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#$Date: 2021-04-29 11:20:54 +0300 (Thu, 29 Apr 2021) $
#$Revision: 264686 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/22/1562246.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_1562246
loop_
_publ_author_name
'Chen, Mao-Long'
'Shi, Yan-Ru'
'Yang, Yu-Chen'
'Zhou, Zhao-Hui'
_publ_section_title
;
 Acidic 1,3-propanediaminetetraacetato lanthanides with luminescent and
 catalytic ester hydrolysis properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              265
_journal_page_last               273
_journal_paper_doi               10.1016/j.jssc.2014.07.037
_journal_volume                  219
_journal_year                    2014
_chemical_formula_moiety         'C11 H27 Ce N2 O13, 2(Cl), 2(H2 O), O'
_chemical_formula_sum            'C11 H33 Ce Cl2 N2 O16'
_chemical_formula_weight         660.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.242(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0761(4)
_cell_length_b                   23.4129(11)
_cell_length_c                   10.0886(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2379.45(17)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21049
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  0.9167
_exptl_absorpt_correction_T_min  0.6659
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0379
_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)+(0.0399P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                3345
_reflns_number_total             4654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-219-265.cif
_cod_data_source_block           2
_cod_database_code               1562246
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.34560(3) 0.205504(12) 0.56089(3) 0.01139(9) Uani 1 1 d . . .
Cl1 Cl 0.29070(12) 0.36941(6) 0.27496(13) 0.0217(3) Uani 1 1 d . . .
Cl2 Cl 0.31896(15) 0.04437(6) 0.22638(15) 0.0298(3) Uani 1 1 d . . .
C1 C 0.3599(5) 0.3420(2) 0.9264(5) 0.0147(11) Uani 1 1 d . . .
H1A H 0.2753 0.3573 0.9599 0.018 Uiso 1 1 calc R . .
H1B H 0.4201 0.3358 1.0039 0.018 Uiso 1 1 calc R . .
C2 C 0.3326(4) 0.2850(2) 0.8607(5) 0.0117(10) Uani 1 1 d U . .
C3 C 0.4937(5) 0.4294(2) 0.9206(5) 0.0176(12) Uani 1 1 d . . .
H3A H 0.4330 0.4449 0.9875 0.021 Uiso 1 1 calc R . .
H3B H 0.5185 0.4614 0.8617 0.021 Uiso 1 1 calc R . .
C4 C 0.6180(5) 0.4081(2) 0.9915(5) 0.0176(12) Uani 1 1 d . . .
C5 C -0.0233(5) 0.3424(2) 0.5402(5) 0.0151(11) Uani 1 1 d . . .
H5A H -0.1001 0.3351 0.4797 0.018 Uiso 1 1 calc R . .
H5B H -0.0581 0.3578 0.6240 0.018 Uiso 1 1 calc R . .
C6 C 0.0467(5) 0.2857(2) 0.5696(5) 0.0132(11) Uani 1 1 d . . .
C7 C -0.0148(5) 0.4305(2) 0.4066(5) 0.0136(11) Uani 1 1 d . . .
H7A H 0.0453 0.4623 0.3835 0.016 Uiso 1 1 calc R . .
H7B H -0.0820 0.4460 0.4670 0.016 Uiso 1 1 calc R . .
C8 C -0.0857(5) 0.4101(2) 0.2797(5) 0.0161(12) Uani 1 1 d . . .
C9 C 0.3196(5) 0.4179(2) 0.7563(5) 0.0174(12) Uani 1 1 d . . .
H9A H 0.3669 0.4458 0.7006 0.021 Uiso 1 1 calc R . .
H9B H 0.2614 0.4397 0.8157 0.021 Uiso 1 1 calc R . .
C10 C 0.2336(5) 0.3801(2) 0.6668(5) 0.0144(11) Uani 1 1 d . . .
H10A H 0.2903 0.3557 0.6112 0.017 Uiso 1 1 calc R . .
H10B H 0.1772 0.3550 0.7211 0.017 Uiso 1 1 calc R . .
C11 C 0.1478(5) 0.4183(2) 0.5802(5) 0.0158(12) Uani 1 1 d . . .
H11A H 0.0888 0.4408 0.6374 0.019 Uiso 1 1 calc R . .
H11B H 0.2057 0.4454 0.5333 0.019 Uiso 1 1 calc R . .
N1 N 0.4200(4) 0.38575(19) 0.8395(4) 0.0133(10) Uani 1 1 d . . .
H1 H 0.474(5) 0.368(2) 0.787(5) 0.016 Uiso 1 1 d . . .
N2 N 0.0637(4) 0.38654(19) 0.4791(4) 0.0128(9) Uani 1 1 d . . .
H2 H 0.120(5) 0.370(2) 0.427(5) 0.015 Uiso 1 1 d . . .
O2 O 0.2616(3) 0.25132(15) 0.9236(4) 0.0187(8) Uani 1 1 d . . .
O1 O 0.3843(3) 0.27497(15) 0.7503(3) 0.0151(8) Uani 1 1 d . . .
O4 O 0.6674(4) 0.44706(16) 1.0637(4) 0.0301(10) Uani 1 1 d . . .
H4 H 0.7291 0.4334 1.1114 0.045 Uiso 1 1 calc R . .
O3 O 0.6595(3) 0.35939(15) 0.9734(3) 0.0163(8) Uani 1 1 d . . .
O6 O -0.0131(3) 0.25314(15) 0.6462(4) 0.0182(8) Uani 1 1 d . . .
O5 O 0.1541(3) 0.27507(15) 0.5147(3) 0.0153(8) Uani 1 1 d . . .
O8 O -0.1556(4) 0.44879(18) 0.2286(4) 0.0375(12) Uani 1 1 d . . .
O7 O -0.0681(3) 0.36139(16) 0.2385(4) 0.0179(8) Uani 1 1 d . . .
O2W O 0.1751(3) 0.18057(16) 0.7332(4) 0.0187(8) Uani 1 1 d D . .
O1W O 0.4528(4) 0.12558(17) 0.4360(4) 0.0261(10) Uani 1 1 d D . .
H1WA H 0.500(5) 0.1038(17) 0.485(5) 0.031 Uiso 1 1 d D . .
H1WB H 0.405(5) 0.1051(17) 0.385(5) 0.031 Uiso 1 1 d D . .
H2WA H 0.105(3) 0.196(2) 0.702(5) 0.031 Uiso 1 1 d D . .
H2WB H 0.203(5) 0.198(2) 0.802(3) 0.031 Uiso 1 1 d D . .
O3W O 0.5935(3) 0.21041(16) 0.6053(4) 0.0213(8) Uani 1 1 d . . .
H3WA H 0.6207 0.1789 0.6443 0.032 Uiso 1 1 d R . .
H3WB H 0.6349 0.2145 0.5301 0.032 Uiso 1 1 d R . .
O4W O 0.4555(4) 0.2930(2) 0.4722(4) 0.0206(9) Uani 1 1 d . . .
H4WA H 0.435(7) 0.304(3) 0.424(7) 0.025 Uiso 1 1 d . . .
H4WB H 0.509(6) 0.303(3) 0.518(6) 0.025 Uiso 1 1 d . . .
O5W O 0.2931(4) 0.21884(17) 0.3082(4) 0.0198(10) Uani 1 1 d . . .
H5WA H 0.367(5) 0.227(2) 0.234(6) 0.024 Uiso 1 1 d D . .
H5WB H 0.249(5) 0.237(3) 0.299(7) 0.024 Uiso 1 1 d D . .
O6W O 0.6114(4) 0.3544(2) 0.6538(5) 0.0360(11) Uani 1 1 d . . .
H6WA H 0.596(6) 0.387(3) 0.609(6) 0.043 Uiso 1 1 d D . .
H6WB H 0.695(6) 0.369(3) 0.698(6) 0.043 Uiso 1 1 d D . .
O7W O 0.6486(4) 0.0574(2) 0.5538(5) 0.0391(11) Uani 1 1 d D . .
H7WA H 0.596(4) 0.033(2) 0.516(6) 0.047 Uiso 1 1 d D . .
H7WB H 0.724(3) 0.054(3) 0.518(6) 0.047 Uiso 1 1 d D . .
O8W O 0.6424(12) 0.4122(5) 0.4158(11) 0.066(3) Uani 0.50 1 d P . .
O8W' O 0.4588(9) 0.4930(4) 0.3742(13) 0.074(4) Uani 0.50 1 d PU . .
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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 Ce1 O3 137.92(11) . 4_565
O1 Ce1 O5 80.32(11) . .
O1 Ce1 O2W 74.14(11) . .
O1 Ce1 O5W 133.18(12) . .
O3 Ce1 O5 76.76(11) 4_565 .
O3 Ce1 O5W 66.57(12) 4_565 .
O5 Ce1 O5W 67.07(12) . .
O7 Ce1 O1 79.49(11) 4_666 .
O7 Ce1 O3 96.63(11) 4_666 4_565
O7 Ce1 O5 140.52(11) 4_666 .
O7 Ce1 O2W 66.34(12) 4_666 .
O7 Ce1 O3W 65.06(12) 4_666 .
O7 Ce1 O5W 145.88(12) 4_666 .
O2W Ce1 O3 66.26(11) . 4_565
O2W Ce1 O5 75.65(12) . .
O2W Ce1 O5W 124.77(11) . .
O1W Ce1 O1 142.70(11) . .
O1W Ce1 O3 72.80(12) . 4_565
O1W Ce1 O5 135.49(12) . .
O1W Ce1 O7 75.41(12) . 4_666
O1W Ce1 O2W 118.48(13) . .
O1W Ce1 O3W 71.88(12) . .
O1W Ce1 O5W 71.32(13) . .
O3W Ce1 O1 72.67(11) . .
O3W Ce1 O3 143.32(12) . 4_565
O3W Ce1 O5 137.77(12) . .
O3W Ce1 O2W 124.72(12) . .
O3W Ce1 O5W 110.21(12) . .
O4W Ce1 O1 71.47(13) . .
O4W Ce1 O3 133.63(12) . 4_565
O4W Ce1 O5 75.65(12) . .
O4W Ce1 O7 127.87(12) . 4_666
O4W Ce1 O2W 138.10(14) . .
O4W Ce1 O1W 103.39(14) . .
O4W Ce1 O3W 65.37(12) . .
O4W Ce1 O5W 68.59(13) . .
N1 C1 C2 115.0(4) . .
O2 C2 C1 115.8(4) . .
O2 C2 O1 125.7(5) . .
O1 C2 C1 118.4(4) . .
N1 C3 C4 115.4(4) . .
O4 C4 C3 110.2(5) . .
O3 C4 C3 121.1(5) . .
O3 C4 O4 128.6(5) . .
N2 C5 C6 114.1(4) . .
O6 C6 C5 115.0(4) . .
O6 C6 O5 125.9(5) . .
O5 C6 C5 119.0(4) . .
N2 C7 C8 115.6(4) . .
O8 C8 C7 111.6(5) . .
O7 C8 C7 120.3(5) . .
O7 C8 O8 128.1(5) . .
N1 C9 C10 114.0(4) . .
C11 C10 C9 108.0(4) . .
N2 C11 C10 113.9(4) . .
C1 N1 C3 110.6(4) . .
C1 N1 C9 113.4(4) . .
C3 N1 C9 106.4(4) . .
C5 N2 C11 112.8(4) . .
C7 N2 C5 111.8(4) . .
C7 N2 C11 106.1(4) . .
C2 O1 Ce1 136.5(3) . .
C4 O3 Ce1 138.6(3) . 4_666
C6 O5 Ce1 134.5(3) . .
C8 O7 Ce1 140.1(3) . 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 O1 2.533(3) .
Ce1 O3 2.555(3) 4_565
Ce1 O5 2.560(3) .
Ce1 O7 2.520(3) 4_666
Ce1 O2W 2.538(4) .
Ce1 O1W 2.513(4) .
Ce1 O3W 2.531(3) .
Ce1 O4W 2.503(4) .
Ce1 O5W 2.611(4) .
C1 C2 1.513(7) .
C1 N1 1.486(6) .
C2 O2 1.248(6) .
C2 O1 1.262(6) .
C3 C4 1.514(7) .
C3 N1 1.497(6) .
C4 O4 1.264(6) .
C4 O3 1.229(6) .
C5 C6 1.530(7) .
C5 N2 1.497(6) .
C6 O6 1.249(6) .
C6 O5 1.251(6) .
C7 C8 1.529(7) .
C7 N2 1.481(6) .
C8 O8 1.252(6) .
C8 O7 1.228(6) .
C9 C10 1.523(7) .
C9 N1 1.502(6) .
C10 C11 1.510(7) .
C11 N2 1.508(6) .
O3 Ce1 2.555(3) 4_666
O7 Ce1 2.520(3) 4_565
