#------------------------------------------------------------------------------
#$Date: 2024-09-06 02:17:00 +0200 (Fri 06 de Sep de 2024) $
#$Revision: 294520 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/89/7248961.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_7248961
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         'C11 H15 N8 O10 Sm, C H4 O'
_chemical_formula_sum            'C12 H19 N8 O11 Sm'
_chemical_formula_weight         601.70
_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                96.710(3)
_cell_angle_beta                 98.034(3)
_cell_angle_gamma                100.381(4)
_cell_formula_units_Z            2
_cell_length_a                   8.1537(3)
_cell_length_b                   10.4239(4)
_cell_length_c                   12.3673(3)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.0120
_cell_measurement_theta_min      3.3150
_cell_volume                     1012.84(6)
_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      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.837
_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  0.0199
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.219
_diffrn_reflns_theta_min         2.801
_exptl_absorpt_coefficient_mu    2.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       plate
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0195P)²+0.3697P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3879
_reflns_number_total             4169
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00450g2.cif
_cod_data_source_block           15
_cod_depositor_comments
'Adding full bibliography for 7248946--7248974.cif.'
_cod_database_code               7248961
_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
Sm1 Sm 0.30021(2) 0.77288(2) 0.28739(2) 0.00973(5) Uani 1 1 d . . . . .
N1A N 0.0447(3) 0.6962(2) 0.37892(17) 0.0114(4) Uani 1 1 d . . . . .
C2A C -0.0194(3) 0.7843(3) 0.4410(2) 0.0156(6) Uani 1 1 d . . . . .
H2A H 0.0351 0.8744 0.4507 0.019 Uiso 1 1 calc R U . . .
C3A C -0.1580(3) 0.7520(3) 0.4910(2) 0.0181(6) Uani 1 1 d . . . . .
H3A H -0.1988 0.8176 0.5336 0.022 Uiso 1 1 calc R U . . .
C4A C -0.2367(3) 0.6199(3) 0.4772(2) 0.0175(6) Uani 1 1 d . . . . .
H4A H -0.3316 0.5934 0.5119 0.021 Uiso 1 1 calc R U . . .
C5A C -0.1768(3) 0.5283(3) 0.4134(2) 0.0148(5) Uani 1 1 d . . . . .
H5A H -0.2301 0.4378 0.4030 0.018 Uiso 1 1 calc R U . . .
C6A C -0.0362(3) 0.5695(2) 0.3638(2) 0.0118(5) Uani 1 1 d . . . . .
N7A N 0.0272(3) 0.4799(2) 0.29694(18) 0.0130(5) Uani 1 1 d . . . . .
C71A C -0.0556(3) 0.3417(2) 0.2669(2) 0.0169(6) Uani 1 1 d . . . . .
H71C H -0.0454 0.3113 0.1906 0.025 Uiso 1 1 calc R U . . .
H71B H -0.1754 0.3319 0.2737 0.025 Uiso 1 1 calc R U . . .
H71A H -0.0017 0.2889 0.3164 0.025 Uiso 1 1 calc R U . . .
N8A N 0.1806(3) 0.5241(2) 0.26833(17) 0.0110(4) Uani 1 1 d . . . . .
C9A C 0.2637(3) 0.4428(3) 0.2252(2) 0.0132(5) Uani 1 1 d . . . . .
H9A H 0.2221 0.3503 0.2128 0.016 Uiso 1 1 calc R U . . .
C10A C 0.4236(3) 0.5009(3) 0.1970(2) 0.0126(5) Uani 1 1 d . . . . .
N11A N 0.5222(3) 0.4346(2) 0.14134(17) 0.0131(5) Uani 1 1 d . . . . .
C11A C 0.4873(4) 0.2935(3) 0.1002(2) 0.0196(6) Uani 1 1 d . . . . .
H11C H 0.5002 0.2440 0.1625 0.029 Uiso 1 1 calc R U . . .
H11B H 0.5669 0.2750 0.0507 0.029 Uiso 1 1 calc R U . . .
H11A H 0.3715 0.2668 0.0598 0.029 Uiso 1 1 calc R U . . .
C12A C 0.6601(3) 0.5260(3) 0.1290(2) 0.0154(6) Uani 1 1 d . . . . .
H12A H 0.7513 0.5096 0.0928 0.018 Uiso 1 1 calc R U . . .
C13A C 0.6404(3) 0.6443(3) 0.1785(2) 0.0156(6) Uani 1 1 d . . . . .
H13A H 0.7174 0.7256 0.1830 0.019 Uiso 1 1 calc R U . . .
N14A N 0.4932(3) 0.6290(2) 0.22104(17) 0.0129(5) Uani 1 1 d . . . . .
N1B N 0.2255(3) 1.0230(2) 0.2221(2) 0.0202(5) Uani 1 1 d . . . . .
O11B O 0.1908(3) 0.98204(18) 0.31086(17) 0.0235(5) Uani 1 1 d . . . . .
O12B O 0.3142(2) 0.96051(18) 0.16838(16) 0.0199(4) Uani 1 1 d . . . . .
O13B O 0.1708(3) 1.1160(2) 0.1898(2) 0.0343(5) Uani 1 1 d . . . . .
N1C N 0.0704(3) 0.6970(2) 0.07199(18) 0.0194(5) Uani 1 1 d . . . . .
O11C O 0.0260(2) 0.7469(2) 0.15888(15) 0.0200(4) Uani 1 1 d . . . . .
O12C O 0.2227(2) 0.68360(18) 0.07974(15) 0.0178(4) Uani 1 1 d . . . . .
O13C O -0.0295(3) 0.6629(3) -0.01463(17) 0.0401(6) Uani 1 1 d . . . . .
N1D N 0.4122(3) 0.7770(2) 0.52805(18) 0.0160(5) Uani 1 1 d . . . . .
O11D O 0.3657(2) 0.87739(17) 0.49203(15) 0.0165(4) Uani 1 1 d . . . . .
O12D O 0.4064(2) 0.67870(17) 0.45673(15) 0.0159(4) Uani 1 1 d . . . . .
O13D O 0.4601(3) 0.7770(2) 0.62658(16) 0.0293(5) Uani 1 1 d . . . . .
O1E O 0.5794(3) 0.9108(2) 0.33678(19) 0.0173(4) Uani 1 1 d . . . . .
H2E H 0.640(4) 0.940(3) 0.295(3) 0.024(9) Uiso 1 1 d . . . . .
H1E H 0.593(4) 0.964(3) 0.384(3) 0.019(9) Uiso 1 1 d . . . . .
O1F O 0.8043(3) 1.0042(3) 0.2119(2) 0.0435(7) Uani 1 1 d . . . . .
H1F H 0.925(10) 1.023(8) 0.243(7) 0.21(4) Uiso 1 1 d . . . . .
C1F C 0.7682(5) 1.0049(4) 0.0954(3) 0.0449(10) Uani 1 1 d . . . . .
H1F3 H 0.8239 1.0895 0.0776 0.067 Uiso 1 1 calc R U . . .
H1F2 H 0.6458 0.9927 0.0721 0.067 Uiso 1 1 calc R U . . .
H1F1 H 0.8102 0.9332 0.0567 0.067 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'
Sm Sm -0.1638 3.4418 '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 Sm1 O11B 86.24(7) . . ?
O1E Sm1 O11C 141.98(7) . . ?
O11B Sm1 O11C 70.59(7) . . ?
O1E Sm1 N14A 75.68(7) . . ?
O11B Sm1 N14A 154.49(7) . . ?
O11C Sm1 N14A 113.82(6) . . ?
O1E Sm1 O12D 80.61(7) . . ?
O11B Sm1 O12D 119.15(6) . . ?
O11C Sm1 O12D 136.87(6) . . ?
N14A Sm1 O12D 75.95(6) . . ?
O1E Sm1 N1A 138.77(7) . . ?
O11B Sm1 N1A 80.10(7) . . ?
O11C Sm1 N1A 67.72(6) . . ?
N14A Sm1 N1A 125.27(7) . . ?
O12D Sm1 N1A 72.83(6) . . ?
O1E Sm1 N8A 134.93(7) . . ?
O11B Sm1 N8A 137.30(7) . . ?
O11C Sm1 N8A 77.59(7) . . ?
N14A Sm1 N8A 65.61(7) . . ?
O12D Sm1 N8A 68.68(6) . . ?
N1A Sm1 N8A 61.56(7) . . ?
O1E Sm1 O12C 112.97(7) . . ?
O11B Sm1 O12C 105.48(6) . . ?
O11C Sm1 O12C 50.08(6) . . ?
N14A Sm1 O12C 66.78(6) . . ?
O12D Sm1 O12C 134.36(6) . . ?
N1A Sm1 O12C 108.15(6) . . ?
N8A Sm1 O12C 72.41(6) . . ?
O1E Sm1 O12B 72.19(7) . . ?
O11B Sm1 O12B 50.23(6) . . ?
O11C Sm1 O12B 69.82(6) . . ?
N14A Sm1 O12B 106.16(7) . . ?
O12D Sm1 O12B 150.94(6) . . ?
N1A Sm1 O12B 122.71(6) . . ?
N8A Sm1 O12B 139.34(6) . . ?
O12C Sm1 O12B 68.19(6) . . ?
O1E Sm1 O11D 67.47(7) . . ?
O11B Sm1 O11D 69.95(6) . . ?
O11C Sm1 O11D 126.61(6) . . ?
N14A Sm1 O11D 117.39(7) . . ?
O12D Sm1 O11D 50.08(6) . . ?
N1A Sm1 O11D 71.30(6) . . ?
N8A Sm1 O11D 110.69(6) . . ?
O12C Sm1 O11D 175.43(6) . . ?
O12B Sm1 O11D 108.11(6) . . ?
O1E Sm1 N1B 80.23(7) . . ?
O11B Sm1 N1B 25.24(6) . . ?
O11C Sm1 N1B 65.87(6) . . ?
N14A Sm1 N1B 131.16(7) . . ?
O12D Sm1 N1B 140.30(6) . . ?
N1A Sm1 N1B 100.65(7) . . ?
N8A Sm1 N1B 143.40(7) . . ?
O12C Sm1 N1B 85.24(6) . . ?
O12B Sm1 N1B 25.17(6) . . ?
O11D Sm1 N1B 90.40(6) . . ?
O1E Sm1 N1C 131.00(7) . . ?
O11B Sm1 N1C 88.21(7) . . ?
O11C Sm1 N1C 24.95(6) . . ?
N14A Sm1 N1C 90.23(7) . . ?
O12D Sm1 N1C 141.58(6) . . ?
N1A Sm1 N1C 87.50(6) . . ?
N8A Sm1 N1C 72.94(7) . . ?
O12C Sm1 N1C 25.14(6) . . ?
O12B Sm1 N1C 67.20(6) . . ?
O11D Sm1 N1C 151.51(7) . . ?
N1B Sm1 N1C 74.66(6) . . ?
C6A N1A C2A 117.2(2) . . ?
C6A N1A Sm1 122.28(16) . . ?
C2A N1A Sm1 120.47(16) . . ?
N1A C2A C3A 124.3(3) . . ?
N1A C2A H2A 117.9 . . ?
C3A C2A H2A 117.9 . . ?
C2A C3A C4A 117.6(2) . . ?
C2A C3A H3A 121.2 . . ?
C4A C3A H3A 121.2 . . ?
C5A C4A C3A 119.7(2) . . ?
C5A C4A H4A 120.1 . . ?
C3A C4A H4A 120.1 . . ?
C4A C5A C6A 119.1(2) . . ?
C4A C5A H5A 120.4 . . ?
C6A C5A H5A 120.4 . . ?
N1A C6A N7A 116.9(2) . . ?
N1A C6A C5A 122.0(2) . . ?
N7A C6A C5A 121.0(2) . . ?
N8A N7A C6A 116.74(19) . . ?
N8A N7A C71A 120.4(2) . . ?
C6A N7A C71A 122.6(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 120.9(2) . . ?
C9A N8A Sm1 118.72(16) . . ?
N7A N8A Sm1 120.28(15) . . ?
N8A C9A C10A 116.0(2) . . ?
N8A C9A H9A 122.0 . . ?
C10A C9A H9A 122.0 . . ?
N14A C10A N11A 110.7(2) . . ?
N14A C10A C9A 124.0(2) . . ?
N11A C10A C9A 125.3(2) . . ?
C10A N11A C12A 106.9(2) . . ?
C10A N11A C11A 126.7(2) . . ?
C12A N11A C11A 126.4(2) . . ?
N11A C11A H11C 109.5 . . ?
N11A C11A H11B 109.5 . . ?
H11C C11A H11B 109.5 . . ?
N11A C11A H11A 109.5 . . ?
H11C C11A H11A 109.5 . . ?
H11B C11A H11A 109.5 . . ?
C13A C12A N11A 106.5(2) . . ?
C13A C12A H12A 126.7 . . ?
N11A C12A H12A 126.7 . . ?
C12A C13A N14A 109.8(2) . . ?
C12A C13A H13A 125.1 . . ?
N14A C13A H13A 125.1 . . ?
C10A N14A C13A 106.0(2) . . ?
C10A N14A Sm1 114.62(16) . . ?
C13A N14A Sm1 137.49(17) . . ?
O13B N1B O12B 122.3(3) . . ?
O13B N1B O11B 121.1(2) . . ?
O12B N1B O11B 116.6(2) . . ?
O13B N1B Sm1 170.54(19) . . ?
O12B N1B Sm1 60.32(13) . . ?
O11B N1B Sm1 56.92(13) . . ?
N1B O11B Sm1 97.84(15) . . ?
N1B O12B Sm1 94.51(15) . . ?
O13C N1C O11C 121.5(2) . . ?
O13C N1C O12C 122.0(2) . . ?
O11C N1C O12C 116.4(2) . . ?
O13C N1C Sm1 177.29(19) . . ?
O11C N1C Sm1 56.66(12) . . ?
O12C N1C Sm1 59.82(12) . . ?
N1C O11C Sm1 98.39(15) . . ?
N1C O12C Sm1 95.04(14) . . ?
O13D N1D O12D 122.0(2) . . ?
O13D N1D O11D 121.6(2) . . ?
O12D N1D O11D 116.4(2) . . ?
O13D N1D Sm1 178.8(2) . . ?
O12D N1D Sm1 56.95(12) . . ?
O11D N1D Sm1 59.42(12) . . ?
N1D O11D Sm1 95.23(13) . . ?
N1D O12D Sm1 98.32(15) . . ?
Sm1 O1E H2E 127(2) . . ?
Sm1 O1E H1E 117(2) . . ?
H2E O1E H1E 105(3) . . ?
C1F O1F H1F 114(5) . . ?
O1F C1F H1F3 109.5 . . ?
O1F C1F H1F2 109.5 . . ?
H1F3 C1F H1F2 109.5 . . ?
O1F C1F H1F1 109.5 . . ?
H1F3 C1F H1F1 109.5 . . ?
H1F2 C1F H1F1 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
Sm1 O1E 2.4184(19) . ?
Sm1 O11B 2.5017(19) . ?
Sm1 O11C 2.5069(19) . ?
Sm1 N14A 2.515(2) . ?
Sm1 O12D 2.5258(19) . ?
Sm1 N1A 2.555(2) . ?
Sm1 N8A 2.572(2) . ?
Sm1 O12C 2.5761(18) . ?
Sm1 O12B 2.578(2) . ?
Sm1 O11D 2.5778(17) . ?
Sm1 N1B 2.958(2) . ?
Sm1 N1C 2.969(2) . ?
N1A C6A 1.345(3) . ?
N1A C2A 1.351(3) . ?
C2A C3A 1.371(4) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.390(4) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.368(4) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.399(4) . ?
C5A H5A 0.9500 . ?
C6A N7A 1.392(3) . ?
N7A N8A 1.362(3) . ?
N7A C71A 1.458(3) . ?
C71A H71C 0.9800 . ?
C71A H71B 0.9800 . ?
C71A H71A 0.9800 . ?
N8A C9A 1.290(3) . ?
C9A C10A 1.442(4) . ?
C9A H9A 0.9500 . ?
C10A N14A 1.334(3) . ?
C10A N11A 1.357(3) . ?
N11A C12A 1.375(3) . ?
N11A C11A 1.463(3) . ?
C11A H11C 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11A 0.9800 . ?
C12A C13A 1.359(4) . ?
C12A H12A 0.9500 . ?
C13A N14A 1.367(3) . ?
C13A H13A 0.9500 . ?
N1B O13B 1.223(3) . ?
N1B O12B 1.262(3) . ?
N1B O11B 1.273(3) . ?
N1C O13C 1.225(3) . ?
N1C O11C 1.266(3) . ?
N1C O12C 1.266(3) . ?
N1D O13D 1.226(3) . ?
N1D O12D 1.261(3) . ?
N1D O11D 1.282(3) . ?
O1E H2E 0.81(4) . ?
O1E H1E 0.74(3) . ?
O1F C1F 1.431(4) . ?
O1F H1F 0.98(8) . ?
C1F H1F3 0.9800 . ?
C1F H1F2 0.9800 . ?
C1F H1F1 0.9800 . ?
