Synthesis and characterization of palladium(II) complexes with the α-stabilized phosphoylide ligand Ph3PC(H)CONMe2
Barco, Isabel C.; Falvello, Larry R.; Fernández, Susana; Navarro, Rafael; Urriolabeitia, Esteban P.; Journal of the Chemical Society, Dalton Transactions  (1998) 1699–; doi:10.1039/a708950c

data_7027964
_publ_section_title
;
 Synthesis and characterization of palladium(II) complexes with the
 \a-stabilized phosphoylide ligand Ph3P&#xE006;C(H)CONMe2
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1699
_journal_paper_doi               10.1039/a708950c
_journal_year                    1998
_chemical_formula_analytical     'C31 H33 Cl N2 O6 P Pd.0.5CH2Cl2'
_chemical_formula_moiety         '[Pd(dmba)(Ph3PCHCONMe2)(OH2)]ClO4.0.5CH2Cl2'
_chemical_formula_sum            'C31.5 H34 Cl2 N2 O6 P Pd'
_chemical_formula_weight         744.88
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2080(10)
_cell_length_b                   10.204(2)
_cell_length_c                   31.345(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      22.5
_cell_volume                     3225.0(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       \w
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.1269
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            6029
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.02
_diffrn_standards_interval_time  10800
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.765
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.967
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5663
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.967
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_obs          0.0616
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1519
_refine_ls_wR_factor_obs         0.1327
_reflns_number_observed          3362
_reflns_number_total             5663
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            c708950sup1.cif
_cod_data_source_block           (1)0.5CH2Cl2
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.0000P] 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^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C31.50 H34 Cl2 N2 O6 P Pd'
_cod_database_code               7027964