Synthesis of homoallylic amines by hydrozirconation-imine addition of allenes.
Wipf, Peter; Pierce, Joshua G.; Organic letters 7 (2005) 3537–3540; doi:10.1021/ol051266j

data_1506646
_publ_section_title
;
 Synthesis of homoallylic amines by hydrozirconation-imine addition of
 allenes.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              3537
_journal_page_last               3540
_journal_paper_doi               10.1021/ol051266j
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C28 H36 N O P Si'
_chemical_formula_weight         461.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_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                90.8020(10)
_cell_angle_beta                 90.8930(10)
_cell_angle_gamma                105.9470(10)
_cell_formula_units_Z            4
_cell_length_a                   10.9347(5)
_cell_length_b                   13.4323(6)
_cell_length_c                   19.5642(9)
_cell_measurement_reflns_used    5882
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.37
_cell_volume                     2762.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24398
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_refine_diff_density_max         0.474
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                6338
_reflns_number_total             10854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol051266jsi20050530_111849.cif
_cod_data_source_block           jp1027s
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1506646