(5) 0.5412(5) 0.6543(2) 0.0620(17) Uani 1 1 d . . .
H64 H 0.7815 0.6125 0.6504 0.074 Uiso 1 1 calc R . .
C65 C 1.0027(5) 0.2971(6) 0.6056(2) 0.085(2) Uani 1 1 d . . .
H65A H 1.0621 0.3246 0.6011 0.101 Uiso 1 1 calc R . .
H65B H 1.0310 0.2268 0.6242 0.101 Uiso 1 1 calc R . .
C60 C 0.7460(5) 0.3945(4) 0.69152(19) 0.0517(14) Uani 1 1 d . . .
H60 H 0.6993 0.3675 0.7128 0.062 Uiso 1 1 calc R . .
C58 C 0.6319(4) 0.5697(4) 0.71503(17) 0.0379(12) Uani 1 1 d . . .
C63 C 0.8814(5) 0.4730(6) 0.6273(2) 0.075(2) Uani 1 1 d . . .
H63 H 0.9250 0.5009 0.6046 0.090 Uiso 1 1 calc R . .
C70 C 0.9528(4) 0.2075(4) 0.39202(17) 0.0434(13) Uani 1 1 d . . .
C73 C 0.9052(4) 0.2047(4) 0.34568(18) 0.0363(12) Uani 1 1 d . . .
N2 N 0.9703(4) 0.2916(5) 0.55711(17) 0.0843(19) Uani 1 1 d . . .
H2A H 0.9042 0.3241 0.5464 0.101 Uiso 1 1 calc R . .
C57 C 0.5859(5) 0.1326(4) 0.37488(17) 0.0442(13) Uani 1 1 d . . .
N1 N 0.4533(6) 0.1059(5) 0.60659(19) 0.0875(18) Uani 1 1 d . . .
H1A H 0.5244 0.0782 0.6008 0.105 Uiso 1 1 calc R . .
C61 C 0.8333(5) 0.3266(5) 0.6657(2) 0.0647(17) Uani 1 1 d . . .
H61 H 0.8448 0.2554 0.6696 0.078 Uiso 1 1 calc R . .
C54 C 0.5452(5) 0.1325(6) 0.42778(18) 0.072(2) Uani 1 1 d . . .
C67 C 1.0310(5) 0.2164(7) 0.4791(2) 0.078(2) Uani 1 1 d . . .
C69 C 0.9906(6) 0.2851(6) 0.3953(2) 0.086(2) Uani 1 1 d . . .
H69 H 0.9897 0.3359 0.3683 0.103 Uiso 1 1 calc R . .
C53 C 0.6163(7) 0.0933(8) 0.4639(2) 0.115(3) Uani 1 1 d . . .
H53 H 0.6931 0.0642 0.4571 0.138 Uiso 1 1 calc R . .
C55 C 0.4315(6) 0.1778(8) 0.4381(2) 0.126(4) Uani 1 1 d . . .
H55 H 0.3832 0.2053 0.4126 0.151 Uiso 1 1 calc R . .
C68 C 1.0311(7) 0.2879(8) 0.4397(3) 0.106(3) Uani 1 1 d . . .
H68 H 1.0581 0.3401 0.4416 0.127 Uiso 1 1 calc R . .
C66 C 1.0692(6) 0.2211(8) 0.5289(3) 0.122(4) Uani 1 1 d . . .
H66A H 1.0980 0.1507 0.5475 0.147 Uiso 1 1 calc R . .
H66B H 1.1285 0.2487 0.5237 0.147 Uiso 1 1 calc R . .
C71 C 0.9544(8) 0.1378(6) 0.4319(2) 0.110(3) Uani 1 1 d . . .
H71 H 0.9268 0.0856 0.4310 0.132 Uiso 1 1 calc R . .
C72 C 0.9963(10) 0.1409(7) 0.4751(3) 0.144(5) Uani 1 1 d . . .
H72 H 0.9999 0.0886 0.5017 0.173 Uiso 1 1 calc R . .
C56 C 0.3880(9) 0.1832(9) 0.4857(3) 0.142(4) Uani 1 1 d U . .
H56 H 0.3112 0.2130 0.4922 0.170 Uiso 1 1 calc R . .
C52 C 0.5718(9) 0.0970(10) 0.5132(3) 0.160(5) Uani 1 1 d . . .
H52 H 0.6187 0.0675 0.5392 0.192 Uiso 1 1 calc R . .
C51 C 0.4572(11) 0.1455(10) 0.5215(4) 0.147(4) Uani 1 1 d U . .
C50 C 0.3834(9) 0.1565(10) 0.5778(4) 0.191(6) Uani 1 1 d . . .
H50A H 0.3496 0.2295 0.5829 0.229 Uiso 1 1 calc R . .
H50B H 0.3253 0.1279 0.5801 0.229 Uiso 1 1 calc R . .
O19 O 0.5135(3) 0.1644(3) 0.34427(11) 0.0414(9) Uani 1 1 d . . .
O20 O 0.8935(3) 0.2773(3) 0.31189(11) 0.0402(8) Uani 1 1 d . . .
O18 O 0.6904(3) 0.0992(3) 0.36636(10) 0.0459(9) Uani 1 1 d . . .
O21 O 0.8774(3) 0.1274(3) 0.34655(11) 0.0462(9) Uani 1 1 d . . .


_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 O14 1.986(3) . ?
Ni1 O5 2.038(3) . ?
Ni1 O20 2.044(3) 2_666 ?
Ni1 O3 2.054(3) . ?
Ni1 O2 2.081(3) . ?
Ni1 O1 2.181(3) . ?
Ni1 Ni4 2.9396(9) . ?
Ni1 Ni2 2.9885(9) . ?
Ni2 O15 1.982(3) . ?
Ni2 O16 2.022(3) . ?
Ni2 O5 2.032(3) . ?
Ni2 O6 2.056(3) . ?
Ni2 O8 2.056(3) . ?
Ni2 O1 2.205(3) . ?
Ni2 Ni3 2.9515(9) . ?
Ni4 O18 2.006(3) 2_666 ?
Ni4 O21 2.029(3) 2_666 ?
Ni4 O11 2.036(3) . ?
Ni4 O2 2.044(3) . ?
Ni4 O12 2.043(3) . ?
Ni4 O1 2.184(3) . ?
Ni4 Ni3 2.9874(9) . ?
Ni3 O19 2.002(3) 2_666 ?
Ni3 O17 2.015(3) . ?
Ni3 O11 2.021(3) . ?
Ni3 O8 2.047(3) . ?
Ni3 O9 2.056(3) . ?
Ni3 O1 2.208(3) . ?
S3 O10 1.432(3) . ?
S3 O9 1.459(3) . ?
S3 C36 1.761(4) . ?
S3 C22 1.758(4) . ?
S1 O4 1.432(3) . ?
S1 O3 1.456(3) . ?
S1 C2 1.766(4) . ?
S1 C16 1.776(4) . ?
S2 O7 1.441(3) . ?
S2 O6 1.451(3) . ?
S2 C12 1.765(4) . ?
S2 C26 1.768(4) . ?
S4 O13 1.431(3) . ?
S4 O12 1.459(3) . ?
S4 C6 1.762(4) . ?
S4 C32 1.774(4) . ?
O2 C1 1.311(5) . ?
C11 O5 1.299(4) . ?
C11 C12 1.427(5) . ?
C11 C16 1.421(6) . ?
O11 C31 1.298(5) . ?
O8 C21 1.312(5) . ?
O14 C41 1.244(5) . ?
O15 C41 1.254(5) . ?
O16 C58 1.246(6) . ?
O17 C58 1.251(6) . ?
C1 C6 1.408(6) . ?
C1 C2 1.423(5) . ?
C4 C3 1.385(6) . ?
C4 C5 1.388(5) . ?
C4 C7 1.535(6) . ?
C6 C5 1.398(6) . ?
C2 C3 1.402(6) . ?
C3 H3 0.9300 . ?
C7 C10 1.534(6) . ?
C7 C9 1.529(6) . ?
C7 C8 1.540(6) . ?
C5 H5 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C14 C15 1.384(6) . ?
C14 C13 1.396(6) . ?
C14 C17 1.525(5) . ?
C12 C13 1.387(6) . ?
C13 H13 0.9300 . ?
C15 C16 1.392(5) . ?
C15 H15 0.9300 . ?
C17 C18 1.516(7) . ?
C17 C20 1.526(6) . ?
C17 C19 1.537(6) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C26 1.402(6) . ?
C21 C22 1.426(5) . ?
C24 C25 1.377(5) . ?
C24 C23 1.385(6) . ?
C24 C27 1.528(6) . ?
C26 C25 1.412(5) . ?
C27 C30 1.468(7) . ?
C27 C28 1.520(7) . ?
C27 C29 1.567(7) . ?
C23 C22 1.390(5) . ?
C23 H23 0.9300 . ?
C25 H25 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C36 1.423(5) . ?
C31 C32 1.428(6) . ?
C34 C35 1.402(6) . ?
C34 C33 1.399(5) . ?
C34 C37 1.530(6) . ?
C33 C32 1.376(6) . ?
C33 H33 0.9300 . ?
C37 C40 1.531(6) . ?
C37 C38 1.523(5) . ?
C37 C39 1.540(6) . ?
C36 C35 1.393(5) . ?
C35 H35 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C42 C43 1.385(7) . ?
C42 C47 1.389(6) . ?
C42 C41 1.504(6) . ?
C44 C43 1.385(7) . ?
C44 C45 1.378(7) . ?
C44 H44 0.9300 . ?
C46 C45 1.371(7) . ?
C46 C47 1.386(7) . ?
C46 H46 0.9300 . ?
C45 C49 1.511(7) . ?
C43 H43 0.9300 . ?
C47 H47 0.9300 . ?
C49 N1 1.553(7) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C59 C60 1.372(7) . ?
C59 C64 1.385(7) . ?
C59 C58 1.486(7) . ?
C62 C63 1.367(9) . ?
C62 C61 1.408(9) . ?
C62 C65 1.513(8) . ?
C64 C63 1.412(8) . ?
C64 H64 0.9300 . ?
C65 N2 1.487(6) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C60 C61 1.389(7) . ?
C60 H60 0.9300 . ?
C63 H63 0.9300 . ?
C70 C71 1.331(8) . ?
C70 C69 1.366(8) . ?
C70 C73 1.511(6) . ?
C73 O20 1.222(5) . ?
C73 O21 1.255(5) . ?
N2 C66 1.518(7) . ?
N2 H2A 0.8600 . ?
C57 O19 1.239(6) . ?
C57 O18 1.261(6) . ?
C57 C54 1.509(7) . ?
N1 C50 1.197(9) . ?
N1 H1A 0.8600 . ?
C61 H61 0.9300 . ?
C54 C53 1.338(9) . ?
C54 C55 1.380(9) . ?
C67 C72 1.317(11) . ?
C67 C68 1.338(10) . ?
C67 C66 1.552(8) . ?
C69 C68 1.416(8) . ?
C69 H69 0.9300 . ?
C53 C52 1.432(10) . ?
C53 H53 0.9300 . ?
C55 C56 1.384(10) . ?
C55 H55 0.9300 . ?
C68 H68 0.9300 . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C71 C72 1.394(9) . ?
C71 H71 0.9300 . ?
C72 H72 0.9300 . ?
C56 C51 1.317(13) . ?
C56 H56 0.9300 . ?
C52 C51 1.386(13) . ?
C52 H52 0.9300 . ?
C51 C50 1.739(13) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
O19 Ni3 2.002(3) 2_666 ?
O20 Ni1 2.044(3) 2_666 ?
O18 Ni4 2.006(3) 2_666 ?
O21 Ni4 2.029(3) 2_666 ?

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
O14 Ni1 O5 93.89(12) . . ?
O14 Ni1 O20 80.06(13) . 2_666 ?
O5 Ni1 O20 173.60(13) . 2_666 ?
O14 Ni1 O3 89.72(12) . . ?
O5 Ni1 O3 88.53(10) . . ?
O20 Ni1 O3 89.36(11) 2_666 . ?
O14 Ni1 O2 176.75(12) . . ?
O5 Ni1 O2 89.30(11) . . ?
O20 Ni1 O2 96.73(12) 2_666 . ?
O3 Ni1 O2 89.69(11) . . ?
O14 Ni1 O1 98.49(12) . . ?
O5 Ni1 O1 83.36(11) . . ?
O20 Ni1 O1 99.50(12) 2_666 . ?
O3 Ni1 O1 168.81(11) . . ?
O2 Ni1 O1 82.53(11) . . ?
O14 Ni1 Ni4 135.06(9) . . ?
O5 Ni1 Ni4 107.35(8) . . ?
O20 Ni1 Ni4 78.63(10) 2_666 . ?
O3 Ni1 Ni4 128.87(8) . . ?
O2 Ni1 Ni4 44.05(7) . . ?
O1 Ni1 Ni4 47.71(8) . . ?
O14 Ni1 Ni2 79.35(9) . . ?
O5 Ni1 Ni2 42.67(8) . . ?
O20 Ni1 Ni2 136.78(9) 2_666 . ?
O3 Ni1 Ni2 127.96(8) . . ?
O2 Ni1 Ni2 103.50(8) . . ?
O1 Ni1 Ni2 47.37(8) . . ?
Ni4 Ni1 Ni2 89.98(2) . . ?
O15 Ni2 O16 79.95(13) . . ?
O15 Ni2 O5 93.44(12) . . ?
O16 Ni2 O5 173.28(13) . . ?
O15 Ni2 O6 91.00(12) . . ?
O16 Ni2 O6 90.29(12) . . ?
O5 Ni2 O6 88.63(11) . . ?
O15 Ni2 O8 175.57(12) . . ?
O16 Ni2 O8 95.62(13) . . ?
O5 Ni2 O8 90.99(11) . . ?
O6 Ni2 O8 89.15(11) . . ?
O15 Ni2 O1 97.40(12) . . ?
O16 Ni2 O1 99.03(12) . . ?
O5 Ni2 O1 82.91(11) . . ?
O6 Ni2 O1 168.39(11) . . ?
O8 Ni2 O1 83.09(11) . . ?
O15 Ni2 Ni3 134.08(9) . . ?
O16 Ni2 Ni3 77.99(10) . . ?
O5 Ni2 Ni3 107.78(8) . . ?
O6 Ni2 Ni3 128.62(8) . . ?
O8 Ni2 Ni3 43.87(7) . . ?
O1 Ni2 Ni3 48.06(7) . . ?
O15 Ni2 Ni1 78.47(9) . . ?
O16 Ni2 Ni1 135.50(10) . . ?
O5 Ni2 Ni1 42.83(7) . . ?
O6 Ni2 Ni1 128.35(8) . . ?
O8 Ni2 Ni1 104.86(8) . . ?
O1 Ni2 Ni1 46.71(7) . . ?
Ni3 Ni2 Ni1 90.00(2) . . ?
O18 Ni4 O21 79.64(13) 2_666 2_666 ?
O18 Ni4 O11 95.77(11) 2_666 . ?
O21 Ni4 O11 170.55(13) 2_666 . ?
O18 Ni4 O2 173.20(12) 2_666 . ?
O21 Ni4 O2 94.14(12) 2_666 . ?
O11 Ni4 O2 90.79(11) . . ?
O18 Ni4 O12 90.41(13) 2_666 . ?
O21 Ni4 O12 84.31(13) 2_666 . ?
O11 Ni4 O12 87.48(11) . . ?
O2 Ni4 O12 91.71(11) . . ?
O18 Ni4 O1 95.59(13) 2_666 . ?
O21 Ni4 O1 104.92(13) 2_666 . ?
O11 Ni4 O1 83.65(11) . . ?
O2 Ni4 O1 83.29(11) . . ?
O12 Ni4 O1 169.74(10) . . ?
O18 Ni4 Ni1 130.22(11) 2_666 . ?
O21 Ni4 Ni1 80.29(10) 2_666 . ?
O11 Ni4 Ni1 108.79(8) . . ?
O2 Ni4 Ni1 45.05(8) . . ?
O12 Ni4 Ni1 131.97(8) . . ?
O1 Ni4 Ni1 47.62(7) . . ?
O18 Ni4 Ni3 79.52(9) 2_666 . ?
O21 Ni4 Ni3 142.83(11) 2_666 . ?
O11 Ni4 Ni3 42.37(8) . . ?
O2 Ni4 Ni3 104.33(8) . . ?
O12 Ni4 Ni3 126.19(8) . . ?
O1 Ni4 Ni3 47.47(7) . . ?
Ni1 Ni4 Ni3 90.25(2) . . ?
O19 Ni3 O17 79.33(13) 2_666 . ?
O19 Ni3 O11 92.95(12) 2_666 . ?
O17 Ni3 O11 170.83(12) . . ?
O19 Ni3 O8 175.98(13) 2_666 . ?
O17 Ni3 O8 96.66(13) . . ?
O11 Ni3 O8 91.07(11) . . ?
O19 Ni3 O9 89.58(12) 2_666 . ?
O17 Ni3 O9 87.07(13) . . ?
O11 Ni3 O9 87.92(11) . . ?
O8 Ni3 O9 90.55(10) . . ?
O19 Ni3 O1 97.25(12) 2_666 . ?
O17 Ni3 O1 102.37(13) . . ?
O11 Ni3 O1 83.40(11) . . ?
O8 Ni3 O1 83.23(10) . . ?
O9 Ni3 O1 169.20(11) . . ?
O19 Ni3 Ni2 134.05(10) 2_666 . ?
O17 Ni3 Ni2 80.86(10) . . ?
O11 Ni3 Ni2 108.20(8) . . ?
O8 Ni3 Ni2 44.12(7) . . ?
O9 Ni3 Ni2 130.24(8) . . ?
O1 Ni3 Ni2 47.97(8) . . ?
O19 Ni3 Ni4 78.68(9) 2_666 . ?
O17 Ni3 Ni4 138.41(10) . . ?
O11 Ni3 Ni4 42.76(7) . . ?
O8 Ni3 Ni4 104.38(8) . . ?
O9 Ni3 Ni4 127.44(8) . . ?
O1 Ni3 Ni4 46.81(8) . . ?
Ni2 Ni3 Ni4 89.77(2) . . ?
O10 S3 O9 115.39(16) . . ?
O10 S3 C36 108.17(18) . . ?
O9 S3 C36 109.83(17) . . ?
O10 S3 C22 108.17(17) . . ?
O9 S3 C22 109.66(18) . . ?
C36 S3 C22 105.11(18) . . ?
O4 S1 O3 115.62(16) . . ?
O4 S1 C2 107.86(19) . . ?
O3 S1 C2 108.93(17) . . ?
O4 S1 C16 107.64(17) . . ?
O3 S1 C16 109.14(18) . . ?
C2 S1 C16 107.34(18) . . ?
O7 S2 O6 116.39(18) . . ?
O7 S2 C12 107.59(18) . . ?
O6 S2 C12 109.92(18) . . ?
O7 S2 C26 107.80(18) . . ?
O6 S2 C26 108.88(18) . . ?
C12 S2 C26 105.73(19) . . ?
O13 S4 O12 115.00(17) . . ?
O13 S4 C6 108.37(19) . . ?
O12 S4 C6 109.24(18) . . ?
O13 S4 C32 107.51(18) . . ?
O12 S4 C32 109.55(18) . . ?
C6 S4 C32 106.86(17) . . ?
C1 O2 Ni4 130.4(3) . . ?
C1 O2 Ni1 131.6(2) . . ?
Ni4 O2 Ni1 90.90(11) . . ?
O5 C11 C12 122.5(4) . . ?
O5 C11 C16 123.9(3) . . ?
C12 C11 C16 113.6(3) . . ?
S3 O9 Ni3 119.18(15) . . ?
S1 O3 Ni1 119.72(15) . . ?
S2 O6 Ni2 119.72(17) . . ?
C31 O11 Ni3 133.0(2) . . ?
C31 O11 Ni4 132.2(2) . . ?
Ni3 O11 Ni4 94.87(12) . . ?
Ni1 O1 Ni4 84.67(10) . . ?
Ni1 O1 Ni2 85.91(10) . . ?
Ni4 O1 Ni2 145.49(14) . . ?
Ni1 O1 Ni3 146.30(14) . . ?
Ni4 O1 Ni3 85.72(10) . . ?
Ni2 O1 Ni3 83.97(10) . . ?
S4 O12 Ni4 118.76(16) . . ?
C21 O8 Ni3 132.1(2) . . ?
C21 O8 Ni2 132.1(3) . . ?
Ni3 O8 Ni2 92.01(10) . . ?
C11 O5 Ni2 133.4(2) . . ?
C11 O5 Ni1 132.1(2) . . ?
Ni2 O5 Ni1 94.50(11) . . ?
C41 O14 Ni1 127.2(3) . . ?
C41 O15 Ni2 128.4(3) . . ?
C58 O16 Ni2 129.4(3) . . ?
C58 O17 Ni3 125.6(3) . . ?
O2 C1 C6 123.3(3) . . ?
O2 C1 C2 122.4(4) . . ?
C6 C1 C2 114.2(4) . . ?
C3 C4 C5 116.8(4) . . ?
C3 C4 C7 123.3(4) . . ?
C5 C4 C7 119.9(4) . . ?
C5 C6 C1 123.0(4) . . ?
C5 C6 S4 115.1(3) . . ?
C1 C6 S4 121.9(3) . . ?
C3 C2 C1 122.2(4) . . ?
C3 C2 S1 116.0(3) . . ?
C1 C2 S1 121.8(3) . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C10 C7 C4 112.4(4) . . ?
C10 C7 C9 108.5(3) . . ?
C4 C7 C9 109.0(3) . . ?
C10 C7 C8 107.6(3) . . ?
C4 C7 C8 109.9(3) . . ?
C9 C7 C8 109.3(4) . . ?
C4 C5 C6 121.7(4) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C14 C13 115.8(4) . . ?
C15 C14 C17 121.0(4) . . ?
C13 C14 C17 123.2(4) . . ?
C13 C12 C11 122.4(4) . . ?
C13 C12 S2 114.2(3) . . ?
C11 C12 S2 123.3(3) . . ?
C12 C13 C14 122.7(4) . . ?
C12 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C14 C15 C16 122.6(4) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C18 C17 C20 108.1(4) . . ?
C18 C17 C14 109.5(3) . . ?
C20 C17 C14 112.3(4) . . ?
C18 C17 C19 109.4(4) . . ?
C20 C17 C19 108.6(4) . . ?
C14 C17 C19 109.0(3) . . ?
C15 C16 C11 122.7(4) . . ?
C15 C16 S1 114.3(3) . . ?
C11 C16 S1 122.9(3) . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O8 C21 C26 123.3(4) . . ?
O8 C21 C22 122.5(3) . . ?
C26 C21 C22 114.2(4) . . ?
C25 C24 C23 115.8(4) . . ?
C25 C24 C27 123.5(4) . . ?
C23 C24 C27 120.6(4) . . ?
C21 C26 C25 122.5(4) . . ?
C21 C26 S2 122.3(3) . . ?
C25 C26 S2 115.2(3) . . ?
C30 C27 C28 112.6(5) . . ?
C30 C27 C24 112.0(4) . . ?
C28 C27 C24 109.2(4) . . ?
C30 C27 C29 108.5(5) . . ?
C28 C27 C29 105.9(4) . . ?
C24 C27 C29 108.4(4) . . ?
C22 C23 C24 123.2(4) . . ?
C22 C23 H23 118.4 . . ?
C24 C23 H23 118.4 . . ?
C23 C22 C21 121.9(4) . . ?
C23 C22 S3 115.4(3) . . ?
C21 C22 S3 122.6(3) . . ?
C24 C25 C26 122.3(4) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O11 C31 C36 123.7(4) . . ?
O11 C31 C32 124.0(3) . . ?
C36 C31 C32 112.2(4) . . ?
C35 C34 C33 115.1(4) . . ?
C35 C34 C37 121.3(3) . . ?
C33 C34 C37 123.4(4) . . ?
C32 C33 C34 122.5(4) . . ?
C32 C33 H33 118.7 . . ?
C34 C33 H33 118.7 . . ?
C40 C37 C38 109.3(4) . . ?
C40 C37 C34 111.7(3) . . ?
C38 C37 C34 110.9(3) . . ?
C40 C37 C39 108.5(4) . . ?
C38 C37 C39 109.3(3) . . ?
C34 C37 C39 107.1(3) . . ?
C35 C36 C31 123.4(4) . . ?
C35 C36 S3 114.4(3) . . ?
C31 C36 S3 122.2(3) . . ?
C33 C32 C31 124.2(3) . . ?
C33 C32 S4 114.1(3) . . ?
C31 C32 S4 121.7(3) . . ?
C36 C35 C34 122.5(4) . . ?
C36 C35 H35 118.8 . . ?
C34 C35 H35 118.8 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C43 C42 C47 119.2(4) . . ?
C43 C42 C41 120.5(4) . . ?
C47 C42 C41 120.3(4) . . ?
O14 C41 O15 126.0(4) . . ?
O14 C41 C42 117.7(4) . . ?
O15 C41 C42 116.3(4) . . ?
C43 C44 C45 120.3(5) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C45 C46 C47 121.9(5) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C46 C45 C44 118.9(5) . . ?
C46 C45 C49 121.4(6) . . ?
C44 C45 C49 119.7(6) . . ?
C44 C43 C42 120.7(5) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C46 C47 C42 119.1(5) . . ?
C46 C47 H47 120.4 . . ?
C42 C47 H47 120.4 . . ?
C45 C49 N1 110.4(4) . . ?
C45 C49 H49A 109.6 . . ?
N1 C49 H49A 109.6 . . ?
C45 C49 H49B 109.6 . . ?
N1 C49 H49B 109.6 . . ?
H49A C49 H49B 108.1 . . ?
C60 C59 C64 119.3(5) . . ?
C60 C59 C58 120.3(5) . . ?
C64 C59 C58 120.4(5) . . ?
C63 C62 C61 118.7(6) . . ?
C63 C62 C65 119.5(7) . . ?
C61 C62 C65 121.8(7) . . ?
C59 C64 C63 118.9(6) . . ?
C59 C64 H64 120.6 . . ?
C63 C64 H64 120.6 . . ?
N2 C65 C62 111.0(5) . . ?
N2 C65 H65A 109.4 . . ?
C62 C65 H65A 109.4 . . ?
N2 C65 H65B 109.4 . . ?
C62 C65 H65B 109.4 . . ?
H65A C65 H65B 108.0 . . ?
C59 C60 C61 122.1(6) . . ?
C59 C60 H60 118.9 . . ?
C61 C60 H60 118.9 . . ?
O16 C58 O17 124.7(5) . . ?
O16 C58 C59 117.1(5) . . ?
O17 C58 C59 118.2(5) . . ?
C62 C63 C64 121.8(6) . . ?
C62 C63 H63 119.1 . . ?
C64 C63 H63 119.1 . . ?
C71 C70 C69 117.4(5) . . ?
C71 C70 C73 121.3(5) . . ?
C69 C70 C73 121.2(5) . . ?
O20 C73 O21 125.9(4) . . ?
O20 C73 C70 118.9(5) . . ?
O21 C73 C70 115.2(5) . . ?
C65 N2 C66 111.2(4) . . ?
C65 N2 H2A 124.4 . . ?
C66 N2 H2A 124.4 . . ?
O19 C57 O18 126.6(4) . . ?
O19 C57 C54 116.9(5) . . ?
O18 C57 C54 116.5(5) . . ?
C50 N1 C49 105.3(9) . . ?
C50 N1 H1A 127.4 . . ?
C49 N1 H1A 127.4 . . ?
C60 C61 C62 119.0(6) . . ?
C60 C61 H61 120.5 . . ?
C62 C61 H61 120.5 . . ?
C53 C54 C55 120.3(6) . . ?
C53 C54 C57 121.7(6) . . ?
C55 C54 C57 117.9(5) . . ?
C72 C67 C68 118.7(6) . . ?
C72 C67 C66 119.6(8) . . ?
C68 C67 C66 121.7(8) . . ?
C70 C69 C68 120.0(7) . . ?
C70 C69 H69 120.0 . . ?
C68 C69 H69 120.0 . . ?
C54 C53 C52 118.6(8) . . ?
C54 C53 H53 120.7 . . ?
C52 C53 H53 120.7 . . ?
C56 C55 C54 121.3(8) . . ?
C56 C55 H55 119.3 . . ?
C54 C55 H55 119.3 . . ?
C67 C68 C69 120.7(7) . . ?
C67 C68 H68 119.7 . . ?
C69 C68 H68 119.7 . . ?
N2 C66 C67 109.3(5) . . ?
N2 C66 H66A 109.8 . . ?
C67 C66 H66A 109.8 . . ?
N2 C66 H66B 109.8 . . ?
C67 C66 H66B 109.8 . . ?
H66A C66 H66B 108.3 . . ?
C70 C71 C72 121.7(7) . . ?
C70 C71 H71 119.2 . . ?
C72 C71 H71 119.2 . . ?
C67 C72 C71 121.5(8) . . ?
C67 C72 H72 119.3 . . ?
C71 C72 H72 119.3 . . ?
C51 C56 C55 118.9(9) . . ?
C51 C56 H56 120.5 . . ?
C55 C56 H56 120.5 . . ?
C51 C52 C53 118.7(8) . . ?
C51 C52 H52 120.7 . . ?
C53 C52 H52 120.7 . . ?
C56 C51 C52 122.0(8) . . ?
C56 C51 C50 110.7(9) . . ?
C52 C51 C50 127.1(10) . . ?
N1 C50 C51 103.8(9) . . ?
N1 C50 H50A 111.0 . . ?
C51 C50 H50A 111.0 . . ?
N1 C50 H50B 111.0 . . ?
C51 C50 H50B 111.0 . . ?
H50A C50 H50B 109.0 . . ?
C57 O19 Ni3 126.8(3) . 2_666 ?
C73 O20 Ni1 128.2(3) . 2_666 ?
C57 O18 Ni4 125.7(3) . 2_666 ?
C73 O21 Ni4 125.1(3) . 2_666 ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 264 94 ' '
2 0.495 -0.500 0.500 1150 354 ' '
3 0.172 0.448 0.936 10 0 ' '
4 0.827 0.552 0.064 10 1 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        22.81
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.083
_exptl_crystal_recrystallization_method 'Solvothermal reaction'
