Syntheses, Structures, FAB Mass Spectra, and Magnetic Properties of Chromium Chalcogenide Cluster Complexes [Cr6Se8(PEt3)6], [Cr6Se8(H)(PEt3)6], and [Cr6S8(H)(PEt3)6]
Satoshi Kamiguchi; Hideo Imoto; Taro Saito; Teiji Chihara; Inorganic Chemistry 37 (1998) 6852–6857; doi:10.1021/ic9807700

data_4323257
_publ_section_title
;
 Syntheses, Structures, FAB Mass Spectra, and Magnetic Properties of
 Chromium Chalcogenide Cluster Complexes [Cr6Se8(PEt3)6],
 [Cr6Se8(H)(PEt3)6], and [Cr6S8(H)(PEt3)6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6852
_journal_page_last               6857
_journal_paper_doi               10.1021/ic9807700
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C44 H107 Cr6 O2 P6 Se8'
_chemical_formula_weight         1797.83
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_date             'Sat May  9 01:38:29 1998'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record             'Fri Jan 23 17:09:10 1998'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.384(4)
_cell_length_b                   17.3843
_cell_length_c                   19.768(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      14.8
_cell_volume                     5173.7(16)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.04310
_diffrn_orient_matrix_UB_12      -0.05030
_diffrn_orient_matrix_UB_13      -0.02905
_diffrn_orient_matrix_UB_21      -0.03803
_diffrn_orient_matrix_UB_22      -0.02919
_diffrn_orient_matrix_UB_23      0.04050
_diffrn_orient_matrix_UB_31      -0.03334
_diffrn_orient_matrix_UB_32      0.03209
_diffrn_orient_matrix_UB_33      -0.00869
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2858
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        0.57
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.304
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_meas      ?
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2679.00
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.700
_exptl_crystal_size_min          0.700
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.73
_refine_ls_extinction_coef       0.00548(10)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   4.021
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    22
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2087
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0378
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0321
_reflns_number_observed          2087
_reflns_number_total             2651
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ic9807700_2.cif
_cod_data_source_block           '[Cr6Se8(H)(PEt3)6].2THF'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00000|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5173(2)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C44 H107 Cr6 O2 P6 Se8 '
_cod_database_code               4323257