Chiral Palladium Bis(acyclic diaminocarbene) Complexes as Enantioselective Catalysts for the Aza-Claisen Rearrangement
Wanniarachchi, Yoshitha A.; Kogiso, Yuri; Slaughter, LeGrande M.; Organometallics 27 (2008) 21–; doi:10.1021/om701029j

data_4070803
_publ_section_title
;
 Chiral Palladium Bis(acyclic diaminocarbene) Complexes as
 Enantioselective Catalysts for the Aza-Claisen Rearrangement
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              21
_journal_paper_doi               10.1021/om701029j
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H28 Br2 F6 N4 Pd, 2(C H4 O)'
_chemical_formula_sum            'C34 H36 Br2 F6 N4 O2 Pd'
_chemical_formula_weight         912.89
_chemical_name_common            'Resolved Pd bis(ADC) dibromide'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.8307(11)
_cell_length_b                   13.1779(15)
_cell_length_c                   30.571(4)
_cell_measurement_reflns_used    9420
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      30.85
_cell_measurement_theta_min      2.40
_cell_volume                     3557.5(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (XP)'
_computing_publication_material  'Bruker SHELXTL (XCIF)'
_computing_structure_refinement  'Bruker SHELXTL (XL)'
_computing_structure_solution    'Bruker SHELXTL (XS)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 0.75
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            85137
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        N/A
_diffrn_standards_interval_count N/A
_diffrn_standards_interval_time  N/A
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_T_max  0.8049
_exptl_absorpt_correction_T_min  0.3313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamondoid
_exptl_crystal_F_000             1816
_exptl_crystal_recrystallization_method 'slow evap of methanol soln'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack (1983), 4823 Friedel pairs'
_refine_ls_abs_structure_Flack   0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         10870
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0308P)^2^+3.8135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                9988
_reflns_number_total             10870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701029j-file003.cif
_cod_data_source_block           lms115_res70
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_cell_volume        3557.6(8)
_cod_database_code               4070803