#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/71/4317164.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_4317164
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-O2CCCH)][BPh4].1.5CH3CN 
;
_chemical_formula_sum            'C68 H89.5 B N7.5 Ni2 O2 S2'
_chemical_formula_weight         1236.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 112.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.208(4)
_cell_length_b                   18.136(4)
_cell_length_c                   20.086(4)
_cell_measurement_temperature    213(2)
_cell_volume                     6476(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.1162
_diffrn_reflns_av_sigmaI/netI    0.2419
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41077
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.8081
_exptl_absorpt_correction_T_min  0.7268
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         15584
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.2141
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0587P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                5102
_reflns_number_total             15584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101574a_si_001_4.cif
_cod_data_source_block           5
_cod_original_cell_volume        6476(2)
_cod_original_formula_sum        'C68 H89.50 B N7.50 Ni2 O2 S2'
_cod_database_code               4317164
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.55838(4) 0.06843(4) 0.19883(4) 0.02766(18) Uani 1 1 d . . .
Ni2 Ni 0.41773(4) 0.20249(4) 0.14462(4) 0.03013(19) Uani 1 1 d . . .
S1 S 0.46421(7) 0.11013(8) 0.08048(7) 0.0305(3) Uani 1 1 d . . .
S2 S 0.55276(7) 0.20086(8) 0.22283(8) 0.0350(4) Uani 1 1 d . . .
O1 O 0.48085(19) 0.0418(2) 0.23975(19) 0.0360(10) Uani 1 1 d . . .
O2 O 0.38590(19) 0.1243(2) 0.19834(19) 0.0327(9) Uani 1 1 d . . .
N1 N 0.5501(2) -0.0487(2) 0.1602(2) 0.0296(11) Uani 1 1 d . . .
N2 N 0.6531(2) 0.0703(3) 0.1685(2) 0.0305(10) Uani 1 1 d . . .
N3 N 0.6494(2) 0.0506(3) 0.3105(2) 0.0371(12) Uani 1 1 d . . .
N4 N 0.3936(2) 0.2840(3) 0.2156(3) 0.0383(12) Uani 1 1 d . . .
N5 N 0.4208(2) 0.2978(3) 0.0834(3) 0.0385(12) Uani 1 1 d . . .
N6 N 0.2982(2) 0.1961(2) 0.0543(2) 0.0324(11) Uani 1 1 d . . .
C1 C 0.3943(3) 0.0415(3) 0.0626(3) 0.0272(12) Uani 1 1 d . . .
C2 C 0.3184(3) 0.0604(3) 0.0342(3) 0.0302(13) Uani 1 1 d . . .
C3 C 0.2642(3) 0.0079(3) 0.0307(3) 0.0349(14) Uani 1 1 d . . .
H3 H 0.2133 0.0217 0.0131 0.042 Uiso 1 1 calc R . .
C4 C 0.2837(3) -0.0646(3) 0.0527(3) 0.0358(14) Uani 1 1 d . A .
C5 C 0.3592(3) -0.0842(3) 0.0723(3) 0.0346(14) Uani 1 1 d . . .
H5 H 0.3734 -0.1336 0.0835 0.042 Uiso 1 1 calc R . .
C6 C 0.4137(3) -0.0325(3) 0.0759(3) 0.0295(13) Uani 1 1 d . . .
C7 C 0.4919(3) -0.0567(3) 0.0863(3) 0.0330(14) Uani 1 1 d . . .
H7A H 0.4899 -0.1087 0.0723 0.040 Uiso 1 1 calc R . .
H7B H 0.5082 -0.0283 0.0532 0.040 Uiso 1 1 calc R . .
C8 C 0.5330(3) -0.1058(3) 0.2042(3) 0.0409(15) Uani 1 1 d . . .
H8A H 0.5265 -0.1530 0.1799 0.061 Uiso 1 1 calc R . .
H8B H 0.4871 -0.0928 0.2109 0.061 Uiso 1 1 calc R . .
H8C H 0.5742 -0.1090 0.2507 0.061 Uiso 1 1 calc R . .
C9 C 0.6236(3) -0.0639(3) 0.1550(3) 0.0397(15) Uani 1 1 d . . .
H9A H 0.6182 -0.1055 0.1222 0.048 Uiso 1 1 calc R . .
H9B H 0.6602 -0.0780 0.2024 0.048 Uiso 1 1 calc R . .
C10 C 0.6527(3) 0.0023(3) 0.1279(3) 0.0412(16) Uani 1 1 d . . .
H10A H 0.7040 -0.0078 0.1312 0.049 Uiso 1 1 calc R . .
H10B H 0.6213 0.0102 0.0771 0.049 Uiso 1 1 calc R . .
C11 C 0.6544(3) 0.1336(3) 0.1225(3) 0.0476(17) Uani 1 1 d . . .
H11A H 0.6999 0.1318 0.1124 0.071 Uiso 1 1 calc R . .
H11B H 0.6533 0.1793 0.1472 0.071 Uiso 1 1 calc R . .
H11C H 0.6109 0.1314 0.0777 0.071 Uiso 1 1 calc R . .
C12 C 0.7228(3) 0.0756(4) 0.2355(3) 0.0411(16) Uani 1 1 d . . .
H12A H 0.7316 0.1274 0.2502 0.049 Uiso 1 1 calc R . .
H12B H 0.7659 0.0585 0.2249 0.049 Uiso 1 1 calc R . .
C13 C 0.7183(3) 0.0309(4) 0.2970(3) 0.0462(17) Uani 1 1 d . . .
H13A H 0.7172 -0.0218 0.2856 0.055 Uiso 1 1 calc R . .
H13B H 0.7630 0.0402 0.3405 0.055 Uiso 1 1 calc R . .
C14 C 0.6351(4) -0.0065(4) 0.3570(3) 0.0575(19) Uani 1 1 d . . .
H14A H 0.6324 -0.0547 0.3350 0.086 Uiso 1 1 calc R . .
H14B H 0.5880 0.0040 0.3622 0.086 Uiso 1 1 calc R . .
H14C H 0.6758 -0.0061 0.4039 0.086 Uiso 1 1 calc R . .
C15 C 0.6659(3) 0.1208(3) 0.3529(3) 0.0402(15) Uani 1 1 d . . .
H15A H 0.7055 0.1109 0.4000 0.048 Uiso 1 1 calc R . .
H15B H 0.6860 0.1565 0.3282 0.048 Uiso 1 1 calc R . .
C16 C 0.6010(3) 0.1553(3) 0.3645(3) 0.0393(15) Uani 1 1 d . . .
C17 C 0.5525(3) 0.2013(3) 0.3100(3) 0.0384(14) Uani 1 1 d . . .
C18 C 0.5032(3) 0.2476(3) 0.3274(3) 0.0419(16) Uani 1 1 d . . .
C19 C 0.4965(3) 0.2399(4) 0.3933(3) 0.059(2) Uani 1 1 d . B .
H19 H 0.4625 0.2705 0.4038 0.071 Uiso 1 1 calc R . .
C20 C 0.5383(3) 0.1883(4) 0.4450(3) 0.060(2) Uani 1 1 d . . .
C21 C 0.5926(3) 0.1499(4) 0.4293(3) 0.0545(19) Uani 1 1 d . B .
H21 H 0.6253 0.1186 0.4647 0.065 Uiso 1 1 calc R . .
C22 C 0.4635(3) 0.3080(3) 0.2773(3) 0.0497(17) Uani 1 1 d . . .
H22A H 0.4983 0.3302 0.2578 0.060 Uiso 1 1 calc R . .
H22B H 0.4497 0.3462 0.3046 0.060 Uiso 1 1 calc R . .
C23 C 0.3379(3) 0.2630(3) 0.2467(3) 0.0446(16) Uani 1 1 d . . .
H23A H 0.3571 0.2218 0.2793 0.067 Uiso 1 1 calc R . .
H23B H 0.2912 0.2488 0.2083 0.067 Uiso 1 1 calc R . .
H23C H 0.3288 0.3045 0.2727 0.067 Uiso 1 1 calc R . .
C24 C 0.3637(3) 0.3491(3) 0.1678(3) 0.0439(16) Uani 1 1 d . . .
H24A H 0.3648 0.3926 0.1972 0.053 Uiso 1 1 calc R . .
H24B H 0.3113 0.3400 0.1361 0.053 Uiso 1 1 calc R . .
C25 C 0.4101(4) 0.3638(3) 0.1229(4) 0.0560(19) Uani 1 1 d . . .
H25A H 0.3855 0.4026 0.0880 0.067 Uiso 1 1 calc R . .
H25B H 0.4595 0.3822 0.1544 0.067 Uiso 1 1 calc R . .
C26 C 0.4922(3) 0.3075(4) 0.0722(4) 0.0573(19) Uani 1 1 d . . .
H26A H 0.5006 0.2651 0.0467 0.086 Uiso 1 1 calc R . .
H26B H 0.5336 0.3121 0.1184 0.086 Uiso 1 1 calc R . .
H26C H 0.4893 0.3517 0.0441 0.086 Uiso 1 1 calc R . .
C27 C 0.3598(3) 0.2918(3) 0.0107(3) 0.0480(17) Uani 1 1 d . . .
H27A H 0.3751 0.2569 -0.0184 0.058 Uiso 1 1 calc R . .
H27B H 0.3522 0.3400 -0.0131 0.058 Uiso 1 1 calc R . .
C28 C 0.2860(3) 0.2661(3) 0.0145(3) 0.0436(16) Uani 1 1 d . . .
H28A H 0.2672 0.3035 0.0387 0.052 Uiso 1 1 calc R . .
H28B H 0.2484 0.2593 -0.0343 0.052 Uiso 1 1 calc R . .
C29 C 0.2338(3) 0.1822(3) 0.0757(3) 0.0464(17) Uani 1 1 d . . .
H29A H 0.2268 0.2242 0.1025 0.070 Uiso 1 1 calc R . .
H29B H 0.2436 0.1385 0.1057 0.070 Uiso 1 1 calc R . .
H29C H 0.1886 0.1748 0.0331 0.070 Uiso 1 1 calc R . .
C30 C 0.2957(3) 0.1359(3) 0.0020(3) 0.0360(14) Uani 1 1 d . . .
H30A H 0.3288 0.1498 -0.0229 0.043 Uiso 1 1 calc R . .
H30B H 0.2444 0.1329 -0.0342 0.043 Uiso 1 1 calc R . .
C31 C 0.2237(3) -0.1210(3) 0.0524(3) 0.0427(16) Uani 1 1 d D . .
C32A C 0.1643(6) -0.0874(7) 0.0765(7) 0.068(4) Uani 0.70 1 d PD A 1
H32A H 0.1389 -0.1264 0.0916 0.102 Uiso 0.70 1 calc PR A 1
H32B H 0.1279 -0.0604 0.0368 0.102 Uiso 0.70 1 calc PR A 1
H32C H 0.1883 -0.0541 0.1164 0.102 Uiso 0.70 1 calc PR A 1
C33A C 0.1877(7) -0.1566(6) -0.0207(5) 0.075(4) Uani 0.70 1 d PD A 1
H33A H 0.2216 -0.1934 -0.0267 0.113 Uiso 0.70 1 calc PR A 1
H33B H 0.1775 -0.1194 -0.0578 0.113 Uiso 0.70 1 calc PR A 1
H33C H 0.1410 -0.1801 -0.0245 0.113 Uiso 0.70 1 calc PR A 1
C34A C 0.2606(6) -0.1835(6) 0.1080(5) 0.064(4) Uani 0.70 1 d PD A 1
H34A H 0.2217 -0.2159 0.1110 0.097 Uiso 0.70 1 calc PR A 1
H34B H 0.2880 -0.1619 0.1548 0.097 Uiso 0.70 1 calc PR A 1
H34C H 0.2949 -0.2116 0.0927 0.097 Uiso 0.70 1 calc PR A 1
C32B C 0.1903(15) -0.0906(19) 0.1034(14) 0.077(8) Uani 0.30 1 d PD A 2
H32D H 0.1462 -0.1191 0.0994 0.115 Uiso 0.30 1 calc PR A 2
H32E H 0.1761 -0.0395 0.0914 0.115 Uiso 0.30 1 calc PR A 2
H32F H 0.2272 -0.0936 0.1522 0.115 Uiso 0.30 1 calc PR A 2
C33B C 0.1659(15) -0.1194(14) -0.0245(13) 0.077(8) Uani 0.30 1 d PD A 2
H33D H 0.1910 -0.1272 -0.0577 0.115 Uiso 0.30 1 calc PR A 2
H33E H 0.1409 -0.0718 -0.0340 0.115 Uiso 0.30 1 calc PR A 2
H33F H 0.1291 -0.1580 -0.0307 0.115 Uiso 0.30 1 calc PR A 2
C34B C 0.2518(16) -0.1988(13) 0.0721(13) 0.077(8) Uani 0.30 1 d PD A 2
H34D H 0.2462 -0.2260 0.0289 0.115 Uiso 0.30 1 calc PR A 2
H34E H 0.2227 -0.2226 0.0963 0.115 Uiso 0.30 1 calc PR A 2
H34F H 0.3044 -0.1977 0.1039 0.115 Uiso 0.30 1 calc PR A 2
C35A C 0.5233(9) 0.1548(8) 0.5162(10) 0.050(5) Uani 0.533(9) 1 d PD B 1
C36A C 0.5931(14) 0.1672(12) 0.5818(18) 0.061(6) Uani 0.533(9) 1 d PD B 1
H36A H 0.5896 0.1400 0.6220 0.092 Uiso 0.533(9) 1 calc PR B 1
H36B H 0.5984 0.2194 0.5932 0.092 Uiso 0.533(9) 1 calc PR B 1
H36C H 0.6366 0.1503 0.5726 0.092 Uiso 0.533(9) 1 calc PR B 1
C37A C 0.4595(9) 0.1991(11) 0.5219(8) 0.088(8) Uani 0.533(9) 1 d PD B 1
H37A H 0.4249 0.2127 0.4741 0.132 Uiso 0.533(9) 1 calc PR B 1
H37B H 0.4793 0.2434 0.5497 0.132 Uiso 0.533(9) 1 calc PR B 1
H37C H 0.4333 0.1699 0.5455 0.132 Uiso 0.533(9) 1 calc PR B 1
C38A C 0.5026(8) 0.0739(8) 0.5113(8) 0.084(6) Uani 0.533(9) 1 d PD B 1
H38A H 0.5389 0.0456 0.4990 0.126 Uiso 0.533(9) 1 calc PR B 1
H38B H 0.4529 0.0669 0.4745 0.126 Uiso 0.533(9) 1 calc PR B 1
H38C H 0.5029 0.0573 0.5573 0.126 Uiso 0.533(9) 1 calc PR B 1
C35B C 0.5228(9) 0.1937(8) 0.5109(11) 0.044(5) Uani 0.467(9) 1 d PD B 2
C36B C 0.5814(15) 0.1423(12) 0.566(2) 0.089(11) Uani 0.467(9) 1 d PD B 2
H36D H 0.5717 0.0916 0.5500 0.133 Uiso 0.467(9) 1 calc PR B 2
H36E H 0.5772 0.1471 0.6127 0.133 Uiso 0.467(9) 1 calc PR B 2
H36F H 0.6316 0.1562 0.5705 0.133 Uiso 0.467(9) 1 calc PR B 2
C37B C 0.4426(10) 0.1595(12) 0.4890(9) 0.092(10) Uani 0.467(9) 1 d PD B 2
H37D H 0.4050 0.1971 0.4667 0.137 Uiso 0.467(9) 1 calc PR B 2
H37E H 0.4361 0.1406 0.5314 0.137 Uiso 0.467(9) 1 calc PR B 2
H37F H 0.4368 0.1196 0.4552 0.137 Uiso 0.467(9) 1 calc PR B 2
C38B C 0.5248(8) 0.2712(8) 0.5447(7) 0.062(5) Uani 0.467(9) 1 d PD B 2
H38D H 0.5766 0.2877 0.5673 0.092 Uiso 0.467(9) 1 calc PR B 2
H38E H 0.5024 0.2685 0.5806 0.092 Uiso 0.467(9) 1 calc PR B 2
H38F H 0.4967 0.3058 0.5074 0.092 Uiso 0.467(9) 1 calc PR B 2
C39 C 0.4185(3) 0.0682(3) 0.2325(3) 0.0314(13) Uani 1 1 d . . .
C40 C 0.3786(4) 0.0289(4) 0.2714(4) 0.056(2) Uani 1 1 d . . .
C41 C 0.3483(4) -0.0010(5) 0.3027(5) 0.099(3) Uani 1 1 d . . .
H41 H 0.3233 -0.0256 0.3285 0.118 Uiso 1 1 calc R . .
B B 0.5127(3) 0.6161(4) 0.1931(3) 0.0307(15) Uani 1 1 d . . .
C101 C 0.5591(3) 0.5388(3) 0.2200(3) 0.0300(13) Uani 1 1 d . . .
C102 C 0.5871(3) 0.4951(3) 0.1767(3) 0.0344(14) Uani 1 1 d . . .
H102 H 0.5771 0.5098 0.1291 0.041 Uiso 1 1 calc R . .
C103 C 0.6281(3) 0.4320(3) 0.2025(3) 0.0434(16) Uani 1 1 d . . .
H103 H 0.6456 0.4046 0.1722 0.052 Uiso 1 1 calc R . .
C104 C 0.6442(3) 0.4081(3) 0.2722(4) 0.0478(17) Uani 1 1 d . . .
H104 H 0.6707 0.3640 0.2891 0.057 Uiso 1 1 calc R . .
C105 C 0.6203(3) 0.4508(3) 0.3160(3) 0.0469(17) Uani 1 1 d . . .
H105 H 0.6326 0.4372 0.3642 0.056 Uiso 1 1 calc R . .
C106 C 0.5791(3) 0.5127(3) 0.2899(3) 0.0415(15) Uani 1 1 d . . .
H106 H 0.5629 0.5398 0.3213 0.050 Uiso 1 1 calc R . .
C201 C 0.4611(3) 0.6225(3) 0.1073(3) 0.0316(13) Uani 1 1 d . . .
C202 C 0.4355(3) 0.6913(3) 0.0765(3) 0.0374(14) Uani 1 1 d . . .
H202 H 0.4559 0.7335 0.1042 0.045 Uiso 1 1 calc R . .
C203 C 0.3818(3) 0.7016(4) 0.0079(3) 0.0475(16) Uani 1 1 d . . .
H203 H 0.3655 0.7491 -0.0097 0.057 Uiso 1 1 calc R . .
C204 C 0.3530(3) 0.6399(4) -0.0341(3) 0.0505(18) Uani 1 1 d . . .
H204 H 0.3170 0.6453 -0.0811 0.061 Uiso 1 1 calc R . .
C205 C 0.3769(3) 0.5710(4) -0.0072(3) 0.0534(18) Uani 1 1 d . . .
H205 H 0.3573 0.5293 -0.0359 0.064 Uiso 1 1 calc R . .
C206 C 0.4300(3) 0.5623(3) 0.0622(3) 0.0388(15) Uani 1 1 d . . .
H206 H 0.4455 0.5144 0.0794 0.047 Uiso 1 1 calc R . .
C301 C 0.5779(3) 0.6799(3) 0.2196(3) 0.0311(13) Uani 1 1 d . . .
C302 C 0.6160(3) 0.7016(3) 0.1759(3) 0.0361(14) Uani 1 1 d . . .
H302 H 0.5992 0.6839 0.1284 0.043 Uiso 1 1 calc R . .
C303 C 0.6778(3) 0.7482(3) 0.2000(3) 0.0469(16) Uani 1 1 d . . .
H303 H 0.7019 0.7609 0.1687 0.056 Uiso 1 1 calc R . .
C304 C 0.7041(3) 0.7758(3) 0.2678(4) 0.0499(18) Uani 1 1 d . . .
H304 H 0.7462 0.8071 0.2838 0.060 Uiso 1 1 calc R . .
C305 C 0.6679(3) 0.7570(3) 0.3127(3) 0.0502(17) Uani 1 1 d . . .
H305 H 0.6853 0.7756 0.3599 0.060 Uiso 1 1 calc R . .
C306 C 0.6052(3) 0.7103(3) 0.2886(3) 0.0452(16) Uani 1 1 d . . .
H306 H 0.5807 0.6991 0.3199 0.054 Uiso 1 1 calc R . .
C401 C 0.4483(3) 0.6232(3) 0.2289(3) 0.0345(14) Uani 1 1 d . . .
C402 C 0.4192(3) 0.6911(3) 0.2417(3) 0.0412(15) Uani 1 1 d . . .
H402 H 0.4424 0.7352 0.2366 0.049 Uiso 1 1 calc R . .
C403 C 0.3577(4) 0.6945(4) 0.2614(3) 0.0528(18) Uani 1 1 d . . .
H403 H 0.3408 0.7408 0.2700 0.063 Uiso 1 1 calc R . .
C404 C 0.3207(4) 0.6324(5) 0.2687(4) 0.066(2) Uani 1 1 d . . .
H404 H 0.2790 0.6356 0.2823 0.079 Uiso 1 1 calc R . .
C405 C 0.3465(4) 0.5640(4) 0.2553(4) 0.066(2) Uani 1 1 d . . .
H405 H 0.3224 0.5204 0.2599 0.079 Uiso 1 1 calc R . .
C406 C 0.4086(3) 0.5612(4) 0.2351(3) 0.0474(17) Uani 1 1 d . . .
H406 H 0.4243 0.5148 0.2251 0.057 Uiso 1 1 calc R . .
N7 N 0.2389(3) 0.4646(4) 0.0614(3) 0.0667(18) Uani 1 1 d D . .
C42 C 0.2440(3) 0.5268(4) 0.0677(3) 0.0481(17) Uani 1 1 d D . .
C43 C 0.2501(3) 0.6064(4) 0.0775(4) 0.064(2) Uani 1 1 d D . .
H43A H 0.2161 0.6228 0.0999 0.096 Uiso 1 1 calc R . .
H43B H 0.2369 0.6302 0.0311 0.096 Uiso 1 1 calc R . .
H43C H 0.3013 0.6192 0.1080 0.096 Uiso 1 1 calc R . .
N8 N 0.0505(9) 0.0749(10) -0.0398(8) 0.114(7) Uani 0.50 1 d PD . .
C44 C 0.0421(8) 0.0825(10) 0.0134(9) 0.082(5) Uani 0.50 1 d PD . .
C45 C 0.0256(9) 0.0750(11) 0.0785(7) 0.111(8) Uani 0.50 1 d PD . .
H45A H 0.0118 0.0244 0.0831 0.166 Uiso 0.50 1 calc PR . .
H45B H -0.0157 0.1075 0.0752 0.166 Uiso 0.50 1 calc PR . .
H45C H 0.0698 0.0883 0.1202 0.166 Uiso 0.50 1 calc PR . .
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'
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 165.06(16) . . ?
O1 Ni1 N1 86.98(15) . . ?
N2 Ni1 N1 82.69(16) . . ?
O1 Ni1 N3 88.56(15) . . ?
N2 Ni1 N3 82.18(16) . . ?
N1 Ni1 N3 97.64(16) . . ?
O1 Ni1 S2 93.46(11) . . ?
N2 Ni1 S2 98.40(13) . . ?
N1 Ni1 S2 171.23(12) . . ?
N3 Ni1 S2 91.13(12) . . ?
O1 Ni1 S1 94.61(11) . . ?
N2 Ni1 S1 96.42(12) . . ?
N1 Ni1 S1 91.53(11) . . ?
N3 Ni1 S1 170.44(13) . . ?
S2 Ni1 S1 79.70(5) . . ?
O2 Ni2 N5 163.70(15) . . ?
O2 Ni2 N4 86.88(16) . . ?
N5 Ni2 N4 83.61(18) . . ?
O2 Ni2 N6 88.44(15) . . ?
N5 Ni2 N6 79.95(16) . . ?
N4 Ni2 N6 98.56(16) . . ?
O2 Ni2 S2 96.29(11) . . ?
N5 Ni2 S2 97.14(13) . . ?
N4 Ni2 S2 91.38(12) . . ?
N6 Ni2 S2 169.22(11) . . ?
O2 Ni2 S1 92.57(11) . . ?
N5 Ni2 S1 98.85(13) . . ?
N4 Ni2 S1 171.13(12) . . ?
N6 Ni2 S1 90.27(12) . . ?
S2 Ni2 S1 79.88(5) . . ?
C1 S1 Ni2 100.73(17) . . ?
C1 S1 Ni1 101.60(18) . . ?
Ni2 S1 Ni1 89.05(5) . . ?
C17 S2 Ni1 102.5(2) . . ?
C17 S2 Ni2 103.59(18) . . ?
Ni1 S2 Ni2 90.03(5) . . ?
C39 O1 Ni1 133.3(4) . . ?
C39 O2 Ni2 132.4(3) . . ?
C8 N1 C9 110.3(4) . . ?
C8 N1 C7 106.0(4) . . ?
C9 N1 C7 106.7(4) . . ?
C8 N1 Ni1 117.3(3) . . ?
C9 N1 Ni1 104.8(3) . . ?
C7 N1 Ni1 111.4(3) . . ?
C10 N2 C11 107.5(4) . . ?
C10 N2 C12 111.4(4) . . ?
C11 N2 C12 106.9(4) . . ?
C10 N2 Ni1 108.6(3) . . ?
C11 N2 Ni1 114.2(3) . . ?
C12 N2 Ni1 108.3(3) . . ?
C14 N3 C13 109.5(5) . . ?
C14 N3 C15 106.5(4) . . ?
C13 N3 C15 107.2(4) . . ?
C14 N3 Ni1 117.4(3) . . ?
C13 N3 Ni1 105.0(3) . . ?
C15 N3 Ni1 110.9(3) . . ?
C23 N4 C24 108.2(4) . . ?
C23 N4 C22 106.8(4) . . ?
C24 N4 C22 107.9(5) . . ?
C23 N4 Ni2 117.3(3) . . ?
C24 N4 Ni2 103.7(3) . . ?
C22 N4 Ni2 112.5(3) . . ?
C26 N5 C27 106.9(4) . . ?
C26 N5 C25 107.9(5) . . ?
C27 N5 C25 111.3(5) . . ?
C26 N5 Ni2 114.4(4) . . ?
C27 N5 Ni2 108.8(3) . . ?
C25 N5 Ni2 107.6(3) . . ?
C28 N6 C29 109.2(4) . . ?
C28 N6 C30 106.9(4) . . ?
C29 N6 C30 105.7(4) . . ?
C28 N6 Ni2 106.7(3) . . ?
C29 N6 Ni2 118.0(3) . . ?
C30 N6 Ni2 109.9(3) . . ?
C2 C1 C6 118.5(5) . . ?
C2 C1 S1 120.6(4) . . ?
C6 C1 S1 120.9(4) . . ?
C3 C2 C1 120.0(5) . . ?
C3 C2 C30 120.7(5) . . ?
C1 C2 C30 119.2(5) . . ?
C4 C3 C2 121.5(5) . . ?
C3 C4 C5 117.1(5) . . ?
C3 C4 C31 121.0(5) . . ?
C5 C4 C31 121.9(5) . . ?
C6 C5 C4 121.8(5) . . ?
C5 C6 C1 120.0(5) . . ?
C5 C6 C7 120.4(5) . . ?
C1 C6 C7 119.3(5) . . ?
N1 C7 C6 116.3(4) . . ?
N1 C9 C10 111.7(4) . . ?
N2 C10 C9 113.0(4) . . ?
N2 C12 C13 113.1(5) . . ?
N3 C13 C12 110.5(5) . . ?
C16 C15 N3 115.9(5) . . ?
C21 C16 C17 119.7(5) . . ?
C21 C16 C15 121.6(6) . . ?
C17 C16 C15 118.3(5) . . ?
C18 C17 C16 118.1(5) . . ?
C18 C17 S2 120.6(5) . . ?
C16 C17 S2 121.4(4) . . ?
C19 C18 C17 119.5(6) . . ?
C19 C18 C22 120.8(6) . . ?
C17 C18 C22 119.5(5) . . ?
C18 C19 C20 122.8(6) . . ?
C21 C20 C19 115.8(6) . . ?
C21 C20 C35B 131.8(9) . . ?
C19 C20 C35B 111.7(8) . . ?
C21 C20 C35A 113.5(7) . . ?
C19 C20 C35A 129.7(7) . . ?
C35B C20 C35A 25.1(7) . . ?
C16 C21 C20 123.2(6) . . ?
C18 C22 N4 114.4(5) . . ?
N4 C24 C25 110.6(5) . . ?
N5 C25 C24 114.1(5) . . ?
N5 C27 C28 112.1(4) . . ?
N6 C28 C27 109.4(4) . . ?
N6 C30 C2 115.8(4) . . ?
C32B C31 C33A 131.5(13) . . ?
C32B C31 C34B 111.4(12) . . ?
C33A C31 C34B 80.9(10) . . ?
C32B C31 C32A 22.2(12) . . ?
C33A C31 C32A 110.9(7) . . ?
C34B C31 C32A 121.7(14) . . ?
C32B C31 C33B 110.3(11) . . ?
C33A C31 C33B 30.0(11) . . ?
C34B C31 C33B 109.6(10) . . ?
C32A C31 C33B 88.2(12) . . ?
C32B C31 C4 105.4(14) . . ?
C33A C31 C4 110.8(7) . . ?
C34B C31 C4 115.3(12) . . ?
C32A C31 C4 112.5(7) . . ?
C33B C31 C4 104.4(12) . . ?
C32B C31 C34A 88.5(13) . . ?
C33A C31 C34A 107.5(6) . . ?
C34B C31 C34A 27.4(10) . . ?
C32A C31 C34A 104.7(6) . . ?
C33B C31 C34A 134.3(12) . . ?
C4 C31 C34A 110.1(6) . . ?
C36A C35A C37A 109.6(14) . . ?
C36A C35A C38A 109.1(13) . . ?
C37A C35A C38A 108.8(13) . . ?
C36A C35A C20 108(2) . . ?
C37A C35A C20 106.2(12) . . ?
C38A C35A C20 115.0(12) . . ?
C20 C35B C36B 105(2) . . ?
C20 C35B C38B 118.3(13) . . ?
C36B C35B C38B 109.7(14) . . ?
C20 C35B C37B 103.6(13) . . ?
C36B C35B C37B 109.5(14) . . ?
C38B C35B C37B 110.0(13) . . ?
O1 C39 O2 129.5(5) . . ?
O1 C39 C40 114.9(5) . . ?
O2 C39 C40 115.5(5) . . ?
C41 C40 C39 178.8(9) . . ?
C201 B C301 112.1(5) . . ?
C201 B C101 116.4(5) . . ?
C301 B C101 104.1(4) . . ?
C201 B C401 101.5(4) . . ?
C301 B C401 114.2(5) . . ?
C101 B C401 109.0(4) . . ?
C106 C101 C102 113.8(5) . . ?
C106 C101 B 122.1(5) . . ?
C102 C101 B 124.0(5) . . ?
C103 C102 C101 122.0(6) . . ?
C102 C103 C104 121.2(6) . . ?
C105 C104 C103 118.0(6) . . ?
C106 C105 C104 120.4(6) . . ?
C105 C106 C101 124.6(6) . . ?
C202 C201 C206 114.7(5) . . ?
C202 C201 B 120.1(5) . . ?
C206 C201 B 124.5(5) . . ?
C203 C202 C201 124.4(6) . . ?
C202 C203 C204 118.2(6) . . ?
C205 C204 C203 120.0(6) . . ?
C204 C205 C206 120.6(6) . . ?
C205 C206 C201 122.1(6) . . ?
C302 C301 C306 115.1(5) . . ?
C302 C301 B 120.8(5) . . ?
C306 C301 B 123.7(5) . . ?
C303 C302 C301 122.4(6) . . ?
C304 C303 C302 121.3(6) . . ?
C303 C304 C305 118.6(6) . . ?
C304 C305 C306 120.4(6) . . ?
C305 C306 C301 122.2(6) . . ?
C406 C401 C402 114.8(5) . . ?
C406 C401 B 120.1(5) . . ?
C402 C401 B 123.9(5) . . ?
C403 C402 C401 122.0(6) . . ?
C404 C403 C402 121.9(6) . . ?
C403 C404 C405 118.1(6) . . ?
C404 C405 C406 119.5(7) . . ?
C401 C406 C405 123.6(6) . . ?
N7 C42 C43 178.5(8) . . ?
N8 C44 C45 167(2) . . ?
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(3) . ?
Ni1 N2 2.127(4) . ?
Ni1 N1 2.247(4) . ?
Ni1 N3 2.284(5) . ?
Ni1 S2 2.4601(17) . ?
Ni1 S1 2.4975(18) . ?
Ni2 O2 2.012(4) . ?
Ni2 N5 2.135(5) . ?
Ni2 N4 2.221(4) . ?
Ni2 N6 2.329(4) . ?
Ni2 S2 2.4716(17) . ?
Ni2 S1 2.4768(16) . ?
S1 C1 1.764(5) . ?
S2 C17 1.753(6) . ?
O1 C39 1.246(6) . ?
O2 C39 1.253(6) . ?
N1 C8 1.476(6) . ?
N1 C9 1.481(6) . ?
N1 C7 1.490(6) . ?
N2 C10 1.477(6) . ?
N2 C11 1.480(6) . ?
N2 C12 1.500(6) . ?
N3 C14 1.489(7) . ?
N3 C13 1.491(6) . ?
N3 C15 1.496(7) . ?
N4 C23 1.479(6) . ?
N4 C24 1.492(7) . ?
N4 C22 1.506(7) . ?
N5 C26 1.482(6) . ?
N5 C27 1.490(7) . ?
N5 C25 1.493(7) . ?
N6 C28 1.471(7) . ?
N6 C29 1.477(6) . ?
N6 C30 1.504(6) . ?
C1 C2 1.392(7) . ?
C1 C6 1.393(7) . ?
C2 C3 1.393(7) . ?
C2 C30 1.506(7) . ?
C3 C4 1.393(7) . ?
C4 C5 1.395(7) . ?
C4 C31 1.539(7) . ?
C5 C6 1.386(7) . ?
C6 C7 1.501(7) . ?
C9 C10 1.511(7) . ?
C12 C13 1.507(8) . ?
C15 C16 1.490(7) . ?
C16 C21 1.376(8) . ?
C16 C17 1.410(8) . ?
C17 C18 1.405(7) . ?
C18 C19 1.384(8) . ?
C18 C22 1.488(8) . ?
C19 C20 1.402(9) . ?
C20 C21 1.387(8) . ?
C20 C35B 1.47(2) . ?
C20 C35A 1.68(2) . ?
C24 C25 1.512(7) . ?
C27 C28 1.519(7) . ?
C31 C32B 1.50(2) . ?
C31 C33A 1.510(10) . ?
C31 C34B 1.51(2) . ?
C31 C32A 1.525(10) . ?
C31 C33B 1.52(2) . ?
C31 C34A 1.561(10) . ?
C35A C36A 1.500(16) . ?
C35A C37A 1.504(16) . ?
C35A C38A 1.513(15) . ?
C35B C36B 1.556(19) . ?
C35B C38B 1.556(17) . ?
C35B C37B 1.561(18) . ?
C39 C40 1.471(8) . ?
C40 C41 1.143(8) . ?
B C201 1.634(8) . ?
B C301 1.639(8) . ?
B C101 1.639(8) . ?
B C401 1.654(8) . ?
C101 C106 1.391(7) . ?
C101 C102 1.423(7) . ?
C102 C103 1.374(7) . ?
C103 C104 1.385(8) . ?
C104 C105 1.375(8) . ?
C105 C106 1.359(7) . ?
C201 C202 1.397(7) . ?
C201 C206 1.400(7) . ?
C202 C203 1.386(7) . ?
C203 C204 1.384(8) . ?
C204 C205 1.369(9) . ?
C205 C206 1.389(7) . ?
C301 C302 1.396(7) . ?
C301 C306 1.396(7) . ?
C302 C303 1.386(7) . ?
C303 C304 1.357(8) . ?
C304 C305 1.374(8) . ?
C305 C306 1.399(8) . ?
C401 C406 1.390(7) . ?
C401 C402 1.415(7) . ?
C402 C403 1.383(7) . ?
C403 C404 1.370(9) . ?
C404 C405 1.398(9) . ?
C405 C406 1.399(8) . ?
N7 C42 1.134(8) . ?
C42 C43 1.456(9) . ?
N8 C44 1.148(14) . ?
C44 C45 1.463(15) . ?
