Addition of Organometallic Compounds to Tin-Containing Cyclic Ketones. Remote Stereocontrol Induced by the Stannyl Group
Asunción Barbero; Francisco J. Pulido; Juan A. Rincón; Journal of the American Chemical Society 125 (2003) 12049–12056; doi:10.1021/ja036340c

data_4114208
_publ_contact_author
;
 Francisco J. Pulido Pelaz
Depart. de Q. Org\'anica
Fac. De Ciencias
47011 Valladolid
      Spain
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_publ_contact_author_email       pulido@qo.uva.es
_publ_contact_author_fax         '0034 983 423013'
_publ_contact_author_phone       '0034 983 423210'
_publ_section_title
;
 Addition of Organometallic Compounds to Tin-Containing Cyclic Ketones.
 Remote Stereocontrol Induced by the Stannyl Group
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12049
_journal_page_last               12056
_journal_paper_doi               10.1021/ja036340c
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C31 H53 N O2 Sn'
_chemical_formula_sum            'C31 H53 N O2 Sn'
_chemical_formula_weight         590.43
_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                98.97(19)
_cell_angle_beta                 99.1(3)
_cell_angle_gamma                111.0(3)
_cell_formula_units_Z            2
_cell_length_a                   10.60(4)
_cell_length_b                   11.945(14)
_cell_length_c                   14.71(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      7
_cell_volume                     1671(10)
_computing_cell_refinement       'CRYSDA (Beurskens et al, 1992)'
_computing_data_collection
;
 Nonius CAD-4 Diffractometer Control Software. Data collection with profile 
analysis over all reflections (Lehmen and Larsen, 1974; Grant and Gable, 
1978)
;
_computing_data_reduction        'THE REFLEX (local program)'
_computing_molecular_graphics
;
 EUCLID (Speck, 1982)
;
_computing_publication_material
;
 All calculations are made at the University of Oviedo on the Scientific 
Computer Centre and X-Ray group ALPHA/AXP-compututer
;
_computing_structure_refinement
;
 Anisotropic least-square carried out with  SHELXS-97 (Sheldrick, 1997).
 Geometric calculations made with PARST (Nardelli, 1983).
;
_computing_structure_solution
;
 direct methods using SHELXS97 (Sheldrick,1997).
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       \w-2\Q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1233
_diffrn_reflns_av_sigmaI/netI    0.1890
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11664
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        13.65
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.2748
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1277P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.2835
_reflns_number_gt                1315
_reflns_number_total             5832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036340csi20030529_012916.cif
_cod_data_source_block           JA036340C
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1277P)^2^+0.0000P] 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^)+(0.1277P)^2^+0.0000P] 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        1671(8)
_cod_database_code               4114208