A layered titanium(iv)-peroxo-pyridine dicarboxylic cluster: crystal structure and photoelectrochemical sensing of dopamine.
Li, Caixia; Tao, Ran; Jin, Zhanbin; Li, Fengyan; Fang, Wencheng; Xu, Lin; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1175–1178; doi:10.1039/c8dt04495c

data_7048312
_publ_section_title
;
 A layered titanium(iv)-peroxo-pyridine dicarboxylic cluster: crystal
 structure and photoelectrochemical sensing of dopamine.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1175
_journal_page_last               1178
_journal_paper_doi               10.1039/c8dt04495c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C21 H21 Cl K3 N3 O28 Ti3'
_chemical_formula_weight         1059.86
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-04 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.084(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4378(16)
_cell_length_b                   21.135(2)
_cell_length_c                   11.9539(10)
_cell_measurement_reflns_used    4210
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.994
_cell_measurement_theta_min      2.584
_cell_volume                     3611.4(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1190
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33570
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         25.057
_diffrn_reflns_theta_min         2.287
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.7817
_exptl_absorpt_correction_T_min  0.7339
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.715
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6382
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+15.2896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4133
_reflns_number_total             6382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04495c2.cif
_cod_data_source_block           111
_cod_depositor_comments          'Adding full bibliography for 7048312.cif.'
_cod_database_code               7048312
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.734
_shelx_estimated_absorpt_t_max   0.782
_shelx_res_checksum              36644