Conjugate addition of diethylzinc to α,β-unsaturated lactones catalyzed by copper‒phosphite complexes
Yan, Ming; Zhou, Zhong-Yuan; Chan, Albert S. C.; Chemical Communications  (2000) 115–; doi:10.1039/a908467c

data_7110770
_publ_section_title
;
 Conjugate addition of diethylzinc to \a,\b-unsaturated lactones catalyzed
 by copper--phosphite complexes
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              115
_journal_paper_doi               10.1039/a908467c
_journal_year                    2000
_chemical_formula_sum            'C73 H70 Cu F3 N2 O9 P2 S'
_chemical_formula_weight         1333.85
_chemical_name_common
;
{bis(acetonitrile) 1,1'-bis[(S)-(1,1'-binaphthalene-2,2'-dioxy)phosphinoxy)]
-3,3',5,5'-tetra-tert-butyl-2,2'-biphenyl}copper(I) triflate    
;
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.518(4)
_cell_length_b                   17.524(4)
_cell_length_c                   27.033(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      1.38
_cell_volume                     8299(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker CCD Area Detector'
_diffrn_measurement_method       'PHI AND OMEGA SCAN'
_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  0.1071
_diffrn_reflns_av_sigmaI/netI    0.2207
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52967
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.9340
_exptl_absorpt_correction_T_min  0.9154
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_coef       0.00000(13)
_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   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         18368
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.2114
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                6846
_reflns_number_total             18368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908467csup1.cif
_cod_data_source_block           ym1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7110770