Stereochemical Investigations of a Novel Class of Chiral Phosphapalladacycle Complexes Derived from 1-[(2,5-Dimethyl)phenyl]ethyldiphenylphosphine
Joseph Kok-Peng Ng; Yongxin Li; Geok-Kheng Tan; Lip-Lin Koh; Jagadese J. Vittal; Pak-Hing Leung; Inorganic Chemistry 44 (2005) 9874–9886; doi:10.1021/ic0509579

data_4310190
_publ_section_title
;
Stereochemical Investigations of a Novel Class of Chiral
Phosphapalladacycle Complexes Derived from
1-[(2,5-Dimethyl)phenyl]ethyldiphenylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9874
_journal_page_last               9886
_journal_paper_doi               10.1021/ic0509579
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C36 H39 Cl N P Pd'
_chemical_formula_weight         658.50
_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                 91.7790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7890(7)
_cell_length_b                   13.1284(7)
_cell_length_c                   21.3695(12)
_cell_measurement_reflns_used    5361
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.05
_cell_measurement_theta_min      2.45
_cell_volume                     3305.8(3)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, 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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26957
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.9335
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.534
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         17997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                15906
_reflns_number_total             17997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0509579si20050614_025722.cif
_cod_data_source_block           1180
_cod_database_code               4310190