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_1558652
_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 N4 Ni O), 3(B C24 F20), C4 H10 O'
_chemical_formula_sum            'C106 H74 B3 F60 N8 Ni2 O3'
_chemical_formula_weight         2797.58
_chemical_name_systematic        '[(NiMe6tren)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             2019-07-22
_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                 110.424(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.694(10)
_cell_length_b                   22.411(8)
_cell_length_c                   19.450(7)
_cell_measurement_reflns_used    2553
_cell_measurement_temperature    100
_cell_measurement_theta_max      13.969
_cell_measurement_theta_min      2.317
_cell_volume                     10904(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0905
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            91959
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        20.718
_diffrn_reflns_theta_max         20.718
_diffrn_reflns_theta_min         1.251
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1172 before and 0.0829 after correction.
The Ratio of minimum to maximum transmission is 0.7268.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5604
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-DFB/Et2O'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1712
_refine_ls_number_reflns         10441
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0399P)^2^+34.6534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8303
_reflns_number_total             10441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03078c2.cif
_cod_data_source_block           kjc181sa
_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        10905(7)
_cod_database_code               1558652
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-C27 \\sim N5-C27A
 with sigma of 0.02
 N8-C30A \\sim N8-C30 \\sim N8-C29A \\sim N8-C29 \\sim N8-C28A \\sim N8-C28
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N5, N7, N8, C24, C25, C26, C27, C28, C29, C30, 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(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)=1-FVAR(1)
 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)=FVAR(1)
 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(2)
 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(2)
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), C23(H23C,H23D),
 C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B), C24A(H24C,H24D), C27A(H27C,
 H27D), C28A(H28C,H28D), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C29A(H29D,H29E,H29F),
 C30A(H30D,H30E,H30F), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C17(H17), C18(H18)
5.d 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)
;
_shelx_res_checksum              87909
_olex2_submission_special_instructions 'No special instructions were received'