Metallacrown of CeIIICuII5: Synthesis, Structural Characterization and Insights for Nanoparticles
Tempesta, Jésio D.; Paiva, Fábio Faria; Ferreira, Leonildo A.; da Silva, Rafaela M. R.; Botelho, Luckerman D. G.; Rosa, Iara M. L.; Candido, Caio Cesar; Gomes, Angelo Marcio; Nunes, Wallace C.; Guedes, Guilherme P.; Marinho, Maria Vanda; Magnetochemistry 10 (2024) 96–; doi:10.3390/magnetochemistry10120096

data_1573429
_publ_section_title
;
 Metallacrown of CeIIICuII5: Synthesis, Structural Characterization and
 Insights for Nanoparticles
;
_journal_issue                   12
_journal_name_full               Magnetochemistry
_journal_page_first              96
_journal_paper_doi               10.3390/magnetochemistry10120096
_journal_volume                  10
_journal_year                    2024
_chemical_formula_moiety         'C30 H39 Ce Cu5 N17 O23, H2 O'
_chemical_formula_sum            'C30 H41 Ce Cu5 N17 O24'
_chemical_formula_weight         1481.62
_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
_atom_sites_solution_primary     difmap
_audit_creation_date             2024-04-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-03 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                79.469(2)
_cell_angle_beta                 87.062(2)
_cell_angle_gamma                81.301(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6894(2)
_cell_length_b                   15.4536(4)
_cell_length_c                   16.1745(5)
_cell_measurement_reflns_used    8793
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7490
_cell_measurement_theta_min      2.5590
_cell_volume                     2838.72(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4186
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -89.00  20.00   1.00   20.86    --  -10.85 -77.00  60.00  109
  2  \w    -37.00  54.00   1.00   20.86    --  -10.85  57.00 -30.00   91
  3  \w    -85.00  16.00   1.00   20.86    --  -10.85 -57.00-180.00  101
  4  \w     11.00  60.00   1.00   20.86    --   12.88  77.00 150.00   49
  5  \w     14.00  41.00   1.00   20.86    --   12.88 -57.00   0.00   27
  6  \w     -8.00  23.00   1.00   20.86    --   12.88  38.00 120.00   31
  7  \w     56.00  84.00   1.00   20.86    --   12.88  38.00 120.00   28
  8  \w    -61.00 -34.00   1.00   20.86    --   12.88 -57.00   0.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0031073000
_diffrn_orient_matrix_UB_12      0.0083292000
_diffrn_orient_matrix_UB_13      -0.0444893000
_diffrn_orient_matrix_UB_21      0.0573582000
_diffrn_orient_matrix_UB_22      -0.0222631000
_diffrn_orient_matrix_UB_23      -0.0029388000
_diffrn_orient_matrix_UB_31      -0.0216964000
_diffrn_orient_matrix_UB_32      -0.0407548000
_diffrn_orient_matrix_UB_33      0.0016701000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26967
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.556
_diffrn_reflns_theta_min         2.204
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.711
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       plate
_exptl_crystal_F_000             1470
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         13295
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0447
_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/[\s^2^(Fo^2^)+(0.0405P)^2^+0.0994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9434
_reflns_number_total             13295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2388656.cif
_cod_data_source_block           ce-ls-cu1
_cod_database_code               1573429
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30 H50 Cu5 N18 O31 Ce1'
_chemical_oxdiff_usercomment     'redundant data'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O24-H24A = O24-H24B
 0.85 with sigma of 0.02
 H24A-H24B
 1.3 with sigma of 0.02
 H13B-H13A
 1.3 with sigma of 0.02
 O13-H13B
 0.85 with sigma of 0.02
 O13-H13A
 0.85 with sigma of 0.02
 O12-H12B = O12-H12A
 0.85 with sigma of 0.01
 H12B-H12A
 1.3 with sigma of 0.02
 H23A-H23B
 1.3 with sigma of 0.02
 O23-H23A = O23-H23B
 0.85 with sigma of 0.02
 O18A-N17A = O18B-N17B = O19A-N17A = O19B-N17B = O20A-N17A = O20B-N17B
 1.22 with sigma of 0.02
 O19B-O20B
 2.15 with sigma of 0.02
 O18B-O19B
 2.15 with sigma of 0.02
 O18B-O20B
 2.15 with sigma of 0.02
 O14-H14A = O14-H14B
 0.85 with sigma of 0.02
 H14A-H14B
 1.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N17A) = Uanis(N17B)
Uanis(O20A) = Uanis(O20B) = Uanis(O18A) = Uanis(O18B) = Uanis(O19A) =
Uanis(O19B)
4. Others
 Sof(N17B)=Sof(O18B)=Sof(O20B)=Sof(O19B)=1-FVAR(1)
 Sof(N17A)=Sof(O18A)=Sof(O20A)=Sof(O19A)=FVAR(1)
5.a Free rotating group:
 O25(H25A,H25B)
5.b Rotating group:
 O22(H22A,H22B), O11(H11A,H11B), O24(H24A,H24B)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C10(H10), C8(H8), C22(H22), C16(H16), C4(H4), C26(H26), C14(H14),
 C28(H28), C2(H2)
5.d Idealised Me refined as rotating group:
 C24(H24C,H24D,H24E), C6(H6A,H6B,H6C), C30(H30A,H30B,H30C), C12(H12C,H12D,
 H12E), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              66965
_shelx_hkl_checksum              10292
_shelx_fab_checksum              93842
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.454
_oxdiff_exptl_absorpt_empirical_full_min 0.798
_publcif_funding_html
;
;