#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:30:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180042 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/36/7033684.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7033684
loop_
_publ_author_name
'Yu, Yanyan'
'Zhang, Lijuan'
'Zhou, Yunshan'
'Zuhra, Zareen'
_publ_section_title
;
 Two series of reactant's ratio-dependent lanthanide organic frameworks
 derived from nicotinic acid N-oxide and oxalate: synthesis, crystal
 structures and luminescence properties.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4601
_journal_page_last               4612
_journal_paper_doi               10.1039/c4dt03668a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C26 H20 N4 O18 Tb2'
_chemical_formula_weight         994.30
_chemical_name_systematic
; 
 ? 
;
_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
_audit_update_record
;
2014-09-09 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                101.508(5)
_cell_angle_beta                 108.666(5)
_cell_angle_gamma                101.022(4)
_cell_formula_units_Z            1
_cell_length_a                   8.2954(4)
_cell_length_b                   9.7473(5)
_cell_length_c                   9.8872(6)
_cell_measurement_reflns_used    3747
_cell_measurement_temperature    102.5
_cell_measurement_theta_max      29.3516
_cell_measurement_theta_min      2.9775
_cell_volume                     713.62(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      102.5
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5412
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    5.013
_exptl_absorpt_correction_T_max  0.6340
_exptl_absorpt_correction_T_min  0.4338
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.886
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2800
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0273
_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)+(0.0255P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                2650
_reflns_number_total             2800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03668a2.cif
_cod_data_source_block           2327
_cod_depositor_comments
'Adding full bibliography for 7033683--7033684.cif.'
_cod_original_cell_volume        713.62(7)
_cod_database_code               7033684
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tb1 Tb 0.40030(2) 0.65347(2) 0.16755(2) 0.00500(8) Uani 1 1 d .
N1 N 0.2306(5) -0.0552(4) 0.1543(4) 0.0106(8) Uani 1 1 d .
N2 N 0.3661(5) 0.6693(4) 0.4936(4) 0.0070(8) Uani 1 1 d .
C1 C 0.4200(5) 0.2855(5) 0.0735(5) 0.0061(9) Uani 1 1 d U
C2 C 0.3286(5) 0.1840(5) 0.1391(5) 0.0072(9) Uani 1 1 d .
C3 C 0.2660(6) 0.2377(5) 0.2481(5) 0.0107(10) Uani 1 1 d .
H3 H 0.2744 0.3364 0.2776 0.013 Uiso 1 1 calc R
C4 C 0.1912(6) 0.1418(5) 0.3117(5) 0.0134(10) Uani 1 1 d .
H4 H 0.1538 0.1763 0.3878 0.016 Uiso 1 1 calc R
C5 C 0.1724(6) -0.0052(5) 0.2616(5) 0.0136(10) Uani 1 1 d .
H5 H 0.1193 -0.0700 0.3024 0.016 Uiso 1 1 calc R
C6 C 0.3095(6) 0.0356(5) 0.0938(5) 0.0097(9) Uani 1 1 d .
H6 H 0.3515 -0.0011 0.0216 0.012 Uiso 1 1 calc R
C7 C 0.2965(6) 1.0191(5) 0.6662(5) 0.0093(9) Uani 1 1 d .
C8 C 0.2832(5) 0.8585(5) 0.6210(5) 0.0077(9) Uani 1 1 d .
C9 C 0.1921(5) 0.7591(5) 0.6741(5) 0.0092(9) Uani 1 1 d .
H9 H 0.1323 0.7890 0.7346 0.011 Uiso 1 1 calc R
C10 C 0.1935(5) 0.6152(5) 0.6340(5) 0.0088(9) Uani 1 1 d .
H10 H 0.1338 0.5473 0.6678 0.011 Uiso 1 1 calc R
C11 C 0.2821(6) 0.5715(5) 0.5448(5) 0.0082(9) Uani 1 1 d .
H11 H 0.2842 0.4748 0.5198 0.010 Uiso 1 1 calc R
C12 C 0.3690(5) 0.8107(5) 0.5303(5) 0.0070(9) Uani 1 1 d .
H12 H 0.4291 0.8763 0.4944 0.008 Uiso 1 1 calc R
C13 C -0.0122(5) 0.5069(4) 0.0755(5) 0.0060(9) Uani 1 1 d .
O1 O 0.2089(4) -0.1967(3) 0.1071(4) 0.0132(7) Uani 1 1 d .
O2 O 0.4920(4) 0.2320(3) -0.0116(4) 0.0107(7) Uani 1 1 d .
O3 O 0.4206(4) 0.4167(3) 0.1077(3) 0.0106(7) Uani 1 1 d .
O4 O 0.4548(4) 0.6271(3) 0.4090(3) 0.0084(6) Uani 1 1 d U
O5 O 0.4394(4) 1.1057(3) 0.6798(3) 0.0085(6) Uani 1 1 d .
O6 O 0.1680(4) 1.0531(3) 0.6898(4) 0.0183(8) Uani 1 1 d .
O7 O -0.1692(4) 0.4741(3) 0.0693(3) 0.0082(6) Uani 1 1 d .
O8 O 0.1258(4) 0.5467(3) 0.1906(3) 0.0086(7) Uani 1 1 d .
O9 O 0.7110(4) 0.6597(3) 0.2539(3) 0.0098(7) Uani 1 1 d .
H9A H 0.7330 0.5982 0.1938 0.015 Uiso 1 1 d R
H9B H 0.7735 0.7447 0.2660 0.015 Uiso 1 1 d R
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'
Tb Tb -0.1723 4.1537 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Tb1 O4 84.86(11) . .
O3 Tb1 O2 105.64(11) . 2_665
O4 Tb1 O2 147.01(10) . 2_665
O3 Tb1 O1 143.13(10) . 1_565
O4 Tb1 O1 112.58(11) . 1_565
O2 Tb1 O1 77.76(11) 2_665 1_565
O3 Tb1 O5 143.48(10) . 2_676
O4 Tb1 O5 77.79(11) . 2_676
O2 Tb1 O5 75.55(11) 2_665 2_676
O1 Tb1 O5 73.36(10) 1_565 2_676
O3 Tb1 O7 72.58(10) . 2_565
O4 Tb1 O7 132.80(11) . 2_565
O2 Tb1 O7 79.93(11) 2_665 2_565
O1 Tb1 O7 71.97(10) 1_565 2_565
O5 Tb1 O7 140.90(10) 2_676 2_565
O3 Tb1 O8 85.38(10) . .
O4 Tb1 O8 69.74(10) . .
O2 Tb1 O8 140.93(10) 2_665 .
O1 Tb1 O8 72.06(11) 1_565 .
O5 Tb1 O8 117.22(10) 2_676 .
O7 Tb1 O8 67.63(10) 2_565 .
O3 Tb1 O9 71.68(10) . .
O4 Tb1 O9 77.58(10) . .
O2 Tb1 O9 76.41(11) 2_665 .
O1 Tb1 O9 141.84(11) 1_565 .
O5 Tb1 O9 73.31(10) 2_676 .
O7 Tb1 O9 129.28(10) 2_565 .
O8 Tb1 O9 141.50(10) . .
O1 N1 C5 119.1(4) . .
O1 N1 C6 119.5(4) . .
C5 N1 C6 121.4(4) . .
O4 N2 C11 119.6(4) . .
O4 N2 C12 118.8(4) . .
C11 N2 C12 121.6(4) . .
O3 C1 O2 124.8(4) . .
O3 C1 C2 117.9(4) . .
O2 C1 C2 117.3(4) . .
C6 C2 C3 119.3(4) . .
C6 C2 C1 120.1(4) . .
C3 C2 C1 120.6(4) . .
C4 C3 C2 118.9(4) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C5 C4 C3 119.7(4) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
N1 C5 C4 120.3(5) . .
N1 C5 H5 119.8 . .
C4 C5 H5 119.8 . .
N1 C6 C2 120.2(4) . .
N1 C6 H6 119.9 . .
C2 C6 H6 119.9 . .
O6 C7 O5 126.7(4) . .
O6 C7 C8 117.0(4) . .
O5 C7 C8 116.3(4) . .
C12 C8 C9 119.6(4) . .
C12 C8 C7 118.7(4) . .
C9 C8 C7 121.6(4) . .
C10 C9 C8 118.2(4) . .
C10 C9 H9 120.9 . .
C8 C9 H9 120.9 . .
C11 C10 C9 120.8(4) . .
C11 C10 H10 119.6 . .
C9 C10 H10 119.6 . .
N2 C11 C10 119.7(4) . .
N2 C11 H11 120.2 . .
C10 C11 H11 120.2 . .
N2 C12 C8 120.1(4) . .
N2 C12 H12 119.9 . .
C8 C12 H12 119.9 . .
O8 C13 O7 126.7(4) . .
O8 C13 C13 117.1(4) . 2_565
O7 C13 C13 116.3(4) . 2_565
N1 O1 Tb1 132.5(2) . 1_545
C1 O2 Tb1 126.3(3) . 2_665
C1 O3 Tb1 175.9(3) . .
N2 O4 Tb1 124.3(2) . .
C7 O5 Tb1 133.3(3) . 2_676
C13 O7 Tb1 118.3(3) . 2_565
C13 O8 Tb1 117.2(3) . .
Tb1 O9 H9A 112.1 . .
Tb1 O9 H9B 109.5 . .
H9A O9 H9B 109.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O3 2.318(3) .
Tb1 O4 2.360(3) .
Tb1 O2 2.369(3) 2_665
Tb1 O1 2.374(3) 1_565
Tb1 O5 2.380(3) 2_676
Tb1 O7 2.399(3) 2_565
Tb1 O8 2.417(3) .
Tb1 O9 2.426(3) .
N1 O1 1.322(5) .
N1 C5 1.345(6) .
N1 C6 1.345(6) .
N2 O4 1.334(5) .
N2 C11 1.347(6) .
N2 C12 1.347(5) .
C1 O3 1.254(5) .
C1 O2 1.266(5) .
C1 C2 1.503(6) .
C2 C6 1.388(6) .
C2 C3 1.393(6) .
C3 C4 1.384(7) .
C3 H3 0.9300 .
C4 C5 1.380(7) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 O6 1.251(5) .
C7 O5 1.267(5) .
C7 C8 1.512(6) .
C8 C12 1.377(6) .
C8 C9 1.401(6) .
C9 C10 1.382(6) .
C9 H9 0.9300 .
C10 C11 1.373(6) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 O8 1.256(5) .
C13 O7 1.259(5) .
C13 C13 1.552(9) 2_565
O1 Tb1 2.374(3) 1_545
O2 Tb1 2.369(3) 2_665
O5 Tb1 2.380(3) 2_676
O7 Tb1 2.399(3) 2_565
O9 H9A 0.8461 .
O9 H9B 0.8528 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 C1 C2 C6 173.9(4) . .
O2 C1 C2 C6 -6.6(6) . .
O3 C1 C2 C3 -7.7(6) . .
O2 C1 C2 C3 171.8(4) . .
C6 C2 C3 C4 1.9(6) . .
C1 C2 C3 C4 -176.5(4) . .
C2 C3 C4 C5 -3.0(6) . .
O1 N1 C5 C4 -179.2(4) . .
C6 N1 C5 C4 0.6(7) . .
C3 C4 C5 N1 1.7(7) . .
O1 N1 C6 C2 178.1(3) . .
C5 N1 C6 C2 -1.7(6) . .
C3 C2 C6 N1 0.4(6) . .
C1 C2 C6 N1 178.8(4) . .
O6 C7 C8 C12 150.0(4) . .
O5 C7 C8 C12 -31.8(6) . .
O6 C7 C8 C9 -32.7(6) . .
O5 C7 C8 C9 145.6(4) . .
C12 C8 C9 C10 0.7(6) . .
C7 C8 C9 C10 -176.7(4) . .
C8 C9 C10 C11 0.1(6) . .
O4 N2 C11 C10 178.8(4) . .
C12 N2 C11 C10 1.5(6) . .
C9 C10 C11 N2 -1.2(6) . .
O4 N2 C12 C8 -178.1(4) . .
C11 N2 C12 C8 -0.7(6) . .
C9 C8 C12 N2 -0.4(6) . .
C7 C8 C12 N2 177.0(4) . .
C5 N1 O1 Tb1 -97.6(4) . 1_545
C6 N1 O1 Tb1 82.6(5) . 1_545
O3 C1 O2 Tb1 -12.6(6) . 2_665
C2 C1 O2 Tb1 167.9(3) . 2_665
O2 C1 O3 Tb1 134(4) . .
C2 C1 O3 Tb1 -46(4) . .
O4 Tb1 O3 C1 87(4) . .
O2 Tb1 O3 C1 -125(4) 2_665 .
O1 Tb1 O3 C1 -34(4) 1_565 .
O5 Tb1 O3 C1 149(4) 2_676 .
O7 Tb1 O3 C1 -51(4) 2_565 .
O8 Tb1 O3 C1 17(4) . .
O9 Tb1 O3 C1 166(4) . .
C11 N2 O4 Tb1 123.0(3) . .
C12 N2 O4 Tb1 -59.6(4) . .
O3 Tb1 O4 N2 -135.4(3) . .
O2 Tb1 O4 N2 113.6(3) 2_665 .
O1 Tb1 O4 N2 10.9(3) 1_565 .
O5 Tb1 O4 N2 76.9(3) 2_676 .
O7 Tb1 O4 N2 -75.0(3) 2_565 .
O8 Tb1 O4 N2 -48.5(3) . .
O9 Tb1 O4 N2 152.2(3) . .
O6 C7 O5 Tb1 28.2(7) . 2_676
C8 C7 O5 Tb1 -149.9(3) . 2_676
O8 C13 O7 Tb1 -165.0(3) . 2_565
C13 C13 O7 Tb1 13.6(6) 2_565 2_565
O7 C13 O8 Tb1 -166.2(3) . .
C13 C13 O8 Tb1 15.3(6) 2_565 .
O3 Tb1 O8 C13 -88.9(3) . .
O4 Tb1 O8 C13 -175.1(3) . .
O2 Tb1 O8 C13 20.4(4) 2_665 .
O1 Tb1 O8 C13 61.6(3) 1_565 .
O5 Tb1 O8 C13 121.2(3) 2_676 .
O7 Tb1 O8 C13 -15.8(3) 2_565 .
O9 Tb1 O8 C13 -141.4(3) . .
