Bis[tris(2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>')ruthenium(II)] hexacyanoferrate(III) chloride octahydrate
Sakai, Ken; Uchida, Yuichi; Kajiwara, Takashi; Ito, Tasuku; Acta Crystallographica Section C 60 (2004) m65–m68; doi:10.1107/S0108270103028841

data_2013834
_publ_section_title
;
 Bis[tris(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')ruthenium(II)]
 hexacyanoferrate(III) chloride octahydrate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m65
_journal_page_last               m68
_journal_paper_doi               10.1107/S0108270103028841
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ru (C10 H8 N2)3]2 [Fe (C N)6] Cl, 8H2 O'
_chemical_formula_moiety         '2(Ru N6 C30 H24), Fe N6 C6, Cl, 8(H2 O)'
_chemical_formula_sum            'C66 H64 Cl Fe N18 O8 Ru2'
_chemical_formula_weight         1530.79
_chemical_name_systematic
;
Bis[tris(2,2'-bipyridine-\k^2^N,N')ruthenium(II)]
hexacyanoferrate(III) chloride octahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.4590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2498(17)
_cell_length_b                   13.6859(10)
_cell_length_c                   22.1298(16)
_cell_measurement_reflns_used    4404
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.04
_cell_volume                     6738.5(9)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'KENX (Sakai, 2002)'
_computing_publication_material
;
SHELXL97, TEXSAN, KENX and ORTEP (Johnson, 1976)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
'Bruker SMART APEX CCD-detector diffractometer'
_diffrn_measurement_method       \w
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20872
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  330
_diffrn_standards_number         58
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3124
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.358
_refine_ls_extinction_expression not_refined
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+26.0458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                4798
_reflns_number_total             7417
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1155.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2013834
_cod_database_fobs_code          2013834