Preparation, Structure, and Reactivity of Dipalladium(I) Complexes Containing the Carbanion 2-C6F4PPh2: Coexistence of Distinct, Noninterconverting Head-to-Head [Dipalladium(0/II)] and Head-to-Tail [Dipalladium(I)] Species
Bhargava, Suresh K.; Privér, Steven H.; Willis, Anthony C.; Bennett, Martin A.; Organometallics 31 (2012) 5561–; doi:10.1021/om300525p

data_4078913
_publ_section_title
;
 Preparation, Structure, and Reactivity of Dipalladium(I) Complexes
 Containing the Carbanion 2-C6F4PPh2: Coexistence of Distinct,
 Noninterconverting Head-to-Head [Dipalladium(0/II)] and Head-to-Tail
 [Dipalladium(I)] Species
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5561
_journal_paper_doi               10.1021/om300525p
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        local
_chemical_formula_moiety         'C72 H50 F8 P4 Pd2'
_chemical_formula_sum            'C72 H50 F8 P4 Pd2'
_chemical_formula_weight         1403.87
_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
_audit_creation_date             08-06-12
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2008-06-12 - Report on C72 H50 F8 P4 Pd2
              by   Anthony C. Willis
              for  Steven Priver and Martin Bennett

2008-06-12 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0380(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9954(1)
_cell_length_b                   22.8850(2)
_cell_length_c                   20.2845(2)
_cell_measurement_reflns_used    104919
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     6024.13(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            123653
_diffrn_reflns_theta_full        27.478
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.610
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9632
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13794
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.002611
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
  Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
  [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
  where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
  Method = Robust Weighting (Prince, 1982)
  W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
  A~i~ are:
  11.3 16.4 8.40 2.53
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0754
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0754
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                9166
_reflns_number_total             13794
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.85
_oxford_diffrn_Wilson_scale      70.17
_oxford_refine_ls_r_factor_ref   0.0509
_oxford_refine_ls_scale          0.12611(2)
_oxford_reflns_number_all        13794
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '6061518 ben0802'
_cod_data_source_file            om300525p_si_001.cif
_cod_data_source_block           complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4078913