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_4063992
_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_sum            'C38 H62 Cl2 Ge2 N4 O2 S2'
_chemical_formula_weight         887.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.3220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8939(7)
_cell_length_b                   16.7399(14)
_cell_length_c                   14.4141(12)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.037
_cell_measurement_theta_min      2.571
_cell_volume                     2133.0(3)
_computing_cell_refinement       'SAINT V7.61A (BRUKER, 2008'
_computing_data_collection       'APEX 2.2-0 (BRUKER, 2008)'
_computing_data_reduction        'SAINT V7.61A (BRUKER, 2008'
_computing_molecular_graphics    'XP in SHELXTL Sheldrick, 2008)'
_computing_publication_material  'XP in SHELXTL Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL in SHELXTL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS in SHELXTL (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 APEXII Quasar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0065
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43618
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.669
_exptl_absorpt_correction_T_max  0.4293
_exptl_absorpt_correction_T_min  0.3808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4198
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0177
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+1.1086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0473
_reflns_number_gt                4078
_reflns_number_total             4198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101074j_si_002.cif
_cod_data_source_block           p21n
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4063992