Activation of a σ-SnSn Bond at Copper, Followed by Double Addition to an Alkyne
Nicolas Lassauque; Pauline Gualco; Sonia Mallet-Ladeira; Karinne Miqueu; Abderrahmane Amgoune; Didier Bourissou; Journal of the American Chemical Society 135 (2013) 13827–13834; doi:10.1021/ja405516j

data_4120792
_publ_section_title
;
 Activation of a \s-SnSn Bond at Copper, Followed by Double Addition to an
 Alkyne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13827
_journal_page_last               13834
_journal_paper_doi               10.1021/ja405516j
_journal_volume                  135
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C32 H12 B F24, C44 H44 Cu O2 P2 Sn2, 2(C H2 Cl2)'
_chemical_formula_sum            'C78 H60 B Cl4 Cu F24 O2 P2 Sn2'
_chemical_formula_weight         2000.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.553(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.154(4)
_cell_length_b                   13.161(2)
_cell_length_c                   31.163(4)
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.33
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     8227(2)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            120510
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.1
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.9153
_exptl_absorpt_correction_T_min  0.7006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       plate
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.539
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         16702
_refine_ls_number_restraints     819
_refine_ls_restrained_S_all      1.18
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+53.6073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                14824
_reflns_number_total             16702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405516j_si_002_5.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4120792