Stereocontrol in the intramolecular Buchner reaction of diazoketones
Maguire, Anita R.; Buckley, N. Rachael; O’Leary, Patrick; Ferguson, George; Journal of the Chemical Society, Perkin Transactions 1  (1998) 4077–; doi:10.1039/a807677d

data_7212966
_publ_section_title
;
 Stereocontrol in the intramolecular Buchner reaction of diazoketones
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              4077
_journal_paper_doi               10.1039/a807677d
_journal_year                    1998
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C20 H20 N4 O4 '
_chemical_formula_sum            'C20 H20 N4 O4'
_chemical_formula_weight         380.40
_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_date             'February 22, 1995'
_audit_creation_method
'from NRCVAX CIF routine and SHELXL93 with Word-Perfect Macro PREPSHEL'
_audit_update_record
;   February 22, 1995  Assembled, pass-1

;
_cell_angle_alpha                101.63(2)
_cell_angle_beta                 93.12(3)
_cell_angle_gamma                112.79(3)
_cell_formula_units_Z            2
_cell_length_a                   7.943(5)
_cell_length_b                   8.000(3)
_cell_length_c                   16.237(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(1)
_cell_measurement_theta_max      13.35
_cell_measurement_theta_min      5.30
_cell_volume                     921.6(7)
_computing_cell_refinement       'Enraf-Nonius SET4 and CELDIM'
_computing_data_collection       'Enraf-Nonius CAD4 (Enraf-Nonius 1992)'
_computing_data_reduction
'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics
'NRCVAX94, PLATON (Spek, 1994a) and PLUTON (Spek 1994b)'
_computing_publication_material  'NRCVAX94, SHELXL93  and WordPerfect'
_computing_structure_refinement  'NRCVAX94 and SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      294(1)
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'Theta/2theta scan b/P/b '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3248
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            reddish-orange
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.835
_refine_ls_goodness_of_fit_obs   1.192
_refine_ls_hydrogen_treatment
'riding (SHELXL defaults, C-H 0.93 to 0.98, N-H 0.86\%A)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.835
_refine_ls_restrained_S_obs      1.192
_refine_ls_R_factor_all          0.1577
_refine_ls_R_factor_obs          0.0541
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1376
_refine_ls_wR_factor_obs         0.1152
_reflns_number_observed          1274
_reflns_number_total             3248
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            807677dsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0649P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        921.6(6)
_cod_database_code               7212966