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_7121498
_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         'C92 H66 O52 S20 Zn12'
_chemical_formula_sum            'C92 H66 O52 S20 Zn12'
_chemical_formula_weight         3429.08
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-02-15
_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                 90.017(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.7128(4)
_cell_length_b                   10.8050(2)
_cell_length_c                   28.5974(5)
_cell_measurement_reflns_used    27286
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      2.28
_cell_measurement_theta_min      30.58
_cell_volume                     7327.1(2)
_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      103.15
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            69087
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.684
_diffrn_reflns_theta_min         2.071
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.974
_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            colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3428
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
'(replace by semicolon in column 1 when used as .sqf)'
_refine_diff_density_max         2.190
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 10455 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1597
_refine_ls_number_reflns         33785
_refine_ls_number_restraints     3450
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+31.2192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.858
_reflns_number_gt                30382
_reflns_number_total             33785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01837e2.cif
_cod_data_source_block           SEC-1
_cod_depositor_comments
'Adding full bibliography for 7121497--7121498.cif.'
_cod_database_code               7121498
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.505(2)
 0.495(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S8-C81 = S14-C82 = S18-C86 = S6-C90
 1.82 with sigma of 0.01
 S7-C81 \\sim S13-C82 \\sim S1-C83 \\sim S15-C84 \\sim S9-C85 \\sim S17-C86
\\sim S3-C87 \\sim S11-C88 ~
 S19-C89 \\sim S5-C90
 with sigma of 0.02
4. Restrained planarity
 C9, C11, C13, C14, C10, C12, S13
 with sigma of 0.1
 C49, C51, C53, C54, C50, C52
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.001 and
sigma for terminal atoms of 0.005
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
 Fixed U12: Zn12(0)
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), C76(H76), C74(H74), C78(H78)
8.b Idealised Me refined as rotating group:
 C83(H83a,H83b,H83c), C84(H84a,H84b,H84c), C85(H85a,H85b,H85c), C86(H86a,H86b,
 H86c), C87(H87a,H87b,H87c), C88(H88a,H88b,H88c), C89(H89a,H89b,H89c), C90(H90a,
 H90b,H90c), C91(H91a,H91b,H91c), C81(H81a,H81b,H81c), C82(H82a,H82b,H82c),
 C92(H92a,H92b,H92c)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_original_sample_id SEC-1
_olex2_submission_special_instructions 'No special instructions were received'