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_7132601
_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         'C54 H76 B3 Cl Ge N6 O, 1.25(C6 H6)'
_chemical_formula_sum            'C61.5 H83.5 B3 Cl Ge N6 O'
_chemical_formula_weight         1063.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                95.160(3)
_cell_angle_beta                 97.087(3)
_cell_angle_gamma                89.930(3)
_cell_formula_units_Z            8
_cell_length_a                   16.4864(6)
_cell_length_b                   16.4582(5)
_cell_length_c                   44.1370(14)
_cell_measurement_reflns_used    102486
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      0.93
_cell_volume                     11835.7(7)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            73606
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.117
_diffrn_reflns_theta_max         25.117
_diffrn_reflns_theta_min         1.242
_diffrn_source                   'Genix Mo HF'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.8960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4532
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.682
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2658
_refine_ls_number_reflns         40545
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1071P)^2^+26.2246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30639
_reflns_number_total             40545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05760g2.cif
_cod_data_source_block           i3480
_cod_depositor_comments
'Adding full bibliography for 7132597--7132603.cif.'
_cod_original_formula_sum        'C61.50 H83.50 B3 Cl Ge N6 O'
_cod_database_code               7132601
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.899
_olex2_refinement_description
;
1. Restrained distances
 C116-C1A \\sim C116-C121
 with sigma of 0.02
 C122-C1A \\sim C122-C121
 with sigma of 0.02
 C1A-C1B \\sim C121-C1C
 with sigma of 0.02
 C116-C1B \\sim C116-C1C
 with sigma of 0.04
 C122-C1B \\sim C122-C1C
 with sigma of 0.04
2. Others
 Fixed Sof: H12G(0.5) H12H(0.5) H12I(0.5) H12J(0.5) H12K(0.5) H12L(0.5)
 C1A(0.5) H1A(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C121(0.5) H121(0.5)
 C1C(0.5) H1CA(0.5) H1CB(0.5) H1CC(0.5)
3.a Ternary CH refined with riding coordinates:
 C145(H145), C187(H187), C90(H90), C49(H49), C190(H190), C175(H175), C81(H81),
 C93(H93), C37(H37), C52(H52), C40(H40), C148(H148), C199(H199), C124(H124),
 C160(H160), C178(H178), C16(H16), C105(H105), C66(H66), C133(H133), C28(H28),
 C214(H214), C202(H202), C25(H25), C69(H69), C157(H157), C13(H13), C211(H211),
 C78(H78), C136(H136), C1A(H1A), C102(H102), C121(H121)
3.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C164(H16G,H16H), C163(H16I,H16J), C2(H2A,H2B), C1(H1B,H1C),
 C56(H56A,H56B), C110(H11A,H11B), C109(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C60(H60), C166(H166), C59(H59), C5(H5), C3(H3), C45(H45), C6(H6), C57(H57),
 C86(H86), C74(H74), C112(H112), C165(H165), C185(H185), C4(H4), C63(H63),
 C88(H88), C75(H75), C183(H183), C114(H114), C113(H113), C9(H9), C47(H47),
 C184(H184), C141(H141), C33(H33), C11(H11), C10(H10), C195(H195), C173(H173),
 C143(H143), C65(H65), C46(H46), C21(H21), C167(H167), C64(H64), C171(H171),
 C168(H168), C58(H58), C76(H76), C23(H23), C35(H35), C196(H196), C142(H142),
 C117(H117), C119(H119), C118(H118), C172(H172), C87(H87), C197(H197), C22(H22),
  C34(H34), C111(H111), C155(H155), C153(H153), C98(H98), C207(H207),
 C129(H129), C131(H131), C209(H209), C130(H130), C100(H100), C154(H154),
 C208(H208), C99(H99), C220(H220), C221(H221), C222(H222), C217(H217),
 C218(H218), C219(H219), C237(H237), C236(H236), C235(H235), C240(H240),
 C239(H239), C238(H238), C245(H245), C246(H246), C241(H241), C242(H242),
 C243(H243), C244(H244), C232(H232), C231(H231), C230(H230), C229(H229),
 C234(H234), C233(H233), C226(H226), C227(H227), C228(H228), C223(H223),
 C224(H224), C225(H225)
3.d Fitted hexagon refined as free rotating group:
 C117(C116,C115,C120,C119,C118), C220(C221,C222,C217,C218,C219), C237(C236,
 C235,C240,C239,C238), C245(C246,C241,C242,C243,C244), C232(C231,C230,C229,C234,
 C233), C226(C227,C228,C223,C224,C225)
3.e Idealised Me refined as rotating group:
 C188(H18A,H18B,H18C), C147(H14A,H14B,H14C), C91(H91A,H91B,H91C), C189(H18D,
 H18E,H18F), C146(H14D,H14E,H14F), C51(H51A,H51B,H51C), C92(H92A,H92B,H92C),
 C50(H50A,H50B,H50C), C192(H19A,H19B,H19C), C191(H19D,H19E,H19F), C83(H83A,H83B,
 H83C), C54(H54A,H54B,H54C), C201(H20A,H20B,H20C), C106(H10C,H10D,H10E),
 C42(H42A,H42B,H42C), C53(H53A,H53B,H53C), C68(H68A,H68B,H68C), C107(H10F,H10G,
 H10H), C95(H95A,H95B,H95C), C203(H20D,H20E,H20F), C82(H82A,H82B,H82C),
 C15(H15J,H15K,H15L), C158(H15A,H15B,H15C), C125(H12A,H12B,H12C), C134(H13A,
 H13B,H13C), C29(H29A,H29B,H29C), C94(H94A,H94B,H94C), C26(H26A,H26B,H26C),
 C149(H14G,H14H,H14I), C176(H17A,H17B,H17C), C41(H41A,H41B,H41C), C204(H20G,
 H20H,H20I), C150(H15D,H15E,H15F), C30(H30A,H30B,H30C), C135(H13D,H13E,H13F),
 C27(H27A,H27B,H27C), C177(H17D,H17E,H17F), C67(H67A,H67B,H67C), C38(H38A,H38B,
 H38C), C14(H14J,H14K,H14L), C126(H12D,H12E,H12F), C39(H39A,H39B,H39C),
 C162(H16A,H16B,H16C), C122(H12G,H12H,H12I), C122(H12J,H12K,H12L), C70(H70A,
 H70B,H70C), C79(H79A,H79B,H79C), C137(H13G,H13H,H13I), C179(H17G,H17H,H17I),
 C200(H20J,H20K,H20L), C212(H21A,H21B,H21C), C213(H21D,H21E,H21F), C180(H18G,
 H18H,H18I), C80(H80A,H80B,H80C), C18(H18J,H18K,H18L), C71(H71A,H71B,H71C),
 C17(H17J,H17K,H17L), C161(H16D,H16E,H16F), C138(H13J,H13K,H13L), C216(H21G,
 H21H,H21I), C215(H21J,H21K,H21L), C159(H15G,H15H,H15I), C1B(H1BA,H1BB,H1BC),
 C104(H10I,H10J,H10K), C103(H10L,H10M,H10N), C1C(H1CA,H1CB,H1CC)
;
_shelx_res_checksum              71845
_shelx_hkl_checksum              14674
_olex2_submission_special_instructions 'No special instructions were received'