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_4078919
_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 RMITU'
_chemical_formula_moiety         'C72 H50 F8 I P4 Pt2 +, P F6 -, 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H54 Cl4 F14 I P5 Pt2'
_chemical_formula_weight         2022.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-05-31
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record
;
2010-05-31- Report on C74 H54 Cl4 F14 I P5 Pt2 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2010-06-01- passes checkcif tests with minor warnings  
;
_cell_angle_alpha                106.5093(10)
_cell_angle_beta                 93.0296(12)
_cell_angle_gamma                105.5032(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8010(2)
_cell_length_b                   14.8766(3)
_cell_length_c                   20.1361(4)
_cell_measurement_reflns_used    45552
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     3508.17(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 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  0.076
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60765
_diffrn_reflns_theta_full        27.468
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         2.546
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.772
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.915
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.18
_refine_diff_density_min         -1.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9763
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         16027
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.0035730
_refine_ls_shift/su_mean         0.0001
_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: 
 7.69 7.49 2.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1118
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1118
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                13226
_reflns_number_total             16029
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.62
_oxford_diffrn_Wilson_scale      139.11
_oxford_refine_ls_r_factor_ref   0.0740
_oxford_refine_ls_scale          0.102983(19)
_oxford_reflns_number_all        16027
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '5281527 ben1004a'
_cod_data_source_file            om300525p_si_001.cif
_cod_data_source_block           complex11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 '
_cod_database_code               4078919