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_4348117
_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         '2(C88 H180 O56 Ti22), 2.67(I3)'
_chemical_formula_sum            'C176 H360 I8 O112 Ti44'
_chemical_formula_weight         7391.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                95.039(4)
_cell_angle_beta                 90.200(4)
_cell_angle_gamma                107.814(4)
_cell_formula_units_Z            2
_cell_length_a                   19.322(7)
_cell_length_b                   26.242(10)
_cell_length_c                   31.425(12)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.21
_cell_volume                     15104(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.969
_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  0.1132
_diffrn_reflns_av_unetI/netI     0.1688
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            197173
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.654
_diffrn_reflns_theta_min         2.187
_exptl_absorpt_coefficient_mu    1.981
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             7408
_refine_diff_density_max         5.017
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2826
_refine_ls_number_reflns         68308
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.2647
_refine_ls_R_factor_gt           0.1486
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1297P)^2^+425.9334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3372
_refine_ls_wR_factor_ref         0.4092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31634
_reflns_number_total             68308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00982_si_004.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        15103(10)
_cod_database_code               4348117
_shelxl_version_number           2013-4
_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
 C58-C60
 1.5 with sigma of 0.02
 C58-C57
 1.5 with sigma of 0.02
 C60-C57
 2.4 with sigma of 0.02
 C112-C114
 1.5 with sigma of 0.02
 C114-C116
 1.5 with sigma of 0.02
 C112-C116
 2.4 with sigma of 0.02
 C117-C115
 1.5 with sigma of 0.02
 C117-C118
 1.5 with sigma of 0.02
 C121-C120
 1.5 with sigma of 0.02
 C109-C120
 1.5 with sigma of 0.02
 C159-C160
 1.5 with sigma of 0.02
 C159-C161
 1.5 with sigma of 0.02
 C97-C96
 1.5 with sigma of 0.02
 C72-C71
 1.5 with sigma of 0.02
 C72-C69
 1.5 with sigma of 0.02
 C157-C155
 1.5 with sigma of 0.02
 C97-C98
 1.5 with sigma of 0.02
 C103-C105
 1.5 with sigma of 0.02
 C126-C130
 1.5 with sigma of 0.02
 O44-C96
 2.4 with sigma of 0.02
 O44-C98
 2.4 with sigma of 0.02
 C123-C124
 1.5 with sigma of 0.02
 C120-O50
 1.5 with sigma of 0.02
 C77-C78
 1.5 with sigma of 0.02
 C123-C124
 1.5 with sigma of 0.02
 C93-C92
 1.5 with sigma of 0.02
 C93-C94
 1.5 with sigma of 0.02
 C107-C105
 1.5 with sigma of 0.02
 C103-O52
 2.35 with sigma of 0.02
 C107-C103
 2.35 with sigma of 0.02
 C103-C105
 1.5 with sigma of 0.02
 C107-C105
 1.5 with sigma of 0.02
 C107-C103
 2.35 with sigma of 0.02
 C94-C92
 2.35 with sigma of 0.02
 C95-C92
 1.5 with sigma of 0.02
 C93-C92
 1.5 with sigma of 0.02
 C93-C94
 1.5 with sigma of 0.02
 C95-C94
 1.5 with sigma of 0.02
 C95-C92
 1.5 with sigma of 0.02
 C94-C92
 2.35 with sigma of 0.02
 C95-C93
 1.1 with sigma of 0.02
 C73-O108
 1.356 with sigma of 0.02
 C73-C70
 1.562 with sigma of 0.02
 C73-C75
 1.2 with sigma of 0.01
 C73-C75
 1.3 with sigma of 0.01
 O108-C70
 2.4 with sigma of 0.01
 C75-O108
 2.2 with sigma of 0.01
3. Rigid bond restraints
 C153, C156
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C176, C178
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C155, C158
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C15, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C114, C116
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C103 \\sim C105 \\sim C107: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.08
Uanis(O89) \\sim Ueq, Uanis(C158) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C116)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C173) \\sim Ueq, Uanis(C122) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: H58(0.33333) H58A(0.66667) C59(0.66667) H59A(0.66667)
 H59B(0.66667) H59C(0.66667) C60(0.33333) H60A(0.33333) H60B(0.33333)
 H60C(0.33333) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C71(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) H72(0.5) H72A(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5)
 C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5) H92A(0.5) H92B(0.5) H92C(0.5) H92D(0.5)
 H92E(0.5) H92F(0.5) C93(0.5) H93(0.5) H94A(0.5) H94B(0.5) H94C(0.5) H94D(0.5)
 H94E(0.5) H94F(0.5) C95(0.5) H95(0.5) C112(0.5) H11D(0.5) H11E(0.5) H11F(0.5)
 C113(0.5) H11G(0.5) H11H(0.5) H11I(0.5) H114(0.5) H11J(0.5) I3(0.75)
 I4(0.33333) I5(0.75) I6(0.33333) I7(0.5) I8(0.33333)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C15(H15), C19(H19), C24(H24), C28(H28), C30(H30), C37(H37), C40(H40),
 C46(H46), C58(H58), C58(H58A), C61(H61), C65(H65), C67(H67), C72(H72),
 C72(H72A), C73(H73), C77(H77), C81(H81), C84(H84), C86(H86), C89(H89),
 C93(H93), C95(H95), C97(H97), C100(H100), C102(H102), C105(H105), C110(H110),
 C114(H114), C114(H11J), C117(H117), C120(H120), C123(H123), C127(H127),
 C129(H129), C130(H130), C148(H148), C150(H150), C153(H153), C155(H155),
 C159(H159), C176(H176), C179(H179)
6.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,
 H7B,H7C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,
 H85B,H85C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C92(H92D,H92E,H92F), C94(H94A,H94B,
 H94C), C94(H94D,H94E,H94F), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C99(H99A,
 H99B,H99C), C101(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L),
 C106(H10M,H10N,H10O), C107(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C109(H10V,
 H10W,H10X), C111(H11A,H11B,H11C), C113(H11G,H11H,H11I), C115(H11K,H11L,H11M),
 C116(H11N,H11O,H11P), C118(H11Q,H11R,H11S), C119(H11T,H11U,H11V), C121(H12A,
 H12B,H12C), C122(H12D,H12E,H12F), C124(H12G,H12H,H12I), C125(H12J,H12K,H12L),
 C126(H12M,H12N,H12O), C128(H12P,H12Q,H12R), C131(H13A,H13B,H13C), C132(H13D,
 H13E,H13F), C135(H13G,H13H,H13I), C138(H13J,H13K,H13L), C139(H13M,H13N,H13O),
 C144(H14D,H14E,H14F), C145(H14G,H14H,H14I), C146(H14J,H14K,H14L), C147(H14M,
 H14N,H14O), C149(H14P,H14Q,H14R), C151(H15A,H15B,H15C), C152(H15D,H15E,H15F),
 C154(H15G,H15H,H15I), C156(H15J,H15K,H15L), C157(H15M,H15N,H15O), C158(H15P,
 H15Q,H15R), C160(H16D,H16E,H16F), C161(H16G,H16H,H16I), C165(H16J,H16K,H16L),
 C167(H16M,H16N,H16O), C169(H16P,H16Q,H16R), C173(H17A,H17B,H17C), C174(H17D,
 H17E,H17F), C175(H17G,H17H,H17I), C177(H17J,H17K,H17L), C178(H17M,H17N,H17O),
 C180(H18A,H18B,H18C), C181(H18D,H18E,H18F)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C18(H18), C35(H35), C53(H53), C140(H140), C142(H142), C168(H168),
 C170(H170)
6.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C50(H50A,H50B,H50C), C112(H11D,H11E,H11F)
;
_shelx_res_checksum              72468
_shelx_hkl_checksum              26394
_olex2_submission_special_instructions 'No special instructions were received'