Orthophosphate and Sulfate Utilization for C-E (E = P, S) Bond Formation via Trichlorosilyl Phosphide and Sulfide Anions.
Geeson, Michael B.; Ríos, Pablo; Transue, Wesley J.; Cummins, Christopher C.; Journal of the American Chemical Society 141 (2019) 6375–6384; doi:10.1021/jacs.9b01475

data_4128660
_publ_section_title
;
 Orthophosphate and Sulfate Utilization for C-E (E = P, S) Bond Formation
 via Trichlorosilyl Phosphide and Sulfide Anions.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6375
_journal_page_last               6384
_journal_paper_doi               10.1021/jacs.9b01475
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C16 H36 Cl3 N S Si'
_chemical_formula_weight         408.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.363(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.253(12)
_cell_length_b                   15.242(11)
_cell_length_c                   18.394(13)
_cell_measurement_reflns_used    9397
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.28
_cell_volume                     4706(6)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            134795
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         1.755
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.156
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         11224
_refine_ls_number_restraints     1420
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+4.8450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8530
_reflns_number_total             11224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01475_si_002.cif
_cod_data_source_block           X8_18045_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4128660
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              85727
_shelx_hkl_checksum              54703