Neutral Pentacoordinate Silicon Fluorides Derived from Amidinate, Guanidinate, and Triazapentadienate Ligands and Base-Induced Disproportionation of Si2Cl6 to Stable Silylenes
Rajendra S. Ghadwal; Kevin Pröpper; Birger Dittrich; Peter G. Jones; Herbert W. Roesky; Inorganic Chemistry 50 (2011) 358–364; doi:10.1021/ic1020548

data_4324169
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie
Georg-August-Universit\"at G\"ottingen 
Tammanstr. 4, 37077 G\"ottingen (Germany)
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_name        'Herbert W. Roesky'
_publ_section_title
;
 Neutral Pentacoordinate Silicon Fluorides Derived from Amidinate,
 Guanidinate, and Triazapentadienate Ligands and Base-Induced
 Disproportionation of Si2Cl6 to Stable Silylenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              358
_journal_page_last               364
_journal_paper_doi               10.1021/ic1020548
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C7 H12 Cl3 N3 Si'
_chemical_formula_sum            'C7 H12 Cl3 N3 Si'
_chemical_formula_weight         272.64
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
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_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2010-09-29T17:49:16-00:00
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 101.155(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4.0
_cell_length_a                   10.6177(3)
_cell_length_b                   8.123(2)
_cell_length_c                   13.5089(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.35
_cell_measurement_theta_min      3.335
_cell_volume                     1143.1(3)
_computing_cell_refinement       'SAINT (Bruker 2009)'
_computing_data_collection       'APEX2 (Bruker 2009)'
_computing_data_reduction        'SAINT (Bruker 2009)'
_computing_molecular_graphics    'Koritsanszky et al, (2003)'
_computing_publication_material  'Koritsanszky et al, (2003)'
_computing_structure_refinement  'Koritsanszky et al, (2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_UB_11      -0.003697
_diffrn_orient_matrix_UB_12      -0.077818
_diffrn_orient_matrix_UB_13      -0.057999
_diffrn_orient_matrix_UB_21      -0.006430
_diffrn_orient_matrix_UB_22      -0.095175
_diffrn_orient_matrix_UB_23      0.045712
_diffrn_orient_matrix_UB_31      -0.095709
_diffrn_orient_matrix_UB_32      0.009388
_diffrn_orient_matrix_UB_33      -0.015472
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24907
_diffrn_reflns_theta_full        72.30
_diffrn_reflns_theta_max         72.35
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    7.994
_exptl_absorpt_correction_T_max  0.4697
_exptl_absorpt_correction_T_min  0.1465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.1393
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
     calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0358
_reflns_number_gt                2200
_reflns_number_total             2214
_reflns_threshold_expression     F>3(\s)F
_cod_data_source_file            ic1020548_si_001.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4324169