Heterometallic Complexes by Transmetalation of Alkynyl Groups from Copper or Silver to Allyl Palladium Complexes: Demetalation Studies and Alkynyl Homocoupling
Meana, Isabel; Espinet, Pablo; Albéniz, Ana C.; Organometallics 33 (2014) 1–; doi:10.1021/om4005498

data_4082239
_publ_contact_author
;
 Ana Carmen Albeniz
 IU CINQUIMA/Quimica Inorganica
 Facultad de Ciencias
 Universidad de Valladolid
 E47071
 Valladolid
 Spain
;
_publ_section_title
;
 Heterometallic Complexes by Transmetalation of Alkynyl Groups from Copper
 or Silver to Allyl Palladium Complexes: Demetalation Studies and Alkynyl
 Homocoupling
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              1
_journal_paper_doi               10.1021/om4005498
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C54 H48 Cl2 Cu2 P2 Pd2'
_chemical_formula_weight         1169.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   20.1012(5)
_cell_length_b                   11.2224(2)
_cell_length_c                   22.9667(5)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4834
_cell_measurement_theta_min      2.8414
_cell_volume                     5180.91(19)
_computing_cell_refinement
;
'Mon May 31 11:44:38 2010'
;
_computing_data_collection
;
'Mon May 31 11:44:38 2010'
;
_computing_data_reduction
;
'Mon May 31 11:44:38 2010'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -42.00   67.00   1.0000  173.8500
omega____ theta____ kappa____ phi______ frames
    -       -9.3771   70.0000  -27.0000 109
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12684
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.2911
_exptl_crystal_size_mid          0.1305
_exptl_crystal_size_min          0.0432
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                3193
_reflns_number_total             4717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4005498_si_003.cif
_cod_data_source_block           imb2582b
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-18343/cifs/4082239.cif.
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4082239