Counteranion-Stabilized Titanium(IV) Isopolyoxocationic Clusters Isolated from Water.
Zhang, Guanyun; Hou, Jie; Li, Mingzhong; Tung, Chen-Ho; Wang, Yifeng; Inorganic chemistry 55 (2016) 4704–4709; doi:10.1021/acs.inorgchem.5b01901

data_4346657
_publ_section_title
;
 Counteranion-Stabilized Titanium(IV) Isopolyoxocationic Clusters Isolated
 from Water.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4704
_journal_page_last               4709
_journal_paper_doi               10.1021/acs.inorgchem.5b01901
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '6(C16 H36 N), H40 O28 Ti6, 14(Br), 4(O)'
_chemical_formula_sum            'C96 H256 Br14 N6 O32 Ti6'
_chemical_formula_weight         3413.19
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.072(2)
_cell_length_b                   24.072(2)
_cell_length_c                   54.827(10)
_cell_measurement_reflns_used    8185
_cell_measurement_temperature    173
_cell_volume                     31770(7)
_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
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1301
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            76625
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.506
_exptl_absorpt_coefficient_mu    3.867
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       cube
_exptl_crystal_F_000             14016
_refine_diff_density_max         1.749
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 3205 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.017(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         13990
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0682P)^2^+90.8765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.599
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8965
_reflns_number_total             13990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01901_si_003.cif
_cod_data_source_block           iba2
_cod_original_cell_volume        31770(8)
_cod_database_code               4346657
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C24-C23
 1.55 with sigma of 0.01
 C25-C23
 1.55 with sigma of 0.01
 C44-C45
 1.55 with sigma of 0.01
 C44-C43
 1.55 with sigma of 0.01
 C46-N4
 1.55 with sigma of 0.01
 C47-C46
 1.55 with sigma of 0.01
 C48-C47
 1.55 with sigma of 0.01
 C43-C42
 1.55 with sigma of 0.01
 C8-C7
 1.55 with sigma of 0.01
 C48-C49
 1.55 with sigma of 0.01
 C47-C49
 2.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N4 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48:
within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.08
C6 \\sim C7 \\sim C8: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.08
C8 \\sim C7 \\sim C6: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 C41, C40, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.01
 C8, C7, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C43
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C24(0.5) H24a(0.5) H24b(0.5) H24c(0.5) C25(0.5) H25a(0.5)
 H25b(0.5) H25c(0.5)
6.a Riding coordinates:
 C23(H23a,H23b), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c)
6.b Rotating group:
 O1(H1d,H1e), O2(H2c,H2d), O4(H4c,H4d), O5(H5c,H5d), O6(H6c,H6d), O8(H8d,H8e),
 O9(H9d,H9e), O11(H11c,H11d), O12(H12c,H12d), O13(H13c,H13d)
6.c Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C11(H11a,H11b), C12(H12a,H12b), C13(H13a,H13b), C14(H14a,
 H14b), C15(H15a,H15b), C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b),
 C21(H21a,H21b), C22(H22a,H22b), C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b),
  C30(H30a,H30b), C31(H31a,H31b), C32(H32a,H32b), C34(H34a,H34b), C35(H35a,
 H35b), C36(H36a,H36b), C38(H38a,H38b), C39(H39a,H39b), C40(H40a,H40b), C2(H2a,
 H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b), C7(H7a,H7b),
 C43(H43a,H43b), C44(H44a,H44b), C45(H45a,H45b), C46(H46a,H46b), C47(H47a,H47b),
  C48(H48a,H48b)
6.d Me refined with riding coordinates:
 C8(H8a,H8b,H8c), C42(H42a,H42b,H42c), C49(H49a,H49b,H49c)
6.e Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C26(H26a,H26b,
 H26c), C33(H33a,H33b,H33c), C37(H37a,H37b,H37c), C41(H41a,H41b,H41c), C1(H1a,
 H1b,H1c)
;
_shelx_res_checksum              35581
_shelx_hkl_checksum              51050
_olex2_submission_special_instructions 'No special instructions were received'