#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:31:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180014 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/08/7030853.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_7030853
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 Dy2 N24 O26'
_chemical_formula_weight         1507.93
_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                110.424(2)
_cell_angle_beta                 94.582(2)
_cell_angle_gamma                105.450(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6459(14)
_cell_length_b                   11.9523(18)
_cell_length_c                   12.8750(19)
_cell_measurement_reflns_used    8207
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.090
_cell_measurement_theta_min      1.92
_cell_volume                     1316.0(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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0186
_diffrn_reflns_av_unetI/netI     0.0305
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11004
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.926
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             746.0
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.011(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   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5800
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0197P)²+2.1710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0568
_reflns_number_gt                4966
_reflns_number_total             5800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00278d2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 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               7030853
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
Dy1 Dy 0.471937(16) 0.199653(14) 0.118180(12) 0.01483(6) Uani 1 1 d .
O8 O 0.6312(2) 0.3075(2) 0.29679(19) 0.0189(5) Uani 1 1 d D
O4 O 0.5192(2) 0.0427(2) 0.16876(18) 0.0196(5) Uani 1 1 d .
O1 O 0.3759(2) 0.3504(2) 0.25012(17) 0.0173(4) Uani 1 1 d .
O11 O 0.1967(3) 0.8358(2) 0.1286(2) 0.0274(5) Uani 1 1 d D
O10 O 0.5827(3) 0.3860(2) 0.08970(19) 0.0214(5) Uani 1 1 d D
O9 O 0.6914(3) 0.1754(3) 0.0600(2) 0.0250(5) Uani 1 1 d D
O5 O 0.3920(2) 0.1089(2) -0.07530(18) 0.0203(5) Uani 1 1 d .
O7 O 0.2604(3) 0.0791(2) 0.1558(2) 0.0299(6) Uani 1 1 d D
O2 O 0.2682(2) 0.2738(2) 0.07184(18) 0.0214(5) Uani 1 1 d .
C7 C 0.2788(3) 0.3440(3) 0.1745(3) 0.0157(6) Uani 1 1 d .
C1 C 0.1759(3) 0.4180(3) 0.2039(3) 0.0163(6) Uani 1 1 d .
C6 C 0.1778(3) 0.4899(3) 0.3153(3) 0.0161(6) Uani 1 1 d .
H3 H 0.2475 0.4933 0.3738 0.019 Uiso 1 1 calc R
C4 C -0.0208(4) 0.5543(3) 0.2559(3) 0.0224(7) Uani 1 1 d .
H7 H -0.0871 0.6014 0.2737 0.027 Uiso 1 1 calc R
C2 C 0.0735(3) 0.4148(3) 0.1178(3) 0.0191(6) Uani 1 1 d .
C5 C 0.0791(3) 0.5571(3) 0.3428(3) 0.0176(6) Uani 1 1 d .
C3 C -0.0234(4) 0.4839(3) 0.1455(3) 0.0227(7) Uani 1 1 d .
H6 H -0.0920 0.4823 0.0873 0.027 Uiso 1 1 calc R
O3 O 0.0678(3) 0.3482(2) 0.00784(19) 0.0248(5) Uani 1 1 d D
N2 N -0.0070(3) 0.6734(2) 0.4867(2) 0.0179(5) Uani 1 1 d .
N1 N 0.0924(3) 0.6247(2) 0.4592(2) 0.0187(5) Uani 1 1 d .
C8 C 0.0132(3) 0.7398(3) 0.6041(3) 0.0165(6) Uani 1 1 d .
N6 N 0.1184(3) 0.7507(2) 0.6839(2) 0.0178(5) Uani 1 1 d .
N3 N -0.0811(3) 0.7977(3) 0.6475(2) 0.0210(6) Uani 1 1 d .
H1 H -0.1590 0.8025 0.6109 0.025 Uiso 1 1 calc R
N5 N 0.0881(3) 0.8188(3) 0.7807(2) 0.0187(5) Uani 1 1 d .
N4 N -0.0314(3) 0.8474(3) 0.7595(2) 0.0202(6) Uani 1 1 d .
C15 C 0.5911(3) -0.0303(3) 0.1660(2) 0.0155(6) Uani 1 1 d .
C14 C 0.6350(3) 0.0491(3) 0.3750(3) 0.0163(6) Uani 1 1 d .
H15 H 0.5712 0.0968 0.3722 0.020 Uiso 1 1 calc R
C9 C 0.6614(3) -0.0276(3) 0.2751(3) 0.0158(6) Uani 1 1 d .
C13 C 0.6992(3) 0.0582(3) 0.4796(3) 0.0175(6) Uani 1 1 d .
C10 C 0.7566(3) -0.0986(3) 0.2790(3) 0.0197(6) Uani 1 1 d .
C12 C 0.7926(4) -0.0134(3) 0.4824(3) 0.0218(7) Uani 1 1 d .
H11 H 0.8371 -0.0086 0.5530 0.026 Uiso 1 1 calc R
C11 C 0.8203(4) -0.0904(3) 0.3843(3) 0.0228(7) Uani 1 1 d .
H12 H 0.8832 -0.1386 0.3878 0.027 Uiso 1 1 calc R
O6 O 0.7889(3) -0.1740(2) 0.1864(2) 0.0275(5) Uani 1 1 d D
N8 N 0.5918(3) 0.1954(2) 0.5819(2) 0.0182(5) Uani 1 1 d .
N7 N 0.6791(3) 0.1336(2) 0.5853(2) 0.0201(6) Uani 1 1 d .
C16 C 0.5775(3) 0.2697(3) 0.6898(3) 0.0180(6) Uani 1 1 d .
N9 N 0.4942(3) 0.3447(3) 0.7011(2) 0.0210(6) Uani 1 1 d .
N12 N 0.6392(3) 0.2774(3) 0.7894(2) 0.0208(6) Uani 1 1 d .
N10 N 0.5055(3) 0.4009(3) 0.8127(2) 0.0233(6) Uani 1 1 d .
N11 N 0.5922(3) 0.3606(3) 0.8650(2) 0.0242(6) Uani 1 1 d .
O12 O 0.6793(3) 0.5560(2) 0.4046(2) 0.0309(6) Uani 1 1 d D
O13 O 0.4003(4) 0.2570(3) 0.4262(3) 0.0536(8) Uani 1 1 d D
H2 H 0.130(5) 0.315(5) 0.003(5) 0.080 Uiso 1 1 d D
H4 H 0.751(6) -0.170(6) 0.132(3) 0.080 Uiso 1 1 d D
H5 H 0.186(4) 0.096(5) 0.164(5) 0.080 Uiso 1 1 d D
H8 H 0.252(6) 0.011(3) 0.155(5) 0.080 Uiso 1 1 d D
H9 H 0.649(5) 0.382(2) 0.326(5) 0.080 Uiso 1 1 d D
H10 H 0.701(4) 0.287(4) 0.311(5) 0.080 Uiso 1 1 d D
H13 H 0.717(5) 0.175(6) 0.002(3) 0.080 Uiso 1 1 d D
H14 H 0.759(4) 0.179(6) 0.103(3) 0.080 Uiso 1 1 d D
H16 H 0.583(6) 0.369(5) 0.0244(19) 0.080 Uiso 1 1 d D
H17 H 0.555(6) 0.445(4) 0.118(4) 0.080 Uiso 1 1 d D
H18 H 0.247(5) 0.817(5) 0.167(4) 0.080 Uiso 1 1 d D
H19 H 0.120(3) 0.782(4) 0.098(4) 0.080 Uiso 1 1 d D
H21 H 0.633(5) 0.581(5) 0.368(4) 0.080 Uiso 1 1 d D
H20 H 0.766(2) 0.595(5) 0.417(5) 0.080 Uiso 1 1 d D
H23 H 0.394(6) 0.328(3) 0.467(4) 0.080 Uiso 1 1 d D
H22 H 0.458(5) 0.271(5) 0.384(4) 0.080 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'
Dy Dy -0.1892 4.4098 '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
O5 Dy1 O4 105.61(8) . .
O5 Dy1 O9 80.08(8) . .
O4 Dy1 O9 72.96(8) . .
O5 Dy1 O7 94.22(9) . .
O4 Dy1 O7 68.86(8) . .
O9 Dy1 O7 138.21(9) . .
O5 Dy1 O10 85.51(8) . .
O4 Dy1 O10 144.01(8) . .
O9 Dy1 O10 75.58(8) . .
O7 Dy1 O10 145.73(8) . .
O5 Dy1 O8 160.52(8) . .
O4 Dy1 O8 74.87(8) . .
O9 Dy1 O8 81.56(8) . .
O7 Dy1 O8 103.81(9) . .
O10 Dy1 O8 83.69(8) . .
O5 Dy1 O1 124.93(7) . .
O4 Dy1 O1 118.17(7) . .
O9 Dy1 O1 141.92(8) . .
O7 Dy1 O1 73.88(8) . .
O10 Dy1 O1 78.30(8) . .
O8 Dy1 O1 68.38(7) . .
O5 Dy1 O2 71.93(7) . .
O4 Dy1 O2 141.56(8) . .
O9 Dy1 O2 140.05(8) . .
O7 Dy1 O2 73.04(8) . .
O10 Dy1 O2 74.36(8) . .
O8 Dy1 O2 120.16(7) . .
O1 Dy1 O2 53.06(7) . .
O5 Dy1 C7 98.58(8) . .
O4 Dy1 C7 134.27(8) . .
O9 Dy1 C7 150.51(9) . .
O7 Dy1 C7 71.20(8) . .
O10 Dy1 C7 74.95(8) . .
O8 Dy1 C7 94.21(8) . .
O1 Dy1 C7 26.40(8) . .
O2 Dy1 C7 26.67(8) . .
Dy1 O8 H9 118(4) . .
Dy1 O8 H10 121(4) . .
H9 O8 H10 111(3) . .
C15 O4 Dy1 150.6(2) . .
C7 O1 Dy1 94.09(17) . .
H18 O11 H19 113(3) . .
Dy1 O10 H16 109(4) . .
Dy1 O10 H17 117(4) . .
H16 O10 H17 114(3) . .
Dy1 O9 H13 128(4) . .
Dy1 O9 H14 122(4) . .
H13 O9 H14 110(3) . .
C15 O5 Dy1 143.3(2) 2_655 .
Dy1 O7 H5 126(4) . .
Dy1 O7 H8 122(4) . .
H5 O7 H8 111(3) . .
C7 O2 Dy1 92.70(18) . .
O1 C7 O2 120.1(3) . .
O1 C7 C1 120.7(3) . .
O2 C7 C1 119.2(3) . .
O1 C7 Dy1 59.51(15) . .
O2 C7 Dy1 60.63(15) . .
C1 C7 Dy1 179.2(2) . .
C6 C1 C2 119.1(3) . .
C6 C1 C7 121.1(3) . .
C2 C1 C7 119.8(3) . .
C1 C6 C5 121.0(3) . .
C1 C6 H3 119.5 . .
C5 C6 H3 119.5 . .
C3 C4 C5 120.3(3) . .
C3 C4 H7 119.8 . .
C5 C4 H7 119.8 . .
O3 C2 C3 118.4(3) . .
O3 C2 C1 121.8(3) . .
C3 C2 C1 119.7(3) . .
C6 C5 C4 119.2(3) . .
C6 C5 N1 114.9(3) . .
C4 C5 N1 125.9(3) . .
C4 C3 C2 120.6(3) . .
C4 C3 H6 119.7 . .
C2 C3 H6 119.7 . .
C2 O3 H2 109(4) . .
N1 N2 C8 112.8(3) . .
N2 N1 C5 115.8(3) . .
N6 C8 N3 111.8(3) . .
N6 C8 N2 127.5(3) . .
N3 C8 N2 120.6(3) . .
C8 N6 N5 104.9(2) . .
C8 N3 N4 104.8(3) . .
C8 N3 H1 127.6 . .
N4 N3 H1 127.6 . .
N4 N5 N6 109.5(2) . .
N5 N4 N3 109.0(2) . .
O4 C15 O5 123.9(3) . 2_655
O4 C15 C9 118.8(3) . .
O5 C15 C9 117.3(3) 2_655 .
C9 C14 C13 121.8(3) . .
C9 C14 H15 119.1 . .
C13 C14 H15 119.1 . .
C14 C9 C10 119.2(3) . .
C14 C9 C15 118.8(3) . .
C10 C9 C15 122.0(3) . .
C14 C13 C12 118.5(3) . .
C14 C13 N7 125.8(3) . .
C12 C13 N7 115.8(3) . .
O6 C10 C11 118.0(3) . .
O6 C10 C9 123.0(3) . .
C11 C10 C9 119.0(3) . .
C11 C12 C13 120.8(3) . .
C11 C12 H11 119.6 . .
C13 C12 H11 119.6 . .
C12 C11 C10 120.7(3) . .
C12 C11 H12 119.7 . .
C10 C11 H12 119.7 . .
C10 O6 H4 110(4) . .
N7 N8 C16 112.7(3) . .
N8 N7 C13 115.4(3) . .
N12 C16 N9 111.9(3) . .
N12 C16 N8 127.9(3) . .
N9 C16 N8 120.2(3) . .
C16 N9 N10 104.5(3) . .
C16 N12 N11 104.6(3) . .
N11 N10 N9 109.2(3) . .
N10 N11 N12 109.7(3) . .
H21 O12 H20 110(3) . .
H23 O13 H22 106(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O5 2.310(2) .
Dy1 O4 2.327(2) .
Dy1 O9 2.357(2) .
Dy1 O7 2.357(2) .
Dy1 O10 2.367(2) .
Dy1 O8 2.371(2) .
Dy1 O1 2.448(2) .
Dy1 O2 2.473(2) .
Dy1 C7 2.834(3) .
O8 H9 0.799(19) .
O8 H10 0.808(19) .
O4 C15 1.244(4) .
O1 C7 1.263(4) .
O11 H18 0.797(19) .
O11 H19 0.797(19) .
O10 H16 0.795(19) .
O10 H17 0.798(19) .
O9 H13 0.810(19) .
O9 H14 0.797(19) .
O5 C15 1.273(4) 2_655
O7 H5 0.799(19) .
O7 H8 0.798(19) .
O2 C7 1.273(4) .
C7 C1 1.485(4) .
C1 C6 1.387(4) .
C1 C2 1.407(4) .
C6 C5 1.392(4) .
C6 H3 0.9500 .
C4 C3 1.370(5) .
C4 C5 1.402(5) .
C4 H7 0.9500 .
C2 O3 1.349(4) .
C2 C3 1.394(4) .
C5 N1 1.408(4) .
C3 H6 0.9500 .
O3 H2 0.80(2) .
N2 N1 1.262(4) .
N2 C8 1.409(4) .
C8 N6 1.331(4) .
C8 N3 1.330(4) .
N6 N5 1.333(4) .
N3 N4 1.343(4) .
N3 H1 0.8800 .
N5 N4 1.321(4) .
C15 O5 1.273(4) 2_655
C15 C9 1.495(4) .
C14 C9 1.383(4) .
C14 C13 1.392(4) .
C14 H15 0.9500 .
C9 C10 1.415(4) .
C13 C12 1.404(4) .
C13 N7 1.408(4) .
C10 O6 1.338(4) .
C10 C11 1.402(5) .
C12 C11 1.374(5) .
C12 H11 0.9500 .
C11 H12 0.9500 .
O6 H4 0.79(2) .
N8 N7 1.267(4) .
N8 C16 1.405(4) .
C16 N12 1.331(4) .
C16 N9 1.335(4) .
N9 N10 1.339(4) .
N12 N11 1.334(4) .
N10 N11 1.318(4) .
O12 H21 0.804(19) .
O12 H20 0.815(19) .
O13 H23 0.852(19) .
O13 H22 0.838(19) .
