#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:33:33 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179251 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/71/4317161.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_4317161
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-O2CC10H15)][BPh4].3CH3CN 
;
_chemical_formula_sum            'C79 H108 B N9 Ni2 O2 S2'
_chemical_formula_weight         1408.09
_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                108.79(3)
_cell_angle_beta                 95.30(3)
_cell_angle_gamma                94.59(3)
_cell_formula_units_Z            2
_cell_length_a                   13.173(3)
_cell_length_b                   16.845(3)
_cell_length_c                   18.155(4)
_cell_measurement_temperature    213(2)
_cell_volume                     3771.7(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34786
_diffrn_reflns_theta_full        29.04
_diffrn_reflns_theta_max         29.04
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.8988
_exptl_absorpt_correction_T_min  0.8391
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         17881
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0402P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                9769
_reflns_number_total             17881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101574a_si_001_1.cif
_cod_data_source_block           19
_cod_original_cell_volume        3771.7(14)
_cod_database_code               4317161
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 0.35412(3) 0.32562(2) 0.048210(19) 0.02446(9) Uani 1 1 d . . .
Ni2 Ni 0.40351(3) 0.44011(2) 0.246332(19) 0.02482(9) Uani 1 1 d . . .
S1 S 0.46188(5) 0.45989(4) 0.12695(4) 0.02558(15) Uani 1 1 d . . .
S2 S 0.25003(5) 0.37861(4) 0.15283(4) 0.02700(15) Uani 1 1 d . . .
O1 O 0.42925(13) 0.25552(11) 0.10055(10) 0.0288(4) Uani 1 1 d . . .
O2 O 0.46144(13) 0.32969(11) 0.22943(10) 0.0284(4) Uani 1 1 d . . .
N1 N 0.46644(16) 0.30075(13) -0.04196(12) 0.0282(5) Uani 1 1 d . . .
N2 N 0.27340(16) 0.37128(14) -0.03577(13) 0.0303(5) Uani 1 1 d . . .
N3 N 0.23693(16) 0.21095(14) -0.00960(13) 0.0309(5) Uani 1 1 d . . .
N4 N 0.32304(17) 0.41487(14) 0.34217(12) 0.0310(5) Uani 1 1 d . . .
N5 N 0.35679(17) 0.56411(14) 0.29540(13) 0.0313(5) Uani 1 1 d . . .
N6 N 0.55554(16) 0.50880(13) 0.31822(12) 0.0287(5) Uani 1 1 d . . .
C1 C 0.58443(19) 0.42504(15) 0.13056(15) 0.0240(6) Uani 1 1 d . . .
C2 C 0.65152(19) 0.45146(16) 0.20030(15) 0.0270(6) Uani 1 1 d . . .
C3 C 0.7431(2) 0.41665(17) 0.20346(16) 0.0319(6) Uani 1 1 d . . .
H3 H 0.7873 0.4348 0.2509 0.038 Uiso 1 1 calc R . .
C4 C 0.7718(2) 0.35579(17) 0.13896(16) 0.0315(6) Uani 1 1 d . . .
C5 C 0.7087(2) 0.33710(17) 0.06826(16) 0.0315(6) Uani 1 1 d . . .
H5 H 0.7285 0.2996 0.0226 0.038 Uiso 1 1 calc R . .
C6 C 0.61756(19) 0.37186(16) 0.06291(15) 0.0264(6) Uani 1 1 d . . .
C7 C 0.6306(2) 0.52558(16) 0.26675(15) 0.0297(6) Uani 1 1 d . . .
H7A H 0.6958 0.5510 0.2996 0.036 Uiso 1 1 calc R . .
H7B H 0.6056 0.5676 0.2449 0.036 Uiso 1 1 calc R . .
C8 C 0.6075(2) 0.46550(19) 0.36723(16) 0.0401(7) Uani 1 1 d . . .
H8A H 0.6156 0.4085 0.3350 0.060 Uiso 1 1 calc R . .
H8B H 0.5665 0.4633 0.4084 0.060 Uiso 1 1 calc R . .
H8C H 0.6744 0.4962 0.3905 0.060 Uiso 1 1 calc R . .
C9 C 0.5327(2) 0.59306(18) 0.36812(17) 0.0417(8) Uani 1 1 d . . .
H9A H 0.5953 0.6331 0.3824 0.050 Uiso 1 1 calc R . .
H9B H 0.5093 0.5887 0.4165 0.050 Uiso 1 1 calc R . .
C10 C 0.4512(2) 0.62501(17) 0.32507(17) 0.0409(8) Uani 1 1 d . . .
H10A H 0.4334 0.6782 0.3604 0.049 Uiso 1 1 calc R . .
H10B H 0.4787 0.6366 0.2808 0.049 Uiso 1 1 calc R . .
C11 C 0.2944(2) 0.59229(18) 0.23827(17) 0.0450(8) Uani 1 1 d . . .
H11A H 0.2754 0.6480 0.2646 0.067 Uiso 1 1 calc R . .
H11B H 0.2328 0.5528 0.2165 0.067 Uiso 1 1 calc R . .
H11C H 0.3341 0.5945 0.1964 0.067 Uiso 1 1 calc R . .
C12 C 0.2958(2) 0.56339(19) 0.36008(18) 0.0449(8) Uani 1 1 d . . .
H12A H 0.2229 0.5506 0.3391 0.054 Uiso 1 1 calc R . .
H12B H 0.3055 0.6200 0.3995 0.054 Uiso 1 1 calc R . .
C13 C 0.3239(3) 0.50019(18) 0.39981(16) 0.0437(8) Uani 1 1 d . . .
H13A H 0.3923 0.5188 0.4296 0.052 Uiso 1 1 calc R . .
H13B H 0.2749 0.4980 0.4368 0.052 Uiso 1 1 calc R . .
C14 C 0.3713(2) 0.36052(19) 0.38166(17) 0.0410(8) Uani 1 1 d . . .
H14A H 0.3376 0.3618 0.4273 0.062 Uiso 1 1 calc R . .
H14B H 0.4435 0.3811 0.3980 0.062 Uiso 1 1 calc R . .
H14C H 0.3645 0.3030 0.3456 0.062 Uiso 1 1 calc R . .
C15 C 0.2145(2) 0.37836(18) 0.31557(16) 0.0358(7) Uani 1 1 d . . .
H15A H 0.1787 0.4183 0.2968 0.043 Uiso 1 1 calc R . .
H15B H 0.1832 0.3737 0.3611 0.043 Uiso 1 1 calc R . .
C16 C 0.1957(2) 0.29361(18) 0.25234(16) 0.0324(7) Uani 1 1 d . . .
C17 C 0.20210(19) 0.28978(16) 0.17449(15) 0.0265(6) Uani 1 1 d . . .
C18 C 0.1612(2) 0.21522(17) 0.11433(16) 0.0315(6) Uani 1 1 d . . .
C19 C 0.1258(2) 0.14510(19) 0.13279(18) 0.0389(7) Uani 1 1 d . . .
H19 H 0.1002 0.0951 0.0916 0.047 Uiso 1 1 calc R . .
C20 C 0.1263(2) 0.1456(2) 0.20968(19) 0.0426(8) Uani 1 1 d . A .
C21 C 0.1592(2) 0.2220(2) 0.26809(18) 0.0409(8) Uani 1 1 d . . .
H21 H 0.1568 0.2255 0.3206 0.049 Uiso 1 1 calc R . .
C22 C 0.1442(2) 0.21554(18) 0.03156(15) 0.0330(7) Uani 1 1 d . . .
H22A H 0.0936 0.1675 0.0013 0.040 Uiso 1 1 calc R . .
H22B H 0.1144 0.2671 0.0320 0.040 Uiso 1 1 calc R . .
C23 C 0.2715(2) 0.12757(17) -0.01902(19) 0.0452(8) Uani 1 1 d . . .
H23A H 0.2156 0.0837 -0.0460 0.068 Uiso 1 1 calc R . .
H23B H 0.2927 0.1237 0.0322 0.068 Uiso 1 1 calc R . .
H23C H 0.3289 0.1204 -0.0494 0.068 Uiso 1 1 calc R . .
C24 C 0.2053(2) 0.21727(18) -0.08759(16) 0.0392(7) Uani 1 1 d . . .
H24A H 0.1419 0.1795 -0.1114 0.047 Uiso 1 1 calc R . .
H24B H 0.2586 0.1988 -0.1215 0.047 Uiso 1 1 calc R . .
C25 C 0.1878(2) 0.30602(19) -0.08268(17) 0.0403(8) Uani 1 1 d . . .
H25A H 0.1779 0.3088 -0.1359 0.048 Uiso 1 1 calc R . .
H25B H 0.1244 0.3193 -0.0593 0.048 Uiso 1 1 calc R . .
C26 C 0.2310(2) 0.45172(19) -0.00072(17) 0.0443(8) Uani 1 1 d . . .
H26A H 0.2039 0.4720 -0.0420 0.066 Uiso 1 1 calc R . .
H26B H 0.2848 0.4932 0.0338 0.066 Uiso 1 1 calc R . .
H26C H 0.1763 0.4427 0.0291 0.066 Uiso 1 1 calc R . .
C27 C 0.3487(2) 0.38609(19) -0.08658(16) 0.0368(7) Uani 1 1 d . . .
H27A H 0.3930 0.4388 -0.0584 0.044 Uiso 1 1 calc R . .
H27B H 0.3121 0.3927 -0.1334 0.044 Uiso 1 1 calc R . .
C28 C 0.4141(2) 0.31562(19) -0.11138(15) 0.0369(7) Uani 1 1 d . . .
H28A H 0.3711 0.2640 -0.1446 0.044 Uiso 1 1 calc R . .
H28B H 0.4654 0.3299 -0.1423 0.044 Uiso 1 1 calc R . .
C29 C 0.4999(2) 0.21594(17) -0.06463(18) 0.0428(8) Uani 1 1 d . . .
H29A H 0.4415 0.1743 -0.0908 0.064 Uiso 1 1 calc R . .
H29B H 0.5285 0.2050 -0.0181 0.064 Uiso 1 1 calc R . .
H29C H 0.5516 0.2125 -0.0999 0.064 Uiso 1 1 calc R . .
C30 C 0.5610(2) 0.36211(17) -0.01529(15) 0.0301(6) Uani 1 1 d . . .
H30A H 0.5422 0.4176 -0.0142 0.036 Uiso 1 1 calc R . .
H30B H 0.6083 0.3453 -0.0547 0.036 Uiso 1 1 calc R . .
C31 C 0.8728(2) 0.31780(19) 0.14461(17) 0.0382(7) Uani 1 1 d . . .
C32 C 0.8728(2) 0.2351(2) 0.0775(2) 0.0587(10) Uani 1 1 d . . .
H32A H 0.9333 0.2087 0.0868 0.088 Uiso 1 1 calc R . .
H32B H 0.8736 0.2465 0.0285 0.088 Uiso 1 1 calc R . .
H32C H 0.8117 0.1975 0.0746 0.088 Uiso 1 1 calc R . .
C33 C 0.8920(2) 0.3000(2) 0.2222(2) 0.0577(10) Uani 1 1 d . . .
H33A H 0.8360 0.2609 0.2257 0.087 Uiso 1 1 calc R . .
H33B H 0.8963 0.3524 0.2657 0.087 Uiso 1 1 calc R . .
H33C H 0.9560 0.2755 0.2241 0.087 Uiso 1 1 calc R . .
C34 C 0.9601(2) 0.3815(2) 0.1410(2) 0.0573(10) Uani 1 1 d . . .
H34A H 0.9584 0.4351 0.1819 0.086 Uiso 1 1 calc R . .
H34B H 0.9520 0.3893 0.0902 0.086 Uiso 1 1 calc R . .
H34C H 1.0254 0.3605 0.1485 0.086 Uiso 1 1 calc R . .
C35 C 0.0867(3) 0.0665(2) 0.2273(2) 0.0598(10) Uani 1 1 d . . .
C36A C -0.0287(7) 0.0468(8) 0.1971(9) 0.109(6) Uani 0.583(12) 1 d P A 1
H36A H -0.0385 0.0362 0.1410 0.164 Uiso 0.583(12) 1 calc PR A 1
H36B H -0.0639 0.0945 0.2234 0.164 Uiso 0.583(12) 1 calc PR A 1
H36C H -0.0565 -0.0028 0.2080 0.164 Uiso 0.583(12) 1 calc PR A 1
C37A C 0.1088(11) 0.0715(7) 0.3079(6) 0.110(6) Uani 0.583(12) 1 d P A 1
H37A H 0.0702 0.1131 0.3403 0.165 Uiso 0.583(12) 1 calc PR A 1
H37B H 0.1816 0.0881 0.3250 0.165 Uiso 0.583(12) 1 calc PR A 1
H37C H 0.0894 0.0169 0.3128 0.165 Uiso 0.583(12) 1 calc PR A 1
C38A C 0.1379(9) -0.0117(5) 0.1737(8) 0.105(5) Uani 0.583(12) 1 d P A 1
H38A H 0.1262 -0.0596 0.1917 0.158 Uiso 0.583(12) 1 calc PR A 1
H38B H 0.2111 0.0039 0.1773 0.158 Uiso 0.583(12) 1 calc PR A 1
H38C H 0.1073 -0.0268 0.1196 0.158 Uiso 0.583(12) 1 calc PR A 1
C36B C 0.0178(15) 0.0969(8) 0.3006(10) 0.111(7) Uani 0.417(12) 1 d P A 2
H36D H -0.0422 0.1198 0.2841 0.166 Uiso 0.417(12) 1 calc PR A 2
H36E H 0.0588 0.1399 0.3447 0.166 Uiso 0.417(12) 1 calc PR A 2
H36F H -0.0039 0.0489 0.3162 0.166 Uiso 0.417(12) 1 calc PR A 2
C37B C 0.1793(10) 0.0342(9) 0.2616(12) 0.111(7) Uani 0.417(12) 1 d P A 2
H37D H 0.1573 -0.0187 0.2691 0.166 Uiso 0.417(12) 1 calc PR A 2
H37E H 0.2082 0.0755 0.3116 0.166 Uiso 0.417(12) 1 calc PR A 2
H37F H 0.2307 0.0254 0.2258 0.166 Uiso 0.417(12) 1 calc PR A 2
C38B C 0.0255(17) 0.0030(11) 0.1679(10) 0.128(10) Uani 0.417(12) 1 d P A 2
H38D H -0.0006 -0.0401 0.1884 0.192 Uiso 0.417(12) 1 calc PR A 2
H38E H 0.0658 -0.0219 0.1260 0.192 Uiso 0.417(12) 1 calc PR A 2
H38F H -0.0315 0.0263 0.1478 0.192 Uiso 0.417(12) 1 calc PR A 2
C39 C 0.46346(19) 0.26534(16) 0.17069(16) 0.0274(6) Uani 1 1 d . . .
C40 C 0.5071(2) 0.18985(17) 0.18606(16) 0.0328(7) Uani 1 1 d . . .
C41 C 0.5965(3) 0.2183(2) 0.2511(2) 0.0612(11) Uani 1 1 d . . .
H41A H 0.5743 0.2557 0.2989 0.073 Uiso 1 1 calc R . .
H41B H 0.6517 0.2501 0.2359 0.073 Uiso 1 1 calc R . .
C42 C 0.4224(3) 0.1407(2) 0.2113(2) 0.0641(11) Uani 1 1 d . . .
H42A H 0.3640 0.1213 0.1698 0.077 Uiso 1 1 calc R . .
H42B H 0.3986 0.1776 0.2587 0.077 Uiso 1 1 calc R . .
C43 C 0.5431(3) 0.1309(2) 0.1123(2) 0.0708(12) Uani 1 1 d . . .
H43A H 0.5981 0.1612 0.0956 0.085 Uiso 1 1 calc R . .
H43B H 0.4860 0.1117 0.0697 0.085 Uiso 1 1 calc R . .
C44 C 0.6374(3) 0.1404(2) 0.2674(3) 0.0709(12) Uani 1 1 d . . .
H44 H 0.6960 0.1595 0.3096 0.085 Uiso 1 1 calc R . .
C45 C 0.4631(3) 0.0640(2) 0.2280(3) 0.0773(13) Uani 1 1 d . . .
H45 H 0.4077 0.0326 0.2442 0.093 Uiso 1 1 calc R . .
C46 C 0.5826(4) 0.0540(3) 0.1297(2) 0.0828(14) Uani 1 1 d . . .
H46 H 0.6051 0.0160 0.0815 0.099 Uiso 1 1 calc R . .
C47 C 0.5513(4) 0.0946(3) 0.2928(2) 0.0806(14) Uani 1 1 d . . .
H47A H 0.5758 0.0464 0.3053 0.097 Uiso 1 1 calc R . .
H47B H 0.5285 0.1326 0.3400 0.097 Uiso 1 1 calc R . .
C48 C 0.4981(4) 0.0069(2) 0.1544(3) 0.0980(17) Uani 1 1 d . . .
H48A H 0.5229 -0.0425 0.1643 0.118 Uiso 1 1 calc R . .
H48B H 0.4403 -0.0129 0.1125 0.118 Uiso 1 1 calc R . .
C49 C 0.6715(3) 0.0832(3) 0.1929(3) 0.0842(14) Uani 1 1 d . . .
H49A H 0.7265 0.1140 0.1765 0.101 Uiso 1 1 calc R . .
H49B H 0.6984 0.0344 0.2026 0.101 Uiso 1 1 calc R . .
B B -0.0170(3) 0.7394(2) 0.33266(19) 0.0315(7) Uani 1 1 d . . .
C101 C 0.0688(2) 0.80405(17) 0.40150(16) 0.0342(7) Uani 1 1 d . . .
C102 C 0.1694(2) 0.7855(2) 0.41147(18) 0.0449(8) Uani 1 1 d . . .
H102 H 0.1894 0.7385 0.3737 0.054 Uiso 1 1 calc R . .
C103 C 0.2416(3) 0.8328(2) 0.4742(2) 0.0568(10) Uani 1 1 d . . .
H103 H 0.3083 0.8173 0.4786 0.068 Uiso 1 1 calc R . .
C104 C 0.2146(3) 0.9027(2) 0.5298(2) 0.0622(10) Uani 1 1 d . . .
H104 H 0.2629 0.9358 0.5721 0.075 Uiso 1 1 calc R . .
C105 C 0.1171(3) 0.9229(2) 0.5226(2) 0.0631(11) Uani 1 1 d . . .
H105 H 0.0978 0.9700 0.5608 0.076 Uiso 1 1 calc R . .
C106 C 0.0460(3) 0.87513(19) 0.45983(18) 0.0470(8) Uani 1 1 d . . .
H106 H -0.0205 0.8913 0.4564 0.056 Uiso 1 1 calc R . .
C201 C -0.0467(2) 0.66406(17) 0.36899(15) 0.0318(6) Uani 1 1 d . . .
C202 C -0.1138(2) 0.6756(2) 0.42638(17) 0.0424(8) Uani 1 1 d . . .
H202 H -0.1451 0.7257 0.4409 0.051 Uiso 1 1 calc R . .
C203 C -0.1362(3) 0.6165(2) 0.46260(19) 0.0522(9) Uani 1 1 d . . .
H203 H -0.1829 0.6264 0.4998 0.063 Uiso 1 1 calc R . .
C204 C -0.0902(3) 0.5433(2) 0.4441(2) 0.0547(9) Uani 1 1 d . . .
H204 H -0.1051 0.5029 0.4684 0.066 Uiso 1 1 calc R . .
C205 C -0.0226(3) 0.5304(2) 0.39015(19) 0.0492(9) Uani 1 1 d . . .
H205 H 0.0101 0.4810 0.3777 0.059 Uiso 1 1 calc R . .
C206 C -0.0016(2) 0.58927(18) 0.35339(17) 0.0395(7) Uani 1 1 d . . .
H206 H 0.0453 0.5782 0.3163 0.047 Uiso 1 1 calc R . .
C301 C -0.1178(2) 0.78533(17) 0.31553(15) 0.0304(6) Uani 1 1 d . . .
C302 C -0.1080(2) 0.86515(18) 0.30674(16) 0.0370(7) Uani 1 1 d . . .
H302 H -0.0417 0.8924 0.3105 0.044 Uiso 1 1 calc R . .
C303 C -0.1911(2) 0.90578(19) 0.29274(17) 0.0419(8) Uani 1 1 d . . .
H303 H -0.1803 0.9592 0.2870 0.050 Uiso 1 1 calc R . .
C304 C -0.2895(2) 0.86835(19) 0.28721(16) 0.0405(7) Uani 1 1 d . . .
H304 H -0.3463 0.8963 0.2790 0.049 Uiso 1 1 calc R . .
C305 C -0.3032(2) 0.78931(19) 0.29389(16) 0.0390(7) Uani 1 1 d . . .
H305 H -0.3699 0.7626 0.2898 0.047 Uiso 1 1 calc R . .
C306 C -0.2191(2) 0.74890(18) 0.30656(16) 0.0352(7) Uani 1 1 d . . .
H306 H -0.2308 0.6942 0.3092 0.042 Uiso 1 1 calc R . .
C401 C 0.0310(2) 0.70543(18) 0.24916(16) 0.0338(7) Uani 1 1 d . . .
C402 C -0.0006(2) 0.62581(18) 0.19276(16) 0.0366(7) Uani 1 1 d . . .
H402 H -0.0505 0.5892 0.2033 0.044 Uiso 1 1 calc R . .
C403 C 0.0397(2) 0.5994(2) 0.12194(17) 0.0442(8) Uani 1 1 d . . .
H403 H 0.0175 0.5451 0.0862 0.053 Uiso 1 1 calc R . .
C404 C 0.1108(3) 0.6509(2) 0.10326(19) 0.0539(9) Uani 1 1 d . . .
H404 H 0.1384 0.6323 0.0555 0.065 Uiso 1 1 calc R . .
C405 C 0.1412(3) 0.7300(2) 0.1553(2) 0.0578(10) Uani 1 1 d . . .
H405 H 0.1888 0.7668 0.1429 0.069 Uiso 1 1 calc R . .
C406 C 0.1017(3) 0.7564(2) 0.22671(18) 0.0478(8) Uani 1 1 d . . .
H406 H 0.1240 0.8112 0.2614 0.057 Uiso 1 1 calc R . .
N7 N 0.7186(4) 0.3421(3) 0.4446(2) 0.1132(18) Uani 1 1 d D . .
C50 C 0.7960(5) 0.3164(3) 0.4363(2) 0.0777(15) Uani 1 1 d D . .
C51 C 0.8906(4) 0.2826(3) 0.4263(2) 0.0907(15) Uani 1 1 d D . .
H51A H 0.9332 0.2995 0.4766 0.136 Uiso 1 1 calc R . .
H51B H 0.9254 0.3036 0.3903 0.136 Uiso 1 1 calc R . .
H51C H 0.8782 0.2215 0.4052 0.136 Uiso 1 1 calc R . .
N8 N 0.3925(8) 1.2036(6) 0.4826(5) 0.310(6) Uani 1 1 d D . .
C52 C 0.3345(8) 1.1561(5) 0.4905(4) 0.188(4) Uani 1 1 d D . .
C53 C 0.2601(5) 1.1025(3) 0.5006(3) 0.1162(19) Uani 1 1 d D . .
H53A H 0.2518 1.1181 0.5558 0.174 Uiso 1 1 calc R . .
H53B H 0.2787 1.0454 0.4823 0.174 Uiso 1 1 calc R . .
H53C H 0.1961 1.1052 0.4710 0.174 Uiso 1 1 calc R . .
N9 N -0.5768(6) 0.8167(5) 0.2630(5) 0.180(3) Uani 1 1 d D B .
C54 C -0.5984(8) 0.8735(6) 0.3146(6) 0.168(4) Uani 1 1 d D . .
C55A C -0.655(2) 0.9331(14) 0.3549(16) 0.075(10) Uani 0.21(2) 1 d PD B 1
H55A H -0.6624 0.9271 0.4056 0.112 Uiso 0.21(2) 1 calc PR B 1
H55B H -0.7226 0.9258 0.3255 0.112 Uiso 0.21(2) 1 calc PR B 1
H55C H -0.6212 0.9888 0.3623 0.112 Uiso 0.21(2) 1 calc PR B 1
C55B C -0.561(2) 0.9358(7) 0.3903(9) 0.312(17) Uani 0.79(2) 1 d PD B 2
H55D H -0.5030 0.9172 0.4143 0.468 Uiso 0.79(2) 1 calc PR B 2
H55E H -0.6154 0.9428 0.4237 0.468 Uiso 0.79(2) 1 calc PR B 2
H55F H -0.5401 0.9893 0.3836 0.468 Uiso 0.79(2) 1 calc PR B 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'
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 164.40(8) . . ?
O1 Ni1 N3 87.65(8) . . ?
N2 Ni1 N3 82.01(9) . . ?
O1 Ni1 N1 88.72(8) . . ?
N2 Ni1 N1 81.51(8) . . ?
N3 Ni1 N1 99.29(8) . . ?
O1 Ni1 S2 94.85(6) . . ?
N2 Ni1 S2 96.94(7) . . ?
N3 Ni1 S2 90.85(7) . . ?
N1 Ni1 S2 169.39(6) . . ?
O1 Ni1 S1 94.10(6) . . ?
N2 Ni1 S1 98.02(7) . . ?
N3 Ni1 S1 170.56(6) . . ?
N1 Ni1 S1 90.03(6) . . ?
S2 Ni1 S1 79.77(4) . . ?
O2 Ni2 N5 165.22(8) . . ?
O2 Ni2 N4 87.93(8) . . ?
N5 Ni2 N4 82.81(8) . . ?
O2 Ni2 N6 89.20(8) . . ?
N5 Ni2 N6 81.03(9) . . ?
N4 Ni2 N6 99.40(8) . . ?
O2 Ni2 S2 94.56(6) . . ?
N5 Ni2 S2 96.95(7) . . ?
N4 Ni2 S2 90.21(6) . . ?
N6 Ni2 S2 169.81(6) . . ?
O2 Ni2 S1 94.20(6) . . ?
N5 Ni2 S1 96.93(7) . . ?
N4 Ni2 S1 169.88(6) . . ?
N6 Ni2 S1 90.52(6) . . ?
S2 Ni2 S1 79.77(3) . . ?
C1 S1 Ni2 100.53(9) . . ?
C1 S1 Ni1 100.93(9) . . ?
Ni2 S1 Ni1 88.35(4) . . ?
C17 S2 Ni1 105.32(9) . . ?
C17 S2 Ni2 105.67(9) . . ?
Ni1 S2 Ni2 90.82(3) . . ?
C39 O1 Ni1 134.27(17) . . ?
C39 O2 Ni2 134.32(17) . . ?
C29 N1 C28 110.2(2) . . ?
C29 N1 C30 106.9(2) . . ?
C28 N1 C30 106.4(2) . . ?
C29 N1 Ni1 115.24(17) . . ?
C28 N1 Ni1 105.79(16) . . ?
C30 N1 Ni1 112.07(15) . . ?
C27 N2 C26 107.5(2) . . ?
C27 N2 C25 110.6(2) . . ?
C26 N2 C25 108.7(2) . . ?
C27 N2 Ni1 106.55(15) . . ?
C26 N2 Ni1 114.27(16) . . ?
C25 N2 Ni1 109.21(16) . . ?
C23 N3 C24 109.6(2) . . ?
C23 N3 C22 107.0(2) . . ?
C24 N3 C22 107.2(2) . . ?
C23 N3 Ni1 117.18(17) . . ?
C24 N3 Ni1 103.56(16) . . ?
C22 N3 Ni1 111.86(16) . . ?
C13 N4 C14 109.1(2) . . ?
C13 N4 C15 107.8(2) . . ?
C14 N4 C15 107.1(2) . . ?
C13 N4 Ni2 103.17(16) . . ?
C14 N4 Ni2 116.46(17) . . ?
C15 N4 Ni2 112.85(16) . . ?
C11 N5 C10 107.3(2) . . ?
C11 N5 C12 108.7(2) . . ?
C10 N5 C12 111.0(2) . . ?
C11 N5 Ni2 114.09(17) . . ?
C10 N5 Ni2 107.69(16) . . ?
C12 N5 Ni2 108.12(16) . . ?
C8 N6 C9 110.2(2) . . ?
C8 N6 C7 107.0(2) . . ?
C9 N6 C7 106.0(2) . . ?
C8 N6 Ni2 115.81(17) . . ?
C9 N6 Ni2 106.32(16) . . ?
C7 N6 Ni2 111.20(15) . . ?
C2 C1 C6 118.4(2) . . ?
C2 C1 S1 121.0(2) . . ?
C6 C1 S1 120.5(2) . . ?
C3 C2 C1 119.8(2) . . ?
C3 C2 C7 120.6(2) . . ?
C1 C2 C7 119.0(2) . . ?
C2 C3 C4 122.4(3) . . ?
C3 C4 C5 116.5(2) . . ?
C3 C4 C31 121.1(3) . . ?
C5 C4 C31 122.1(3) . . ?
C6 C5 C4 122.2(3) . . ?
C5 C6 C1 119.9(2) . . ?
C5 C6 C30 120.6(2) . . ?
C1 C6 C30 119.1(2) . . ?
N6 C7 C2 116.8(2) . . ?
N6 C9 C10 110.5(2) . . ?
N5 C10 C9 112.7(2) . . ?
N5 C12 C13 113.9(2) . . ?
N4 C13 C12 111.6(2) . . ?
N4 C15 C16 116.7(2) . . ?
C21 C16 C17 119.8(3) . . ?
C21 C16 C15 121.1(3) . . ?
C17 C16 C15 118.5(2) . . ?
C18 C17 C16 118.2(2) . . ?
C18 C17 S2 120.7(2) . . ?
C16 C17 S2 120.9(2) . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 C22 120.5(3) . . ?
C17 C18 C22 119.4(2) . . ?
C18 C19 C20 122.8(3) . . ?
C21 C20 C19 116.3(3) . . ?
C21 C20 C35 122.6(3) . . ?
C19 C20 C35 121.0(3) . . ?
C20 C21 C16 122.7(3) . . ?
N3 C22 C18 115.6(2) . . ?
N3 C24 C25 112.0(2) . . ?
N2 C25 C24 113.9(2) . . ?
N2 C27 C28 112.6(2) . . ?
N1 C28 C27 110.6(2) . . ?
N1 C30 C6 117.1(2) . . ?
C32 C31 C34 109.1(3) . . ?
C32 C31 C4 111.6(2) . . ?
C34 C31 C4 108.2(2) . . ?
C32 C31 C33 108.1(3) . . ?
C34 C31 C33 108.8(3) . . ?
C4 C31 C33 111.0(2) . . ?
C38B C35 C37A 127.0(7) . . ?
C38B C35 C20 117.9(6) . . ?
C37A C35 C20 114.7(4) . . ?
C38B C35 C37B 112.4(10) . . ?
C37A C35 C37B 54.5(6) . . ?
C20 C35 C37B 107.7(5) . . ?
C38B C35 C36A 44.3(9) . . ?
C37A C35 C36A 112.9(7) . . ?
C20 C35 C36A 107.3(5) . . ?
C37B C35 C36A 144.7(6) . . ?
C38B C35 C38A 60.6(9) . . ?
C37A C35 C38A 108.5(6) . . ?
C20 C35 C38A 108.0(4) . . ?
C37B C35 C38A 59.3(7) . . ?
C36A C35 C38A 104.9(7) . . ?
C38B C35 C36B 106.5(10) . . ?
C37A C35 C36B 49.8(6) . . ?
C20 C35 C36B 107.3(5) . . ?
C37B C35 C36B 104.1(9) . . ?
C36A C35 C36B 69.4(7) . . ?
C38A C35 C36B 144.2(5) . . ?
O2 C39 O1 126.5(2) . . ?
O2 C39 C40 116.8(2) . . ?
O1 C39 C40 116.7(2) . . ?
C41 C40 C42 108.4(3) . . ?
C41 C40 C43 108.7(3) . . ?
C42 C40 C43 108.6(3) . . ?
C41 C40 C39 111.3(2) . . ?
C42 C40 C39 108.2(2) . . ?
C43 C40 C39 111.4(2) . . ?
C40 C41 C44 110.3(3) . . ?
C40 C42 C45 110.1(3) . . ?
C40 C43 C46 109.6(3) . . ?
C47 C44 C49 110.5(3) . . ?
C47 C44 C41 108.1(3) . . ?
C49 C44 C41 109.0(3) . . ?
C47 C45 C48 110.1(3) . . ?
C47 C45 C42 109.2(3) . . ?
C48 C45 C42 109.3(4) . . ?
C49 C46 C48 110.0(4) . . ?
C49 C46 C43 109.6(4) . . ?
C48 C46 C43 109.9(4) . . ?
C45 C47 C44 109.7(3) . . ?
C46 C48 C45 109.7(3) . . ?
C46 C49 C44 109.5(3) . . ?
C101 B C301 112.2(2) . . ?
C101 B C401 110.8(2) . . ?
C301 B C401 106.3(2) . . ?
C101 B C201 102.7(2) . . ?
C301 B C201 111.7(2) . . ?
C401 B C201 113.2(2) . . ?
C102 C101 C106 114.4(3) . . ?
C102 C101 B 121.3(3) . . ?
C106 C101 B 123.9(3) . . ?
C103 C102 C101 123.5(3) . . ?
C104 C103 C102 119.4(3) . . ?
C105 C104 C103 119.1(3) . . ?
C104 C105 C106 120.8(3) . . ?
C105 C106 C101 122.7(3) . . ?
C206 C201 C202 114.2(3) . . ?
C206 C201 B 124.8(3) . . ?
C202 C201 B 120.7(3) . . ?
C203 C202 C201 123.1(3) . . ?
C204 C203 C202 120.1(3) . . ?
C205 C204 C203 118.9(3) . . ?
C204 C205 C206 120.8(3) . . ?
C205 C206 C201 123.0(3) . . ?
C306 C301 C302 114.1(3) . . ?
C306 C301 B 124.1(2) . . ?
C302 C301 B 121.8(3) . . ?
C303 C302 C301 123.3(3) . . ?
C304 C303 C302 120.3(3) . . ?
C305 C304 C303 118.7(3) . . ?
C304 C305 C306 120.3(3) . . ?
C305 C306 C301 123.3(3) . . ?
C406 C401 C402 114.6(3) . . ?
C406 C401 B 122.0(3) . . ?
C402 C401 B 123.3(3) . . ?
C403 C402 C401 122.1(3) . . ?
C404 C403 C402 121.2(3) . . ?
C405 C404 C403 118.7(3) . . ?
C404 C405 C406 120.2(3) . . ?
C405 C406 C401 123.1(3) . . ?
N7 C50 C51 178.5(5) . . ?
N8 C52 C53 176.2(14) . . ?
N9 C54 C55A 158.7(18) . . ?
N9 C54 C55B 144.7(14) . . ?
C55A C54 C55B 56.6(13) . . ?
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 2.0031(18) . ?
Ni1 N2 2.153(2) . ?
Ni1 N3 2.266(2) . ?
Ni1 N1 2.269(2) . ?
Ni1 S2 2.4227(11) . ?
Ni1 S1 2.4904(13) . ?
Ni2 O2 2.0097(18) . ?
Ni2 N5 2.155(2) . ?
Ni2 N4 2.253(2) . ?
Ni2 N6 2.286(2) . ?
Ni2 S2 2.4372(13) . ?
Ni2 S1 2.4763(9) . ?
S1 C1 1.764(3) . ?
S2 C17 1.751(3) . ?
O1 C39 1.264(3) . ?
O2 C39 1.256(3) . ?
N1 C29 1.470(3) . ?
N1 C28 1.482(3) . ?
N1 C30 1.488(3) . ?
N2 C27 1.474(3) . ?
N2 C26 1.478(3) . ?
N2 C25 1.492(3) . ?
N3 C23 1.473(3) . ?
N3 C24 1.478(3) . ?
N3 C22 1.485(3) . ?
N4 C13 1.479(3) . ?
N4 C14 1.479(3) . ?
N4 C15 1.481(3) . ?
N5 C11 1.483(3) . ?
N5 C10 1.485(4) . ?
N5 C12 1.485(3) . ?
N6 C8 1.476(3) . ?
N6 C9 1.489(3) . ?
N6 C7 1.492(3) . ?
C1 C2 1.396(3) . ?
C1 C6 1.398(3) . ?
C2 C3 1.387(3) . ?
C2 C7 1.496(4) . ?
C3 C4 1.391(4) . ?
C4 C5 1.392(4) . ?
C4 C31 1.531(4) . ?
C5 C6 1.386(3) . ?
C6 C30 1.494(3) . ?
C9 C10 1.504(4) . ?
C12 C13 1.516(4) . ?
C15 C16 1.501(4) . ?
C16 C21 1.387(4) . ?
C16 C17 1.405(4) . ?
C17 C18 1.400(4) . ?
C18 C19 1.386(4) . ?
C18 C22 1.501(4) . ?
C19 C20 1.393(4) . ?
C20 C21 1.384(4) . ?
C20 C35 1.530(4) . ?
C24 C25 1.506(4) . ?
C27 C28 1.498(4) . ?
C31 C32 1.528(4) . ?
C31 C34 1.530(4) . ?
C31 C33 1.534(4) . ?
C35 C38B 1.384(14) . ?
C35 C37A 1.439(9) . ?
C35 C37B 1.534(13) . ?
C35 C36A 1.540(10) . ?
C35 C38A 1.605(10) . ?
C35 C36B 1.648(12) . ?
C39 C40 1.530(4) . ?
C40 C41 1.517(4) . ?
C40 C42 1.527(4) . ?
C40 C43 1.530(4) . ?
C41 C44 1.560(4) . ?
C42 C45 1.542(4) . ?
C43 C46 1.545(5) . ?
C44 C47 1.510(5) . ?
C44 C49 1.517(5) . ?
C45 C47 1.503(5) . ?
C45 C48 1.509(6) . ?
C46 C49 1.493(6) . ?
C46 C48 1.500(6) . ?
B C101 1.641(4) . ?
B C301 1.643(4) . ?
B C401 1.644(4) . ?
B C201 1.645(4) . ?
C101 C102 1.394(4) . ?
C101 C106 1.395(4) . ?
C102 C103 1.389(4) . ?
C103 C104 1.378(5) . ?
C104 C105 1.360(5) . ?
C105 C106 1.384(4) . ?
C201 C206 1.393(4) . ?
C201 C202 1.405(4) . ?
C202 C203 1.386(4) . ?
C203 C204 1.374(4) . ?
C204 C205 1.361(5) . ?
C205 C206 1.387(4) . ?
C301 C306 1.396(4) . ?
C301 C302 1.402(4) . ?
C302 C303 1.382(4) . ?
C303 C304 1.376(4) . ?
C304 C305 1.375(4) . ?
C305 C306 1.385(4) . ?
C401 C406 1.393(4) . ?
C401 C402 1.403(4) . ?
C402 C403 1.388(4) . ?
C403 C404 1.366(4) . ?
C404 C405 1.364(5) . ?
C405 C406 1.392(4) . ?
N7 C50 1.143(6) . ?
C50 C51 1.414(6) . ?
N8 C52 1.114(7) . ?
C52 C53 1.345(7) . ?
N9 C54 1.179(8) . ?
C54 C55A 1.361(13) . ?
C54 C55B 1.448(14) . ?
