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_4333707
_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         'C16 H32 Na O8 +,C13 H27 B P Si2 -'
_chemical_formula_sum            'C29 H59 B Na O8 P Si2'
_chemical_formula_weight         656.71
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.293(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.851(8)
_cell_length_b                   11.927(3)
_cell_length_c                   22.254(6)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      3.3
_cell_volume                     7464(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6946
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37659
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       slab
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         10809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0472P)^2^+2.4766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                8422
_reflns_number_total             10809
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302205b_si_001_3.cif
_cod_data_source_block           ki334_compound_14
_cod_original_cell_volume        7464(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4333707