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_4069414
_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 H66 Cl2 N4 P2 Pd'
_chemical_formula_sum            'C60 H66 Cl2 N4 P2 Pd'
_chemical_formula_weight         1082.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 98.309(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.363(2)
_cell_length_b                   22.507(5)
_cell_length_c                   13.716(2)
_cell_measurement_reflns_used    376
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     2860.1(10)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19621
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6848
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.8400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                4234
_reflns_number_total             6848
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900185r_si_003.cif
_cod_data_source_block           pdcl1m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        2860.2(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4069414