#------------------------------------------------------------------------------
#$Date: 2016-08-17 04:16:35 +0300 (Wed, 17 Aug 2016) $
#$Revision: 185836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/18/2241815.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_2241815
loop_
_publ_author_name
'Alfonso, Monserrat'
'Stoeckli-Evans, Helen'
_publ_section_title
;
 A two-dimensional CdII coordination polymer:
 poly[diaqua[μ₃-5,6-bis(pyridin-2-yl)pyrazine-2,3-dicarboxylato-κ⁵O²:O³:O³,N⁴,N⁵]cadmium]
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1297
_journal_page_last               1300
_journal_paper_doi               10.1107/S2056989016012858
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Cd (C16 H8 N4 O4) (H2 O)2]'
_chemical_formula_moiety         'C16 H12 Cd N4 O6'
_chemical_formula_sum            'C16 H12 Cd N4 O6'
_chemical_formula_weight         468.70
_chemical_name_systematic
Poly[diaqua[μ₃-5,6-bis(pyridin-2-yl)pyrazine-2,3-dicarboxylato-κ⁵O²:O³:O³,N⁴,N⁵]cadmium]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 96.236(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6854(12)
_cell_length_b                   7.0799(6)
_cell_length_c                   13.4537(10)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     1579.9(2)
_computing_cell_refinement
;
CELL in IPDS-I (Stoe & Cie, 2004)
;
_computing_data_collection
;
EXPOSE in IPDS-I (Stoe & Cie, 2004)
;
_computing_data_reduction
;
INTEGRATE in IPDS-I (Stoe & Cie, 2004)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015), PLATON (Spek, 2009) and
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '1 circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 1 image plate'
_diffrn_measurement_method       'φ rotation'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1294
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11782
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.924
_diffrn_reflns_theta_min         2.456
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(MULABS; Spek, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.587
_refine_ls_extinction_coef       0.00055(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   0.747
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3056
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.747
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0062P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                1781
_reflns_number_total             3056
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            pk2589sup1.cif
_cod_data_source_block           I
_cod_database_code               2241815
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_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_occupancy
Cd Cd1 0.39911(3) 0.63678(6) 0.47689(3) 0.01231(13) Uani d 1
O O1 0.4663(2) 0.3932(6) 0.5741(2) 0.0160(9) Uani d 1
O O2 0.4579(2) 0.1638(6) 0.6875(3) 0.0266(10) Uani d 1
O O3 0.3636(2) 0.1259(6) 0.8712(2) 0.0207(9) Uani d 1
O O4 0.3010(3) -0.0413(6) 0.7454(3) 0.0436(14) Uani d 1
O O1W 0.4770(3) 0.8162(6) 0.5928(3) 0.0412(13) Uani d 1
H H1WA 0.520(2) 0.780(9) 0.623(4) 0.062 Uiso d 1
H H1WB 0.457(3) 0.898(7) 0.628(4) 0.062 Uiso d 1
O O2W 0.3837(2) 0.8219(5) 0.3341(2) 0.0189(10) Uani d 1
H H2WA 0.355(2) 0.766(7) 0.287(3) 0.028 Uiso d 1
H H2WB 0.4295(16) 0.833(8) 0.312(3) 0.028 Uiso d 1
N N1 0.3193(3) 0.5188(6) 0.6031(3) 0.0130(10) Uani d 1
N N2 0.2284(3) 0.3495(7) 0.7347(3) 0.0156(10) Uani d 1
N N3 0.2853(2) 0.8351(6) 0.5067(3) 0.0131(10) Uani d 1
N N4 0.0603(3) 0.5341(6) 0.6152(3) 0.0222(12) Uani d 1
C C1 0.2472(3) 0.5920(7) 0.6161(3) 0.0096(12) Uani d 1
C C2 0.2003(3) 0.4982(7) 0.6816(4) 0.0128(13) Uani d 1
C C3 0.3478(3) 0.3673(9) 0.6546(3) 0.0100(10) Uani d 1
C C4 0.3025(3) 0.2842(7) 0.7250(4) 0.0102(13) Uani d 1
C C5 0.2290(3) 0.7774(7) 0.5650(4) 0.0122(13) Uani d 1
C C6 0.1657(3) 0.8955(8) 0.5818(3) 0.0186(14) Uani d 1
H H6 0.1260 0.8536 0.6211 0.022 Uiso calc 1
C C7 0.1608(4) 1.0747(7) 0.5410(4) 0.0196(14) Uani d 1
H H7 0.1174 1.1544 0.5516 0.024 Uiso calc 1
C C8 0.2194(3) 1.1351(9) 0.4850(3) 0.0166(11) Uani d 1
H H8 0.2175 1.2573 0.4576 0.020 Uiso calc 1
C C9 0.2815(3) 1.0138(7) 0.4696(4) 0.0156(13) Uani d 1
H H9 0.3224 1.0560 0.4322 0.019 Uiso calc 1
C C10 0.1146(4) 0.5462(7) 0.6958(4) 0.0179(14) Uani d 1
C C11 0.0946(4) 0.5917(8) 0.7907(4) 0.0249(15) Uani d 1
H H11 0.1347 0.6018 0.8453 0.030 Uiso calc 1
C C12 0.0141(4) 0.6216(10) 0.8025(4) 0.0285(14) Uani d 1
H H12 -0.0016 0.6492 0.8660 0.034 Uiso calc 1
C C13 -0.0426(4) 0.6106(9) 0.7204(5) 0.0333(16) Uani d 1
H H13 -0.0974 0.6328 0.7263 0.040 Uiso calc 1
C C14 -0.0169(4) 0.5661(8) 0.6298(5) 0.0294(17) Uani d 1
H H14 -0.0560 0.5574 0.5741 0.035 Uiso calc 1
C C15 0.4309(3) 0.3025(7) 0.6364(4) 0.0140(14) Uani d 1
C C16 0.3259(3) 0.1061(8) 0.7857(4) 0.0146(13) 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'
Cd Cd -0.8075 1.2024 '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'
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
Cd1 O1 Cd1 . 3_666 107.74(13) y
O1W Cd1 O3 . 4_565 157.41(15) y
O1 Cd1 O1 . 3_666 72.26(13) y
O1 Cd1 N1 . . 67.98(13) y
N1 Cd1 N3 . . 65.40(14) y
O2W Cd1 N3 . . 78.01(13) y
O2W Cd1 O1 . 3_666 80.65(13) y
O1W Cd1 O2W . . 104.67(16) y
O1W Cd1 O1 . . 80.18(15) y
O1W Cd1 N1 . . 91.62(16) y
O1W Cd1 N3 . . 87.87(15) y
O1W Cd1 O1 . 3_666 76.59(15) y
O2W Cd1 O3 . 4_565 87.05(13) y
O1 Cd1 O3 . 4_565 80.38(12) y
O3 Cd1 N1 4_565 . 91.67(13) y
O3 Cd1 O1 4_565 3_666 86.60(12) y
O3 Cd1 N3 4_565 . 113.74(13) y
O2W Cd1 N1 . . 139.31(15) ?
O2W Cd1 O1 . . 150.65(13) ?
N1 Cd1 O1 . 3_666 139.91(14) ?
O1 Cd1 N3 . . 131.34(12) ?
O1 Cd1 N3 3_666 . 149.40(14) ?
C15 O1 Cd1 . . 120.8(3) ?
C15 O1 Cd1 . 3_666 131.4(4) ?
C16 O3 Cd1 . 4_566 121.8(4) ?
Cd1 O1W H1WA . . 124(4) ?
Cd1 O1W H1WB . . 122(4) ?
H1WA O1W H1WB . . 109(3) ?
Cd1 O2W H2WA . . 111(4) ?
Cd1 O2W H2WB . . 109(4) ?
H2WA O2W H2WB . . 104(3) ?
C3 N1 C1 . . 121.2(4) ?
C3 N1 Cd1 . . 116.7(3) ?
C1 N1 Cd1 . . 121.9(3) ?
C2 N2 C4 . . 119.7(4) ?
C5 N3 C9 . . 119.1(4) ?
C5 N3 Cd1 . . 121.8(3) ?
C9 N3 Cd1 . . 118.9(3) ?
C10 N4 C14 . . 116.5(5) ?
N1 C1 C2 . . 117.9(5) ?
N1 C1 C5 . . 114.8(4) ?
C2 C1 C5 . . 127.0(5) ?
N2 C2 C1 . . 121.6(5) ?
N2 C2 C10 . . 113.3(4) ?
C1 C2 C10 . . 125.1(5) ?
N1 C3 C4 . . 120.0(5) ?
N1 C3 C15 . . 116.3(4) ?
C4 C3 C15 . . 123.6(5) ?
N2 C4 C3 . . 119.4(5) ?
N2 C4 C16 . . 114.6(4) ?
C3 C4 C16 . . 125.6(5) ?
N3 C5 C6 . . 120.2(5) ?
N3 C5 C1 . . 114.3(5) ?
C6 C5 C1 . . 125.1(5) ?
C7 C6 C5 . . 120.3(5) ?
C7 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C8 C7 C6 . . 119.4(5) ?
C8 C7 H7 . . 120.3 ?
C6 C7 H7 . . 120.3 ?
C7 C8 C9 . . 118.9(5) ?
C7 C8 H8 . . 120.6 ?
C9 C8 H8 . . 120.6 ?
N3 C9 C8 . . 122.1(5) ?
N3 C9 H9 . . 119.0 ?
C8 C9 H9 . . 119.0 ?
N4 C10 C11 . . 123.3(5) ?
N4 C10 C2 . . 116.9(5) ?
C11 C10 C2 . . 119.7(5) ?
C12 C11 C10 . . 118.2(6) ?
C12 C11 H11 . . 120.9 ?
C10 C11 H11 . . 120.9 ?
C13 C12 C11 . . 119.3(5) ?
C13 C12 H12 . . 120.4 ?
C11 C12 H12 . . 120.4 ?
C14 C13 C12 . . 118.2(6) ?
C14 C13 H13 . . 120.9 ?
C12 C13 H13 . . 120.9 ?
N4 C14 C13 . . 124.4(6) ?
N4 C14 H14 . . 117.8 ?
C13 C14 H14 . . 117.8 ?
O2 C15 O1 . . 126.9(5) ?
O2 C15 C3 . . 115.6(5) ?
O1 C15 C3 . . 117.5(5) ?
O4 C16 O3 . . 127.6(5) ?
O4 C16 C4 . . 114.3(5) ?
O3 C16 C4 . . 118.0(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
Cd1 O1 . 2.371(4) y
Cd1 O3 4_565 2.377(4) y
Cd1 N1 . 2.418(4) y
Cd1 O1 3_666 2.427(4) y
Cd1 N3 . 2.430(4) y
Cd1 O1W . 2.301(4) y
Cd1 O2W . 2.317(3) y
O1 C15 . 1.255(6) ?
O1 Cd1 3_666 2.427(3) ?
O2 C15 . 1.253(6) ?
O3 C16 . 1.258(6) ?
O3 Cd1 4_566 2.377(4) ?
O4 C16 . 1.227(6) ?
O1W H1WA . 0.82(2) ?
O1W H1WB . 0.837(19) ?
O2W H2WA . 0.847(19) ?
O2W H2WB . 0.852(19) ?
N1 C3 . 1.335(7) ?
N1 C1 . 1.339(6) ?
N2 C2 . 1.328(7) ?
N2 C4 . 1.341(7) ?
N3 C5 . 1.351(6) ?
N3 C9 . 1.359(6) ?
N4 C10 . 1.338(7) ?
N4 C14 . 1.344(7) ?
C1 C2 . 1.407(7) ?
C1 C5 . 1.498(7) ?
C2 C10 . 1.502(8) ?
C3 C4 . 1.403(7) ?
C3 C15 . 1.506(7) ?
C4 C16 . 1.530(7) ?
C5 C6 . 1.384(7) ?
C6 C7 . 1.381(7) ?
C6 H6 . 0.9400 ?
C7 C8 . 1.366(7) ?
C7 H7 . 0.9400 ?
C8 C9 . 1.378(7) ?
C8 H8 . 0.9400 ?
C9 H9 . 0.9400 ?
C10 C11 . 1.392(7) ?
C11 C12 . 1.386(8) ?
C11 H11 . 0.9400 ?
C12 C13 . 1.376(8) ?
C12 H12 . 0.9400 ?
C13 C14 . 1.373(8) ?
C13 H13 . 0.9400 ?
C14 H14 . 0.9400 ?
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 H1WA O3 2_656 0.82(2) 2.22(3) 2.974(6) 152(5)
O1W H1WB O2 1_565 0.84(2) 2.05(4) 2.805(6) 150(7)
O2W H2WA O4 4_565 0.85(2) 1.88(3) 2.630(6) 146(5)
O2W H2WB O2 3_666 0.85(2) 1.88(2) 2.692(5) 159(5)
C9 H9 O3 4_575 0.94 2.52 3.245(6) 134
C14 H14 N4 3_566 0.94 2.62 3.372(8) 137
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
C3 N1 C1 C2 . -3.4(7)
Cd1 N1 C1 C2 . 171.5(3)
C3 N1 C1 C5 . 171.2(4)
Cd1 N1 C1 C5 . -13.9(6)
C4 N2 C2 C1 . -1.1(8)
C4 N2 C2 C10 . 176.2(5)
N1 C1 C2 N2 . 4.7(7)
C5 C1 C2 N2 . -169.2(5)
N1 C1 C2 C10 . -172.3(5)
C5 C1 C2 C10 . 13.8(8)
C1 N1 C3 C4 . -1.2(7)
Cd1 N1 C3 C4 . -176.3(4)
C1 N1 C3 C15 . -177.7(4)
Cd1 N1 C3 C15 . 7.1(5)
C2 N2 C4 C3 . -3.6(7)
C2 N2 C4 C16 . -176.7(5)
N1 C3 C4 N2 . 4.8(8)
C15 C3 C4 N2 . -178.9(5)
N1 C3 C4 C16 . 177.2(5)
C15 C3 C4 C16 . -6.5(8)
C9 N3 C5 C6 . 3.7(7)
Cd1 N3 C5 C6 . 178.9(4)
C9 N3 C5 C1 . -169.7(4)
Cd1 N3 C5 C1 . 5.5(6)
N1 C1 C5 N3 . 5.2(6)
C2 C1 C5 N3 . 179.3(5)
N1 C1 C5 C6 . -167.8(5)
C2 C1 C5 C6 . 6.3(9)
N3 C5 C6 C7 . -1.5(8)
C1 C5 C6 C7 . 171.1(5)
C5 C6 C7 C8 . -0.8(8)
C6 C7 C8 C9 . 1.0(8)
C5 N3 C9 C8 . -3.6(7)
Cd1 N3 C9 C8 . -178.9(4)
C7 C8 C9 N3 . 1.2(8)
C14 N4 C10 C11 . -0.9(8)
C14 N4 C10 C2 . 176.1(5)
N2 C2 C10 N4 . -117.2(5)
C1 C2 C10 N4 . 60.0(7)
N2 C2 C10 C11 . 59.9(7)
C1 C2 C10 C11 . -122.9(6)
N4 C10 C11 C12 . 1.5(8)
C2 C10 C11 C12 . -175.3(5)
C10 C11 C12 C13 . -1.7(9)
C11 C12 C13 C14 . 1.3(10)
C10 N4 C14 C13 . 0.4(9)
C12 C13 C14 N4 . -0.7(10)
Cd1 O1 C15 O2 . 175.2(4)
Cd1 O1 C15 O2 3_666 -2.5(8)
Cd1 O1 C15 C3 . -6.1(6)
Cd1 O1 C15 C3 3_666 176.2(3)
N1 C3 C15 O2 . 177.9(4)
C4 C3 C15 O2 . 1.5(8)
N1 C3 C15 O1 . -0.9(7)
C4 C3 C15 O1 . -177.3(5)
Cd1 O3 C16 O4 4_566 1.6(8)
Cd1 O3 C16 C4 4_566 177.4(3)
N2 C4 C16 O4 . 82.7(6)
C3 C4 C16 O4 . -90.0(7)
N2 C4 C16 O3 . -93.7(6)
C3 C4 C16 O3 . 93.6(6)

_cod_database_fobs_code 2241815
