Synthesis of Silaketenimine Anion and Its Coupling with Isocyanide.
Zhu, Lizhao; Zhang, Jianying; Yang, Hao; Cui, Chunming; Journal of the American Chemical Society 141 (2019) 19600–19604; doi:10.1021/jacs.9b11913

data_4133901
_publ_section_title
;
 Synthesis of Silaketenimine Anion and Its Coupling with Isocyanide.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19600
_journal_page_last               19604
_journal_paper_doi               10.1021/jacs.9b11913
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C65 H91 B3 Li N7 Si'
_chemical_formula_sum            'C65 H91 B3 Li N7 Si'
_chemical_formula_weight         1037.90
_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             2019-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 100.59(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.469(3)
_cell_length_b                   23.666(5)
_cell_length_c                   21.590(4)
_cell_measurement_reflns_used    9075
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.9504
_cell_measurement_theta_min      1.7210
_cell_volume                     6263(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1259
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.149
_diffrn_reflns_theta_max         24.149
_diffrn_reflns_theta_min         1.721
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
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_refine_diff_density_min         -0.332
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1267P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2173
_refine_ls_wR_factor_ref         0.2411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6842
_reflns_number_total             10009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11913_si_002.cif
_cod_data_source_block           zlz
_cod_database_code               4133901
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C37(H37), C51(H51), C34(H34), C63(H63), C25(H25), C60(H60), C48(H48),
 C11(H11), C7(H7), C9(H9), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C5(H5A,H5B), C4(H4A,H4B), C10(H10A,H10B),
 C3(H3A,H3B), C6(H6A,H6B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C14(H14), C15(H15), C41(H41), C46(H46), C32(H32), C57(H57),
 C44(H44), C58(H58), C56(H56), C45(H45), C30(H30), C31(H31), C18(H18), C20(H20),
  C19(H19)
2.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C), C53(H53A,H53B,
 H53C), C64(H64A,H64B,H64C), C27(H27A,H27B,H27C), C65(H65A,H65B,H65C), C49(H49A,
 H49B,H49C), C52(H52A,H52B,H52C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C),
 C50(H50A,H50B,H50C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C24(H24A,H24B,
 H24C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              52037
_shelx_hkl_checksum              8732
_olex2_submission_special_instructions 'No special instructions were received'