#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:31:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180014 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/08/7030854.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_7030854
loop_
_publ_author_name
'Chen, Wen-Bin'
'Li, Zhi-Xin'
'Yu, Xin-Wei'
'Yang, Meng'
'Qiu, Yan-Xuan'
'Dong, Wen'
'Sun, Ya-Qiu'
_publ_section_title
;
 Syntheses, structures and properties of 5-azotetrazolyl salicylic acid
 and its dilanthanide complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9090
_journal_page_last               9097
_journal_paper_doi               10.1039/c4dt00278d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C32 H46 N24 O26 Tb2'
_chemical_formula_weight         1500.79
_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
_cell_angle_alpha                110.617(2)
_cell_angle_beta                 94.603(2)
_cell_angle_gamma                105.596(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6491(13)
_cell_length_b                   11.9680(17)
_cell_length_c                   12.9137(18)
_cell_measurement_reflns_used    5783
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.030
_cell_measurement_theta_min      1.72
_cell_volume                     1318.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0166
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11019
_diffrn_reflns_theta_full        27.03
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  0.473
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            light-orange
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744.0
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5783
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0241P)²+2.1988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                5183
_reflns_number_total             5783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00278d2.cif
_cod_data_source_block           2
_cod_depositor_comments
;Adding full bibliography for 7030851--7030857.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7030854
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 0.529269(15) 0.802225(13) 0.382703(11) 0.01522(6) Uani 1 1 d .
O4 O 0.4804(2) 0.9579(2) 0.32952(17) 0.0193(4) Uani 1 1 d .
O9 O 0.3688(2) 0.6922(2) 0.20301(18) 0.0190(4) Uani 1 1 d D
O7 O 0.4172(3) 0.6151(2) 0.41046(18) 0.0224(5) Uani 1 1 d D
O1 O 0.6246(2) 0.64999(19) 0.24998(17) 0.0180(4) Uani 1 1 d .
O11 O 0.8032(3) 0.1657(2) 0.3725(2) 0.0266(5) Uani 1 1 d D
O5 O 0.6086(2) 0.8906(2) 0.57710(17) 0.0218(5) Uani 1 1 d .
O3 O 0.9319(2) 0.6511(2) 0.49190(18) 0.0244(5) Uani 1 1 d D
O8 O 0.7416(3) 0.9226(2) 0.3439(2) 0.0310(6) Uani 1 1 d D
O2 O 0.7326(2) 0.7264(2) 0.42780(17) 0.0209(4) Uani 1 1 d .
O10 O 0.3092(3) 0.8279(3) 0.44122(19) 0.0272(5) Uani 1 1 d D
O12 O 0.3202(3) 0.4435(2) 0.0954(2) 0.0276(5) Uani 1 1 d D
C7 C 0.7215(3) 0.6566(3) 0.3253(2) 0.0156(5) Uani 1 1 d .
C6 C 0.8228(3) 0.5106(3) 0.1844(2) 0.0167(6) Uani 1 1 d .
H3 H 0.7538 0.5077 0.1259 0.020 Uiso 1 1 calc R
C1 C 0.8245(3) 0.5822(3) 0.2958(2) 0.0155(5) Uani 1 1 d .
C2 C 0.9269(3) 0.5850(3) 0.3818(2) 0.0190(6) Uani 1 1 d .
C5 C 0.9208(3) 0.4429(3) 0.1572(2) 0.0173(6) Uani 1 1 d .
C3 C 1.0239(3) 0.5155(3) 0.3546(3) 0.0219(6) Uani 1 1 d .
H6 H 1.0923 0.5172 0.4128 0.026 Uiso 1 1 calc R
C4 C 1.0202(4) 0.4447(3) 0.2437(3) 0.0235(6) Uani 1 1 d .
H7 H 1.0853 0.3967 0.2256 0.028 Uiso 1 1 calc R
N2 N 1.0069(3) 0.3262(2) 0.0134(2) 0.0188(5) Uani 1 1 d .
N1 N 0.9067(3) 0.3750(2) 0.0404(2) 0.0187(5) Uani 1 1 d .
C8 C 0.9865(3) 0.2602(3) -0.1038(2) 0.0165(6) Uani 1 1 d .
N3 N 1.0807(3) 0.2018(2) -0.1473(2) 0.0201(5) Uani 1 1 d .
H1 H 1.1586 0.1971 -0.1109 0.024 Uiso 1 1 calc R
N6 N 0.8807(3) 0.2487(2) -0.1838(2) 0.0178(5) Uani 1 1 d .
N5 N 0.9115(3) 0.1807(2) -0.2804(2) 0.0189(5) Uani 1 1 d .
N4 N 1.0306(3) 0.1519(2) -0.2590(2) 0.0206(5) Uani 1 1 d .
C15 C 0.5921(3) 0.9692(3) 0.6679(2) 0.0153(5) Uani 1 1 d .
C14 C 0.6355(3) 1.0490(3) 0.8767(2) 0.0169(6) Uani 1 1 d .
H11 H 0.5724 1.0971 0.8741 0.020 Uiso 1 1 calc R
C10 C 0.7568(3) 0.9013(3) 0.7809(3) 0.0191(6) Uani 1 1 d .
C9 C 0.6620(3) 0.9718(3) 0.7763(2) 0.0163(6) Uani 1 1 d .
C11 C 0.8214(3) 0.9100(3) 0.8859(3) 0.0233(6) Uani 1 1 d .
H14 H 0.8854 0.8629 0.8894 0.028 Uiso 1 1 calc R
C13 C 0.6993(3) 1.0574(3) 0.9806(2) 0.0173(6) Uani 1 1 d .
C12 C 0.7925(3) 0.9864(3) 0.9838(3) 0.0217(6) Uani 1 1 d .
H13 H 0.8363 0.9910 1.0544 0.026 Uiso 1 1 calc R
N8 N 0.5919(3) 1.1951(2) 1.0823(2) 0.0188(5) Uani 1 1 d .
N7 N 0.6798(3) 1.1342(2) 1.0864(2) 0.0199(5) Uani 1 1 d .
O6 O 0.7890(3) 0.8252(2) 0.68827(19) 0.0274(5) Uani 1 1 d D
C16 C 0.5776(3) 1.2705(3) 1.1906(2) 0.0176(6) Uani 1 1 d .
N9 N 0.4946(3) 1.3456(2) 1.2012(2) 0.0215(5) Uani 1 1 d .
N12 N 0.6387(3) 1.2778(2) 1.2897(2) 0.0206(5) Uani 1 1 d .
N10 N 0.5052(3) 1.4016(2) 1.3127(2) 0.0231(5) Uani 1 1 d .
N11 N 0.5915(3) 1.3612(3) 1.3653(2) 0.0245(6) Uani 1 1 d .
O13 O 0.4015(4) 0.2590(3) 0.9260(3) 0.0484(7) Uani 1 1 d D
H8 H 0.812(4) 0.902(5) 0.330(5) 0.073 Uiso 1 1 d D
H9 H 0.748(6) 0.991(3) 0.346(5) 0.073 Uiso 1 1 d D
H4 H 0.404(6) 0.623(5) 0.473(2) 0.073 Uiso 1 1 d D
H5 H 0.443(6) 0.555(4) 0.381(4) 0.073 Uiso 1 1 d D
H16 H 0.249(5) 0.835(5) 0.400(3) 0.073 Uiso 1 1 d D
H15 H 0.298(4) 0.711(4) 0.188(5) 0.073 Uiso 1 1 d D
H19 H 0.759(5) 0.194(5) 0.337(4) 0.073 Uiso 1 1 d D
H21 H 0.234(2) 0.403(4) 0.080(5) 0.073 Uiso 1 1 d D
H18 H 0.884(3) 0.213(4) 0.400(4) 0.073 Uiso 1 1 d D
H20 H 0.368(4) 0.414(5) 0.125(4) 0.073 Uiso 1 1 d D
H17 H 0.280(5) 0.821(5) 0.496(3) 0.073 Uiso 1 1 d D
H10 H 0.748(6) 0.835(5) 0.638(3) 0.073 Uiso 1 1 d D
H2 H 0.877(5) 0.691(5) 0.495(5) 0.073 Uiso 1 1 d D
H12 H 0.354(5) 0.618(2) 0.173(4) 0.073 Uiso 1 1 d D
H22 H 0.463(5) 0.279(5) 0.887(4) 0.073 Uiso 1 1 d D
H23 H 0.441(5) 0.227(5) 0.963(4) 0.073 Uiso 1 1 d D
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
O5 Tb1 O4 107.31(7) .
O5 Tb1 O8 95.36(9) .
O4 Tb1 O8 68.96(8) .
O5 Tb1 O10 79.91(8) .
O4 Tb1 O10 72.73(8) .
O8 Tb1 O10 137.96(9) .
O5 Tb1 O7 84.65(8) .
O4 Tb1 O7 143.55(8) .
O8 Tb1 O7 145.76(8) .
O10 Tb1 O7 75.89(8) .
O5 Tb1 O9 160.11(8) .
O4 Tb1 O9 74.32(7) .
O8 Tb1 O9 103.47(9) .
O10 Tb1 O9 81.81(8) .
O7 Tb1 O9 83.36(8) .
O5 Tb1 O1 124.56(7) .
O4 Tb1 O1 117.62(7) .
O8 Tb1 O1 73.75(8) .
O10 Tb1 O1 142.07(8) .
O7 Tb1 O1 78.16(7) .
O9 Tb1 O1 68.06(7) .
O5 Tb1 O2 71.92(7) .
O4 Tb1 O2 142.06(8) .
O8 Tb1 O2 73.32(8) .
O10 Tb1 O2 140.32(8) .
O7 Tb1 O2 74.21(8) .
O9 Tb1 O2 119.47(7) .
O1 Tb1 O2 52.74(7) .
C15 O4 Tb1 150.35(19) 2_676
Tb1 O9 H15 122(4) .
Tb1 O9 H12 117(4) .
H15 O9 H12 111(3) .
Tb1 O7 H4 117(4) .
Tb1 O7 H5 118(4) .
H4 O7 H5 112(3) .
C7 O1 Tb1 94.01(17) .
H19 O11 H18 110(3) .
C15 O5 Tb1 142.95(19) .
C2 O3 H2 108(4) .
Tb1 O8 H8 126(4) .
Tb1 O8 H9 120(4) .
H8 O8 H9 114(3) .
C7 O2 Tb1 92.83(17) .
Tb1 O10 H16 119(4) .
Tb1 O10 H17 128(4) .
H16 O10 H17 112(3) .
H21 O12 H20 111(3) .
O1 C7 O2 120.4(3) .
O1 C7 C1 120.7(3) .
O2 C7 C1 118.9(3) .
C1 C6 C5 120.8(3) .
C1 C6 H3 119.6 .
C5 C6 H3 119.6 .
C6 C1 C2 118.9(3) .
C6 C1 C7 121.1(3) .
C2 C1 C7 119.9(3) .
O3 C2 C3 118.1(3) .
O3 C2 C1 121.6(3) .
C3 C2 C1 120.2(3) .
C6 C5 C4 119.6(3) .
C6 C5 N1 114.5(3) .
C4 C5 N1 125.9(3) .
C4 C3 C2 120.0(3) .
C4 C3 H6 120.0 .
C2 C3 H6 120.0 .
C3 C4 C5 120.4(3) .
C3 C4 H7 119.8 .
C5 C4 H7 119.8 .
N1 N2 C8 112.3(2) .
N2 N1 C5 115.1(2) .
N3 C8 N6 111.8(3) .
N3 C8 N2 120.5(3) .
N6 C8 N2 127.6(3) .
C8 N3 N4 104.7(2) .
C8 N3 H1 127.7 .
N4 N3 H1 127.7 .
C8 N6 N5 104.7(2) .
N4 N5 N6 109.6(2) .
N5 N4 N3 109.2(2) .
O4 C15 O5 123.7(3) 2_676
O4 C15 C9 119.0(2) 2_676
O5 C15 C9 117.3(3) .
C13 C14 C9 121.5(3) .
C13 C14 H11 119.2 .
C9 C14 H11 119.2 .
O6 C10 C11 117.7(3) .
O6 C10 C9 122.8(3) .
C11 C10 C9 119.5(3) .
C14 C9 C10 118.9(3) .
C14 C9 C15 118.7(3) .
C10 C9 C15 122.4(3) .
C12 C11 C10 120.4(3) .
C12 C11 H14 119.8 .
C10 C11 H14 119.8 .
C14 C13 C12 118.9(3) .
C14 C13 N7 125.3(3) .
C12 C13 N7 115.8(3) .
C11 C12 C13 120.8(3) .
C11 C12 H13 119.6 .
C13 C12 H13 119.6 .
N7 N8 C16 112.5(2) .
N8 N7 C13 115.2(2) .
C10 O6 H10 104(4) .
N12 C16 N9 112.3(3) .
N12 C16 N8 127.6(3) .
N9 C16 N8 120.1(3) .
C16 N9 N10 104.3(2) .
C16 N12 N11 104.4(3) .
N11 N10 N9 109.3(2) .
N10 N11 N12 109.7(2) .
H22 O13 H23 105(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O5 2.322(2) .
Tb1 O4 2.343(2) .
Tb1 O8 2.369(2) .
Tb1 O10 2.371(2) .
Tb1 O7 2.374(2) .
Tb1 O9 2.386(2) .
Tb1 O1 2.461(2) .
Tb1 O2 2.481(2) .
O4 C15 1.249(4) 2_676
O9 H15 0.802(19) .
O9 H12 0.800(19) .
O7 H4 0.798(19) .
O7 H5 0.801(19) .
O1 C7 1.260(4) .
O11 H19 0.810(19) .
O11 H18 0.798(19) .
O5 C15 1.273(3) .
O3 C2 1.351(4) .
O3 H2 0.80(2) .
O8 H8 0.797(19) .
O8 H9 0.789(19) .
O2 C7 1.270(3) .
O10 H16 0.804(19) .
O10 H17 0.799(19) .
O12 H21 0.811(19) .
O12 H20 0.800(19) .
C7 C1 1.490(4) .
C6 C1 1.387(4) .
C6 C5 1.393(4) .
C6 H3 0.9500 .
C1 C2 1.411(4) .
C2 C3 1.399(4) .
C5 C4 1.403(4) .
C5 N1 1.414(4) .
C3 C4 1.375(4) .
C3 H6 0.9500 .
C4 H7 0.9500 .
N2 N1 1.269(3) .
N2 C8 1.408(4) .
C8 N3 1.333(4) .
C8 N6 1.335(4) .
N3 N4 1.340(4) .
N3 H1 0.8800 .
N6 N5 1.335(3) .
N5 N4 1.321(3) .
C15 O4 1.249(3) 2_676
C15 C9 1.490(4) .
C14 C13 1.389(4) .
C14 C9 1.392(4) .
C14 H11 0.9500 .
C10 O6 1.341(4) .
C10 C11 1.403(4) .
C10 C9 1.413(4) .
C11 C12 1.375(4) .
C11 H14 0.9500 .
C13 C12 1.401(4) .
C13 N7 1.414(4) .
C12 H13 0.9500 .
N8 N7 1.267(4) .
N8 C16 1.413(4) .
O6 H10 0.80(2) .
C16 N12 1.330(4) .
C16 N9 1.336(4) .
N9 N10 1.339(4) .
N12 N11 1.337(4) .
N10 N11 1.320(4) .
O13 H22 0.845(19) .
O13 H23 0.838(19) .
