#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:33:33 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179251 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/71/4317163.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_4317163
loop_
_publ_author_name
'Ulrike Lehmann'
'Julia Klingele'
'Vasile Lozan'
'Gunther Steinfeld'
'Marco H. Klingele'
'Steffen Käss'
'Axel Rodenstein'
'Berthold Kersting'
_publ_contact_author_address
; Institut fuer Anorganische Chemie
  Universitaet Leipzig, Johannisallee 29
  04103 Leipzig
  Germany
;
_publ_contact_author_email       b.kersting@uni-leipzig.de
_publ_contact_author_fax         '+49/(0)341/973 6199'
_publ_contact_author_name        'Prof. Dr Berthold Kersting'
_publ_contact_author_phone       '+49/(0)341/973 6143'
_publ_section_title
;
 Dependence of the Chemical Properties of Macrocyclic [NiII2L(μ-O2CR)]+
 Complexes on the Basicity of the Carboxylato Coligands (L2-= macrocyclic
 N6S2ligand)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11018
_journal_page_last               11029
_journal_paper_doi               10.1021/ic101574a
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source
;
 Crystals were grown by slow evaporation from a mixed ethanol/
 acetonitrile solvent system
;
_chemical_formula_structural
; 
 [Ni2L(u-O2CCCl3)][BPh4].2CH3CN.EtOH 
;
_chemical_formula_sum            'C70 H96 B Cl3 N8 Ni2 O3 S2'
_chemical_formula_weight         1396.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                116.099(3)
_cell_angle_beta                 109.190(3)
_cell_angle_gamma                94.799(3)
_cell_formula_units_Z            2
_cell_length_a                   14.256(3)
_cell_length_b                   17.082(3)
_cell_length_c                   17.772(3)
_cell_measurement_temperature    213(2)
_cell_volume                     3535.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  BRUKER-AXS
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31938
_diffrn_reflns_theta_full        28.84
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.8635
_exptl_absorpt_correction_T_min  0.8394
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         16416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0531P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                8672
_reflns_number_total             16416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101574a_si_001_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        3535.3(11)
_cod_database_code               4317163
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.10852(3) 0.38419(3) 0.31553(3) 0.02763(11) Uani 1 1 d . . .
Ni2 Ni 0.27831(3) 0.60267(3) 0.43654(3) 0.02651(11) Uani 1 1 d . . .
S1 S 0.29878(6) 0.44818(6) 0.40172(6) 0.0300(2) Uani 1 1 d . . .
S2 S 0.12179(6) 0.53334(6) 0.43754(6) 0.0294(2) Uani 1 1 d . . .
Cl1 Cl 0.19333(10) 0.58173(8) 0.14331(8) 0.0673(3) Uani 1 1 d . . .
Cl2 Cl 0.07855(12) 0.39598(8) 0.04495(7) 0.0847(5) Uani 1 1 d . . .
Cl3 Cl -0.00834(10) 0.53508(10) 0.13625(10) 0.0825(4) Uani 1 1 d . . .
O1 O 0.10188(17) 0.42598(15) 0.22461(14) 0.0312(5) Uani 1 1 d . . .
O2 O 0.21509(17) 0.56390(15) 0.30081(15) 0.0307(5) Uani 1 1 d . . .
N1 N 0.1286(2) 0.25288(18) 0.21618(19) 0.0332(7) Uani 1 1 d . . .
N2 N 0.0869(2) 0.30603(19) 0.37789(19) 0.0347(7) Uani 1 1 d . . .
N3 N -0.0650(2) 0.35211(19) 0.25989(19) 0.0336(7) Uani 1 1 d . . .
N4 N 0.2310(2) 0.72925(18) 0.46369(19) 0.0305(6) Uani 1 1 d . . .
N5 N 0.3700(2) 0.67826(19) 0.58327(18) 0.0329(7) Uani 1 1 d . . .
N6 N 0.4366(2) 0.64470(18) 0.43852(18) 0.0304(7) Uani 1 1 d . . .
C1 C 0.3399(2) 0.4205(2) 0.3120(2) 0.0274(7) Uani 1 1 d . . .
C2 C 0.3005(2) 0.3346(2) 0.2336(2) 0.0306(8) Uani 1 1 d . . .
C3 C 0.3295(3) 0.3168(2) 0.1614(2) 0.0339(8) Uani 1 1 d . . .
H3 H 0.3000 0.2595 0.1082 0.041 Uiso 1 1 calc R . .
C4 C 0.4006(3) 0.3807(2) 0.1652(2) 0.0324(8) Uani 1 1 d . . .
C5 C 0.4454(3) 0.4630(2) 0.2471(2) 0.0327(8) Uani 1 1 d . . .
H5 H 0.4966 0.5064 0.2530 0.039 Uiso 1 1 calc R . .
C6 C 0.4178(2) 0.4836(2) 0.3199(2) 0.0306(8) Uani 1 1 d . . .
C7 C 0.2400(3) 0.2588(2) 0.2346(2) 0.0350(8) Uani 1 1 d . . .
H7A H 0.2440 0.2016 0.1888 0.042 Uiso 1 1 calc R . .
H7B H 0.2744 0.2639 0.2948 0.042 Uiso 1 1 calc R . .
C8 C 0.0736(3) 0.2202(3) 0.1170(2) 0.0477(10) Uani 1 1 d . . .
H8A H 0.0898 0.1651 0.0822 0.071 Uiso 1 1 calc R . .
H8B H 0.0951 0.2661 0.1034 0.071 Uiso 1 1 calc R . .
H8C H -0.0001 0.2080 0.1004 0.071 Uiso 1 1 calc R . .
C9 C 0.0936(3) 0.1835(2) 0.2376(3) 0.0465(10) Uani 1 1 d . . .
H9A H 0.1249 0.1335 0.2167 0.056 Uiso 1 1 calc R . .
H9B H 0.0185 0.1591 0.2050 0.056 Uiso 1 1 calc R . .
C10 C 0.1237(3) 0.2247(3) 0.3392(3) 0.0469(10) Uani 1 1 d . . .
H10A H 0.0953 0.1793 0.3512 0.056 Uiso 1 1 calc R . .
H10B H 0.1990 0.2412 0.3705 0.056 Uiso 1 1 calc R . .
C11 C 0.1440(3) 0.3539(3) 0.4789(3) 0.0550(11) Uani 1 1 d . . .
H11A H 0.1305 0.3142 0.5021 0.083 Uiso 1 1 calc R . .
H11B H 0.1216 0.4077 0.5062 0.083 Uiso 1 1 calc R . .
H11C H 0.2173 0.3711 0.4947 0.083 Uiso 1 1 calc R . .
C12 C -0.0246(3) 0.2801(3) 0.3563(3) 0.0461(10) Uani 1 1 d . . .
H12A H -0.0386 0.3259 0.4057 0.055 Uiso 1 1 calc R . .
H12B H -0.0412 0.2225 0.3549 0.055 Uiso 1 1 calc R . .
C13 C -0.0943(3) 0.2705(2) 0.2663(3) 0.0463(10) Uani 1 1 d . . .
H13A H -0.0903 0.2173 0.2157 0.056 Uiso 1 1 calc R . .
H13B H -0.1657 0.2609 0.2603 0.056 Uiso 1 1 calc R . .
C14 C -0.1199(3) 0.3333(3) 0.1645(2) 0.0474(10) Uani 1 1 d . . .
H14A H -0.0999 0.2848 0.1236 0.071 Uiso 1 1 calc R . .
H14B H -0.1019 0.3874 0.1612 0.071 Uiso 1 1 calc R . .
H14C H -0.1937 0.3155 0.1462 0.071 Uiso 1 1 calc R . .
C15 C -0.1030(3) 0.4230(2) 0.3183(2) 0.0353(8) Uani 1 1 d . . .
H15A H -0.0753 0.4299 0.3798 0.042 Uiso 1 1 calc R . .
H15B H -0.1782 0.4012 0.2932 0.042 Uiso 1 1 calc R . .
C16 C -0.0771(3) 0.5149(2) 0.3279(2) 0.0311(8) Uani 1 1 d . . .
C17 C 0.0234(2) 0.5730(2) 0.3870(2) 0.0282(7) Uani 1 1 d . . .
C18 C 0.0401(2) 0.6642(2) 0.4106(2) 0.0297(8) Uani 1 1 d . . .
C19 C -0.0392(3) 0.6946(2) 0.3716(2) 0.0341(8) Uani 1 1 d . . .
H19 H -0.0258 0.7558 0.3871 0.041 Uiso 1 1 calc R . .
C20 C -0.1378(3) 0.6380(2) 0.3105(2) 0.0336(8) Uani 1 1 d . . .
C21 C -0.1538(3) 0.5483(2) 0.2907(2) 0.0345(8) Uani 1 1 d . . .
H21 H -0.2199 0.5085 0.2502 0.041 Uiso 1 1 calc R . .
C22 C 0.1395(2) 0.7310(2) 0.4867(2) 0.0344(8) Uani 1 1 d . . .
H22A H 0.1296 0.7919 0.5071 0.041 Uiso 1 1 calc R . .
H22B H 0.1545 0.7200 0.5386 0.041 Uiso 1 1 calc R . .
C23 C 0.2112(3) 0.7541(2) 0.3907(3) 0.0423(9) Uani 1 1 d . . .
H23A H 0.2125 0.8175 0.4160 0.063 Uiso 1 1 calc R . .
H23B H 0.1441 0.7175 0.3413 0.063 Uiso 1 1 calc R . .
H23C H 0.2640 0.7433 0.3670 0.063 Uiso 1 1 calc R . .
C24 C 0.3195(3) 0.7995(2) 0.5476(2) 0.0409(9) Uani 1 1 d . . .
H24A H 0.2998 0.8561 0.5729 0.049 Uiso 1 1 calc R . .
H24B H 0.3771 0.8109 0.5319 0.049 Uiso 1 1 calc R . .
C25 C 0.3538(3) 0.7705(2) 0.6193(2) 0.0412(9) Uani 1 1 d . . .
H25A H 0.4183 0.8141 0.6698 0.049 Uiso 1 1 calc R . .
H25B H 0.3016 0.7720 0.6443 0.049 Uiso 1 1 calc R . .
C26 C 0.3455(3) 0.6357(3) 0.6340(2) 0.0514(11) Uani 1 1 d . . .
H26A H 0.3593 0.5768 0.6127 0.077 Uiso 1 1 calc R . .
H26B H 0.2734 0.6287 0.6234 0.077 Uiso 1 1 calc R . .
H26C H 0.3880 0.6739 0.6992 0.077 Uiso 1 1 calc R . .
C27 C 0.4790(2) 0.6833(3) 0.5980(2) 0.0376(9) Uani 1 1 d . . .
H27A H 0.4914 0.6243 0.5865 0.045 Uiso 1 1 calc R . .
H27B H 0.5234 0.7279 0.6621 0.045 Uiso 1 1 calc R . .
C28 C 0.5069(2) 0.7094(2) 0.5363(2) 0.0356(9) Uani 1 1 d . . .
H28A H 0.5011 0.7708 0.5516 0.043 Uiso 1 1 calc R . .
H28B H 0.5784 0.7089 0.5455 0.043 Uiso 1 1 calc R . .
C29 C 0.4389(3) 0.6843(2) 0.3797(3) 0.0409(9) Uani 1 1 d . . .
H29A H 0.5064 0.6915 0.3784 0.061 Uiso 1 1 calc R . .
H29B H 0.4247 0.7429 0.4043 0.061 Uiso 1 1 calc R . .
H29C H 0.3870 0.6445 0.3179 0.061 Uiso 1 1 calc R . .
C30 C 0.4807(2) 0.5659(2) 0.4109(2) 0.0330(8) Uani 1 1 d . . .
H30A H 0.4946 0.5481 0.4581 0.040 Uiso 1 1 calc R . .
H30B H 0.5473 0.5861 0.4111 0.040 Uiso 1 1 calc R . .
C31 C 0.4360(3) 0.3643(2) 0.0884(2) 0.0385(9) Uani 1 1 d . . .
C32 C 0.3737(3) 0.2746(3) 0.0011(3) 0.0600(12) Uani 1 1 d . . .
H32A H 0.3808 0.2253 0.0141 0.090 Uiso 1 1 calc R . .
H32B H 0.3990 0.2671 -0.0454 0.090 Uiso 1 1 calc R . .
H32C H 0.3016 0.2741 -0.0210 0.090 Uiso 1 1 calc R . .
C33 C 0.5500(3) 0.3624(3) 0.1217(3) 0.0572(12) Uani 1 1 d . . .
H33A H 0.5917 0.4200 0.1758 0.086 Uiso 1 1 calc R . .
H33B H 0.5736 0.3517 0.0735 0.086 Uiso 1 1 calc R . .
H33C H 0.5563 0.3143 0.1366 0.086 Uiso 1 1 calc R . .
C34 C 0.4271(4) 0.4411(3) 0.0664(3) 0.0656(13) Uani 1 1 d . . .
H34A H 0.3556 0.4426 0.0453 0.098 Uiso 1 1 calc R . .
H34B H 0.4513 0.4312 0.0187 0.098 Uiso 1 1 calc R . .
H34C H 0.4687 0.4983 0.1212 0.098 Uiso 1 1 calc R . .
C35 C -0.2263(3) 0.6722(3) 0.2714(3) 0.0421(9) Uani 1 1 d . . .
C36 C -0.1940(3) 0.7719(3) 0.3015(4) 0.0710(15) Uani 1 1 d . . .
H36A H -0.1643 0.8072 0.3680 0.106 Uiso 1 1 calc R . .
H36B H -0.2538 0.7904 0.2768 0.106 Uiso 1 1 calc R . .
H36C H -0.1433 0.7818 0.2790 0.106 Uiso 1 1 calc R . .
C37 C -0.3116(3) 0.6581(3) 0.3029(3) 0.0587(12) Uani 1 1 d . . .
H37A H -0.3366 0.5942 0.2811 0.088 Uiso 1 1 calc R . .
H37B H -0.3680 0.6799 0.2782 0.088 Uiso 1 1 calc R . .
H37C H -0.2840 0.6914 0.3695 0.088 Uiso 1 1 calc R . .
C38 C -0.2706(3) 0.6174(4) 0.1663(3) 0.0733(15) Uani 1 1 d . . .
H38A H -0.2165 0.6233 0.1458 0.110 Uiso 1 1 calc R . .
H38B H -0.3255 0.6400 0.1407 0.110 Uiso 1 1 calc R . .
H38C H -0.2977 0.5541 0.1459 0.110 Uiso 1 1 calc R . .
C39 C 0.1465(3) 0.4959(2) 0.2322(2) 0.0319(8) Uani 1 1 d . . .
C40 C 0.1074(3) 0.5015(2) 0.1426(2) 0.0423(9) Uani 1 1 d . . .
B B -0.2574(3) 0.0799(3) -0.2096(3) 0.0347(10) Uani 1 1 d . . .
C101 C -0.3035(3) 0.0153(2) -0.3224(2) 0.0366(9) Uani 1 1 d . . .
C102 C -0.3445(3) 0.0461(3) -0.3837(3) 0.0477(10) Uani 1 1 d . . .
H102 H -0.3539 0.1046 -0.3604 0.057 Uiso 1 1 calc R . .
C103 C -0.3719(3) -0.0051(3) -0.4772(3) 0.0596(12) Uani 1 1 d . . .
H103 H -0.4005 0.0185 -0.5158 0.071 Uiso 1 1 calc R . .
C104 C -0.3575(3) -0.0903(3) -0.5137(3) 0.0590(12) Uani 1 1 d . . .
H104 H -0.3754 -0.1251 -0.5771 0.071 Uiso 1 1 calc R . .
C105 C -0.3167(3) -0.1237(3) -0.4566(3) 0.0537(11) Uani 1 1 d . . .
H105 H -0.3063 -0.1819 -0.4807 0.064 Uiso 1 1 calc R . .
C106 C -0.2906(3) -0.0719(3) -0.3631(3) 0.0445(10) Uani 1 1 d . . .
H106 H -0.2630 -0.0965 -0.3254 0.053 Uiso 1 1 calc R . .
C201 C -0.2732(3) 0.0242(2) -0.1579(2) 0.0355(8) Uani 1 1 d . . .
C202 C -0.3584(3) -0.0490(2) -0.1958(3) 0.0415(9) Uani 1 1 d . . .
H202 H -0.4048 -0.0725 -0.2571 0.050 Uiso 1 1 calc R . .
C203 C -0.3775(3) -0.0883(3) -0.1468(3) 0.0482(10) Uani 1 1 d . . .
H203 H -0.4369 -0.1362 -0.1746 0.058 Uiso 1 1 calc R . .
C204 C -0.3098(4) -0.0575(3) -0.0574(3) 0.0547(11) Uani 1 1 d . . .
H204 H -0.3216 -0.0851 -0.0245 0.066 Uiso 1 1 calc R . .
C205 C -0.2253(4) 0.0137(3) -0.0174(3) 0.0581(12) Uani 1 1 d . . .
H205 H -0.1789 0.0360 0.0437 0.070 Uiso 1 1 calc R . .
C206 C -0.2080(3) 0.0532(3) -0.0668(3) 0.0524(11) Uani 1 1 d . . .
H206 H -0.1493 0.1021 -0.0375 0.063 Uiso 1 1 calc R . .
C301 C -0.1356(3) 0.1216(2) -0.1815(2) 0.0376(9) Uani 1 1 d . . .
C302 C -0.1016(3) 0.1951(2) -0.1901(3) 0.0450(10) Uani 1 1 d . . .
H302 H -0.1503 0.2244 -0.2077 0.054 Uiso 1 1 calc R . .
C303 C -0.0014(3) 0.2273(3) -0.1746(3) 0.0575(12) Uani 1 1 d . . .
H303 H 0.0171 0.2773 -0.1813 0.069 Uiso 1 1 calc R . .
C304 C 0.0711(3) 0.1856(3) -0.1491(3) 0.0681(14) Uani 1 1 d . . .
H304 H 0.1399 0.2072 -0.1378 0.082 Uiso 1 1 calc R . .
C305 C 0.0434(3) 0.1124(4) -0.1403(3) 0.0708(14) Uani 1 1 d . . .
H305 H 0.0929 0.0833 -0.1234 0.085 Uiso 1 1 calc R . .
C306 C -0.0582(3) 0.0815(3) -0.1563(3) 0.0565(12) Uani 1 1 d . . .
H306 H -0.0759 0.0312 -0.1500 0.068 Uiso 1 1 calc R . .
C401 C -0.3153(3) 0.1602(3) -0.1777(3) 0.0400(9) Uani 1 1 d . . .
C402 C -0.4212(3) 0.1465(3) -0.2227(3) 0.0547(11) Uani 1 1 d . . .
H402 H -0.4599 0.0900 -0.2749 0.066 Uiso 1 1 calc R . .
C403 C -0.4713(4) 0.2120(4) -0.1940(4) 0.0703(14) Uani 1 1 d . . .
H403 H -0.5424 0.1998 -0.2273 0.084 Uiso 1 1 calc R . .
C404 C -0.4184(5) 0.2953(4) -0.1170(4) 0.0739(16) Uani 1 1 d . . .
H404 H -0.4525 0.3403 -0.0979 0.089 Uiso 1 1 calc R . .
C405 C -0.3146(4) 0.3113(3) -0.0685(3) 0.0641(13) Uani 1 1 d . . .
H405 H -0.2774 0.3671 -0.0148 0.077 Uiso 1 1 calc R . .
C406 C -0.2647(3) 0.2447(3) -0.0993(3) 0.0484(10) Uani 1 1 d . . .
H406 H -0.1936 0.2574 -0.0656 0.058 Uiso 1 1 calc R . .
N7 N 0.0002(6) -0.0931(5) -0.4347(5) 0.186(3) Uani 1 1 d . . .
C41 C -0.0381(5) -0.0352(4) -0.4201(4) 0.0893(18) Uani 1 1 d . . .
C42 C -0.0854(4) 0.0348(3) -0.4031(4) 0.0862(17) Uani 1 1 d . . .
H42A H -0.1289 0.0300 -0.3724 0.129 Uiso 1 1 calc R . .
H42B H -0.1273 0.0308 -0.4607 0.129 Uiso 1 1 calc R . .
H42C H -0.0332 0.0924 -0.3643 0.129 Uiso 1 1 calc R . .
N8 N -0.3762(4) 0.1462(4) 0.1321(4) 0.1129(19) Uani 1 1 d . . .
C43 C -0.4008(4) 0.1357(4) 0.0611(4) 0.0731(15) Uani 1 1 d . . .
C44 C -0.4317(4) 0.1235(4) -0.0298(4) 0.0909(18) Uani 1 1 d . . .
H44A H -0.3964 0.0837 -0.0615 0.136 Uiso 1 1 calc R . .
H44B H -0.4139 0.1817 -0.0258 0.136 Uiso 1 1 calc R . .
H44C H -0.5056 0.0970 -0.0634 0.136 Uiso 1 1 calc R . .
O3 O -0.2338(8) 0.0902(8) 0.2569(8) 0.335(6) Uiso 1 1 d . . .
H3A H -0.1915 0.1136 0.3103 0.502 Uiso 1 1 d R . .
C45 C -0.2367(10) 0.0099(9) 0.2161(9) 0.248(6) Uiso 1 1 d . . .
H45A H -0.1670 0.0024 0.2265 0.298 Uiso 1 1 calc R . .
H45B H -0.2770 -0.0166 0.1500 0.298 Uiso 1 1 calc R . .
C46 C -0.2826(8) -0.0299(7) 0.2514(7) 0.216(5) Uiso 1 1 d . . .
H46A H -0.2353 -0.0123 0.3132 0.324 Uiso 1 1 calc R . .
H46B H -0.3008 -0.0952 0.2133 0.324 Uiso 1 1 calc R . .
H46C H -0.3444 -0.0107 0.2528 0.324 Uiso 1 1 calc R . .
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'
B B 0.0013 0.0007 '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
_geom_angle_publ_flag
O1 Ni1 N2 163.91(10) . . ?
O1 Ni1 N3 87.97(10) . . ?
N2 Ni1 N3 82.90(11) . . ?
O1 Ni1 N1 86.92(10) . . ?
N2 Ni1 N1 81.76(11) . . ?
N3 Ni1 N1 100.40(10) . . ?
O1 Ni1 S2 94.59(7) . . ?
N2 Ni1 S2 98.65(8) . . ?
N3 Ni1 S2 90.17(7) . . ?
N1 Ni1 S2 169.38(7) . . ?
O1 Ni1 S1 93.66(7) . . ?
N2 Ni1 S1 97.93(8) . . ?
N3 Ni1 S1 168.47(8) . . ?
N1 Ni1 S1 91.09(7) . . ?
S2 Ni1 S1 78.33(3) . . ?
O2 Ni2 N5 163.15(10) . . ?
O2 Ni2 N4 87.70(10) . . ?
N5 Ni2 N4 82.55(10) . . ?
O2 Ni2 N6 88.08(9) . . ?
N5 Ni2 N6 80.11(10) . . ?
N4 Ni2 N6 99.70(10) . . ?
O2 Ni2 S2 95.49(7) . . ?
N5 Ni2 S2 98.41(8) . . ?
N4 Ni2 S2 91.25(7) . . ?
N6 Ni2 S2 168.62(7) . . ?
O2 Ni2 S1 91.56(7) . . ?
N5 Ni2 S1 100.52(8) . . ?
N4 Ni2 S1 169.39(7) . . ?
N6 Ni2 S1 90.85(7) . . ?
S2 Ni2 S1 78.27(3) . . ?
C1 S1 Ni1 101.78(11) . . ?
C1 S1 Ni2 100.99(11) . . ?
Ni1 S1 Ni2 89.89(3) . . ?
C17 S2 Ni2 105.81(11) . . ?
C17 S2 Ni1 106.37(11) . . ?
Ni2 S2 Ni1 91.98(3) . . ?
C39 O1 Ni1 133.0(2) . . ?
C39 O2 Ni2 132.6(2) . . ?
C8 N1 C9 109.5(3) . . ?
C8 N1 C7 106.6(3) . . ?
C9 N1 C7 106.1(3) . . ?
C8 N1 Ni1 117.3(2) . . ?
C9 N1 Ni1 105.5(2) . . ?
C7 N1 Ni1 111.27(19) . . ?
C11 N2 C10 107.6(3) . . ?
C11 N2 C12 107.9(3) . . ?
C10 N2 C12 110.8(3) . . ?
C11 N2 Ni1 114.3(2) . . ?
C10 N2 Ni1 107.8(2) . . ?
C12 N2 Ni1 108.4(2) . . ?
C14 N3 C13 109.9(3) . . ?
C14 N3 C15 107.0(3) . . ?
C13 N3 C15 106.5(3) . . ?
C14 N3 Ni1 116.7(2) . . ?
C13 N3 Ni1 103.0(2) . . ?
C15 N3 Ni1 113.2(2) . . ?
C24 N4 C23 109.0(3) . . ?
C24 N4 C22 106.8(3) . . ?
C23 N4 C22 107.9(3) . . ?
C24 N4 Ni2 103.4(2) . . ?
C23 N4 Ni2 116.3(2) . . ?
C22 N4 Ni2 112.9(2) . . ?
C27 N5 C26 107.3(3) . . ?
C27 N5 C25 110.6(3) . . ?
C26 N5 C25 109.4(3) . . ?
C27 N5 Ni2 107.4(2) . . ?
C26 N5 Ni2 114.0(2) . . ?
C25 N5 Ni2 108.2(2) . . ?
C29 N6 C30 107.4(3) . . ?
C29 N6 C28 110.7(3) . . ?
C30 N6 C28 105.3(3) . . ?
C29 N6 Ni2 115.9(2) . . ?
C30 N6 Ni2 110.33(19) . . ?
C28 N6 Ni2 106.63(19) . . ?
C2 C1 C6 118.2(3) . . ?
C2 C1 S1 121.5(3) . . ?
C6 C1 S1 120.2(2) . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 C7 120.3(3) . . ?
C1 C2 C7 119.0(3) . . ?
C4 C3 C2 122.3(3) . . ?
C3 C4 C5 116.5(3) . . ?
C3 C4 C31 124.4(3) . . ?
C5 C4 C31 119.0(3) . . ?
C6 C5 C4 122.9(3) . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 C30 120.0(3) . . ?
C1 C6 C30 119.7(3) . . ?
N1 C7 C2 117.7(3) . . ?
N1 C9 C10 110.3(3) . . ?
N2 C10 C9 113.0(3) . . ?
N2 C12 C13 113.9(3) . . ?
N3 C13 C12 111.4(3) . . ?
N3 C15 C16 116.9(3) . . ?
C21 C16 C17 119.3(3) . . ?
C21 C16 C15 120.6(3) . . ?
C17 C16 C15 119.3(3) . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 S2 121.0(3) . . ?
C16 C17 S2 120.4(3) . . ?
C19 C18 C17 120.1(3) . . ?
C19 C18 C22 119.8(3) . . ?
C17 C18 C22 119.6(3) . . ?
C18 C19 C20 122.5(3) . . ?
C19 C20 C21 116.4(3) . . ?
C19 C20 C35 122.5(3) . . ?
C21 C20 C35 120.9(3) . . ?
C16 C21 C20 123.1(3) . . ?
N4 C22 C18 115.8(3) . . ?
N4 C24 C25 111.1(3) . . ?
N5 C25 C24 113.6(3) . . ?
N5 C27 C28 111.9(3) . . ?
N6 C28 C27 109.9(3) . . ?
N6 C30 C6 117.4(3) . . ?
C32 C31 C4 112.5(3) . . ?
C32 C31 C34 109.0(3) . . ?
C4 C31 C34 109.8(3) . . ?
C32 C31 C33 108.0(3) . . ?
C4 C31 C33 108.4(3) . . ?
C34 C31 C33 109.1(3) . . ?
C36 C35 C20 113.2(3) . . ?
C36 C35 C38 108.7(4) . . ?
C20 C35 C38 108.8(3) . . ?
C36 C35 C37 108.0(3) . . ?
C20 C35 C37 109.3(3) . . ?
C38 C35 C37 108.8(3) . . ?
O1 C39 O2 130.5(3) . . ?
O1 C39 C40 114.1(3) . . ?
O2 C39 C40 115.3(3) . . ?
C39 C40 Cl1 113.5(3) . . ?
C39 C40 Cl2 111.9(2) . . ?
Cl1 C40 Cl2 109.1(2) . . ?
C39 C40 Cl3 105.1(3) . . ?
Cl1 C40 Cl3 108.5(2) . . ?
Cl2 C40 Cl3 108.6(2) . . ?
C201 B C301 112.6(3) . . ?
C201 B C401 104.4(3) . . ?
C301 B C401 111.6(3) . . ?
C201 B C101 113.1(3) . . ?
C301 B C101 102.9(3) . . ?
C401 B C101 112.6(3) . . ?
C102 C101 C106 114.3(4) . . ?
C102 C101 B 123.6(3) . . ?
C106 C101 B 121.5(3) . . ?
C103 C102 C101 123.3(4) . . ?
C104 C103 C102 120.1(4) . . ?
C105 C104 C103 119.1(4) . . ?
C104 C105 C106 120.1(4) . . ?
C105 C106 C101 123.1(4) . . ?
C206 C201 C202 114.1(3) . . ?
C206 C201 B 121.9(3) . . ?
C202 C201 B 123.6(3) . . ?
C203 C202 C201 122.9(4) . . ?
C204 C203 C202 120.4(4) . . ?
C205 C204 C203 118.8(4) . . ?
C204 C205 C206 120.1(4) . . ?
C205 C206 C201 123.6(4) . . ?
C302 C301 C306 113.9(4) . . ?
C302 C301 B 122.5(3) . . ?
C306 C301 B 123.3(3) . . ?
C303 C302 C301 124.2(4) . . ?
C304 C303 C302 119.1(4) . . ?
C305 C304 C303 120.2(4) . . ?
C304 C305 C306 119.4(4) . . ?
C305 C306 C301 123.2(4) . . ?
C406 C401 C402 114.7(4) . . ?
C406 C401 B 122.6(3) . . ?
C402 C401 B 122.5(4) . . ?
C403 C402 C401 122.9(4) . . ?
C404 C403 C402 120.8(5) . . ?
C405 C404 C403 118.6(4) . . ?
C404 C405 C406 119.9(5) . . ?
C401 C406 C405 123.1(4) . . ?
N7 C41 C42 179.4(9) . . ?
N8 C43 C44 179.2(8) . . ?
O3 C45 C46 105.3(12) . . ?
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 2.014(2) . ?
Ni1 N2 2.136(3) . ?
Ni1 N3 2.255(3) . ?
Ni1 N1 2.277(3) . ?
Ni1 S2 2.4532(10) . ?
Ni1 S1 2.4894(10) . ?
Ni2 O2 2.033(2) . ?
Ni2 N5 2.166(3) . ?
Ni2 N4 2.214(3) . ?
Ni2 N6 2.294(3) . ?
Ni2 S2 2.4464(10) . ?
Ni2 S1 2.4987(11) . ?
S1 C1 1.763(3) . ?
S2 C17 1.761(3) . ?
Cl1 C40 1.754(4) . ?
Cl2 C40 1.757(4) . ?
Cl3 C40 1.776(4) . ?
O1 C39 1.235(4) . ?
O2 C39 1.254(4) . ?
N1 C8 1.478(4) . ?
N1 C9 1.490(4) . ?
N1 C7 1.498(4) . ?
N2 C11 1.481(4) . ?
N2 C10 1.483(4) . ?
N2 C12 1.484(4) . ?
N3 C14 1.482(4) . ?
N3 C13 1.486(4) . ?
N3 C15 1.487(4) . ?
N4 C24 1.480(4) . ?
N4 C23 1.485(4) . ?
N4 C22 1.489(4) . ?
N5 C27 1.477(4) . ?
N5 C26 1.485(4) . ?
N5 C25 1.488(4) . ?
N6 C29 1.481(4) . ?
N6 C30 1.487(4) . ?
N6 C28 1.492(4) . ?
C1 C2 1.399(4) . ?
C1 C6 1.408(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.503(4) . ?
C3 C4 1.389(5) . ?
C4 C5 1.393(5) . ?
C4 C31 1.529(5) . ?
C5 C6 1.382(4) . ?
C6 C30 1.493(4) . ?
C9 C10 1.504(5) . ?
C12 C13 1.507(5) . ?
C15 C16 1.502(5) . ?
C16 C21 1.385(4) . ?
C16 C17 1.413(4) . ?
C17 C18 1.398(4) . ?
C18 C19 1.389(4) . ?
C18 C22 1.500(4) . ?
C19 C20 1.391(5) . ?
C20 C21 1.391(5) . ?
C20 C35 1.525(5) . ?
C24 C25 1.515(5) . ?
C27 C28 1.498(5) . ?
C31 C32 1.523(5) . ?
C31 C34 1.530(5) . ?
C31 C33 1.545(5) . ?
C35 C36 1.517(5) . ?
C35 C38 1.533(5) . ?
C35 C37 1.539(5) . ?
C39 C40 1.553(5) . ?
B C201 1.633(5) . ?
B C301 1.638(5) . ?
B C401 1.642(5) . ?
B C101 1.654(5) . ?
C101 C102 1.395(5) . ?
C101 C106 1.400(5) . ?
C102 C103 1.383(5) . ?
C103 C104 1.374(6) . ?
C104 C105 1.369(6) . ?
C105 C106 1.388(5) . ?
C201 C206 1.400(5) . ?
C201 C202 1.401(5) . ?
C202 C203 1.386(5) . ?
C203 C204 1.380(5) . ?
C204 C205 1.367(5) . ?
C205 C206 1.386(5) . ?
C301 C302 1.395(5) . ?
C301 C306 1.401(5) . ?
C302 C303 1.377(5) . ?
C303 C304 1.371(6) . ?
C304 C305 1.369(6) . ?
C305 C306 1.388(6) . ?
C401 C406 1.393(5) . ?
C401 C402 1.398(5) . ?
C402 C403 1.377(6) . ?
C403 C404 1.376(7) . ?
C404 C405 1.376(7) . ?
C405 C406 1.394(5) . ?
N7 C41 1.140(7) . ?
C41 C42 1.389(7) . ?
N8 C43 1.117(6) . ?
C43 C44 1.439(7) . ?
O3 C45 1.226(14) . ?
C45 C46 1.363(13) . ?
