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#$Date: 2024-05-05 06:01:38 +0300 (Sun, 05 May 2024) $
#$Revision: 291639 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/56/7715637.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_7715637
loop_
_publ_author_name
'Potočňák, Ivan'
'Bukrynov, Oleksandr'
'Kliuikov, Andrii'
'Holub, Mariia'
'Vitushkina, Svitlana'
'Samoľová, Erika'
'Čižmár, Erik'
'Váhovská, Lucia'
_publ_section_title
;
 Influence of the phonon-bottleneck effect and low-energy vibrational
 modes on the slow spin-phonon relaxation in Kramers-ions-based Cu(II) and
 Co(II) complexes with 4-amino-3,5-bis-(pyridin-2-yl)-1,2,4-triazole and
 dicyanamide.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6950
_journal_page_last               6964
_journal_paper_doi               10.1039/d4dt00219a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H20 Cu N18'
_chemical_formula_sum            'C28 H20 Cu N18'
_chemical_formula_weight         672.16
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-01-15 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                91.450(3)
_cell_angle_beta                 113.458(3)
_cell_angle_gamma                96.047(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1722(3)
_cell_length_b                   9.1044(3)
_cell_length_c                   10.0931(4)
_cell_measurement_reflns_used    7114
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.2530
_cell_measurement_theta_min      4.1510
_cell_volume                     683.20(5)
_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    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT(Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.1783
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_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            9544
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       prism
_exptl_crystal_F_000             343
_exptl_crystal_recrystallization_method 'from synthesis'
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.257
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0238
_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/[σ²(Fo²)+(0.0202P)²+0.5533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2745
_reflns_number_total             2823
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00219a32.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7715637--7715638.cif.'
_cod_original_cell_volume        683.19(5)
_cod_database_code               7715637
_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_min   0.740
_shelx_estimated_absorpt_t_max   0.827
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
Cu01 Cu 0.500000 0.000000 0.500000 0.01288(8) Uani 1 2 d S . P . .
N6 N 0.26068(16) 0.08722(13) 0.44858(13) 0.0125(2) Uani 1 1 d . . . . .
N4 N 0.54775(16) 0.41650(13) 0.66148(13) 0.0121(2) Uani 1 1 d . . . . .
N2 N 0.59177(16) 0.20361(13) 0.58933(13) 0.0133(2) Uani 1 1 d . . . . .
N1 N 0.75698(16) 0.28259(14) 0.66101(13) 0.0141(3) Uani 1 1 d . . . . .
N5 N 0.83057(17) 0.65651(14) 0.82477(14) 0.0161(3) Uani 1 1 d . . . . .
N3 N 0.45580(18) 0.53031(15) 0.68701(15) 0.0165(3) Uani 1 1 d . . . . .
N7 N 0.33908(19) 0.09342(15) 0.00776(15) 0.0218(3) Uani 1 1 d . . . . .
N8 N 0.50099(19) 0.07443(16) 0.26997(15) 0.0215(3) Uani 1 1 d . . . . .
N9 N 0.37660(19) 0.30092(16) -0.13323(15) 0.0231(3) Uani 1 1 d . . . . .
C3 C 0.46654(19) 0.28416(16) 0.58899(15) 0.0122(3) Uani 1 1 d . . . . .
C14 C 0.27776(19) 0.22429(16) 0.51217(15) 0.0125(3) Uani 1 1 d . . . . .
C10 C 0.0956(2) 0.02181(17) 0.36510(16) 0.0150(3) Uani 1 1 d . . . . .
H10 H 0.082624 -0.073451 0.318800 0.018 Uiso 1 1 calc R U . . .
C11 C -0.0577(2) 0.08793(17) 0.34351(16) 0.0167(3) Uani 1 1 d . . . . .
H11 H -0.173114 0.039604 0.281625 0.020 Uiso 1 1 calc R U . . .
C8 C 0.4307(2) 0.09043(16) 0.14757(17) 0.0160(3) Uani 1 1 d . . . . .
C15 C 0.8752(2) 0.52639(16) 0.79218(15) 0.0135(3) Uani 1 1 d . . . . .
C5 C 0.72834(19) 0.41124(16) 0.70545(15) 0.0128(3) Uani 1 1 d . . . . .
C9 C 0.36558(19) 0.20719(17) -0.06123(16) 0.0157(3) Uani 1 1 d . . . . .
C13 C 0.1305(2) 0.29543(17) 0.49884(16) 0.0153(3) Uani 1 1 d . . . . .
H13 H 0.146029 0.390079 0.547109 0.018 Uiso 1 1 calc R U . . .
C16 C 1.0507(2) 0.49391(17) 0.83854(16) 0.0161(3) Uani 1 1 d . . . . .
H16 H 1.075720 0.401088 0.811049 0.019 Uiso 1 1 calc R U . . .
C12 C -0.0404(2) 0.22476(17) 0.41310(16) 0.0167(3) Uani 1 1 d . . . . .
H12 H -0.143932 0.270128 0.402553 0.020 Uiso 1 1 calc R U . . .
C19 C 0.9665(2) 0.75736(17) 0.90910(17) 0.0189(3) Uani 1 1 d . . . . .
H19 H 0.938632 0.850119 0.933801 0.023 Uiso 1 1 calc R U . . .
C18 C 1.1456(2) 0.73404(17) 0.96232(17) 0.0198(3) Uani 1 1 d . . . . .
H18 H 1.237225 0.808629 1.022759 0.024 Uiso 1 1 calc R U . . .
C17 C 1.1884(2) 0.60004(17) 0.92581(17) 0.0182(3) Uani 1 1 d . . . . .
H17 H 1.310103 0.581318 0.960037 0.022 Uiso 1 1 calc R U . . .
H1N3 H 0.429(3) 0.501(2) 0.761(2) 0.026(5) Uiso 1 1 d . . . . .
H2N3 H 0.538(3) 0.606(2) 0.722(2) 0.027(5) Uiso 1 1 d . . . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N2 Cu01 N2 180.0 . 2_656 ?
N2 Cu01 N6 100.17(5) . 2_656 ?
N2 Cu01 N6 79.83(5) 2_656 2_656 ?
N2 Cu01 N6 79.83(5) . . ?
N2 Cu01 N6 100.17(5) 2_656 . ?
N6 Cu01 N6 180.0 2_656 . ?
N2 Cu01 N8 88.78(5) . 2_656 ?
N2 Cu01 N8 91.22(5) 2_656 2_656 ?
N6 Cu01 N8 88.68(5) 2_656 2_656 ?
N6 Cu01 N8 91.32(5) . 2_656 ?
N2 Cu01 N8 91.22(5) . . ?
N2 Cu01 N8 88.78(5) 2_656 . ?
N6 Cu01 N8 91.32(5) 2_656 . ?
N6 Cu01 N8 88.68(5) . . ?
N8 Cu01 N8 180.0 2_656 . ?
C10 N6 C14 118.27(12) . . ?
C10 N6 Cu01 127.18(10) . . ?
C14 N6 Cu01 114.51(10) . . ?
C3 N4 C5 105.78(12) . . ?
C3 N4 N3 124.48(12) . . ?
C5 N4 N3 129.71(12) . . ?
C3 N2 N1 109.52(12) . . ?
C3 N2 Cu01 114.56(10) . . ?
N1 N2 Cu01 135.78(10) . . ?
C5 N1 N2 106.10(12) . . ?
C19 N5 C15 116.47(13) . . ?
N4 N3 H1N3 103.9(13) . . ?
N4 N3 H2N3 104.3(13) . . ?
H1N3 N3 H2N3 105.9(18) . . ?
C9 N7 C8 120.91(14) . . ?
C8 N8 Cu01 152.66(12) . . ?
N2 C3 N4 108.50(13) . . ?
N2 C3 C14 119.19(13) . . ?
N4 C3 C14 132.26(13) . . ?
N6 C14 C13 122.49(13) . . ?
N6 C14 C3 111.09(12) . . ?
C13 C14 C3 126.39(13) . . ?
N6 C10 C11 122.43(14) . . ?
N6 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C12 C11 C10 119.14(14) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N8 C8 N7 173.11(17) . . ?
N5 C15 C16 123.90(14) . . ?
N5 C15 C5 117.64(13) . . ?
C16 C15 C5 118.44(13) . . ?
N1 C5 N4 110.09(13) . . ?
N1 C5 C15 122.67(13) . . ?
N4 C5 C15 127.23(13) . . ?
N9 C9 N7 173.76(17) . . ?
C14 C13 C12 118.36(14) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C17 C16 C15 118.36(14) . . ?
C17 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
C11 C12 C13 119.23(14) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
N5 C19 C18 123.71(15) . . ?
N5 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
C17 C18 C19 118.79(15) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C16 C17 C18 118.77(15) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
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
Cu01 N2 1.9738(12) . ?
Cu01 N2 1.9738(12) 2_656 ?
Cu01 N6 2.0652(12) 2_656 ?
Cu01 N6 2.0652(12) . ?
Cu01 N8 2.4378(14) 2_656 ?
Cu01 N8 2.4378(14) . ?
N6 C10 1.3361(19) . ?
N6 C14 1.3566(19) . ?
N4 C3 1.3519(19) . ?
N4 C5 1.3681(19) . ?
N4 N3 1.4175(17) . ?
N2 C3 1.3194(19) . ?
N2 N1 1.3619(17) . ?
N1 C5 1.3201(19) . ?
N5 C19 1.340(2) . ?
N5 C15 1.3460(19) . ?
N3 H1N3 0.90(2) . ?
N3 H2N3 0.87(2) . ?
N7 C9 1.309(2) . ?
N7 C8 1.311(2) . ?
N8 C8 1.157(2) . ?
N9 C9 1.154(2) . ?
C3 C14 1.459(2) . ?
C14 C13 1.388(2) . ?
C10 C11 1.389(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(2) . ?
C11 H11 0.9500 . ?
C15 C16 1.388(2) . ?
C15 C5 1.469(2) . ?
C13 C12 1.390(2) . ?
C13 H13 0.9500 . ?
C16 C17 1.384(2) . ?
C16 H16 0.9500 . ?
C12 H12 0.9500 . ?
C19 C18 1.385(2) . ?
C19 H19 0.9500 . ?
C18 C17 1.384(2) . ?
C18 H18 0.9500 . ?
C17 H17 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C10 H10 N1 0.95 2.39 3.1813(19) 140.4 2_656 yes
C13 H13 N3 0.95 2.53 3.134(2) 121.4 . yes
C16 H16 N9 0.95 2.57 3.266(2) 130.6 1_656 yes
N3 H1N3 N9 0.90(2) 2.22(2) 2.986(2) 143.0(17) 1_556 yes
N3 H2N3 N5 0.87(2) 2.18(2) 2.9019(19) 139.9(18) . yes
