Solution-Phase Synthesis of a Base-Free Benzoborirene and a Three-Dimensional Inorganic Analogue.
Zhang, Hui; Wang, Junyi; Yang, Weiguang; Xiang, Libo; Sun, Weicheng; Ming, Wenbo; Li, Yinxin; Lin, Zhenyang; Ye, Qing; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c06538

data_4135263
_publ_section_title
;
 Solution-Phase Synthesis of a Base-Free Benzoborirene and a
 Three-Dimensional Inorganic Analogue.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c06538
_journal_year                    2020
_chemical_formula_moiety         'C19 H48 B11 N3 Si2'
_chemical_formula_sum            'C19 H48 B11 N3 Si2'
_chemical_formula_weight         493.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.683(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6845(5)
_cell_length_b                   19.2174(11)
_cell_length_c                   16.6527(8)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      27.503
_cell_measurement_theta_min      2.357
_cell_volume                     3095.9(3)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      104.02
_diffrn_measured_fraction_theta_full 0.9868
_diffrn_measured_fraction_theta_max 0.9868
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19979
_diffrn_reflns_theta_full        24.9978
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1400 before and 0.0788 after correction. The Ratio of minimum to maximum transmission is 0.5661. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.0592
_exptl_crystal_description       block
_exptl_crystal_F_000             1064.8443
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.6510
_refine_diff_density_min         -0.4410
_refine_diff_density_rms         0.0718
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             8.6408
_refine_ls_goodness_of_fit_ref   1.0398
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0398
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+1.7406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -11
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -8
_reflns_number_gt                4746
_reflns_number_total             5393
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c06538_si_002.cif
_cod_data_source_block           14
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4135263
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C12(H12)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C11(H11a,H11b,H11c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c),
 C16(H16a,H16b,H16c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,
 H20c)
2.c Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2a), B3(H3), B0aa(H0aa), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9),
 B10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'