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_4064706
_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         'C46 H78 K2 N4 O4 S4 Si2, C4 H8 O'
_chemical_formula_sum            'C50 H86 K2 N4 O5 S4 Si2'
_chemical_formula_weight         1085.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.130(3)
_cell_angle_beta                 72.379(4)
_cell_angle_gamma                74.688(3)
_cell_formula_units_Z            1
_cell_length_a                   11.1594(8)
_cell_length_b                   11.4396(8)
_cell_length_c                   12.4599(9)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.03
_cell_measurement_theta_min      2.99
_cell_volume                     1461.40(18)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30020
_diffrn_reflns_theta_full        31.15
_diffrn_reflns_theta_max         31.15
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.8917
_exptl_absorpt_correction_T_min  0.8592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         9322
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.4166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                7762
_reflns_number_total             9322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200285u_si_001.cif
_cod_data_source_block           scw256s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_database_code               4064706