A π-conjugated covalent organic framework enables interlocked nickel/photoredox catalysis for light-harvesting cross-coupling reactions.
Jati, Ayan; Dam, Suranjana; Kumar, Shekhar; Kumar, Kundan; Maji, Biplab; Chemical science 14 (2023) 8624–8634; doi:10.1039/d3sc02440g

data_1569558
_publ_section_title
;
 A &#x3c0;-conjugated covalent organic framework enables interlocked
 nickel/photoredox catalysis for light-harvesting cross-coupling
 reactions.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              8624
_journal_page_last               8634
_journal_paper_doi               10.1039/d3sc02440g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C18 H22 O S'
_chemical_formula_sum            'C18 H22 O S'
_chemical_formula_weight         286.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-11-01 deposited with the CCDC.	2023-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                69.336(2)
_cell_angle_beta                 76.155(2)
_cell_angle_gamma                85.5380(10)
_cell_formula_units_Z            2
_cell_length_a                   6.46020(10)
_cell_length_b                   10.5870(2)
_cell_length_c                   11.9686(3)
_cell_measurement_reflns_used    8063
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.9940
_cell_measurement_theta_min      4.0330
_cell_volume                     743.65(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     17.00 108.00   0.50    0.20    --   40.33  64.00   0.00  182
  2  \w     17.00 108.00   0.50    0.20    --   40.33  64.00 -60.00  182
  3  \w     14.00 109.00   0.50    0.20    --   40.33  77.00-150.00  190
  4  \w     21.00 107.00   0.50    0.20    --   40.33  50.00-150.00  172
  5  \w     99.00 164.00   0.50    0.28    --   96.67 117.00 -60.00  130
  6  \w     70.00 158.00   0.50    0.28    --   96.67 161.00  22.00  176
  7  \w     99.00 163.00   0.50    0.28    --   96.67 118.00-129.00  128
  8  \w     81.00 164.00   0.50    0.28    --   96.67 145.00-180.00  166
  9  \w     99.00 164.00   0.50    0.28    --   96.67 117.00-150.00  130
 10  \w     83.00 164.00   0.50    0.28    --   96.67  33.00 -90.00  162
 11  \w     80.00 163.00   0.50    0.28    --   96.67  42.00 -60.00  166
 12  \w     70.00 165.00   0.50    0.28    --   96.67  77.00 150.00  190
 13  \w     83.00 164.00   0.50    0.28    --   96.67  33.00 150.00  162
 14  \w     70.00 165.00   0.50    0.28    --   96.67  77.00  30.00  190
 15  \w     80.00 163.00   0.50    0.28    --   96.67  42.00  30.00  166
 16  \w     83.00 164.00   0.50    0.28    --   96.67  33.00   0.00  162
 17  \w     28.00 105.00   0.50    0.28    --   96.67 -77.00  30.00  154
 18  \w     30.00  57.00   0.50    0.28    --   96.67 -50.00  90.00   54
 19  \w     28.00 105.00   0.50    0.28    --   96.67 -77.00 120.00  154
 20  \w     30.00  57.00   0.50    0.28    --   96.67 -50.00 150.00   54
 21  \w     29.00  83.00   0.50    0.28    --   96.67 -68.00   0.00  108
 22  \w     30.00  57.00   0.50    0.28    --   96.67 -50.00 120.00   54
 23  \w     28.00 105.00   0.50    0.28    --   96.67 -77.00 -60.00  154
 24  \w     30.00  57.00   0.50    0.28    --   96.67 -50.00-180.00   54
 25  \w     30.00  57.00   0.50    0.28    --   96.67 -50.00-150.00   54
 26  \w     30.00  57.00   0.50    0.28    --   96.67 -50.00 -60.00   54
 27  \w    -30.00  31.00   0.50    0.20    --   40.33 -25.00 150.00  122
 28  \w    -26.00  43.00   0.50    0.20    --   40.33 -38.00  60.00  138
 29  \w     18.00  79.00   0.50    0.20    --   40.33-104.00 -30.00  122
 30  \w     52.00 113.00   0.50    0.20    --   40.33-161.00  -7.00  122
 31  \w     30.00 109.00   0.50    0.28    --   96.67-117.00 -30.00  158
 32  \w     30.00 109.00   0.50    0.28    --   96.67-117.00-120.00  158
 33  \w     52.00 136.00   0.50    0.28    --   96.67-161.00  -7.00  168
 34  \w     22.00 106.00   0.50    0.28    --   96.67 -96.00-120.00  168
 35  \w     30.00 109.00   0.50    0.28    --   96.67-117.00  30.00  158
 36  \w     30.00 110.00   0.50    0.28    --   96.67-118.00 144.00  160
 37  \w     29.00  87.00   0.50    0.20    --   40.33-118.00 144.00  116
 38  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 150.00  192
 39  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 120.00  192
 40  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00  60.00  192
 41  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00  90.00  182
 42  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00   0.00  182
 43  \w   -107.00 -21.00   0.50    0.20    --  -40.33 -50.00  90.00  172
 44  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 -30.00  192
 45  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 -90.00  192
 46  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00-150.00  192
 47  \w   -150.00 -58.00   0.50    0.28    --  -82.50 -68.00-120.00  184
 48  \w   -150.00 -69.00   0.50    0.28    --  -82.50 -33.00-180.00  162
 49  \w   -142.00 -49.00   0.50    0.28    --  -82.50-161.00  -7.00  186
 50  \w   -109.00 -49.00   0.50    0.20    --  -40.33-161.00  -7.00  120
 51  \w   -149.00 -77.00   0.50    0.28    --  -82.50-118.00 144.00  144
 52  \w   -150.00 -69.00   0.50    0.28    --  -82.50 -33.00  90.00  162
 53  \w    -47.00 -15.00   0.50    0.28    --  -82.50  42.00   0.00   64
 54  \w    -57.00 -16.00   0.50    0.28    --  -82.50  50.00-120.00   82
 55  \w    -57.00 -16.00   0.50    0.28    --  -82.50  50.00 -30.00   82
 56  \w    -47.00 -15.00   0.50    0.28    --  -82.50  42.00  90.00   64
 57  \w    -47.00 -15.00   0.50    0.28    --  -82.50  42.00 120.00   64
 58  \w    -57.00  26.00   0.50    0.20    --  -40.33  50.00  30.00  166
 59  \w    -24.00  35.00   0.50    0.20    --  -40.33  12.00  60.00  118
 60  \w    -31.00  30.00   0.50    0.20    --  -40.33  25.00 -60.00  122
 61  \w    -31.00  30.00   0.50    0.20    --  -40.33  25.00-180.00  122
 62  \w    -84.00  -7.00   0.50    0.20    --  -40.33 118.00-129.00  154
 63  \w    -85.00 -16.00   0.50    0.28    --  -82.50 118.00-129.00  138
 64  \w   -111.00 -30.00   0.50    0.20    --  -40.33 161.00  22.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12139
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.333
_diffrn_reflns_theta_min         4.053
_exptl_absorpt_coefficient_mu    1.857
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       plate
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0523P)^2^+0.0967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2439
_reflns_number_total             2656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02440g2.cif
_cod_data_source_block           ayj-adash_1
_cod_depositor_comments
'Adding full bibliography for 1569557--1569560.cif.'
_cod_database_code               1569558
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.808
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C13(H13), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C10(H10A,H10B), C18(H18A,H18B), C16(H16A,H16B), C12(H12A,
 H12B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C8(H8), C7(H7)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;