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#$Date: 2024-07-05 19:26:22 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293070 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/63/7716322.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716322
loop_
_publ_author_name
'Kim, Dongwon'
'Kim, Gyeongmin'
'Kim, Gyeongwoo'
'Park, Junmyeong'
'Han, Jihun'
'Hossain, Mohammad Mozammal'
'Jung, Ok-Sang'
'Lee, Young-A'
_publ_section_title
;
 M(II) effect on encapsulation of guests into a series of
 M₃L₂ chiral cages: enantio-recognition.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10704
_journal_page_last               10711
_journal_paper_doi               10.1039/d4dt01198h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C111 H104 N12 Ni3 O31, 6(ClO4), 6(C4H10O)'
_chemical_formula_sum            'C135 H174 Cl6 N12 Ni3 O61'
_chemical_formula_weight         3329.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2024-03-02 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.225(5)
_cell_length_b                   24.677(5)
_cell_length_c                   14.453(3)
_cell_measurement_reflns_used    199445
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_cell_volume                     8283(3)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57407
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.388
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             3484
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 6314 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         15250
_refine_ls_number_restraints     1353
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1768P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2253
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14569
_reflns_number_total             15250
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01198h2.cif
_cod_data_source_block           sr-Ni3L2_R-BuOH
_cod_depositor_comments
'Adding full bibliography for 7716315--7716324.cif.'
_cod_database_code               7716322
_shelx_shelxl_version_number     2019/2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.885
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.500000 0.500000 0.94481(6) 0.0489(2) Uani 1 2 d S T P . .
N2 N 0.2757(2) 0.61430(16) 0.6480(3) 0.0470(9) Uani 1 1 d . U . . .
H2 H 0.260737 0.593374 0.691049 0.056 Uiso 1 1 calc R U . . .
C2 C 0.3305(3) 0.5623(2) 0.9895(4) 0.0551(12) Uani 1 1 d . U . . .
H2A H 0.299895 0.553627 1.030410 0.066 Uiso 1 1 calc R U . . .
C1 C 0.3815(3) 0.5372(2) 0.9976(4) 0.0543(12) Uani 1 1 d . U . . .
H1 H 0.385833 0.510963 1.045242 0.065 Uiso 1 1 calc R U . . .
N3 N 0.4052(2) 0.64346(19) 0.3352(3) 0.0543(10) Uani 1 1 d . U . . .
C3 C 0.3228(3) 0.6009(2) 0.9216(4) 0.0531(11) Uani 1 1 d . U . . .
H3 H 0.287125 0.619357 0.915037 0.064 Uiso 1 1 calc R U . . .
N4 N 0.3020(2) 0.42969(15) 0.3555(3) 0.0464(9) Uani 1 1 d . U . . .
H4 H 0.280366 0.458744 0.361417 0.056 Uiso 1 1 calc R U . . .
C4 C 0.3689(2) 0.6119(2) 0.8629(3) 0.0457(10) Uani 1 1 d . U . . .
N5 N 0.3105(2) 0.37308(16) 0.7781(3) 0.0491(10) Uani 1 1 d . U . . .
H5 H 0.294885 0.357786 0.729142 0.059 Uiso 1 1 calc R U . . .
C5 C 0.4205(3) 0.5846(2) 0.8739(4) 0.0500(11) Uani 1 1 d . U . . .
H5A H 0.451643 0.592241 0.833418 0.060 Uiso 1 1 calc R U . . .
N6 N 0.4673(2) 0.2899(2) 0.5039(3) 0.0556(10) Uani 1 1 d . U . . .
C6 C 0.3653(2) 0.6492(2) 0.7824(4) 0.0497(11) Uani 1 1 d . U . . .
C8 C 0.3005(3) 0.70849(19) 0.7022(4) 0.0521(11) Uani 1 1 d . U . . .
H8 H 0.334596 0.720477 0.665216 0.062 Uiso 1 1 calc R U . . .
C9 C 0.2621(3) 0.7560(2) 0.7327(4) 0.0575(13) Uani 1 1 d . U . . .
H9A H 0.274644 0.770648 0.793194 0.069 Uiso 1 1 calc R U . . .
H9B H 0.262460 0.785500 0.686293 0.069 Uiso 1 1 calc R U . . .
O10 O 0.33764(18) 0.61959(13) 0.5280(3) 0.0530(9) Uani 1 1 d . U . . .
O11 O 0.4207(2) 0.4799(2) 0.2806(4) 0.0691(11) Uani 1 1 d . U . . .
O12 O 0.3369(2) 0.48104(15) 0.1993(2) 0.0558(9) Uani 1 1 d . U . . .
O13 O 0.3710(2) 0.37777(15) 0.4192(3) 0.0578(9) Uani 1 1 d . U . . .
O14 O 0.4492(2) 0.3386(2) 0.7789(3) 0.0687(11) Uani 1 1 d . U . . .
O15 O 0.3743(2) 0.28104(15) 0.7952(3) 0.0600(10) Uani 1 1 d . U . . .
O16 O 0.3588(2) 0.44483(16) 0.8360(3) 0.0685(13) Uani 1 1 d . U . . .
C1B C 0.500000 0.500000 0.7010(7) 0.071(2) Uani 1 2 d DS TU P . .
C2B C 0.5140(7) 0.5564(7) 0.6738(11) 0.150(6) Uani 1 1 d . U . . .
H2BA H 0.549023 0.556521 0.635864 0.225 Uiso 1 1 calc R U . . .
H2BB H 0.520337 0.578325 0.729404 0.225 Uiso 1 1 calc R U . . .
H2BC H 0.482034 0.571654 0.638069 0.225 Uiso 1 1 calc R U . . .
N1 N 0.42717(19) 0.54722(16) 0.9413(3) 0.0475(9) Uani 1 1 d . U . . .
Ni2 Ni 0.46733(3) 0.67910(3) 0.41941(5) 0.0531(2) Uani 1 1 d . . . . .
C7 C 0.2592(3) 0.6717(2) 0.6465(3) 0.0511(11) Uani 1 1 d . U . . .
H7 H 0.257888 0.684458 0.580916 0.061 Uiso 1 1 calc R U . . .
O8 O 0.39952(19) 0.65064(17) 0.7206(3) 0.0614(10) Uani 1 1 d . U . . .
O9 O 0.31645(17) 0.67971(14) 0.7857(2) 0.0503(8) Uani 1 1 d . U . . .
C10 C 0.2041(3) 0.7308(2) 0.7396(4) 0.0545(12) Uani 1 1 d . U . . .
C11 C 0.2013(3) 0.6817(2) 0.6913(4) 0.0548(12) Uani 1 1 d . U . . .
C12 C 0.1525(3) 0.6508(3) 0.6879(6) 0.0771(19) Uani 1 1 d . U . . .
H12 H 0.152257 0.617084 0.656148 0.093 Uiso 1 1 calc R U . . .
C13 C 0.1032(4) 0.6699(4) 0.7323(9) 0.102(3) Uani 1 1 d . U . . .
H13 H 0.068324 0.649805 0.729347 0.123 Uiso 1 1 calc R U . . .
C14 C 0.1055(4) 0.7192(4) 0.7816(6) 0.086(2) Uani 1 1 d . U . . .
H14 H 0.072195 0.731397 0.813606 0.103 Uiso 1 1 calc R U . . .
C15 C 0.1534(3) 0.7491(3) 0.7841(4) 0.0653(15) Uani 1 1 d . U . . .
H15 H 0.153407 0.782725 0.816036 0.078 Uiso 1 1 calc R U . . .
C16 C 0.3116(2) 0.59246(19) 0.5881(3) 0.0434(9) Uani 1 1 d . U . . .
C17 C 0.3582(3) 0.6689(2) 0.3061(4) 0.0604(13) Uani 1 1 d . U . . .
H17 H 0.354728 0.706539 0.319076 0.072 Uiso 1 1 calc R U . . .
C18 C 0.3139(3) 0.6442(3) 0.2581(4) 0.0644(14) Uani 1 1 d . U . . .
H18 H 0.280653 0.663877 0.239858 0.077 Uiso 1 1 calc R U . . .
C19 C 0.3197(3) 0.5902(3) 0.2377(4) 0.0609(13) Uani 1 1 d . U . . .
H19 H 0.290121 0.571719 0.204990 0.073 Uiso 1 1 calc R U . . .
C20 C 0.3687(3) 0.5630(2) 0.2651(3) 0.0534(12) Uani 1 1 d . U . . .
C21 C 0.4095(3) 0.5917(2) 0.3127(4) 0.0545(12) Uani 1 1 d . U . . .
H21 H 0.443445 0.572983 0.331023 0.065 Uiso 1 1 calc R U . . .
C22 C 0.3793(3) 0.5038(2) 0.2498(3) 0.0540(12) Uani 1 1 d . U . . .
C23 C 0.2997(3) 0.3987(2) 0.2695(3) 0.0521(11) Uani 1 1 d . U . . .
H23 H 0.311639 0.360497 0.282495 0.063 Uiso 1 1 calc R U . . .
C24 C 0.3392(3) 0.4223(2) 0.1927(4) 0.0559(13) Uani 1 1 d . U . . .
H24 H 0.379426 0.407937 0.196170 0.067 Uiso 1 1 calc R U . . .
C25 C 0.3092(4) 0.4073(3) 0.1025(4) 0.0670(16) Uani 1 1 d . U . . .
H25A H 0.314567 0.436091 0.055502 0.080 Uiso 1 1 calc R U . . .
H25B H 0.324327 0.372765 0.077687 0.080 Uiso 1 1 calc R U . . .
C26 C 0.2481(4) 0.4021(2) 0.1282(4) 0.0675(15) Uani 1 1 d . U . . .
C27 C 0.2419(3) 0.3981(2) 0.2245(4) 0.0607(13) Uani 1 1 d . U . . .
C28 C 0.1874(4) 0.3932(3) 0.2665(7) 0.084(2) Uani 1 1 d . U . . .
H28 H 0.184630 0.390776 0.331938 0.101 Uiso 1 1 calc R U . . .
C29 C 0.1386(5) 0.3918(5) 0.2140(9) 0.110(3) Uani 1 1 d . U . . .
H29 H 0.101719 0.388445 0.241947 0.132 Uiso 1 1 calc R U . . .
C30 C 0.1447(5) 0.3956(5) 0.1152(9) 0.108(3) Uani 1 1 d . U . . .
H30 H 0.111340 0.395582 0.077010 0.130 Uiso 1 1 calc R U . . .
C31 C 0.2008(4) 0.3995(4) 0.0737(7) 0.096(3) Uani 1 1 d . U . . .
H31 H 0.204714 0.400219 0.008243 0.116 Uiso 1 1 calc R U . . .
C32 C 0.3356(2) 0.41528(18) 0.4242(3) 0.0444(10) Uani 1 1 d . U . . .
C33 C 0.4240(3) 0.2630(3) 0.4663(4) 0.0614(13) Uani 1 1 d . U . . .
H33 H 0.425347 0.255240 0.401919 0.074 Uiso 1 1 calc R U . . .
C34 C 0.3775(3) 0.2458(3) 0.5160(5) 0.0664(15) Uani 1 1 d . U . . .
H34 H 0.347536 0.226219 0.486308 0.080 Uiso 1 1 calc R U . . .
C35 C 0.3739(3) 0.2568(3) 0.6092(5) 0.0642(14) Uani 1 1 d . U . . .
H35 H 0.342060 0.244895 0.645054 0.077 Uiso 1 1 calc R U . . .
C36 C 0.4187(3) 0.2860(2) 0.6489(4) 0.0569(12) Uani 1 1 d . U . . .
C37 C 0.4649(3) 0.3016(2) 0.5944(4) 0.0540(11) Uani 1 1 d . U . . .
H37 H 0.495677 0.321128 0.621909 0.065 Uiso 1 1 calc R U . . .
C38 C 0.4164(3) 0.3046(2) 0.7469(4) 0.0590(13) Uani 1 1 d . U . . .
C39 C 0.3092(3) 0.3447(2) 0.8659(3) 0.0572(13) Uani 1 1 d . U . . .
H39 H 0.309760 0.372402 0.916389 0.069 Uiso 1 1 calc R U . . .
C40 C 0.3605(3) 0.3051(2) 0.8818(4) 0.0647(15) Uani 1 1 d . U . . .
H40 H 0.394344 0.323087 0.911612 0.078 Uiso 1 1 calc R U . . .
C41 C 0.3327(5) 0.2604(3) 0.9443(5) 0.084(2) Uani 1 1 d . U . . .
H41A H 0.348214 0.224268 0.928185 0.101 Uiso 1 1 calc R U . . .
H41B H 0.340994 0.267682 1.010391 0.101 Uiso 1 1 calc R U . . .
C1C C 0.1776(6) 0.5396(7) 0.4076(16) 0.161(6) Uani 1 1 d . U . . .
H1C H 0.142212 0.528796 0.372828 0.193 Uiso 1 1 calc R U . . .
O1C O 0.2207(3) 0.5182(3) 0.3599(6) 0.103(2) Uani 1 1 d . U . . .
H1C1 H 0.218809 0.528646 0.304683 0.154 Uiso 1 1 calc R U . . .
C2C C 0.1661(11) 0.5222(9) 0.5072(17) 0.187(7) Uani 1 1 d . U . . .
H2C1 H 0.194549 0.539520 0.548840 0.224 Uiso 1 1 calc R U . . .
H2C2 H 0.127211 0.534346 0.526095 0.224 Uiso 1 1 calc R U . . .
C3C C 0.1701(9) 0.4637(8) 0.5156(19) 0.197(8) Uani 1 1 d . U . . .
H3C1 H 0.134716 0.449673 0.543639 0.296 Uiso 1 1 calc R U . . .
H3C2 H 0.203103 0.454334 0.554622 0.296 Uiso 1 1 calc R U . . .
H3C3 H 0.175152 0.447728 0.454044 0.296 Uiso 1 1 calc R U . . .
C4C C 0.1787(8) 0.6063(7) 0.4021(16) 0.169(7) Uani 1 1 d . U . . .
H4C1 H 0.215089 0.619757 0.427756 0.254 Uiso 1 1 calc R U . . .
H4C2 H 0.146486 0.621034 0.437892 0.254 Uiso 1 1 calc R U . . .
H4C3 H 0.175276 0.617804 0.337444 0.254 Uiso 1 1 calc R U . . .
C42 C 0.2701(4) 0.2627(3) 0.9267(4) 0.0760(19) Uani 1 1 d . U . . .
C43 C 0.2553(4) 0.3094(3) 0.8789(4) 0.0661(15) Uani 1 1 d . U . . .
C44 C 0.1990(4) 0.3191(3) 0.8537(5) 0.0756(18) Uani 1 1 d . U . . .
H44 H 0.188800 0.351034 0.820968 0.091 Uiso 1 1 calc R U . . .
C45 C 0.1585(5) 0.2816(4) 0.8771(7) 0.101(3) Uani 1 1 d . U . . .
H45 H 0.119718 0.288082 0.859201 0.121 Uiso 1 1 calc R U . . .
C46 C 0.1704(5) 0.2364(4) 0.9237(7) 0.101(3) Uani 1 1 d . U . . .
H46 H 0.140404 0.211924 0.939546 0.122 Uiso 1 1 calc R U . . .
C47 C 0.2265(6) 0.2252(4) 0.9488(6) 0.104(3) Uani 1 1 d . U . . .
H47 H 0.235548 0.192645 0.980721 0.125 Uiso 1 1 calc R U . . .
C48 C 0.3349(2) 0.4220(2) 0.7696(3) 0.0471(10) Uani 1 1 d . U . . .
C49 C 0.3314(2) 0.44861(19) 0.6781(3) 0.0441(10) Uani 1 1 d . U . . .
C50 C 0.3248(2) 0.50537(17) 0.6766(3) 0.0398(9) Uani 1 1 d . U . . .
H50 H 0.323159 0.525056 0.733012 0.048 Uiso 1 1 calc R U . . .
C51 C 0.3207(2) 0.53232(18) 0.5935(3) 0.0420(9) Uani 1 1 d . U . . .
C52 C 0.3252(2) 0.50405(19) 0.5105(3) 0.0417(9) Uani 1 1 d . U . . .
H52 H 0.324133 0.523128 0.453431 0.050 Uiso 1 1 calc R U . . .
C53 C 0.3313(2) 0.44752(18) 0.5107(3) 0.0423(9) Uani 1 1 d . U . . .
C54 C 0.3355(2) 0.42058(17) 0.5954(3) 0.0418(9) Uani 1 1 d . U . . .
H54 H 0.341326 0.382478 0.596299 0.050 Uiso 1 1 calc R U . . .
O2 O 0.4675(2) 0.74577(17) 0.3335(3) 0.0677(11) Uani 1 1 d . . . A 1
O1 O 0.5292(2) 0.6413(2) 0.3429(4) 0.0772(13) Uani 1 1 d . . . B 1
O3 O 0.40362(19) 0.7109(2) 0.5028(3) 0.0654(10) Uani 1 1 d . . . C 1
O4 O 0.4590(2) 0.6093(2) 0.5049(4) 0.0696(11) Uani 1 1 d . . . D 1
O5 O 0.500000 0.500000 1.0885(4) 0.0588(12) Uani 1 2 d S T P E 1
O6 O 0.5526(2) 0.56635(17) 0.9476(5) 0.0815(16) Uani 1 1 d . . . F 1
Cl1A Cl 0.50188(8) 0.66086(6) 1.10336(9) 0.0627(4) Uani 1 1 d . U . G 2
Cl2A Cl 0.28110(8) 0.80406(8) 0.45045(12) 0.0751(5) Uani 1 1 d . U . H 2
Cl3A Cl 0.1880(2) 0.50351(18) 0.8131(4) 0.1641(17) Uani 1 1 d D U . I 2
O1A O 0.4772(2) 0.70591(19) 1.1494(4) 0.0750(12) Uani 1 1 d . U . G 2
O2A O 0.5643(3) 0.6719(3) 1.1012(7) 0.109(2) Uani 1 1 d . U . G 2
O3A O 0.4883(4) 0.6564(2) 1.0118(3) 0.104(2) Uani 1 1 d . U . G 2
O4A O 0.5031(3) 0.6126(2) 1.1561(3) 0.0763(12) Uani 1 1 d . U . G 2
O5A O 0.2415(6) 0.8252(4) 0.5206(4) 0.141(3) Uani 1 1 d . U . H 2
O6A O 0.3406(4) 0.8050(4) 0.4624(13) 0.187(6) Uani 1 1 d . U . H 2
O7A O 0.2602(4) 0.8219(3) 0.3691(4) 0.116(3) Uani 1 1 d . U . H 2
O8A O 0.2700(4) 0.7472(3) 0.4554(8) 0.132(3) Uani 1 1 d . U . H 2
O9A O 0.2190(3) 0.5525(2) 0.7974(5) 0.0960(18) Uani 1 1 d D U . I 2
O10A O 0.2269(8) 0.4563(5) 0.8320(16) 0.324(11) Uani 1 1 d D U . I 2
O11A O 0.1538(10) 0.4896(10) 0.7243(12) 0.398(13) Uani 1 1 d D U . I 2
O12A O 0.1462(7) 0.5084(7) 0.8903(11) 0.272(9) Uani 1 1 d D U . I 2
O1B O 0.500000 0.500000 0.7957(7) 0.139(4) Uani 1 2 d DS TU P E .
O2B O 0.500000 0.500000 0.4361(15) 0.228(12) Uani 1 2 d S T P . .
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 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1472 0.1563 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3447 1.0913 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O6 Ni1 O6 177.7(4) 2_665 . ?
O6 Ni1 N1 92.18(18) 2_665 2_665 ?
O6 Ni1 N1 87.88(18) . 2_665 ?
O6 Ni1 N1 87.88(18) 2_665 . ?
O6 Ni1 N1 92.18(18) . . ?
N1 Ni1 N1 177.2(2) 2_665 . ?
O6 Ni1 O5 88.87(19) 2_665 . ?
O6 Ni1 O5 88.87(19) . . ?
N1 Ni1 O5 91.40(12) 2_665 . ?
N1 Ni1 O5 91.39(12) . . ?
O6 Ni1 O1B 91.13(19) 2_665 . ?
O6 Ni1 O1B 91.13(19) . . ?
N1 Ni1 O1B 88.60(12) 2_665 . ?
N1 Ni1 O1B 88.61(12) . . ?
O5 Ni1 O1B 180.0 . . ?
C16 N2 C7 123.4(4) . . ?
C1 C2 C3 119.8(5) . . ?
C2 C1 N1 123.5(5) . . ?
C21 N3 C17 116.2(5) . . ?
C21 N3 Ni2 119.9(4) . . ?
C17 N3 Ni2 123.7(4) . . ?
C2 C3 C4 117.9(5) . . ?
C32 N4 C23 121.6(4) . . ?
C5 C4 C3 120.0(5) . . ?
C5 C4 C6 116.2(5) . . ?
C3 C4 C6 123.6(5) . . ?
C48 N5 C39 121.6(4) . . ?
N1 C5 C4 121.1(5) . . ?
C33 N6 C37 118.5(5) . . ?
C33 N6 Ni2 119.7(4) . 2_665 ?
C37 N6 Ni2 121.4(4) . 2_665 ?
O8 C6 O9 124.3(5) . . ?
O8 C6 C4 124.4(5) . . ?
O9 C6 C4 111.3(4) . . ?
O9 C8 C9 106.4(4) . . ?
O9 C8 C7 107.7(4) . . ?
C9 C8 C7 103.8(5) . . ?
C10 C9 C8 103.0(5) . . ?
C22 O12 C24 115.1(5) . . ?
C38 O15 C40 116.3(5) . . ?
O1B C1B C2B 105.4(8) . 2_665 ?
O1B C1B C2B 105.4(8) . . ?
C2B C1B C2B 149.2(15) 2_665 . ?
C5 N1 C1 117.7(5) . . ?
C5 N1 Ni1 120.0(4) . . ?
C1 N1 Ni1 121.7(4) . . ?
O1 Ni2 O2 92.1(2) . . ?
O1 Ni2 O3 174.9(2) . . ?
O2 Ni2 O3 92.9(2) . . ?
O1 Ni2 N3 88.74(18) . . ?
O2 Ni2 N3 89.22(19) . . ?
O3 Ni2 N3 90.29(19) . . ?
O1 Ni2 N6 88.4(2) . 2_665 ?
O2 Ni2 N6 93.35(19) . 2_665 ?
O3 Ni2 N6 92.29(18) . 2_665 ?
N3 Ni2 N6 176.3(2) . 2_665 ?
O1 Ni2 O4 90.5(2) . . ?
O2 Ni2 O4 174.7(2) . . ?
O3 Ni2 O4 84.5(2) . . ?
N3 Ni2 O4 86.27(19) . . ?
N6 Ni2 O4 91.29(19) 2_665 . ?
N2 C7 C11 112.6(4) . . ?
N2 C7 C8 113.5(4) . . ?
C11 C7 C8 103.4(4) . . ?
C6 O9 C8 117.1(4) . . ?
C11 C10 C15 117.5(6) . . ?
C11 C10 C9 111.8(5) . . ?
C15 C10 C9 130.6(6) . . ?
C12 C11 C10 122.8(5) . . ?
C12 C11 C7 129.0(5) . . ?
C10 C11 C7 108.3(5) . . ?
C11 C12 C13 118.4(8) . . ?
C12 C13 C14 119.5(9) . . ?
C15 C14 C13 121.4(7) . . ?
C14 C15 C10 120.3(6) . . ?
O10 C16 N2 122.9(4) . . ?
O10 C16 C51 119.8(4) . . ?
N2 C16 C51 117.3(4) . . ?
N3 C17 C18 124.1(6) . . ?
C19 C18 C17 117.7(7) . . ?
C18 C19 C20 119.5(6) . . ?
C21 C20 C19 117.6(6) . . ?
C21 C20 C22 117.7(6) . . ?
C19 C20 C22 124.7(5) . . ?
N3 C21 C20 124.8(6) . . ?
O11 C22 O12 125.1(6) . . ?
O11 C22 C20 123.5(5) . . ?
O12 C22 C20 111.4(5) . . ?
N4 C23 C27 114.2(5) . . ?
N4 C23 C24 112.9(4) . . ?
C27 C23 C24 102.9(5) . . ?
O12 C24 C25 106.3(5) . . ?
O12 C24 C23 107.8(4) . . ?
C25 C24 C23 104.5(5) . . ?
C26 C25 C24 104.2(5) . . ?
C31 C26 C27 119.5(8) . . ?
C31 C26 C25 129.7(7) . . ?
C27 C26 C25 110.7(6) . . ?
C26 C27 C28 121.6(7) . . ?
C26 C27 C23 110.0(6) . . ?
C28 C27 C23 128.4(6) . . ?
C29 C28 C27 120.6(9) . . ?
C28 C29 C30 117.9(11) . . ?
C31 C30 C29 120.5(9) . . ?
C26 C31 C30 119.7(9) . . ?
O13 C32 N4 123.5(5) . . ?
O13 C32 C53 119.6(5) . . ?
N4 C32 C53 116.9(4) . . ?
N6 C33 C34 122.7(6) . . ?
C33 C34 C35 120.1(6) . . ?
C34 C35 C36 117.5(6) . . ?
C37 C36 C35 119.3(6) . . ?
C37 C36 C38 118.9(6) . . ?
C35 C36 C38 121.7(6) . . ?
N6 C37 C36 121.9(5) . . ?
O14 C38 O15 123.8(6) . . ?
O14 C38 C36 123.2(6) . . ?
O15 C38 C36 112.9(5) . . ?
N5 C39 C43 113.5(5) . . ?
N5 C39 C40 114.6(5) . . ?
C43 C39 C40 104.4(5) . . ?
O15 C40 C39 107.7(5) . . ?
O15 C40 C41 107.8(5) . . ?
C39 C40 C41 102.3(6) . . ?
C42 C41 C40 106.2(6) . . ?
O1C C1C C2C 120.8(19) . . ?
O1C C1C C4C 111.2(15) . . ?
C2C C1C C4C 109.1(14) . . ?
C3C C2C C1C 110(2) . . ?
C43 C42 C47 118.8(10) . . ?
C43 C42 C41 111.1(6) . . ?
C47 C42 C41 130.1(8) . . ?
C44 C43 C42 120.7(7) . . ?
C44 C43 C39 129.9(6) . . ?
C42 C43 C39 109.4(7) . . ?
C45 C44 C43 118.2(9) . . ?
C46 C45 C44 123.3(12) . . ?
C45 C46 C47 119.8(9) . . ?
C46 C47 C42 119.2(9) . . ?
O16 C48 N5 121.8(5) . . ?
O16 C48 C49 121.0(4) . . ?
N5 C48 C49 117.2(4) . . ?
C54 C49 C50 119.4(4) . . ?
C54 C49 C48 123.1(4) . . ?
C50 C49 C48 117.4(4) . . ?
C51 C50 C49 120.1(4) . . ?
C50 C51 C52 120.3(4) . . ?
C50 C51 C16 122.2(4) . . ?
C52 C51 C16 117.4(4) . . ?
C51 C52 C53 120.3(4) . . ?
C54 C53 C52 118.9(4) . . ?
C54 C53 C32 118.6(4) . . ?
C52 C53 C32 122.5(4) . . ?
C49 C54 C53 120.9(4) . . ?
O3A Cl1A O4A 117.3(3) . . ?
O3A Cl1A O1A 115.2(3) . . ?
O4A Cl1A O1A 114.6(3) . . ?
O3A Cl1A O2A 102.8(6) . . ?
O4A Cl1A O2A 98.5(4) . . ?
O1A Cl1A O2A 105.2(4) . . ?
O7A Cl2A O6A 117.5(8) . . ?
O7A Cl2A O8A 107.5(6) . . ?
O6A Cl2A O8A 100.8(6) . . ?
O7A Cl2A O5A 105.2(5) . . ?
O6A Cl2A O5A 122.1(9) . . ?
O8A Cl2A O5A 101.7(6) . . ?
O9A Cl3A O12A 112.4(7) . . ?
O9A Cl3A O10A 112.5(8) . . ?
O12A Cl3A O10A 108.7(8) . . ?
O9A Cl3A O11A 108.4(9) . . ?
O12A Cl3A O11A 107.8(9) . . ?
O10A Cl3A O11A 106.7(9) . . ?
C1B O1B Ni1 180.0 . . ?
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 O6 2.043(5) 2_665 ?
Ni1 O6 2.043(5) . ?
Ni1 N1 2.054(4) 2_665 ?
Ni1 N1 2.054(4) . ?
Ni1 O5 2.077(5) . ?
Ni1 O1B 2.155(10) . ?
N2 C16 1.318(7) . ?
N2 C7 1.466(6) . ?
C2 C1 1.341(9) . ?
C2 C3 1.379(8) . ?
C1 N1 1.360(8) . ?
N3 C21 1.323(7) . ?
N3 C17 1.329(9) . ?
N3 Ni2 2.082(5) . ?
C3 C4 1.394(8) . ?
N4 C32 1.312(7) . ?
N4 C23 1.461(6) . ?
C4 C5 1.383(8) . ?
C4 C6 1.485(7) . ?
N5 C48 1.340(7) . ?
N5 C39 1.449(6) . ?
C5 N1 1.351(7) . ?
N6 C33 1.323(8) . ?
N6 C37 1.340(8) . ?
N6 Ni2 2.093(5) 2_665 ?
C6 O8 1.196(7) . ?
C6 O9 1.362(7) . ?
C8 O9 1.449(6) . ?
C8 C9 1.538(7) . ?
C8 C7 1.546(8) . ?
C9 C10 1.485(10) . ?
O10 C16 1.252(6) . ?
O11 C22 1.212(8) . ?
O12 C22 1.348(7) . ?
O12 C24 1.454(6) . ?
O13 C32 1.239(6) . ?
O14 C38 1.224(8) . ?
O15 C38 1.335(8) . ?
O15 C40 1.423(7) . ?
O16 C48 1.242(6) . ?
C1B O1B 1.369(11) . ?
C1B C2B 1.483(13) 2_665 ?
C1B C2B 1.483(13) . ?
Ni2 O1 2.039(5) . ?
Ni2 O2 2.062(5) . ?
Ni2 O3 2.063(4) . ?
Ni2 O4 2.128(5) . ?
C7 C11 1.514(8) . ?
C10 C11 1.399(8) . ?
C10 C15 1.417(9) . ?
C11 C12 1.367(10) . ?
C12 C13 1.395(11) . ?
C13 C14 1.411(15) . ?
C14 C15 1.335(13) . ?
C16 C51 1.501(6) . ?
C17 C18 1.383(9) . ?
C18 C19 1.370(9) . ?
C19 C20 1.381(10) . ?
C20 C21 1.369(8) . ?
C20 C22 1.497(8) . ?
C23 C27 1.491(9) . ?
C23 C24 1.554(8) . ?
C24 C25 1.524(8) . ?
C25 C26 1.474(12) . ?
C26 C31 1.353(11) . ?
C26 C27 1.401(9) . ?
C27 C28 1.410(12) . ?
C28 C29 1.364(15) . ?
C29 C30 1.439(18) . ?
C30 C31 1.439(17) . ?
C32 C53 1.486(7) . ?
C33 C34 1.365(9) . ?
C34 C35 1.377(10) . ?
C35 C36 1.388(9) . ?
C36 C37 1.386(9) . ?
C36 C38 1.489(9) . ?
C39 C43 1.536(9) . ?
C39 C40 1.559(10) . ?
C40 C41 1.565(8) . ?
C41 C42 1.479(14) . ?
C1C O1C 1.323(14) . ?
C1C C2C 1.53(3) . ?
C1C C4C 1.65(2) . ?
C2C C3C 1.45(3) . ?
C42 C43 1.387(10) . ?
C42 C47 1.407(12) . ?
C43 C44 1.378(12) . ?
C44 C45 1.362(11) . ?
C45 C46 1.333(17) . ?
C46 C47 1.380(19) . ?
C48 C49 1.479(7) . ?
C49 C54 1.384(6) . ?
C49 C50 1.409(6) . ?
C50 C51 1.376(6) . ?
C51 C52 1.392(6) . ?
C52 C53 1.402(6) . ?
C53 C54 1.396(6) . ?
Cl1A O3A 1.366(5) . ?
Cl1A O4A 1.415(5) . ?
Cl1A O1A 1.416(5) . ?
Cl1A O2A 1.476(7) . ?
Cl2A O7A 1.347(6) . ?
Cl2A O6A 1.393(10) . ?
Cl2A O8A 1.429(8) . ?
Cl2A O5A 1.464(9) . ?
Cl3A O9A 1.426(6) . ?
Cl3A O12A 1.484(9) . ?
Cl3A O10A 1.500(10) . ?
Cl3A O11A 1.547(10) . ?
