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_4348119
_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         'C69 H161 O55 Ti22, 2.67(I1.5)'
_chemical_formula_sum            'C69 H161 I4 O55 Ti22'
_chemical_formula_weight         3432.37
_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             2015-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.2087(7)
_cell_length_b                   17.5165(5)
_cell_length_c                   27.5141(7)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.49
_cell_volume                     13362.8(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            127068
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         0.734
_exptl_absorpt_coefficient_mu    2.231
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       block
_exptl_crystal_F_000             6844
_refine_diff_density_max         3.294
_refine_diff_density_min         -2.583
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1422
_refine_ls_number_reflns         30652
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0589P)^2^+73.4111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22459
_reflns_number_total             30652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00982_si_003.cif
_cod_data_source_block           p21n
_cod_database_code               4348119
_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
 C10-C11
 1.55 with sigma of 0.01
 C12-C10
 1.55 with sigma of 0.01
 C3-C8
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C73) \\sim Ueq, Uanis(I1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C71(0.5) H71(0.5) C70(0.5) H70A(0.5) H70B(0.5) H70C(0.5) C72(0.5)
 H72A(0.5) H72B(0.5) H72C(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5) H28A(0.5)
 H28(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C46(0.5) H46(0.5) H47D(0.5)
 H47E(0.5) H47F(0.5) H47A(0.5) H47B(0.5) H47C(0.5) H48D(0.5) H48E(0.5)
 H48F(0.5) H48A(0.5) H48B(0.5) H48C(0.5) H55(0.5) H55A(0.5) C56(0.5) H56A(0.5)
 H56B(0.5) H56C(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5)
5.a Ternary CH refined with riding coordinates:
 C71(H71), C1B(H1B), C4(H4), C7(H7), C8(H8), C10(H10), C16(H16), C19(H19),
 C22(H22), C25(H25), C28(H28A), C28(H28), C31(H31), C34(H34), C37(H37),
 C40(H40), C43(H43), C46(H46), C49(H49), C52(H52), C55(H55), C55(H55A),
 C58(H58), C62(H62), C64(H64), C67(H67)
5.b Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C9(H9A,H9B,
 H9C), C73(H73A,H73B,H73C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C),
 C47(H47D,H47E,H47F), C47(H47A,H47B,H47C), C48(H48D,H48E,H48F), C48(H48A,H48B,
 H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C69(H69A,
 H69B,H69C)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              92010
_shelx_hkl_checksum              60093
_olex2_submission_special_instructions 'No special instructions were received'