Ligand-directed assembly engineering of trapezoidal {Ti<sub>5</sub>} building blocks stabilized by dimethylglyoxime.
Ding, Qing-Rong; Xu, Gui-Lan; Zhang, Lei; Zhang, Jian; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9916–9919; doi:10.1039/c9dt02032b

data_1551220
_publ_section_title
;
 Ligand-directed assembly engineering of trapezoidal {Ti<sub>5</sub>}
 building blocks stabilized by dimethylglyoxime.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9916
_journal_page_last               9919
_journal_paper_doi               10.1039/c9dt02032b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C196 H358 N12 O72 Ti20'
_chemical_formula_sum            'C196 H358 N12 O72 Ti20'
_chemical_formula_weight         4992.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-06-03 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.487(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.1405(13)
_cell_length_b                   26.7150(10)
_cell_length_c                   25.288(3)
_cell_measurement_reflns_used    4680
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      48.3330
_cell_measurement_theta_min      5.6020
_cell_volume                     12889.5(19)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3530
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.1651
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            50338
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.424
_diffrn_reflns_theta_min         3.505
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.583
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.33803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            crimson
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             5268
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1351
_refine_ls_number_reflns         24068
_refine_ls_number_restraints     1337
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.2870
_refine_ls_R_factor_gt           0.1490
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3694
_refine_ls_wR_factor_ref         0.4859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7474
_reflns_number_total             24068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02032b2.cif
_cod_data_source_block           b_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1551215--1551222.cif.'
_cod_database_code               1551220
_oxdiff_exptl_absorpt_empirical_full_min 0.596
_oxdiff_exptl_absorpt_empirical_full_max 2.009
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014-3
_shelx_res_checksum              59085
_shelx_fab_checksum              4709