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_7248348
_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         'C279 H346 N4 O54 Tb2 Ti13'
_chemical_formula_sum            'C279 H346 N4 O54 Tb2 Ti13'
_chemical_formula_weight         5560.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2022-12-25 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                94.269(2)
_cell_angle_beta                 93.7680(10)
_cell_angle_gamma                90.1350(10)
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_cell_measurement_temperature    190(2)
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_cell_volume                     18861.4(11)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
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_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
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_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
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_diffrn_reflns_point_group_measured_fraction_full 0.990
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_diffrn_reflns_theta_full        45.970
_diffrn_reflns_theta_max         45.969
_diffrn_reflns_theta_min         2.814
_exptl_absorpt_coefficient_mu    4.438
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
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_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
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_refine_ls_number_reflns         31751
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1168P)^2^+149.8386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22575
_reflns_number_total             31751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01275a2.cif
_cod_data_source_block           cu_wyy05_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7248348--7248351.cif.'
_cod_database_code               7248348
_shelx_shelxl_version_number     2014/7
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_shelx_estimated_absorpt_t_max   0.687
_shelx_res_checksum              34366
_shelx_fab_checksum              64062