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_7224150
_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, 4(B F4), C H4 O, 7.5(H2 O)'
_chemical_formula_sum            'C69 H79 B4 Co2 F8 Fe2 N34 O12.5'
_chemical_formula_weight         2009.46
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-28 deposited with the CCDC.
2016-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                85.0580(10)
_cell_angle_beta                 78.2870(10)
_cell_angle_gamma                84.8430(10)
_cell_formula_units_Z            2
_cell_length_a                   15.0458(3)
_cell_length_b                   17.5052(4)
_cell_length_c                   19.0698(5)
_cell_measurement_reflns_used    6882
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.21
_cell_measurement_theta_min      2.35
_cell_volume                     4886.2(2)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72381
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.422
_diffrn_reflns_theta_min         1.863
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2058
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1283
_refine_ls_number_reflns         17946
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1048P)^2^+0.2584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10402
_reflns_number_total             17946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra00191b2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C69 H79 B4 Co2 F8 Fe2 N34 O12.50'
_cod_database_code               7224150
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              52137