#------------------------------------------------------------------------------
#$Date: 2019-11-25 21:41:16 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241879 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/17/4131710.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_4131710
loop_
_publ_author_name
'Wu, Lipeng'
'Chitnis, Saurabh S.'
'Jiao, Haijun'
'Annibale, Vincent T.'
'Manners, Ian'
_publ_section_title
;
 Non-Metal-Catalyzed Heterodehydrocoupling of Phosphines and Hydrosilanes:
 Mechanistic Studies of B(C₆F₅)₃-Mediated
 Formation of P-Si Bonds.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16780
_journal_page_last               16790
_journal_paper_doi               10.1021/jacs.7b09175
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C32 H42 P2 Si4'
_chemical_formula_weight         600.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                95.921(2)
_cell_angle_beta                 90.442(3)
_cell_angle_gamma                111.095(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7920(3)
_cell_length_b                   10.0353(4)
_cell_length_c                   11.4214(5)
_cell_measurement_reflns_used    3840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.774
_cell_measurement_theta_min      1.795
_cell_volume                     827.83(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14463
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.774
_diffrn_reflns_theta_min         1.795
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Apex 2'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       Plate
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0310P)²+1.8369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3323
_reflns_number_total             3840
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b09175_si_001.cif
_cod_data_source_block           3e
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4131710
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.901
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
P1 P 0.93411(9) 0.22221(7) 0.32554(6) 0.01334(15) Uani 1 1 d . .
Si1 Si 0.69784(9) 0.30113(8) 0.33073(6) 0.01443(16) Uani 1 1 d . .
Si2 Si 0.17526(9) 0.00882(8) 0.75555(6) 0.01409(16) Uani 1 1 d . .
C1 C 1.0749(3) 0.3328(3) 0.2170(2) 0.0163(5) Uani 1 1 d . .
C2 C 1.0385(4) 0.3067(3) 0.0955(3) 0.0270(6) Uani 1 1 d . .
H2 H 0.9352 0.2261 0.0633 0.032 Uiso 1 1 calc R U
C3 C 1.1526(5) 0.3979(4) 0.0209(3) 0.0339(7) Uani 1 1 d . .
H3 H 1.1263 0.3794 -0.0618 0.041 Uiso 1 1 calc R U
C4 C 1.3029(4) 0.5144(3) 0.0661(3) 0.0297(7) Uani 1 1 d . .
H4 H 1.3808 0.5757 0.0147 0.036 Uiso 1 1 calc R U
C5 C 1.3407(4) 0.5424(3) 0.1864(3) 0.0282(7) Uani 1 1 d . .
H5 H 1.4441 0.6234 0.2179 0.034 Uiso 1 1 calc R U
C6 C 1.2273(4) 0.4519(3) 0.2614(3) 0.0214(6) Uani 1 1 d . .
H6 H 1.2541 0.4716 0.3440 0.026 Uiso 1 1 calc R U
C7 C 0.5443(4) 0.2434(3) 0.1938(2) 0.0219(6) Uani 1 1 d . .
H7A H 0.4648 0.3001 0.1938 0.033 Uiso 1 1 calc R U
H7B H 0.4680 0.1413 0.1912 0.033 Uiso 1 1 calc R U
H7C H 0.6196 0.2587 0.1246 0.033 Uiso 1 1 calc R U
C8 C 0.8019(4) 0.5015(3) 0.3535(3) 0.0236(6) Uani 1 1 d . .
H8A H 0.7039 0.5410 0.3610 0.035 Uiso 1 1 calc R U
H8B H 0.8748 0.5367 0.2860 0.035 Uiso 1 1 calc R U
H8C H 0.8818 0.5320 0.4255 0.035 Uiso 1 1 calc R U
C9 C 0.5584(3) 0.2273(3) 0.4587(2) 0.0139(5) Uani 1 1 d . .
C10 C 0.3720(4) 0.2085(3) 0.4572(2) 0.0168(5) Uani 1 1 d . .
H10 H 0.3202 0.2380 0.3937 0.020 Uiso 1 1 calc R U
C11 C 0.2605(3) 0.1475(3) 0.5464(2) 0.0159(5) Uani 1 1 d . .
H11 H 0.1342 0.1364 0.5429 0.019 Uiso 1 1 calc R U
C12 C 0.3309(3) 0.1022(3) 0.6415(2) 0.0144(5) Uani 1 1 d . .
C13 C 0.5189(3) 0.1238(3) 0.6443(2) 0.0159(5) Uani 1 1 d . .
H13 H 0.5711 0.0957 0.7084 0.019 Uiso 1 1 calc R U
C14 C 0.6305(3) 0.1856(3) 0.5553(2) 0.0158(5) Uani 1 1 d . .
H14 H 0.7577 0.1997 0.5600 0.019 Uiso 1 1 calc R U
C15 C -0.0297(4) 0.0630(3) 0.7666(3) 0.0220(6) Uani 1 1 d . .
H15A H 0.0106 0.1666 0.7908 0.033 Uiso 1 1 calc R U
H15B H -0.1109 0.0108 0.8250 0.033 Uiso 1 1 calc R U
H15C H -0.0966 0.0402 0.6897 0.033 Uiso 1 1 calc R U
C16 C 0.3039(4) 0.0595(3) 0.9025(2) 0.0231(6) Uani 1 1 d . .
H16A H 0.4075 0.0259 0.9000 0.035 Uiso 1 1 calc R U
H16B H 0.2210 0.0149 0.9632 0.035 Uiso 1 1 calc R U
H16C H 0.3504 0.1643 0.9212 0.035 Uiso 1 1 calc R U
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'
Si Si 0.0817 0.0704 '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'
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
C1 P1 Si1 99.92(8) .
C1 P1 Si2 108.16(9) 2_656
Si1 P1 Si2 107.66(4) 2_656
C8 Si1 C7 109.32(13) .
C8 Si1 C9 111.36(12) .
C7 Si1 C9 108.82(12) .
C8 Si1 P1 106.40(10) .
C7 Si1 P1 114.10(9) .
C9 Si1 P1 106.85(8) .
C15 Si2 C12 110.90(12) .
C15 Si2 C16 108.31(13) .
C12 Si2 C16 109.20(12) .
C15 Si2 P1 105.33(10) 2_656
C12 Si2 P1 102.63(8) 2_656
C16 Si2 P1 120.25(10) 2_656
C6 C1 C2 118.3(2) .
C6 C1 P1 116.8(2) .
C2 C1 P1 124.9(2) .
C1 C2 C3 120.4(3) .
C1 C2 H2 119.8 .
C3 C2 H2 119.8 .
C4 C3 C2 120.5(3) .
C4 C3 H3 119.8 .
C2 C3 H3 119.8 .
C3 C4 C5 119.9(3) .
C3 C4 H4 120.0 .
C5 C4 H4 120.0 .
C4 C5 C6 119.9(3) .
C4 C5 H5 120.0 .
C6 C5 H5 120.0 .
C5 C6 C1 120.9(3) .
C5 C6 H6 119.5 .
C1 C6 H6 119.5 .
Si1 C7 H7A 109.5 .
Si1 C7 H7B 109.5 .
H7A C7 H7B 109.5 .
Si1 C7 H7C 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
Si1 C8 H8A 109.5 .
Si1 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
Si1 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C10 C9 C14 117.5(2) .
C10 C9 Si1 119.09(19) .
C14 C9 Si1 123.35(19) .
C11 C10 C9 121.4(2) .
C11 C10 H10 119.3 .
C9 C10 H10 119.3 .
C10 C11 C12 121.2(2) .
C10 C11 H11 119.4 .
C12 C11 H11 119.4 .
C11 C12 C13 117.3(2) .
C11 C12 Si2 120.60(19) .
C13 C12 Si2 122.01(19) .
C14 C13 C12 121.4(2) .
C14 C13 H13 119.3 .
C12 C13 H13 119.3 .
C13 C14 C9 121.0(2) .
C13 C14 H14 119.5 .
C9 C14 H14 119.5 .
Si2 C15 H15A 109.5 .
Si2 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
Si2 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
Si2 C16 H16A 109.5 .
Si2 C16 H16B 109.5 .
H16A C16 H16B 109.5 .
Si2 C16 H16C 109.5 .
H16A C16 H16C 109.5 .
H16B C16 H16C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C1 1.844(3) .
P1 Si1 2.2498(9) .
P1 Si2 2.2544(9) 2_656
Si1 C8 1.866(3) .
Si1 C7 1.870(3) .
Si1 C9 1.880(3) .
Si2 C15 1.865(3) .
Si2 C12 1.872(3) .
Si2 C16 1.874(3) .
Si2 P1 2.2544(9) 2_656
C1 C6 1.393(4) .
C1 C2 1.393(4) .
C2 C3 1.394(4) .
C2 H2 0.9500 .
C3 C4 1.373(5) .
C3 H3 0.9500 .
C4 C5 1.381(5) .
C4 H4 0.9500 .
C5 C6 1.391(4) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.395(3) .
C9 C14 1.401(3) .
C10 C11 1.388(3) .
C10 H10 0.9500 .
C11 C12 1.399(4) .
C11 H11 0.9500 .
C12 C13 1.401(3) .
C13 C14 1.389(3) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
