Synthesis and structural study of late transition metal complexes of N-[(diphenylphosphino)methyl]-2-pyridinamine and N-cyclohexyl-N-[(diphenylphosphino)methyl]-2-pyridinamine
Hai-Bin Song; Zheng-Zhi Zhang; Thomas C. W. Mak; J. Chem. Soc., Dalton Trans.  (2002) 1336–1343; doi:10.1039/b109191n

data_7011213
_publ_section_title
;
 Synthesis and structural study of late transition metal complexes of
 N-[(diphenylphosphino)methyl]-2-pyridinamine and
 N-cyclohexyl-N-[(diphenylphosphino)methyl]-2-pyridinamine
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1336
_journal_page_last               1343
_journal_paper_doi               10.1039/b109191n
_journal_year                    2002
_chemical_formula_sum            'C36 H34 Cl2 N4 O8 P2 Pd'
_chemical_formula_weight         889.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.442(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6439(18)
_cell_length_b                   21.221(4)
_cell_length_c                   18.761(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3797.9(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25481
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6924
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0031(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   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9136
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                5578
_reflns_number_total             9136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109191n.txt
_cod_data_source_block           compd3
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3798.0(12)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011213