#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:20:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179372 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/69/4326955.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_4326955
loop_
_publ_author_name
'Michael T. Mock'
'Robert G. Potter'
'Molly J. O'Hagan'
'Donald M. Camaioni'
'William G. Dougherty'
'W. Scott Kassel'
'Daniel L. DuBois'
_publ_section_title
;
 Synthesis and Hydride Transfer Reactions of Cobalt and Nickel Hydride
 Complexes to BX3 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11914
_journal_page_last               11928
_journal_paper_doi               10.1021/ic200857x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C24 H43 Co P4 S2'
_chemical_formula_weight         578.51
_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                 96.6510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6910(2)
_cell_length_b                   11.9736(2)
_cell_length_c                   24.4141(5)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.08
_cell_measurement_theta_min      3.65
_cell_volume                     2813.85(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14531
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.37
_diffrn_reflns_theta_min         3.65
_exptl_absorpt_coefficient_mu    8.394
_exptl_absorpt_correction_T_max  0.2846
_exptl_absorpt_correction_T_min  0.2300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0353
_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)+(0.0587P)²+1.6831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                4831
_reflns_number_total             5076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200857x_si_001_02.cif
_cod_data_source_block           pnl012a_Codmpe2SPh_HSPh
_cod_database_code               4326955
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
Co1 Co 0.40281(3) 0.72448(3) 0.142975(13) 0.01055(11) Uani 1 1 d .
P1 P 0.36559(5) 0.64781(5) 0.22285(2) 0.01338(13) Uani 1 1 d .
P2 P 0.21488(5) 0.63190(4) 0.10820(2) 0.01315(13) Uani 1 1 d .
P3 P 0.60329(5) 0.80072(5) 0.17606(2) 0.01357(13) Uani 1 1 d .
P4 P 0.46264(6) 0.76173(4) 0.06028(2) 0.01300(13) Uani 1 1 d .
S1 S 0.26430(6) 0.87495(4) 0.16553(2) 0.01716(13) Uani 1 1 d .
S2 S 0.80657(6) 0.51002(5) 0.07269(2) 0.02297(14) Uani 1 1 d .
H2S H 0.803(3) 0.501(3) 0.0254(12) 0.028 Uiso 1 1 d .
C1 C 0.4890(2) 0.5461(2) 0.25439(10) 0.0220(5) Uani 1 1 d .
H1A H 0.4468 0.5044 0.2827 0.033 Uiso 1 1 calc R
H1B H 0.5723 0.5847 0.2714 0.033 Uiso 1 1 calc R
H1C H 0.5145 0.4944 0.2261 0.033 Uiso 1 1 calc R
C2 C 0.3391(3) 0.7376(2) 0.28102(10) 0.0231(5) Uani 1 1 d .
H2A H 0.3228 0.6914 0.3128 0.035 Uiso 1 1 calc R
H2B H 0.2584 0.7859 0.2710 0.035 Uiso 1 1 calc R
H2C H 0.4218 0.7839 0.2906 0.035 Uiso 1 1 calc R
C3 C 0.2026(2) 0.5674(2) 0.21340(10) 0.0238(5) Uani 1 1 d .
H3A H 0.2231 0.4879 0.2066 0.029 Uiso 1 1 calc R
H3B H 0.1555 0.5719 0.2472 0.029 Uiso 1 1 calc R
C4 C 0.1076(2) 0.6145(2) 0.16443(9) 0.0196(5) Uani 1 1 d .
H4A H 0.0684 0.6872 0.1742 0.024 Uiso 1 1 calc R
H4B H 0.0300 0.5624 0.1534 0.024 Uiso 1 1 calc R
C5 C 0.2369(2) 0.48755(19) 0.08657(10) 0.0222(5) Uani 1 1 d .
H5A H 0.1462 0.4503 0.0817 0.033 Uiso 1 1 calc R
H5B H 0.2987 0.4482 0.1148 0.033 Uiso 1 1 calc R
H5C H 0.2774 0.4867 0.0516 0.033 Uiso 1 1 calc R
C6 C 0.0985(2) 0.6879(2) 0.05136(9) 0.0200(5) Uani 1 1 d .
H6A H 0.0101 0.6474 0.0485 0.030 Uiso 1 1 calc R
H6B H 0.1406 0.6794 0.0170 0.030 Uiso 1 1 calc R
H6C H 0.0819 0.7673 0.0579 0.030 Uiso 1 1 calc R
C7 C 0.6189(2) 0.8952(2) 0.23485(9) 0.0196(5) Uani 1 1 d .
H7A H 0.7039 0.9396 0.2350 0.029 Uiso 1 1 calc R
H7B H 0.6230 0.8518 0.2690 0.029 Uiso 1 1 calc R
H7C H 0.5382 0.9451 0.2322 0.029 Uiso 1 1 calc R
C8 C 0.7493(2) 0.7061(2) 0.19207(10) 0.0212(5) Uani 1 1 d .
H8A H 0.8349 0.7494 0.2005 0.032 Uiso 1 1 calc R
H8B H 0.7579 0.6576 0.1603 0.032 Uiso 1 1 calc R
H8C H 0.7339 0.6602 0.2240 0.032 Uiso 1 1 calc R
C9 C 0.6640(2) 0.88475(19) 0.12080(9) 0.0181(5) Uani 1 1 d .
H9A H 0.6107 0.9553 0.1160 0.022 Uiso 1 1 calc R
H9B H 0.7637 0.9032 0.1298 0.022 Uiso 1 1 calc R
C10 C 0.6419(2) 0.8146(2) 0.06812(9) 0.0184(5) Uani 1 1 d .
H10A H 0.7082 0.7514 0.0705 0.022 Uiso 1 1 calc R
H10B H 0.6578 0.8608 0.0358 0.022 Uiso 1 1 calc R
C11 C 0.4726(2) 0.64496(19) 0.01367(9) 0.0178(5) Uani 1 1 d .
H11A H 0.5126 0.6701 -0.0193 0.027 Uiso 1 1 calc R
H11B H 0.3791 0.6152 0.0029 0.027 Uiso 1 1 calc R
H11C H 0.5314 0.5864 0.0321 0.027 Uiso 1 1 calc R
C12 C 0.3707(3) 0.8675(2) 0.01615(9) 0.0202(5) Uani 1 1 d .
H12A H 0.4083 0.8694 -0.0194 0.030 Uiso 1 1 calc R
H12B H 0.3829 0.9408 0.0339 0.030 Uiso 1 1 calc R
H12C H 0.2716 0.8490 0.0102 0.030 Uiso 1 1 calc R
C13 C 0.1033(2) 1.0019(2) 0.08828(9) 0.0216(5) Uani 1 1 d .
H13A H 0.0340 0.9462 0.0899 0.026 Uiso 1 1 calc R
C14 C 0.0743(3) 1.0954(2) 0.05509(10) 0.0267(5) Uani 1 1 d .
H14A H -0.0141 1.1024 0.0341 0.032 Uiso 1 1 calc R
C15 C 0.1726(3) 1.1779(2) 0.05242(10) 0.0272(6) Uani 1 1 d .
H15A H 0.1527 1.2414 0.0295 0.033 Uiso 1 1 calc R
C16 C 0.3012(3) 1.1670(2) 0.08363(10) 0.0247(5) Uani 1 1 d .
H16A H 0.3692 1.2237 0.0824 0.030 Uiso 1 1 calc R
C17 C 0.3307(2) 1.0736(2) 0.11660(9) 0.0198(5) Uani 1 1 d .
H17A H 0.4190 1.0674 0.1377 0.024 Uiso 1 1 calc R
C18 C 0.2332(2) 0.98880(18) 0.11935(9) 0.0163(4) Uani 1 1 d .
C19 C 0.6374(3) 0.3881(2) 0.13375(10) 0.0234(5) Uani 1 1 d .
H19A H 0.5808 0.4529 0.1339 0.028 Uiso 1 1 calc R
C20 C 0.5993(3) 0.2923(2) 0.15984(10) 0.0269(5) Uani 1 1 d .
H20A H 0.5186 0.2929 0.1785 0.032 Uiso 1 1 calc R
C21 C 0.6771(3) 0.1952(2) 0.15911(10) 0.0291(6) Uani 1 1 d .
H21A H 0.6494 0.1291 0.1764 0.035 Uiso 1 1 calc R
C22 C 0.7961(3) 0.1968(2) 0.13262(10) 0.0286(6) Uani 1 1 d .
H22A H 0.8504 0.1309 0.1317 0.034 Uiso 1 1 calc R
C23 C 0.8368(3) 0.2922(2) 0.10761(10) 0.0247(5) Uani 1 1 d .
H23A H 0.9197 0.2911 0.0903 0.030 Uiso 1 1 calc R
C24 C 0.7589(2) 0.3916(2) 0.10690(9) 0.0195(5) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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
P4 Co1 P3 86.45(2)
P4 Co1 P2 92.40(2)
P3 Co1 P2 173.88(3)
P4 Co1 P1 166.31(3)
P3 Co1 P1 94.30(2)
P2 Co1 P1 85.40(2)
P4 Co1 S1 106.07(2)
P3 Co1 S1 95.70(2)
P2 Co1 S1 90.40(2)
P1 Co1 S1 87.47(2)
C1 P1 C2 102.17(11)
C1 P1 C3 102.47(12)
C2 P1 C3 102.11(12)
C1 P1 Co1 118.92(8)
C2 P1 Co1 119.44(8)
C3 P1 Co1 109.28(8)
C6 P2 C5 102.24(11)
C6 P2 C4 105.04(11)
C5 P2 C4 101.81(11)
C6 P2 Co1 121.27(8)
C5 P2 Co1 117.78(8)
C4 P2 Co1 106.45(8)
C8 P3 C7 103.07(11)
C8 P3 C9 101.05(11)
C7 P3 C9 103.57(11)
C8 P3 Co1 116.72(8)
C7 P3 Co1 122.25(8)
C9 P3 Co1 107.51(8)
C11 P4 C12 102.84(11)
C11 P4 C10 102.28(10)
C12 P4 C10 102.32(11)
C11 P4 Co1 117.17(8)
C12 P4 Co1 121.15(8)
C10 P4 Co1 108.62(7)
C18 S1 Co1 120.01(7)
C4 C3 P1 109.57(15)
C3 C4 P2 106.60(16)
C10 C9 P3 106.93(15)
C9 C10 P4 108.39(15)
C14 C13 C18 120.9(2)
C15 C14 C13 120.6(2)
C14 C15 C16 119.2(2)
C17 C16 C15 120.4(2)
C16 C17 C18 121.3(2)
C17 C18 C13 117.6(2)
C17 C18 S1 121.67(18)
C13 C18 S1 120.41(18)
C20 C19 C24 121.3(2)
C19 C20 C21 121.0(2)
C20 C21 C22 118.5(2)
C23 C22 C21 121.1(3)
C22 C23 C24 121.8(2)
C23 C24 C19 116.3(2)
C23 C24 S2 121.65(18)
C19 C24 S2 121.97(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 P4 2.2097(6)
Co1 P3 2.2129(6)
Co1 P2 2.2154(6)
Co1 P1 2.2223(6)
Co1 S1 2.3500(6)
P1 C1 1.814(2)
P1 C2 1.823(2)
P1 C3 1.842(2)
P2 C6 1.812(2)
P2 C5 1.827(2)
P2 C4 1.828(2)
P3 C8 1.820(2)
P3 C7 1.820(2)
P3 C9 1.834(2)
P4 C11 1.812(2)
P4 C12 1.826(2)
P4 C10 1.838(2)
S1 C18 1.772(2)
S2 C24 1.735(2)
C3 C4 1.530(3)
C9 C10 1.531(3)
C13 C14 1.391(4)
C13 C18 1.402(3)
C14 C15 1.379(4)
C15 C16 1.389(4)
C16 C17 1.387(3)
C17 C18 1.394(3)
C19 C20 1.384(4)
C19 C24 1.413(3)
C20 C21 1.386(4)
C21 C22 1.386(4)
C22 C23 1.374(4)
C23 C24 1.408(3)
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
P4 Co1 P1 C1 31.55(15)
P3 Co1 P1 C1 -61.09(10)
P2 Co1 P1 C1 112.78(10)
S1 Co1 P1 C1 -156.62(10)
P4 Co1 P1 C2 157.60(14)
P3 Co1 P1 C2 64.96(10)
P2 Co1 P1 C2 -121.17(10)
S1 Co1 P1 C2 -30.57(10)
P4 Co1 P1 C3 -85.48(14)
P3 Co1 P1 C3 -178.12(9)
P2 Co1 P1 C3 -4.26(9)
S1 Co1 P1 C3 86.35(9)
P4 Co1 P2 C6 -46.29(10)
P3 Co1 P2 C6 -125.3(2)
P1 Co1 P2 C6 147.25(10)
S1 Co1 P2 C6 59.82(9)
P4 Co1 P2 C5 80.60(9)
P3 Co1 P2 C5 1.6(3)
P1 Co1 P2 C5 -85.86(9)
S1 Co1 P2 C5 -173.30(9)
P4 Co1 P2 C4 -166.02(8)
P3 Co1 P2 C4 115.0(2)
P1 Co1 P2 C4 27.51(9)
S1 Co1 P2 C4 -59.92(9)
P4 Co1 P3 C8 -94.50(9)
P2 Co1 P3 C8 -15.2(3)
P1 Co1 P3 C8 71.80(9)
S1 Co1 P3 C8 159.68(9)
P4 Co1 P3 C7 137.41(10)
P2 Co1 P3 C7 -143.3(2)
P1 Co1 P3 C7 -56.29(10)
S1 Co1 P3 C7 31.59(10)
P4 Co1 P3 C9 18.07(8)
P2 Co1 P3 C9 97.4(2)
P1 Co1 P3 C9 -175.63(8)
S1 Co1 P3 C9 -87.74(8)
P3 Co1 P4 C11 121.77(9)
P2 Co1 P4 C11 -52.20(9)
P1 Co1 P4 C11 28.19(15)
S1 Co1 P4 C11 -143.31(9)
P3 Co1 P4 C12 -111.21(10)
P2 Co1 P4 C12 74.81(10)
P1 Co1 P4 C12 155.21(13)
S1 Co1 P4 C12 -16.30(10)
P3 Co1 P4 C10 6.61(8)
P2 Co1 P4 C10 -167.37(8)
P1 Co1 P4 C10 -86.97(13)
S1 Co1 P4 C10 101.52(8)
P4 Co1 S1 C18 -1.76(10)
P3 Co1 S1 C18 86.18(9)
P2 Co1 S1 C18 -94.37(9)
P1 Co1 S1 C18 -179.75(9)
C1 P1 C3 C4 -152.25(17)
C2 P1 C3 C4 102.19(18)
Co1 P1 C3 C4 -25.24(19)
P1 C3 C4 P2 47.0(2)
C6 P2 C4 C3 -179.88(16)
C5 P2 C4 C3 73.83(18)
Co1 P2 C4 C3 -50.10(17)
C8 P3 C9 C10 78.49(17)
C7 P3 C9 C10 -174.99(15)
Co1 P3 C9 C10 -44.32(17)
P3 C9 C10 P4 49.94(18)
C11 P4 C10 C9 -160.06(16)
C12 P4 C10 C9 93.66(17)
Co1 P4 C10 C9 -35.56(17)
C18 C13 C14 C15 -0.6(3)
C13 C14 C15 C16 -0.4(4)
C14 C15 C16 C17 0.7(3)
C15 C16 C17 C18 0.1(3)
C16 C17 C18 C13 -1.0(3)
C16 C17 C18 S1 -174.72(17)
C14 C13 C18 C17 1.3(3)
C14 C13 C18 S1 175.07(18)
Co1 S1 C18 C17 -80.35(19)
Co1 S1 C18 C13 106.16(17)
C24 C19 C20 C21 -1.9(4)
C19 C20 C21 C22 1.4(4)
C20 C21 C22 C23 0.1(4)
C21 C22 C23 C24 -1.1(4)
C22 C23 C24 C19 0.6(3)
C22 C23 C24 S2 -177.14(19)
C20 C19 C24 C23 0.9(3)
C20 C19 C24 S2 178.59(19)
