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_4133899
_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         'C71 H101 B3 Li N7 O Si'
_chemical_formula_sum            'C71 H101 B3 Li N7 O Si'
_chemical_formula_weight         1136.04
_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   mixed
_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                90
_cell_angle_beta                 96.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.249(3)
_cell_length_b                   22.895(5)
_cell_length_c                   23.084(5)
_cell_measurement_reflns_used    14620
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9304
_cell_measurement_theta_min      1.7790
_cell_volume                     6951(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113.1500
_diffrn_measured_fraction_theta_full 0.999
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83624
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.902
_diffrn_reflns_theta_min         1.690
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.951
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         16591
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0904P)^2^+4.8328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13219
_reflns_number_total             16591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11913_si_003.cif
_cod_data_source_block           zlz0001
_cod_original_cell_volume        6952(2)
_cod_database_code               4133899
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.992
_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. Rigid bond restraints
 C68, C69
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C69, C70
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C68, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 C24(H24), C36(H36), C27(H27), C39(H39), C53(H53), C50(H50), C62(H62), C8(H8),
 C11(H11), C65(H65)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C69(H69A,H69B), C71(H71A,H71B), C70(H70A,
 H70B), C68(H68A,H68B)
4.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C43(H43), C42(H42), C20(H20), C22(H22), C46(H46),
 C34(H34), C21(H21), C58(H58), C4(H4), C60(H60), C32(H32), C33(H33), C48(H48),
 C6(H6), C47(H47), C5(H5), C59(H59)
4.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C41(H41A,H41B,
 H41C), C40(H40A,H40B,H40C), C37(H37A,H37B,H37C), C10(H10A,H10B,H10C), C63(H63A,
 H63B,H63C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C54(H54A,H54B,H54C),
 C64(H64A,H64B,H64C), C52(H52A,H52B,H52C), C55(H55A,H55B,H55C), C67(H67A,H67B,
 H67C), C66(H66A,H66B,H66C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C)
;
_shelx_res_checksum              26872
_shelx_hkl_checksum              7968
_olex2_submission_special_instructions 'No special instructions were received'