Asymmetric Propargylation/Allylation/Pauson-Khand Cyclization of a Planar Chiral Anisole Tricarbonylchromium Complex
Anna Quattropani; Gary Anderson; Gérald Bernardinelli; E. Peter Kündig; Journal of the American Chemical Society 119 (1997) 4773–4774; doi:10.1021/ja964256+

data_4116978
_publ_contact_author
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  Prof. E.P. Kundig
    D\'epartement de Chimie Organique
     Universit\'e de Gen\`eve
     30, quai E. Ansermet
     CH - 1212 Gen=E8ve 4
     Switzerland
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_publ_contact_author_email       Peter.Kundig@chiorg.unige.ch
_publ_contact_author_fax         '(+[41] 22) 328 73 96'
_publ_contact_author_phone       '(+[41] 22) 702 60 93'
_publ_section_title
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 Asymmetric Propargylation/Allylation/Pauson-Khand Cyclization of a Planar
 Chiral Anisole Tricarbonylchromium Complex
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4773
_journal_page_last               4774
_journal_paper_doi               10.1021/ja964256+
_journal_volume                  119
_journal_year                    1997
_chemical_formula_moiety         'C19 H30 O2 Si2'
_chemical_formula_structural     'C19 H30 O2 Si2'
_chemical_formula_sum            'C19 H30 O2 Si2'
_chemical_formula_weight         346.6
_chemical_melting_point          399(1)
_chemical_name_systematic
;
3,7-Bis-trimethylsilanyl-1,4a,5,8a,9,9a-hexahydro-4H-cyclopenta[\b]
naphthalene-2,6-dione.
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             96-11-27
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             '96-11-27 G. Bernardinelli'
_cell_angle_alpha                106.602(6)
_cell_angle_beta                 93.405(5)
_cell_angle_gamma                101.127(5)
_cell_formula_units_Z            4
_cell_length_a                   6.8483(5)
_cell_length_b                   14.531(2)
_cell_length_c                   22.560(2)
_cell_measurement_pressure       100
_cell_measurement_reflns_used    22
_cell_measurement_temperature    290
_cell_measurement_theta_max      34.5
_cell_measurement_theta_min      21.5
_cell_measurement_wavelength     1.5418
_cell_volume                     2095.3(4)
_computing_cell_refinement       xtal_LATCON=20
_computing_data_collection       Enraf-Nonius_CAD4_version_5.0
_computing_data_reduction        xtal_REFCAL_LSABS__SORTRF
_computing_molecular_graphics    xtal_ORTEP
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    '(MULTAN-87 (Main & al.)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      290
_diffrn_measurement_device       Enraf-Nonius_CAD4_4circle_diffractometertaC
_diffrn_measurement_method       omega-twotheta_scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focus_Philips_t
_diffrn_radiation_type           x-ray
_diffrn_radiation_wavelength     1.54183
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    .039
_diffrn_reflns_limit_h_max       7
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
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_diffrn_reflns_theta_max         55
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        5.5
_diffrn_standards_interval_time  30
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.58
_exptl_absorpt_correction_T_max  .78869
_exptl_absorpt_correction_T_min  .579854
_exptl_absorpt_correction_type   Analytical_integration
_exptl_absorpt_process_details   'xtal LSABS (Blanc & Schwarzenbach, 1991)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         .359
_refine_diff_density_min         -.461
_refine_ls_goodness_of_fit_all   5.912
_refine_ls_goodness_of_fit_obs   5.404
_refine_ls_hydrogen_treatment    'refxyz except methyl groups'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     487
_refine_ls_number_reflns         4375
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .09
_refine_ls_R_factor_obs          .076
_refine_ls_shift/esd_max         .00046
_refine_ls_shift/esd_mean        .00010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w =3D 1/(\s^2^(F))'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .06
_refine_ls_wR_factor_obs         .052
_reflns_d_resolution_high        .942
_reflns_d_resolution_low         21.367
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_observed          4410
_reflns_number_total             5255
_reflns_observed_criterion       'refl observed if F > 4.00 sigma(F)'
_cod_data_source_file            ja9642562B.cif
_cod_data_source_block           GARY
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w =3D 1/(\s^2^(F))' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w =3D 1/(\s^2^(F))'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4116978