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_7244030
_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 N24 Ru1, 2(B1 F4)'
_chemical_formula_sum            'C24 H48 B2 F8 N24 Ru'
_chemical_formula_weight         947.55
_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             2020-06-26
_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                   10.77425(13)
_cell_length_b                   10.77425(13)
_cell_length_c                   31.8415(5)
_cell_measurement_reflns_used    10564
_cell_measurement_temperature    81(2)
_cell_measurement_theta_max      74.0700
_cell_measurement_theta_min      4.1530
_cell_volume                     3201.09(7)
_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      81(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -44.00 -18.00   0.50    0.13    --  -52.43 125.00-180.00   52
  2  \w     37.00  93.00   0.50    0.13    --   68.73-125.00 120.00  112
  3  \w     37.00  67.00   0.50    0.13    --   68.73-125.00-180.00   60
  4  \w     37.00  99.00   0.50    0.13    --   69.88   0.00   0.00  124
  5  \w     49.00  77.00   0.50    0.13    --   75.25-121.00 119.37   56
  6  \w     89.00 114.00   0.50    0.13    --   75.25  53.00  63.52   50
  7  \w     56.00 101.00   0.50    0.13    --   75.25   1.00 -76.41   90
  8  \w     63.00  89.00   0.50    0.13    --   75.25  21.00 108.03   52
  9  \w     45.00  74.00   0.50    0.13    --   75.25-107.00-178.71   58
 10  \w     81.00 118.00   0.50    0.13    --   75.25  19.00 -92.53   74
 11  \w     49.00  76.00   0.50    0.13    --   75.25   6.00 157.58   54
 12  \w     46.00  81.00   0.50    0.13    --   75.25  12.00 104.34   70
 13  \w     67.00  93.00   0.50    0.13    --   75.25 172.00-101.20   52
 14  \w     43.00  87.00   0.50    0.13    --   75.25-111.00-104.07   88
 15  \w     56.00  81.00   0.50    0.13    --   75.25   8.00  -4.75   50
 16  \w     63.00  88.00   0.50    0.13    --   75.25-107.00 -15.59   50
 17  \w     66.00  96.00   0.50    0.13    --   75.25  21.00  54.03   60
 18  \w     89.00 114.00   0.50    0.13    --   75.25  11.00-165.37   50
 19  \w     63.00  98.00   0.50    0.13    --   75.25  21.00 155.88   70
 20  \w     47.00  72.00   0.50    0.13    --   75.25 -89.00  35.65   50
 21  \w     52.00 111.00   0.50    0.13    --   75.25  13.00  14.48  118
 22  \w     48.00  73.00   0.50    0.13    --   75.25  12.00 141.20   50
 23  \w     72.00 100.00   0.50    0.13    --   75.25-143.00 -89.43   56
 24  \w     86.00 112.00   0.50    0.13    --   75.25   6.00 157.58   52
 25  \w     52.00 105.00   0.50    0.13    --   75.25-153.00 130.77  106
 26  \w     32.00  57.00   0.50    0.13    --   24.00  74.00 173.51   50
 27  \w    -41.00 -13.00   0.50    0.13    --  -52.43 125.00  60.00   56
 28  \w    -66.00 -23.00   0.50    0.13    --  -52.43   0.00  90.00   86
 29  \w    -77.00 -41.00   0.50    0.13    --  -52.43 125.00 -30.00   72
 30  \w    -49.00 -24.00   0.50    0.13    --  -52.43 -15.00-120.00   50
 31  \w    -85.00 -54.00   0.50    0.13    --  -52.43 -15.00-120.00   62
 32  \w     40.00  66.00   0.50    0.13    --   68.73-125.00 -90.00   52
 33  \w     36.00  62.00   0.50    0.13    --   69.88-125.00-150.00   52
 34  \w     63.00  95.00   0.50    0.13    --   69.88-125.00-150.00   64
 35  \w     39.00  68.00   0.50    0.13    --   69.88   0.00-120.00   58
 36  \w     62.00  95.00   0.50    0.13    --   69.88-125.00 -90.00   66
 37  \w     34.00  65.00   0.50    0.13    --   69.88-125.00-120.00   62
 38  \w     45.00  95.00   0.50    0.13    --   69.88-125.00   0.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0417837000
_diffrn_orient_matrix_UB_12      0.0471348000
_diffrn_orient_matrix_UB_13      0.0407492000
_diffrn_orient_matrix_UB_21      0.0652001000
_diffrn_orient_matrix_UB_22      0.1535220000
_diffrn_orient_matrix_UB_23      -0.0173657000
_diffrn_orient_matrix_UB_31      -0.1457994000
_diffrn_orient_matrix_UB_32      -0.0382999000
_diffrn_orient_matrix_UB_33      -0.0194487000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            12059
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.166
_diffrn_reflns_theta_min         4.165
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.740
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.407
_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            'pale brown'
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0190P)^2^+10.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1459
_reflns_number_total             1460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp04321h25.cif
_cod_data_source_block           RuFe_batch1_80K_quenched
_cod_depositor_comments
'Adding full bibliography for 7244027--7244031.cif.'
_cod_original_cell_volume        3201.09(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7244030
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru1 N24 F8 B2 C24 H48'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              6267
_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 1.919
_oxdiff_exptl_absorpt_empirical_full_min 0.595