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_4348183
_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 Br Mg O31 Ti11'
_chemical_formula_sum            'C51 H119 Br Mg O31 Ti11'
_chemical_formula_weight         1859.57
_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                 90.234(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.110(3)
_cell_length_b                   14.173(3)
_cell_length_c                   20.714(5)
_cell_measurement_reflns_used    3786
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.37
_cell_measurement_theta_min      2.44
_cell_volume                     4435.9(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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.1250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27632
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.698
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.746
_diffrn_reflns_theta_min         2.436
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1924
_refine_diff_density_max         2.855
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 1517 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.411(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         14567
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.2153
_refine_ls_R_factor_gt           0.1035
_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^)+(0.1994P)^2^+5.4371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2759
_refine_ls_wR_factor_ref         0.3603
_reflns_Friedel_coverage         0.403
_reflns_Friedel_fraction_full    0.429
_reflns_Friedel_fraction_max     0.401
_reflns_number_gt                6503
_reflns_number_total             14567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11MgBr}
_cod_original_cell_volume        4435.8(17)
_cod_database_code               4348183
_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
2. Restrained distances
 C44-C43
 1.5 with sigma of 0.02
 C45-C43
 1.5 with sigma of 0.02
 C44-C45
 2.4 with sigma of 0.02
 C34-C36
 1.5 with sigma of 0.02
 C34-C35
 1.5 with sigma of 0.02
 C8-C7
 1.5 with sigma of 0.02
 C31-C33
 1.5 with sigma of 0.02
 C37-C39
 1.5 with sigma of 0.02
 C34-C35
 1.5 with sigma of 0.02
 O18-C31
 1.5 with sigma of 0.02
 C49-C50
 1.5 with sigma of 0.02
 C25-C27
 1.5 with sigma of 0.02
 C27-C26
 2.5 with sigma of 0.02
 C3-C2
 2.5 with sigma of 0.02
 C16-C18
 1.5 with sigma of 0.02
 C4-C6
 1.5 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.02
 C32-C31
 1.5 with sigma of 0.02
 C1-C3
 1.5 with sigma of 0.02
 C13-C14
 1.5 with sigma of 0.02
 C40-C42
 1.5 with sigma of 0.02
 C22-C23
 1.5 with sigma of 0.02
 Ti6-O17
 1.7 with sigma of 0.1
 C28-O17
 1.5 with sigma of 0.02
 C28-C29
 1.5 with sigma of 0.02
 C28-C30
 1.5 with sigma of 0.02
 O17-C29
 2.4 with sigma of 0.02
 C30-O17
 2.4 with sigma of 0.02
 C22-C24
 1.5 with sigma of 0.02
 C21-O15
 2.35 with sigma of 0.02
 C19-C21
 1.5 with sigma of 0.02
 C19-C20
 1.5 with sigma of 0.02
 O15-C19
 1.5 with sigma of 0.02
 C22-O15
 1.5 with sigma of 0.02
 C22-C24
 1.5 with sigma of 0.02
 C32-C33
 2.35 with sigma of 0.02
 O18-C33
 2.35 with sigma of 0.02
 C32-O18
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: C19(0.5) H19(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), 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), C52(H52)
5.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C45(H45A,H45B,H45C), C47(H47A,
 H47B,H47C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              54245
_shelx_hkl_checksum              22105
_olex2_submission_special_instructions 'No special instructions were received'