Synergistic ligand effect for the construction of titanium-oxo clusters with planar chirality and high solution stability.
Ding, Qing-Rong; Xu, Gui-Lan; Zhang, Jian; Zhang, Lei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4030–4033; doi:10.1039/d0dt00197j

data_7703961
_publ_section_title
;
 Synergistic ligand effect for the construction of titanium-oxo clusters
 with planar chirality and high solution stability.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4030
_journal_page_last               4033
_journal_paper_doi               10.1039/d0dt00197j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C67 H126 N4 O29 Ti8'
_chemical_formula_sum            'C67 H126 N4 O29 Ti8'
_chemical_formula_weight         1834.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-02-21 deposited with the CCDC.	2020-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.243(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.9555(7)
_cell_length_b                   12.7596(6)
_cell_length_c                   19.0307(6)
_cell_measurement_reflns_used    5926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8140
_cell_measurement_theta_min      3.5990
_cell_volume                     4601.8(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2083
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18843
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.400
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_platon_squeeze_details
;

;
_refine_diff_density_max         2.418
_refine_diff_density_min         -1.976
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8088
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0946
_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^)+(0.1810P)^2^+12.7760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2823
_refine_ls_wR_factor_ref         0.3003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6236
_reflns_number_total             8088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00197j2.cif
_cod_data_source_block           PTC-67
_cod_database_code               7703961
_shelx_shelxl_version_number     2018/1
_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
 C27-C29
 1.52 with sigma of 0.01
 C30-C31
 1.52 with sigma of 0.01
3. Rigid bond restraints
 O2, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Ti1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 Ti4, O14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ti4, O13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C10 \\sim O2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C30 \\sim C31 \\sim C32 \\sim O11: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C18 \\sim C17 \\sim C1 \\sim C23 \\sim C3 \\sim C19 \\sim C22 \\sim C20 \\sim
C2 \\sim C21 \\sim C14 \\sim C4 \\sim C11 \\sim C15 \\sim C30 \\sim C13 \\sim
C5 \\sim C12 \\sim C16 \\sim C24 \\sim C28 \\sim C32 \\sim C10 \\sim C27 \\sim
C7 \\sim C26 \\sim C6 \\sim C31 \\sim C9 \\sim C8 \\sim C25 \\sim C29: within
3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) = Uanis(C26) = Uanis(C25)
Uanis(O13) = Uanis(C24)
Uanis(C8) = Uanis(C10) = Uanis(C9)
Uanis(O2) = Uanis(C8)
Uanis(C27) = Uanis(C28) = Uanis(C29)
Uanis(O14) = Uanis(C27)
Uanis(C30) = Uanis(C31)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C11(H11), C30(H30), C5(H5), C24(H24), C27(H27), C8(H8)
5.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C),
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C26(H26A,H26B,H26C), C6(H6A,H6B,
 H6C), C31(H31A,H31B,H31C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C), C29(H29A,H29B,
 H29C)
5.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C20(H20), C21(H21)
;
_shelx_res_checksum              61080
_shelx_fab_checksum              65303
_olex2_submission_special_instructions 'No special instructions were received'