Synthesis and Characterization ofN-Heterocyclic Carbene Phospha-Palladacycles and Their Properties in Heck Catalysis†
Frey, Guido D.; Schütz, Jan; Herdtweck, Eberhardt; Herrmann, Wolfgang A.; Organometallics 24 (2005) 4416–; doi:10.1021/om049001g

data_4075642
_publ_section_title
;
 Synthesis and Characterization ofN-Heterocyclic Carbene
 Phospha-Palladacycles and Their Properties in Heck Catalysis&#x2020;
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4416
_journal_paper_doi               10.1021/om049001g
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C51 H68 N4 P Pd, C6 H12 O2, C2 H3 O2'
_chemical_formula_sum            'C59 H83 N4 O4 P Pd'
_chemical_formula_weight         1049.68
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.103(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6600(1)
_cell_length_b                   13.4585(2)
_cell_length_c                   38.2426(9)
_cell_measurement_reflns_used    7938
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      1.60
_cell_volume                     5472.51(16)
_computing_cell_refinement       'DENZO (Nonius, 2001b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_data_reduction        'DENZO (Nonius, 2001b)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            83297
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.062
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         9981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0375P)^2^+2.6313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                7779
_reflns_number_total             9981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om049001gsi20041216_061503.cif
_cod_data_source_block           FREE-4353-123
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075642