Reactions of an Isolable Dialkylsilylene with Carbon Dioxide and Related Heterocumulenes
Liu, Xupeng; Xiao, Xu-Qiong; Xu, Zheng; Yang, Xuemin; Li, Zhifang; Dong, Zhaowen; Yan, Chenting; Lai, Guoqiao; Kira, Mitsuo; Organometallics 33 (2014) 5434–; doi:10.1021/om500736h

data_4084709
_publ_section_title
;
 Reactions of an Isolable Dialkylsilylene with Carbon Dioxide and Related
 Heterocumulenes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5434
_journal_paper_doi               10.1021/om500736h
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C29 H57 N S2 Si5'
_chemical_formula_weight         624.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                77.249(3)
_cell_angle_beta                 68.794(3)
_cell_angle_gamma                74.553(3)
_cell_formula_units_Z            2
_cell_length_a                   11.323(2)
_cell_length_b                   11.883(2)
_cell_length_c                   15.335(3)
_cell_measurement_reflns_used    3807
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.79
_cell_volume                     1836.3(6)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13849
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.894
_diffrn_reflns_theta_min         1.795
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         8576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0906P)^2^+0.2074P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6202
_reflns_number_total             8576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500736h_si_003.cif
_cod_data_source_block           siS2C
_cod_original_cell_volume        1836.2(6)
_cod_database_code               4084709
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-2
_shelx_res_checksum              55591
_shelx_hkl_checksum              40745