Cascade Cyclizations and Couplings Involving Nickel Enolates
Gireesh M. Mahandru; Andy R. L. Skauge; Sanjoy K. Chowdhury; Kande K. D. Amarasinghe; Mary Jane Heeg; John Montgomery; Journal of the American Chemical Society 125 (2003) 13481–13485; doi:10.1021/ja037423w

data_4114320
_publ_section_title
;
 Cascade Cyclizations and Couplings Involving Nickel Enolates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13481
_journal_page_last               13485
_journal_paper_doi               10.1021/ja037423w
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C17 H20 O'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 98.632(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   16.0423(15)
_cell_length_b                   16.0437(16)
_cell_length_c                   21.991(2)
_cell_measurement_reflns_used    861
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.
_cell_measurement_theta_min      2.7
_cell_volume                     5595.9(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_method       'SMART CCD'
_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  0.12
_diffrn_reflns_av_sigmaI/netI    0.2799
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9891
_exptl_absorpt_correction_T_min  0.9864
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       'rectangular squares'
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0024(3)
_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_ref   0.766
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         13279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.766
_refine_ls_R_factor_all          0.2863
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0929P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                3041
_reflns_number_total             13279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037423wsi20030715_122150.cif
_cod_data_source_block           girs
_cod_original_cell_volume        5596.0(10)
_cod_database_code               4114320