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_4348181
_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 I Ni O31 Ti11'
_chemical_formula_sum            'C51 H119 I Ni O31 Ti11'
_chemical_formula_weight         1940.96
_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                 90.141(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1113(5)
_cell_length_b                   13.9459(4)
_cell_length_c                   20.8851(6)
_cell_measurement_reflns_used    3054
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.59
_cell_measurement_theta_min      2.70
_cell_volume                     4401.3(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 0.888
_diffrn_measured_fraction_theta_max 0.901
_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  0.1231
_diffrn_reflns_av_unetI/netI     0.2772
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32074
_diffrn_reflns_point_group_measured_fraction_full 0.644
_diffrn_reflns_point_group_measured_fraction_max 0.641
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.696
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 1236 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.57(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         12984
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.421
_reflns_Friedel_fraction_full    0.399
_reflns_Friedel_fraction_max     0.380
_reflns_number_gt                5603
_reflns_number_total             12984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11NiI}
_cod_database_code               4348181
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O15-C31
 1.4 with sigma of 0.02
 C31-C32
 1.5 with sigma of 0.02
 C28-C29
 1.5 with sigma of 0.02
 C22-C24
 1.5 with sigma of 0.02
 C40-C42
 1.5 with sigma of 0.02
 C20-C19
 1.5 with sigma of 0.02
 C19-C6AA
 1.5 with sigma of 0.02
 C2AA-C5AA
 1.5 with sigma of 0.02
 C2AA-C5
 1.5 with sigma of 0.02
 C3AA-C12
 1.5 with sigma of 0.02
 C3AA-C11
 1.5 with sigma of 0.02
 C12-O6
 2.5 with sigma of 0.02
 C31-C10
 1.45 with sigma of 0.02
 C31-C7
 1.45 with sigma of 0.02
 C46-C1
 1.45 with sigma of 0.02
 C6-C46
 1.45 with sigma of 0.02
 C25-C50
 1.45 with sigma of 0.02
 C25-C21
 1.45 with sigma of 0.02
 O18-C21
 2.35 with sigma of 0.02
 C7-O15
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10 \\sim C7 \\sim C31 \\sim C32: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O17) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O31) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H31(0.5) H31A(0.5) H25A(0.5) H25(0.5) H46(0.5) H46A(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C1(0.5)
 H1A(0.5) H1B(0.5) H1C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
5.a Ternary CH refined with riding coordinates:
 C3AA(H3AA), C31(H31), C31(H31A), C13(H13), C16(H16), C0AA(H0AA), C2AA(H2AA),
 C4AA(H4AA), C28(H28), C19(H19), C22(H22), C25(H25A), C25(H25), C40(H40),
 C49(H49), C46(H46), C46(H46A), C43(H43), C34(H34), C37(H37)
5.b Me refined with riding coordinates:
 C5AA(H5AA,H5AB,H5AC), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C50(H50A,H50B,H50C)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C1AA(H1AA,H1AB,
 H1AC), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C17(H17A,
 H17B,H17C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C30(H30A,H30B,
 H30C), C29(H29A,H29B,H29C), C6AA(H6AA,H6AB,H6AC), C20(H20A,H20B,H20C),
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C51(H51A,H51B,H51C), C7AA(H7AA,H7AB,H7AC),
 C48(H48A,H48B,H48C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C), C36(H36A,H36B,
 H36C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              56800
_shelx_hkl_checksum              41755
_olex2_submission_special_instructions 'No special instructions were received'