Precisely Embedding Active Sites into a Mesoporous Zr-Framework through Linker Installation for High-Efficiency Photocatalysis.
Pang, Jiandong; Di, Zhengyi; Qin, Jun-Sheng; Yuan, Shuai; Lollar, Christina T.; Li, Jialuo; Zhang, Peng; Wu, Mingyan; Yuan, Daqiang; Hong, Maochun; Zhou, Hong-Cai; Journal of the American Chemical Society 142 (2020) 15020–15026; doi:10.1021/jacs.0c05758

data_4135203
_publ_section_title
;
 Precisely Embedding Active Sites into a Mesoporous Zr-Framework through
 Linker Installation for High-Efficiency Photocatalysis.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15020
_journal_page_last               15026
_journal_paper_doi               10.1021/jacs.0c05758
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C13.75 H8.5 O4.5 Zr0.75'
_chemical_formula_sum            'C14.25 H10 F1.5 O4.5 Zr0.75'
_chemical_formula_weight         350.14
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            24
_cell_length_a                   41.321(4)
_cell_length_b                   41.321
_cell_length_c                   19.208(2)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.0720
_cell_measurement_theta_min      2.6108
_cell_volume                     28402(4)
_computing_cell_refinement       'SAINT+ ver. (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'SAINT+ ver. (Bruker, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.38
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.923
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51030
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        66.240
_diffrn_reflns_theta_max         66.240
_diffrn_reflns_theta_min         2.138
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.574
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6163
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.682
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.000033(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         8479
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0797P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5184
_reflns_number_total             8479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c05758_si_003.cif
_cod_data_source_block           PCN-808-BPDC
_cod_depositor_comments
'Adding full bibliography for 4135202--4135205.cif.'
_cod_original_cell_volume        28403(6)
_cod_original_formula_sum        'C14.25 H10 F1.50 O4.50 Zr0.75'
_cod_database_code               4135203
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C14
 1.39 with sigma of 0.02
 C14-C14_$1
 1.39 with sigma of 0.02
 C13-C12
 1.39 with sigma of 0.02
 C12-C14_$1
 2.4 with sigma of 0.02
 C14-C12_$1
 2.4 with sigma of 0.02
 C13-C14
 2.4 with sigma of 0.02
 C12-C12_$1
 2.8 with sigma of 0.02
 C14-C13_$1
 2.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C15) = Uanis(O3) = Uanis(C8)
Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20)
4. Others
 Fixed Sof: H15A(0.5) H15B(0.5) H15C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C19(H19), C10(H10), C3(H3), C18(H18), C4(H4), C14(H14),
 C13(H13)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'