#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:41:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179073 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/35/4303575.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_4303575
loop_
_publ_author_name
'Kuppuswamy Arumugam'
'Mohamed C. Shaw'
'P. Chandrasekaran'
'Dino Villagrán'
'Thomas G. Gray'
'Joel T. Mague'
'James P. Donahue'
_publ_contact_author             'James P. Donahue'
_publ_contact_author_address
;
   James P. Donahue
   Department of Chemistry
   Tulane University
   Percival Stern Hall, Room 2015
   6400 Freret Street
   New Orleans, Louisiana 70118-5698
;
_publ_contact_author_email       donahue@tulane.edu
_publ_section_title
;
Synthesis, Structures, and Properties of 1,2,4,5-Benzenetetrathiolate
Linked Group 10 Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10591
_journal_page_last               10607
_journal_paper_doi               10.1021/ic901257s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C58 H46 Ni2 P4 S4'
_chemical_formula_weight         1112.49
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.976(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.971(2)
_cell_length_b                   15.318(3)
_cell_length_c                   15.200(3)
_cell_measurement_reflns_used    5318
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.299
_cell_measurement_theta_min      2.3135
_cell_volume                     2507.7(8)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18197
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.9620
_exptl_absorpt_correction_T_min  0.8114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0616
_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)+(0.0861P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                2923
_reflns_number_total             4413
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic901257s_si_001_10.cif
_cod_data_source_block           jpd155
_cod_original_cell_volume        2507.5(8)
_cod_database_code               4303575
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 0.77786(6) 0.20140(4) 0.36344(4) 0.0312(2) Uani 1 1 d . A .
S1 S 0.90041(13) 0.10532(9) 0.32288(8) 0.0333(3) Uani 1 1 d . . .
S2 S 0.81663(14) 0.15811(10) 0.50084(9) 0.0398(4) Uani 1 1 d . . .
P1 P 0.75553(15) 0.27009(10) 0.23730(10) 0.0377(4) Uani 1 1 d . . .
P2 P 0.62451(15) 0.27634(10) 0.39171(10) 0.0372(4) Uani 1 1 d . . .
C1 C 0.9585(5) 0.0473(3) 0.4214(3) 0.0277(12) Uani 1 1 d . . .
C2 C 0.9168(5) 0.0685(3) 0.5004(3) 0.0292(12) Uani 1 1 d . . .
C3 C 0.9590(5) 0.0217(3) 0.5771(3) 0.0299(12) Uani 1 1 d . . .
H3 H 0.9311 0.0369 0.6305 0.036 Uiso 1 1 calc R . .
C4A C 0.8989(9) 0.3287(6) 0.2184(6) 0.0325(18) Uiso 0.735(13) 1 d P A 1
C5A C 0.9967(9) 0.2817(6) 0.2009(6) 0.038(2) Uiso 0.735(13) 1 d P A 1
H5A H 0.9926 0.2197 0.2003 0.045 Uiso 0.735(13) 1 calc PR A 1
C6A C 1.1020(10) 0.3229(7) 0.1841(7) 0.055(3) Uiso 0.735(13) 1 d P A 1
H6A H 1.1694 0.2899 0.1708 0.066 Uiso 0.735(13) 1 calc PR A 1
C7A C 1.1077(11) 0.4134(9) 0.1871(7) 0.057(3) Uiso 0.735(13) 1 d P A 1
H7A H 1.1803 0.4420 0.1763 0.068 Uiso 0.735(13) 1 calc PR A 1
C8A C 1.0130(14) 0.4612(8) 0.2051(7) 0.053(3) Uiso 0.735(13) 1 d P A 1
H8A H 1.0188 0.5231 0.2063 0.063 Uiso 0.735(13) 1 calc PR A 1
C9A C 0.9039(10) 0.4199(7) 0.2221(6) 0.049(2) Uiso 0.735(13) 1 d P A 1
H9A H 0.8367 0.4531 0.2356 0.059 Uiso 0.735(13) 1 calc PR A 1
C4B C 0.862(3) 0.3367(17) 0.2183(17) 0.0325(18) Uiso 0.265(13) 1 d P A 2
C5B C 0.979(3) 0.3048(19) 0.2147(18) 0.038(2) Uiso 0.265(13) 1 d P A 2
H5B H 0.9888 0.2434 0.2212 0.045 Uiso 0.265(13) 1 calc PR A 2
C6B C 1.090(3) 0.354(2) 0.202(2) 0.055(3) Uiso 0.265(13) 1 d P A 2
H6B H 1.1652 0.3266 0.1941 0.066 Uiso 0.265(13) 1 calc PR A 2
C7B C 1.074(4) 0.442(2) 0.203(2) 0.057(3) Uiso 0.265(13) 1 d P A 2
H7B H 1.1437 0.4791 0.2032 0.068 Uiso 0.265(13) 1 calc PR A 2
C8B C 0.957(3) 0.479(2) 0.2046(17) 0.053(3) Uiso 0.265(13) 1 d P A 2
H8B H 0.9498 0.5403 0.2006 0.063 Uiso 0.265(13) 1 calc PR A 2
C9B C 0.847(3) 0.4303(18) 0.2117(18) 0.049(2) Uiso 0.265(13) 1 d P A 2
H9B H 0.7699 0.4582 0.2119 0.059 Uiso 0.265(13) 1 calc PR A 2
C10 C 0.6985(5) 0.2122(4) 0.1327(3) 0.0366(13) Uani 1 1 d . A .
C11 C 0.6719(6) 0.2567(5) 0.0523(4) 0.0533(17) Uani 1 1 d . . .
H11 H 0.6902 0.3172 0.0509 0.064 Uiso 1 1 calc R A .
C12 C 0.6197(6) 0.2152(5) -0.0251(4) 0.0576(19) Uani 1 1 d . A .
H12 H 0.5979 0.2476 -0.0790 0.069 Uiso 1 1 calc R . .
C13 C 0.5991(7) 0.1295(5) -0.0257(5) 0.070(2) Uani 1 1 d . . .
H13 H 0.5683 0.1003 -0.0805 0.084 Uiso 1 1 calc R A .
C14 C 0.6228(8) 0.0835(5) 0.0538(5) 0.086(3) Uani 1 1 d . A .
H14 H 0.6046 0.0229 0.0537 0.103 Uiso 1 1 calc R . .
C15 C 0.6724(7) 0.1243(5) 0.1333(4) 0.0589(19) Uani 1 1 d . . .
H15 H 0.6885 0.0922 0.1877 0.071 Uiso 1 1 calc R A .
C16 C 0.6371(6) 0.3423(3) 0.4919(4) 0.0373(14) Uani 1 1 d . A .
C17 C 0.7513(7) 0.3720(5) 0.5342(5) 0.0615(19) Uani 1 1 d . . .
H17 H 0.8247 0.3536 0.5150 0.074 Uiso 1 1 calc R A .
C18 C 0.7576(8) 0.4298(5) 0.6059(5) 0.081(2) Uani 1 1 d . A .
H18 H 0.8360 0.4514 0.6352 0.097 Uiso 1 1 calc R . .
C19 C 0.6514(8) 0.4561(5) 0.6349(5) 0.065(2) Uani 1 1 d . . .
H19 H 0.6569 0.4964 0.6830 0.078 Uiso 1 1 calc R A .
C20 C 0.5405(7) 0.4247(4) 0.5949(4) 0.0523(18) Uani 1 1 d . A .
H20 H 0.4680 0.4418 0.6161 0.063 Uiso 1 1 calc R . .
C21 C 0.5302(6) 0.3680(4) 0.5236(4) 0.0476(16) Uani 1 1 d . . .
H21 H 0.4511 0.3462 0.4959 0.057 Uiso 1 1 calc R A .
C22A C 0.4907(10) 0.2071(7) 0.3964(7) 0.0358(19) Uiso 0.680(10) 1 d P A 1
C23A C 0.4938(10) 0.1479(6) 0.4641(6) 0.039(2) Uiso 0.680(10) 1 d P A 1
H23A H 0.5668 0.1417 0.5086 0.046 Uiso 0.680(10) 1 calc PR A 1
C24A C 0.3916(10) 0.0972(8) 0.4678(8) 0.055(3) Uiso 0.680(10) 1 d P A 1
H24A H 0.3926 0.0552 0.5139 0.066 Uiso 0.680(10) 1 calc PR A 1
C25A C 0.2874(13) 0.1096(7) 0.4022(10) 0.052(3) Uiso 0.680(10) 1 d P A 1
H25A H 0.2152 0.0769 0.4065 0.062 Uiso 0.680(10) 1 calc PR A 1
C26A C 0.2809(12) 0.1633(10) 0.3341(10) 0.067(3) Uiso 0.680(10) 1 d P A 1
H26A H 0.2081 0.1669 0.2890 0.081 Uiso 0.680(10) 1 calc PR A 1
C27A C 0.3830(11) 0.2141(8) 0.3302(8) 0.056(3) Uiso 0.680(10) 1 d P A 1
H27A H 0.3806 0.2542 0.2822 0.067 Uiso 0.680(10) 1 calc PR A 1
C22B C 0.480(2) 0.2208(15) 0.3715(15) 0.0358(19) Uiso 0.320(10) 1 d P A 2
C23B C 0.459(2) 0.1634(14) 0.4366(15) 0.039(2) Uiso 0.320(10) 1 d P A 2
H23B H 0.5232 0.1577 0.4878 0.046 Uiso 0.320(10) 1 calc PR A 2
C24B C 0.351(3) 0.1121(16) 0.435(2) 0.055(3) Uiso 0.320(10) 1 d P A 2
H24B H 0.3387 0.0734 0.4818 0.066 Uiso 0.320(10) 1 calc PR A 2
C25B C 0.268(2) 0.1264(19) 0.359(2) 0.052(3) Uiso 0.320(10) 1 d P A 2
H25B H 0.1909 0.0972 0.3520 0.062 Uiso 0.320(10) 1 calc PR A 2
C26B C 0.287(2) 0.1803(16) 0.288(2) 0.067(3) Uiso 0.320(10) 1 d P A 2
H26B H 0.2258 0.1837 0.2347 0.081 Uiso 0.320(10) 1 calc PR A 2
C27B C 0.398(2) 0.2297(16) 0.2976(17) 0.056(3) Uiso 0.320(10) 1 d P A 2
H27B H 0.4116 0.2683 0.2516 0.067 Uiso 0.320(10) 1 calc PR A 2
C28A C 0.6489(10) 0.3589(6) 0.2387(6) 0.0363(19) Uiso 0.744(17) 1 d P A 3
H28A H 0.6367 0.4026 0.1935 0.044 Uiso 0.744(17) 1 calc PR A 3
C29A C 0.5889(10) 0.3604(6) 0.3054(5) 0.0365(19) Uiso 0.744(17) 1 d P A 3
H29A H 0.5285 0.4041 0.3088 0.044 Uiso 0.744(17) 1 calc PR A 3
C28B C 0.602(3) 0.3368(17) 0.2232(17) 0.0363(19) Uiso 0.256(17) 1 d P A 4
H28B H 0.5677 0.3663 0.1691 0.044 Uiso 0.256(17) 1 calc PR A 4
C29B C 0.544(3) 0.3384(18) 0.2989(16) 0.0365(19) Uiso 0.256(17) 1 d P A 4
H29B H 0.4690 0.3694 0.3003 0.044 Uiso 0.256(17) 1 calc PR A 4
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'
P P 0.1023 0.0942 '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
P2 Ni1 S2 89.32(6) . . ?
P2 Ni1 P1 87.50(6) . . ?
S2 Ni1 P1 168.06(7) . . ?
P2 Ni1 S1 167.22(7) . . ?
S2 Ni1 S1 92.76(6) . . ?
P1 Ni1 S1 92.87(6) . . ?
C1 S1 Ni1 104.25(17) . . ?
C2 S2 Ni1 104.15(17) . . ?
C4B P1 C28A 90.9(10) . . ?
C4B P1 C10 106.9(9) . . ?
C28A P1 C10 105.2(4) . . ?
C28A P1 C4A 101.9(5) . . ?
C10 P1 C4A 104.9(3) . . ?
C4B P1 C28B 106.7(13) . . ?
C10 P1 C28B 90.7(9) . . ?
C4A P1 C28B 117.7(9) . . ?
C4B P1 Ni1 120.2(9) . . ?
C28A P1 Ni1 108.8(3) . . ?
C10 P1 Ni1 119.93(19) . . ?
C4A P1 Ni1 114.3(3) . . ?
C28B P1 Ni1 107.6(7) . . ?
C22B P2 C29B 79.9(13) . . ?
C22B P2 C16 109.7(7) . . ?
C29B P2 C16 108.3(8) . . ?
C29B P2 C22A 93.3(11) . . ?
C16 P2 C22A 103.0(4) . . ?
C22B P2 C29A 98.7(8) . . ?
C16 P2 C29A 100.5(3) . . ?
C22A P2 C29A 112.0(5) . . ?
C22B P2 Ni1 114.6(7) . . ?
C29B P2 Ni1 114.6(8) . . ?
C16 P2 Ni1 122.0(2) . . ?
C22A P2 Ni1 111.4(3) . . ?
C29A P2 Ni1 107.6(3) . . ?
C3 C1 C2 118.7(5) 3_756 . ?
C3 C1 S1 122.0(4) 3_756 . ?
C2 C1 S1 119.3(4) . . ?
C3 C2 C1 119.6(5) . . ?
C3 C2 S2 121.0(4) . . ?
C1 C2 S2 119.4(4) . . ?
C2 C3 C1 121.7(5) . 3_756 ?
C5A C4A C9A 120.8(9) . . ?
C5A C4A P1 119.4(7) . . ?
C9A C4A P1 119.9(7) . . ?
C4A C5A C6A 120.8(8) . . ?
C7A C6A C5A 119.0(9) . . ?
C8A C7A C6A 121.3(11) . . ?
C7A C8A C9A 120.4(10) . . ?
C4A C9A C8A 117.7(9) . . ?
C5B C4B C9B 116(2) . . ?
C5B C4B P1 119(2) . . ?
C9B C4B P1 125(2) . . ?
C4B C5B C6B 129(3) . . ?
C7B C6B C5B 113(3) . . ?
C6B C7B C8B 121(3) . . ?
C7B C8B C9B 125(3) . . ?
C8B C9B C4B 116(3) . . ?
C15 C10 C11 118.6(6) . . ?
C15 C10 P1 120.5(4) . . ?
C11 C10 P1 120.7(5) . . ?
C12 C11 C10 121.1(6) . . ?
C13 C12 C11 120.6(6) . . ?
C12 C13 C14 119.6(7) . . ?
C15 C14 C13 120.9(7) . . ?
C14 C15 C10 119.1(6) . . ?
C17 C16 C21 119.6(6) . . ?
C17 C16 P2 119.7(5) . . ?
C21 C16 P2 120.6(5) . . ?
C16 C17 C18 118.7(7) . . ?
C19 C18 C17 121.0(7) . . ?
C20 C19 C18 119.8(7) . . ?
C19 C20 C21 120.9(7) . . ?
C20 C21 C16 119.9(6) . . ?
C23A C22A C27A 119.2(10) . . ?
C23A C22A P2 120.7(8) . . ?
C27A C22A P2 120.1(7) . . ?
C22A C23A C24A 120.1(10) . . ?
C23A C24A C25A 117.6(10) . . ?
C26A C25A C24A 124.6(13) . . ?
C25A C26A C27A 117.8(12) . . ?
C26A C27A C22A 120.5(11) . . ?
C27B C22B C23B 120(2) . . ?
C27B C22B P2 123.3(18) . . ?
C23B C22B P2 116.8(16) . . ?
C22B C23B C24B 127(2) . . ?
C25B C24B C23B 110(2) . . ?
C24B C25B C26B 126(3) . . ?
C25B C26B C27B 119(2) . . ?
C22B C27B C26B 118(2) . . ?
C29A C28A P1 116.5(7) . . ?
C28A C29A P2 118.2(7) . . ?
C29B C28B P1 115.7(18) . . ?
C28B C29B P2 113.5(18) . . ?
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 P2 2.1466(16) . ?
Ni1 S2 2.1549(15) . ?
Ni1 P1 2.1597(16) . ?
Ni1 S1 2.1608(15) . ?
S1 C1 1.754(5) . ?
S2 C2 1.759(5) . ?
P1 C4B 1.61(3) . ?
P1 C28A 1.797(8) . ?
P1 C10 1.824(6) . ?
P1 C4A 1.881(10) . ?
P1 C28B 1.95(3) . ?
P2 C22B 1.77(2) . ?
P2 C29B 1.79(2) . ?
P2 C16 1.811(6) . ?
P2 C22A 1.824(11) . ?
P2 C29A 1.827(8) . ?
C1 C3 1.389(7) 3_756 ?
C1 C2 1.401(7) . ?
C2 C3 1.371(7) . ?
C3 C1 1.389(7) 3_756 ?
C4A C5A 1.360(12) . ?
C4A C9A 1.399(13) . ?
C5A C6A 1.383(14) . ?
C6A C7A 1.387(15) . ?
C7A C8A 1.342(14) . ?
C8A C9A 1.420(14) . ?
C4B C5B 1.39(4) . ?
C4B C9B 1.44(4) . ?
C5B C6B 1.48(4) . ?
C6B C7B 1.36(4) . ?
C7B C8B 1.41(4) . ?
C8B C9B 1.43(4) . ?
C10 C15 1.377(8) . ?
C10 C11 1.381(7) . ?
C11 C12 1.363(9) . ?
C12 C13 1.331(9) . ?
C13 C14 1.380(9) . ?
C14 C15 1.377(9) . ?
C16 C17 1.372(9) . ?
C16 C21 1.406(8) . ?
C17 C18 1.397(9) . ?
C18 C19 1.381(11) . ?
C19 C20 1.342(10) . ?
C20 C21 1.377(8) . ?
C22A C23A 1.366(13) . ?
C22A C27A 1.403(16) . ?
C23A C24A 1.373(14) . ?
C24A C25A 1.379(16) . ?
C25A C26A 1.313(16) . ?
C26A C27A 1.374(17) . ?
C22B C27B 1.31(3) . ?
C22B C23B 1.38(3) . ?
C23B C24B 1.42(3) . ?
C24B C25B 1.35(4) . ?
C25B C26B 1.40(4) . ?
C26B C27B 1.42(3) . ?
C28A C29A 1.309(11) . ?
C28B C29B 1.42(3) . ?
