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_4348650
_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 Fe2 N4 P3, C5 H12'
_chemical_formula_sum            'C44 H72 Cl Fe2 N4 P3'
_chemical_formula_weight         897.11
_chemical_name_common            LFeFeCl
_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                 101.0640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8877(6)
_cell_length_b                   16.2378(8)
_cell_length_c                   23.9950(12)
_cell_measurement_reflns_used    10355
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.52
_cell_volume                     4545.7(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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52098
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         1.523
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.472
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         10365
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0514P)^2^+6.8730P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7801
_reflns_number_total             10365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01487_si_001.cif
_cod_data_source_block           12185zz_complex_1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348650
_shelxl_version_number           2013-2
_shelx_res_checksum              83893
_shelx_hkl_checksum              97884