Effects of Substitutional Dopants on the Photoresponse of a Polyoxotitanate Cluster.
Hu, Junyi; Zhan, Lijie; Zhang, Guanyun; Zhang, Qun; Du, Lin; Tung, Chen-Ho; Wang, Yifeng; Inorganic chemistry 55 (2016) 8493–8501; doi:10.1021/acs.inorgchem.6b01071

data_4348174
_publ_section_title
;
 Effects of Substitutional Dopants on the Photoresponse of a
 Polyoxotitanate Cluster.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8493
_journal_page_last               8501
_journal_paper_doi               10.1021/acs.inorgchem.6b01071
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C54 H126 O32 Ti11'
_chemical_formula_sum            'C54 H126 O32 Ti11'
_chemical_formula_weight         1814.44
_chemical_name_systematic        Ti11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.356(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.302(3)
_cell_length_b                   14.391(3)
_cell_length_c                   19.729(4)
_cell_measurement_reflns_used    504
_cell_measurement_temperature    173
_cell_measurement_theta_max      15.029
_cell_measurement_theta_min      2.831
_cell_volume                     4627.2(16)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2003)'
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1493
_diffrn_reflns_av_unetI/netI     0.2281
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22624
_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         25.000
_diffrn_reflns_theta_min         1.888
_exptl_absorpt_coefficient_mu    0.960
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_preparation       'in isopropanol'
_exptl_crystal_recrystallization_method 'block crystal'
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8118
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1991
_refine_ls_R_factor_gt           0.0966
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1274P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2366
_refine_ls_wR_factor_ref         0.2842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3083
_reflns_number_total             8118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11}
_cod_original_cell_volume        4627.1(14)
_cod_database_code               4348174
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C4
 1.5 with sigma of 0.02
 C5-C4
 1.5 with sigma of 0.02
 C5-C6
 2.35 with sigma of 0.02
 C16-O12
 1.5 with sigma of 0.02
 C18-C16
 1.5 with sigma of 0.02
 C18-O12
 2.35 with sigma of 0.02
 C16-C17
 1.5 with sigma of 0.02
 C17-O12
 2.35 with sigma of 0.02
 C18-C17
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C21 \\sim C2 \\sim C7 \\sim C11 \\sim C12 \\sim C9 \\sim C19
\\sim C15 \\sim C10 \\sim C3 \\sim C26 \\sim C4 \\sim C20 \\sim C14 \\sim C8
\\sim C25 \\sim C24 \\sim C22 \\sim C27 \\sim C13 \\sim C1 \\sim C23 \\sim C16
\\sim C17 \\sim C18: within 1.7A with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Others
 Fixed Sof: Ti5(0.9) Ti6(0.6)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C10(H10), C4(H4), C25(H25), C22(H22), C13(H13), C1(H1),
 C16(H16)
5.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C3(H3A,H3B,H3C), C26(H26A,H26B,
 H26C), C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C24(H24A,
 H24B,H24C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              66249
_shelx_hkl_checksum              61768
_olex2_exptl_crystal_mounting_method 'in N2 flow'
_olex2_submission_original_sample_id Ti11
_olex2_submission_special_instructions 'No special instructions were received'