#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:45:54 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/88/7048861.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_7048861
loop_
_publ_author_name
'Gusev, Alexey'
'Nemec, Ivan'
'Herchel, Radovan'
'Shul'gin, Victor'
'Ryush, Irina'
'Kiskin, Michail'
'Efimov, Nickolay'
'Ugolkova, Elena'
'Minin, Vadim'
'Lyssenko, Konstantin'
'Eremenko, Igor'
'Linert, Wolfgang'
_publ_section_title
;
 Copper(ii) self-assembled clusters of
 bis((pyridin-2-yl)-1,2,4-triazol-3-yl)alkanes. Unusual rearrangement of
 ligands under reaction conditions.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3052
_journal_page_last               3060
_journal_paper_doi               10.1039/c8dt04816a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C16 H14 Cl2 Cu N8 O8'
_chemical_formula_weight         580.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-14 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.745(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0990(11)
_cell_length_b                   11.6970(7)
_cell_length_c                   14.5274(12)
_cell_measurement_reflns_used    5455
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.2377
_cell_measurement_theta_min      3.0239
_cell_volume                     2052.8(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXLS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6730
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0250
_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)+(0.0416P)²+1.2874P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1595
_reflns_number_total             1819
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04816a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7048860--7048863.cif.'
_cod_database_code               7048861
_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   0.641
_shelx_estimated_absorpt_t_max   0.749
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
C1 C 0.59145(17) 0.02357(18) 0.37296(16) 0.0189(5) Uani 1 1 d . . .
H1 H 0.5750 -0.0162 0.3119 0.023 Uiso 1 1 calc R U .
C2 C 0.63070(18) -0.03768(19) 0.46117(17) 0.0214(5) Uani 1 1 d . . .
H2 H 0.6387 -0.1183 0.4601 0.026 Uiso 1 1 calc R U .
C3 C 0.65808(18) 0.0191(2) 0.55062(17) 0.0219(5) Uani 1 1 d . . .
H3 H 0.6827 -0.0219 0.6118 0.026 Uiso 1 1 calc R U .
C4 C 0.60827(17) 0.19236(18) 0.45888(16) 0.0159(4) Uani 1 1 d . . .
C5 C 0.59668(16) 0.31660(18) 0.44908(15) 0.0152(4) Uani 1 1 d . . .
C6 C 0.64903(18) 0.1371(2) 0.54968(16) 0.0206(5) Uani 1 1 d . . .
H6 H 0.6704 0.1790 0.6103 0.025 Uiso 1 1 calc R U .
C7 C 0.54463(16) 0.47424(17) 0.37069(15) 0.0158(4) Uani 1 1 d . . .
C8 C 0.48869(18) 0.56576(17) 0.29848(15) 0.0167(5) Uani 1 1 d . . .
H8A H 0.5121 0.6405 0.3320 0.020 Uiso 1 1 calc R U .
H8B H 0.4079 0.5588 0.2801 0.020 Uiso 1 1 calc R U .
O1 O 0.27317(15) 0.40371(14) 0.29344(12) 0.0325(4) Uani 1 1 d . . .
O2 O 0.35756(14) 0.29208(14) 0.43680(12) 0.0277(4) Uani 1 1 d . . .
O3 O 0.32405(13) 0.21335(14) 0.27855(12) 0.0251(4) Uani 1 1 d . . .
O4 O 0.17613(17) 0.25105(17) 0.32634(17) 0.0476(6) Uani 1 1 d . . .
N1 N 0.57564(14) 0.13770(14) 0.37029(13) 0.0148(4) Uani 1 1 d . . .
N2 N 0.54624(14) 0.36103(14) 0.35603(13) 0.0143(4) Uani 1 1 d . . .
N3 N 0.59605(14) 0.49202(15) 0.46877(13) 0.0179(4) Uani 1 1 d . . .
H3A H 0.6072 0.5602 0.4965 0.021 Uiso 1 1 calc R U .
N4 N 0.62926(15) 0.39286(16) 0.52095(13) 0.0189(4) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.24447(3) 0.2500 0.01446(13) Uani 1 2 d S T P
Cl Cl 0.28156(4) 0.29033(4) 0.33299(4) 0.01863(15) 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 0.0030 0.0020 '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'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 '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
N1 C1 C2 122.5(2) . .
C3 C2 C1 119.5(2) . .
C2 C3 C6 118.8(2) . .
N1 C4 C6 123.57(19) . .
N1 C4 C5 113.28(17) . .
C6 C4 C5 123.15(19) . .
N4 C5 N2 114.53(18) . .
N4 C5 C4 127.46(19) . .
N2 C5 C4 118.00(17) . .
C4 C6 C3 118.5(2) . .
N3 C7 N2 106.87(18) . .
N3 C7 C8 123.43(18) . .
N2 C7 C8 129.42(19) . .
C7 C8 C8 115.39(16) . 2_655
C1 N1 C4 116.91(18) . .
C1 N1 Cu1 129.90(15) . .
C4 N1 Cu1 113.09(13) . .
C7 N2 C5 104.54(17) . .
C7 N2 Cu1 142.00(15) . .
C5 N2 Cu1 113.45(13) . .
C7 N3 N4 112.46(17) . .
C5 N4 N3 101.55(17) . .
N2 Cu1 N2 92.35(10) 2_655 .
N2 Cu1 N1 169.59(7) 2_655 .
N2 Cu1 N1 81.65(7) . .
N2 Cu1 N1 81.65(7) 2_655 2_655
N2 Cu1 N1 169.59(7) . 2_655
N1 Cu1 N1 105.49(10) . 2_655
O4 Cl O1 110.47(12) . .
O4 Cl O3 109.32(10) . .
O1 Cl O3 110.09(10) . .
O4 Cl O2 109.45(12) . .
O1 Cl O2 108.62(10) . .
O3 Cl O2 108.85(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.349(3) .
C1 C2 1.382(3) .
C2 C3 1.378(3) .
C3 C6 1.384(3) .
C4 N1 1.350(3) .
C4 C6 1.378(3) .
C4 C5 1.462(3) .
C5 N4 1.313(3) .
C5 N2 1.358(3) .
C7 N3 1.336(3) .
C7 N2 1.343(3) .
C7 C8 1.480(3) .
C8 C8 1.547(4) 2_655
O1 Cl 1.4326(17) .
O2 Cl 1.4509(17) .
O3 Cl 1.4444(16) .
O4 Cl 1.4228(19) .
N1 Cu1 2.0630(17) .
N2 Cu1 1.9690(17) .
N3 N4 1.362(3) .
Cu1 N2 1.9690(17) 2_655
Cu1 N1 2.0631(17) 2_655
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 O2 0.95 2.51 3.301(3) 140.4 5_656
C8 H8A O4 0.99 2.54 3.181(3) 122.6 3
C8 H8B O1 0.99 2.59 3.378(3) 136.6 .
N3 H3A O2 0.88 1.95 2.826(2) 176.0 5_666
N3 H3A Cl 0.88 2.92 3.7116(18) 150.6 5_666
