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_1551362
_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         'C12 H10 N2 O2 S'
_chemical_formula_sum            'C12 H10 N2 O2 S'
_chemical_formula_weight         246.78
_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   mixed
_cell_angle_alpha                97.595(4)
_cell_angle_beta                 100.424(4)
_cell_angle_gamma                90.636(4)
_cell_formula_units_Z            4
_cell_length_a                   7.4654(4)
_cell_length_b                   8.3783(4)
_cell_length_c                   17.0551(8)
_cell_measurement_reflns_used    6073
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.314
_cell_measurement_theta_min      1.198
_cell_volume                     1039.27(9)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.8.1-g1afca60c-release-hotfix1'
_computing_data_collection       'Diamond Light Source, I19, GUI'
_computing_data_reduction
'XIA2 0.5.474-gb1e580cd-dials-1.8 (Winter, G., 2010)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_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 0.984
_diffrn_measurement_device       "'Fixed \c 3-circle diffractometer"
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1287
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13950
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.849
_diffrn_reflns_theta_min         2.376
_diffrn_source                   'Diamond Light Source Beamline I19-1'
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.991434307221
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.046: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.058
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0789
_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^)+(0.0920P)^2^+1.7113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2170
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3782
_reflns_number_total             4351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41557_2018_141_MOESM16_ESM.cif
_cod_data_source_block           Sulfone_Diamine_100K
_cod_depositor_comments
;

2022-03-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C24 H21 N4 O4 S2'
_cod_original_formula_weight         493.57
_cod_original_formula_moiety         '2(C12 H10 N2 O2 S)'
_cod_original_formula_units_Z            2
_cod_database_code               1551362
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C11-N2 \\sim N2-C9
 with sigma of 0.01
 C1-N1 \\sim N1-C3
 with sigma of 0.01
 C13-N3 \\sim N3-C15
 with sigma of 0.01
 C24-N4 \\sim N4-C22
 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C1(H1), C11(H11), C9(H9), C8(H8), C13(H13), C15(H15),
 C16(H16), C21(H21), C22(H22), C24(H24)
3.b Fitted hexagon refined as free rotating group:
 C6(C5,C4,C3,C2,C1), C12(C11,C10,C9,C8,C7), C18(C13,C14,C15,C16,C17), C19(C20,
 C21,C22,C23,C24)
;
_shelx_res_checksum              28097
_shelx_hkl_checksum              62460