#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/34/2223432.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_2223432
loop_
_publ_author_name
'Zhu, Hui-Lan'
'Lai, Hui-Ling'
'Han, Lu'
'Luo, Yi-Fan'
'Zeng, Rong-Hua'
_publ_section_title
;Poly[[aqua(μ₂-oxalato)(μ₂-2-oxidopyridinium-3-carboxylato)holmium(III)]
 monohydrate]
;
_journal_coeditor_code           HY2226
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1217
_journal_page_last               m1218
_journal_paper_doi               10.1107/S1600536809036344
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ho (C2 O4) (C6 H4 N O3) (H2 O)] , H2 O'
_chemical_formula_moiety         'C8 H6 Ho N O8 , H2 O'
_chemical_formula_sum            'C8 H8 Ho N O9'
_chemical_formula_weight         427.08
_chemical_name_systematic
;
Poly[[aqua(μ₂-oxalato)(μ₂-2-oxidopyridinium-3-carboxylato)holmium(III)]
monohydrate]
;
_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           SHELXL97
_cell_angle_alpha                71.810(2)
_cell_angle_beta                 78.862(2)
_cell_angle_gamma                80.359(2)
_cell_formula_units_Z            2
_cell_length_a                   6.5391(11)
_cell_length_b                   9.5305(16)
_cell_length_c                   9.7391(16)
_cell_measurement_reflns_used    2285
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.23
_cell_volume                     562.01(16)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and 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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2884
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.085
_exptl_absorpt_correction_T_max  0.3788
_exptl_absorpt_correction_T_min  0.3315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.745
_refine_diff_density_min         -2.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         1983
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0342
_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)+(0.0695P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                1862
_reflns_number_total             1983
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2226.cif
_cod_data_source_block           I
_cod_database_code               2223432
_cod_database_fobs_code          2223432
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho Ho1 0.09083(4) 0.29059(3) 0.30045(3) 0.01784(15) Uani d . 1 . .
O O4 -0.1655(7) 0.3863(5) 0.1370(5) 0.0219(10) Uani d . 1 . .
O O3 0.1549(8) 0.1295(6) 0.1626(5) 0.0311(11) Uani d . 1 . .
O O6 0.1351(9) 0.3228(5) 0.5267(6) 0.0338(12) Uani d . 1 . .
O O1 0.2127(8) 0.0581(5) 0.4520(5) 0.0251(10) Uani d . 1 . .
O O5 -0.2292(7) 0.5458(5) -0.0767(5) 0.0258(10) Uani d . 1 . .
N N1 0.2729(11) -0.0557(8) 0.0581(7) 0.0366(15) Uani d . 1 . .
H H1 0.2407 0.0054 -0.0227 0.044 Uiso calc R 1 . .
C C6 0.2307(12) -0.0067(8) 0.1802(8) 0.0266(15) Uani d . 1 . .
C C8 0.0606(11) 0.4422(8) 0.5578(8) 0.0261(15) Uani d . 1 . .
C C5 0.3624(14) -0.1948(10) 0.0574(10) 0.044(2) Uani d . 1 . .
H H5 0.3862 -0.2213 -0.0290 0.052 Uiso calc R 1 . .
C C4 0.4170(14) -0.2947(9) 0.1807(10) 0.048(3) Uani d . 1 . .
H H4 0.4851 -0.3882 0.1795 0.057 Uiso calc R 1 . .
C C3 0.3695(13) -0.2550(9) 0.3094(10) 0.0396(19) Uani d . 1 . .
H H3 0.3999 -0.3250 0.3960 0.048 Uiso calc R 1 . .
C C2 0.2776(10) -0.1133(7) 0.3126(7) 0.0251(15) Uani d . 1 . .
C C1 0.2306(10) -0.0747(7) 0.4529(7) 0.0236(14) Uani d . 1 . .
C C7 -0.1147(10) 0.4807(7) 0.0161(7) 0.0190(13) Uani d . 1 . .
O O2W 0.2278(13) 0.0635(9) 0.7646(8) 0.0621(19) Uani d D 1 . .
O O2 0.2125(7) -0.1813(5) 0.5703(5) 0.0262(10) Uani d . 1 . .
O O7 0.0730(9) 0.4748(6) 0.6691(5) 0.0358(13) Uani d . 1 . .
O O1W 0.4526(8) 0.2970(7) 0.2822(6) 0.0427(15) Uani d D 1 . .
H H3W 0.164(16) 0.149(7) 0.758(10) 0.064 Uiso d D 1 . .
H H4W 0.203(16) 0.041(10) 0.691(6) 0.064 Uiso d D 1 . .
H H1W 0.508(12) 0.263(11) 0.359(5) 0.064 Uiso d D 1 . .
H H2W 0.549(10) 0.332(11) 0.215(6) 0.064 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'
Ho Ho -0.2175 4.6783 '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
O3 Ho1 O1W . . 90.4(2) ?
O3 Ho1 O2 . 2_556 90.37(18) ?
O1W Ho1 O2 . 2_556 148.26(17) ?
O3 Ho1 O1 . . 73.45(17) ?
O1W Ho1 O1 . . 75.15(18) ?
O2 Ho1 O1 2_556 . 74.69(16) ?
O3 Ho1 O5 . 2_565 81.80(17) ?
O1W Ho1 O5 . 2_565 67.83(16) ?
O2 Ho1 O5 2_556 2_565 143.49(16) ?
O1 Ho1 O5 . 2_565 134.91(16) ?
O3 Ho1 O7 . 2_566 148.06(18) ?
O1W Ho1 O7 . 2_566 105.7(2) ?
O2 Ho1 O7 2_556 2_566 89.77(18) ?
O1 Ho1 O7 . 2_566 136.83(16) ?
O5 Ho1 O7 2_565 2_566 79.25(18) ?
O3 Ho1 O6 . . 144.55(17) ?
O1W Ho1 O6 . . 75.0(2) ?
O2 Ho1 O6 2_556 . 86.35(18) ?
O1 Ho1 O6 . . 71.64(16) ?
O5 Ho1 O6 2_565 . 119.81(18) ?
O7 Ho1 O6 2_566 . 67.30(17) ?
O3 Ho1 O4 . . 77.17(17) ?
O1W Ho1 O4 . . 135.57(16) ?
O2 Ho1 O4 2_556 . 75.25(15) ?
O1 Ho1 O4 . . 137.32(16) ?
O5 Ho1 O4 2_565 . 68.24(14) ?
O7 Ho1 O4 2_566 . 72.00(17) ?
O6 Ho1 O4 . . 135.14(16) ?
C7 O4 Ho1 . . 118.2(4) ?
C6 O3 Ho1 . . 136.0(5) ?
C8 O6 Ho1 . . 120.3(5) ?
C1 O1 Ho1 . . 136.8(4) ?
C7 O5 Ho1 . 2_565 119.9(4) ?
C5 N1 C6 . . 123.9(7) ?
C5 N1 H1 . . 118.0 ?
C6 N1 H1 . . 118.0 ?
O3 C6 N1 . . 116.8(7) ?
O3 C6 C2 . . 127.2(7) ?
N1 C6 C2 . . 116.1(7) ?
O7 C8 O6 . . 127.4(7) ?
O7 C8 C8 . 2_566 117.7(8) ?
O6 C8 C8 . 2_566 114.9(8) ?
C4 C5 N1 . . 120.6(8) ?
C4 C5 H5 . . 119.7 ?
N1 C5 H5 . . 119.7 ?
C5 C4 C3 . . 118.5(8) ?
C5 C4 H4 . . 120.7 ?
C3 C4 H4 . . 120.7 ?
C4 C3 C2 . . 121.7(8) ?
C4 C3 H3 . . 119.1 ?
C2 C3 H3 . . 119.1 ?
C3 C2 C6 . . 119.1(7) ?
C3 C2 C1 . . 120.1(7) ?
C6 C2 C1 . . 120.8(6) ?
O1 C1 O2 . . 122.8(6) ?
O1 C1 C2 . . 119.9(6) ?
O2 C1 C2 . . 117.3(6) ?
O5 C7 O4 . . 126.5(6) ?
O5 C7 C7 . 2_565 117.4(7) ?
O4 C7 C7 . 2_565 116.0(7) ?
H3W O2W H4W . . 105(9) ?
C1 O2 Ho1 . 2_556 128.4(4) ?
C8 O7 Ho1 . 2_566 119.8(5) ?
Ho1 O1W H1W . . 119(6) ?
Ho1 O1W H2W . . 136(6) ?
H1W O1W H2W . . 106(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
Ho1 O1 . 2.354(5) y
Ho1 O2 2_556 2.348(5) y
Ho1 O3 . 2.279(5) y
Ho1 O4 . 2.406(4) y
Ho1 O5 2_565 2.364(5) y
Ho1 O6 . 2.394(5) y
Ho1 O7 2_566 2.392(5) y
Ho1 O1W . 2.348(5) y
O4 C7 . 1.262(8) ?
O3 C6 . 1.279(9) ?
O6 C8 . 1.263(9) ?
O1 C1 . 1.249(8) ?
O5 C7 . 1.232(8) ?
O5 Ho1 2_565 2.364(4) ?
N1 C5 . 1.358(11) ?
N1 C6 . 1.373(10) ?
N1 H1 . 0.8600 ?
C6 C2 . 1.421(10) ?
C8 O7 . 1.237(9) ?
C8 C8 2_566 1.546(15) ?
C5 C4 . 1.347(13) ?
C5 H5 . 0.9300 ?
C4 C3 . 1.384(11) ?
C4 H4 . 0.9300 ?
C3 C2 . 1.390(10) ?
C3 H3 . 0.9300 ?
C2 C1 . 1.487(10) ?
C1 O2 . 1.271(8) ?
C7 C7 2_565 1.554(12) ?
O2W H3W . 0.84(7) ?
O2W H4W . 0.86(7) ?
O1W H1W . 0.84(6) ?
O1W H2W . 0.85(7) ?
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
O1W H1W O2 2_656 0.84(6) 2.02(6) 2.737(7) 142(8) y
O1W H2W O4 1_655 0.85(7) 1.96(4) 2.749(7) 154(8) y
O2W H3W O6 . 0.84(7) 2.36(11) 2.882(10) 121(8) y
O2W H4W O1 . 0.86(7) 2.27(3) 3.082(8) 157(9) y
N1 H1 O2W 1_554 0.86 1.99 2.781(10) 153.5 y
