Correlations between ligand field ΔO, spin crossover T1/2 and redox potential Epa in a family of five dinuclear helicates
Singh, Sandhya; Brooker, Sally; Chemical Science  (2021) –; doi:10.1039/D1SC01458G

data_1563755
_publ_section_title
;
 Correlations between ligand field \DO, spin crossover T1/2 and redox
 potential Epa in a family of five dinuclear helicates
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01458G
_journal_year                    2021
_chemical_formula_moiety         'C72 H74 Fe2 N24 S6, 4(B F4)'
_chemical_formula_sum            'C72 H74 B4 F16 Fe2 N24 S6'
_chemical_formula_weight         1926.85
_chemical_name_common
'diiron(II) helicate of ditopic thiazole-triazole ligand'
_chemical_name_systematic
'Iron(II) helicate of 1,3-Bis(4-isobutyl-5-(thiazol-4-yl)-4H-1,2,4-triazol-3-yl)benzene'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-02-05 deposited with the CCDC.	2021-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.743(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1754(4)
_cell_length_b                   25.7678(7)
_cell_length_c                   29.1091(9)
_cell_measurement_reflns_used    11298
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1740
_cell_measurement_theta_min      3.9070
_cell_volume                     9848.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.3449
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -125.00 -94.00   1.00   10.00    --  -42.04 -88.00 -65.00   31
  2  \w      7.00 122.00   1.00   10.00    --   42.04  19.00-180.00  115
  3  \w     23.00  69.00   1.00   10.00    --   42.04-125.00  30.00   46
  4  \w     62.00  98.00   1.00   10.00    --   42.04  38.00-120.00   36
  5  \w     53.00 109.00   1.00   30.00    --  112.00-125.00  60.00   56
  6  \w    101.00 136.00   1.00   30.00    --  112.00 -77.00  30.00   35
  7  \w     37.00 110.00   1.00   30.00    --  112.00 -95.00  90.00   73
  8  \w     95.00 176.00   1.00   30.00    --  112.00 125.00  90.00   81
  9  \w    109.00 154.00   1.00   30.00    --  112.00 125.00  60.00   45
 10  \w     35.00  86.00   1.00   30.00    --  112.00 -95.00  60.00   51
 11  \w     87.00 176.00   1.00   30.00    --  112.00  45.00-180.00   89
 12  \w    102.00 153.00   1.00   30.00    --  112.00 125.00 120.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20758
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.597
_diffrn_reflns_theta_min         3.754
_exptl_absorpt_coefficient_mu    4.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             3944
_exptl_crystal_preparation
'Magnetic properties,redox, ligand field strength, UV-Visible spectra, Evans method NMR, DOSY NMR'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN by diethylether ether vapour diffusion'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.241
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0914
_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^)+(0.1750P)^2^+26.8188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2552
_refine_ls_wR_factor_ref         0.2612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9167
_reflns_number_total             10075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01458g2.cif
_cod_data_source_block           ss376
_cod_database_code               1563755
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.701
_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. Others
 Fixed Sof: F22(0.6) F23(0.6) F24(0.6) F25(0.4) F26(0.4) F27(0.4)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C18(H18), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C29(H29A,H29B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C11(H11), C12(H12), C13(H13), C15(H15), C23(H23), C24(H24),
 C25(H25), C26(H26), C35(H35), C36(H36), C37(H37)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              70965
_shelx_hkl_checksum              8580
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_platon_squeeze_void_probe_radius 1.20