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_4348186
_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 Cl O31 Ti11 Zn, C3 H8 O'
_chemical_formula_sum            'C54 H127 Cl O32 Ti11 Zn'
_chemical_formula_weight         1916.27
_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   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                 90.041(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.044(4)
_cell_length_b                   13.924(4)
_cell_length_c                   20.850(5)
_cell_measurement_reflns_used    3946
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.46
_cell_measurement_theta_min      2.79
_cell_volume                     4368(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.986
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24725
_diffrn_reflns_point_group_measured_fraction_full 0.744
_diffrn_reflns_point_group_measured_fraction_max 0.729
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.445
_diffrn_reflns_theta_min         2.791
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 2772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.213(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         14531
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+5.1290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.477
_reflns_Friedel_fraction_full    0.495
_reflns_Friedel_fraction_max     0.471
_reflns_number_gt                10051
_reflns_number_total             14531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11ZnCl}
_cod_original_cell_volume        4367(2)
_cod_database_code               4348186
_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
 C28-C29
 1.5 with sigma of 0.02
 C28-C29
 1.5 with sigma of 0.02
 C33-C31
 1.5 with sigma of 0.02
 C22-C24
 1.5 with sigma of 0.02
 C16-C18
 1.5 with sigma of 0.02
 C2-C8
 1.45 with sigma of 0.02
 C2-C5
 1.45 with sigma of 0.02
 C5-C8
 2.35 with sigma of 0.02
 C5-C8
 2.35 with sigma of 0.02
 C2-C5
 1.45 with sigma of 0.02
 C8-C5
 2.35 with sigma of 0.02
 C2-O1
 1.45 with sigma of 0.02
 O1-C5
 2.35 with sigma of 0.02
 O1-C2
 1.45 with sigma of 0.02
 C19-C20
 1.5 with sigma of 0.02
 C19-C20
 1.5 with sigma of 0.02
 C13-C15
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C28, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.1
 C28, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.1
 C22, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C29) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C29) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C18) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Riding coordinates:
 O1(HG)
5.b Ternary CH refined with riding coordinates:
 C1AA(H1AA), C3AA(H3AA), C4AA(H4AA), 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), C2(H)
5.c Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C5(HA,HB,HC),
 C8(HD,HE,HF)
5.d Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C2AA(H2AA,H2AB,H2AC), C5AA(H5AA,H5AB,H5AC), C6(H6A,H6B,
 H6C), C6AA(H6AA,H6AB,H6AC), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), 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), C48(H48A,H48B,H48C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              34208
_shelx_hkl_checksum              51990
_olex2_submission_special_instructions 'No special instructions were received'