#------------------------------------------------------------------------------
#$Date: 2020-08-06 16:01:59 +0200 (jue 06 de ago de 2020) $
#$Revision: 254984 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/46/7704604.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_7704604
loop_
_publ_author_name
'Pantalon Juraj, Natalija'
'Krklec, Marko'
'Novosel, Tiana'
'Perić, Berislav'
'Vianello, Robert'
'Raić-Malić, Silvana'
'Kirin, Srećko I'
_publ_section_title
;
 Copper(ii) and zinc(ii) complexes of mono- and
 bis-1,2,3-triazole-substituted heterocyclic ligands.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9002
_journal_page_last               9015
_journal_paper_doi               10.1039/d0dt01244k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C54 H48 Cu N16 S2 2+, F6 Si, 2-, 3.6(H2 O)'
_chemical_formula_sum            'C54 H55.2 Cu F6 N16 O3.6 S2 Si'
_chemical_formula_weight         1255.7
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc24xv97
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-13 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.089(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5387(5)
_cell_length_b                   16.3557(5)
_cell_length_c                   16.1961(7)
_cell_measurement_reflns_used    2263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      61.0430
_cell_measurement_theta_min      4.7930
_cell_volume                     2936.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8576
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        62.144
_diffrn_reflns_theta_max         62.144
_diffrn_reflns_theta_min         3.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.05
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       cube
_exptl_crystal_F_000             1298.0
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0586
_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)+(0.1033P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3263
_reflns_number_total             4517
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01244k3.cif
_cod_data_source_block           10cCu
_cod_depositor_comments
'Adding full bibliography for 7704600--7704605.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7704604
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Cu1 Cu 0.500000 0.500000 0.500000 0.0391(2) Uani 1 2 d S . P . .
C1 C 0.7718(3) 0.4744(2) 0.4732(2) 0.0471(8) Uani 1 1 d . . . . .
S1 S 0.84471(9) 0.49603(6) 0.58068(7) 0.0582(3) Uani 1 1 d . . . . .
C2 C 0.9122(3) 0.5789(2) 0.5449(3) 0.0527(9) Uani 1 1 d . . . . .
C3 C 0.9937(4) 0.6341(3) 0.5939(3) 0.0701(11) Uani 1 1 d . . . . .
H3 H 1.020769 0.629039 0.653403 0.084 Uiso 1 1 calc R U . . .
C4 C 1.0335(4) 0.6965(3) 0.5519(4) 0.0723(13) Uani 1 1 d . . . . .
H4 H 1.087013 0.735133 0.583299 0.087 Uiso 1 1 calc R U . . .
C5 C 0.9943(4) 0.7022(3) 0.4633(3) 0.0686(12) Uani 1 1 d . . . . .
H5 H 1.022281 0.744925 0.436060 0.082 Uiso 1 1 calc R U . . .
C6 C 0.9154(3) 0.6467(2) 0.4145(3) 0.0618(10) Uani 1 1 d . . . . .
H6 H 0.890730 0.650944 0.354921 0.074 Uiso 1 1 calc R U . . .
C7 C 0.8732(3) 0.5838(2) 0.4565(2) 0.0508(9) Uani 1 1 d . . . . .
N1 N 0.7919(3) 0.52299(19) 0.4155(2) 0.0522(8) Uani 1 1 d . . . . .
N2 N 0.6874(3) 0.41203(18) 0.4526(2) 0.0524(7) Uani 1 1 d . . . . .
C81_1 C 0.6301(3) 0.3982(2) 0.3618(2) 0.0535(9) Uani 1 1 d . . . . .
H8A_1 H 0.594633 0.343934 0.354263 0.064 Uiso 1 1 calc R U . . .
H8B_1 H 0.690767 0.400247 0.330709 0.064 Uiso 1 1 calc R U . . .
C9_1 C 0.5345(3) 0.4597(2) 0.3248(2) 0.0478(8) Uani 1 1 d . . . . .
C10_1 C 0.4888(4) 0.4877(3) 0.2439(2) 0.0597(11) Uani 1 1 d . . . . .
H10_1 H 0.511059 0.472043 0.195212 0.072 Uiso 1 1 calc R U . . .
N3_1 N 0.4743(3) 0.49908(16) 0.37412(19) 0.0457(7) Uani 1 1 d . . . . .
N4_1 N 0.3953(3) 0.5502(2) 0.32759(19) 0.0579(8) Uani 1 1 d . . . . .
N5_1 N 0.4046(3) 0.5427(2) 0.24826(19) 0.0607(8) Uani 1 1 d . . . . .
C11_1 C 0.3286(5) 0.5927(4) 0.1782(3) 0.0891(15) Uani 1 1 d . . . . .
H11B_1 H 0.284254 0.557061 0.132387 0.107 Uiso 1 1 calc R U . . .
H11A_1 H 0.379771 0.627750 0.154957 0.107 Uiso 1 1 calc R U . . .
C12_1 C 0.2426(5) 0.6437(3) 0.2083(3) 0.0775(13) Uani 1 1 d . . . . .
C13_1 C 0.1280(6) 0.6226(5) 0.2017(5) 0.121(2) Uani 1 1 d . . . . .
H13_1 H 0.098431 0.573138 0.176136 0.145 Uiso 1 1 calc R U . . .
C14_1 C 0.0525(10) 0.6737(10) 0.2324(9) 0.201(7) Uani 1 1 d . . . . .
H14_1 H -0.027619 0.659658 0.225732 0.242 Uiso 1 1 calc R U . . .
C15_1 C 0.0989(15) 0.7452(9) 0.2725(8) 0.196(8) Uani 1 1 d . . . . .
H15_1 H 0.048891 0.778980 0.293648 0.235 Uiso 1 1 calc R U . . .
C16_1 C 0.2180(12) 0.7691(5) 0.2830(5) 0.151(4) Uani 1 1 d . . . . .
H16_1 H 0.248824 0.817307 0.311067 0.182 Uiso 1 1 calc R U . . .
C17_1 C 0.2870(6) 0.7177(4) 0.2496(3) 0.0977(17) Uani 1 1 d . . . . .
H17_1 H 0.366568 0.732202 0.254407 0.117 Uiso 1 1 calc R U . . .
C8_2 C 0.6907(3) 0.3433(2) 0.5106(3) 0.0528(9) Uani 1 1 d . . . . .
H8A_2 H 0.738222 0.357816 0.568083 0.063 Uiso 1 1 calc R U . . .
H8B_2 H 0.728644 0.296668 0.491675 0.063 Uiso 1 1 calc R U . . .
C9_2 C 0.5663(3) 0.3212(2) 0.5120(2) 0.0454(8) Uani 1 1 d . . . . .
C10_2 C 0.5145(3) 0.2490(2) 0.5230(3) 0.0492(9) Uani 1 1 d . . . . .
H10_2 H 0.550514 0.197611 0.530047 0.059 Uiso 1 1 calc R U . . .
N3_2 N 0.4802(2) 0.37900(17) 0.50407(17) 0.0430(7) Uani 1 1 d . . . . .
N4_2 N 0.3785(3) 0.34686(17) 0.51039(18) 0.0462(7) Uani 1 1 d . . . . .
N5_2 N 0.4007(3) 0.26700(17) 0.52144(19) 0.0483(7) Uani 1 1 d . . . . .
C11_2 C 0.3056(3) 0.2128(2) 0.5343(2) 0.0569(10) Uani 1 1 d . . . . .
H11A_2 H 0.317399 0.158543 0.513712 0.068 Uiso 1 1 calc R U . . .
H11B_2 H 0.228082 0.232630 0.499774 0.068 Uiso 1 1 calc R U . . .
C12_2 C 0.3024(3) 0.2064(2) 0.6259(3) 0.0547(9) Uani 1 1 d . . . . .
C13_2 C 0.3547(4) 0.2625(3) 0.6887(3) 0.0709(12) Uani 1 1 d . . . . .
H13_2 H 0.400417 0.305164 0.676258 0.085 Uiso 1 1 calc R U . . .
C14_2 C 0.3396(5) 0.2557(4) 0.7695(3) 0.0927(17) Uani 1 1 d . . . . .
H14_2 H 0.373756 0.294603 0.811048 0.111 Uiso 1 1 calc R U . . .
C15_2 C 0.2746(5) 0.1922(5) 0.7898(4) 0.0966(18) Uani 1 1 d . . . . .
H15_2 H 0.265835 0.187329 0.844940 0.116 Uiso 1 1 calc R U . . .
C16_2 C 0.2231(6) 0.1365(4) 0.7281(4) 0.0946(16) Uani 1 1 d . . . . .
H16_2 H 0.178264 0.093563 0.741065 0.114 Uiso 1 1 calc R U . . .
C17_2 C 0.2368(4) 0.1430(3) 0.6474(3) 0.0763(13) Uani 1 1 d . . . . .
H17_2 H 0.201409 0.104245 0.606132 0.092 Uiso 1 1 calc R U . . .
Si1 Si 0.500000 0.000000 0.500000 0.0568(4) Uani 1 2 d S . P . .
F1 F 0.3737(3) 0.01416(19) 0.5286(2) 0.0979(9) Uani 1 1 d . . . . .
F2 F 0.4588(3) 0.07510(14) 0.42685(15) 0.0802(8) Uani 1 1 d . . . . .
F3 F 0.4330(3) -0.06746(15) 0.42441(17) 0.0966(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 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.12117558.v1 2020
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
N3_1 Cu1 N3_1 180.0 . 3_666 ?
N3_1 Cu1 N3_2 92.33(11) . . ?
N3_1 Cu1 N3_2 87.67(11) 3_666 . ?
N3_1 Cu1 N3_2 87.67(11) . 3_666 ?
N3_1 Cu1 N3_2 92.33(11) 3_666 3_666 ?
N3_2 Cu1 N3_2 180.0 . 3_666 ?
N1 C1 N2 122.1(3) . . ?
N1 C1 S1 117.5(3) . . ?
N2 C1 S1 120.1(3) . . ?
C2 S1 C1 87.86(18) . . ?
C7 C2 C3 122.1(4) . . ?
C7 C2 S1 110.1(3) . . ?
C3 C2 S1 127.8(3) . . ?
C4 C3 C2 117.9(4) . . ?
C3 C4 C5 120.4(4) . . ?
C6 C5 C4 121.8(4) . . ?
C5 C6 C7 118.3(4) . . ?
C2 C7 C6 119.4(4) . . ?
C2 C7 N1 115.7(3) . . ?
C6 C7 N1 124.8(4) . . ?
C1 N1 C7 108.9(3) . . ?
C1 N2 C81_1 116.8(3) . . ?
C1 N2 C8_2 121.4(3) . . ?
C81_1 N2 C8_2 117.0(3) . . ?
N2 C81_1 C9_1 112.4(3) . . ?
C10_1 C9_1 N3_1 106.5(3) . . ?
C10_1 C9_1 C81_1 131.8(3) . . ?
N3_1 C9_1 C81_1 121.7(3) . . ?
N5_1 C10_1 C9_1 105.7(3) . . ?
N4_1 N3_1 C9_1 110.6(3) . . ?
N4_1 N3_1 Cu1 118.0(2) . . ?
C9_1 N3_1 Cu1 131.0(2) . . ?
N3_1 N4_1 N5_1 105.6(3) . . ?
N4_1 N5_1 C10_1 111.6(3) . . ?
N4_1 N5_1 C11_1 120.3(3) . . ?
C10_1 N5_1 C11_1 128.1(3) . . ?
N5_1 C11_1 C12_1 111.7(4) . . ?
C13_1 C12_1 C17_1 118.7(6) . . ?
C13_1 C12_1 C11_1 124.4(6) . . ?
C17_1 C12_1 C11_1 116.8(5) . . ?
C12_1 C13_1 C14_1 121.1(9) . . ?
C15_1 C14_1 C13_1 118.6(12) . . ?
C14_1 C15_1 C16_1 122.6(12) . . ?
C17_1 C16_1 C15_1 116.2(11) . . ?
C16_1 C17_1 C12_1 122.7(8) . . ?
N2 C8_2 C9_2 110.1(3) . . ?
N3_2 C9_2 C10_2 106.4(3) . . ?
N3_2 C9_2 C8_2 121.1(3) . . ?
C10_2 C9_2 C8_2 132.5(3) . . ?
N5_2 C10_2 C9_2 105.7(3) . . ?
N4_2 N3_2 C9_2 111.2(3) . . ?
N4_2 N3_2 Cu1 120.8(2) . . ?
C9_2 N3_2 Cu1 127.5(2) . . ?
N3_2 N4_2 N5_2 105.1(3) . . ?
N4_2 N5_2 C10_2 111.7(3) . . ?
N4_2 N5_2 C11_2 119.1(3) . . ?
C10_2 N5_2 C11_2 129.1(3) . . ?
N5_2 C11_2 C12_2 114.0(3) . . ?
C13_2 C12_2 C17_2 118.0(4) . . ?
C13_2 C12_2 C11_2 124.0(3) . . ?
C17_2 C12_2 C11_2 117.8(4) . . ?
C14_2 C13_2 C12_2 120.4(5) . . ?
C13_2 C14_2 C15_2 120.7(5) . . ?
C16_2 C15_2 C14_2 119.2(5) . . ?
C15_2 C16_2 C17_2 120.5(5) . . ?
C16_2 C17_2 C12_2 121.2(5) . . ?
F1 Si1 F1 180.0 3_656 . ?
F1 Si1 F3 88.15(18) 3_656 . ?
F1 Si1 F3 91.85(18) . . ?
F1 Si1 F3 91.85(18) 3_656 3_656 ?
F1 Si1 F3 88.15(18) . 3_656 ?
F3 Si1 F3 180.0 . 3_656 ?
F1 Si1 F2 90.23(14) 3_656 . ?
F1 Si1 F2 89.77(14) . . ?
F3 Si1 F2 89.03(13) . . ?
F3 Si1 F2 90.97(13) 3_656 . ?
F1 Si1 F2 89.77(14) 3_656 3_656 ?
F1 Si1 F2 90.22(14) . 3_656 ?
F3 Si1 F2 90.97(13) . 3_656 ?
F3 Si1 F2 89.03(13) 3_656 3_656 ?
F2 Si1 F2 180.0 . 3_656 ?
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
Cu1 N3_1 1.977(3) . ?
Cu1 N3_1 1.977(3) 3_666 ?
Cu1 N3_2 1.995(3) . ?
Cu1 N3_2 1.995(3) 3_666 ?
C1 N1 1.297(5) . ?
C1 N2 1.385(5) . ?
C1 S1 1.746(4) . ?
S1 C2 1.740(4) . ?
C2 C7 1.379(5) . ?
C2 C3 1.385(6) . ?
C3 C4 1.374(7) . ?
C4 C5 1.384(7) . ?
C5 C6 1.370(6) . ?
C6 C7 1.395(5) . ?
C7 N1 1.401(5) . ?
N2 C81_1 1.454(5) . ?
N2 C8_2 1.459(5) . ?
C81_1 C9_1 1.491(5) . ?
C9_1 C10_1 1.349(5) . ?
C9_1 N3_1 1.358(4) . ?
C10_1 N5_1 1.340(5) . ?
N3_1 N4_1 1.310(4) . ?
N4_1 N5_1 1.324(4) . ?
N5_1 C11_1 1.475(5) . ?
C11_1 C12_1 1.480(7) . ?
C12_1 C13_1 1.341(8) . ?
C12_1 C17_1 1.409(8) . ?
C13_1 C14_1 1.394(14) . ?
C14_1 C15_1 1.372(19) . ?
C15_1 C16_1 1.393(17) . ?
C16_1 C17_1 1.368(10) . ?
C8_2 C9_2 1.486(5) . ?
C9_2 N3_2 1.352(4) . ?
C9_2 C10_2 1.359(5) . ?
C10_2 N5_2 1.339(4) . ?
N3_2 N4_2 1.315(4) . ?
N4_2 N5_2 1.333(4) . ?
N5_2 C11_2 1.470(5) . ?
C11_2 C12_2 1.497(5) . ?
C12_2 C13_2 1.379(6) . ?
C12_2 C17_2 1.385(6) . ?
C13_2 C14_2 1.372(7) . ?
C14_2 C15_2 1.373(8) . ?
C15_2 C16_2 1.362(8) . ?
C16_2 C17_2 1.363(7) . ?
Si1 F1 1.663(3) 3_656 ?
Si1 F1 1.663(3) . ?
Si1 F3 1.670(3) . ?
Si1 F3 1.670(3) 3_656 ?
Si1 F2 1.681(2) . ?
Si1 F2 1.681(2) 3_656 ?
