Ligand-directed structure evolution from a titanium-oxo cluster to coordination capsule and one-dimensional coordination polymer based on {Ti3O} units
Meng, Min; Liao, Lingrong; Zheng, Qi; Xuan, Weimin; New Journal of Chemistry 47 (2023) 11312–11317; doi:10.1039/D3NJ01172K

data_7062479
_publ_section_title
;
 Ligand-directed structure evolution from a titanium-oxo cluster to
 coordination capsule and one-dimensional coordination polymer based on
 {Ti3O} units
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11312
_journal_page_last               11317
_journal_paper_doi               10.1039/D3NJ01172K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C42 H80 N2 O24 P2 Ti6'
_chemical_formula_sum            'C42 H80 N2 O24 P2 Ti6'
_chemical_formula_weight         1346.42
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-12 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                70.8620(10)
_cell_angle_beta                 73.9500(10)
_cell_angle_gamma                84.3280(10)
_cell_formula_units_Z            1
_cell_length_a                   11.3702(3)
_cell_length_b                   11.9984(4)
_cell_length_c                   12.4292(4)
_cell_measurement_reflns_used    9413
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.347
_cell_measurement_theta_min      2.905
_cell_volume                     1539.42(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       Apex4
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Bruker D8 venture single crystal diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32051
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.360
_diffrn_reflns_theta_min         2.577
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.9110.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5571
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0275P)^2^+0.6784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5272
_reflns_number_total             5571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01172k2.cif
_cod_data_source_block           mo_mm0909mo_0m
_cod_depositor_comments
'Adding full bibliography for 7062479--7062482.cif.'
_cod_database_code               7062479
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.544
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C11 = C13-C16 = C13-C7 = C15-C1
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Others
 Sof(C13)=Sof(H13)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C1)=Sof(H1A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C3(H3), C5(H5), C2(H2), C13(H13), C1(H1A)
5.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C19(H19), C20(H20), C24(H24)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C),
 C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              4621
_shelx_hkl_checksum              25550
_olex2_submission_special_instructions 'No special instructions were received'