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_4346626
_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            'C55 H78 N4 O Si'
_chemical_formula_weight         839.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.024(4)
_cell_length_b                   18.708(4)
_cell_length_c                   14.086(3)
_cell_measurement_reflns_used    1726
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      18.7298
_cell_measurement_theta_min      2.4263
_cell_volume                     5013.2(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1634
_diffrn_reflns_av_unetI/netI     0.2283
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43439
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.304
_refine_ls_abs_structure_details
;
Flack x determined using 1423 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         9071
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0130P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                4322
_reflns_number_total             9071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01818_si_001.cif
_cod_data_source_block           I
_cod_database_code               4346626
_shelx_res_checksum              96187
_shelx_hkl_checksum              56449