Palladium(II) Pyrazolin-4-ylidenes: Remote N-Heterocyclic Carbene Complexes and Their Catalytic Application in Aqueous Suzuki−Miyaura Coupling
Han, Yuan; Huynh, Han Vinh; Tan, Geok Kheng; Organometallics 26 (2007) 6581–; doi:10.1021/om7009107

data_4074074
_publ_section_title
;
 Palladium(II) Pyrazolin-4-ylidenes: Remote N-Heterocyclic Carbene
 Complexes and Their Catalytic Application in Aqueous
 Suzuki&#x2212;Miyaura Coupling
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6581
_journal_paper_doi               10.1021/om7009107
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C46 H46 Cl2 F3 I N2 O3 P2 Pd S'
_chemical_formula_weight         1130.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0914(5)
_cell_length_b                   22.4737(11)
_cell_length_c                   20.9892(11)
_cell_measurement_reflns_used    2756
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      21.09
_cell_measurement_theta_min      2.42
_cell_volume                     4760.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32206
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.9253
_exptl_absorpt_correction_T_min  0.7262
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5584
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+17.9330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                4057
_reflns_number_total             5584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7009107-file003.cif
_cod_data_source_block           6350a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      Pnma
_cod_database_code               4074074