Structures of alkyl-substituted Tröger's base derivatives illustrate the importance of <i>Z</i>' for packing in the absence of strong crystal synthons
Vande Velde, Christophe M. L.; Tylleman, Benoît; Zeller, Matthias; Sergeyev, Sergey; Acta Crystallographica Section B 66 (2010) 472–481; doi:10.1107/S0108768110021981

data_2104804
_publ_section_title
;
 Structures of alkyl-substituted Tr\"oger's base derivatives illustrate
 the importance of <i>Z</i>' for packing in the absence of strong
 crystal synthons
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              472
_journal_page_last               481
_journal_paper_doi               10.1107/S0108768110021981
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C23 H30 N2'
_chemical_formula_sum            'C23 H30 N2'
_chemical_formula_weight         334.49
_chemical_melting_point          481.0(10)
_chemical_name_common            'tert-butyltr\:oger's base'
_chemical_name_systematic
;
 2,8-bis(tert-butyl)-6H,12H-5,11-methanodibenzo[bf][1,5]diazocine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.147(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.529(4)
_cell_length_b                   12.186(3)
_cell_length_c                   10.764(2)
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.61
_cell_volume                     1912.3(8)
_computing_cell_refinement       'Bruker Saint 7.43'
_computing_data_collection       'Bruker Saint 7.43'
_computing_data_reduction        'Bruker Saint 7.43'
_computing_molecular_graphics    'ORTEP, Mercury'
_computing_publication_material  'WinGX, PLATON'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'area detector diffractometer Bruker APEXII'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31760
_diffrn_reflns_theta_full        26.59
_diffrn_reflns_theta_max         26.59
_diffrn_reflns_theta_min         1.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/4'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0213P)^2^+2.0631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                3197
_reflns_number_total             3955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ry5032.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '480-482' was changed to '481.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2104804
_cod_database_fobs_code          2104804