Solvent-polarity-controlled assembly of polynuclear titanium-calixarene complexes: constructing isolated {Ti7}, {Ti13}, {Ti24} and {Tb2Ti13} clusters
Wang, Yanyan; Xiong, Ying; Liao, Wuping; CrystEngComm 26 (2024) 2287–2296; doi:10.1039/D3CE01275A

data_7248351
_publ_section_title
;
 Solvent-polarity-controlled assembly of polynuclear titanium-calixarene
 complexes: constructing isolated {Ti7}, {Ti13}, {Ti24} and {Tb2Ti13}
 clusters
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2287
_journal_page_last               2296
_journal_paper_doi               10.1039/D3CE01275A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C358 H430 N2 O72 Ti24'
_chemical_formula_sum            'C358 H430 N2 O72 Ti24'
_chemical_formula_weight         7062.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-12-25 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                111.5900(10)
_cell_angle_beta                 108.5490(10)
_cell_angle_gamma                96.5950(10)
_cell_formula_units_Z            1
_cell_length_a                   22.9160(6)
_cell_length_b                   23.1929(6)
_cell_length_c                   25.3092(6)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      54.9549
_cell_measurement_theta_min      3.3358
_cell_volume                     11440.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            225026
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        55.129
_diffrn_reflns_theta_max         55.129
_diffrn_reflns_theta_min         3.224
_exptl_absorpt_coefficient_mu    3.814
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.087
_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     2053
_refine_ls_number_reflns         28358
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+46.6994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.2461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21056
_reflns_number_total             28358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01275a2.cif
_cod_data_source_block           10a_sq
_cod_depositor_comments
'Adding full bibliography for 7248348--7248351.cif.'
_cod_database_code               7248351
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.601
_shelx_estimated_absorpt_t_max   0.696
_shelx_res_checksum              19065
_shelx_fab_checksum              55229