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_7127725
_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         'C106 H146 O20 Ti4'
_chemical_formula_sum            'C106 H146 O20 Ti4'
_chemical_formula_weight         1931.82
_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
_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                 93.955(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6214(11)
_cell_length_b                   28.2561(17)
_cell_length_c                   14.3350(9)
_cell_measurement_reflns_used    2856
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.56
_cell_measurement_theta_min      1.85
_cell_volume                     5908.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.26a (Rigaku OD, 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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -18.00  11.00   0.50   30.00    --    5.62  80.00  24.00   58
  2  \w     19.00  47.00   0.50   30.00    --    5.62  80.00  24.00   56
  3  \w    -56.00  20.00   0.50   30.00    --    5.62 -19.00 -60.00  152
  4  \w     13.00  39.00   0.50   30.00    --    5.62 -99.00-150.00   52
  5  \w     -8.00  35.00   0.50   30.00    --    5.62 -99.00-180.00   86
  6  \w    -22.00  15.00   0.50   30.00    --   -6.01 -99.00-150.00   74
  7  \w    -22.00  16.00   0.50   30.00    --   -6.01 -99.00 -30.00   76
  8  \w    -21.00  26.00   0.50   30.00    --    5.62 -99.00  30.00   94
  9  \w    -11.00  34.00   0.50   30.00    --    5.62 -99.00 120.00   90
 10  \w    -23.00   8.00   0.50   30.00    --   -6.01 -99.00  90.00   62
 11  \w    -66.00  31.00   0.50   30.00    --    5.62 -80.00 -99.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0240960000
_diffrn_orient_matrix_UB_12      0.0173648000
_diffrn_orient_matrix_UB_13      -0.0243184000
_diffrn_orient_matrix_UB_21      0.0413981000
_diffrn_orient_matrix_UB_22      -0.0127553000
_diffrn_orient_matrix_UB_23      0.0095119000
_diffrn_orient_matrix_UB_31      -0.0084512000
_diffrn_orient_matrix_UB_32      -0.0128977000
_diffrn_orient_matrix_UB_33      -0.0421280000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3476
_diffrn_reflns_av_unetI/netI     0.1479
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            74449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.498
_diffrn_reflns_theta_max         24.498
_diffrn_reflns_theta_min         2.007
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  1.2
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         9802
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1839
_refine_ls_R_factor_gt           0.1038
_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^)+(0.1167P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2251
_refine_ls_wR_factor_ref         0.2580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4971
_reflns_number_total             9802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05336h2.cif
_cod_data_source_block           Ti4-2
_cod_database_code               7127725
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C83 H83 O83 N83 Ti83 '
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.857
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C38-C40
 1.6 with sigma of 0.1
 C38-C7
 1.6 with sigma of 0.1
 C38-C41
 1.6 with sigma of 0.1
 C38-C39 \\sim C38-C41 \\sim C38-C26 \\sim C38-C40 \\sim C38-C6 \\sim C38-C7
 with sigma of 0.01
 C28-C29 \\sim C28-C27 \\sim C28-C5
 with sigma of 0.01
 C50-C53 \\sim C50-C51 \\sim C50-C52
 with sigma of 0.01
 C1-C2 \\sim C1-C3 \\sim C1-C4
 with sigma of 0.01
3. Rigid bond restraints
 C38, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C42(H42A,H42B), C45(H45A,H45B), C30(H30A,H30B)
6.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C36(H36), C34(H34), C8(H8), C47(H47), C24(H24), C17(H17), C49(H49)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C51(H51A,H51B,H51C), C29(H29A,H29B,H29C), C18(H18A,H18B,
 H18C), C12(H12A,H12B,H12C), C52(H52A,H52B,H52C), C27(H27A,H27B,H27C), C4(H4A,
 H4B,H4C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C3(H3A,H3B,H3C), C31(H31A,H31B,H31C), C13(H13A,
 H13B,H13C), C26(H26A,H26B,H26C), C6(H6A,H6B,H6C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C7(H7A,H7B,H7C), C41(H41A,H41B,H41C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49628
_shelx_fab_checksum              37939
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.676
_oxdiff_exptl_absorpt_empirical_full_min 0.379