#------------------------------------------------------------------------------
#$Date: 2025-07-06 19:39:12 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 301072 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/37/7063757.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_7063757
loop_
_publ_author_name
'Tolstikov, Svyatoslav E.'
'Kolesnikov, Andrey E.'
'Smirnova, Kristina A.'
'Letyagin, Gleb A.'
'Bogomyakov, Artem S.'
'Romanenko, Galina V.'
'Ovcharenko, Victor I.'
_publ_section_title
;
 Heterospin molecular complexes of Cu(hfac)2 with pyridyl-substituted
 nitronyl nitroxides: peculiarities of structure and magnetic properties
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7655
_journal_page_last               7660
_journal_paper_doi               10.1039/D5NJ00967G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_sum            'C44 H34 Cl2 Cu2 F24 N6 O12'
_chemical_formula_weight         1492.75
_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_block_doi                 10.5517/ccdc.csd.cc2bjct2
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-22 deposited with the CCDC.	2025-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                94.536(2)
_cell_angle_beta                 105.712(2)
_cell_angle_gamma                113.2450(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8746(3)
_cell_length_b                   11.1848(3)
_cell_length_c                   15.1435(4)
_cell_measurement_reflns_used    7567
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.06
_cell_measurement_theta_min      2.34
_cell_volume                     1446.28(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24794
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.385
_diffrn_reflns_theta_min         2.027
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.5789
_exptl_absorpt_correction_T_min  0.4690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0410
_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)+(0.0563P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4434
_reflns_number_total             7094
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5nj00967g2.cif
_cod_data_source_block           1094s
_cod_depositor_comments
'Adding full bibliography for 7063753--7063771.cif.'
_cod_database_code               7063757
_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. 
;
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
Cu Cu 0.46471(3) 1.02302(3) 0.26099(2) 0.04194(11) Uani 1 1 d . . . . .
O1 O 0.2865(2) 0.88570(16) 0.15549(11) 0.0500(4) Uani 1 1 d . . . . .
C1 C 0.0372(4) 0.7138(4) 0.0726(3) 0.0767(9) Uani 1 1 d . . . . .
F1 F 0.1024(19) 0.6698(15) 0.0286(10) 0.135(6) Uani 0.5 1 d . . P A 1
F2 F -0.0359(12) 0.7741(9) 0.0119(5) 0.142(4) Uani 0.5 1 d . . P A 1
F3 F -0.0635(14) 0.6268(10) 0.0878(8) 0.154(5) Uani 0.5 1 d . . P A 1
F1A F 0.0897(19) 0.7060(16) 0.0054(10) 0.143(7) Uani 0.5 1 d . . P A 2
F2A F -0.1031(9) 0.7021(11) 0.0438(7) 0.131(4) Uani 0.5 1 d . . P A 2
F3A F 0.0114(14) 0.5951(8) 0.1042(8) 0.140(5) Uani 0.5 1 d . . P A 2
C2 C 0.1492(3) 0.8285(2) 0.15661(17) 0.0470(6) Uani 1 1 d . . . . .
C3 C 0.0892(3) 0.8567(2) 0.22482(18) 0.0516(6) Uani 1 1 d . . . . .
H3A H -0.012853 0.801798 0.220373 0.062 Uiso 1 1 calc R U . . .
C4 C 0.1784(3) 0.9642(2) 0.29838(16) 0.0407(5) Uani 1 1 d . . . . .
C5 C 0.1070(3) 0.9971(3) 0.36866(19) 0.0532(6) Uani 1 1 d . . . . .
F4 F -0.0333(2) 0.9079(2) 0.35777(16) 0.1118(8) Uani 1 1 d . . . . .
F5 F 0.1936(2) 1.0094(2) 0.45549(12) 0.0932(6) Uani 1 1 d . . . . .
F6 F 0.1012(2) 1.11236(18) 0.36576(14) 0.0878(6) Uani 1 1 d . . . . .
O2 O 0.31905(18) 1.04571(15) 0.31697(11) 0.0436(4) Uani 1 1 d . . . . .
O3 O 0.60464(19) 0.99144(16) 0.20300(11) 0.0474(4) Uani 1 1 d . . . . .
C6 C 0.7583(4) 0.9905(4) 0.1101(2) 0.0600(7) Uani 1 1 d . . . . .
F7 F 0.9064(16) 1.071(2) 0.1568(16) 0.097(5) Uani 0.5 1 d . . P B 1
F8 F 0.7390(13) 0.9751(14) 0.0210(6) 0.103(4) Uani 0.5 1 d . . P B 1
F9 F 0.734(2) 0.8688(17) 0.1326(13) 0.107(4) Uani 0.5 1 d . . P B 1
F7A F 0.8980(19) 1.040(2) 0.1674(16) 0.116(6) Uani 0.5 1 d . . P B 2
F8A F 0.7720(14) 1.0147(14) 0.0300(6) 0.118(4) Uani 0.5 1 d . . P B 2
F9A F 0.705(2) 0.8656(13) 0.1006(12) 0.110(5) Uani 0.5 1 d . . P B 2
C7 C 0.6570(3) 1.0465(2) 0.14202(16) 0.0456(6) Uani 1 1 d . . . . .
C8 C 0.6430(3) 1.1515(3) 0.10522(18) 0.0561(7) Uani 1 1 d . . . . .
H8A H 0.686740 1.177857 0.058770 0.067 Uiso 1 1 calc R U . . .
C9 C 0.5655(3) 1.2209(2) 0.13478(17) 0.0487(6) Uani 1 1 d . . . . .
C10 C 0.5780(4) 1.3478(3) 0.0977(2) 0.0691(8) Uani 1 1 d . . . . .
F10 F 0.6776(3) 1.45436(19) 0.16350(16) 0.1216(8) Uani 1 1 d . . . . .
F11 F 0.4448(3) 1.3580(2) 0.07730(15) 0.1029(7) Uani 1 1 d . . . . .
F12 F 0.6204(3) 1.3574(2) 0.02299(14) 0.1096(7) Uani 1 1 d . . . . .
O4 O 0.4929(2) 1.19578(16) 0.19031(12) 0.0549(5) Uani 1 1 d . . . . .
O1R O 0.4402(2) 0.84069(16) 0.35000(12) 0.0592(5) Uani 1 1 d . . . . .
N2R N 0.3981(2) 0.71671(18) 0.34957(12) 0.0405(4) Uani 1 1 d . . . . .
C3R C 0.4573(3) 0.6334(2) 0.30180(17) 0.0477(6) Uani 1 1 d . . . . .
C4R C 0.4382(5) 0.6520(3) 0.2018(2) 0.0963(13) Uani 1 1 d . . . . .
H4RA H 0.475999 0.598836 0.171822 0.144 Uiso 1 1 calc R U . . .
H4RB H 0.329876 0.624803 0.167968 0.144 Uiso 1 1 calc R U . . .
H4RC H 0.496844 0.744022 0.202187 0.144 Uiso 1 1 calc R U . . .
C5R C 0.6292(3) 0.6862(3) 0.3610(3) 0.0836(10) Uani 1 1 d . . . . .
H5RA H 0.675739 0.637741 0.334891 0.125 Uiso 1 1 calc R U . . .
H5RB H 0.682651 0.778935 0.361142 0.125 Uiso 1 1 calc R U . . .
H5RC H 0.637306 0.675002 0.424132 0.125 Uiso 1 1 calc R U . . .
C6R C 0.3546(3) 0.4916(2) 0.31214(17) 0.0464(6) Uani 1 1 d . . . . .
C7R C 0.2080(4) 0.4131(3) 0.2282(2) 0.0914(11) Uani 1 1 d . . . . .
H7RA H 0.236206 0.389236 0.175854 0.137 Uiso 1 1 calc R U . . .
H7RB H 0.142210 0.333885 0.243543 0.137 Uiso 1 1 calc R U . . .
H7RC H 0.152899 0.466610 0.212067 0.137 Uiso 1 1 calc R U . . .
C8R C 0.4424(4) 0.4086(3) 0.3424(2) 0.0708(9) Uani 1 1 d . . . . .
H8RA H 0.478270 0.386980 0.293192 0.106 Uiso 1 1 calc R U . . .
H8RB H 0.530275 0.458237 0.398100 0.106 Uiso 1 1 calc R U . . .
H8RC H 0.374067 0.328000 0.355106 0.106 Uiso 1 1 calc R U . . .
N9R N 0.2994(2) 0.52446(18) 0.39011(13) 0.0430(5) Uani 1 1 d . . . . .
O10R O 0.2343(2) 0.43868(16) 0.43382(13) 0.0651(5) Uani 1 1 d . . . . .
C11R C 0.3172(3) 0.6505(2) 0.40205(15) 0.0368(5) Uani 1 1 d . . . . .
C12R C 0.2697(3) 0.7103(2) 0.47061(15) 0.0366(5) Uani 1 1 d . . . . .
C13R C 0.3835(3) 0.8023(2) 0.54841(15) 0.0404(5) Uani 1 1 d . . . . .
H13A H 0.487117 0.828099 0.552293 0.048 Uiso 1 1 calc R U . . .
N14R N 0.3552(2) 0.85740(17) 0.61912(13) 0.0380(4) Uani 1 1 d . . . . .
C15R C 0.2046(3) 0.8217(2) 0.60994(17) 0.0458(6) Uani 1 1 d . . . . .
H15A H 0.181841 0.859746 0.657461 0.055 Uiso 1 1 calc R U . . .
C16R C 0.0827(3) 0.7325(3) 0.53478(18) 0.0500(6) Uani 1 1 d . . . . .
H16A H -0.019882 0.710632 0.531763 0.060 Uiso 1 1 calc R U . . .
C17R C 0.1146(3) 0.6753(2) 0.46329(16) 0.0415(5) Uani 1 1 d . . . . .
Cl18 Cl -0.03398(7) 0.56469(7) 0.36606(5) 0.0635(2) Uani 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O2 Cu O3 177.35(7) . . ?
O2 Cu O1 89.88(7) . . ?
O3 Cu O1 88.02(7) . . ?
O2 Cu N14R 88.94(7) . 2_676 ?
O3 Cu N14R 92.90(7) . 2_676 ?
O1 Cu N14R 171.49(7) . 2_676 ?
O2 Cu O4 94.45(6) . . ?
O3 Cu O4 87.40(6) . . ?
O1 Cu O4 96.59(7) . . ?
N14R Cu O4 91.90(7) 2_676 . ?
O2 Cu O1R 83.73(6) . . ?
O3 Cu O1R 94.53(6) . . ?
O1 Cu O1R 86.72(7) . . ?
N14R Cu O1R 84.78(7) 2_676 . ?
O4 Cu O1R 176.23(6) . . ?
C2 O1 Cu 124.56(15) . . ?
F3 C1 F1 111.0(9) . . ?
F1A C1 F2A 112.3(10) . . ?
F3 C1 F2 105.8(8) . . ?
F1 C1 F2 105.7(9) . . ?
F1A C1 F3A 105.7(9) . . ?
F2A C1 F3A 100.0(7) . . ?
F3 C1 C2 115.6(5) . . ?
F1 C1 C2 114.4(8) . . ?
F1A C1 C2 114.9(8) . . ?
F2A C1 C2 115.0(4) . . ?
F2 C1 C2 103.1(4) . . ?
F3A C1 C2 107.3(5) . . ?
O1 C2 C3 127.7(2) . . ?
O1 C2 C1 114.9(2) . . ?
C3 C2 C1 117.4(3) . . ?
O1 C2 Cu 34.51(11) . . ?
C3 C2 Cu 93.43(15) . . ?
C1 C2 Cu 148.9(2) . . ?
C4 C3 C2 121.0(2) . . ?
O2 C4 C3 127.9(2) . . ?
O2 C4 C5 112.2(2) . . ?
C3 C4 C5 119.9(2) . . ?
O2 C4 Cu 33.39(9) . . ?
C3 C4 Cu 95.21(15) . . ?
C5 C4 Cu 144.40(17) . . ?
F4 C5 F6 107.8(2) . . ?
F4 C5 F5 106.5(2) . . ?
F6 C5 F5 105.5(2) . . ?
F4 C5 C4 114.2(2) . . ?
F6 C5 C4 111.5(2) . . ?
F5 C5 C4 110.8(2) . . ?
C4 O2 Cu 125.67(14) . . ?
C7 O3 Cu 128.37(15) . . ?
F9A C6 F7A 106.9(13) . . ?
F9A C6 F8A 105.8(10) . . ?
F7A C6 F8A 105.4(11) . . ?
F8 C6 F7 108.5(11) . . ?
F8 C6 F9 106.7(9) . . ?
F7 C6 F9 106.0(12) . . ?
F9A C6 C7 112.7(8) . . ?
F7A C6 C7 112.5(11) . . ?
F8A C6 C7 113.1(6) . . ?
F8 C6 C7 115.6(6) . . ?
F7 C6 C7 108.4(10) . . ?
F9 C6 C7 111.3(7) . . ?
O3 C7 C8 129.9(2) . . ?
O3 C7 C6 113.1(2) . . ?
C8 C7 C6 116.9(2) . . ?
O3 C7 Cu 31.71(10) . . ?
C8 C7 Cu 98.38(15) . . ?
C6 C7 Cu 144.73(19) . . ?
C7 C8 C9 123.0(2) . . ?
O4 C9 C8 127.8(2) . . ?
O4 C9 C10 114.7(2) . . ?
C8 C9 C10 117.4(2) . . ?
O4 C9 Cu 37.66(11) . . ?
C8 C9 Cu 90.17(15) . . ?
C10 C9 Cu 152.29(18) . . ?
F12 C10 F10 108.3(3) . . ?
F12 C10 F11 107.1(3) . . ?
F10 C10 F11 104.4(3) . . ?
F12 C10 C9 114.5(2) . . ?
F10 C10 C9 110.2(2) . . ?
F11 C10 C9 111.7(3) . . ?
C9 O4 Cu 122.81(15) . . ?
N2R O1R Cu 149.24(14) . . ?
O1R N2R C11R 124.51(18) . . ?
O1R N2R C3R 123.25(18) . . ?
C11R N2R C3R 111.51(17) . . ?
N2R C3R C4R 109.9(2) . . ?
N2R C3R C5R 104.3(2) . . ?
C4R C3R C5R 111.5(3) . . ?
N2R C3R C6R 101.34(17) . . ?
C4R C3R C6R 115.4(2) . . ?
C5R C3R C6R 113.2(2) . . ?
N9R C6R C7R 105.7(2) . . ?
N9R C6R C8R 108.7(2) . . ?
C7R C6R C8R 111.2(2) . . ?
N9R C6R C3R 101.12(17) . . ?
C7R C6R C3R 114.2(2) . . ?
C8R C6R C3R 114.9(2) . . ?
O10R N9R C11R 125.20(19) . . ?
O10R N9R C6R 122.94(18) . . ?
C11R N9R C6R 111.70(18) . . ?
N2R C11R N9R 110.30(18) . . ?
N2R C11R C12R 125.00(19) . . ?
N9R C11R C12R 124.4(2) . . ?
C13R C12R C17R 117.76(19) . . ?
C13R C12R C11R 118.62(19) . . ?
C17R C12R C11R 123.6(2) . . ?
N14R C13R C12R 124.4(2) . . ?
N14R C13R Cu 36.57(11) . 2_676 ?
C12R C13R Cu 160.22(15) . 2_676 ?
C13R N14R C15R 116.4(2) . . ?
C13R N14R Cu 120.60(15) . 2_676 ?
C15R N14R Cu 122.80(15) . 2_676 ?
N14R C15R C16R 123.8(2) . . ?
N14R C15R Cu 35.16(11) . 2_676 ?
C16R C15R Cu 158.53(16) . 2_676 ?
C15R C16R C17R 118.8(2) . . ?
C16R C17R C12R 118.8(2) . . ?
C16R C17R Cl18 120.83(19) . . ?
C12R C17R Cl18 120.32(18) . . ?
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
Cu O2 1.9408(15) . ?
Cu O3 1.9489(15) . ?
Cu O1 1.9909(17) . ?
Cu N14R 2.0586(19) 2_676 ?
Cu O4 2.2407(16) . ?
Cu O1R 2.5013(15) . ?
O1 C2 1.256(3) . ?
C1 F3 1.176(7) . ?
C1 F1 1.237(12) . ?
C1 F1A 1.272(12) . ?
C1 F2A 1.284(8) . ?
C1 F2 1.393(9) . ?
C1 F3A 1.400(10) . ?
C1 C2 1.532(4) . ?
C2 C3 1.395(3) . ?
C3 C4 1.373(3) . ?
C4 O2 1.260(3) . ?
C4 C5 1.521(3) . ?
C5 F4 1.304(3) . ?
C5 F6 1.316(3) . ?
C5 F5 1.323(3) . ?
O3 C7 1.264(3) . ?
C6 F9A 1.263(14) . ?
C6 F7A 1.279(17) . ?
C6 F8A 1.293(10) . ?
C6 F8 1.298(10) . ?
C6 F7 1.322(16) . ?
C6 F9 1.373(17) . ?
C6 C7 1.529(3) . ?
C7 C8 1.378(3) . ?
C8 C9 1.410(3) . ?
C9 O4 1.227(3) . ?
C9 C10 1.540(4) . ?
C10 F12 1.306(3) . ?
C10 F10 1.318(3) . ?
C10 F11 1.320(4) . ?
O1R N2R 1.280(2) . ?
N2R C11R 1.337(3) . ?
N2R C3R 1.511(3) . ?
C3R C4R 1.516(3) . ?
C3R C5R 1.529(4) . ?
C3R C6R 1.557(3) . ?
C6R N9R 1.505(3) . ?
C6R C7R 1.519(4) . ?
C6R C8R 1.521(3) . ?
N9R O10R 1.271(2) . ?
N9R C11R 1.341(3) . ?
C11R C12R 1.465(3) . ?
C12R C13R 1.375(3) . ?
C12R C17R 1.392(3) . ?
C13R N14R 1.341(3) . ?
N14R C15R 1.341(3) . ?
C15R C16R 1.368(3) . ?
C16R C17R 1.384(3) . ?
C17R Cl18 1.721(2) . ?
