Steroid-Like Ring Skeletons by Cyclohexadiene Annulation to Enamines with Alkynylcarbene Complexes of Chromium and Tungsten via Pyran-2-ylidene Complexes
Rudolf Aumann; Adam G. Meyer; Roland Fröhlich; Journal of the American Chemical Society 118 (1996) 10853–10861; doi:10.1021/ja961020x

data_4117199
_publ_contact_author
;
        Rudolf Aumann
        Organisch-Chemisches Institut 
        der Universit\"at M\"unster
        Corrensstrasse 40
        D-48149 M\"unster
        Bundesrepublik Deutschland
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_publ_contact_author_email       aumannr@uni-muenster.de
_publ_contact_author_fax         '49 251 83-9772'
_publ_contact_author_phone       '49 251 83-3219'
_publ_section_title
;
 Steroid-Like Ring Skeletons by Cyclohexadiene Annulation to Enamines with
 Alkynylcarbene Complexes of Chromium and Tungsten via Pyran-2-ylidene
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10853
_journal_page_last               10861
_journal_paper_doi               10.1021/ja961020x
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C28 H31 N O'
_chemical_formula_weight         397.54
_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
_cell_angle_alpha                81.39(1)
_cell_angle_beta                 75.84(1)
_cell_angle_gamma                71.32(1)
_cell_formula_units_Z            2
_cell_length_a                   8.987(1)
_cell_length_b                   9.876(1)
_cell_length_c                   13.434(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      46.59
_cell_measurement_theta_min      40.22
_cell_volume                     1091.9(2)
_computing_cell_refinement       'Enraf-Nonius Express (1995)'
_computing_data_collection       'Enraf-Nonius Express (1995)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'SCHAKAL-92 (Keller, 1992)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4750
_diffrn_reflns_theta_max         74.28
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       'irregular blocks'
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0072(8)
_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_all   1.028
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_obs          0.0462
_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^)+(0.0716P)^2^+0.3337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1354
_refine_ls_wR_factor_obs         0.1272
_reflns_number_observed          3941
_reflns_number_total             4452
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja961020x_2.cif
_cod_data_source_block           aum_387
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.3337P] 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^)+(0.0716P)^2^+0.3337P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4117199