The Silicon Version of Phosphine Chalcogenides: Synthesis and Bonding Analysis of Stabilized Heavy Silaaldehydes.
Lutters, Dennis; Merk, Anastasia; Schmidtmann, Marc; Müller, Thomas; Inorganic chemistry 55 (2016) 9026–9032; doi:10.1021/acs.inorgchem.6b01510

data_4348675
_publ_section_title
;
 The Silicon Version of Phosphine Chalcogenides: Synthesis and Bonding
 Analysis of Stabilized Heavy Silaaldehydes.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9026
_journal_page_last               9032
_journal_paper_doi               10.1021/acs.inorgchem.6b01510
_journal_volume                  55
_journal_year                    2016
_chemical_formula_structural     'SiHS(C7H12N2)(C36H49) *0.5C14H10 *1.5C7H8'
_chemical_formula_sum            'C60.5 H79 N2 S Si'
_chemical_formula_weight         894.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.3592(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4030(8)
_cell_length_b                   17.2623(9)
_cell_length_c                   20.5674(11)
_cell_measurement_reflns_used    9215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.29
_cell_volume                     5219.6(5)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            158672
_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         27.102
_diffrn_reflns_theta_min         1.462
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         11527
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0900P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8859
_reflns_number_total             11527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01510_si_003.cif
_cod_data_source_block           dlp157
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C60.50 H79 N2 S Si'
_cod_database_code               4348675
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              41549
_shelx_hkl_checksum              74994