#------------------------------------------------------------------------------
#$Date: 2016-11-16 16:32:58 +0200 (Wed, 16 Nov 2016) $
#$Revision: 188514 $
#$URL: file:///home/coder/svn-repositories/cod/cif/3/50/00/3500005.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_3500005
loop_
_publ_author_name
'Mohammad Abul Haj'
'Miguel Quirós'
'Juan M. Salas'
_journal_name_full               'Personal communication to COD'
_journal_year                    2011
_chemical_formula_sum            'C22 H25 N14 O9.75 Pd Pt'
_chemical_formula_weight         943.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 102.083(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.130(3)
_cell_length_b                   16.618(2)
_cell_length_c                   9.5517(10)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    297(1)
_cell_measurement_theta_max      15.4
_cell_measurement_theta_min      12.5
_cell_volume                     4055.7(8)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 1.05 - 1.25, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6107
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        15.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.947
_exptl_absorpt_correction_T_max  0.5400
_exptl_absorpt_correction_T_min  0.3039
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
   Psi Scan Reflections used    Mu * R = 0.42  

      H       K       L     2Theta   Chi   Imin/Imax
    2.000   2.000   0.000     5.9    68.3    0.646
    4.000   2.000   0.000     8.1    70.9    0.688
   14.000   6.000   0.000    27.0    69.1    0.487
   12.000   8.000   0.000    27.7    72.1    0.003
;
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1828
_refine_diff_density_max         2.107
_refine_diff_density_min         -2.356
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       0.00072(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         6107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.1823
_refine_ls_R_factor_gt           0.1103
_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)+(0.1000P)²+80.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2492
_refine_ls_wR_factor_ref         0.3005
_reflns_number_gt                3475
_reflns_number_total             6107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ptpdfen.cif
_cod_data_source_block           ptpdfen
_cod_original_cell_volume        4055.6(8)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               3500005
_cod_database_fobs_code          3500005
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_attached_hydrogens
Pt Pt 0.24600(3) 0.5000 0.25433(8) 0.0646(3) Uani 1 2 d S . . 0
Pd Pd 0.34390(6) 0.5000 0.50502(17) 0.0622(4) Uani 1 2 d S . . 0
N1 N 0.1803(5) 0.3201(9) 0.4700(16) 0.085(4) Uani 1 1 d . . . 0
C2 C 0.1839(6) 0.3718(11) 0.3694(18) 0.079(4) Uani 1 1 d . . . 0
H2 H 0.1568 0.3790 0.2900 0.095 Uiso 1 1 d R . . 0
N3 N 0.2281(5) 0.4133(8) 0.3865(13) 0.070(3) Uani 1 1 d . . . 0
C3A C 0.2555(6) 0.3887(9) 0.5122(15) 0.062(3) Uani 1 1 d . . . 0
N4 N 0.3007(5) 0.4137(7) 0.5800(13) 0.069(3) Uani 1 1 d . . . 0
C5 C 0.3180(7) 0.3779(11) 0.7122(17) 0.080(4) Uani 1 1 d . . . 0
H5 H 0.3506 0.3935 0.7649 0.097 Uiso 1 1 d R . . 0
C6 C 0.2917(8) 0.3222(11) 0.7704(19) 0.087(5) Uani 1 1 d . . . 0
H6 H 0.3055 0.3021 0.8612 0.105 Uiso 1 1 d R . . 0
C7 C 0.2429(7) 0.2947(9) 0.6940(18) 0.075(4) Uani 1 1 d . . . 0
O7 O 0.2151(6) 0.2423(8) 0.7321(14) 0.101(4) Uani 1 1 d . . . 0
N8 N 0.2269(5) 0.3334(7) 0.5637(13) 0.068(3) Uani 1 1 d . . . 0
N1M N 0.2625(6) 0.4128(8) 0.1195(13) 0.080(4) Uani 1 1 d . . . 0
H1M H 0.2789 0.3717 0.1703 0.096 Uiso 1 1 d R . . 0
H2M H 0.2831 0.4331 0.0643 0.096 Uiso 1 1 d R . . 0
H3M H 0.2328 0.3952 0.0641 0.096 Uiso 1 1 d R . . 0
N1F N 0.3917(5) 0.4212(8) 0.4364(13) 0.070(3) Uani 1 1 d . . . 0
C1AF C 0.4282(6) 0.4581(10) 0.3779(14) 0.072(4) Uani 1 1 d . . . 0
C2F C 0.3882(7) 0.3426(12) 0.4317(18) 0.085(5) Uani 1 1 d . . . 0
H2F H 0.3607 0.3175 0.4624 0.102 Uiso 1 1 d R . . 0
C3F C 0.4251(9) 0.2953(14) 0.382(2) 0.107(6) Uani 1 1 d . . . 0
H3F H 0.4241 0.2394 0.3864 0.128 Uiso 1 1 d R . . 0
C4F C 0.4634(9) 0.335(2) 0.326(2) 0.126(9) Uani 1 1 d . . . 0
H4F H 0.4876 0.3045 0.2906 0.151 Uiso 1 1 d R . . 0
C4AF C 0.4667(7) 0.4166(15) 0.3214(19) 0.090(5) Uani 1 1 d . . . 0
C5F C 0.5038(6) 0.4614(14) 0.2647(18) 0.111(9) Uani 1 1 d . . . 0
H5F H 0.5288 0.4342 0.2266 0.134 Uiso 1 1 d R . . 0
N1N N 0.3819(11) 0.5000 0.005(3) 0.115(9) Uani 1 2 d S . . 0
O1N O 0.4099(8) 0.5000 -0.077(2) 0.116(7) Uani 1 2 d S . . 0
O2N O 0.3685(7) 0.4367(14) 0.0524(18) 0.149(7) Uani 1 1 d . . . 0
N2N N 0.185(2) 0.5000 0.783(5) 0.191(16) Uiso 1 2 d S . . 0
O3N O 0.1812(15) 0.5000 0.644(4) 0.207(14) Uiso 1 2 d S . . 0
O4N O 0.2288(19) 0.5000 0.819(5) 0.175(15) Uiso 0.75 2 d SP . . 0
O5N O 0.176(3) 0.424(5) 0.835(8) 0.15(2) Uiso 0.25 1 d P . . 0
O1W O 0.4414(10) 0.3159(17) -0.043(3) 0.165(9) Uiso 0.75 1 d P . . 2
O2W O 0.1580(14) 0.306(2) 0.952(4) 0.144(12) Uiso 0.50 1 d P . . 2
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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
N3 Pt N3 90.2(7) 6_565 . ?
N3 Pt N1M 178.9(5) 6_565 . ?
N3 Pt N1M 89.7(5) . . ?
N3 Pt N1M 89.7(5) 6_565 6_565 ?
N3 Pt N1M 178.9(5) . 6_565 ?
N1M Pt N1M 90.3(7) . 6_565 ?
N3 Pt Pd 77.4(4) 6_565 . ?
N3 Pt Pd 77.4(4) . . ?
N1M Pt Pd 103.7(4) . . ?
N1M Pt Pd 103.7(4) 6_565 . ?
N1F Pd N1F 81.2(8) . 6_565 ?
N1F Pd N4 175.1(5) . 6_565 ?
N1F Pd N4 94.8(5) 6_565 6_565 ?
N1F Pd N4 94.8(5) . . ?
N1F Pd N4 175.1(5) 6_565 . ?
N4 Pd N4 89.1(7) 6_565 . ?
N1F Pd Pt 102.4(3) . . ?
N1F Pd Pt 102.4(3) 6_565 . ?
N4 Pd Pt 81.1(3) 6_565 . ?
N4 Pd Pt 81.1(3) . . ?
C2 N1 N8 100.5(13) . . ?
N1 C2 N3 116.5(15) . . ?
C2 N3 C3A 104.0(13) . . ?
C2 N3 Pt 126.9(11) . . ?
C3A N3 Pt 128.9(11) . . ?
N4 C3A N3 128.2(14) . . ?
N4 C3A N8 123.9(14) . . ?
N3 C3A N8 107.8(13) . . ?
C3A N4 C5 114.2(14) . . ?
C3A N4 Pd 124.3(10) . . ?
C5 N4 Pd 121.5(11) . . ?
C6 C5 N4 125.2(17) . . ?
C5 C6 C7 119.9(16) . . ?
O7 C7 N8 120.5(17) . . ?
O7 C7 C6 126.9(16) . . ?
N8 C7 C6 112.6(14) . . ?
C3A N8 N1 111.0(13) . . ?
C3A N8 C7 124.2(14) . . ?
N1 N8 C7 124.7(13) . . ?
C2F N1F C1AF 119.4(14) . . ?
C2F N1F Pd 128.0(12) . . ?
C1AF N1F Pd 112.3(11) . . ?
N1F C1AF C1AF 117.0(9) . 6_565 ?
N1F C1AF C4AF 123.8(17) . . ?
C1AF C1AF C4AF 119.1(12) 6_565 . ?
N1F C2F C3F 121.5(18) . . ?
C2F C3F C4F 117(2) . . ?
C4AF C4F C3F 123(2) . . ?
C4F C4AF C1AF 115(2) . . ?
C4F C4AF C5F 126(2) . . ?
C1AF C4AF C5F 119(2) . . ?
C5F C5F C4AF 121.7(12) 6_565 . ?
O1N N1N O2N 120.7(17) . 6_565 ?
O1N N1N O2N 120.7(17) . . ?
O2N N1N O2N 118(3) 6_565 . ?
O4N N2N O3N 100(5) . . ?
O4N N2N O5N 97(4) . . ?
O3N N2N O5N 112(4) . . ?
O4N N2N O5N 97(4) . 6_565 ?
O3N N2N O5N 112(4) . 6_565 ?
O5N N2N O5N 131(8) . 6_565 ?
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
Pt N3 2.034(12) 6_565 ?
Pt N3 2.034(12) . ?
Pt N1M 2.044(12) . ?
Pt N1M 2.044(12) 6_565 ?
Pt Pd 3.1166(18) . ?
Pd N1F 2.012(12) . ?
Pd N1F 2.012(12) 6_565 ?
Pd N4 2.045(12) 6_565 ?
Pd N4 2.045(12) . ?
N1 C2 1.31(2) . ?
N1 N8 1.370(17) . ?
C2 N3 1.325(19) . ?
N3 C3A 1.328(18) . ?
C3A N4 1.291(18) . ?
C3A N8 1.340(18) . ?
N4 C5 1.38(2) . ?
C5 C6 1.34(2) . ?
C6 C7 1.41(2) . ?
C7 O7 1.236(19) . ?
C7 N8 1.386(19) . ?
N1F C2F 1.31(2) . ?
N1F C1AF 1.349(18) . ?
C1AF C1AF 1.39(3) 6_565 ?
C1AF C4AF 1.42(2) . ?
C2F C3F 1.40(2) . ?
C3F C4F 1.40(3) . ?
C4F C4AF 1.35(3) . ?
C4AF C5F 1.42(3) . ?
C5F C5F 1.28(5) 6_565 ?
N1N O1N 1.18(3) . ?
N1N O2N 1.22(2) 6_565 ?
N1N O2N 1.22(2) . ?
N2N O4N 1.12(5) . ?
N2N O3N 1.32(5) . ?
N2N O5N 1.39(8) . ?
N2N O5N 1.39(8) 6_565 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1M H2M O2N 0.89 2.26 3.00(2) 139.6 .
N1M H1M O7 0.89 2.10 2.940(18) 155.8 7_556
