Stepwise Assembly of Site Specifically Functionalized Dehydrobenzo[18]annulenes
Joshua J. Pak; Timothy J. R. Weakley; Michael M. Haley; Journal of the American Chemical Society 121 (1999) 8182–8192; doi:10.1021/ja991749g

data_4116530
_publ_contact_author_address
;Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 Stepwise Assembly of Site Specifically Functionalized
 Dehydrobenzo[18]annulenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8182
_journal_page_last               8192
_journal_paper_doi               10.1021/ja991749g
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C38 H28 N2 O2 '
_chemical_formula_sum            'C38 H28 N2 O2'
_chemical_formula_weight         544.65
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_cell_angle_alpha                90
_cell_angle_beta                 114.464(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7761(10)
_cell_length_b                   31.232(4)
_cell_length_c                   10.954(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      14.8
_cell_measurement_theta_min      12.6
_cell_volume                     3044.3(10)
_diffrn_ambient_temperature      294
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.00594
_diffrn_orient_matrix_UB_12      0.03184
_diffrn_orient_matrix_UB_13      0.01047
_diffrn_orient_matrix_UB_21      0.11011
_diffrn_orient_matrix_UB_22      -0.00108
_diffrn_orient_matrix_UB_23      0.02271
_diffrn_orient_matrix_UB_31      -0.02167
_diffrn_orient_matrix_UB_32      0.00318
_diffrn_orient_matrix_UB_33      -0.09712
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.110
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3226
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        -1.25
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144.00
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       '3.9(4) \\times 10^-7^'
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.26
_refine_ls_goodness_of_fit_ref   1.27
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     378
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.079
_refine_ls_R_factor_gt           0.053
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.098
_refine_ls_wR_factor_ref         0.045
_reflns_number_gt                1873
_reflns_number_total             3045
_reflns_threshold_expression     I>\s(I)
_cod_data_source_file            ja991749g_3.cif
_cod_data_source_block           C38H28N2O2_isomer_1
_cod_original_cell_volume        3044.2(9)
_cod_original_sg_symbol_H-M      'I a '
_cod_original_formula_sum        'C38 H28 N2 O2 '
_cod_database_code               4116530