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#$Date: 2024-03-04 22:25:31 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290214 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/50/7715068.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715068
loop_
_publ_author_name
'Sirenko, Valerii Y.'
'Kucheriv, Olesia I.'
'Shova, Sergiu'
'Shylin, Sergii I.'
'Ksenofontov, Vadim'
'Fritsky, Igor O.'
'Tremel, Wolfgang'
'Gural'skiy, Il'ya A.'
_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         'C17 H16 Ag3 Fe N9'
_chemical_formula_sum            'C17 H16 Ag3 Fe N9'
_chemical_formula_weight         725.85
_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
_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                104.052(6)
_cell_angle_beta                 101.170(6)
_cell_angle_gamma                97.383(6)
_cell_formula_units_Z            1
_cell_length_a                   7.5786(16)
_cell_length_b                   8.5161(19)
_cell_length_c                   9.630(2)
_cell_measurement_reflns_used    5298
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.941
_cell_measurement_theta_min      2.243
_cell_volume                     581.4(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8506
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.949
_diffrn_reflns_theta_min         2.242
_exptl_absorpt_coefficient_mu    3.122
_exptl_absorpt_correction_T_max  0.5620
_exptl_absorpt_correction_T_min  0.5558
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
'Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.19
_exptl_crystal_size_rad          0.14
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0415P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2511
_reflns_number_total             2778
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt04372j2.cif
_cod_data_source_block           ig_925_rt_0m
_cod_depositor_comments
'Adding full bibliography for 7715067--7715070.cif.'
_cod_original_cell_volume        581.3(2)
_cod_database_code               7715068
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.588
_shelx_estimated_absorpt_t_min   0.408
_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. Shared sites
{C3, N3}
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(N3)
4. Others
 Fixed Sof: C3(0.5) N3(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag2 Ag 0.12764(3) 0.83322(3) 0.68696(3) 0.04442(11) Uani 1 1 d . . . . .
Ag1 Ag 0.000000 0.000000 1.000000 0.04847(13) Uani 1 2 d S . P . .
Fe1 Fe 0.500000 0.500000 1.000000 0.02184(13) Uani 1 2 d S . P . .
C2 C 0.2281(4) 0.6989(4) 0.8283(3) 0.0353(6) Uani 1 1 d . . . . .
C3 C 0.0226(4) 0.9661(4) 0.5422(3) 0.0482(7) Uani 0.5 1 d . . P A 3
N2 N 0.3047(3) 0.6220(3) 0.8913(2) 0.0353(5) Uani 1 1 d . . . . .
N4 N 0.4140(3) 0.5966(3) 1.2097(2) 0.0292(4) Uani 1 1 d . . . . .
N1 N 0.2873(3) 0.2851(3) 0.9546(3) 0.0369(5) Uani 1 1 d . . . . .
C1 C 0.1819(4) 0.1824(4) 0.9642(3) 0.0389(6) Uani 1 1 d . . . . .
C5 C 0.4679(4) 0.6979(3) 1.4726(3) 0.0300(5) Uani 1 1 d . . . . .
C4 C 0.5293(3) 0.6523(3) 1.3430(3) 0.0306(5) Uani 1 1 d . . . . .
H4 H 0.654372 0.660873 1.349630 0.037 Uiso 1 1 calc R U . . .
C7 C 0.2349(4) 0.5893(4) 1.2046(3) 0.0369(6) Uani 1 1 d . . . . .
H7 H 0.150509 0.552649 1.114200 0.044 Uiso 1 1 calc R U . . .
C6 C 0.1744(4) 0.6361(4) 1.3332(3) 0.0427(7) Uani 1 1 d . . . . .
H6 H 0.049563 0.631489 1.326108 0.051 Uiso 1 1 calc R U . . .
N5 N 0.2880(3) 0.6874(3) 1.4666(3) 0.0404(6) Uani 1 1 d . . . . .
C8 C 0.5972(4) 0.7635(4) 1.6229(3) 0.0383(6) Uani 1 1 d . . . . .
H8A H 0.718428 0.742927 1.615279 0.046 Uiso 1 1 calc R U . . .
H8B H 0.556697 0.704936 1.689080 0.046 Uiso 1 1 calc R U . . .
C9 C 0.6077(5) 0.9477(4) 1.6872(4) 0.0506(8) Uani 1 1 d . . . . .
H9A H 0.654575 1.006726 1.624942 0.076 Uiso 1 1 calc R U . . .
H9B H 0.687542 0.983239 1.783855 0.076 Uiso 1 1 calc R U . . .
H9C H 0.487714 0.968921 1.693336 0.076 Uiso 1 1 calc R U . . .
N3 N 0.0226(4) 0.9661(4) 0.5422(3) 0.0482(7) Uani 0.5 1 d . . P A 4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Ag2 C3 179.12(13) . . ?
C2 Ag2 N3 179.12(13) . . ?
C1 Ag1 C1 180.0 . 2_557 ?
N2 Fe1 N2 180.00(10) . 2_667 ?
N2 Fe1 N4 91.13(9) 2_667 . ?
N2 Fe1 N4 88.87(9) . . ?
N2 Fe1 N4 88.87(9) 2_667 2_667 ?
N2 Fe1 N4 91.13(9) . 2_667 ?
N2 Fe1 N1 90.02(10) . 2_667 ?
N2 Fe1 N1 89.98(10) . . ?
N2 Fe1 N1 90.02(10) 2_667 . ?
N2 Fe1 N1 89.98(10) 2_667 2_667 ?
N4 Fe1 N4 180.0 . 2_667 ?
N1 Fe1 N4 87.19(9) 2_667 2_667 ?
N1 Fe1 N4 87.19(9) . . ?
N1 Fe1 N4 92.81(9) . 2_667 ?
N1 Fe1 N4 92.81(9) 2_667 . ?
N1 Fe1 N1 180.0 . 2_667 ?
N2 C2 Ag2 168.1(2) . . ?
C3 C3 Ag2 174.0(4) 2_576 . ?
C2 N2 Fe1 168.1(2) . . ?
C4 N4 Fe1 124.25(18) . . ?
C4 N4 C7 117.0(2) . . ?
C7 N4 Fe1 118.56(17) . . ?
C1 N1 Fe1 164.6(2) . . ?
N1 C1 Ag1 175.3(3) . . ?
C4 C5 C8 122.5(2) . . ?
N5 C5 C4 120.2(2) . . ?
N5 C5 C8 117.2(2) . . ?
N4 C4 C5 122.3(2) . . ?
N4 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
N4 C7 H7 119.7 . . ?
N4 C7 C6 120.5(3) . . ?
C6 C7 H7 119.7 . . ?
C7 C6 H6 118.6 . . ?
N5 C6 C7 122.7(3) . . ?
N5 C6 H6 118.6 . . ?
C6 N5 C5 117.1(2) . . ?
C5 C8 H8A 109.2 . . ?
C5 C8 H8B 109.2 . . ?
C5 C8 C9 112.3(2) . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag2 C2 2.078(3) . ?
Ag2 C3 2.104(3) . ?
Ag2 N3 2.104(3) . ?
Ag1 C1 2.079(3) 2_557 ?
Ag1 C1 2.079(3) . ?
Fe1 N2 2.165(2) . ?
Fe1 N2 2.166(2) 2_667 ?
Fe1 N4 2.241(2) . ?
Fe1 N4 2.241(2) 2_667 ?
Fe1 N1 2.172(2) . ?
Fe1 N1 2.172(2) 2_667 ?
C2 N2 1.135(4) . ?
C3 C3 1.132(6) 2_576 ?
N4 C4 1.341(3) . ?
N4 C7 1.342(4) . ?
N1 C1 1.141(4) . ?
C5 C4 1.400(4) . ?
C5 N5 1.343(4) . ?
C5 C8 1.511(4) . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.389(4) . ?
C6 H6 0.9300 . ?
C6 N5 1.337(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.525(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ag2 C2 N2 Fe1 32(2) . . . . ?
Fe1 N4 C4 C5 -174.2(2) . . . . ?
Fe1 N4 C7 C6 175.1(3) . . . . ?
N4 C7 C6 N5 -1.1(5) . . . . ?
C4 N4 C7 C6 -0.7(5) . . . . ?
C4 C5 N5 C6 -1.5(4) . . . . ?
C4 C5 C8 C9 107.6(3) . . . . ?
C7 N4 C4 C5 1.4(4) . . . . ?
C7 C6 N5 C5 2.2(5) . . . . ?
N5 C5 C4 N4 -0.2(4) . . . . ?
N5 C5 C8 C9 -71.1(4) . . . . ?
C8 C5 C4 N4 -178.9(3) . . . . ?
C8 C5 N5 C6 177.2(3) . . . . ?
