Discrete RhIII/FeII and RhIII/FeII/CoIII Cyanide-Bridged Mixed Valence Compounds
Paul V. Bernhardt; Manuel Martínez; Carlos Rodríguez; Marta Vazquez; Inorganic Chemistry 50 (2011) 1429–1440; doi:10.1021/ic102061s

data_4324465
_publ_section_title
;
 Discrete RhIII/FeII and RhIII/FeII/CoIII Cyanide-Bridged Mixed Valence
 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1429
_journal_page_last               1440
_journal_paper_doi               10.1021/ic102061s
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H54 Co Fe N14 Rh S2, 2(Cl O4), 14(H2 O)'
_chemical_formula_sum            'C29 H82 Cl2 Co Fe N14 O22 Rh S2'
_chemical_formula_weight         1331.8
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.2541(15)
_cell_length_b                   9.8188(7)
_cell_length_c                   16.7885(12)
_cell_measurement_reflns_used    4845
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.8658
_cell_measurement_theta_min      2.9287
_cell_measurement_wavelength     0.71073
_cell_volume                     5646.5(6)
_computing_cell_refinement
;
 ?
;
_computing_data_collection
;
 ?
;
_computing_data_reduction
;
 ?
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0424557
_diffrn_orient_matrix_UB_12      0.0019049
_diffrn_orient_matrix_UB_13      -0.0302692
_diffrn_orient_matrix_UB_21      -0.0139961
_diffrn_orient_matrix_UB_22      -0.0574109
_diffrn_orient_matrix_UB_23      0.0806106
_diffrn_orient_matrix_UB_31      -0.0049958
_diffrn_orient_matrix_UB_32      0.1459107
_diffrn_orient_matrix_UB_33      0.0318456
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1292
_diffrn_reflns_av_unetI/netI     0.074
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37473
_diffrn_reflns_theta_full        62.48
_diffrn_reflns_theta_max         62.48
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    8.918
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       prism
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         4796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1796
_reflns_number_gt                2583
_reflns_number_total             4796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102061s_si_002.cif
_cod_data_source_block           479
_cod_database_code               4324465