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_7120342
_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            'C94 H82 O28 P4 Ti6'
_chemical_formula_weight         2070.76
_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                 97.922(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.8073(7)
_cell_length_b                   15.8321(4)
_cell_length_c                   21.8036(15)
_cell_measurement_reflns_used    2837
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      59.2800
_cell_measurement_theta_min      5.5790
_cell_volume                     8823.6(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1274
_diffrn_reflns_av_unetI/netI     0.1688
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.9995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12441
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.9995
_diffrn_reflns_theta_full        62.240
_diffrn_reflns_theta_max         62.240
_diffrn_reflns_theta_min         3.458
_exptl_absorpt_coefficient_mu    5.797
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.000017(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1979
_refine_ls_R_factor_gt           0.1183
_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^)+(0.1799P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2792
_refine_ls_wR_factor_ref         0.3534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3004
_reflns_number_total             6462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_depositor_comments
;

2018-10-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C376 H0 Cl0 N0 O112 P16 Ti24'
_cod_original_formula_weight         7952.16
_cod_original_formula_units_Z            1
_cod_data_source_file            c7cc04388k2.cif
_cod_data_source_block           PTC-61
_cod_database_code               7120342
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              33652