Controlling Molecular Organization by Using Phenyl Embraces of Multiple Trityl Groups.
Duong, Adam; Levesque, Alexandre; Homand, Clara; Maris, Thierry; Wuest, James D.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b02974

data_4038004
_publ_section_title
;
 Controlling Molecular Organization by Using Phenyl Embraces of Multiple
 Trityl Groups.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02974
_journal_year                    2020
_chemical_formula_moiety         'C26 H19 N'
_chemical_formula_sum            'C26 H19 N'
_chemical_formula_weight         345.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0812(2)
_cell_length_b                   34.7282(6)
_cell_length_c                   7.2597(1)
_cell_measurement_reflns_used    9115
_cell_measurement_temperature    150
_cell_measurement_theta_max      67.516
_cell_measurement_theta_min      2.545
_cell_volume                     3802.22(10)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection       'APEX2 v2.1-0 (Bruker AXS, 2006a)'
_computing_data_reduction        'SAINT v7.46A (Bruker, 2008)'
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.091
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            61578
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.014
_diffrn_reflns_theta_min         2.545
_diffrn_source                   'Bruker Microstar Rotating Anode Generator'
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/4 (Bruker,2007/4) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0911 after correction.
The Ratio of minimum to maximum transmission is 0.8408.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3449
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0885P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2957
_reflns_number_total             3449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02974_si_001.cif
_cod_data_source_block           jw1344
_cod_database_code               4038004
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C15-C16 = C16-C17 = C17-C18 = C18-C19 = C19-C20 = C20-C15
 1.39 with sigma of 0.001
 C1-C2 = C2-C3 = C3-C4 = C4-C5 = C5-N1 = N1-C1
 1.39 with sigma of 0.001
 C1B-C2B = C2B-C3 = C3-C4B = C4B-C5B = C5B-N1 = N1-C1B
 1.39 with sigma of 0.001
3. Restrained planarity
 C1, C2, C3, C4, C5, N1
 with sigma of 0.01
 C3, C1B, C2B, N1, C4B, C5B
 with sigma of 0.01
 C15, C16, C17, C18, C19, C20
 with sigma of 0.001
4. Others
 Fixed Sof: C15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5)
 C19(0.5) H19(0.5) C20(0.5) H20(0.5) C15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5)
 H17B(0.5) C18B(0.5) H18B(0.5) C19B(0.5) H19B(0.5) C20B(0.5) H20B(0.5) C1(0.5)
 H1(0.5) C2(0.5) H2(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) C1B(0.5) H1B(0.5)
 C2B(0.5) H2B(0.5) C4B(0.5) H4B(0.5) C5B(0.5) H5B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B),
 C20B(H20B), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C1(H1), C2(H2),
 C4(H4), C5(H5), C1B(H1B), C2B(H2B), C4B(H4B), C5B(H5B)
;
_shelx_res_checksum              76452
_shelx_hkl_checksum              40924
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'