#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/05/2230575.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_2230575
loop_
_publ_author_name
'Zhang, Gang'
'Wang, Yong'
_publ_section_title
;
 Diaquabis(4-carboxy-2-ethyl-1H-imidazole-5-carboxylato-κ²N³,O⁴)cadmium
 dihydrate
;
_journal_coeditor_code           BH2359
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m890
_journal_paper_doi               10.1107/S1600536811021428
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cd (C7 H7 N2 O4)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C14 H18 Cd N4 O10, 2(H2 O)'
_chemical_formula_sum            'C14 H22 Cd N4 O12'
_chemical_formula_weight         550.76
_chemical_name_systematic
;
Diaquabis(4-carboxy-2-ethyl-1H-imidazole-5-carboxylato-
κ²N³,O⁴)cadmium dihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.844(2)
_cell_length_b                   17.084(3)
_cell_length_c                   12.855(3)
_cell_measurement_reflns_used    1702
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.449
_cell_volume                     2113.0(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8379
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.8263
_exptl_absorpt_correction_T_min  0.7333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.784
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1898
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0280
_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)+(0.0164P)²+5.0177P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                1560
_reflns_number_total             1898
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bh2359.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2230575
_cod_database_fobs_code          2230575
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_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
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd1 0.0000 0.20278(3) 0.2500 0.03340(14) Uani d S 1 2 . .
O O1 0.5880(2) 0.14665(16) 0.0777(2) 0.0399(7) Uani d . 1 1 . .
O O2 0.5052(3) 0.26839(16) 0.0774(2) 0.0439(7) Uani d . 1 1 . .
O O3 0.3063(3) 0.33738(16) 0.1245(2) 0.0470(7) Uani d . 1 1 . .
H H3 0.3668 0.3140 0.1034 0.071 Uiso d R 1 1 . .
O O4 0.1229(2) 0.30656(16) 0.1896(2) 0.0414(6) Uani d . 1 1 . .
N N1 0.3597(3) 0.08847(17) 0.1520(2) 0.0288(7) Uani d . 1 1 . .
H H9 0.4044 0.0442 0.1391 0.035 Uiso d R 1 1 . .
N N2 0.1837(3) 0.14937(18) 0.1946(2) 0.0287(7) Uani d . 1 1 . .
C C1 0.2678(3) 0.2036(2) 0.1605(2) 0.0244(7) Uani d . 1 1 . .
C C2 0.3782(3) 0.1654(2) 0.1332(3) 0.0266(8) Uani d . 1 1 . .
C C3 0.2420(3) 0.0805(2) 0.1895(3) 0.0311(8) Uani d . 1 1 . .
C C4 0.1894(4) 0.0046(3) 0.2202(4) 0.0506(11) Uani d . 1 1 . .
H H4A 0.2676 -0.0260 0.2578 0.061 Uiso calc R 1 1 . .
H H4B 0.1289 0.0145 0.2693 0.061 Uiso calc R 1 1 . .
C C5 0.1137(8) -0.0418(4) 0.1323(6) 0.127(3) Uani d . 1 1 . .
H H5A 0.0380 -0.0115 0.0927 0.190 Uiso calc R 1 1 . .
H H5B 0.0780 -0.0880 0.1595 0.190 Uiso calc R 1 1 . .
H H5C 0.1750 -0.0565 0.0867 0.190 Uiso calc R 1 1 . .
C C6 0.5001(3) 0.1949(2) 0.0929(3) 0.0316(8) Uani d . 1 1 . .
C C7 0.2289(3) 0.2871(2) 0.1586(3) 0.0320(8) Uani d . 1 1 . .
O O1W -0.1380(3) 0.1871(2) 0.0846(2) 0.0691(11) Uani d D 1 1 . .
H H2W -0.2184 0.1706 0.0594 0.104 Uiso d RD 1 1 . .
H H1W -0.1026 0.2090 0.0386 0.104 Uiso d RD 1 1 . .
O O2W -0.0139(3) 0.45120(19) 0.1075(3) 0.0695(10) Uani d D 1 1 . .
H H4W 0.0458 0.4235 0.1478 0.104 Uiso d RD 1 1 . .
H H3W -0.0307 0.4344 0.0448 0.104 Uiso d RD 1 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
N2 Cd1 N2 2 . 132.60(15) ?
N2 Cd1 O1W 2 . 83.59(10) ?
N2 Cd1 O1W . . 91.00(11) ?
N2 Cd1 O1W 2 2 91.00(11) ?
N2 Cd1 O1W . 2 83.59(10) ?
O1W Cd1 O1W . 2 166.5(2) ?
N2 Cd1 O4 2 . 154.13(10) ?
N2 Cd1 O4 . . 72.67(10) ?
O1W Cd1 O4 . . 91.54(10) ?
O1W Cd1 O4 2 . 98.55(11) ?
N2 Cd1 O4 2 2 72.67(10) ?
N2 Cd1 O4 . 2 154.13(10) ?
O1W Cd1 O4 . 2 98.55(11) ?
O1W Cd1 O4 2 2 91.54(10) ?
O4 Cd1 O4 . 2 83.03(12) ?
C7 O3 H3 . . 108.4 ?
C7 O4 Cd1 . . 115.4(2) ?
C3 N1 C2 . . 108.6(3) ?
C3 N1 H9 . . 117.7 ?
C2 N1 H9 . . 133.5 ?
C3 N2 C1 . . 106.7(3) ?
C3 N2 Cd1 . . 139.4(2) ?
C1 N2 Cd1 . . 113.7(2) ?
N2 C1 C2 . . 108.9(3) ?
N2 C1 C7 . . 119.0(3) ?
C2 C1 C7 . . 132.1(3) ?
N1 C2 C1 . . 105.8(3) ?
N1 C2 C6 . . 122.5(3) ?
C1 C2 C6 . . 131.7(3) ?
N2 C3 N1 . . 110.1(3) ?
N2 C3 C4 . . 126.1(3) ?
N1 C3 C4 . . 123.9(3) ?
C5 C4 C3 . . 114.9(4) ?
C5 C4 H4A . . 108.5 ?
C3 C4 H4A . . 108.5 ?
C5 C4 H4B . . 108.5 ?
C3 C4 H4B . . 108.5 ?
H4A C4 H4B . . 107.5 ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
O1 C6 O2 . . 125.3(3) ?
O1 C6 C2 . . 118.1(4) ?
O2 C6 C2 . . 116.6(3) ?
O4 C7 O3 . . 122.1(4) ?
O4 C7 C1 . . 119.1(3) ?
O3 C7 C1 . . 118.8(3) ?
Cd1 O1W H2W . . 136.5 ?
Cd1 O1W H1W . . 110.6 ?
H2W O1W H1W . . 112.2 ?
H4W O2W H3W . . 111.6 ?
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 N2 2 2.270(3) ?
Cd1 N2 . 2.270(3) ?
Cd1 O1W . 2.284(3) ?
Cd1 O1W 2 2.284(3) ?
Cd1 O4 . 2.368(3) ?
Cd1 O4 2 2.368(3) ?
O1 C6 . 1.239(4) ?
O2 C6 . 1.275(5) ?
O3 C7 . 1.284(4) ?
O3 H3 . 0.8096 ?
O4 C7 . 1.239(4) ?
N1 C3 . 1.353(4) ?
N1 C2 . 1.356(5) ?
N1 H9 . 0.9080 ?
N2 C3 . 1.317(5) ?
N2 C1 . 1.375(4) ?
C1 C2 . 1.375(5) ?
C1 C7 . 1.476(5) ?
C2 C6 . 1.491(5) ?
C3 C4 . 1.481(5) ?
C4 C5 . 1.450(7) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 H5A . 0.9600 ?
C5 H5B . 0.9600 ?
C5 H5C . 0.9600 ?
O1W H2W . 0.8388 ?
O1W H1W . 0.8355 ?
O2W H4W . 0.8424 ?
O2W H3W . 0.8381 ?
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
O3 H3 O2 . 0.81 1.66 2.468(4) 171.8 yes
O2W H4W O4 . 0.84 2.16 2.904(4) 146.6 yes
O2W H3W O1 7 0.84 2.08 2.874(4) 157.2 yes
O1W H1W O2 7 0.84 1.97 2.788(4) 164.5 yes
O1W H2W O1 1_455 0.84 2.01 2.768(3) 149.8 yes
N1 H9 O2W 3_545 0.91 1.86 2.771(4) 176.5 yes
