Calix[8]arene-constructed stable polyoxo-titanium clusters for efficient CO2 photoreduction
Li, Ning; Liu, Jing-Jing; Sun, Jia-Wei; Dong, Bao-Xia; Dong, Long-Zhang; Yao, Su-Juan; Xin, Zhifeng; Li, Shun-Li; Lan, Ya-Qian; Green Chemistry 22 (2020) 5325–5332; doi:10.1039/D0GC01497D

data_7240907
_publ_section_title
;
 Calix[8]arene-constructed stable polyoxo-titanium clusters for efficient
 CO2 photoreduction
;
_journal_issue                   16
_journal_name_full               'Green Chemistry'
_journal_page_first              5325
_journal_page_last               5332
_journal_paper_doi               10.1039/D0GC01497D
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C68 H76 O24 Ti7'
_chemical_formula_sum            'C68 H76 O24 Ti7'
_chemical_formula_weight         1612.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-14
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-04-25 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.63(3)
_cell_length_b                   19.10(3)
_cell_length_c                   14.90(2)
_cell_measurement_reflns_used    409
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.890
_cell_measurement_theta_min      2.699
_cell_volume                     7009(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.533
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0871 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.7216.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.52(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6208
_refine_ls_number_restraints     267
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1629
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0656P)^2^+40.2284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                3635
_reflns_number_total             6208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0gc01497d2.cif
_cod_data_source_block           mo_4hao_0ma
_cod_depositor_comments
;Adding full bibliography for 7240906--7240907.cif.

 Adding full bibliography for 7240906--7240907.cif.
;
_cod_original_cell_volume        7008(17)
_cod_database_code               7240907
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48(8)
 0.52(8)
2. 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
3. Rigid bond restraints
 O12, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O10, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C30 \\sim C20 \\sim C22 \\sim C31 \\sim C10 \\sim C29 \\sim C27 \\sim C28 \\sim
C7 \\sim C15 \\sim C17 \\sim C1 \\sim C8 \\sim C23 \\sim C9 \\sim C6 \\sim C16
\\sim C14 \\sim C37 \\sim C11 \\sim C13 \\sim C38 \\sim C21 \\sim C19 \\sim C24
\\sim C26 \\sim C2 \\sim C33 \\sim C18 \\sim C4 \\sim C25 \\sim C32 \\sim C3
\\sim C12 \\sim C5 \\sim C34 \\sim C36 \\sim O7 \\sim O6 \\sim O5 \\sim O11
\\sim O4 \\sim O12 \\sim O1 \\sim O14 \\sim O13 \\sim O10 \\sim O3 \\sim O8
\\sim O2 \\sim O9: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
5. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C29(H29A,H29B), C15(H15A,H15B), C1(H1A,H1B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C17(H17), C11(H11), C19(H19), C24(H24), C26(H26), C18(H18), C4(H4),
 C25(H25), C3(H3), C12(H12), C5(H5)
6.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              81250
_olex2_submission_special_instructions 'No special instructions were received'