Substituted Benzophenone Imines for COF Synthesis via Formal Transimination
Sprachmann, Josefine; Grabicki, Niklas; Möckel, Anna; Maltitz, Jeremy; del Refugio Monroy Gómez, José; Smales, Glen J.; Dumele, Oliver; Chemical Communications  (2023) –; doi:10.1039/D3CC03735E

data_7132227
_publ_section_title
;
 Substituted Benzophenone Imines for COF Synthesis via Formal
 Transimination
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03735E
_journal_year                    2023
_chemical_formula_moiety         'C42 H24 F12 N2'
_chemical_formula_sum            'C42 H24 F12 N2'
_chemical_formula_weight         784.63
_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             2019-07-22
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-22 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                80.515(4)
_cell_angle_beta                 85.368(4)
_cell_angle_gamma                83.032(4)
_cell_formula_units_Z            1
_cell_length_a                   5.5923(4)
_cell_length_b                   10.4164(7)
_cell_length_c                   14.6091(11)
_cell_measurement_reflns_used    3743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.102
_cell_measurement_theta_min      2.833
_cell_volume                     831.56(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_min         2.258
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1042 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.9120.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       plate
_exptl_crystal_F_000             398
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method
'recrystalization from ortho-Dichlorobenzene'
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0558P)^2^+0.6503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2175
_reflns_number_total             3048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03735e2.cif
_cod_data_source_block           solv_i
_cod_database_code               7132227
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C2(H2), C3(H3), C5(H5), C6(H6), C13(H13), C20(H20), C10(H10),
 C9(H9), C17(H17), C12(H12), C18(H18)
;
_shelx_res_checksum              56542
_shelx_hkl_checksum              69795
_olex2_submission_original_sample_id MJE-04
_olex2_submission_special_instructions 'No special instructions were received'