Bis[μ-bis(diphenylphosphino)methane-κ^2^<i>P</i>:<i>P</i>']bis[(saccharinato-κ<i>N</i>)palladium(I)] dichloromethane solvate
Henderson, William; Nicholson, Brian K.; Chung, Dong C.; Acta Crystallographica Section E 58 (2002) m432–m433; doi:10.1107/S1600536802012515

data_2201634
_publ_section_title
;Bis[\m-bis(diphenylphosphino)methane-\k^2^<i>P</i>:<i>P</i>']bis[(saccharinato-\k<i>N</i>)palladium(I)]
 dichloromethane solvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m432
_journal_page_last               m433
_journal_paper_doi               10.1107/S1600536802012515
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Pd2 (C7 H4 NO3 S)2 (C25 H22 P2)2], C H2 Cl2'
_chemical_formula_moiety         'C64 H52 N2 O6 P4 Pd2 S2, C H2 Cl2'
_chemical_formula_sum            'C65 H54 Cl2 N2 O6 P4 Pd2 S2'
_chemical_formula_weight         1430.80
_chemical_melting_point_gt       503.15
_chemical_name_systematic
;
Bis[\m-bis(diphenylphosphino)methane-\k^2^P:P']bis[(saccharinato-
\kN)palladium(I)] dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.819(4)
_cell_length_b                   22.550(7)
_cell_length_c                   20.230(6)
_cell_measurement_reflns_used    5200
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     5977(3)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SADABS (Sheldrick, 1996)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX(Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens CCD'
_diffrn_measurement_method       multi-scan
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.016
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            74438
_diffrn_reflns_theta_full        26.4
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         12130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.031
_refine_ls_R_factor_gt           0.025
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0324P)^2^+6.6496P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.065
_refine_ls_wR_factor_ref         0.068
_reflns_number_gt                10579
_reflns_number_total             12130
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6069.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>230 degrees celcius'
was changed to '503.15' - it was converted from degrees Celsius(C) to
Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>230 degrees celcius'
was changed to '503.15' - it was converted from degrees Celsius(C) to
Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 /n'
_cod_database_code               2201634
_cod_database_fobs_code          2201634