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_1558650
_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
'C30 H64 N8 Ni2 O2, 2(B C24 F20), 2(C4 H8 O), C4 H10 O'
_chemical_formula_sum            'C90 H90 B2 F40 N8 Ni2 O5'
_chemical_formula_weight         2262.73
_chemical_name_systematic        '[(NiMe6tren)2(C6H4O2)][B(C6F5)4]2'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-18
_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                97.774(3)
_cell_angle_beta                 90.679(3)
_cell_angle_gamma                101.898(2)
_cell_formula_units_Z            1
_cell_length_a                   12.015(2)
_cell_length_b                   12.540(2)
_cell_length_c                   16.083(3)
_cell_measurement_reflns_used    2066
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.011
_cell_measurement_theta_min      2.720
_cell_volume                     2347.4(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 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  0.0514
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         34.098
_diffrn_reflns_theta_min         1.719
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.9035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1552 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.9353. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Et2O'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         17900
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.5168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15061
_reflns_number_total             17900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03078c2.cif
_cod_data_source_block           kjc182s
_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        2347.5(7)
_cod_database_code               1558650
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.929
_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
 O1S-C2S = O1S-C3S
 1.34 with sigma of 0.02
 C2S-C1S = C4S-C3S
 1.54 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O1S, C1S, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H3TC)=Sof(H3TD)=Sof(C5T)=Sof(H5TA)=Sof(H5TB)=1-FVAR(1)
 Sof(H3TA)=Sof(H3TB)=Sof(C4T)=Sof(H4TA)=Sof(H4TB)=FVAR(1)
 Fixed Sof: O1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
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), C1T(H1TA,H1TB), C2T(H2TA,H2TB), C3T(H3TC,H3TD), C3T(H3TA,H3TB),
 C4T(H4TA,H4TB), C5T(H5TA,H5TB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
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)
;
_shelx_res_checksum              94304
_olex2_submission_special_instructions 'No special instructions were received'