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_4348120
_publ_section_title
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 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         'C99 H209 I O68 Ti22, I3.05, C3 H8 O'
_chemical_formula_sum            'C102 H217 I4.05 O69 Ti22'
_chemical_formula_weight         4115.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.403(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3241(10)
_cell_length_b                   30.6429(18)
_cell_length_c                   30.9343(18)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      24.361
_cell_measurement_theta_min      2.478
_cell_volume                     17292.5(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 0.894
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            123191
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.937
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             8319
_refine_diff_density_max         1.506
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1839
_refine_ls_number_reflns         30396
_refine_ls_number_restraints     483
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0636P)^2^+181.3154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.2320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17601
_reflns_number_total             30396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00982_si_005.cif
_cod_data_source_block           p
_cod_database_code               4348120
_shelxl_version_number           2013-4
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 C98-C96
 1.55 with sigma of 0.01
 C93-C92
 2.35 with sigma of 0.01
 C92-C94
 2.35 with sigma of 0.01
 C93-C94
 2.35 with sigma of 0.01
 C37-C39
 1.55 with sigma of 0.01
 C38-C37
 1.55 with sigma of 0.01
 C21-C20
 2.35 with sigma of 0.01
 C19-C21
 1.55 with sigma of 0.01
 C18-C16
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20 \\sim C21 \\sim O40: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.08
C7 \\sim C9 \\sim O38: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.08
I1AA \\sim I2AA \\sim I3 \\sim I3AA \\sim I4 \\sim I4AA: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: I1AA(0.57) I2(0.26) I2AA(0.33) I3(0.28) I3AA(0.27) I4(0.23)
 I4AA(0.35) I5(0.4) I6(0.28) I7(0.08)
5.a Rotating group:
 O1(H1A,H1B)
5.b 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), C100(H100)
5.c Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 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), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C82(H82A,H82B,H82C), C83(H83A,
 H83B,H83C), C84(H84A,H84B,H84C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C),
 C89(H89A,H89B,H89C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,
 H94C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C),
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F)
5.d Idealised tetrahedral OH refined as rotating group:
 O33(H33)
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_olex2_submission_special_instructions 'No special instructions were received'