Unsymmetrical Chiral PCN Pincer Palladium(II) and Nickel(II) Complexes of (Imidazolinyl)aryl Phosphinite Ligands: Synthesis via Ligand C−H Activation, Crystal Structures, and Catalytic Studies
Zhang, Ben-Shang; Wang, Wei; Shao, Dan-Dan; Hao, Xin-Qi; Gong, Jun-Fang; Song, Mao-Ping; Organometallics 29 (2010) 2579–; doi:10.1021/om100232n

data_4065967
_publ_section_title
;
 Unsymmetrical Chiral PCN Pincer Palladium(II) and Nickel(II) Complexes of
 (Imidazolinyl)aryl Phosphinite Ligands: Synthesis via Ligand C&#x2212;H
 Activation, Crystal Structures, and Catalytic Studies
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2579
_journal_paper_doi               10.1021/om100232n
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C31 H31 Cl N2 O3 P Pd'
_chemical_formula_weight         652.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.395(3)
_cell_length_b                   13.024(3)
_cell_length_c                   15.650(3)
_cell_measurement_reflns_used    397
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2
_cell_volume                     3096.1(11)
_computing_cell_refinement       raxis
_computing_data_collection       raxis
_computing_data_reduction        raxis
_computing_molecular_graphics    texsan
_computing_publication_material  texsan
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  R-AXIS-IV
_diffrn_measurement_method       'Oscillation  frames'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9622
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.8738
_exptl_absorpt_correction_T_min  0.8612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0096(6)
_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   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5281
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0510P)^2^+12.8116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                4858
_reflns_number_total             5281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100232n_si_002.cif
_cod_data_source_block           Complex-3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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        3095.9(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065967