One synthesis: two redox states. Temperature-oriented crystallization of a charge transfer {Fe2Co2} square complex in a {FeIILSCoIIILS}2 diamagnetic or {FeIIILSCoIIHS}2 paramagnetic state.
De, Siddhartha; Jimenez, Juan Ramòn; Li, Yanling; Chamoreau, Lise-Marie; Journaux, Yves; Bousseksou, Azzedine; flambard, alexandrine; Lescouëzec, Rodrigue; RSC Adv.  (2016) –; doi:10.1039/C6RA00191B

data_7224149
_publ_section_title
;
 One synthesis: two redox states. Temperature-oriented crystallization of
 a charge transfer {Fe2Co2} square complex in a {FeIILSCoIIILS}2
 diamagnetic or {FeIIILSCoIIHS}2 paramagnetic state.
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA00191B
_journal_year                    2016
_chemical_formula_moiety
'C68 H60 B2 Co2 Fe2 N34 O4, 2(B F4), 2(C H4 O)'
_chemical_formula_sum            'C70 H68 B4 Co2 F8 Fe2 N34 O6'
_chemical_formula_weight         1906.38
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-28 deposited with the CCDC.
2016-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                115.4550(10)
_cell_angle_beta                 92.8150(10)
_cell_angle_gamma                116.9930(10)
_cell_formula_units_Z            1
_cell_length_a                   13.5576(4)
_cell_length_b                   14.0743(4)
_cell_length_c                   14.1481(4)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.06
_cell_measurement_theta_min      2.78
_cell_volume                     2069.58(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59614
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.087
_diffrn_reflns_theta_min         2.136
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         14369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+1.0555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12378
_reflns_number_total             14369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra00191b2.cif
_cod_data_source_block           sdc95_0m
_cod_original_cell_volume        2069.57(11)
_cod_database_code               7224149
_shelxl_version_number           2013-4
_shelx_res_checksum              96713