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_7004653
_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 As B Cl2 N O5 W'
_chemical_formula_weight         541.66
_chemical_name_systematic
;
?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.14(3)
_cell_angle_beta                 100.66(3)
_cell_angle_gamma                103.98(3)
_cell_formula_units_Z            4
_cell_length_a                   8.9480(18)
_cell_length_b                   12.013(2)
_cell_length_c                   15.729(3)
_cell_measurement_reflns_used    5965
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      1.37
_cell_volume                     1545.4(7)
_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      100(1)
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'STOE-IPDS diffractometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11701
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.956
_exptl_absorpt_correction_T_max  0.6223
_exptl_absorpt_correction_T_min  0.2147
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.884
_refine_diff_density_min         -6.328
_refine_diff_density_rms         0.458
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                5153
_reflns_number_total             6192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809773a.txt
_cod_data_source_block           acl1
_cod_original_cell_volume        1545.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004653