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_4078920
_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 RMIT University'
_chemical_formula_moiety         'C54 H35 F8 I2 P3 Pd2, 0.5(C5 H12), 0.5(C6 H6)'
_chemical_formula_sum            'C59.5 H44 F8 I2 P3 Pd2'
_chemical_formula_weight         1470.52
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-04-14
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2009-04-15- Report on C119 H88 F16 I4 P6 Pd4 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-04-01- passes checkcif tests with minor warnings  
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3916(2)
_cell_length_b                   21.7240(4)
_cell_length_c                   44.4879(8)
_cell_measurement_reflns_used    259723
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     11009.5(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.048
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            84781
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.559
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5728
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.77
_refine_ls_abs_structure_details 'Flack (1983), 8714 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.032(15)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.7691
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         19307
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.036267
_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: 
 20.5 29.6 14.9 4.08 0.00 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0937
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0937
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              52
_reflns_limit_l_min              0
_reflns_number_gt                16087
_reflns_number_total             19318
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.87
_oxford_diffrn_Wilson_scale      136.21
_oxford_refine_ls_r_factor_ref   0.0405
_oxford_refine_ls_scale          0.096091(13)
_oxford_reflns_number_all        19307
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '4091457 ben0909'
_cod_data_source_file            om300525p_si_001.cif
_cod_data_source_block           complex12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C119 H88 F16 I4 P6 Pd4'
_cod_original_formula_weight         2941.04
_cod_original_formula_moiety
;
2(C54 H35 F8 I2 P3 Pd2), C5 H12, C6 H6
;
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4078920