Thermosalience coupled to abrupt spin crossover with dynamic ligand motion in an iron(II) molecular crystal
Hagiwara, Hiroaki; Konomura, Souta; CrystEngComm  (2022) –; doi:10.1039/D2CE00501H

data_7244930
_publ_section_title
;
 Thermosalience coupled to abrupt spin crossover with dynamic ligand
 motion in an iron(II) molecular crystal
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00501H
_journal_year                    2022
_chemical_formula_moiety         'C24 H24 Fe N10 S2'
_chemical_formula_sum            'C24 H24 Fe N10 S2'
_chemical_formula_weight         572.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-28 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.288(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1742(7)
_cell_length_b                   11.4148(5)
_cell_length_c                   20.2335(12)
_cell_measurement_reflns_used    7110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4130
_cell_measurement_theta_min      1.9750
_cell_volume                     2553.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -80.00 100.00   0.50   10.00   0.00  20.00   0.00    --   360
  2  \w    -19.50  27.50   0.50   10.00    --   20.00  90.00   0.00   94
  3  \w    -19.50  27.50   0.50   10.00    --   20.00  90.00  90.00   94
  4  \w    -19.50  27.50   0.50   10.00    --   20.00  90.00 180.00   94
  5  \w    -19.50  27.50   0.50   10.00    --   20.00  90.00 270.00   94
;
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0168180000
_diffrn_orient_matrix_UB_12      -0.0125525000
_diffrn_orient_matrix_UB_13      -0.0317114000
_diffrn_orient_matrix_UB_21      -0.0504126000
_diffrn_orient_matrix_UB_22      0.0324393000
_diffrn_orient_matrix_UB_23      -0.0156225000
_diffrn_orient_matrix_UB_31      0.0358815000
_diffrn_orient_matrix_UB_32      0.0515538000
_diffrn_orient_matrix_UB_33      0.0020403000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20932
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.861
_diffrn_reflns_theta_min         1.842
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         7210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0398P)^2^+3.4169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5167
_reflns_number_total             7210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00501h1.cif
_cod_data_source_block           1_100K
_cod_database_code               7244930
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 89.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.79
_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:
 C10(H10A,H10B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              11559
_olex2_exptl_crystal_mounting_method Fiber
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.220
_oxdiff_exptl_absorpt_empirical_full_min 0.718