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_4302869
_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         'C24 H52 Ge4 N8 Pd6 S12 , (CH4O)'
_chemical_formula_sum            'C25 H56 Ge4 N8 O Pd6 S12'
_chemical_formula_weight         1798.26
_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                 94.50
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.994
_cell_length_b                   18.081
_cell_length_c                   23.356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.09
_cell_measurement_theta_min      9.61
_cell_volume                     5049.450
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.1007
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27778
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         4.80
_exptl_absorpt_coefficient_mu    4.957
_exptl_absorpt_correction_T_max  0.6128
_exptl_absorpt_correction_T_min  0.4402
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.365
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.871
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         10381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                5977
_reflns_number_total             10381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900853e_si_002.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        5049.4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4302869