The Stannylphosphide Anion Reagent Sodium Bis(triphenylstannyl) Phosphide: Synthesis, Structural Characterization, and Reactions with Indium, Tin, and Gold Electrophiles.
Cummins, Christopher C.; Huang, Chao; Miller, Tabitha J.; Reintinger, Markus W.; Stauber, Julia M.; Tannou, Isabelle; Tofan, Daniel; Toubaei, Abouzar; Velian, Alexandra; Wu, Gang; Inorganic chemistry 53 (2014) 3678–; doi:10.1021/ic403178j

data_4338022
_publ_section_title
;
 The Stannylphosphide Anion Reagent Sodium Bis(triphenylstannyl)
 Phosphide: Synthesis, Structural Characterization, and Reactions with
 Indium, Tin, and Gold Electrophiles.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3678
_journal_paper_doi               10.1021/ic403178j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C50 H50 Na O5 P Sn2'
_chemical_formula_weight         1022.24
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 97.656(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.252(2)
_cell_length_b                   20.081(5)
_cell_length_c                   22.705(5)
_cell_measurement_reflns_used    9389
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.75
_cell_measurement_theta_min      2.31
_cell_volume                     4632.6(18)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            112029
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.359
_diffrn_source                   'fine-focus sealed tube, graphite'
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6874
_refine_diff_density_max         1.894
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
; 
 Flack x determined using 10297 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         28151
_refine_ls_number_restraints     415
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+3.0738P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                24048
_reflns_number_total             28151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic403178j_si_003.cif
_cod_data_source_block           13008-p21
_cod_depositor_comments
'Adding full bibliography for 4338021--4338024.cif.'
_cod_original_cell_volume        4632.5(18)
_cod_database_code               4338022
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2012-9
_shelx_res_checksum              54289
_shelx_hkl_checksum              84602