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_7132602
_publ_section_title
;
 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 Br3 N6 O Si)'
_chemical_formula_sum            'C108 H152 B6 Br6 N12 O2 Si2'
_chemical_formula_weight         2250.91
_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
;
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                   19.58760(10)
_cell_length_b                   23.29940(10)
_cell_length_c                   24.94380(10)
_cell_measurement_reflns_used    153105
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      79.9640
_cell_measurement_theta_min      3.7700
_cell_volume                     11383.83(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 0.996
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            236655
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.369
_diffrn_reflns_theta_min         3.439
_exptl_absorpt_coefficient_mu    3.144
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.081
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.313
_exptl_crystal_description       plate
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 10827 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.228(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1287
_refine_ls_number_reflns         24733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0619P)^2^+5.6004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                24022
_reflns_number_total             24733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05760g2.cif
_cod_data_source_block           exp_3094_auto
_cod_depositor_comments
'Adding full bibliography for 7132597--7132603.cif.'
_cod_original_cell_volume        11383.84(9)
_cod_database_code               7132602
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.528
_olex2_refinement_description
;
1. Others
 Sof(C107)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C108)=Sof(H10J)=Sof(H10K)=
 Sof(H10L)=Sof(C1A)=Sof(H1A)=1-FVAR(1)
 Sof(C106)=Sof(H106)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C1C)=Sof(H1CA)=
 Sof(H1CB)=Sof(H1CC)=FVAR(1)
2.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28), C37(H37), C40(H40), C49(H49),
 C52(H52), C67(H67), C70(H70), C79(H79), C82(H82), C91(H91), C94(H94),
 C103(H103), C106(H106), C1A(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C2(H2A,H2B), C55(H55A,H55B), C56(H56A,H56B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C21(H21),
 C22(H22), C23(H23), C33(H33), C34(H34), C35(H35), C45(H45), C46(H46), C47(H47),
  C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C64(H64), C65(H65),
 C75(H75), C76(H76), C77(H77), C87(H87), C88(H88), C89(H89), C99(H99),
 C100(H100), C101(H101)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C92(H92A,H92B,H92C), C93(H93A,H93B,
 H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C104(H10A,H10B,H10C),
 C105(H10D,H10E,H10F), C107(H10G,H10H,H10I), C108(H10J,H10K,H10L), C1B(H1BA,
 H1BB,H1BC), C1C(H1CA,H1CB,H1CC)
;
_shelx_res_checksum              15777
_shelx_hkl_checksum              55642
_olex2_submission_special_instructions 'No special instructions were received'