Synthesis and Chemistry of Bis(borylphosphino)silanes and -germanes
Tuqiang Chen; Eileen N. Duesler; Robert T. Paine; Heinrich Nöth; Inorganic Chemistry 38 (1999) 4993–4999; doi:10.1021/ic990507e

data_4322355
_publ_section_title
;
 Synthesis and Chemistry of Bis(borylphosphino)silanes and -germanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4993
_journal_page_last               4999
_journal_paper_doi               10.1021/ic990507e
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C44 H94 B2 Li2 N4 O4 P2 Si5'
_chemical_formula_weight         981.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.939(2)
_cell_length_b                   24.516(3)
_cell_length_c                   21.572(3)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8.35
_cell_measurement_theta_min      2.00
_cell_volume                     6186.9(16)
_computing_cell_refinement       'XSCANS V2.2 (Siemens, 1994)'
_computing_data_collection       'XSCANS V2.2 (Siemens, 1994)'
_computing_data_reduction        'XSCANS V2.2 (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL V5.0 (Siemens, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .975
_diffrn_measured_fraction_theta_max .975
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_sigmaI/netI    0.2258
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18448
_diffrn_reflns_theta_full        23.51
_diffrn_reflns_theta_max         23.51
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.8792
_exptl_absorpt_correction_T_min  0.8707
_exptl_absorpt_correction_type   'psi-scan corrections'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .163
_refine_diff_density_min         -.172
_refine_diff_density_rms         .033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [0.00000+1.00000exp(8.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0600P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                3267
_reflns_number_total             8951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990507e_3.cif
_cod_data_source_block           rtp961a/15
_cod_original_cell_volume        6186.9(15)
_cod_database_code               4322355