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_4128661
_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 N O9 P3 Si0.5'
_chemical_formula_weight         493.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1805(17)
_cell_length_b                   18.929(2)
_cell_length_c                   19.042(2)
_cell_measurement_reflns_used    7925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.17
_cell_volume                     4750.9(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            69898
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.018
_diffrn_reflns_theta_min         1.883
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.059
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.7042
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0399P)^2^+2.7119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4750
_reflns_number_total             6953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01475_si_001.cif
_cod_data_source_block           X8_17115
_cod_original_cell_volume        4751.1(10)
_cod_original_formula_sum        'C16 H36 N O9 P3 Si0.50'
_cod_database_code               4128661
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              44207
_shelx_hkl_checksum              62861