Synthesis, Structures, and Solid State Self-Assemblies of Formyl and Acetyl Substituted Triptycenes and Their Derivatives
Peng-Fei Li; Chuan-Feng Chen; Journal of Organic Chemistry 77 (2012) 9250–9259; doi:10.1021/jo301820v

data_4027620
_publ_section_title
;
 Synthesis, Structures, and Solid State Self-Assemblies of Formyl and
 Acetyl Substituted Triptycenes and Their Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9250
_journal_page_last               9259
_journal_paper_doi               10.1021/jo301820v
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C26 H23 N3 O3, C4 H8 O'
_chemical_formula_sum            'C30 H31 N3 O4'
_chemical_formula_weight         497.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.972(3)
_cell_length_b                   23.832(5)
_cell_length_c                   9.0202(18)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4836
_cell_measurement_theta_min      1.7090
_cell_volume                     2632.2(11)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
 Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_av_sigmaI/netI    0.1195
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14449
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.1991
_refine_ls_R_factor_gt           0.1419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+5.4393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2340
_refine_ls_wR_factor_ref         0.2582
_reflns_number_gt                3072
_reflns_number_total             4641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301820v_si_006.cif
_cod_data_source_block           a
_cod_original_cell_volume        2632.1(9)
_cod_database_code               4027620