Heterometal Substitution in the Dimensional Reduction of Cluster Frameworks: Synthesis of Soluble [Re6-nOsnSe8Cl6](4-n) (n = 1-3) Cluster-Containing Solids
Eric G. Tulsky; Jeffrey R. Long; Inorganic Chemistry 40 (2001) 6990–7002; doi:10.1021/ic010867d

data_4320800
_publ_contact_author
;
       Jeffrey R. Long
       Department of Chemistry
       University of California, Berkeley
       United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 Heterometal Substitution in the Dimensional Reduction of Cluster
 Frameworks: Synthesis of Soluble [Re6-nOsnSe8Cl6](4-n) (n = 1-3)
 Cluster-Containing Solids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6990
_journal_page_last               7002
_journal_paper_doi               10.1021/ic010867d
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthetic
_chemical_formula_sum            'Cl6.5 K Os2.5 Re3.5 Se7.5'
_chemical_formula_weight         1988.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           201
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ab 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9553(3)
_cell_length_b                   12.9553(3)
_cell_length_c                   12.9553(3)
_cell_measurement_temperature    160(2)
_cell_volume                     2174.41(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8686
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    47.485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    6.076
_exptl_crystal_description       'cubic blocks'
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.017
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       0.000266(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.883
_refine_ls_goodness_of_fit_obs   0.993
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.883
_refine_ls_restrained_S_obs      0.993
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_obs          0.0224
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0332
_refine_ls_wR_factor_obs         0.0309
_reflns_number_observed          461
_reflns_number_total             661
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010867d_4.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.0105P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2174.42(9)
_cod_original_sg_symbol_H-M      'P n -3'
_cod_original_formula_sum        'Cl6.50 K Os2.50 Re3.50 Se7.50'
_cod_database_code               4320800