Synthesis of ene-1,1-diamines and pyrrolo[1,2-a]imidazolediones by 4,5-dihydroimidazole N-oxide cycloaddition and isoxazoline ring opening
Jones, Raymond C. F.; Martin, Jason N.; Smith, Paul; Gelbrich, Tomas; Light, Mark E.; Hursthouse, Michael B.; Chemical Communications  (2000) 1949–; doi:10.1039/b005530l

data_7115167
_publ_section_title
;
 Synthesis of ene-1,1-diamines and pyrrolo[1,2-a]imidazolediones by
 4,5-dihydroimidazole N-oxide cycloaddition and isoxazoline ring opening
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1949
_journal_paper_doi               10.1039/b005530l
_journal_year                    2000
_chemical_formula_sum            'C26 H31 N2 O3'
_chemical_formula_weight         419.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.243(4)
_cell_angle_beta                 99.513(4)
_cell_angle_gamma                103.536(4)
_cell_formula_units_Z            4
_cell_length_a                   9.4057(6)
_cell_length_b                   13.8445(11)
_cell_length_c                   18.9676(14)
_cell_measurement_reflns_used    na
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      na
_cell_measurement_theta_min      na
_cell_volume                     2360.5(3)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
;
DENZO and COLLECT
;
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '9.091 pixels/mm'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method       'Phi and Omega scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12951
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        na
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.9923
_exptl_absorpt_correction_type   'Empirical, SORTAV'
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0085(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         5590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                3391
_reflns_number_total             5590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005530l.txt
_cod_data_source_block           s91
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115167