Synthesis and Characterization of an Amidinate-Stabilized Siladithiocarboxylate and Its Germanium(II) Complex
Zhang, Shu-Hua; Xi, Hong-Wei; Lim, Kok Hwa; So, Cheuk-Wai; Organometallics 30 (2011) 3686–; doi:10.1021/om200285u

data_4064707
_publ_section_title
;
 Synthesis and Characterization of an Amidinate-Stabilized
 Siladithiocarboxylate and Its Germanium(II) Complex
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3686
_journal_paper_doi               10.1021/om200285u
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C30 H46 Ge N4 S4 Si2'
_chemical_formula_sum            'C30 H46 Ge N4 S4 Si2'
_chemical_formula_weight         719.72
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.3290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.1519(4)
_cell_length_b                   8.74720(10)
_cell_length_c                   17.9561(3)
_cell_measurement_reflns_used    9689
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      33.36
_cell_measurement_theta_min      2.46
_cell_volume                     3557.15(10)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34833
_diffrn_reflns_theta_full        34.55
_diffrn_reflns_theta_max         34.55
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.7167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         7539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+2.2026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                5523
_reflns_number_total             7539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200285u_si_001.cif
_cod_data_source_block           scw283s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3557.15(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4064707