Crown-ether coordination compounds of zirconium, hafnium and scandium using metal nanoparticles.
Faden, Lara-Pauline; Bayarjargal, Lkhamsuren; Milman, Victor; Winkler, Björn; Feldmann, Claus; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9670–9678; doi:10.1039/d5dt00968e

data_7718805
_publ_section_title
;
 Crown-ether coordination compounds of zirconium, hafnium and scandium
 using metal nanoparticles.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9670
_journal_page_last               9678
_journal_paper_doi               10.1039/d5dt00968e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C12 H24 Cl2 O6 Sc, Al Cl4'
_chemical_formula_sum            'C12 H24 Al Cl6 O6 Sc'
_chemical_formula_weight         548.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-04-14 deposited with the CCDC.	2025-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.413(9)
_cell_length_b                   11.237(3)
_cell_length_c                   21.092(7)
_cell_measurement_reflns_used    1527
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.79
_cell_volume                     4601(3)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      '173 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25099
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.053
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.8041
_exptl_absorpt_correction_T_min  0.4006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         7583
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.868
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                4795
_reflns_number_total             7583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00968e2.cif
_cod_data_source_block           '[sccl2(18c6)][alcl4]'
_cod_depositor_comments
'Adding full bibliography for 7718804--7718807.cif.'
_cod_database_code               7718805
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.717
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.42(6)
 0.58(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
3. Restrained distances
 O12A-C22 \\sim O12-C22 \\sim O12A-C23 \\sim O12-C23
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C22 \\sim O12A \\sim C23: within 1.7A with sigma of 0.03 and sigma for terminal
atoms of 0.06 within 1.7A
5. Others
 Sof(H22C)=Sof(H22D)=Sof(H23C)=Sof(H23D)=Sof(O12A)=1-FVAR(1)
 Sof(O12)=Sof(H22A)=Sof(H22B)=Sof(H23A)=Sof(H23B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C12(H12A,H12B), C4(H4A,H4B), C1(H1A,H1B), C11(H11A,
 H11B), C10(H10A,H10B), C3(H3A,H3B), C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B),
 C6(H6A,H6B), C24(H24A,H24B), C13(H13A,H13B), C14(H14A,H14B), C22(H22C,H22D),
 C22(H22A,H22B), C17(H17A,H17B), C19(H19A,H19B), C18(H18A,H18B), C23(H23C,H23D),
  C23(H23A,H23B), C16(H16A,H16B), C15(H15A,H15B), C20(H20A,H20B), C21(H21A,H21B)
;
_shelx_res_checksum              47309
_shelx_hkl_checksum              12431
_olex2_submission_special_instructions 'No special instructions were received'