Comparison of the Geometries of 3,7,10-Tribenzyl-3,7,10-triaza[3.3.3]propellane, (1), 7,10-Dibenzyl-3-<i>p</i>-tolyl-3,7,10-triaza[3.3.3]propellane, (2), and 7,10-Dibenzyl-3-oxa-7,10-diaza[3.3.3]propellane, (3)
Herbstein, F. H.; Kapon, M.; Reisner, G. M.; Acta Crystallographica Section C 52 (1996) 1539–1543; doi:10.1107/S0108270195016039

data_2005023
_publ_section_title
;
 Comparison of the Geometries of
 3,7,10-Tribenzyl-3,7,10-triaza[3.3.3]propellane, (1),
 7,10-Dibenzyl-3-<i>p</i>-tolyl-3,7,10-triaza[3.3.3]propellane, (2),
 and 7,10-Dibenzyl-3-oxa-7,10-diaza[3.3.3]propellane, (3)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1539
_journal_page_last               1543
_journal_paper_doi               10.1107/S0108270195016039
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C22 H26 N2 O1'
_chemical_formula_sum            'C22 H26 N2 O'
_chemical_formula_weight         334.45
_chemical_melting_point          348.6(5)
_chemical_name_common
3-oxa-7,10-dibenzyl-7,10-triaza[3.3.3]propellane
_chemical_name_systematic        ?
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            8
_cell_length_a                   35.656(20)
_cell_length_b                   9.652(5)
_cell_length_c                   11.018(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.9
_cell_measurement_theta_min      2.8
_cell_volume                     3792(4)
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Philips PW1100 computer-controlled'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_sigmaI/netI    0.1366
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2475
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        2.2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.982
_refine_ls_goodness_of_fit_obs   1.220
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         2475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_restrained_S_obs      1.220
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_obs          0.0702
_refine_ls_shift/esd_max         0.074
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0324P)^2^ + 2.4800P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1691
_refine_ls_wR_factor_obs         0.1271
_reflns_number_observed          1096
_reflns_number_total             2475
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1166.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '75-76 C' was changed to '348.6(5)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3792.(4)
_cod_original_sg_symbol_H-M      'P b c a'
_cod_original_formula_sum        'C22 H26 N2 O1'
_cod_database_code               2005023