Semiquinone radical-bridged M2 (M = Fe, Co, Ni) complexes with strong magnetic exchange giving rise to slow magnetic relaxation
Chakarawet, Khetpakorn; Harris, T. David; Long, Jeffrey R.; Chemical Science  (2020) –; doi:10.1039/D0SC03078C

data_1558653
_publ_section_title
;
 Semiquinone radical-bridged M2 (M = Fe, Co, Ni) complexes with strong
 magnetic exchange giving rise to slow magnetic relaxation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03078C
_journal_year                    2020
_chemical_formula_moiety         '2(C15 H32 Co N4 O), 3(B C24 F20), C4 H10 O'
_chemical_formula_sum            'C106 H74 B3 Co2 F60 N8 O3'
_chemical_formula_weight         2798.02
_chemical_name_systematic        '[(CoMe6tren)2(C6H4O2)][B(C6F5)4]3'
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-11 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.625(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.750(10)
_cell_length_b                   22.475(8)
_cell_length_c                   19.437(7)
_cell_measurement_reflns_used    3574
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.002
_cell_measurement_theta_min      2.184
_cell_volume                     10937(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            119921
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.068
_diffrn_reflns_theta_max         23.068
_diffrn_reflns_theta_min         1.249
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0961 before and 0.0715 after correction.
The Ratio of minimum to maximum transmission is 0.8137.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5596
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-DFB/Et2O'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1804
_refine_ls_number_reflns         14215
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0617
_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^)+75.1564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11420
_reflns_number_total             14215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03078c2.cif
_cod_data_source_block           kjc185sa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        10936(7)
_cod_database_code               1558653
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Co2-N7A \\sim Co2-N7
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N5, N6, N7, N8, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5A, N6A, N7A, N8A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A,
 C28A, C29A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N5A)=Sof(N6A)=Sof(N7A)=Sof(N8A)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=
 Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=
 Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=
 Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=
 Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(N5)=Sof(N6)=Sof(N7)=Sof(N8)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,
 H13B), C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B),
 C27(H27A,H27B), C28(H28A,H28B), C19A(H19C,H19D), C20A(H20C,H20D), C23A(H23C,
 H23D), C24A(H24C,H24D), C27A(H27C,H27D), C28A(H28C,H28D), C2S(H2SA,H2SB),
 C3S(H3SA,H3SB)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C1S(H1SA,
 H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              69282
_olex2_submission_special_instructions 'No special instructions were received'