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#$Date: 2024-09-06 03:17:00 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294520 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/89/7248958.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_7248958
loop_
_publ_author_name
'Prętka, Dominika'
'Marcinkowski, Dawid'
'Siwiak, Agnieszka'
'Kubicki, Maciej'
'Consiglio, Giuseppe'
'Patroniak, Violetta'
'Gorczyński, Adam'
_publ_section_title
;
 Crystal engineering of monometallic lanthanide(iii) supramolecular
 systems within the N3-tridentate hydrazone Schiff-base ligand
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4167
_journal_page_last               4180
_journal_paper_doi               10.1039/D4CE00450G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C12 H17 La N8 O10, C2 H3 N'
_chemical_formula_sum            'C14 H20 La N9 O10'
_chemical_formula_weight         613.30
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-06 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                109.919(6)
_cell_angle_beta                 106.972(4)
_cell_angle_gamma                93.483(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2733(4)
_cell_length_b                   11.4426(7)
_cell_length_c                   13.5163(7)
_cell_measurement_reflns_used    2932
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      26.4710
_cell_measurement_theta_min      4.0660
_cell_volume                     1132.21(12)
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_collection       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      130(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.795
_diffrn_measured_fraction_theta_max 0.721
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.795
_diffrn_reflns_Laue_measured_fraction_max 0.721
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5084
_diffrn_reflns_point_group_measured_fraction_full 0.795
_diffrn_reflns_point_group_measured_fraction_max 0.721
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.531
_diffrn_reflns_theta_min         3.218
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.34a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.662
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0512P)²+0.2846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3317
_reflns_number_total             3393
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00450g2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7248946--7248974.cif.'
_cod_database_code               7248958
_shelx_shelxl_version_number     2014/7
_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.
;
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 0.31327(2) 0.34366(2) 0.74634(2) 0.01169(8) Uani 1 1 d . . . . .
N1A N 0.0290(3) 0.4345(2) 0.6824(2) 0.0144(5) Uani 1 1 d . . . . .
C2A C -0.0334(4) 0.5031(3) 0.7610(3) 0.0184(7) Uani 1 1 d . . . . .
H2A H 0.0318 0.5230 0.8371 0.022 Uiso 1 1 calc R U . . .
C3A C -0.1854(4) 0.5459(3) 0.7374(3) 0.0206(7) Uani 1 1 d . . . . .
H3A H -0.2261 0.5926 0.7953 0.025 Uiso 1 1 calc R U . . .
C4A C -0.2787(4) 0.5189(3) 0.6256(3) 0.0204(7) Uani 1 1 d . . . . .
H4A H -0.3833 0.5491 0.6065 0.024 Uiso 1 1 calc R U . . .
C5A C -0.2198(4) 0.4491(3) 0.5438(3) 0.0180(7) Uani 1 1 d . . . . .
H5A H -0.2821 0.4311 0.4676 0.022 Uiso 1 1 calc R U . . .
C6A C -0.0659(4) 0.4043(3) 0.5739(2) 0.0134(6) Uani 1 1 d . . . . .
N7A N -0.0035(3) 0.3293(3) 0.4943(2) 0.0161(6) Uani 1 1 d . . . . .
C71A C -0.1042(4) 0.2759(3) 0.3755(2) 0.0186(7) Uani 1 1 d . . . . .
H71C H -0.0581 0.3205 0.3365 0.028 Uiso 1 1 calc R U . . .
H71B H -0.2242 0.2854 0.3657 0.028 Uiso 1 1 calc R U . . .
H71A H -0.0978 0.1861 0.3447 0.028 Uiso 1 1 calc R U . . .
N8A N 0.1564(3) 0.3022(2) 0.5300(2) 0.0138(5) Uani 1 1 d . . . . .
C9A C 0.2272(4) 0.2431(3) 0.4588(2) 0.0143(6) Uani 1 1 d . . . . .
H9A H 0.1711 0.2184 0.3808 0.017 Uiso 1 1 calc R U . . .
C10A C 0.3956(4) 0.2161(3) 0.5029(3) 0.0150(6) Uani 1 1 d . . . . .
N11A N 0.4816(3) 0.1444(2) 0.4404(2) 0.0167(6) Uani 1 1 d . . . . .
C11A C 0.4229(4) 0.0811(3) 0.3195(3) 0.0256(8) Uani 1 1 d . . . . .
H11 H 0.3065 0.0331 0.2937 0.038 Uiso 1 1 calc R U . . .
H11B H 0.5005 0.0235 0.2980 0.038 Uiso 1 1 calc R U . . .
H11A H 0.4223 0.1442 0.2854 0.038 Uiso 1 1 calc R U . . .
C12A C 0.6337(4) 0.1384(3) 0.5128(3) 0.0185(7) Uani 1 1 d . . . . .
H12A H 0.7213 0.0950 0.4938 0.022 Uiso 1 1 calc R U . . .
C13A C 0.6338(4) 0.2068(3) 0.6168(3) 0.0180(7) Uani 1 1 d . . . . .
H13A H 0.7238 0.2191 0.6839 0.022 Uiso 1 1 calc R U . . .
N14A N 0.4858(3) 0.2556(2) 0.6113(2) 0.0157(5) Uani 1 1 d . . . . .
N1B N 0.0814(3) 0.0873(3) 0.6492(2) 0.0219(6) Uani 1 1 d . . . . .
O11B O 0.2420(3) 0.0967(2) 0.6683(2) 0.0293(6) Uani 1 1 d . . . . .
O12B O 0.0264(3) 0.1896(2) 0.6803(2) 0.0227(5) Uani 1 1 d . . . . .
O13B O -0.0147(3) -0.0145(2) 0.6036(3) 0.0445(8) Uani 1 1 d . . . . .
N1C N 0.4075(3) 0.6269(3) 0.8073(2) 0.0182(6) Uani 1 1 d . . . . .
O11C O 0.4055(3) 0.5459(2) 0.71550(18) 0.0189(5) Uani 1 1 d . . . . .
O12C O 0.3645(3) 0.5866(2) 0.87452(18) 0.0205(5) Uani 1 1 d . . . . .
O13C O 0.4488(3) 0.7407(2) 0.8310(2) 0.0316(6) Uani 1 1 d . . . . .
N1D N 0.6682(3) 0.3344(3) 0.8960(2) 0.0204(6) Uani 1 1 d . . . . .
O11D O 0.5565(3) 0.2361(2) 0.84269(19) 0.0245(5) Uani 1 1 d . . . . .
O12D O 0.6213(3) 0.4381(2) 0.89050(18) 0.0209(5) Uani 1 1 d . . . . .
O13D O 0.8149(3) 0.3345(3) 0.9499(2) 0.0353(7) Uani 1 1 d . . . . .
O1E O 0.2443(3) 0.3549(3) 0.9175(2) 0.0227(6) Uani 1 1 d . . . . .
H1E H 0.285(5) 0.408(4) 0.967(3) 0.016(10) Uiso 1 1 d . . . . .
C1E C 0.1959(5) 0.2506(4) 0.9453(3) 0.0312(9) Uani 1 1 d . . . . .
H1E3 H 0.1248 0.1805 0.8771 0.047 Uiso 1 1 calc R U . . .
H1E2 H 0.1305 0.2769 0.9966 0.047 Uiso 1 1 calc R U . . .
H1E1 H 0.2993 0.2231 0.9811 0.047 Uiso 1 1 calc R U . . .
N1F N 0.0205(5) 0.1103(5) 0.1551(3) 0.0634(13) Uani 1 1 d . . . . .
C2F C -0.1035(5) 0.0899(4) 0.0851(3) 0.0374(9) Uani 1 1 d . . . . .
C3F C -0.2650(6) 0.0627(4) -0.0052(4) 0.0453(11) Uani 1 1 d . . . . .
H3F3 H -0.3068 -0.0287 -0.0395 0.068 Uiso 1 1 calc R U . . .
H3F2 H -0.2472 0.0933 -0.0614 0.068 Uiso 1 1 calc R U . . .
H3F1 H -0.3497 0.1052 0.0244 0.068 Uiso 1 1 calc 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'
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'
La La -0.2871 2.4523 '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
_geom_angle_publ_flag
O1E La1 O12B 72.93(8) . . ?
O1E La1 O11C 121.73(8) . . ?
O12B La1 O11C 134.78(6) . . ?
O1E La1 O12D 82.29(8) . . ?
O12B La1 O12D 148.35(6) . . ?
O11C La1 O12D 75.28(6) . . ?
O1E La1 N14A 148.95(8) . . ?
O12B La1 N14A 109.59(8) . . ?
O11C La1 N14A 79.47(7) . . ?
O12D La1 N14A 82.05(7) . . ?
O1E La1 O11B 90.57(9) . . ?
O12B La1 O11B 48.74(7) . . ?
O11C La1 O11B 147.68(8) . . ?
O12D La1 O11B 113.81(7) . . ?
N14A La1 O11B 71.69(8) . . ?
O1E La1 O12C 72.95(8) . . ?
O12B La1 O12C 123.58(7) . . ?
O11C La1 O12C 48.82(7) . . ?
O12D La1 O12C 64.42(7) . . ?
N14A La1 O12C 122.67(7) . . ?
O11B La1 O12C 163.51(8) . . ?
O1E La1 N1A 88.34(8) . . ?
O12B La1 N1A 64.18(7) . . ?
O11C La1 N1A 73.27(7) . . ?
O12D La1 N1A 135.57(8) . . ?
N14A La1 N1A 121.23(7) . . ?
O11B La1 N1A 109.60(8) . . ?
O12C La1 N1A 71.29(7) . . ?
O1E La1 O11D 77.74(8) . . ?
O12B La1 O11D 105.90(7) . . ?
O11C La1 O11D 118.71(7) . . ?
O12D La1 O11D 48.40(7) . . ?
N14A La1 O11D 71.81(7) . . ?
O11B La1 O11D 65.71(7) . . ?
O12C La1 O11D 108.99(7) . . ?
N1A La1 O11D 165.06(8) . . ?
O1E La1 N8A 140.59(8) . . ?
O12B La1 N8A 72.87(7) . . ?
O11C La1 N8A 72.77(7) . . ?
O12D La1 N8A 136.18(7) . . ?
N14A La1 N8A 63.33(7) . . ?
O11B La1 N8A 81.31(8) . . ?
O12C La1 N8A 111.66(7) . . ?
N1A La1 N8A 59.21(8) . . ?
O11D La1 N8A 130.72(8) . . ?
O1E La1 N1B 82.15(8) . . ?
O12B La1 N1B 24.31(7) . . ?
O11C La1 N1B 147.08(7) . . ?
O12D La1 N1B 134.41(6) . . ?
N14A La1 N1B 89.98(8) . . ?
O11B La1 N1B 24.48(7) . . ?
O12C La1 N1B 146.58(8) . . ?
N1A La1 N1B 86.34(7) . . ?
O11D La1 N1B 86.42(7) . . ?
N8A La1 N1B 74.63(7) . . ?
O1E La1 N1C 97.50(8) . . ?
O12B La1 N1C 134.06(7) . . ?
O11C La1 N1C 24.26(7) . . ?
O12D La1 N1C 67.56(6) . . ?
N14A La1 N1C 101.01(8) . . ?
O11B La1 N1C 171.93(8) . . ?
O12C La1 N1C 24.56(7) . . ?
N1A La1 N1C 70.85(7) . . ?
O11D La1 N1C 115.93(7) . . ?
N8A La1 N1C 92.39(7) . . ?
N1B La1 N1C 157.17(7) . . ?
C2A N1A C6A 118.0(3) . . ?
C2A N1A La1 118.53(17) . . ?
C6A N1A La1 123.1(2) . . ?
N1A C2A C3A 123.6(3) . . ?
N1A C2A H2A 118.2 . . ?
C3A C2A H2A 118.2 . . ?
C2A C3A C4A 117.9(3) . . ?
C2A C3A H3A 121.0 . . ?
C4A C3A H3A 121.0 . . ?
C5A C4A C3A 120.0(3) . . ?
C5A C4A H4A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C4A C5A C6A 119.0(3) . . ?
C4A C5A H5A 120.5 . . ?
C6A C5A H5A 120.5 . . ?
N1A C6A N7A 117.3(3) . . ?
N1A C6A C5A 121.2(3) . . ?
N7A C6A C5A 121.5(3) . . ?
N8A N7A C6A 117.8(2) . . ?
N8A N7A C71A 119.7(3) . . ?
C6A N7A C71A 122.5(2) . . ?
N7A C71A H71C 109.5 . . ?
N7A C71A H71B 109.5 . . ?
H71C C71A H71B 109.5 . . ?
N7A C71A H71A 109.5 . . ?
H71C C71A H71A 109.5 . . ?
H71B C71A H71A 109.5 . . ?
C9A N8A N7A 120.2(2) . . ?
C9A N8A La1 118.35(17) . . ?
N7A N8A La1 121.00(18) . . ?
N8A C9A C10A 117.0(3) . . ?
N8A C9A H9A 121.5 . . ?
C10A C9A H9A 121.5 . . ?
N14A C10A N11A 110.7(3) . . ?
N14A C10A C9A 124.3(3) . . ?
N11A C10A C9A 124.9(3) . . ?
C10A N11A C12A 107.2(3) . . ?
C10A N11A C11A 127.1(3) . . ?
C12A N11A C11A 125.7(3) . . ?
N11A C11A H11 109.5 . . ?
N11A C11A H11B 109.5 . . ?
H11 C11A H11B 109.5 . . ?
N11A C11A H11A 109.5 . . ?
H11 C11A H11A 109.5 . . ?
H11B C11A H11A 109.5 . . ?
C13A C12A N11A 106.2(3) . . ?
C13A C12A H12A 126.9 . . ?
N11A C12A H12A 126.9 . . ?
C12A C13A N14A 110.3(3) . . ?
C12A C13A H13A 124.8 . . ?
N14A C13A H13A 124.8 . . ?
C10A N14A C13A 105.5(3) . . ?
C10A N14A La1 115.27(19) . . ?
C13A N14A La1 136.59(19) . . ?
O13B N1B O12B 121.7(3) . . ?
O13B N1B O11B 122.0(3) . . ?
O12B N1B O11B 116.3(2) . . ?
O13B N1B La1 175.7(2) . . ?
O12B N1B La1 57.68(13) . . ?
O11B N1B La1 58.79(15) . . ?
N1B O11B La1 96.73(18) . . ?
N1B O12B La1 98.01(16) . . ?
O13C N1C O11C 121.5(3) . . ?
O13C N1C O12C 120.9(3) . . ?
O11C N1C O12C 117.6(2) . . ?
O13C N1C La1 178.5(3) . . ?
O11C N1C La1 57.44(13) . . ?
O12C N1C La1 60.23(15) . . ?
N1C O11C La1 98.30(15) . . ?
N1C O12C La1 95.21(19) . . ?
O13D N1D O11D 123.1(3) . . ?
O13D N1D O12D 120.4(3) . . ?
O11D N1D O12D 116.5(2) . . ?
N1D O11D La1 96.44(16) . . ?
N1D O12D La1 98.43(16) . . ?
C1E O1E La1 127.0(2) . . ?
C1E O1E H1E 109(3) . . ?
La1 O1E H1E 118(3) . . ?
O1E C1E H1E3 109.5 . . ?
O1E C1E H1E2 109.5 . . ?
H1E3 C1E H1E2 109.5 . . ?
O1E C1E H1E1 109.5 . . ?
H1E3 C1E H1E1 109.5 . . ?
H1E2 C1E H1E1 109.5 . . ?
N1F C2F C3F 179.4(5) . . ?
C2F C3F H3F3 109.5 . . ?
C2F C3F H3F2 109.5 . . ?
H3F3 C3F H3F2 109.5 . . ?
C2F C3F H3F1 109.5 . . ?
H3F3 C3F H3F1 109.5 . . ?
H3F2 C3F H3F1 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O1E 2.505(2) . ?
La1 O12B 2.593(2) . ?
La1 O11C 2.596(2) . ?
La1 O12D 2.606(2) . ?
La1 N14A 2.612(3) . ?
La1 O11B 2.617(2) . ?
La1 O12C 2.657(2) . ?
La1 N1A 2.661(2) . ?
La1 O11D 2.669(2) . ?
La1 N8A 2.687(2) . ?
La1 N1B 3.038(3) . ?
La1 N1C 3.048(3) . ?
N1A C2A 1.347(4) . ?
N1A C6A 1.355(4) . ?
C2A C3A 1.367(4) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.395(4) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.362(5) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.403(4) . ?
C5A H5A 0.9500 . ?
C6A N7A 1.382(4) . ?
N7A N8A 1.364(3) . ?
N7A C71A 1.460(4) . ?
C71A H71C 0.9800 . ?
C71A H71B 0.9800 . ?
C71A H71A 0.9800 . ?
N8A C9A 1.289(4) . ?
C9A C10A 1.444(4) . ?
C9A H9A 0.9500 . ?
C10A N14A 1.333(4) . ?
C10A N11A 1.358(4) . ?
N11A C12A 1.372(4) . ?
N11A C11A 1.455(4) . ?
C11A H11 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11A 0.9800 . ?
C12A C13A 1.356(5) . ?
C12A H12A 0.9500 . ?
C13A N14A 1.370(4) . ?
C13A H13A 0.9500 . ?
N1B O13B 1.217(4) . ?
N1B O12B 1.263(3) . ?
N1B O11B 1.268(4) . ?
N1C O13C 1.230(3) . ?
N1C O11C 1.266(4) . ?
N1C O12C 1.272(3) . ?
N1D O13D 1.219(3) . ?
N1D O11D 1.253(4) . ?
N1D O12D 1.290(3) . ?
O1E C1E 1.435(4) . ?
O1E H1E 0.71(4) . ?
C1E H1E3 0.9800 . ?
C1E H1E2 0.9800 . ?
C1E H1E1 0.9800 . ?
N1F C2F 1.121(5) . ?
C2F C3F 1.452(5) . ?
C3F H3F3 0.9800 . ?
C3F H3F2 0.9800 . ?
C3F H3F1 0.9800 . ?
