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_4348655
_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_absolute_configuration unk
_chemical_formula_moiety         'C51 H84 Cl Fe2 Li N4 O3 P3, 0.5(C4 H8 O)'
_chemical_formula_sum            'C53 H88 Cl Fe2 Li N4 O3.5 P3'
_chemical_formula_weight         1084.27
_chemical_name_common            LFeFe(ClLi)(THF)3
_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                 91.217(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3390(16)
_cell_length_b                   22.659(2)
_cell_length_c                   17.0592(18)
_cell_measurement_reflns_used    20645
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      1.49
_cell_volume                     5927.9(10)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, 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 0.975
_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  0.1259
_diffrn_reflns_av_unetI/netI     0.2476
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44626
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_min         1.494
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.8503
_exptl_absorpt_correction_T_min  0.7871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       needle
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
Squeeze results consistent with removing one disordered THF 
molecule per asymmteric unit
;
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 2771 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1195
_refine_ls_number_reflns         20645
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.1820
_refine_ls_R_factor_gt           0.0751
_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^)+(0.0477P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1570
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                9122
_reflns_number_total             20645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01487_si_001.cif
_cod_data_source_block           12121_ljcsqz
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C106 H176 Cl2 Fe4 Li2 N8 O7 P6'
_cod_original_formula_weight         2168.55
_cod_original_formula_moiety         '2(C51 H84 Cl Fe2 Li N4 O3 P3), C4 H8 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5927.8(11)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4348655
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.937
_shelxl_version_number           2013-2
_shelx_res_checksum              24924
_shelx_hkl_checksum              33252