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_7244029
_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             2020-07-01
_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                   10.79309(13)
_cell_length_b                   10.79309(13)
_cell_length_c                   32.1264(4)
_cell_measurement_reflns_used    7393
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      74.0320
_cell_measurement_theta_min      4.0890
_cell_volume                     3241.04(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      149(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -47.00 -13.00   0.50    0.25    --  -52.43 125.00-180.00   68
  2  \w     35.00  75.00   0.50    0.25    --   68.73-125.00-180.00   80
  3  \w     38.00  65.00   0.50    0.25    --   68.73-108.00  22.00   54
  4  \w     45.00 111.00   0.50    0.25    --   69.88  15.00  60.00  132
  5  \w     78.00 103.00   0.50    0.25    --   72.00  80.00  34.57   50
  6  \w     75.00 108.00   0.50    0.25    --   75.25 155.00 -41.85   66
  7  \w     71.00  97.00   0.50    0.25    --   75.25  20.00 -56.50   52
  8  \w     92.00 117.00   0.50    0.25    --   75.25  51.00  62.15   50
  9  \w     60.00 113.00   0.50    0.25    --   75.25   8.00  31.21  106
 10  \w     83.00 117.00   0.50    0.25    --   75.25  27.00 153.33   68
 11  \w     63.00  88.00   0.50    0.25    --   75.25  20.00 -19.58   50
 12  \w     58.00  84.00   0.50    0.25    --   75.25  19.00  57.72   52
 13  \w     90.00 115.00   0.50    0.25    --   75.25  19.00  57.72   50
 14  \w     48.00  74.00   0.50    0.25    --   75.25  14.00 130.81   52
 15  \w     39.00  68.00   0.50    0.25    --   75.25-105.00-120.06   58
 16  \w     54.00  79.00   0.50    0.25    --   75.25  15.00 -42.57   50
 17  \w     66.00 116.00   0.50    0.25    --   75.25  15.00-132.61  100
 18  \w     86.00 112.00   0.50    0.25    --   75.25  14.00 130.81   52
 19  \w     35.00  60.00   0.50    0.25    --   75.25 -55.00  64.02   50
 20  \w     79.00 111.00   0.50    0.25    --   75.25   4.00 152.48   64
 21  \w     89.00 114.00   0.50    0.25    --   75.25  58.00 -24.46   50
 22  \w     46.00  89.00   0.50    0.25    --   75.25   4.00 -10.60   86
 23  \w     43.00  68.00   0.50    0.25    --   75.25 -83.00 -69.50   50
 24  \w     56.00  81.00   0.50    0.25    --   75.25-117.00 -68.00   50
 25  \w     47.00  81.00   0.50    0.25    --   75.25-101.00  95.09   68
 26  \w     49.00  92.00   0.50    0.25    --   75.25-150.00-129.90   86
;
_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      0.0510814000
_diffrn_orient_matrix_UB_12      -0.0400627000
_diffrn_orient_matrix_UB_13      -0.0399082000
_diffrn_orient_matrix_UB_21      0.1518956000
_diffrn_orient_matrix_UB_22      0.0659875000
_diffrn_orient_matrix_UB_23      0.0183181000
_diffrn_orient_matrix_UB_31      -0.0383838000
_diffrn_orient_matrix_UB_32      -0.1455980000
_diffrn_orient_matrix_UB_33      0.0192734000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            8246
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.287
_diffrn_reflns_theta_min         4.128
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.694
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.347
_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    1.456
_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         0.736
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0432P)^2^+9.1494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1474
_reflns_number_total             1479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp04321h25.cif
_cod_data_source_block           RuFe_batch1_150K
_cod_depositor_comments
'Adding full bibliography for 7244027--7244031.cif.'
_cod_original_cell_volume        3241.04(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7244029
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.479
_shelx_estimated_absorpt_t_min   0.344
_reflns_odcompleteness_completeness 99.92
_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)
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              89355
_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 2.184
_oxdiff_exptl_absorpt_empirical_full_min 0.508