Synthesis and characterization of complexes of PdII and PtII containing the iminophosphorane ligand Ph3PNCN
Falvello, Larry R.; Fernández, Susana; García, María M.; Navarro, Rafael; Urriolabeitia, Esteban P.; Journal of the Chemical Society, Dalton Transactions  (1998) 3745–; doi:10.1039/a805147j

data_7026999
_publ_section_title
;
 Synthesis and characterization of complexes of PdII and PtII containing
 the iminophosphorane ligand Ph3P&#xE006;NC&#xE007;N
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3745
_journal_paper_doi               10.1039/a805147j
_journal_year                    1998
_chemical_formula_sum            'C38 H30 Cl2 N4 P2 Pd'
_chemical_formula_weight         781.90
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.862(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5452(7)
_cell_length_b                   12.9923(5)
_cell_length_c                   13.8799(7)
_cell_measurement_temperature    150(2)
_cell_volume                     1717.39(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3226
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.85904
_exptl_absorpt_correction_T_min  0.69596
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_obs          0.0349
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1006
_refine_ls_wR_factor_obs         0.0937
_reflns_number_observed          2595
_reflns_number_total             3022
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            805147jsup1.cif
_cod_data_source_block           cad6
_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 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.4530P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.4530P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1717.4(2)
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               7026999