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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/7/24/58/7245890.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_7245890
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            'C56 H44 Cu4 I8 N4 O12'
_chemical_formula_weight         2234.31
_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
;
2022-08-04 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                   17.7012(4)
_cell_length_b                   17.7012(4)
_cell_length_c                   20.5023(8)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2770
_cell_measurement_theta_min      2.5682
_cell_volume                     6424.0(3)
_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 0.998
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33846
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.578
_diffrn_reflns_theta_min         1.520
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    5.212
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5680
_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            grass-green
_exptl_crystal_density_diffrn    2.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0345
_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)+(0.0223P)²+58.3205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3719
_reflns_number_total             4515
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce01393b2.cif
_cod_data_source_block           BM438-1_a
_cod_depositor_comments
'Adding full bibliography for 7245877--7245890.cif.'
_cod_original_cell_volume        6424.0(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7245890
_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   0.489
_shelx_estimated_absorpt_t_max   0.903
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
I1 I 0.58027(2) 0.63192(2) 0.42794(2) 0.04008(10) Uani 1 1 d . . . . .
C1 C 0.5308(2) 0.5960(2) 0.1626(2) 0.0255(8) Uani 1 1 d . . . . .
N1 N 0.6601(2) 0.8061(2) 0.26042(18) 0.0269(7) Uani 1 1 d . . . . .
O1 O 0.58544(18) 0.67290(17) 0.28161(14) 0.0286(6) Uani 1 1 d . . . . .
Cu1 Cu 0.62321(3) 0.72094(3) 0.20604(2) 0.02500(12) Uani 1 1 d . . . . .
I2 I 0.44111(2) 0.35377(2) 0.30780(2) 0.04114(10) Uani 1 1 d . . . . .
C2 C 0.5287(2) 0.5645(2) 0.2296(2) 0.0246(8) Uani 1 1 d . . . . .
O2 O 0.56758(18) 0.65607(18) 0.14905(15) 0.0316(7) Uani 1 1 d . . . . .
O3 O 0.49512(18) 0.56189(17) 0.11818(15) 0.0301(6) Uani 1 1 d . . . . .
C3 C 0.5556(2) 0.6055(2) 0.2841(2) 0.0229(7) Uani 1 1 d . . . . .
C4 C 0.5472(2) 0.5698(2) 0.3456(2) 0.0252(8) Uani 1 1 d . . . . .
C6 C 0.4896(2) 0.4613(2) 0.2985(2) 0.0263(8) Uani 1 1 d . . . . .
C5 C 0.5158(2) 0.4992(2) 0.3530(2) 0.0264(8) Uani 1 1 d . . . . .
H5 H 0.512242 0.476838 0.395032 0.032 Uiso 1 1 calc R U . . .
C8 C 0.7214(2) 0.8461(2) 0.2451(2) 0.0284(8) Uani 1 1 d . . . . .
H8 H 0.748218 0.833749 0.206443 0.034 Uiso 1 1 calc R U . . .
C7 C 0.4952(2) 0.4932(2) 0.2371(2) 0.0263(8) Uani 1 1 d . . . . .
H7 H 0.476392 0.466909 0.200151 0.032 Uiso 1 1 calc R U . . .
C9 C 0.7473(3) 0.9048(3) 0.2832(2) 0.0322(9) Uani 1 1 d . . . . .
H9 H 0.791806 0.931143 0.270929 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7087(3) 0.9255(3) 0.3392(2) 0.0350(10) Uani 1 1 d . . . . .
C11 C 0.7357(4) 0.9921(4) 0.3790(3) 0.0521(15) Uani 1 1 d . . . . .
H11A H 0.785679 0.979254 0.397572 0.062 Uiso 1 1 calc R U . . .
H11B H 0.743134 1.035351 0.349042 0.062 Uiso 1 1 calc R U . . .
C12 C 0.6858(4) 1.0174(3) 0.4334(3) 0.0492(14) Uani 1 1 d . . . . .
H12A H 0.635324 1.028747 0.416295 0.074 Uiso 1 1 calc . U . . .
H12B H 0.707072 1.062869 0.453545 0.074 Uiso 1 1 calc . U . . .
H12C H 0.682084 0.977213 0.466127 0.074 Uiso 1 1 calc . U . . .
C13 C 0.6452(3) 0.8832(3) 0.3554(2) 0.0319(9) Uani 1 1 d . . . . .
H13 H 0.617199 0.894896 0.393637 0.038 Uiso 1 1 calc R U . . .
C14 C 0.6231(2) 0.8242(2) 0.3160(2) 0.0286(9) Uani 1 1 d . . . . .
H14 H 0.580185 0.795237 0.328225 0.034 Uiso 1 1 calc R U . . .
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
O3 C1 O2 119.8(4) . . ?
O3 C1 C2 118.4(4) . . ?
O2 C1 C2 121.8(4) . . ?
C8 N1 C14 117.8(4) . . ?
C8 N1 Cu1 122.6(3) . . ?
C14 N1 Cu1 119.6(3) . . ?
C3 O1 Cu1 125.9(3) . . ?
O1 Cu1 O2 92.78(13) . . ?
O1 Cu1 O3 160.92(14) . 12_766 ?
O2 Cu1 O3 87.62(14) . 12_766 ?
O1 Cu1 N1 89.85(14) . . ?
O2 Cu1 N1 165.67(15) . . ?
O3 Cu1 N1 94.47(14) 12_766 . ?
C7 C2 C3 121.0(4) . . ?
C7 C2 C1 116.8(4) . . ?
C3 C2 C1 122.1(4) . . ?
C1 O2 Cu1 129.0(3) . . ?
C1 O3 Cu1 113.0(3) . 15_565 ?
O1 C3 C2 125.0(4) . . ?
O1 C3 C4 118.9(4) . . ?
C2 C3 C4 116.1(4) . . ?
C5 C4 C3 123.1(4) . . ?
C5 C4 I1 119.9(3) . . ?
C3 C4 I1 117.0(3) . . ?
C7 C6 C5 120.9(4) . . ?
C7 C6 I2 118.9(3) . . ?
C5 C6 I2 120.2(3) . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
N1 C8 C9 122.6(4) . . ?
N1 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C6 C7 C2 119.9(4) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
C8 C9 C10 120.3(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C13 117.0(4) . . ?
C9 C10 C11 119.8(5) . . ?
C13 C10 C11 123.1(5) . . ?
C12 C11 C10 116.8(5) . . ?
C12 C11 H11A 108.1 . . ?
C10 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
C10 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C10 119.8(4) . . ?
C14 C13 H13 120.1 . . ?
C10 C13 H13 120.1 . . ?
N1 C14 C13 122.5(4) . . ?
N1 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
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
I1 C4 2.099(4) . ?
C1 O3 1.262(5) . ?
C1 O2 1.277(5) . ?
C1 C2 1.482(6) . ?
N1 C8 1.334(6) . ?
N1 C14 1.353(6) . ?
N1 Cu1 1.985(4) . ?
O1 C3 1.307(5) . ?
O1 Cu1 1.890(3) . ?
Cu1 O2 1.911(3) . ?
Cu1 O3 1.954(3) 12_766 ?
I2 C6 2.097(4) . ?
C2 C7 1.403(6) . ?
C2 C3 1.415(6) . ?
C3 C4 1.417(6) . ?
C4 C5 1.376(6) . ?
C6 C7 1.382(6) . ?
C6 C5 1.385(6) . ?
C5 H5 0.9500 . ?
C8 C9 1.376(6) . ?
C8 H8 0.9500 . ?
C7 H7 0.9500 . ?
C9 C10 1.386(7) . ?
C9 H9 0.9500 . ?
C10 C13 1.390(7) . ?
C10 C11 1.512(7) . ?
C11 C12 1.492(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.377(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
