A Post-Functionalizable Iso-Polyoxotitanate Cage Cluster.
Hou, Jie; Hu, Junyi; Sun, Qing; Zhang, Guanyun; Tung, Chen-Ho; Wang, Yifeng; Inorganic chemistry 55 (2016) 7075–7078; doi:10.1021/acs.inorgchem.6b00982

data_4348118
_publ_section_title
;
 A Post-Functionalizable Iso-Polyoxotitanate Cage Cluster.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7075
_journal_page_last               7078
_journal_paper_doi               10.1021/acs.inorgchem.6b00982
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '3(C54 H126 O32 Ti12), 6(I3)'
_chemical_formula_sum            'C162 H378 I18 O96 Ti36'
_chemical_formula_weight         7871.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0141(14)
_cell_length_b                   51.767(5)
_cell_length_c                   38.161(4)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      20.78
_cell_measurement_theta_min      2.42
_cell_volume                     29391(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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  0.1126
_diffrn_reflns_av_unetI/netI     0.1882
_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       63
_diffrn_reflns_limit_k_min       -67
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            171053
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.392
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       irregular
_exptl_crystal_F_000             15456
_refine_diff_density_max         3.128
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.161
_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     2711
_refine_ls_number_reflns         66794
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.2447
_refine_ls_R_factor_gt           0.0971
_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^)+(0.0968P)^2^+99.0714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25832
_reflns_number_total             66794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00982_si_002.cif
_cod_data_source_block           p21c
_cod_original_cell_volume        29392(5)
_cod_database_code               4348118
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5C,H5B,H5A} of C5, All C(H,H) groups
 At 1.5 times of:
  {H15S,H15T,H15U} of C159, {H15G,H15H,H15I} of C153, {H15P,H15Q,H15R} of
  C157, {H15A,H15B,H15C} of C150, {H15M,H15N,H15O} of C156, {H15D,H15E,H15F} of
  C151, {H15J,H15K,H15L} of C154, {H16D,H16E,H16F} of C160, {H64A,H64B,H64C} of
  C64, {H53A,H53B,H53C} of C53, {H56A,H56B,H56C} of C56, {H62A,H62B,H62C} of
  C62, {H59A,H59B,H59C} of C59, {H52A,H52B,H52C} of C52, {H55A,H55B,H55C} of
  C55, {H58A,H58B,H58C} of C58, {H61A,H61B,H61C} of C61, {H71A,H71B,H71C} of
  C71, {H76A,H76B,H76C} of C76, {H74A,H74B,H74C} of C74, {H82A,H82B,H82C} of
  C82, {H83A,H83B,H83C} of C83, {H80A,H80B,H80C} of C80, {H70A,H70B,H70C} of
  C70, {H67A,H67B,H67C} of C67, {H68A,H68B,H68C} of C68, {H65A,H65B,H65C} of
  C65, {H77A,H77B,H77C} of C77, {H73A,H73B,H73C} of C73, {H79A,H79B,H79C} of
  C79, {H14G,H14H,H14I} of C142, {H13Z,H,HA} of C139, {H14P,H14Q,H14R} of C147,
  {H13W,H13X,H13Y} of C138, {H14M,H14N,H14O} of C145, {H13Q,H13R,H13S} of C136,
  {H14J,H14K,H14L} of C144, {H13T,H13U,H13V} of C137, {H13D,H13E,H13F} of C130,
  {H13M,H13N,H13O} of C134, {H13G,H13H,H13I} of C131, {H14D,H14E,H14F} of C141,
  {H13J,H13K,H13L} of C133, {H14S,H14T,H14U} of C148, {H10S,H10T,H10U} of C103,
  {H10V,H10W,H10X} of C104, {H95A,H95B,H95C} of C95, {H92A,H92B,H92C} of C92,
  {H88A,H88B,H88C} of C88, {H89A,H89B,H89C} of C89, {H91A,H91B,H91C} of C91,
  {H98A,H98B,H98C} of C98, {H10P,H10Q,H10R} of C101, {H85A,H85B,H85C} of C85,
  {H86A,H86B,H86C} of C86, {H97A,H97B,H97C} of C97, {H94A,H94B,H94C} of C94,
  {H10M,H10N,H10O} of C100, {H12A,H12B,H12C} of C121, {H11J,H11K,H11L} of C113,
  {H11P,H11Q,H11R} of C116, {H12M,H12N,H12O} of C127, {H11M,H11N,H11O} of C115,
  {H11S,H11T,H11U} of C118, {H12P,H12Q,H12R} of C128, {H11V,H11W,H11X} of C119,
  {H11D,H11E,H11F} of C110, {H12D,H12E,H12F} of C122, {H11G,H11H,H11I} of C112,
  {H12G,H12H,H12I} of C124, {H12J,H12K,H12L} of C125, {H20A,H20B,H20C} of C20,
  {H23A,H23B,H23C} of C23, {H13A,H13B,H13C} of C13, {H19A,H19B,H19C} of C19,
  {H25A,H25B,H25C} of C25, {H9AA,H9AB,H9AC} of C9AA, {H11A,H11B,H11C} of C11,
  {H16A,H16B,H16C} of C16, {H22A,H22B,H22C} of C22, {H14A,H14B,H14C} of C14,
  {H10A,H10B,H10C} of C10, {H17A,H17B,H17C} of C17, {H38A,H38B,H38C} of C38,
  {H44A,H44B,H44C} of C44, {H37A,H37B,H37C} of C37, {H41A,H41B,H41C} of C41,
  {H35A,H35B,H35C} of C35, {H32A,H32B,H32C} of C32, {H43A,H43B,H43C} of C43,
  {H28A,H28B,H28C} of C28, {H31A,H31B,H31C} of C31, {H29A,H29B,H29C} of C29,
  {H34A,H34B,H34C} of C34, {H26A,H26B,H26C} of C26, {H40A,H40B,H40C} of C40,
  {H49A,H49B,H49C} of C49, {H46A,H46B,H46C} of C46, {H50A,H50B,H50C} of C50,
  {H47A,H47B,H47C} of C47, {H10J,H10K,H10L} of C108, {H10G,H10H,H10I} of C107,
  {H10D,H10E,H10F} of C106, {H8BA,H8BB,H8BC} of C8BA, {H6A,H6B,H6C} of C6, {H2A,
  H2B,H2C} of C2, {H6AA,H6AB,H6AC} of C6AA, {H8CA,H8CB,H8CC} of C8CA, {H7A,H7B,
  H7C} of C7, {H3A,H3B,H3C} of C3, {H4A,H4B,H4C} of C4, {H8A,H8B,H8C} of C8
2. Restrained distances
 C21-C22
 1.5 with sigma of 0.02
 C21-C23
 1.5 with sigma of 0.02
 C22-C23
 2.35 with sigma of 0.02
 O80-C12
 1.4 with sigma of 0.02
 C12-C14
 1.45 with sigma of 0.02
 C12-C13
 1.45 with sigma of 0.02
 C39-O65
 1.45 with sigma of 0.02
 C48-O66
 1.45 with sigma of 0.02
 C33-O67
 1.45 with sigma of 0.02
 C39-O65
 1.45 with sigma of 0.02
 C40-C41
 2.35 with sigma of 0.02
 C41-C39
 1.45 with sigma of 0.02
 C27-O85
 1.45 with sigma of 0.02
 C27-C29
 1.45 with sigma of 0.02
 C120-C122
 1.45 with sigma of 0.02
 C117-C118
 1.5 with sigma of 0.02
 C84-C86
 1.5 with sigma of 0.02
 C39-C40
 1.5 with sigma of 0.02
 C39-C41
 1.5 with sigma of 0.02
 C27-O85
 1.4 with sigma of 0.02
 C27-C29
 1.5 with sigma of 0.02
 C27-C28
 1.5 with sigma of 0.02
 C5-O6BA
 1.384 with sigma of 0.01
 C4-C5
 1.49 with sigma of 0.01
 C5-C7
 1.298 with sigma of 0.01
 C5-C6
 1.383 with sigma of 0.01
 C6-C7
 0.747 with sigma of 0.01
 C123-C125
 1.35 with sigma of 0.02
 C5-C8
 1.5 with sigma of 0.02
 C7-C8
 0.735 with sigma of 0.02
 C6-C8
 1.5 with sigma of 0.02
 O9-C135
 1.37 with sigma of 0.001
 C137-C139
 2.4 with sigma of 0.001
 C136-C138
 2.54 with sigma of 0.02
 C137-C138
 1.373 with sigma of 0.001
 C139-C138
 1.706 with sigma of 0.02
 C136-C139
 1.876 with sigma of 0.02
 C136-C137
 2 with sigma of 0.02
 C87-C88
 1.4 with sigma of 0.02
 C89-C87
 1.4 with sigma of 0.02
 Ti27-C135
 3.08 with sigma of 0.001
 C137-C135
 1.37 with sigma of 0.001
 C139-C135
 1.488 with sigma of 0.02
3. Rigid bond restraints
 O55, C81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C122)
\\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H5C(0.33) H5B(0.33) H5A(0.34) C6(0.33) H6A(0.33) H6B(0.33)
 H6C(0.33) C7(0.33) H7A(0.33) H7B(0.33) H7C(0.33) C8(0.34) H8A(0.34) H8B(0.34)
 H8C(0.34) H135(0.5) H13P(0.5) C136(0.5) H13Q(0.5) H13R(0.5) H13S(0.5)
 C137(0.5) H13T(0.5) H13U(0.5) H13V(0.5) C138(0.5) H13W(0.5) H13X(0.5)
 H13Y(0.5) C139(0.5) H13Z(0.5) H(0.5) HA(0.5)
6.a Ternary CH refined with riding coordinates:
 C0GA(H0GA), C1(H1), C1GA(H1GA), C5(H5C), C5(H5B), C5(H5A), C9(H9), C12(H12),
 C15(H15), C18(H18), C21(H21), C24(H24), C27(H27), C30(H30), C33(H33), C36(H36),
  C39(H39), C42(H42), C45(H45), C48(H48), C105(H105), C109(H109), C111(H111),
 C114(H114), C117(H117), C120(H120), C123(H123), C126(H126), C129(H129),
 C132(H132), C135(H135), C135(H13P), C140(H140), C143(H143), C146(H146),
 C149(H149), C152(H152), C155(H155), C158(H158), C51(H51), C54(H54), C57(H57),
 C60(H60), C63(H63), C66(H66), C69(H69), C72(H72), C75(H75), C78(H78), C81(H81),
  C84(H84), C87(H87), C90(H90), C93(H93), C96(H96), C99(H99), C102(H102)
6.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C6AA(H6AA,
 H6AB,H6AC), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C8BA(H8BA,H8BB,H8BC), C8CA(H8CA,
 H8CB,H8CC), C9AA(H9AA,H9AB,H9AC), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C25(H25A,H25B,H25C), 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), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C106(H10D,H10E,H10F), C107(H10G,H10H,H10I), C108(H10J,H10K,H10L),
 C110(H11D,H11E,H11F), C112(H11G,H11H,H11I), C113(H11J,H11K,H11L), C115(H11M,
 H11N,H11O), C116(H11P,H11Q,H11R), C118(H11S,H11T,H11U), C119(H11V,H11W,H11X),
 C121(H12A,H12B,H12C), C122(H12D,H12E,H12F), C124(H12G,H12H,H12I), C125(H12J,
 H12K,H12L), C127(H12M,H12N,H12O), C128(H12P,H12Q,H12R), C130(H13D,H13E,H13F),
 C131(H13G,H13H,H13I), C136(H13Q,H13R,H13S), C137(H13T,H13U,H13V), C138(H13W,
 H13X,H13Y), C139(H13Z,H,HA), C141(H14D,H14E,H14F), C142(H14G,H14H,H14I),
 C144(H14J,H14K,H14L), C145(H14M,H14N,H14O), C147(H14P,H14Q,H14R), C148(H14S,
 H14T,H14U), C150(H15A,H15B,H15C), C151(H15D,H15E,H15F), C153(H15G,H15H,H15I),
 C154(H15J,H15K,H15L), C156(H15M,H15N,H15O), C157(H15P,H15Q,H15R), C159(H15S,
 H15T,H15U), C160(H16D,H16E,H16F), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C61(H61A,H61B,H61C), 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), C83(H83A,H83B,H83C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C),
 C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C94(H94A,H94B,
 H94C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C),
 C100(H10M,H10N,H10O), C101(H10P,H10Q,H10R), C103(H10S,H10T,H10U), C104(H10V,
 H10W,H10X)
6.c Idealised Me refined as rotating group:
 C133(H13J,H13K,H13L), C134(H13M,H13N,H13O), C85(H85A,H85B,H85C)
;
_shelx_res_checksum              6054
_shelx_hkl_checksum              2338
_olex2_submission_special_instructions 'No special instructions were received'