Phosphido-Borane and Phosphido-Bis(Borane) Complexes of the Alkali Metals, a Comparative Study
Keith Izod; James M. Watson; William Clegg; Ross W. Harrington; Inorganic Chemistry 52 (2013) 1466–1475; doi:10.1021/ic302205b

data_4333710
_publ_section_title
;
 Phosphido-Borane and Phosphido-Bis(Borane) Complexes of the Alkali
 Metals, a Comparative Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1466
_journal_page_last               1475
_journal_paper_doi               10.1021/ic302205b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H46 B2 Na O2 P Si2'
_chemical_formula_sum            'C21 H46 B2 Na O2 P Si2'
_chemical_formula_weight         462.34
_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                85.291(18)
_cell_angle_beta                 71.807(19)
_cell_angle_gamma                81.117(16)
_cell_formula_units_Z            2
_cell_length_a                   9.661(3)
_cell_length_b                   12.453(2)
_cell_length_c                   12.956(4)
_cell_measurement_reflns_used    240
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     1462.1(7)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23357
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.95
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+1.1159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                4089
_reflns_number_total             5118
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302205b_si_001_6.cif
_cod_data_source_block           ki320_compound_17
_cod_depositor_comments
;

2021-05-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1462.0(6)
_cod_original_formula_moiety     'C42 H92 B4 Na2 O4 P2 Si4'
_cod_original_formula_sum        'C42 H92 B4 Na2 O4 P2 Si4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     924.68
_cod_database_code               4333710