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_4133900
_publ_section_title
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 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         'C80 H114 B3 Li N8 O Si, C7 H8'
_chemical_formula_sum            'C87 H122 B3 Li N8 O Si'
_chemical_formula_weight         1363.39
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
????
;
_cell_angle_alpha                76.41(3)
_cell_angle_beta                 80.00(3)
_cell_angle_gamma                69.32(3)
_cell_formula_units_Z            2
_cell_length_a                   13.644(3)
_cell_length_b                   17.783(4)
_cell_length_c                   18.523(4)
_cell_measurement_reflns_used    7588
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9024
_cell_measurement_theta_min      1.1366
_cell_volume                     4066.6(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.1500
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36563
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         1.25
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8657
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         12968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1136P)^2^+0.4455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2080
_reflns_number_gt                9971
_reflns_number_total             12968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b11913_si_004.cif
_cod_data_source_block           zlz
_cod_original_cell_volume        4066.5(14)
_cod_database_code               4133900
_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:
 C48(H48), C59(H59), C36(H36), C45(H45), C17(H17), C33(H33), C71(H71),
 C74(H74), C10(H10), C62(H62), C19(H19), C21(H21), C7(H7), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C23(H23A,H23B), C15(H15A,H15B), C14(H14A,H14B), C6(H6A,H6B),
 C16(H16A,H16B), C11(H11A,H11B), C5(H5A,H5B), C20(H20A,H20B), C13(H13A,H13B),
 C22(H22A,H22B), C18(H18A,H18B), C9(H9A,H9B), C12(H12A,H12B), C79(H79A,H79B),
 C78(H78A,H78B), C77(H77A,H77B), C80(H80A,H80B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C51(H51), C52(H52), C43(H43), C29(H29), C41(H41),
 C31(H31), C67(H67), C42(H42), C69(H69), C57(H57), C30(H30), C68(H68), C55(H55),
  C56(H56), C85(H85), C83(H83), C86(H86), C81(H81), C82(H82)
2.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C60(H60A,H60B,
 H60C), C64(H64A,H64B,H64C), C73(H73A,H73B,H73C), C47(H47A,H47B,H47C), C75(H75A,
 H75B,H75C), C63(H63A,H63B,H63C), C34(H34A,H34B,H34C), C61(H61A,H61B,H61C),
 C37(H37A,H37B,H37C), C76(H76A,H76B,H76C), C38(H38A,H38B,H38C), C72(H72A,H72B,
 H72C), C35(H35A,H35B,H35C), C87(H87A,H87B,H87C)
;
_olex2_submission_special_instructions 'No special instructions were received'