New phosphino-oxazoline and related phosphino-iminolate palladium complexes; structure of an unusual zwitterionic dinuclear Pd(ii) complex
Apfelbacher, Andreas; Braunstein, Pierre; Brissieux, Luc; Welter, Richard; Dalton Transactions  (2003) 1669–; doi:10.1039/b300321n

data_7012706
_publ_section_title
;
 New phosphino-oxazoline and related phosphino-iminolate palladium
 complexes; structure of an unusual zwitterionic dinuclear Pd(ii)
 complex
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1669
_journal_paper_doi               10.1039/b300321n
_journal_year                    2003
_chemical_formula_moiety         'C23 H23 Cl N O P Pd'
_chemical_formula_sum            'C23 H23 Cl N O P Pd'
_chemical_formula_weight         502.24
_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                 107.690(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.998(5)
_cell_length_b                   8.647(5)
_cell_length_c                   12.017(5)
_cell_measurement_reflns_used    6402
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1088.8(9)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5518
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5517
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.1665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                5076
_reflns_number_total             5517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300321n.txt
_cod_data_source_block           wel4
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7012706