#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:05:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179825 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/21/7012107.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_7012107
loop_
_publ_author_name
'Mandal, Swadhin K.'
'Nagana Gowda, G. A.'
'Krishnamurthy, Setharampattu S.'
'Nethaji, Munirathinam'
_publ_section_title
;
 Palladium(ii) allyl complexes of chiral diphosphazane ligands:
 ambident coordination behaviour and stereodynamic studies in
 solutionOrganometallic chemistry of diphosphazanes. Part
 17.11g.Electronic supplementary information (ESI) available: NMR and
 crystallographic data, stereodynamic behaviour schemes. See
 http://www.rsc.org/suppdata/dt/b2/b207447h/
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              1016
_journal_paper_doi               10.1039/b207447h
_journal_year                    2003
_chemical_formula_moiety
;
[Pd(eta-3-Me2-C3H3){eta-2-Ph2P(S)N(CHMe2)PPh(N2C3HMe2-3,5)}](PF6) 
;
_chemical_formula_sum            'C31 H38 F6 N3 P3 Pd S'
_chemical_formula_weight         798.01
_chemical_melting_point          '155- 159 0C dec.'
_chemical_name_systematic
;
(eta-3-dimethylallyl)[eta-2-{N,N-(diphenylthiophosphinyl)
(phenyl, 3,5-dimethylpyrazolylphosphino)isopropyl amine}  
-kappa-P,S]palladium(II)hexafluorophosphate
;
_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                 97.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.836(5)
_cell_length_b                   10.758(2)
_cell_length_c                   33.860(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      1.2
_cell_volume                     3556(2)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4(Harms and Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-32 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profile omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\alpha
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            8208
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                4971
_reflns_number_total             7756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207447h.txt
_cod_data_source_block           complex_12a
_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_sg_symbol_H-M      P21/n
_cod_database_code               7012107
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.42906(4) 0.17433(3) 0.123627(10) 0.05253(14) Uani 1 1 d . . .
S1 S 0.42722(15) 0.07358(11) 0.06237(3) 0.0650(4) Uani 1 1 d . . .
P1 P 0.48186(11) -0.00429(9) 0.15730(3) 0.0424(3) Uani 1 1 d . . .
P2 P 0.50707(12) -0.09323(10) 0.07743(3) 0.0441(3) Uani 1 1 d . . .
P3 P 0.92851(16) 0.37639(16) 0.11751(5) 0.0758(4) Uani 1 1 d . . .
N1 N 0.5507(3) -0.1068(3) 0.12673(9) 0.0401(7) Uani 1 1 d . . .
N2 N 0.3572(4) -0.0870(3) 0.17730(10) 0.0486(8) Uani 1 1 d . . .
N3 N 0.3900(4) -0.2011(3) 0.19468(12) 0.0557(10) Uani 1 1 d . . .
C1 C 0.4531(11) 0.3042(7) 0.2098(2) 0.119(3) Uani 1 1 d . . .
H1A H 0.3902 0.2483 0.2202 0.178 Uiso 1 1 calc R . .
H1B H 0.4471 0.3845 0.2218 0.178 Uiso 1 1 calc R . .
H1C H 0.5447 0.2727 0.2157 0.178 Uiso 1 1 calc R . .
C2 C 0.4209(13) 0.3140(5) 0.1697(2) 0.142(4) Uani 1 1 d . . .
H2 H 0.3211 0.3192 0.1688 0.171 Uiso 1 1 calc R . .
C3 C 0.4321(9) 0.3670(5) 0.13772(19) 0.095(2) Uani 1 1 d . . .
H3 H 0.5316 0.3792 0.1414 0.114 Uiso 1 1 calc R . .
C4 C 0.4139(10) 0.3638(5) 0.0997(2) 0.109(3) Uani 1 1 d . . .
H4 H 0.3138 0.3705 0.0962 0.131 Uiso 1 1 calc R . .
C5 C 0.4357(11) 0.4051(6) 0.0635(2) 0.147(4) Uani 1 1 d . . .
H5A H 0.3681 0.3705 0.0437 0.220 Uiso 1 1 calc R . .
H5B H 0.5254 0.3802 0.0582 0.220 Uiso 1 1 calc R . .
H5C H 0.4294 0.4941 0.0629 0.220 Uiso 1 1 calc R . .
C6 C 0.6150(5) 0.0188(4) 0.19854(12) 0.0467(10) Uani 1 1 d . . .
C7 C 0.7253(5) 0.0913(5) 0.18990(14) 0.0594(12) Uani 1 1 d . . .
H7 H 0.7314 0.1161 0.1639 0.071 Uiso 1 1 calc R . .
C8 C 0.8261(6) 0.1265(6) 0.22026(18) 0.0754(15) Uani 1 1 d . . .
H8 H 0.9007 0.1734 0.2145 0.090 Uiso 1 1 calc R . .
C9 C 0.8151(6) 0.0922(6) 0.25801(16) 0.0789(17) Uani 1 1 d . . .
H9 H 0.8825 0.1163 0.2783 0.095 Uiso 1 1 calc R . .
C10 C 0.7064(6) 0.0222(6) 0.26714(16) 0.0816(17) Uani 1 1 d . . .
H10 H 0.7003 0.0003 0.2934 0.098 Uiso 1 1 calc R . .
C11 C 0.6060(5) -0.0156(5) 0.23746(13) 0.0606(12) Uani 1 1 d . . .
H11 H 0.5330 -0.0638 0.2436 0.073 Uiso 1 1 calc R . .
C12 C 0.2173(5) -0.0704(5) 0.17225(15) 0.0634(13) Uani 1 1 d . . .
C13 C 0.1467(6) 0.0411(7) 0.1531(2) 0.100(2) Uani 1 1 d . . .
H13A H 0.2138 0.0994 0.1462 0.150 Uiso 1 1 calc R . .
H13B H 0.0921 0.0795 0.1714 0.150 Uiso 1 1 calc R . .
H13C H 0.0889 0.0163 0.1296 0.150 Uiso 1 1 calc R . .
C14 C 0.1654(5) -0.1751(5) 0.18676(19) 0.0746(16) Uani 1 1 d . . .
H14 H 0.0730 -0.1920 0.1874 0.090 Uiso 1 1 calc R . .
C15 C 0.2726(5) -0.2526(5) 0.20035(16) 0.0625(13) Uani 1 1 d . . .
C16 C 0.2669(7) -0.3794(6) 0.2182(2) 0.098(2) Uani 1 1 d . . .
H16A H 0.3583 -0.4104 0.2250 0.148 Uiso 1 1 calc R . .
H16B H 0.2170 -0.4343 0.1993 0.148 Uiso 1 1 calc R . .
H16C H 0.2217 -0.3750 0.2417 0.148 Uiso 1 1 calc R . .
C17 C 0.6426(4) -0.2111(4) 0.14549(13) 0.0472(10) Uani 1 1 d . . .
H17 H 0.6328 -0.2093 0.1739 0.057 Uiso 1 1 calc R . .
C18 C 0.7930(5) -0.1889(5) 0.14288(17) 0.0683(14) Uani 1 1 d . . .
H18A H 0.8174 -0.1067 0.1523 0.102 Uiso 1 1 calc R . .
H18B H 0.8105 -0.1969 0.1157 0.102 Uiso 1 1 calc R . .
H18C H 0.8466 -0.2489 0.1590 0.102 Uiso 1 1 calc R . .
C19 C 0.5965(5) -0.3386(4) 0.13133(15) 0.0595(12) Uani 1 1 d . . .
H19A H 0.5009 -0.3484 0.1337 0.089 Uiso 1 1 calc R . .
H19B H 0.6481 -0.4003 0.1472 0.089 Uiso 1 1 calc R . .
H19C H 0.6112 -0.3485 0.1040 0.089 Uiso 1 1 calc R . .
C20 C 0.3808(5) -0.2082(4) 0.05993(13) 0.0509(11) Uani 1 1 d . . .
C21 C 0.2942(5) -0.2580(5) 0.08500(16) 0.0615(12) Uani 1 1 d . . .
H21 H 0.3072 -0.2383 0.1119 0.074 Uiso 1 1 calc R . .
C22 C 0.1897(6) -0.3359(5) 0.0708(2) 0.0839(18) Uani 1 1 d . . .
H22 H 0.1321 -0.3689 0.0879 0.101 Uiso 1 1 calc R . .
C23 C 0.1703(7) -0.3655(7) 0.0305(3) 0.096(2) Uani 1 1 d . . .
H23 H 0.1016 -0.4210 0.0209 0.115 Uiso 1 1 calc R . .
C24 C 0.2511(7) -0.3137(6) 0.0049(2) 0.093(2) Uani 1 1 d . . .
H24 H 0.2344 -0.3309 -0.0222 0.112 Uiso 1 1 calc R . .
C25 C 0.3585(6) -0.2353(5) 0.01920(16) 0.0721(15) Uani 1 1 d . . .
H25 H 0.4149 -0.2012 0.0019 0.087 Uiso 1 1 calc R . .
C26 C 0.6601(5) -0.1154(5) 0.05432(14) 0.0587(12) Uani 1 1 d . . .
C27 C 0.7502(6) -0.0139(6) 0.05663(18) 0.0808(17) Uani 1 1 d . . .
H27 H 0.7247 0.0611 0.0673 0.097 Uiso 1 1 calc R . .
C28 C 0.8764(8) -0.0250(9) 0.0432(3) 0.121(3) Uani 1 1 d . . .
H28 H 0.9384 0.0407 0.0456 0.145 Uiso 1 1 calc R . .
C29 C 0.9083(9) -0.1350(11) 0.0261(3) 0.131(4) Uani 1 1 d . . .
H29 H 0.9926 -0.1423 0.0165 0.157 Uiso 1 1 calc R . .
C30 C 0.8195(9) -0.2360(8) 0.0224(2) 0.111(3) Uani 1 1 d . . .
H30 H 0.8434 -0.3092 0.0104 0.133 Uiso 1 1 calc R . .
C31 C 0.6940(6) -0.2254(6) 0.03721(15) 0.0746(15) Uani 1 1 d . . .
H31 H 0.6335 -0.2921 0.0355 0.090 Uiso 1 1 calc R . .
F1 F 0.8126(6) 0.3885(7) 0.1438(2) 0.188(3) Uani 1 1 d . . .
F2 F 0.8627(10) 0.2578(6) 0.1004(2) 0.225(4) Uani 1 1 d . . .
F3 F 0.9908(10) 0.4970(7) 0.1350(2) 0.239(4) Uani 1 1 d . . .
F4 F 0.9976(9) 0.3045(8) 0.1523(3) 0.252(4) Uani 1 1 d . . .
F5 F 0.8527(10) 0.4506(7) 0.08386(18) 0.239(4) Uani 1 1 d . . .
F6 F 1.0338(10) 0.3591(11) 0.0912(4) 0.317(7) Uani 1 1 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'
F F 0.0171 0.0103 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C3 Pd1 C2 33.5(2) . . ?
C3 Pd1 C4 34.4(2) . . ?
C2 Pd1 C4 67.4(3) . . ?
C3 Pd1 P1 135.96(19) . . ?
C2 Pd1 P1 104.6(2) . . ?
C4 Pd1 P1 167.8(2) . . ?
C3 Pd1 S1 130.49(18) . . ?
C2 Pd1 S1 163.7(2) . . ?
C4 Pd1 S1 96.34(18) . . ?
P1 Pd1 S1 91.70(4) . . ?
P2 S1 Pd1 103.28(6) . . ?
N1 P1 N2 105.04(17) . . ?
N1 P1 C6 104.66(19) . . ?
N2 P1 C6 104.51(19) . . ?
N1 P1 Pd1 109.05(11) . . ?
N2 P1 Pd1 120.47(13) . . ?
C6 P1 Pd1 111.83(14) . . ?
N1 P2 C26 107.2(2) . . ?
N1 P2 C20 110.47(19) . . ?
C26 P2 C20 110.3(2) . . ?
N1 P2 S1 112.08(13) . . ?
C26 P2 S1 109.39(17) . . ?
C20 P2 S1 107.38(16) . . ?
F6 P3 F4 97.3(7) . . ?
F6 P3 F5 85.9(7) . . ?
F4 P3 F5 176.8(6) . . ?
F6 P3 F2 87.8(6) . . ?
F4 P3 F2 89.8(6) . . ?
F5 P3 F2 90.5(5) . . ?
F6 P3 F3 93.7(6) . . ?
F4 P3 F3 90.7(5) . . ?
F5 P3 F3 88.9(4) . . ?
F2 P3 F3 178.3(5) . . ?
F6 P3 F1 176.6(6) . . ?
F4 P3 F1 83.4(5) . . ?
F5 P3 F1 93.4(5) . . ?
F2 P3 F1 88.8(4) . . ?
F3 P3 F1 89.6(5) . . ?
C17 N1 P2 122.9(3) . . ?
C17 N1 P1 118.7(3) . . ?
P2 N1 P1 118.36(19) . . ?
C12 N2 N3 110.2(4) . . ?
C12 N2 P1 129.3(3) . . ?
N3 N2 P1 119.1(3) . . ?
C15 N3 N2 105.8(4) . . ?
C3 C2 C1 150.7(10) . . ?
C3 C2 Pd1 71.2(4) . . ?
C1 C2 Pd1 129.6(5) . . ?
C2 C3 C4 148.2(7) . . ?
C2 C3 Pd1 75.3(4) . . ?
C4 C3 Pd1 75.6(3) . . ?
C3 C4 C5 152.9(9) . . ?
C3 C4 Pd1 70.0(3) . . ?
C5 C4 Pd1 129.2(5) . . ?
C11 C6 C7 119.4(4) . . ?
C11 C6 P1 125.0(4) . . ?
C7 C6 P1 115.0(3) . . ?
C8 C7 C6 120.0(5) . . ?
C9 C8 C7 119.6(6) . . ?
C8 C9 C10 121.2(5) . . ?
C9 C10 C11 120.3(5) . . ?
C6 C11 C10 119.5(5) . . ?
C14 C12 N2 105.2(4) . . ?
C14 C12 C13 130.6(5) . . ?
N2 C12 C13 124.2(5) . . ?
C12 C14 C15 108.5(4) . . ?
N3 C15 C14 110.2(4) . . ?
N3 C15 C16 121.3(5) . . ?
C14 C15 C16 128.4(5) . . ?
C19 C17 C18 112.6(4) . . ?
C19 C17 N1 113.4(3) . . ?
C18 C17 N1 113.1(4) . . ?
C21 C20 C25 119.3(5) . . ?
C21 C20 P2 121.1(4) . . ?
C25 C20 P2 119.0(4) . . ?
C22 C21 C20 121.0(5) . . ?
C21 C22 C23 119.5(6) . . ?
C24 C23 C22 120.6(6) . . ?
C23 C24 C25 120.2(6) . . ?
C24 C25 C20 119.3(6) . . ?
C31 C26 C27 120.6(5) . . ?
C31 C26 P2 123.8(5) . . ?
C27 C26 P2 115.5(4) . . ?
C28 C27 C26 120.2(7) . . ?
C29 C28 C27 118.4(8) . . ?
C28 C29 C30 122.6(7) . . ?
C29 C30 C31 118.6(8) . . ?
C26 C31 C30 119.5(7) . . ?
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 C3 2.126(5) . ?
Pd1 C2 2.173(6) . ?
Pd1 C4 2.192(5) . ?
Pd1 P1 2.2622(11) . ?
Pd1 S1 2.3383(14) . ?
S1 P2 1.9997(16) . ?
P1 N1 1.707(3) . ?
P1 N2 1.720(4) . ?
P1 C6 1.811(4) . ?
P2 N1 1.678(3) . ?
P2 C26 1.796(5) . ?
P2 C20 1.801(5) . ?
P3 F6 1.459(7) . ?
P3 F4 1.501(7) . ?
P3 F5 1.511(6) . ?
P3 F2 1.514(6) . ?
P3 F3 1.524(6) . ?
P3 F1 1.536(5) . ?
N1 C17 1.531(5) . ?
N2 C12 1.377(6) . ?
N2 N3 1.383(5) . ?
N3 C15 1.315(6) . ?
C1 C2 1.361(10) . ?
C2 C3 1.240(9) . ?
C3 C4 1.279(9) . ?
C4 C5 1.344(9) . ?
C6 C11 1.382(6) . ?
C6 C7 1.396(6) . ?
C7 C8 1.391(7) . ?
C8 C9 1.347(8) . ?
C9 C10 1.373(8) . ?
C10 C11 1.381(7) . ?
C12 C14 1.354(7) . ?
C12 C13 1.493(8) . ?
C14 C15 1.378(7) . ?
C15 C16 1.496(8) . ?
C17 C19 1.504(6) . ?
C17 C18 1.511(7) . ?
C20 C21 1.382(7) . ?
C20 C25 1.400(7) . ?
C21 C22 1.367(7) . ?
C22 C23 1.391(10) . ?
C23 C24 1.363(10) . ?
C24 C25 1.392(8) . ?
C26 C31 1.376(8) . ?
C26 C27 1.402(8) . ?
C27 C28 1.379(9) . ?
C28 C29 1.371(13) . ?
C29 C30 1.391(13) . ?
C30 C31 1.392(9) . ?
