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_1551217
_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         'C82 H169 N5 O36 Ti10'
_chemical_formula_sum            'C82 H169 N5 O36 Ti10'
_chemical_formula_weight         2311.89
_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   geom
_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                82.343(4)
_cell_angle_beta                 85.367(3)
_cell_angle_gamma                70.160(4)
_cell_formula_units_Z            1
_cell_length_a                   11.8011(4)
_cell_length_b                   13.8482(7)
_cell_length_c                   18.9934(7)
_cell_measurement_reflns_used    6798
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      74.3000
_cell_measurement_theta_min      4.3020
_cell_volume                     2891.6(2)
_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      99.98(13)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20280
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.491
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1213
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.446
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         11438
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2412P)^2^+6.2584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2935
_refine_ls_wR_factor_ref         0.3370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8505
_reflns_number_total             11438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02032b2.cif
_cod_data_source_block           a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1551215--1551222.cif.'
_cod_database_code               1551217
_oxdiff_exptl_absorpt_empirical_full_min 0.688
_oxdiff_exptl_absorpt_empirical_full_max 3.541
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014-3
_shelx_res_checksum              57273