#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:28:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229591 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/52/7045238.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_7045238
loop_
_publ_author_name
'Hang, Xinxin'
'Liu, Bing'
'Wang, Shentang'
'Liu, Yunling'
'Liao, Wuping'
_publ_section_title
;
 A metal-calixarene coordination nanotube with
 5-(pyrimidin-5-yl)isophthalic acid.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1782
_journal_page_last               1785
_journal_paper_doi               10.1039/c7dt04838f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C256 H236 Cl4 N16 Ni18.8 O54.8 S16'
_chemical_formula_weight         6171.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.0460(12)
_cell_length_b                   30.0460(12)
_cell_length_c                   21.8685(18)
_cell_measurement_reflns_used    9736
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.24
_cell_volume                     19742(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            111403
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.119
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_min         1.779
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             6346
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         9043
_refine_ls_number_restraints     737
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0854P)²+75.2376P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5729
_reflns_number_total             9043
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04838f2.cif
_cod_data_source_block           hxx12_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7045237--7045238.cif.'
_cod_original_formula_sum        'C256 H236 Cl4 N16 Ni18.80 O54.80 S16'
_cod_database_code               7045238
_shelx_shelxl_version_number     2017/1
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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
C1 C 0.2252(4) 0.3160(5) 0.0884(6) 0.0416(17) Uani 1 1 d . . . . .
C2 C 0.2246(5) 0.2905(4) 0.1420(8) 0.0466(12) Uani 1 1 d . U . . .
C3 C 0.1846(5) 0.2805(5) 0.1735(7) 0.068(4) Uani 1 1 d . . . . .
H3 H 0.185399 0.264206 0.209616 0.081 Uiso 1 1 calc R U . . .
C4 C 0.1436(4) 0.2953(6) 0.1497(9) 0.121(5) Uani 1 1 d D . . . .
C5 C 0.1457(5) 0.3222(6) 0.0970(8) 0.066(4) Uani 1 1 d . . . . .
H5 H 0.119488 0.334972 0.082841 0.079 Uiso 1 1 calc R U . . .
C6 C 0.1841(5) 0.3304(5) 0.0655(8) 0.051(3) Uani 1 1 d . . . . .
C7 C 0.3180(5) 0.2241(4) 0.0904(7) 0.0413(13) Uani 1 1 d . U . . .
C8 C 0.2913(4) 0.2233(5) 0.1429(8) 0.0457(12) Uani 1 1 d . U . . .
C9 C 0.2801(6) 0.1831(5) 0.1683(7) 0.076(5) Uani 1 1 d . . . . .
H9 H 0.260115 0.183031 0.200752 0.091 Uiso 1 1 calc R U . . .
C10 C 0.2965(5) 0.1429(4) 0.1486(6) 0.070(3) Uani 1 1 d D . . . .
C11 C 0.3189(6) 0.1428(5) 0.0931(8) 0.069(4) Uani 1 1 d . . . . .
H11 H 0.325578 0.115878 0.074094 0.082 Uiso 1 1 calc R U . . .
C12 C 0.3316(5) 0.1829(5) 0.0656(7) 0.049(3) Uani 1 1 d . . . . .
C13 C 0.4170(5) 0.2989(4) 0.1139(7) 0.041(3) Uani 1 1 d D . . . .
C14 C 0.4605(6) 0.3128(16) 0.1438(14) 0.045(4) Uani 0.5 1 d DG U P A 1
C19 C 0.4608(8) 0.3306(16) 0.2025(14) 0.066(5) Uani 0.5 1 d DG U P A 1
H19 H 0.434077 0.337595 0.221769 0.079 Uiso 0.5 1 calc R U P A 1
C18 C 0.5009(11) 0.3381(10) 0.2323(12) 0.046(5) Uani 0.5 1 d DG . P A 1
C17 C 0.5408(8) 0.3276(13) 0.2035(16) 0.040(6) Uani 0.5 1 d DG . P A 1
H17 H 0.567718 0.332618 0.223410 0.048 Uiso 0.5 1 calc R U P A 1
C16 C 0.5406(6) 0.3098(16) 0.1448(16) 0.041(9) Uani 0.5 1 d DG U P A 1
C15 C 0.5004(7) 0.3024(13) 0.1150(12) 0.041(3) Uani 0.5 1 d DG U P A 1
H15 H 0.500189 0.290409 0.075786 0.049 Uiso 0.5 1 calc R U P A 1
C20 C 0.5834(5) 0.3016(4) 0.1135(7) 0.045(3) Uani 1 1 d . . . . .
C21B C 0.5048(5) 0.3539(4) 0.2980(4) 0.049(3) Uani 0.5 1 d G U P A 1
C24B C 0.4685(4) 0.3763(4) 0.3226(6) 0.063(7) Uani 0.5 1 d G U P A 1
H24B H 0.442955 0.380512 0.299303 0.075 Uiso 0.5 1 calc R U P A 1
N2B N 0.4704(4) 0.3925(4) 0.3821(6) 0.086(5) Uani 0.5 1 d G U P A 1
C23B C 0.5086(5) 0.3863(5) 0.4169(4) 0.108(7) Uani 0.5 1 d G U P A 1
H23B H 0.509877 0.397124 0.456749 0.129 Uiso 0.5 1 calc R U P A 1
N1B N 0.5449(4) 0.3639(5) 0.3923(6) 0.115(6) Uani 0.5 1 d G U P A 1
C22B C 0.5430(4) 0.3477(4) 0.3328(6) 0.102(7) Uani 0.5 1 d G U P A 1
H22B H 0.567246 0.332710 0.316325 0.123 Uiso 0.5 1 calc R U P A 1
C26 C 0.2841(4) 0.0975(4) 0.1790(6) 0.096(3) Uani 1 1 d D U . . .
C27 C 0.2604(5) 0.1026(4) 0.2372(6) 0.143(5) Uani 1 1 d D U . . .
H27A H 0.238493 0.125715 0.233341 0.215 Uiso 1 1 calc R U . . .
H27B H 0.246022 0.075142 0.247619 0.215 Uiso 1 1 calc R U . . .
H27C H 0.281239 0.110452 0.268696 0.215 Uiso 1 1 calc R U . . .
C28 C 0.2459(6) 0.0774(5) 0.1417(9) 0.189(6) Uani 1 1 d D U . . .
H28A H 0.255943 0.071638 0.100762 0.284 Uiso 1 1 calc R U . . .
H28B H 0.236505 0.049998 0.160274 0.284 Uiso 1 1 calc R U . . .
H28C H 0.221440 0.097871 0.140670 0.284 Uiso 1 1 calc R U . . .
C29 C 0.3210(5) 0.0647(4) 0.1661(9) 0.175(6) Uani 1 1 d D U . . .
H29A H 0.330826 0.068022 0.124566 0.263 Uiso 1 1 calc R U . . .
H29B H 0.345481 0.070221 0.193300 0.263 Uiso 1 1 calc R U . . .
H29C H 0.310264 0.034911 0.172223 0.263 Uiso 1 1 calc R U . . .
C30 C 0.1009(3) 0.2890(4) 0.1863(5) 0.145(3) Uani 1 1 d D U . . .
C31 C 0.0759(4) 0.3320(4) 0.1999(7) 0.145(3) Uani 1 1 d D U . . .
H31A H 0.093531 0.350457 0.226355 0.218 Uiso 1 1 calc R U . . .
H31B H 0.048167 0.325150 0.219637 0.218 Uiso 1 1 calc R U . . .
H31C H 0.070154 0.347573 0.162390 0.218 Uiso 1 1 calc R U . . .
C32 C 0.0678(4) 0.2664(5) 0.1436(6) 0.145(3) Uani 1 1 d D U . . .
H32A H 0.078006 0.236953 0.134251 0.218 Uiso 1 1 calc R U . . .
H32B H 0.065240 0.283355 0.106562 0.218 Uiso 1 1 calc R U . . .
H32C H 0.039245 0.264786 0.163241 0.218 Uiso 1 1 calc R U . . .
C33 C 0.1093(4) 0.2785(6) 0.2535(6) 0.145(3) Uani 1 1 d D U . . .
H33A H 0.121480 0.249021 0.257043 0.218 Uiso 1 1 calc R U . . .
H33B H 0.081815 0.280090 0.275665 0.218 Uiso 1 1 calc R U . . .
H33C H 0.130030 0.299611 0.270070 0.218 Uiso 1 1 calc R U . . .
O1 O 0.2605(3) 0.3277(3) 0.0632(4) 0.0402(14) Uani 1 1 d . . . . .
O2 O 0.3276(3) 0.2636(3) 0.0632(4) 0.0411(14) Uani 1 1 d . . . . .
O3 O 0.3820(3) 0.3163(3) 0.1376(5) 0.0488(19) Uani 1 1 d . . . . .
O4 O 0.4196(3) 0.2777(3) 0.0637(4) 0.0434(18) Uani 1 1 d . . . . .
O5 O 0.5801(3) 0.2792(3) 0.0658(4) 0.051(2) Uani 1 1 d . . . . .
O6 O 0.6176(3) 0.3156(3) 0.1382(5) 0.047(2) Uani 1 1 d . . . . .
S1 S 0.27601(12) 0.27593(12) 0.17622(6) 0.0456(3) Uani 1 1 d . . . . .
S2 S 0.3673(2) 0.18419(19) 0.000000 0.0489(11) Uani 1 2 d S T P . .
S3 S 0.18428(19) 0.3668(2) 0.000000 0.0489(11) Uani 1 2 d S T P . .
Cl1 Cl 0.35009(18) 0.35097(18) 0.000000 0.0417(4) Uani 1 2 d S T P . .
O7 O 0.6333(4) 0.3657(4) 0.3707(2) 0.0248(12) Uani 0.5 1 d . U P . .
H7A H 0.666068 0.350561 0.385009 0.037 Uiso 0.5 1 d R U P . .
H7B H 0.628683 0.351511 0.322964 0.037 Uiso 0.5 1 d R U P . .
O8 O 0.5422(8) 0.4584(8) 0.500000 0.0051(14) Uani 0.35 2 d S TU P . .
O9 O 0.6440(4) 0.4296(4) 0.500000 0.0051(14) Uani 0.35 2 d S TU P . .
Ni1 Ni 0.32065(6) 0.32059(6) 0.10317(3) 0.03755(19) Uani 1 1 d . . . . .
Ni2 Ni 0.37401(8) 0.26746(9) 0.000000 0.0378(6) Uani 1 2 d S T P . .
Ni3 Ni 0.26762(9) 0.37395(8) 0.000000 0.0385(6) Uani 1 2 d S T P . .
Ni4 Ni 0.58654(19) 0.41341(19) 0.42715(8) 0.0506(5) Uani 0.35 1 d . . P . .
C14A C 0.4603(6) 0.3087(16) 0.1465(15) 0.045(4) Uani 0.5 1 d DG U P A 2
C19A C 0.4599(9) 0.3355(16) 0.1983(16) 0.066(5) Uani 0.5 1 d DG U P A 2
H19A H 0.432944 0.343803 0.215809 0.079 Uiso 0.5 1 calc R U P A 2
C18A C 0.4997(12) 0.3500(10) 0.2238(14) 0.069(10) Uani 0.5 1 d DG . P A 2
C17A C 0.5400(9) 0.3376(14) 0.1975(19) 0.061(12) Uani 0.5 1 d DG . P A 2
H17A H 0.566636 0.347284 0.214631 0.073 Uiso 0.5 1 calc R U P A 2
C16A C 0.5404(6) 0.3108(16) 0.1458(18) 0.047(10) Uani 0.5 1 d DG U P A 2
C15A C 0.5006(7) 0.2963(13) 0.1202(13) 0.041(3) Uani 0.5 1 d DG U P A 2
H15A H 0.500934 0.278382 0.085582 0.049 Uiso 0.5 1 calc R U P A 2
C21A C 0.4999(6) 0.3802(4) 0.2765(6) 0.081(4) Uani 0.5 1 d G U P A 2
C24A C 0.4678(5) 0.4135(5) 0.2785(7) 0.126(8) Uani 0.5 1 d G U P A 2
H24A H 0.446047 0.414950 0.248342 0.151 Uiso 0.5 1 calc R U P A 2
N2A N 0.4683(6) 0.4446(5) 0.3255(8) 0.162(9) Uani 0.5 1 d G U P A 2
C23A C 0.5009(7) 0.4424(5) 0.3706(7) 0.131(7) Uani 0.5 1 d G U P A 2
H23A H 0.501227 0.463213 0.402027 0.157 Uiso 0.5 1 calc R U P A 2
N1A N 0.5330(6) 0.4091(5) 0.3686(7) 0.114(7) Uani 0.5 1 d G U P A 2
C22A C 0.5325(5) 0.3780(5) 0.3215(7) 0.091(9) Uani 0.5 1 d G U P A 2
H22A H 0.553926 0.355682 0.320207 0.110 Uiso 0.5 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O1 C1 C2 122.4(13) . .
O1 C1 C6 120.4(14) . .
C2 C1 C6 117.0(13) . .
C1 C2 C3 122.4(14) . .
C1 C2 S1 118.5(11) . .
C3 C2 S1 118.8(12) . .
C4 C3 C2 119.6(14) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C5 C4 C3 116.4(12) . .
C5 C4 C30 122.5(13) . .
C3 C4 C30 120.2(14) . .
C6 C5 C4 123.6(14) . .
C6 C5 H5 118.2 . .
C4 C5 H5 118.2 . .
C5 C6 C1 120.6(15) . .
C5 C6 S3 120.9(12) . .
C1 C6 S3 117.9(12) . .
O2 C7 C8 119.7(12) . .
O2 C7 C12 122.5(13) . .
C8 C7 C12 117.7(13) . .
C9 C8 C7 119.1(14) . .
C9 C8 S1 123.2(12) . .
C7 C8 S1 117.6(11) . .
C8 C9 C10 124.0(14) . .
C8 C9 H9 118.0 . .
C10 C9 H9 118.0 . .
C9 C10 C11 116.8(12) . .
C9 C10 C26 123.2(12) . .
C11 C10 C26 119.1(12) . .
C10 C11 C12 120.4(14) . .
C10 C11 H11 119.8 . .
C12 C11 H11 119.8 . .
C11 C12 C7 120.8(14) . .
C11 C12 S2 121.7(12) . .
C7 C12 S2 117.5(11) . .
O4 C13 O3 127.0(14) . .
O4 C13 C14A 116.8(15) . .
O3 C13 C14A 115.8(15) . .
O4 C13 C14 117.2(15) . .
O3 C13 C14 114.8(15) . .
C19 C14 C15 120.0 . .
C19 C14 C13 120.6(15) . .
C15 C14 C13 118.9(14) . .
C14 C19 C18 120.0 . .
C14 C19 H19 120.0 . .
C18 C19 H19 120.0 . .
C19 C18 C17 120.0 . .
C19 C18 C21B 124(2) . .
C17 C18 C21B 116(2) . .
C16 C17 C18 120.0 . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C15 C16 C17 120.0 . .
C15 C16 C20 120.8(19) . .
C17 C16 C20 119(2) . .
C16 C15 C14 120.0 . .
C16 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
O6 C20 O5 128.3(16) . .
O6 C20 C16 117.6(17) . .
O5 C20 C16 114.0(17) . .
O6 C20 C16A 116.6(18) . .
O5 C20 C16A 115.1(18) . .
C24B C21B C22B 120.0 . .
C24B C21B C18 117.4(15) . .
C22B C21B C18 122.6(16) . .
C21B C24B N2B 120.0 . .
C21B C24B H24B 120.0 . .
N2B C24B H24B 120.0 . .
C23B N2B C24B 120.0 . .
C23B N2B Ni4 117.5(8) . 4_565
C24B N2B Ni4 121.1(8) . 4_565
N1B C23B N2B 120.0 . .
N1B C23B H23B 120.0 . .
N2B C23B H23B 120.0 . .
C22B N1B C23B 120.0 . .
N1B C22B C21B 120.0 . .
N1B C22B H22B 120.0 . .
C21B C22B H22B 120.0 . .
C27 C26 C29 126.0(12) . .
C27 C26 C28 98.2(12) . .
C29 C26 C28 101.2(12) . .
C27 C26 C10 113.1(10) . .
C29 C26 C10 108.3(10) . .
C28 C26 C10 107.3(11) . .
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C26 C28 H28A 109.5 . .
C26 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C26 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C26 C29 H29A 109.5 . .
C26 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C26 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C33 C30 C32 127.3(11) . .
C33 C30 C31 94.0(10) . .
C32 C30 C31 100.1(10) . .
C33 C30 C4 113.1(11) . .
C32 C30 C4 106.4(10) . .
C31 C30 C4 114.5(11) . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C30 C33 H33A 109.5 . .
C30 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C30 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C1 O1 Ni3 126.9(9) . .
C1 O1 Ni1 122.8(9) . .
Ni3 O1 Ni1 106.3(4) . .
C7 O2 Ni1 123.6(8) . .
C7 O2 Ni2 120.6(8) . .
Ni1 O2 Ni2 110.0(4) . .
C13 O3 Ni1 129.1(10) . .
C13 O4 Ni2 130.1(10) . .
C20 O5 Ni3 129.2(10) . 3_655
C20 O6 Ni1 128.7(11) . 3_655
C2 S1 C8 105.7(3) . .
C2 S1 Ni1 93.8(5) . .
C8 S1 Ni1 94.4(5) . .
C12 S2 C12 106.2(10) . 10
C12 S2 Ni2 94.0(5) . .
C12 S2 Ni2 94.0(5) 10 .
C6 S3 C6 105.4(10) 10 .
C6 S3 Ni3 93.2(5) 10 .
C6 S3 Ni3 93.2(5) . .
Ni3 Cl1 Ni1 76.44(12) . 10
Ni3 Cl1 Ni1 76.44(12) . .
Ni1 Cl1 Ni1 121.20(7) 10 .
Ni3 Cl1 Ni2 121.55(7) . .
Ni1 Cl1 Ni2 75.83(12) 10 .
Ni1 Cl1 Ni2 75.83(12) . .
Ni4 O7 H7A 128.4 . .
Ni4 O7 H7B 129.5 . .
H7A O7 H7B 102.1 . .
Ni4 O9 Ni4 83.2(4) . 10_556
O2 Ni1 O3 90.8(4) . .
O2 Ni1 O6 175.0(4) . 4_565
O3 Ni1 O6 89.15(15) . 4_565
O2 Ni1 O1 89.68(14) . .
O3 Ni1 O1 175.7(4) . .
O6 Ni1 O1 90.0(4) 4_565 .
O2 Ni1 S1 82.6(3) . .
O3 Ni1 S1 102.8(3) . .
O6 Ni1 S1 102.3(3) 4_565 .
O1 Ni1 S1 81.5(3) . .
O2 Ni1 Cl1 83.2(3) . .
O3 Ni1 Cl1 92.1(3) . .
O6 Ni1 Cl1 91.8(3) 4_565 .
O1 Ni1 Cl1 83.8(3) . .
S1 Ni1 Cl1 159.49(5) . .
O2 Ni2 O2 89.3(5) 10 .
O2 Ni2 O4 90.3(4) 10 10
O2 Ni2 O4 174.4(4) . 10
O2 Ni2 O4 174.4(4) 10 .
O2 Ni2 O4 90.3(4) . .
O4 Ni2 O4 89.6(5) 10 .
O2 Ni2 S2 83.4(3) 10 .
O2 Ni2 S2 83.4(3) . .
O4 Ni2 S2 102.1(3) 10 .
O4 Ni2 S2 102.1(3) . .
O2 Ni2 Cl1 82.0(3) 10 .
O2 Ni2 Cl1 82.0(3) . .
O4 Ni2 Cl1 92.4(3) 10 .
O4 Ni2 Cl1 92.4(3) . .
S2 Ni2 Cl1 159.4(2) . .
O1 Ni3 O1 89.0(5) . 10
O1 Ni3 O5 90.1(4) . 4_565
O1 Ni3 O5 176.1(4) 10 4_565
O1 Ni3 O5 176.1(4) . 11_565
O1 Ni3 O5 90.1(4) 10 11_565
O5 Ni3 O5 90.6(5) 4_565 11_565
O1 Ni3 S3 80.3(3) . .
O1 Ni3 S3 80.3(3) 10 .
O5 Ni3 S3 103.3(3) 4_565 .
O5 Ni3 S3 103.3(3) 11_565 .
O1 Ni3 Cl1 85.2(3) . .
O1 Ni3 Cl1 85.2(3) 10 .
O5 Ni3 Cl1 91.0(3) 4_565 .
O5 Ni3 Cl1 91.0(3) 11_565 .
S3 Ni3 Cl1 159.5(2) . .
N1A Ni4 O7 95.9(6) . .
N2B Ni4 O7 94.2(6) 3_655 .
N1A Ni4 O9 170.9(6) . .
N2B Ni4 O9 86.0(10) 3_655 .
O7 Ni4 O9 92.4(4) . .
N1A Ni4 O8 90.8(7) . .
N2B Ni4 O8 91.0(8) 3_655 .
O7 Ni4 O8 171.6(2) . .
O9 Ni4 O8 81.4(6) . .
C19A C14A C15A 120.0 . .
C19A C14A C13 119.2(15) . .
C15A C14A C13 120.2(15) . .
C14A C19A C18A 120.0 . .
C14A C19A H19A 120.0 . .
C18A C19A H19A 120.0 . .
C19A C18A C17A 120.0 . .
C19A C18A C21A 121(2) . .
C17A C18A C21A 119(2) . .
C16A C17A C18A 120.0 . .
C16A C17A H17A 120.0 . .
C18A C17A H17A 120.0 . .
C15A C16A C17A 120.0 . .
C15A C16A C20 120(2) . .
C17A C16A C20 120(2) . .
C16A C15A C14A 120.0 . .
C16A C15A H15A 120.0 . .
C14A C15A H15A 120.0 . .
C24A C21A C22A 120.0 . .
C24A C21A C18A 117.9(17) . .
C22A C21A C18A 122.0(17) . .
N2A C24A C21A 120.0 . .
N2A C24A H24A 120.0 . .
C21A C24A H24A 120.0 . .
C24A N2A C23A 120.0 . .
N1A C23A N2A 120.0 . .
N1A C23A H23A 120.0 . .
N2A C23A H23A 120.0 . .
C23A N1A C22A 120.0 . .
C23A N1A Ni4 118.5(10) . .
C22A N1A Ni4 120.7(10) . .
N1A C22A C21A 120.0 . .
N1A C22A H22A 120.0 . .
C21A C22A H22A 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.244(14) .
C1 C2 1.400(19) .
C1 C6 1.401(17) .
C2 C3 1.417(19) .
C2 S1 1.773(15) .
C3 C4 1.408(19) .
C3 H3 0.9300 .
C4 C5 1.41(2) .
C4 C30 1.524(5) .
C5 C6 1.366(19) .
C5 H5 0.9300 .
C6 S3 1.802(16) .
C7 O2 1.358(14) .
C7 C8 1.401(19) .
C7 C12 1.413(18) .
C8 C9 1.372(19) .
C8 S1 1.800(15) .
C9 C10 1.375(17) .
C9 H9 0.9300 .
C10 C11 1.387(19) .
C10 C26 1.564(11) .
C11 C12 1.400(19) .
C11 H11 0.9300 .
C12 S2 1.792(15) .
C13 O4 1.271(15) .
C13 O3 1.284(15) .
C13 C14A 1.513(18) .
C13 C14 1.519(18) .
C14 C19 1.3900 .
C14 C15 1.3900 .
C19 C18 1.3900 .
C19 H19 0.9300 .
C18 C17 1.3900 .
C18 C21B 1.52(2) .
C17 C16 1.3900 .
C17 H17 0.9300 .
C16 C15 1.3900 .
C16 C20 1.48(3) .
C15 H15 0.9300 .
C20 O6 1.236(16) .
C20 O5 1.246(15) .
C20 C16A 1.50(3) .
C21B C24B 1.3900 .
C21B C22B 1.3900 .
C24B N2B 1.3900 .
C24B H24B 0.9300 .
N2B C23B 1.3900 .
N2B Ni4 2.074(11) 4_565
C23B N1B 1.3900 .
C23B H23B 0.9300 .
N1B C22B 1.3900 .
C22B H22B 0.9300 .
C26 C27 1.466(12) .
C26 C29 1.511(12) .
C26 C28 1.530(14) .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C30 C33 1.524(5) .
C30 C32 1.524(5) .
C30 C31 1.524(5) .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C33 H33A 0.9600 .
C33 H33B 0.9600 .
C33 H33C 0.9600 .
O1 Ni3 1.972(9) .
O1 Ni1 2.019(8) .
O2 Ni1 1.933(8) .
O2 Ni2 1.967(9) .
O3 Ni1 1.996(8) .
O4 Ni2 1.978(9) .
O5 Ni3 2.024(9) 3_655
O6 Ni1 2.014(9) 3_655
S1 Ni1 2.4801(14) .
S2 Ni2 2.510(6) .
S3 Ni3 2.513(6) .
Cl1 Ni3 2.572(7) .
Cl1 Ni1 2.5897(11) 10
Cl1 Ni1 2.5897(11) .
Cl1 Ni2 2.610(7) .
O7 Ni4 2.356(6) .
O7 H7A 1.1287 .
O7 H7B 1.1371 .
O8 Ni4 2.479(7) .
O9 Ni4 2.399(10) .
O9 Ni4 2.399(10) 10_556
Ni4 N1A 2.061(13) .
C14A C19A 1.3900 .
C14A C15A 1.3900 .
C19A C18A 1.3900 .
C19A H19A 0.9300 .
C18A C17A 1.3900 .
C18A C21A 1.47(3) .
C17A C16A 1.3900 .
C17A H17A 0.9300 .
C16A C15A 1.3900 .
C15A H15A 0.9300 .
C21A C24A 1.3900 .
C21A C22A 1.3900 .
C24A N2A 1.3900 .
C24A H24A 0.9300 .
N2A C23A 1.3900 .
C23A N1A 1.3900 .
C23A H23A 0.9300 .
N1A C22A 1.3900 .
C22A H22A 0.9300 .
