Synthesis and Reactivity of (PCP) Palladium Hydroxy Carbonyl and Related Complexes toward CO2and Phenylacetylene
Johansson, Roger; Wendt, Ola F.; Organometallics 26 (2007) 2426–; doi:10.1021/om0611709

data_4072965
_publ_section_title
;
 Synthesis and Reactivity of (PCP) Palladium Hydroxy Carbonyl and Related
 Complexes toward CO2and Phenylacetylene
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2426
_journal_paper_doi               10.1021/om0611709
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C24 H44 P2 Pd'
_chemical_formula_weight         500.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           110
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_symmetry_space_group_name_Hall  'I 4bw -2c'
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.36170(10)
_cell_length_b                   16.36170(10)
_cell_length_c                   19.3825(3)
_cell_measurement_reflns_used    4808
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0943
_cell_measurement_theta_min      2.4373
_cell_volume                     5188.80(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.0 (release 06-01-2006 CrysAlis171 .NET)
(compiled Jan  6 2006,18:17:31)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.0 (release 06-01-2006 CrysAlis171 .NET)
(compiled Jan  6 2006,18:17:31)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.0 (release 06-01-2006 CrysAlis171 .NET)
(compiled Jan  6 2006,18:17:31)
;
_computing_molecular_graphics    'Diamond (Brandenburg)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1829
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0642
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_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
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_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25312
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         33.08
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.0 (release 06-01-2006 CrysAlis171 .NET)
(compiled Jan  6 2006,18:17:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         3862
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                1576
_reflns_number_total             3862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0611709si20070215_095617.cif
_cod_data_source_block           compound4
_cod_original_sg_symbol_H-M      I4(1)cd
_cod_database_code               4072965