#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:15:02 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178891 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/20/4112079.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_4112079
loop_
_publ_author_name
'Marilyn V. Rampersad'
'Stephen P. Jeffery'
'Melissa L. Golden'
'Jonghyuk Lee'
'Joseph H. Reibenspies'
'Donald J. Darensbourg'
'Marcetta Y. Darensbourg'
_publ_section_title
;
 Characterization of Steric and Electronic Properties of NiN2S2 Complexes
 as S-Donor Metallodithiolate Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17323
_journal_page_last               17334
_journal_paper_doi               10.1021/ja055051g
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C17 H28 Cl2 N2 Ni O4 S2 W'
_chemical_formula_weight         701.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.3245(11)
_cell_length_b                   12.7484(7)
_cell_length_c                   20.5750(12)
_cell_measurement_reflns_used    904
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      2.27
_cell_volume                     4806.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1057
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22168
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    5.987
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.456
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0604P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                2838
_reflns_number_total             4089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055051gsi20050726_033402.cif
_cod_data_source_block           mdni
_cod_database_code               4112079
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
Ni1 Ni 0.22573(5) 0.17010(8) 0.08427(5) 0.0229(3) Uani 1 1 d .
W1 W 0.081918(17) 0.14273(2) 0.154047(15) 0.02139(14) Uani 1 1 d .
Cl1 Cl 0.83970(16) 0.4519(2) 0.15567(16) 0.0635(8) Uani 1 1 d .
Cl2 Cl 0.96241(15) 0.4561(2) 0.06581(12) 0.0520(7) Uani 1 1 d .
S1 S 0.21527(11) 0.08285(15) 0.17362(10) 0.0231(5) Uani 1 1 d .
S2 S 0.13718(11) 0.08431(15) 0.04070(10) 0.0247(5) Uani 1 1 d .
O1 O 0.1056(4) 0.3863(5) 0.1681(3) 0.0442(17) Uani 1 1 d .
O2 O 0.0290(4) 0.1776(5) 0.2957(3) 0.0448(17) Uani 1 1 d .
O3 O 0.0311(3) -0.0900(5) 0.1868(3) 0.0363(15) Uani 1 1 d .
O4 O -0.0725(3) 0.1888(5) 0.0984(3) 0.0415(17) Uani 1 1 d .
N1 N 0.3175(3) 0.2255(5) 0.1151(3) 0.0248(16) Uani 1 1 d .
N2 N 0.2261(4) 0.2729(5) 0.0136(3) 0.0262(16) Uani 1 1 d .
C1 C 0.1004(5) 0.3012(7) 0.1601(4) 0.031(2) Uani 1 1 d .
C2 C 0.0481(5) 0.1660(7) 0.2438(4) 0.030(2) Uani 1 1 d .
C3 C 0.0529(5) -0.0093(7) 0.1710(4) 0.029(2) Uani 1 1 d .
C4 C -0.0151(5) 0.1708(6) 0.1200(4) 0.031(2) Uani 1 1 d .
C5 C 0.2748(4) 0.1670(6) 0.2259(4) 0.0231(18) Uani 1 1 d .
C6 C 0.3317(5) 0.0917(7) 0.2587(4) 0.036(2) Uani 1 1 d .
H6A H 0.3593 0.1304 0.2917 0.054 Uiso 1 1 calc R
H6B H 0.3654 0.0648 0.2256 0.054 Uiso 1 1 calc R
H6C H 0.3061 0.0330 0.2792 0.054 Uiso 1 1 calc R
C7 C 0.2296(5) 0.2202(7) 0.2794(4) 0.032(2) Uani 1 1 d .
H7A H 0.2046 0.1666 0.3053 0.048 Uiso 1 1 calc R
H7B H 0.1933 0.2667 0.2594 0.048 Uiso 1 1 calc R
H7C H 0.2619 0.2613 0.3075 0.048 Uiso 1 1 calc R
C8 C 0.3100(5) 0.2533(6) 0.1841(4) 0.0275(19) Uani 1 1 d .
H8A H 0.2802 0.3178 0.1876 0.033 Uiso 1 1 calc R
H8B H 0.3590 0.2693 0.2018 0.033 Uiso 1 1 calc R
C9 C 0.3357(5) 0.3184(6) 0.0741(4) 0.032(2) Uani 1 1 d .
H9A H 0.3140 0.3825 0.0932 0.039 Uiso 1 1 calc R
H9B H 0.3893 0.3278 0.0722 0.039 Uiso 1 1 calc R
C10 C 0.3063(5) 0.3010(7) 0.0078(4) 0.035(2) Uani 1 1 d .
H10A H 0.3332 0.2434 -0.0137 0.042 Uiso 1 1 calc R
H10B H 0.3121 0.3654 -0.0186 0.042 Uiso 1 1 calc R
C11 C 0.1959(5) 0.2253(7) -0.0457(4) 0.034(2) Uani 1 1 d .
H11A H 0.2334 0.1786 -0.0648 0.040 Uiso 1 1 calc R
H11B H 0.1860 0.2818 -0.0775 0.040 Uiso 1 1 calc R
C12 C 0.1246(5) 0.1608(6) -0.0358(4) 0.0263(19) Uani 1 1 d .
C13 C 0.0548(5) 0.2214(7) -0.0360(4) 0.040(2) Uani 1 1 d .
H13A H 0.0548 0.2704 -0.0727 0.060 Uiso 1 1 calc R
H13B H 0.0503 0.2606 0.0047 0.060 Uiso 1 1 calc R
H13C H 0.0136 0.1728 -0.0403 0.060 Uiso 1 1 calc R
C14 C 0.1209(5) 0.0809(7) -0.0906(4) 0.036(2) Uani 1 1 d .
H14A H 0.0781 0.0360 -0.0846 0.054 Uiso 1 1 calc R
H14B H 0.1652 0.0377 -0.0902 0.054 Uiso 1 1 calc R
H14C H 0.1172 0.1176 -0.1323 0.054 Uiso 1 1 calc R
C15 C 0.3763(5) 0.1449(6) 0.1028(4) 0.031(2) Uani 1 1 d .
H15A H 0.4237 0.1736 0.1158 0.046 Uiso 1 1 calc R
H15B H 0.3775 0.1273 0.0564 0.046 Uiso 1 1 calc R
H15C H 0.3660 0.0815 0.1281 0.046 Uiso 1 1 calc R
C16 C 0.1847(5) 0.3705(6) 0.0297(4) 0.035(2) Uani 1 1 d .
H16A H 0.1962 0.4251 -0.0022 0.053 Uiso 1 1 calc R
H16B H 0.1985 0.3946 0.0733 0.053 Uiso 1 1 calc R
H16C H 0.1322 0.3557 0.0287 0.053 Uiso 1 1 calc R
C17 C 0.9338(5) 0.4388(7) 0.1472(4) 0.038(2) Uani 1 1 d .
H17A H 0.9487 0.3683 0.1623 0.046 Uiso 1 1 calc R
H17B H 0.9584 0.4914 0.1750 0.046 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'
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'
W W -0.8490 6.8722 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 Ni1 N2 89.8(3)
N1 Ni1 S2 168.3(2)
N2 Ni1 S2 91.9(2)
N1 Ni1 S1 89.2(2)
N2 Ni1 S1 168.1(2)
S2 Ni1 S1 91.49(9)
N1 Ni1 W1 130.2(2)
N2 Ni1 W1 115.7(2)
S2 Ni1 W1 58.78(6)
S1 Ni1 W1 57.18(6)
C4 W1 C2 91.3(4)
C4 W1 C3 89.9(3)
C2 W1 C3 84.3(4)
C4 W1 C1 89.5(4)
C2 W1 C1 81.2(3)
C3 W1 C1 165.5(3)
C4 W1 S1 166.6(3)
C2 W1 S1 101.2(3)
C3 W1 S1 86.5(3)
C1 W1 S1 97.2(3)
C4 W1 S2 94.9(3)
C2 W1 S2 170.9(2)
C3 W1 S2 89.0(3)
C1 W1 S2 105.5(2)
S1 W1 S2 72.16(6)
C4 W1 Ni1 127.3(3)
C2 W1 Ni1 134.6(3)
C3 W1 Ni1 114.8(3)
C1 W1 Ni1 76.8(2)
S1 W1 Ni1 44.39(5)
S2 W1 Ni1 44.01(5)
C5 S1 Ni1 98.2(3)
C5 S1 W1 118.0(3)
Ni1 S1 W1 78.43(7)
C12 S2 Ni1 100.3(3)
C12 S2 W1 123.3(3)
Ni1 S2 W1 77.21(7)
C8 N1 C9 112.0(6)
C8 N1 C15 113.0(7)
C9 N1 C15 106.6(6)
C8 N1 Ni1 108.9(5)
C9 N1 Ni1 107.5(5)
C15 N1 Ni1 108.6(5)
C11 N2 C16 109.7(7)
C11 N2 C10 113.5(6)
C16 N2 C10 108.2(6)
C11 N2 Ni1 109.8(5)
C16 N2 Ni1 113.0(5)
C10 N2 Ni1 102.7(5)
O1 C1 W1 173.1(8)
O2 C2 W1 178.8(8)
O3 C3 W1 171.4(8)
O4 C4 W1 178.3(8)
C7 C5 C8 108.2(6)
C7 C5 C6 108.7(7)
C8 C5 C6 113.5(7)
C7 C5 S1 110.5(6)
C8 C5 S1 109.5(5)
C6 C5 S1 106.5(5)
N1 C8 C5 114.0(6)
C10 C9 N1 108.6(7)
C9 C10 N2 108.4(7)
N2 C11 C12 115.2(6)
C13 C12 C14 107.8(7)
C13 C12 C11 116.4(7)
C14 C12 C11 107.1(7)
C13 C12 S2 112.2(6)
C14 C12 S2 106.3(5)
C11 C12 S2 106.4(5)
Cl1 C17 Cl2 112.1(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 N1 1.930(7)
Ni1 N2 1.958(6)
Ni1 S2 2.152(2)
Ni1 S1 2.157(2)
Ni1 W1 3.0211(11)
W1 C4 1.944(9)
W1 C2 1.970(9)
W1 C3 2.040(9)
W1 C1 2.052(9)
W1 S1 2.592(2)
W1 S2 2.649(2)
Cl1 C17 1.741(10)
Cl2 C17 1.769(9)
S1 C5 1.870(8)
S2 C12 1.866(8)
O1 C1 1.103(10)
O2 C2 1.134(10)
O3 C3 1.150(10)
O4 C4 1.165(10)
N1 C8 1.470(10)
N1 C9 1.492(10)
N1 C15 1.511(10)
N2 C11 1.470(10)
N2 C16 1.495(10)
N2 C10 1.517(11)
C5 C7 1.535(10)
C5 C8 1.539(10)
C5 C6 1.570(11)
C9 C10 1.483(11)
C11 C12 1.556(12)
C12 C13 1.494(12)
C12 C14 1.520(11)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 Ni1 W1 C4 138.7(4)
N2 Ni1 W1 C4 25.0(4)
S2 Ni1 W1 C4 -50.6(3)
S1 Ni1 W1 C4 -165.9(3)
N1 Ni1 W1 C2 -3.5(4)
N2 Ni1 W1 C2 -117.1(4)
S2 Ni1 W1 C2 167.3(3)
S1 Ni1 W1 C2 52.0(4)
N1 Ni1 W1 C3 -111.0(4)
N2 Ni1 W1 C3 135.4(3)
S2 Ni1 W1 C3 59.8(3)
S1 Ni1 W1 C3 -55.5(3)
N1 Ni1 W1 C1 59.6(4)
N2 Ni1 W1 C1 -54.0(3)
S2 Ni1 W1 C1 -129.6(3)
S1 Ni1 W1 C1 115.1(3)
N1 Ni1 W1 S1 -55.5(3)
N2 Ni1 W1 S1 -169.1(2)
S2 Ni1 W1 S1 115.28(10)
N1 Ni1 W1 S2 -170.7(3)
N2 Ni1 W1 S2 75.6(2)
S1 Ni1 W1 S2 -115.28(10)
N1 Ni1 S1 C5 23.9(3)
N2 Ni1 S1 C5 -61.2(10)
S2 Ni1 S1 C5 -167.8(3)
W1 Ni1 S1 C5 -117.1(3)
N1 Ni1 S1 W1 141.04(19)
N2 Ni1 S1 W1 55.9(10)
S2 Ni1 S1 W1 -50.67(7)
C4 W1 S1 C5 149.9(11)
C2 W1 S1 C5 -51.9(4)
C3 W1 S1 C5 -135.4(4)
C1 W1 S1 C5 30.5(4)
S2 W1 S1 C5 134.5(3)
Ni1 W1 S1 C5 93.2(3)
C4 W1 S1 Ni1 56.7(11)
C2 W1 S1 Ni1 -145.1(3)
C3 W1 S1 Ni1 131.4(2)
C1 W1 S1 Ni1 -62.7(2)
S2 W1 S1 Ni1 41.30(6)
N1 Ni1 S2 C12 -95.2(10)
N2 Ni1 S2 C12 2.9(3)
S1 Ni1 S2 C12 171.5(3)
W1 Ni1 S2 C12 122.1(3)
N1 Ni1 S2 W1 142.8(10)
N2 Ni1 S2 W1 -119.1(2)
S1 Ni1 S2 W1 49.48(7)
C4 W1 S2 C12 47.9(4)
C2 W1 S2 C12 -180(25)
C3 W1 S2 C12 137.7(4)
C1 W1 S2 C12 -43.0(4)
S1 W1 S2 C12 -135.7(3)
Ni1 W1 S2 C12 -94.0(3)
C4 W1 S2 Ni1 141.9(2)
C2 W1 S2 Ni1 -85.7(17)
C3 W1 S2 Ni1 -128.3(2)
C1 W1 S2 Ni1 51.1(3)
S1 W1 S2 Ni1 -41.64(6)
N2 Ni1 N1 C8 126.1(5)
S2 Ni1 N1 C8 -135.6(9)
S1 Ni1 N1 C8 -42.0(5)
W1 Ni1 N1 C8 1.8(6)
N2 Ni1 N1 C9 4.6(5)
S2 Ni1 N1 C9 102.9(10)
S1 Ni1 N1 C9 -163.6(5)
W1 Ni1 N1 C9 -119.8(5)
N2 Ni1 N1 C15 -110.4(5)
S2 Ni1 N1 C15 -12.1(14)
S1 Ni1 N1 C15 81.5(5)
W1 Ni1 N1 C15 125.3(4)
N1 Ni1 N2 C11 143.1(6)
S2 Ni1 N2 C11 -25.3(5)
S1 Ni1 N2 C11 -131.8(9)
W1 Ni1 N2 C11 -81.3(5)
N1 Ni1 N2 C16 -94.1(6)
S2 Ni1 N2 C16 97.5(5)
S1 Ni1 N2 C16 -9.0(14)
W1 Ni1 N2 C16 41.5(6)
N1 Ni1 N2 C10 22.2(5)
S2 Ni1 N2 C10 -146.2(5)
S1 Ni1 N2 C10 107.2(10)
W1 Ni1 N2 C10 157.8(4)
C4 W1 C1 O1 71(7)
C2 W1 C1 O1 -21(7)
C3 W1 C1 O1 -17(8)
S1 W1 C1 O1 -121(7)
S2 W1 C1 O1 165(7)
Ni1 W1 C1 O1 -161(7)
C4 W1 C2 O2 118(43)
C3 W1 C2 O2 28(43)
C1 W1 C2 O2 -153(43)
S1 W1 C2 O2 -58(43)
S2 W1 C2 O2 -15(44)
Ni1 W1 C2 O2 -92(43)
C4 W1 C3 O3 -71(5)
C2 W1 C3 O3 20(5)
C1 W1 C3 O3 17(6)
S1 W1 C3 O3 122(5)
S2 W1 C3 O3 -166(5)
Ni1 W1 C3 O3 157(5)
C2 W1 C4 O4 142(28)
C3 W1 C4 O4 -133(28)
C1 W1 C4 O4 61(28)
S1 W1 C4 O4 -59(29)
S2 W1 C4 O4 -44(28)
Ni1 W1 C4 O4 -12(29)
Ni1 S1 C5 C7 114.2(5)
W1 S1 C5 C7 33.0(6)
Ni1 S1 C5 C8 -4.8(6)
W1 S1 C5 C8 -86.0(6)
Ni1 S1 C5 C6 -127.8(5)
W1 S1 C5 C6 151.0(4)
C9 N1 C8 C5 167.0(7)
C15 N1 C8 C5 -72.5(9)
Ni1 N1 C8 C5 48.2(8)
C7 C5 C8 N1 -146.3(7)
C6 C5 C8 N1 93.0(8)
S1 C5 C8 N1 -25.8(8)
C8 N1 C9 C10 -151.3(7)
C15 N1 C9 C10 84.5(8)
Ni1 N1 C9 C10 -31.7(8)
N1 C9 C10 N2 52.3(9)
C11 N2 C10 C9 -163.7(7)
C16 N2 C10 C9 74.3(8)
Ni1 N2 C10 C9 -45.3(7)
C16 N2 C11 C12 -79.3(9)
C10 N2 C11 C12 159.6(7)
Ni1 N2 C11 C12 45.4(8)
N2 C11 C12 C13 84.5(9)
N2 C11 C12 C14 -154.9(7)
N2 C11 C12 S2 -41.4(9)
Ni1 S2 C12 C13 -110.3(6)
W1 S2 C12 C13 -28.9(7)
Ni1 S2 C12 C14 132.0(5)
W1 S2 C12 C14 -146.6(5)
Ni1 S2 C12 C11 18.1(6)
W1 S2 C12 C11 99.5(5)
