#------------------------------------------------------------------------------
#$Date: 2016-12-05 20:40:37 +0200 (Mon, 05 Dec 2016) $
#$Revision: 188901 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/68/4086803.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_4086803
loop_
_publ_author_name
'Fischer, Reinald'
'Görls, Helmar'
'Westerhausen, Matthias'
_publ_section_title
;
 Reactivity Studies of [(thf)2Mg{μ-C(CH3)2C2H4C(CH3)2}]2: Scrambling
 Reactions and Diverse Reactions with Dichlorophenylphosphane
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              3861
_journal_paper_doi               10.1021/acs.organomet.6b00743
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C28 H42 P2 S2'
_chemical_formula_sum            'C28 H42 P2 S2'
_chemical_formula_weight         504.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.061(5)
_cell_angle_beta                 93.960(5)
_cell_angle_gamma                112.432(5)
_cell_formula_units_Z            1
_cell_length_a                   8.0198(7)
_cell_length_b                   9.2558(8)
_cell_length_c                   11.4204(9)
_cell_measurement_reflns_used    7212
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.62
_cell_volume                     710.04(11)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7212
_diffrn_reflns_theta_full        27.83
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0698
_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)+(0.0858P)²+0.9989P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                2520
_reflns_number_total             3231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00743_si_001.cif
_cod_data_source_block           FO5588
_cod_original_cell_volume        710.04(10)
_cod_database_code               4086803
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
P1 P 0.42454(11) 0.85595(10) 0.46971(8) 0.0289(2) Uani 1 1 d .
S1 S 0.18729(11) 0.75802(11) 0.34594(9) 0.0381(3) Uani 1 1 d .
C1 C 0.5765(5) 0.7501(4) 0.4010(3) 0.0312(7) Uani 1 1 d .
C2 C 0.6266(5) 0.7938(5) 0.2866(4) 0.0355(8) Uani 1 1 d .
H2B H 0.520(5) 0.780(4) 0.232(3) 0.024(8) Uiso 1 1 d .
H2A H 0.712(5) 0.912(5) 0.325(4) 0.032(9) Uiso 1 1 d .
C3 C 0.7067(6) 0.6830(5) 0.1986(4) 0.0390(8) Uani 1 1 d .
H3B H 0.620(6) 0.573(6) 0.157(4) 0.042(11) Uiso 1 1 d .
H3A H 0.811(6) 0.689(6) 0.257(4) 0.056(13) Uiso 1 1 d .
C4 C 0.7715(6) 0.7356(6) 0.0927(4) 0.0500(10) Uani 1 1 d .
H4A H 0.6582 0.7180 0.0362 0.060 Uiso 1 1 calc R
C5 C 0.9014(9) 0.9167(8) 0.1373(6) 0.0812(18) Uani 1 1 d .
H5A H 0.8407 0.9890 0.1785 0.122 Uiso 1 1 calc R
H5B H 0.9398 0.9389 0.0634 0.122 Uiso 1 1 calc R
H5C H 1.0108 0.9436 0.1998 0.122 Uiso 1 1 calc R
C6 C 0.8438(9) 0.6149(9) 0.0079(5) 0.0640(14) Uani 1 1 d .
H6C H 0.949(7) 0.640(6) 0.056(4) 0.052(13) Uiso 1 1 d .
H6B H 0.887(8) 0.654(7) -0.060(6) 0.081(17) Uiso 1 1 d .
H6A H 0.747(8) 0.492(8) -0.025(5) 0.076(17) Uiso 1 1 d .
C7 C 0.4508(6) 0.5573(5) 0.3568(4) 0.0384(8) Uani 1 1 d .
H7C H 0.390(6) 0.528(5) 0.430(4) 0.048(11) Uiso 1 1 d .
H7B H 0.530(7) 0.501(6) 0.335(4) 0.062(13) Uiso 1 1 d .
H7A H 0.350(6) 0.515(6) 0.286(4) 0.048(12) Uiso 1 1 d .
C8 C 0.7492(5) 0.8016(5) 0.5008(4) 0.0376(8) Uani 1 1 d .
H8C H 0.829(5) 0.920(5) 0.532(3) 0.027(9) Uiso 1 1 d .
H8B H 0.811(6) 0.743(6) 0.456(4) 0.054(12) Uiso 1 1 d .
H8A H 0.722(5) 0.775(5) 0.573(4) 0.041(10) Uiso 1 1 d .
C9 C 0.3944(5) 0.8256(4) 0.6184(3) 0.0337(7) Uani 1 1 d .
C10 C 0.2182(5) 0.7136(5) 0.6178(4) 0.0407(9) Uani 1 1 d .
H10 H 0.124(6) 0.663(5) 0.548(4) 0.042(11) Uiso 1 1 d .
C11 C 0.1895(7) 0.6799(5) 0.7255(5) 0.0506(11) Uani 1 1 d .
H11 H 0.078(6) 0.605(6) 0.721(4) 0.049(12) Uiso 1 1 d .
C12 C 0.3311(7) 0.7564(5) 0.8338(4) 0.0509(11) Uani 1 1 d .
H12 H 0.305(7) 0.738(7) 0.904(5) 0.069(15) Uiso 1 1 d .
C13 C 0.5044(7) 0.8688(5) 0.8359(4) 0.0466(10) Uani 1 1 d .
H13 H 0.600(6) 0.931(6) 0.910(4) 0.048(12) Uiso 1 1 d .
C14 C 0.5367(6) 0.9034(5) 0.7289(4) 0.0378(8) Uani 1 1 d .
H14 H 0.644(5) 0.968(5) 0.727(3) 0.030(9) Uiso 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 0.0033 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'
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_3
C9 P1 C1 105.93(15) .
C9 P1 S1 112.30(12) .
C1 P1 S1 111.44(12) .
C9 P1 P1 106.43(12) 2_676
C1 P1 P1 110.04(11) 2_676
S1 P1 P1 110.48(6) 2_676
C8 C1 C2 111.8(3) .
C8 C1 C7 108.6(3) .
C2 C1 C7 111.9(3) .
C8 C1 P1 113.3(2) .
C2 C1 P1 107.4(2) .
C7 C1 P1 103.5(2) .
C3 C2 C1 114.3(3) .
C3 C2 H2B 106(2) .
C1 C2 H2B 112(2) .
C3 C2 H2A 112(2) .
C1 C2 H2A 105(2) .
H2B C2 H2A 108(3) .
C4 C3 C2 114.5(3) .
C4 C3 H3B 105(3) .
C2 C3 H3B 110(3) .
C4 C3 H3A 112(3) .
C2 C3 H3A 106(3) .
H3B C3 H3A 110(4) .
C5 C4 C3 114.7(4) .
C5 C4 C6 112.5(4) .
C3 C4 C6 110.6(4) .
C5 C4 H4A 106.1 .
C3 C4 H4A 106.1 .
C6 C4 H4A 106.1 .
C4 C5 H5A 109.5 .
C4 C5 H5B 109.5 .
H5A C5 H5B 109.5 .
C4 C5 H5C 109.5 .
H5A C5 H5C 109.5 .
H5B C5 H5C 109.5 .
C4 C6 H6C 105(3) .
C4 C6 H6B 108(3) .
H6C C6 H6B 102(4) .
C4 C6 H6A 110(3) .
H6C C6 H6A 116(4) .
H6B C6 H6A 115(4) .
C1 C7 H7C 113(2) .
C1 C7 H7B 106(3) .
H7C C7 H7B 108(4) .
C1 C7 H7A 112(3) .
H7C C7 H7A 106(3) .
H7B C7 H7A 112(4) .
C1 C8 H8C 111(2) .
C1 C8 H8B 105(3) .
H8C C8 H8B 107(3) .
C1 C8 H8A 114(2) .
H8C C8 H8A 109(3) .
H8B C8 H8A 111(4) .
C14 C9 C10 118.7(3) .
C14 C9 P1 124.0(3) .
C10 C9 P1 117.2(3) .
C11 C10 C9 119.7(4) .
C11 C10 H10 120(3) .
C9 C10 H10 120(3) .
C12 C11 C10 121.1(4) .
C12 C11 H11 121(3) .
C10 C11 H11 118(3) .
C11 C12 C13 119.5(4) .
C11 C12 H12 118(3) .
C13 C12 H12 122(3) .
C12 C13 C14 120.3(4) .
C12 C13 H13 122(3) .
C14 C13 H13 118(3) .
C13 C14 C9 120.6(4) .
C13 C14 H14 122(3) .
C9 C14 H14 118(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C9 1.836(3) .
P1 C1 1.884(3) .
P1 S1 1.9574(12) .
P1 P1 2.2693(16) 2_676
C1 C8 1.527(5) .
C1 C2 1.536(5) .
C1 C7 1.538(5) .
C2 C3 1.525(4) .
C2 H2B 0.96(4) .
C2 H2A 0.95(4) .
C3 C4 1.513(5) .
C3 H3B 0.90(4) .
C3 H3A 1.00(5) .
C4 C5 1.461(7) .
C4 C6 1.522(6) .
C4 H4A 1.0000 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6C 0.88(5) .
C6 H6B 1.00(6) .
C6 H6A 1.00(6) .
C7 H7C 1.07(4) .
C7 H7B 0.96(5) .
C7 H7A 0.95(5) .
C8 H8C 0.94(4) .
C8 H8B 0.92(5) .
C8 H8A 0.96(4) .
C9 C14 1.391(5) .
C9 C10 1.395(5) .
C10 C11 1.388(6) .
C10 H10 0.90(4) .
C11 C12 1.372(7) .
C11 H11 0.88(5) .
C12 C13 1.374(6) .
C12 H12 0.90(5) .
C13 C14 1.387(5) .
C13 H13 0.93(4) .
C14 H14 0.85(4) .
