#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/63/2236336.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_2236336
loop_
_publ_author_name
'Mi, Jun-Long'
'Huang, Jing'
'Chen, Hong-Ji'
_publ_section_title
;
 Poly[[diaquabis(μ-oxalato-κ⁴O¹,O²:O^1'^,O^2'^)bis(μ₃-5-oxidopyridin-1-ium-3-carboxylato-κ³O³:O^3'^:O⁵)diholmium(III)]
 dihydrate]
;
_journal_coeditor_code           HY2567
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1146
_journal_page_last               m1147
_journal_paper_doi               10.1107/S1600536812032916
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ho2 (C6 H4 N O3)2 (C2 O4)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C16 H12 Ho2 N2 O16, 2(H2 O)'
_chemical_formula_sum            'C16 H16 Ho2 N2 O18'
_chemical_formula_weight         854.16
_chemical_name_systematic
;
Poly[[diaquabis(μ-oxalato-
κ⁴O¹,O²:O^1'^,O^2'^)bis(μ₃-5-
oxidopyridin-1-ium-3-carboxylato-
κ³O³:O^3'^:O⁵)diholmium(III)] dihydrate]
;
_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                110.912(3)
_cell_angle_beta                 96.862(3)
_cell_angle_gamma                95.770(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7786(16)
_cell_length_b                   8.0562(17)
_cell_length_c                   9.505(2)
_cell_measurement_reflns_used    4550
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.33
_cell_volume                     545.8(2)
_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  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4550
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    7.295
_exptl_absorpt_correction_T_max  0.6687
_exptl_absorpt_correction_T_min  0.3535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.491
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2295
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0158
_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)+(0.0160P)²+0.6363P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0379
_reflns_number_gt                2160
_reflns_number_total             2295
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2567.cif
_cod_data_source_block           I
_cod_database_code               2236336
_cod_database_fobs_code          2236336
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_symmetry_multiplicity
C C1 0.6934(4) 1.2898(4) 1.1270(3) 0.0109(5) Uani d . 1 1
C C2 0.7746(4) 0.4547(4) 0.2648(3) 0.0123(6) Uani d . 1 1
C C3 0.7041(4) 0.5062(4) 0.3987(3) 0.0117(6) Uani d . 1 1
H H3 0.5989 0.4387 0.4032 0.014 Uiso calc R 1 1
C C4 0.7864(4) 0.6576(4) 0.5285(3) 0.0124(6) Uani d . 1 1
C C5 0.9393(4) 0.7518(4) 0.5123(3) 0.0158(6) Uani d . 1 1
H H5 0.9999 0.8543 0.5962 0.019 Uiso calc R 1 1
C C6 0.9258(4) 0.5562(4) 0.2565(4) 0.0162(6) Uani d . 1 1
H H6 0.9743 0.5245 0.1651 0.019 Uiso calc R 1 1
C C7 0.9532(4) 0.9560(4) 1.0490(3) 0.0106(6) Uani d . 1 1
C C8 0.4187(4) 0.9302(4) 0.4887(3) 0.0116(6) Uani d . 1 1
Ho Ho1 0.647369(16) 0.971506(16) 0.803507(14) 0.00854(5) Uani d . 1 1
N N1 1.0014(3) 0.6993(4) 0.3802(3) 0.0168(5) Uani d D 1 1
O O1 0.7614(3) 1.2593(3) 1.0082(2) 0.0162(5) Uani d . 1 1
O O2 0.4346(3) 0.8128(3) 0.8643(2) 0.0136(4) Uani d . 1 1
O O3 0.7231(3) 0.7072(3) 0.6565(2) 0.0150(4) Uani d . 1 1
O O4 0.7922(3) 0.8943(3) 1.0004(2) 0.0133(4) Uani d . 1 1
O O5 0.9595(3) 1.0464(3) 0.8342(2) 0.0123(4) Uani d . 1 1
O O6 0.4182(3) 0.8477(3) 0.5761(2) 0.0161(4) Uani d . 1 1
O O7 0.7033(3) 1.0868(3) 0.6190(2) 0.0135(4) Uani d . 1 1
O O8 0.4335(3) 1.1739(3) 0.8101(3) 0.0197(5) Uani d D 1 1
O O9 0.3549(5) 0.5133(4) 0.1651(4) 0.0462(8) Uani d D 1 1
H H1 1.102(3) 0.760(4) 0.373(4) 0.011(8) Uiso d D 1 1
H H7 0.489(6) 1.275(4) 0.822(6) 0.061(17) Uiso d D 1 1
H H8 0.363(6) 1.155(7) 0.866(5) 0.065(17) Uiso d D 1 1
H H9 0.331(8) 0.448(7) 0.216(6) 0.08(2) Uiso d D 1 1
H H10 0.269(6) 0.501(9) 0.096(5) 0.09(2) Uiso d D 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'
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'
Ho Ho -0.2175 4.6783 '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
O2 C1 O1 2_677 . 123.0(3)
O2 C1 C2 2_677 1_566 119.6(3)
O1 C1 C2 . 1_566 117.4(3)
C3 C2 C6 . . 119.6(3)
C3 C2 C1 . 1_544 122.1(3)
C6 C2 C1 . 1_544 118.3(3)
C2 C3 C4 . . 121.0(3)
C2 C3 H3 . . 119.5
C4 C3 H3 . . 119.5
O3 C4 C5 . . 121.8(3)
O3 C4 C3 . . 122.0(3)
C5 C4 C3 . . 116.2(3)
N1 C5 C4 . . 120.9(3)
N1 C5 H5 . . 119.5
C4 C5 H5 . . 119.5
N1 C6 C2 . . 118.5(3)
N1 C6 H6 . . 120.7
C2 C6 H6 . . 120.7
O5 C7 O4 2_777 . 126.2(3)
O5 C7 C7 2_777 2_777 118.1(3)
O4 C7 C7 . 2_777 115.7(3)
O6 C8 O7 . 2_676 126.3(3)
O6 C8 C8 . 2_676 118.0(3)
O7 C8 C8 2_676 2_676 115.6(3)
O2 Ho1 O3 . . 88.38(8)
O2 Ho1 O7 . . 141.51(7)
O3 Ho1 O7 . . 88.96(8)
O2 Ho1 O4 . . 75.56(7)
O3 Ho1 O4 . . 81.26(8)
O7 Ho1 O4 . . 141.63(7)
O2 Ho1 O5 . . 143.17(7)
O3 Ho1 O5 . . 78.02(7)
O7 Ho1 O5 . . 73.02(7)
O4 Ho1 O5 . . 68.67(7)
O2 Ho1 O1 . . 112.36(7)
O3 Ho1 O1 . . 143.48(8)
O7 Ho1 O1 . . 91.68(7)
O4 Ho1 O1 . . 75.80(7)
O5 Ho1 O1 . . 67.35(7)
O2 Ho1 O8 . . 83.88(8)
O3 Ho1 O8 . . 142.95(8)
O7 Ho1 O8 . . 75.53(8)
O4 Ho1 O8 . . 130.78(7)
O5 Ho1 O8 . . 126.55(8)
O1 Ho1 O8 . . 71.62(8)
O2 Ho1 O6 . . 74.25(7)
O3 Ho1 O6 . . 74.55(8)
O7 Ho1 O6 . . 68.06(7)
O4 Ho1 O6 . . 141.48(7)
O5 Ho1 O6 . . 132.12(7)
O1 Ho1 O6 . . 138.53(7)
O8 Ho1 O6 . . 68.47(8)
C6 N1 C5 . . 123.8(3)
C6 N1 H1 . . 117(2)
C5 N1 H1 . . 119(2)
C1 O1 Ho1 . . 115.09(18)
C1 O2 Ho1 2_677 . 169.7(2)
C4 O3 Ho1 . . 132.61(19)
C7 O4 Ho1 . . 118.19(18)
C7 O5 Ho1 2_777 . 116.85(18)
C8 O6 Ho1 . . 115.09(18)
C8 O7 Ho1 2_676 . 119.68(18)
Ho1 O8 H7 . . 108(4)
Ho1 O8 H8 . . 106(4)
H7 O8 H8 . . 126(5)
H9 O9 H10 . . 111(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 O2 2_677 1.259(4)
C1 O1 . 1.260(4)
C1 C2 1_566 1.507(4)
C2 C3 . 1.388(4)
C2 C6 . 1.390(4)
C2 C1 1_544 1.507(4)
C3 C4 . 1.414(4)
C3 H3 . 0.9500
C4 O3 . 1.311(4)
C4 C5 . 1.400(4)
C5 N1 . 1.340(4)
C5 H5 . 0.9500
C6 N1 . 1.337(4)
C6 H6 . 0.9500
C7 O5 2_777 1.237(3)
C7 O4 . 1.266(4)
C7 C7 2_777 1.559(6)
C8 O6 . 1.235(4)
C8 O7 2_676 1.269(3)
C8 C8 2_676 1.545(6)
Ho1 O2 . 2.245(2)
Ho1 O3 . 2.271(2)
Ho1 O7 . 2.322(2)
Ho1 O4 . 2.372(2)
Ho1 O5 . 2.399(2)
Ho1 O1 . 2.429(2)
Ho1 O8 . 2.435(2)
Ho1 O6 . 2.455(2)
N1 H1 . 0.900(10)
O8 H7 . 0.850(10)
O8 H8 . 0.850(10)
O9 H9 . 0.850(10)
O9 H10 . 0.850(10)
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
N1 H1 O7 2_776 0.900(10) 1.830(10) 2.727(3) 171(3)
O8 H7 O9 2_676 0.850(10) 1.950(10) 2.787(4) 171(5)
O8 H8 O4 2_677 0.850(10) 1.960(10) 2.811(3) 177(6)
O9 H9 O3 2_666 0.850(10) 2.080(10) 2.929(4) 178(6)
O9 H10 O1 2_676 0.850(10) 2.48(6) 3.003(4) 120(5)
