Room Temperature Hysteretic Spin Crossover in a New Cyanoheterometallic Framework
Hiiuk, Volodymyr M.; Sova, Sergiu; Rotaru, Aurelian; Ksenofontov, Vadim; Fritsky, Igor O.; Gural'skiy, Il'ya A.; Chemical Communications  (2019) –; doi:10.1039/C8CC10260K

data_7123007
_publ_section_title
;
 Room Temperature Hysteretic Spin Crossover in a New Cyanoheterometallic
 Framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10260K
_journal_year                    2019
_chemical_formula_moiety         'C20 H12 Ag2 Fe N8'
_chemical_formula_sum            'C20 H12 Ag2 Fe N8'
_chemical_formula_weight         635.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-09 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4739(8)
_cell_length_b                   13.8064(7)
_cell_length_c                   20.7510(11)
_cell_measurement_reflns_used    3115
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0600
_cell_measurement_theta_min      2.0200
_cell_volume                     4146.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_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    -73.00 -35.00   1.00   25.00    --  -23.85-178.00  60.00   38
  2  \w      7.00  88.00   1.00   25.00    --   26.35  38.00  30.00   81
  3  \w    -29.00  50.00   1.00   25.00    --   26.35 -19.00-150.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0074167000
_diffrn_orient_matrix_UB_12      -0.0239693000
_diffrn_orient_matrix_UB_13      -0.0297912000
_diffrn_orient_matrix_UB_21      0.0453184000
_diffrn_orient_matrix_UB_22      0.0194324000
_diffrn_orient_matrix_UB_23      -0.0014060000
_diffrn_orient_matrix_UB_31      0.0169978000
_diffrn_orient_matrix_UB_32      -0.0410854000
_diffrn_orient_matrix_UB_33      0.0167451000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12137
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.263
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0661
_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^)+47.1399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3011
_reflns_number_total             3661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc10260k2.cif
_cod_data_source_block           shi_3798_ilgu
_cod_database_code               7123007
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C20  H12  Ag2  Fe1  N8'
_chemical_oxdiff_usercomment     HV79_RT
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.626
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2)
Uanis(N1) = Uanis(N3)
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C5(H5), C11(H11), C12(H12), C7(H7), C9(H9), C20(H20), C8(H8),
 C17(H17), C19(H19), C15(H15), C16(H16)
;
_olex2_date_sample_data_collection 2018-07-12
_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 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.853