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_2005021
_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         'C29 H33 N3'
_chemical_formula_sum            'C29 H33 N3'
_chemical_formula_weight         423.58
_chemical_melting_point          372.6(15)
_chemical_name_common            3,7,10-tribenzyl-3,7,10-triaza[3.3.3]propellane
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_audit_creation_method           SHELXL93
_cell_angle_alpha                107.21(5)
_cell_angle_beta                 107.21(5)
_cell_angle_gamma                107.21(5)
_cell_formula_units_Z            2
_cell_length_a                   11.354(5)
_cell_length_b                   11.354(5)
_cell_length_c                   11.354(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.4
_cell_measurement_theta_min      3.0
_cell_volume                     1211.9(13)
_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_R_equivalents  0.0103
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_number            683
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.10
_refine_diff_density_min         -0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.131
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         659
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_obs          0.0544
_refine_ls_shift/esd_max         0.15
_refine_ls_shift/esd_mean        0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.052P)^2^]
where P = [max(F~o~^2^,0) + 2F~c~^2^]/3
;
_refine_ls_wR_factor_all         0.1357
_refine_ls_wR_factor_obs         0.1153
_reflns_number_observed          659
_reflns_number_total             683
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1166.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '98-101 C' was changed to '372.6(15)'
- 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        1211.9(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2005021