Nitrogen- vs Carbon-Coordination of the α-Cyano-Stabilized Phosphorus Ylide Ph3PC(H)CN. X-ray Crystal Structure of {Pd(dmba)[P(OMe)3][N\τbCC(H)PPh3]}(ClO4)
Larry R. Falvello; Susana Fernández; Rafael Navarro; Esteban P. Urriolabeitia; Inorganic Chemistry 36 (1997) 1136–1142; doi:10.1021/ic960904e

data_4323338
_publ_section_title
;
 Nitrogen- vs Carbon-Coordination of the \a-Cyano-Stabilized Phosphorus
 Ylide Ph3PC(H)CN. X-ray Crystal Structure of
 {Pd(dmba)[P(OMe)3][N\\tbCC(H)PPh3]}(ClO4)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1136
_journal_page_last               1142
_journal_paper_doi               10.1021/ic960904e
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C32 H37 Cl N2 O7 P2 Pd'
_chemical_formula_weight         765.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5690(10)
_cell_length_b                   17.857(2)
_cell_length_c                   14.729(2)
_cell_measurement_temperature    150(1)
_cell_volume                     3302.5(6)
_computing_cell_refinement       'CAD4-PC V1.5'
_computing_data_collection       'CAD4-PC V1.5'
_computing_data_reduction        'XCAD4B (Harms, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measurement_device       'Nonius CAD-4'
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6085
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.098
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5790
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_obs          0.0384
_refine_ls_shift/esd_max         -0.484
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+2.8963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1003
_refine_ls_wR_factor_obs         0.0961
_reflns_number_observed          4881
_reflns_number_total             5790
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960904e.cif
_cod_data_source_block           nieve
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+2.8963P] 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^)+(0.0532P)^2^+2.8963P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323338