# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_NiCe
_database_code_depnum_ccdc_archive 'CCDC 2165408'
loop_
_audit_author_name
_audit_author_address
'Zhong Zhang'
;Guangxi Normal University
China
;
_audit_update_record             
;
2022-04-08 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C15 H24 N3 Ni O6), Ce H16 O8, H3 O'
_chemical_formula_sum            'C60 H115 Ce N12 Ni4 O33'
_chemical_formula_weight         1907.60

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   18.4701(5)
_cell_length_b                   18.7158(5)
_cell_length_c                   25.6171(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8855.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3630
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      23.23

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3972
_exptl_absorpt_coefficient_mu    1.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 Smart Apex CCD II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29575
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         27.00
_reflns_number_total             17223
_reflns_number_gt                13844
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0800P)²+1.5500P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.492(12)
_refine_ls_number_reflns         17223
_refine_ls_number_parameters     1019
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
C1 C 0.3027(3) 0.2540(3) 0.0924(2) 0.0428(14) Uani 1 1 d . . .
H1A H 0.3532 0.2607 0.0834 0.051 Uiso 1 1 calc R . .
H1B H 0.2986 0.2527 0.1301 0.051 Uiso 1 1 calc R . .
C2 C 0.2576(3) 0.3151(3) 0.0706(2) 0.0464(15) Uani 1 1 d . . .
H2A H 0.2098 0.3139 0.0863 0.056 Uiso 1 1 calc R . .
H2B H 0.2801 0.3601 0.0801 0.056 Uiso 1 1 calc R . .
C3 C 0.3214(4) 0.3229(4) -0.0140(2) 0.0534(17) Uani 1 1 d . . .
H3A H 0.3605 0.3198 0.0111 0.064 Uiso 1 1 calc R . .
H3B H 0.3223 0.3703 -0.0294 0.064 Uiso 1 1 calc R . .
C4 C 0.3319(3) 0.2678(3) -0.0559(2) 0.0441(13) Uani 1 1 d . . .
H4A H 0.2997 0.2779 -0.0848 0.053 Uiso 1 1 calc R . .
H4B H 0.3813 0.2702 -0.0687 0.053 Uiso 1 1 calc R . .
C5 C 0.3727(3) 0.1729(3) 0.0024(2) 0.0447(12) Uani 1 1 d . . .
H5A H 0.4019 0.2139 0.0121 0.054 Uiso 1 1 calc R . .
H5B H 0.4044 0.1378 -0.0135 0.054 Uiso 1 1 calc R . .
C6 C 0.3390(4) 0.1415(3) 0.0504(2) 0.0457(15) Uani 1 1 d . . .
H6A H 0.3751 0.1390 0.0778 0.055 Uiso 1 1 calc R . .
H6B H 0.3231 0.0932 0.0429 0.055 Uiso 1 1 calc R . .
C7 C 0.2325(3) 0.1428(3) 0.1077(2) 0.0412(13) Uani 1 1 d . . .
H7A H 0.2633 0.1304 0.1370 0.049 Uiso 1 1 calc R . .
H7B H 0.2170 0.0986 0.0913 0.049 Uiso 1 1 calc R . .
C8 C 0.1664(3) 0.1823(3) 0.1278(2) 0.0437(14) Uani 1 1 d . . .
H8A H 0.1430 0.1518 0.1533 0.052 Uiso 1 1 calc R . .
H8B H 0.1834 0.2243 0.1464 0.052 Uiso 1 1 calc R . .
C9 C 0.1107(3) 0.2060(3) 0.0910(2) 0.0371(12) Uani 1 1 d . . .
C10 C 0.1920(3) 0.3613(3) -0.0040(2) 0.0424(12) Uani 1 1 d . . .
H10A H 0.1479 0.3493 0.0146 0.051 Uiso 1 1 calc R . .
H10B H 0.2056 0.4094 0.0060 0.051 Uiso 1 1 calc R . .
C11 C 0.1767(4) 0.3603(4) -0.0608(2) 0.0512(16) Uani 1 1 d . . .
H11A H 0.2210 0.3737 -0.0786 0.061 Uiso 1 1 calc R . .
H11B H 0.1416 0.3977 -0.0678 0.061 Uiso 1 1 calc R . .
C12 C 0.1487(4) 0.2920(3) -0.0867(2) 0.0452(14) Uani 1 1 d . . .
C13 C 0.3116(4) 0.1423(3) -0.0800(2) 0.0458(14) Uani 1 1 d . . .
H13A H 0.2742 0.1585 -0.1039 0.055 Uiso 1 1 calc R . .
H13B H 0.3571 0.1424 -0.0990 0.055 Uiso 1 1 calc R . .
C14 C 0.2953(3) 0.0689(3) -0.0646(2) 0.0446(14) Uani 1 1 d . . .
H14A H 0.3345 0.0530 -0.0423 0.053 Uiso 1 1 calc R . .
H14B H 0.2972 0.0400 -0.0960 0.053 Uiso 1 1 calc R . .
C15 C 0.2276(3) 0.0514(3) -0.0379(2) 0.0453(14) Uani 1 1 d . . .
C16 C 0.0993(3) 0.9108(3) 0.2957(2) 0.0429(14) Uani 1 1 d . . .
H16A H 0.1489 0.8944 0.2991 0.051 Uiso 1 1 calc R . .
H16B H 0.0785 0.9134 0.3304 0.051 Uiso 1 1 calc R . .
C17 C 0.0575(3) 0.8587(3) 0.2636(2) 0.0418(13) Uani 1 1 d . . .
H17A H 0.0853 0.8462 0.2328 0.050 Uiso 1 1 calc R . .
H17B H 0.0497 0.8154 0.2837 0.050 Uiso 1 1 calc R . .
C18 C -0.0648(3) 0.8955(3) 0.2927(2) 0.0404(13) Uani 1 1 d . . .
H18A H -0.1021 0.8591 0.2901 0.049 Uiso 1 1 calc R . .
H18B H -0.0388 0.8882 0.3251 0.049 Uiso 1 1 calc R . .
C19 C -0.0992(4) 0.9679(3) 0.2929(2) 0.0482(15) Uani 1 1 d . . .
H19A H -0.1355 0.9703 0.2656 0.058 Uiso 1 1 calc R . .
H19B H -0.1232 0.9756 0.3261 0.058 Uiso 1 1 calc R . .
C20 C 0.0037(3) 1.0344(3) 0.3292(2) 0.0431(14) Uani 1 1 d . . .
H20A H -0.0028 0.9950 0.3533 0.052 Uiso 1 1 calc R . .
H20B H -0.0085 1.0783 0.3473 0.052 Uiso 1 1 calc R . .
C21 C 0.0821(3) 1.0372(3) 0.3116(2) 0.0415(13) Uani 1 1 d . . .
H21A H 0.0925 1.0844 0.2979 0.050 Uiso 1 1 calc R . .
H21B H 0.1134 1.0294 0.3415 0.050 Uiso 1 1 calc R . .
C22 C 0.1690(3) 1.0024(3) 0.2463(2) 0.0416(11) Uani 1 1 d . . .
H22A H 0.2066 1.0039 0.2727 0.050 Uiso 1 1 calc R . .
H22B H 0.1654 1.0496 0.2308 0.050 Uiso 1 1 calc R . .
C23 C 0.1895(3) 0.9479(3) 0.2041(2) 0.0447(14) Uani 1 1 d . . .
H23A H 0.2377 0.9600 0.1920 0.054 Uiso 1 1 calc R . .
H23B H 0.1930 0.9016 0.2209 0.054 Uiso 1 1 calc R . .
C24 C 0.1432(3) 0.9388(3) 0.1570(2) 0.0424(13) Uani 1 1 d . . .
C25 C -0.0462(3) 0.8449(3) 0.2040(2) 0.0387(12) Uani 1 1 d . . .
H25A H -0.0126 0.8443 0.1749 0.046 Uiso 1 1 calc R . .
H25B H -0.0518 0.7961 0.2160 0.046 Uiso 1 1 calc R . .
C26 C -0.1170(3) 0.8709(3) 0.1851(2) 0.0396(12) Uani 1 1 d . . .
H26A H -0.1503 0.8705 0.2144 0.047 Uiso 1 1 calc R . .
H26B H -0.1350 0.8367 0.1598 0.047 Uiso 1 1 calc R . .
C27 C -0.1202(3) 0.9452(3) 0.1601(2) 0.0408(13) Uani 1 1 d . . .
C28 C -0.0834(3) 1.0948(3) 0.2716(2) 0.0378(13) Uani 1 1 d . . .
H28A H -0.1144 1.0868 0.2416 0.045 Uiso 1 1 calc R . .
H28B H -0.1143 1.1074 0.3008 0.045 Uiso 1 1 calc R . .
C29 C -0.0343(3) 1.1569(3) 0.2600(2) 0.0416(13) Uani 1 1 d . . .
H29A H -0.0642 1.1961 0.2479 0.050 Uiso 1 1 calc R . .
H29B H -0.0125 1.1719 0.2927 0.050 Uiso 1 1 calc R . .
C30 C 0.0252(4) 1.1465(3) 0.2213(2) 0.0438(14) Uani 1 1 d . . .
C31 C 0.0841(3) 1.0717(3) 0.7121(2) 0.0441(14) Uani 1 1 d . . .
H31A H 0.0896 1.0447 0.6800 0.053 Uiso 1 1 calc R . .
H31B H 0.1222 1.1073 0.7133 0.053 Uiso 1 1 calc R . .
C32 C 0.0131(3) 1.1077(3) 0.7121(2) 0.0408(13) Uani 1 1 d . . .
H32A H 0.0120 1.1427 0.7400 0.049 Uiso 1 1 calc R . .
H32B H 0.0068 1.1329 0.6794 0.049 Uiso 1 1 calc R . .
C33 C -0.0545(3) 1.0093(3) 0.6727(2) 0.0433(13) Uani 1 1 d . . .
H33A H -0.0127 1.0153 0.6501 0.052 Uiso 1 1 calc R . .
H33B H -0.0972 1.0228 0.6531 0.052 Uiso 1 1 calc R . .
C34 C -0.0605(4) 0.9307(3) 0.6888(2) 0.0478(15) Uani 1 1 d . . .
H34A H -0.1083 0.9216 0.7031 0.057 Uiso 1 1 calc R . .
H34B H -0.0539 0.9003 0.6585 0.057 Uiso 1 1 calc R . .
C35 C 0.0701(3) 0.9129(3) 0.7058(2) 0.0369(13) Uani 1 1 d . . .
H35A H 0.0859 0.8637 0.7021 0.044 Uiso 1 1 calc R . .
H35B H 0.0696 0.9344 0.6714 0.044 Uiso 1 1 calc R . .
C36 C 0.1224(3) 0.9521(3) 0.7395(2) 0.0463(14) Uani 1 1 d . . .
H36A H 0.1670 0.9599 0.7203 0.056 Uiso 1 1 calc R . .
H36B H 0.1336 0.9235 0.7700 0.056 Uiso 1 1 calc R . .
C37 C 0.1359(3) 1.0510(3) 0.8007(2) 0.0415(13) Uani 1 1 d . . .
H37A H 0.1857 1.0559 0.7893 0.050 Uiso 1 1 calc R . .
H37B H 0.1349 1.0164 0.8290 0.050 Uiso 1 1 calc R . .
C38 C 0.1090(3) 1.1232(3) 0.8211(2) 0.0416(13) Uani 1 1 d . . .
H38A H 0.1435 1.1401 0.8469 0.050 Uiso 1 1 calc R . .
H38B H 0.1099 1.1568 0.7923 0.050 Uiso 1 1 calc R . .
C39 C 0.0349(4) 1.1262(3) 0.8453(2) 0.0427(14) Uani 1 1 d . . .
C40 C -0.1124(3) 1.0937(3) 0.7399(2) 0.0435(14) Uani 1 1 d . . .
H40A H -0.1232 1.1346 0.7180 0.052 Uiso 1 1 calc R . .
H40B H -0.1018 1.1113 0.7746 0.052 Uiso 1 1 calc R . .
C41 C -0.1790(3) 1.0460(3) 0.7425(2) 0.0414(13) Uani 1 1 d . . .
H41A H -0.2206 1.0752 0.7514 0.050 Uiso 1 1 calc R . .
H41B H -0.1876 1.0257 0.7082 0.050 Uiso 1 1 calc R . .
C42 C -0.1729(3) 0.9869(3) 0.7811(2) 0.0467(14) Uani 1 1 d . . .
C43 C -0.0215(3) 0.8449(3) 0.7527(2) 0.0399(12) Uani 1 1 d . . .
H43A H -0.0222 0.8088 0.7255 0.048 Uiso 1 1 calc R . .
H43B H -0.0699 0.8474 0.7672 0.048 Uiso 1 1 calc R . .
C44 C 0.0299(3) 0.8194(3) 0.7959(2) 0.0417(13) Uani 1 1 d . . .
H44A H 0.0130 0.7732 0.8079 0.050 Uiso 1 1 calc R . .
H44B H 0.0773 0.8120 0.7804 0.050 Uiso 1 1 calc R . .
C45 C 0.0395(4) 0.8663(3) 0.8428(2) 0.0444(14) Uani 1 1 d . . .
C46 C 0.7281(3) 0.7263(3) 0.8973(2) 0.0413(13) Uani 1 1 d . . .
H46A H 0.7361 0.7619 0.8704 0.050 Uiso 1 1 calc R . .
H46B H 0.7172 0.6814 0.8801 0.050 Uiso 1 1 calc R . .
C47 C 0.6662(3) 0.7476(3) 0.9288(2) 0.0398(13) Uani 1 1 d . . .
H47A H 0.6267 0.7155 0.9203 0.048 Uiso 1 1 calc R . .
H47B H 0.6517 0.7949 0.9172 0.048 Uiso 1 1 calc R . .
C48 C 0.6503(3) 0.6803(3) 1.0091(2) 0.0401(13) Uani 1 1 d . . .
H48A H 0.6515 0.6427 0.9831 0.048 Uiso 1 1 calc R . .
H48B H 0.6023 0.6825 1.0244 0.048 Uiso 1 1 calc R . .
C49 C 0.7073(3) 0.6702(4) 1.0496(2) 0.0490(15) Uani 1 1 d . . .
H49A H 0.7045 0.7098 1.0739 0.059 Uiso 1 1 calc R . .
H49B H 0.6962 0.6270 1.0689 0.059 Uiso 1 1 calc R . .
C50 C 0.7983(3) 0.6134(3) 0.9892(2) 0.0392(13) Uani 1 1 d . . .
H50A H 0.8294 0.5763 1.0034 0.047 Uiso 1 1 calc R . .
H50B H 0.7542 0.5909 0.9770 0.047 Uiso 1 1 calc R . .
C51 C 0.8347(3) 0.6476(3) 0.9454(2) 0.0425(14) Uani 1 1 d . . .
H51A H 0.8350 0.6152 0.9158 0.051 Uiso 1 1 calc R . .
H51B H 0.8845 0.6576 0.9548 0.051 Uiso 1 1 calc R . .
C52 C 0.8554(4) 0.7584(3) 0.8910(2) 0.0467(14) Uani 1 1 d . . .
H52A H 0.9039 0.7465 0.9025 0.056 Uiso 1 1 calc R . .
H52B H 0.8496 0.7395 0.8560 0.056 Uiso 1 1 calc R . .
C53 C 0.8493(3) 0.8368(3) 0.8884(2) 0.0459(14) Uani 1 1 d . . .
H53A H 0.8158 0.8472 0.8602 0.055 Uiso 1 1 calc R . .
H53B H 0.8962 0.8543 0.8772 0.055 Uiso 1 1 calc R . .
C54 C 0.8271(3) 0.8821(3) 0.9328(2) 0.0453(14) Uani 1 1 d . . .
C55 C 0.6266(3) 0.8067(3) 1.0074(2) 0.0384(12) Uani 1 1 d . . .
H55A H 0.5770 0.7967 0.9975 0.046 Uiso 1 1 calc R . .
H55B H 0.6405 0.8512 0.9907 0.046 Uiso 1 1 calc R . .
C56 C 0.6290(3) 0.8177(3) 1.0666(2) 0.0394(12) Uani 1 1 d . . .
H56A H 0.5972 0.8574 1.0748 0.047 Uiso 1 1 calc R . .
H56B H 0.6083 0.7755 1.0827 0.047 Uiso 1 1 calc R . .
C57 C 0.7003(3) 0.8319(4) 1.0927(2) 0.0472(15) Uani 1 1 d . . .
C58 C 0.8307(4) 0.6599(3) 1.0751(2) 0.0453(15) Uani 1 1 d . . .
H58A H 0.8251 0.6133 1.0912 0.054 Uiso 1 1 calc R . .
H58B H 0.8174 0.6955 1.1009 0.054 Uiso 1 1 calc R . .
C59 C 0.9109(3) 0.6703(3) 1.0607(2) 0.0444(14) Uani 1 1 d . . .
H59A H 0.9394 0.6615 1.0919 0.053 Uiso 1 1 calc R . .
H59B H 0.9237 0.6337 1.0356 0.053 Uiso 1 1 calc R . .
C60 C 0.9340(4) 0.7406(3) 1.0388(2) 0.0463(14) Uani 1 1 d . . .
Ce1 Ce 0.987333(18) 0.001424(17) 0.002284(13) 0.04355(9) Uani 1 1 d . . .
N1 N 0.2754(3) 0.1846(3) 0.06949(18) 0.0403(11) Uani 1 1 d . . .
N2 N 0.2505(3) 0.3111(3) 0.01288(19) 0.0453(12) Uani 1 1 d . . .
N3 N 0.3172(3) 0.1952(3) -0.03586(18) 0.0443(12) Uani 1 1 d . . .
N4 N 0.0986(3) 0.9836(3) 0.27138(19) 0.0438(11) Uani 1 1 d . . .
N5 N -0.0135(3) 0.8885(2) 0.24749(18) 0.0404(10) Uani 1 1 d . . .
N6 N -0.0443(3) 1.0252(3) 0.28448(18) 0.0419(11) Uani 1 1 d . . .
N7 N 0.0914(3) 1.0236(3) 0.75663(18) 0.0441(11) Uani 1 1 d . . .
N8 N -0.0470(3) 1.0576(2) 0.71908(18) 0.0398(11) Uani 1 1 d . . .
N9 N -0.0050(2) 0.9143(2) 0.72818(18) 0.0376(11) Uani 1 1 d . . .
N10 N 0.7972(3) 0.7178(3) 0.92951(19) 0.0428(12) Uani 1 1 d . . .
N11 N 0.6724(3) 0.7500(2) 0.98693(16) 0.0395(11) Uani 1 1 d . . .
N12 N 0.7803(3) 0.6651(3) 1.03119(19) 0.0428(11) Uani 1 1 d . . .
Ni1 Ni 0.21957(4) 0.20614(4) 0.00187(3) 0.03958(16) Uani 1 1 d . . .
Ni2 Ni 0.01292(4) 0.98962(4) 0.22100(3) 0.03913(17) Uani 1 1 d . . .
Ni3 Ni -0.01121(4) 0.99679(4) 0.78150(3) 0.04037(16) Uani 1 1 d . . .
Ni4 Ni 0.78048(4) 0.76789(4) 1.00017(3) 0.04006(16) Uani 1 1 d . . .
O1 O 0.1189(2) 0.1978(2) 0.04213(14) 0.0400(9) Uani 1 1 d . . .
O2 O 0.0553(2) 0.2336(2) 0.10924(16) 0.0450(9) Uani 1 1 d . . .
O3 O 0.1486(2) 0.2349(2) -0.05968(15) 0.0415(9) Uani 1 1 d . . .
O4 O 0.1377(2) 0.2982(2) -0.13407(15) 0.0442(9) Uani 1 1 d . . .
O5 O 0.2035(2) 0.09336(19) -0.00229(17) 0.0450(9) Uani 1 1 d . . .
O6 O 0.1947(2) -0.0047(2) -0.04917(15) 0.0483(9) Uani 1 1 d . . .
O7 O 0.0738(2) 0.9343(2) 0.16316(15) 0.0418(9) Uani 1 1 d . . .
O8 O 0.1727(2) 0.9312(2) 0.11441(15) 0.0427(9) Uani 1 1 d . . .
O9 O -0.0718(2) 0.9886(2) 0.16873(14) 0.0408(9) Uani 1 1 d . . .
O10 O -0.1746(2) 0.9563(2) 0.13172(15) 0.0442(10) Uani 1 1 d . . .
O11 O 0.0187(2) 1.1066(2) 0.18280(15) 0.0449(9) Uani 1 1 d . . .
O12 O 0.0828(2) 1.1785(2) 0.23533(16) 0.0464(10) Uani 1 1 d . . .
O13 O -0.0112(2) 1.0775(2) 0.83559(15) 0.0407(9) Uani 1 1 d . . .
O14 O 0.0229(2) 1.1776(2) 0.87410(15) 0.0434(9) Uani 1 1 d . . .
O15 O -0.1155(2) 0.9825(2) 0.80868(14) 0.0408(9) Uani 1 1 d . . .
O16 O -0.2216(2) 0.9426(2) 0.78322(16) 0.0472(10) Uani 1 1 d . . .
O17 O 0.0206(2) 0.93007(19) 0.84106(14) 0.0374(8) Uani 1 1 d . . .
O18 O 0.0663(2) 0.8366(2) 0.88144(16) 0.0476(10) Uani 1 1 d . . .
O19 O 0.7805(2) 0.8672(2) 0.96585(15) 0.0418(9) Uani 1 1 d . . .
O20 O 0.8682(2) 0.9341(2) 0.93332(17) 0.0475(10) Uani 1 1 d . . .
O21 O 0.7588(2) 0.8200(2) 1.06878(15) 0.0438(10) Uani 1 1 d . . .
O22 O 0.6971(2) 0.8544(2) 1.13854(16) 0.0508(11) Uani 1 1 d . . .
O23 O 0.8967(2) 0.7702(2) 1.00389(17) 0.0443(9) Uani 1 1 d . . .
O24 O 0.9924(2) 0.7639(2) 1.05463(15) 0.0410(9) Uani 1 1 d . . .
O1W O 0.9364(2) 0.0659(2) 0.08643(14) 0.0423(9) Uani 1 1 d . . .
H1X H 0.9678 0.1046 0.0960 0.051 Uiso 1 1 d R . .
H1Y H 0.9341 0.0321 0.1145 0.051 Uiso 1 1 d R . .
O2W O 1.0910(2) 0.0421(2) 0.05398(16) 0.0469(10) Uani 1 1 d . . .
H2X H 1.1269 0.0050 0.0557 0.056 Uiso 1 1 d R . .
H2Y H 1.0748 0.0534 0.0886 0.056 Uiso 1 1 d R . .
O3W O 0.9842(2) 0.1431(2) -0.00725(16) 0.0488(9) Uani 1 1 d . . .
H3X H 1.0298 0.1603 -0.0202 0.059 Uiso 1 1 d R . .
H3Y H 0.9750 0.1636 0.0265 0.059 Uiso 1 1 d R . .
O4W O 1.0670(2) 0.0177(2) -0.06833(15) 0.0429(9) Uani 1 1 d . . .
H4X H 1.1073 0.0465 -0.0574 0.051 Uiso 1 1 d R . .
H4Y H 1.0419 0.0414 -0.0962 0.051 Uiso 1 1 d R . .
O5W O 0.9028(2) 0.0473(2) -0.07574(15) 0.0427(10) Uani 1 1 d . . .
H5X H 0.8973 0.0982 -0.0735 0.051 Uiso 1 1 d R . .
H5Y H 0.9246 0.0352 -0.1086 0.051 Uiso 1 1 d R . .
O6W O 0.9920(2) -0.1217(2) -0.03881(15) 0.0482(10) Uani 1 1 d . . .
H6X H 1.0041 -0.1175 -0.0751 0.058 Uiso 1 1 d R . .
H6Y H 0.9456 -0.1444 -0.0354 0.058 Uiso 1 1 d R . .
O7W O 0.8550(2) -0.0283(2) 0.03399(15) 0.0440(9) Uani 1 1 d . . .
H7X H 0.8556 -0.0359 0.0710 0.053 Uiso 1 1 d R . .
H7Y H 0.8380 -0.0708 0.0169 0.053 Uiso 1 1 d R . .
O8W O 1.0075(2) -0.08779(19) 0.06696(15) 0.0418(9) Uani 1 1 d . . .
H8X H 0.9829 -0.1309 0.0572 0.050 Uiso 1 1 d R . .
H8Y H 0.9892 -0.0714 0.0999 0.050 Uiso 1 1 d R . .
O9W O 0.7517(6) 0.7326(6) 0.2378(4) 0.016(2) Uani 0.25 1 d P . .
H91 H 0.7218 0.7007 0.2281 0.019 Uiso 0.25 1 d PR . .
H92 H 0.7873 0.7129 0.2531 0.019 Uiso 0.25 1 d PR . .
H93 H 0.7667 0.7556 0.2113 0.019 Uiso 0.25 1 d PR . .
O10W O 0.4995(8) 0.0031(7) 0.0014(6) 0.048(4) Uani 0.25 1 d P . .
H101 H 0.5132 0.0427 0.0143 0.058 Uiso 0.25 1 d PR . .
H102 H 0.5362 -0.0210 -0.0079 0.058 Uiso 0.25 1 d PR . .
H103 H 0.4758 -0.0202 0.0242 0.058 Uiso 0.25 1 d PR . .
O11W O 0.7460(8) 0.2280(8) 0.2325(6) 0.041(4) Uani 0.25 1 d P . .
H111 H 0.7215 0.2059 0.2095 0.049 Uiso 0.25 1 d PR . .
H112 H 0.7671 0.1980 0.2522 0.049 Uiso 0.25 1 d PR . .
H113 H 0.7775 0.2541 0.2176 0.049 Uiso 0.25 1 d PR . .
O12W O 0.5943(7) 0.0158(7) 0.9295(6) 0.039(3) Uani 0.25 1 d P . .
H121 H 0.6221 0.0415 0.9481 0.046 Uiso 0.25 1 d PR . .
H122 H 0.5505 0.0244 0.9374 0.046 Uiso 0.25 1 d PR . .
H123 H 0.6035 -0.0281 0.9349 0.046 Uiso 0.25 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.511(7) . ?
C1 C2 1.521(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.487(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.496(8) . ?
C3 C4 1.500(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N3 1.478(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N3 1.479(7) . ?
C5 C6 1.497(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.506(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.481(7) . ?
C7 C8 1.520(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.463(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O2 1.237(7) . ?
C9 O1 1.271(6) . ?
C10 C11 1.484(8) . ?
C10 N2 1.495(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.530(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O4 1.236(7) . ?
C12 O3 1.273(7) . ?
C13 C14 1.461(8) . ?
C13 N3 1.506(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.462(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O6 1.247(7) . ?
C15 O5 1.283(7) . ?
C16 C17 1.491(8) . ?
C16 N4 1.499(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N5 1.484(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.496(8) . ?
C18 N5 1.502(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N6 1.492(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N6 1.459(7) . ?
C20 C21 1.518(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N4 1.470(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N4 1.491(7) . ?
C22 C23 1.536(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.489(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 O8 1.227(7) . ?
C24 O7 1.295(7) . ?
C25 C26 1.477(8) . ?
C25 N5 1.507(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.532(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 O9 1.228(7) . ?
C27 O10 1.258(7) . ?
C28 C29 1.504(8) . ?
C28 N6 1.526(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.494(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 O11 1.243(7) . ?
C30 O12 1.273(8) . ?
C31 N7 1.460(8) . ?
C31 C32 1.475(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 N8 1.463(8) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 N8 1.499(7) . ?
C33 C34 1.532(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N9 1.471(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.487(8) . ?
C35 N9 1.501(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 N7 1.521(7) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 N7 1.488(7) . ?
C37 C38 1.533(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.503(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 O14 1.233(7) . ?
C39 O13 1.271(7) . ?
C40 N8 1.483(7) . ?
C40 C41 1.521(8) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.489(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 O16 1.224(7) . ?
C42 O15 1.276(7) . ?
C43 N9 1.476(7) . ?
C43 C44 1.534(8) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.499(8) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 O18 1.237(7) . ?
C45 O17 1.245(7) . ?
C46 C47 1.455(8) . ?
C46 N10 1.529(7) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 N11 1.495(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 N11 1.480(7) . ?
C48 C49 1.490(8) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 N12 1.431(8) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C51 1.457(8) . ?
C50 N12 1.483(7) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 N10 1.539(8) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.473(8) . ?
C52 N10 1.646(8) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.475(8) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 O20 1.235(7) . ?
C54 O19 1.240(7) . ?
C55 N11 1.455(7) . ?
C55 C56 1.530(7) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 C57 1.500(8) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 O22 1.249(7) . ?
C57 O21 1.263(7) . ?
C58 N12 1.463(8) . ?
C58 C59 1.540(9) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.492(8) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 O24 1.232(7) . ?
C60 O23 1.257(7) . ?
Ce1 O4W 2.352(4) . ?
Ce1 O8W 2.382(4) . ?
Ce1 O2W 2.450(4) . ?
Ce1 O6W 2.534(4) . ?
Ce1 O7W 2.635(4) . ?
Ce1 O1W 2.644(4) . ?
Ce1 O3W 2.664(4) . ?
Ce1 O5W 2.677(4) . ?
N1 Ni1 2.056(5) . ?
N2 Ni1 2.065(5) . ?
N3 Ni1 2.056(5) . ?
N4 Ni2 2.046(5) . ?
N5 Ni2 2.069(5) . ?
N6 Ni2 2.050(4) . ?
N7 Ni3 2.061(5) . ?
N8 Ni3 2.071(5) . ?
N9 Ni3 2.064(4) . ?
N10 Ni4 2.062(5) . ?
N11 Ni4 2.053(5) . ?
N12 Ni4 2.082(5) . ?
Ni1 O3 2.120(4) . ?
Ni1 O1 2.132(4) . ?
Ni1 O5 2.134(4) . ?
Ni2 O9 2.059(4) . ?
Ni2 O7 2.129(4) . ?
Ni2 O11 2.400(4) . ?
Ni3 O13 2.050(4) . ?
Ni3 O17 2.057(4) . ?
Ni3 O15 2.065(4) . ?
Ni4 O21 2.050(4) . ?
Ni4 O19 2.056(4) . ?
Ni4 O23 2.150(4) . ?
O1W H1X 0.9599 . ?
O1W H1Y 0.9601 . ?
O2W H2X 0.9599 . ?
O2W H2Y 0.9598 . ?
O3W H3X 0.9598 . ?
O3W H3Y 0.9602 . ?
O4W H4X 0.9601 . ?
O4W H4Y 0.9598 . ?
O5W H5X 0.9599 . ?
O5W H5Y 0.9601 . ?
O6W H6X 0.9601 . ?
O6W H6Y 0.9600 . ?
O7W H7X 0.9599 . ?
O7W H7Y 0.9601 . ?
O8W H8X 0.9600 . ?
O8W H8Y 0.9599 . ?
O9W H91 0.8500 . ?
O9W H92 0.8500 . ?
O9W H93 0.8499 . ?
O10W H101 0.8499 . ?
O10W H102 0.8500 . ?
O10W H103 0.8499 . ?
O11W H111 0.8500 . ?
O11W H112 0.8499 . ?
O11W H113 0.8500 . ?
O12W H121 0.8500 . ?
O12W H122 0.8500 . ?
O12W H123 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 108.8(5) . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 112.0(5) . . ?
N2 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 C4 110.0(5) . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 111.2(5) . . ?
N3 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N3 C5 C6 111.5(5) . . ?
N3 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N3 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 N1 112.4(5) . . ?
C5 C6 H6A 109.1 . . ?
N1 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
N1 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N1 C7 C8 113.4(5) . . ?
N1 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
N1 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C7 119.6(5) . . ?
C9 C8 H8A 107.4 . . ?
C7 C8 H8A 107.4 . . ?
C9 C8 H8B 107.4 . . ?
C7 C8 H8B 107.4 . . ?
H8A C8 H8B 107.0 . . ?
O2 C9 O1 121.3(5) . . ?
O2 C9 C8 117.7(5) . . ?
O1 C9 C8 121.0(5) . . ?
C11 C10 N2 114.4(5) . . ?
C11 C10 H10A 108.7 . . ?
N2 C10 H10A 108.7 . . ?
C11 C10 H10B 108.7 . . ?
N2 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C10 C11 C12 120.0(6) . . ?
C10 C11 H11A 107.3 . . ?
C12 C11 H11A 107.3 . . ?
C10 C11 H11B 107.3 . . ?
C12 C11 H11B 107.3 . . ?
H11A C11 H11B 106.9 . . ?
O4 C12 O3 127.8(6) . . ?
O4 C12 C11 113.7(5) . . ?
O3 C12 C11 117.8(5) . . ?
C14 C13 N3 115.4(5) . . ?
C14 C13 H13A 108.4 . . ?
N3 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
N3 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C13 C14 C15 120.9(5) . . ?
C13 C14 H14A 107.1 . . ?
C15 C14 H14A 107.1 . . ?
C13 C14 H14B 107.1 . . ?
C15 C14 H14B 107.1 . . ?
H14A C14 H14B 106.8 . . ?
O6 C15 O5 120.7(6) . . ?
O6 C15 C14 119.8(5) . . ?
O5 C15 C14 119.5(5) . . ?
C17 C16 N4 111.2(5) . . ?
C17 C16 H16A 109.4 . . ?
N4 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
N4 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N5 C17 C16 111.4(5) . . ?
N5 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
N5 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
C19 C18 N5 110.5(5) . . ?
C19 C18 H18A 109.5 . . ?
N5 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
N5 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N6 C19 C18 111.2(5) . . ?
N6 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
N6 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
N6 C20 C21 110.5(4) . . ?
N6 C20 H20A 109.5 . . ?
C21 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
N4 C21 C20 112.5(5) . . ?
N4 C21 H21A 109.1 . . ?
C20 C21 H21A 109.1 . . ?
N4 C21 H21B 109.1 . . ?
C20 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
N4 C22 C23 111.2(5) . . ?
N4 C22 H22A 109.4 . . ?
C23 C22 H22A 109.4 . . ?
N4 C22 H22B 109.4 . . ?
C23 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 C22 120.4(5) . . ?
C24 C23 H23A 107.2 . . ?
C22 C23 H23A 107.2 . . ?
C24 C23 H23B 107.2 . . ?
C22 C23 H23B 107.2 . . ?
H23A C23 H23B 106.9 . . ?
O8 C24 O7 122.8(5) . . ?
O8 C24 C23 118.5(5) . . ?
O7 C24 C23 118.5(5) . . ?
C26 C25 N5 114.8(5) . . ?
C26 C25 H25A 108.6 . . ?
N5 C25 H25A 108.6 . . ?
C26 C25 H25B 108.6 . . ?
N5 C25 H25B 108.6 . . ?
H25A C25 H25B 107.5 . . ?
C25 C26 C27 118.0(5) . . ?
C25 C26 H26A 107.8 . . ?
C27 C26 H26A 107.8 . . ?
C25 C26 H26B 107.8 . . ?
C27 C26 H26B 107.8 . . ?
H26A C26 H26B 107.1 . . ?
O9 C27 O10 125.2(6) . . ?
O9 C27 C26 119.8(5) . . ?
O10 C27 C26 115.0(6) . . ?
C29 C28 N6 114.6(5) . . ?
C29 C28 H28A 108.6 . . ?
N6 C28 H28A 108.6 . . ?
C29 C28 H28B 108.6 . . ?
N6 C28 H28B 108.6 . . ?
H28A C28 H28B 107.6 . . ?
C30 C29 C28 118.3(5) . . ?
C30 C29 H29A 107.7 . . ?
C28 C29 H29A 107.7 . . ?
C30 C29 H29B 107.7 . . ?
C28 C29 H29B 107.7 . . ?
H29A C29 H29B 107.1 . . ?
O11 C30 O12 126.0(6) . . ?
O11 C30 C29 122.2(6) . . ?
O12 C30 C29 111.5(5) . . ?
N7 C31 C32 111.3(5) . . ?
N7 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
N7 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
N8 C32 C31 112.4(5) . . ?
N8 C32 H32A 109.1 . . ?
C31 C32 H32A 109.1 . . ?
N8 C32 H32B 109.1 . . ?
C31 C32 H32B 109.1 . . ?
H32A C32 H32B 107.9 . . ?
N8 C33 C34 111.8(5) . . ?
N8 C33 H33A 109.3 . . ?
C34 C33 H33A 109.3 . . ?
N8 C33 H33B 109.3 . . ?
C34 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
N9 C34 C33 109.5(5) . . ?
N9 C34 H34A 109.8 . . ?
C33 C34 H34A 109.8 . . ?
N9 C34 H34B 109.8 . . ?
C33 C34 H34B 109.8 . . ?
H34A C34 H34B 108.2 . . ?
C36 C35 N9 111.7(5) . . ?
C36 C35 H35A 109.3 . . ?
N9 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
N9 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 N7 110.9(5) . . ?
C35 C36 H36A 109.5 . . ?
N7 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
N7 C36 H36B 109.5 . . ?
H36A C36 H36B 108.0 . . ?
N7 C37 C38 112.5(5) . . ?
N7 C37 H37A 109.1 . . ?
C38 C37 H37A 109.1 . . ?
N7 C37 H37B 109.1 . . ?
C38 C37 H37B 109.1 . . ?
H37A C37 H37B 107.8 . . ?
C39 C38 C37 117.9(5) . . ?
C39 C38 H38A 107.8 . . ?
C37 C38 H38A 107.8 . . ?
C39 C38 H38B 107.8 . . ?
C37 C38 H38B 107.8 . . ?
H38A C38 H38B 107.2 . . ?
O14 C39 O13 123.8(6) . . ?
O14 C39 C38 116.0(6) . . ?
O13 C39 C38 120.2(5) . . ?
N8 C40 C41 114.1(5) . . ?
N8 C40 H40A 108.7 . . ?
C41 C40 H40A 108.7 . . ?
N8 C40 H40B 108.7 . . ?
C41 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
C42 C41 C40 113.9(5) . . ?
C42 C41 H41A 108.8 . . ?
C40 C41 H41A 108.8 . . ?
C42 C41 H41B 108.8 . . ?
C40 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
O16 C42 O15 123.0(5) . . ?
O16 C42 C41 118.5(5) . . ?
O15 C42 C41 118.5(5) . . ?
N9 C43 C44 117.0(5) . . ?
N9 C43 H43A 108.1 . . ?
C44 C43 H43A 108.1 . . ?
N9 C43 H43B 108.1 . . ?
C44 C43 H43B 108.1 . . ?
H43A C43 H43B 107.3 . . ?
C45 C44 C43 118.0(5) . . ?
C45 C44 H44A 107.8 . . ?
C43 C44 H44A 107.8 . . ?
C45 C44 H44B 107.8 . . ?
C43 C44 H44B 107.8 . . ?
H44A C44 H44B 107.1 . . ?
O18 C45 O17 124.9(5) . . ?
O18 C45 C44 115.1(5) . . ?
O17 C45 C44 120.0(5) . . ?
C47 C46 N10 112.7(4) . . ?
C47 C46 H46A 109.1 . . ?
N10 C46 H46A 109.1 . . ?
C47 C46 H46B 109.1 . . ?
N10 C46 H46B 109.1 . . ?
H46A C46 H46B 107.8 . . ?
C46 C47 N11 120.0(5) . . ?
C46 C47 H47A 107.3 . . ?
N11 C47 H47A 107.3 . . ?
C46 C47 H47B 107.3 . . ?
N11 C47 H47B 107.3 . . ?
H47A C47 H47B 106.9 . . ?
N11 C48 C49 100.6(5) . . ?
N11 C48 H48A 111.7 . . ?
C49 C48 H48A 111.7 . . ?
N11 C48 H48B 111.7 . . ?
C49 C48 H48B 111.7 . . ?
H48A C48 H48B 109.4 . . ?
N12 C49 C48 116.4(5) . . ?
N12 C49 H49A 108.2 . . ?
C48 C49 H49A 108.2 . . ?
N12 C49 H49B 108.2 . . ?
C48 C49 H49B 108.2 . . ?
H49A C49 H49B 107.3 . . ?
C51 C50 N12 112.0(5) . . ?
C51 C50 H50A 109.2 . . ?
N12 C50 H50A 109.2 . . ?
C51 C50 H50B 109.2 . . ?
N12 C50 H50B 109.2 . . ?
H50A C50 H50B 107.9 . . ?
C50 C51 N10 111.8(5) . . ?
C50 C51 H51A 109.3 . . ?
N10 C51 H51A 109.3 . . ?
C50 C51 H51B 109.3 . . ?
N10 C51 H51B 109.3 . . ?
H51A C51 H51B 107.9 . . ?
C53 C52 N10 115.9(5) . . ?
C53 C52 H52A 108.3 . . ?
N10 C52 H52A 108.3 . . ?
C53 C52 H52B 108.3 . . ?
N10 C52 H52B 108.3 . . ?
H52A C52 H52B 107.4 . . ?
C52 C53 C54 124.0(5) . . ?
C52 C53 H53A 106.3 . . ?
C54 C53 H53A 106.3 . . ?
C52 C53 H53B 106.3 . . ?
C54 C53 H53B 106.3 . . ?
H53A C53 H53B 106.4 . . ?
O20 C54 O19 126.6(6) . . ?
O20 C54 C53 106.9(5) . . ?
O19 C54 C53 126.2(6) . . ?
N11 C55 C56 116.0(5) . . ?
N11 C55 H55A 108.3 . . ?
C56 C55 H55A 108.3 . . ?
N11 C55 H55B 108.3 . . ?
C56 C55 H55B 108.3 . . ?
H55A C55 H55B 107.4 . . ?
C57 C56 C55 119.4(5) . . ?
C57 C56 H56A 107.5 . . ?
C55 C56 H56A 107.5 . . ?
C57 C56 H56B 107.5 . . ?
C55 C56 H56B 107.5 . . ?
H56A C56 H56B 107.0 . . ?
O22 C57 O21 123.7(6) . . ?
O22 C57 C56 116.0(5) . . ?
O21 C57 C56 120.2(5) . . ?
N12 C58 C59 114.8(5) . . ?
N12 C58 H58A 108.6 . . ?
C59 C58 H58A 108.6 . . ?
N12 C58 H58B 108.6 . . ?
C59 C58 H58B 108.6 . . ?
H58A C58 H58B 107.5 . . ?
C60 C59 C58 118.5(5) . . ?
C60 C59 H59A 107.7 . . ?
C58 C59 H59A 107.7 . . ?
C60 C59 H59B 107.7 . . ?
C58 C59 H59B 107.7 . . ?
H59A C59 H59B 107.1 . . ?
O24 C60 O23 123.9(6) . . ?
O24 C60 C59 116.0(5) . . ?
O23 C60 C59 119.9(5) . . ?
O4W Ce1 O8W 121.91(13) . . ?
O4W Ce1 O2W 83.47(14) . . ?
O8W Ce1 O2W 73.71(13) . . ?
O4W Ce1 O6W 77.14(13) . . ?
O8W Ce1 O6W 69.29(12) . . ?
O2W Ce1 O6W 118.70(14) . . ?
O4W Ce1 O7W 147.66(13) . . ?
O8W Ce1 O7W 77.42(13) . . ?
O2W Ce1 O7W 128.63(13) . . ?
O6W Ce1 O7W 88.12(13) . . ?
O4W Ce1 O1W 142.24(13) . . ?
O8W Ce1 O1W 78.96(13) . . ?
O2W Ce1 O1W 72.29(13) . . ?
O6W Ce1 O1W 139.98(13) . . ?
O7W Ce1 O1W 60.99(13) . . ?
O4W Ce1 O3W 79.26(13) . . ?
O8W Ce1 O3W 139.92(13) . . ?
O2W Ce1 O3W 75.96(13) . . ?
O6W Ce1 O3W 150.19(13) . . ?
O7W Ce1 O3W 102.63(13) . . ?
O1W Ce1 O3W 67.20(12) . . ?
O4W Ce1 O5W 75.46(13) . . ?
O8W Ce1 O5W 146.65(12) . . ?
O2W Ce1 O5W 139.44(13) . . ?
O6W Ce1 O5W 90.08(13) . . ?
O7W Ce1 O5W 75.94(11) . . ?
O1W Ce1 O5W 104.75(12) . . ?
O3W Ce1 O5W 66.40(12) . . ?
C7 N1 C6 110.4(5) . . ?
C7 N1 C1 112.1(4) . . ?
C6 N1 C1 109.0(5) . . ?
C7 N1 Ni1 113.1(3) . . ?
C6 N1 Ni1 102.9(3) . . ?
C1 N1 Ni1 109.0(4) . . ?
C2 N2 C10 108.7(5) . . ?
C2 N2 C3 111.9(5) . . ?
C10 N2 C3 114.0(5) . . ?
C2 N2 Ni1 102.0(4) . . ?
C10 N2 Ni1 111.0(3) . . ?
C3 N2 Ni1 108.6(4) . . ?
C4 N3 C5 111.2(5) . . ?
C4 N3 C13 110.8(4) . . ?
C5 N3 C13 111.1(5) . . ?
C4 N3 Ni1 103.4(4) . . ?
C5 N3 Ni1 108.9(4) . . ?
C13 N3 Ni1 111.0(4) . . ?
C21 N4 C22 108.7(4) . . ?
C21 N4 C16 109.3(4) . . ?
C22 N4 C16 112.7(5) . . ?
C21 N4 Ni2 104.1(3) . . ?
C22 N4 Ni2 112.9(3) . . ?
C16 N4 Ni2 108.6(4) . . ?
C17 N5 C18 112.1(4) . . ?
C17 N5 C25 110.9(4) . . ?
C18 N5 C25 111.3(5) . . ?
C17 N5 Ni2 103.2(4) . . ?
C18 N5 Ni2 108.8(3) . . ?
C25 N5 Ni2 110.3(3) . . ?
C20 N6 C19 112.6(5) . . ?
C20 N6 C28 110.9(4) . . ?
C19 N6 C28 108.8(4) . . ?
C20 N6 Ni2 110.4(3) . . ?
C19 N6 Ni2 103.5(3) . . ?
C28 N6 Ni2 110.5(3) . . ?
C31 N7 C37 115.6(5) . . ?
C31 N7 C36 110.6(4) . . ?
C37 N7 C36 108.3(4) . . ?
C31 N7 Ni3 107.9(4) . . ?
C37 N7 Ni3 110.9(3) . . ?
C36 N7 Ni3 102.8(4) . . ?
C32 N8 C40 111.7(4) . . ?
C32 N8 C33 111.1(4) . . ?
C40 N8 C33 118.9(5) . . ?
C32 N8 Ni3 101.8(4) . . ?
C40 N8 Ni3 103.5(3) . . ?
C33 N8 Ni3 108.1(3) . . ?
C34 N9 C43 109.4(5) . . ?
C34 N9 C35 112.8(4) . . ?
C43 N9 C35 109.8(4) . . ?
C34 N9 Ni3 105.0(3) . . ?
C43 N9 Ni3 111.4(3) . . ?
C35 N9 Ni3 108.5(3) . . ?
C46 N10 C51 127.4(4) . . ?
C46 N10 C52 100.0(4) . . ?
C51 N10 C52 105.0(4) . . ?
C46 N10 Ni4 107.6(4) . . ?
C51 N10 Ni4 102.9(3) . . ?
C52 N10 Ni4 114.5(3) . . ?
C55 N11 C48 110.2(4) . . ?
C55 N11 C47 109.7(4) . . ?
C48 N11 C47 109.6(4) . . ?
C55 N11 Ni4 112.7(3) . . ?
C48 N11 Ni4 110.4(3) . . ?
C47 N11 Ni4 104.1(4) . . ?
C49 N12 C58 110.5(5) . . ?
C49 N12 C50 119.6(5) . . ?
C58 N12 C50 111.8(5) . . ?
C49 N12 Ni4 93.8(4) . . ?
C58 N12 Ni4 110.7(4) . . ?
C50 N12 Ni4 109.0(3) . . ?
N1 Ni1 N3 86.38(19) . . ?
N1 Ni1 N2 86.2(2) . . ?
N3 Ni1 N2 85.2(2) . . ?
N1 Ni1 O3 170.61(17) . . ?
N3 Ni1 O3 102.60(17) . . ?
N2 Ni1 O3 91.78(17) . . ?
N1 Ni1 O1 90.89(17) . . ?
N3 Ni1 O1 170.03(18) . . ?
N2 Ni1 O1 104.16(18) . . ?
O3 Ni1 O1 80.72(15) . . ?
N1 Ni1 O5 85.27(18) . . ?
N3 Ni1 O5 89.97(18) . . ?
N2 Ni1 O5 170.43(17) . . ?
O3 Ni1 O5 97.36(16) . . ?
O1 Ni1 O5 80.24(15) . . ?
N4 Ni2 N6 85.18(19) . . ?
N4 Ni2 O9 176.09(18) . . ?
N6 Ni2 O9 97.32(17) . . ?
N4 Ni2 N5 85.7(2) . . ?
N6 Ni2 N5 85.14(19) . . ?
O9 Ni2 N5 91.50(18) . . ?
N4 Ni2 O7 90.23(17) . . ?
N6 Ni2 O7 169.13(18) . . ?
O9 Ni2 O7 86.79(15) . . ?
N5 Ni2 O7 84.69(17) . . ?
N4 Ni2 O11 105.85(18) . . ?
N6 Ni2 O11 92.89(17) . . ?
O9 Ni2 O11 77.09(15) . . ?
N5 Ni2 O11 168.11(18) . . ?
O7 Ni2 O11 97.85(15) . . ?
O13 Ni3 O17 86.92(15) . . ?
O13 Ni3 N7 91.67(18) . . ?
O17 Ni3 N7 96.59(18) . . ?
O13 Ni3 N9 176.63(18) . . ?
O17 Ni3 N9 91.21(17) . . ?
N7 Ni3 N9 85.76(19) . . ?
O13 Ni3 O15 82.39(16) . . ?
O17 Ni3 O15 86.44(15) . . ?
N7 Ni3 O15 173.20(18) . . ?
N9 Ni3 O15 100.29(17) . . ?
O13 Ni3 N8 96.71(17) . . ?
O17 Ni3 N8 175.81(17) . . ?
N7 Ni3 N8 85.45(19) . . ?
N9 Ni3 N8 85.27(19) . . ?
O15 Ni3 N8 91.94(17) . . ?
O21 Ni4 N11 91.68(16) . . ?
O21 Ni4 O19 86.35(16) . . ?
N11 Ni4 O19 94.39(17) . . ?
O21 Ni4 N10 176.87(19) . . ?
N11 Ni4 N10 85.76(19) . . ?
O19 Ni4 N10 92.05(17) . . ?
O21 Ni4 N12 96.45(19) . . ?
N11 Ni4 N12 84.86(19) . . ?
O19 Ni4 N12 177.12(18) . . ?
N10 Ni4 N12 85.12(19) . . ?
O21 Ni4 O23 98.49(16) . . ?
N11 Ni4 O23 169.14(17) . . ?
O19 Ni4 O23 90.07(16) . . ?
N10 Ni4 O23 84.19(19) . . ?
N12 Ni4 O23 90.19(18) . . ?
C9 O1 Ni1 124.8(4) . . ?
C12 O3 Ni1 128.0(4) . . ?
C15 O5 Ni1 126.3(4) . . ?
C24 O7 Ni2 125.2(4) . . ?
C27 O9 Ni2 132.5(4) . . ?
C30 O11 Ni2 103.3(3) . . ?
C39 O13 Ni3 131.3(4) . . ?
C42 O15 Ni3 125.5(3) . . ?
C45 O17 Ni3 133.6(4) . . ?
C54 O19 Ni4 119.7(4) . . ?
C57 O21 Ni4 131.9(4) . . ?
C60 O23 Ni4 124.7(4) . . ?
Ce1 O1W H1X 109.7 . . ?
Ce1 O1W H1Y 109.0 . . ?
H1X O1W H1Y 109.5 . . ?
Ce1 O2W H2X 109.8 . . ?
Ce1 O2W H2Y 109.0 . . ?
H2X O2W H2Y 109.5 . . ?
Ce1 O3W H3X 110.3 . . ?
Ce1 O3W H3Y 108.5 . . ?
H3X O3W H3Y 109.5 . . ?
Ce1 O4W H4X 109.4 . . ?
Ce1 O4W H4Y 109.3 . . ?
H4X O4W H4Y 109.5 . . ?
Ce1 O5W H5X 109.6 . . ?
Ce1 O5W H5Y 109.5 . . ?
H5X O5W H5Y 109.5 . . ?
Ce1 O6W H6X 109.6 . . ?
Ce1 O6W H6Y 109.5 . . ?
H6X O6W H6Y 109.5 . . ?
Ce1 O7W H7X 108.9 . . ?
Ce1 O7W H7Y 109.7 . . ?
H7X O7W H7Y 109.5 . . ?
Ce1 O8W H8X 109.5 . . ?
Ce1 O8W H8Y 109.5 . . ?
H8X O8W H8Y 109.5 . . ?
H91 O9W H92 109.4 . . ?
H91 O9W H93 109.5 . . ?
H92 O9W H93 109.5 . . ?
H101 O10W H102 109.5 . . ?
H101 O10W H103 109.5 . . ?
H102 O10W H103 109.5 . . ?
H111 O11W H112 109.5 . . ?
H111 O11W H113 109.5 . . ?
H112 O11W H113 109.5 . . ?
H121 O12W H122 109.5 . . ?
H121 O12W H123 109.5 . . ?
H122 O12W H123 109.5 . . ?

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
N1 C1 C2 N2 -48.7(6) . . . . ?
N2 C3 C4 N3 -48.6(7) . . . . ?
N3 C5 C6 N1 -44.2(7) . . . . ?
N1 C7 C8 C9 59.5(6) . . . . ?
C7 C8 C9 O2 175.0(5) . . . . ?
C7 C8 C9 O1 -4.3(8) . . . . ?
N2 C10 C11 C12 62.7(8) . . . . ?
C10 C11 C12 O4 179.6(6) . . . . ?
C10 C11 C12 O3 -9.3(9) . . . . ?
N3 C13 C14 C15 61.8(8) . . . . ?
C13 C14 C15 O6 140.6(6) . . . . ?
C13 C14 C15 O5 -41.0(8) . . . . ?
N4 C16 C17 N5 -46.5(7) . . . . ?
N5 C18 C19 N6 -46.1(6) . . . . ?
N6 C20 C21 N4 -42.3(6) . . . . ?
N4 C22 C23 C24 63.3(7) . . . . ?
C22 C23 C24 O8 138.9(6) . . . . ?
C22 C23 C24 O7 -45.7(8) . . . . ?
N5 C25 C26 C27 63.0(7) . . . . ?
C25 C26 C27 O9 -20.0(8) . . . . ?
C25 C26 C27 O10 160.2(5) . . . . ?
N6 C28 C29 C30 50.1(7) . . . . ?
C28 C29 C30 O11 33.6(8) . . . . ?
C28 C29 C30 O12 -141.2(5) . . . . ?
N7 C31 C32 N8 -49.5(7) . . . . ?
N8 C33 C34 N9 -46.2(7) . . . . ?
N9 C35 C36 N7 -45.7(6) . . . . ?
N7 C37 C38 C39 64.1(7) . . . . ?
C37 C38 C39 O14 159.9(5) . . . . ?
C37 C38 C39 O13 -20.2(8) . . . . ?
N8 C40 C41 C42 67.0(7) . . . . ?
C40 C41 C42 O16 -174.6(5) . . . . ?
C40 C41 C42 O15 1.9(8) . . . . ?
N9 C43 C44 C45 58.5(7) . . . . ?
C43 C44 C45 O18 162.9(5) . . . . ?
C43 C44 C45 O17 -16.7(9) . . . . ?
N10 C46 C47 N11 -7.5(8) . . . . ?
N11 C48 C49 N12 -62.3(6) . . . . ?
N12 C50 C51 N10 -45.3(6) . . . . ?
N10 C52 C53 C54 33.5(9) . . . . ?
C52 C53 C54 O20 136.5(6) . . . . ?
C52 C53 C54 O19 -37.5(10) . . . . ?
N11 C55 C56 C57 56.2(7) . . . . ?
C55 C56 C57 O22 166.1(5) . . . . ?
C55 C56 C57 O21 -15.0(9) . . . . ?
N12 C58 C59 C60 62.7(7) . . . . ?
C58 C59 C60 O24 139.5(6) . . . . ?
C58 C59 C60 O23 -45.0(8) . . . . ?
C8 C7 N1 C6 -178.8(5) . . . . ?
C8 C7 N1 C1 59.5(6) . . . . ?
C8 C7 N1 Ni1 -64.2(5) . . . . ?
C5 C6 N1 C7 165.2(5) . . . . ?
C5 C6 N1 C1 -71.3(6) . . . . ?
C5 C6 N1 Ni1 44.3(6) . . . . ?
C2 C1 N1 C7 -104.9(5) . . . . ?
C2 C1 N1 C6 132.6(5) . . . . ?
C2 C1 N1 Ni1 21.0(5) . . . . ?
C1 C2 N2 C10 166.4(4) . . . . ?
C1 C2 N2 C3 -66.8(6) . . . . ?
C1 C2 N2 Ni1 49.2(5) . . . . ?
C11 C10 N2 C2 -177.4(5) . . . . ?
C11 C10 N2 C3 57.1(7) . . . . ?
C11 C10 N2 Ni1 -66.0(6) . . . . ?
C4 C3 N2 C2 134.0(5) . . . . ?
C4 C3 N2 C10 -102.1(6) . . . . ?
C4 C3 N2 Ni1 22.2(6) . . . . ?
C3 C4 N3 C5 -68.4(7) . . . . ?
C3 C4 N3 C13 167.5(5) . . . . ?
C3 C4 N3 Ni1 48.4(6) . . . . ?
C6 C5 N3 C4 132.7(5) . . . . ?
C6 C5 N3 C13 -103.3(6) . . . . ?
C6 C5 N3 Ni1 19.4(6) . . . . ?
C14 C13 N3 C4 -178.5(5) . . . . ?
C14 C13 N3 C5 57.3(7) . . . . ?
C14 C13 N3 Ni1 -64.1(6) . . . . ?
C20 C21 N4 C22 164.8(5) . . . . ?
C20 C21 N4 C16 -71.7(6) . . . . ?
C20 C21 N4 Ni2 44.2(5) . . . . ?
C23 C22 N4 C21 179.6(5) . . . . ?
C23 C22 N4 C16 58.2(6) . . . . ?
C23 C22 N4 Ni2 -65.4(5) . . . . ?
C17 C16 N4 C21 133.5(5) . . . . ?
C17 C16 N4 C22 -105.4(6) . . . . ?
C17 C16 N4 Ni2 20.5(6) . . . . ?
C16 C17 N5 C18 -70.2(6) . . . . ?
C16 C17 N5 C25 164.7(5) . . . . ?
C16 C17 N5 Ni2 46.6(5) . . . . ?
C19 C18 N5 C17 132.2(5) . . . . ?
C19 C18 N5 C25 -103.0(6) . . . . ?
C19 C18 N5 Ni2 18.8(6) . . . . ?
C26 C25 N5 C17 -179.7(5) . . . . ?
C26 C25 N5 C18 54.8(6) . . . . ?
C26 C25 N5 Ni2 -66.1(5) . . . . ?
C21 C20 N6 C19 132.4(5) . . . . ?
C21 C20 N6 C28 -105.5(5) . . . . ?
C21 C20 N6 Ni2 17.3(6) . . . . ?
C18 C19 N6 C20 -70.6(6) . . . . ?
C18 C19 N6 C28 166.0(5) . . . . ?
C18 C19 N6 Ni2 48.6(5) . . . . ?
C29 C28 N6 C20 57.8(6) . . . . ?
C29 C28 N6 C19 -177.8(5) . . . . ?
C29 C28 N6 Ni2 -64.9(5) . . . . ?
C32 C31 N7 C37 -102.1(6) . . . . ?
C32 C31 N7 C36 134.3(5) . . . . ?
C32 C31 N7 Ni3 22.7(6) . . . . ?
C38 C37 N7 C31 55.4(7) . . . . ?
C38 C37 N7 C36 -179.9(5) . . . . ?
C38 C37 N7 Ni3 -67.8(5) . . . . ?
C35 C36 N7 C31 -67.5(6) . . . . ?
C35 C36 N7 C37 164.8(5) . . . . ?
C35 C36 N7 Ni3 47.4(5) . . . . ?
C31 C32 N8 C40 157.3(5) . . . . ?
C31 C32 N8 C33 -67.4(6) . . . . ?
C31 C32 N8 Ni3 47.4(5) . . . . ?
C41 C40 N8 C32 173.8(5) . . . . ?
C41 C40 N8 C33 42.4(7) . . . . ?
C41 C40 N8 Ni3 -77.4(5) . . . . ?
C34 C33 N8 C32 131.2(5) . . . . ?
C34 C33 N8 C40 -97.1(6) . . . . ?
C34 C33 N8 Ni3 20.3(6) . . . . ?
C33 C34 N9 C43 166.6(5) . . . . ?
C33 C34 N9 C35 -71.0(6) . . . . ?
C33 C34 N9 Ni3 46.9(5) . . . . ?
C44 C43 N9 C34 -178.7(5) . . . . ?
C44 C43 N9 C35 57.1(6) . . . . ?
C44 C43 N9 Ni3 -63.1(5) . . . . ?
C36 C35 N9 C34 134.8(5) . . . . ?
C36 C35 N9 C43 -103.0(5) . . . . ?
C36 C35 N9 Ni3 19.0(5) . . . . ?
C47 C46 N10 C51 106.4(6) . . . . ?
C47 C46 N10 C52 -135.9(5) . . . . ?
C47 C46 N10 Ni4 -16.1(6) . . . . ?
C50 C51 N10 C46 -78.4(7) . . . . ?
C50 C51 N10 C52 166.1(5) . . . . ?
C50 C51 N10 Ni4 46.0(5) . . . . ?
C53 C52 N10 C46 72.4(6) . . . . ?
C53 C52 N10 C51 -154.3(5) . . . . ?
C53 C52 N10 Ni4 -42.2(6) . . . . ?
C56 C55 N11 C48 61.3(6) . . . . ?
C56 C55 N11 C47 -177.9(5) . . . . ?
C56 C55 N11 Ni4 -62.4(5) . . . . ?
C49 C48 N11 C55 -101.8(5) . . . . ?
C49 C48 N11 C47 137.4(5) . . . . ?
C49 C48 N11 Ni4 23.3(5) . . . . ?
C46 C47 N11 C55 147.6(5) . . . . ?
C46 C47 N11 C48 -91.4(6) . . . . ?
C46 C47 N11 Ni4 26.7(6) . . . . ?
C48 C49 N12 C58 176.4(5) . . . . ?
C48 C49 N12 C50 -51.8(7) . . . . ?
C48 C49 N12 Ni4 62.6(5) . . . . ?
C59 C58 N12 C49 -167.5(5) . . . . ?
C59 C58 N12 C50 56.7(7) . . . . ?
C59 C58 N12 Ni4 -65.0(6) . . . . ?
C51 C50 N12 C49 126.0(6) . . . . ?
C51 C50 N12 C58 -102.7(6) . . . . ?
C51 C50 N12 Ni4 20.0(6) . . . . ?
C7 N1 Ni1 N3 -144.9(4) . . . . ?
C6 N1 Ni1 N3 -25.8(4) . . . . ?
C1 N1 Ni1 N3 89.8(4) . . . . ?
C7 N1 Ni1 N2 129.7(4) . . . . ?
C6 N1 Ni1 N2 -111.2(4) . . . . ?
C1 N1 Ni1 N2 4.3(4) . . . . ?
C7 N1 Ni1 O1 25.6(4) . . . . ?
C6 N1 Ni1 O1 144.6(4) . . . . ?
C1 N1 Ni1 O1 -99.8(3) . . . . ?
C7 N1 Ni1 O5 -54.6(4) . . . . ?
C6 N1 Ni1 O5 64.5(4) . . . . ?
C1 N1 Ni1 O5 -179.9(4) . . . . ?
C4 N3 Ni1 N1 -114.0(4) . . . . ?
C5 N3 Ni1 N1 4.4(4) . . . . ?
C13 N3 Ni1 N1 127.0(4) . . . . ?
C4 N3 Ni1 N2 -27.6(3) . . . . ?
C5 N3 Ni1 N2 90.8(4) . . . . ?
C13 N3 Ni1 N2 -146.5(4) . . . . ?
C4 N3 Ni1 O3 63.2(4) . . . . ?
C5 N3 Ni1 O3 -178.4(4) . . . . ?
C13 N3 Ni1 O3 -55.8(4) . . . . ?
C4 N3 Ni1 O5 160.7(3) . . . . ?
C5 N3 Ni1 O5 -80.9(4) . . . . ?
C13 N3 Ni1 O5 41.8(4) . . . . ?
C2 N2 Ni1 N1 -28.3(4) . . . . ?
C10 N2 Ni1 N1 -143.9(4) . . . . ?
C3 N2 Ni1 N1 90.0(4) . . . . ?
C2 N2 Ni1 N3 -115.0(4) . . . . ?
C10 N2 Ni1 N3 129.4(4) . . . . ?
C3 N2 Ni1 N3 3.3(4) . . . . ?
C2 N2 Ni1 O3 142.5(4) . . . . ?
C10 N2 Ni1 O3 26.9(4) . . . . ?
C3 N2 Ni1 O3 -99.2(4) . . . . ?
C2 N2 Ni1 O1 61.6(4) . . . . ?
C10 N2 Ni1 O1 -54.0(4) . . . . ?
C3 N2 Ni1 O1 179.9(4) . . . . ?
C21 N4 Ni2 N6 -26.6(3) . . . . ?
C22 N4 Ni2 N6 -144.4(4) . . . . ?
C16 N4 Ni2 N6 89.8(4) . . . . ?
C21 N4 Ni2 N5 -112.1(3) . . . . ?
C22 N4 Ni2 N5 130.1(4) . . . . ?
C16 N4 Ni2 N5 4.3(4) . . . . ?
C21 N4 Ni2 O7 163.2(3) . . . . ?
C22 N4 Ni2 O7 45.5(4) . . . . ?
C16 N4 Ni2 O7 -80.4(4) . . . . ?
C21 N4 Ni2 O11 65.0(3) . . . . ?
C22 N4 Ni2 O11 -52.8(4) . . . . ?
C16 N4 Ni2 O11 -178.6(3) . . . . ?
C20 N6 Ni2 N4 5.4(4) . . . . ?
C19 N6 Ni2 N4 -115.3(4) . . . . ?
C28 N6 Ni2 N4 128.4(4) . . . . ?
C20 N6 Ni2 O9 -177.7(4) . . . . ?
C19 N6 Ni2 O9 61.6(4) . . . . ?
C28 N6 Ni2 O9 -54.6(4) . . . . ?
C20 N6 Ni2 N5 91.4(4) . . . . ?
C19 N6 Ni2 N5 -29.3(4) . . . . ?
C28 N6 Ni2 N5 -145.5(4) . . . . ?
C20 N6 Ni2 O7 70.7(11) . . . . ?
C19 N6 Ni2 O7 -50.0(11) . . . . ?
C28 N6 Ni2 O7 -166.3(8) . . . . ?
C20 N6 Ni2 O11 -100.3(4) . . . . ?
C19 N6 Ni2 O11 139.0(4) . . . . ?
C28 N6 Ni2 O11 22.7(4) . . . . ?
C17 N5 Ni2 N4 -27.2(3) . . . . ?
C18 N5 Ni2 N4 91.9(4) . . . . ?
C25 N5 Ni2 N4 -145.7(4) . . . . ?
C17 N5 Ni2 N6 -112.8(3) . . . . ?
C18 N5 Ni2 N6 6.4(4) . . . . ?
C25 N5 Ni2 N6 128.8(4) . . . . ?
C17 N5 Ni2 O9 150.0(3) . . . . ?
C18 N5 Ni2 O9 -90.8(3) . . . . ?
C25 N5 Ni2 O9 31.5(4) . . . . ?
C17 N5 Ni2 O7 63.4(3) . . . . ?
C18 N5 Ni2 O7 -177.5(4) . . . . ?
C25 N5 Ni2 O7 -55.1(4) . . . . ?
C17 N5 Ni2 O11 166.4(7) . . . . ?
C18 N5 Ni2 O11 -74.5(9) . . . . ?
C25 N5 Ni2 O11 47.9(9) . . . . ?
C31 N7 Ni3 O13 -93.9(4) . . . . ?
C37 N7 Ni3 O13 33.7(4) . . . . ?
C36 N7 Ni3 O13 149.2(3) . . . . ?
C31 N7 Ni3 O17 179.0(4) . . . . ?
C37 N7 Ni3 O17 -53.4(4) . . . . ?
C36 N7 Ni3 O17 62.1(3) . . . . ?
C31 N7 Ni3 N9 88.3(4) . . . . ?
C37 N7 Ni3 N9 -144.2(4) . . . . ?
C36 N7 Ni3 N9 -28.6(3) . . . . ?
C31 N7 Ni3 N8 2.7(4) . . . . ?
C37 N7 Ni3 N8 130.3(4) . . . . ?
C36 N7 Ni3 N8 -114.2(3) . . . . ?
C34 N9 Ni3 O17 149.1(3) . . . . ?
C43 N9 Ni3 O17 30.8(4) . . . . ?
C35 N9 Ni3 O17 -90.1(3) . . . . ?
C34 N9 Ni3 N7 -114.4(4) . . . . ?
C43 N9 Ni3 N7 127.3(4) . . . . ?
C35 N9 Ni3 N7 6.4(3) . . . . ?
C34 N9 Ni3 O15 62.5(4) . . . . ?
C43 N9 Ni3 O15 -55.8(4) . . . . ?
C35 N9 Ni3 O15 -176.7(3) . . . . ?
C34 N9 Ni3 N8 -28.6(4) . . . . ?
C43 N9 Ni3 N8 -146.9(4) . . . . ?
C35 N9 Ni3 N8 92.2(3) . . . . ?
C32 N8 Ni3 O13 64.8(3) . . . . ?
C40 N8 Ni3 O13 -51.2(4) . . . . ?
C33 N8 Ni3 O13 -178.2(3) . . . . ?
C32 N8 Ni3 N7 -26.4(3) . . . . ?
C40 N8 Ni3 N7 -142.4(4) . . . . ?
C33 N8 Ni3 N7 90.7(4) . . . . ?
C32 N8 Ni3 N9 -112.5(3) . . . . ?
C40 N8 Ni3 N9 131.5(4) . . . . ?
C33 N8 Ni3 N9 4.6(4) . . . . ?
C32 N8 Ni3 O15 147.3(3) . . . . ?
C40 N8 Ni3 O15 31.4(4) . . . . ?
C33 N8 Ni3 O15 -95.6(3) . . . . ?
C55 N11 Ni4 O21 32.0(4) . . . . ?
C48 N11 Ni4 O21 -91.6(3) . . . . ?
C47 N11 Ni4 O21 150.8(3) . . . . ?
C55 N11 Ni4 O19 -54.4(3) . . . . ?
C48 N11 Ni4 O19 -178.1(3) . . . . ?
C47 N11 Ni4 O19 64.4(3) . . . . ?
C55 N11 Ni4 N10 -146.2(4) . . . . ?
C48 N11 Ni4 N10 90.2(3) . . . . ?
C47 N11 Ni4 N10 -27.4(3) . . . . ?
C55 N11 Ni4 N12 128.4(4) . . . . ?
C48 N11 Ni4 N12 4.7(3) . . . . ?
C47 N11 Ni4 N12 -112.8(4) . . . . ?
C55 N11 Ni4 O23 -168.5(8) . . . . ?
C48 N11 Ni4 O23 67.9(10) . . . . ?
C47 N11 Ni4 O23 -49.6(11) . . . . ?
C46 N10 Ni4 N11 24.9(3) . . . . ?
C51 N10 Ni4 N11 -111.7(3) . . . . ?
C52 N10 Ni4 N11 135.0(4) . . . . ?
C46 N10 Ni4 O19 -69.3(3) . . . . ?
C51 N10 Ni4 O19 154.1(3) . . . . ?
C52 N10 Ni4 O19 40.8(4) . . . . ?
C46 N10 Ni4 N12 110.1(4) . . . . ?
C51 N10 Ni4 N12 -26.5(3) . . . . ?
C52 N10 Ni4 N12 -139.8(4) . . . . ?
C46 N10 Ni4 O23 -159.2(3) . . . . ?
C51 N10 Ni4 O23 64.2(3) . . . . ?
C52 N10 Ni4 O23 -49.1(4) . . . . ?
C49 N12 Ni4 O21 59.4(4) . . . . ?
C58 N12 Ni4 O21 -54.2(4) . . . . ?
C50 N12 Ni4 O21 -177.6(4) . . . . ?
C49 N12 Ni4 N11 -31.8(4) . . . . ?
C58 N12 Ni4 N11 -145.4(4) . . . . ?
C50 N12 Ni4 N11 91.3(4) . . . . ?
C58 N12 Ni4 N10 128.5(4) . . . . ?
C50 N12 Ni4 N10 5.1(4) . . . . ?
C49 N12 Ni4 O23 157.9(4) . . . . ?
C58 N12 Ni4 O23 44.3(4) . . . . ?
C50 N12 Ni4 O23 -79.0(4) . . . . ?
O2 C9 O1 Ni1 145.3(4) . . . . ?
C8 C9 O1 Ni1 -35.4(7) . . . . ?
N1 Ni1 O1 C9 22.9(5) . . . . ?
N2 Ni1 O3 C12 19.1(5) . . . . ?
O1 Ni1 O3 C12 123.2(5) . . . . ?
O5 Ni1 O3 C12 -158.0(5) . . . . ?
O6 C15 O5 Ni1 -151.7(4) . . . . ?
C14 C15 O5 Ni1 29.9(8) . . . . ?
N1 Ni1 O5 C15 -116.2(5) . . . . ?
N3 Ni1 O5 C15 -29.8(5) . . . . ?
O1 Ni1 O5 C15 152.1(5) . . . . ?
O8 C24 O7 Ni2 -150.3(5) . . . . ?
C23 C24 O7 Ni2 34.5(7) . . . . ?
N4 Ni2 O7 C24 -32.7(5) . . . . ?
N6 Ni2 O7 C24 -97.5(10) . . . . ?
O9 Ni2 O7 C24 149.9(5) . . . . ?
N5 Ni2 O7 C24 -118.3(5) . . . . ?
O11 Ni2 O7 C24 73.4(5) . . . . ?
O10 C27 O9 Ni2 169.4(4) . . . . ?
C26 C27 O9 Ni2 -10.3(8) . . . . ?
N6 Ni2 O9 C27 -81.9(5) . . . . ?
N5 Ni2 O9 C27 3.4(5) . . . . ?
O7 Ni2 O9 C27 88.0(5) . . . . ?
O11 Ni2 O9 C27 -173.2(5) . . . . ?
O12 C30 O11 Ni2 105.9(6) . . . . ?
C29 C30 O11 Ni2 -68.1(6) . . . . ?
N4 Ni2 O11 C30 -49.7(4) . . . . ?
N6 Ni2 O11 C30 36.1(4) . . . . ?
O9 Ni2 O11 C30 132.9(4) . . . . ?
N5 Ni2 O11 C30 116.2(8) . . . . ?
O7 Ni2 O11 C30 -142.2(4) . . . . ?
O14 C39 O13 Ni3 169.0(4) . . . . ?
C38 C39 O13 Ni3 -10.9(8) . . . . ?
O17 Ni3 O13 C39 100.3(5) . . . . ?
N7 Ni3 O13 C39 3.8(5) . . . . ?
O15 Ni3 O13 C39 -172.9(5) . . . . ?
N8 Ni3 O13 C39 -81.8(5) . . . . ?
O16 C42 O15 Ni3 133.7(5) . . . . ?
C41 C42 O15 Ni3 -42.6(7) . . . . ?
O13 Ni3 O15 C42 120.0(5) . . . . ?
O17 Ni3 O15 C42 -152.6(5) . . . . ?
N9 Ni3 O15 C42 -62.0(5) . . . . ?
N8 Ni3 O15 C42 23.5(5) . . . . ?
O18 C45 O17 Ni3 169.9(5) . . . . ?
C44 C45 O17 Ni3 -10.5(9) . . . . ?
O13 Ni3 O17 C45 -173.9(6) . . . . ?
N7 Ni3 O17 C45 -82.6(6) . . . . ?
N9 Ni3 O17 C45 3.3(6) . . . . ?
O15 Ni3 O17 C45 103.5(6) . . . . ?
O20 C54 O19 Ni4 -126.3(5) . . . . ?
C53 C54 O19 Ni4 46.6(7) . . . . ?
O21 Ni4 O19 C54 138.2(5) . . . . ?
N11 Ni4 O19 C54 -130.4(4) . . . . ?
N10 Ni4 O19 C54 -44.5(5) . . . . ?
O23 Ni4 O19 C54 39.7(5) . . . . ?
O22 C57 O21 Ni4 167.7(4) . . . . ?
C56 C57 O21 Ni4 -11.1(9) . . . . ?
N11 Ni4 O21 C57 2.7(6) . . . . ?
O19 Ni4 O21 C57 97.0(6) . . . . ?
N12 Ni4 O21 C57 -82.3(6) . . . . ?
O23 Ni4 O21 C57 -173.5(6) . . . . ?
O24 C60 O23 Ni4 -148.0(5) . . . . ?
C59 C60 O23 Ni4 36.8(8) . . . . ?
O21 Ni4 O23 C60 62.3(5) . . . . ?
N11 Ni4 O23 C60 -97.0(10) . . . . ?
O19 Ni4 O23 C60 148.6(5) . . . . ?
N10 Ni4 O23 C60 -119.4(5) . . . . ?
N12 Ni4 O23 C60 -34.3(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.109
####################################################################### 
# 
# 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_3_NiLa
_database_code_depnum_ccdc_archive 'CCDC 2165410'
loop_
_audit_author_name
_audit_author_address
'Zhong Zhang'
;Guangxi Normal University
China
;
_audit_update_record             
;
2022-04-08 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H72 N6 Ni5 O24, La N6 O18, Cl, 2(H2 O)'
_chemical_formula_sum            'C30 H76 Cl La N12 Ni5 O44'
_chemical_formula_weight         1776.94

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'
La La -0.2871 2.4523 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

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

_cell_length_a                   11.9438(19)
_cell_length_b                   11.9438(19)
_cell_length_c                   26.820(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3313.4(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    5933
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      25.45

_exptl_crystal_description       plate
_exptl_crystal_colour            light-purple
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1812
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(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 Smart Apex CCD II'
_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            26532
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         26.07
_reflns_number_total             2251
_reflns_number_gt                1692
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0824P)²+0.0000P] 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         2251
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1327
_refine_ls_wR_factor_gt          0.1316
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
C1 C 0.3344(5) 0.4926(5) 0.05331(18) 0.0393(12) Uani 1 1 d . . .
H1A H 0.3072 0.4242 0.0779 0.047 Uiso 1 1 calc R . .
H1B H 0.3705 0.4705 0.0251 0.047 Uiso 1 1 calc R . .
C2 C 0.4987(5) 0.7173(5) 0.0363(2) 0.0441(13) Uani 1 1 d . . .
H2A H 0.4491 0.6884 0.0057 0.053 Uiso 1 1 calc R . .
H2B H 0.5848 0.7318 0.0296 0.053 Uiso 1 1 calc R . .
C3 C 0.5310(4) 0.5939(5) 0.1026(2) 0.0391(12) Uani 1 1 d . . .
H3A H 0.5697 0.5608 0.0794 0.047 Uiso 1 1 calc R . .
H3B H 0.4858 0.5281 0.1278 0.047 Uiso 1 1 calc R . .
C4 C 0.6379(4) 0.7134(5) 0.1277(2) 0.0373(12) Uani 1 1 d . . .
H4A H 0.6979 0.6901 0.1421 0.045 Uiso 1 1 calc R . .
H4B H 0.6844 0.7767 0.1018 0.045 Uiso 1 1 calc R . .
C5 C 0.6034(4) 0.7791(4) 0.16749(17) 0.0295(10) Uani 1 1 d . . .
La1 La 1.0000 0.0000 0.0000 0.0283(2) Uani 1 6 d S . .
Cl1 Cl 0.66667 0.33333 0.1943(2) 0.0558(12) Uani 0.50 3 d SP . .
N1 N 0.4357(4) 0.6162(4) 0.07537(14) 0.0319(9) Uani 1 1 d . . .
N2 N 0.8554(4) 0.0995(4) 0.06358(17) 0.0409(10) Uani 1 1 d . . .
Ni1 Ni 0.33333 0.66667 0.12299(4) 0.0254(3) Uani 1 3 d S . .
Ni2 Ni 0.69270(10) 0.98073(10) 0.2500 0.0474(3) Uani 1 2 d S . .
O1 O 0.4892(3) 0.7590(3) 0.17014(12) 0.0345(8) Uani 1 1 d . . .
O2 O 0.6925(3) 0.8549(3) 0.19527(13) 0.0453(9) Uani 1 1 d . . .
O3 O 0.4890(5) 0.8919(5) 0.2500 0.0450(12) Uani 1 2 d S . .
H3D H 0.4602 0.8575 0.2783 0.068 Uiso 0.50 1 d PR . .
H3C H 0.4665 0.8305 0.2292 0.068 Uiso 0.50 1 d PR . .
O4 O 0.8870(5) 1.0752(5) 0.2500 0.0530(14) Uani 1 2 d S . .
H4C H 0.8958 1.1226 0.2250 0.079 Uiso 1 1 d R . .
O5 O 0.6897(4) 1.0917(4) 0.19105(15) 0.0632(11) Uani 1 1 d . . .
H5C H 0.6700 1.0808 0.1603 0.095 Uiso 1 1 d R . .
H5D H 0.6737 1.1488 0.2022 0.095 Uiso 1 1 d R . .
O6 O 0.8570(3) -0.0033(3) 0.07580(14) 0.0453(9) Uani 1 1 d . . .
O7 O 0.9210(3) 0.1617(3) 0.02675(14) 0.0438(9) Uani 1 1 d . . .
O8 O 0.7871(4) 0.1317(4) 0.08702(18) 0.0687(13) Uani 1 1 d . . .
O9 O 0.0000 1.0000 0.1717(3) 0.065(2) Uani 1 3 d S . .
H9C H 0.0281 0.9540 0.1849 0.098 Uiso 0.66667 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.485(6) . ?
C1 C2 1.508(7) 3_565 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.488(6) . ?
C2 C1 1.508(7) 2_665 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.485(6) . ?
C3 C4 1.515(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.499(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O2 1.243(5) . ?
C5 O1 1.263(5) . ?
La1 O7 2.637(3) 3_765 ?
La1 O7 2.637(3) 9_545 ?
La1 O7 2.637(3) 2_645 ?
La1 O7 2.637(3) 7_755 ?
La1 O7 2.637(3) 8_665 ?
La1 O7 2.637(3) . ?
La1 O6 2.643(4) 3_765 ?
La1 O6 2.643(4) 9_545 ?
La1 O6 2.643(4) 2_645 ?
La1 O6 2.643(4) . ?
La1 O6 2.643(4) 8_665 ?
La1 O6 2.643(4) 7_755 ?
N1 Ni1 2.056(4) . ?
N2 O8 1.233(5) . ?
N2 O7 1.249(5) . ?
N2 O6 1.280(5) . ?
Ni1 N1 2.056(4) 3_565 ?
Ni1 N1 2.056(4) 2_665 ?
Ni1 O1 2.056(3) 2_665 ?
Ni1 O1 2.056(3) . ?
Ni1 O1 2.056(3) 3_565 ?
Ni2 O4 2.010(5) . ?
Ni2 O5 2.075(4) 10_556 ?
Ni2 O5 2.075(4) . ?
Ni2 O2 2.100(3) . ?
Ni2 O2 2.100(3) 10_556 ?
Ni2 O3 2.112(5) . ?
O3 H3D 0.8505 . ?
O3 H3C 0.8504 . ?
O4 H4C 0.8499 . ?
O5 H5C 0.8504 . ?
O5 H5D 0.8497 . ?
O9 H9C 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.8(4) . 3_565 ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 3_565 . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 3_565 . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C1 110.2(4) . 2_665 ?
N1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 2_665 . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 2_665 . ?
H2A C2 H2B 108.1 . . ?
N1 C3 C4 114.2(4) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4A 107.5 . . ?
C3 C4 H4A 107.5 . . ?
C5 C4 H4B 107.5 . . ?
C3 C4 H4B 107.5 . . ?
H4A C4 H4B 107.0 . . ?
O2 C5 O1 123.7(4) . . ?
O2 C5 C4 116.7(4) . . ?
O1 C5 C4 119.6(4) . . ?
O7 La1 O7 180.00(17) 3_765 9_545 ?
O7 La1 O7 112.89(7) 3_765 2_645 ?
O7 La1 O7 67.11(7) 9_545 2_645 ?
O7 La1 O7 67.11(7) 3_765 7_755 ?
O7 La1 O7 112.89(7) 9_545 7_755 ?
O7 La1 O7 67.11(7) 2_645 7_755 ?
O7 La1 O7 67.11(7) 3_765 8_665 ?
O7 La1 O7 112.89(7) 9_545 8_665 ?
O7 La1 O7 180.00(19) 2_645 8_665 ?
O7 La1 O7 112.89(7) 7_755 8_665 ?
O7 La1 O7 112.89(7) 3_765 . ?
O7 La1 O7 67.11(7) 9_545 . ?
O7 La1 O7 112.89(7) 2_645 . ?
O7 La1 O7 180.00(19) 7_755 . ?
O7 La1 O7 67.11(7) 8_665 . ?
O7 La1 O6 48.42(10) 3_765 3_765 ?
O7 La1 O6 131.58(10) 9_545 3_765 ?
O7 La1 O6 112.14(11) 2_645 3_765 ?
O7 La1 O6 109.93(11) 7_755 3_765 ?
O7 La1 O6 67.86(11) 8_665 3_765 ?
O7 La1 O6 70.07(11) . 3_765 ?
O7 La1 O6 131.58(10) 3_765 9_545 ?
O7 La1 O6 48.42(10) 9_545 9_545 ?
O7 La1 O6 67.86(11) 2_645 9_545 ?
O7 La1 O6 70.07(11) 7_755 9_545 ?
O7 La1 O6 112.14(11) 8_665 9_545 ?
O7 La1 O6 109.93(11) . 9_545 ?
O6 La1 O6 180.00(10) 3_765 9_545 ?
O7 La1 O6 70.07(11) 3_765 2_645 ?
O7 La1 O6 109.93(11) 9_545 2_645 ?
O7 La1 O6 48.42(10) 2_645 2_645 ?
O7 La1 O6 67.86(11) 7_755 2_645 ?
O7 La1 O6 131.58(10) 8_665 2_645 ?
O7 La1 O6 112.14(11) . 2_645 ?
O6 La1 O6 67.21(13) 3_765 2_645 ?
O6 La1 O6 112.79(13) 9_545 2_645 ?
O7 La1 O6 112.14(11) 3_765 . ?
O7 La1 O6 67.86(11) 9_545 . ?
O7 La1 O6 70.07(11) 2_645 . ?
O7 La1 O6 131.58(10) 7_755 . ?
O7 La1 O6 109.93(11) 8_665 . ?
O7 La1 O6 48.42(10) . . ?
O6 La1 O6 67.21(13) 3_765 . ?
O6 La1 O6 112.79(13) 9_545 . ?
O6 La1 O6 67.21(13) 2_645 . ?
O7 La1 O6 109.93(11) 3_765 8_665 ?
O7 La1 O6 70.07(11) 9_545 8_665 ?
O7 La1 O6 131.58(10) 2_645 8_665 ?
O7 La1 O6 112.14(11) 7_755 8_665 ?
O7 La1 O6 48.42(10) 8_665 8_665 ?
O7 La1 O6 67.86(11) . 8_665 ?
O6 La1 O6 112.79(13) 3_765 8_665 ?
O6 La1 O6 67.21(13) 9_545 8_665 ?
O6 La1 O6 180.00(18) 2_645 8_665 ?
O6 La1 O6 112.79(13) . 8_665 ?
O7 La1 O6 67.86(11) 3_765 7_755 ?
O7 La1 O6 112.14(11) 9_545 7_755 ?
O7 La1 O6 109.93(11) 2_645 7_755 ?
O7 La1 O6 48.42(10) 7_755 7_755 ?
O7 La1 O6 70.07(11) 8_665 7_755 ?
O7 La1 O6 131.58(10) . 7_755 ?
O6 La1 O6 112.79(13) 3_765 7_755 ?
O6 La1 O6 67.21(13) 9_545 7_755 ?
O6 La1 O6 112.79(13) 2_645 7_755 ?
O6 La1 O6 180.00(16) . 7_755 ?
O6 La1 O6 67.21(13) 8_665 7_755 ?
C1 N1 C3 109.5(4) . . ?
C1 N1 C2 110.9(4) . . ?
C3 N1 C2 111.7(4) . . ?
C1 N1 Ni1 103.4(3) . . ?
C3 N1 Ni1 111.6(3) . . ?
C2 N1 Ni1 109.4(3) . . ?
O8 N2 O7 122.3(4) . . ?
O8 N2 O6 119.8(4) . . ?
O7 N2 O6 117.8(4) . . ?
O8 N2 La1 174.2(4) . . ?
O7 N2 La1 58.8(2) . . ?
O6 N2 La1 59.2(2) . . ?
N1 Ni1 N1 85.47(16) 3_565 2_665 ?
N1 Ni1 N1 85.47(16) 3_565 . ?
N1 Ni1 N1 85.47(16) 2_665 . ?
N1 Ni1 O1 96.93(14) 3_565 2_665 ?
N1 Ni1 O1 91.60(14) 2_665 2_665 ?
N1 Ni1 O1 176.07(13) . 2_665 ?
N1 Ni1 O1 176.07(13) 3_565 . ?
N1 Ni1 O1 96.93(14) 2_665 . ?
N1 Ni1 O1 91.60(14) . . ?
O1 Ni1 O1 86.14(13) 2_665 . ?
N1 Ni1 O1 91.60(14) 3_565 3_565 ?
N1 Ni1 O1 176.07(13) 2_665 3_565 ?
N1 Ni1 O1 96.93(13) . 3_565 ?
O1 Ni1 O1 86.14(13) 2_665 3_565 ?
O1 Ni1 O1 86.14(13) . 3_565 ?
O4 Ni2 O5 91.45(16) . 10_556 ?
O4 Ni2 O5 91.45(16) . . ?
O5 Ni2 O5 99.3(2) 10_556 . ?
O4 Ni2 O2 89.40(15) . . ?
O5 Ni2 O2 174.62(15) 10_556 . ?
O5 Ni2 O2 86.01(15) . . ?
O4 Ni2 O2 89.40(15) . 10_556 ?
O5 Ni2 O2 86.01(15) 10_556 10_556 ?
O5 Ni2 O2 174.62(15) . 10_556 ?
O2 Ni2 O2 88.7(2) . 10_556 ?
O4 Ni2 O3 176.7(2) . . ?
O5 Ni2 O3 86.43(15) 10_556 . ?
O5 Ni2 O3 86.43(15) . . ?
O2 Ni2 O3 92.95(14) . . ?
O2 Ni2 O3 92.95(14) 10_556 . ?
C5 O1 Ni1 132.0(3) . . ?
C5 O2 Ni2 129.4(3) . . ?
Ni2 O3 H3D 109.2 . . ?
Ni2 O3 H3C 102.8 . . ?
H3D O3 H3C 106.9 . . ?
Ni2 O4 H4C 95.6 . . ?
Ni2 O5 H5C 137.2 . . ?
Ni2 O5 H5D 109.1 . . ?
H5C O5 H5D 107.9 . . ?
N2 O6 La1 96.2(3) . . ?
N2 O7 La1 97.4(3) . . ?

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
N1 C3 C4 C5 61.7(6) . . . . ?
C3 C4 C5 O2 162.6(4) . . . . ?
C3 C4 C5 O1 -19.8(7) . . . . ?
C2 C1 N1 C3 165.9(4) 3_565 . . . ?
C2 C1 N1 C2 -70.4(5) 3_565 . . . ?
C2 C1 N1 Ni1 46.8(4) 3_565 . . . ?
C4 C3 N1 C1 -178.9(4) . . . . ?
C4 C3 N1 C2 57.9(5) . . . . ?
C4 C3 N1 Ni1 -65.0(5) . . . . ?
C1 C2 N1 C1 132.9(4) 2_665 . . . ?
C1 C2 N1 C3 -104.6(5) 2_665 . . . ?
C1 C2 N1 Ni1 19.6(5) 2_665 . . . ?
O7 La1 N2 O7 88.5(2) 3_765 . . . ?
O7 La1 N2 O7 -91.5(2) 9_545 . . . ?
O7 La1 N2 O7 -155.1(3) 2_645 . . . ?
O7 La1 N2 O7 180.0 7_755 . . . ?
O7 La1 N2 O7 24.9(3) 8_665 . . . ?
O6 La1 N2 O7 91.4(3) 3_765 . . . ?
O6 La1 N2 O7 -88.6(3) 9_545 . . . ?
O6 La1 N2 O7 156.5(3) 2_645 . . . ?
O6 La1 N2 O7 175.6(4) . . . . ?
O6 La1 N2 O7 -23.5(3) 8_665 . . . ?
O6 La1 N2 O7 -4.4(4) 7_755 . . . ?
O7 La1 N2 O6 -87.1(3) 3_765 . . . ?
O7 La1 N2 O6 92.9(3) 9_545 . . . ?
O7 La1 N2 O6 29.3(3) 2_645 . . . ?
O7 La1 N2 O6 4.4(4) 7_755 . . . ?
O7 La1 N2 O6 -150.7(3) 8_665 . . . ?
O7 La1 N2 O6 -175.6(4) . . . . ?
O6 La1 N2 O6 -84.2(3) 3_765 . . . ?
O6 La1 N2 O6 95.8(3) 9_545 . . . ?
O6 La1 N2 O6 -19.1(3) 2_645 . . . ?
O6 La1 N2 O6 160.9(3) 8_665 . . . ?
O6 La1 N2 O6 180.0 7_755 . . . ?
C1 N1 Ni1 N1 -27.6(3) . . . 3_565 ?
C3 N1 Ni1 N1 -145.2(3) . . . 3_565 ?
C2 N1 Ni1 N1 90.6(3) . . . 3_565 ?
C1 N1 Ni1 N1 -113.4(2) . . . 2_665 ?
C3 N1 Ni1 N1 129.0(3) . . . 2_665 ?
C2 N1 Ni1 N1 4.8(3) . . . 2_665 ?
C1 N1 Ni1 O1 149.8(3) . . . . ?
C3 N1 Ni1 O1 32.2(3) . . . . ?
C2 N1 Ni1 O1 -92.0(3) . . . . ?
C1 N1 Ni1 O1 63.5(3) . . . 3_565 ?
C3 N1 Ni1 O1 -54.1(3) . . . 3_565 ?
C2 N1 Ni1 O1 -178.3(3) . . . 3_565 ?
O2 C5 O1 Ni1 167.8(3) . . . . ?
C4 C5 O1 Ni1 -9.6(6) . . . . ?
N1 Ni1 O1 C5 -82.7(4) 2_665 . . . ?
N1 Ni1 O1 C5 2.9(4) . . . . ?
O1 Ni1 O1 C5 -173.9(4) 2_665 . . . ?
O1 Ni1 O1 C5 99.8(5) 3_565 . . . ?
O1 C5 O2 Ni2 -4.7(7) . . . . ?
C4 C5 O2 Ni2 172.7(3) . . . . ?
O4 Ni2 O2 C5 -164.2(4) . . . . ?
O5 Ni2 O2 C5 -72.7(4) . . . . ?
O2 Ni2 O2 C5 106.4(4) 10_556 . . . ?
O3 Ni2 O2 C5 13.5(4) . . . . ?
O8 N2 O6 La1 173.4(4) . . . . ?
O7 N2 O6 La1 -4.3(4) . . . . ?
O7 La1 O6 N2 103.9(3) 3_765 . . . ?
O7 La1 O6 N2 -76.1(3) 9_545 . . . ?
O7 La1 O6 N2 -148.6(3) 2_645 . . . ?
O7 La1 O6 N2 -177.6(2) 7_755 . . . ?
O7 La1 O6 N2 31.4(3) 8_665 . . . ?
O7 La1 O6 N2 2.4(2) . . . . ?
O6 La1 O6 N2 85.4(3) 3_765 . . . ?
O6 La1 O6 N2 -94.6(3) 9_545 . . . ?
O6 La1 O6 N2 159.2(3) 2_645 . . . ?
O6 La1 O6 N2 -20.8(3) 8_665 . . . ?
O8 N2 O7 La1 -173.3(4) . . . . ?
O6 N2 O7 La1 4.3(4) . . . . ?
O7 La1 O7 N2 -102.4(2) 3_765 . . . ?
O7 La1 O7 N2 77.6(2) 9_545 . . . ?
O7 La1 O7 N2 27.2(3) 2_645 . . . ?
O7 La1 O7 N2 -152.8(3) 8_665 . . . ?
O6 La1 O7 N2 -79.2(3) 3_765 . . . ?
O6 La1 O7 N2 100.8(3) 9_545 . . . ?
O6 La1 O7 N2 -25.5(3) 2_645 . . . ?
O6 La1 O7 N2 -2.4(2) . . . . ?
O6 La1 O7 N2 154.5(3) 8_665 . . . ?
O6 La1 O7 N2 177.6(2) 7_755 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.07
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.150
####################################################################### 
# 
# 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_6_CoTb
_database_code_depnum_ccdc_archive 'CCDC 2165414'
loop_
_audit_author_name
_audit_author_address
'Zhong Zhang'
;Guangxi Normal University
China
;
_audit_update_record             
;
2022-04-08 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'6(C5 H8 Co0.33 N O2.50 Tb0.17), Cl O4, 2(Cl), 5(H2 O)'
_chemical_formula_sum            'C30 H58 Cl3 Co2 N6 O24 Tb'
_chemical_formula_weight         1269.95

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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'

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

_cell_length_a                   9.0019(13)
_cell_length_b                   9.0019(13)
_cell_length_c                   30.036(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2107.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6794
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      26.08

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1284
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 Smart Apex CCD II'
_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            23690
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         26.00
_reflns_number_total             852
_reflns_number_gt                796
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0900P)²+60.0000P] 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         852
_refine_ls_number_parameters     82
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.2069
_refine_ls_wR_factor_gt          0.2054
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.084
_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
C1 C 0.107(2) 0.6310(19) 0.0620(4) 0.074(4) Uani 1 1 d U . .
H1A H -0.0059 0.6080 0.0712 0.089 Uiso 1 1 calc R . .
H1B H 0.1242 0.6731 0.0317 0.089 Uiso 1 1 calc R . .
C2 C 0.088(2) 0.781(2) 0.1160(6) 0.033(4) Uani 0.50 1 d P . .
H2A H 0.1434 0.8681 0.1388 0.040 Uiso 0.25 1 calc PR . .
H2B H 0.0360 0.8245 0.0952 0.040 Uiso 0.25 1 calc PR . .
C3 C -0.058(3) 0.624(3) 0.1384(6) 0.040(5) Uani 0.50 1 d P . .
H3A H -0.1359 0.5516 0.1152 0.048 Uiso 0.50 1 calc PR . .
H3B H -0.1206 0.6619 0.1569 0.048 Uiso 0.50 1 calc PR . .
C4 C 0.5032(10) 0.4968(10) 0.1708(5) 0.060(5) Uani 1 2 d S . .
Cl1 Cl 1.0000 0.0000 0.0000 0.40(3) Uani 1 12 d SDU . .
Cl2 Cl 0.66667 0.33333 0.0522(2) 0.0385(14) Uani 1 6 d S . .
Co1 Co 0.33333 0.66667 0.12879(9) 0.0230(7) Uani 1 6 d S . .
N1 N 0.2333(8) 0.7667(8) 0.0900(3) 0.044(3) Uani 1 2 d S . .
O1 O 0.4286(7) 0.5714(7) 0.1677(3) 0.061(4) Uani 1 2 d S . .
O2 O 0.5547(7) 0.4453(7) 0.1991(3) 0.048(3) Uani 1 2 d S . .
O3 O 0.8286(16) 0.1714(16) 0.2500 0.104(9) Uani 1 4 d S . .
H3C H 0.7763 0.0620 0.2313 0.155 Uiso 0.25 1 d PR . .
H3D H 0.8320 0.1177 0.2795 0.155 Uiso 0.25 1 d PR . .
O4 O 1.0000 0.0000 0.0480(4) 0.40(3) Uani 0.50 6 d SPDU . .
O5 O 0.911(3) 0.089(3) 0.012(6) 0.40(3) Uani 0.50 2 d SPDU . .
O6 O 0.1957(14) 0.391(3) 0.2500 0.069(5) Uani 1 4 d S . .
H6C H 0.1909 0.3347 0.2265 0.103 Uiso 0.25 1 d PR . .
H6D H 0.2165 0.4875 0.2408 0.103 Uiso 0.25 1 d PR . .
O7 O 1.0000 1.0000 0.196(4) 0.47(8) Uani 1 6 d S . .
H7C H 0.9570 0.9141 0.1772 0.709 Uiso 0.33333 2 d SPR . .
H7D H 0.9225 1.0266 0.1990 0.709 Uiso 0.16667 1 d PR . .
Tb1 Tb 0.66667 0.33333 0.2500 0.0238(5) Uani 1 12 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C1 1.40(3) 24_565 ?
C1 N1 1.451(14) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.52(3) . ?
C2 N1 1.59(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.73(2) 5_565 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O1 1.17(2) . ?
C4 O2 1.169(18) . ?
C4 C3 1.73(2) 3_665 ?
C4 C3 1.73(2) 20 ?
Cl1 O4 1.441(11) 13_755 ?
Cl1 O4 1.441(11) . ?
Cl1 O5 1.441(11) 17_545 ?
Cl1 O5 1.441(11) 5_765 ?
Cl1 O5 1.441(11) 15_665 ?
Cl1 O5 1.441(11) 3_645 ?
Cl1 O5 1.441(11) . ?
Cl1 O5 1.441(11) 13_755 ?
Co1 O1 1.889(10) 3_665 ?
Co1 O1 1.889(10) 5_565 ?
Co1 O1 1.889(10) . ?
Co1 N1 1.946(11) . ?
Co1 N1 1.946(11) 3_665 ?
Co1 N1 1.946(11) 5_565 ?
N1 C1 1.451(15) 22_665 ?
N1 C2 1.59(2) 22_665 ?
O2 Tb1 2.320(9) . ?
O3 Tb1 2.52(2) . ?
O3 H3C 1.0213 . ?
O3 H3D 1.0181 . ?
O4 O5 1.75(15) 3_645 ?
O4 O5 1.75(15) . ?
O4 O5 1.75(15) 5_765 ?
O5 O5 1.58(13) 17_545 ?
O5 O5 1.58(13) 15_665 ?
O6 H6C 0.8589 . ?
O6 H6D 0.8352 . ?
O7 H7C 0.8672 . ?
O7 H7D 0.8500 . ?
Tb1 O2 2.320(10) 3_655 ?
Tb1 O2 2.320(10) 14_666 ?
Tb1 O2 2.320(10) 18_656 ?
Tb1 O2 2.320(10) 5_665 ?
Tb1 O2 2.320(9) 16_556 ?
Tb1 O3 2.52(2) 3_655 ?
Tb1 O3 2.52(2) 14_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
C1 C1 N1 116.8(7) 24_565 . ?
C1 C1 H1A 108.1 24_565 . ?
N1 C1 H1A 108.1 . . ?
C1 C1 H1B 108.1 24_565 . ?
N1 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C3 C2 N1 120.1(14) . . ?
C3 C2 H2A 107.3 . . ?
N1 C2 H2A 107.3 . . ?
C3 C2 H2B 107.3 . . ?
N1 C2 H2B 107.3 . . ?
H2A C2 H2B 106.9 . . ?
C2 C3 C4 118.2(15) . 5_565 ?
C2 C3 H3A 107.8 . . ?
C4 C3 H3A 107.8 5_565 . ?
C2 C3 H3B 107.8 . . ?
C4 C3 H3B 107.8 5_565 . ?
H3A C3 H3B 107.1 . . ?
O1 C4 O2 138.0(15) . . ?
O1 C4 C3 100.7(10) . 3_665 ?
O2 C4 C3 104.5(10) . 3_665 ?
O1 C4 C3 100.7(10) . 20 ?
O2 C4 C3 104.5(10) . 20 ?
C3 C4 C3 105.0(16) 3_665 20 ?
O4 Cl1 O4 180.0 13_755 . ?
O4 Cl1 O5 75(7) 13_755 17_545 ?
O4 Cl1 O5 105(7) . 17_545 ?
O4 Cl1 O5 105(7) 13_755 5_765 ?
O4 Cl1 O5 75(7) . 5_765 ?
O5 Cl1 O5 180(10) 17_545 5_765 ?
O4 Cl1 O5 75(7) 13_755 15_665 ?
O4 Cl1 O5 105(7) . 15_665 ?
O5 Cl1 O5 114(6) 17_545 15_665 ?
O5 Cl1 O5 66(6) 5_765 15_665 ?
O4 Cl1 O5 105(7) 13_755 3_645 ?
O4 Cl1 O5 75(7) . 3_645 ?
O5 Cl1 O5 66(6) 17_545 3_645 ?
O5 Cl1 O5 114(6) 5_765 3_645 ?
O5 Cl1 O5 180(10) 15_665 3_645 ?
O4 Cl1 O5 105(7) 13_755 . ?
O4 Cl1 O5 75(7) . . ?
O5 Cl1 O5 66(6) 17_545 . ?
O5 Cl1 O5 114(6) 5_765 . ?
O5 Cl1 O5 66(6) 15_665 . ?
O5 Cl1 O5 114(6) 3_645 . ?
O4 Cl1 O5 75(7) 13_755 13_755 ?
O4 Cl1 O5 105(7) . 13_755 ?
O5 Cl1 O5 114(6) 17_545 13_755 ?
O5 Cl1 O5 66(6) 5_765 13_755 ?
O5 Cl1 O5 114(6) 15_665 13_755 ?
O5 Cl1 O5 66(6) 3_645 13_755 ?
O5 Cl1 O5 180(10) . 13_755 ?
O1 Co1 O1 85.8(4) 3_665 5_565 ?
O1 Co1 O1 85.8(4) 3_665 . ?
O1 Co1 O1 85.8(4) 5_565 . ?
O1 Co1 N1 93.2(3) 3_665 . ?
O1 Co1 N1 93.2(3) 5_565 . ?
O1 Co1 N1 178.5(5) . . ?
O1 Co1 N1 178.5(5) 3_665 3_665 ?
O1 Co1 N1 93.2(3) 5_565 3_665 ?
O1 Co1 N1 93.2(3) . 3_665 ?
N1 Co1 N1 87.9(5) . 3_665 ?
O1 Co1 N1 93.2(3) 3_665 5_565 ?
O1 Co1 N1 178.5(5) 5_565 5_565 ?
O1 Co1 N1 93.2(3) . 5_565 ?
N1 Co1 N1 87.9(5) . 5_565 ?
N1 Co1 N1 87.9(5) 3_665 5_565 ?
C1 N1 C1 108.8(12) . 22_665 ?
C1 N1 C2 128.9(11) . 22_665 ?
C1 N1 C2 91.2(10) 22_665 22_665 ?
C1 N1 C2 91.2(10) . . ?
C1 N1 C2 128.9(11) 22_665 . ?
C2 N1 C2 43.7(15) 22_665 . ?
C1 N1 Co1 107.8(8) . . ?
C1 N1 Co1 107.8(8) 22_665 . ?
C2 N1 Co1 109.7(8) 22_665 . ?
C2 N1 Co1 109.7(8) . . ?
C4 O1 Co1 146.4(11) . . ?
C4 O2 Tb1 174.6(11) . . ?
Tb1 O3 H3C 115.9 . . ?
Tb1 O3 H3D 116.0 . . ?
H3C O3 H3D 97.4 . . ?
Cl1 O4 O5 53(4) . 3_645 ?
Cl1 O4 O5 53(4) . . ?
O5 O4 O5 87(5) 3_645 . ?
Cl1 O4 O5 53(4) . 5_765 ?
O5 O4 O5 87(5) 3_645 5_765 ?
O5 O4 O5 87(5) . 5_765 ?
Cl1 O5 O5 57(3) . 17_545 ?
Cl1 O5 O5 57(3) . 15_665 ?
O5 O5 O5 100(10) 17_545 15_665 ?
Cl1 O5 O4 52(4) . . ?
O5 O5 O4 86(7) 17_545 . ?
O5 O5 O4 86(7) 15_665 . ?
H6C O6 H6D 105.2 . . ?
H7C O7 H7D 105.4 . . ?
O2 Tb1 O2 135.81(18) 3_655 14_666 ?
O2 Tb1 O2 82.4(5) 3_655 18_656 ?
O2 Tb1 O2 81.3(4) 14_666 18_656 ?
O2 Tb1 O2 81.3(4) 3_655 5_665 ?
O2 Tb1 O2 82.4(5) 14_666 5_665 ?
O2 Tb1 O2 135.81(18) 18_656 5_665 ?
O2 Tb1 O2 135.81(18) 3_655 16_556 ?
O2 Tb1 O2 81.3(4) 14_666 16_556 ?
O2 Tb1 O2 81.3(4) 18_656 16_556 ?
O2 Tb1 O2 135.81(18) 5_665 16_556 ?
O2 Tb1 O2 81.3(4) 3_655 . ?
O2 Tb1 O2 135.81(18) 14_666 . ?
O2 Tb1 O2 135.81(18) 18_656 . ?
O2 Tb1 O2 81.3(4) 5_665 . ?
O2 Tb1 O2 82.4(5) 16_556 . ?
O2 Tb1 O3 67.90(9) 3_655 . ?
O2 Tb1 O3 67.90(9) 14_666 . ?
O2 Tb1 O3 67.90(9) 18_656 . ?
O2 Tb1 O3 67.90(9) 5_665 . ?
O2 Tb1 O3 138.8(3) 16_556 . ?
O2 Tb1 O3 138.8(3) . . ?
O2 Tb1 O3 138.8(3) 3_655 3_655 ?
O2 Tb1 O3 67.90(9) 14_666 3_655 ?
O2 Tb1 O3 138.8(3) 18_656 3_655 ?
O2 Tb1 O3 67.90(9) 5_665 3_655 ?
O2 Tb1 O3 67.90(9) 16_556 3_655 ?
O2 Tb1 O3 67.90(9) . 3_655 ?
O3 Tb1 O3 120.000(4) . 3_655 ?
O2 Tb1 O3 67.90(9) 3_655 14_666 ?
O2 Tb1 O3 138.8(3) 14_666 14_666 ?
O2 Tb1 O3 67.90(9) 18_656 14_666 ?
O2 Tb1 O3 138.8(3) 5_665 14_666 ?
O2 Tb1 O3 67.90(9) 16_556 14_666 ?
O2 Tb1 O3 67.90(9) . 14_666 ?
O3 Tb1 O3 120.000(2) . 14_666 ?
O3 Tb1 O3 120.000(2) 3_655 14_666 ?

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
N1 C2 C3 C4 47(2) . . . 5_565 ?
C1 C1 N1 C1 104.9(10) 24_565 . . 22_665 ?
C1 C1 N1 C2 -147.3(11) 24_565 . . 22_665 ?
C1 C1 N1 C2 -122.9(8) 24_565 . . . ?
C1 C1 N1 Co1 -11.8(7) 24_565 . . . ?
C3 C2 N1 C1 55.7(16) . . . . ?
C3 C2 N1 C1 171.4(13) . . . 22_665 ?
C3 C2 N1 C2 -152.0(13) . . . 22_665 ?
C3 C2 N1 Co1 -53.7(16) . . . . ?
O1 Co1 N1 C1 -164.3(8) 3_665 . . . ?
O1 Co1 N1 C1 -78.3(8) 5_565 . . . ?
N1 Co1 N1 C1 14.7(9) 3_665 . . . ?
N1 Co1 N1 C1 102.7(7) 5_565 . . . ?
O1 Co1 N1 C1 78.3(8) 3_665 . . 22_665 ?
O1 Co1 N1 C1 164.3(8) 5_565 . . 22_665 ?
N1 Co1 N1 C1 -102.7(7) 3_665 . . 22_665 ?
N1 Co1 N1 C1 -14.7(9) 5_565 . . 22_665 ?
O1 Co1 N1 C2 -19.7(8) 3_665 . . 22_665 ?
O1 Co1 N1 C2 66.3(8) 5_565 . . 22_665 ?
N1 Co1 N1 C2 159.3(8) 3_665 . . 22_665 ?
N1 Co1 N1 C2 -112.7(9) 5_565 . . 22_665 ?
O1 Co1 N1 C2 -66.3(8) 3_665 . . . ?
O1 Co1 N1 C2 19.7(8) 5_565 . . . ?
N1 Co1 N1 C2 112.7(9) 3_665 . . . ?
N1 Co1 N1 C2 -159.3(8) 5_565 . . . ?
O2 C4 O1 Co1 180.000(3) . . . . ?
C3 C4 O1 Co1 -53.8(8) 3_665 . . . ?
C3 C4 O1 Co1 53.8(8) 20 . . . ?
O1 Co1 O1 C4 -136.97(19) 3_665 . . . ?
O1 Co1 O1 C4 136.97(19) 5_565 . . . ?
N1 Co1 O1 C4 44.0(2) 3_665 . . . ?
N1 Co1 O1 C4 -44.0(2) 5_565 . . . ?
O5 Cl1 O4 O5 60.000(2) 17_545 . . 3_645 ?
O5 Cl1 O4 O5 -120.000(2) 5_765 . . 3_645 ?
O5 Cl1 O4 O5 180.000(2) 15_665 . . 3_645 ?
O5 Cl1 O4 O5 120.000(2) . . . 3_645 ?
O5 Cl1 O4 O5 -60.000(2) 13_755 . . 3_645 ?
O5 Cl1 O4 O5 -60.000(3) 17_545 . . . ?
O5 Cl1 O4 O5 120.000(3) 5_765 . . . ?
O5 Cl1 O4 O5 60.000(3) 15_665 . . . ?
O5 Cl1 O4 O5 -120.000(3) 3_645 . . . ?
O5 Cl1 O4 O5 180.000(2) 13_755 . . . ?
O5 Cl1 O4 O5 180.0 17_545 . . 5_765 ?
O5 Cl1 O4 O5 -60.0 15_665 . . 5_765 ?
O5 Cl1 O4 O5 120.000(1) 3_645 . . 5_765 ?
O5 Cl1 O4 O5 -120.000(1) . . . 5_765 ?
O5 Cl1 O4 O5 60.0 13_755 . . 5_765 ?
O4 Cl1 O5 O5 66(10) 13_755 . . 17_545 ?
O4 Cl1 O5 O5 -114(10) . . . 17_545 ?
O5 Cl1 O5 O5 180.0 5_765 . . 17_545 ?
O5 Cl1 O5 O5 132(20) 15_665 . . 17_545 ?
O5 Cl1 O5 O5 -48(20) 3_645 . . 17_545 ?
O4 Cl1 O5 O5 -66(10) 13_755 . . 15_665 ?
O4 Cl1 O5 O5 114(10) . . . 15_665 ?
O5 Cl1 O5 O5 -132(20) 17_545 . . 15_665 ?
O5 Cl1 O5 O5 48(20) 5_765 . . 15_665 ?
O5 Cl1 O5 O5 180.0 3_645 . . 15_665 ?
O4 Cl1 O5 O4 180.000(2) 13_755 . . . ?
O5 Cl1 O5 O4 114(10) 17_545 . . . ?
O5 Cl1 O5 O4 -66(10) 5_765 . . . ?
O5 Cl1 O5 O4 -114(10) 15_665 . . . ?
O5 Cl1 O5 O4 66(10) 3_645 . . . ?
O5 O4 O5 Cl1 -43(2) 3_645 . . . ?
O5 O4 O5 Cl1 43(2) 5_765 . . . ?
Cl1 O4 O5 O5 50(8) . . . 17_545 ?
O5 O4 O5 O5 6(11) 3_645 . . 17_545 ?
O5 O4 O5 O5 93(6) 5_765 . . 17_545 ?
Cl1 O4 O5 O5 -50(8) . . . 15_665 ?
O5 O4 O5 O5 -93(6) 3_645 . . 15_665 ?
O5 O4 O5 O5 -6(11) 5_765 . . 15_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.557
_refine_diff_density_min         -1.897
_refine_diff_density_rms         0.203
####################################################################### 
# 
# 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 2165409'
loop_
_audit_author_name
_audit_author_address
'Zhong Zhang'
;Guangxi Normal University
China
;
_audit_update_record             
;
2022-07-03 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H24 Co N3 O6, 4(H2 O)'
_chemical_formula_sum            'C15 H32 Co N3 O10'
_chemical_formula_weight         473.37

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'

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

_cell_length_a                   13.4684(16)
_cell_length_b                   13.4684(16)
_cell_length_c                   13.0934(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2056.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1085
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      24.00

_exptl_crystal_description       plate
_exptl_crystal_colour            purple-red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 Smart Apex CCD II'
_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            6815
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1350
_reflns_number_gt                930
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0350P)²+0.5000P] 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         1350
_refine_ls_number_parameters     87
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0824
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
C1 C 0.4785(2) 0.7077(2) 0.44376(19) 0.0348(7) Uani 1 1 d . . .
H1A H 0.5602 0.7434 0.4568 0.042 Uiso 1 1 calc R . .
H1B H 0.4411 0.7088 0.5067 0.042 Uiso 1 1 calc R . .
C2 C 0.4145(2) 0.8471(2) 0.40931(18) 0.0330(6) Uani 1 1 d . . .
H2A H 0.4182 0.9026 0.3601 0.040 Uiso 1 1 calc R . .
H2B H 0.4623 0.8883 0.4673 0.040 Uiso 1 1 calc R . .
C3 C 0.5635(2) 0.8512(2) 0.30378(19) 0.0322(6) Uani 1 1 d . . .
H3A H 0.6187 0.9077 0.3505 0.039 Uiso 1 1 calc R . .
H3B H 0.5455 0.8920 0.2527 0.039 Uiso 1 1 calc R . .
C4 C 0.6184(2) 0.7907(2) 0.2513(2) 0.0360(7) Uani 1 1 d . . .
H4A H 0.6857 0.8478 0.2151 0.043 Uiso 1 1 calc R . .
H4B H 0.6446 0.7582 0.3036 0.043 Uiso 1 1 calc R . .
C5 C 0.5454(2) 0.6969(2) 0.17705(18) 0.0284(6) Uani 1 1 d . . .
Co1 Co 0.33333 0.66667 0.27295(4) 0.02308(18) Uani 1 3 d S . .
N1 N 0.45680(17) 0.77386(17) 0.36167(14) 0.0271(5) Uani 1 1 d . . .
O1 O 0.43466(14) 0.64502(14) 0.18377(12) 0.0282(4) Uani 1 1 d . . .
O2 O 0.59297(15) 0.66843(16) 0.11217(13) 0.0388(5) Uani 1 1 d . . .
O3 O 0.7828(2) 0.8061(2) -0.0087(2) 0.0819(8) Uani 1 1 d . . .
H3C H 0.7168 0.7840 0.0165 0.123 Uiso 1 1 d R . .
H3D H 0.8255 0.8200 0.0432 0.123 Uiso 1 1 d R . .
O4 O 1.0000 1.0000 0.1355(4) 2.00(17) Uiso 1 3 d SD . .
H4C H 0.9330 0.9601 0.1602 3.000 Uiso 0.66667 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.509(4) 3_565 ?
C1 N1 1.515(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.499(3) . ?
C2 C1 1.509(4) 2_665 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.492(3) . ?
C3 C4 1.512(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.506(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O2 1.235(3) . ?
C5 O1 1.295(3) . ?
Co1 O1 1.9258(17) 2_665 ?
Co1 O1 1.9258(17) 3_565 ?
Co1 O1 1.9258(17) . ?
Co1 N1 1.949(2) 2_665 ?
Co1 N1 1.949(2) . ?
Co1 N1 1.949(2) 3_565 ?
O3 H3C 0.8498 . ?
O3 H3D 0.8497 . ?
O4 H4C 0.8501 . ?

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
C2 C1 N1 109.57(19) 3_565 . ?
C2 C1 H1A 109.8 3_565 . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 3_565 . ?
N1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N1 C2 C1 108.7(2) . 2_665 ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 2_665 . ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 2_665 . ?
H2A C2 H2B 108.3 . . ?
N1 C3 C4 114.5(2) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C3 117.1(2) . . ?
C5 C4 H4A 108.0 . . ?
C3 C4 H4A 108.0 . . ?
C5 C4 H4B 108.0 . . ?
C3 C4 H4B 108.0 . . ?
H4A C4 H4B 107.3 . . ?
O2 C5 O1 121.0(2) . . ?
O2 C5 C4 118.8(2) . . ?
O1 C5 C4 120.1(2) . . ?
O1 Co1 O1 87.05(7) 2_665 3_565 ?
O1 Co1 O1 87.05(7) 2_665 . ?
O1 Co1 O1 87.05(7) 3_565 . ?
O1 Co1 N1 93.83(8) 2_665 2_665 ?
O1 Co1 N1 91.04(7) 3_565 2_665 ?
O1 Co1 N1 177.85(8) . 2_665 ?
O1 Co1 N1 91.04(7) 2_665 . ?
O1 Co1 N1 177.85(8) 3_565 . ?
O1 Co1 N1 93.83(8) . . ?
N1 Co1 N1 88.11(8) 2_665 . ?
O1 Co1 N1 177.85(8) 2_665 3_565 ?
O1 Co1 N1 93.83(8) 3_565 3_565 ?
O1 Co1 N1 91.04(7) . 3_565 ?
N1 Co1 N1 88.11(8) 2_665 3_565 ?
N1 Co1 N1 88.11(8) . 3_565 ?
C3 N1 C2 107.56(19) . . ?
C3 N1 C1 111.7(2) . . ?
C2 N1 C1 109.89(18) . . ?
C3 N1 Co1 112.42(14) . . ?
C2 N1 Co1 105.75(14) . . ?
C1 N1 Co1 109.35(15) . . ?
C5 O1 Co1 132.18(16) . . ?
H3C O3 H3D 103.9 . . ?

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
N1 C3 C4 C5 56.8(3) . . . . ?
C3 C4 C5 O2 159.4(2) . . . . ?
C3 C4 C5 O1 -22.8(3) . . . . ?
C4 C3 N1 C2 179.45(19) . . . . ?
C4 C3 N1 C1 58.8(3) . . . . ?
C4 C3 N1 Co1 -64.5(2) . . . . ?
C1 C2 N1 C3 164.9(2) 2_665 . . . ?
C1 C2 N1 C1 -73.3(3) 2_665 . . . ?
C1 C2 N1 Co1 44.6(2) 2_665 . . . ?
C2 C1 N1 C3 -104.1(2) 3_565 . . . ?
C2 C1 N1 C2 136.7(2) 3_565 . . . ?
C2 C1 N1 Co1 21.0(3) 3_565 . . . ?
O1 Co1 N1 C3 -49.99(17) 2_665 . . . ?
O1 Co1 N1 C3 37.12(17) . . . . ?
N1 Co1 N1 C3 -143.8(2) 2_665 . . . ?
N1 Co1 N1 C3 128.0(2) 3_565 . . . ?
O1 Co1 N1 C2 67.10(15) 2_665 . . . ?
O1 Co1 N1 C2 154.21(14) . . . . ?
N1 Co1 N1 C2 -26.70(16) 2_665 . . . ?
N1 Co1 N1 C2 -114.87(11) 3_565 . . . ?
O1 Co1 N1 C1 -174.62(16) 2_665 . . . ?
O1 Co1 N1 C1 -87.51(16) . . . . ?
N1 Co1 N1 C1 91.58(12) 2_665 . . . ?
N1 Co1 N1 C1 3.40(16) 3_565 . . . ?
O2 C5 O1 Co1 -179.52(16) . . . . ?
C4 C5 O1 Co1 2.7(3) . . . . ?
O1 Co1 O1 C5 81.5(2) 2_665 . . . ?
O1 Co1 O1 C5 168.7(2) 3_565 . . . ?
N1 Co1 O1 C5 -9.3(2) . . . . ?
N1 Co1 O1 C5 -97.5(2) 3_565 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.069
####################################################################### 
# 
# 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_3_NiCe
_database_code_depnum_ccdc_archive 'CCDC 2165411'
loop_
_audit_author_name
_audit_author_address
'Zhong Zhang'
;Guangxi Normal University
China
;
_audit_update_record             
;
2022-04-08 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H72 N6 Ni5 O24, Ce N6 O18, Cl, 2(H2 O)'
_chemical_formula_sum            'C30 H76 Ce Cl N12 Ni5 O44'
_chemical_formula_weight         1778.15

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

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

_cell_length_a                   11.999(4)
_cell_length_b                   11.999(4)
_cell_length_c                   26.786(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3340(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    3630
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      25.37

_exptl_crystal_description       plate
_exptl_crystal_colour            light-purple
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1814
_exptl_absorpt_coefficient_mu    2.197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(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 Smart Apex CCD II'
_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            17389
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         26.16
_reflns_number_total             2276
_reflns_number_gt                1688
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0716P)²+0.0000P] 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         2276
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1169
_refine_ls_wR_factor_gt          0.1158
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
Ni1 Ni 0.66667 0.33333 0.12290(3) 0.0255(2) Uani 1 3 d S . .
Ni2 Ni 0.30683(9) 0.01905(9) 0.2500 0.0475(3) Uani 1 2 d S . .
O1 O 0.5103(3) 0.2405(3) 0.16978(11) 0.0342(7) Uani 1 1 d . . .
O2 O 0.3080(3) 0.1451(3) 0.19528(12) 0.0450(8) Uani 1 1 d . . .
O3 O 0.5117(4) 0.1095(4) 0.2500 0.0451(11) Uani 1 2 d S . .
H3C H 0.5433 0.1344 0.2834 0.068 Uiso 0.50 1 d PR . .
H3D H 0.5469 0.1843 0.2290 0.068 Uiso 0.50 1 d PR . .
O4 O 0.1134(4) -0.0746(5) 0.2500 0.0499(12) Uani 1 2 d S . .
H4C H 0.1046 -0.1220 0.2250 0.075 Uiso 1 1 d R . .
O5 O 0.3111(4) -0.0908(4) 0.19094(13) 0.0623(11) Uani 1 1 d . . .
H5C H 0.3308 -0.0799 0.1602 0.093 Uiso 1 1 d R . .
H5D H 0.3271 -0.1476 0.2021 0.093 Uiso 1 1 d R . .
N1 N 0.5640(3) 0.3840(3) 0.07513(13) 0.0316(8) Uani 1 1 d . . .
C1 C 0.6660(4) 0.5071(4) 0.05308(17) 0.0406(11) Uani 1 1 d . . .
H1A H 0.6931 0.5751 0.0777 0.049 Uiso 1 1 calc R . .
H1B H 0.6306 0.5295 0.0248 0.049 Uiso 1 1 calc R . .
C2 C 0.5011(5) 0.2831(4) 0.03608(19) 0.0429(12) Uani 1 1 d . . .
H2A H 0.5503 0.3119 0.0054 0.052 Uiso 1 1 calc R . .
H2B H 0.4153 0.2685 0.0295 0.052 Uiso 1 1 calc R . .
C3 C 0.4693(4) 0.4059(4) 0.10284(18) 0.0387(11) Uani 1 1 d . . .
H3A H 0.4310 0.4397 0.0798 0.046 Uiso 1 1 calc R . .
H3B H 0.5147 0.4709 0.1282 0.046 Uiso 1 1 calc R . .
C4 C 0.3623(4) 0.2867(4) 0.12781(18) 0.0363(11) Uani 1 1 d . . .
H4A H 0.3030 0.3101 0.1425 0.044 Uiso 1 1 calc R . .
H4B H 0.3157 0.2240 0.1019 0.044 Uiso 1 1 calc R . .
C5 C 0.3971(4) 0.2213(4) 0.16725(16) 0.0306(9) Uani 1 1 d . . .
Ce1 Ce 0.0000 1.0000 0.0000 0.02880(19) Uani 1 6 d S . .
O6 O 0.1430(3) 1.0033(3) 0.07578(13) 0.0456(8) Uani 1 1 d . . .
O7 O 0.0785(3) 0.8382(3) 0.02672(12) 0.0417(8) Uani 1 1 d . . .
O8 O 0.2125(4) 0.8686(4) 0.08695(15) 0.0669(11) Uani 1 1 d . . .
N2 N 0.1445(4) 0.9005(4) 0.06349(15) 0.0424(9) Uani 1 1 d . . .
Cl1 Cl 0.33333 0.66667 0.19476(17) 0.0541(11) Uani 0.50 3 d SP . .
O9 O 1.0000 0.0000 0.1725(2) 0.0590(17) Uani 1 3 d S . .
H9C H 0.9719 0.0460 0.1853 0.089 Uiso 0.66667 1 d PR . .


_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 O1 2.061(3) 3_655 ?
Ni1 O1 2.061(3) 5_665 ?
Ni1 O1 2.061(3) . ?
Ni1 N1 2.067(3) 3_655 ?
Ni1 N1 2.067(4) 5_665 ?
Ni1 N1 2.067(3) . ?
Ni2 O4 2.011(5) . ?
Ni2 O5 2.076(4) . ?
Ni2 O5 2.076(4) 10_556 ?
Ni2 O2 2.102(3) 10_556 ?
Ni2 O2 2.102(3) . ?
Ni2 O3 2.134(5) . ?
O1 C5 1.261(5) . ?
O2 C5 1.251(5) . ?
O3 H3C 0.9592 . ?
O3 H3D 0.9598 . ?
O4 H4C 0.8503 . ?
O5 H5C 0.8486 . ?
O5 H5D 0.8494 . ?
N1 C3 1.487(5) . ?
N1 C2 1.488(6) . ?
N1 C1 1.491(5) . ?
C1 C2 1.513(6) 5_665 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C1 1.513(6) 3_655 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.518(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.495(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
Ce1 O7 2.645(3) 9_455 ?
Ce1 O7 2.645(3) 3_675 ?
Ce1 O7 2.645(3) 11_665 ?
Ce1 O7 2.645(3) 5_465 ?
Ce1 O7 2.645(3) . ?
Ce1 O7 2.645(3) 7_575 ?
Ce1 O6 2.645(3) 9_455 ?
Ce1 O6 2.645(3) 7_575 ?
Ce1 O6 2.645(3) . ?
Ce1 O6 2.645(3) 3_675 ?
Ce1 O6 2.645(3) 5_465 ?
Ce1 O6 2.645(3) 11_665 ?
O6 N2 1.286(5) . ?
O7 N2 1.251(5) . ?
O8 N2 1.232(5) . ?
O9 H9C 0.8497 . ?

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
O1 Ni1 O1 86.76(12) 3_655 5_665 ?
O1 Ni1 O1 86.76(12) 3_655 . ?
O1 Ni1 O1 86.76(12) 5_665 . ?
O1 Ni1 N1 91.18(13) 3_655 3_655 ?
O1 Ni1 N1 176.06(12) 5_665 3_655 ?
O1 Ni1 N1 96.48(13) . 3_655 ?
O1 Ni1 N1 96.48(13) 3_655 5_665 ?
O1 Ni1 N1 91.18(13) 5_665 5_665 ?
O1 Ni1 N1 176.06(12) . 5_665 ?
N1 Ni1 N1 85.71(15) 3_655 5_665 ?
O1 Ni1 N1 176.06(12) 3_655 . ?
O1 Ni1 N1 96.48(13) 5_665 . ?
O1 Ni1 N1 91.18(13) . . ?
N1 Ni1 N1 85.71(15) 3_655 . ?
N1 Ni1 N1 85.71(15) 5_665 . ?
O4 Ni2 O5 91.90(15) . . ?
O4 Ni2 O5 91.90(15) . 10_556 ?
O5 Ni2 O5 99.3(2) . 10_556 ?
O4 Ni2 O2 89.57(13) . 10_556 ?
O5 Ni2 O2 174.35(14) . 10_556 ?
O5 Ni2 O2 86.12(15) 10_556 10_556 ?
O4 Ni2 O2 89.57(13) . . ?
O5 Ni2 O2 86.12(15) . . ?
O5 Ni2 O2 174.35(14) 10_556 . ?
O2 Ni2 O2 88.44(19) 10_556 . ?
O4 Ni2 O3 177.2(2) . . ?
O5 Ni2 O3 86.27(14) . . ?
O5 Ni2 O3 86.27(14) 10_556 . ?
O2 Ni2 O3 92.46(13) 10_556 . ?
O2 Ni2 O3 92.46(13) . . ?
C5 O1 Ni1 132.3(3) . . ?
C5 O2 Ni2 129.8(3) . . ?
Ni2 O3 H3C 109.5 . . ?
Ni2 O3 H3D 109.4 . . ?
H3C O3 H3D 109.6 . . ?
Ni2 O4 H4C 95.5 . . ?
Ni2 O5 H5C 137.3 . . ?
Ni2 O5 H5D 109.2 . . ?
H5C O5 H5D 107.9 . . ?
C3 N1 C2 111.9(3) . . ?
C3 N1 C1 110.1(3) . . ?
C2 N1 C1 111.0(4) . . ?
C3 N1 Ni1 111.3(3) . . ?
C2 N1 Ni1 109.3(3) . . ?
C1 N1 Ni1 102.8(3) . . ?
N1 C1 C2 112.4(4) . 5_665 ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 5_665 . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 5_665 . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C1 110.3(4) . 3_655 ?
N1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 3_655 . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 3_655 . ?
H2A C2 H2B 108.1 . . ?
N1 C3 C4 114.4(4) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 H4A 107.6 . . ?
C3 C4 H4A 107.6 . . ?
C5 C4 H4B 107.6 . . ?
C3 C4 H4B 107.6 . . ?
H4A C4 H4B 107.1 . . ?
O2 C5 O1 123.4(4) . . ?
O2 C5 C4 116.5(4) . . ?
O1 C5 C4 120.0(4) . . ?
O7 Ce1 O7 180.00(13) 9_455 3_675 ?
O7 Ce1 O7 112.97(6) 9_455 11_665 ?
O7 Ce1 O7 67.03(6) 3_675 11_665 ?
O7 Ce1 O7 67.03(6) 9_455 5_465 ?
O7 Ce1 O7 112.97(6) 3_675 5_465 ?
O7 Ce1 O7 180.0 11_665 5_465 ?
O7 Ce1 O7 67.03(6) 9_455 . ?
O7 Ce1 O7 112.97(6) 3_675 . ?
O7 Ce1 O7 67.03(6) 11_665 . ?
O7 Ce1 O7 112.97(6) 5_465 . ?
O7 Ce1 O7 112.97(6) 9_455 7_575 ?
O7 Ce1 O7 67.03(6) 3_675 7_575 ?
O7 Ce1 O7 112.97(6) 11_665 7_575 ?
O7 Ce1 O7 67.03(6) 5_465 7_575 ?
O7 Ce1 O7 180.00(13) . 7_575 ?
O7 Ce1 O6 48.48(10) 9_455 9_455 ?
O7 Ce1 O6 131.52(10) 3_675 9_455 ?
O7 Ce1 O6 70.05(10) 11_665 9_455 ?
O7 Ce1 O6 109.95(10) 5_465 9_455 ?
O7 Ce1 O6 67.59(10) . 9_455 ?
O7 Ce1 O6 112.41(10) 7_575 9_455 ?
O7 Ce1 O6 70.05(10) 9_455 7_575 ?
O7 Ce1 O6 109.95(10) 3_675 7_575 ?
O7 Ce1 O6 112.41(10) 11_665 7_575 ?
O7 Ce1 O6 67.59(10) 5_465 7_575 ?
O7 Ce1 O6 131.52(10) . 7_575 ?
O7 Ce1 O6 48.48(10) 7_575 7_575 ?
O6 Ce1 O6 67.48(12) 9_455 7_575 ?
O7 Ce1 O6 109.95(10) 9_455 . ?
O7 Ce1 O6 70.05(10) 3_675 . ?
O7 Ce1 O6 67.59(10) 11_665 . ?
O7 Ce1 O6 112.41(10) 5_465 . ?
O7 Ce1 O6 48.48(10) . . ?
O7 Ce1 O6 131.52(10) 7_575 . ?
O6 Ce1 O6 112.52(12) 9_455 . ?
O6 Ce1 O6 180.00(19) 7_575 . ?
O7 Ce1 O6 131.52(10) 9_455 3_675 ?
O7 Ce1 O6 48.48(10) 3_675 3_675 ?
O7 Ce1 O6 109.95(10) 11_665 3_675 ?
O7 Ce1 O6 70.05(10) 5_465 3_675 ?
O7 Ce1 O6 112.41(10) . 3_675 ?
O7 Ce1 O6 67.59(10) 7_575 3_675 ?
O6 Ce1 O6 180.00(9) 9_455 3_675 ?
O6 Ce1 O6 112.52(12) 7_575 3_675 ?
O6 Ce1 O6 67.48(12) . 3_675 ?
O7 Ce1 O6 67.59(10) 9_455 5_465 ?
O7 Ce1 O6 112.41(10) 3_675 5_465 ?
O7 Ce1 O6 131.52(10) 11_665 5_465 ?
O7 Ce1 O6 48.48(10) 5_465 5_465 ?
O7 Ce1 O6 70.05(10) . 5_465 ?
O7 Ce1 O6 109.95(10) 7_575 5_465 ?
O6 Ce1 O6 112.52(12) 9_455 5_465 ?
O6 Ce1 O6 112.52(12) 7_575 5_465 ?
O6 Ce1 O6 67.48(12) . 5_465 ?
O6 Ce1 O6 67.48(12) 3_675 5_465 ?
O7 Ce1 O6 112.41(10) 9_455 11_665 ?
O7 Ce1 O6 67.59(10) 3_675 11_665 ?
O7 Ce1 O6 48.48(10) 11_665 11_665 ?
O7 Ce1 O6 131.52(10) 5_465 11_665 ?
O7 Ce1 O6 109.95(10) . 11_665 ?
O7 Ce1 O6 70.05(10) 7_575 11_665 ?
O6 Ce1 O6 67.48(12) 9_455 11_665 ?
O6 Ce1 O6 67.48(12) 7_575 11_665 ?
O6 Ce1 O6 112.52(12) . 11_665 ?
O6 Ce1 O6 112.52(12) 3_675 11_665 ?
O6 Ce1 O6 180.00(15) 5_465 11_665 ?
N2 O6 Ce1 96.3(3) . . ?
N2 O7 Ce1 97.3(3) . . ?
O8 N2 O7 122.5(4) . . ?
O8 N2 O6 119.7(4) . . ?
O7 N2 O6 117.8(4) . . ?

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
O1 Ni1 O1 C5 -174.4(4) 3_655 . . . ?
O1 Ni1 O1 C5 98.6(4) 5_665 . . . ?
N1 Ni1 O1 C5 -83.6(4) 3_655 . . . ?
N1 Ni1 O1 C5 2.2(4) . . . . ?
O4 Ni2 O2 C5 -164.2(4) . . . . ?
O5 Ni2 O2 C5 -72.3(4) . . . . ?
O2 Ni2 O2 C5 106.2(4) 10_556 . . . ?
O3 Ni2 O2 C5 13.8(4) . . . . ?
O1 Ni1 N1 C3 -54.4(3) 5_665 . . . ?
O1 Ni1 N1 C3 32.5(3) . . . . ?
N1 Ni1 N1 C3 128.9(3) 3_655 . . . ?
N1 Ni1 N1 C3 -145.1(3) 5_665 . . . ?
O1 Ni1 N1 C2 -178.5(3) 5_665 . . . ?
O1 Ni1 N1 C2 -91.7(3) . . . . ?
N1 Ni1 N1 C2 4.7(3) 3_655 . . . ?
N1 Ni1 N1 C2 90.8(2) 5_665 . . . ?
O1 Ni1 N1 C1 63.5(3) 5_665 . . . ?
O1 Ni1 N1 C1 150.3(3) . . . . ?
N1 Ni1 N1 C1 -113.2(2) 3_655 . . . ?
N1 Ni1 N1 C1 -27.2(3) 5_665 . . . ?
C3 N1 C1 C2 165.3(4) . . . 5_665 ?
C2 N1 C1 C2 -70.2(5) . . . 5_665 ?
Ni1 N1 C1 C2 46.6(4) . . . 5_665 ?
C3 N1 C2 C1 -104.3(4) . . . 3_655 ?
C1 N1 C2 C1 132.2(4) . . . 3_655 ?
Ni1 N1 C2 C1 19.5(5) . . . 3_655 ?
C2 N1 C3 C4 57.2(5) . . . . ?
C1 N1 C3 C4 -178.8(4) . . . . ?
Ni1 N1 C3 C4 -65.4(4) . . . . ?
N1 C3 C4 C5 61.8(6) . . . . ?
Ni2 O2 C5 O1 -4.4(6) . . . . ?
Ni2 O2 C5 C4 172.8(3) . . . . ?
Ni1 O1 C5 O2 168.2(3) . . . . ?
Ni1 O1 C5 C4 -8.9(6) . . . . ?
C3 C4 C5 O2 162.7(4) . . . . ?
C3 C4 C5 O1 -19.9(6) . . . . ?
O7 Ce1 O6 N2 31.4(3) 9_455 . . . ?
O7 Ce1 O6 N2 -148.6(3) 3_675 . . . ?
O7 Ce1 O6 N2 -76.0(3) 11_665 . . . ?
O7 Ce1 O6 N2 104.0(3) 5_465 . . . ?
O7 Ce1 O6 N2 2.5(2) . . . . ?
O7 Ce1 O6 N2 -177.5(2) 7_575 . . . ?
O6 Ce1 O6 N2 -20.8(3) 9_455 . . . ?
O6 Ce1 O6 N2 159.2(3) 3_675 . . . ?
O6 Ce1 O6 N2 85.2(3) 5_465 . . . ?
O6 Ce1 O6 N2 -94.8(3) 11_665 . . . ?
O7 Ce1 O7 N2 -153.0(3) 9_455 . . . ?
O7 Ce1 O7 N2 27.0(3) 3_675 . . . ?
O7 Ce1 O7 N2 77.2(2) 11_665 . . . ?
O7 Ce1 O7 N2 -102.8(2) 5_465 . . . ?
O6 Ce1 O7 N2 154.1(3) 9_455 . . . ?
O6 Ce1 O7 N2 177.4(2) 7_575 . . . ?
O6 Ce1 O7 N2 -2.6(2) . . . . ?
O6 Ce1 O7 N2 -25.9(3) 3_675 . . . ?
O6 Ce1 O7 N2 -79.7(3) 5_465 . . . ?
O6 Ce1 O7 N2 100.3(3) 11_665 . . . ?
Ce1 O7 N2 O8 -173.5(4) . . . . ?
Ce1 O7 N2 O6 4.5(4) . . . . ?
Ce1 O6 N2 O8 173.5(4) . . . . ?
Ce1 O6 N2 O7 -4.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.16
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.127
####################################################################### 
# 
# 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_6_CoTb_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2165413'
loop_
_audit_author_name
_audit_author_address
'Zhong Zhang'
;Guangxi Normal University
China
;
_audit_update_record             
;
2022-09-07 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'6(C5 H9 Co0.33 N O2.50 Tb0.17), Cl O4, 2(Cl), 5(H2 O)'
_chemical_formula_sum            'C30 H64 Cl3 Co2 N6 O24 Tb'
_chemical_formula_weight         1276.00

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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'

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

_cell_length_a                   9.0019(13)
_cell_length_b                   9.0019(13)
_cell_length_c                   30.036(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2107.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6794
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      26.08

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 Smart Apex CCD II'
_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            23690
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         26.00
_reflns_number_total             852
_reflns_number_gt                796
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0600P)²+70.0000P] 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         852
_refine_ls_number_parameters     82
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1819
_refine_ls_wR_factor_gt          0.1809
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.015
_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
C1 C 0.1064(14) 0.6303(17) 0.0613(4) 0.097(6) Uani 1 1 d . . .
H1A H -0.0064 0.6075 0.0705 0.117 Uiso 1 1 calc R . .
H1B H 0.1239 0.6727 0.0309 0.117 Uiso 1 1 calc R . .
C2 C 0.088(2) 0.781(2) 0.1155(6) 0.036(4) Uani 0.50 1 d P . .
H2A H 0.1439 0.8706 0.1375 0.043 Uiso 0.25 1 calc PR . .
H2B H 0.0333 0.8198 0.0943 0.043 Uiso 0.25 1 calc PR . .
C3 C -0.056(2) 0.623(3) 0.1395(6) 0.040(4) Uani 0.50 1 d P . .
H3A H -0.1373 0.5501 0.1170 0.048 Uiso 0.50 1 calc PR . .
H3B H -0.1160 0.6635 0.1584 0.048 Uiso 0.50 1 calc PR . .
C4 C 0.5026(10) 0.4974(10) 0.1715(4) 0.061(5) Uani 1 2 d S . .
Cl1 Cl 1.0000 0.0000 0.0000 0.36(3) Uani 1 12 d SDU . .
Cl2 Cl 0.66667 0.33333 0.05209(18) 0.0391(13) Uani 1 6 d S . .
Co1 Co 0.33333 0.66667 0.12877(8) 0.0229(7) Uani 1 6 d S . .
N1 N 0.2336(7) 0.7664(7) 0.0895(3) 0.045(3) Uani 1 2 d S . .
O1 O 0.4287(6) 0.5713(6) 0.1682(3) 0.063(4) Uani 1 2 d S . .
O2 O 0.5550(6) 0.4450(6) 0.1994(3) 0.047(3) Uani 1 2 d S . .
O3 O 0.8267(14) 0.1733(14) 0.2500 0.108(8) Uani 1 4 d S . .
H3C H 0.7849 0.0866 0.2323 0.161 Uiso 0.50 1 d PR . .
H3D H 0.8316 0.1277 0.2747 0.161 Uiso 0.50 1 d PR . .
O4 O 1.0000 0.0000 0.0479(3) 0.36(3) Uani 0.50 6 d SPDU . .
O5 O 0.912(3) 0.088(3) 0.015(4) 0.36(3) Uani 0.50 2 d SPDU . .
O6 O 0.1956(13) 0.391(3) 0.2500 0.070(5) Uani 1 4 d S . .
H6C H 0.1883 0.3348 0.2265 0.104 Uiso 0.25 1 d PR . .
H6D H 0.2160 0.4886 0.2408 0.104 Uiso 0.25 1 d PR . .
O7 O 1.0000 1.0000 0.208(2) 0.37(5) Uani 1 6 d S . .
H7C H 0.9620 0.9241 0.1823 0.561 Uiso 0.33333 2 d SPR . .
H7D H 0.9225 1.0266 0.2034 0.561 Uiso 0.16667 1 d PR . .
Tb1 Tb 0.66667 0.33333 0.2500 0.0237(4) Uani 1 12 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C1 1.39(3) 24_565 ?
C1 N1 1.459(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.54(2) . ?
C2 N1 1.585(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.71(2) 5_565 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O1 1.156(19) . ?
C4 O2 1.171(17) . ?
C4 C3 1.71(2) 3_665 ?
C4 C3 1.71(2) 20 ?
Cl1 O4 1.439(10) 13_755 ?
Cl1 O4 1.439(10) . ?
Cl1 O5 1.443(10) 5_765 ?
Cl1 O5 1.443(10) 17_545 ?
Cl1 O5 1.443(10) 13_755 ?
Cl1 O5 1.443(10) 3_645 ?
Cl1 O5 1.443(10) 15_665 ?
Cl1 O5 1.443(10) . ?
Co1 O1 1.902(10) 3_665 ?
Co1 O1 1.902(10) 5_565 ?
Co1 O1 1.902(10) . ?
Co1 N1 1.952(10) . ?
Co1 N1 1.952(10) 3_665 ?
Co1 N1 1.952(10) 5_565 ?
N1 C1 1.459(12) 22_665 ?
N1 C2 1.585(19) 22_665 ?
O2 Tb1 2.312(9) . ?
O3 Tb1 2.50(2) . ?
O3 H3C 0.8593 . ?
O3 H3D 0.8604 . ?
O4 O5 1.69(11) 3_645 ?
O4 O5 1.69(11) . ?
O4 O5 1.69(11) 5_765 ?
O5 O5 1.64(10) 17_545 ?
O5 O5 1.64(10) 15_665 ?
O6 H6C 0.8523 . ?
O6 H6D 0.8467 . ?
O7 H7C 0.9737 . ?
O7 H7D 0.8548 . ?
Tb1 O2 2.312(9) 14_666 ?
Tb1 O2 2.312(9) 3_655 ?
Tb1 O2 2.312(9) 18_656 ?
Tb1 O2 2.312(9) 5_665 ?
Tb1 O2 2.312(9) 16_556 ?
Tb1 O3 2.50(2) 3_655 ?
Tb1 O3 2.50(2) 14_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
C1 C1 N1 116.6(7) 24_565 . ?
C1 C1 H1A 108.1 24_565 . ?
N1 C1 H1A 108.1 . . ?
C1 C1 H1B 108.1 24_565 . ?
N1 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C3 C2 N1 120.4(14) . . ?
C3 C2 H2A 107.2 . . ?
N1 C2 H2A 107.2 . . ?
C3 C2 H2B 107.2 . . ?
N1 C2 H2B 107.2 . . ?
H2A C2 H2B 106.9 . . ?
C2 C3 C4 119.4(14) . 5_565 ?
C2 C3 H3A 107.5 . . ?
C4 C3 H3A 107.5 5_565 . ?
C2 C3 H3B 107.5 . . ?
C4 C3 H3B 107.5 5_565 . ?
H3A C3 H3B 107.0 . . ?
O1 C4 O2 139.1(14) . . ?
O1 C4 C3 100.6(10) . 3_665 ?
O2 C4 C3 103.9(10) . 3_665 ?
O1 C4 C3 100.6(10) . 20 ?
O2 C4 C3 103.9(10) . 20 ?
C3 C4 C3 105.3(15) 3_665 20 ?
O4 Cl1 O4 180.0 13_755 . ?
O4 Cl1 O5 108(5) 13_755 5_765 ?
O4 Cl1 O5 72(5) . 5_765 ?
O4 Cl1 O5 72(5) 13_755 17_545 ?
O4 Cl1 O5 108(5) . 17_545 ?
O5 Cl1 O5 180(7) 5_765 17_545 ?
O4 Cl1 O5 72(5) 13_755 13_755 ?
O4 Cl1 O5 108(5) . 13_755 ?
O5 Cl1 O5 69(5) 5_765 13_755 ?
O5 Cl1 O5 111(5) 17_545 13_755 ?
O4 Cl1 O5 108(5) 13_755 3_645 ?
O4 Cl1 O5 72(5) . 3_645 ?
O5 Cl1 O5 111(5) 5_765 3_645 ?
O5 Cl1 O5 69(5) 17_545 3_645 ?
O5 Cl1 O5 69(5) 13_755 3_645 ?
O4 Cl1 O5 72(5) 13_755 15_665 ?
O4 Cl1 O5 108(5) . 15_665 ?
O5 Cl1 O5 69(5) 5_765 15_665 ?
O5 Cl1 O5 111(5) 17_545 15_665 ?
O5 Cl1 O5 111(5) 13_755 15_665 ?
O5 Cl1 O5 180(7) 3_645 15_665 ?
O4 Cl1 O5 108(5) 13_755 . ?
O4 Cl1 O5 72(5) . . ?
O5 Cl1 O5 111(5) 5_765 . ?
O5 Cl1 O5 69(5) 17_545 . ?
O5 Cl1 O5 180(7) 13_755 . ?
O5 Cl1 O5 111(5) 3_645 . ?
O5 Cl1 O5 69(5) 15_665 . ?
O1 Co1 O1 85.3(4) 3_665 5_565 ?
O1 Co1 O1 85.3(4) 3_665 . ?
O1 Co1 O1 85.3(4) 5_565 . ?
O1 Co1 N1 93.7(3) 3_665 . ?
O1 Co1 N1 93.7(3) 5_565 . ?
O1 Co1 N1 178.6(4) . . ?
O1 Co1 N1 178.6(4) 3_665 3_665 ?
O1 Co1 N1 93.7(3) 5_565 3_665 ?
O1 Co1 N1 93.7(3) . 3_665 ?
N1 Co1 N1 87.3(4) . 3_665 ?
O1 Co1 N1 93.7(3) 3_665 5_565 ?
O1 Co1 N1 178.6(4) 5_565 5_565 ?
O1 Co1 N1 93.7(3) . 5_565 ?
N1 Co1 N1 87.3(4) . 5_565 ?
N1 Co1 N1 87.3(4) 3_665 5_565 ?
C1 N1 C1 108.6(10) . 22_665 ?
C1 N1 C2 128.8(11) . 22_665 ?
C1 N1 C2 91.1(10) 22_665 22_665 ?
C1 N1 C2 91.1(10) . . ?
C1 N1 C2 128.8(11) 22_665 . ?
C1 N1 Co1 108.2(7) . . ?
C1 N1 Co1 108.2(7) 22_665 . ?
C2 N1 Co1 109.3(7) 22_665 . ?
C2 N1 Co1 109.3(7) . . ?
C4 O1 Co1 146.3(10) . . ?
C4 O2 Tb1 175.4(10) . . ?
Tb1 O3 H3C 114.0 . . ?
Tb1 O3 H3D 117.2 . . ?
H3C O3 H3D 101.8 . . ?
Cl1 O4 O5 54(3) . 3_645 ?
Cl1 O4 O5 54(3) . . ?
O5 O4 O5 89(4) 3_645 . ?
Cl1 O4 O5 54(3) . 5_765 ?
O5 O4 O5 89(4) 3_645 5_765 ?
O5 O4 O5 89(4) . 5_765 ?
Cl1 O5 O5 55(2) . 17_545 ?
Cl1 O5 O5 55(2) . 15_665 ?
O5 O5 O5 93(10) 17_545 15_665 ?
Cl1 O5 O4 54(3) . . ?
O5 O5 O4 89(4) 17_545 . ?
O5 O5 O4 89(4) 15_665 . ?
H6C O6 H6D 105.0 . . ?
H7C O7 H7D 91.1 . . ?
O2 Tb1 O2 135.75(17) 14_666 3_655 ?
O2 Tb1 O2 81.4(4) 14_666 18_656 ?
O2 Tb1 O2 82.3(5) 3_655 18_656 ?
O2 Tb1 O2 82.3(5) 14_666 5_665 ?
O2 Tb1 O2 81.4(4) 3_655 5_665 ?
O2 Tb1 O2 135.75(17) 18_656 5_665 ?
O2 Tb1 O2 135.75(17) 14_666 . ?
O2 Tb1 O2 81.4(4) 3_655 . ?
O2 Tb1 O2 135.75(17) 18_656 . ?
O2 Tb1 O2 81.4(4) 5_665 . ?
O2 Tb1 O2 81.4(4) 14_666 16_556 ?
O2 Tb1 O2 135.75(17) 3_655 16_556 ?
O2 Tb1 O2 81.4(4) 18_656 16_556 ?
O2 Tb1 O2 135.75(17) 5_665 16_556 ?
O2 Tb1 O2 82.3(5) . 16_556 ?
O2 Tb1 O3 67.88(8) 14_666 . ?
O2 Tb1 O3 67.88(8) 3_655 . ?
O2 Tb1 O3 67.88(8) 18_656 . ?
O2 Tb1 O3 67.88(8) 5_665 . ?
O2 Tb1 O3 138.9(2) . . ?
O2 Tb1 O3 138.9(2) 16_556 . ?
O2 Tb1 O3 67.88(8) 14_666 3_655 ?
O2 Tb1 O3 138.9(2) 3_655 3_655 ?
O2 Tb1 O3 138.9(2) 18_656 3_655 ?
O2 Tb1 O3 67.88(8) 5_665 3_655 ?
O2 Tb1 O3 67.88(8) . 3_655 ?
O2 Tb1 O3 67.88(8) 16_556 3_655 ?
O3 Tb1 O3 120.000(4) . 3_655 ?
O2 Tb1 O3 138.9(2) 14_666 14_666 ?
O2 Tb1 O3 67.88(8) 3_655 14_666 ?
O2 Tb1 O3 67.88(8) 18_656 14_666 ?
O2 Tb1 O3 138.9(2) 5_665 14_666 ?
O2 Tb1 O3 67.88(8) . 14_666 ?
O2 Tb1 O3 67.88(8) 16_556 14_666 ?
O3 Tb1 O3 120.000(3) . 14_666 ?
O3 Tb1 O3 120.000(2) 3_655 14_666 ?

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
N1 C2 C3 C4 45(2) . . . 5_565 ?
C1 C1 N1 C1 105.2(9) 24_565 . . 22_665 ?
C1 C1 N1 C2 -147.5(10) 24_565 . . 22_665 ?
C1 C1 N1 C2 -122.9(7) 24_565 . . . ?
C1 C1 N1 Co1 -12.2(7) 24_565 . . . ?
C3 C2 N1 C1 58.1(15) . . . . ?
C3 C2 N1 C1 173.3(12) . . . 22_665 ?
C3 C2 N1 C2 -149.8(12) . . . 22_665 ?
C3 C2 N1 Co1 -51.7(16) . . . . ?
O1 Co1 N1 C1 -164.0(7) 3_665 . . . ?
O1 Co1 N1 C1 -78.5(7) 5_565 . . . ?
N1 Co1 N1 C1 15.1(8) 3_665 . . . ?
N1 Co1 N1 C1 102.5(6) 5_565 . . . ?
O1 Co1 N1 C1 78.5(7) 3_665 . . 22_665 ?
O1 Co1 N1 C1 164.0(7) 5_565 . . 22_665 ?
N1 Co1 N1 C1 -102.5(6) 3_665 . . 22_665 ?
N1 Co1 N1 C1 -15.1(8) 5_565 . . 22_665 ?
O1 Co1 N1 C2 -19.4(8) 3_665 . . 22_665 ?
O1 Co1 N1 C2 66.1(8) 5_565 . . 22_665 ?
N1 Co1 N1 C2 159.6(7) 3_665 . . 22_665 ?
N1 Co1 N1 C2 -113.0(8) 5_565 . . 22_665 ?
O1 Co1 N1 C2 -66.1(8) 3_665 . . . ?
O1 Co1 N1 C2 19.4(8) 5_565 . . . ?
N1 Co1 N1 C2 113.0(8) 3_665 . . . ?
N1 Co1 N1 C2 -159.6(7) 5_565 . . . ?
O2 C4 O1 Co1 180.000(2) . . . . ?
C3 C4 O1 Co1 -54.0(8) 3_665 . . . ?
C3 C4 O1 Co1 54.0(8) 20 . . . ?
O1 Co1 O1 C4 -137.18(18) 3_665 . . . ?
O1 Co1 O1 C4 137.18(18) 5_565 . . . ?
N1 Co1 O1 C4 43.8(2) 3_665 . . . ?
N1 Co1 O1 C4 -43.8(2) 5_565 . . . ?
O5 Cl1 O4 O5 -120.000(1) 5_765 . . 3_645 ?
O5 Cl1 O4 O5 60.000(2) 17_545 . . 3_645 ?
O5 Cl1 O4 O5 -60.000(2) 13_755 . . 3_645 ?
O5 Cl1 O4 O5 180.0 15_665 . . 3_645 ?
O5 Cl1 O4 O5 120.000(2) . . . 3_645 ?
O5 Cl1 O4 O5 120.000(2) 5_765 . . . ?
O5 Cl1 O4 O5 -60.000(3) 17_545 . . . ?
O5 Cl1 O4 O5 180.000(2) 13_755 . . . ?
O5 Cl1 O4 O5 -120.000(2) 3_645 . . . ?
O5 Cl1 O4 O5 60.0 15_665 . . . ?
O5 Cl1 O4 O5 180.000(1) 17_545 . . 5_765 ?
O5 Cl1 O4 O5 60.0 13_755 . . 5_765 ?
O5 Cl1 O4 O5 120.0 3_645 . . 5_765 ?
O5 Cl1 O4 O5 -60.000(3) 15_665 . . 5_765 ?
O5 Cl1 O4 O5 -120.0 . . . 5_765 ?
O4 Cl1 O5 O5 62(7) 13_755 . . 17_545 ?
O4 Cl1 O5 O5 -118(7) . . . 17_545 ?
O5 Cl1 O5 O5 180.0 5_765 . . 17_545 ?
O5 Cl1 O5 O5 -57(13) 3_645 . . 17_545 ?
O5 Cl1 O5 O5 123(13) 15_665 . . 17_545 ?
O4 Cl1 O5 O5 -62(7) 13_755 . . 15_665 ?
O4 Cl1 O5 O5 118(7) . . . 15_665 ?
O5 Cl1 O5 O5 57(13) 5_765 . . 15_665 ?
O5 Cl1 O5 O5 -123(13) 17_545 . . 15_665 ?
O5 Cl1 O5 O5 180.0 3_645 . . 15_665 ?
O4 Cl1 O5 O4 180.000(2) 13_755 . . . ?
O5 Cl1 O5 O4 -62(7) 5_765 . . . ?
O5 Cl1 O5 O4 118(7) 17_545 . . . ?
O5 Cl1 O5 O4 62(7) 3_645 . . . ?
O5 Cl1 O5 O4 -118(7) 15_665 . . . ?
O5 O4 O5 Cl1 -44.6(18) 3_645 . . . ?
O5 O4 O5 Cl1 44.6(18) 5_765 . . . ?
Cl1 O4 O5 O5 46(6) . . . 17_545 ?
O5 O4 O5 O5 2(7) 3_645 . . 17_545 ?
O5 O4 O5 O5 91(4) 5_765 . . 17_545 ?
Cl1 O4 O5 O5 -46(6) . . . 15_665 ?
O5 O4 O5 O5 -91(4) 3_645 . . 15_665 ?
O5 O4 O5 O5 -2(7) 5_765 . . 15_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.921
_refine_diff_density_rms         0.195
####################################################################### 
# 
# 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_4_Ni
_database_code_depnum_ccdc_archive 'CCDC 2165412'
loop_
_audit_author_name
_audit_author_address
'Zhong Zhang'
;Guangxi Normal University
China
;
_audit_update_record             
;
2022-07-03 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H132 N12 Ni9 O42, 6(Cl O4), 10(H2 O)'
_chemical_formula_sum            'C60 H152 Cl6 N12 Ni9 O76'
_chemical_formula_weight         2999.03

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'
Cl Cl 0.1484 0.1585 '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           Monoclinic
_symmetry_space_group_name_H-M   'C2/m  '
_symmetry_space_group_name_Hall  '-C 2y '

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

_cell_length_a                   12.7937(5)
_cell_length_b                   28.8770(11)
_cell_length_c                   15.5362(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.944(4)
_cell_angle_gamma                90.00
_cell_volume                     5593.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    3832
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      28.39

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3116
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      294(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 Smart Apex CCD II'
_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            11567
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5613
_reflns_number_gt                4417
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_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)+(0.0900P)²+2.0000P] 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         5613
_refine_ls_number_parameters     392
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1499
_refine_ls_wR_factor_gt          0.1384
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.057
_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
C1 C 0.6284(4) 0.18886(17) 0.8082(3) 0.0441(11) Uani 1 1 d . . .
H1A H 0.6124 0.2159 0.8400 0.053 Uiso 1 1 calc R . .
H1B H 0.5670 0.1683 0.7994 0.053 Uiso 1 1 calc R . .
C2 C 0.6466(4) 0.20373(16) 0.7189(3) 0.0428(11) Uani 1 1 d . . .
H2A H 0.5785 0.2121 0.6806 0.051 Uiso 1 1 calc R . .
H2B H 0.6926 0.2308 0.7264 0.051 Uiso 1 1 calc R . .
C3 C 0.7891(4) 0.18357(16) 0.6425(3) 0.0431(11) Uani 1 1 d . . .
H3A H 0.7666 0.2108 0.6064 0.052 Uiso 1 1 calc R . .
H3B H 0.8115 0.1602 0.6055 0.052 Uiso 1 1 calc R . .
C4 C 0.8835(4) 0.19617(17) 0.7178(3) 0.0449(11) Uani 1 1 d . . .
H4A H 0.9471 0.2006 0.6946 0.054 Uiso 1 1 calc R . .
H4B H 0.8683 0.2251 0.7443 0.054 Uiso 1 1 calc R . .
C5 C 0.9198(4) 0.17864(16) 0.8771(3) 0.0440(11) Uani 1 1 d . . .
H5A H 0.9729 0.2031 0.8845 0.053 Uiso 1 1 calc R . .
H5B H 0.9464 0.1547 0.9203 0.053 Uiso 1 1 calc R . .
C6 C 0.8152(4) 0.19797(16) 0.8934(3) 0.0448(11) Uani 1 1 d . . .
H6A H 0.8230 0.2036 0.9561 0.054 Uiso 1 1 calc R . .
H6B H 0.7996 0.2273 0.8628 0.054 Uiso 1 1 calc R . .
C7 C 0.6913(4) 0.14075(16) 0.9357(3) 0.0408(10) Uani 1 1 d . . .
H7A H 0.6350 0.1188 0.9113 0.049 Uiso 1 1 calc R . .
H7B H 0.6612 0.1634 0.9695 0.049 Uiso 1 1 calc R . .
C8 C 0.7799(4) 0.11516(16) 0.9977(3) 0.0406(10) Uani 1 1 d . . .
H8A H 0.7498 0.1015 1.0439 0.049 Uiso 1 1 calc R . .
H8B H 0.8328 0.1377 1.0257 0.049 Uiso 1 1 calc R . .
C9 C 0.8381(3) 0.07717(15) 0.9594(3) 0.0315(9) Uani 1 1 d . . .
C10 C 0.6196(3) 0.14266(15) 0.6041(3) 0.0350(9) Uani 1 1 d . . .
H10A H 0.6568 0.1186 0.5793 0.042 Uiso 1 1 calc R . .
H10B H 0.5943 0.1652 0.5579 0.042 Uiso 1 1 calc R . .
C11 C 0.5231(3) 0.12122(15) 0.6304(3) 0.0382(10) Uani 1 1 d . . .
H11A H 0.4740 0.1105 0.5771 0.046 Uiso 1 1 calc R . .
H11B H 0.4866 0.1454 0.6556 0.046 Uiso 1 1 calc R . .
C12 C 0.5444(3) 0.08103(15) 0.6956(3) 0.0332(9) Uani 1 1 d . . .
C13 C 0.9987(3) 0.13006(18) 0.7806(3) 0.0459(11) Uani 1 1 d . . .
H13A H 1.0066 0.1058 0.8247 0.055 Uiso 1 1 calc R . .
H13B H 1.0625 0.1492 0.7950 0.055 Uiso 1 1 calc R . .
C14 C 0.9936(3) 0.10783(19) 0.6917(3) 0.0473(12) Uani 1 1 d . . .
H14A H 0.9897 0.1324 0.6486 0.057 Uiso 1 1 calc R . .
H14B H 1.0607 0.0916 0.6946 0.057 Uiso 1 1 calc R . .
C15 C 0.9034(3) 0.07434(15) 0.6568(3) 0.0364(10) Uani 1 1 d . . .
Cl1 Cl 1.0000 0.22631(7) 0.5000 0.0603(5) Uani 1 2 d S . .
Cl2 Cl 0.68356(10) 0.16583(5) 0.19111(9) 0.0573(4) Uani 1 1 d . . .
N1 N 0.7235(3) 0.16494(12) 0.8617(2) 0.0348(8) Uani 1 1 d . . .
N2 N 0.6975(3) 0.16568(12) 0.6765(2) 0.0325(8) Uani 1 1 d . . .
N3 N 0.9045(3) 0.15907(12) 0.7873(2) 0.0365(8) Uani 1 1 d . . .
Ni1 Ni 0.76776(4) 0.118967(17) 0.77392(3) 0.02645(16) Uani 1 1 d . . .
Ni2 Ni 1.0000 0.0000 1.0000 0.0258(2) Uani 1 4 d S . .
Ni3 Ni 0.45894(6) 0.0000 0.78022(5) 0.0351(2) Uani 1 2 d S . .
Ni4 Ni 0.80927(6) 0.0000 0.52591(5) 0.0346(2) Uani 1 2 d S . .
O1 O 0.8315(2) 0.07462(9) 0.87716(18) 0.0329(6) Uani 1 1 d . . .
O2 O 0.8920(2) 0.05021(11) 1.01446(19) 0.0420(7) Uani 1 1 d . . .
O3 O 0.6321(2) 0.07888(10) 0.75204(18) 0.0340(6) Uani 1 1 d . . .
O4 O 0.4708(2) 0.05184(11) 0.6914(2) 0.0431(8) Uani 1 1 d . . .
O5 O 0.8216(2) 0.07363(10) 0.69043(19) 0.0355(7) Uani 1 1 d . . .
O6 O 0.9129(2) 0.04946(11) 0.5929(2) 0.0407(7) Uani 1 1 d . . .
O7 O 1.0492(3) 0.0000 1.1381(2) 0.0305(8) Uani 1 2 d S . .
H7C H 1.1050 0.0163 1.1572 0.046 Uiso 0.50 1 d PR . .
H7D H 1.0622 -0.0271 1.1593 0.046 Uiso 0.50 1 d PR . .
O8 O 0.6217(3) 0.0000 0.8386(3) 0.0345(9) Uani 1 2 d S . .
H8C H 0.6512 0.0240 0.8227 0.052 Uiso 0.50 1 d PR . .
H8D H 0.6506 -0.0238 0.8217 0.052 Uiso 0.50 1 d PR . .
O9 O 0.2970(3) 0.0000 0.7271(3) 0.0552(13) Uani 1 2 d S . .
H9C H 0.2718 -0.0250 0.7431 0.083 Uiso 0.50 1 d PR . .
H9D H 0.2725 0.0221 0.7530 0.083 Uiso 0.50 1 d PR . .
O10 O 0.4431(3) -0.05001(11) 0.8726(2) 0.0528(9) Uani 1 1 d . . .
H10C H 0.3774 -0.0576 0.8634 0.079 Uiso 1 1 d R . .
H10D H 0.4527 -0.0344 0.9202 0.079 Uiso 1 1 d R . .
O11 O 0.7096(3) 0.0000 0.6144(3) 0.0382(10) Uani 1 2 d S . .
H11C H 0.7362 0.0197 0.6540 0.057 Uiso 0.50 1 d PR . .
H11D H 0.7107 -0.0265 0.6382 0.057 Uiso 0.50 1 d PR . .
O12 O 0.7139(3) 0.05002(12) 0.4555(2) 0.0522(8) Uani 1 1 d . . .
H12C H 0.7127 0.0731 0.4891 0.078 Uiso 1 1 d R . .
H12D H 0.7428 0.0588 0.4140 0.078 Uiso 1 1 d R . .
O13 O 0.8992(3) 0.0000 0.4280(3) 0.0437(11) Uani 1 2 d S . .
H13C H 0.8711 -0.0160 0.3828 0.066 Uiso 0.50 1 d PR . .
H13D H 0.9584 -0.0128 0.4518 0.066 Uiso 0.50 1 d PR . .
O14 O 0.9318(4) 0.25329(18) 0.5370(4) 0.1025(17) Uani 1 1 d . . .
O15 O 0.9528(9) 0.1983(4) 0.4381(6) 0.267(6) Uani 1 1 d U . .
O16 O 0.6548(4) 0.18729(17) 0.2634(3) 0.0919(15) Uani 1 1 d . . .
O17 O 0.7613(4) 0.19141(14) 0.1599(4) 0.0893(15) Uani 1 1 d . . .
O18 O 0.5925(4) 0.1581(3) 0.1224(4) 0.160(3) Uani 1 1 d DU . .
O19 O 0.7278(5) 0.12087(15) 0.2156(4) 0.1053(19) Uani 1 1 d . . .
O20 O 0.7815(5) 0.1353(2) 0.4284(4) 0.1110(19) Uani 1 1 d . . .
H20C H 0.8368 0.1229 0.4163 0.166 Uiso 1 1 d R . .
H20D H 0.7596 0.1534 0.3850 0.166 Uiso 1 1 d R . .
O21 O 1.0000 0.2651(6) 0.0000 0.301(19) Uani 0.50 2 d SPU . .
H21C H 0.9593 0.2422 0.0025 0.451 Uiso 0.25 1 d PR . .
H21D H 1.0048 0.2781 0.0499 0.451 Uiso 0.25 1 d PR . .
O22 O 0.6629(4) 0.0000 0.0192(3) 0.0593(14) Uani 1 2 d S . .
H22C H 0.7304 0.0000 0.0242 0.089 Uiso 1 2 d SRD . .
H22D H 0.6387 0.0100 -0.0329 0.089 Uiso 0.50 1 d PR . .
O23 O 0.1425(6) 0.0214(3) 0.8124(5) 0.094(3) Uani 0.50 1 d P . .
H23C H 0.1757 0.0000 0.8454 0.141 Uiso 1 2 d SR . .
H23D H 0.1903 0.0402 0.8038 0.141 Uiso 0.50 1 d PR . .
O24 O 0.5000 0.0233(5) 0.5000 0.105(5) Uani 0.50 2 d SP . .
H24C H 0.4782 0.0127 0.4480 0.158 Uiso 0.25 1 d PR . .
H24D H 0.5019 0.0000 0.5332 0.158 Uiso 0.50 2 d SPR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.482(6) . ?
C1 C2 1.518(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.502(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.482(5) . ?
C3 C4 1.526(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N3 1.501(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N3 1.478(6) . ?
C5 C6 1.522(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.507(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.481(6) . ?
C7 C8 1.506(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.521(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O2 1.245(5) . ?
C9 O1 1.263(5) . ?
C10 N2 1.484(5) . ?
C10 C11 1.517(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.524(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O4 1.255(5) . ?
C12 O3 1.262(5) . ?
C13 N3 1.490(6) . ?
C13 C14 1.512(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.510(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O6 1.253(5) . ?
C15 O5 1.270(5) . ?
Cl1 O15 1.298(7) . ?
Cl1 O15 1.298(7) 2_756 ?
Cl1 O14 1.387(5) 2_756 ?
Cl1 O14 1.387(5) . ?
Cl2 O16 1.402(4) . ?
Cl2 O17 1.409(4) . ?
Cl2 O18 1.410(5) . ?
Cl2 O19 1.434(5) . ?
N1 Ni1 2.070(3) . ?
N2 Ni1 2.075(3) . ?
N3 Ni1 2.070(3) . ?
Ni1 O3 2.050(3) . ?
Ni1 O5 2.067(3) . ?
Ni1 O1 2.072(3) . ?
Ni2 O2 2.050(3) 2_757 ?
Ni2 O2 2.050(3) . ?
Ni2 O2 2.050(3) 6 ?
Ni2 O2 2.050(3) 5_757 ?
Ni2 O7 2.096(4) 5_757 ?
Ni2 O7 2.096(4) . ?
Ni3 O9 2.051(5) . ?
Ni3 O4 2.064(3) . ?
Ni3 O4 2.064(3) 6 ?
Ni3 O8 2.077(4) . ?
Ni3 O10 2.078(3) 6 ?
Ni3 O10 2.078(3) . ?
Ni4 O12 2.043(3) . ?
Ni4 O12 2.043(3) 6 ?
Ni4 O6 2.064(3) . ?
Ni4 O6 2.064(3) 6 ?
Ni4 O11 2.074(4) . ?
Ni4 O13 2.103(4) . ?
O7 H7C 0.8502 . ?
O7 H7D 0.8501 . ?
O8 H8C 0.8500 . ?
O8 H8D 0.8500 . ?
O9 H9C 0.8498 . ?
O9 H9D 0.8501 . ?
O10 H10C 0.8497 . ?
O10 H10D 0.8502 . ?
O11 H11C 0.8501 . ?
O11 H11D 0.8498 . ?
O12 H12C 0.8502 . ?
O12 H12D 0.8501 . ?
O13 H13C 0.8500 . ?
O13 H13D 0.8498 . ?
O20 H20C 0.8501 . ?
O20 H20D 0.8498 . ?
O21 H21C 0.8497 . ?
O21 H21D 0.8501 . ?
O22 H22C 0.8496 . ?
O22 H22D 0.8501 . ?
O23 O23 1.238(19) 6 ?
O23 H23C 0.8530 . ?
O23 H23D 0.8497 . ?
O24 O24 1.35(3) 5_656 ?
O24 H24C 0.8502 . ?
O24 H24D 0.8454 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.7(4) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C1 111.3(3) . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 111.3(4) . . ?
N2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N3 C4 C3 111.4(3) . . ?
N3 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N3 C5 C6 111.3(4) . . ?
N3 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N3 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N1 C6 C5 111.2(3) . . ?
N1 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N1 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N1 C7 C8 115.3(4) . . ?
N1 C7 H7A 108.4 . . ?
C8 C7 H7A 108.4 . . ?
N1 C7 H7B 108.4 . . ?
C8 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 C9 117.9(4) . . ?
C7 C8 H8A 107.8 . . ?
C9 C8 H8A 107.8 . . ?
C7 C8 H8B 107.8 . . ?
C9 C8 H8B 107.8 . . ?
H8A C8 H8B 107.2 . . ?
O2 C9 O1 124.1(4) . . ?
O2 C9 C8 115.2(4) . . ?
O1 C9 C8 120.7(4) . . ?
N2 C10 C11 115.3(3) . . ?
N2 C10 H10A 108.4 . . ?
C11 C10 H10A 108.4 . . ?
N2 C10 H10B 108.4 . . ?
C11 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
C10 C11 C12 117.0(3) . . ?
C10 C11 H11A 108.0 . . ?
C12 C11 H11A 108.0 . . ?
C10 C11 H11B 108.0 . . ?
C12 C11 H11B 108.0 . . ?
H11A C11 H11B 107.3 . . ?
O4 C12 O3 122.9(4) . . ?
O4 C12 C11 117.2(4) . . ?
O3 C12 C11 119.9(4) . . ?
N3 C13 C14 115.6(4) . . ?
N3 C13 H13A 108.4 . . ?
C14 C13 H13A 108.4 . . ?
N3 C13 H13B 108.4 . . ?
C14 C13 H13B 108.4 . . ?
H13A C13 H13B 107.4 . . ?
C15 C14 C13 118.3(4) . . ?
C15 C14 H14A 107.7 . . ?
C13 C14 H14A 107.7 . . ?
C15 C14 H14B 107.7 . . ?
C13 C14 H14B 107.7 . . ?
H14A C14 H14B 107.1 . . ?
O6 C15 O5 123.5(4) . . ?
O6 C15 C14 116.8(4) . . ?
O5 C15 C14 119.7(4) . . ?
O15 Cl1 O15 102.9(12) . 2_756 ?
O15 Cl1 O14 105.9(4) . 2_756 ?
O15 Cl1 O14 115.2(6) 2_756 2_756 ?
O15 Cl1 O14 115.2(6) . . ?
O15 Cl1 O14 105.9(4) 2_756 . ?
O14 Cl1 O14 111.6(4) 2_756 . ?
O16 Cl2 O17 112.1(3) . . ?
O16 Cl2 O18 110.8(3) . . ?
O17 Cl2 O18 110.5(4) . . ?
O16 Cl2 O19 110.3(3) . . ?
O17 Cl2 O19 107.4(3) . . ?
O18 Cl2 O19 105.6(5) . . ?
C7 N1 C1 108.6(3) . . ?
C7 N1 C6 112.1(4) . . ?
C1 N1 C6 111.7(4) . . ?
C7 N1 Ni1 111.9(3) . . ?
C1 N1 Ni1 103.9(3) . . ?
C6 N1 Ni1 108.3(3) . . ?
C3 N2 C10 109.6(3) . . ?
C3 N2 C2 110.9(3) . . ?
C10 N2 C2 112.1(3) . . ?
C3 N2 Ni1 103.8(3) . . ?
C10 N2 Ni1 111.7(2) . . ?
C2 N2 Ni1 108.4(2) . . ?
C5 N3 C13 110.0(3) . . ?
C5 N3 C4 111.7(4) . . ?
C13 N3 C4 111.7(4) . . ?
C5 N3 Ni1 103.8(3) . . ?
C13 N3 Ni1 110.9(3) . . ?
C4 N3 Ni1 108.4(3) . . ?
O3 Ni1 O5 85.82(11) . . ?
O3 Ni1 N3 176.24(13) . . ?
O5 Ni1 N3 91.37(13) . . ?
O3 Ni1 N1 97.18(13) . . ?
O5 Ni1 N1 176.48(13) . . ?
N3 Ni1 N1 85.70(14) . . ?
O3 Ni1 O1 87.19(11) . . ?
O5 Ni1 O1 88.03(11) . . ?
N3 Ni1 O1 95.23(13) . . ?
N1 Ni1 O1 90.28(12) . . ?
O3 Ni1 N2 91.94(12) . . ?
O5 Ni1 N2 96.03(12) . . ?
N3 Ni1 N2 85.85(13) . . ?
N1 Ni1 N2 85.73(13) . . ?
O1 Ni1 N2 175.77(12) . . ?
O2 Ni2 O2 89.98(18) 2_757 . ?
O2 Ni2 O2 180.00(12) 2_757 6 ?
O2 Ni2 O2 90.02(18) . 6 ?
O2 Ni2 O2 90.02(18) 2_757 5_757 ?
O2 Ni2 O2 180.00(16) . 5_757 ?
O2 Ni2 O2 89.98(18) 6 5_757 ?
O2 Ni2 O7 86.74(11) 2_757 5_757 ?
O2 Ni2 O7 93.26(11) . 5_757 ?
O2 Ni2 O7 93.26(11) 6 5_757 ?
O2 Ni2 O7 86.74(11) 5_757 5_757 ?
O2 Ni2 O7 93.26(11) 2_757 . ?
O2 Ni2 O7 86.74(11) . . ?
O2 Ni2 O7 86.74(11) 6 . ?
O2 Ni2 O7 93.26(11) 5_757 . ?
O7 Ni2 O7 180.000(1) 5_757 . ?
O9 Ni3 O4 87.11(12) . . ?
O9 Ni3 O4 87.11(12) . 6 ?
O4 Ni3 O4 92.99(19) . 6 ?
O9 Ni3 O8 177.91(17) . . ?
O4 Ni3 O8 94.32(11) . . ?
O4 Ni3 O8 94.32(11) 6 . ?
O9 Ni3 O10 91.83(14) . 6 ?
O4 Ni3 O10 89.48(13) . 6 ?
O4 Ni3 O10 177.27(13) 6 6 ?
O8 Ni3 O10 86.67(13) . 6 ?
O9 Ni3 O10 91.83(14) . . ?
O4 Ni3 O10 177.27(14) . . ?
O4 Ni3 O10 89.48(13) 6 . ?
O8 Ni3 O10 86.67(13) . . ?
O10 Ni3 O10 88.04(19) 6 . ?
O12 Ni4 O12 89.97(19) . 6 ?
O12 Ni4 O6 91.14(13) . . ?
O12 Ni4 O6 176.44(13) 6 . ?
O12 Ni4 O6 176.44(13) . 6 ?
O12 Ni4 O6 91.14(13) 6 6 ?
O6 Ni4 O6 87.56(18) . 6 ?
O12 Ni4 O11 88.45(13) . . ?
O12 Ni4 O11 88.45(13) 6 . ?
O6 Ni4 O11 94.96(11) . . ?
O6 Ni4 O11 94.96(11) 6 . ?
O12 Ni4 O13 88.30(13) . . ?
O12 Ni4 O13 88.30(13) 6 . ?
O6 Ni4 O13 88.35(12) . . ?
O6 Ni4 O13 88.35(12) 6 . ?
O11 Ni4 O13 175.41(16) . . ?
C9 O1 Ni1 132.3(3) . . ?
C9 O2 Ni2 130.5(3) . . ?
C12 O3 Ni1 132.5(3) . . ?
C12 O4 Ni3 128.3(3) . . ?
C15 O5 Ni1 132.0(3) . . ?
C15 O6 Ni4 129.1(3) . . ?
Ni2 O7 H7C 113.2 . . ?
Ni2 O7 H7D 112.7 . . ?
H7C O7 H7D 107.2 . . ?
Ni3 O8 H8C 109.8 . . ?
Ni3 O8 H8D 109.2 . . ?
H8C O8 H8D 108.5 . . ?
Ni3 O9 H9C 107.3 . . ?
Ni3 O9 H9D 104.8 . . ?
H9C O9 H9D 107.0 . . ?
Ni3 O10 H10C 108.0 . . ?
Ni3 O10 H10D 102.4 . . ?
H10C O10 H10D 103.2 . . ?
Ni4 O11 H11C 105.9 . . ?
Ni4 O11 H11D 109.6 . . ?
H11C O11 H11D 108.8 . . ?
Ni4 O12 H12C 108.5 . . ?
Ni4 O12 H12D 107.9 . . ?
H12C O12 H12D 107.6 . . ?
Ni4 O13 H13C 113.5 . . ?
Ni4 O13 H13D 105.3 . . ?
H13C O13 H13D 107.0 . . ?
H20C O20 H20D 103.0 . . ?
H21C O21 H21D 102.9 . . ?
H22C O22 H22D 103.4 . . ?
H23C O23 H23D 106.1 . . ?
H24C O24 H24D 104.6 . . ?

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
N1 C1 C2 N2 45.0(5) . . . . ?
N2 C3 C4 N3 45.5(5) . . . . ?
N3 C5 C6 N1 45.3(5) . . . . ?
N1 C7 C8 C9 -59.1(6) . . . . ?
C7 C8 C9 O2 -164.0(4) . . . . ?
C7 C8 C9 O1 16.9(6) . . . . ?
N2 C10 C11 C12 -64.5(5) . . . . ?
C10 C11 C12 O4 -152.0(4) . . . . ?
C10 C11 C12 O3 29.8(6) . . . . ?
N3 C13 C14 C15 -61.1(6) . . . . ?
C13 C14 C15 O6 -165.8(4) . . . . ?
C13 C14 C15 O5 16.6(7) . . . . ?
C8 C7 N1 C1 -179.0(4) . . . . ?
C8 C7 N1 C6 -55.1(5) . . . . ?
C8 C7 N1 Ni1 66.8(4) . . . . ?
C2 C1 N1 C7 -165.1(4) . . . . ?
C2 C1 N1 C6 70.8(5) . . . . ?
C2 C1 N1 Ni1 -45.7(4) . . . . ?
C5 C6 N1 C7 105.3(4) . . . . ?
C5 C6 N1 C1 -132.5(4) . . . . ?
C5 C6 N1 Ni1 -18.7(4) . . . . ?
C4 C3 N2 C10 -165.3(4) . . . . ?
C4 C3 N2 C2 70.3(4) . . . . ?
C4 C3 N2 Ni1 -45.9(4) . . . . ?
C11 C10 N2 C3 178.1(4) . . . . ?
C11 C10 N2 C2 -58.3(5) . . . . ?
C11 C10 N2 Ni1 63.6(4) . . . . ?
C1 C2 N2 C3 -132.7(4) . . . . ?
C1 C2 N2 C10 104.4(4) . . . . ?
C1 C2 N2 Ni1 -19.3(4) . . . . ?
C6 C5 N3 C13 -165.6(4) . . . . ?
C6 C5 N3 C4 69.8(5) . . . . ?
C6 C5 N3 Ni1 -46.8(4) . . . . ?
C14 C13 N3 C5 -180.0(4) . . . . ?
C14 C13 N3 C4 -55.3(5) . . . . ?
C14 C13 N3 Ni1 65.7(5) . . . . ?
C3 C4 N3 C5 -133.5(4) . . . . ?
C3 C4 N3 C13 102.8(4) . . . . ?
C3 C4 N3 Ni1 -19.7(5) . . . . ?
C5 N3 Ni1 O5 -149.6(3) . . . . ?
C13 N3 Ni1 O5 -31.4(3) . . . . ?
C4 N3 Ni1 O5 91.5(3) . . . . ?
C5 N3 Ni1 N1 28.4(3) . . . . ?
C13 N3 Ni1 N1 146.6(3) . . . . ?
C4 N3 Ni1 N1 -90.5(3) . . . . ?
C5 N3 Ni1 O1 -61.4(3) . . . . ?
C13 N3 Ni1 O1 56.7(3) . . . . ?
C4 N3 Ni1 O1 179.7(3) . . . . ?
C5 N3 Ni1 N2 114.5(3) . . . . ?
C13 N3 Ni1 N2 -127.4(3) . . . . ?
C4 N3 Ni1 N2 -4.4(3) . . . . ?
C7 N1 Ni1 O3 52.8(3) . . . . ?
C1 N1 Ni1 O3 -64.3(3) . . . . ?
C6 N1 Ni1 O3 176.8(3) . . . . ?
C7 N1 Ni1 N3 -129.7(3) . . . . ?
C1 N1 Ni1 N3 113.3(3) . . . . ?
C6 N1 Ni1 N3 -5.6(3) . . . . ?
C7 N1 Ni1 O1 -34.4(3) . . . . ?
C1 N1 Ni1 O1 -151.5(3) . . . . ?
C6 N1 Ni1 O1 89.6(3) . . . . ?
C7 N1 Ni1 N2 144.2(3) . . . . ?
C1 N1 Ni1 N2 27.2(3) . . . . ?
C6 N1 Ni1 N2 -91.7(3) . . . . ?
C3 N2 Ni1 O3 -149.6(3) . . . . ?
C10 N2 Ni1 O3 -31.6(3) . . . . ?
C2 N2 Ni1 O3 92.5(3) . . . . ?
C3 N2 Ni1 O5 -63.6(3) . . . . ?
C10 N2 Ni1 O5 54.4(3) . . . . ?
C2 N2 Ni1 O5 178.5(3) . . . . ?
C3 N2 Ni1 N3 27.4(3) . . . . ?
C10 N2 Ni1 N3 145.4(3) . . . . ?
C2 N2 Ni1 N3 -90.6(3) . . . . ?
C3 N2 Ni1 N1 113.4(3) . . . . ?
C10 N2 Ni1 N1 -128.6(3) . . . . ?
C2 N2 Ni1 N1 -4.6(3) . . . . ?
O2 C9 O1 Ni1 -169.9(3) . . . . ?
C8 C9 O1 Ni1 9.2(6) . . . . ?
O3 Ni1 O1 C9 -97.5(4) . . . . ?
O5 Ni1 O1 C9 176.6(4) . . . . ?
N3 Ni1 O1 C9 85.4(4) . . . . ?
N1 Ni1 O1 C9 -0.3(4) . . . . ?
O1 C9 O2 Ni2 8.8(6) . . . . ?
C8 C9 O2 Ni2 -170.3(3) . . . . ?
O2 Ni2 O2 C9 72.0(4) 2_757 . . . ?
O2 Ni2 O2 C9 -108.0(4) 6 . . . ?
O7 Ni2 O2 C9 -14.7(4) 5_757 . . . ?
O7 Ni2 O2 C9 165.3(4) . . . . ?
O4 C12 O3 Ni1 177.9(3) . . . . ?
C11 C12 O3 Ni1 -4.0(6) . . . . ?
O5 Ni1 O3 C12 -91.1(4) . . . . ?
N1 Ni1 O3 C12 90.8(4) . . . . ?
O1 Ni1 O3 C12 -179.3(4) . . . . ?
N2 Ni1 O3 C12 4.8(4) . . . . ?
O3 C12 O4 Ni3 9.6(6) . . . . ?
C11 C12 O4 Ni3 -168.5(3) . . . . ?
O9 Ni3 O4 C12 158.7(4) . . . . ?
O4 Ni3 O4 C12 -114.3(3) 6 . . . ?
O8 Ni3 O4 C12 -19.7(4) . . . . ?
O10 Ni3 O4 C12 66.9(4) 6 . . . ?
O6 C15 O5 Ni1 -164.1(3) . . . . ?
C14 C15 O5 Ni1 13.4(6) . . . . ?
O3 Ni1 O5 C15 172.3(4) . . . . ?
N3 Ni1 O5 C15 -5.2(4) . . . . ?
O1 Ni1 O5 C15 -100.4(4) . . . . ?
N2 Ni1 O5 C15 80.8(4) . . . . ?
O5 C15 O6 Ni4 -2.2(6) . . . . ?
C14 C15 O6 Ni4 -179.8(3) . . . . ?
O12 Ni4 O6 C15 79.2(4) . . . . ?
O6 Ni4 O6 C15 -104.1(4) 6 . . . ?
O11 Ni4 O6 C15 -9.4(4) . . . . ?
O13 Ni4 O6 C15 167.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.091
