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_2005022
_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_sum            'C29 H33 N3'
_chemical_formula_weight         423.58
_chemical_melting_point          412.1(10)
_chemical_name_common
3-p-tolyl-7,10-dibenzyl3,7,10-triaza[3.3.3]propellane
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                103.94(5)
_cell_angle_beta                 96.87(5)
_cell_angle_gamma                104.87(5)
_cell_formula_units_Z            2
_cell_length_a                   13.283(7)
_cell_length_b                   11.748(6)
_cell_length_c                   8.533(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      7.9
_cell_measurement_theta_min      2.5
_cell_volume                     1225.5(12)
_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    0.0721
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2994
_diffrn_reflns_theta_max         22.02
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        5.4
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       Rhombic
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.184
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.184
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_obs          0.0610
_refine_ls_shift/esd_max         0.13
_refine_ls_shift/esd_mean        0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0084P)^2^ + 0.5631P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1365
_refine_ls_wR_factor_obs         0.1159
_reflns_number_observed          1953
_reflns_number_total             2994
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1166.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '138-140 C' was changed to
'412.1(10)' - 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        1225.5(11)
_cod_database_code               2005022