A Protocol for the exo-Mono and exo,exo-Bis Functionalization of the Diazocine Ring of Tröger's Base.
Dawaigher, Sami; Månsson, Kristoffer; Ascic, Erhad; Artacho, Josep; Mårtensson, Roger; Loganathan, Nagarajan; Wendt, Ola F.; Harmata, Michael; Snieckus, Victor; Wärnmark, Kenneth; The Journal of organic chemistry 80 (2015) 12006–12014; doi:10.1021/acs.joc.5b01921

data_4031746
_publ_section_title
;
 A Protocol for the exo-Mono and exo,exo-Bis Functionalization of the
 Diazocine Ring of Tr\"oger's Base.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12006
_journal_page_last               12014
_journal_paper_doi               10.1021/acs.joc.5b01921
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C24 H24 N2'
_chemical_formula_sum            'C24 H24 N2'
_chemical_formula_weight         340.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
;

CrysAlis RED, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov  6 2009,16:24:50)

;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.401(4)
_cell_length_b                   10.577(3)
_cell_length_c                   17.112(5)
_cell_measurement_reflns_used    1776
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      33.0245
_cell_measurement_theta_min      2.4286
_cell_volume                     1834.2(11)
_computing_cell_refinement
;

CrysAlis RED, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov  6 2009,16:24:50)

;
_computing_data_collection
;

CrysAlis CCD, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov  6 2009,16:24:50)

;
_computing_data_reduction
;

CrysAlis RED, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov  6 2009,16:24:50)

;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 16.1829
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_sigmaI/netI    0.1322
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13422
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.96974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

CrysAlis RED, Oxford Diffraction Ltd.,

Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)

(compiled Nov  6 2009,16:24:50)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                1443
_reflns_number_total             3993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b01921_si_002.cif
_cod_data_source_block           TBBn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4031745--4031746.cif.
;
_cod_original_cell_volume        1834.3(10)
_cod_original_sg_symbol_Hall     -P2ybC
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4031746