Synthesis and reactivity of bimetallic palladium(ii) methyl complexes with new functional phosphine ligands
Sub Kim, Jang; Sen, Ayusman; Guzei, Ilia A.; Liable-Sands, Louise M.; Rheingold, Arnold L.; Journal of the Chemical Society, Dalton Transactions  (2002) 4726–; doi:10.1039/b208060p

data_7012151
_publ_section_title
;
 Synthesis and reactivity of bimetallic palladium(ii) methyl complexes
 with new functional phosphine ligands
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4726
_journal_paper_doi               10.1039/b208060p
_journal_year                    2002
_chemical_formula_sum            'C20 H17 Cl4 O P Pd'
_chemical_formula_weight         552.51
_chemical_name_systematic
; 
? 
;
_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
_cell_angle_alpha                94.835(5)
_cell_angle_beta                 90.362(11)
_cell_angle_gamma                91.245(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7474(10)
_cell_length_b                   9.2402(7)
_cell_length_c                   13.0328(13)
_cell_measurement_temperature    243(2)
_cell_volume                     1049.38(18)
_computing_cell_refinement       Siemens/XSCANS
_computing_data_collection       Siemens/XSCANS
_computing_data_reduction        Siemens/XSCANS
_computing_molecular_graphics    XP-5.03
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      243(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10868
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.478
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.763
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.856
_refine_ls_goodness_of_fit_obs   0.875
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_restrained_S_obs      0.875
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_obs          0.0325
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1193
_refine_ls_wR_factor_obs         0.1030
_reflns_number_observed          5545
_reflns_number_total             6114
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b208060p.txt
_cod_data_source_block           sen06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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_cell_volume        1049.4(2)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7012151