Deep Eutectic-Solvothermal Synthesis of Titanium-Oxo Clusters Protected by π-Conjugate Chromophores
Narayanam, Nagaraju; Fang, Wei-Hui; Chintakrinda, Kalpana; Zhang, Lei; Zhang, Jian; Chem. Commun.  (2017) –; doi:10.1039/C7CC04388K

data_7120345
_publ_section_title
;
 Deep Eutectic-Solvothermal Synthesis of Titanium-Oxo Clusters Protected
 by \p-Conjugate Chromophores
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04388K
_journal_year                    2017
_chemical_formula_sum            'C326 H178 Cl8 N28 O74 Ti28'
_chemical_formula_weight         7295.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-05 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.402(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.438(4)
_cell_length_b                   19.8705(6)
_cell_length_c                   40.975(3)
_cell_measurement_reflns_used    10833
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.0990
_cell_measurement_theta_min      3.7650
_cell_volume                     32698(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            47617
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        62.302
_diffrn_reflns_theta_max         62.302
_diffrn_reflns_theta_min         3.769
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    6.751
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       Rod
_exptl_crystal_F_000             14696
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1855
_refine_ls_number_reflns         25188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1561P)^2^+72.4553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2170
_refine_ls_wR_factor_ref         0.2829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14039
_reflns_number_total             25188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04388k2.cif
_cod_data_source_block           PTC-64
_cod_database_code               7120345
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              79851