A bromo(boryloxy) silylene and its heavier analogues.
Guthardt, Robin; Jones, Cameron; Chemical communications (Cambridge, England) 60 (2024) 1583–1586; doi:10.1039/d3cc05760g

data_7132600
_publ_section_title
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 A bromo(boryloxy) silylene and its heavier analogues.
;
_journal_issue                   12
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1583
_journal_page_last               1586
_journal_paper_doi               10.1039/d3cc05760g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C54 H76 B3 Cl3 N6 O Si)'
_chemical_formula_sum            'C108 H152 B6 Cl6 N12 O2 Si2'
_chemical_formula_weight         1984.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-10-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
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2023-11-23 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.47230(10)
_cell_length_b                   23.17940(10)
_cell_length_c                   24.88890(10)
_cell_measurement_reflns_used    38517
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      79.4140
_cell_measurement_theta_min      3.7780
_cell_volume                     11233.76(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            66695
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.402
_diffrn_reflns_theta_min         3.456
_exptl_absorpt_coefficient_mu    1.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 8673 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   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1307
_refine_ls_number_reflns         22991
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0656P)^2^+3.5453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                21315
_reflns_number_total             22991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05760g2.cif
_cod_data_source_block           BOSiCl3_auto
_cod_depositor_comments
'Adding full bibliography for 7132597--7132603.cif.'
_cod_database_code               7132600
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
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1. Restrained distances
 C66-C71 \\sim C66-C72
 with sigma of 0.02
 C71-C76 \\sim C72-C75
 with sigma of 0.02
 C71-C73 \\sim C72-C74
 with sigma of 0.02
 C66-C76 \\sim C66-C75
 with sigma of 0.04
 C66-C73 \\sim C66-C74
 with sigma of 0.04
 C76-C73 \\sim C75-C74
 with sigma of 0.04
2. Rigid body (RIGU) restrains
 C71, C76, C73, C72, C75, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C72)=Sof(H72)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C74)=Sof(H74A)=
 Sof(H74B)=Sof(H74C)=1-FVAR(1)
 Sof(C71)=Sof(H71)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C73)=Sof(H73A)=
 Sof(H73B)=Sof(H73C)=FVAR(1)
 Fixed Sof: H67(0.5) H67A(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C69(0.5)
 H69A(0.5) H69B(0.5) H69C(0.5) C68(0.5) H68A(0.5) H68B(0.5) H68C(0.5) C70(0.5)
 H70A(0.5) H70B(0.5) H70C(0.5)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C25(H25), C28(H28), C52(H52), C40(H40), C16(H16), C37(H37),
 C49(H49), C83(H83), C85(H85), C97(H97), C106(H106), C71(H71), C109(H109),
 C94(H94), C67(H67), C67(H67A), C72(H72)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C55(H55A,H55B), C56(H56A,H56B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C33(H33), C34(H34), C5(H5), C4(H4), C59(H59), C35(H35), C6(H6),
 C23(H23), C11(H11), C57(H57), C58(H58), C81(H81), C47(H47), C63(H63), C9(H9),
 C79(H79), C22(H22), C45(H45), C80(H80), C60(H60), C46(H46), C10(H10), C21(H21),
  C64(H64), C65(H65), C92(H92), C90(H90), C102(H102), C91(H91), C104(H104),
 C103(H103)
4.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C50(H50A,H50B,H50C), C15(H15A,H15B,H15C), C02E(H02A,H02B,
 H02C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C), C18(H18A,
 H18B,H18C), C17(H17A,H17B,H17C), C38(H38A,H38B,H38C), C84(H84A,H84B,H84C),
 C53(H53A,H53B,H53C), C02V(H02D,H02E,H02F), C98(H98A,H98B,H98C), C30(H30A,H30B,
 H30C), C39(H39A,H39B,H39C), C99(H99A,H99B,H99C), C51(H51A,H51B,H51C),
 C108(H10A,H10B,H10C), C42(H42A,H42B,H42C), C96(H96A,H96B,H96C), C110(H11A,H11B,
 H11C), C86(H86A,H86B,H86C), C54(H54A,H54B,H54C), C111(H11D,H11E,H11F),
 C95(H95A,H95B,H95C), C107(H10D,H10E,H10F), C87(H87A,H87B,H87C), C76(H76A,H76B,
 H76C), C41(H41A,H41B,H41C), C69(H69A,H69B,H69C), C68(H68A,H68B,H68C), C70(H70A,
 H70B,H70C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              73238
_shelx_hkl_checksum              32027
_olex2_submission_special_instructions 'No special instructions were received'