Diphenylprolinol-Derived Symmetrical and Unsymmetrical Chiral Pincer Palladium(II) and Nickel(II) Complexes: Synthesis via One-Pot Phosphorylation/Metalation Reaction and C−H Activation
Niu, Jun-Long; Chen, Qing-Tao; Hao, Xin-Qi; Zhao, Qing-Xiang; Gong, Jun-Fang; Song, Mao-Ping; Organometallics 29 (2010) 2148–; doi:10.1021/om100234q

data_4065983
_publ_section_title
;
 Diphenylprolinol-Derived Symmetrical and Unsymmetrical Chiral Pincer
 Palladium(II) and Nickel(II) Complexes: Synthesis via One-Pot
 Phosphorylation/Metalation Reaction and C&#x2212;H Activation
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2148
_journal_paper_doi               10.1021/om100234q
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration s
_chemical_formula_sum            'C36 H37 Cl N3 Ni O3 P'
_chemical_formula_weight         684.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.66(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.232(2)
_cell_length_b                   9.4811(19)
_cell_length_c                   17.026(3)
_cell_measurement_reflns_used    4663
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2038
_cell_measurement_theta_min      2.1479
_cell_volume                     1640.6(6)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       dtprofit.ref'
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10882
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.8625
_exptl_absorpt_correction_T_min  0.8625
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISMATIC
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.029(19)
_refine_ls_extinction_coef       0.033(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   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6083
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                4430
_reflns_number_total             6083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100234q_si_002.cif
_cod_data_source_block           complex-4
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1640.5(6)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4065983