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_4078922
_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        ' from RMIT University'
_chemical_formula_moiety         'C55 H38 F8 I P3 Pd2, C6 H6'
_chemical_formula_sum            'C61 H44 F8 I P3 Pd2'
_chemical_formula_weight         1361.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-03-31
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2009-04-01- Report on C61 H44 F8 I P3 Pd2 
             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                 94.7219(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0043(4)
_cell_length_b                   17.8269(5)
_cell_length_c                   18.8760(5)
_cell_measurement_reflns_used    593093
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      2.6
_cell_volume                     6037.9(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), 
SQUEEZE (van der Sluis & Spek, 1990) 

;
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.090
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            90356
_diffrn_reflns_theta_full        27.360
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_min         2.594
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.725
_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    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.03
_refine_diff_density_min         -1.99
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8295
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         13911
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.016704
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1118
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1118
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7677
_reflns_number_total             13915
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.71
_oxford_diffrn_Wilson_scale      57.90
_oxford_refine_ls_r_factor_ref   0.0976
_oxford_refine_ls_scale          0.13976(4)
_oxford_reflns_number_all        13911
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '3301142 ben0908a  squeezed'
_cod_data_source_file            om300525p_si_001.cif
_cod_data_source_block           complex14
_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/a 1 '
_cod_database_code               4078922