#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/00/2220044.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_2220044
loop_
_publ_author_name
'Jiang, Mei-Xiang'
'Feng, Yun-Long'
_publ_section_title
;
 Tetraaquabis(5-hydroxynicotinato-κN)cadmium(II)
;
_journal_coeditor_code           AT2660
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1517
_journal_paper_doi               10.1107/S1600536808035903
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cd (C6 H4 N O3 )2 (H2 O)4]'
_chemical_formula_moiety         'C12 H16 Cd N2 O10'
_chemical_formula_sum            'C12 H16 Cd N2 O10'
_chemical_formula_weight         460.68
_chemical_name_systematic
;
Tetraaquabis(5-hydroxynicotinato-κN)cadmium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.3770(10)
_cell_angle_beta                 68.1540(10)
_cell_angle_gamma                65.7170(10)
_cell_formula_units_Z            1
_cell_length_a                   7.21900(10)
_cell_length_b                   7.25100(10)
_cell_length_c                   8.92600(10)
_cell_measurement_reflns_used    5615
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.52
_cell_volume                     385.971(9)
_computing_cell_refinement       'SAINT  (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'XPREP  (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω scans'
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6067
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_T_max  .903
_exptl_absorpt_correction_T_min  .667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             230
_exptl_crystal_size_max          .270
_exptl_crystal_size_mid          .166
_exptl_crystal_size_min          .069
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1759
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0157
_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)+(0.0249P)²+0.1253P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0424
_reflns_number_gt                1754
_reflns_number_total             1759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            at2660.cif
_cod_data_source_block           I
_cod_original_cell_volume        385.972(9)
_cod_database_code               2220044
_cod_database_fobs_code          2220044
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.02626(6) Uani d S 1
O O1 0.8938(2) 0.7990(2) 0.32463(16) 0.0427(3) Uani d . 1
O O1W 0.2684(3) 0.3168(3) 1.07212(17) 0.0482(4) Uani d D 1
H H1WA 0.287(5) 0.249(4) 1.009(3) 0.072 Uiso d D 1
H H1WB 0.209(5) 0.270(4) 1.163(2) 0.072 Uiso d D 1
O O2 0.6901(2) 0.8709(2) 0.16430(15) 0.0429(3) Uani d . 1
O O2W 0.7595(2) 0.2074(2) 0.92481(18) 0.0478(4) Uani d D 1
H H2WA 0.881(3) 0.189(4) 0.865(3) 0.072 Uiso d D 1
H H2WB 0.762(5) 0.098(3) 0.994(3) 0.072 Uiso d D 1
O O3 0.0066(2) 0.7675(2) 0.58671(17) 0.0400(3) Uani d D 1
H H3 0.002(4) 0.785(4) 0.491(2) 0.053(7) Uiso d D 1
N N1 0.4459(2) 0.6297(2) 0.74305(16) 0.0264(3) Uani d . 1
C C1 0.5945(2) 0.6740(2) 0.60554(19) 0.0267(3) Uani d . 1
H H1A 0.7280 0.6483 0.6138 0.032 Uiso calc R 1
C C2 0.5560(2) 0.7568(2) 0.45137(18) 0.0245(3) Uani d . 1
C C3 0.3595(3) 0.7885(2) 0.43778(19) 0.0263(3) Uani d . 1
H H3A 0.3310 0.8402 0.3354 0.032 Uiso calc R 1
C C4 0.2061(2) 0.7415(2) 0.5802(2) 0.0270(3) Uani d . 1
C C5 0.2549(2) 0.6655(3) 0.73035(19) 0.0276(3) Uani d . 1
H H5A 0.1507 0.6383 0.8260 0.033 Uiso calc R 1
C C6 0.7273(3) 0.8123(2) 0.30121(19) 0.0288(3) Uani d . 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cd1 0.02499(9) 0.03841(10) 0.01604(8) -0.01493(7) -0.00552(6) -0.00099(6)
O1 0.0313(6) 0.0688(9) 0.0266(6) -0.0259(6) -0.0010(5) -0.0044(6)
O1W 0.0589(9) 0.0749(10) 0.0276(6) -0.0484(8) -0.0017(6) -0.0091(7)
O2 0.0587(8) 0.0592(8) 0.0199(6) -0.0385(7) -0.0088(5) 0.0028(5)
O2W 0.0368(7) 0.0424(7) 0.0347(7) -0.0075(6) 0.0072(6) 0.0013(6)
O3 0.0285(6) 0.0620(8) 0.0326(7) -0.0220(6) -0.0135(5) 0.0007(6)
N1 0.0258(6) 0.0362(7) 0.0187(6) -0.0141(5) -0.0068(5) -0.0018(5)
C1 0.0252(7) 0.0376(8) 0.0208(7) -0.0155(6) -0.0064(6) -0.0037(6)
C2 0.0278(7) 0.0271(7) 0.0195(7) -0.0128(6) -0.0046(6) -0.0033(5)
C3 0.0312(7) 0.0288(7) 0.0207(7) -0.0120(6) -0.0109(6) -0.0005(5)
C4 0.0249(7) 0.0305(7) 0.0281(7) -0.0112(6) -0.0107(6) -0.0026(6)
C5 0.0254(7) 0.0358(8) 0.0219(7) -0.0143(6) -0.0053(6) -0.0023(6)
C6 0.0340(8) 0.0319(8) 0.0206(7) -0.0166(6) -0.0025(6) -0.0038(6)
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
O2W Cd1 O2W . 2_667 180.0
O2W Cd1 N1 . 2_667 87.79(5)
O2W Cd1 N1 2_667 2_667 92.21(5)
O2W Cd1 N1 . . 92.21(5)
O2W Cd1 N1 2_667 . 87.79(5)
N1 Cd1 N1 2_667 . 180.0000(10)
O2W Cd1 O1W . . 85.72(6)
O2W Cd1 O1W 2_667 . 94.28(6)
N1 Cd1 O1W 2_667 . 90.57(5)
N1 Cd1 O1W . . 89.43(5)
O2W Cd1 O1W . 2_667 94.28(6)
O2W Cd1 O1W 2_667 2_667 85.72(6)
N1 Cd1 O1W 2_667 2_667 89.43(5)
N1 Cd1 O1W . 2_667 90.57(5)
O1W Cd1 O1W . 2_667 180.0
Cd1 O1W H1WA . . 117(2)
Cd1 O1W H1WB . . 127(2)
H1WA O1W H1WB . . 110(2)
Cd1 O2W H2WA . . 131(2)
Cd1 O2W H2WB . . 117(2)
H2WA O2W H2WB . . 105(2)
C4 O3 H3 . . 108.2(19)
C5 N1 C1 . . 118.64(13)
C5 N1 Cd1 . . 117.86(10)
C1 N1 Cd1 . . 123.49(10)
N1 C1 C2 . . 122.29(14)
N1 C1 H1A . . 118.9
C2 C1 H1A . . 118.9
C3 C2 C1 . . 118.97(14)
C3 C2 C6 . . 121.06(14)
C1 C2 C6 . . 119.96(14)
C2 C3 C4 . . 118.68(14)
C2 C3 H3A . . 120.7
C4 C3 H3A . . 120.7
O3 C4 C5 . . 115.78(14)
O3 C4 C3 . . 125.40(14)
C5 C4 C3 . . 118.81(14)
N1 C5 C4 . . 122.55(14)
N1 C5 H5A . . 118.7
C4 C5 H5A . . 118.7
O2 C6 O1 . . 125.02(15)
O2 C6 C2 . . 117.26(15)
O1 C6 C2 . . 117.71(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cd1 O2W . 2.2830(14)
Cd1 O2W 2_667 2.2830(14)
Cd1 N1 2_667 2.2831(13)
Cd1 N1 . 2.2831(13)
Cd1 O1W . 2.3291(13)
Cd1 O1W 2_667 2.3291(13)
O1 C6 . 1.255(2)
O1W H1WA . 0.809(17)
O1W H1WB . 0.794(17)
O2 C6 . 1.244(2)
O2W H2WA . 0.823(17)
O2W H2WB . 0.822(17)
O3 C4 . 1.3543(19)
O3 H3 . 0.830(17)
N1 C5 . 1.335(2)
N1 C1 . 1.3411(19)
C1 C2 . 1.387(2)
C1 H1A . 0.9300
C2 C3 . 1.385(2)
C2 C6 . 1.517(2)
C3 C4 . 1.389(2)
C3 H3A . 0.9300
C4 C5 . 1.386(2)
C5 H5A . 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
O1W H1WA O2 2_666 0.809(17) 1.941(17) 2.742(2) 171(3)
O1W H1WB O3 2_567 0.794(17) 2.201(18) 2.9728(19) 164(3)
O2W H2WA O1 2_766 0.823(17) 1.867(18) 2.6556(18) 160(3)
O2W H2WB O2 1_546 0.822(17) 1.933(17) 2.7349(19) 165(3)
O3 H3 O1 1_455 0.830(17) 1.878(19) 2.6637(19) 157(3)
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
O2W Cd1 N1 C5 . 119.15(12)
O2W Cd1 N1 C5 2_667 -60.85(12)
O1W Cd1 N1 C5 . 33.45(13)
O1W Cd1 N1 C5 2_667 -146.55(13)
O2W Cd1 N1 C1 . -61.78(13)
O2W Cd1 N1 C1 2_667 118.22(13)
O1W Cd1 N1 C1 . -147.47(13)
O1W Cd1 N1 C1 2_667 32.53(13)
C5 N1 C1 C2 . 0.5(2)
Cd1 N1 C1 C2 . -178.62(11)
N1 C1 C2 C3 . -2.2(2)
N1 C1 C2 C6 . 177.42(14)
C1 C2 C3 C4 . 1.8(2)
C6 C2 C3 C4 . -177.83(14)
C2 C3 C4 O3 . 178.81(15)
C2 C3 C4 C5 . 0.2(2)
C1 N1 C5 C4 . 1.7(2)
Cd1 N1 C5 C4 . -179.16(12)
O3 C4 C5 N1 . 179.22(15)
C3 C4 C5 N1 . -2.1(2)
C3 C2 C6 O2 . -5.8(2)
C1 C2 C6 O2 . 174.61(15)
C3 C2 C6 O1 . 173.06(16)
C1 C2 C6 O1 . -6.6(2)
