Rapid, Scalable Construction of Highly Crystalline Acylhydrazone Two-Dimensional Covalent Organic Frameworks via Dipole-Induced Antiparallel Stacking.
Li, Xing; Qiao, Jingsi; Chee, See Wee; Xu, Hai-Sen; Zhao, Xiaoxu; Choi, Hwa Seob; Yu, Wei; Quek, Su Ying; Mirsaidov, Utkur; Loh, Kian Ping; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00553

data_4134321
_publ_section_title
;
 Rapid, Scalable Construction of Highly Crystalline Acylhydrazone
 Two-Dimensional Covalent Organic Frameworks via Dipole-Induced
 Antiparallel Stacking.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00553
_journal_year                    2020
_chemical_formula_sum            'C31 H37 N5 O5'
_chemical_formula_weight         559.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5394(2)
_cell_length_b                   14.4953(5)
_cell_length_c                   26.6114(8)
_cell_measurement_reflns_used    8961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.72
_cell_measurement_theta_min      3.32
_cell_volume                     2908.25(15)
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21912
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.711
_diffrn_reflns_theta_min         3.321
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.3(3)
_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     381
_refine_ls_number_reflns         5653
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0688P)^2^+0.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4768
_reflns_number_total             5653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00553_si_003.cif
_cod_data_source_block           H553
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'Not Measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               4134321
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.944
_computing_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_shelx_res_checksum              61432
_shelx_hkl_checksum              98108