#------------------------------------------------------------------------------
#$Date: 2023-03-04 19:07:37 +0100 (Sat 04 de Mar de 2023) $
#$Revision: 281404 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/58/7245885.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_7245885
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            'C50 H47.8 Cl4 Cu3 I4 N6 O6'
_chemical_formula_weight         1668.76
_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
_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                89.2500(10)
_cell_angle_beta                 85.6180(10)
_cell_angle_gamma                89.7730(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5657(2)
_cell_length_b                   11.8674(2)
_cell_length_c                   13.5591(3)
_cell_measurement_reflns_used    9395
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.4963
_cell_measurement_theta_min      2.7220
_cell_volume                     1374.16(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.534
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    3.645
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6383
_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            greenish-brown
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_description       block
_exptl_crystal_F_000             805
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         8388
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0222P)²+0.3077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7365
_reflns_number_total             8388
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce01393b2.cif
_cod_data_source_block           BM408_a
_cod_depositor_comments
'Adding full bibliography for 7245877--7245890.cif.'
_cod_original_formula_sum        'C50 H47.80 Cl4 Cu3 I4 N6 O6'
_cod_database_code               7245885
_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   0.500
_shelx_estimated_absorpt_t_max   0.581
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
C1 C 0.6720(2) 0.14059(17) 0.20780(15) 0.0220(4) Uani 1 1 d . . . . .
H1 H 0.577143 0.101835 0.199660 0.026 Uiso 1 1 calc R U . . .
C2 C 0.8035(3) 0.11460(19) 0.14659(15) 0.0257(4) Uani 1 1 d . . . . .
H2 H 0.798023 0.057921 0.098153 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9432(3) 0.17072(18) 0.15549(16) 0.0251(4) Uani 1 1 d . . . . .
C4 C 1.0889(3) 0.1458(2) 0.0901(2) 0.0430(7) Uani 1 1 d . . . . .
H4A H 1.080144 0.071104 0.061127 0.064 Uiso 1 1 calc . U . . .
H4B H 1.180167 0.147378 0.129453 0.064 Uiso 1 1 calc . U . . .
H4C H 1.101257 0.202795 0.037119 0.064 Uiso 1 1 calc . U . . .
C5 C 0.9439(3) 0.25212(18) 0.22788(16) 0.0261(4) Uani 1 1 d . . . . .
H5 H 1.036669 0.293373 0.236429 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8094(2) 0.27290(18) 0.28741(16) 0.0233(4) Uani 1 1 d . . . . .
H6 H 0.812631 0.328189 0.337239 0.028 Uiso 1 1 calc R U . . .
C7 C 0.1537(2) 0.27179(17) 0.45105(15) 0.0194(4) Uani 1 1 d . . . . .
H7 H 0.137404 0.216726 0.402681 0.023 Uiso 1 1 calc R U . . .
C8 C 0.0266(2) 0.30837(17) 0.51082(16) 0.0222(4) Uani 1 1 d . . . . .
H8 H -0.074434 0.278370 0.503356 0.027 Uiso 1 1 calc R U . . .
C9 C 0.0465(2) 0.38938(16) 0.58216(14) 0.0192(4) Uani 1 1 d . . . . .
C10 C -0.0901(3) 0.4313(2) 0.64854(17) 0.0285(5) Uani 1 1 d . . . . .
H10A H -0.081885 0.401928 0.715840 0.043 Uiso 1 1 calc . U . . .
H10B H -0.188083 0.405357 0.623726 0.043 Uiso 1 1 calc . U . . .
H10C H -0.089113 0.513858 0.649205 0.043 Uiso 1 1 calc . U . . .
C11 C 0.1971(2) 0.42915(17) 0.58882(15) 0.0200(4) Uani 1 1 d . . . . .
H11 H 0.216528 0.484339 0.636475 0.024 Uiso 1 1 calc R U . . .
C12 C 0.3194(2) 0.38884(16) 0.52638(14) 0.0183(4) Uani 1 1 d . . . . .
H12 H 0.421578 0.417767 0.532030 0.022 Uiso 1 1 calc R U . . .
C13 C 0.4254(2) 0.42997(16) 0.25155(14) 0.0172(4) Uani 1 1 d . . . . .
C14 C 0.3836(2) 0.50279(15) 0.16649(13) 0.0153(3) Uani 1 1 d . . . . .
C16 C 0.2770(2) 0.52265(16) 0.00782(14) 0.0173(4) Uani 1 1 d . . . . .
C17 C 0.3228(2) 0.63453(16) 0.00121(14) 0.0191(4) Uani 1 1 d . . . . .
H17 H 0.303375 0.678918 -0.055395 0.023 Uiso 1 1 calc R U . . .
C18 C 0.3974(2) 0.68088(16) 0.07838(14) 0.0179(4) Uani 1 1 d . . . . .
C19 C 0.4257(2) 0.61741(16) 0.16338(14) 0.0169(4) Uani 1 1 d . . . . .
C20 C 0.8258(2) -0.00408(16) 0.41896(14) 0.0182(4) Uani 1 1 d . . . . .
H20 H 0.838046 0.049937 0.468862 0.022 Uiso 1 1 calc R U . . .
C21 C 0.9553(2) -0.03476(17) 0.35856(15) 0.0210(4) Uani 1 1 d . . . . .
H21 H 1.053892 -0.001023 0.366450 0.025 Uiso 1 1 calc R U . . .
C22 C 0.9415(2) -0.11515(17) 0.28604(15) 0.0218(4) Uani 1 1 d . . . . .
C23 C 1.0819(3) -0.1508(2) 0.2199(2) 0.0383(6) Uani 1 1 d . . . . .
H23A H 1.102979 -0.094170 0.167383 0.057 Uiso 1 1 calc . U . . .
H23B H 1.060844 -0.223598 0.190340 0.057 Uiso 1 1 calc . U . . .
H23C H 1.173187 -0.157900 0.258950 0.057 Uiso 1 1 calc . U . . .
C24 C 0.7935(2) -0.15923(17) 0.27683(15) 0.0210(4) Uani 1 1 d . . . . .
H24 H 0.778361 -0.213864 0.227902 0.025 Uiso 1 1 calc R U . . .
C25 C 0.6679(2) -0.12326(16) 0.33931(14) 0.0177(4) Uani 1 1 d . . . . .
H25 H 0.567111 -0.153530 0.331609 0.021 Uiso 1 1 calc R U . . .
N1 N 0.67415(19) 0.21877(14) 0.27832(12) 0.0187(3) Uani 1 1 d . . . . .
N2 N 0.29917(18) 0.31041(13) 0.45814(11) 0.0154(3) Uani 1 1 d . . . . .
N3 N 0.68365(18) -0.04730(13) 0.41016(11) 0.0153(3) Uani 1 1 d . . . . .
O1 O 0.38559(16) 0.32691(11) 0.25225(10) 0.0191(3) Uani 1 1 d . . . . .
O2 O 0.50069(17) 0.47286(12) 0.31771(10) 0.0218(3) Uani 1 1 d . . . . .
Cl1 Cl 0.62280(5) 0.22516(4) 0.50450(3) 0.01796(9) Uani 1 1 d . . . . .
Cl2 Cl 0.36817(5) 0.05348(4) 0.36112(3) 0.01625(8) Uani 1 1 d . . . . .
Cu1 Cu 0.48222(3) 0.25626(2) 0.36947(2) 0.01508(5) Uani 1 1 d . . . . .
Cu2 Cu 0.500000 0.000000 0.500000 0.01496(6) Uani 1 2 d S . P . .
I1 I 0.16083(2) 0.45184(2) -0.10685(2) 0.02390(4) Uani 1 1 d . . . . .
I2 I 0.47941(2) 0.84738(2) 0.06737(2) 0.02559(4) Uani 1 1 d . . . . .
O3 O 0.49174(19) 0.66720(13) 0.23732(11) 0.0201(3) Uani 0.9 1 d D . P A 1
H1X H 0.506(3) 0.6122(18) 0.2749(17) 0.024 Uiso 0.9 1 d D U P B 1
C15 C 0.3081(2) 0.45626(16) 0.08891(14) 0.0161(3) Uani 1 1 d . . . C 1
H15 H 0.278120 0.379232 0.091736 0.019 Uiso 1 1 calc R U . C 1
O3X O 0.2684(19) 0.3485(13) 0.0907(12) 0.029(3) Uiso 0.1 1 d . . P D 2
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'
Cl Cl 0.1484 0.1585 '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
N1 C1 C2 122.2(2) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C1 C2 C3 120.4(2) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C5 117.05(19) . . ?
C2 C3 C4 122.3(2) . . ?
C5 C3 C4 120.7(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C3 119.7(2) . . ?
C6 C5 H5 120.2 . . ?
C3 C5 H5 120.2 . . ?
N1 C6 C5 123.1(2) . . ?
N1 C6 H6 118.4 . . ?
C5 C6 H6 118.4 . . ?
N2 C7 C8 122.95(18) . . ?
N2 C7 H7 118.5 . . ?
C8 C7 H7 118.5 . . ?
C7 C8 C9 119.90(18) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C11 C9 C8 116.81(17) . . ?
C11 C9 C10 121.99(19) . . ?
C8 C9 C10 121.20(19) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C9 120.30(18) . . ?
C12 C11 H11 119.9 . . ?
C9 C11 H11 119.9 . . ?
N2 C12 C11 122.46(18) . . ?
N2 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
O2 C13 O1 123.18(17) . . ?
O2 C13 C14 118.66(17) . . ?
O1 C13 C14 118.14(17) . . ?
C15 C14 C19 120.20(17) . . ?
C15 C14 C13 120.09(17) . . ?
C19 C14 C13 119.67(17) . . ?
C15 C16 C17 120.98(18) . . ?
C15 C16 I1 119.31(14) . . ?
C17 C16 I1 119.71(14) . . ?
C16 C17 C18 119.12(18) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C19 121.51(18) . . ?
C17 C18 I2 120.09(14) . . ?
C19 C18 I2 118.35(14) . . ?
O3 C19 C18 119.19(18) . . ?
O3 C19 C14 122.63(17) . . ?
C18 C19 C14 118.18(17) . . ?
N3 C20 C21 122.65(18) . . ?
N3 C20 H20 118.7 . . ?
C21 C20 H20 118.7 . . ?
C20 C21 C22 119.95(18) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C24 C22 C21 117.15(18) . . ?
C24 C22 C23 122.0(2) . . ?
C21 C22 C23 120.8(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C22 119.79(19) . . ?
C25 C24 H24 120.1 . . ?
C22 C24 H24 120.1 . . ?
N3 C25 C24 122.34(18) . . ?
N3 C25 H25 118.8 . . ?
C24 C25 H25 118.8 . . ?
C6 N1 C1 117.57(17) . . ?
C6 N1 Cu1 120.03(14) . . ?
C1 N1 Cu1 122.40(14) . . ?
C7 N2 C12 117.58(16) . . ?
C7 N2 Cu1 122.12(13) . . ?
C12 N2 Cu1 120.29(13) . . ?
C20 N3 C25 118.09(16) . . ?
C20 N3 Cu2 120.96(13) . . ?
C25 N3 Cu2 120.94(13) . . ?
C13 O1 Cu1 105.58(12) . . ?
Cu2 Cl2 Cu1 89.944(15) . . ?
N2 Cu1 O1 89.54(6) . . ?
N2 Cu1 N1 173.98(7) . . ?
O1 Cu1 N1 88.44(6) . . ?
N2 Cu1 Cl1 90.22(5) . . ?
O1 Cu1 Cl1 163.88(4) . . ?
N1 Cu1 Cl1 90.14(5) . . ?
N2 Cu1 Cl2 92.77(5) . . ?
O1 Cu1 Cl2 99.29(4) . . ?
N1 Cu1 Cl2 93.16(5) . . ?
Cl1 Cu1 Cl2 96.819(17) . . ?
N3 Cu2 N3 180.0 2_656 . ?
N3 Cu2 Cl2 89.39(5) 2_656 2_656 ?
N3 Cu2 Cl2 90.61(5) . 2_656 ?
N3 Cu2 Cl2 90.61(5) 2_656 . ?
N3 Cu2 Cl2 89.39(5) . . ?
Cl2 Cu2 Cl2 180.00(2) 2_656 . ?
C19 O3 H1X 101.5(19) . . ?
C16 C15 C14 119.90(18) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
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 N1 1.342(2) . ?
C1 C2 1.383(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.386(3) . ?
C2 H2 0.9500 . ?
C3 C5 1.387(3) . ?
C3 C4 1.505(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.379(3) . ?
C5 H5 0.9500 . ?
C6 N1 1.342(3) . ?
C6 H6 0.9500 . ?
C7 N2 1.340(2) . ?
C7 C8 1.379(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(3) . ?
C8 H8 0.9500 . ?
C9 C11 1.385(3) . ?
C9 C10 1.508(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.384(3) . ?
C11 H11 0.9500 . ?
C12 N2 1.342(2) . ?
C12 H12 0.9500 . ?
C13 O2 1.258(2) . ?
C13 O1 1.271(2) . ?
C13 C14 1.496(3) . ?
C14 C15 1.397(3) . ?
C14 C19 1.408(3) . ?
C16 C15 1.386(3) . ?
C16 C17 1.386(3) . ?
C16 I1 2.0954(19) . ?
C17 C18 1.388(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.404(3) . ?
C18 I2 2.0994(19) . ?
C19 O3 1.334(2) . ?
C20 N3 1.338(2) . ?
C20 C21 1.378(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.391(3) . ?
C21 H21 0.9500 . ?
C22 C24 1.388(3) . ?
C22 C23 1.507(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.387(3) . ?
C24 H24 0.9500 . ?
C25 N3 1.341(2) . ?
C25 H25 0.9500 . ?
N1 Cu1 2.0313(16) . ?
N2 Cu1 2.0102(16) . ?
N3 Cu2 1.9979(15) . ?
O1 Cu1 2.0187(13) . ?
Cl1 Cu1 2.2921(5) . ?
Cl2 Cu2 2.3478(4) . ?
Cl2 Cu1 2.6079(5) . ?
O3 H1X 0.837(16) . ?
C15 H15 0.9500 . ?
