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_4116529
_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 H44 N4 O4 ), (C H2 Cl2 )''
_chemical_formula_sum            'C47 H46 Cl2 N4 O4'
_chemical_formula_weight         801.81
_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                74.555(9)
_cell_angle_beta                 86.062(9)
_cell_angle_gamma                79.597(10)
_cell_formula_units_Z            2
_cell_length_a                   10.023(1)
_cell_length_b                   13.922(2)
_cell_length_c                   16.577(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      10.3
_cell_measurement_theta_min      8.0
_cell_volume                     2192.5(5)
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_UB_11      -0.00243
_diffrn_orient_matrix_UB_12      -0.02949
_diffrn_orient_matrix_UB_13      0.06197
_diffrn_orient_matrix_UB_21      -0.05577
_diffrn_orient_matrix_UB_22      0.06445
_diffrn_orient_matrix_UB_23      0.00733
_diffrn_orient_matrix_UB_31      -0.08471
_diffrn_orient_matrix_UB_32      -0.02630
_diffrn_orient_matrix_UB_33      -0.00497
_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  0.027
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5758
_diffrn_reflns_theta_max         22.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        2.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       prism
_exptl_crystal_F_000             844.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.34
_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_obs   1.69
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         3317
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.1011
_refine_ls_shift/esd_max         0.071
_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_obs         0.0534
_reflns_number_observed          3317
_reflns_number_total             5376
_reflns_observed_criterion       I>\s(I)
_cod_data_source_file            ja991749g_2.cif
_cod_data_source_block           C47H46Cl2N4O4
_cod_original_cell_volume        2192.5(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C47 H46 Cl2 N4 O4 '
_cod_database_code               4116529