Push-Pull Stabilization of Parent Monochlorosilylenes.
Hickox, Hunter P.; Wang, Yuzhong; Xie, Yaoming; Wei, Pingrong; Schaefer, 3rd, Henry F; Robinson, Gregory H.; Journal of the American Chemical Society 138 (2016) 9799–9802; doi:10.1021/jacs.6b06726

data_4130787
_publ_section_title
;
 Push-Pull Stabilization of Parent Monochlorosilylenes.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9799
_journal_page_last               9802
_journal_paper_doi               10.1021/jacs.6b06726
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C71 H90 Cl2 Fe N4 O3 Si2'
_chemical_formula_weight         1230.39
_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   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 92.636(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.251(3)
_cell_length_b                   16.018(2)
_cell_length_c                   21.996(3)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.25
_cell_volume                     6775.6(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'OMEGA\PHI SCANS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74550
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.920
_diffrn_source                   'SEALED TUBE'
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         12272
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0701
_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^)+(0.1106P)^2^+7.6522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8466
_reflns_number_total             12272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06726_si_002.cif
_cod_data_source_block           j1
_cod_original_cell_volume        6775.9(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4130787
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2014/6
_shelx_res_checksum              82367
_shelx_hkl_checksum              80723