#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/19/2221920.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_2221920
loop_
_publ_author_name
'Natarajan, S.'
'Moovendaran, K.'
'Dhas, S. A. Martin Britto'
'Suresh, J.'
'Lakshman, P. L. Nilantha'
_publ_section_title
;
 Hexaaquacadmium(II) dipicrate monohydrate
;
_journal_coeditor_code           BQ2135
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m620
_journal_paper_doi               10.1107/S1600536809015049
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Cd (H2 O)6] (C6 H2 N3 O7)2, H2 O'
_chemical_formula_moiety         'Cd H12 O6 2+, 2(C6 H2 N3 O7 -), 2(H2 O)'
_chemical_formula_sum            'C12 H20 Cd N6 O22'
_chemical_formula_weight         712.75
_chemical_name_systematic
;
Hexaaquacadmium(II) dipicrate monohydrate
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ab'
_symmetry_space_group_name_H-M   'P b n b'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2823(2)
_cell_length_b                   13.2249(4)
_cell_length_c                   25.3798(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     2444.27(13)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1996)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius MACH-3'
_diffrn_measurement_method       ω-2θ
_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  0.0096
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2247
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.380
_refine_ls_extinction_coef       0.0029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2142
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0273
_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)+(0.0314P)²+3.7212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                1513
_reflns_number_total             2142
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bq2135.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2221920
_cod_database_fobs_code          2221920
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x-1/2, -y, 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_disorder_assembly
_atom_site_disorder_group
Cd Cd 0.0000 0.5000 0.0000 0.03236(15) Uani d S 1 . .
O O11 0.1978(4) 0.5718(3) 0.05990(11) 0.0393(7) Uani d . 1 . .
O O1 0.4465(5) 0.2509(2) 0.11321(10) 0.0581(9) Uani d . 1 . .
O O5 0.6784(4) 0.6893(2) 0.18800(10) 0.0430(7) Uani d . 1 . .
O O7 0.4862(4) 0.4516(2) 0.10554(9) 0.0390(7) Uani d . 1 . .
O O2 0.3391(4) 0.1969(2) 0.18648(10) 0.0435(7) Uani d . 1 . .
O O6 0.5121(4) 0.6525(2) 0.12019(9) 0.0415(7) Uani d . 1 . .
O O4 0.5772(5) 0.5100(2) 0.34801(10) 0.0463(7) Uani d . 1 . .
N N3 0.5092(4) 0.4393(2) 0.32448(11) 0.0297(7) Uani d . 1 . .
O O8 -0.0269(6) 0.3512(2) 0.04266(13) 0.0609(10) Uani d D 1 . .
O O9 0.2500(5) 0.4420(3) -0.03995(13) 0.0554(9) Uani d D 1 . .
O O3 0.4428(4) 0.3650(2) 0.34660(10) 0.0430(7) Uani d . 1 . .
O O10 0.5209(5) 0.3302(2) 0.00923(13) 0.0457(8) Uani d . 1 . .
N N2 0.5770(4) 0.6320(2) 0.16356(11) 0.0301(7) Uani d . 1 . .
C C4 0.5398(5) 0.5320(3) 0.24176(14) 0.0280(8) Uani d . 1 . .
H H4 0.5694 0.5898 0.2608 0.034 Uiso calc R 1 . .
N N1 0.4123(5) 0.2622(2) 0.15992(11) 0.0336(7) Uani d . 1 . .
C C2 0.4606(5) 0.3554(3) 0.23989(13) 0.0290(8) Uani d . 1 . .
H H2 0.4336 0.2958 0.2577 0.035 Uiso calc R 1 . .
C C3 0.5024(5) 0.4423(3) 0.26750(12) 0.0279(8) Uani d . 1 . .
C C6 0.4911(5) 0.4481(3) 0.15474(13) 0.0272(7) Uani d . 1 . .
C C1 0.4592(5) 0.3581(3) 0.18566(13) 0.0286(8) Uani d . 1 . .
C C5 0.5328(5) 0.5350(3) 0.18776(13) 0.0258(8) Uani d . 1 . .
H H8W 0.517(8) 0.337(5) 0.043(3) 0.09(2) Uiso d . 1 . .
H H1W 0.172(8) 0.607(4) 0.081(2) 0.07(2) Uiso d . 1 . .
H H3W -0.009(7) 0.350(4) 0.074(2) 0.065(16) Uiso d . 1 . .
H H5W 0.302(7) 0.475(4) -0.0643(19) 0.063(16) Uiso d . 1 . .
H H2W 0.276(8) 0.536(4) 0.0788(19) 0.067(17) Uiso d . 1 . .
H H6W 0.317(5) 0.402(3) -0.0255(15) 0.045(13) Uiso d D 1 . .
H H9W 0.612(8) 0.349(4) -0.0004(19) 0.06(2) Uiso d . 1 . .
H H4W -0.007(7) 0.297(2) 0.0302(19) 0.065(17) Uiso d 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
_geom_angle_publ_flag
O9 Cd O9 5_565 . 180.00(15) ?
O9 Cd O8 5_565 5_565 89.37(14) ?
O9 Cd O8 . 5_565 90.63(14) ?
O9 Cd O8 5_565 . 90.63(14) ?
O9 Cd O8 . . 89.37(14) ?
O8 Cd O8 5_565 . 180.00(16) ?
O9 Cd O11 5_565 . 93.97(13) ?
O9 Cd O11 . . 86.03(13) ?
O8 Cd O11 5_565 . 84.41(13) ?
O8 Cd O11 . . 95.59(13) ?
O9 Cd O11 5_565 5_565 86.03(13) ?
O9 Cd O11 . 5_565 93.97(13) ?
O8 Cd O11 5_565 5_565 95.59(13) ?
O8 Cd O11 . 5_565 84.41(13) ?
O11 Cd O11 . 5_565 180.00(11) ?
Cd O11 H1W . . 126(5) ?
Cd O11 H2W . . 123(3) ?
H1W O11 H2W . . 96(5) ?
O4 N3 O3 . . 123.4(3) ?
O4 N3 C3 . . 118.9(3) ?
O3 N3 C3 . . 117.7(3) ?
Cd O8 H3W . . 118(4) ?
Cd O8 H4W . . 126(4) ?
H3W O8 H4W . . 110(5) ?
Cd O9 H5W . . 122(3) ?
Cd O9 H6W . . 121(3) ?
H5W O9 H6W . . 113(5) ?
H8W O10 H9W . . 108(5) ?
O5 N2 O6 . . 123.3(3) ?
O5 N2 C5 . . 117.6(3) ?
O6 N2 C5 . . 119.1(3) ?
C5 C4 C3 . . 119.3(3) ?
C5 C4 H4 . . 120.4 ?
C3 C4 H4 . . 120.4 ?
O2 N1 O1 . . 122.7(3) ?
O2 N1 C1 . . 117.9(3) ?
O1 N1 C1 . . 119.4(3) ?
C1 C2 C3 . . 119.2(3) ?
C1 C2 H2 . . 120.4 ?
C3 C2 H2 . . 120.4 ?
C2 C3 C4 . . 121.2(3) ?
C2 C3 N3 . . 119.5(3) ?
C4 C3 N3 . . 119.3(3) ?
O7 C6 C1 . . 124.7(3) ?
O7 C6 C5 . . 123.5(3) ?
C1 C6 C5 . . 111.8(3) ?
C2 C1 C6 . . 124.3(3) ?
C2 C1 N1 . . 115.1(3) ?
C6 C1 N1 . . 120.5(3) ?
C4 C5 C6 . . 124.1(3) ?
C4 C5 N2 . . 115.9(3) ?
C6 C5 N2 . . 119.9(3) ?
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
Cd O9 5_565 2.221(3) ?
Cd O9 . 2.221(3) ?
Cd O8 5_565 2.255(3) ?
Cd O8 . 2.255(3) ?
Cd O11 . 2.299(3) ?
Cd O11 5_565 2.299(3) ?
O11 H1W . 0.73(5) ?
O11 H2W . 0.88(6) ?
O1 N1 . 1.220(4) ?
O5 N2 . 1.226(4) ?
O7 C6 . 1.250(4) ?
O2 N1 . 1.219(4) ?
O6 N2 . 1.228(4) ?
O4 N3 . 1.216(4) ?
N3 O3 . 1.231(4) ?
N3 C3 . 1.447(4) ?
O8 H3W . 0.79(5) ?
O8 H4W . 0.80(2) ?
O9 H5W . 0.85(5) ?
O9 H6W . 0.81(4) ?
O10 H8W . 0.87(7) ?
O10 H9W . 0.75(6) ?
N2 C5 . 1.459(5) ?
C4 C5 . 1.372(5) ?
C4 C3 . 1.382(5) ?
C4 H4 . 0.9300 ?
N1 C1 . 1.467(4) ?
C2 C1 . 1.377(5) ?
C2 C3 . 1.380(5) ?
C2 H2 . 0.9300 ?
C6 C1 . 1.444(5) ?
C6 C5 . 1.454(5) ?
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
O11 H1W O1 7_665 0.73(5) 2.25(6) 2.923(4) 155(6)
O8 H3W O3 4 0.79(5) 2.09(5) 2.882(4) 172(5)
O8 H4W O10 3_455 0.80(2) 1.96(2) 2.758(5) 171(5)
O9 H5W O6 5_665 0.85(5) 2.59(5) 2.951(4) 107(4)
O9 H5W O7 5_665 0.85(5) 2.10(5) 2.905(5) 159(5)
O10 H9W O11 5_665 0.75(6) 2.30(5) 2.993(5) 154(5)
C4 H4 O2 6_566 0.93 2.57 3.195(4) 124.9
O11 H2W O6 . 0.88(6) 2.54(5) 2.953(4) 109(4)
O11 H2W O7 . 0.88(6) 2.01(6) 2.877(4) 166(5)
O9 H6W O10 . 0.81(4) 1.97(2) 2.763(5) 167(5)
O10 H8W O1 . 0.87(7) 2.18(7) 2.891(4) 140(5)
O10 H8W O7 . 0.87(7) 2.20(7) 2.936(4) 142(6)
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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 C2 C3 C4 . . . . 1.1(6) ?
C1 C2 C3 N3 . . . . -178.2(3) ?
C5 C4 C3 C2 . . . . 0.8(6) ?
C5 C4 C3 N3 . . . . -179.8(3) ?
O4 N3 C3 C2 . . . . 167.0(3) ?
O3 N3 C3 C2 . . . . -14.0(5) ?
O4 N3 C3 C4 . . . . -12.3(5) ?
O3 N3 C3 C4 . . . . 166.7(3) ?
C3 C2 C1 C6 . . . . -2.9(6) ?
C3 C2 C1 N1 . . . . -179.7(3) ?
O7 C6 C1 C2 . . . . -178.4(4) ?
C5 C6 C1 C2 . . . . 2.5(5) ?
O7 C6 C1 N1 . . . . -1.8(6) ?
C5 C6 C1 N1 . . . . 179.1(3) ?
O2 N1 C1 C2 . . . . 16.5(5) ?
O1 N1 C1 C2 . . . . -163.9(4) ?
O2 N1 C1 C6 . . . . -160.4(3) ?
O1 N1 C1 C6 . . . . 19.2(5) ?
C3 C4 C5 C6 . . . . -1.1(5) ?
C3 C4 C5 N2 . . . . -179.0(3) ?
O7 C6 C5 C4 . . . . -179.6(4) ?
C1 C6 C5 C4 . . . . -0.4(5) ?
O7 C6 C5 N2 . . . . -1.8(5) ?
C1 C6 C5 N2 . . . . 177.4(3) ?
O5 N2 C5 C4 . . . . 26.6(5) ?
O6 N2 C5 C4 . . . . -153.5(3) ?
O5 N2 C5 C6 . . . . -151.4(3) ?
O6 N2 C5 C6 . . . . 28.5(5) ?
