Reactivity of chiral diiminodiphosphine ligands towards PdCl2(PhCN)2: synthesis and crystal structures of two unexpected dinuclear palladium(II) complexes
Wong, Wai-Kwok; Zhang, Li-Lu; Chen, Yang; Wong, Wai-Yeung; Wong, Wing-Tak; Xue, Feng; Mak, Thomas C. W.; Journal of the Chemical Society, Dalton Transactions  (2000) 1397–; doi:10.1039/b001245i

data_7009466
_publ_section_title
;
 Reactivity of chiral diiminodiphosphine ligands towards PdCl2(PhCN)2:
 synthesis and crystal structures of two unexpected dinuclear
 palladium(II) complexes
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1397
_journal_paper_doi               10.1039/b001245i
_journal_year                    2000
_chemical_formula_sum            'C65 H55 Cl4 N2 O P3 Pd2'
_chemical_formula_weight         1327.62
_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-97
_cell_angle_alpha                80.03(1)
_cell_angle_beta                 75.67(1)
_cell_angle_gamma                81.04(1)
_cell_formula_units_Z            2
_cell_length_a                   12.574(1)
_cell_length_b                   13.636(1)
_cell_length_c                   20.058(1)
_cell_measurement_reflns_used    159
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3258.8(4)
_computing_cell_refinement       'BioteX 1.0 (MSC, 1995)'
_computing_data_collection       'BioteX 1.0 (MSC, 1995)'
_computing_data_reduction        'BioteX 1.0 (MSC, 1995)'
_computing_molecular_graphics    'SHELXTL-PC (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.754
_diffrn_measured_fraction_theta_max 0.754
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
Data was collected to 0.82\%A and 85% completeness by taking
28 oscillation photos in the range of 0 - 162\%, \D\f = 6\%,
8 min. per frame.  Crystal to detector distance is 78.146mm,
background level -50.
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;
Rigaku RU-200 rotating-anode generator powered at 50kV/90mA
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9163
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.144
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0056(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     1113
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                7937
_reflns_number_total             9163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001245i.txt
_cod_data_source_block           XF138
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009466