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_4348188
_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         'C51 H119 Cd Cl O31 Ti11'
_chemical_formula_sum            'C51 H119 Cd Cl O31 Ti11'
_chemical_formula_weight         1903.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.979(9)
_cell_length_b                   13.904(6)
_cell_length_c                   15.104(6)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.70
_cell_volume                     4406(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.674
_diffrn_measured_fraction_theta_max 0.723
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.1309
_diffrn_reflns_Laue_measured_fraction_full 0.674
_diffrn_reflns_Laue_measured_fraction_max 0.723
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24619
_diffrn_reflns_point_group_measured_fraction_full 0.625
_diffrn_reflns_point_group_measured_fraction_max 0.663
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         2.697
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 3259 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.374(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         13370
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.577
_reflns_Friedel_fraction_max     0.602
_reflns_number_gt                9358
_reflns_number_total             13370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11CdCl}
_cod_database_code               4348188
_shelxl_version_number           2014-3
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C25-C26
 1.5 with sigma of 0.02
 C13-C14
 1.5 with sigma of 0.02
 C25-C27
 1.5 with sigma of 0.02
 C34-C35
 1.5 with sigma of 0.02
 O6-C0AA
 1.5 with sigma of 0.02
 C0AA-C15
 1.5 with sigma of 0.02
 C0AA-C14
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C0AA(0.5) H0AA(0.5) C13(0.5) H13(0.5) H14D(0.5) H14E(0.5)
 H14F(0.5) H14A(0.5) H14B(0.5) H14C(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
 H15A(0.5) H15B(0.5) H15C(0.5)
5.a Ternary CH refined with riding coordinates:
 C0AA(H0AA), C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19),
 C22(H22), C25(H25), C28(H28), C31(H31), C34(H34), C37(H37), C40(H40), C43(H43),
  C46(H46), C49(H49)
5.b Me refined with riding coordinates:
 C14(H14D,H14E,H14F), C14(H14A,H14B,H14C), C15(H15D,H15E,H15F), C15(H15A,H15B,
 H15C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C48(H48A,
 H48B,H48C)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              76380
_shelx_hkl_checksum              23716
_olex2_submission_special_instructions 'No special instructions were received'