#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/17/2221712.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2221712
loop_
_publ_author_name
'Jiang, Xuan-Feng'
'Lian, Heng-Chi'
'Min, Zhong'
'Wang, Xiu-Jian'
'Lin, Jia-Huang'
_publ_section_title
'[μ-N,N,N',N'-Tetrakis(diphenylphosphinomethyl)benzene-1,4-diamine-κ⁴P,P':P'',P''']bis[bis(nitrato-κO)palladium(II)]'
_journal_coeditor_code           HK2653
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m597
_journal_page_last               m598
_journal_paper_doi               10.1107/S160053680901486X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Pd2 (N O3)4 (C58 H52 N2 P4)]'
_chemical_formula_moiety         'C58 H52 N6 O12 P4 Pd2'
_chemical_formula_sum            'C58 H52 N6 O12 P4 Pd2'
_chemical_formula_weight         1361.74
_chemical_name_systematic
;[μ-N,N,N',N'-Tetrakis(diphenylphosphinomethyl)benzene-
1,4-diamine-κ⁴P/i>,P/i>':P/i>'',P/i>''']bis[bis(nitrato-
\kO)palladium(II)]
;
_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                 92.937(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0715(2)
_cell_length_b                   21.3419(7)
_cell_length_c                   16.0283(5)
_cell_measurement_reflns_used    4249
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      11.3
_cell_volume                     2757.43(14)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'Gemini S Untra'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.1503
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13871
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.23
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.370
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.796
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.796
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0313P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                3511
_reflns_number_total             6838
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hk2653.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2221712
_cod_database_fobs_code          2221712
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 1.39486(3) 1.789182(12) 0.214196(13) 0.02504(8) Uani d . 1 . .
P P1 1.22599(9) 1.78487(4) 0.10059(4) 0.02366(18) Uani d . 1 . .
P P2 1.30017(9) 1.88209(4) 0.24940(5) 0.02471(19) Uani d . 1 . .
O O1 1.4811(3) 1.60188(12) 0.22173(15) 0.0613(8) Uani d . 1 . .
O O2 1.3721(3) 1.67330(12) 0.29761(14) 0.0461(6) Uani d . 1 . .
O O3 1.4938(2) 1.69934(10) 0.18353(12) 0.0311(5) Uani d . 1 . .
O O4 1.8332(3) 1.83114(12) 0.33338(14) 0.0518(7) Uani d . 1 . .
O O5 1.7301(3) 1.81444(13) 0.20792(14) 0.0486(7) Uani d . 1 . .
O O6 1.5755(2) 1.80091(10) 0.31524(11) 0.0298(5) Uani d . 1 . .
N N1 1.0910(3) 1.90013(12) 0.11125(14) 0.0271(6) Uani d . 1 . .
N N2 1.4459(3) 1.65651(15) 0.23480(18) 0.0391(7) Uani d . 1 . .
N N3 1.7185(3) 1.81587(13) 0.28399(18) 0.0372(7) Uani d . 1 . .
C C1 0.9830(3) 1.93941(14) -0.02623(17) 0.0299(8) Uani d . 1 . .
H H1A 0.9729 1.8985 -0.0457 0.036 Uiso calc R 1 . .
C C2 1.0433(3) 1.94993(14) 0.05573(16) 0.0240(7) Uani d . 1 . .
C C3 1.0617(3) 2.01198(14) 0.07878(18) 0.0286(8) Uani d . 1 . .
H H3A 1.1061 2.0212 0.1320 0.034 Uiso calc R 1 . .
C C4 1.0437(3) 1.83578(14) 0.09201(17) 0.0264(7) Uani d . 1 . .
H H4A 0.9936 1.8335 0.0358 0.032 Uiso calc R 1 . .
H H4B 0.9624 1.8217 0.1304 0.032 Uiso calc R 1 . .
C C5 1.3384(3) 1.80561(14) 0.00986(17) 0.0264(7) Uani d . 1 . .
C C6 1.5000(4) 1.82739(15) 0.0189(2) 0.0352(8) Uani d . 1 . .
H H6A 1.5527 1.8304 0.0717 0.042 Uiso calc R 1 . .
C C7 1.5828(4) 1.84462(17) -0.0511(2) 0.0417(9) Uani d . 1 . .
H H7A 1.6916 1.8589 -0.0451 0.050 Uiso calc R 1 . .
C C8 1.5067(4) 1.84081(16) -0.1282(2) 0.0390(8) Uani d . 1 . .
H H8A 1.5637 1.8523 -0.1748 0.047 Uiso calc R 1 . .
C C9 1.3461(4) 1.82008(16) -0.1380(2) 0.0378(9) Uani d . 1 . .
H H9A 1.2945 1.8180 -0.1911 0.045 Uiso calc R 1 . .
C C10 1.2609(4) 1.80238(15) -0.06993(18) 0.0321(8) Uani d . 1 . .
H H10A 1.1520 1.7883 -0.0769 0.039 Uiso calc R 1 . .
C C11 1.1447(3) 1.70636(15) 0.08770(17) 0.0249(7) Uani d . 1 . .
C C12 1.2026(4) 1.66574(15) 0.02931(19) 0.0305(8) Uani d . 1 . .
H H12A 1.2794 1.6793 -0.0081 0.037 Uiso calc R 1 . .
C C13 1.1461(5) 1.60480(16) 0.0265(2) 0.0422(9) Uani d . 1 . .
H H13A 1.1848 1.5774 -0.0132 0.051 Uiso calc R 1 . .
C C14 1.0363(4) 1.58451(16) 0.0802(2) 0.0438(9) Uani d . 1 . .
H H14A 0.9999 1.5432 0.0776 0.053 Uiso calc R 1 . .
C C15 0.9767(5) 1.62465(18) 0.1396(2) 0.0497(10) Uani d . 1 . .
H H15A 0.8998 1.6104 0.1765 0.060 Uiso calc R 1 . .
C C16 1.0314(4) 1.68549(16) 0.1437(2) 0.0387(9) Uani d . 1 . .
H H16A 0.9928 1.7126 0.1839 0.046 Uiso calc R 1 . .
C C17 1.1050(3) 1.91098(15) 0.20009(16) 0.0267(7) Uani d . 1 . .
H H17A 1.0131 1.8906 0.2258 0.032 Uiso calc R 1 . .
H H17B 1.0963 1.9556 0.2105 0.032 Uiso calc R 1 . .
C C18 1.4595(4) 1.93885(15) 0.23045(18) 0.0279(7) Uani d . 1 . .
C C19 1.4731(4) 1.96391(15) 0.15109(19) 0.0353(8) Uani d . 1 . .
H H19A 1.3939 1.9545 0.1088 0.042 Uiso calc R 1 . .
C C20 1.6040(4) 2.00260(17) 0.1352(2) 0.0411(9) Uani d . 1 . .
H H20A 1.6123 2.0196 0.0822 0.049 Uiso calc R 1 . .
C C21 1.7229(4) 2.01633(16) 0.1973(2) 0.0404(9) Uani d . 1 . .
H H21A 1.8105 2.0429 0.1863 0.048 Uiso calc R 1 . .
C C22 1.7118(4) 1.99062(17) 0.2755(2) 0.0398(9) Uani d . 1 . .
H H22A 1.7926 1.9995 0.3172 0.048 Uiso calc R 1 . .
C C23 1.5816(4) 1.95192(15) 0.29200(19) 0.0348(8) Uani d . 1 . .
H H23A 1.5752 1.9344 0.3448 0.042 Uiso calc R 1 . .
C C24 1.2525(3) 1.88447(15) 0.35784(17) 0.0258(7) Uani d . 1 . .
C C25 1.2340(4) 1.83006(16) 0.40314(18) 0.0320(8) Uani d . 1 . .
H H25A 1.2617 1.7917 0.3802 0.038 Uiso calc R 1 . .
C C26 1.1751(4) 1.83253(18) 0.4817(2) 0.0410(9) Uani d . 1 . .
H H26A 1.1623 1.7957 0.5117 0.049 Uiso calc R 1 . .
C C27 1.1346(4) 1.8891(2) 0.5166(2) 0.0490(10) Uani d . 1 . .
H H27A 1.0932 1.8903 0.5696 0.059 Uiso calc R 1 . .
C C28 1.1551(4) 1.9432(2) 0.4734(2) 0.0479(10) Uani d . 1 . .
H H28A 1.1301 1.9814 0.4976 0.058 Uiso calc R 1 . .
C C29 1.2133(4) 1.94164(17) 0.39349(19) 0.0374(8) Uani d . 1 . .
H H29A 1.2260 1.9787 0.3639 0.045 Uiso calc R 1 . .
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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P2 Pd1 P1 . . 92.34(3) yes
O3 Pd1 P1 . . 89.72(5) yes
O3 Pd1 P2 . . 177.92(5) yes
O3 Pd1 O6 . . 91.77(8) yes
O6 Pd1 P1 . . 173.04(6) yes
O6 Pd1 P2 . . 86.15(6) yes
C4 P1 Pd1 . . 119.67(10) ?
C5 P1 Pd1 . . 109.72(9) ?
C5 P1 C4 . . 103.24(13) ?
C11 P1 Pd1 . . 109.65(9) ?
C11 P1 C4 . . 104.84(13) ?
C11 P1 C5 . . 109.21(14) ?
C17 P2 Pd1 . . 119.53(10) ?
C18 P2 Pd1 . . 107.51(10) ?
C18 P2 C17 . . 107.81(14) ?
C24 P2 Pd1 . . 111.46(11) ?
C24 P2 C17 . . 100.67(13) ?
C24 P2 C18 . . 109.47(14) ?
N2 O3 Pd1 . . 110.94(18) ?
N3 O6 Pd1 . . 108.45(16) ?
C2 N1 C4 . . 120.8(2) ?
C2 N1 C17 . . 120.1(2) ?
C17 N1 C4 . . 111.6(2) ?
O1 N2 O2 . . 122.5(3) ?
O1 N2 O3 . . 118.9(3) ?
O2 N2 O3 . . 118.5(3) ?
O4 N3 O5 . . 123.5(3) ?
O4 N3 O6 . . 117.6(3) ?
O5 N3 O6 . . 118.9(2) ?
C2 C1 H1A . . 119.2 ?
C3 C1 C2 3_795 . 121.6(3) ?
C3 C1 H1A 3_795 . 119.2 ?
C1 C2 N1 . . 122.5(3) ?
C3 C2 C1 . . 115.7(3) ?
C3 C2 N1 . . 121.7(2) ?
C1 C3 C2 3_795 . 122.6(3) ?
C1 C3 H3A 3_795 . 118.7 ?
C2 C3 H3A . . 118.7 ?
P1 C4 H4A . . 109.6 ?
P1 C4 H4B . . 109.6 ?
N1 C4 P1 . . 110.08(19) ?
N1 C4 H4A . . 109.6 ?
N1 C4 H4B . . 109.6 ?
H4A C4 H4B . . 108.2 ?
C6 C5 P1 . . 120.5(2) ?
C6 C5 C10 . . 119.2(3) ?
C10 C5 P1 . . 120.3(2) ?
C5 C6 H6A . . 120.1 ?
C7 C6 C5 . . 119.7(3) ?
C7 C6 H6A . . 120.1 ?
C6 C7 H7A . . 119.7 ?
C8 C7 C6 . . 120.5(3) ?
C8 C7 H7A . . 119.7 ?
C7 C8 C9 . . 120.4(3) ?
C7 C8 H8A . . 119.8 ?
C9 C8 H8A . . 119.8 ?
C8 C9 C10 . . 120.5(3) ?
C8 C9 H9A . . 119.7 ?
C10 C9 H9A . . 119.7 ?
C5 C10 H10A . . 120.2 ?
C9 C10 C5 . . 119.7(3) ?
C9 C10 H10A . . 120.2 ?
C12 C11 P1 . . 121.9(2) ?
C12 C11 C16 . . 119.8(3) ?
C16 C11 P1 . . 118.1(2) ?
C11 C12 C13 . . 119.6(3) ?
C11 C12 H12A . . 120.2 ?
C13 C12 H12A . . 120.2 ?
C12 C13 H13A . . 119.5 ?
C14 C13 C12 . . 120.9(3) ?
C14 C13 H13A . . 119.5 ?
C13 C14 C15 . . 120.4(3) ?
C13 C14 H14A . . 119.8 ?
C15 C14 H14A . . 119.8 ?
C14 C15 H15A . . 120.1 ?
C16 C15 C14 . . 119.8(3) ?
C16 C15 H15A . . 120.1 ?
C11 C16 H16A . . 120.2 ?
C15 C16 C11 . . 119.6(3) ?
C15 C16 H16A . . 120.2 ?
P2 C17 H17A . . 108.9 ?
P2 C17 H17B . . 108.9 ?
N1 C17 P2 . . 113.2(2) ?
N1 C17 H17A . . 108.9 ?
N1 C17 H17B . . 108.9 ?
H17A C17 H17B . . 107.7 ?
C19 C18 P2 . . 120.2(2) ?
C23 C18 P2 . . 120.1(2) ?
C23 C18 C19 . . 119.1(3) ?
C18 C19 H19A . . 120.0 ?
C20 C19 C18 . . 119.9(3) ?
C20 C19 H19A . . 120.0 ?
C19 C20 C21 . . 120.5(3) ?
C19 C20 H20A . . 119.8 ?
C21 C20 H20A . . 119.8 ?
C20 C21 H21A . . 120.1 ?
C22 C21 C20 . . 119.8(3) ?
C22 C21 H21A . . 120.1 ?
C21 C22 H22A . . 119.9 ?
C23 C22 C21 . . 120.1(3) ?
C23 C22 H22A . . 119.9 ?
C18 C23 H23A . . 119.8 ?
C22 C23 C18 . . 120.5(3) ?
C22 C23 H23A . . 119.8 ?
C25 C24 C29 . . 119.3(3) ?
C25 C24 P2 . . 121.2(2) ?
C29 C24 P2 . . 119.1(2) ?
C24 C25 H25A . . 119.9 ?
C26 C25 C24 . . 120.2(3) ?
C26 C25 H25A . . 119.9 ?
C25 C26 C27 . . 120.5(4) ?
C25 C26 H26A . . 119.8 ?
C27 C26 H26A . . 119.8 ?
C26 C27 H27A . . 120.0 ?
C28 C27 C26 . . 120.0(3) ?
C28 C27 H27A . . 120.0 ?
C27 C28 C29 . . 120.4(4) ?
C27 C28 H28A . . 119.8 ?
C29 C28 H28A . . 119.8 ?
C24 C29 H29A . . 120.2 ?
C28 C29 C24 . . 119.7(3) ?
C28 C29 H29A . . 120.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 P1 . 2.2198(7) yes
Pd1 P2 . 2.2087(9) yes
Pd1 O3 . 2.144(2) yes
Pd1 O6 . 2.1377(17) yes
P1 C4 . 1.829(3) ?
P1 C5 . 1.808(3) ?
P1 C11 . 1.807(3) ?
P2 C17 . 1.833(3) ?
P2 C18 . 1.803(3) ?
P2 C24 . 1.800(3) ?
O1 N2 . 1.221(4) ?
O2 N2 . 1.248(3) ?
O3 N2 . 1.301(3) ?
O4 N3 . 1.231(3) ?
O5 N3 . 1.228(3) ?
O6 N3 . 1.320(3) ?
N1 C2 . 1.426(3) ?
N1 C4 . 1.454(4) ?
N1 C17 . 1.441(3) ?
C1 C2 . 1.396(4) ?
C1 C3 3_795 1.373(4) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.381(4) ?
C3 C1 3_795 1.373(4) ?
C3 H3A . 0.9300 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 C6 . 1.386(4) ?
C5 C10 . 1.396(4) ?
C6 C7 . 1.384(4) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.354(4) ?
C7 H7A . 0.9300 ?
C8 C9 . 1.371(4) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.372(4) ?
C9 H9A . 0.9300 ?
C10 H10A . 0.9300 ?
C11 C12 . 1.375(4) ?
C11 C16 . 1.388(4) ?
C12 C13 . 1.378(4) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.338(5) ?
C13 H13A . 0.9300 ?
C14 C15 . 1.385(5) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.372(5) ?
C15 H15A . 0.9300 ?
C16 H16A . 0.9300 ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C18 C19 . 1.389(4) ?
C18 C23 . 1.387(4) ?
C19 C20 . 1.375(4) ?
C19 H19A . 0.9300 ?
C20 C21 . 1.378(4) ?
C20 H20A . 0.9300 ?
C21 C22 . 1.376(4) ?
C21 H21A . 0.9300 ?
C22 C23 . 1.373(4) ?
C22 H22A . 0.9300 ?
C23 H23A . 0.9300 ?
C24 C25 . 1.381(4) ?
C24 C29 . 1.391(4) ?
C25 C26 . 1.370(4) ?
C25 H25A . 0.9300 ?
C26 C27 . 1.376(5) ?
C26 H26A . 0.9300 ?
C27 C28 . 1.360(5) ?
C27 H27A . 0.9300 ?
C28 C29 . 1.387(4) ?
C28 H28A . 0.9300 ?
C29 H29A . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C4 H4B O5 1_455 0.97 2.31 3.248(3) 163.00 yes
