Highly Stereoselective Olefin Cyclopropanation of Diazooxindoles Catalyzed by a C2-Symmetric Spiroketal Bisphosphine/Au(I) Complex
Zhong-Yan Cao; Xiaoming Wang; Chen Tan; Xiao-Li Zhao; Jian Zhou; Kuiling Ding; Journal of the American Chemical Society 135 (2013) 8197–8200; doi:10.1021/ja4040895

data_4119872
_publ_section_title
;
 Highly Stereoselective Olefin Cyclopropanation of Diazooxindoles
 Catalyzed by a C2-Symmetric Spiroketal Bisphosphine/Au(I) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8197
_journal_page_last               8200
_journal_paper_doi               10.1021/ja4040895
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C45 H38 Au2 Cl4 O2.66667 P2'
_chemical_formula_weight         1219.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.724(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   14.3605(9)
_cell_length_b                   33.178(2)
_cell_length_c                   14.9816(9)
_cell_measurement_temperature    296(2)
_cell_volume                     6836.1(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            79512
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    6.772
_exptl_absorpt_correction_T_max  0.2529
_exptl_absorpt_correction_T_min  0.1776
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.059
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1480
_refine_ls_number_reflns         23549
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+9.0638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                18012
_reflns_number_total             23549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4040895_si_004.cif
_cod_data_source_block           z
_cod_database_code               4119872