Dinuclear Cyano-Bridged CoIII−FeIIComplexes as Precursors for Molecular Mixed-Valence Complexes of Higher Nuclearity
Bernhardt, Paul V.; Bozoglián, Fernando; González, Gabriel; Martínez, Manuel; Macpherson, Brendan P.; Sienra, Beatriz; Inorganic Chemistry 45 (2006) 74–82; doi:10.1021/ic0511423

data_4331585
_publ_section_title
;
 Dinuclear Cyano-Bridged CoIII&#x2212;FeIIComplexes as Precursors for
 Molecular Mixed-Valence Complexes of Higher Nuclearity
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              74
_journal_page_last               82
_journal_paper_doi               10.1021/ic0511423
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H89 Cl Co2 Fe N16 O20'
_chemical_formula_structural     'C36 H89 CL CO2 Fe N16 O20'
_chemical_formula_sum            'C36 H89 Cl Co2 Fe N16 O20'
_chemical_formula_weight         1275.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2005-06-07T14:03:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                71.471(8)
_cell_angle_beta                 76.752(9)
_cell_angle_gamma                85.140(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9350(10)
_cell_length_b                   17.133(2)
_cell_length_c                   17.882(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.247
_cell_measurement_theta_min      11.351
_cell_measurement_wavelength     0.71073
_cell_volume                     2809.0(6)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.62341E-1
_diffrn_orient_matrix_UB_12      0.48076E-1
_diffrn_orient_matrix_UB_13      -0.17706E-1
_diffrn_orient_matrix_UB_21      -0.03923
_diffrn_orient_matrix_UB_22      -0.3439E-2
_diffrn_orient_matrix_UB_23      0.57674E-1
_diffrn_orient_matrix_UB_31      0.72592E-1
_diffrn_orient_matrix_UB_32      0.38299E-1
_diffrn_orient_matrix_UB_33      -0.2452E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10492
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        -1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.97
_exptl_absorpt_correction_T_max  0.9152
_exptl_absorpt_correction_T_min  0.7711
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   4
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.869
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+2.5353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                6810
_reflns_number_total             9869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0511423sup1.cif
_cod_data_source_block           1948mm8
_cod_original_cell_volume        2809.0(5)
_cod_database_code               4331585
_exptl_absorpt_factor_mur        0.088
_exptl_absorpt_correction_t_ave  0.8505
_diffrn_standards_decay_corr_max 1.019
_diffrn_standards_decay_corr_min 0.91