Redox Pairs of Diiron and Iron-Cobalt Complexes with High-Spin Ground States.
Miller, Deanna L.; Siedschlag, Randall B.; Clouston, Laura J.; Young, Jr, Victor G; Chen, Yu-Sheng; Bill, Eckhard; Gagliardi, Laura; Lu, Connie C.; Inorganic chemistry 55 (2016) 9725–9735; doi:10.1021/acs.inorgchem.6b01487

data_4348656
_publ_section_title
;
 Redox Pairs of Diiron and Iron-Cobalt Complexes with High-Spin Ground
 States.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9725
_journal_page_last               9735
_journal_paper_doi               10.1021/acs.inorgchem.6b01487
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C39 H60 Cl Co1.05 Fe0.95 N4 P3, C5 H12'
_chemical_formula_sum            'C44 H72 Cl Co1.05 Fe0.95 N4 P3'
_chemical_formula_weight         900.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.6410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7539(8)
_cell_length_b                   16.2480(11)
_cell_length_c                   23.9122(15)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      2.20
_cell_volume                     4472.8(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4133
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.1023
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            104812
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        14.358
_diffrn_reflns_theta_max         23.450
_diffrn_reflns_theta_min         1.784
_diffrn_source                   '15 ID-B APS'
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.101
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         32426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.3642P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20225
_reflns_number_total             32426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01487_si_002.cif
_cod_data_source_block           30kevz_compound3_FeCoCl_anomalous_scattering
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348656
_shelxl_version_number           2013-2
_shelx_res_checksum              37262
_shelx_hkl_checksum              12341