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_4116531
_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_sum            'C38 H28 N2 O2'
_chemical_formula_weight         544.65
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                70.552(16)
_cell_angle_beta                 78.929(12)
_cell_angle_gamma                64.781(17)
_cell_formula_units_Z            2
_cell_length_a                   10.7692(18)
_cell_length_b                   11.4492(29)
_cell_length_c                   14.3082(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    273
_cell_measurement_theta_max      11.8
_cell_measurement_theta_min      10.2
_cell_volume                     1502.4(5)
_diffrn_ambient_temperature      273
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_orient_matrix_UB_11      -0.01422
_diffrn_orient_matrix_UB_12      0.00636
_diffrn_orient_matrix_UB_13      -0.06884
_diffrn_orient_matrix_UB_21      -0.05444
_diffrn_orient_matrix_UB_22      -0.05748
_diffrn_orient_matrix_UB_23      0.02777
_diffrn_orient_matrix_UB_31      -0.08602
_diffrn_orient_matrix_UB_32      0.08240
_diffrn_orient_matrix_UB_33      -0.00098
_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  0.063
_diffrn_reflns_av_sigmaI/netI    0.260
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5587
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        -0.02
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       red
_exptl_crystal_F_000             572.00
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.42
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       '3.3(9) \\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   1.17
_refine_ls_goodness_of_fit_ref   1.37
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     380
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.316
_refine_ls_R_factor_gt           0.147
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.082
_refine_ls_wR_factor_ref         0.067
_reflns_number_gt                2749
_reflns_number_total             5276
_reflns_threshold_expression     I>0.50\s(I)
_cod_data_source_file            ja991749g_4.cif
_cod_data_source_block           C38H38N2O2_isomer_2
_cod_original_cell_volume        1502.4(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C38 H28 N2 O2 '
_cod_database_code               4116531