#------------------------------------------------------------------------------
#$Date: 2017-03-29 15:46:26 +0300 (Wed, 29 Mar 2017) $
#$Revision: 194583 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/79/2207930.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_2207930
loop_
_publ_author_name
'Tian, Dong-Kui'
'Li, Song-Lin'
'Hou, Jian-Feng'
_publ_section_title
;catena-Poly[[[diaquacalcium(II)]bis[μ-2-(pyridinium-1-yl)butanedioato-κO¹:O⁴]]
 2.5-hydrate]
;
_journal_coeditor_code           WW6432
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m130
_journal_page_last               m132
_journal_paper_doi               10.1107/S160053680504122X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ca (C9 H8 N O4)2 (H2 O)2], 2.5H2 O'
_chemical_formula_moiety         'C18 H20 Ca N2 O10, 2.5H2 O'
_chemical_formula_sum            'C18 H25 Ca N2 O12.5'
_chemical_formula_weight         509.48
_chemical_name_systematic
;
catena-Poly[[[diaquacalcium(II)]bis[μ-2-(pyridinium-1-yl)butanedioato-
\kO¹:O⁴]] 2.5-hydrate]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.018(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.766(14)
_cell_length_b                   9.8281(13)
_cell_length_c                   14.2746(16)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.758
_cell_measurement_theta_min      9.337
_cell_volume                     4342(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5549
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 120
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0561
_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)+(0.0429P)²+15.5672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                3569
_reflns_number_total             4744
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ww6432.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Removing the "\" symbol from the _chemical_name_systematic
 data item value.

 Antanas Vaitkus,
 2017-03-29
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C18 H25 Ca1 N2 O12.5'
_cod_database_code               2207930
_cod_database_fobs_code          2207930
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'
'-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_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_type_symbol
Ca1 0.10310(2) 0.85722(6) 0.11548(4) 0.02100(16) Uani d . 1 Ca
O1W 0.17903(8) 0.8520(3) 0.1582(2) 0.0578(9) Uani d . 1 O
H10A 0.2008 0.8030 0.1465 0.087 Uiso d . 1 H
H10B 0.1886 0.9348 0.1953 0.087 Uiso d . 1 H
O2W 0.03000(8) 0.8373(3) 0.13758(18) 0.0407(6) Uani d . 1 O
H20A 0.0225 0.7773 0.1688 0.061 Uiso d . 1 H
H20B 0.0040 0.8684 0.1147 0.061 Uiso d . 1 H
O3W 0.0000 0.6206(4) 0.2500 0.0400(8) Uani d S 1 O
H30A -0.0191 0.5599 0.2179 0.060 Uiso d . 1 H
O4W 0.25432(8) 0.8002(3) -0.1230(2) 0.0455(7) Uani d . 1 O
H40A 0.2298 0.8366 -0.1524 0.068 Uiso d . 1 H
H40B 0.2626 0.8451 -0.0733 0.068 Uiso d . 1 H
O5W 0.23427(9) 0.4527(3) 0.4536(2) 0.0528(7) Uani d . 1 O
H50A 0.2112 0.4896 0.4096 0.079 Uiso d . 1 H
H50B 0.2343 0.3685 0.4259 0.079 Uiso d . 1 H
O1 0.09401(8) 0.6924(2) -0.00371(15) 0.0308(5) Uani d . 1 O
O2 0.06406(8) 0.5464(2) -0.11898(15) 0.0298(5) Uani d . 1 O
C1 0.08151(10) 0.6563(3) -0.0905(2) 0.0212(6) Uani d . 1 C
C2 0.08985(10) 0.7640(3) -0.16370(19) 0.0207(6) Uani d . 1 C
H2A 0.0771 0.8497 -0.1486 0.031 Uiso calc R 1 H
O3 0.18469(8) 0.9338(3) -0.2195(2) 0.0496(8) Uani d . 1 O
O4 0.11479(7) 0.9771(2) -0.26199(16) 0.0306(5) Uani d . 1 O
C3 0.14634(10) 0.9096(3) -0.2186(2) 0.0256(7) Uani d . 1 C
C4 0.13776(10) 0.7901(3) -0.1560(2) 0.0244(6) Uani d . 1 C
H4A 0.1508 0.7085 -0.1751 0.029 Uiso calc R 1 H
H4B 0.1515 0.8087 -0.0894 0.029 Uiso calc R 1 H
N1 0.06770(8) 0.7259(2) -0.26315(16) 0.0198(5) Uani d . 1 N
C5 0.03723(10) 0.8091(3) -0.3143(2) 0.0243(6) Uani d . 1 C
H5A 0.0311 0.8909 -0.2875 0.029 Uiso calc R 1 H
C6 0.01534(10) 0.7751(3) -0.4043(2) 0.0285(7) Uani d . 1 C
H6A -0.0060 0.8322 -0.4385 0.034 Uiso calc R 1 H
C7 0.02524(11) 0.6544(4) -0.4447(2) 0.0302(7) Uani d . 1 C
H7A 0.0105 0.6295 -0.5062 0.036 Uiso calc R 1 H
C8 0.05714(11) 0.5715(3) -0.3930(2) 0.0282(7) Uani d . 1 C
H8A 0.0644 0.4909 -0.4197 0.034 Uiso calc R 1 H
C9 0.07825(10) 0.6093(3) -0.3013(2) 0.0233(6) Uani d . 1 C
H9A 0.0998 0.5539 -0.2658 0.028 Uiso calc R 1 H
O5 0.11345(8) 0.6873(2) 0.23276(15) 0.0336(6) Uani d . 1 O
O6 0.16197(9) 0.5620(3) 0.33267(17) 0.0400(6) Uani d . 1 O
C10 0.13792(10) 0.6617(3) 0.3132(2) 0.0250(6) Uani d . 1 C
C11 0.13551(10) 0.7675(3) 0.3923(2) 0.0232(6) Uani d . 1 C
H11A 0.1486 0.8518 0.3757 0.035 Uiso calc R 1 H
O7 0.11610(10) 0.9750(3) 0.5084(2) 0.0539(8) Uani d . 1 O
O8 0.04608(10) 0.9668(3) 0.4507(3) 0.0590(9) Uani d . 1 O
C12 0.08327(12) 0.9224(3) 0.4563(3) 0.0343(8) Uani d . 1 C
C13 0.08896(10) 0.8001(3) 0.3955(2) 0.0272(7) Uani d . 1 C
H13A 0.0726 0.8157 0.3303 0.033 Uiso calc R 1 H
H13B 0.0766 0.7212 0.4200 0.033 Uiso calc R 1 H
C14 0.19645(11) 0.7932(4) 0.5320(3) 0.0344(8) Uani d . 1 C
H14A 0.2041 0.8726 0.5045 0.041 Uiso calc R 1 H
N2 0.16145(8) 0.7216(3) 0.48709(17) 0.0233(5) Uani d . 1 N
C15 0.22087(13) 0.7485(5) 0.6188(3) 0.0461(10) Uani d . 1 C
H15A 0.2454 0.7965 0.6491 0.055 Uiso calc R 1 H
C16 0.20904(13) 0.6328(5) 0.6606(3) 0.0471(10) Uani d . 1 C
H16A 0.2252 0.6029 0.7197 0.056 Uiso calc R 1 H
C17 0.17325(12) 0.5619(4) 0.6147(2) 0.0380(8) Uani d . 1 C
H17A 0.1648 0.4837 0.6423 0.046 Uiso calc R 1 H
C18 0.14988(11) 0.6074(3) 0.5274(2) 0.0274(7) Uani d . 1 C
H18A 0.1257 0.5589 0.4957 0.033 Uiso calc R 1 H
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
;
Ca Ca 0.2262 0.3064
;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
O1 Ca1 O5 . . 90.03(8) yes
O1 Ca1 O7 . 6_575 91.38(10) yes
O5 Ca1 O7 . 6_575 162.23(10) yes
O1 Ca1 O1W . . 97.24(10) yes
O5 Ca1 O1W . . 80.08(11) yes
O7 Ca1 O1W 6_575 . 82.14(12) yes
O1 Ca1 O4 . 6_576 178.11(9) yes
O5 Ca1 O4 . 6_576 89.36(8) yes
O7 Ca1 O4 6_575 6_576 88.66(10) yes
O1W Ca1 O4 . 6_576 80.89(9) yes
O1 Ca1 O2W . . 94.27(9) yes
O5 Ca1 O2W . . 80.38(9) yes
O7 Ca1 O2W 6_575 . 117.15(10) yes
O1W Ca1 O2W . . 157.27(11) yes
O4 Ca1 O2W 6_576 . 87.40(9) yes
O1 Ca1 C12 . 6_575 88.80(8) ?
O5 Ca1 C12 . 6_575 176.38(10) ?
O7 Ca1 C12 6_575 6_575 21.29(10) ?
O1W Ca1 C12 . 6_575 103.46(12) ?
O4 Ca1 C12 6_576 6_575 91.91(9) ?
O2W Ca1 C12 . 6_575 96.29(9) ?
Ca1 O1W H10A . . 139.4 ?
Ca1 O1W H10B . . 107.3 ?
H10A O1W H10B . . 113.0 ?
Ca1 O2W H20A . . 122.8 ?
Ca1 O2W H20B . . 141.1 ?
H20A O2W H20B . . 95.2 ?
H40A O4W H40B . . 105.7 ?
H50A O5W H50B . . 97.9 ?
C1 O1 Ca1 . . 151.0(2) yes
O2 C1 O1 . . 125.8(3) yes
O2 C1 C2 . . 120.3(2) ?
O1 C1 C2 . . 113.9(3) ?
N1 C2 C4 . . 111.3(2) ?
N1 C2 C1 . . 110.9(2) ?
C4 C2 C1 . . 112.7(2) ?
N1 C2 H2A . . 107.2 ?
C4 C2 H2A . . 107.2 ?
C1 C2 H2A . . 107.2 ?
C3 O4 Ca1 . 6_575 135.4(2) yes
O3 C3 O4 . . 125.0(3) yes
O3 C3 C4 . . 117.1(3) yes
O4 C3 C4 . . 117.9(3) ?
C2 C4 C3 . . 113.1(2) ?
C2 C4 H4A . . 109.0 ?
C3 C4 H4A . . 109.0 ?
C2 C4 H4B . . 109.0 ?
C3 C4 H4B . . 109.0 ?
H4A C4 H4B . . 107.8 ?
C9 N1 C5 . . 120.8(3) ?
C9 N1 C2 . . 119.7(2) ?
C5 N1 C2 . . 119.5(2) ?
N1 C5 C6 . . 121.0(3) ?
N1 C5 H5A . . 119.5 ?
C6 C5 H5A . . 119.5 ?
C5 C6 C7 . . 119.2(3) ?
C5 C6 H6A . . 120.4 ?
C7 C6 H6A . . 120.4 ?
C8 C7 C6 . . 119.5(3) ?
C8 C7 H7A . . 120.3 ?
C6 C7 H7A . . 120.3 ?
C7 C8 C9 . . 119.3(3) ?
C7 C8 H8A . . 120.3 ?
C9 C8 H8A . . 120.3 ?
N1 C9 C8 . . 120.1(3) ?
N1 C9 H9A . . 119.9 ?
C8 C9 H9A . . 119.9 ?
C10 O5 Ca1 . . 139.1(2) yes
O6 C10 O5 . . 126.0(3) yes
O6 C10 C11 . . 119.9(3) ?
O5 C10 C11 . . 114.1(3) ?
N2 C11 C13 . . 112.3(2) ?
N2 C11 C10 . . 110.5(2) ?
C13 C11 C10 . . 111.7(3) ?
N2 C11 H11A . . 107.3 ?
C13 C11 H11A . . 107.3 ?
C10 C11 H11A . . 107.3 ?
C12 O7 Ca1 . 6_576 115.6(2) ?
O8 C12 O7 . . 123.1(4) yes
O8 C12 C13 . . 118.3(4) ?
O7 C12 C13 . . 118.5(3) ?
O8 C12 Ca1 . 6_576 80.5(2) ?
C13 C12 Ca1 . 6_576 160.4(2) ?
C12 C13 C11 . . 115.2(3) ?
C12 C13 H13A . . 108.5 ?
C11 C13 H13A . . 108.5 ?
C12 C13 H13B . . 108.5 ?
C11 C13 H13B . . 108.5 ?
H13A C13 H13B . . 107.5 ?
N2 C14 C15 . . 119.9(4) ?
N2 C14 H14A . . 120.1 ?
C15 C14 H14A . . 120.1 ?
C14 N2 C18 . . 120.3(3) ?
C14 N2 C11 . . 120.2(3) ?
C18 N2 C11 . . 119.5(3) ?
C16 C15 C14 . . 120.1(4) ?
C16 C15 H15A . . 120.0 ?
C14 C15 H15A . . 120.0 ?
C17 C16 C15 . . 119.4(4) ?
C17 C16 H16A . . 120.3 ?
C15 C16 H16A . . 120.3 ?
C16 C17 C18 . . 119.3(4) ?
C16 C17 H17A . . 120.3 ?
C18 C17 H17A . . 120.3 ?
N2 C18 C17 . . 121.0(3) ?
N2 C18 H18A . . 119.5 ?
C17 C18 H18A . . 119.5 ?
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
Ca1 O1 . 2.320(2) yes
Ca1 O5 . 2.335(2) yes
Ca1 O7 6_575 2.348(3) yes
Ca1 O1W . 2.352(3) yes
Ca1 O4 6_576 2.357(2) yes
Ca1 O2W . 2.421(3) yes
Ca1 C12 6_575 3.100(4) ?
O1W H10A . 0.8890 ?
O1W H10B . 0.9814 ?
O2W H20A . 0.8066 ?
O2W H20B . 0.8721 ?
O3W H30A . 0.8990 ?
O4W H40A . 0.8738 ?
O4W H40B . 0.8271 ?
O5W H50A . 0.9252 ?
O5W H50B . 0.9178 ?
O1 C1 . 1.263(3) yes
O2 C1 . 1.240(4) yes
C1 C2 . 1.551(4) ?
C2 N1 . 1.483(3) ?
C2 C4 . 1.523(4) ?
C2 H2A . 0.9800 ?
O3 C3 . 1.244(4) yes
O4 C3 . 1.245(4) yes
O4 Ca1 6_575 2.357(2) ?
C3 C4 . 1.536(4) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
N1 C9 . 1.343(4) ?
N1 C5 . 1.349(4) ?
C5 C6 . 1.358(4) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.386(5) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.377(5) ?
C7 H7A . 0.9300 ?
C8 C9 . 1.381(4) ?
C8 H8A . 0.9300 ?
C9 H9A . 0.9300 ?
O5 C10 . 1.259(4) yes
O6 C10 . 1.235(4) yes
C10 C11 . 1.549(4) ?
C11 N2 . 1.487(4) ?
C11 C13 . 1.524(4) ?
C11 H11A . 0.9800 ?
O7 C12 . 1.248(5) yes
O7 Ca1 6_576 2.348(3) ?
O8 C12 . 1.245(4) yes
C12 C13 . 1.517(5) ?
C12 Ca1 6_576 3.100(4) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C14 N2 . 1.350(4) ?
C14 C15 . 1.377(5) ?
C14 H14A . 0.9300 ?
N2 C18 . 1.350(4) ?
C15 C16 . 1.376(6) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.368(6) ?
C16 H16A . 0.9300 ?
C17 C18 . 1.373(5) ?
C17 H17A . 0.9300 ?
C18 H18A . 0.9300 ?
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
_geom_hbond_publ_flag
O1W H10A O4W 7_565 0.89 1.84 2.730(4) 179 y
O1W H10B O3 6_576 0.98 1.80 2.715(4) 154 y
O2W H20A O3W . 0.81 2.14 2.951(4) 178 y
O2W H20B O8 2 0.87 1.92 2.771(4) 166 y
O3W H30A O2 5_565 0.90 2.05 2.935(3) 167 y
O4W H40A O3 . 0.87 1.81 2.672(4) 170 y
O4W H40B O5W 4 0.83 1.99 2.798(4) 165 y
O5W H50A O6 . 0.93 1.84 2.761(4) 174 y
O5W H50B O4W 6_566 0.92 1.96 2.845(4) 162 y
