U-Shaped Helical Azaarenes: Synthesis, Structures, and Properties.
Zhao, Kexiang; Long, Guankui; Liu, Wenbo; Li, Dong-Sheng; Gao, Weibo; Zhang, Qichun; The Journal of organic chemistry 85 (2020) 291–295; doi:10.1021/acs.joc.9b02895

data_4037628
_publ_section_title
;
 U-Shaped Helical Azaarenes: Synthesis, Structures, and Properties.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              291
_journal_page_last               295
_journal_paper_doi               10.1021/acs.joc.9b02895
_journal_volume                  85
_journal_year                    2020
_chemical_formula_sum            'C91 H105.5 Cl1.5 N8 Si4'
_chemical_formula_weight         1476.86
_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
_cell_angle_alpha                78.420(3)
_cell_angle_beta                 87.087(3)
_cell_angle_gamma                80.742(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6965(13)
_cell_length_b                   17.3542(18)
_cell_length_c                   19.577(2)
_cell_measurement_reflns_used    6481
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.9764
_cell_measurement_theta_min      2.6230
_cell_volume                     4169.9(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2017)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Multilayer Mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.1247
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15223
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1578
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.846
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1375
_refine_ls_number_reflns         15223
_refine_ls_number_restraints     2916
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_gt           0.1222
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1851P)^2^+9.5079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3172
_refine_ls_wR_factor_ref         0.3785
_reflns_number_gt                8414
_reflns_number_total             15223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02895_si_004.cif
_cod_data_source_block           zqc95m_tw
_cod_depositor_comments
'Adding full bibliography for 4037628--4037630.cif.'
_cod_original_formula_sum        'C91 H105.50 Cl1.50 N8 Si4'
_cod_database_code               4037628
_shelx_res_checksum              62211
_shelx_hkl_checksum              38253