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_7244031
_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 Ru, 2(B F4)'
_chemical_formula_sum            'C24 H48 B2 F8 N24 Ru'
_chemical_formula_weight         947.55
_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
_audit_creation_date             2020-07-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.9202(14)
_cell_angle_beta                 99.0617(17)
_cell_angle_gamma                89.4706(17)
_cell_formula_units_Z            2
_cell_length_a                   11.7827(3)
_cell_length_b                   10.88012(19)
_cell_length_c                   16.3802(3)
_cell_measurement_reflns_used    26080
_cell_measurement_temperature    80.0(5)
_cell_measurement_theta_max      74.2570
_cell_measurement_theta_min      4.0020
_cell_volume                     2073.37(8)
_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(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.974
_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    -88.00 -36.00   0.50    0.25    --  -52.43 -15.00 120.00  104
  2  \w    -79.00 -32.00   0.50    0.25    --  -52.43 -15.00   0.00   94
  3  \w   -102.00 -77.00   0.50    0.25    --  -60.50 -45.00-102.55   50
  4  \w     43.00  74.00   0.50    0.25    --   68.73-125.00 120.00   62
  5  \w     43.00  69.00   0.50    0.25    --   68.73-125.00  60.00   52
  6  \w     35.00  67.00   0.50    0.25    --   68.73-125.00   0.00   64
  7  \w     47.00  97.00   0.50    0.25    --   68.73  15.00  60.00  100
  8  \w     35.00  64.00   0.50    0.25    --   68.73-125.00-150.00   58
  9  \w     40.00  83.00   0.50    0.25    --   68.73  15.00-150.00   86
 10  \w     38.00  95.00   0.50    0.25    --   69.88-125.00 -90.00  114
 11  \w     40.00  95.00   0.50    0.25    --   69.88-125.00-180.00  110
 12  \w     39.00 103.00   0.50    0.25    --   69.88   0.00   0.00  128
 13  \w     56.00  99.00   0.50    0.25    --   69.88   0.00 120.00   86
 14  \w     70.00  95.00   0.50    0.25    --   69.88-125.00 -30.00   50
 15  \w     70.00  95.00   0.50    0.25    --   69.88-125.00  90.00   50
 16  \w     50.00  94.00   0.50    0.25    --   72.00-118.00-154.36   88
 17  \w     39.00  70.00   0.50    0.25    --   75.25-128.00-162.77   62
 18  \w     50.00 101.00   0.50    0.25    --   75.25-126.00  34.88  102
 19  \w     59.00 106.00   0.50    0.25    --   75.25-135.00  76.98   94
 20  \w     70.00  95.00   0.50    0.25    --   75.25-114.00   5.38   50
 21  \w     41.00  67.00   0.50    0.25    --   75.25-123.00  80.61   52
 22  \w     36.00  63.00   0.50    0.25    --   75.25-114.00   5.38   54
 23  \w     66.00  96.00   0.50    0.25    --   75.25-115.00 -16.72   60
 24  \w     74.00  99.00   0.50    0.25    --   75.25-123.00  80.61   50
 25  \w     41.00  93.00   0.50    0.25    --   75.25-113.00-123.42  104
 26  \w     48.00  84.00   0.50    0.25    --   75.25-113.00 165.58   72
 27  \w     45.00  71.00   0.50    0.25    --   75.25 -86.00 109.06   52
 28  \w     48.00  73.00   0.50    0.25    --   75.25 -83.00  -2.30   50
 29  \w     58.00  97.00   0.50    0.25    --   75.25-127.00-158.31   78
 30  \w     79.00 110.00   0.50    0.25    --   75.25  20.00  76.28   62
 31  \w     45.00  71.00   0.50    0.25    --   75.25-120.00  86.84   52
 32  \w     91.00 116.00   0.50    0.25    --   75.25  51.00  80.15   50
 33  \w     36.00  61.00   0.50    0.25    --   75.25 -57.00  -1.27   50
 34  \w     47.00 100.00   0.50    0.25    --   75.25-124.00-143.79  106
 35  \w     40.00  92.00   0.50    0.25    --   75.25-111.00 -52.49  104
 36  \w     38.00  67.00   0.50    0.25    --   75.25-113.00-104.96   58
 37  \w     55.00  99.00   0.50    0.25    --   75.25-122.00 160.89   88
 38  \w     55.00 101.00   0.50    0.25    --   75.25-126.00 170.59   92
 39  \w     72.00  97.00   0.50    0.25    --   75.25-117.00 -70.48   50
 40  \w     88.00 114.00   0.50    0.25    --   75.25  12.00-140.01   52
 41  \w     43.00  68.00   0.50    0.25    --   75.25 -87.00 -15.67   50
 42  \w     37.00 100.00   0.50    0.25    --   75.25-124.00 -86.93  126
 43  \w     44.00  69.00   0.50    0.25    --   75.25 -80.00  14.91   50
 44  \w     44.00  78.00   0.50    0.25    --   75.25   6.00 155.72   68
 45  \w     83.00 111.00   0.50    0.25    --   75.25   6.00 155.72   56
 46  \w     87.00 112.00   0.50    0.25    --   75.25  64.00-177.83   50
 47  \w     42.00  67.00   0.50    0.25    --   75.25 -89.00  36.34   50
 48  \w     56.00  83.00   0.50    0.25    --   75.25 -98.00  80.23   54
 49  \w     36.00  96.00   0.50    0.25    --   75.25-115.00-139.50  120
 50  \w     43.00  74.00   0.50    0.25    --   75.25   3.00 -52.98   62
 51  \w     86.00 112.00   0.50    0.25    --   75.25   3.00 -52.98   52
 52  \w     36.00  71.00   0.50    0.25    --   75.25-113.00-131.72   70
 53  \w     36.00  61.00   0.50    0.25    --   75.25 -55.00-171.02   50
 54  \w     58.00  83.00   0.50    0.25    --   75.25  19.00 165.79   50
 55  \w     49.00  75.00   0.50    0.25    --   75.25   2.00  70.89   52
 56  \w     84.00 111.00   0.50    0.25    --   75.25   2.00  70.89   54
 57  \w     90.00 115.00   0.50    0.25    --   75.25  47.00 -57.23   50
 58  \w     61.00 102.00   0.50    0.25    --   75.25-128.00 -14.04   82
 59  \w     57.00 115.00   0.50    0.25    --   75.25  17.00 -34.34  116
 60  \w     82.00 108.00   0.50    0.25    --   75.25   9.00-172.36   52
 61  \w     56.00 112.00   0.50    0.25    --   75.25  18.00  44.40  112
 62  \w     59.00  85.00   0.50    0.25    --   75.25-115.00 -71.51   52
 63  \w     81.00 106.00   0.50    0.25    --   75.25  79.00 -67.22   50
 64  \w     56.00  81.00   0.50    0.25    --   75.25   9.00-172.36   50
 65  \w     56.00  97.00   0.50    0.25    --   75.25  17.00-162.44   82
 66  \w     91.00 116.00   0.50    0.25    --   75.25  34.00 -82.49   50
 67  \w     74.00 102.00   0.50    0.25    --   75.25-128.00-162.77   56
 68  \w     52.00  97.00   0.50    0.25    --   75.25-118.00 135.29   90
 69  \w     70.00 110.00   0.50    0.25    --   75.25   6.00 -14.64   80
 70  \w     65.00  90.00   0.50    0.25    --   75.25  22.00   6.02   50
 71  \w     73.00  98.00   0.50    0.25    --   75.25-120.00  86.84   50
 72  \w     71.00  96.00   0.50    0.25    --   75.25-116.00-148.60   50
 73  \w     55.00  81.00   0.50    0.25    --   75.25-116.00   0.30   52
 74  \w     54.00 109.00   0.50    0.25    --   75.25  11.00  24.12  110
 75  \w     67.00  92.00   0.50    0.25    --   75.25-112.00 -64.68   50
;
_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      0.1315294396
_diffrn_orient_matrix_UB_12      0.0009723612
_diffrn_orient_matrix_UB_13      0.0042018326
_diffrn_orient_matrix_UB_21      0.0082923209
_diffrn_orient_matrix_UB_22      0.1086090258
_diffrn_orient_matrix_UB_23      0.0621149503
_diffrn_orient_matrix_UB_31      0.0127203687
_diffrn_orient_matrix_UB_32      -0.0908744037
_diffrn_orient_matrix_UB_33      0.0720866113
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47423
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.193
_diffrn_reflns_theta_min         2.732
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.850
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.183
_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            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.162
_refine_diff_density_max         2.949
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         8226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0714
_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^)+(0.1616P)^2^+2.6108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6879
_reflns_number_total             8226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp04321h25.cif
_cod_data_source_block           RuFe_batch1_80K_tric
_cod_depositor_comments
'Adding full bibliography for 7244027--7244031.cif.'
_cod_original_cell_volume        2073.38(7)
_cod_database_code               7244031
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru1 C24 N24 H48 B2 F8'
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,
 H11B), C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B),
 C22(H22A,H22B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C9(H9), C13(H13), C17(H17), C21(H21)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              37744
_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 2.278
_oxdiff_exptl_absorpt_empirical_full_min 0.552