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_4116528
_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         'C46 H46 N2 '
_chemical_formula_sum            'C46 H46 N2'
_chemical_formula_weight         626.88
_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                73.260(18)
_cell_angle_beta                 82.468(20)
_cell_angle_gamma                74.29(3)
_cell_formula_units_Z            2
_cell_length_a                   9.420(3)
_cell_length_b                   12.022(4)
_cell_length_c                   18.224(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295.2
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      11.0
_cell_volume                     1899.4(10)
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.03232
_diffrn_orient_matrix_UB_12      0.08946
_diffrn_orient_matrix_UB_13      -0.01326
_diffrn_orient_matrix_UB_21      0.02042
_diffrn_orient_matrix_UB_22      0.00337
_diffrn_orient_matrix_UB_23      -0.05572
_diffrn_orient_matrix_UB_31      -0.10359
_diffrn_orient_matrix_UB_32      -0.00382
_diffrn_orient_matrix_UB_33      -0.00334
_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  0.019
_diffrn_reflns_av_sigmaI/netI    0.120
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7127
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown-yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.28
_refine_ls_goodness_of_fit_ref   3.15
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     421
_refine_ls_number_reflns         3303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.210
_refine_ls_R_factor_gt           0.096
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.099
_refine_ls_wR_factor_ref         0.093
_reflns_number_gt                3303
_reflns_number_total             6680
_reflns_threshold_expression     I>\s(I)
_cod_data_source_file            ja991749g_1.cif
_cod_data_source_block           C46H46N2
_cod_original_cell_volume        1899.4(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C46 H46 N2 '
_cod_database_code               4116528