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_7132603
_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         '3(C54 H76 B3 Cl N6 O Sn)'
_chemical_formula_sum            'C162 H228 B9 Cl3 N18 O3 Sn3'
_chemical_formula_weight         3035.32
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 106.314(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.8728(4)
_cell_length_b                   16.2163(2)
_cell_length_c                   33.9145(6)
_cell_measurement_reflns_used    49287
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      30.3910
_cell_measurement_theta_min      3.1530
_cell_volume                     16295.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.8941
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -24.00 105.00   0.50   47.05    --   22.17  42.00-155.00  258
  2  \w    -63.00  52.00   0.50   47.05    --   22.17 -42.00  51.00  230
  3  \w    -23.00  30.00   0.50   47.05    --  -22.33 -99.00 -30.00  106
  4  \w    -23.00  30.00   0.50   47.05    --  -22.33 -99.00   0.00  106
  5  \w    -23.00  30.00   0.50   47.05    --  -22.33 -99.00-180.00  106
  6  \w   -117.00 -63.00   0.50   47.05    --  -22.33-178.00   0.00  108
  7  \w   -117.00 -63.00   0.50   47.05    --  -22.33-178.00 150.00  108
  8  \w     42.00  67.00   0.50   47.05    --   22.17 178.00  60.00   50
  9  \w    -69.00  62.00   0.50   47.05    --   22.17 -19.00 150.00  262
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0210237000
_diffrn_orient_matrix_UB_12      -0.0142057000
_diffrn_orient_matrix_UB_13      0.0019478000
_diffrn_orient_matrix_UB_21      -0.0111287000
_diffrn_orient_matrix_UB_22      0.0181413000
_diffrn_orient_matrix_UB_23      -0.0192165000
_diffrn_orient_matrix_UB_31      0.0026246000
_diffrn_orient_matrix_UB_32      -0.0371763000
_diffrn_orient_matrix_UB_33      -0.0101020000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            224156
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.043
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       plate
_exptl_crystal_F_000             6384
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1861
_refine_ls_number_reflns         46657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+7.1619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29845
_reflns_number_total             46657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05760g2.cif
_cod_data_source_block           cj1639
_cod_depositor_comments
'Adding full bibliography for 7132597--7132603.cif.'
_cod_database_code               7132603
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.888
_diffrn_oxdiff_ac3_digest_hkl    016db15c6d64a8291496cb092a22b0c01e5c24
_olex2_refinement_description
;
1. Others
 Sof(C37A)=Sof(H37A)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C38A)=
 Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(H39C)=FVAR(1)
2.a Ternary CH refined with riding coordinates:
 C160(H160), C79(H79), C49(H49), C91(H91), C136(H136), C82(H82), C106(H106),
 C157(H157), C94(H94), C25(H25), C133(H133), C28(H28), C67(H67), C70(H70),
 C16(H16), C148(H148), C52(H52), C40(H40), C13(H13), C121(H121), C145(H145),
 C37(H37), C103(H103), C124(H124), C37A(H37A)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C55(H55A,H55B), C56(H56A,H56B), C109(H10A,H10B),
 C110(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C129(H129), C114(H114), C21(H21), C57(H57), C131(H131), C58(H58), C155(H155),
 C113(H113), C10(H10), C75(H75), C130(H130), C6(H6), C11(H11), C153(H153),
 C87(H87), C9(H9), C154(H154), C4(H4), C111(H111), C63(H63), C89(H89), C88(H88),
  C45(H45), C22(H22), C5(H5), C118(H118), C142(H142), C112(H112), C23(H23),
 C3(H3), C143(H143), C141(H141), C60(H60), C101(H101), C65(H65), C99(H99),
 C46(H46), C76(H76), C64(H64), C33(H33), C35(H35), C77(H77), C34(H34),
 C100(H100), C47(H47), C59(H59), C119(H119), C117(H117)
2.d Idealised Me refined as rotating group:
 C161(H16A,H16B,H16C), C50(H50A,H50B,H50C), C80(H80A,H80B,H80C), C162(H16D,
 H16E,H16F), C51(H51A,H51B,H51C), C137(H13A,H13B,H13C), C69(H69A,H69B,H69C),
 C93(H93A,H93B,H93C), C83(H83A,H83B,H83C), C81(H81A,H81B,H81C), C92(H92A,H92B,
 H92C), C26(H26A,H26B,H26C), C96(H96A,H96B,H96C), C71(H71A,H71B,H71C),
 C107(H10C,H10D,H10E), C17(H17A,H17B,H17C), C138(H13D,H13E,H13F), C68(H68A,H68B,
 H68C), C159(H15D,H15E,H15F), C84(H84A,H84B,H84C), C95(H95A,H95B,H95C),
 C158(H15G,H15H,H15I), C135(H13G,H13H,H13I), C42(H42A,H42B,H42C), C72(H72A,H72B,
 H72C), C41(H41A,H41B,H41C), C123(H12A,H12B,H12C), C27(H27A,H27B,H27C),
 C149(H14D,H14E,H14F), C122(H12D,H12E,H12F), C134(H13J,H13K,H13L), C53(H53A,
 H53B,H53C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C),
 C108(H10F,H10G,H10H), C54(H54A,H54B,H54C), C150(H15J,H15K,H15L), C30(H30A,H30B,
 H30C), C146(H14G,H14H,H14I), C104(H10I,H10J,H10K), C147(H14J,H14K,H14L),
 C14(H14A,H14B,H14C), C125(H12G,H12H,H12I), C105(H10L,H10M,H10N), C38(H38A,H38B,
 H38C), C126(H12J,H12K,H12L), C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F),
 C38A(H38D,H38E,H38F)
;
_shelx_res_checksum              56622
_shelx_hkl_checksum              35117
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.777
_oxdiff_exptl_absorpt_empirical_full_min 0.402