Synthesis of β-P,N Aminophosphines and Coordination Chemistry to PdII. X-ray Structures of [PdCl2(Ph2PCH2CH(Ph)NHPh-κP,κN)] and [PdCl(η3-C3H5)(Ph2PCH2CH(Ph)NHPh-κP)]
Jacques Andrieu; Jean-Michel Camus; Jochen Dietz; Philippe Richard; Rinaldo Poli; Inorganic Chemistry 40 (2001) 1597–1605; doi:10.1021/ic000867y

data_4319443
_publ_contact_author_address
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L.S.E.O. faculte des sciences, 6 Bd Gabriel 21000 Dijon, FRANCE
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_publ_contact_author_email       jandrieu@satie.u-bourgogne.fr
_publ_contact_author_fax         +33-0380396073
_publ_contact_author_name        'Dr. J. Andrieu'
_publ_contact_author_phone       +33-0380396880
_publ_section_title
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 Synthesis of \b-P,N Aminophosphines and Coordination Chemistry to PdII.
 X-ray Structures of [PdCl2(Ph2PCH2CH(Ph)NHPh-\kP,\kN)] and
 [PdCl(\h3-C3H5)(Ph2PCH2CH(Ph)NHPh-\kP)]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1597
_journal_page_last               1605
_journal_paper_doi               10.1021/ic000867y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C29 H29 Cl N P Pd'
_chemical_formula_weight         564.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.651(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9120(10)
_cell_length_b                   17.194(2)
_cell_length_c                   14.169(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.16
_cell_measurement_theta_min      10.44
_cell_volume                     2612.6(5)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       omega-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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2779
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.30
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         2776
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.680
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.5797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                2588
_reflns_number_total             2776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000867y_2.cif
_cod_data_source_block           p15a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4319443