Interaction of PdCl2-2-(β-diphenylphosphine)ethylpyridine Complex with Diols and CO: Synthesis of New Alkoxycarbonyl Complexes, Key Intermediates to Cyclic Carbonates
Giannoccaro, Potenzo; Cornacchia, Daniele; Doronzo, Salvatore; Mesto, Ernesto; Quaranta, Eugenio; Aresta, Michele; Organometallics 25 (2006) 2872–; doi:10.1021/om060012e

data_4075054
_publ_section_title
;
 Interaction of PdCl2-2-(\b-diphenylphosphine)ethylpyridine Complex with
 Diols and CO:&#x00A0; Synthesis of New Alkoxycarbonyl Complexes, Key
 Intermediates to Cyclic Carbonates
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2872
_journal_paper_doi               10.1021/om060012e
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C24 H27 Cl1 N1 O3 P1 Pd1'
_chemical_formula_sum            'C24 H27 Cl N O3 P Pd'
_chemical_formula_weight         550.31
_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             06-03-15
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                103.270(10)
_cell_angle_beta                 97.060(10)
_cell_angle_gamma                89.980(10)
_cell_formula_units_Z            4
_cell_length_a                   11.0550(10)
_cell_length_b                   12.4860(10)
_cell_length_c                   19.6470(10)
_cell_measurement_reflns_used    4362
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2618.4(4)
_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    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44408
_diffrn_reflns_theta_full        20.823
_diffrn_reflns_theta_max         20.823
_diffrn_reflns_theta_min         1.676
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       plate
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.66
_refine_ls_goodness_of_fit_ref   1.0835
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1162
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.032963
_refine_ls_structure_factor_coef F
_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: 
 67.6 -77.4 36.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0938
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0644
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                1162
_reflns_number_total             5470
_reflns_threshold_expression     I>5.00u(I)
_cod_data_source_file            om060012esi20060321_040518.cif
_cod_data_source_block           4d_cif
_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.

'_refine_ls_hydrogen_treatment' value 'refu' changed to
'refU' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C24 H27 Cl1 N1 O3 P1 Pd1'
_cod_database_code               4075054