#------------------------------------------------------------------------------
#$Date: 2021-03-23 11:11:20 +0200 (Tue, 23 Mar 2021) $
#$Revision: 263249 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/12/1561205.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_1561205
loop_
_publ_author_name
'Guo, Meng Yue'
'Zhang, Xin'
'Zhao, Liang'
'Li, Yue Kang'
'Chen, Dian Yu'
'Yang, Gao Wen'
'Li, Qiao Yun'
_publ_section_title
;
 Regulation of deprotonation of 3,3-di(1H-tetrazol-5-yl)pentanedioic acid:
 Solvothermal synthesis of La(III) and heterometallic La(III)/Cu(II)
 compounds for ablation of A549 cells
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              104
_journal_page_last               109
_journal_paper_doi               10.1016/j.jssc.2018.01.006
_journal_volume                  259
_journal_year                    2018
_chemical_formula_moiety         'C7 H13 La N8 O8, 4(H2 O)'
_chemical_formula_sum            'C7 H21 La N8 O12'
_chemical_formula_weight         548.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                97.443(2)
_cell_angle_beta                 91.4580(10)
_cell_angle_gamma                96.6640(10)
_cell_formula_units_Z            2
_cell_length_a                   7.9759(12)
_cell_length_b                   10.7082(12)
_cell_length_c                   11.600(2)
_cell_measurement_reflns_used    22714
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.56
_cell_volume                     974.9(2)
_computing_molecular_graphics    'SHELXL-2014 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker Apex Duo II'
_diffrn_measurement_method       'phi and omiga scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9281
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         1.772
_exptl_absorpt_coefficient_mu    2.265
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3489
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0156P)²+3.6097P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3442
_reflns_number_total             3489
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           t
_cod_database_code               1561205
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.636
_shelx_estimated_absorpt_t_max   0.660
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.02660(2) 0.34748(2) -0.12575(2) 0.01507(7) Uani 1 1 d . . . . .
O1 O 0.1463(3) 0.4765(2) 0.0793(2) 0.0251(5) Uani 1 1 d . . . . .
O2 O 0.2852(3) 0.3240(3) 0.0043(2) 0.0381(7) Uani 1 1 d . . . . .
O3 O 0.8203(3) 0.2789(2) 0.0233(2) 0.0274(5) Uani 1 1 d . . . . .
O4 O 0.7850(3) 0.4522(2) 0.1457(2) 0.0239(5) Uani 1 1 d . . . . .
O5 O 0.2549(4) 0.2806(3) -0.2644(2) 0.0377(6) Uani 1 1 d . . . . .
H5B H 0.3090 0.3342 -0.3028 0.057 Uiso 1 1 d R U . . .
H5C H 0.2995 0.2198 -0.2404 0.057 Uiso 1 1 d R U . . .
O6 O 0.0479(3) 0.1137(2) -0.1252(2) 0.0339(6) Uani 1 1 d . . . . .
H6A H -0.0147 0.0708 -0.1803 0.051 Uiso 1 1 d R U . . .
H6B H 0.1499 0.1000 -0.1347 0.051 Uiso 1 1 d R U . . .
O7 O -0.2245(4) 0.2177(3) -0.2449(3) 0.0467(8) Uani 1 1 d . . . . .
H7A H -0.2367 0.2477 -0.3086 0.070 Uiso 1 1 d R U . . .
H7B H -0.2074 0.1405 -0.2592 0.070 Uiso 1 1 d R U . . .
O8 O -0.0285(3) 0.4234(3) -0.3232(2) 0.0443(8) Uani 1 1 d . . . . .
H8A H 0.0575 0.4166 -0.3644 0.066 Uiso 1 1 d R U . . .
H8B H -0.0974 0.3983 -0.4012 0.066 Uiso 1 1 d R U . . .
C5 C 0.7426(4) 0.3398(3) 0.1018(3) 0.0182(6) Uani 1 1 d . . . . .
N1 N 0.6250(4) 0.5145(3) 0.3817(2) 0.0225(6) Uani 1 1 d . . . . .
N2 N 0.7192(4) 0.5121(3) 0.4791(2) 0.0265(6) Uani 1 1 d . . . . .
N3 N 0.7299(4) 0.3938(3) 0.4947(3) 0.0337(7) Uani 1 1 d . . . . .
N4 N 0.6439(4) 0.3168(3) 0.4078(3) 0.0315(7) Uani 1 1 d . . . . .
N5 N 0.2698(4) 0.1427(3) 0.2068(3) 0.0313(7) Uani 1 1 d . . . . .
H5A H 0.3096 0.1029 0.1463 0.038 Uiso 1 1 calc R U . . .
N6 N 0.1330(4) 0.1024(3) 0.2642(3) 0.0391(8) Uani 1 1 d . U . . .
N7 N 0.1087(5) 0.1861(3) 0.3513(3) 0.0434(9) Uani 1 1 d . . . . .
N8 N 0.2323(4) 0.2827(3) 0.3505(3) 0.0288(7) Uani 1 1 d . . . . .
C1 C 0.2710(4) 0.4136(3) 0.0817(3) 0.0180(6) Uani 1 1 d . U . . .
C2 C 0.4051(4) 0.4546(3) 0.1790(3) 0.0183(6) Uani 1 1 d . . . . .
H2A H 0.3566 0.5058 0.2418 0.022 Uiso 1 1 calc R U . . .
H2B H 0.4971 0.5078 0.1500 0.022 Uiso 1 1 calc R U . . .
C3 C 0.4785(4) 0.3435(3) 0.2289(3) 0.0146(6) Uani 1 1 d . . . . .
C4 C 0.5852(4) 0.2667(3) 0.1430(3) 0.0175(6) Uani 1 1 d . U . . .
H4A H 0.6195 0.1968 0.1798 0.021 Uiso 1 1 calc R U . . .
H4B H 0.5137 0.2305 0.0752 0.021 Uiso 1 1 calc R U . . .
C6 C 0.5828(4) 0.3936(3) 0.3399(3) 0.0174(6) Uani 1 1 d . . . . .
C7 C 0.3303(4) 0.2543(3) 0.2614(3) 0.0185(6) Uani 1 1 d . . . . .
O9 O 0.2811(3) -0.0050(2) 0.9835(2) 0.0339(6) Uani 1 1 d . . . . .
H9A H 0.1759 -0.0266 0.9890 0.051 Uiso 1 1 d R U . . .
H9B H 0.3336 -0.0695 0.9851 0.051 Uiso 1 1 d R U . . .
O10 O 0.4614(4) 0.1020(3) 0.7974(3) 0.0466(7) Uani 1 1 d . . . . .
H10A H 0.5614 0.1081 0.8264 0.070 Uiso 1 1 d R U . . .
H10B H 0.4188 0.0246 0.7882 0.070 Uiso 1 1 d R U . . .
O11 O 0.4019(9) 0.9467(4) 0.5869(4) 0.122(2) Uani 1 1 d . . . . .
H11A H 0.3625 1.0068 0.5581 0.183 Uiso 1 1 d R U . . .
H11B H 0.5022 0.9713 0.6136 0.183 Uiso 1 1 d R U . . .
O12 O 0.1010(10) 0.8997(6) 0.4592(5) 0.152(3) Uani 1 1 d . . . . .
H12A H 0.1019 0.9504 0.4084 0.229 Uiso 1 1 d R U . . .
H12B H -0.0003 0.8783 0.4764 0.229 Uiso 1 1 d R U . . .
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'
La La -0.2871 2.4523 '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'
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
O1 La1 O4 73.77(8) 2_565 2_665
O1 La1 O6 146.45(8) 2_565 .
O4 La1 O6 139.01(8) 2_665 .
O1 La1 O3 73.59(8) 2_565 1_455
O4 La1 O3 134.81(7) 2_665 1_455
O6 La1 O3 75.01(8) . 1_455
O1 La1 O8 75.83(9) 2_565 .
O4 La1 O8 68.88(8) 2_665 .
O6 La1 O8 117.47(10) . .
O3 La1 O8 130.01(9) 1_455 .
O1 La1 O7 89.76(10) 2_565 .
O4 La1 O7 134.91(9) 2_665 .
O6 La1 O7 70.78(10) . .
O3 La1 O7 74.84(9) 1_455 .
O8 La1 O7 66.43(9) . .
O1 La1 O5 140.31(8) 2_565 .
O4 La1 O5 74.29(8) 2_665 .
O6 La1 O5 70.89(9) . .
O3 La1 O5 145.77(8) 1_455 .
O8 La1 O5 71.08(10) . .
O7 La1 O5 96.45(10) . .
O1 La1 O2 121.37(8) 2_565 .
O4 La1 O2 78.71(9) 2_665 .
O6 La1 O2 71.44(9) . .
O3 La1 O2 92.63(9) 1_455 .
O8 La1 O2 137.23(9) . .
O7 La1 O2 142.10(10) . .
O5 La1 O2 73.87(9) . .
O1 La1 O1 72.69(8) 2_565 .
O4 La1 O1 66.73(7) 2_665 .
O6 La1 O1 109.57(8) . .
O3 La1 O1 74.26(8) 1_455 .
O8 La1 O1 130.91(9) . .
O7 La1 O1 147.70(9) . .
O5 La1 O1 114.49(8) . .
O2 La1 O1 48.90(7) . .
O1 La1 C1 97.30(8) 2_565 .
O4 La1 C1 70.29(8) 2_665 .
O6 La1 C1 90.79(8) . .
O3 La1 C1 83.85(8) 1_455 .
O8 La1 C1 138.89(9) . .
O7 La1 C1 154.67(9) . .
O5 La1 C1 93.53(9) . .
O2 La1 C1 24.11(8) . .
O1 La1 C1 24.81(8) . .
O1 La1 La1 38.06(5) 2_565 2_565
O4 La1 La1 65.08(5) 2_665 2_565
O6 La1 La1 135.42(6) . 2_565
O3 La1 La1 69.92(5) 1_455 2_565
O8 La1 La1 106.09(8) . 2_565
O7 La1 La1 122.90(8) . 2_565
O5 La1 La1 136.53(7) . 2_565
O2 La1 La1 83.42(6) . 2_565
O1 La1 La1 34.63(5) . 2_565
C1 La1 La1 59.31(6) . 2_565
C1 O1 La1 159.0(2) . 2_565
C1 O1 La1 92.38(18) . .
La1 O1 La1 107.31(8) 2_565 .
C1 O2 La1 98.0(2) . .
C5 O3 La1 133.1(2) . 1_655
C5 O4 La1 144.5(2) . 2_665
La1 O5 H5B 120.7 . .
La1 O5 H5C 109.5 . .
H5B O5 H5C 122.7 . .
La1 O6 H6A 109.6 . .
La1 O6 H6B 109.2 . .
H6A O6 H6B 109.5 . .
La1 O7 H7A 109.1 . .
La1 O7 H7B 110.2 . .
H7A O7 H7B 109.5 . .
La1 O8 H8A 109.5 . .
La1 O8 H8B 142.4 . .
H8A O8 H8B 85.0 . .
O3 C5 O4 125.3(3) . .
O3 C5 C4 115.5(3) . .
O4 C5 C4 119.2(3) . .
C6 N1 N2 104.6(3) . .
N3 N2 N1 109.6(3) . .
N2 N3 N4 109.0(3) . .
C6 N4 N3 105.2(3) . .
C7 N5 N6 106.5(3) . .
C7 N5 H5A 126.7 . .
N6 N5 H5A 126.7 . .
N7 N6 N5 110.5(3) . .
N6 N7 N8 106.3(3) . .
C7 N8 N7 108.5(3) . .
O2 C1 O1 120.6(3) . .
O2 C1 C2 121.5(3) . .
O1 C1 C2 117.9(3) . .
O2 C1 La1 57.93(17) . .
O1 C1 La1 62.81(16) . .
C2 C1 La1 174.4(2) . .
C1 C2 C3 114.6(2) . .
C1 C2 H2A 108.6 . .
C3 C2 H2A 108.6 . .
C1 C2 H2B 108.6 . .
C3 C2 H2B 108.6 . .
H2A C2 H2B 107.6 . .
C6 C3 C4 109.7(2) . .
C6 C3 C7 107.2(2) . .
C4 C3 C7 108.3(2) . .
C6 C3 C2 109.8(2) . .
C4 C3 C2 114.2(2) . .
C7 C3 C2 107.4(2) . .
C5 C4 C3 116.1(2) . .
C5 C4 H4A 108.2 . .
C3 C4 H4A 108.2 . .
C5 C4 H4B 108.2 . .
C3 C4 H4B 108.2 . .
H4A C4 H4B 107.4 . .
N1 C6 N4 111.7(3) . .
N1 C6 C3 126.1(3) . .
N4 C6 C3 122.2(3) . .
N5 C7 N8 108.2(3) . .
N5 C7 C3 127.8(3) . .
N8 C7 C3 123.8(3) . .
H9A O9 H9B 109.5 . .
H10A O10 H10B 109.5 . .
H11A O11 H11B 109.5 . .
H12A O12 H12B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O1 2.474(2) 2_565
La1 O4 2.512(2) 2_665
La1 O6 2.530(2) .
La1 O3 2.535(2) 1_455
La1 O8 2.571(3) .
La1 O7 2.563(3) .
La1 O5 2.563(3) .
La1 O2 2.580(2) .
La1 O1 2.684(2) .
La1 C1 3.015(3) .
La1 La1 4.1565(5) 2_565
O1 C1 1.266(4) .
O1 La1 2.474(2) 2_565
O2 C1 1.244(4) .
O3 C5 1.268(4) .
O3 La1 2.535(2) 1_655
O4 C5 1.250(4) .
O4 La1 2.512(2) 2_665
O5 H5B 0.8561 .
O5 H5C 0.8509 .
O6 H6A 0.8498 .
O6 H6B 0.8500 .
O7 H7A 0.8500 .
O7 H7B 0.8500 .
O8 H8A 0.8500 .
O8 H8B 1.0353 .
C5 C4 1.521(4) .
N1 C6 1.324(4) .
N1 N2 1.345(4) .
N2 N3 1.314(4) .
N3 N4 1.336(4) .
N4 C6 1.332(4) .
N5 C7 1.310(4) .
N5 N6 1.350(4) .
N5 H5A 0.8600 .
N6 N7 1.295(5) .
N7 N8 1.345(4) .
N8 C7 1.337(4) .
C1 C2 1.521(4) .
C2 C3 1.554(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C6 1.516(4) .
C3 C4 1.545(4) .
C3 C7 1.518(4) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
O9 H9A 0.8499 .
O9 H9B 0.8500 .
O10 H10A 0.8500 .
O10 H10B 0.8501 .
O11 H11A 0.8499 .
O11 H11B 0.8501 .
O12 H12A 0.8500 .
O12 H12B 0.8501 .
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
La1 O3 C5 O4 -21.0(5) 1_655 . . .
La1 O3 C5 C4 158.7(2) 1_655 . . .
La1 O4 C5 O3 12.5(6) 2_665 . . .
La1 O4 C5 C4 -167.2(2) 2_665 . . .
C6 N1 N2 N3 -0.9(4) . . . .
N1 N2 N3 N4 0.4(4) . . . .
N2 N3 N4 C6 0.3(4) . . . .
C7 N5 N6 N7 0.2(5) . . . .
N5 N6 N7 N8 0.0(5) . . . .
N6 N7 N8 C7 -0.1(5) . . . .
La1 O2 C1 O1 4.0(3) . . . .
La1 O2 C1 C2 -173.5(2) . . . .
La1 O1 C1 O2 -163.6(4) 2_565 . . .
La1 O1 C1 O2 -3.9(3) . . . .
La1 O1 C1 C2 14.0(8) 2_565 . . .
La1 O1 C1 C2 173.8(2) . . . .
La1 O1 C1 La1 -159.8(6) 2_565 . . .
O2 C1 C2 C3 -40.8(4) . . . .
O1 C1 C2 C3 141.6(3) . . . .
C1 C2 C3 C6 -168.6(3) . . . .
C1 C2 C3 C4 67.8(3) . . . .
C1 C2 C3 C7 -52.3(3) . . . .
O3 C5 C4 C3 -173.7(3) . . . .
O4 C5 C4 C3 6.1(4) . . . .
C6 C3 C4 C5 -62.2(3) . . . .
C7 C3 C4 C5 -178.9(3) . . . .
C2 C3 C4 C5 61.5(3) . . . .
N2 N1 C6 N4 1.1(4) . . . .
N2 N1 C6 C3 -178.8(3) . . . .
N3 N4 C6 N1 -0.9(4) . . . .
N3 N4 C6 C3 179.0(3) . . . .
C4 C3 C6 N1 118.2(3) . . . .
C7 C3 C6 N1 -124.4(3) . . . .
C2 C3 C6 N1 -8.1(4) . . . .
C4 C3 C6 N4 -61.7(4) . . . .
C7 C3 C6 N4 55.6(4) . . . .
C2 C3 C6 N4 172.0(3) . . . .
N6 N5 C7 N8 -0.3(4) . . . .
N6 N5 C7 C3 -176.7(3) . . . .
N7 N8 C7 N5 0.3(4) . . . .
N7 N8 C7 C3 176.9(3) . . . .
C6 C3 C7 N5 -136.1(4) . . . .
C4 C3 C7 N5 -17.8(5) . . . .
C2 C3 C7 N5 106.0(4) . . . .
C6 C3 C7 N8 48.0(4) . . . .
C4 C3 C7 N8 166.3(3) . . . .
C2 C3 C7 N8 -70.0(4) . . . .
