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_4304801
_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         'C97 H100 Cl2 Ge4 Ni6 S12 '
_chemical_formula_sum            'C97 H100 Cl2 Ge4 Ni6 S12'
_chemical_formula_weight         2364.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.493(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   22.913(7)
_cell_length_b                   16.604(4)
_cell_length_c                   27.451(11)
_cell_measurement_reflns_used    3130
_cell_measurement_temperature    193.1
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      3.1
_cell_volume                     10234(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_detector_area_resol_mean 12.20
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Quantum'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.123
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            96655
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4816.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.31
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         23294
_refine_ls_R_factor_gt           0.1156
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3044
_reflns_number_gt                12129
_reflns_number_total             23294
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic702379y-file010_3.cif
_cod_data_source_block           '_(DmpGeS3)4Ni6'
_cod_original_formula_sum        'C97 H100 Cl2 Ge4 Ni6 S12 '
_cod_database_code               4304801