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_4348185
_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         'C57 H134 Ca O33 Ti11, C3 H7 O, Br'
_chemical_formula_sum            'C60 H141 Br Ca O34 Ti11'
_chemical_formula_weight         2053.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.4617(9)
_cell_length_b                   14.9124(6)
_cell_length_c                   24.3861(10)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.17
_cell_measurement_theta_min      2.65
_cell_volume                     9622.9(6)
_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 0.994
_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  0.0962
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            65438
_diffrn_reflns_point_group_measured_fraction_full 0.762
_diffrn_reflns_point_group_measured_fraction_max 0.738
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_min         2.651
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             4280
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 2311 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.039(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         16378
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0494P)^2^+28.1816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.450
_reflns_Friedel_fraction_full    0.513
_reflns_Friedel_fraction_max     0.470
_reflns_number_gt                9095
_reflns_number_total             16378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11CaBr}
_cod_database_code               4348185
_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
 C35-C36
 1.5 with sigma of 0.02
 C35-C37
 1.5 with sigma of 0.02
 C37-C36
 2.4 with sigma of 0.02
 O15-H15
 0.85 with sigma of 0.01
 C26-C28
 1.45 with sigma of 0.02
 C11-C13
 1.45 with sigma of 0.02
 C53-C54
 1.45 with sigma of 0.02
 C8-C9
 1.45 with sigma of 0.02
 C59-C60
 1.5 with sigma of 0.02
 C59-C61
 1.5 with sigma of 0.02
 O34-C61
 2.35 with sigma of 0.02
 O34-C60
 2.35 with sigma of 0.02
 O35-C60
 2.35 with sigma of 0.02
 O35-C61
 2.35 with sigma of 0.02
 C4-O4
 1.45 with sigma of 0.02
 O16-H16
 0.85 with sigma of 0.01
 O4-C5
 1.45 with sigma of 0.02
 C7-C5
 1.45 with sigma of 0.02
 C5-C6
 1.45 with sigma of 0.02
 C5-C4
 0.6 with sigma of 0.02
 C20-H15
 1.976622 with sigma of 0.02
 Ca1-H15
 2.896651 with sigma of 0.02
 C23-H16
 1.919133 with sigma of 0.02
 Ca1-H16
 3.009204 with sigma of 0.02
3. Rigid bond restraints
 C53, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 H30A, C53, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9
 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(C13) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C4(0.6667) H4(0.6667) C5(0.33333) H5(0.33333) H6BD(0.6667)
 H6BE(0.6667) H6BF(0.6667) H6AA(0.33333) H6AB(0.33333) H6AC(0.33333)
 H7BD(0.6667) H7BE(0.6667) H7BF(0.6667) H7AA(0.33333) H7AB(0.33333)
 H7AC(0.33333) O34(0.5) H34(0.5) O35(0.5) H35A(0.5)
6.a Riding coordinates:
 O16(H16)
6.b Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C8(H8), C14(H14), C17(H17), C20(H20), C23(H23),
 C26(H26), C29(H29), C32(H32), C35(H35), C38(H38), C41(H41), C44(H44), C47(H47),
  C50(H50), C53(H53), C56(H56)
6.c Me refined with riding coordinates:
 C6(H6BD,H6BE,H6BF), C6(H6AA,H6AB,H6AC), C7(H7BD,H7BE,H7BF), C7(H7AA,H7AB,
 H7AC), C9(H9A,H9B,H9C), C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C), C40(H40A,H40B,H40C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
6.d Tetrahedral OH refined with riding coordinates:
 O34(H34), O35(H35A)
6.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              27805
_shelx_hkl_checksum              88477
_olex2_submission_special_instructions 'No special instructions were received'