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#$Date: 2023-03-04 20:07:37 +0200 (Sat, 04 Mar 2023) $
#$Revision: 281404 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/58/7245884.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_7245884
loop_
_publ_author_name
'Bondarenko, Mikhail A.'
'Abramov, Pavel A.'
'Korolkov, Ilya V.'
'Bogomyakov, Artem S.'
'Sokolov, Maxim N.'
'Adonin, Sergey A.'
_publ_section_title
;
 Cu(ii) 3,5-diiodosalicylate complexes: precursor-dependent formation of
 mono-, di-, tri- and tetranuclear compounds and 1D coordination polymers
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              130
_journal_page_last               136
_journal_paper_doi               10.1039/D2CE01393B
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C52 H36 Cu4 I8 N4 O12'
_chemical_formula_weight         2178.21
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-11-03 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7967(6)
_cell_length_b                   17.7967(6)
_cell_length_c                   19.2988(9)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.4165
_cell_measurement_theta_min      2.2888
_cell_volume                     6112.4(4)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46730
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.521
_diffrn_reflns_theta_min         2.289
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    5.474
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.779
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0326
_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)+(0.0421P)²+25.9649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4011
_reflns_number_total             4683
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce01393b2.cif
_cod_data_source_block           BM546
_cod_depositor_comments
'Adding full bibliography for 7245877--7245890.cif.'
_cod_original_cell_volume        6112.4(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7245884
_shelx_shelxl_version_number     2017/1
_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   0.560
_shelx_estimated_absorpt_t_max   0.669
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
C1 C 0.47029(19) 0.09735(19) 0.83380(16) 0.0277(6) Uani 1 1 d . . . . .
C2 C 0.47295(18) 0.06598(18) 0.76251(16) 0.0251(6) Uani 1 1 d . . . . .
C3 C 0.44181(18) 0.10456(18) 0.70520(16) 0.0252(6) Uani 1 1 d . . . . .
C4 C 0.45017(18) 0.06906(19) 0.63933(16) 0.0263(6) Uani 1 1 d . . . . .
C5 C 0.48635(19) 0.00150(19) 0.63077(17) 0.0282(6) Uani 1 1 d . . . . .
H5 H 0.490692 -0.020376 0.586052 0.034 Uiso 1 1 calc R U . . .
C6 C 0.51665(19) -0.03460(18) 0.68856(17) 0.0279(6) Uani 1 1 d . . . . .
C7 C 0.51032(18) -0.00245(19) 0.75354(16) 0.0271(6) Uani 1 1 d . . . . .
H7 H 0.531609 -0.027131 0.792522 0.033 Uiso 1 1 calc R U . . .
C8 C 0.2818(2) 0.3481(2) 0.75123(19) 0.0337(7) Uani 1 1 d . . . . .
H8 H 0.256166 0.336601 0.793070 0.040 Uiso 1 1 calc R U . . .
C9 C 0.2566(2) 0.4077(2) 0.7120(2) 0.0392(8) Uani 1 1 d . . . . .
H9 H 0.213479 0.435239 0.725915 0.047 Uiso 1 1 calc R U . . .
C10 C 0.2709(3) 0.4931(3) 0.6085(3) 0.0674(16) Uani 1 1 d . . . . .
H10A H 0.283268 0.539803 0.632880 0.101 Uiso 1 1 calc R U . . .
H10B H 0.216595 0.490620 0.600644 0.101 Uiso 1 1 calc R U . . .
H10C H 0.297177 0.491937 0.563862 0.101 Uiso 1 1 calc R U . . .
C11 C 0.2951(2) 0.4271(2) 0.6516(2) 0.0409(9) Uani 1 1 d . . . . .
C12 C 0.3561(2) 0.3838(2) 0.6337(2) 0.0394(8) Uani 1 1 d . . . . .
H12 H 0.384007 0.395566 0.593176 0.047 Uiso 1 1 calc R U . . .
C13 C 0.3773(2) 0.3234(2) 0.6742(2) 0.0348(7) Uani 1 1 d . . . . .
H13 H 0.418784 0.293419 0.660162 0.042 Uiso 1 1 calc R U . . .
N1 N 0.34057(17) 0.30585(16) 0.73320(15) 0.0297(6) Uani 1 1 d . . . . .
O1 O 0.50709(14) 0.06313(14) 0.88025(12) 0.0316(5) Uani 1 1 d . . . . .
O2 O 0.43320(15) 0.15539(15) 0.84870(13) 0.0341(5) Uani 1 1 d . . . . .
O3 O 0.40776(15) 0.16958(14) 0.70822(12) 0.0334(5) Uani 1 1 d . . . . .
Cu1 Cu 0.37589(2) 0.21944(2) 0.78955(2) 0.02757(10) Uani 1 1 d . . . . .
I1 I 0.57026(2) -0.13865(2) 0.67667(2) 0.03821(8) Uani 1 1 d . . . . .
I2 I 0.40905(2) 0.12560(2) 0.55204(2) 0.04219(9) 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'
I I -0.4742 1.8119 '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 C1 O1 120.3(3) . . ?
O2 C1 C2 122.4(3) . . ?
O1 C1 C2 117.3(3) . . ?
C7 C2 C3 120.8(3) . . ?
C7 C2 C1 117.2(3) . . ?
C3 C2 C1 121.9(3) . . ?
O3 C3 C2 125.2(3) . . ?
O3 C3 C4 118.7(3) . . ?
C2 C3 C4 116.1(3) . . ?
C5 C4 C3 122.9(3) . . ?
C5 C4 I2 119.2(2) . . ?
C3 C4 I2 117.9(2) . . ?
C4 C5 C6 119.2(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C5 120.2(3) . . ?
C7 C6 I1 120.1(2) . . ?
C5 C6 I1 119.7(2) . . ?
C6 C7 C2 120.8(3) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
N1 C8 C9 123.1(4) . . ?
N1 C8 H8 118.5 . . ?
C9 C8 H8 118.5 . . ?
C8 C9 C11 119.3(4) . . ?
C8 C9 H9 120.3 . . ?
C11 C9 H9 120.3 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C9 117.2(4) . . ?
C12 C11 C10 121.7(5) . . ?
C9 C11 C10 121.0(4) . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
N1 C13 C12 121.7(4) . . ?
N1 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C8 N1 C13 118.0(3) . . ?
C8 N1 Cu1 122.8(2) . . ?
C13 N1 Cu1 119.2(3) . . ?
C1 O1 Cu1 113.4(2) . 16_657 ?
C1 O2 Cu1 129.3(2) . . ?
C3 O3 Cu1 126.3(2) . . ?
O3 Cu1 O2 93.21(10) . . ?
O3 Cu1 O1 158.39(12) . 11_667 ?
O2 Cu1 O1 87.67(11) . 11_667 ?
O3 Cu1 N1 90.21(11) . . ?
O2 Cu1 N1 163.60(12) . . ?
O1 Cu1 N1 95.01(11) 11_667 . ?
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
C1 O2 1.259(4) . ?
C1 O1 1.266(4) . ?
C1 C2 1.486(4) . ?
C2 C7 1.398(5) . ?
C2 C3 1.415(4) . ?
C3 O3 1.308(4) . ?
C3 C4 1.427(4) . ?
C4 C5 1.374(5) . ?
C4 I2 2.094(3) . ?
C5 C6 1.395(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(4) . ?
C6 I1 2.096(3) . ?
C7 H7 0.9500 . ?
C8 N1 1.334(5) . ?
C8 C9 1.378(5) . ?
C8 H8 0.9500 . ?
C9 C11 1.396(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.502(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.375(6) . ?
C12 C13 1.382(6) . ?
C12 H12 0.9500 . ?
C13 N1 1.349(5) . ?
C13 H13 0.9500 . ?
N1 Cu1 1.986(3) . ?
O1 Cu1 1.954(2) 16_657 ?
O2 Cu1 1.908(3) . ?
O3 Cu1 1.890(2) . ?
