#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/26/2212699.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_2212699
loop_
_publ_author_name
'Nie, Xu-Liang'
'Wen, Hui-Liang'
'Wu, Zi-Sheng'
'Liu, Da-Bo'
'Liu, Chong-Bo'
_publ_section_title
Diaquabis(5-carboxy-2-methyl-1H-imidazole-4-carboxylato-κ²N³,O⁴)cadmium(II)
_journal_coeditor_code           SJ2219
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m753
_journal_page_last               m755
_journal_paper_doi               10.1107/S1600536807006472
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cd (C6 H7 N2 O5)2]'
_chemical_formula_moiety         'C12 H14 Cd N4 O10'
_chemical_formula_sum            'C12 H14 Cd N4 O10'
_chemical_formula_weight         486.67
_chemical_name_systematic
;
diaquabis[5-carboxy-2-methyl-1H-imidazole-4-carboxylato-
κ²N³,O⁴]cadmium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.957(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0540(14)
_cell_length_b                   9.2501(12)
_cell_length_c                   7.4506(10)
_cell_measurement_reflns_used    2435
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.2
_cell_volume                     818.23(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 2005)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9684
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.548
_refine_diff_density_min         -0.416
_refine_ls_extinction_coef       0.033(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1929
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0365P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                1605
_reflns_number_total             1929
_reflns_threshold_expression     'I>2σ (I)'
_cod_data_source_file            sj2219.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212699
_cod_database_fobs_code          2212699
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
Cd Cd1 0.5000 0.5000 1.0000 0.00937(10) Uani d S 1
O O1 0.43259(9) 0.26469(12) 1.01015(15) 0.0129(3) Uani d . 1
O O2 0.29496(9) 0.11477(13) 0.88841(15) 0.0133(3) Uani d . 1
O O3 0.10072(10) 0.12804(14) 0.69348(18) 0.0195(3) Uani d D 1
H H3 0.1627(15) 0.113(2) 0.761(3) 0.023 Uiso d D 1
O O4 -0.00625(10) 0.30220(16) 0.5515(2) 0.0226(3) Uani d . 1
O O5 0.46972(12) 0.53924(16) 1.28686(18) 0.0182(3) Uani d D 1
H H5A 0.4174(19) 0.4970(17) 1.334(4) 0.022 Uiso d D 1
H H5B 0.5029(15) 0.603(2) 1.355(2) 0.022 Uiso d D 1
N N1 0.31039(15) 0.50408(12) 0.8737(2) 0.0106(3) Uani d . 1
N N2 0.14321(16) 0.51737(15) 0.7025(3) 0.0137(4) Uani d . 1
H H2 0.0868 0.5508 0.6360 0.016 Uiso d R 1
C C1 0.23308(14) 0.59308(19) 0.7858(2) 0.0128(4) Uani d . 1
C C2 0.26811(14) 0.36681(19) 0.8445(2) 0.0104(3) Uani d . 1
C C3 0.16232(13) 0.37380(19) 0.7361(2) 0.0112(3) Uani d . 1
C C4 0.24189(15) 0.75314(18) 0.7767(3) 0.0195(4) Uani d . 1
H H4A 0.3084 0.7792 0.7244 0.029 Uiso calc R 1
H H4B 0.2489 0.7937 0.8997 0.029 Uiso calc R 1
H H4C 0.1742 0.7920 0.7000 0.029 Uiso calc R 1
C C5 0.33632(14) 0.24015(18) 0.9195(2) 0.0110(3) Uani d . 1
C C6 0.07894(14) 0.26467(19) 0.6537(2) 0.0154(4) 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'
Cd Cd -0.8075 1.2024 '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
O5 Cd1 O5 3_667 . 180.0
O5 Cd1 N1 3_667 3_667 94.15(6)
O5 Cd1 N1 . 3_667 85.86(6)
O5 Cd1 N1 3_667 . 85.85(6)
O5 Cd1 N1 . . 94.14(6)
N1 Cd1 N1 3_667 . 180.0
O5 Cd1 O1 3_667 . 89.71(5)
O5 Cd1 O1 . . 90.29(5)
N1 Cd1 O1 3_667 . 107.27(4)
N1 Cd1 O1 . . 72.73(4)
O5 Cd1 O1 3_667 3_667 90.29(5)
O5 Cd1 O1 . 3_667 89.71(5)
N1 Cd1 O1 3_667 3_667 72.73(4)
N1 Cd1 O1 . 3_667 107.27(4)
O1 Cd1 O1 . 3_667 180.0
C5 O1 Cd1 . . 116.47(10)
C6 O3 H3 . . 114.9(15)
Cd1 O5 H5A . . 124.0(17)
Cd1 O5 H5B . . 123.4(13)
H5A O5 H5B . . 112.3(18)
C1 N1 C2 . . 106.61(15)
C1 N1 Cd1 . . 140.28(12)
C2 N1 Cd1 . . 111.27(11)
C1 N2 C3 . . 108.93(15)
C1 N2 H2 . . 126.4
C3 N2 H2 . . 124.6
N1 C1 N2 . . 110.16(16)
N1 C1 C4 . . 126.18(16)
N2 C1 C4 . . 123.66(15)
N1 C2 C3 . . 109.15(15)
N1 C2 C5 . . 120.31(15)
C3 C2 C5 . . 130.50(16)
N2 C3 C2 . . 105.15(15)
N2 C3 C6 . . 120.43(15)
C2 C3 C6 . . 134.35(16)
C1 C4 H4A . . 109.5
C1 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C1 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
O1 C5 O2 . . 124.06(15)
O1 C5 C2 . . 117.34(15)
O2 C5 C2 . . 118.59(14)
O4 C6 O3 . . 121.94(16)
O4 C6 C3 . . 120.22(16)
O3 C6 C3 . . 117.84(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cd1 O5 3_667 2.2589(14)
Cd1 O5 . 2.2589(14)
Cd1 N1 3_667 2.3167(18)
Cd1 N1 . 2.3167(18)
Cd1 O1 . 2.3292(12)
Cd1 O1 3_667 2.3292(12)
O1 C5 . 1.2582(19)
O2 C5 . 1.268(2)
O3 C6 . 1.314(2)
O3 H3 . 0.836(17)
O4 C6 . 1.218(2)
O5 H5A . 0.87(2)
O5 H5B . 0.833(16)
N1 C1 . 1.328(2)
N1 C2 . 1.372(2)
N2 C1 . 1.348(2)
N2 C3 . 1.364(2)
N2 H2 . 0.8287
C1 C4 . 1.487(2)
C2 C3 . 1.388(2)
C2 C5 . 1.484(2)
C3 C6 . 1.481(2)
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
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
N2 H2 O4 3_566 0.83 2.07 2.830(2) 152.9 yes
O5 H5B O1 2_657 0.833(16) 1.894(17) 2.7216(17) 173(2) yes
O5 H5A O2 4_566 0.87(2) 1.903(18) 2.7551(19) 168(2) yes
O3 H3 O2 . 0.836(17) 1.710(17) 2.5358(16) 169(2) yes
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
O5 Cd1 O1 C5 3_667 -73.79(11)
O5 Cd1 O1 C5 . 106.20(11)
N1 Cd1 O1 C5 3_667 -168.04(11)
N1 Cd1 O1 C5 . 11.95(11)
O5 Cd1 N1 C1 3_667 -81.3(2)
O5 Cd1 N1 C1 . 98.7(2)
O1 Cd1 N1 C1 . -172.3(2)
O1 Cd1 N1 C1 3_667 7.7(2)
O5 Cd1 N1 C2 3_667 80.31(13)
O5 Cd1 N1 C2 . -99.69(13)
O1 Cd1 N1 C2 . -10.67(12)
O1 Cd1 N1 C2 3_667 169.33(12)
C2 N1 C1 N2 . 0.2(2)
Cd1 N1 C1 N2 . 162.30(16)
C2 N1 C1 C4 . -179.38(15)
Cd1 N1 C1 C4 . -17.3(3)
C3 N2 C1 N1 . -0.2(2)
C3 N2 C1 C4 . 179.35(16)
C1 N1 C2 C3 . -0.1(2)
Cd1 N1 C2 C3 . -167.92(11)
C1 N1 C2 C5 . 177.78(14)
Cd1 N1 C2 C5 . 9.9(2)
C1 N2 C3 C2 . 0.2(2)
C1 N2 C3 C6 . -177.27(15)
N1 C2 C3 N2 . -0.1(2)
C5 C2 C3 N2 . -177.63(17)
N1 C2 C3 C6 . 176.86(18)
C5 C2 C3 C6 . -0.7(3)
Cd1 O1 C5 O2 . 168.90(12)
Cd1 O1 C5 C2 . -10.84(18)
N1 C2 C5 O1 . 0.4(2)
C3 C2 C5 O1 . 177.72(17)
N1 C2 C5 O2 . -179.38(16)
C3 C2 C5 O2 . -2.0(3)
N2 C3 C6 O4 . 1.8(3)
C2 C3 C6 O4 . -174.79(19)
N2 C3 C6 O3 . -178.76(16)
C2 C3 C6 O3 . 4.7(3)
