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_7062480
_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         'C28 H45 N2 O12 P Ti3'
_chemical_formula_sum            'C28 H45 N2 O12 P Ti3'
_chemical_formula_weight         776.33
_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
_audit_creation_date             2023-02-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-03-12 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                112.778(2)
_cell_angle_beta                 94.618(2)
_cell_angle_gamma                110.303(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0582(6)
_cell_length_b                   12.1208(7)
_cell_length_c                   14.3450(9)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    149.98
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.36
_cell_volume                     1756.13(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       Apex4
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker D8 venture single crystal diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29775
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.385
_diffrn_reflns_theta_min         2.909
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1004 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.9129.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6433
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0440P)^2^+1.7726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5764
_reflns_number_total             6433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01172k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7062479--7062482.cif.'
_cod_database_code               7062480
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.861
_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
 O00G-C28 \\sim O00G-C16
 with sigma of 0.02
 C28-C14 \\sim C16-C30
 with sigma of 0.02
 C28-C12 \\sim C16-C8
 with sigma of 0.02
 C30-C8 \\sim C12-C14
 with sigma of 0.02
 C6-C27 \\sim C6A-C27A
 with sigma of 0.02
 C27-C10 \\sim C27A-C10A
 with sigma of 0.02
 O008-C27 \\sim O008-C27A
 with sigma of 0.02
 C10-C6 \\sim C10A-C6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O00G \\sim C8 \\sim C12 \\sim C14 \\sim C16 \\sim C28 \\sim C30: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O008 \\sim C6 \\sim C10 \\sim C27 \\sim C27A \\sim C10A \\sim C6A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C12, C14, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C8, C16, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C10A, C27A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C27, C10, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C16)=Sof(H16)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C28)=Sof(H28)=FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(2)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C27)=Sof(H27)=FVAR(2)
6.a Riding coordinates:
 P04(H04)
6.b Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C16(H16), C18(H18), C27(H27), C28(H28), C27A(H27A)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C15(H15), C17(H17), C19(H19), C21(H21), C23(H23), C25(H25),
 C29(H29)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C10A(H10D,H10E,H10F), C6A(H6AA,H6AB,H6AC)
;
_shelx_res_checksum              8693
_shelx_hkl_checksum              66053
_olex2_submission_special_instructions 'No special instructions were received'