Cascade Covalent and Coordination Bonds Formation for Ti-Based Cage Assembly: Catalysis and Coordination Bi-functions of TiCl4
Tong, Jing; Xu, Tingting; Liu, Shengjun; Zhang, Junxiang; Hou, Xudong; Liu, Bo; Dalton Transactions  (2018) –; doi:10.1039/C7DT04367H

data_7045445
_publ_section_title
;
 Cascade Covalent and Coordination Bonds Formation for Ti-Based Cage
 Assembly: Catalysis and Coordination Bi-functions of TiCl4
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04367H
_journal_year                    2018
_chemical_formula_moiety         'C36 H32 Cl8 N4 O14 Ti4, 2(H4 O2)'
_chemical_formula_sum            'C36 H40 Cl8 N4 O18 Ti4'
_chemical_formula_weight         1291.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d'
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-10-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-20 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0920(19)
_cell_length_b                   18.0920(19)
_cell_length_c                   17.592(4)
_cell_measurement_reflns_used    3990
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      2.25
_cell_volume                     5758.2(16)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18898
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.251
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1430
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0739
_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^)+(0.1613P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                891
_reflns_number_total             1430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04367h2.cif
_cod_data_source_block           tj150315_3_0m
_cod_original_cell_volume        5758.2(17)
_cod_database_code               7045445
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C4_$1-C4_$2
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C3)=Sof(H3)=1-FVAR(1)
 Sof(C8)=Sof(H8)=FVAR(1)
 Sof(C4)=Sof(H4)=1-FVAR(2)
 Sof(C9)=Sof(H9)=FVAR(2)
 Fixed Sof: C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) O5(0.25) H5A(0.25) H5B(0.25)
 O4(0.25) H4A(0.25) H4B(0.25)
5.a Riding coordinates:
 O5(H5A,H5B), O4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C8(H8), C9(H9)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'