Sulfone-containing covalent organic frameworks for photocatalytic hydrogen evolution from water
Xiaoyan Wang; Linjiang Chen; Samantha Y. Chong; Marc A. Little; Yongzhen Wu; Wei-Hong Zhu; Rob Clowes; Yong Yan; Martijn A. Zwijnenburg; Reiner Sebastian Sprick; Andrew I. Cooper; Nature Chemistry 10 (2018) 1180–1189; doi:10.1038/s41557-018-0141-5

data_1551363
_publ_section_title
;
 Sulfone-containing covalent organic frameworks for photocatalytic
 hydrogen evolution from water
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              1180
_journal_page_last               1189
_journal_paper_doi               10.1038/s41557-018-0141-5
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'C18 H12 N2 O4 S2'
_chemical_formula_sum            'C18 H12 N2 O4 S2'
_chemical_formula_weight         384.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 97.082(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.8666(2)
_cell_length_b                   10.0313(3)
_cell_length_c                   13.5015(4)
_cell_measurement_reflns_used    6289
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.8814490923
_cell_measurement_theta_min      2.45808164136
_cell_volume                     788.50(4)
_computing_data_collection
'Diamond Light Source I19, UK, data collection software'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            PILATUS_2M_S_N_24_0107_Diamond
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9602
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.572
_diffrn_reflns_theta_min         2.947
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.989088483908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.044: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       needle
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.037
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1776
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0710P)^2^+1.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1353
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1578
_reflns_number_total             1776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41557_2018_141_MOESM17_ESM.cif
_cod_data_source_block           Fused_Sulfone_Diamine_100K
_cod_database_code               1551363
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C6-N1 \\sim N1-C8
 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C8(H8), C9(H9)
3.b Fitted hexagon refined as free rotating group:
 C5(C6,C7,C8,C9,C4)
;
_shelx_res_checksum              80956
_shelx_hkl_checksum              9878