Platinum and Palladium Imido and Oxo Complexes with Small Natural Bite Angle Diphosphine Ligands
U. Anandhi; Todd Holbert; Dennis Lueng; Paul R. Sharp; Inorganic Chemistry 42 (2003) 1282–1295; doi:10.1021/ic025987f

data_4313163
_publ_contact_author
;
 Paul R. Sharp
 Department of Chemistry
 University of Missouri
 Columbia, MO  65211
;
_publ_contact_author_email       SharpP@missouri.edu
_publ_contact_author_fax         573-882-2754
_publ_contact_author_phone       573-882-7715
_publ_section_title
;
 Platinum and Palladium Imido and Oxo Complexes with Small Natural Bite
 Angle Diphosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1282
_journal_page_last               1295
_journal_paper_doi               10.1021/ic025987f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C44 H46 Cl2 F6 N2 O6 P2 Pd S2'
_chemical_formula_weight         1116.19
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.659(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.678(2)
_cell_length_b                   12.1036(19)
_cell_length_c                   31.804(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4878.3(13)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
 ORTEP (Johnson, 1976), ORTEP 3 for Windows
 L. J. Farrugia, 1997' 
;
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement
;
 SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
 SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            29654
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.8708
_exptl_absorpt_correction_T_min  0.7401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).   
;
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         10722
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.644
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+6.0632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                8436
_reflns_number_total             10722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025987f-2_s1_4.cif
_cod_data_source_block
'[Pd(NH2-4-tol)2(dppip)](OTf)2_7_(L2=dppip,X=OTf)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4878.4(13)
_cod_database_code               4313163