Synthesis of Aminoiminophosphoranate Complexes of Palladium and Platinum and X-ray Diffractional Investigation of the Weak C−H···Pd Interactions Affecting the Geometry of the PdNPN Metallacycles
Peganova, Tat’yana A.; Valyaeva, Anna V.; Kalsin, Alexander M.; Petrovskii, Pavel V.; Borissova, Alexandra O.; Lyssenko, Konstantin A.; Ustynyuk, Nikolai A.; Organometallics 28 (2009) 3021–; doi:10.1021/om900185r

data_4069413
_publ_section_title
;
 Synthesis of Aminoiminophosphoranate Complexes of Palladium and Platinum
 and X-ray Diffractional Investigation of the Weak
 C&#x2212;H&#x00B7;&#x00B7;&#x00B7;Pd Interactions Affecting the Geometry
 of the PdNPN Metallacycles
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3021
_journal_paper_doi               10.1021/om900185r
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C60 H64 N4 P2 Pd'
_chemical_formula_sum            'C60 H64 N4 P2 Pd'
_chemical_formula_weight         1009.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                85.5530(10)
_cell_angle_beta                 70.2530(10)
_cell_angle_gamma                79.4690(10)
_cell_formula_units_Z            1
_cell_length_a                   9.3444(2)
_cell_length_b                   11.5954(2)
_cell_length_c                   12.9651(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      3
_cell_volume                     1299.72(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       '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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79234
_diffrn_reflns_theta_full        50.00
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.504
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         25522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.5124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                22940
_reflns_number_total             25522
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900185r_si_002.cif
_cod_data_source_block           pd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4069413