#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:48:47 +0100 (vie 25 de mar de 2016) $
#$Revision: 179816 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/12/7011214.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7011214
loop_
_publ_author_name
'Hai-Bin Song'
'Zheng-Zhi Zhang'
'Thomas C. W. Mak'
_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            'C19 H19 Cl4 N2 P Pd'
_chemical_formula_weight         554.53
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.913(5)
_cell_angle_beta                 103.563(4)
_cell_angle_gamma                113.954(4)
_cell_formula_units_Z            2
_cell_length_a                   9.703(2)
_cell_length_b                   10.229(2)
_cell_length_c                   12.939(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1101.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7548
_diffrn_reflns_theta_full        28.11
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0592P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                3574
_reflns_number_total             5232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109191n.txt
_cod_data_source_block           compd4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_database_code               7011214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.23164(4) 0.71230(4) 0.09411(3) 0.03174(12) Uani 1 1 d . . .
Cl1 Cl 0.17167(16) 0.80405(14) 0.24102(10) 0.0464(3) Uani 1 1 d . . .
Cl2 Cl 0.31253(18) 0.64237(16) -0.04821(11) 0.0545(4) Uani 1 1 d . . .
P1 P 0.31302(13) 0.56806(13) 0.18170(10) 0.0321(3) Uani 1 1 d . . .
N1 N -0.1592(5) 0.1565(4) -0.0038(3) 0.0372(9) Uani 1 1 d . . .
N2 N 0.1041(4) 0.3144(4) 0.0261(3) 0.0371(9) Uani 1 1 d . . .
H2B H 0.0725 0.3655 -0.0283 0.045 Uiso 1 1 d R . .
C1 C 0.5261(5) 0.6643(5) 0.2510(4) 0.0348(10) Uani 1 1 d . . .
C2 C 0.5879(6) 0.7988(6) 0.3252(5) 0.0592(15) Uani 1 1 d . . .
H2A H 0.5213 0.8377 0.3408 0.071 Uiso 1 1 calc R . .
C3 C 0.7535(7) 0.8775(7) 0.3775(5) 0.0730(19) Uani 1 1 d . . .
H3A H 0.7958 0.9688 0.4282 0.088 Uiso 1 1 calc R . .
C4 C 0.8527(6) 0.8234(7) 0.3556(5) 0.0558(15) Uani 1 1 d . . .
H4A H 0.9619 0.8762 0.3910 0.067 Uiso 1 1 calc R . .
C5 C 0.7893(6) 0.6903(7) 0.2808(5) 0.0576(15) Uani 1 1 d . . .
H5A H 0.8562 0.6526 0.2639 0.069 Uiso 1 1 calc R . .
C6 C 0.6270(6) 0.6106(6) 0.2297(4) 0.0468(12) Uani 1 1 d . . .
H6A H 0.5858 0.5188 0.1799 0.056 Uiso 1 1 calc R . .
C7 C 0.2211(5) 0.4974(5) 0.2826(4) 0.0368(10) Uani 1 1 d . . .
C8 C 0.3042(6) 0.4674(6) 0.3702(4) 0.0545(14) Uani 1 1 d . . .
H8A H 0.4109 0.4916 0.3814 0.065 Uiso 1 1 calc R . .
C9 C 0.2304(8) 0.4012(8) 0.4421(5) 0.0707(19) Uani 1 1 d . . .
H9A H 0.2866 0.3822 0.5020 0.085 Uiso 1 1 calc R . .
C10 C 0.0723(8) 0.3647(8) 0.4226(6) 0.077(2) Uani 1 1 d . . .
H10A H 0.0220 0.3206 0.4704 0.092 Uiso 1 1 calc R . .
C11 C -0.0140(7) 0.3909(7) 0.3350(5) 0.0654(17) Uani 1 1 d . . .
H11A H -0.1215 0.3637 0.3231 0.079 Uiso 1 1 calc R . .
C12 C 0.0616(6) 0.4590(6) 0.2641(4) 0.0478(12) Uani 1 1 d . . .
H12A H 0.0052 0.4785 0.2046 0.057 Uiso 1 1 calc R . .
C13 C 0.2716(5) 0.3946(5) 0.0866(4) 0.0382(11) Uani 1 1 d . . .
H13A H 0.3319 0.4173 0.0358 0.046 Uiso 1 1 calc R . .
H13B H 0.3040 0.3340 0.1281 0.046 Uiso 1 1 calc R . .
C14 C -0.0066(6) 0.1967(5) 0.0493(4) 0.0337(10) Uani 1 1 d . . .
C15 C 0.0364(7) 0.1193(6) 0.1218(4) 0.0476(13) Uani 1 1 d . . .
H15A H 0.1430 0.1494 0.1594 0.057 Uiso 1 1 calc R . .
C16 C -0.0804(8) -0.0007(6) 0.1363(5) 0.0560(15) Uani 1 1 d . . .
H16A H -0.0541 -0.0529 0.1843 0.067 Uiso 1 1 calc R . .
C17 C -0.2392(7) -0.0445(6) 0.0789(5) 0.0593(16) Uani 1 1 d . . .
H17A H -0.3203 -0.1269 0.0869 0.071 Uiso 1 1 calc R . .
C18 C -0.2732(7) 0.0370(6) 0.0101(5) 0.0515(13) Uani 1 1 d . . .
H18A H -0.3791 0.0085 -0.0282 0.062 Uiso 1 1 calc R . .
C19 C 0.5141(15) 0.8375(13) -0.3724(8) 0.186(6) Uani 1 1 d D . .
H19A H 0.5659 0.7895 -0.4071 0.224 Uiso 1 1 calc R . .
H19B H 0.5885 0.9420 -0.3436 0.224 Uiso 1 1 calc R . .
Cl3 Cl 0.4805(4) 0.7703(4) -0.2700(3) 0.1665(13) Uani 1 1 d D . .
Cl4 Cl 0.3470(3) 0.8192(3) -0.4742(2) 0.1142(8) Uani 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 P1 176.55(11) 2_565 . ?
N1 Pd1 Cl2 88.29(11) 2_565 . ?
P1 Pd1 Cl2 88.26(5) . . ?
N1 Pd1 Cl1 90.16(11) 2_565 . ?
P1 Pd1 Cl1 93.29(5) . . ?
Cl2 Pd1 Cl1 174.52(5) . . ?
C1 P1 C7 106.8(2) . . ?
C1 P1 C13 106.7(2) . . ?
C7 P1 C13 101.4(2) . . ?
C1 P1 Pd1 110.56(15) . . ?
C7 P1 Pd1 117.85(16) . . ?
C13 P1 Pd1 112.57(16) . . ?
C14 N1 C18 119.3(4) . . ?
C14 N1 Pd1 122.6(3) . 2_565 ?
C18 N1 Pd1 117.7(3) . 2_565 ?
C14 N2 C13 126.1(4) . . ?
C6 C1 C2 119.0(5) . . ?
C6 C1 P1 122.8(4) . . ?
C2 C1 P1 118.2(4) . . ?
C1 C2 C3 119.1(5) . . ?
C4 C3 C2 121.4(6) . . ?
C3 C4 C5 118.6(5) . . ?
C4 C5 C6 120.8(5) . . ?
C1 C6 C5 121.1(5) . . ?
C8 C7 C12 120.1(5) . . ?
C8 C7 P1 120.4(4) . . ?
C12 C7 P1 119.1(4) . . ?
C7 C8 C9 120.7(5) . . ?
C10 C9 C8 118.3(6) . . ?
C11 C10 C9 122.3(5) . . ?
C10 C11 C12 119.0(5) . . ?
C7 C12 C11 119.6(5) . . ?
N2 C13 P1 109.6(3) . . ?
N1 C14 N2 116.2(4) . . ?
N1 C14 C15 121.2(4) . . ?
N2 C14 C15 122.6(4) . . ?
C16 C15 C14 119.0(5) . . ?
C15 C16 C17 119.7(5) . . ?
C18 C17 C16 118.4(5) . . ?
N1 C18 C17 122.4(5) . . ?
Cl3 C19 Cl4 116.2(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.116(4) 2_565 ?
Pd1 P1 2.2520(12) . ?
Pd1 Cl2 2.3000(13) . ?
Pd1 Cl1 2.3029(13) . ?
P1 C1 1.812(5) . ?
P1 C7 1.818(5) . ?
P1 C13 1.847(5) . ?
N1 C14 1.335(6) . ?
N1 C18 1.344(6) . ?
N1 Pd1 2.116(4) 2_565 ?
N2 C14 1.376(5) . ?
N2 C13 1.439(6) . ?
C1 C6 1.363(6) . ?
C1 C2 1.368(7) . ?
C2 C3 1.406(7) . ?
C3 C4 1.352(8) . ?
C4 C5 1.359(8) . ?
C5 C6 1.379(7) . ?
C7 C8 1.378(7) . ?
C7 C12 1.383(6) . ?
C8 C9 1.388(7) . ?
C9 C10 1.372(9) . ?
C10 C11 1.371(8) . ?
C11 C12 1.394(7) . ?
C14 C15 1.404(6) . ?
C15 C16 1.364(7) . ?
C16 C17 1.391(8) . ?
C17 C18 1.373(7) . ?
C19 Cl3 1.614(9) . ?
C19 Cl4 1.757(10) . ?
