Synthesis, characterization, and catalytic activity of N-heterocyclic carbene (NHC) palladacycle complexes.
Viciu, Mihai S.; Kelly, 3rd, Roy A; Stevens, Edwin D.; Naud, Frédéric; Studer, Martin; Nolan, Steven P.; Organic letters 5 (2003) 1479–1482; doi:10.1021/ol034264c

data_1507287
_publ_section_title
;
 Synthesis, characterization, and catalytic activity of N-heterocyclic
 carbene (NHC) palladacycle complexes.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              1479
_journal_page_last               1482
_journal_paper_doi               10.1021/ol034264c
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C41 H50 Cl N3 Pd'
_chemical_formula_weight         726.69
_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                84.1240(10)
_cell_angle_beta                 88.6030(10)
_cell_angle_gamma                79.4620(10)
_cell_formula_units_Z            4
_cell_length_a                   9.7883(7)
_cell_length_b                   19.5135(13)
_cell_length_c                   19.8075(13)
_cell_measurement_reflns_used    20066
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.846
_cell_measurement_theta_min      2.191
_cell_volume                     3699.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.891
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36619
_diffrn_reflns_theta_full        29.06
_diffrn_reflns_theta_max         29.06
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.647005
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       wedge
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.083
_refine_diff_density_min         -1.821
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.0007(2)
_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   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         17634
_refine_ls_number_restraints     824
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+2.1614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                12794
_reflns_number_total             17634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol034264csi20030214_080355.cif
_cod_data_source_block           nol105
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1507287