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_4320798
_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 Cs3 H4 O2 Os Re5 Se8'
_chemical_formula_weight         2400.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 113.9180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7255(7)
_cell_length_b                   12.8958(9)
_cell_length_c                   11.8300(9)
_cell_measurement_temperature    161(2)
_cell_volume                     1356.29(17)
_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      161(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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6365
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    42.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            'dark wine-red'
_exptl_crystal_density_diffrn    5.878
_exptl_crystal_description       'rectangular prisms'
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.406
_refine_diff_density_min         -2.946
_refine_diff_density_rms         0.597
_refine_ls_extinction_coef       0.00013(9)
_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   1.053
_refine_ls_goodness_of_fit_obs   1.142
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      1.142
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_obs          0.0589
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1651
_refine_ls_wR_factor_obs         0.1606
_reflns_number_observed          1947
_reflns_number_total             2407
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010867d_2.cif
_cod_data_source_block           compound2
_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^)+(0.1109P)^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^)+(0.1109P)^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        1356.3(2)
_cod_original_formula_sum        'H4 Cl6 Cs3 O2 Os Re5 Se8'
_cod_database_code               4320798