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_4348178
_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         '2(C51 H119 Co N O34 Ti11)'
_chemical_formula_sum            'C102 H238 Co2 N2 O68 Ti22'
_chemical_formula_weight         3752.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 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                 112.47(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.935(17)
_cell_length_b                   13.625(7)
_cell_length_c                   26.060(10)
_cell_measurement_reflns_used    93
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      63.29
_cell_measurement_theta_min      37.75
_cell_volume                     8838(8)
_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 0.864
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_unetI/netI     0.1483
_diffrn_reflns_Laue_measured_fraction_full 0.864
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46685
_diffrn_reflns_point_group_measured_fraction_full 0.623
_diffrn_reflns_point_group_measured_fraction_max 0.684
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.756
_diffrn_reflns_theta_min         1.775
_exptl_absorpt_coefficient_mu    10.023
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             3892
_refine_diff_density_max         1.557
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 2376 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.113(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         19950
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1703
_refine_ls_R_factor_gt           0.0947
_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^)+(0.1526P)^2^+12.2032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2387
_refine_ls_wR_factor_ref         0.2894
_reflns_Friedel_coverage         0.443
_reflns_Friedel_fraction_full    0.383
_reflns_Friedel_fraction_max     0.420
_reflns_number_gt                11488
_reflns_number_total             19950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01071_si_002.cif
_cod_data_source_block           {Ti11CoNO3}
_cod_database_code               4348178
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O20-N1
 1.3 with sigma of 0.02
 N1-O21
 1.3 with sigma of 0.02
 C107-C109
 1.45 with sigma of 0.02
 C30-C31
 1.45 with sigma of 0.02
 C32-C31
 2.35 with sigma of 0.02
 C15-C16
 1.45 with sigma of 0.02
 C11-C12
 1.45 with sigma of 0.02
 C103-C104
 1.45 with sigma of 0.02
 C42-C39
 1.45 with sigma of 0.02
 C46-C47
 1.45 with sigma of 0.02
 C46-C48
 1.45 with sigma of 0.02
 C30-C32
 1.45 with sigma of 0.02
 C21-O15
 1.45 with sigma of 0.02
 C21-C23
 1.45 with sigma of 0.02
 C21-C22
 1.45 with sigma of 0.02
 O15-C22
 2.35 with sigma of 0.02
 O15-C23
 2.35 with sigma of 0.02
 C23-C22
 2.35 with sigma of 0.02
 O7-C14
 1.5 with sigma of 0.02
 O3-C2
 1.5 with sigma of 0.02
 C56-C57
 1.5 with sigma of 0.02
 H76C-H77A
 2 with sigma of 0.02
 C81-C83
 1.5 with sigma of 0.02
3. Others
 Fixed Sof: C1(0.5) H1(0.5) C2(0.5) H2(0.5) H3BD(0.5) H3BE(0.5) H3BF(0.5)
 H3AA(0.5) H3AB(0.5) H3AC(0.5) H4BD(0.5) H4BE(0.5) H4BF(0.5) H4AA(0.5)
 H4AB(0.5) H4AC(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) H16D(0.5) H16E(0.5)
 H16F(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H17D(0.5) H17E(0.5) H17F(0.5)
 H17A(0.5) H17B(0.5) H17C(0.5) H39(0.5) H39A(0.5) C41(0.5) H41A(0.5) H41B(0.5)
 H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) H46(0.5) H46A(0.5) C47(0.5)
 H47A(0.5) H47B(0.5) H47C(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) H59A(0.5)
 H59(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5) H61B(0.5)
 H61C(0.5) H90(0.5) H90A(0.5) C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C93(0.5)
 H93A(0.5) H93B(0.5) H93C(0.5) H10J(0.5) H103(0.5) C104(0.5) H10K(0.5)
 H10L(0.5) H10M(0.5) C105(0.5) H10N(0.5) H10O(0.5) H10P(0.5)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C8(H8), C11(H11), C14(H14), C15(H15), C18(H18),
 C21(H21), C24(H24), C27(H27), C30(H30), C33(H33), C36(H36), C39(H39),
 C39(H39A), C43(H43), C46(H46), C46(H46A), C50(H50), C53(H53), C56(H56),
 C59(H59A), C59(H59), C63(H63), C66(H66), C69(H69), C72(H72), C75(H75),
 C78(H78), C81(H81), C84(H84), C87(H87), C90(H90), C90(H90A), C94(H94),
 C97(H97), C100(H100), C103(H10J), C103(H103), C107(H107)
4.b Me refined with riding coordinates:
 C3(H3BD,H3BE,H3BF), C3(H3AA,H3AB,H3AC), C4(H4BD,H4BE,H4BF), C4(H4AA,H4AB,
 H4AC), C16(H16D,H16E,H16F), C16(H16A,H16B,H16C), C17(H17D,H17E,H17F), C17(H17A,
 H17B,H17C), C25(H25A,H25B,H25C), C42(H42A,H42B,H42C), C57(H57A,H57B,H57C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C83(H83A,H83B,H83C), C104(H10K,H10L,
 H10M)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C58(H58A,H58B,H58C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C82(H82A,
 H82B,H82C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C),
 C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,
 H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C99(H99A,
 H99B,H99C), C101(H10D,H10E,H10F), C102(H10G,H10H,H10I), C105(H10N,H10O,H10P),
 C106(H10Q,H10R,H10S), C108(H10T,H10U,H10V), C109(H10W,H10X,H10Y)
;
_shelx_res_checksum              53601
_shelx_hkl_checksum              97800
_olex2_submission_special_instructions 'No special instructions were received'