Tröger's base quasiracemates and crystal packing tendencies
Cross, Jacob T.; Rossi, Nicholas A.; Serafin, Mateusz; Wheeler, Kraig A.; CrystEngComm 16 (2014) 7251–; doi:10.1039/C4CE00323C

data_7217453
_publ_section_title
;
 Tr\"oger's base quasiracemates and crystal packing tendencies
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              7251
_journal_paper_doi               10.1039/C4CE00323C
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C16.23 H15.68 Br0.77 N2, C15 H12 Br1.96 N2'
_chemical_formula_sum            'C31.23 H27.68 Br2.74 N4'
_chemical_formula_weight         677.57
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                82.302(4)
_cell_angle_beta                 75.969(3)
_cell_angle_gamma                82.058(3)
_cell_formula_units_Z            1
_cell_length_a                   6.3568(4)
_cell_length_b                   10.4138(7)
_cell_length_c                   10.7105(7)
_cell_measurement_reflns_used    7874
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.345
_cell_measurement_theta_min      3.229
_cell_volume                     677.53(8)
_computing_cell_refinement       APEX2
_computing_data_collection       APEX2
_computing_data_reduction
;
SAINT (Bruker, 2010) and XPREP (Bruker, 2010)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega 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  0.0575
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21743
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.183
_diffrn_reflns_theta_min         1.971
_exptl_absorpt_coefficient_mu    4.105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             338.8
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.477
_exptl_transmission_factor_min   0.280
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 3069 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.067(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7721
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                6901
_reflns_number_total             7721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00323c2.cif
_cod_data_source_block           COCR
_cod_database_code               7217453
_shelx_estimated_absorpt_t_min   0.280
_shelx_estimated_absorpt_t_max   0.477
_shelxl_version_number           2013-4
_shelx_res_checksum              70560