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_7062481
_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         'C56 H90 N4 O24 P2 Ti6'
_chemical_formula_sum            'C56 H90 N4 O24 P2 Ti6'
_chemical_formula_weight         1552.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-07 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.759(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8651(5)
_cell_length_b                   20.8697(9)
_cell_length_c                   17.8564(8)
_cell_measurement_reflns_used    9345
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.341
_cell_measurement_theta_min      2.357
_cell_volume                     3538.1(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            108420
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_min         2.357
_diffrn_source_current           1.41
_diffrn_source_power             0.0705
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.8960.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6490
_refine_ls_number_restraints     781
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0429P)^2^+4.3209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5604
_reflns_number_total             6490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01172k2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7062479--7062482.cif.'
_cod_database_code               7062481
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.927
_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
 C25-C23 = C15-C29 = C23-C13
 1.51 with sigma of 0.02
 C3-C5 = C27-C5
 1.5 with sigma of 0.02
 O5-C23 = O3-C29
 1.45 with sigma of 0.02
 C29-C15
 1.51 with sigma of 0.02
 C23-C13 = C25-C23
 1.5 with sigma of 0.02
 C7-C29
 1.7 with sigma of 0.02
 C7-C15
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O5)=Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C13)=
 Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(1)
 Sof(C29)=Sof(H29)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(O3)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C12(H12), C20(H20), C5(H5), C23(H23), C29(H29)
6.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C7(H7A,H7B,H7C)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C14(H14), C16(H16), C24(H24), C9(H9), C19(H19), C21(H21),
 C11(H11)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C3(H3A,H3B,H3C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              16113
_shelx_hkl_checksum              99786
_olex2_submission_special_instructions 'No special instructions were received'