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_2104805
_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          449.5(5)
_chemical_name_common            'tert-butyltr\:oger's base'
_chemical_name_systematic
;
 S,S-2,8-bis(tert-butyl)-6H,12H-5,11-methanodibenzo[bf][1,5]diazocine
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 105.9400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.370(2)
_cell_length_b                   6.6841(5)
_cell_length_c                   21.6271(16)
_cell_measurement_reflns_used    2307
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.77
_cell_volume                     3943.4(5)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Saint'
_computing_data_reduction        'Bruker Saint'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'area detector diffractometer Bruker APEXII'
_diffrn_measurement_method       '\w scans'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17606
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.73
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6393
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0437P)^2^+1.8840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                4971
_reflns_number_total             6393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ry5032.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '449-450' was changed to '449.5(5)' -
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      C2
_cod_database_code               2104805
_cod_database_fobs_code          2104805