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_4323256
_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            'C36 H90 Cr6 P6 Se8'
_chemical_formula_weight         1652.61
_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'
_audit_creation_date             'Sat May  9 01:46:19 1998'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record             'Tue Mar 25 19:11:17'
_cell_angle_alpha                111.23(2)
_cell_angle_beta                 108.25(3)
_cell_angle_gamma                109.86(2)
_cell_formula_units_Z            2
_cell_length_a                   12.887(2)
_cell_length_b                   25.332(7)
_cell_length_c                   12.061(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    230.2
_cell_measurement_theta_max      6.8
_cell_measurement_theta_min      5.2
_cell_volume                     2994(2)
_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      230.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00883
_diffrn_orient_matrix_UB_12      -0.02167
_diffrn_orient_matrix_UB_13      0.05433
_diffrn_orient_matrix_UB_21      -0.00676
_diffrn_orient_matrix_UB_22      -0.03667
_diffrn_orient_matrix_UB_23      -0.07681
_diffrn_orient_matrix_UB_31      0.09446
_diffrn_orient_matrix_UB_32      0.02482
_diffrn_orient_matrix_UB_33      0.04078
_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  0.029
_diffrn_reflns_av_sigmaI/netI    0.083
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14356
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0.12
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.099
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624.00\
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.89
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   1.548
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9491
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0453
_refine_ls_shift/esd_max         0.0020
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00004|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0373
_reflns_number_observed          9491
_reflns_number_total             13746
_reflns_observed_criterion       >1.5sigma(I)
_cod_data_source_file            ic9807700_1.cif
_cod_data_source_block           '[Cr6Se8(PEt3)6]'
_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) +
0.00004|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) + 0.00004|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H90 Cr6 P6 Se8 '
_cod_database_code               4323256