#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:41:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180444 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/13/7211381.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_7211381
loop_
_publ_author_name
'Białońska, Agata'
'Drabent, Krzysztof'
'Filipowicz, Barbara'
'Siczek, Miłosz'
_publ_section_title
;
 Reversible guest vapour sorption in breathing crystals of a discrete
 ionic binuclear Cu(i) complex
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              9859
_journal_paper_doi               10.1039/c3ce41461b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C36 H28 Cl4 Cu2 N16, 2(Cl O4), 2(C Cl4)'
_chemical_formula_sum            'C38 H28 Cl14 Cu2 N16 O8'
_chemical_formula_weight         1460.14
_chemical_name_systematic
;
bis(μ₂-4-(E)-(4-chlorobenzylidene)amino-4H-1,2,4-triazole)-bis((E)-4-(chlor
obenzylidene)amino-4H-1,2,4-triazole)-di-copper(i) diperchlorate tetrachloromethane 
disolvate
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.971(2)
_cell_length_b                   17.912(3)
_cell_length_c                   22.289(3)
_cell_measurement_reflns_used    838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3419
_cell_measurement_theta_min      2.7494
_cell_volume                     2769.6(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1637
_diffrn_reflns_av_unetI/netI     0.3718
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11580
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.403
_diffrn_reflns_theta_min         2.923
_exptl_absorpt_coefficient_mu    1.508
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       needle
_exptl_crystal_F_000             1456
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.2930
_refine_ls_R_factor_gt           0.1050
_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)+(0.0213P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1847
_reflns_number_total             5417
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce41461b.txt
_cod_data_source_block           1-CCl4
_cod_database_code               7211381
#BEGIN Tags that were not found in dictionaries:
_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.
;
#END Tags that were not found in dictionaries
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
Cu1 Cu 0.4490(2) 0.57501(9) 0.04781(6) 0.0226(4) Uani 1 1 d . .
Cl5 Cl 0.1278(5) 0.12139(19) 0.40603(12) 0.0339(9) Uani 1 1 d . U
Cl15 Cl 0.0636(4) 0.93303(18) 0.45957(11) 0.0255(8) Uani 1 1 d . U
N1 N 0.4313(13) 0.4715(5) 0.0733(3) 0.017(2) Uani 1 1 d . .
N2 N 0.4463(12) 0.4133(5) 0.0337(3) 0.017(2) Uani 1 1 d . U
N3 N 0.3691(13) 0.3675(6) 0.1184(4) 0.023(2) Uani 1 1 d . U
N4 N 0.3287(13) 0.3111(5) 0.1595(3) 0.018(3) Uani 1 1 d . .
N11 N 0.3715(13) 0.6693(5) 0.0805(4) 0.020(3) Uani 1 1 d . .
N12 N 0.3566(14) 0.7351(6) 0.0464(4) 0.028(3) Uani 1 1 d . U
N13 N 0.2891(14) 0.7590(6) 0.1396(4) 0.026(3) Uani 1 1 d . U
N14 N 0.2398(14) 0.8044(5) 0.1861(4) 0.023(3) Uani 1 1 d . .
C1 C 0.3189(16) 0.3337(7) 0.2140(5) 0.021(3) Uani 1 1 d . U
H1A H 0.3397 0.3847 0.2244 0.025 Uiso 1 1 calc R U
C2 C 0.2746(16) 0.2787(7) 0.2600(5) 0.017(3) Uani 1 1 d . U
C3 C 0.2425(16) 0.2040(7) 0.2470(5) 0.024(3) Uani 1 1 d . .
H3A H 0.2505 0.1858 0.2072 0.029 Uiso 1 1 calc R U
C4 C 0.1988(15) 0.1561(7) 0.2920(5) 0.020(3) Uani 1 1 d . .
H4A H 0.1790 0.1046 0.2836 0.024 Uiso 1 1 calc R U
C5 C 0.1837(18) 0.1831(8) 0.3495(5) 0.031(3) Uani 1 1 d . U
C6 C 0.2117(17) 0.2572(7) 0.3635(5) 0.024(3) Uani 1 1 d . .
H6A H 0.2020 0.2749 0.4033 0.029 Uiso 1 1 calc R U
C7 C 0.2546(16) 0.3057(7) 0.3178(4) 0.021(3) Uani 1 1 d . .
H7A H 0.2704 0.3575 0.3260 0.025 Uiso 1 1 calc R U
C8 C 0.3868(16) 0.4421(7) 0.1240(4) 0.020(3) Uani 1 1 d . U
H8A H 0.3696 0.4695 0.1595 0.024 Uiso 1 1 calc R U
C9 C 0.4092(16) 0.3527(7) 0.0622(4) 0.022(3) Uani 1 1 d . U
H9A H 0.4104 0.3040 0.0453 0.026 Uiso 1 1 calc R U
C11 C 0.2327(15) 0.7709(7) 0.2377(4) 0.019(3) Uani 1 1 d . .
H11A H 0.2582 0.7188 0.2409 0.022 Uiso 1 1 calc R U
C12 C 0.1863(16) 0.8123(8) 0.2899(4) 0.025(4) Uani 1 1 d . .
C13 C 0.1452(17) 0.8884(7) 0.2875(5) 0.024(3) Uani 1 1 d . .
H13A H 0.1441 0.9150 0.2506 0.029 Uiso 1 1 calc R U
C14 C 0.1061(15) 0.9247(7) 0.3399(4) 0.021(3) Uani 1 1 d . U
H14A H 0.0754 0.9764 0.3387 0.025 Uiso 1 1 calc R U
C15 C 0.1114(16) 0.8859(7) 0.3945(4) 0.021(2) Uani 1 1 d . U
C16 C 0.1526(16) 0.8112(7) 0.3974(5) 0.019(3) Uani 1 1 d . U
H16A H 0.1548 0.7852 0.4347 0.023 Uiso 1 1 calc R U
C17 C 0.1914(15) 0.7736(8) 0.3451(5) 0.031(4) Uani 1 1 d . .
H17A H 0.2213 0.7219 0.3467 0.037 Uiso 1 1 calc R U
C18 C 0.3280(18) 0.6850(8) 0.1350(5) 0.027(3) Uani 1 1 d . .
H18A H 0.3243 0.6497 0.1667 0.032 Uiso 1 1 calc R U
C19 C 0.3077(17) 0.7874(7) 0.0840(4) 0.027(3) Uani 1 1 d . U
H19A H 0.2881 0.8384 0.0734 0.033 Uiso 1 1 calc R U
Cl1 Cl 0.3238(5) 0.5409(2) 0.28057(13) 0.0332(9) Uani 1 1 d . .
O1 O 0.2115(11) 0.5513(5) 0.2225(3) 0.035(2) Uani 1 1 d . .
O2 O 0.4902(14) 0.4960(6) 0.2711(4) 0.061(3) Uani 1 1 d . .
O3 O 0.3855(13) 0.6114(5) 0.3043(3) 0.046(3) Uani 1 1 d . .
O4 O 0.2096(15) 0.5036(6) 0.3201(4) 0.066(3) Uani 1 1 d . .
C21 C 0.261(2) 0.4108(10) 0.5333(6) 0.064(5) Uani 1 1 d . .
Cl21 Cl 0.0764(8) 0.3470(4) 0.5373(2) 0.123(2) Uani 1 1 d . .
Cl22 Cl 0.2570(7) 0.4780(3) 0.59076(17) 0.0858(17) Uani 1 1 d . .
Cl23 Cl 0.2423(7) 0.4543(3) 0.46320(17) 0.0837(16) Uani 1 1 d . .
Cl24 Cl 0.4808(7) 0.3636(3) 0.54434(19) 0.0855(16) 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'
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'
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_3
N11 Cu1 N1 133.9(3) .
N11 Cu1 N2 112.6(4) 3_665
N1 Cu1 N2 113.4(3) 3_665
C8 N1 N2 106.8(9) .
C8 N1 Cu1 131.4(8) .
N2 N1 Cu1 121.5(6) .
C9 N2 N1 106.7(8) .
C9 N2 Cu1 129.1(8) 3_665
N1 N2 Cu1 123.5(7) 3_665
C9 N3 C8 104.9(9) .
C9 N3 N4 122.7(10) .
C8 N3 N4 132.4(9) .
C1 N4 N3 114.8(9) .
C18 N11 N12 108.1(10) .
C18 N11 Cu1 129.3(9) .
N12 N11 Cu1 122.6(6) .
C19 N12 N11 105.3(8) .
C19 N13 C18 105.0(9) .
C19 N13 N14 121.0(10) .
C18 N13 N14 133.9(9) .
C11 N14 N13 115.0(10) .
N4 C1 C2 118.6(11) .
N4 C1 H1A 120.7 .
C2 C1 H1A 120.7 .
C3 C2 C7 120.0(10) .
C3 C2 C1 122.8(10) .
C7 C2 C1 117.1(11) .
C4 C3 C2 119.5(10) .
C4 C3 H3A 120.3 .
C2 C3 H3A 120.3 .
C3 C4 C5 120.1(11) .
C3 C4 H4A 120.0 .
C5 C4 H4A 120.0 .
C6 C5 C4 121.7(11) .
C6 C5 Cl5 119.0(9) .
C4 C5 Cl5 119.3(10) .
C5 C6 C7 118.2(10) .
C5 C6 H6A 120.9 .
C7 C6 H6A 120.9 .
C6 C7 C2 120.5(11) .
C6 C7 H7A 119.8 .
C2 C7 H7A 119.8 .
N1 C8 N3 110.3(9) .
N1 C8 H8A 124.8 .
N3 C8 H8A 124.8 .
N2 C9 N3 111.3(11) .
N2 C9 H9A 124.3 .
N3 C9 H9A 124.3 .
N14 C11 C12 120.4(11) .
N14 C11 H11A 119.8 .
C12 C11 H11A 119.8 .
C13 C12 C17 120.1(11) .
C13 C12 C11 122.2(10) .
C17 C12 C11 117.6(12) .
C14 C13 C12 118.9(10) .
C14 C13 H13A 120.6 .
C12 C13 H13A 120.6 .
C13 C14 C15 120.6(11) .
C13 C14 H14A 119.7 .
C15 C14 H14A 119.7 .
C16 C15 C14 121.0(10) .
C16 C15 Cl15 119.4(8) .
C14 C15 Cl15 119.6(9) .
C15 C16 C17 119.2(10) .
C15 C16 H16A 120.4 .
C17 C16 H16A 120.4 .
C16 C17 C12 120.2(12) .
C16 C17 H17A 119.9 .
C12 C17 H17A 119.9 .
N11 C18 N13 110.2(10) .
N11 C18 H18A 124.9 .
N13 C18 H18A 124.9 .
N12 C19 N13 111.4(11) .
N12 C19 H19A 124.3 .
N13 C19 H19A 124.3 .
O4 Cl1 O3 111.0(5) .
O4 Cl1 O2 109.8(6) .
O3 Cl1 O2 109.3(6) .
O4 Cl1 O1 109.1(6) .
O3 Cl1 O1 109.5(5) .
O2 Cl1 O1 108.1(5) .
Cl21 C21 Cl23 110.6(9) .
Cl21 C21 Cl24 108.7(10) .
Cl23 C21 Cl24 109.2(7) .
Cl21 C21 Cl22 110.5(7) .
Cl23 C21 Cl22 110.0(10) .
Cl24 C21 Cl22 107.8(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N11 1.936(9) .
Cu1 N1 1.947(9) .
Cu1 N2 2.033(7) 3_665
Cl5 C5 1.748(12) .
Cl15 C15 1.739(10) .
N1 C8 1.310(11) .
N1 N2 1.377(11) .
N2 C9 1.297(13) .
N2 Cu1 2.033(7) 3_665
N3 C9 1.337(11) .
N3 C8 1.346(14) .
N3 N4 1.410(11) .
N4 C1 1.288(11) .
N11 C18 1.312(12) .
N11 N12 1.400(12) .
N12 C19 1.324(13) .
N13 C19 1.357(12) .
N13 C18 1.359(15) .
N13 N14 1.388(11) .
N14 C11 1.301(12) .
C1 C2 1.476(13) .
C1 H1A 0.9500 .
C2 C3 1.383(15) .
C2 C7 1.396(13) .
C3 C4 1.377(14) .
C3 H3A 0.9500 .
C4 C5 1.383(14) .
C4 H4A 0.9500 .
C5 C6 1.373(17) .
C6 C7 1.394(14) .
C6 H6A 0.9500 .
C7 H7A 0.9500 .
C8 H8A 0.9500 .
C9 H9A 0.9500 .
C11 C12 1.445(14) .
C11 H11A 0.9500 .
C12 C13 1.393(16) .
C12 C17 1.408(15) .
C13 C14 1.386(13) .
C13 H13A 0.9500 .
C14 C15 1.399(13) .
C14 H14A 0.9500 .
C15 C16 1.369(15) .
C16 C17 1.396(14) .
C16 H16A 0.9500 .
C17 H17A 0.9500 .
C18 H18A 0.9500 .
C19 H19A 0.9500 .
Cl1 O4 1.411(8) .
Cl1 O3 1.419(9) .
Cl1 O2 1.444(9) .
Cl1 O1 1.457(8) .
C21 Cl21 1.729(17) .
C21 Cl23 1.741(14) .
C21 Cl24 1.747(15) .
C21 Cl22 1.759(16) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C8 N1 N2 C9 0.4(12) . .
Cu1 N1 N2 C9 -173.6(8) . .
C8 N1 N2 Cu1 -170.6(7) . 3_665
Cu1 N1 N2 Cu1 15.4(11) . 3_665
C9 N3 N4 C1 171.0(10) . .
C8 N3 N4 C1 -5.3(17) . .
C18 N11 N12 C19 1.2(12) . .
Cu1 N11 N12 C19 -177.8(8) . .
C19 N13 N14 C11 -177.9(10) . .
C18 N13 N14 C11 2.0(18) . .
N3 N4 C1 C2 179.2(9) . .
N4 C1 C2 C3 -0.2(17) . .
N4 C1 C2 C7 -176.6(11) . .
C7 C2 C3 C4 -2.7(17) . .
C1 C2 C3 C4 -178.9(10) . .
C2 C3 C4 C5 1.2(17) . .
C3 C4 C5 C6 -0.1(19) . .
C3 C4 C5 Cl5 179.9(9) . .
C4 C5 C6 C7 0.5(19) . .
Cl5 C5 C6 C7 -179.5(9) . .
C5 C6 C7 C2 -2.1(18) . .
C3 C2 C7 C6 3.2(18) . .
C1 C2 C7 C6 179.6(10) . .
N2 N1 C8 N3 -1.1(12) . .
Cu1 N1 C8 N3 172.1(8) . .
C9 N3 C8 N1 1.4(13) . .
N4 N3 C8 N1 178.1(10) . .
N1 N2 C9 N3 0.5(12) . .
Cu1 N2 C9 N3 170.8(7) 3_665 .
C8 N3 C9 N2 -1.1(13) . .
N4 N3 C9 N2 -178.3(9) . .
N13 N14 C11 C12 178.9(9) . .
N14 C11 C12 C13 0.9(17) . .
N14 C11 C12 C17 -176.5(11) . .
C17 C12 C13 C14 -1.3(18) . .
C11 C12 C13 C14 -178.6(10) . .
C12 C13 C14 C15 1.2(17) . .
C13 C14 C15 C16 -0.9(18) . .
C13 C14 C15 Cl15 179.5(9) . .
C14 C15 C16 C17 0.5(18) . .
Cl15 C15 C16 C17 -179.8(8) . .
C15 C16 C17 C12 -0.6(17) . .
C13 C12 C17 C16 0.9(18) . .
C11 C12 C17 C16 178.4(10) . .
N12 N11 C18 N13 -1.5(13) . .
Cu1 N11 C18 N13 177.4(8) . .
C19 N13 C18 N11 1.2(14) . .
N14 N13 C18 N11 -178.8(11) . .
N11 N12 C19 N13 -0.5(13) . .
C18 N13 C19 N12 -0.4(13) . .
N14 N13 C19 N12 179.5(10) . .
