#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/07/2230754.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230754
loop_
_publ_author_name
'Dong, Gui-Ying'
'He, Cui-Hong'
'Tong-Fei, Liu'
'Deng, Xiao-Chen'
'Shi, Xiao-Ge'
_publ_section_title
;
 [μ-1,4-Bis(1,2,4-triazol-1-ylmethyl)benzene]bis[aqua(pyridine-2,6-dicarboxylato)copper(II)]
 monohydrate
;
_journal_coeditor_code           JH2295
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m944
_journal_paper_doi               10.1107/S1600536811022756
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Cu2 (C7 H3 N O4)2 (C12 H12 N6) (H2 O)2], H2 O'
_chemical_formula_moiety         'C26 H22 Cu2 N8 O10, H2 O'
_chemical_formula_sum            'C26 H24 Cu2 N8 O11'
_chemical_formula_weight         751.63
_chemical_name_systematic
;
[μ-1,4-Bis(1,2,4-triazol-1-ylmethyl)benzene]bis[aqua(pyridine-2,6-
dicarboxylato)copper(II)] monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.5410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.9017(4)
_cell_length_b                   10.3022(9)
_cell_length_c                   30.178(3)
_cell_measurement_reflns_used    3568
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      3.56
_cell_measurement_theta_min      22.32
_cell_volume                     1521.0(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            7340
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_T_max  0.9012
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.398
_refine_diff_density_min         -0.403
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0469
_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)+(0.1045P)²+1.8845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                2256
_reflns_number_total             2678
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            jh2295.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230754
_cod_database_fobs_code          2230754
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.08344(10) 0.98034(5) 0.149509(16) 0.0318(2) Uani d . 1 1 . .
O O3 -0.1809(6) 0.9403(3) 0.19769(10) 0.0376(7) Uani d . 1 1 . .
O O1 0.3528(6) 0.9508(3) 0.10311(10) 0.0392(7) Uani d . 1 1 . .
N N1 0.1905(7) 0.8071(3) 0.16460(11) 0.0300(8) Uani d . 1 1 . .
C C7 -0.1409(9) 0.8318(4) 0.21771(14) 0.0328(9) Uani d . 1 1 . .
O O4 -0.2555(7) 0.7960(3) 0.25024(11) 0.0469(8) Uani d . 1 1 . .
N N4 -0.0779(7) 1.1422(3) 0.12697(12) 0.0346(8) Uani d . 1 1 . .
C C2 0.3801(9) 0.7519(4) 0.14164(14) 0.0335(9) Uani d . 1 1 . .
C C3 0.4592(10) 0.6261(4) 0.15103(16) 0.0419(11) Uani d . 1 1 . .
H H3 0.5917 0.5859 0.1350 0.050 Uiso calc R 1 1 . .
C C6 0.0697(8) 0.7462(4) 0.19736(13) 0.0309(9) Uani d . 1 1 . .
O O2 0.6818(8) 0.8113(4) 0.08671(12) 0.0565(10) Uani d . 1 1 . .
C C11 -0.1952(9) 1.4310(5) 0.02197(15) 0.0415(11) Uani d . 1 1 . .
C C1 0.4833(9) 0.8436(4) 0.10695(14) 0.0358(10) Uani d . 1 1 . .
C C5 0.1422(10) 0.6216(4) 0.20832(16) 0.0417(11) Uani d . 1 1 . .
H H5 0.0613 0.5787 0.2312 0.050 Uiso calc R 1 1 . .
C C12 -0.0882(11) 1.3819(5) -0.01557(17) 0.0486(12) Uani d . 1 1 . .
H H12 -0.1473 1.3016 -0.0266 0.058 Uiso calc R 1 1 . .
C C4 0.3384(10) 0.5605(5) 0.18465(17) 0.0453(11) Uani d . 1 1 . .
H H4 0.3890 0.4754 0.1914 0.054 Uiso calc R 1 1 . .
O O1W 0.3552(8) 1.0793(4) 0.20033(14) 0.0698(13) Uani d . 1 1 . .
N N2 -0.2780(8) 1.2853(4) 0.08451(13) 0.0439(10) Uani d . 1 1 . .
C C13 -0.1072(11) 1.5492(5) 0.03729(17) 0.0492(12) Uani d . 1 1 . .
H H13 -0.1788 1.5841 0.0625 0.059 Uiso calc R 1 1 . .
C C10 -0.4037(11) 1.3552(6) 0.04620(19) 0.0576(15) Uani d . 1 1 . .
H H10A -0.5411 1.4144 0.0562 0.069 Uiso calc R 1 1 . .
H H10B -0.4942 1.2936 0.0259 0.069 Uiso calc R 1 1 . .
C C9 -0.1903(11) 1.1643(5) 0.08746(16) 0.0465(12) Uani d . 1 1 . .
H H9 -0.2064 1.1037 0.0646 0.056 Uiso calc R 1 1 . .
N N3 -0.2233(16) 1.3460(5) 0.12323(17) 0.092(2) Uani d . 1 1 . .
C C8 -0.1028(17) 1.2542(6) 0.14744(19) 0.080(2) Uani d . 1 1 . .
H H8 -0.0398 1.2672 0.1768 0.096 Uiso calc R 1 1 . .
O O2W 0.746(3) 0.9295(7) 0.0049(2) 0.092(4) Uani d P 0.50 1 . .
H H2WA 0.9152 0.9472 0.0077 0.137 Uiso d PR 0.50 1 . .
H H2WB 0.5966 0.9714 0.0018 0.137 Uiso d PR 0.50 1 . .
H H1WA 0.3201 1.1370 0.2183 0.137 Uiso d R 1 1 . .
H H1WB 0.5177 1.0475 0.2023 0.137 Uiso d R 1 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Cu1 N4 . . 169.43(16) ?
N1 Cu1 O1 . . 80.88(13) ?
N4 Cu1 O1 . . 99.00(14) ?
N1 Cu1 O3 . . 79.57(13) ?
N4 Cu1 O3 . . 99.15(13) ?
O1 Cu1 O3 . . 159.60(14) ?
N1 Cu1 O1W . . 96.92(16) ?
N4 Cu1 O1W . . 93.53(15) ?
O1 Cu1 O1W . . 99.18(15) ?
O3 Cu1 O1W . . 88.91(16) ?
C7 O3 Cu1 . . 115.2(3) ?
C1 O1 Cu1 . . 114.5(3) ?
C2 N1 C6 . . 122.9(4) ?
C2 N1 Cu1 . . 118.0(3) ?
C6 N1 Cu1 . . 119.1(3) ?
O4 C7 O3 . . 125.5(4) ?
O4 C7 C6 . . 120.6(4) ?
O3 C7 C6 . . 113.9(3) ?
C9 N4 C8 . . 103.3(4) ?
C9 N4 Cu1 . . 127.5(3) ?
C8 N4 Cu1 . . 129.2(3) ?
N1 C2 C3 . . 119.7(4) ?
N1 C2 C1 . . 111.6(4) ?
C3 C2 C1 . . 128.7(4) ?
C2 C3 C4 . . 118.9(4) ?
C2 C3 H3 . . 120.6 ?
C4 C3 H3 . . 120.6 ?
N1 C6 C5 . . 119.9(4) ?
N1 C6 C7 . . 111.7(3) ?
C5 C6 C7 . . 128.5(4) ?
C13 C11 C12 . . 118.7(5) ?
C13 C11 C10 . . 120.4(5) ?
C12 C11 C10 . . 120.9(5) ?
O2 C1 O1 . . 126.7(4) ?
O2 C1 C2 . . 118.8(4) ?
O1 C1 C2 . . 114.4(4) ?
C6 C5 C4 . . 118.7(4) ?
C6 C5 H5 . . 120.6 ?
C4 C5 H5 . . 120.6 ?
C11 C12 C13 . 3_585 120.7(5) ?
C11 C12 H12 . . 119.7 ?
C13 C12 H12 3_585 . 119.7 ?
C3 C4 C5 . . 120.0(4) ?
C3 C4 H4 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
Cu1 O1W H1WA . . 129.9 ?
Cu1 O1W H1WB . . 112.7 ?
H1WA O1W H1WB . . 117.2 ?
C9 N2 N3 . . 109.6(4) ?
C9 N2 C10 . . 129.6(5) ?
N3 N2 C10 . . 120.7(4) ?
C11 C13 C12 . 3_585 120.6(5) ?
C11 C13 H13 . . 119.7 ?
C12 C13 H13 3_585 . 119.7 ?
N2 C10 C11 . . 111.8(4) ?
N2 C10 H10A . . 109.2 ?
C11 C10 H10A . . 109.2 ?
N2 C10 H10B . . 109.2 ?
C11 C10 H10B . . 109.2 ?
H10A C10 H10B . . 107.9 ?
N4 C9 N2 . . 110.2(4) ?
N4 C9 H9 . . 124.9 ?
N2 C9 H9 . . 124.9 ?
C8 N3 N2 . . 102.0(5) ?
N3 C8 N4 . . 114.9(5) ?
N3 C8 H8 . . 122.5 ?
N4 C8 H8 . . 122.5 ?
H2WA O2W H2WB . . 137.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N1 . 1.908(3) ?
Cu1 N4 . 1.950(3) ?
Cu1 O1 . 2.006(3) ?
Cu1 O3 . 2.048(3) ?
Cu1 O1W . 2.217(4) ?
O3 C7 . 1.280(5) ?
O1 C1 . 1.278(5) ?
N1 C2 . 1.322(5) ?
N1 C6 . 1.339(5) ?
C7 O4 . 1.218(5) ?
C7 C6 . 1.517(6) ?
N4 C9 . 1.302(6) ?
N4 C8 . 1.318(7) ?
C2 C3 . 1.377(6) ?
C2 C1 . 1.520(6) ?
C3 C4 . 1.382(7) ?
C3 H3 . 0.9300 ?
C6 C5 . 1.367(6) ?
O2 C1 . 1.226(5) ?
C11 C13 . 1.364(8) ?
C11 C12 . 1.374(7) ?
C11 C10 . 1.510(7) ?
C5 C4 . 1.384(7) ?
C5 H5 . 0.9300 ?
C12 C13 3_585 1.389(7) ?
C12 H12 . 0.9300 ?
C4 H4 . 0.9300 ?
O1W H1WA . 0.8301 ?
O1W H1WB . 0.8599 ?
N2 C9 . 1.319(6) ?
N2 N3 . 1.338(6) ?
N2 C10 . 1.466(6) ?
C13 C12 3_585 1.389(7) ?
C13 H13 . 0.9300 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C9 H9 . 0.9300 ?
N3 C8 . 1.313(7) ?
C8 H8 . 0.9300 ?
O2W H2WA . 0.8500 ?
O2W H2WB . 0.8482 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O2W H2WA O2W 3_775 0.85 2.147 2.920(5) 151.00
O2W H2WB O2W 3_675 0.85 1.959 2.807(5) 179.11
O1W H1WA O4 2_555 0.83 1.928 2.746(5) 167.54
O1W H1WB O3 1_655 0.86 1.859 2.692(5) 163.64
