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_4082241
_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 Ag Cl P2 Pd2'
_chemical_formula_weight         1115.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_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                 101.392(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1373(10)
_cell_length_b                   18.8145(19)
_cell_length_c                   24.316(5)
_cell_measurement_reflns_used    1539
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5246
_cell_measurement_theta_min      3.0891
_cell_volume                     4994.9(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.1088
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18190
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97213
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.2911
_exptl_crystal_size_mid          0.1305
_exptl_crystal_size_min          0.0432
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9075
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.815
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                4014
_reflns_number_total             9075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4005498_si_003.cif
_cod_data_source_block           imb293
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-18343/cifs/4082241.cif.
;
_cod_original_cell_volume        4994.9(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4082241