#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:17:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179370 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/67/4326707.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_4326707
loop_
_publ_author_name
'Juan Xiao'
'Bao-Yu Liu'
'Gang Wei'
'Xiao-Chun Huang'
_publ_section_title
;
 Solvent Induced Diverse Dimensional Coordination Assemblies of Cupric
 Benzotriazole-5-carboxylate: Syntheses, Crystal Structures, and Magnetic
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11032
_journal_page_last               11038
_journal_paper_doi               10.1021/ic201571n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '{Cu (C7H3N3O2) 3.5(H2O)}8, 16(H2O)'
_chemical_formula_sum            'C56 H112 Cu8 N24 O60'
_chemical_formula_weight         2590.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   28.4502(18)
_cell_length_b                   28.4502(18)
_cell_length_c                   7.1490(9)
_cell_measurement_reflns_used    1468
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.01
_cell_volume                     5786.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16806
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       column
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1468
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0997P)²+86.0169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.2106
_reflns_number_gt                1351
_reflns_number_total             1468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201571n_si_001_2.cif
_cod_data_source_block           2
_cod_database_code               4326707
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.18245(3) 0.18245(3) 0.0000 0.0331(5) Uani 1 4 d SU . .
Cu2 Cu 0.27008(5) 0.0000 0.0000 0.0326(5) Uani 1 4 d SU . .
N1 N 0.2705(2) 0.0698(2) 0.0000 0.0339(16) Uani 1 2 d SU D .
N2 N 0.2291(2) 0.0924(2) 0.0000 0.0321(15) Uani 1 2 d SU . .
N3 N 0.2368(2) 0.1379(2) 0.0000 0.0292(15) Uani 1 2 d SU D .
C1 C 0.3543(3) 0.0973(3) 0.0000 0.043(2) Uani 1 2 d SU . .
H1A H 0.3686 0.0679 0.0000 0.052 Uiso 1 2 calc SR . .
C2 C 0.3806(3) 0.1381(3) 0.0000 0.039(2) Uani 1 2 d SU . .
H2A H 0.4132 0.1359 0.0000 0.047 Uiso 1 2 calc SR . .
C3 C 0.3592(3) 0.1833(3) 0.0000 0.0282(17) Uani 1 2 d SU . .
C4 C 0.3107(3) 0.1870(3) 0.0000 0.0263(16) Uani 1 2 d SU D .
H4A H 0.2960 0.2162 0.0000 0.032 Uiso 1 2 calc SR . .
C5 C 0.2845(3) 0.1459(3) 0.0000 0.0234(15) Uani 1 2 d SU . .
C6 C 0.3052(3) 0.1018(3) 0.0000 0.0301(17) Uani 1 2 d SU D .
C7 C 0.3898(3) 0.2267(3) 0.0000 0.0275(16) Uani 1 2 d SU . .
O1 O 0.4332(2) 0.2218(2) 0.0000 0.0406(15) Uani 1 2 d SU . .
O1W O 0.4307(5) 0.0000 -0.192(2) 0.069(3) Uani 0.50 2 d SPU A 1
H1WA H 0.4447 -0.0243 -0.2336 0.083 Uiso 0.50 1 d PR A 1
O1W' O 0.4270(5) 0.0000 -0.405(2) 0.069(3) Uani 0.50 2 d SPU . 2
H1WB H 0.4519 0.0000 -0.4713 0.083 Uiso 0.50 2 d SPR . 2
H1WC H 0.4355 0.0000 -0.2916 0.083 Uiso 0.50 2 d SPR . 2
O2 O 0.3698(2) 0.2655(2) 0.0000 0.0450(16) Uani 1 2 d SU . .
O2W' O 0.4167(16) 0.3488(16) -0.125(8) 0.081(7) Uani 0.17 1 d PU . 1
H2WC H 0.4280 0.3451 -0.2344 0.097 Uiso 0.17 1 d PR . 1
H2WD H 0.4037 0.3236 -0.0889 0.097 Uiso 0.17 1 d PR . 1
O2W O 0.4205(13) 0.3470(13) 0.0000 0.081(7) Uani 0.33 2 d SPU B 2
H2WA H 0.4279 0.3181 0.0000 0.097 Uiso 0.33 2 d SPR B 2
H2WB H 0.4460 0.3627 0.0000 0.097 Uiso 0.33 2 d SPR B 2
O3 O 0.3314(5) 0.0000 -0.312(2) 0.048(3) Uani 0.50 2 d SPU C 1
H3A H 0.3486 0.0236 -0.2881 0.057 Uiso 0.50 1 d PR C 1
O3' O 0.3193(5) 0.0000 -0.206(2) 0.053(4) Uani 0.50 2 d SPU D 2
H3'B H 0.3231 0.0274 -0.2509 0.064 Uiso 0.50 1 d PR D 2
O3W O 0.4304(16) 0.3343(16) -0.095(8) 0.081(7) Uani 0.17 1 d PU . 3
H3WA H 0.4222 0.3627 -0.1132 0.097 Uiso 0.17 1 d PR . 3
H3WB H 0.4268 0.3185 -0.1947 0.097 Uiso 0.17 1 d PR . 3
O4 O 0.2209(10) 0.0000 0.269(3) 0.083(5) Uani 0.50 2 d SPU D 1
H4B H 0.2036 -0.0243 0.2717 0.100 Uiso 0.50 1 d PR D 1
O4' O 0.2134(10) 0.0000 0.199(3) 0.083(5) Uani 0.50 2 d SPU D 2
H4'A H 0.2071 0.0254 0.2569 0.100 Uiso 0.50 1 d PR D 2
O5 O 0.1314(6) 0.1314(6) 0.0000 0.068(6) Uani 0.50 4 d SPU E 1
H5A H 0.1141 0.1340 -0.0963 0.081 Uiso 0.25 1 d PR E 1
O5' O 0.1328(8) 0.1328(8) 0.140(5) 0.067(8) Uani 0.25 2 d SPU E 2
H5'A H 0.1478 0.1083 0.1835 0.081 Uiso 0.25 1 d PR E 2
O6 O 0.2052(2) 0.2052(2) 0.2632(12) 0.071(2) Uani 1 2 d SU E .
H6A H 0.2160 0.1815 0.3235 0.085 Uiso 1 1 d R . .
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'
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
N3 Cu1 N3 168.7(4) . 7
N3 Cu1 O5 95.64(19) . .
N3 Cu1 O5 95.64(19) 7 .
N3 Cu1 O6 87.54(8) . .
N3 Cu1 O6 87.54(8) 7 .
O5 Cu1 O6 115.9(3) . .
N3 Cu1 O6 87.54(8) . 18
N3 Cu1 O6 87.54(8) 7 18
O5 Cu1 O6 115.9(3) . 18
O6 Cu1 O6 128.2(5) . 18
N3 Cu1 O5' 95.04(17) . 18
N3 Cu1 O5' 95.04(17) 7 18
O5 Cu1 O5' 26.6(9) . 18
O6 Cu1 O5' 142.5(9) . 18
O6 Cu1 O5' 89.3(10) 18 18
N3 Cu1 O5' 95.04(17) . .
N3 Cu1 O5' 95.04(17) 7 .
O5 Cu1 O5' 26.6(9) . .
O6 Cu1 O5' 89.3(10) . .
O6 Cu1 O5' 142.5(9) 18 .
O5' Cu1 O5' 53.3(18) 18 .
N1 Cu2 N1 179.4(4) 21 .
N1 Cu2 O3' 89.79(13) 21 18
N1 Cu2 O3' 89.79(13) . 18
N1 Cu2 O3' 89.79(13) 21 .
N1 Cu2 O3' 89.79(13) . .
O3' Cu2 O3' 92.9(9) 18 .
N1 Cu2 O4' 90.23(15) 21 18
N1 Cu2 O4' 90.23(15) . 18
O3' Cu2 O4' 175.0(8) 18 18
O3' Cu2 O4' 92.0(8) . 18
N1 Cu2 O4' 90.23(15) 21 .
N1 Cu2 O4' 90.23(15) . .
O3' Cu2 O4' 92.0(8) 18 .
O3' Cu2 O4' 175.0(8) . .
O4' Cu2 O4' 83.0(13) 18 .
N1 Cu2 O4 90.18(11) 21 18
N1 Cu2 O4 90.18(11) . 18
O3' Cu2 O4 172.5(8) 18 18
O3' Cu2 O4 79.5(8) . 18
O4' Cu2 O4 12.5(11) 18 18
O4' Cu2 O4 95.5(6) . 18
N1 Cu2 O4 90.18(11) 21 .
N1 Cu2 O4 90.18(11) . .
O3' Cu2 O4 79.5(8) 18 .
O3' Cu2 O4 172.5(8) . .
O4' Cu2 O4 95.5(6) 18 .
O4' Cu2 O4 12.5(11) . .
O4 Cu2 O4 108.0(13) 18 .
N2 N1 C6 108.8(6) . .
N2 N1 Cu2 118.2(5) . .
C6 N1 Cu2 133.0(5) . .
N3 N2 N1 109.0(6) . .
N2 N3 C5 109.1(6) . .
N2 N3 Cu1 119.8(5) . .
C5 N3 Cu1 131.1(5) . .
C2 C1 C6 117.6(7) . .
C2 C1 H1A 121.2 . .
C6 C1 H1A 121.2 . .
C1 C2 C3 121.8(8) . .
C1 C2 H2A 119.1 . .
C3 C2 H2A 119.1 . .
C4 C3 C2 119.7(7) . .
C4 C3 C7 120.7(7) . .
C2 C3 C7 119.5(7) . .
C3 C4 C5 118.0(7) . .
C3 C4 H4A 121.0 . .
C5 C4 H4A 121.0 . .
N3 C5 C6 105.6(7) . .
N3 C5 C4 132.0(7) . .
C6 C5 C4 122.5(7) . .
N1 C6 C5 107.6(7) . .
N1 C6 C1 132.1(7) . .
C5 C6 C1 120.4(7) . .
O2 C7 O1 123.8(8) . .
O2 C7 C3 117.5(7) . .
O1 C7 C3 118.7(7) . .
H1WA O1W H1WC 64.5 . .
O1W' O1W' H1WB 56.4 18_554 .
O1W' O1W' H1WC 163.4 18_554 .
H1WB O1W' H1WC 107.0 . .
O2W' O2W' H2WC 156.5 18 .
O2W' O2W' H2WD 72.1 18 .
H2WC O2W' H2WD 110.0 . .
O2W' O2W' H2WA 46.1 18 .
H2WC O2W' H2WA 117.3 . .
H2WD O2W' H2WA 47.3 . .
O2W' O2W' H2WB 45.8 18 .
H2WC O2W' H2WB 115.7 . .
H2WD O2W' H2WB 109.2 . .
H2WA O2W' H2WB 64.2 . .
O2W' O2W' H3WA 78.4 18 .
H2WC O2W' H3WA 99.2 . .
H2WD O2W' H3WA 150.0 . .
H2WA O2W' H3WA 112.9 . .
H2WB O2W' H3WA 49.2 . .
O2W' O2W' H3WB 118.6 18 .
H2WC O2W' H3WB 49.7 . .
H2WD O2W' H3WB 64.1 . .
H2WA O2W' H3WB 72.5 . .
H2WB O2W' H3WB 114.2 . .
H3WA O2W' H3WB 139.1 . .
H2WD O2W H2WA 59.4 . .
H2WD O2W H2WB 136.9 . .
H2WA O2W H2WB 107.4 . .
H2WD O2W H3WA 78.3 . .
H2WA O2W H3WA 117.0 . .
H2WB O2W H3WA 72.7 . .
H3A O3 H3'B 52.0 . .
Cu2 O3' H3A 144.9 . .
Cu2 O3' H3'B 111.0 . .
H3A O3' H3'B 39.5 . .
O3W O3W H2WC 162.5 18 .
O3W O3W H2WD 87.0 18 .
H2WC O3W H2WD 95.7 . .
O3W O3W H2WA 34.6 18 .
H2WC O3W H2WA 160.7 . .
H2WD O3W H2WA 70.4 . .
O3W O3W H2WB 53.6 18 .
H2WC O3W H2WB 112.6 . .
H2WD O3W H2WB 126.1 . .
H2WA O3W H2WB 86.7 . .
O3W O3W H3WA 98.8 18 .
H2WC O3W H3WA 63.7 . .
H2WD O3W H3WA 96.1 . .
H2WA O3W H3WA 129.4 . .
H2WB O3W H3WA 61.8 . .
O3W O3W H3WB 147.0 18 .
H2WC O3W H3WB 49.3 . .
H2WD O3W H3WB 74.6 . .
H2WA O3W H3WB 112.4 . .
H2WB O3W H3WB 156.9 . .
H3WA O3W H3WB 110.0 . .
Cu2 O4 H4B 111.0 . .
Cu2 O4 H4'A 101.2 . .
H4B O4 H4'A 115.9 . .
Cu2 O4' H4B 127.4 . .
Cu2 O4' H4'A 118.7 . .
H4B O4' H4'A 107.9 . .
Cu1 O5 H5A 110.3 . .
Cu1 O5' H5'A 110.9 . .
Cu1 O6 H6A 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N3 1.999(6) .
Cu1 N3 1.999(6) 7
Cu1 O5 2.05(2) .
Cu1 O6 2.092(8) .
Cu1 O6 2.092(8) 18
Cu1 O5' 2.23(3) 18
Cu1 O5' 2.23(3) .
Cu2 N1 1.987(7) 21
Cu2 N1 1.987(7) .
Cu2 O3' 2.034(17) 18
Cu2 O3' 2.034(17) .
Cu2 O4' 2.15(3) 18
Cu2 O4' 2.15(3) .
Cu2 O4 2.38(3) 18
Cu2 O4 2.38(3) .
N1 N2 1.340(9) .
N1 C6 1.343(10) .
N2 N3 1.314(9) .
N3 C5 1.378(10) .
C1 C2 1.382(12) .
C1 C6 1.402(11) .
C1 H1A 0.9300 .
C2 C3 1.423(11) .
C2 H2A 0.9300 .
C3 C4 1.386(11) .
C3 C7 1.512(11) .
C4 C5 1.385(11) .
C4 H4A 0.9300 .
C5 C6 1.385(10) .
C7 O2 1.240(10) .
C7 O1 1.243(10) .
O1W H1WA 0.8500 .
O1W H1WC 0.7238 .
O1W' O1W' 1.35(3) 18_554
O1W' H1WB 0.8502 .
O1W' H1WC 0.8500 .
O2W' O2W' 1.79(11) 18
O2W' H2WC 0.8500 .
O2W' H2WD 0.8497 .
O2W' H2WA 1.2922 .
O2W' H2WB 1.2848 .
O2W' H3WA 0.4329 .
O2W' H3WB 1.0363 .
O2W H2WD 1.0386 .
O2W H2WA 0.8502 .
O2W H2WB 0.8499 .
O2W H3WA 0.9252 .
O3 H3A 0.8497 .
O3 H3'B 0.9248 .
O3' H3A 1.2199 .
O3' H3'B 0.8501 .
O3W O3W 1.36(11) 18
O3W H2WC 1.0453 .
O3W H2WD 0.8220 .
O3W H2WA 0.8250 .
O3W H2WB 1.1433 .
O3W H3WA 0.8501 .
O3W H3WB 0.8500 .
O4 H4B 0.8498 .
O4 H4'A 0.8274 .
O4' H4B 0.9077 .
O4' H4'A 0.8501 .
O5 H5A 0.8488 .
O5' H5'A 0.8737 .
O6 H6A 0.8582 .
