Monocarboxylate-driven structural growth in Calix[n]arene-polyoxotitanate hybrid systems: utility in hydrogen production from water.
Yang, Xin-Xue; Yu, Wei-Dong; Yi, Xiao-Yi; Li, Lei-Jiao; Liu, Chao; Chemical communications (Cambridge, England) 56 (2020) 14035–14038; doi:10.1039/d0cc05336h

data_7127732
_publ_section_title
;
 Monocarboxylate-driven structural growth in Calix[n]arene-polyoxotitanate
 hybrid systems: utility in hydrogen production from water.
;
_journal_issue                   90
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14035
_journal_page_last               14038
_journal_paper_doi               10.1039/d0cc05336h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C128 H164 O30 Ti6'
_chemical_formula_sum            'C128 H164 O30 Ti6'
_chemical_formula_weight         2469.98
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-10-06 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6540(7)
_cell_length_b                   15.3326(5)
_cell_length_c                   24.8024(11)
_cell_measurement_reflns_used    8406
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.791
_cell_measurement_theta_min      2.513
_cell_volume                     6453.6(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70838
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.416
_diffrn_reflns_theta_min         2.235
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6918
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         11864
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0575P)^2^+10.2771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7972
_reflns_number_total             11864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05336h2.cif
_cod_data_source_block           Ti6-3
_cod_database_code               7127732
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.785
_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
2. Restrained distances
 C10-C12 \\sim C10-C62 \\sim C10-C13 \\sim C10-C63 \\sim C10-C11 \\sim C10-C64
 with sigma of 0.01
 C65-C66 \\sim C65-C67 \\sim C65-C68 \\sim C65-C70 \\sim C65-C71 \\sim C65-C7
 with sigma of 0.01
 C59-C44 \\sim C59-C45 \\sim C59-C69
 with sigma of 0.01
 C1-C2 \\sim C1-C3 \\sim C4-C5 \\sim C4-C6
 with sigma of 0.01
3. Rigid bond restraints
 O6, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C65, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O6 \\sim C54: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
within 2A
C65 \\sim C7: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
within 2A
Uanis(C70) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=1-FVAR(1)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(1)
 Sof(C4)=Sof(H4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C1)=
 Sof(H1)=FVAR(2)
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 1-FVAR(3)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 FVAR(3)
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=1-FVAR(4)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C34(H34), C52(H52), C1(H1), C4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C36(H36A,H36B), C40(H40A,H40B), C43(H43A,H43B)
6.c Aromatic/amide H refined with riding coordinates:
 C60(H60), C61(H61), C18(H18), C19(H19), C27(H27), C29(H29), C38(H38),
 C41(H41), C48(H48), C49(H49), C50(H50), C54(H54), C55(H55), C57(H57)
6.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C69(H69A,H69B,H69C), C45(H45A,H45B,H45C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C35(H35A,H35B,H35C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C63(H63A,H63B,H63C), C62(H62A,H62B,H62C), C51(H51A,H51B,
 H51C), C53(H53A,H53B,H53C), C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C7(H7A,
 H7B,H7C), C71(H71A,H71B,H71C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C),
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C64(H64A,
 H64B,H64C)
;
_shelx_res_checksum              28262
_olex2_submission_special_instructions 'No special instructions were received'