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_7718806
_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 Cl2 Hf O5, Al4 Cl16 Na2'
_chemical_formula_sum            'C10 H20 Al4 Cl18 Hf Na2 O5'
_chemical_formula_weight         1190.75
_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                 102.438(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9975(11)
_cell_length_b                   14.909(2)
_cell_length_c                   12.5159(13)
_cell_measurement_reflns_used    11752
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.56
_cell_volume                     2004.0(4)
_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      293.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'IPDS II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25099
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.666
_exptl_absorpt_coefficient_mu    3.936
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.4924
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9231
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      0.791
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0371P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5309
_reflns_number_total             9231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00968e2.cif
_cod_data_source_block           '[hfcl2(15c5)][na2al4cl16]'
_cod_depositor_comments
'Adding full bibliography for 7718804--7718807.cif.'
_cod_database_code               7718806
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.46(3)
 0.54(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
O1_1 \\sim O2_1 \\sim O3_1 \\sim O4_1 \\sim O5_1 \\sim C1_1 \\sim C2_1 \\sim
C3_1 \\sim C4_1 \\sim C5_1 \\sim C6_1 \\sim C7_1 \\sim C8_1 \\sim C9_1 \\sim
C10_1 \\sim O1_2 \\sim O2_2 \\sim O3_2 \\sim O4_2 \\sim O5_2 \\sim C1_2 \\sim
C2_2 \\sim C3_2 \\sim C4_2 \\sim C5_2 \\sim C6_2 \\sim C7_2 \\sim C8_2 \\sim
C9_2 \\sim C10_2: within 1.7A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 1.7A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_1, O2_1, O3_1, O4_1, O5_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1,
 C9_1, C10_1
 O1_2, O2_2, O3_2, O4_2, O5_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2,
 C9_2, C10_2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{O1_2, O2_2, O3_2, O4_2, O5_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2,
C9_2, C10_2}
as
{O1_1, O2_1, O3_1, O4_1, O5_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1,
C9_1, C10_1} sigma for 1-2: 0.02 1-3: 0.04
6. Others
 Fixed Sof: O1(0.62) O2(0.62) O3(0.62) O4(0.62) O5(0.62) C1(0.62) H1A(0.62)
 H1B(0.62) C2(0.62) H2A(0.62) H2B(0.62) C3(0.62) H3A(0.62) H3B(0.62) C4(0.62)
 H4A(0.62) H4B(0.62) C5(0.62) H5A(0.62) H5B(0.62) C6(0.62) H6A(0.62) H6B(0.62)
 C7(0.62) H7A(0.62) H7B(0.62) C8(0.62) H8A(0.62) H8B(0.62) C9(0.62) H9A(0.62)
 H9B(0.62) C10(0.62) H10A(0.62) H10B(0.62) O1(0.38) O2(0.38) O3(0.38) O4(0.38)
 O5(0.38) C1(0.38) H1A(0.38) H1B(0.38) C2(0.38) H2A(0.38) H2B(0.38) C3(0.38)
 H3A(0.38) H3B(0.38) C4(0.38) H4A(0.38) H4B(0.38) C5(0.38) H5A(0.38) H5B(0.38)
 C6(0.38) H6A(0.38) H6B(0.38) C7(0.38) H7A(0.38) H7B(0.38) C8(0.38) H8A(0.38)
 H8B(0.38) C9(0.38) H9A(0.38) H9B(0.38) C10(0.38) H10A(0.38) H10B(0.38)
7.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), 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              41265
_shelx_hkl_checksum              97472
_olex2_submission_special_instructions 'No special instructions were received'