Palladium-Allyl Phosphoramidite Complexes: Solid-State Structures and Solution Dynamics
Filipuzzi, Serena; Pregosin, Paul S.; Albinati, Alberto; Rizzato, Silvia; Organometallics 25 (2006) 5955–; doi:10.1021/om060726p

data_4074519
_publ_section_title
;
 Palladium-Allyl Phosphoramidite Complexes:&#x00A0; Solid-State Structures
 and Solution Dynamics
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5955
_journal_paper_doi               10.1021/om060726p
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C80 H76 Cl2 N2 O12 P2 Pd2'
_chemical_formula_weight         1603.07
_chemical_name_common            '[PdCl(2-methallyl)(phosphoramidite)]'
_space_group_IT_number           1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.181(8)
_cell_angle_beta                 89.777(8)
_cell_angle_gamma                77.530(8)
_cell_formula_units_Z            2
_cell_length_a                   9.710(3)
_cell_length_b                   13.593(4)
_cell_length_c                   15.154(5)
_cell_measurement_reflns_used    2177
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.37
_cell_measurement_theta_min      2.15
_cell_volume                     1945.8(11)
_computing_cell_refinement       'SAINTPLUS  (Bruker AXS, 1999)'
_computing_data_collection       'SMART      (Bruker AXS, 2001)'
_computing_data_reduction        'SAINTPLUS  (Bruker AXS, 1999)'
_computing_molecular_graphics
'ORTEP for Windows v1.074 (L.J. Farrugia 1997)'
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia,J. Appl. Cryst.,1999,32, 837)'
_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_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.1419
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16316
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4625
_exptl_absorpt_correction_type   'empirical, multiscan'
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.832
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         13490
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0913
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.106
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.2406
_reflns_number_gt                10212
_reflns_number_total             13490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060726psi20060809_103629.cif
_cod_data_source_block           preg109
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 
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_cod_database_code               4074519
_compound_number                 4