#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/66/2216695.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_2216695
loop_
_publ_author_name
'Martin, David P.'
'LaDuca, Robert L.'
_publ_section_title
;catena-Poly[[[diaquacopper(II)]-μ-pyridine-2,4-dicarboxylato-κ³N,O²:O⁴]
 0.625-hydrate]
;
_journal_coeditor_code           NG2377
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3203
_journal_page_last               m3203
_journal_paper_doi               10.1107/S1600536807061946
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu (C7 H3 N1 O4) (H2 O)2] , 0.625H2 O'
_chemical_formula_moiety         'C7 H7 Cu N O6 , 0.625H2 O'
_chemical_formula_sum            'C7 H8.25 Cu N O6.625'
_chemical_formula_weight         275.94
_chemical_name_systematic
;
catena-Poly[[[diaquacopper(II)]-μ-pyridine-2,4-dicarboxylato-
κ³N,O²:O⁴] 0.625-hydrate]
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.324(4)
_cell_length_b                   12.057(2)
_cell_length_c                   7.4706(16)
_cell_measurement_reflns_used    7418
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.00
_cell_volume                     1830.6(6)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'COSMO (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEXII'
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7418
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.408
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1114
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.691
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2152
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0426P)²+0.2838P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                1517
_reflns_number_total             2152
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2377.cif
_cod_data_source_block           I
_cod_original_cell_volume        1830.7(6)
_cod_original_sg_symbol_H-M      Pnna
_cod_database_code               2216695
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-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
Cu Cu1 0.631799(18) 0.45906(4) 0.18172(6) 0.01542(15) Uani d . 1
O O1 0.67326(11) 0.7225(2) 0.4821(3) 0.0251(7) Uani d . 1
O O1W 0.7500 0.5000 -0.3147(6) 0.104(3) Uani d SDU 1
H H1W 0.7590 0.5513 -0.3903 0.124 Uiso d RD 1
O O2W 0.7243(11) 0.2500 -0.2500 0.108(10) Uani d SPDU 0.25
H H2W 0.7513 0.2379 -0.1577 0.130 Uiso d PRD 0.25
O O2 0.68258(10) 0.5671(2) 0.3219(3) 0.0174(6) Uani d . 1
O O3 0.42732(10) 0.8454(2) 0.5840(3) 0.0166(6) Uani d . 1
O O4 0.35590(11) 0.7053(2) 0.5432(4) 0.0320(8) Uani d . 1
O O5 0.64138(12) 0.5631(2) -0.0813(4) 0.0231(7) Uani d D 1
H H5A 0.6535(18) 0.6282(18) -0.066(5) 0.028 Uiso d D 1
H H5B 0.6750(13) 0.560(3) -0.142(4) 0.028 Uiso d D 1
O O6 0.71189(11) 0.3848(2) 0.1122(4) 0.0208(6) Uani d D 1
H H6A 0.7049(18) 0.3176(17) 0.106(5) 0.025 Uiso d D 1
H H6B 0.7394(14) 0.371(3) 0.188(4) 0.025 Uiso d D 1
N N1 0.55748(12) 0.5464(2) 0.2784(4) 0.0128(7) Uani d . 1
C C1 0.57573(15) 0.6319(3) 0.3852(5) 0.0129(8) Uani d . 1
C C2 0.53100(15) 0.7009(3) 0.4690(5) 0.0136(8) Uani d . 1
H H2 0.5454 0.7614 0.5407 0.016 Uiso calc R 1
C C3 0.46437(15) 0.6796(3) 0.4454(5) 0.0130(8) Uani d . 1
C C4 0.44555(15) 0.5921(3) 0.3370(4) 0.0163(8) Uani d . 1
H H4 0.4003 0.5766 0.3188 0.020 Uiso calc R 1
C C5 0.49278(15) 0.5276(3) 0.2556(5) 0.0154(8) Uani d . 1
H H5 0.4793 0.4679 0.1808 0.018 Uiso calc R 1
C C6 0.64987(15) 0.6440(3) 0.4010(5) 0.0152(8) Uani d . 1
C C7 0.41055(15) 0.7489(3) 0.5317(5) 0.0176(8) Uani d . 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
O6 Cu1 O2 . . 90.46(10)
O6 Cu1 O3 . 8_655 95.30(11)
O2 Cu1 O3 . 8_655 169.33(10)
O6 Cu1 N1 . . 171.84(11)
O2 Cu1 N1 . . 81.58(10)
O3 Cu1 N1 8_655 . 92.30(10)
O6 Cu1 O5 . . 87.36(11)
O2 Cu1 O5 . . 92.78(9)
O3 Cu1 O5 8_655 . 96.48(10)
N1 Cu1 O5 . . 94.86(11)
C6 O2 Cu1 . . 116.7(2)
C7 O3 Cu1 . 8_666 125.9(2)
Cu1 O5 H5A . . 115(3)
Cu1 O5 H5B . . 120(3)
H5A O5 H5B . . 83(3)
Cu1 O6 H6A . . 109(3)
Cu1 O6 H6B . . 119(3)
H6A O6 H6B . . 87(3)
C5 N1 C1 . . 118.1(3)
C5 N1 Cu1 . . 127.7(2)
C1 N1 Cu1 . . 114.1(2)
N1 C1 C2 . . 122.8(3)
N1 C1 C6 . . 113.0(3)
C2 C1 C6 . . 124.1(3)
C1 C2 C3 . . 118.3(3)
C1 C2 H2 . . 120.8
C3 C2 H2 . . 120.8
C4 C3 C2 . . 119.0(3)
C4 C3 C7 . . 117.8(3)
C2 C3 C7 . . 123.2(3)
C5 C4 C3 . . 119.6(3)
C5 C4 H4 . . 120.2
C3 C4 H4 . . 120.2
N1 C5 C4 . . 122.1(3)
N1 C5 H5 . . 118.9
C4 C5 H5 . . 118.9
O1 C6 O2 . . 125.8(3)
O1 C6 C1 . . 120.0(3)
O2 C6 C1 . . 114.2(3)
O4 C7 O3 . . 127.6(3)
O4 C7 C3 . . 116.4(3)
O3 C7 C3 . . 116.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 O6 . 1.931(2)
Cu1 O2 . 1.963(2)
Cu1 O3 8_655 1.964(2)
Cu1 N1 . 1.980(3)
Cu1 O5 . 2.339(3)
O1 C6 . 1.219(4)
O1W H1W . 0.8563
O2W H2W . 0.8920
O2 C6 . 1.285(4)
O3 C7 . 1.273(4)
O4 C7 . 1.234(4)
O5 H5A . 0.831(18)
O5 H5B . 0.822(18)
O6 H6A . 0.824(18)
O6 H6B . 0.815(18)
N1 C5 . 1.348(4)
N1 C1 . 1.353(4)
C1 C2 . 1.383(4)
C1 C6 . 1.522(4)
C2 C3 . 1.392(4)
C2 H2 . 0.9500
C3 C4 . 1.382(5)
C3 C7 . 1.521(4)
C4 C5 . 1.378(4)
C4 H4 . 0.9500
C5 H5 . 0.9500
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
O1W H1W O2 1_554 0.86 2.65 3.145(5) 117.1
O2W H2W O1 3_645 0.89 2.02 2.904(17) 168.4
O5 H5A O1 4_565 0.831(18) 1.95(2) 2.765(4) 168(4)
O5 H5B O1W . 0.822(18) 2.12(2) 2.914(4) 162(4)
O6 H6A O4 8_655 0.824(18) 1.89(2) 2.618(4) 146(4)
O6 H6B O2 2_665 0.815(18) 2.02(2) 2.719(3) 144(4)
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_site_symmetry_1
_geom_torsion
O6 Cu1 O2 C6 . 178.6(3)
O3 Cu1 O2 C6 8_655 -58.7(7)
N1 Cu1 O2 C6 . -3.2(3)
O5 Cu1 O2 C6 . 91.2(3)
O2 Cu1 N1 C5 . -176.9(3)
O3 Cu1 N1 C5 8_655 -5.7(3)
O5 Cu1 N1 C5 . 91.1(3)
O2 Cu1 N1 C1 . 0.3(2)
O3 Cu1 N1 C1 8_655 171.5(2)
O5 Cu1 N1 C1 . -91.7(2)
C5 N1 C1 C2 . -0.9(5)
Cu1 N1 C1 C2 . -178.4(3)
C5 N1 C1 C6 . 179.7(3)
Cu1 N1 C1 C6 . 2.2(4)
N1 C1 C2 C3 . 1.6(5)
C6 C1 C2 C3 . -179.1(3)
C1 C2 C3 C4 . -1.3(5)
C1 C2 C3 C7 . 179.4(3)
C2 C3 C4 C5 . 0.4(5)
C7 C3 C4 C5 . 179.7(3)
C1 N1 C5 C4 . -0.1(5)
Cu1 N1 C5 C4 . 177.0(3)
C3 C4 C5 N1 . 0.3(6)
Cu1 O2 C6 O1 . -174.1(3)
Cu1 O2 C6 C1 . 5.1(4)
N1 C1 C6 O1 . 174.5(3)
C2 C1 C6 O1 . -4.9(6)
N1 C1 C6 O2 . -4.8(5)
C2 C1 C6 O2 . 175.8(3)
Cu1 O3 C7 O4 8_666 -5.5(6)
Cu1 O3 C7 C3 8_666 174.6(2)
C4 C3 C7 O4 . 20.4(5)
C2 C3 C7 O4 . -160.3(4)
C4 C3 C7 O3 . -159.7(3)
C2 C3 C7 O3 . 19.6(5)
