Enhancing structural control in covalent organic frameworks through steric interaction-driven linker design.
Winter, Alena; Hamdi, Farzad; Eichhöfer, Andreas; Saalwächter, Kay; Kastritis, Panagiotis L.; Haase, Frederik; Chemical science 15 (2024) 14449–14457; doi:10.1039/d4sc03461a

data_1572337
_publ_section_title
;
 Enhancing structural control in covalent organic frameworks through
 steric interaction-driven linker design.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14449
_journal_page_last               14457
_journal_paper_doi               10.1039/d4sc03461a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C28 H22 N2 O2'
_chemical_formula_sum            'C28 H22 N2 O2'
_chemical_formula_weight         418.47
_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             2023-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.539(10)
_cell_angle_beta                 73.454(11)
_cell_angle_gamma                76.360(11)
_cell_formula_units_Z            2
_cell_length_a                   9.9945(16)
_cell_length_b                   10.1084(12)
_cell_length_c                   11.4916(15)
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.09
_cell_measurement_theta_min      1.85
_cell_volume                     1079.1(3)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      '667 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_unetI/netI     0.1396
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8450
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.853
_diffrn_source                   'Mo GeniX 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Mo
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1826
_refine_ls_R_factor_gt           0.1171
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2769
_refine_ls_wR_factor_ref         0.3287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2078
_reflns_number_total             4194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03461a2.cif
_cod_data_source_block           awi-51-1ster
_cod_depositor_comments
'Adding full bibliography for 1572336--1572337.cif.'
_cod_database_code               1572337
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              38185
_shelx_hkl_checksum              36324
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   6.0
_stoe_evaluation_integration_b   0.0
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 86.2
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 66.7
_stoe_evaluation_lana_max_2theta_desired 66.7
_stoe_evaluation_lana_mean_redundancy 1.8
_stoe_evaluation_lana_number_refls_after_or 13260
_stoe_evaluation_lana_number_refls_outliers 1037
_stoe_evaluation_lana_number_refls_total 14297
_stoe_evaluation_lana_number_refls_unique 7225
_stoe_evaluation_lana_number_refls_written 13260
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta           6.4   13.6   20.8   28.0   35.2   42.4   49.6   56.8   64.0
<Resolution>    5.26   2.89   1.94   1.46   1.17   0.98   0.85   0.75   0.69
N(total)         110    373    712   1290   1963   2516   2943   3169   1221
<Redundancy>     2.6    2.2    2.0    2.1    2.1    2.0    1.9    1.7    1.3
Complet. [%%]   100.0   99.3   99.7   99.1   99.2   98.3   98.0   95.2   49.1
<I/sigma>      114.0   60.1   28.5   10.1    6.7    2.7    1.1    0.6    0.4
R(int)         0.057  0.086  0.090  0.126  0.166  0.208  0.324  0.426  0.527
;
_stoe_measurement_identifier     Awi-51-1ster
_stoe_measurement_max_exposure_per_frame '20.0 s'
_stoe_measurement_mean_exposure_per_frame '20.0 s'
_stoe_measurement_min_exposure_per_frame '20.0 s'
_stoe_measurement_total_exposure_time '3.7 h'
_stoe_measurement_total_frame_number 667
_stoe_measurement_total_run_number 9
_stoe_measurement_tube_power     '50.0 W'