Synthesis and Structure of [{PhC(NtBu)2}2Ge2(μ-S)2Cl2] and a Germanium Dithiocarboxylate Analogue
Sen, Sakya S.; Ghadwal, Rajendra S.; Kratzert, Daniel; Stern, Daniel; Roesky, Herbert W.; Stalke, Dietmar; Organometallics 30 (2011) 1030–; doi:10.1021/om101074j

data_4063993
_publ_section_title
;
 Synthesis and Structure of [{PhC(NtBu)2}2Ge2(\m-S)2Cl2] and a Germanium
 Dithiocarboxylate Analogue
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1030
_journal_paper_doi               10.1021/om101074j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C30 H46 GE2 K2 N4 S4, C8 H16 O2'
_chemical_formula_sum            'C38 H62 Ge2 K2 N4 O2 S4'
_chemical_formula_weight         958.54
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.3330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.3432(12)
_cell_length_b                   8.8382(6)
_cell_length_c                   16.5578(12)
_cell_measurement_reflns_used    7554
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.8525
_cell_measurement_theta_min      2.4665
_cell_volume                     2312.6(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2008.11'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC mirror optics'
_diffrn_radiation_source         'INCOATEC Mo Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58293
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  0.7850
_exptl_absorpt_correction_T_min  0.7850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5315
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+1.9175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                4436
_reflns_number_total             5315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101074j_si_003.cif
_cod_data_source_block           p21c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4063993