#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/47/2234758.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_2234758
loop_
_publ_author_name
'Zhang, Qing'
'Wang, Xing'
'Wang, Shen-Tang'
'Liu, Chun-Bo'
'Che, Guang-Bo'
_publ_section_title
;
 Poly[[tri-μ₃-hydroxido-tris(μ₄-pyridine-2,5-dicarboxylato)trineodymium(III)]
 monohydrate]
;
_journal_coeditor_code           QK2031
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m541
_journal_page_last               m542
_journal_paper_doi               10.1107/S160053681201286X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Nd3 (C7 H3 N O4)3 (O H)3], H2 O'
_chemical_formula_moiety         'C21 H12 N3 Nd3 O15, H2 O1'
_chemical_formula_sum            'C21 H14 N3 Nd3 O16'
_chemical_formula_weight         997.07
_chemical_name_systematic
;
Poly[[tri-μ₃-hydroxido-tris(μ₄-pyridine-2,5-
dicarboxylato)trineodymium(III)] monohydrate]
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   23.081(3)
_cell_length_b                   23.081(3)
_cell_length_c                   8.9690(18)
_cell_measurement_reflns_used    3338
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29.0051
_cell_measurement_theta_min      3.0517
_cell_volume                     4137.9(11)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3454
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.645
_exptl_absorpt_correction_T_max  0.538
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2814
_exptl_crystal_size_max          0.1600
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1100
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.654
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0188
_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)+(0.0210P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                1558
_reflns_number_total             1679
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qk2031.cif
_cod_data_source_block           I
_cod_original_cell_volume        4138.0(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2234758
_cod_database_fobs_code          2234758
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Nd Nd1 0.041666(9) 0.128240(9) 0.329953(18) 0.00891(7) Uani d . 1 1
C C1 0.03699(16) 0.21892(16) 0.0150(4) 0.0131(7) Uani d . 1 1
C C2 0.0445(2) 0.26676(18) -0.0868(4) 0.0253(9) Uani d . 1 1
H H2 0.0244 0.2544 -0.1801 0.030 Uiso calc R 1 1
C C3 0.0822(2) 0.33329(18) -0.0484(4) 0.0290(10) Uani d . 1 1
H H3 0.0873 0.3664 -0.1150 0.035 Uiso calc R 1 1
C C4 0.11239(17) 0.35025(16) 0.0903(4) 0.0157(7) Uani d . 1 1
C C5 0.10166(17) 0.29858(16) 0.1863(4) 0.0137(7) Uani d . 1 1
H H5 0.1211 0.3095 0.2804 0.016 Uiso calc R 1 1
C C6 -0.00545(16) 0.14569(16) -0.0166(4) 0.0121(7) Uani d . 1 1
C C7 0.15650(17) 0.42256(17) 0.1364(4) 0.0150(8) Uani d . 1 1
N N1 0.06494(13) 0.23415(13) 0.1504(3) 0.0113(6) Uani d . 1 1
O O1 0.19772(12) 0.43481(11) 0.2386(3) 0.0186(6) Uani d . 1 1
O O2 0.14805(13) 0.46471(12) 0.0684(3) 0.0261(6) Uani d . 1 1
O O3 -0.02355(11) 0.12927(11) -0.1493(2) 0.0147(5) Uani d . 1 1
O O4 -0.02057(12) 0.10561(11) 0.0918(3) 0.0167(5) Uani d . 1 1
O O1w 0.0000 0.0000 0.1697(6) 0.0634(18) Uani d S 1 3
O O5 0.03467(11) 0.10550(12) 0.6017(3) 0.0118(5) Uani d . 1 1
H H1 0.0397(19) 0.1334(18) 0.650(5) 0.018 Uiso 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'
Nd Nd -0.1943 3.0179 '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 Nd1 O3 6_455 11 133.07(8)
O2 Nd1 O1 6_455 16 80.41(9)
O3 Nd1 O1 11 16 77.55(8)
O2 Nd1 O4 6_455 . 85.50(9)
O3 Nd1 O4 11 . 78.54(8)
O1 Nd1 O4 16 . 130.65(8)
O2 Nd1 O5 6_455 . 81.79(8)
O3 Nd1 O5 11 . 131.58(7)
O1 Nd1 O5 16 . 77.64(8)
O4 Nd1 O5 . . 146.31(7)
O2 Nd1 O5 6_455 12_556 77.35(8)
O3 Nd1 O5 11 12_556 138.97(8)
O1 Nd1 O5 16 12_556 142.14(8)
O4 Nd1 O5 . 12_556 77.63(8)
O5 Nd1 O5 . 12_556 69.19(8)
O2 Nd1 O5 6_455 11_556 150.20(8)
O3 Nd1 O5 11 11_556 69.18(8)
O1 Nd1 O5 16 11_556 87.76(8)
O4 Nd1 O5 . 11_556 122.15(8)
O5 Nd1 O5 . 11_556 68.94(8)
O5 Nd1 O5 12_556 11_556 96.63(11)
O2 Nd1 N1 6_455 . 65.27(8)
O3 Nd1 N1 11 . 68.36(8)
O1 Nd1 N1 16 . 70.02(8)
O4 Nd1 N1 . . 61.14(8)
O5 Nd1 N1 . . 136.65(8)
O5 Nd1 N1 12_556 . 124.92(8)
O5 Nd1 N1 11_556 . 135.26(8)
O2 Nd1 Nd1 6_455 12_556 65.95(6)
O3 Nd1 Nd1 11 12_556 160.68(5)
O1 Nd1 Nd1 16 12_556 106.55(6)
O4 Nd1 Nd1 . 12_556 110.13(5)
O5 Nd1 Nd1 . 12_556 36.42(5)
O5 Nd1 Nd1 12_556 12_556 35.97(5)
O5 Nd1 Nd1 11_556 12_556 91.90(6)
N1 Nd1 Nd1 . 12_556 130.94(6)
O2 Nd1 Nd1 6_455 11_556 114.28(7)
O3 Nd1 Nd1 11 11_556 96.13(6)
O1 Nd1 Nd1 16 11_556 69.98(5)
O4 Nd1 Nd1 . 11_556 155.32(5)
O5 Nd1 Nd1 . 11_556 36.03(5)
O5 Nd1 Nd1 12_556 11_556 91.91(6)
O5 Nd1 Nd1 11_556 11_556 36.09(5)
N1 Nd1 Nd1 . 11_556 139.35(5)
Nd1 Nd1 Nd1 12_556 11_556 68.623(13)
N1 C1 C2 . . 122.8(3)
N1 C1 C6 . . 115.2(3)
C2 C1 C6 . . 122.0(3)
C1 C2 C3 . . 119.0(3)
C1 C2 H2 . . 120.5
C3 C2 H2 . . 120.5
C2 C3 C4 . . 119.2(3)
C2 C3 H3 . . 120.4
C4 C3 H3 . . 120.4
C3 C4 C5 . . 117.8(3)
C3 C4 C7 . . 121.6(3)
C5 C4 C7 . . 120.7(3)
N1 C5 C4 . . 123.4(3)
N1 C5 H5 . . 118.3
C4 C5 H5 . . 118.3
O3 C6 O4 . . 125.4(3)
O3 C6 C1 . . 116.8(3)
O4 C6 C1 . . 117.8(3)
O2 C7 O1 . . 125.7(3)
O2 C7 C4 . . 116.5(3)
O1 C7 C4 . . 117.8(3)
C5 N1 C1 . . 117.8(3)
C5 N1 Nd1 . . 125.8(2)
C1 N1 Nd1 . . 116.4(2)
C7 O1 Nd1 . 16 133.4(2)
C7 O2 Nd1 . 8_554 142.0(2)
C6 O3 Nd1 . 12 148.7(2)
C6 O4 Nd1 . . 126.1(2)
Nd1 O5 Nd1 . 11_556 108.00(8)
Nd1 O5 Nd1 . 12_556 107.49(8)
Nd1 O5 Nd1 11_556 12_556 130.61(10)
Nd1 O5 H1 . . 115(3)
Nd1 O5 H1 11_556 . 104(3)
Nd1 O5 H1 12_556 . 91(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
Nd1 O2 6_455 2.395(2) yes
Nd1 O3 11 2.426(2) yes
Nd1 O1 16 2.452(2) yes
Nd1 O4 . 2.480(2) yes
Nd1 O5 . 2.482(2) yes
Nd1 O5 12_556 2.485(2) yes
Nd1 O5 11_556 2.501(2) yes
Nd1 N1 . 2.747(3) yes
C1 N1 . 1.337(4) ?
C1 C2 . 1.375(5) ?
C1 C6 . 1.497(4) ?
C2 C3 . 1.377(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.384(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.389(5) ?
C4 C7 . 1.515(5) ?
C5 N1 . 1.331(4) ?
C5 H5 . 0.9300 ?
C6 O3 . 1.256(4) ?
C6 O4 . 1.264(4) ?
C7 O2 . 1.244(4) ?
C7 O1 . 1.247(4) ?
O1 Nd1 16 2.452(2) ?
O2 Nd1 8_554 2.395(2) ?
O3 Nd1 12 2.426(2) ?
O5 Nd1 11_556 2.485(2) ?
O5 Nd1 12_556 2.501(2) ?
O5 H1 . 0.73(4) ?
