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_4078916
_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_absolute_configuration ad
_chemical_compound_source        'from RMITU'
_chemical_formula_moiety         'C46 H38 F8 N2 P2 Pd2'
_chemical_formula_sum            'C46 H38 F8 N2 P2 Pd2'
_chemical_formula_weight         1045.55
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-07-10
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2008-07-10 - Report on C46 H38 F8 N2 P2 Pd2
              by   Anthony C. Willis
              for  Steven Priver and Martin Bennett

2008-07-10 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2048(2)
_cell_length_b                   12.2048(2)
_cell_length_c                   30.1528(4)
_cell_measurement_reflns_used    91602
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.6
_cell_volume                     4491.47(12)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.039
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            68853
_diffrn_reflns_theta_full        30.011
_diffrn_reflns_theta_max         30.011
_diffrn_reflns_theta_min         3.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.42
_refine_ls_abs_structure_details 'Flack (1983), 2748 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.022(19)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.041084
_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:
  19.1 28.7 16.9 7.07 1.29
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0537
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0537
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              42
_reflns_limit_l_min              0
_reflns_number_gt                5518
_reflns_number_total             6518
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      9.57
_oxford_refine_ls_r_factor_ref   0.0268
_oxford_refine_ls_scale          0.36626(19)
_oxford_reflns_number_all        6514
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '7091629 ben0803'
_cod_data_source_file            om300525p_si_001.cif
_cod_data_source_block           complex8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 41 21 2 '
_cod_database_code               4078916