Electroswitching of the single-molecule magnet behaviour in an octahedral spin crossover cobalt(ii) complex with a redox-active pyridinediimine ligand.
Rabelo, Renato; Toma, Luminita; Moliner, Nicolás; Julve, Miguel; Lloret, Francesc; Pasán, Jorge; Ruiz-Pérez, Catalina; Ruiz-García, Rafael; Cano, Joan; Chemical communications (Cambridge, England) 56 (2020) 12242–12245; doi:10.1039/d0cc03357j

data_7127226
_publ_section_title
;
 Electroswitching of the single-molecule magnet behaviour in an octahedral
 spin crossover cobalt(ii) complex with a redox-active pyridinediimine
 ligand.
;
_journal_issue                   81
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12242
_journal_page_last               12245
_journal_paper_doi               10.1039/d0cc03357j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'18.8(Br3), 5.2(Br5), 8(C42 H38 Co N6 O4), 2(O)'
_chemical_formula_sum            'C336 H304 Br82.4 Co8 N48 O34'
_chemical_formula_weight         12614.28
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-10 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   24.552(5)
_cell_length_b                   24.552(5)
_cell_length_c                   17.693(4)
_cell_measurement_reflns_used    43052
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.856
_cell_measurement_theta_min      2.302
_cell_volume                     10665(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43052
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.856
_diffrn_reflns_theta_max         22.856
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.084
_exptl_absorpt_correction_T_max  0.8698
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0799 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.5286.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_description       prism
_exptl_crystal_F_000             6028
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.084
_refine_diff_density_max         2.577
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3798
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+104.7597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3616
_reflns_number_total             3798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03357j2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 7127226--7127227.cif.'
_cod_original_cell_volume        10665(5)
_cod_original_formula_sum        'C336 H304 Br82.40 Co8 N48 O34'
_cod_database_code               7127226
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(3)
 0.07(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O2-C21 = O2-C21A
 1.35 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C21A)
5. Rigid body (RIGU) restrains
 O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C21, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Fixed Sof: Br7(0.325) Br8(0.65) Br9(0.65) Br10(0.35) Br11(0.175)
7.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20)
;
_shelx_res_checksum              34873
_olex2_submission_special_instructions 'No special instructions were received'