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_4135260
_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         'C22 H32 B Cl2 N Si2 Zr'
_chemical_formula_sum            'C22 H32 B Cl2 N Si2 Zr'
_chemical_formula_weight         539.59
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 87.971(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4049(12)
_cell_length_b                   16.8227(13)
_cell_length_c                   18.9102(14)
_cell_measurement_reflns_used    4449
_cell_measurement_temperature    145
_cell_measurement_theta_max      27.045
_cell_measurement_theta_min      2.421
_cell_volume                     5215.5(7)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      145
_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_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2113
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72778
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.249
_diffrn_reflns_theta_max         24.249
_diffrn_reflns_theta_min         2.421
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6049
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.545
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8424
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0727P)^2^+3.1129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5141
_reflns_number_total             8424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c06538_si_002.cif
_cod_data_source_block           5
_cod_database_code               4135260
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N00C, B016
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M),
 C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00S(H00S), C00U(H00U),
 C00V(H00V), C00W(H00W), C00Y(H00Y), C00Z(H00Z), C010(H010), C013(H013),
 C014(H014), C018(H018), C01A(H01J), C01D(H01N), C3(H3), C01H(H01R), C2(H2),
 C4(H4), C1(H1), C5(H5)
4.b Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C00T(H00D,H00F,H00H), C00X(H00I,H00R,H00T), C011(H01V,
 H01W,H01X), C012(H01A,H01B,H01C), C015(H01D,H01E,H01F), C017(H01G,H01H,H01I),
 C01B(H01K,H01L,H01M), C01C(H01Y,H,HA), C01E(H01O,H01P,H01Q), C01G(H01Z,HB,HC),
 C01I(H01S,H01T,H01U)
;
_olex2_submission_special_instructions 'No special instructions were received'