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_4348184
_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 H127 Ca Cl O32 Ti11, C3 H8 O'
_chemical_formula_sum            'C57 H135 Ca Cl O33 Ti11'
_chemical_formula_weight         1951.07
_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'
_atom_sites_solution_hydrogens   mixed
_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                 92.091(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.036(4)
_cell_length_b                   15.163(4)
_cell_length_c                   39.981(10)
_cell_measurement_reflns_used    5248
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.58
_cell_measurement_theta_min      2.48
_cell_volume                     9109(4)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.1202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            59008
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.476
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         20819
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1245P)^2^+0.7990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2130
_refine_ls_wR_factor_ref         0.2747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8526
_reflns_number_total             20819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11CaCl}
_cod_database_code               4348184
_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 O(H) groups
2. Restrained distances
 C55-C56
 1.5 with sigma of 0.02
 C55-C57
 1.5 with sigma of 0.02
 C55-O33
 1.5 with sigma of 0.04
 C55-O33
 1.5 with sigma of 0.02
 C57-O33
 2.4 with sigma of 0.02
 O33-C56
 2.4 with sigma of 0.02
 C56-C57
 2.4 with sigma of 0.02
 C55-C57
 1.5 with sigma of 0.02
 O18-H18
 0.87 with sigma of 0.01
 C46-C48
 1.5 with sigma of 0.02
 C47-C46
 1.5 with sigma of 0.02
 C10-C11
 1.5 with sigma of 0.02
 C10-C12
 1.5 with sigma of 0.02
 C11-C10
 1.5 with sigma of 0.02
 C10-C12
 1.5 with sigma of 0.02
 C11-C10
 1.5 with sigma of 0.01
 C12-C10
 1.5 with sigma of 0.01
 C12-C11
 2.5 with sigma of 0.02
 C37-C38
 1.5 with sigma of 0.02
 C37-C39
 1.5 with sigma of 0.02
 C55-O33
 1.5 with sigma of 0.02
 C52-C54
 1.45 with sigma of 0.02
 C25-C26
 1.5 with sigma of 0.02
 C34-H18
 1.941584 with sigma of 0.02
 Ca1-H18
 2.944561 with sigma of 0.02
3. Rigid bond restraints
 C22, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C25, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C10, C11
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 C1, C3
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 C40, C42
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 C43, C44
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 C43, C45
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 C46, C48
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
4. Uiso/Uaniso restraints and constraints
C11 \\sim C10 \\sim C12: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C56 \\sim C55 \\sim C57 \\sim O33: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.08
C3 \\sim C1 \\sim C2: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
Uanis(C48) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5.a Ternary CH refined with riding coordinates:
 C34(H34), C31(H31), C46(H46), C28(H28), C10(H10), C22(H22), C19(H19),
 C40(H40), C49(H49), C7(H7), C43(H43), C4(H4), C1(H1), C52(H52), C13(H13),
 C37(H37), C16(H16), C25(H25), C55(H55)
5.b Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C54(H54A,H54B,
 H54C)
5.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C30(H30A,H30B,
 H30C), C9(H9A,H9B,H9C), C50(H50A,H50B,H50C), C12(H12A,H12B,H12C), C29(H29A,
 H29B,H29C), C45(H45A,H45B,H45C), C21(H21A,H21B,H21C), C47(H47A,H47B,H47C),
 C5(H5A,H5B,H5C), C15(H15A,H15B,H15C), C3(H3A,H3B,H3C), C26(H26A,H26B,H26C),
 C14(H14A,H14B,H14C), C33(H33A,H33B,H33C), C51(H51A,H51B,H51C), C6(H6A,H6B,H6C),
  C27(H27A,H27B,H27C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C42(H42A,H42B,
 H42C), C39(H39A,H39B,H39C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C8(H8A,
 H8B,H8C), C48(H48A,H48B,H48C), C53(H53A,H53B,H53C), C38(H38A,H38B,H38C),
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C20(H20A,H20B,H20C), C23(H23A,H23B,
 H23C)
5.d Idealised tetrahedral OH refined as rotating group:
 O33(H33)
;
_shelx_res_checksum              70545
_shelx_hkl_checksum              50523
_olex2_submission_special_instructions 'No special instructions were received'