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_4075641
_publ_section_title
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 Synthesis and Characterization ofN-Heterocyclic Carbene
 Phospha-Palladacycles and Their Properties in Heck Catalysis&#x2020;
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_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         'C43 H38 N3 O2 P Pd'
_chemical_formula_sum            'C43 H38 N3 O2 P Pd'
_chemical_formula_weight         766.15
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                109.4464(4)
_cell_angle_beta                 92.8248(4)
_cell_angle_gamma                112.4486(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4761(1)
_cell_length_b                   12.1957(1)
_cell_length_c                   16.3896(1)
_cell_measurement_reflns_used    6529
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      1.90
_cell_volume                     1787.13(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40884
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
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_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.054
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         6532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0220P)^2^+1.4947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                5888
_reflns_number_total             6532
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om049001gsi20041216_061503.cif
_cod_data_source_block           JSCE-4351-123
_cod_depositor_comments
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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_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 
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_cod_database_code               4075641