Synthesis of a Bent 2-Silaallene with a Perturbed Electronic Structure from a Cyclic Alkyl(amino) Carbene-Diiodosilylene.
Li, Yan; Chan, Yuk-Chi; Li, Yongxin; Purushothaman, Indu; De, Susmita; Parameswaran, Pattiyil; So, Cheuk-Wai; Inorganic chemistry 55 (2016) 9091–9098; doi:10.1021/acs.inorgchem.6b01716

data_4348846
_publ_section_title
;
 Synthesis of a Bent 2-Silaallene with a Perturbed Electronic Structure
 from a Cyclic Alkyl(amino) Carbene-Diiodosilylene.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9091
_journal_page_last               9098
_journal_paper_doi               10.1021/acs.inorgchem.6b01716
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C40 H64 I2 N2 Si2'
_chemical_formula_weight         882.91
_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                 93.9117(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9335(4)
_cell_length_b                   14.2589(3)
_cell_length_c                   18.5741(5)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    153.(2)
_cell_measurement_theta_max      25.8958
_cell_measurement_theta_min      2.4677
_cell_volume                     4210.10(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2014)'
_diffrn_ambient_temperature      153.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0765
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78316
_diffrn_reflns_theta_full        31.11
_diffrn_reflns_theta_max         31.11
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.579
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         13499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+4.2945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                9235
_reflns_number_total             13499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01716_si_001.cif
_cod_data_source_block           I
_cod_database_code               4348846
_shelx_res_checksum              89126
_shelx_hkl_checksum              10548