#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/73/2217365.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_2217365
loop_
_publ_author_name
'Tsai, Chia-Jung'
'Liu, Yen-Hsiang'
_publ_section_title
Poly[diaquabis(2,2'-bipyridine)tris(μ₄-2,2'-bipyridine-4,4'-dicarboxylato)dineodymium(III)]
_journal_coeditor_code           WW2111
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m260
_journal_page_last               m261
_journal_paper_doi               10.1107/S1600536807067396
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Nd2 (C12 H6 N2 O4)3 (C10 H8 N2)2 (H2 O)2]'
_chemical_formula_moiety         'C28 H19 N5 Nd1 O7'
_chemical_formula_sum            'C28 H19 N5 Nd O7'
_chemical_formula_weight         681.72
_chemical_name_systematic
;
Poly[diaquabis(2,2'-bipyridine)tris(μ₄-2,2'-bipyridine-4,4'-
dicarboxylato)dineodymium(III)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                67.809(2)
_cell_angle_beta                 88.645(2)
_cell_angle_gamma                75.4370(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9914(2)
_cell_length_b                   12.5409(3)
_cell_length_c                   12.7455(3)
_cell_measurement_reflns_used    12726
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     1283.89(6)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16411
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    2.081
_exptl_absorpt_correction_T_max  0.6597
_exptl_absorpt_correction_T_min  0.3981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.968
_refine_ls_extinction_coef       0.0065(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0265P)²+1.2551P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                4460
_reflns_number_total             4669
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ww2111.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C28 H19 N5 Nd1 O7'
_cod_database_code               2217365
_cod_database_fobs_code          2217365
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
Nd Nd1 0.302446(16) 0.648646(11) 0.499494(11) 0.01470(8) Uani d . 1
O O1 0.4250(2) 0.69456(18) 0.32145(16) 0.0229(5) Uani d . 1
O O2 0.6003(2) 0.53012(18) 0.32891(16) 0.0235(5) Uani d . 1
O O3 0.5424(2) 0.65947(18) -0.43231(16) 0.0223(4) Uani d . 1
O O4 0.7188(3) 0.49332(18) -0.41903(17) 0.0241(5) Uani d . 1
O O5 0.0710(2) 0.77124(17) 0.38374(17) 0.0225(4) Uani d . 1
O O6 -0.1170(3) 0.68020(19) 0.39864(18) 0.0284(5) Uani d . 1
O O7 0.0896(2) 0.55410(18) 0.58438(17) 0.0233(4) Uani d . 1
H H7A 0.0142 0.5913 0.5371 0.035 Uiso d R 1
H H7B 0.1141 0.4849 0.592 0.035 Uiso d R 1
N N1 0.1807(3) 0.7494(2) 0.6388(2) 0.0215(5) Uani d . 1
N N2 0.3019(3) 0.8746(2) 0.4497(2) 0.0223(5) Uani d . 1
N N3 0.4653(3) 0.7593(2) -0.0901(2) 0.0258(6) Uani d . 1
N N4 0.7976(3) 0.5136(3) -0.0406(2) 0.0291(6) Uani d . 1
N N5 -0.1566(3) 0.9404(2) -0.0166(2) 0.0234(5) Uani d . 1
C C1 0.1138(4) 0.6873(3) 0.7282(2) 0.0251(7) Uani d . 1
H H1 0.1275 0.6047 0.7452 0.03 Uiso calc R 1
C C2 0.0265(4) 0.7370(3) 0.7965(3) 0.0312(7) Uani d . 1
H H2 -0.0176 0.6897 0.8598 0.037 Uiso calc R 1
C C3 0.0047(4) 0.8573(3) 0.7704(3) 0.0369(8) Uani d . 1
H H3 -0.0571 0.8947 0.8147 0.044 Uiso calc R 1
C C4 0.0731(4) 0.9226(3) 0.6797(3) 0.0323(8) Uani d . 1
H H4 0.0592 1.0055 0.6611 0.039 Uiso calc R 1
C C5 0.1628(4) 0.8665(3) 0.6156(2) 0.0221(6) Uani d . 1
C C6 0.2415(4) 0.9319(3) 0.5180(3) 0.0235(6) Uani d . 1
C C7 0.2558(5) 1.0458(3) 0.4987(3) 0.0376(8) Uani d . 1
H H7 0.2134 1.0844 0.5481 0.045 Uiso calc R 1
C C8 0.3316(5) 1.1022(3) 0.4078(3) 0.0426(9) Uani d . 1
H H8 0.3426 1.1796 0.3943 0.051 Uiso calc R 1
C C9 0.3913(5) 1.0454(3) 0.3366(3) 0.0382(8) Uani d . 1
H H9 0.4428 1.0828 0.2726 0.046 Uiso calc R 1
C C10 0.3740(4) 0.9320(3) 0.3610(3) 0.0306(7) Uani d . 1
H H10 0.4157 0.8925 0.3121 0.037 Uiso calc R 1
C C11 0.5080(3) 0.6300(2) 0.2764(2) 0.0178(6) Uani d . 1
C C12 0.4949(3) 0.6758(2) 0.1476(2) 0.0173(6) Uani d . 1
C C13 0.5869(3) 0.6123(2) 0.0900(2) 0.0187(6) Uani d . 1
H H13 0.6611 0.5394 0.1309 0.022 Uiso calc R 1
C C14 0.5690(3) 0.6570(2) -0.0282(2) 0.0187(6) Uani d . 1
C C15 0.3785(4) 0.8189(3) -0.0329(3) 0.0306(8) Uani d . 1
H H15 0.3048 0.8915 -0.0754 0.037 Uiso calc R 1
C C16 0.3893(4) 0.7814(3) 0.0843(2) 0.0248(7) Uani d . 1
H H16 0.3252 0.8275 0.1206 0.03 Uiso calc R 1
C C17 0.6656(3) 0.5932(2) -0.0944(2) 0.0193(6) Uani d . 1
C C18 0.6182(3) 0.6167(2) -0.2056(2) 0.0183(6) Uani d . 1
H H18 0.5249 0.6749 -0.2412 0.022 Uiso calc R 1
C C19 0.7085(3) 0.5544(2) -0.2641(2) 0.0177(6) Uani d . 1
C C20 0.8448(4) 0.4715(3) -0.2093(3) 0.0267(7) Uani d . 1
H H20 0.9094 0.4265 -0.2464 0.032 Uiso calc R 1
C C21 0.8844(4) 0.4559(3) -0.0993(3) 0.0347(8) Uani d . 1
H H21 0.9795 0.4007 -0.063 0.042 Uiso calc R 1
C C22 0.6534(3) 0.5710(2) -0.3818(2) 0.0182(6) Uani d . 1
C C23 -0.0411(3) 0.7506(2) 0.3433(2) 0.0190(6) Uani d . 1
C C24 -0.0843(3) 0.8186(2) 0.2173(2) 0.0197(6) Uani d . 1
C C25 -0.0014(3) 0.8963(2) 0.1525(2) 0.0189(6) Uani d . 1
H H25 0.082 0.9084 0.187 0.023 Uiso calc R 1
C C26 -0.0414(3) 0.9566(2) 0.0364(2) 0.0181(6) Uani d . 1
C C27 -0.2347(4) 0.8644(3) 0.0472(3) 0.0307(7) Uani d . 1
H H27 -0.3158 0.8519 0.0107 0.037 Uiso calc R 1
C C28 -0.2040(4) 0.8027(3) 0.1641(3) 0.0294(7) Uani d . 1
H H28 -0.2641 0.7508 0.2062 0.035 Uiso calc 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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
O5 Nd1 O3 . 1_556 141.66(7) ?
O5 Nd1 O4 . 2_665 85.16(7) y
O3 Nd1 O4 1_556 2_665 123.72(7) ?
O5 Nd1 O1 . . 85.06(7) y
O3 Nd1 O1 1_556 . 81.99(7) y
O4 Nd1 O1 2_665 . 71.54(7) y
O5 Nd1 O2 . 2_666 142.08(7) ?
O3 Nd1 O2 1_556 2_666 72.10(7) y
O4 Nd1 O2 2_665 2_666 83.53(7) y
O1 Nd1 O2 . 2_666 124.64(7) ?
O5 Nd1 O7 . . 73.07(7) y
O3 Nd1 O7 1_556 . 136.56(7) ?
O4 Nd1 O7 2_665 . 70.18(7) y
O1 Nd1 O7 . . 137.04(7) ?
O2 Nd1 O7 2_666 . 69.04(7) y
O5 Nd1 N1 . . 82.69(7) y
O3 Nd1 N1 1_556 . 84.74(7) y
O4 Nd1 N1 2_665 . 143.82(8) ?
O1 Nd1 N1 . . 140.45(7) ?
O2 Nd1 N1 2_666 . 85.45(7) y
O7 Nd1 N1 . . 73.68(7) y
O5 Nd1 N2 . . 72.54(7) y
O3 Nd1 N2 1_556 . 69.59(7) y
O4 Nd1 N2 2_665 . 144.11(7) ?
O1 Nd1 N2 . . 78.68(7) y
O2 Nd1 N2 2_666 . 130.91(7) ?
O7 Nd1 N2 . . 126.03(7) ?
N1 Nd1 N2 . . 61.78(7) y
C11 O1 Nd1 . . 132.49(18) ?
C11 O2 Nd1 . 2_666 152.00(19) ?
C22 O3 Nd1 . 1_554 124.74(17) ?
C22 O4 Nd1 . 2_665 148.51(19) ?
C23 O5 Nd1 . . 134.30(17) ?
Nd1 O7 H7A . . 105 ?
Nd1 O7 H7B . . 109.2 ?
H7A O7 H7B . . 109.9 ?
C1 N1 C5 . . 118.2(3) ?
C1 N1 Nd1 . . 118.68(19) ?
C5 N1 Nd1 . . 122.42(19) ?
C10 N2 C6 . . 117.7(3) ?
C10 N2 Nd1 . . 120.7(2) ?
C6 N2 Nd1 . . 121.29(19) ?
C15 N3 C14 . . 116.9(3) ?
C21 N4 C17 . . 116.9(3) ?
C27 N5 C26 . . 117.3(3) ?
N1 C1 C2 . . 123.4(3) ?
N1 C1 H1 . . 118.3 ?
C2 C1 H1 . . 118.3 ?
C1 C2 C3 . . 118.2(3) ?
C1 C2 H2 . . 120.9 ?
C3 C2 H2 . . 120.9 ?
C4 C3 C2 . . 119.4(3) ?
C4 C3 H3 . . 120.3 ?
C2 C3 H3 . . 120.3 ?
C3 C4 C5 . . 119.6(3) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
N1 C5 C4 . . 121.2(3) ?
N1 C5 C6 . . 116.8(3) ?
C4 C5 C6 . . 122.0(3) ?
N2 C6 C7 . . 121.3(3) ?
N2 C6 C5 . . 116.7(3) ?
C7 C6 C5 . . 121.9(3) ?
C8 C7 C6 . . 119.8(3) ?
C8 C7 H7 . . 120.1 ?
C6 C7 H7 . . 120.1 ?
C9 C8 C7 . . 119.3(3) ?
C9 C8 H8 . . 120.4 ?
C7 C8 H8 . . 120.4 ?
C8 C9 C10 . . 118.0(3) ?
C8 C9 H9 . . 121 ?
C10 C9 H9 . . 121 ?
N2 C10 C9 . . 123.9(3) ?
N2 C10 H10 . . 118.1 ?
C9 C10 H10 . . 118.1 ?
O1 C11 O2 . . 125.5(3) ?
O1 C11 C12 . . 117.3(2) ?
O2 C11 C12 . . 117.2(2) ?
C16 C12 C13 . . 118.2(3) ?
C16 C12 C11 . . 120.5(3) ?
C13 C12 C11 . . 121.3(2) ?
C12 C13 C14 . . 119.2(3) ?
C12 C13 H13 . . 120.4 ?
C14 C13 H13 . . 120.4 ?
N3 C14 C13 . . 122.8(3) ?
N3 C14 C17 . . 115.7(2) ?
C13 C14 C17 . . 121.5(3) ?
N3 C15 C16 . . 124.1(3) ?
N3 C15 H15 . . 118 ?
C16 C15 H15 . . 118 ?
C12 C16 C15 . . 118.8(3) ?
C12 C16 H16 . . 120.6 ?
C15 C16 H16 . . 120.6 ?
N4 C17 C18 . . 122.9(3) ?
N4 C17 C14 . . 116.5(2) ?
C18 C17 C14 . . 120.6(3) ?
C19 C18 C17 . . 119.3(3) ?
C19 C18 H18 . . 120.3 ?
C17 C18 H18 . . 120.3 ?
C18 C19 C20 . . 118.4(3) ?
C18 C19 C22 . . 120.3(3) ?
C20 C19 C22 . . 121.2(3) ?
C21 C20 C19 . . 118.3(3) ?
C21 C20 H20 . . 120.8 ?
C19 C20 H20 . . 120.8 ?
N4 C21 C20 . . 124.2(3) ?
N4 C21 H21 . . 117.9 ?
C20 C21 H21 . . 117.9 ?
O4 C22 O3 . . 125.5(3) ?
O4 C22 C19 . . 117.3(3) ?
O3 C22 C19 . . 117.1(2) ?
O6 C23 O5 . . 125.5(3) ?
O6 C23 C24 . . 118.5(3) ?
O5 C23 C24 . . 116.1(2) ?
C28 C24 C25 . . 118.7(3) ?
C28 C24 C23 . . 121.0(3) ?
C25 C24 C23 . . 120.3(3) ?
C24 C25 C26 . . 119.4(3) ?
C24 C25 H25 . . 120.3 ?
C26 C25 H25 . . 120.3 ?
N5 C26 C25 . . 122.4(3) ?
N5 C26 C26 . 2_575 116.1(3) ?
C25 C26 C26 . 2_575 121.5(3) ?
N5 C27 C28 . . 123.8(3) ?
N5 C27 H27 . . 118.1 ?
C28 C27 H27 . . 118.1 ?
C24 C28 C27 . . 118.4(3) ?
C24 C28 H28 . . 120.8 ?
C27 C28 H28 . . 120.8 ?
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 O5 . 2.386(2) y
Nd1 O3 1_556 2.399(2) y
Nd1 O4 2_665 2.4120(19) y
Nd1 O1 . 2.4309(19) y
Nd1 O2 2_666 2.4443(19) y
Nd1 O7 . 2.513(2) y
Nd1 N1 . 2.618(2) y
Nd1 N2 . 2.659(2) y
O1 C11 . 1.252(3) y
O2 C11 . 1.256(3) y
O2 Nd1 2_666 2.4443(19) ?
O3 C22 . 1.255(4) y
O3 Nd1 1_554 2.399(2) ?
O4 C22 . 1.252(3) y
O4 Nd1 2_665 2.4120(19) ?
O5 C23 . 1.267(4) y
O6 C23 . 1.246(4) y
O7 H7A . 0.8298 ?
O7 H7B . 0.8078 ?
N1 C1 . 1.341(4) ?
N1 C5 . 1.351(4) ?
N2 C10 . 1.342(4) ?
N2 C6 . 1.350(4) ?
N3 C15 . 1.338(4) ?
N3 C14 . 1.344(4) ?
N4 C21 . 1.337(4) ?
N4 C17 . 1.343(4) ?
N5 C27 . 1.336(4) ?
N5 C26 . 1.347(4) ?
C1 C2 . 1.376(4) ?
C1 H1 . 0.95 ?
C2 C3 . 1.379(5) ?
C2 H2 . 0.95 ?
C3 C4 . 1.374(5) ?
C3 H3 . 0.95 ?
C4 C5 . 1.390(4) ?
C4 H4 . 0.95 ?
C5 C6 . 1.484(4) ?
C6 C7 . 1.394(4) ?
C7 C8 . 1.376(5) ?
C7 H7 . 0.95 ?
C8 C9 . 1.376(5) ?
C8 H8 . 0.95 ?
C9 C10 . 1.385(5) ?
C9 H9 . 0.95 ?
C10 H10 . 0.95 ?
C11 C12 . 1.517(4) ?
C12 C16 . 1.379(4) ?
C12 C13 . 1.392(4) ?
C13 C14 . 1.392(4) ?
C13 H13 . 0.95 ?
C14 C17 . 1.494(4) ?
C15 C16 . 1.384(4) ?
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
C17 C18 . 1.388(4) ?
C18 C19 . 1.385(4) ?
C18 H18 . 0.95 ?
C19 C20 . 1.386(4) ?
C19 C22 . 1.512(4) ?
C20 C21 . 1.384(5) ?
C20 H20 . 0.95 ?
C21 H21 . 0.95 ?
C23 C24 . 1.512(4) ?
C24 C28 . 1.380(4) ?
C24 C25 . 1.384(4) ?
C25 C26 . 1.390(4) ?
C25 H25 . 0.95 ?
C26 C26 2_575 1.488(6) ?
C27 C28 . 1.391(5) ?
C27 H27 . 0.95 ?
C28 H28 . 0.95 ?
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
O7 H7A O6 . 0.83 1.92 2.731(3) 164
O7 H7A O5 . 0.83 2.53 2.918(3) 110
O7 H7B O6 2_566 0.81 2.02 2.811(3) 165
