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_4135202
_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         '0.33(C288 H156 O108 Zr18)'
_chemical_formula_sum            'C96 H52 O36 Zr6'
_chemical_formula_weight         2328.69
_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
_audit_creation_date             2018-09-26
_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            3
_cell_length_a                   40.5456(7)
_cell_length_b                   40.546
_cell_length_c                   19.6333(4)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.1845
_cell_measurement_theta_min      2.5784
_cell_volume                     27952.2(7)
_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      99.98
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            72653
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        62.360
_diffrn_reflns_theta_max         62.360
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  0.7521
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1024 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.7831.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         8210
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5837
_reflns_number_total             8210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c05758_si_003.cif
_cod_data_source_block           PCN-808
_cod_depositor_comments
'Adding full bibliography for 4135202--4135205.cif.'
_cod_original_cell_volume        27951.9(11)
_cod_database_code               4135202
_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
 C14_$1-C13 = C15_$1-C13 = C14_$1-C14_$2
 1.4 with sigma of 0.005
 C15_$1-C13
 1.4 with sigma of 0.005
 C15-C15_$3 \\sim C15_$1-C15_$2 \\sim C14_$1-C14_$2 \\sim C14-C14_$3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C8)
4. Others
 Fixed Sof: H0AB(0.5) H0AC(0.5) C15(0.5) C14(0.5)
5.a Me refined with everything fixed:
 C0AA(H0AA,H0AB,H0AC)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C10(H10), C4(H4)
;
_shelx_res_checksum              14802
_shelx_hkl_checksum              65035
_shelx_fab_checksum              22969
_olex2_submission_special_instructions 'No special instructions were received'