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_4348654
_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 Co Fe N4 P3, C4 H8 O'
_chemical_formula_sum            'C43 H68 Co Fe N4 O P3'
_chemical_formula_weight         864.70
_chemical_name_common            LFeCo
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.343(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.837(2)
_cell_length_b                   15.715(3)
_cell_length_c                   11.986(2)
_cell_measurement_reflns_used    2925
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.3825
_cell_measurement_theta_min      2.164
_cell_volume                     2186.1(7)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18111
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.164
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABs, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.807
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9688
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0918P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                7996
_reflns_number_total             9688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01487_si_001.cif
_cod_data_source_block           12184zz_Compound_4
_cod_original_cell_volume        2186.2(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4348654
_shelxl_version_number           2013-2
_shelx_res_checksum              30023
_shelx_hkl_checksum              25337