2^4^,4,8-Trioxa-2^1^-aza-1,3,6(1,2)-tribenzena-2(2,3)-bicyclo[3.3.0]octanacyclooctaphane
Seshadri, P. R.; Balakrishnan, B.; Ilangovan, K.; Purushothaman, S.; Raghunathan, R.; Acta Crystallographica Section E 65 (2009) o670–; doi:10.1107/S160053680900720X

data_2221542
_publ_section_title
2^4^,4,8-Trioxa-2^1^-aza-1,3,6(1,2)-tribenzena-2(2,3)-bicyclo[3.3.0]octanacyclooctaphane
_journal_coeditor_code           WN2311
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o670
_journal_paper_doi               10.1107/S160053680900720X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C26 H25 N O3'
_chemical_formula_moiety         'C26 H25 N O3'
_chemical_formula_sum            'C26 H25 N O3'
_chemical_formula_weight         399.47
_chemical_name_common
;
1,6-Dioxa[6.2]orthocyclophane-[13,14]pyrrolo[2,1-<i>b</i>]oxazole
;
_chemical_name_systematic
;
2^4^,4,8-Trioxa-2^1^-aza-1,3,6(1,2)-tribenzena-2(2,3)-
bicyclo[3.3.0]octanacyclooctaphane
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.4680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.1942(7)
_cell_length_b                   8.3992(2)
_cell_length_c                   16.0323(4)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      1.33
_cell_volume                     4116.70(17)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Kappa APEXII area-detector'
_diffrn_measurement_method       \w
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22005
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9834
_exptl_absorpt_correction_T_min  0.9793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0585
_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^)+(0.1118P)^2^+1.2039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2132
_reflns_number_gt                2790
_reflns_number_total             5004
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn2311.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     C2/c
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2221542
_cod_database_fobs_code          2221542