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_4082240
_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            'C58 H40 Cl2 Cu2 P2 Pd2'
_chemical_formula_weight         1209.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.057(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7943(3)
_cell_length_b                   17.6745(5)
_cell_length_c                   13.7175(4)
_cell_measurement_reflns_used    4589
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6927
_cell_measurement_theta_min      3.0014
_cell_volume                     2584.45(13)
_computing_cell_refinement
;
'Thu May 27 19:52:38 2010'
;
_computing_data_collection
;
'Thu May 27 19:52:38 2010'
;
_computing_data_reduction
;
'Thu May 27 19:52:38 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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -13.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3979   77.0000  -60.0000 89

  2 omega   -3.00   67.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3979   37.0000 -120.0000 70

;
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9534
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
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            YELLOW
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.1921
_exptl_crystal_size_mid          0.1136
_exptl_crystal_size_min          0.0890
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                3276
_reflns_number_total             4686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4005498_si_003.cif
_cod_data_source_block           imb261
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-18343/cifs/4082240.cif.
;
_cod_original_cell_volume        2584.44(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4082240
_cell_oxdiff_length_a            10.7948(3)
_cell_oxdiff_length_b            17.6714(6)
_cell_oxdiff_length_c            13.7180(6)
_cell_oxdiff_angle_alpha         89.925(3)
_cell_oxdiff_angle_beta          99.022(3)
_cell_oxdiff_angle_gamma         89.982(3)
_cell_oxdiff_volume              2584.44(17)
_cell_oxdiff_measurement_reflns_used 4589