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#$Date: 2016-03-22 11:15:02 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178891 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/20/4112080.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_4112080
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            'C14 H20 N2 Ni O4 S2 W'
_chemical_formula_weight         587.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   13.397(4)
_cell_length_b                   12.386(4)
_cell_length_c                   11.005(3)
_cell_measurement_temperature    110(2)
_cell_volume                     1826.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.765
_diffrn_measured_fraction_theta_max 0.765
_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  0.1165
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3982
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    7.574
_exptl_absorpt_correction_T_max  0.5180
_exptl_absorpt_correction_T_min  0.2097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.412
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1291
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0271
_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)+(0.0094P)²+3.5164P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                1240
_reflns_number_total             1291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055051gsi20050726_033412.cif
_cod_data_source_block           niwco4
_cod_original_cell_volume        1826.2(10)
_cod_database_code               4112080
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
W1 W 0.15196(2) 0.2500 0.44255(2) 0.01831(15) Uani 1 2 d S
Ni2 Ni 0.17222(8) 0.2500 0.74597(7) 0.0162(2) Uani 1 2 d S
S5 S 0.21863(11) 0.12751(9) 0.61406(9) 0.0186(4) Uani 1 1 d .
C7 C 0.0152(5) 0.1449(3) 0.8845(4) 0.0230(14) Uani 1 1 d .
H7A H -0.0195 0.0838 0.8447 0.028 Uiso 1 1 calc R
H7B H 0.0037 0.1390 0.9731 0.028 Uiso 1 1 calc R
O2 O 0.0918(3) 0.0729(4) 0.2527(3) 0.0339(12) Uani 1 1 d .
N2 N 0.1288(4) 0.1358(3) 0.8591(3) 0.0204(12) Uani 1 1 d .
C2 C 0.1151(5) 0.1383(4) 0.3254(4) 0.0268(14) Uani 1 1 d .
C1 C 0.0068(10) 0.2500 0.4920(6) 0.032(2) Uani 1 2 d S
C6 C 0.1490(4) 0.0237(4) 0.8088(4) 0.0211(15) Uani 1 1 d .
H6A H 0.1037 -0.0294 0.8474 0.025 Uiso 1 1 calc R
H6B H 0.2187 0.0022 0.8266 0.025 Uiso 1 1 calc R
O1 O -0.0800(7) 0.2500 0.5070(6) 0.049(2) Uani 1 2 d S
C4 C 0.2923(7) 0.2500 0.3691(6) 0.023(2) Uani 1 2 d S
C10 C 0.1671(6) 0.2500 1.0440(5) 0.0107(16) Uani 1 2 d SU
H10A H 0.0961 0.2500 1.0690 0.013 Uiso 1 2 calc SR
H10B H 0.2079 0.2500 1.1190 0.013 Uiso 1 2 calc SR
C11 C -0.0294(7) 0.2500 0.8391(6) 0.0251(16) Uani 1 2 d SU
H11A H -0.0250 0.2500 0.7493 0.030 Uiso 1 2 calc SR
H11B H -0.1012 0.2500 0.8604 0.030 Uiso 1 2 calc SR
C12 C 0.1319(5) 0.0254(4) 0.6719(4) 0.0265(15) Uani 1 1 d .
H12A H 0.0621 0.0454 0.6529 0.032 Uiso 1 1 calc R
H12B H 0.1464 -0.0461 0.6359 0.032 Uiso 1 1 calc R
C13 C 0.1879(6) 0.1454(4) 0.9751(4) 0.0218(14) Uani 1 1 d .
H13A H 0.2600 0.1416 0.9557 0.026 Uiso 1 1 calc R
H13B H 0.1717 0.0833 1.0283 0.026 Uiso 1 1 calc R
O4 O 0.3684(5) 0.2500 0.3199(6) 0.0341(15) Uani 1 2 d S
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'
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
C2 W1 C2 90.1(3) 7_565 .
C2 W1 C1 86.3(2) 7_565 .
C2 W1 C1 86.3(2) . .
C2 W1 C4 88.4(2) 7_565 .
C2 W1 C4 88.4(2) . .
C1 W1 C4 172.4(3) . .
C2 W1 S5 170.34(18) 7_565 .
C2 W1 S5 98.84(16) . .
C1 W1 S5 97.83(16) . .
C4 W1 S5 88.33(16) . .
C2 W1 S5 98.84(16) 7_565 7_565
C2 W1 S5 170.34(18) . 7_565
C1 W1 S5 97.83(17) . 7_565
C4 W1 S5 88.33(16) . 7_565
S5 W1 S5 72.00(5) . 7_565
N2 Ni2 N2 91.7(2) 7_565 .
N2 Ni2 S5 90.29(12) 7_565 7_565
N2 Ni2 S5 177.62(12) . 7_565
N2 Ni2 S5 177.62(12) 7_565 .
N2 Ni2 S5 90.29(12) . .
S5 Ni2 S5 87.70(7) 7_565 .
C12 S5 Ni2 93.87(17) . .
C12 S5 W1 116.1(2) . .
Ni2 S5 W1 88.81(5) . .
C11 C7 N2 112.9(5) . .
C11 C7 H7A 109.0 . .
N2 C7 H7A 109.0 . .
C11 C7 H7B 109.0 . .
N2 C7 H7B 109.0 . .
H7A C7 H7B 107.8 . .
C13 N2 C6 106.7(4) . .
C13 N2 C7 110.9(4) . .
C6 N2 C7 107.9(4) . .
C13 N2 Ni2 108.9(3) . .
C6 N2 Ni2 111.9(3) . .
C7 N2 Ni2 110.5(3) . .
O2 C2 W1 178.2(5) . .
O1 C1 W1 172.5(6) . .
N2 C6 C12 108.7(4) . .
N2 C6 H6A 110.0 . .
C12 C6 H6A 110.0 . .
N2 C6 H6B 110.0 . .
C12 C6 H6B 110.0 . .
H6A C6 H6B 108.3 . .
O4 C4 W1 175.3(6) . .
C13 C10 C13 116.1(5) 7_565 .
C13 C10 H10A 108.3 7_565 .
C13 C10 H10A 108.3 . .
C13 C10 H10B 108.3 7_565 .
C13 C10 H10B 108.3 . .
H10A C10 H10B 107.4 . .
C7 C11 C7 118.2(6) 7_565 .
C7 C11 H11A 107.8 7_565 .
C7 C11 H11A 107.8 . .
C7 C11 H11B 107.8 7_565 .
C7 C11 H11B 107.8 . .
H11A C11 H11B 107.1 . .
C6 C12 S5 105.0(4) . .
C6 C12 H12A 110.8 . .
S5 C12 H12A 110.8 . .
C6 C12 H12B 110.8 . .
S5 C12 H12B 110.8 . .
H12A C12 H12B 108.8 . .
N2 C13 C10 113.1(5) . .
N2 C13 H13A 109.0 . .
C10 C13 H13A 109.0 . .
N2 C13 H13B 109.0 . .
C10 C13 H13B 109.0 . .
H13A C13 H13B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C2 1.955(5) 7_565
W1 C2 1.955(5) .
W1 C1 2.019(13) .
W1 C4 2.047(9) .
W1 S5 2.5811(12) .
W1 S5 2.5811(12) 7_565
Ni2 N2 1.972(4) 7_565
Ni2 N2 1.972(4) .
Ni2 S5 2.1900(13) 7_565
Ni2 S5 2.1900(13) .
S5 C12 1.831(5) .
C7 C11 1.517(6) .
C7 N2 1.551(9) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
O2 C2 1.180(6) .
N2 C13 1.507(6) .
N2 C6 1.518(6) .
C1 O1 1.175(12) .
C6 C12 1.524(6) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C4 O4 1.154(10) .
C10 C13 1.527(6) 7_565
C10 C13 1.527(6) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C7 1.517(6) 7_565
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
