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_7248350
_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         'C185 H235 O42 Ti13'
_chemical_formula_sum            'C185 H235 O42 Ti13'
_chemical_formula_weight         3753.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 112.768(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_c                   37.7482(10)
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_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      47.46
_cell_measurement_theta_min      2.96
_cell_volume                     53438(2)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.1486
_diffrn_reflns_av_unetI/netI     0.1056
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -57
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_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        47.558
_diffrn_reflns_theta_max         47.558
_diffrn_reflns_theta_min         1.897
_exptl_absorpt_coefficient_mu    3.537
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_description       block
_exptl_crystal_F_000             15736
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2071
_refine_ls_number_reflns         24515
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0897
_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^)+(0.1353P)^2^+452.3015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2570
_refine_ls_wR_factor_ref         0.2885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15025
_reflns_number_total             24515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01275a2.cif
_cod_data_source_block           wyy82a_a_sq
_cod_depositor_comments
'Adding full bibliography for 7248348--7248351.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7248350
_shelx_shelxl_version_number     2014/7
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_shelx_estimated_absorpt_t_max   0.808
_shelx_res_checksum              10187
_shelx_fab_checksum              48406