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_1551219
_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         'C111 H220 N4 O57 Ti16'
_chemical_formula_sum            'C111 H220 N4 O57 Ti16'
_chemical_formula_weight         3288.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                109.617(3)
_cell_angle_beta                 96.107(3)
_cell_angle_gamma                95.889(3)
_cell_formula_units_Z            1
_cell_length_a                   15.4097(7)
_cell_length_b                   15.8879(6)
_cell_length_c                   17.9294(7)
_cell_measurement_reflns_used    6703
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6570
_cell_measurement_theta_min      3.6990
_cell_volume                     4066.3(3)
_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 16.2083
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29913
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.553
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.78515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.004
_refine_diff_density_min         -2.184
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         14264
_refine_ls_number_restraints     560
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1695
_refine_ls_R_factor_gt           0.1228
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3639
_refine_ls_wR_factor_ref         0.4190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8534
_reflns_number_total             14264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02032b2.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 1551215--1551222.cif.'
_cod_database_code               1551219
_shelxl_version_number           2014-3
_shelx_res_checksum              76377
_shelx_fab_checksum              33662