Facile Access to Halogenated Cationic B=C-centered Organoboron Isoelectronic with Alkenyl Halides
Xiang, Libo; Wang, Junyi; Su, Wei; Lin, Zhenyang; Ye, Qing; Dalton Transactions  (2021) –; doi:10.1039/D1DT03325E

data_7708772
_publ_section_title
;
 Facile Access to Halogenated Cationic B=C-centered Organoboron
 Isoelectronic with Alkenyl Halides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03325E
_journal_year                    2021
_chemical_formula_moiety         'Br, C47 H43 B Br O P2, C H2 Cl2'
_chemical_formula_sum            'C48 H45 B Br2 Cl2 O P2'
_chemical_formula_weight         941.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2180(10)
_cell_length_b                   13.9664(8)
_cell_length_c                   18.1404(10)
_cell_measurement_reflns_used    7735
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.842
_cell_measurement_theta_min      2.188
_cell_volume                     4362.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_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            48419
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.245
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5544
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 2244 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7660
_refine_ls_number_restraints     301
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1160P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1818
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5966
_reflns_number_total             7660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03325e2.cif
_cod_data_source_block           5
_cod_database_code               7708772
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.818
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C1S)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10A) \\sim Ueq,
Uanis(C9A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(H8BC)=Sof(H8BD)=Sof(H11C)=Sof(H11D)=Sof(C10A)=Sof(H10C)=Sof(H10D)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(H11A)=Sof(H11B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8AA,H8AB), C8(H8BC,H8BD), C11(H11A,H11B), C11(H11C,H11D), C1S(H1SA,H1SB),
 C10(H10A,H10B), C9(H9A,H9B), C10A(H10C,H10D), C9A(H9AA,H9AB)
4.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C27(H27), C29(H29), C30(H30), C36(H36), C23(H23), C26(H26),
 C28(H28), C42(H42), C41(H41), C38(H38), C32(H32), C48(H48), C40(H40), C19(H19),
  C20(H20), C21(H21), C13(H13), C17(H17), C35(H35), C33(H33), C39(H39),
 C15(H15), C46(H46), C16(H16), C47(H47), C7(H7), C45(H45), C44(H44), C4(H4),
 C3(H3), C5(H5), C6(H6), C14(H14), C34(H34)
;
_shelx_res_checksum              38159
_olex2_submission_special_instructions 'No special instructions were received'