Optical microscopy imaging of the thermally-induced spin transition and isothermal multi-stepped relaxation in a low-spin stabilized spin-crossover material.
Chakraborty, Pradip; Sy, Mouhamadou; Fourati, Houcem; Delgado, Teresa; Dutta, Mousumi; Das, Chinmoy; Besnard, Céline; Hauser, Andreas; Enachescu, Cristian; Boukheddaden, Kamel; Physical chemistry chemical physics : PCCP 24 (2022) 982–994; doi:10.1039/d1cp04321h

data_7244028
_publ_section_title
;
 Optical microscopy imaging of the thermally-induced spin transition and
 isothermal multi-stepped relaxation in a low-spin stabilized
 spin-crossover material.
;
_journal_issue                   2
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              982
_journal_page_last               994
_journal_paper_doi               10.1039/d1cp04321h
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C24 H48 Fe0.661 N24 Ru0.339, 2(B1 F4)'
_chemical_formula_sum            'C24 H48 B2 F8 Fe0.66 N24 Ru0.34'
_chemical_formula_weight         917.71
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.7344(4)
_cell_length_b                   10.7344(4)
_cell_length_c                   32.0067(16)
_cell_measurement_reflns_used    3885
_cell_measurement_temperature    80.0(6)
_cell_measurement_theta_max      27.8700
_cell_measurement_theta_min      3.7820
_cell_volume                     3193.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      80.0(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.892
_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    -18.00  90.00   1.00    5.07    --   11.70  77.00  30.00  108
  2  \w    -10.00  91.00   1.00    5.07    --   11.70  77.00 -90.00  101
  3  \w    -15.00  90.00   1.00    5.07    --   11.70  77.00 150.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0008708000
_diffrn_orient_matrix_UB_12      -0.0306884000
_diffrn_orient_matrix_UB_13      -0.0195386000
_diffrn_orient_matrix_UB_21      -0.0536073000
_diffrn_orient_matrix_UB_22      0.0143931000
_diffrn_orient_matrix_UB_23      -0.0075851000
_diffrn_orient_matrix_UB_31      0.0543070000
_diffrn_orient_matrix_UB_32      0.0684251000
_diffrn_orient_matrix_UB_33      -0.0071628000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            7566
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.063
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.53a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       prism
_exptl_crystal_F_000             1422
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0157P)^2^+6.0739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1423
_reflns_number_total             1552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp04321h25.cif
_cod_data_source_block           RuFe_batch2_80K_quenched
_cod_depositor_comments
'Adding full bibliography for 7244027--7244031.cif.'
_cod_original_cell_volume        3193.9(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7244028
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H24 B1 F4 Fe0.331 N12 Ru0.169'
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.842
_reflns_odcompleteness_completeness 97.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Shared sites
{Ru1, Fe1}
3. Uiso/Uaniso restraints and constraints
Uanis(Ru1) = Uanis(Fe1)
4. Others
 Sof(Fe1)=0.16667*(1-FVAR(2))
 Sof(Ru1)=0.16667*FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              92027
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.632
_oxdiff_exptl_absorpt_empirical_full_min 0.707