From Unsymmetrically Substituted Benzamidinato and Guanidinato Dichlorohydridosilanes to Novel Hydrido N-Heterocyclic Silylene Iron Complexes
Blom, Burgert; Pohl, Markus; Tan, Gengwen; Gallego, Daniel; Driess, Matthias; Organometallics 33 (2014) 5272–; doi:10.1021/om5005918

data_4084380
_publ_section_title
;
 From Unsymmetrically Substituted Benzamidinato and Guanidinato
 Dichlorohydridosilanes to Novel Hydrido N-Heterocyclic Silylene Iron
 Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5272
_journal_paper_doi               10.1021/om5005918
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C21 H30 Cl2 N2 Si'
_chemical_formula_weight         409.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.835(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2180(8)
_cell_length_b                   11.3381(4)
_cell_length_c                   12.6332(6)
_cell_measurement_reflns_used    3202
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.3140
_cell_measurement_theta_min      4.9100
_cell_volume                     2107.11(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7947
_diffrn_reflns_theta_full        67.47
_diffrn_reflns_theta_max         67.47
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    3.361
_exptl_absorpt_correction_T_max  0.8500
_exptl_absorpt_correction_T_min  0.4753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.0013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2446
_reflns_number_gt                2960
_reflns_number_total             3788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5005918_si_002.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 4084377--4084381.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4084380