Trivinylphosphineborane (CH2CH)3PBH3 and related compounds
Monkowius, Uwe; Nogai, Stefan; Schmidbaur, Hubert; Dalton Transactions  (2003) 987–; doi:10.1039/b210991c

data_7012440
_publ_section_title
;
 Trivinylphosphineborane (CH2&#xE001;CH)3PBH3 and related compounds
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              987
_journal_paper_doi               10.1039/b210991c
_journal_year                    2003
_chemical_formula_sum            'C6 H9 B Br3 P'
_chemical_formula_weight         362.64
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.1093(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.95430(10)
_cell_length_b                   11.3363(2)
_cell_length_c                   14.5709(2)
_cell_measurement_reflns_used    45210
_cell_measurement_temperature    143(2)
_cell_volume                     1147.02(3)
_computing_cell_refinement       DENZO
_computing_data_collection       XPRESS
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius DIP 2020'
_diffrn_measurement_method       phi-rotation
_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  0.050
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45210
_diffrn_reflns_theta_full        31.90
_diffrn_reflns_theta_max         31.90
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    10.633
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type   delabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0000P)^2^+0.3640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                3467
_reflns_number_total             3930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210991c.txt
_cod_data_source_block           uwe10
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012440