Generation of thiyl radicals in a zinc(ii) porous coordination polymer by light-induced post-synthetic deprotection.
Kusaka, Shinpei; Matsuda, Ryotaro; Kitagawa, Susumu; Chemical communications (Cambridge, England) 54 (2018) 4782–4785; doi:10.1039/c8cc01837e

data_7121497
_publ_section_title
;
 Generation of thiyl radicals in a zinc(ii) porous coordination polymer by
 light-induced post-synthetic deprotection.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4782
_journal_page_last               4785
_journal_paper_doi               10.1039/c8cc01837e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C86 H30 N2 O51 S13.88 Zn12'
_chemical_formula_sum            'C86 H30 N2 O52 S13.97 Zn12'
_chemical_formula_weight         3155.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 1'
_symmetry_space_group_name_Hall  'P 2y'
_symmetry_space_group_name_H-M   'P 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-02 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.096(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.5616(11)
_cell_length_b                   10.8170(4)
_cell_length_c                   28.5728(9)
_cell_measurement_reflns_used    10188
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.8780
_cell_measurement_theta_min      2.2220
_cell_volume                     7282.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Rigaku XtaLab P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52414
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.023
_diffrn_reflns_theta_min         1.869
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_standards_decay_%        0.5(1)
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             3119
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.778
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details
;
 Flack x determined using 4667 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1562
_refine_ls_number_reflns         27641
_refine_ls_number_restraints     3511
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.1032
_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^)+(0.1981P)^2^+9.4782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2637
_refine_ls_wR_factor_ref         0.3119
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.769
_reflns_number_gt                16519
_reflns_number_total             27641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01837e2.cif
_cod_data_source_block           SEC-2
_cod_depositor_comments
'Adding full bibliography for 7121497--7121498.cif.'
_cod_database_code               7121497
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.506(3)
 0.494(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 S3-S4A = S3-S4B = S3-S4C = S5-S6 = S19-S20A = S19-S20B = S7-S8A = S7-S8B =
 S13-S14A = S13-S14B = S9-S10A = S9-S10B
 2.06 with sigma of 0.02
 O46-C81
 1.21 with sigma of 0.02
 N1-C81
 1.34 with sigma of 0.02
 N1-C82 = N1-C83
 1.47 with sigma of 0.02
 O41-C84
 1.21 with sigma of 0.02
 N2-C84
 1.34 with sigma of 0.02
 N2-C85 = N2-C86
 1.47 with sigma of 0.02
 C9-C10 = C10-C11 = C11-C12 = C12-C13 = C13-C14 = C14-C9
 1.39 with sigma of 0.02
 C25-C26 = C26-C27 = C27-C28 = C28-C29 = C29-C30 = C30-C25
 1.39 with sigma of 0.02
 C41-C42 = C42-C43 = C43-C44 = C44-C45 = C45-C46 = C46-C41
 1.39 with sigma of 0.02
 C49-C50 = C50-C51 = C51-C52 = C52-C53 = C53-C54 = C54-C49
 1.39 with sigma of 0.02
 C65-C66 = C66-C67 = C67-C68 = C68-C69 = C69-C70 = C70-C65
 1.39 with sigma of 0.02
 C73-C74 = C74-C75 = C75-C76 = C76-C77 = C77-C78 = C78-C73
 1.39 with sigma of 0.02
 C1-C7 = C3-C8
 1.5 with sigma of 0.02
 C9-C15 = C11-C16
 1.5 with sigma of 0.02
 C17-C23 = C19-C24
 1.5 with sigma of 0.02
 C25-C31 = C27-C32
 1.5 with sigma of 0.02
 C33-C39 = C35-C40
 1.5 with sigma of 0.02
 C41-C47 = C43-C48
 1.5 with sigma of 0.02
 C49-C55 = C51-C56
 1.5 with sigma of 0.02
 C57-C63 = C59-C64
 1.5 with sigma of 0.02
 C65-C71 = C67-C72
 1.5 with sigma of 0.02
 C73-C79 = C75-C80
 1.5 with sigma of 0.02
 C77-S15
 1.82 with sigma of 0.02
 C13-S4A = C13-S4B = C13-S4C = C29-S6 = C37-S20A = C37-S20B = C45-S8A = C45-
 S8B = C53-S14A = C53-S14B = C69-S10A = C69-S10B
 3.02 with sigma of 0.04
 C82-C83
 2.5 with sigma of 0.04
 C85-C86
 2.5 with sigma of 0.04
 C9-C11 = C10-C12 = C11-C13 = C12-C14 = C13-C9 = C14-C10
 2.4 with sigma of 0.04
 C25-C27 = C26-C28 = C27-C29 = C28-C30 = C29-C25 = C30-C26
 2.4 with sigma of 0.04
 C41-C43 = C42-C44 = C43-C45 = C44-C46 = C45-C41 = C46-C42
 2.4 with sigma of 0.04
 C49-C51 = C50-C52 = C51-C53 = C52-C54 = C53-C49 = C54-C50
 2.4 with sigma of 0.04
 C65-C67 = C66-C68 = C67-C69 = C68-C70 = C69-C65 = C70-C66
 2.4 with sigma of 0.04
 C73-C75 = C74-C76 = C75-C77 = C76-C78 = C77-C73 = C78-C74
 2.4 with sigma of 0.04
4. Restrained planarity
 O46, N1, C81, C82, C83
 with sigma of 0.1
 O41, N2, C84, C85, C86
 with sigma of 0.1
 C1, C2, C3, C4, C5, C6
 with sigma of 0.1
 C9, C10, C11, C12, C13, C14
 with sigma of 0.1
 C17, C18, C19, C20, C21, C22
 with sigma of 0.1
 C25, C26, C27, C28, C29, C30
 with sigma of 0.1
 C33, C34, C35, C36, C37, C38
 with sigma of 0.1
 C41, C42, C43, C44, C45, C46
 with sigma of 0.1
 C49, C50, C51, C52, C53, C54, C55, C56
 with sigma of 0.1
 C57, C58, C59, C60, C61, C62
 with sigma of 0.1
 C65, C66, C67, C68, C69, C70
 with sigma of 0.1
 S15, C73, C74, C75, C76, C77, C78, C79
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.003 and
sigma for terminal atoms of 0.01
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
7. Others
 Sof(S8B)=1-FVAR(1)
 Sof(S8A)=FVAR(1)
 Fixed Sof: S4B(0.26896) S4A(0.27241) S20B(0.21058) S14B(0.31704) S4C(0.4981)
 S6(0.28514) S20A(0.28617) S14A(0.30681)
8.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14), C18(H18), C20(H20),
 C22(H22), C26(H26), C28(H28), C30(H30), C34(H34), C36(H36), C38(H38), C42(H42),
  C44(H44), C46(H46), C50(H50), C52(H52), C54(H54), C58(H58), C60(H60),
 C62(H62), C66(H66), C68(H68), C70(H70), C74(H74), C76(H76), C78(H78)
;
_olex2_submission_original_sample_id SEC-2
_olex2_submission_special_instructions 'No special instructions were received'