Optically active asymmetric di(tertiary phosphines). Crystal and molecular structure of [SP-4-3-(SP,S )]-{1-[(2-chlorophenyl)methylphosphino]-2-(dimethylphosphino)benzene-P,P ' }{1-[1-(dimethylamino)ethyl]naphthyl-C 2,N }palladium(II) hexafluorophosphate
Chatterjee, Swarup; George, Mark D.; Salem, Geoffrey; Willis, Anthony C.; Journal of the Chemical Society, Dalton Transactions  (2001) 1890–; doi:10.1039/b101182k

data_7010616
_publ_section_title
;
 Optically active asymmetric di(tertiary phosphines). Crystal and
 molecular structure of
 [SP-4-3-(SP,S&#x200A;)]-{1-[(2-chlorophenyl)methylphosphino]-2-(dimethylphosphino)benzene-P,P&#x200A;'&#x200A;}{1-[1-(dimethylamino)ethyl]naphthyl-C&#x200A;2,N&#x200A;}palladium(II)
 hexafluorophosphate
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1890
_journal_paper_doi               10.1039/b101182k
_journal_year                    2001
_chemical_formula_moiety         'C29 H33 Cl N P2 Pd 1+, F6 P 1-'
_chemical_formula_sum            'C29 H33 Cl F6 N P3 Pd'
_chemical_formula_weight         744.35
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             1999-10-06
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2001-02-07 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 102.87(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.982(2)
_cell_length_b                   13.436(2)
_cell_length_c                   13.797(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      16.5
_cell_volume                     1623.2(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02368
_diffrn_orient_matrix_UB_12      0.07279
_diffrn_orient_matrix_UB_13      -0.00198
_diffrn_orient_matrix_UB_21      -0.00690
_diffrn_orient_matrix_UB_22      -0.00247
_diffrn_orient_matrix_UB_23      0.07131
_diffrn_orient_matrix_UB_31      0.11151
_diffrn_orient_matrix_UB_32      0.01531
_diffrn_orient_matrix_UB_33      0.02095
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03500
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5016
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        -0.58
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             752.00
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details
;
The absolute structure was determined by comparing the
agreement factors given below with those obtained from refinement
of a model with all coordinates transformed by  (-x,-y,-z) --
R = 0.0324, Rw = 0.0277 and S = 1.61.
This indicates that the original model corresponds to the absolute
configuration.
Even more definitive is the fact that it is consistent with the
known chirality of the synthetic precursors.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.418
_refine_ls_goodness_of_fit_ref   1.515
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     369
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.0070
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0282
_refine_ls_wR_factor_ref         0.0260
_reflns_number_gt                3259
_reflns_number_total             3899
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            b101182k.txt
_cod_data_source_block           sxc6
_cod_original_sg_symbol_H-M      'P 21       '
_cod_original_formula_sum        'C29 H33 Cl F6 N P3 Pd '
_cod_database_code               7010616