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_7132228
_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         'C38 H28 N2'
_chemical_formula_sum            'C38 H28 N2'
_chemical_formula_weight         512.62
_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             2023-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-10 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                88.246(4)
_cell_angle_beta                 81.362(4)
_cell_angle_gamma                89.566(4)
_cell_formula_units_Z            4
_cell_length_a                   9.5460(18)
_cell_length_b                   15.907(3)
_cell_length_c                   18.545(4)
_cell_measurement_reflns_used    4723
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.34
_cell_measurement_theta_min      2.22
_cell_volume                     2782.8(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4000
_diffrn_reflns_av_unetI/netI     0.3408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            86855
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.552
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1161 before and 0.0844 after correction. The Ratio of minimum to maximum transmission is 0.8497. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1080
_exptl_crystal_preparation       synthetic
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         11521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.3014
_refine_ls_R_factor_gt           0.0955
_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^)+(0.0757P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.2133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4041
_reflns_number_total             11521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03735e2.cif
_cod_data_source_block           p-1_gni001b
_cod_original_cell_volume        2782.8(9)
_cod_database_code               7132228
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00G(H00G), C00I(H00I), C00J(H00J), C00N(H00N), C00O(H00O),
 C00P(H00P), C00R(H00R), C00S(H00S), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C010(H010), C011(H011), C012(H012), C014(H014),
 C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
 C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H),
 C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N),
 C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T),
 C01U(H01U), C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020),
 C021(H021), C022(H022), C023(H023), C024(H024), C025(H025), C026(H026),
 C027(H027), C028(H028)
;
_olex2_exptl_crystal_mounting_method 'in oil in plastic loop'
_olex2_submission_special_instructions 'No special instructions were received'