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_4320801
_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            'C56 H128 Cl6 N3 O2 Os Re5 Se8'
_chemical_formula_weight         2841.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                85.7140(10)
_cell_angle_beta                 76.9010(10)
_cell_angle_gamma                72.1220(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5328(4)
_cell_length_b                   12.5489(5)
_cell_length_c                   13.9561(5)
_cell_measurement_temperature    161(2)
_cell_volume                     2034.54(13)
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9768
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    12.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    2.319
_exptl_crystal_description       'irregular rods'
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.685
_refine_diff_density_min         -2.654
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.854
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_obs          0.0530
_refine_ls_shift/esd_max         0.246
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1383
_refine_ls_wR_factor_obs         0.1240
_reflns_number_observed          3756
_reflns_number_total             6827
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010867d_5.cif
_cod_data_source_block           compound5
_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^)+(0.0694P)^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^)+(0.0694P)^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_database_code               4320801