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_7718807
_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         'C10 H20 Al4 Cl18 Na2 O5 Zr'
_chemical_formula_sum            'C10 H20 Al4 Cl18 Na2 O5 Zr'
_chemical_formula_weight         1103.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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                 102.298(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8277(8)
_cell_length_b                   14.5595(9)
_cell_length_c                   12.2538(11)
_cell_measurement_reflns_used    27580
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.89
_cell_measurement_theta_min      2.20
_cell_volume                     1887.4(3)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.139.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area LANA 1.71.6.0 (STOE, 2017)
;
_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      100.15
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
 691 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26442
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         2.202
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_T_max  0.7021
_exptl_absorpt_correction_T_min  0.2638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.43(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7713
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0726P)^2^+4.5009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                6480
_reflns_number_total             7713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00968e2.cif
_cod_data_source_block           '[zrcl2(15c5)][na2al4cl16]'
_cod_depositor_comments
'Adding full bibliography for 7718804--7718807.cif.'
_cod_database_code               7718807
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.57(11)
 0.43(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
;
_shelx_res_checksum              17004
_shelx_hkl_checksum              92716
_olex2_submission_special_instructions 'No special instructions were received'