Phosphine and arsine adducts of N-donor palladacycles as catalysts in the Suzuki coupling of aryl bromides
Robin B. Bedford; Catherine S. J. Cazin; Simon J. Coles; Thomas Gelbrich; Michael B. Hursthouse; Véronique J. M. Scordia; Dalton Trans.  (2003) 3350–3356; doi:10.1039/B304053D

data_7013078
_publ_section_title
;
 Phosphine and arsine adducts of N-donor palladacycles as catalysts in
 the Suzuki coupling of aryl bromides
;
_journal_issue                   17
_journal_name_full               'Dalton Trans.'
_journal_page_first              3350
_journal_page_last               3356
_journal_paper_doi               10.1039/B304053D
_journal_year                    2003
_chemical_formula_sum            'C27.5 H27 Cl1.5 N O0.5 P Pd'
_chemical_formula_weight         570.05
_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-97
_cell_angle_alpha                64.56(2)
_cell_angle_beta                 86.38(3)
_cell_angle_gamma                73.77(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4871(19)
_cell_length_b                   13.833(3)
_cell_length_c                   15.203(4)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      5.11
_cell_volume                     1726.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.725
_diffrn_measured_fraction_theta_max 0.725
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8990
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.9727
_exptl_absorpt_correction_T_min  0.8079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             579
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.418
_refine_diff_density_min         -2.359
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5746
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.1043
_refine_ls_shift/su_max          0.151
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1121P)^2^+32.4493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2581
_refine_ls_wR_factor_ref         0.2677
_reflns_number_gt                4739
_reflns_number_total             5746
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            B304053D.txt
_cod_data_source_block           10f
_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 
;
_cod_original_cell_volume        1726.2(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C27.50 H27 Cl1.50 N O0.50 P Pd'
_cod_database_code               7013078