A Dinuclear Palladium(I) Ethynyl Complex: Synthesis, Structure, and Dynamics
Krause, Jochen; Goddard, Richard; Mynott, Richard; Pörschke, Klaus-Richard; Organometallics 20 (2001) 1992–; doi:10.1021/om000765f

data_4077215
_publ_section_title
;
 A Dinuclear Palladium(I) Ethynyl Complex:&#x00A0; Synthesis, Structure,
 and Dynamics
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1992
_journal_paper_doi               10.1021/om000765f
_journal_volume                  20
_journal_year                    2001
_chemical_compound_source        'see paper'
_chemical_formula_sum            'C23 H48 P2 Pd2'
_chemical_formula_weight         599.35
_chemical_name_systematic
; 
  (\m^2^-\h^1^,\h^2^-ethynyl)(\m^2^-allyl)-bis(triphenylphosphine)-di-
  palladium(i)
;
_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                90.00
_cell_angle_beta                 100.400(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6670(12)
_cell_length_b                   15.6860(14)
_cell_length_c                   15.0290(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      21.4
_cell_measurement_theta_min      10.4
_cell_volume                     2705.3(4)
_computing_cell_refinement
'EXPRESS / CAD4 software (Enraf-Nonius, 1995)'
_computing_data_collection
'EXPRESS / CAD4 software (Enraf-Nonius, 1995)'
_computing_data_reduction
' DATAP (Coppens,Leiserowitz & Rabinovich, 1965)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8251
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
'Dwiggins, C.W., (1975), Acta Cryst., A31, 395-396'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.479
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         7854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.6501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                6304
_reflns_number_total             7854
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om000765f.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4077215