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_4031745
_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_sum            'C21 H26 N2 O2'
_chemical_formula_weight         338.44
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;

CrysAlisPro, Agilent Technologies,

Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)

(compiled Jan 20 2011,15:58:25)

;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.641(4)
_cell_length_b                   13.069(4)
_cell_length_c                   10.529(2)
_cell_measurement_reflns_used    1018
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7238
_cell_measurement_theta_min      2.8923
_cell_volume                     1877.0(9)
_computing_cell_refinement
;

CrysAlisPro, Agilent Technologies,

Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)

(compiled Jan 20 2011,15:58:25)

;
_computing_data_collection
;

CrysAlisPro, Agilent Technologies,

Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)

(compiled Jan 20 2011,15:58:25)

;
_computing_data_reduction
;

CrysAlisPro, Agilent Technologies,

Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)

(compiled Jan 20 2011,15:58:25)

;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1829
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Eos'
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8921
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.64493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

CrysAlisPro, Agilent Technologies,

Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)

(compiled Jan 20 2011,15:58:25)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1654
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0726P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.2071
_reflns_number_gt                895
_reflns_number_total             2026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b01921_si_001.cif
_cod_data_source_block           TB(MOM)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to 'constr'
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        1877.1(8)
_cod_original_sg_symbol_Hall     '-P 2ab 2ac '
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               4031745