Nature of cyanoargentate bridges defining spin crossover in new 2D Hofmann clathrate analogues.
Sirenko, Valerii Y.; Kucheriv, Olesia I.; Shova, Sergiu; Shylin, Sergii I.; Ksenofontov, Vadim; Fritsky, Igor O.; Tremel, Wolfgang; Gural'skiy, Il'ya A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4251–4259; doi:10.1039/d3dt04372j

data_7715069
_publ_section_title
;
 Nature of cyanoargentate bridges defining spin crossover in new 2D
 Hofmann clathrate analogues.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4251
_journal_page_last               4259
_journal_paper_doi               10.1039/d3dt04372j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H16 Ag2 Fe N8'
_chemical_formula_sum            'C16 H16 Ag2 Fe N8'
_chemical_formula_weight         591.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2024-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.440(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4042(7)
_cell_length_b                   10.5890(5)
_cell_length_c                   17.3831(16)
_cell_measurement_reflns_used    2108
_cell_measurement_temperature    304(5)
_cell_measurement_theta_max      28.6760
_cell_measurement_theta_min      2.0140
_cell_volume                     2281.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      304.15
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     11.00  95.00   1.00    6.00    --   26.35  38.00 -60.00   84
  2  \w     -1.00  26.00   1.00    6.00    --   26.35  19.00 120.00   27
  3  \w    -43.00  44.00   1.00    6.00    --   26.35 -38.00 120.00   87
  4  \w     42.00  80.00   1.00    6.00    --   26.35-126.00 -36.00   38
  5  \w    -32.00  -7.00   1.00    6.00    --  -24.01 -57.00 -60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9189
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.978
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4036
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+6.4624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2909
_reflns_number_total             4036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04372j2.cif
_cod_data_source_block           shi_3710_ilgu
_cod_depositor_comments
'Adding full bibliography for 7715067--7715070.cif.'
_cod_database_code               7715069
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.419
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C16
 2.5 with sigma of 0.01
 C9-C10B
 1.54 with sigma of 0.02
 C9-C10A
 1.54 with sigma of 0.02
 C16-C15
 1.54 with sigma of 0.02
 C9-C6 \\sim C12-C15
 with sigma of 0.01
3. Restrained planarity
 N5, C8, N6, C7, C5, C6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C16)
Uanis(C10B) = Uanis(C10A)
5. Others
 Fixed Sof: H9BC(0.37) H9BD(0.37) H9AA(0.63) H9AB(0.63) C10B(0.37) H10A(0.37)
 H10B(0.37) H10C(0.37) C10A(0.63) H10D(0.63) H10E(0.63) H10F(0.63)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C9(H9BC,H9BD), C9(H9AA,H9AB)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C7(H7), C14(H14), C13(H13), C5(H5)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C10B(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              78259
_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
;