#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:36:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179148 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/09/4310950.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_4310950
loop_
_publ_author_name
'Valerie Autissier'
'William Clegg'
'Ross W. Harrington'
'Richard A. Henderson'
_publ_section_title
;
 Proton Transfer to Nickel-Thiolate Complexes. 1. Protonation of
 [Ni(SC6H4R-4)2(Ph2PCH2CH2PPh2)] (R = Me, MeO, H, Cl, or NO2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3098
_journal_page_last               3105
_journal_paper_doi               10.1021/ic030322e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C38 H34 Ni P2 S2'
_chemical_formula_sum            'C38 H34 Ni P2 S2'
_chemical_formula_weight         675.42
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 92.756(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3764(16)
_cell_length_b                   15.9241(12)
_cell_length_c                   14.1357(13)
_cell_measurement_reflns_used    14678
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2.35
_cell_volume                     3232.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4735
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0456
_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)+(0.0755P)²+5.2535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                4108
_reflns_number_total             4737
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic030322e_s_1.cif
_cod_data_source_block           rah49
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4310950
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.75265(3) 0.2500 0.01652(13) Uani 1 2 d S . .
P1 P 0.49025(4) 0.85111(4) 0.35440(5) 0.01877(16) Uani 1 1 d . . .
S1 S 0.49127(4) 0.66473(4) 0.12905(5) 0.01974(16) Uani 1 1 d . . .
C1 C 0.51928(17) 0.95372(15) 0.30100(19) 0.0259(6) Uani 1 1 d . . .
H1A H 0.4913 1.0001 0.3366 0.031 Uiso 1 1 calc R . .
H1B H 0.5876 0.9618 0.3031 0.031 Uiso 1 1 calc R . .
C2 C 0.56337(16) 0.84537(15) 0.4627(2) 0.0234(6) Uani 1 1 d . . .
C3 C 0.5279(2) 0.82651(19) 0.5501(2) 0.0343(7) Uani 1 1 d . . .
H3 H 0.4628 0.8193 0.5555 0.041 Uiso 1 1 calc R . .
C4 C 0.5882(3) 0.8182(2) 0.6296(3) 0.0494(9) Uani 1 1 d . . .
H4 H 0.5635 0.8049 0.6889 0.059 Uiso 1 1 calc R . .
C5 C 0.6822(3) 0.8289(2) 0.6243(3) 0.0564(11) Uani 1 1 d . . .
H5 H 0.7221 0.8241 0.6795 0.068 Uiso 1 1 calc R . .
C6 C 0.7188(2) 0.8469(2) 0.5372(3) 0.0527(11) Uani 1 1 d . . .
H6 H 0.7841 0.8538 0.5325 0.063 Uiso 1 1 calc R . .
C7 C 0.65992(18) 0.85459(19) 0.4578(3) 0.0380(7) Uani 1 1 d . . .
H7 H 0.6854 0.8664 0.3984 0.046 Uiso 1 1 calc R . .
C8 C 0.37138(15) 0.86258(16) 0.39259(19) 0.0206(5) Uani 1 1 d . . .
C9 C 0.34498(17) 0.92807(17) 0.4507(2) 0.0293(6) Uani 1 1 d . . .
H9 H 0.3880 0.9714 0.4676 0.035 Uiso 1 1 calc R . .
C10 C 0.25541(18) 0.93003(19) 0.4842(2) 0.0340(7) Uani 1 1 d . . .
H10 H 0.2380 0.9741 0.5251 0.041 Uiso 1 1 calc R . .
C11 C 0.19174(17) 0.86822(18) 0.4582(2) 0.0323(7) Uani 1 1 d . . .
H11 H 0.1311 0.8694 0.4819 0.039 Uiso 1 1 calc R . .
C12 C 0.21611(17) 0.80483(18) 0.3979(2) 0.0317(7) Uani 1 1 d . . .
H12 H 0.1716 0.7634 0.3785 0.038 Uiso 1 1 calc R . .
C13 C 0.30604(16) 0.80143(17) 0.3653(2) 0.0255(6) Uani 1 1 d . . .
H13 H 0.3229 0.7573 0.3243 0.031 Uiso 1 1 calc R . .
C14 C 0.54954(15) 0.56855(15) 0.15600(18) 0.0195(5) Uani 1 1 d . . .
C15 C 0.51059(18) 0.49470(16) 0.1194(2) 0.0268(6) Uani 1 1 d . . .
H15 H 0.4523 0.4965 0.0848 0.032 Uiso 1 1 calc R . .
C16 C 0.5563(2) 0.41772(17) 0.1331(2) 0.0334(6) Uani 1 1 d . . .
H16 H 0.5297 0.3679 0.1066 0.040 Uiso 1 1 calc R . .
C17 C 0.63961(19) 0.41416(18) 0.1847(2) 0.0333(7) Uani 1 1 d . . .
H17 H 0.6703 0.3618 0.1942 0.040 Uiso 1 1 calc R . .
C18 C 0.67911(17) 0.48693(18) 0.2230(2) 0.0301(6) Uani 1 1 d . . .
H18 H 0.7361 0.4842 0.2599 0.036 Uiso 1 1 calc R . .
C19 C 0.63483(15) 0.56408(16) 0.20718(19) 0.0243(6) Uani 1 1 d . . .
H19 H 0.6631 0.6140 0.2315 0.029 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'
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
P1 Ni1 P1 87.05(4) . 2_655 ?
P1 Ni1 S1 169.99(3) . . ?
P1 Ni1 S1 86.24(2) 2_655 . ?
P1 Ni1 S1 86.24(2) . 2_655 ?
P1 Ni1 S1 169.99(3) 2_655 2_655 ?
S1 Ni1 S1 101.33(4) . 2_655 ?
Ni1 P1 C1 109.73(9) . . ?
Ni1 P1 C2 118.99(8) . . ?
Ni1 P1 C8 111.50(9) . . ?
C1 P1 C2 104.76(12) . . ?
C1 P1 C8 105.32(11) . . ?
C2 P1 C8 105.52(12) . . ?
Ni1 S1 C14 111.81(9) . . ?
P1 C1 C1 107.88(12) . 2_655 ?
P1 C2 C3 122.49(19) . . ?
P1 C2 C7 119.1(2) . . ?
C3 C2 C7 118.2(3) . . ?
C2 C3 C4 119.8(3) . . ?
C3 C4 C5 121.5(4) . . ?
C4 C5 C6 119.4(3) . . ?
C5 C6 C7 119.6(3) . . ?
C2 C7 C6 121.4(3) . . ?
P1 C8 C9 122.35(19) . . ?
P1 C8 C13 118.42(19) . . ?
C9 C8 C13 119.2(2) . . ?
C8 C9 C10 120.0(3) . . ?
C9 C10 C11 120.3(3) . . ?
C10 C11 C12 120.1(2) . . ?
C11 C12 C13 120.0(3) . . ?
C8 C13 C12 120.3(3) . . ?
S1 C14 C15 118.12(19) . . ?
S1 C14 C19 123.25(19) . . ?
C15 C14 C19 118.5(2) . . ?
C14 C15 C16 120.7(3) . . ?
C15 C16 C17 120.1(3) . . ?
C16 C17 C18 120.2(2) . . ?
C17 C18 C19 119.8(2) . . ?
C14 C19 C18 120.7(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 P1 2.1624(7) . ?
Ni1 P1 2.1624(7) 2_655 ?
Ni1 S1 2.2086(7) . ?
Ni1 S1 2.2086(7) 2_655 ?
P1 C1 1.856(3) . ?
P1 C2 1.818(3) . ?
P1 C8 1.826(2) . ?
S1 C14 1.778(2) . ?
C1 C1 1.520(5) 2_655 ?
C2 C3 1.392(4) . ?
C2 C7 1.401(3) . ?
C3 C4 1.391(4) . ?
C4 C5 1.368(5) . ?
C5 C6 1.392(6) . ?
C6 C7 1.379(5) . ?
C8 C9 1.392(4) . ?
C8 C13 1.394(4) . ?
C9 C10 1.393(3) . ?
C10 C11 1.382(4) . ?
C11 C12 1.377(4) . ?
C12 C13 1.394(3) . ?
C14 C15 1.391(4) . ?
C14 C19 1.395(3) . ?
C15 C16 1.400(4) . ?
C16 C17 1.373(4) . ?
C17 C18 1.389(4) . ?
C18 C19 1.397(4) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 Ni1 P1 C1 -11.29(8) 2_655 . . . ?
P1 Ni1 P1 C2 -131.83(10) 2_655 . . . ?
P1 Ni1 P1 C8 105.00(9) 2_655 . . . ?
S1 Ni1 P1 C1 -59.24(16) . . . . ?
S1 Ni1 P1 C1 161.27(9) 2_655 . . . ?
S1 Ni1 P1 C2 -179.78(15) . . . . ?
S1 Ni1 P1 C2 40.74(10) 2_655 . . . ?
S1 Ni1 P1 C8 57.05(17) . . . . ?
S1 Ni1 P1 C8 -82.43(9) 2_655 . . . ?
P1 Ni1 S1 C14 -167.98(14) . . . . ?
P1 Ni1 S1 C14 144.02(8) 2_655 . . . ?
S1 Ni1 S1 C14 -29.36(8) 2_655 . . . ?
Ni1 P1 C1 C1 36.7(2) . . . 2_655 ?
C2 P1 C1 C1 165.5(2) . . . 2_655 ?
C8 P1 C1 C1 -83.5(2) . . . 2_655 ?
Ni1 P1 C2 C3 -108.0(2) . . . . ?
Ni1 P1 C2 C7 67.6(2) . . . . ?
C1 P1 C2 C3 129.0(2) . . . . ?
C1 P1 C2 C7 -55.4(2) . . . . ?
C8 P1 C2 C3 18.1(3) . . . . ?
C8 P1 C2 C7 -166.3(2) . . . . ?
P1 C2 C3 C4 176.3(2) . . . . ?
C7 C2 C3 C4 0.7(4) . . . . ?
C2 C3 C4 C5 0.5(5) . . . . ?
C3 C4 C5 C6 -1.2(5) . . . . ?
C4 C5 C6 C7 0.7(5) . . . . ?
C5 C6 C7 C2 0.5(5) . . . . ?
P1 C2 C7 C6 -177.0(2) . . . . ?
C3 C2 C7 C6 -1.2(4) . . . . ?
Ni1 P1 C8 C9 -172.2(2) . . . . ?
Ni1 P1 C8 C13 10.4(2) . . . . ?
C1 P1 C8 C9 -53.2(3) . . . . ?
C1 P1 C8 C13 129.4(2) . . . . ?
C2 P1 C8 C9 57.3(3) . . . . ?
C2 P1 C8 C13 -120.1(2) . . . . ?
P1 C8 C9 C10 -174.7(2) . . . . ?
C13 C8 C9 C10 2.7(4) . . . . ?
C8 C9 C10 C11 -1.5(4) . . . . ?
C9 C10 C11 C12 -0.9(4) . . . . ?
C10 C11 C12 C13 2.0(4) . . . . ?
C11 C12 C13 C8 -0.8(4) . . . . ?
P1 C8 C13 C12 175.9(2) . . . . ?
C9 C8 C13 C12 -1.6(4) . . . . ?
Ni1 S1 C14 C15 143.15(18) . . . . ?
Ni1 S1 C14 C19 -40.7(2) . . . . ?
S1 C14 C15 C16 175.9(2) . . . . ?
C19 C14 C15 C16 -0.5(4) . . . . ?
C14 C15 C16 C17 1.4(4) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C16 C17 C18 C19 -1.3(4) . . . . ?
S1 C14 C19 C18 -177.5(2) . . . . ?
C15 C14 C19 C18 -1.3(4) . . . . ?
C17 C18 C19 C14 2.3(4) . . . . ?
