Cluster-to-Metal Magnetic Coupling: Synthesis and Characterization of 25-Electron [Re6-nOsnSe8(CN)6](5-n)- (n = 1, 2) Clusters and {Re6-nOsnSe8[CNCu(Me6tren)]6}9+ (n = 0, 1, 2) Assemblies
Eric G. Tulsky; Nathan R. M. Crawford; Stéphane A. Baudron; Patrick Batail; Jeffrey R. Long; Journal of the American Chemical Society 125 (2003) 15543–15553; doi:10.1021/ja037444q

data_4114482
_publ_section_title
;
 Cluster-to-Metal Magnetic Coupling: Synthesis and Characterization of
 25-Electron [Re6-nOsnSe8(CN)6](5-n)- (n = 1, 2) Clusters and
 {Re6-nOsnSe8[CNCu(Me6tren)]6}9+ (n = 0, 1, 2) Assemblies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15543
_journal_page_last               15553
_journal_paper_doi               10.1021/ja037444q
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C78 H60 N6 Os P3 Re5 Se8'
_chemical_formula_weight         2927.11
_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                91.5910(10)
_cell_angle_beta                 91.1040(10)
_cell_angle_gamma                104.4740(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1760(3)
_cell_length_b                   13.4661(3)
_cell_length_c                   23.1766(5)
_cell_measurement_temperature    159(2)
_cell_volume                     3978.70(15)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20354
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    12.932
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_description       block
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.551
_refine_diff_density_min         -2.141
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.000046(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   0.903
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         12819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_obs          0.0408
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0946
_refine_ls_wR_factor_obs         0.0878
_reflns_number_observed          8129
_reflns_number_total             12819
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja037444qsi20031002_112603_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0469P)^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^)+(0.0469P)^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        3978.7(2)
_cod_database_code               4114482