Synthesis and chemistry of diphenyl-2-pyridylphosphine complexes of palladium(0). X-Ray characterisation of Pd(Ph2Ppy)2(η2-DMAD) and trans-Pd(Ph2Ppy)2(PhCCH2)(CF3CO2)
Dervisi, Athanasia; Edwards, Peter G.; Newman, Paul D.; Tooze, Robert P.; Journal of the Chemical Society, Dalton Transactions  (2000) 523–; doi:10.1039/a908050c

data_7009008
_publ_section_title
;
 Synthesis and chemistry of diphenyl-2-pyridylphosphine complexes of
 palladium(0). X-Ray characterisation of Pd(Ph2Ppy)2(\h2-DMAD) and
 trans-Pd(Ph2Ppy)2(PhC&#xE006;CH2)(CF3CO2)
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              523
_journal_paper_doi               10.1039/a908050c
_journal_year                    2000
_chemical_formula_sum            'C44 H35 F3 N2 O2 P2 Pd'
_chemical_formula_weight         849.08
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.32(7)
_cell_angle_beta                 103.28(2)
_cell_angle_gamma                110.28(3)
_cell_formula_units_Z            2
_cell_length_a                   11.837(2)
_cell_length_b                   13.342(7)
_cell_length_c                   13.729(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1943.8(14)
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_sigmaI/netI    0.5634
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7136
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.614
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_F_000             864
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.437
_refine_ls_goodness_of_fit_obs   0.645
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5013
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.511
_refine_ls_restrained_S_obs      0.797
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         7.713
_refine_ls_shift/esd_mean        0.125
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0740
_refine_ls_wR_factor_obs         0.0587
_reflns_number_observed          1828
_reflns_number_total             5014
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908050c.txt
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_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1943.8(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009008