Photo-induced free radical production in a tetraphenylethylene ligand-based metal-organic framework.
Xu, Kui; Yu, Bing; Li, Yuanyuan; Su, Huifang; Wang, Bingnan; Sun, Kai; Liu, Yuanyuan; Peng, Qiuchen; Hou, Hongwei; Li, Kai; Chemical communications (Cambridge, England) 54 (2018) 12942–12945; doi:10.1039/c8cc06662k

data_7122399
_publ_section_title
;
 Photo-induced free radical production in a tetraphenylethylene
 ligand-based metal-organic framework.
;
_journal_issue                   92
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12942
_journal_page_last               12945
_journal_paper_doi               10.1039/c8cc06662k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C68 H64 Cd2 N4 O12'
_chemical_formula_sum            'C68 H64 Cd2 N4 O12'
_chemical_formula_weight         1354.03
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc20cd71
_audit_creation_date             2018-07-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-25 deposited with the CCDC.
2018-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.86(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.222(8)
_cell_length_b                   10.281(4)
_cell_length_c                   36.345(18)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.29
_cell_volume                     6274(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            109752
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.627
_diffrn_reflns_theta_min         2.063
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1031 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.8967.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.205
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         14493
_refine_ls_number_restraints     1683
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0857
_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^)+(0.0541P)^2^+47.5237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11426
_reflns_number_total             14493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06662k4.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7122399.cif.'
_cod_database_code               7122399
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.910
_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
 C24-C31
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C17, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C24, C31
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C5' \\sim C6 \\sim C7 \\sim C8
\\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16
\\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24
\\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32
\\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40
\\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48
\\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56
\\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64
\\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim N1 \\sim N2 \\sim N3 \\sim N4:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C5(0.5) H5a(0.5) H5b(0.5) H5c(0.5) C5'(0.5) H5'a(0.5) H5'b(0.5)
 H5'c(0.5)
6.a Me refined with riding coordinates:
 C2(H2a,H2b,H2c), C5(H5a,H5b,H5c), C5'(H5'a,H5'b,H5'c), C6(H6a,H6b,H6c),
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C15(H15), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C43(H43),
 C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
 C65(H65), C67(H67)
6.c Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,C22,C23), C25(C26,C27,C28,C29,C30), C31(C32,C33,C34,C35,C36)
6.d Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c)
;
_shelx_res_checksum              17405
_olex2_submission_special_instructions 'No special instructions were received'