Crystal Structure and Energy Transfer in Double-Complex Salts Composed of Tris(2,2'-bipyridine)ruthenium(II) or Tris(2,2'-bipyridine)osmium(II) and Hexacyanochromate(III)
Takuhiro Otsuka; Naoto Takahashi; Naoki Fujigasaki; Akiko Sekine; Yuji Ohashi; Youkoh Kaizu; Inorganic Chemistry 38 (1999) 1340–1347; doi:10.1021/ic9810541

data_4321838
_publ_section_title
;
 Crystal Structure and Energy Transfer in Double-Complex Salts Composed of
 Tris(2,2'-bipyridine)ruthenium(II) or Tris(2,2'-bipyridine)osmium(II) and
 Hexacyanochromate(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1340
_journal_page_last               1347
_journal_paper_doi               10.1021/ic9810541
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         '2(Os C30 H24 N6), Cr C6 N6, Cl, 8(H2 O)'
_chemical_formula_sum            'C66 H48 Cl Cr N18 O8 Os2'
_chemical_formula_weight         1689.07
_chemical_name_systematic
; 
bis[tris(2,2'-bipyridine)osmium(II)] [hexacyanochromate(III)] chloride
octahydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 90.70(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.384(4)
_cell_length_b                   13.827(4)
_cell_length_c                   22.186(3)
_cell_measurement_temperature    293(2)
_cell_volume                     6866(3)
_computing_cell_refinement
;
Rigaku(1994). SCALE. R-AXIS IICS Data Processing Software, Japan
;
_computing_data_collection
;
Rigaku(1994). OSCILL. R-AXIS IICS Data Processing Software, Japan.
;
_computing_data_reduction
;
Rigaku(1994). SCALE. R-AXIS IICS Data Processing Software, Japan
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku R-AXIS IICS'
_diffrn_radiation_detector       'Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9876
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    3.953
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3308
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         5.313
_refine_diff_density_min         -5.455
_refine_diff_density_rms         .302
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         8240
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_obs          0.0788
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2075
_refine_ls_wR_factor_obs         0.1930
_reflns_number_observed          8234
_reflns_number_total             8298
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9810541.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1534P)^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^)+( 0.1534P)^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        6866.5(23)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4321838