Acid/base responsive assembly/dis-assembly of a family of zirconium(IV) clusters with a cyclic imide-dioxime ligand.
Passadis, Stamatis S.; Hadjithoma, Sofia; Papanikolaou, Michael G.; Keramidas, Anastasios D.; Miras, Haralampos N.; Kabanos, Themistoklis A.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1806–1818; doi:10.1039/d1dt03641f

data_7709175
_publ_section_title
;
 Acid/base responsive assembly/dis-assembly of a family of zirconium(IV)
 clusters with a cyclic imide-dioxime ligand.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1806
_journal_page_last               1818
_journal_paper_doi               10.1039/d1dt03641f
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C10 H19.60 N6 O6 Zr, C H4 O, 2(Cl), H2 O '
_chemical_formula_sum            'C11 H25.6 Cl2 N6 O8 Zr'
_chemical_formula_weight         532.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-17 deposited with the CCDC.	2021-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9010(6)
_cell_length_b                   14.1221(5)
_cell_length_c                   17.6833(9)
_cell_measurement_reflns_used    5016
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      30.5160
_cell_measurement_theta_min      2.6330
_cell_volume                     3970.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      174(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17472
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             2173
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3310
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+2.9682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2573
_reflns_number_total             3310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03641f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7709175--7709176.cif.'
_cod_original_formula_sum        'C11 H25.60 Cl2 N6 O8 Zr'
_cod_database_code               7709175
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              80585