Synthesis of an N-Heterocyclic-Carbene-Stabilized Siladiimide.
Seow, Celestine; Yim, Wai-Leung; Li, Yongxin; Ganguly, Rakesh; So, Cheuk-Wai; Inorganic chemistry 55 (2016) 4–6; doi:10.1021/acs.inorgchem.5b01818

data_4346625
_publ_section_title
;
 Synthesis of an N-Heterocyclic-Carbene-Stabilized Siladiimide.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4
_journal_page_last               6
_journal_paper_doi               10.1021/acs.inorgchem.5b01818
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C78 H106 N6 Si'
_chemical_formula_weight         1155.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 110.043(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.153(2)
_cell_length_b                   23.334(3)
_cell_length_c                   20.830(3)
_cell_measurement_reflns_used    2634
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      18.0230
_cell_measurement_theta_min      2.7169
_cell_volume                     6919.0(16)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2014)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1880
_diffrn_reflns_av_unetI/netI     0.1306
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_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            86762
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         12115
_refine_ls_number_restraints     569
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.2093
_reflns_number_gt                6465
_reflns_number_total             12115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01818_si_001.cif
_cod_data_source_block           I
_cod_original_cell_volume        6919.0(18)
_cod_database_code               4346625
_shelx_res_checksum              84186
_shelx_hkl_checksum              14048