Radical-Type Reactivity of the 1,3-Dibora-2,4-Diphosphoniocyclobutane-1,3-diyl
Hideki Amii; Lidija Vranicar; Heinz Gornitzka; Didier Bourissou; Guy Bertrand; Journal of the American Chemical Society 126 (2004) 1344–1345; doi:10.1021/ja039920i

data_4112191
_publ_section_title
;
 Radical-Type Reactivity of the
 1,3-Dibora-2,4-Diphosphoniocyclobutane-1,3-diyl
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1344
_journal_page_last               1345
_journal_paper_doi               10.1021/ja039920i
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C20.5 H46 B2 Br Cl P2'
_chemical_formula_weight         491.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 110.408(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.684(2)
_cell_length_b                   10.1828(11)
_cell_length_c                   14.0169(16)
_cell_measurement_reflns_used    7146
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.449
_cell_measurement_theta_min      2.284
_cell_volume                     2633.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker CCD detector'
_diffrn_measurement_method       'phi and omega 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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11658
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.816885
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0338P)^2^+2.5428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                3283
_reflns_number_total             3786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039920isi20031203_074816.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C20.50 H46 B2 Br Cl P2'
_cod_database_code               4112191