Unsymmetrical Chiral PCN Pincer Palladium(II) and Nickel(II) Complexes with Aryl-Based Aminophosphine‒Imidazoline Ligands: Synthesis via Aryl C‒H Activation and Asymmetric Addition of Diarylphosphines to Enones
Yang, Ming-Jun; Liu, Yan-Jing; Gong, Jun-Fang; Song, Mao-Ping; Organometallics 30 (2011) 3793–; doi:10.1021/om200350h

data_4064810
_publ_section_title
;
 Unsymmetrical Chiral PCN Pincer Palladium(II) and Nickel(II) Complexes
 with Aryl-Based Aminophosphine--Imidazoline Ligands: Synthesis via Aryl
 C--H Activation and Asymmetric Addition of Diarylphosphines to Enones
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3793
_journal_paper_doi               10.1021/om200350h
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration s
_chemical_formula_sum            'C34 H29 Cl N3 P Pd'
_chemical_formula_weight         652.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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                   11.8793(2)
_cell_length_b                   12.50471(19)
_cell_length_c                   20.1538(4)
_cell_measurement_reflns_used    12983
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.4800
_cell_measurement_theta_min      3.0261
_cell_volume                     2993.79(9)
_computing_cell_refinement       'Oxford Diffraction Ltd.'
_computing_data_collection       'Oxford Diffraction Ltd.'
_computing_data_reduction        'Oxford Diffraction Ltd.'
_computing_molecular_graphics    olex2
_computing_publication_material  olex2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w 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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20205
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.8579
_exptl_absorpt_correction_T_min  0.7694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Oxford Diffraction Ltd.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.1043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                5526
_reflns_number_total             6113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200350h_si_003.cif
_cod_data_source_block           complex-4c
_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_cell_volume        2993.78(9)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4064810