Facile Access to the Hydrazone Functionalized PdGeS Cluster [{RNGe(μ-S)3}4Pd6] from the Thiogermanate Anion [{RNGe}2(μ-S)2S2]2-
Mohammad Reza Halvagar; Zohreh Hassanzadeh Fard; Lin Xiong; Stefanie Dehnen; Inorganic Chemistry 48 (2009) 7373–7377; doi:10.1021/ic900853e

data_4302868
_publ_contact_author
;
Dehnen, Stefanie

Fachbereich Chemie der Philipps-Universitaet
Hans-Meerwein-Str.
D-35043 Marburg, Germany
;
_publ_contact_author_email       dehnen@chemie.uni-marburg.de
_publ_contact_author_fax         +6421-2825653
_publ_contact_author_phone       +6421-2825751
_publ_section_title
;
Facile Access to the Hydrazone Functionalized PdGeS Cluster
[{RNGe(\m-S)3}4Pd6] from the Thiogermanate Anion [{RNGe}2(\m-S)2S2]2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7373
_journal_page_last               7377
_journal_paper_doi               10.1021/ic900853e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '(C12 H26 Ge2 N4 S4), 2(N2H5)'
_chemical_formula_sum            'C12 H36 Ge2 N8 S4'
_chemical_formula_weight         565.91
_chemical_melting_point          171
_chemical_name_systematic
; 
 ? 
;
_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                 110.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.411(5)
_cell_length_b                   8.445(3)
_cell_length_c                   29.410(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      4.62
_cell_volume                     4736(2)
_computing_cell_refinement       'Stoe X-Area'
_computing_data_collection       'Stoe X-Area'
_computing_data_reduction        'Stoe X-Area'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  IPDS2T
_diffrn_measurement_method       /w
_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  0.1269
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            14876
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         4.62
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.815
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0017(3)
_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   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0960P)^2^+3.7458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                3981
_reflns_number_total             4953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900853e_si_001.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_Hall     ' -C 2yc'
_cod_database_code               4302868