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_7708771
_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 P2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C47.5 H44 B Br2 Cl P2'
_chemical_formula_weight         882.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 109.757(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8309(14)
_cell_length_b                   18.9924(13)
_cell_length_c                   20.3151(11)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.409
_cell_measurement_theta_min      2.285
_cell_volume                     8290.4(9)
_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  0.1119
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            127726
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.285
_exptl_absorpt_coefficient_mu    2.131
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1218 before and 0.0881 after correction.
The Ratio of minimum to maximum transmission is 0.8188.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         14584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+16.5844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11004
_reflns_number_total             14584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03325e2.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C47.50 H44 B Br2 Cl P2'
_cod_database_code               7708771
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.815
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C80(H80), C82(H82), C86(H86), C92(H92), C70(H70), C62(H62), C91(H91),
 C58(H58), C85(H85), C88(H88), C79(H79), C31(H31), C89(H89), C64(H64), C83(H83),
  C35(H35), C76(H76), C84(H84), C74(H74), C47(H47), C90(H90), C61(H61),
 C71(H71), C78(H78), C68(H68), C32(H32), C34(H34), C65(H65), C72(H72), C73(H73),
  C59(H59), C67(H67), C60(H60), C46(H46), C66(H66), C41(H41), C37(H37),
 C17(H17), C33(H33), C25(H25), C77(H77), C43(H43), C29(H29), C13(H13), C28(H28),
  C45(H45), C15(H15), C19(H19), C14(H14), C16(H16), C40(H40), C27(H27),
 C26(H26), C44(H44), C5(H5), C23(H23), C38(H38), C39(H39), C50(H50), C22(H22),
 C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C53(H53A,H53B,H53C), C11(H11A,H11B,H11C), C8(H8A,H8B,
 H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C)
;
_shelx_res_checksum              96211
_shelx_fab_checksum              5335
_olex2_submission_special_instructions 'No special instructions were received'