#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007252.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_2007252
loop_
_publ_author_name
'Wu, Y.-L.'
'Tong, Y.-X.'
'Chen, X.-M.'
'Mak, T. C. W.'
_publ_section_title
;
 Diaquachlorobis(4-pyridinioacetate-<i>O</i>)copper(II) Perchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              606
_journal_page_last               608
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[CuCl(C7 H7 N O2)2 (H2 O)2]Cl O4'
_chemical_formula_sum            'C14 H18 Cl2 Cu N2 O10'
_chemical_formula_weight         508.74
_chemical_name_systematic
;
Diaquachlorobis(pyridinioacetato)copper(II) perchlorate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.186(6)
_cell_length_b                   5.2790(10)
_cell_length_c                   27.288(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.2
_cell_volume                     1899.5(10)
_computing_cell_refinement       SHELXTL/PC
_computing_data_collection       'SHELXTL/PC (Sheldrick, 1990)'
_computing_data_reduction        SHELXTL/PC
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    SHELXTL/PC
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_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  0.027
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            2326
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   'psi-scan (Kopfmann & Huber, 1968)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.38
_refine_ls_abs_structure_details 'Flack  (1983) parameter = 0.01(2)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         2000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_obs          0.0346
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.4389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0827
_refine_ls_wR_factor_obs         0.0773
_reflns_number_observed          1736
_reflns_number_total             2000
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    mu1368.cif
_[local]_cod_data_source_block   cupyb1
_[local]_cod_cif_authors_sg_H-M  P_n_a_21
_cod_database_code               2007252
loop_
_symmetry_equiv_pos_as_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'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.0261(3) 0.0389(3) 0.0336(3) -0.0073(3) 0.0094(3) -0.0138(4)
Cl1 0.0252(5) 0.0347(6) 0.0388(6) -0.0025(4) 0.0043(7) -0.0028(8)
O1w 0.036(2) 0.091(4) 0.059(3) -0.024(2) 0.019(2) -0.036(3)
O2w 0.045(2) 0.029(2) 0.049(3) -0.008(2) 0.011(2) -0.005(2)
O11 0.027(2) 0.038(2) 0.042(2) -0.004(2) 0.013(2) -0.012(2)
O12 0.041(2) 0.033(2) 0.042(2) -0.011(2) 0.021(2) -0.011(2)
C11 0.031(3) 0.021(2) 0.029(3) 0.002(2) 0.005(2) -0.001(2)
C12 0.032(3) 0.032(3) 0.045(3) -0.005(2) 0.015(2) -0.012(3)
N1 0.034(2) 0.026(2) 0.024(2) 0.003(2) 0.006(2) -0.006(2)
C13 0.037(3) 0.031(3) 0.037(3) 0.003(3) 0.006(3) 0.004(3)
C14 0.032(3) 0.039(3) 0.047(4) 0.005(3) 0.005(3) -0.004(3)
C15 0.040(3) 0.048(4) 0.038(3) -0.006(3) 0.016(3) -0.015(3)
C16 0.065(4) 0.039(3) 0.032(3) 0.001(3) 0.012(3) 0.006(3)
C17 0.046(3) 0.032(3) 0.031(3) 0.011(3) 0.000(3) -0.003(3)
O21 0.031(2) 0.040(2) 0.042(2) -0.004(2) 0.011(2) -0.015(2)
O22 0.043(2) 0.052(3) 0.049(3) -0.017(2) 0.013(2) -0.019(2)
C21 0.032(3) 0.040(3) 0.029(3) 0.001(3) 0.002(2) -0.007(2)
C22 0.036(3) 0.039(3) 0.029(3) -0.002(3) 0.001(2) -0.011(2)
N2 0.034(2) 0.030(2) 0.023(2) 0.006(2) 0.002(2) -0.005(2)
C23 0.040(3) 0.052(4) 0.023(3) 0.012(3) -0.003(2) -0.003(3)
C24 0.056(4) 0.045(4) 0.039(3) 0.012(3) 0.009(3) 0.009(3)
C25 0.049(4) 0.044(4) 0.051(4) -0.007(3) 0.011(3) -0.002(3)
C26 0.030(3) 0.067(4) 0.049(4) 0.004(3) -0.005(3) -0.002(4)
C27 0.041(3) 0.042(3) 0.034(3) 0.010(3) -0.006(3) 0.002(3)
Cl2 0.0509(8) 0.0314(7) 0.0312(7) -0.0020(6) 0.0058(6) -0.0032(6)
O1 0.066(3) 0.034(2) 0.078(4) -0.001(2) 0.016(3) 0.007(2)
O2 0.144(6) 0.083(4) 0.098(5) -0.045(5) -0.067(5) 0.011(4)
O3 0.067(3) 0.067(3) 0.036(2) 0.002(3) 0.014(2) 0.000(2)
O4 0.108(5) 0.072(3) 0.095(4) 0.044(4) 0.063(4) 0.021(4)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cu1 0.32258(4) 0.87436(12) 0.3612 0.0329(2) Uani d . 1 Cu
Cl1 0.47474(8) 1.0686(2) 0.36302(7) 0.0329(3) Uani d . 1 Cl
O1w 0.1875(3) 0.7412(11) 0.3491(2) 0.062(2) Uani d . 1 O
H1wA 0.2070(3) 0.5836(11) 0.3299(2) 0.080 Uiso d R 1 H
H1wB 0.1368(3) 0.7550(11) 0.3681(2) 0.080 Uiso d R 1 H
O2w 0.3767(3) 0.5666(8) 0.4186(2) 0.0412(11) Uani d . 1 O
H2wA 0.3527(3) 0.4132(8) 0.4153(2) 0.080 Uiso d R 1 H
H2wB 0.4317(3) 0.6025(8) 0.4109(2) 0.080 Uiso d R 1 H
O11 0.2658(3) 1.1081(8) 0.4116(2) 0.0356(9) Uani d . 1 O
O12 0.1136(3) 0.9418(7) 0.4303(2) 0.0385(10) Uani d . 1 O
C11 0.1811(4) 1.1022(9) 0.4338(2) 0.0268(11) Uani d . 1 C
C12 0.1686(4) 1.3235(10) 0.4688(2) 0.0364(14) Uani d . 1 C
H12A 0.1724(4) 1.4783(10) 0.4505(2) 0.080 Uiso d R 1 H
H12B 0.2239(4) 1.3224(10) 0.4918(2) 0.080 Uiso d R 1 H
N1 0.0722(3) 1.3197(8) 0.4963(2) 0.0280(10) Uani d . 1 N
C13 0.0023(4) 1.4975(10) 0.4871(2) 0.0352(13) Uani d . 1 C
H13A 0.0144(4) 1.6220(10) 0.4621(2) 0.080 Uiso d R 1 H
C14 -0.0856(4) 1.5035(11) 0.5133(2) 0.0394(14) Uani d . 1 C
H14A -0.1365(4) 1.6284(11) 0.5062(2) 0.080 Uiso d R 1 H
C15 -0.1021(5) 1.3286(11) 0.5499(2) 0.042(2) Uani d . 1 C
H15A -0.1618(5) 1.3374(11) 0.5699(2) 0.080 Uiso d R 1 H
C16 -0.0314(5) 1.1451(12) 0.5572(2) 0.045(2) Uani d . 1 C
H16A -0.0443(5) 1.0142(12) 0.5808(2) 0.080 Uiso d R 1 H
C17 0.0569(5) 1.1418(11) 0.5308(2) 0.0366(13) Uani d . 1 C
H17A 0.1075(5) 1.0150(11) 0.5370(2) 0.080 Uiso d R 1 H
O21 0.3665(3) 0.6765(7) 0.3022(2) 0.0377(10) Uani d . 1 O
O22 0.2598(3) 0.3440(8) 0.3032(2) 0.0477(11) Uani d . 1 O
C21 0.3347(4) 0.4615(11) 0.2891(2) 0.0336(12) Uani d . 1 C
C22 0.3979(4) 0.3297(11) 0.2495(2) 0.0349(13) Uani d . 1 C
H22A 0.3546(4) 0.2896(11) 0.2222(2) 0.080 Uiso d R 1 H
H22B 0.4240(4) 0.1735(11) 0.2623(2) 0.080 Uiso d R 1 H
N2 0.4827(3) 0.4839(9) 0.2320(2) 0.0292(9) Uani d . 1 N
C23 0.4662(5) 0.6610(12) 0.1975(2) 0.0382(14) Uani d . 1 C
H23A 0.4006(5) 0.6737(12) 0.1824(2) 0.080 Uiso d R 1 H
C24 0.5428(5) 0.8192(12) 0.1833(2) 0.047(2) Uani d . 1 C
H24A 0.5308(5) 0.9485(12) 0.1592(2) 0.080 Uiso d R 1 H
C25 0.6373(5) 0.7937(13) 0.2036(3) 0.048(2) Uani d . 1 C
H25A 0.6923(5) 0.8997(13) 0.1930(3) 0.080 Uiso d R 1 H
C26 0.6518(5) 0.6119(14) 0.2394(3) 0.049(2) Uani d . 1 C
H26A 0.7169(5) 0.5952(14) 0.2548(3) 0.080 Uiso d R 1 H
C27 0.5747(5) 0.4625(11) 0.2526(2) 0.0392(14) Uani d . 1 C
H27A 0.5854(5) 0.3354(11) 0.2772(2) 0.080 Uiso d R 1 H
Cl2 0.20312(12) 0.6343(3) 0.61007(6) 0.0378(3) Uani d . 1 Cl
O1 0.2016(4) 0.3687(8) 0.6184(2) 0.0593(13) Uani d . 1 O
O2 0.2845(6) 0.7403(14) 0.6368(3) 0.108(3) Uani d . 1 O
O3 0.2194(4) 0.6869(10) 0.5595(2) 0.0566(13) Uani d . 1 O
O4 0.1090(5) 0.7398(12) 0.6242(2) 0.092(2) Uani d . 1 O
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1w Cu1 O11 . . 89.8(2) yes
O1w Cu1 O21 . . 86.6(2) yes
O11 Cu1 O21 . . 170.1(2) yes
O1w Cu1 Cl1 . . 169.9(2) yes
O11 Cu1 Cl1 . . 92.16(11) yes
O21 Cu1 Cl1 . . 89.86(13) yes
O1w Cu1 O2w . . 98.1(2) yes
O11 Cu1 O2w . . 94.7(2) yes
O21 Cu1 O2w . . 95.0(2) yes
Cl1 Cu1 O2w . . 91.69(12) yes
Cu1 O1w O22 . . 92.1(2) ?
Cu1 O1w O12 . . 92.9(2) ?
O22 O1w O12 . . 148.8(3) ?
Cu1 O2w O11 . 1_545 112.7(2) ?
Cu1 O2w Cl1 . 1_545 111.1(2) ?
O11 O2w Cl1 1_545 1_545 59.39(11) ?
C11 O11 Cu1 . . 130.1(3) yes
C11 O12 O1w . . 94.3(3) yes
O12 C11 O11 . . 127.9(5) yes
O12 C11 C12 . . 120.0(5) ?
O11 C11 C12 . . 112.1(4) ?
N1 C12 C11 . . 113.7(4) ?
C13 N1 C17 . . 121.1(5) ?
C13 N1 C12 . . 119.3(5) ?
C17 N1 C12 . . 119.6(5) ?
N1 C13 C14 . . 120.3(5) ?
C13 C14 C15 . . 119.9(5) ?
C16 C15 C14 . . 118.5(5) ?
C15 C16 C17 . . 121.0(6) ?
N1 C17 C16 . . 119.2(5) ?
C21 O21 Cu1 . . 126.9(4) yes
C21 O22 O1w . . 92.2(4) yes
O22 C21 O21 . . 129.2(5) yes
O22 C21 C22 . . 115.4(5) ?
O21 C21 C22 . . 115.4(5) ?
N2 C22 C21 . . 113.1(4) ?
C27 N2 C23 . . 119.9(5) ?
C27 N2 C22 . . 120.5(5) ?
C23 N2 C22 . . 119.4(5) ?
N2 C23 C24 . . 120.2(5) ?
C23 C24 C25 . . 119.8(6) ?
C24 C25 C26 . . 118.6(6) ?
C27 C26 C25 . . 119.7(6) ?
C26 C27 N2 . . 121.7(6) ?
O2 Cl2 O4 . . 111.7(5) ?
O2 Cl2 O1 . . 108.6(4) ?
O4 Cl2 O1 . . 109.4(4) ?
O2 Cl2 O3 . . 108.0(4) ?
O4 Cl2 O3 . . 108.6(3) ?
O1 Cl2 O3 . . 110.5(3) ?
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 O1w . 1.944(4) yes
Cu1 O11 . 1.994(4) yes
Cu1 O21 . 2.004(4) yes
Cu1 Cl1 . 2.2538(15) yes
Cu1 O2w . 2.367(4) yes
O1w O22 . 2.623(7) yes
O1w O12 . 2.642(6) yes
O2w O11 1_545 2.834(6) yes
O2w Cl1 1_545 3.299(4) yes
O11 C11 . 1.271(6) yes
O12 C11 . 1.231(6) yes
C11 C12 . 1.519(7) ?
C12 N1 . 1.475(7) ?
N1 C13 . 1.339(7) ?
N1 C17 . 1.346(7) ?
C13 C14 . 1.362(8) ?
C14 C15 . 1.377(9) ?
C15 C16 . 1.359(9) ?
C16 C17 . 1.369(9) ?
O21 C21 . 1.262(7) yes
O22 C21 . 1.228(7) yes
C21 C22 . 1.532(7) ?
C22 N2 . 1.463(7) ?
N2 C27 . 1.342(7) ?
N2 C23 . 1.345(7) ?
C23 C24 . 1.367(9) ?
C24 C25 . 1.371(9) ?
C25 C26 . 1.383(10) ?
C26 C27 . 1.336(9) ?
Cl2 O2 . 1.413(6) ?
Cl2 O4 . 1.414(6) ?
Cl2 O1 . 1.421(4) ?
Cl2 O3 . 1.424(5) ?