#------------------------------------------------------------------------------
#$Date: 2016-02-20 21:30:07 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/22/2222290.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_2222290
loop_
_publ_author_name
'Yan, Liu-Shui'
'Huang, De-He'
'Liu, Chong-Bo'
_publ_section_title
;
 Poly[μ-5-ammonioisophthalato-aqua-μ-oxalato-dysprosium(III)]
;
_journal_coeditor_code           DN2450
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m750
_journal_paper_doi               10.1107/S1600536809019199
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Dy (C8 H6 N O4) (C2 O4) (H2 O)]'
_chemical_formula_moiety         'C10 H8 Dy N O9'
_chemical_formula_sum            'C10 H8 Dy N O9'
_chemical_formula_weight         448.67
_chemical_name_systematic
;
poly[μ-5-ammonioisophthalato-aqua-μ-oxalato-dysprosium(III)]
;
_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                 118.478(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.951(4)
_cell_length_b                   9.3967(18)
_cell_length_c                   13.598(3)
_cell_measurement_reflns_used    5702
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.46
_cell_volume                     2240.8(8)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.1092
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8393
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    6.723
_exptl_absorpt_correction_T_max  0.5676
_exptl_absorpt_correction_T_min  0.4992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.286
_refine_diff_density_min         -1.556
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0094P)²+0.8384P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                1901
_reflns_number_total             2089
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2450.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2222290
_cod_database_fobs_code          2222290
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_disorder_assembly
_atom_site_disorder_group
C C1 0.5101(3) 0.9321(4) 0.8770(5) 0.0176(11) Uani d . 1 . .
C C2 0.5866(3) 0.9047(4) 0.9083(4) 0.0168(10) Uani d . 1 . .
H H2 0.6038 0.8119 0.9121 0.020 Uiso calc R 1 . .
C C3 0.6362(2) 1.0187(5) 0.9335(4) 0.0161(10) Uani d . 1 . .
C C4 0.6139(3) 1.1553(5) 0.9341(4) 0.0198(10) Uani d . 1 . .
H H4 0.6489 1.2293 0.9532 0.024 Uiso calc R 1 . .
C C5 0.5376(2) 1.1837(4) 0.9057(4) 0.0159(9) Uani d . 1 . .
C C6 0.4854(3) 1.0707(4) 0.8733(4) 0.0154(10) Uani d . 1 . .
H H6 0.4340 1.0889 0.8492 0.018 Uiso calc R 1 . .
C C7 0.4569(3) 0.8075(5) 0.8484(4) 0.0170(10) Uani d . 1 . .
C C8 0.5160(3) 1.3320(4) 0.9189(4) 0.0171(10) Uani d . 1 . .
C C9 0.2265(2) 0.7844(4) 0.6760(4) 0.0143(9) Uani d . 1 . .
C C10 0.2352(2) 0.7786(4) 0.7938(4) 0.0142(9) Uani d . 1 . .
Dy Dy1 0.367163(11) 0.562032(19) 0.814740(18) 0.01134(10) Uani d . 1 . .
N N1 0.7158(2) 0.9903(4) 0.9663(4) 0.0198(9) Uani d . 1 . .
H H1A 0.7278 1.0315 0.9178 0.030 Uiso calc R 1 . .
H H1B 0.7231 0.8968 0.9667 0.030 Uiso calc R 1 . .
H H1C 0.7452 1.0254 1.0344 0.030 Uiso calc R 1 . .
O O1 0.48363(19) 0.6844(3) 0.8541(3) 0.0234(8) Uani d . 1 . .
O O2 0.38806(19) 0.8260(3) 0.8218(3) 0.0238(8) Uani d . 1 . .
O O3 0.56915(19) 1.4094(3) 0.9915(3) 0.0183(7) Uani d . 1 . .
O O4 0.44868(18) 1.3699(3) 0.8570(3) 0.0218(8) Uani d . 1 . .
O O5 0.26983(18) 0.6716(3) 0.8522(3) 0.0200(7) Uani d . 1 . .
O O6 0.26011(19) 0.6905(3) 0.6506(3) 0.0256(8) Uani d . 1 . .
O O7 0.20849(18) 0.8801(3) 0.8235(3) 0.0193(7) Uani d . 1 . .
O O8 0.18745(18) 0.8842(3) 0.6150(3) 0.0199(7) Uani d . 1 . .
O O9 0.3929(2) 0.5616(3) 0.6572(3) 0.0240(8) Uani d . 1 . .
H H1W 0.4336 0.5912 0.6625 0.036 Uiso d R 1 . .
H H2W 0.3713 0.5057 0.6041 0.036 Uiso d R 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'
Dy Dy -0.1892 4.4098 '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
C6 C1 C2 . . 120.2(4) ?
C6 C1 C7 . . 121.9(4) ?
C2 C1 C7 . . 118.0(4) ?
C3 C2 C1 . . 118.7(4) ?
C3 C2 H2 . . 120.7 ?
C1 C2 H2 . . 120.7 ?
C4 C3 C2 . . 122.3(4) ?
C4 C3 N1 . . 118.9(4) ?
C2 C3 N1 . . 118.7(4) ?
C3 C4 C5 . . 119.4(4) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
C6 C5 C4 . . 119.1(4) ?
C6 C5 C8 . . 122.0(4) ?
C4 C5 C8 . . 118.7(4) ?
C1 C6 C5 . . 120.1(4) ?
C1 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
O2 C7 O1 . . 121.2(4) ?
O2 C7 C1 . . 120.5(4) ?
O1 C7 C1 . . 118.3(4) ?
O4 C8 O3 . . 126.0(4) ?
O4 C8 C5 . . 117.6(4) ?
O3 C8 C5 . . 116.3(4) ?
O8 C9 O6 . . 126.4(5) ?
O8 C9 C10 . . 116.5(4) ?
O6 C9 C10 . . 117.2(4) ?
O7 C10 O5 . . 126.4(4) ?
O7 C10 C9 . . 117.3(4) ?
O5 C10 C9 . . 116.2(4) ?
O4 Dy1 O3 1_545 5_677 82.50(12) ?
O4 Dy1 O1 1_545 . 80.12(11) ?
O3 Dy1 O1 5_677 . 75.29(12) ?
O4 Dy1 O8 1_545 4_546 76.05(11) ?
O3 Dy1 O8 5_677 4_546 74.89(11) ?
O1 Dy1 O8 . 4_546 143.78(12) ?
O4 Dy1 O9 1_545 . 78.37(12) ?
O3 Dy1 O9 5_677 . 140.02(12) ?
O1 Dy1 O9 . . 67.07(12) ?
O8 Dy1 O9 4_546 . 132.03(11) ?
O4 Dy1 O7 1_545 4_546 75.48(11) ?
O3 Dy1 O7 5_677 4_546 138.61(10) ?
O1 Dy1 O7 . 4_546 132.63(11) ?
O8 Dy1 O7 4_546 4_546 66.07(11) ?
O9 Dy1 O7 . 4_546 68.59(11) ?
O4 Dy1 O5 1_545 . 143.90(11) ?
O3 Dy1 O5 5_677 . 77.07(11) ?
O1 Dy1 O5 . . 121.80(11) ?
O8 Dy1 O5 4_546 . 70.08(10) ?
O9 Dy1 O5 . . 134.73(12) ?
O7 Dy1 O5 4_546 . 101.09(11) ?
O4 Dy1 O2 1_545 . 132.70(11) ?
O3 Dy1 O2 5_677 . 81.48(11) ?
O1 Dy1 O2 . . 52.80(10) ?
O8 Dy1 O2 4_546 . 139.77(10) ?
O9 Dy1 O2 . . 86.23(10) ?
O7 Dy1 O2 4_546 . 138.39(11) ?
O5 Dy1 O2 . . 73.20(10) ?
O4 Dy1 O6 1_545 . 141.86(12) ?
O3 Dy1 O6 5_677 . 135.64(11) ?
O1 Dy1 O6 . . 106.59(11) ?
O8 Dy1 O6 4_546 . 109.04(11) ?
O9 Dy1 O6 . . 70.64(11) ?
O7 Dy1 O6 4_546 . 72.89(10) ?
O5 Dy1 O6 . . 64.31(11) ?
O2 Dy1 O6 . . 67.58(11) ?
C3 N1 H1A . . 109.5 ?
C3 N1 H1B . . 109.5 ?
H1A N1 H1B . . 109.5 ?
C3 N1 H1C . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C7 O1 Dy1 . . 95.1(3) ?
C7 O2 Dy1 . . 90.7(3) ?
C8 O3 Dy1 . 5_677 138.0(3) ?
C8 O4 Dy1 . 1_565 142.5(3) ?
C10 O5 Dy1 . . 116.9(3) ?
C9 O6 Dy1 . . 115.4(3) ?
C10 O7 Dy1 . 4_556 119.0(3) ?
C9 O8 Dy1 . 4_556 120.8(3) ?
Dy1 O9 H1W . . 122.3 ?
Dy1 O9 H2W . . 121.9 ?
H1W O9 H2W . . 111.7 ?
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
C1 C6 . 1.385(6) ?
C1 C2 . 1.399(7) ?
C1 C7 . 1.502(6) ?
C2 C3 . 1.386(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.359(6) ?
C3 N1 . 1.455(5) ?
C4 C5 . 1.408(6) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.403(6) ?
C5 C8 . 1.494(6) ?
C6 H6 . 0.9300 ?
C7 O2 . 1.254(5) ?
C7 O1 . 1.260(5) ?
C8 O4 . 1.249(6) ?
C8 O3 . 1.277(6) ?
C9 O8 . 1.248(5) ?
C9 O6 . 1.252(5) ?
C9 C10 . 1.528(6) ?
C10 O7 . 1.250(5) ?
C10 O5 . 1.263(5) ?
Dy1 O4 1_545 2.312(3) ?
Dy1 O3 5_677 2.332(4) ?
Dy1 O1 . 2.413(3) ?
Dy1 O8 4_546 2.426(3) ?
Dy1 O9 . 2.429(3) ?
Dy1 O7 4_546 2.455(3) ?
Dy1 O5 . 2.456(3) ?
Dy1 O2 . 2.509(3) ?
Dy1 O6 . 2.541(4) ?
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
N1 H1C . 0.8900 ?
O9 H1W . 0.8287 ?
O9 H2W . 0.8292 ?
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
O9 H2W O3 2_646 0.83 2.32 2.858(4) 122.9 yes
O9 H1W O1 2_656 0.83 1.97 2.790(4) 167.8 yes
N1 H1B O6 2_656 0.89 2.63 3.379(5) 142.2 yes
N1 H1A O8 2_656 0.89 2.39 2.824(5) 110.6 yes
N1 H1A O5 3 0.89 1.99 2.840(5) 160.2 yes
N1 H1C O7 5_677 0.89 1.92 2.796(6) 169.0 yes
C2 H2 O9 2_656 0.93 2.55 3.421(5) 157.0 yes
C4 H4 O5 5_677 0.93 2.53 3.169(6) 126.0 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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -1.0(8) ?
C7 C1 C2 C3 . . . . 179.1(5) ?
C1 C2 C3 C4 . . . . 3.3(7) ?
C1 C2 C3 N1 . . . . 179.9(4) ?
C2 C3 C4 C5 . . . . -1.6(8) ?
N1 C3 C4 C5 . . . . -178.2(4) ?
C3 C4 C5 C6 . . . . -2.3(8) ?
C3 C4 C5 C8 . . . . 173.4(4) ?
C2 C1 C6 C5 . . . . -2.9(8) ?
C7 C1 C6 C5 . . . . 177.0(5) ?
C4 C5 C6 C1 . . . . 4.6(8) ?
C8 C5 C6 C1 . . . . -171.0(5) ?
C6 C1 C7 O2 . . . . -1.2(8) ?
C2 C1 C7 O2 . . . . 178.7(5) ?
C6 C1 C7 O1 . . . . -179.7(5) ?
C2 C1 C7 O1 . . . . 0.2(7) ?
C6 C5 C8 O4 . . . . -31.5(7) ?
C4 C5 C8 O4 . . . . 152.8(4) ?
C6 C5 C8 O3 . . . . 149.9(4) ?
C4 C5 C8 O3 . . . . -25.7(6) ?
O8 C9 C10 O7 . . . . -6.1(5) ?
O6 C9 C10 O7 . . . . 172.8(4) ?
O8 C9 C10 O5 . . . . 174.8(4) ?
O6 C9 C10 O5 . . . . -6.3(5) ?
O2 C7 O1 Dy1 . . . . -3.7(5) ?
C1 C7 O1 Dy1 . . . . 174.8(4) ?
O4 Dy1 O1 C7 1_545 . . . -173.2(3) ?
O3 Dy1 O1 C7 5_677 . . . -88.4(3) ?
O8 Dy1 O1 C7 4_546 . . . -123.9(3) ?
O9 Dy1 O1 C7 . . . . 105.3(3) ?
O7 Dy1 O1 C7 4_546 . . . 127.2(3) ?
O5 Dy1 O1 C7 . . . . -24.2(3) ?
O2 Dy1 O1 C7 . . . . 2.0(3) ?
O6 Dy1 O1 C7 . . . . 45.4(3) ?
O1 C7 O2 Dy1 . . . . 3.5(5) ?
C1 C7 O2 Dy1 . . . . -174.9(4) ?
O4 Dy1 O2 C7 1_545 . . . 4.5(3) ?
O3 Dy1 O2 C7 5_677 . . . 76.0(3) ?
O1 Dy1 O2 C7 . . . . -2.0(3) ?
O8 Dy1 O2 C7 4_546 . . . 130.2(3) ?
O9 Dy1 O2 C7 . . . . -65.8(3) ?
O7 Dy1 O2 C7 4_546 . . . -117.2(3) ?
O5 Dy1 O2 C7 . . . . 155.0(3) ?
O6 Dy1 O2 C7 . . . . -136.4(3) ?
O4 C8 O3 Dy1 . . . 5_677 103.1(5) ?
C5 C8 O3 Dy1 . . . 5_677 -78.5(5) ?
O3 C8 O4 Dy1 . . . 1_565 -0.3(8) ?
C5 C8 O4 Dy1 . . . 1_565 -178.6(3) ?
O7 C10 O5 Dy1 . . . . -149.7(4) ?
C9 C10 O5 Dy1 . . . . 29.4(4) ?
O4 Dy1 O5 C10 1_545 . . . -172.7(3) ?
O3 Dy1 O5 C10 5_677 . . . 130.1(3) ?
O1 Dy1 O5 C10 . . . . 66.8(4) ?
O8 Dy1 O5 C10 4_546 . . . -151.5(3) ?
O9 Dy1 O5 C10 . . . . -21.4(4) ?
O7 Dy1 O5 C10 4_546 . . . -92.2(3) ?
O2 Dy1 O5 C10 . . . . 45.3(3) ?
O6 Dy1 O5 C10 . . . . -27.5(3) ?
O8 C9 O6 Dy1 . . . . 160.0(4) ?
C10 C9 O6 Dy1 . . . . -18.8(4) ?
O4 Dy1 O6 C9 1_545 . . . 170.5(3) ?
O3 Dy1 O6 C9 5_677 . . . -8.6(4) ?
O1 Dy1 O6 C9 . . . . -94.4(3) ?
O8 Dy1 O6 C9 4_546 . . . 79.0(3) ?
O9 Dy1 O6 C9 . . . . -152.0(3) ?
O7 Dy1 O6 C9 4_546 . . . 135.3(3) ?
O5 Dy1 O6 C9 . . . . 23.5(3) ?
O2 Dy1 O6 C9 . . . . -58.0(3) ?
O5 C10 O7 Dy1 . . . 4_556 -174.0(3) ?
C9 C10 O7 Dy1 . . . 4_556 7.0(5) ?
O6 C9 O8 Dy1 . . . 4_556 -176.7(3) ?
C10 C9 O8 Dy1 . . . 4_556 2.1(5) ?
