#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/95/2219585.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_2219585
loop_
_publ_author_name
'Hao, Lujiang'
'Mu, Chunhua'
'Kong, Binbin'
_publ_section_title
;catena-Poly[[[triaquacopper(II)]-μ-pyridine-2,3-dicarboxylato-κ³N,O²:O³]
 monohydrate]
;
_journal_coeditor_code           HB2747
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1229
_journal_paper_doi               10.1107/S1600536808025439
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu (C7 H3 N O4) (H2 O)3], H2 O'
_chemical_formula_moiety         'C7 H9 Cu N O7, H2 O'
_chemical_formula_sum            'C7 H11 Cu N O8'
_chemical_formula_weight         300.71
_chemical_name_systematic
;
catena-Poly[[[triaquacopper(II)]-μ-pyridine-2,3-dicarboxylato-
κ³N,O²:O³] monohydrate]
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.486(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.513(3)
_cell_length_b                   17.983(3)
_cell_length_c                   7.493(3)
_cell_measurement_reflns_used    2692
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.88
_cell_volume                     1043.9(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            2686
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.652
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.600
_refine_ls_abs_structure_details 'Flack (1983), 290 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         1322
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0297
_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)+(0.079P)²+0.0702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                1310
_reflns_number_total             1322
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2747.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2219585
_cod_database_fobs_code          2219585
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_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
Cu Cu1 0.00453(5) 0.118674(19) 0.25189(5) 0.0226(2) Uani d . 1
C C1 -0.1893(6) 0.1125(2) -0.2173(8) 0.0257(10) Uani d . 1
C C2 0.0162(7) 0.2776(2) 0.2417(8) 0.0261(9) Uani d . 1
C C3 0.1909(5) 0.2542(2) 0.2398(6) 0.0220(8) Uani d . 1
C C4 0.3188(5) 0.3044(2) 0.2468(6) 0.0224(8) Uani d . 1
C C5 0.4612(5) 0.2816(2) 0.2256(6) 0.0222(9) Uani d . 1
H H5 0.5443 0.3154 0.2266 0.027 Uiso calc R 1
C C6 0.4781(6) 0.2094(3) 0.2034(7) 0.0325(10) Uani d . 1
H H6 0.5747 0.1922 0.1878 0.039 Uiso calc R 1
C C7 0.3554(7) 0.1592(3) 0.2028(8) 0.0350(10) Uani d . 1
H H7 0.3719 0.1088 0.1890 0.042 Uiso calc R 1
N N1 0.2118(5) 0.18178(19) 0.2218(6) 0.0262(7) Uani d . 1
O O1 -0.1400(5) 0.0911(2) -0.0470(5) 0.0356(8) Uani d . 1
O O2 -0.2392(5) 0.07157(19) -0.3667(5) 0.0363(7) Uani d . 1
O O3 -0.0834(4) 0.22671(17) 0.2399(6) 0.0323(7) Uani d . 1
O O4 -0.0130(6) 0.34452(16) 0.2387(9) 0.0401(8) Uani d . 1
O O5 0.1420(5) 0.12328(17) 0.5699(7) 0.0311(9) Uani d D 1
O O6 0.1266(5) 0.01799(18) 0.2664(7) 0.0427(9) Uani d D 1
O O7 -0.2021(4) 0.07356(18) 0.2898(5) 0.0309(7) Uani d D 1
O O8 0.4601(7) -0.0181(3) 0.4257(10) 0.0777(18) Uani d D 1
H H1W 0.553(6) -0.004(6) 0.515(11) 0.093 Uiso d D 1
H H2W 0.377(7) -0.006(6) 0.451(14) 0.093 Uiso d D 1
H H4W 0.105(10) 0.080(2) 0.551(16) 0.093 Uiso d D 1
H H5W 0.092(12) -0.008(5) 0.167(10) 0.093 Uiso d D 1
H H6W 0.229(5) 0.011(5) 0.340(12) 0.093 Uiso d D 1
H H7W -0.214(15) 0.067(5) 0.393(9) 0.093 Uiso d D 1
H H8W -0.195(16) 0.034(3) 0.238(13) 0.093 Uiso d D 1
H H3W 0.248(3) 0.126(4) 0.620(19) 0.093 Uiso d D 1
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 0.0221(3) 0.0153(3) 0.0307(3) -0.0014(2) 0.0111(2) 0.0008(2)
C1 0.024(2) 0.021(2) 0.033(3) 0.0026(14) 0.013(2) 0.0011(15)
C2 0.0229(19) 0.0210(17) 0.0315(18) 0.0045(18) 0.0084(15) -0.0004(19)
C3 0.0223(19) 0.0198(18) 0.0229(18) 0.0031(15) 0.0083(15) 0.0014(14)
C4 0.0208(18) 0.0218(19) 0.0220(17) 0.0000(14) 0.0064(15) 0.0016(15)
C5 0.026(2) 0.0141(17) 0.032(2) 0.0009(13) 0.017(2) 0.0013(15)
C6 0.034(3) 0.027(2) 0.042(3) 0.0042(18) 0.022(2) 0.0008(16)
C7 0.045(3) 0.0219(18) 0.044(2) 0.0067(19) 0.025(2) 0.0011(18)
N1 0.0284(18) 0.0215(16) 0.0293(17) 0.0018(14) 0.0125(15) -0.0001(14)
O1 0.0475(19) 0.0275(18) 0.0292(16) -0.0008(15) 0.0133(15) 0.0000(14)
O2 0.055(2) 0.0236(14) 0.0343(16) -0.0049(14) 0.0230(16) -0.0069(13)
O3 0.0226(17) 0.0253(16) 0.0519(19) 0.0004(12) 0.0185(14) 0.0011(14)
O4 0.0274(17) 0.0214(15) 0.073(2) 0.0041(14) 0.0220(17) -0.0029(19)
O5 0.0266(16) 0.0281(19) 0.033(2) -0.0011(11) 0.0062(16) -0.0014(12)
O6 0.0362(17) 0.0247(16) 0.056(2) 0.0078(15) 0.0077(15) -0.0088(16)
O7 0.0313(16) 0.0262(15) 0.0355(16) -0.0074(13) 0.0142(14) -0.0040(14)
O8 0.035(2) 0.054(3) 0.108(4) 0.0047(18) -0.006(3) -0.023(3)
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_3
_geom_angle
O7 Cu1 O6 . 95.00(16)
O7 Cu1 O3 . 93.52(13)
O6 Cu1 O3 . 171.34(14)
O7 Cu1 O1 . 84.19(14)
O6 Cu1 O1 . 84.83(16)
O3 Cu1 O1 . 97.60(15)
O7 Cu1 O5 . 88.09(15)
O6 Cu1 O5 . 86.87(16)
O3 Cu1 O5 . 91.87(14)
O1 Cu1 O5 . 168.12(14)
O7 Cu1 N1 . 171.80(13)
O6 Cu1 N1 . 92.89(17)
O3 Cu1 N1 . 78.54(13)
O1 Cu1 N1 . 98.75(15)
O5 Cu1 N1 . 90.13(15)
O1 C1 O2 . 125.8(4)
O1 C1 C4 4_454 118.0(4)
O2 C1 C4 4_454 116.1(4)
O4 C2 O3 . 126.1(5)
O4 C2 C3 . 117.0(5)
O3 C2 C3 . 116.8(4)
N1 C3 C4 . 120.1(4)
N1 C3 C2 . 115.9(4)
C4 C3 C2 . 123.9(4)
C5 C4 C3 . 121.5(4)
C5 C4 C1 4 115.3(4)
C3 C4 C1 4 123.2(4)
C6 C5 C4 . 117.5(4)
C6 C5 H5 . 121.2
C4 C5 H5 . 121.2
C5 C6 C7 . 121.3(5)
C5 C6 H6 . 119.3
C7 C6 H6 . 119.3
N1 C7 C6 . 121.4(4)
N1 C7 H7 . 119.3
C6 C7 H7 . 119.3
C3 N1 C7 . 118.0(4)
C3 N1 Cu1 . 110.5(3)
C7 N1 Cu1 . 131.3(3)
C1 O1 Cu1 . 145.4(3)
C2 O3 Cu1 . 117.2(3)
Cu1 O5 H4W . 77(8)
Cu1 O5 H3W . 119(10)
H4W O5 H3W . 114(4)
Cu1 O6 H5W . 118(7)
Cu1 O6 H6W . 122(7)
H5W O6 H6W . 114(9)
Cu1 O7 H7W . 129(8)
Cu1 O7 H8W . 92(8)
H7W O7 H8W . 112(9)
H1W O8 H2W . 111(4)
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 O7 . 2.061(3) y
Cu1 O6 . 2.068(3) y
Cu1 O3 . 2.071(3) y
Cu1 O1 . 2.119(4) y
Cu1 O5 . 2.178(5) y
Cu1 N1 . 2.187(4) y
C1 O1 . 1.228(7) ?
C1 O2 . 1.258(6) ?
C1 C4 4_454 1.525(5) ?
C2 O4 . 1.227(5) ?
C2 O3 . 1.244(6) ?
C2 C3 . 1.552(6) ?
C3 N1 . 1.328(5) ?
C3 C4 . 1.399(6) ?
C4 C5 . 1.349(6) ?
C4 C1 4 1.525(5) ?
C5 C6 . 1.325(6) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.379(7) ?
C6 H6 . 0.9300 ?
C7 N1 . 1.350(6) ?
C7 H7 . 0.9300 ?
O5 H4W . 0.82(2) ?
O5 H3W . 0.82(9) ?
O6 H5W . 0.82(7) ?
O6 H6W . 0.83(7) ?
O7 H7W . 0.83(8) ?
O7 H8W . 0.83(8) ?
O8 H1W . 0.84(8) ?
O8 H2W . 0.83(8) ?
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
O5 H3W O4 4 0.82(9) 1.93(8) 2.735(6) 167(8)
O5 H4W O6 2 0.82(2) 2.35(8) 2.966(5) 132(10)
O6 H5W O5 2_554 0.82(7) 2.29(7) 2.966(5) 140(9)
O7 H7W O2 1_556 0.83(8) 1.90(9) 2.720(5) 169(8)
O7 H8W O2 2 0.83(8) 2.03(4) 2.825(5) 162(11)
