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_7718804
_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         'Al2 Cl8 Na, C8 H16 Al Cl2 O4'
_chemical_formula_sum            'C8 H16 Al3 Cl10 Na O4'
_chemical_formula_weight         634.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 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            4
_cell_length_a                   6.9873(8)
_cell_length_b                   12.6813(13)
_cell_length_c                   27.426(3)
_cell_measurement_reflns_used    6312
_cell_measurement_temperature    213
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      4.31
_cell_volume                     2430.2(5)
_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      213.00
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 124 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  0.0191
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.485
_exptl_absorpt_coefficient_mu    1.286
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.0820
_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    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.5(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0851
_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^)+(0.1243P)^2^+30.2583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2513
_refine_ls_wR_factor_ref         0.2583
_reflns_Friedel_coverage         0.728
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3375
_reflns_number_total             4273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00968e2.cif
_cod_data_source_block           '[alcl2(12c4)][naal2cl8]'
_cod_depositor_comments
'Adding full bibliography for 7718804--7718807.cif.'
_cod_original_cell_volume        2430.1(4)
_cod_database_code               7718804
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.699
_shelx_estimated_absorpt_t_min   0.699
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5(4)
 0.5(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C2(H2A,H2B), C1(H1A,H1B), C7(H7A,H7B), C8(H8A,H8B),
 C4(H4A,H4B), C6(H6A,H6B)
;
_shelx_res_checksum              67743
_shelx_hkl_checksum              22609
_olex2_submission_special_instructions 'No special instructions were received'