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_7127728
_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         'C137 H169 O26 Ti6'
_chemical_formula_sum            'C137 H169 O26 Ti6'
_chemical_formula_weight         2519.11
_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
_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                 105.645(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.124(2)
_cell_length_b                   15.607(2)
_cell_length_c                   25.066(3)
_cell_measurement_reflns_used    2308
_cell_measurement_temperature    150
_cell_measurement_theta_max      19.910
_cell_measurement_theta_min      3.221
_cell_volume                     6827.5(14)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'olex2.solve 1.3 (Bourhis et al., 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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.1645
_diffrn_reflns_av_unetI/netI     0.1921
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35931
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.749
_diffrn_reflns_theta_max         24.749
_diffrn_reflns_theta_min         2.610
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0609 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.8873.
The \l/2 correction factor is 0.0015.
;
_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    1.225
_exptl_crystal_description       prism
_exptl_crystal_F_000             2662
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         11617
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.2189
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4641
_reflns_number_total             11617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05336h2.cif
_cod_data_source_block           Ti6-1
_cod_original_cell_volume        6827.4(15)
_cod_database_code               7127728
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.825
_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
 C80-C78
 1.45 with sigma of 0.01
 C21-C22 \\sim C21-C23 \\sim C21-C24 \\sim C21-C25 \\sim C21-C26 \\sim C21-C27
 with sigma of 0.01
 C35-C36 \\sim C35-C37 \\sim C35-C38 \\sim C35-C39 \\sim C35-C40 \\sim C35-C41
 with sigma of 0.01
 C13-C7 \\sim C13-C8 \\sim C13-C9 \\sim C13-C10 \\sim C13-C11 \\sim C13-C12
 with sigma of 0.01
 C53-C54 \\sim C53-C55 \\sim C53-C56
 with sigma of 0.01
 C57-C76 \\sim C57-C75
 with sigma of 0.01
3. Rigid bond restraints
 C13, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C78, C79
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C11, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C13 \\sim C7: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C78 \\sim C79: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C11 \\sim C13: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C27) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C79) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(2)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(3)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(3)
 Fixed Sof: C79(0.25) H79A(0.25) H79B(0.25) H79C(0.25) C80(0.25) H80A(0.25)
 H80B(0.25) H80C(0.25)
6.a Ternary CH refined with riding coordinates:
 C50(H50), C57(H57), C72(H72)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C28(H28A,H28B), C42(H42A,H42B), C46(H46A,H46B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18(H18), C20(H20), C30(H30), C32(H32), C47(H47), C49(H49),
 C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C67(H67), C68(H68), C69(H69),
  C70(H70), C71(H71)
6.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C74(H74A,H74B,H74C), C79(H79A,H79B,H79C), C80(H80A,
 H80B,H80C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C7(H7A,
 H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C),
 C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C76(H76A,
 H76B,H76C), C75(H75A,H75B,H75C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              59728
_olex2_submission_special_instructions 'No special instructions were received'