#------------------------------------------------------------------------------
#$Date: 2024-09-07 08:28:40 +0300 (Sat, 07 Sep 2024) $
#$Revision: 294673 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023228.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023228
loop_
_publ_author_name
'Loukopoulos, Edward'
'Papatriantafyllopoulou, Constantina'
'Moushi, Eleni'
'Kitos, Alexandros A.'
'Tasiopoulos, Anastasios J.'
'Perlepes, Spyros P.'
'Nastopoulos, Vassilios'
_publ_section_title
;
 Solvatomorphism in a series of copper(II) complexes with the
 5-phenylimidazole/perchlorate system as ligands.
;
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              347
_journal_page_last               359
_journal_paper_doi               10.1107/S2052520624005948
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         'C36 H32 Cl2 Cu N8 O8, 2(C3 H7 N O)'
_chemical_formula_sum            'C42 H46 Cl2 Cu N10 O10'
_chemical_formula_weight         985.33
_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-2014/7
_cell_angle_alpha                91.493(4)
_cell_angle_beta                 107.948(5)
_cell_angle_gamma                109.075(5)
_cell_formula_units_Z            1
_cell_length_a                   9.1544(4)
_cell_length_b                   9.8343(5)
_cell_length_c                   14.2557(8)
_cell_measurement_reflns_used    4143
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9180
_cell_measurement_theta_min      4.3940
_cell_volume                     1142.38(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics
'PLATON v.270519 (Spek, 2009); MERCURY v.2020.3.0 (Macrae et al., 2020)'
_computing_publication_material
'WINGX v.2018.3 (Farrugia, 2012); OLEX2 v.1.3.0 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution
'SHELXT-2018/2 (Sheldrick, 2015); SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova with Atlas CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8820
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.991
_diffrn_reflns_theta_min         3.034
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             511
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4905
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0358P)²+1.1070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4337
_reflns_number_total             4905
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            aw5090sup1.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 2023223--2023233.cif.'
_cod_database_code               2023228
_cod_database_fobs_code          2023228
_shelx_shelxl_version_number     2014/7
_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   0.852
_shelx_estimated_absorpt_t_max   0.907
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 0.5000 0.5000 0.5000 0.01613(10) Uani 1 2 d S . P . .
N1B N 0.6099(2) 0.41667(19) 0.24823(12) 0.0206(3) Uani 1 1 d D . . . .
H1B H 0.670(3) 0.397(3) 0.2187(17) 0.031 Uiso 1 1 d D U . . .
C2B C 0.6479(2) 0.4455(2) 0.34702(15) 0.0204(4) Uani 1 1 d . . . . .
H2B H 0.7496 0.4519 0.3948 0.024 Uiso 1 1 calc R U . . .
N3B N 0.52469(19) 0.46387(17) 0.36893(12) 0.0176(3) Uani 1 1 d . . . . .
C4B C 0.4023(2) 0.4462(2) 0.27900(14) 0.0189(4) Uani 1 1 d . . . . .
H4B H 0.2983 0.4532 0.2712 0.023 Uiso 1 1 calc R U . . .
C5B C 0.4535(2) 0.4171(2) 0.20304(15) 0.0194(4) Uani 1 1 d . . . . .
C6B C 0.3668(3) 0.3892(2) 0.09512(15) 0.0221(4) Uani 1 1 d . . . . .
C7B C 0.4091(3) 0.3127(3) 0.03085(16) 0.0283(5) Uani 1 1 d . . . . .
H7B H 0.4991 0.2805 0.0560 0.034 Uiso 1 1 calc R U . . .
C8B C 0.3192(3) 0.2832(3) -0.07055(17) 0.0352(5) Uani 1 1 d . . . . .
H8B H 0.3481 0.2301 -0.1141 0.042 Uiso 1 1 calc R U . . .
C9B C 0.1890(3) 0.3300(3) -0.10851(17) 0.0351(5) Uani 1 1 d . . . . .
H9B H 0.1276 0.3084 -0.1777 0.042 Uiso 1 1 calc R U . . .
C10B C 0.1485(3) 0.4085(3) -0.04507(17) 0.0336(5) Uani 1 1 d . . . . .
H10B H 0.0601 0.4425 -0.0709 0.040 Uiso 1 1 calc R U . . .
C11B C 0.2362(3) 0.4380(3) 0.05616(16) 0.0285(5) Uani 1 1 d . . . . .
H11B H 0.2072 0.4917 0.0993 0.034 Uiso 1 1 calc R U . . .
N1A N 0.8173(2) 0.92475(18) 0.57926(12) 0.0191(3) Uani 1 1 d D . . . .
H1A H 0.831(3) 1.0142(13) 0.5911(18) 0.029 Uiso 1 1 d D U . . .
C2A C 0.6699(2) 0.8184(2) 0.54604(14) 0.0199(4) Uani 1 1 d . . . . .
H2A H 0.5681 0.8329 0.5323 0.024 Uiso 1 1 calc R U . . .
N3A N 0.6856(2) 0.69092(17) 0.53513(12) 0.0179(3) Uani 1 1 d . . . . .
C4A C 0.8516(2) 0.7179(2) 0.56183(14) 0.0182(4) Uani 1 1 d . . . . .
H4A H 0.8997 0.6460 0.5608 0.022 Uiso 1 1 calc R U . . .
C5A C 0.9366(2) 0.8634(2) 0.59000(14) 0.0183(4) Uani 1 1 d . . . . .
C6A C 1.1128(2) 0.9470(2) 0.62694(14) 0.0192(4) Uani 1 1 d . . . . .
C7A C 1.1738(3) 1.0970(2) 0.65597(15) 0.0222(4) Uani 1 1 d . . . . .
H7A H 1.1000 1.1477 0.6511 0.027 Uiso 1 1 calc R U . . .
C8A C 1.3420(3) 1.1724(2) 0.69201(16) 0.0270(5) Uani 1 1 d . . . . .
H8A H 1.3823 1.2746 0.7111 0.032 Uiso 1 1 calc R U . . .
C9A C 1.4513(3) 1.1004(3) 0.70042(17) 0.0312(5) Uani 1 1 d . . . . .
H9A H 1.5661 1.1526 0.7258 0.037 Uiso 1 1 calc R U . . .
C10A C 1.3917(3) 0.9511(3) 0.67148(18) 0.0324(5) Uani 1 1 d . . . . .
H10A H 1.4660 0.9008 0.6769 0.039 Uiso 1 1 calc R U . . .
C11A C 1.2237(3) 0.8752(2) 0.63465(17) 0.0267(5) Uani 1 1 d . . . . .
H11A H 1.1839 0.7732 0.6145 0.032 Uiso 1 1 calc R U . . .
Cl Cl 0.84244(6) 0.34590(5) 0.62943(4) 0.02129(12) Uani 1 1 d . . . . .
O1 O 0.69153(19) 0.35784(18) 0.56906(12) 0.0321(4) Uani 1 1 d . . . . .
O2 O 0.8987(3) 0.4350(2) 0.72287(14) 0.0566(6) Uani 1 1 d . . . . .
O3 O 0.9597(2) 0.3927(2) 0.5795(2) 0.0617(6) Uani 1 1 d . . . . .
O4 O 0.8185(2) 0.19824(19) 0.64519(14) 0.0428(5) Uani 1 1 d . . . . .
N2 N 0.8939(2) 0.1620(2) 0.09945(16) 0.0338(5) Uani 1 1 d . . . . .
C12 C 0.8756(3) 0.2478(2) 0.16407(16) 0.0249(4) Uani 1 1 d . . . . .
H12 H 0.9553 0.2742 0.2289 0.030 Uiso 1 1 calc R U . . .
C13 C 0.7800(4) 0.1220(3) -0.0032(2) 0.0506(7) Uani 1 1 d . . . . .
H13A H 0.6996 0.1705 -0.0121 0.076 Uiso 1 1 calc R U . . .
H13B H 0.7230 0.0165 -0.0169 0.076 Uiso 1 1 calc R U . . .
H13C H 0.8412 0.1524 -0.0492 0.076 Uiso 1 1 calc R U . . .
C14 C 1.0252(3) 0.1026(3) 0.1280(2) 0.0435(7) Uani 1 1 d . . . . .
H14A H 1.0973 0.1449 0.1963 0.065 Uiso 1 1 calc R U . . .
H14B H 1.0888 0.1262 0.0827 0.065 Uiso 1 1 calc R U . . .
H14C H 0.9780 -0.0032 0.1241 0.065 Uiso 1 1 calc R U . . .
O5 O 0.7639(2) 0.29644(19) 0.14732(12) 0.0345(4) 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'
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'
Cu Cu 0.3201 1.2651 '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
N3B Cu N3B 180.0 2_666 . ?
N3B Cu N3A 88.25(7) 2_666 . ?
N3B Cu N3A 91.75(7) . . ?
N3B Cu N3A 91.74(7) 2_666 2_666 ?
N3B Cu N3A 88.26(7) . 2_666 ?
N3A Cu N3A 180.0 . 2_666 ?
C2B N1B C5B 108.22(16) . . ?
C2B N1B H1B 125.7(17) . . ?
C5B N1B H1B 126.0(17) . . ?
N3B C2B N1B 110.77(17) . . ?
N3B C2B H2B 124.6 . . ?
N1B C2B H2B 124.6 . . ?
C2B N3B C4B 106.01(16) . . ?
C2B N3B Cu 130.49(14) . . ?
C4B N3B Cu 123.44(13) . . ?
C5B C4B N3B 109.64(17) . . ?
C5B C4B H4B 125.2 . . ?
N3B C4B H4B 125.2 . . ?
C4B C5B N1B 105.37(17) . . ?
C4B C5B C6B 129.71(18) . . ?
N1B C5B C6B 124.91(18) . . ?
C7B C6B C11B 119.02(19) . . ?
C7B C6B C5B 121.69(19) . . ?
C11B C6B C5B 119.27(19) . . ?
C6B C7B C8B 119.9(2) . . ?
C6B C7B H7B 120.1 . . ?
C8B C7B H7B 120.1 . . ?
C9B C8B C7B 120.9(2) . . ?
C9B C8B H8B 119.6 . . ?
C7B C8B H8B 119.6 . . ?
C8B C9B C10B 119.4(2) . . ?
C8B C9B H9B 120.3 . . ?
C10B C9B H9B 120.3 . . ?
C9B C10B C11B 120.4(2) . . ?
C9B C10B H10B 119.8 . . ?
C11B C10B H10B 119.8 . . ?
C10B C11B C6B 120.4(2) . . ?
C10B C11B H11B 119.8 . . ?
C6B C11B H11B 119.8 . . ?
C2A N1A C5A 108.48(16) . . ?
C2A N1A H1A 123.9(17) . . ?
C5A N1A H1A 127.6(17) . . ?
N3A C2A N1A 110.71(17) . . ?
N3A C2A H2A 124.6 . . ?
N1A C2A H2A 124.6 . . ?
C2A N3A C4A 106.15(16) . . ?
C2A N3A Cu 124.59(14) . . ?
C4A N3A Cu 128.99(13) . . ?
C5A C4A N3A 109.92(17) . . ?
C5A C4A H4A 125.0 . . ?
N3A C4A H4A 125.0 . . ?
C4A C5A N1A 104.74(17) . . ?
C4A C5A C6A 131.54(18) . . ?
N1A C5A C6A 123.70(18) . . ?
C11A C6A C7A 118.71(19) . . ?
C11A C6A C5A 119.43(18) . . ?
C7A C6A C5A 121.86(18) . . ?
C8A C7A C6A 120.2(2) . . ?
C8A C7A H7A 119.9 . . ?
C6A C7A H7A 119.9 . . ?
C9A C8A C7A 120.8(2) . . ?
C9A C8A H8A 119.6 . . ?
C7A C8A H8A 119.6 . . ?
C8A C9A C10A 119.4(2) . . ?
C8A C9A H9A 120.3 . . ?
C10A C9A H9A 120.3 . . ?
C11A C10A C9A 120.2(2) . . ?
C11A C10A H10A 119.9 . . ?
C9A C10A H10A 119.9 . . ?
C10A C11A C6A 120.7(2) . . ?
C10A C11A H11A 119.6 . . ?
C6A C11A H11A 119.6 . . ?
O2 Cl O3 110.28(15) . . ?
O2 Cl O1 108.93(10) . . ?
O3 Cl O1 108.75(13) . . ?
O2 Cl O4 109.46(12) . . ?
O3 Cl O4 109.25(12) . . ?
O1 Cl O4 110.16(11) . . ?
C12 N2 C14 121.4(2) . . ?
C12 N2 C13 120.4(2) . . ?
C14 N2 C13 118.3(2) . . ?
O5 C12 N2 125.3(2) . . ?
O5 C12 H12 117.3 . . ?
N2 C12 H12 117.3 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 H14A 109.5 . . ?
N2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
Cu N3B 1.9866(16) 2_666 ?
Cu N3B 1.9867(16) . ?
Cu N3A 2.0009(16) . ?
Cu N3A 2.0009(16) 2_666 ?
N1B C2B 1.341(3) . ?
N1B C5B 1.378(3) . ?
N1B H1B 0.853(10) . ?
C2B N3B 1.323(3) . ?
C2B H2B 0.9500 . ?
N3B C4B 1.380(2) . ?
C4B C5B 1.363(3) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.468(3) . ?
C6B C7B 1.389(3) . ?
C6B C11B 1.395(3) . ?
C7B C8B 1.393(3) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.378(4) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.382(4) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.387(3) . ?
C10B H10B 0.9500 . ?
C11B H11B 0.9500 . ?
N1A C2A 1.340(3) . ?
N1A C5A 1.383(2) . ?
N1A H1A 0.851(10) . ?
C2A N3A 1.318(3) . ?
C2A H2A 0.9500 . ?
N3A C4A 1.378(2) . ?
C4A C5A 1.365(3) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.463(3) . ?
C6A C11A 1.395(3) . ?
C6A C7A 1.395(3) . ?
C7A C8A 1.390(3) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.382(3) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.389(3) . ?
C9A H9A 0.9500 . ?
C10A C11A 1.389(3) . ?
C10A H10A 0.9500 . ?
C11A H11A 0.9500 . ?
Cl O2 1.4242(18) . ?
Cl O3 1.427(2) . ?
Cl O1 1.4288(15) . ?
Cl O4 1.4307(17) . ?
N2 C12 1.318(3) . ?
N2 C14 1.456(3) . ?
N2 C13 1.464(3) . ?
C12 O5 1.227(3) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
