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_4348175
_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 Co O31 Ti11, C3 H8 O'
_chemical_formula_sum            'C54 H127 Cl Co O32 Ti11'
_chemical_formula_weight         1909.83
_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                 90.123(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.047(3)
_cell_length_b                   13.919(3)
_cell_length_c                   20.904(5)
_cell_measurement_reflns_used    3752
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.07
_cell_measurement_theta_min      2.71
_cell_volume                     4378.1(17)
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24956
_diffrn_reflns_point_group_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.707
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             1986
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 3463 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         16315
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0527P)^2^+7.1626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.640
_reflns_Friedel_fraction_full    0.697
_reflns_Friedel_fraction_max     0.635
_reflns_number_gt                10663
_reflns_number_total             16315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11CoCl}
_cod_original_cell_volume        4378.0(17)
_cod_database_code               4348175
_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, All O(H) groups
2. Restrained distances
 C26-C28
 1.5 with sigma of 0.02
 C26-C27
 1.5 with sigma of 0.02
 C14-C15
 1.5 with sigma of 0.02
 C54-C55
 1.45 with sigma of 0.02
 C54-C56
 1.45 with sigma of 0.02
 C56-C55
 2.35 with sigma of 0.02
 C48-C49
 1.45 with sigma of 0.02
 C54-O32
 1.45 with sigma of 0.02
 C55-O32
 2.35 with sigma of 0.02
 C32-C34
 1.45 with sigma of 0.02
 C54-O32
 1.4 with sigma of 0.02
 C36-C38
 1.4 with sigma of 0.02
 C14-C13
 0.8 with sigma of 0.02
 C14-C16
 1.45 with sigma of 0.02
 C14-O7
 1.45 with sigma of 0.02
3. Rigid bond restraints
 C26, O17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C48, O30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C28
 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(C21) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C21) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C7) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C13(0.5) H13(0.5) C14(0.5) H14(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
 H15D(0.5) H15E(0.5) H15F(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5)
 H16E(0.5) H16F(0.5) C35(0.5) H35(0.5) C36(0.5) H36(0.5) H37A(0.5) H37B(0.5)
 H37C(0.5) H37D(0.5) H37E(0.5) H37F(0.5) H38A(0.5) H38B(0.5) H38C(0.5)
 H38D(0.5) H38E(0.5) H38F(0.5)
6.a Riding coordinates:
 O32(H32A)
6.b Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C14(H14), C17(H17), C20(H20),
 C23(H23), C26(H26), C29(H29), C32(H32), C35(H35), C36(H36), C39(H39), C42(H42),
  C45(H45), C48(H48), C51(H51), C54(H54)
6.c Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C15(H15D,H15E,H15F), C16(H16A,H16B,H16C), C16(H16D,H16E,
 H16F), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C37(H37D,
 H37E,H37F), C38(H38A,H38B,H38C), C38(H38D,H38E,H38F), C55(H55A,H55B,H55C),
 C56(H56A,H56B,H56C)
6.d 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), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C30(H30A,H30B,
 H30C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              8961
_shelx_hkl_checksum              47811
_olex2_submission_special_instructions 'No special instructions were received'