Selective halogenation at the pnictogen atom in Lewis-acid/base-stabilised phosphanylboranes and arsanylboranes
Schwan, Karl-Christian; Adolf, Ariane; Thoms, Christine; Zabel, Manfred; Timoshkin, Alexey Y.; Scheer, Manfred; Dalton Transactions  (2008) 5054–5058; doi:10.1039/b809773a

data_7004652
_publ_section_title
;
 Selective halogenation at the pnictogen atom in
 Lewis-acid/base-stabilised phosphanylboranes and arsanylboranes
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              5054
_journal_page_last               5058
_journal_paper_doi               10.1039/b809773a
_journal_year                    2008
_chemical_formula_sum            'C8 H11 B Br2 N O5 P W'
_chemical_formula_weight         586.63
_chemical_name_systematic
;
?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 131.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.639(6)
_cell_length_b                   7.3060(15)
_cell_length_c                   20.260(4)
_cell_measurement_reflns_used    1335
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      2.75
_cell_volume                     3262.3(19)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    SIEMENS-XP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9641
_diffrn_reflns_theta_full        22.35
_diffrn_reflns_theta_max         22.35
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    6.493
_exptl_absorpt_correction_T_max  0.3448
_exptl_absorpt_correction_T_min  0.2258
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+7.0264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                3654
_reflns_number_total             4062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809773a.txt
_cod_data_source_block           br6a
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7004652