Synthesis of Ge2NiS4 Clusters and the Thermal Transformation to a Ge4Ni6S12 Cluster
Tsuyoshi Matsumoto; Yosuke Matsui; Mikinao Ito; Kazuyuki Tatsumi; Inorganic Chemistry 47 (2008) 1901–1903; doi:10.1021/ic702379y

data_4304800
_publ_section_title
;
Synthesis of Ge2NiS4 Clusters and the Thermal Transformation to a
Ge4Ni6S12 Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1901
_journal_page_last               1903
_journal_paper_doi               10.1021/ic702379y
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '2(C84 H80 Ge2 Ni P2 S4), 3(C7 H8)'
_chemical_formula_sum            'C189 H184 Ge4 Ni2 P4 S8'
_chemical_formula_weight         3243.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                106.910(6)
_cell_angle_beta                 107.7173(13)
_cell_angle_gamma                95.117(2)
_cell_formula_units_Z            1
_cell_length_a                   14.0364(14)
_cell_length_b                   18.010(3)
_cell_length_c                   18.085(3)
_cell_measurement_reflns_used    18881
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4086.7(11)
_computing_cell_refinement       D*TREK
_computing_data_collection       D*TREK
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 12.20
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku Quantum'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.143
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18477
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1690.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.14
_refine_diff_density_min         -0.80
_refine_ls_extinction_coef       0.0052(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     908
_refine_ls_number_reflns         18477
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0866P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2050
_reflns_number_gt                7740
_reflns_number_total             18477
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic702379y-file010_2.cif
_cod_data_source_block           '_[DmpGeS2]S2Ni(PPh3)2-1.5t'
_cod_original_cell_volume        4086.6(9)
_cod_original_formula_sum        'C189 H184 Ge4 Ni2 P4 S8 '
_cod_database_code               4304800