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_4348652
_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 Fe2 N4 P3'
_chemical_formula_sum            'C39 H60 Fe2 N4 P3'
_chemical_formula_weight         789.52
_chemical_name_common            LFe2
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.8611(16)
_cell_length_b                   15.8611(16)
_cell_length_c                   11.7814(12)
_cell_measurement_reflns_used    9070
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      1.48
_cell_volume                     2566.8(4)
_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 0.999
_diffrn_measurement_device_type  'Bruker 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  0.0740
_diffrn_reflns_av_unetI/netI     0.1124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9068
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.320
_diffrn_reflns_theta_min         1.482
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_correction_T_min  0.9044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_description       plate
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
Squeeze results consistent with 6 molecules of disordered benzene in the unit cell
;
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         3451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.774
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0157P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2285
_reflns_number_total             3451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01487_si_001.cif
_cod_data_source_block           12253sqz2_compound_2
_cod_original_cell_volume        2566.8(6)
_cod_database_code               4348652
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2013-2
_shelx_res_checksum              77847
_shelx_hkl_checksum              1986