Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2003
data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Lippert Bernhard'
'A. Albinati'
'Bettina Beck'
'Andrea Erxleben'
'Eva Freisinger'
'Dagmar Holthenrich'
'Lucio Randaccio'
'Alexandra Schneider'
'Ennio Zangrando'
_publ_contact_author_name 'Prof. Bernhard Lippert'
_publ_contact_author_address
;
Fachbereich Chemie
Universitaet Dortmund
Otto-Hahn-Str. 6
D-44221 Dortmund
Germany
;
_publ_contact_author_email lippert@pop.uni-dortmund.de
_publ_contact_author_fax 'Int. code + (231) 755-3797'
_publ_contact_author_phone '231 755-3840'
_publ_contact_letter ?
_publ_requested_journal 'Dalton Trans.'
_publ_section_title
;
Inter- and intramolecular condensation patterns of enPdII with
trans-[a2PtL2]2+ (a = am(m)ine, L = 2-aminopyridine): PtPd3
and Pt2Pd4 species with multiple amide bridges. Unexpected
trapping of a pair of nitrate ions by a Pt2Pd4 double cone.
;
data_1a
_database_code_CSD 203709
_audit_creation_method SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_structural tr-[(NH3)2Pt(2-ampy)Cl]NO4
_chemical_formula_analytical ?
_chemical_formula_sum 'C5 H12 Cl N5 O3 Pt'
_chemical_formula_weight 420.74
_chemical_melting_point ?
_chemical_compound_source ?
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 11.811(2)
_cell_length_b 8.233(2)
_cell_length_c 11.746(2)
_cell_angle_alpha 90.00
_cell_angle_beta 97.46(3)
_cell_angle_gamma 90.00
_cell_volume 1132.5(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 3976
_cell_measurement_theta_min 4.60
_cell_measurement_theta_max 25.64
_exptl_crystal_description square
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.88
_exptl_crystal_size_mid 0.53
_exptl_crystal_size_min 0.50
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.468
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 784
_exptl_absorpt_coefficient_mu 12.623
_exptl_absorpt_correction_type SCALEPACK
_exptl_absorpt_correction_T_min 0.0318
_exptl_absorpt_correction_T_max 0.0614
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device Enraf-Nonius-KappaCCD
_diffrn_measurement_method
;
360 frames via \w-rotation (\D\w\=1\%) and two times 8s per frame
;
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 3976
_diffrn_reflns_av_R_equivalents 0.047
_diffrn_reflns_av_sigmaI/netI 0.033
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 4.60
_diffrn_reflns_theta_max 25.64
_reflns_number_total 2038
_reflns_number_observed 1645
_reflns_observed_criterion >2sigma(I)
_computing_data_collection 'KappaCCD (Nonius BV, Netherlands)'
_computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material SHELXL-93
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary patterson
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment refU
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0059(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 2036
_refine_ls_number_parameters 142
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0335
_refine_ls_R_factor_obs 0.0241
_refine_ls_wR_factor_all 0.0587
_refine_ls_wR_factor_obs 0.0553
_refine_ls_goodness_of_fit_all 1.008
_refine_ls_goodness_of_fit_obs 1.089
_refine_ls_restrained_S_all 1.028
_refine_ls_restrained_S_obs 1.089
_refine_ls_shift/esd_max 0.002
_refine_ls_shift/esd_mean 0.000
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pt1 Pt 0.63894(2) 0.87367(3) 0.391257(14) 0.03250(12) Uani 1 d . .
Cl1 Cl 0.51362(13) 0.8479(2) 0.22563(13) 0.0438(4) Uani 1 d . .
N10 N 0.5700(4) 0.6714(6) 0.4552(4) 0.0468(12) Uani 1 d . .
H10A H 0.5401(32) 0.6084(25) 0.3974(4) 0.079(10) Uiso 1 calc R .
H10B H 0.5157(25) 0.7005(6) 0.4969(30) 0.079(10) Uiso 1 calc R .
H10C H 0.6243(8) 0.6169(27) 0.4991(29) 0.079(10) Uiso 1 calc R .
N10A N 0.7051(4) 1.0773(6) 0.3259(4) 0.0425(11) Uani 1 d . .
H10D H 0.6487(5) 1.1453(21) 0.3010(31) 0.079(10) Uiso 1 calc R .
H10E H 0.7426(29) 1.0499(8) 0.2678(23) 0.079(10) Uiso 1 calc R .
H10F H 0.7528(27) 1.1255(28) 0.3804(10) 0.079(10) Uiso 1 calc R .
N1 N 0.7475(4) 0.9011(5) 0.5379(4) 0.0371(11) Uani 1 d . .
C2 C 0.8593(5) 0.8576(7) 0.5454(5) 0.0428(13) Uani 1 d . .
N2 N 0.8947(4) 0.7867(8) 0.4544(5) 0.066(2) Uani 1 d . .
H2A H 0.8474(4) 0.7698(8) 0.3935(5) 0.098(21) Uiso 1 calc R .
H2B H 0.9650(4) 0.7578(8) 0.4565(5) 0.098(21) Uiso 1 calc R .
C3 C 0.9317(6) 0.8914(8) 0.6449(6) 0.055(2) Uani 1 d . .
H3 H 1.0083(6) 0.8621(8) 0.6502(6) 0.064(10) Uiso 1 calc R .
C4 C 0.8920(6) 0.9674(8) 0.7356(5) 0.051(2) Uani 1 d . .
H4 H 0.9417(6) 0.9911(8) 0.8016(5) 0.064(10) Uiso 1 calc R .
C5 C 0.7794(5) 1.0084(8) 0.7289(5) 0.0504(15) Uani 1 d . .
H5 H 0.7510(5) 1.0586(8) 0.7902(5) 0.064(10) Uiso 1 calc R .
C6 C 0.7087(5) 0.9735(7) 0.6291(4) 0.0426(13) Uani 1 d . .
H6 H 0.6318(5) 1.0006(7) 0.6241(4) 0.064(10) Uiso 1 calc R .
N20 N 0.7987(5) 1.3639(7) 0.5493(4) 0.0485(13) Uani 1 d . .
O21 O 0.6934(4) 1.3608(6) 0.5243(5) 0.0736(15) Uani 1 d . .
O22 O 0.8583(4) 1.2837(7) 0.4898(4) 0.0688(14) Uani 1 d . .
O23 O 0.8463(5) 1.4363(9) 0.6321(5) 0.100(2) Uani 1 d . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0311(2) 0.0361(2) 0.0302(2) 0.00028(8) 0.00403(8) 0.00147(9)
Cl1 0.0409(8) 0.0524(10) 0.0358(7) -0.0005(6) -0.0036(6) -0.0025(7)
N10 0.048(3) 0.045(3) 0.048(3) 0.002(2) 0.008(2) -0.004(2)
N10A 0.043(3) 0.046(3) 0.039(2) 0.005(2) 0.006(2) 0.002(2)
N1 0.033(2) 0.039(3) 0.040(3) -0.001(2) 0.006(2) 0.002(2)
C2 0.037(3) 0.047(3) 0.045(3) 0.001(3) 0.004(2) 0.008(3)
N2 0.041(3) 0.103(5) 0.055(3) -0.023(3) 0.006(3) 0.017(3)
C3 0.045(4) 0.067(4) 0.050(4) 0.004(3) -0.003(3) 0.006(3)
C4 0.060(4) 0.053(4) 0.037(3) -0.004(3) -0.004(3) -0.005(3)
C5 0.057(4) 0.052(4) 0.041(3) -0.006(3) 0.003(3) -0.002(3)
C6 0.040(3) 0.052(4) 0.036(3) -0.005(2) 0.006(2) 0.006(3)
N20 0.054(3) 0.055(3) 0.038(3) 0.008(3) 0.009(2) -0.002(3)
O21 0.035(3) 0.085(4) 0.100(4) 0.008(3) 0.003(2) 0.012(3)
O22 0.050(3) 0.088(4) 0.071(3) -0.017(3) 0.014(2) 0.011(3)
O23 0.107(5) 0.145(6) 0.054(3) -0.048(4) 0.029(3) -0.057(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1 N1 2.022(5) . ?
Pt1 N10 2.039(5) . ?
Pt1 N10A 2.041(5) . ?
Pt1 Cl1 2.296(2) . ?
N10 H10A 0.89 . ?
N10 H10B 0.89 . ?
N10 H10C 0.89 . ?
N10A H10D 0.89 . ?
N10A H10E 0.89 . ?
N10A H10F 0.89 . ?
N1 C6 1.356(7) . ?
N1 C2 1.360(7) . ?
C2 N2 1.333(8) . ?
C2 C3 1.384(9) . ?
N2 H2A 0.86 . ?
N2 H2B 0.86 . ?
C3 C4 1.370(9) . ?
C3 H3 0.93 . ?
C4 C5 1.364(8) . ?
C4 H4 0.93 . ?
C5 C6 1.378(7) . ?
C5 H5 0.93 . ?
C6 H6 0.93 . ?
N20 O23 1.215(7) . ?
N20 O21 1.240(7) . ?
N20 O22 1.244(7) . ?
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 Pt1 N10 91.0(2) . . ?
N1 Pt1 N10A 89.9(2) . . ?
N10 Pt1 N10A 179.0(2) . . ?
N1 Pt1 Cl1 178.69(13) . . ?
N10 Pt1 Cl1 89.55(14) . . ?
N10A Pt1 Cl1 89.62(13) . . ?
Pt1 N10 H10A 109.47(13) . . ?
Pt1 N10 H10B 109.47(14) . . ?
H10A N10 H10B 109.5 . . ?
Pt1 N10 H10C 109.47(14) . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
Pt1 N10A H10D 109.47(13) . . ?
Pt1 N10A H10E 109.47(13) . . ?
H10D N10A H10E 109.5 . . ?
Pt1 N10A H10F 109.47(13) . . ?
H10D N10A H10F 109.5 . . ?
H10E N10A H10F 109.5 . . ?
C6 N1 C2 119.3(5) . . ?
C6 N1 Pt1 118.7(4) . . ?
C2 N1 Pt1 121.9(4) . . ?
N2 C2 N1 117.9(5) . . ?
N2 C2 C3 122.8(5) . . ?
N1 C2 C3 119.4(5) . . ?
C2 N2 H2A 120.0(3) . . ?
C2 N2 H2B 120.0(3) . . ?
H2A N2 H2B 120.0 . . ?
C4 C3 C2 120.8(6) . . ?
C4 C3 H3 119.6(4) . . ?
C2 C3 H3 119.6(4) . . ?
C5 C4 C3 119.8(6) . . ?
C5 C4 H4 120.1(3) . . ?
C3 C4 H4 120.1(4) . . ?
C4 C5 C6 118.4(6) . . ?
C4 C5 H5 120.8(3) . . ?
C6 C5 H5 120.8(4) . . ?
N1 C6 C5 122.3(6) . . ?
N1 C6 H6 118.9(3) . . ?
C5 C6 H6 118.9(4) . . ?
O23 N20 O21 123.1(6) . . ?
O23 N20 O22 118.2(6) . . ?
O21 N20 O22 118.7(6) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 Pt1 N1 C6 -81.4(4) . . . . ?
N10A Pt1 N1 C6 98.0(4) . . . . ?
Cl1 Pt1 N1 C6 31.6(60) . . . . ?
N10 Pt1 N1 C2 102.4(4) . . . . ?
N10A Pt1 N1 C2 -78.2(4) . . . . ?
Cl1 Pt1 N1 C2 -144.5(56) . . . . ?
C6 N1 C2 N2 180.0(6) . . . . ?
Pt1 N1 C2 N2 -3.8(8) . . . . ?
C6 N1 C2 C3 -1.4(8) . . . . ?
Pt1 N1 C2 C3 174.7(4) . . . . ?
N2 C2 C3 C4 178.7(7) . . . . ?
N1 C2 C3 C4 0.2(9) . . . . ?
C2 C3 C4 C5 1.0(10) . . . . ?
C3 C4 C5 C6 -1.0(10) . . . . ?
C2 N1 C6 C5 1.5(9) . . . . ?
Pt1 N1 C6 C5 -174.8(5) . . . . ?
C4 C5 C6 N1 -0.3(9) . . . . ?
_refine_diff_density_max 1.078
_refine_diff_density_min -0.768
_refine_diff_density_rms 0.150
#===END
data_1b
_database_code_CSD 203710
_audit_creation_method SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_structural tr-[(NH3)2Pt(2-ampy)Cl]ClO4
_chemical_formula_analytical ?
_chemical_formula_sum 'C5 H12 Cl2 N4 O4 Pt'
_chemical_formula_weight 458.18
_chemical_melting_point ?
_chemical_compound_source ?
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'
Pt Pt -1.7033 8.3905 '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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/n
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'
_cell_length_a 8.830(2)
_cell_length_b 14.135(3)
_cell_length_c 10.635(2)
_cell_angle_alpha 90.00
_cell_angle_beta 113.97(3)
_cell_angle_gamma 90.00
_cell_volume 1212.9(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 3787
_cell_measurement_theta_min 4.81
_cell_measurement_theta_max 24.70
_exptl_crystal_description 'faceted crystal'
_exptl_crystal_colour colourless
_exptl_crystal_size_max 1.38
_exptl_crystal_size_mid 0.76
_exptl_crystal_size_min 0.75
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.509
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 856
_exptl_absorpt_coefficient_mu 12.014
_exptl_absorpt_correction_type SCALEPACK
_exptl_absorpt_correction_T_min 0.0215
_exptl_absorpt_correction_T_max 0.0401
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device Enraf-Nonius-KappaCCD
_diffrn_measurement_method
;
360 frames via \w-rotation (\D\w\=1\%) and two times 4s per frame
;
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 3787
_diffrn_reflns_av_R_equivalents 0.074
_diffrn_reflns_av_sigmaI/netI 0.0758
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 0
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 4.81
_diffrn_reflns_theta_max 24.70
_reflns_number_total 2060
_reflns_number_observed 1501
_reflns_observed_criterion >2sigma(I)
_computing_data_collection 'KappaCCD (Nonius BV, Netherlands)'
_computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material SHELXL-93
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment refU
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0106(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 2058
_refine_ls_number_parameters 169
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0507
_refine_ls_R_factor_obs 0.0328
_refine_ls_wR_factor_all 0.0778
_refine_ls_wR_factor_obs 0.0732
_refine_ls_goodness_of_fit_all 0.920
_refine_ls_goodness_of_fit_obs 1.044
_refine_ls_restrained_S_all 0.934
_refine_ls_restrained_S_obs 1.044
_refine_ls_shift/esd_max 0.001
_refine_ls_shift/esd_mean 0.000
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pt1 Pt 0.02595(4) 0.83579(2) 0.40429(3) 0.0430(2) Uani 1 d . .
Cl1 Cl 0.0558(3) 0.8627(2) 0.6255(2) 0.0630(7) Uani 1 d . .
N10a N 0.1873(9) 0.9442(6) 0.4261(9) 0.063(2) Uani 1 d . .
H10A H 0.2691(48) 0.9421(31) 0.5097(27) 0.092(17) Uiso 1 calc R .
H10B H 0.1340(22) 0.9991(6) 0.4150(73) 0.092(17) Uiso 1 calc R .
H10C H 0.2290(67) 0.9388(29) 0.3630(47) 0.092(17) Uiso 1 calc R .
N10 N -0.1330(11) 0.7277(6) 0.3910(9) 0.065(2) Uani 1 d . .
H11A H -0.1586(71) 0.7291(31) 0.4637(38) 0.092(17) Uiso 1 calc R .
H11B H -0.0849(35) 0.6728(6) 0.3889(76) 0.092(17) Uiso 1 calc R .
H11C H -0.2250(38) 0.7341(29) 0.3145(39) 0.092(17) Uiso 1 calc R .
N1 N -0.0015(9) 0.8128(5) 0.2084(8) 0.048(2) Uani 1 d . .
C2 C -0.0747(10) 0.8759(7) 0.1068(9) 0.049(2) Uani 1 d . .
N2 N -0.1356(10) 0.9556(6) 0.1359(8) 0.068(2) Uani 1 d . .
H2A H -0.1275(10) 0.9658(6) 0.2181(8) 0.079(25) Uiso 1 calc R .
H2B H -0.1828(10) 0.9968(6) 0.0723(8) 0.079(25) Uiso 1 calc R .
C3 C -0.0819(11) 0.8593(7) -0.0262(9) 0.053(2) Uani 1 d . .
H3 H -0.1300(11) 0.9040(7) -0.0951(9) 0.062(14) Uiso 1 calc R .
C4 C -0.0195(13) 0.7789(9) -0.0537(10) 0.065(3) Uani 1 d . .
H4 H -0.0247(13) 0.7676(9) -0.1415(10) 0.062(14) Uiso 1 calc R .
C5 C 0.0535(12) 0.7124(8) 0.0515(10) 0.060(2) Uani 1 d . .
H5 H 0.0980(12) 0.6563(8) 0.0355(10) 0.062(14) Uiso 1 calc R .
C6 C 0.0568(13) 0.7324(7) 0.1763(10) 0.059(3) Uani 1 d . .
H6 H 0.1027(13) 0.6875(7) 0.2454(10) 0.062(14) Uiso 1 calc R .
Cl2 Cl 0.4765(3) 0.9560(2) 0.2182(2) 0.0502(6) Uani 1 d . .
O21 O 0.5061(13) 1.0316(7) 0.1462(11) 0.107(3) Uani 1 d . .
O22 O 0.4286(37) 0.9986(21) 0.3320(34) 0.153(13) Uani 0.58 d P .
O22A O 0.4991(35) 0.9790(25) 0.3442(25) 0.100(12) Uani 0.42 d P .
O23 O 0.3295(13) 0.9143(9) 0.1333(12) 0.162(5) Uani 1 d . .
O24 O 0.6166(21) 0.9050(16) 0.2894(19) 0.098(6) Uani 0.58 d P .
O24A O 0.5686(38) 0.8768(19) 0.2015(35) 0.109(10) Uani 0.42 d P .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0407(2) 0.0422(2) 0.0390(2) 0.0003(2) 0.00890(14) 0.0010(2)
Cl1 0.079(2) 0.059(2) 0.0420(12) -0.0018(10) 0.0152(12) 0.0029(12)
N10a 0.057(4) 0.058(5) 0.067(5) -0.001(4) 0.017(4) -0.004(4)
N10 0.069(5) 0.062(5) 0.063(5) -0.013(4) 0.027(4) -0.012(4)
N1 0.048(4) 0.050(5) 0.046(4) 0.002(3) 0.021(3) 0.002(3)
C2 0.033(4) 0.052(5) 0.052(6) 0.007(5) 0.006(4) 0.001(4)
N2 0.082(6) 0.065(5) 0.046(5) 0.005(4) 0.016(4) 0.028(5)
C3 0.056(5) 0.064(7) 0.040(5) 0.000(4) 0.019(4) -0.002(5)
C4 0.066(6) 0.087(8) 0.042(5) -0.009(5) 0.022(5) -0.012(6)
C5 0.060(6) 0.073(7) 0.056(6) -0.005(5) 0.033(5) 0.008(5)
C6 0.074(7) 0.044(6) 0.063(6) -0.001(5) 0.033(6) 0.005(5)
Cl2 0.0494(11) 0.0499(13) 0.0513(13) 0.0043(10) 0.0204(10) -0.0006(10)
O21 0.140(7) 0.088(7) 0.133(8) 0.037(6) 0.098(7) 0.009(6)
O22 0.217(28) 0.132(18) 0.218(27) 0.058(17) 0.199(24) 0.051(18)
O22A 0.117(21) 0.159(29) 0.049(11) -0.073(16) 0.060(13) -0.068(20)
O23 0.111(7) 0.157(10) 0.134(9) -0.014(8) -0.037(7) -0.054(8)
O24 0.059(9) 0.123(18) 0.103(14) 0.048(12) 0.023(10) 0.047(11)
O24A 0.127(26) 0.058(12) 0.174(32) -0.017(19) 0.094(24) 0.033(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1 N1 2.024(8) . ?
Pt1 N10 2.040(8) . ?
Pt1 N10a 2.041(8) . ?
Pt1 Cl1 2.290(3) . ?
N10a H10A 0.89 . ?
N10a H10B 0.89 . ?
N10a H10C 0.89 . ?
N10 H11A 0.89 . ?
N10 H11B 0.89 . ?
N10 H11C 0.89 . ?
N1 C2 1.347(12) . ?
N1 C6 1.347(12) . ?
C2 N2 1.338(12) . ?
C2 C3 1.409(13) . ?
N2 H2A 0.86 . ?
N2 H2B 0.86 . ?
C3 C4 1.346(14) . ?
C3 H3 0.93 . ?
C4 C5 1.401(14) . ?
C4 H4 0.93 . ?
C5 C6 1.346(13) . ?
C5 H5 0.93 . ?
C6 H6 0.93 . ?
Cl2 O22A 1.31(2) . ?
Cl2 O24 1.36(2) . ?
Cl2 O23 1.377(9) . ?
Cl2 O21 1.400(8) . ?
Cl2 O24A 1.44(2) . ?
Cl2 O22 1.56(3) . ?
O22 O22A 0.64(5) . ?
O22A O24 1.73(3) . ?
O24 O24A 0.94(3) . ?
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 Pt1 N10 91.0(3) . . ?
N1 Pt1 N10a 91.4(3) . . ?
N10 Pt1 N10a 177.6(3) . . ?
N1 Pt1 Cl1 179.6(2) . . ?
N10 Pt1 Cl1 89.1(2) . . ?
N10a Pt1 Cl1 88.6(3) . . ?
Pt1 N10a H10A 109.5(2) . . ?
Pt1 N10a H10B 109.5(2) . . ?
H10A N10a H10B 109.5 . . ?
Pt1 N10a H10C 109.5(2) . . ?
H10A N10a H10C 109.47(7) . . ?
H10B N10a H10C 109.5 . . ?
Pt1 N10 H11A 109.5(2) . . ?
Pt1 N10 H11B 109.5(3) . . ?
H11A N10 H11B 109.5 . . ?
Pt1 N10 H11C 109.5(3) . . ?
H11A N10 H11C 109.5 . . ?
H11B N10 H11C 109.5 . . ?
C2 N1 C6 117.7(8) . . ?
C2 N1 Pt1 122.5(7) . . ?
C6 N1 Pt1 119.9(6) . . ?
N2 C2 N1 118.7(9) . . ?
N2 C2 C3 120.9(8) . . ?
N1 C2 C3 120.4(9) . . ?
C2 N2 H2A 120.0(5) . . ?
C2 N2 H2B 120.0(5) . . ?
H2A N2 H2B 120.0 . . ?
C4 C3 C2 120.2(9) . . ?
C4 C3 H3 119.9(6) . . ?
C2 C3 H3 119.9(6) . . ?
C3 C4 C5 119.3(9) . . ?
C3 C4 H4 120.4(6) . . ?
C5 C4 H4 120.4(6) . . ?
C6 C5 C4 117.7(10) . . ?
C6 C5 H5 121.2(6) . . ?
C4 C5 H5 121.2(6) . . ?
C5 C6 N1 124.7(10) . . ?
C5 C6 H6 117.6(6) . . ?
N1 C6 H6 117.6(5) . . ?
O22A Cl2 O24 80.6(18) . . ?
O22A Cl2 O23 119.2(13) . . ?
O24 Cl2 O23 122.6(11) . . ?
O22A Cl2 O21 112.6(15) . . ?
O24 Cl2 O21 112.2(10) . . ?
O23 Cl2 O21 107.7(8) . . ?
O22A Cl2 O24A 117.4(22) . . ?
O24 Cl2 O24A 39.3(11) . . ?
O23 Cl2 O24A 90.9(14) . . ?
O21 Cl2 O24A 106.6(14) . . ?
O22A Cl2 O22 24.1(21) . . ?
O24 Cl2 O22 104.2(15) . . ?
O23 Cl2 O22 101.2(13) . . ?
O21 Cl2 O22 107.4(11) . . ?
O24A Cl2 O22 138.1(18) . . ?
O22A O22 Cl2 56.2(33) . . ?
O22 O22A Cl2 99.7(47) . . ?
O22 O22A O24 148.6(45) . . ?
Cl2 O22A O24 51.0(10) . . ?
O24A O24 Cl2 74.5(21) . . ?
O24A O24 O22A 119.9(26) . . ?
Cl2 O24 O22A 48.4(11) . . ?
O24 O24A Cl2 66.3(18) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 Pt1 N1 C2 113.7(7) . . . . ?
N10a Pt1 N1 C2 -66.7(7) . . . . ?
Cl1 Pt1 N1 C2 10.9(309) . . . . ?
N10 Pt1 N1 C6 -67.3(8) . . . . ?
N10a Pt1 N1 C6 112.4(7) . . . . ?
Cl1 Pt1 N1 C6 -170.0(300) . . . . ?
C6 N1 C2 N2 179.1(8) . . . . ?
Pt1 N1 C2 N2 -1.9(12) . . . . ?
C6 N1 C2 C3 -3.0(12) . . . . ?
Pt1 N1 C2 C3 176.1(6) . . . . ?
N2 C2 C3 C4 179.7(9) . . . . ?
N1 C2 C3 C4 1.8(13) . . . . ?
C2 C3 C4 C5 -0.4(14) . . . . ?
C3 C4 C5 C6 0.3(15) . . . . ?
C4 C5 C6 N1 -1.6(16) . . . . ?
C2 N1 C6 C5 3.0(14) . . . . ?
Pt1 N1 C6 C5 -176.1(8) . . . . ?
O22A Cl2 O22 O22A 0.00(3) . . . . ?
O24 Cl2 O22 O22A 12.8(57) . . . . ?
O23 Cl2 O22 O22A 140.8(52) . . . . ?
O21 Cl2 O22 O22A -106.5(53) . . . . ?
O24A Cl2 O22 O22A 36.6(65) . . . . ?
Cl2 O22 O22A Cl2 0.000(11) . . . . ?
Cl2 O22 O22A O24 -18.9(82) . . . . ?
O24 Cl2 O22A O22 -167.5(56) . . . . ?
O23 Cl2 O22A O22 -45.3(60) . . . . ?
O21 Cl2 O22A O22 82.3(52) . . . . ?
O24A Cl2 O22A O22 -153.3(50) . . . . ?
O22 Cl2 O22A O22 0.00(3) . . . . ?
O24 Cl2 O22A O24 0.000(11) . . . . ?
O23 Cl2 O22A O24 122.2(14) . . . . ?
O21 Cl2 O22A O24 -110.3(12) . . . . ?
O24A Cl2 O22A O24 14.1(22) . . . . ?
O22 Cl2 O22A O24 167.5(56) . . . . ?
O22A Cl2 O24 O24A 160.0(33) . . . . ?
O23 Cl2 O24 O24A 41.2(33) . . . . ?
O21 Cl2 O24 O24A -89.3(30) . . . . ?
O24A Cl2 O24 O24A 0.00(2) . . . . ?
O22 Cl2 O24 O24A 154.7(30) . . . . ?
O22A Cl2 O24 O22A 0.000(13) . . . . ?
O23 Cl2 O24 O22A -118.7(16) . . . . ?
O21 Cl2 O24 O22A 110.7(14) . . . . ?
O24A Cl2 O24 O22A -160.0(33) . . . . ?
O22 Cl2 O24 O22A -5.2(22) . . . . ?
O22 O22A O24 O24A 1.9(130) . . . . ?
Cl2 O22A O24 O24A -22.4(37) . . . . ?
O22 O22A O24 Cl2 24.2(108) . . . . ?
Cl2 O22A O24 Cl2 0.000(14) . . . . ?
Cl2 O24 O24A Cl2 0.00(2) . . . . ?
O22A O24 O24A Cl2 17.2(28) . . . . ?
O22A Cl2 O24A O24 -22.4(36) . . . . ?
O24 Cl2 O24A O24 0.00(3) . . . . ?
O23 Cl2 O24A O24 -146.3(28) . . . . ?
O21 Cl2 O24A O24 105.0(28) . . . . ?
O22 Cl2 O24A O24 -38.3(42) . . . . ?
_refine_diff_density_max 0.971
_refine_diff_density_min -1.056
_refine_diff_density_rms 0.153
#===END
data_3a
_database_code_CSD 203711
_audit_creation_method SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C12 H22 N8 O6 Pt'
_chemical_formula_weight 569.47
_chemical_melting_point ?
_chemical_compound_source ?
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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/n
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'
_cell_length_a 8.013(2)
_cell_length_b 9.394(2)
_cell_length_c 12.320(3)
_cell_angle_alpha 90.00
_cell_angle_beta 91.27(2)
_cell_angle_gamma 90.00
_cell_volume 927.1(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 50
_cell_measurement_theta_min 7.0
_cell_measurement_theta_max 14.9
_exptl_crystal_description block
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_size_max 0.288
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.096
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.040
_exptl_crystal_density_method ?
_exptl_crystal_F_000 552
_exptl_absorpt_coefficient_mu 7.615
_exptl_absorpt_correction_type psi-scans
_exptl_absorpt_correction_T_min 0.703
_exptl_absorpt_correction_T_max 0.794
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device 'Nicolet R3m/V'
_diffrn_measurement_method omega/2theta
_diffrn_standards_number 5
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time 150min.
_diffrn_standards_decay_% ?
_diffrn_reflns_number 1847
_diffrn_reflns_av_R_equivalents 0.0476
_diffrn_reflns_av_sigmaI/netI 0.0527
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 2.73
_diffrn_reflns_theta_max 25.04
_reflns_number_total 1775
_reflns_number_observed 917
_reflns_observed_criterion >2sigma(I)
_computing_data_collection 'Nicolet R3m/V software'
_computing_cell_refinement 'Nicolet R3m/V software'
_computing_data_reduction 'Nicolet R3m/V software'
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material SHELXL-93
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary Patterson
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment
'Uiso=1.2xU(attached) and 1.5xU(attached) for methyl groups'
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1775
_refine_ls_number_parameters 119
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0598
_refine_ls_R_factor_obs 0.0283
_refine_ls_wR_factor_all 0.1544
_refine_ls_wR_factor_obs 0.0739
_refine_ls_goodness_of_fit_all 0.968
_refine_ls_goodness_of_fit_obs 1.186
_refine_ls_restrained_S_all 1.861
_refine_ls_restrained_S_obs 1.186
_refine_ls_shift/esd_max 0.000
_refine_ls_shift/esd_mean 0.000
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pt1 Pt 0.0000 0.0000 0.0000 0.0244(3) Uani 1 d S .
C1 C 0.3001(21) -0.1487(15) 0.0997(14) 0.059(7) Uani 1 d . .
H1A H 0.3669(21) -0.1724(15) 0.1628(14) 0.088 Uiso 1 d R .
H1B H 0.3659(21) -0.0950(15) 0.0501(14) 0.088 Uiso 1 d R .
H1C H 0.2616(21) -0.2345(15) 0.0650(14) 0.088 Uiso 1 d R .
C2 C 0.0735(20) 0.3034(12) 0.0712(12) 0.037(5) Uani 1 d . .
C3 C 0.1611(21) 0.4280(13) 0.0722(13) 0.035(5) Uani 1 d . .
H3 H 0.1419(21) 0.4961(13) 0.1253(13) 0.042 Uiso 1 d R .
C4 C 0.2810(25) 0.4516(13) -0.0050(16) 0.038(6) Uani 1 d . .
H4 H 0.3365(25) 0.5384(13) -0.0083(16) 0.046 Uiso 1 d R .
C5 C 0.3195(19) 0.3447(12) -0.0791(14) 0.042(6) Uani 1 d . .
H5 H 0.3954(19) 0.3617(12) -0.1337(14) 0.050 Uiso 1 d R .
C6 C 0.2391(21) 0.2179(13) -0.0719(13) 0.032(5) Uani 1 d . .
H6 H 0.2713(21) 0.1445(13) -0.1175(13) 0.038 Uiso 1 d R .
N1 N 0.1174(15) 0.1951(9) -0.0017(9) 0.026(2) Uiso 1 d . .
N2 N -0.0488(18) 0.2784(13) 0.1429(11) 0.039(5) Uani 1 d . .
H2A H -0.0955(18) 0.1913(13) 0.1441(11) 0.047 Uiso 1 d R .
H2B H -0.0813(18) 0.3455(13) 0.1901(11) 0.047 Uiso 1 d R .
N3 N 0.1543(17) -0.0553(10) 0.1296(10) 0.042(5) Uani 1 d . .
H3A H 0.1912(17) 0.0244(10) 0.1628(10) 0.050 Uiso 1 d R .
H3B H 0.0951(17) -0.1051(10) 0.1779(10) 0.050 Uiso 1 d R .
N4 N -0.0317(20) -0.3095(11) 0.3038(14) 0.051(6) Uani 1 d . .
O1 O -0.1247(20) -0.4104(12) 0.3229(13) 0.083(8) Uani 1 d . .
O2 O -0.0819(17) -0.1842(11) 0.3084(11) 0.064(5) Uani 1 d . .
O3 O 0.1135(17) -0.3326(11) 0.2738(14) 0.060(6) Uani 1 d . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0250(4) 0.0200(3) 0.0282(4) -0.0002(4) -0.0007(4) -0.0036(4)
C1 0.050(12) 0.064(9) 0.061(12) -0.012(9) -0.024(13) 0.021(9)
C2 0.050(11) 0.030(6) 0.030(8) -0.002(6) -0.024(10) -0.002(7)
C3 0.032(9) 0.032(7) 0.041(9) -0.012(7) -0.005(11) 0.000(7)
C4 0.036(12) 0.022(6) 0.058(11) 0.007(7) 0.003(14) -0.012(6)
C5 0.030(9) 0.034(7) 0.062(12) 0.012(8) 0.011(12) -0.016(7)
C6 0.026(9) 0.030(6) 0.040(10) -0.003(7) 0.027(12) 0.000(7)
N2 0.041(11) 0.048(7) 0.029(8) -0.003(7) 0.025(12) -0.012(7)
N3 0.049(9) 0.020(4) 0.055(8) -0.003(5) -0.018(10) -0.009(5)
N4 0.066(11) 0.024(6) 0.064(11) 0.003(7) -0.016(13) 0.017(7)
O1 0.088(13) 0.039(6) 0.122(15) 0.029(8) 0.009(16) -0.014(8)
O2 0.063(10) 0.059(7) 0.070(10) -0.014(7) 0.002(11) 0.020(7)
O3 0.043(8) 0.054(7) 0.082(12) 0.008(7) 0.013(13) 0.021(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1 N1 2.060(10) 3 ?
Pt1 N1 2.060(10) . ?
Pt1 N3 2.064(8) 3 ?
Pt1 N3 2.064(8) . ?
C1 N3 1.51(2) . ?
C2 N2 1.35(2) . ?
C2 C3 1.37(2) . ?
C2 N1 1.41(2) . ?
C3 C4 1.39(3) . ?
C4 C5 1.40(2) . ?
C5 C6 1.36(2) . ?
C6 N1 1.34(2) . ?
N4 O1 1.23(2) . ?
N4 O2 1.245(14) . ?
N4 O3 1.25(3) . ?
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 Pt1 N1 180.0 3 . ?
N1 Pt1 N3 88.0(3) 3 3 ?
N1 Pt1 N3 92.0(3) . 3 ?
N1 Pt1 N3 92.0(3) 3 . ?
N1 Pt1 N3 88.0(3) . . ?
N3 Pt1 N3 180.0 3 . ?
N2 C2 C3 121.4(15) . . ?
N2 C2 N1 119.1(12) . . ?
C3 C2 N1 119.4(18) . . ?
C2 C3 C4 119.7(15) . . ?
C3 C4 C5 120.1(14) . . ?
C6 C5 C4 118.4(20) . . ?
N1 C6 C5 122.5(16) . . ?
C6 N1 C2 119.6(12) . . ?
C6 N1 Pt1 119.3(9) . . ?
C2 N1 Pt1 121.1(12) . . ?
C1 N3 Pt1 114.2(9) . . ?
O1 N4 O2 121.4(19) . . ?
O1 N4 O3 119.7(14) . . ?
O2 N4 O3 118.8(16) . . ?
_refine_diff_density_max 0.500
_refine_diff_density_min -0.780
_refine_diff_density_rms 0.146
#===END
data_3b
_database_code_CSD 203712
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
trans-bis(methylamine)-bis(2-aminopyridine)-platinum(II)
diperchlorate
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '(C12 H22 N6 Pt 2+) 2(Cl O4 1-)'
_chemical_formula_sum 'C12 H22 Cl2 N6 O8 Pt'
_chemical_formula_weight 644.35
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'
Pt Pt -1.7033 8.3905 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P21/n
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'
_cell_length_a 9.394(1)
_cell_length_b 11.127(1)
_cell_length_c 10.174(1)
_cell_angle_alpha 90.00
_cell_angle_beta 98.71(1)
_cell_angle_gamma 90.00
_cell_volume 1051.19(18)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description prism
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.036
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 624
_exptl_absorpt_coefficient_mu 6.980
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type Mok\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'image plate dip1030'
_diffrn_measurement_method 'laser scanner'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 4857
_diffrn_reflns_av_R_equivalents 0.0383
_diffrn_reflns_av_sigmaI/netI 0.0558
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 2.86
_diffrn_reflns_theta_max 28.28
_reflns_number_total 2575
_reflns_number_gt 1863
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Nonius Xpress'
_computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)'
_computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)'
_computing_structure_solution 'SHELX97 (Sheldrick, 1998)'
_computing_structure_refinement 'SHELX97 (Sheldrick, 1998)'
_computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)'
_computing_publication_material 'Wingx 1.64.04 (Farrugia, 1999)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 2575
_refine_ls_number_parameters 162
_refine_ls_number_restraints 57
_refine_ls_R_factor_all 0.0515
_refine_ls_R_factor_gt 0.0377
_refine_ls_wR_factor_ref 0.1027
_refine_ls_wR_factor_gt 0.0953
_refine_ls_goodness_of_fit_ref 1.043
_refine_ls_restrained_S_all 1.154
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.001
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
Pt Pt 0.0000 0.0000 0.0000 0.04642(17) Uani 1 2 d S . .
N1 N 0.0637(5) 0.0576(4) 0.1896(4) 0.0478(10) Uani 1 1 d . . .
N2 N 0.0018(7) 0.2539(5) 0.1364(6) 0.0755(17) Uani 1 1 d . . .
H2A H -0.0242 0.2320 0.0553 0.091 Uiso 1 1 calc R . .
H2B H -0.0056 0.3280 0.1585 0.091 Uiso 1 1 calc R . .
N3 N -0.2080(7) -0.0182(4) 0.0385(7) 0.0571(13) Uani 1 1 d . . .
H3A H -0.2277 0.0438 0.0897 0.069 Uiso 1 1 calc R . .
H3B H -0.2684 -0.0132 -0.0389 0.069 Uiso 1 1 calc R . .
C1 C -0.2367(8) -0.1301(6) 0.1046(10) 0.090(2) Uani 1 1 d . . .
H1A H -0.2074 -0.1970 0.0555 0.134 Uiso 1 1 calc R . .
H1B H -0.3379 -0.1362 0.1088 0.134 Uiso 1 1 calc R . .
H1C H -0.1838 -0.1309 0.1931 0.134 Uiso 1 1 calc R . .
C2 C 0.0543(6) 0.1721(5) 0.2291(6) 0.0530(13) Uani 1 1 d . . .
C3 C 0.0960(7) 0.2047(7) 0.3619(6) 0.0673(16) Uani 1 1 d . . .
H3 H 0.0886 0.2841 0.3886 0.081 Uiso 1 1 calc R . .
C4 C 0.1480(7) 0.1182(7) 0.4521(6) 0.0745(18) Uani 1 1 d . . .
H4 H 0.1771 0.1392 0.5405 0.089 Uiso 1 1 calc R . .
C5 C 0.1578(13) 0.0002(6) 0.4132(10) 0.075(2) Uani 1 1 d . . .
H5 H 0.1916 -0.0591 0.4744 0.090 Uiso 1 1 calc R . .
C6 C 0.1160(9) -0.0271(7) 0.2817(8) 0.0652(18) Uani 1 1 d . . .
H6 H 0.1236 -0.1062 0.2540 0.078 Uiso 1 1 calc R . .
Cl Cl 0.01924(17) 0.39571(14) -0.25170(15) 0.0619(4) Uani 1 1 d . . .
O1 O -0.0491(12) 0.5035(4) -0.2961(11) 0.105(3) Uani 1 1 d D . .
O2 O 0.028(2) 0.393(2) -0.1135(12) 0.153(9) Uani 0.438(15) 1 d PDU . .
O3 O 0.1436(15) 0.3605(11) -0.2910(18) 0.091(6) Uani 0.438(15) 1 d PDU . .
O4 O -0.0895(19) 0.3049(12) -0.299(3) 0.158(9) Uani 0.438(15) 1 d PDU . .
O5 O 0.036(2) 0.3304(12) -0.3672(13) 0.160(7) Uani 0.562(15) 1 d PDU . .
O6 O 0.1616(12) 0.4245(15) -0.1932(17) 0.158(8) Uani 0.562(15) 1 d PDU . .
O7 O -0.0418(12) 0.3221(9) -0.1693(13) 0.086(4) Uani 0.562(15) 1 d PDU . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt 0.0497(2) 0.0429(2) 0.0468(2) -0.00465(11) 0.00780(12) 0.00301(11)
N1 0.054(3) 0.046(2) 0.042(2) -0.005(2) 0.0057(19) 0.002(2)
N2 0.105(5) 0.051(3) 0.069(4) -0.007(3) 0.008(3) 0.010(3)
N3 0.048(3) 0.065(3) 0.060(3) -0.006(2) 0.012(2) 0.002(2)
C1 0.071(4) 0.082(5) 0.125(7) 0.023(5) 0.043(4) -0.002(4)
C2 0.057(3) 0.051(3) 0.053(3) -0.009(2) 0.014(2) 0.001(2)
C3 0.073(4) 0.071(4) 0.060(4) -0.020(3) 0.017(3) -0.007(3)
C4 0.076(4) 0.098(5) 0.048(3) -0.009(4) 0.006(3) -0.001(4)
C5 0.087(6) 0.076(6) 0.058(4) 0.007(3) -0.001(4) 0.003(3)
C6 0.074(5) 0.064(4) 0.057(4) 0.000(3) 0.007(3) 0.008(3)
Cl 0.0667(9) 0.0597(8) 0.0602(8) 0.0065(7) 0.0124(6) 0.0045(7)
O1 0.116(7) 0.076(5) 0.115(7) 0.017(3) -0.009(6) 0.024(3)
O2 0.164(15) 0.24(2) 0.055(8) 0.007(10) 0.002(9) 0.051(14)
O3 0.081(9) 0.076(8) 0.130(12) 0.025(8) 0.062(9) 0.014(6)
O4 0.131(13) 0.085(10) 0.25(2) -0.029(12) 0.017(13) -0.044(9)
O5 0.261(18) 0.138(11) 0.090(8) -0.043(7) 0.053(10) 0.025(12)
O6 0.100(9) 0.150(13) 0.191(14) 0.073(11) -0.079(9) -0.046(8)
O7 0.095(8) 0.072(6) 0.101(8) 0.024(6) 0.050(6) -0.005(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1 2.035(4) 3 ?
Pt N1 2.035(4) . ?
Pt N3 2.060(6) 3 ?
Pt N3 2.060(6) . ?
N1 C2 1.343(6) . ?
N1 C6 1.367(9) . ?
N2 C2 1.349(8) . ?
N3 C1 1.461(8) . ?
C2 C3 1.396(8) . ?
C3 C4 1.369(9) . ?
C4 C5 1.378(8) . ?
C5 C6 1.371(13) . ?
Cl O3 1.349(10) . ?
Cl O7 1.360(8) . ?
Cl O2 1.396(12) . ?
Cl O1 1.402(6) . ?
Cl O5 1.410(10) . ?
Cl O6 1.415(9) . ?
Cl O4 1.466(13) . ?
O2 O7 1.124(19) . ?
O2 O6 1.63(2) . ?
O3 O6 1.214(17) . ?
O3 O5 1.226(17) . ?
O4 O7 1.34(2) . ?
O4 O5 1.479(19) . ?
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 Pt N1 180.00(10) 3 . ?
N1 Pt N3 90.1(2) 3 3 ?
N1 Pt N3 89.9(2) . 3 ?
N1 Pt N3 89.9(2) 3 . ?
N1 Pt N3 90.1(2) . . ?
N3 Pt N3 180.0(4) 3 . ?
C2 N1 C6 118.8(6) . . ?
C2 N1 Pt 124.0(4) . . ?
C6 N1 Pt 117.1(5) . . ?
C1 N3 Pt 114.7(4) . . ?
N1 C2 N2 117.7(5) . . ?
N1 C2 C3 121.0(6) . . ?
N2 C2 C3 121.3(5) . . ?
C4 C3 C2 119.0(6) . . ?
C3 C4 C5 120.7(7) . . ?
C6 C5 C4 118.0(7) . . ?
N1 C6 C5 122.4(7) . . ?
O3 Cl O7 118.2(6) . . ?
O3 Cl O2 111.7(9) . . ?
O7 Cl O2 48.1(9) . . ?
O3 Cl O1 121.8(7) . . ?
O7 Cl O1 119.9(6) . . ?
O2 Cl O1 107.3(8) . . ?
O3 Cl O5 52.7(7) . . ?
O7 Cl O5 108.2(7) . . ?
O2 Cl O5 146.2(10) . . ?
O1 Cl O5 105.9(7) . . ?
O3 Cl O6 52.0(8) . . ?
O7 Cl O6 109.7(7) . . ?
O2 Cl O6 70.9(9) . . ?
O1 Cl O6 107.4(7) . . ?
O5 Cl O6 104.6(9) . . ?
O3 Cl O4 107.1(8) . . ?
O7 Cl O4 56.6(8) . . ?
O2 Cl O4 104.5(10) . . ?
O1 Cl O4 102.8(8) . . ?
O5 Cl O4 61.9(9) . . ?
O6 Cl O4 149.5(9) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Pt N1 C2 0.0(3) 3 . . . ?
N3 Pt N1 C2 95.0(4) 3 . . . ?
N3 Pt N1 C2 -85.0(4) . . . . ?
N1 Pt N1 C6 0.0(3) 3 . . . ?
N3 Pt N1 C6 -86.5(5) 3 . . . ?
N3 Pt N1 C6 93.5(5) . . . . ?
N1 Pt N3 C1 97.6(6) 3 . . . ?
N1 Pt N3 C1 -82.4(6) . . . . ?
N3 Pt N3 C1 0.0(4) 3 . . . ?
C6 N1 C2 N2 -179.8(6) . . . . ?
Pt N1 C2 N2 -1.3(7) . . . . ?
C6 N1 C2 C3 -0.5(8) . . . . ?
Pt N1 C2 C3 178.0(4) . . . . ?
N1 C2 C3 C4 0.5(9) . . . . ?
N2 C2 C3 C4 179.7(6) . . . . ?
C2 C3 C4 C5 -0.7(11) . . . . ?
C3 C4 C5 C6 1.0(14) . . . . ?
C2 N1 C6 C5 0.8(12) . . . . ?
Pt N1 C6 C5 -177.8(8) . . . . ?
C4 C5 C6 N1 -1.0(15) . . . . ?
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full 28.28
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max 1.309
_refine_diff_density_min -0.641
_refine_diff_density_rms 0.289
#===END
data_5
_database_code_CSD 203713
_audit_creation_method SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_structural
;
[trans-{(CH3NH2)2Pt(ampy-N1,N2,N2')2}2{enPd}4](NO3)8*5H2O
;
_chemical_formula_analytical ?
_chemical_formula_sum 'C16 H41 N14 O14.50 Pd2 Pt'
_chemical_formula_weight 1069.52
_chemical_melting_point ?
_chemical_compound_source ?
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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.447(2)
_cell_length_b 13.201(3)
_cell_length_c 13.673(3)
_cell_angle_alpha 108.51(3)
_cell_angle_beta 103.75(3)
_cell_angle_gamma 110.50(3)
_cell_volume 1687.7(6)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 5905
_cell_measurement_theta_min 4.54
_cell_measurement_theta_max 25.62
_exptl_crystal_description square
_exptl_crystal_colour yellow-orange
_exptl_crystal_size_max 0.63
_exptl_crystal_size_mid 0.51
_exptl_crystal_size_min 0.50
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.105
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1042
_exptl_absorpt_coefficient_mu 5.270
_exptl_absorpt_correction_type SCALEPACK
_exptl_absorpt_correction_T_min 0.1360
_exptl_absorpt_correction_T_max 0.1780
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device Enraf-Nonius-KappaCCD
_diffrn_measurement_method
;
360 frames via \w-rotation (\D\w\=1\%) and two times 10s per frame
;
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 5905
_diffrn_reflns_av_R_equivalents 0.042
_diffrn_reflns_av_sigmaI/netI 0.0532
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 4.54
_diffrn_reflns_theta_max 25.62
_reflns_number_total 5905
_reflns_number_observed 4461
_reflns_observed_criterion >2sigma(I)
_computing_data_collection 'KappaCCD (Nonius BV, Netherlands)'
_computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material SHELXL-93
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens
;
geom, except H2 and H2' difmap
;
_refine_ls_hydrogen_treatment
;
mixed: refU, except H2 and H2' xyz refall and U=1.5U(bonded)
;
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5901
_refine_ls_number_parameters 444
_refine_ls_number_restraints 10
_refine_ls_R_factor_all 0.0498
_refine_ls_R_factor_obs 0.0323
_refine_ls_wR_factor_all 0.0733
_refine_ls_wR_factor_obs 0.0695
_refine_ls_goodness_of_fit_all 0.937
_refine_ls_goodness_of_fit_obs 1.048
_refine_ls_restrained_S_all 0.954
_refine_ls_restrained_S_obs 1.054
_refine_ls_shift/esd_max 0.004
_refine_ls_shift/esd_mean 0.000
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pt1 Pt 0.84690(2) 0.70445(2) 0.47353(2) 0.03390(8) Uani 1 d . .
N7 N 1.0386(5) 0.7210(5) 0.5301(4) 0.0431(12) Uani 1 d . .
H7A H 1.0517(5) 0.6806(5) 0.4705(4) 0.046(9) Uiso 1 calc R .
H7B H 1.0981(5) 0.7993(5) 0.5582(4) 0.046(9) Uiso 1 calc R .
N7' N 0.6524(5) 0.6796(5) 0.4108(5) 0.0479(13) Uani 1 d . .
H7'1 H 0.6469(5) 0.7418(5) 0.4576(5) 0.046(9) Uiso 1 calc R .
H7'2 H 0.6372(5) 0.6831(5) 0.3445(5) 0.046(9) Uiso 1 calc R .
C7 C 1.0729(8) 0.6792(8) 0.6153(7) 0.070(2) Uani 1 d . .
H7C H 1.1610(23) 0.6835(44) 0.6282(32) 0.097(12) Uiso 1 calc R .
H7D H 1.0067(30) 0.5974(16) 0.5895(19) 0.097(12) Uiso 1 calc R .
H7E H 1.0732(51) 0.7294(29) 0.6840(14) 0.097(12) Uiso 1 calc R .
C7' C 0.5437(7) 0.5684(8) 0.3937(8) 0.080(3) Uani 1 d . .
H7'3 H 0.5424(32) 0.5008(8) 0.3387(30) 0.097(12) Uiso 1 calc R .
H7'4 H 0.4583(9) 0.5690(21) 0.3681(41) 0.097(12) Uiso 1 calc R .
H7'5 H 0.5587(27) 0.5620(23) 0.4632(11) 0.097(12) Uiso 1 calc R .
Pd1 Pd 0.84869(4) 0.88730(4) 0.21759(4) 0.03686(12) Uani 1 d . .
N11 N 0.6617(5) 0.7440(5) 0.1170(5) 0.0518(14) Uani 1 d . .
H11A H 0.6666(5) 0.6937(5) 0.0575(5) 0.085(10) Uiso 1 calc R .
H11B H 0.6328(5) 0.7033(5) 0.1553(5) 0.085(10) Uiso 1 calc R .
C11 C 0.5664(7) 0.7862(7) 0.0787(7) 0.076(2) Uani 1 d . .
H11C H 0.5369(7) 0.8168(7) 0.1375(7) 0.106(16) Uiso 1 calc R .
H11D H 0.4873(7) 0.7205(7) 0.0136(7) 0.106(16) Uiso 1 calc R .
C12 C 0.6355(8) 0.8823(8) 0.0498(8) 0.087(3) Uani 1 d . .
H12A H 0.5783(8) 0.9191(8) 0.0328(8) 0.106(16) Uiso 1 calc R .
H12B H 0.6530(8) 0.8488(8) -0.0161(8) 0.106(16) Uiso 1 calc R .
N12 N 0.7650(5) 0.9742(5) 0.1452(5) 0.059(2) Uani 1 d . .
H12C H 0.7501(5) 1.0258(5) 0.1958(5) 0.085(10) Uiso 1 calc R .
H12D H 0.8221(5) 1.0163(5) 0.1210(5) 0.085(10) Uiso 1 calc R .
Pd2 Pd 0.88364(4) 1.09614(4) 0.70094(4) 0.03675(12) Uani 1 d . .
N21 N 0.7020(5) 0.9965(5) 0.7020(6) 0.061(2) Uani 1 d . .
H21A H 0.6585(5) 0.9241(5) 0.6419(6) 0.085(10) Uiso 1 calc R .
H21B H 0.7164(5) 0.9844(5) 0.7640(6) 0.085(10) Uiso 1 calc R .
C21 C 0.6182(8) 1.0572(8) 0.6997(11) 0.111(4) Uani 1 d . .
H21C H 0.5346(8) 1.0043(8) 0.6335(11) 0.184(28) Uiso 1 calc R .
H21D H 0.5943(8) 1.0667(8) 0.7644(11) 0.184(28) Uiso 1 calc R .
C22 C 0.6687(8) 1.1648(8) 0.6993(10) 0.104(4) Uani 1 d . .
H22A H 0.6531(8) 1.2192(8) 0.7554(10) 0.184(28) Uiso 1 calc R .
H22B H 0.6184(8) 1.1565(8) 0.6268(10) 0.184(28) Uiso 1 calc R .
N22 N 0.8138(5) 1.2204(5) 0.7212(5) 0.057(2) Uani 1 d . .
H22C H 0.8606(5) 1.2797(5) 0.7917(5) 0.085(10) Uiso 1 calc R .
H22D H 0.8271(5) 1.2533(5) 0.6738(5) 0.085(10) Uiso 1 calc R .
N1 N 0.8344(4) 0.6244(4) 0.3156(4) 0.0363(11) Uani 1 d . .
C2 C 0.8759(5) 0.6797(5) 0.2532(5) 0.0335(13) Uani 1 d . .
N2 N 0.9299(5) 0.8055(4) 0.2984(4) 0.0357(11) Uani 1 d . .
H2 H 0.9271(65) 0.8212(60) 0.3606(55) 0.054 Uiso 1 d . .
C3 C 0.8671(5) 0.6138(5) 0.1470(5) 0.0408(15) Uani 1 d . .
H3 H 0.8950(5) 0.6527(5) 0.1045(5) 0.051(7) Uiso 1 calc R .
C4 C 0.8169(6) 0.4907(6) 0.1052(6) 0.048(2) Uani 1 d . .
H4 H 0.8109(6) 0.4460(6) 0.0345(6) 0.051(7) Uiso 1 calc R .
C5 C 0.7753(6) 0.4337(6) 0.1697(6) 0.046(2) Uani 1 d . .
H5 H 0.7422(6) 0.3508(6) 0.1430(6) 0.051(7) Uiso 1 calc R .
C6 C 0.7838(6) 0.5011(5) 0.2723(5) 0.0409(15) Uani 1 d . .
H6 H 0.7546(6) 0.4626(5) 0.3147(5) 0.051(7) Uiso 1 calc R .
N1' N 0.8504(5) 0.7633(4) 0.6316(4) 0.0379(12) Uani 1 d . .
C2' C 0.9035(5) 0.8785(5) 0.7090(5) 0.0341(13) Uani 1 d . .
N2' N 0.9587(5) 0.9723(4) 0.6804(4) 0.0379(12) Uani 1 d . .
H2' H 0.9497(64) 0.9408(59) 0.6113(57) 0.057 Uiso 1 d . .
C3' C 0.9030(6) 0.9046(6) 0.8148(5) 0.046(2) Uani 1 d . .
H3' H 0.9405(6) 0.9844(6) 0.8672(5) 0.051(7) Uiso 1 calc R .
C4' C 0.8472(6) 0.8133(6) 0.8433(6) 0.054(2) Uani 1 d . .
H4' H 0.8461(6) 0.8303(6) 0.9144(6) 0.051(7) Uiso 1 calc R .
C5' C 0.7928(6) 0.6953(6) 0.7640(6) 0.051(2) Uani 1 d . .
H5' H 0.7548(6) 0.6316(6) 0.7809(6) 0.051(7) Uiso 1 calc R .
C6' C 0.7960(6) 0.6743(6) 0.6617(6) 0.047(2) Uani 1 d . .
H6' H 0.7590(6) 0.5948(6) 0.6089(6) 0.051(7) Uiso 1 calc R .
N10 N 0.7457(6) -0.0212(5) 0.4169(5) 0.0536(14) Uani 1 d . .
O11 O 0.8609(5) -0.0076(4) 0.4577(4) 0.0617(14) Uani 1 d . .
O12 O 0.7257(5) 0.0494(5) 0.3799(6) 0.091(2) Uani 1 d . .
O13 O 0.6487(5) -0.1037(6) 0.4100(7) 0.116(3) Uani 1 d . .
N20 N 0.8618(8) 0.1799(7) 0.0183(7) 0.076(2) Uani 1 d . .
O21 O 0.8140(8) 0.0714(6) -0.0316(6) 0.118(3) Uani 1 d . .
O22 O 0.8692(8) 0.2207(7) 0.1153(7) 0.116(2) Uani 1 d . .
O23 O 0.9093(8) 0.2504(7) -0.0180(6) 0.129(3) Uani 1 d . .
N30 N 1.5714(9) 1.2946(7) 0.4063(8) 0.102(3) Uani 1 d D .
O31 O 1.6768(6) 1.3890(5) 0.4519(6) 0.089(2) Uani 1 d D .
O32 O 1.5079(12) 1.2523(11) 0.3019(10) 0.105(4) Uiso 0.60 d PD 1
O33 O 1.5185(19) 1.2462(16) 0.4617(14) 0.143(7) Uiso 0.60 d PD 1
O32A O 1.4475(15) 1.2621(18) 0.3688(17) 0.116(6) Uiso 0.40 d PD 2
O33A O 1.5765(27) 1.2449(22) 0.4759(18) 0.130(9) Uiso 0.40 d PD 2
N40 N 0.5833(6) 0.4900(6) -0.1281(5) 0.058(2) Uani 1 d . .
O41 O 0.6891(5) 0.5867(5) -0.0789(4) 0.0692(15) Uani 1 d . .
O42 O 0.5841(6) 0.3946(6) -0.1768(5) 0.094(2) Uani 1 d . .
O43 O 0.4737(5) 0.4891(5) -0.1306(6) 0.089(2) Uani 1 d . .
O1W O 0.1106(5) 0.4978(5) 0.1469(5) 0.079(2) Uani 1 d . .
O2W O 0.1256(5) 0.5944(5) 0.3655(5) 0.076(2) Uani 1 d . .
O3WA O 0.5521(39) 0.0771(36) 0.1702(32) 0.145(14) Uiso 0.25 d P .
O3WB O 0.6166(33) 0.1153(29) 0.1532(27) 0.113(10) Uiso 0.25 d P .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.03485(13) 0.02729(13) 0.03652(14) 0.01452(10) 0.01428(10) 0.01063(9)
N7 0.041(3) 0.042(3) 0.038(3) 0.013(3) 0.016(2) 0.014(2)
N7' 0.044(3) 0.040(3) 0.053(4) 0.018(3) 0.017(3) 0.017(2)
C7 0.070(5) 0.106(7) 0.072(5) 0.061(5) 0.036(4) 0.057(5)
C7' 0.043(4) 0.086(6) 0.104(7) 0.055(6) 0.019(4) 0.017(4)
Pd1 0.0339(2) 0.0324(3) 0.0403(3) 0.0148(2) 0.0145(2) 0.0123(2)
N11 0.040(3) 0.050(3) 0.051(4) 0.018(3) 0.011(2) 0.012(2)
C11 0.038(4) 0.075(6) 0.096(7) 0.039(5) 0.012(4) 0.015(4)
C12 0.064(5) 0.085(6) 0.093(7) 0.042(6) 0.000(5) 0.032(5)
N12 0.049(3) 0.056(4) 0.072(4) 0.033(3) 0.017(3) 0.025(3)
Pd2 0.0335(2) 0.0314(3) 0.0407(3) 0.0149(2) 0.0133(2) 0.0118(2)
N21 0.045(3) 0.051(4) 0.098(5) 0.040(4) 0.034(3) 0.023(3)
C21 0.040(5) 0.072(6) 0.231(13) 0.068(8) 0.059(6) 0.031(4)
C22 0.049(5) 0.082(6) 0.216(12) 0.087(8) 0.060(6) 0.041(5)
N22 0.049(3) 0.044(3) 0.079(4) 0.024(3) 0.028(3) 0.024(3)
N1 0.038(3) 0.029(3) 0.037(3) 0.015(2) 0.012(2) 0.012(2)
C2 0.025(3) 0.034(3) 0.036(3) 0.014(3) 0.009(2) 0.011(2)
N2 0.041(3) 0.030(3) 0.034(3) 0.013(2) 0.016(2) 0.013(2)
C3 0.033(3) 0.040(4) 0.040(4) 0.013(3) 0.011(3) 0.013(3)
C4 0.051(4) 0.039(4) 0.042(4) 0.008(3) 0.012(3) 0.023(3)
C5 0.047(4) 0.031(3) 0.052(4) 0.013(3) 0.014(3) 0.019(3)
C6 0.046(4) 0.030(3) 0.043(4) 0.017(3) 0.014(3) 0.015(3)
N1' 0.044(3) 0.030(3) 0.044(3) 0.020(2) 0.022(2) 0.015(2)
C2' 0.040(3) 0.030(3) 0.039(4) 0.018(3) 0.021(3) 0.017(3)
N2' 0.040(3) 0.036(3) 0.033(3) 0.017(2) 0.013(2) 0.011(2)
C3' 0.051(4) 0.043(4) 0.039(4) 0.017(3) 0.021(3) 0.017(3)
C4' 0.061(4) 0.062(5) 0.050(4) 0.032(4) 0.029(3) 0.028(4)
C5' 0.055(4) 0.047(4) 0.057(5) 0.035(4) 0.027(3) 0.016(3)
C6' 0.049(4) 0.042(4) 0.055(4) 0.029(3) 0.027(3) 0.016(3)
N10 0.048(4) 0.043(3) 0.066(4) 0.020(3) 0.023(3) 0.020(3)
O11 0.055(3) 0.078(4) 0.056(3) 0.030(3) 0.024(3) 0.035(3)
O12 0.062(3) 0.071(4) 0.152(6) 0.067(4) 0.037(3) 0.031(3)
O13 0.052(4) 0.080(4) 0.219(8) 0.097(5) 0.037(4) 0.018(3)
N20 0.104(5) 0.072(5) 0.061(5) 0.028(5) 0.041(4) 0.045(4)
O21 0.185(7) 0.066(5) 0.103(5) 0.024(4) 0.070(5) 0.059(5)
O22 0.157(6) 0.118(6) 0.094(6) 0.040(5) 0.066(5) 0.080(5)
O23 0.149(6) 0.112(6) 0.082(5) 0.055(5) 0.033(5) 0.012(5)
N30 0.117(7) 0.068(5) 0.133(8) 0.047(6) 0.053(7) 0.050(5)
O31 0.065(3) 0.061(4) 0.118(5) 0.038(4) 0.032(3) 0.010(3)
N40 0.046(4) 0.068(4) 0.052(4) 0.028(3) 0.017(3) 0.017(3)
O41 0.052(3) 0.076(4) 0.053(3) 0.028(3) 0.016(2) 0.004(3)
O42 0.119(5) 0.075(4) 0.089(5) 0.021(4) 0.042(4) 0.058(4)
O43 0.052(3) 0.092(4) 0.125(5) 0.053(4) 0.036(3) 0.030(3)
O1W 0.085(4) 0.089(4) 0.081(4) 0.036(3) 0.039(3) 0.055(3)
O2W 0.083(4) 0.088(4) 0.077(4) 0.035(3) 0.038(3) 0.057(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1 N1 2.025(5) . ?
Pt1 N1' 2.037(5) . ?
Pt1 N7' 2.050(5) . ?
Pt1 N7 2.052(5) . ?
N7 C7 1.469(8) . ?
N7 N7' 7.123(8) 2_776 ?
N7 H7A 0.90 . ?
N7 H7B 0.90 . ?
N7' C7' 1.458(8) . ?
N7' H7'1 0.90 . ?
N7' H7'2 0.90 . ?
C7 H7C 0.96 . ?
C7 H7D 0.96 . ?
C7 H7E 0.96 . ?
C7' H7'3 0.96 . ?
C7' H7'4 0.96 . ?
C7' H7'5 0.96 . ?
Pd1 N11 2.041(5) . ?
Pd1 N2 2.056(5) . ?
Pd1 N12 2.062(5) . ?
Pd1 N2' 2.068(5) 2_776 ?
Pd1 Pd2 2.9036(10) 2_776 ?
N11 C11 1.453(9) . ?
N11 H11A 0.90 . ?
N11 H11B 0.90 . ?
C11 C12 1.469(11) . ?
C11 H11C 0.97 . ?
C11 H11D 0.97 . ?
C12 N12 1.478(9) . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
N12 H12C 0.90 . ?
N12 H12D 0.90 . ?
Pd2 N22 2.035(5) . ?
Pd2 N21 2.040(5) . ?
Pd2 N2 2.069(5) 2_776 ?
Pd2 N2' 2.073(5) . ?
Pd2 Pd1 2.9036(10) 2_776 ?
N21 C21 1.451(9) . ?
N21 H21A 0.90 . ?
N21 H21B 0.90 . ?
C21 C22 1.334(11) . ?
C21 H21C 0.97 . ?
C21 H21D 0.97 . ?
C22 N22 1.470(9) . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
N22 H22C 0.90 . ?
N22 H22D 0.90 . ?
N1 C2 1.353(7) . ?
N1 C6 1.378(7) . ?
C2 C3 1.395(8) . ?
C2 N2 1.403(7) . ?
N2 Pd2 2.069(5) 2_776 ?
N2 N2' 4.859(7) . ?
N2 H2 0.82(6) . ?
C3 C4 1.378(8) . ?
C3 H3 0.93 . ?
C4 C5 1.393(9) . ?
C4 H4 0.93 . ?
C5 C6 1.361(8) . ?
C5 H5 0.93 . ?
C6 H6 0.93 . ?
N1' C2' 1.352(7) . ?
N1' C6' 1.361(7) . ?
C2' C3' 1.379(8) . ?
C2' N2' 1.401(7) . ?
N2' Pd1 2.068(5) 2_776 ?
N2' H2' 0.87(7) . ?
C3' C4' 1.375(9) . ?
C3' H3' 0.93 . ?
C4' C5' 1.385(9) . ?
C4' H4' 0.93 . ?
C5' C6' 1.348(9) . ?
C5' H5' 0.93 . ?
C6' H6' 0.93 . ?
N10 O13 1.210(7) . ?
N10 O11 1.226(6) . ?
N10 O12 1.253(7) . ?
N20 O21 1.212(9) . ?
N20 O23 1.215(9) . ?
N20 O22 1.232(9) . ?
N30 O31 1.222(8) . ?
N30 O32A 1.244(13) . ?
N30 O32 1.263(10) . ?
N30 O33 1.267(12) . ?
N30 O33A 1.318(14) . ?
N40 O42 1.228(8) . ?
N40 O41 1.239(7) . ?
N40 O43 1.242(7) . ?
O3WA O3WB 0.87(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 Pt1 N1' 172.6(2) . . ?
N1 Pt1 N7' 90.1(2) . . ?
N1' Pt1 N7' 90.0(2) . . ?
N1 Pt1 N7 87.7(2) . . ?
N1' Pt1 N7 92.0(2) . . ?
N7' Pt1 N7 177.1(2) . . ?
C7 N7 Pt1 117.9(4) . . ?
C7 N7 N7' 126.9(4) . 2_776 ?
Pt1 N7 N7' 92.7(2) . 2_776 ?
C7 N7 H7A 107.8(4) . . ?
Pt1 N7 H7A 107.84(14) . . ?
N7' N7 H7A 101.39(7) 2_776 . ?
C7 N7 H7B 107.8(4) . . ?
Pt1 N7 H7B 107.84(15) . . ?
N7' N7 H7B 19.48(6) 2_776 . ?
H7A N7 H7B 107.2 . . ?
C7' N7' Pt1 117.1(4) . . ?
C7' N7' H7'1 108.0(4) . . ?
Pt1 N7' H7'1 108.0(2) . . ?
C7' N7' H7'2 108.0(4) . . ?
Pt1 N7' H7'2 108.0(2) . . ?
H7'1 N7' H7'2 107.3 . . ?
N7 C7 H7C 109.5(3) . . ?
N7 C7 H7D 109.5(4) . . ?
H7C C7 H7D 109.5 . . ?
N7 C7 H7E 109.5(4) . . ?
H7C C7 H7E 109.47(7) . . ?
H7D C7 H7E 109.47(7) . . ?
N7' C7' H7'3 109.5(4) . . ?
N7' C7' H7'4 109.5(4) . . ?
H7'3 C7' H7'4 109.5 . . ?
N7' C7' H7'5 109.5(4) . . ?
H7'3 C7' H7'5 109.5 . . ?
H7'4 C7' H7'5 109.5 . . ?
N11 Pd1 N2 98.3(2) . . ?
N11 Pd1 N12 82.4(2) . . ?
N2 Pd1 N12 176.4(2) . . ?
N11 Pd1 N2' 177.7(2) . 2_776 ?
N2 Pd1 N2' 79.7(2) . 2_776 ?
N12 Pd1 N2' 99.7(2) . 2_776 ?
N11 Pd1 Pd2 132.2(2) . 2_776 ?
N2 Pd1 Pd2 45.45(13) . 2_776 ?
N12 Pd1 Pd2 136.0(2) . 2_776 ?
N2' Pd1 Pd2 45.55(14) 2_776 2_776 ?
C11 N11 Pd1 109.7(4) . . ?
C11 N11 H11A 109.7(4) . . ?
Pd1 N11 H11A 109.7(2) . . ?
C11 N11 H11B 109.7(4) . . ?
Pd1 N11 H11B 109.7(2) . . ?
H11A N11 H11B 108.2 . . ?
N11 C11 C12 107.9(6) . . ?
N11 C11 H11C 110.1(4) . . ?
C12 C11 H11C 110.1(6) . . ?
N11 C11 H11D 110.1(4) . . ?
C12 C11 H11D 110.1(5) . . ?
H11C C11 H11D 108.4 . . ?
C11 C12 N12 109.4(7) . . ?
C11 C12 H12A 109.8(5) . . ?
N12 C12 H12A 109.8(4) . . ?
C11 C12 H12B 109.8(6) . . ?
N12 C12 H12B 109.8(5) . . ?
H12A C12 H12B 108.2 . . ?
C12 N12 Pd1 108.3(5) . . ?
C12 N12 H12C 110.0(5) . . ?
Pd1 N12 H12C 110.0(2) . . ?
C12 N12 H12D 110.0(5) . . ?
Pd1 N12 H12D 110.0(2) . . ?
H12C N12 H12D 108.4 . . ?
N22 Pd2 N21 82.0(2) . . ?
N22 Pd2 N2 99.5(2) . 2_776 ?
N21 Pd2 N2 178.4(2) . 2_776 ?
N22 Pd2 N2' 178.7(2) . . ?
N21 Pd2 N2' 99.3(2) . . ?
N2 Pd2 N2' 79.3(2) 2_776 . ?
N22 Pd2 Pd1 133.5(2) . 2_776 ?
N21 Pd2 Pd1 133.4(2) . 2_776 ?
N2 Pd2 Pd1 45.07(14) 2_776 2_776 ?
N2' Pd2 Pd1 45.41(13) . 2_776 ?
C21 N21 Pd2 110.8(5) . . ?
C21 N21 H21A 109.5(5) . . ?
Pd2 N21 H21A 109.5(2) . . ?
C21 N21 H21B 109.5(6) . . ?
Pd2 N21 H21B 109.5(2) . . ?
H21A N21 H21B 108.1 . . ?
C22 C21 N21 118.3(6) . . ?
C22 C21 H21C 107.7(7) . . ?
N21 C21 H21C 107.7(5) . . ?
C22 C21 H21D 107.7(7) . . ?
N21 C21 H21D 107.7(6) . . ?
H21C C21 H21D 107.1 . . ?
C21 C22 N22 115.8(7) . . ?
C21 C22 H22A 108.3(7) . . ?
N22 C22 H22A 108.3(5) . . ?
C21 C22 H22B 108.3(7) . . ?
N22 C22 H22B 108.3(5) . . ?
H22A C22 H22B 107.4 . . ?
C22 N22 Pd2 110.8(5) . . ?
C22 N22 H22C 109.5(5) . . ?
Pd2 N22 H22C 109.5(2) . . ?
C22 N22 H22D 109.5(5) . . ?
Pd2 N22 H22D 109.5(2) . . ?
H22C N22 H22D 108.1 . . ?
C2 N1 C6 118.7(5) . . ?
C2 N1 Pt1 126.8(4) . . ?
C6 N1 Pt1 114.4(4) . . ?
N1 C2 C3 121.0(5) . . ?
N1 C2 N2 118.6(5) . . ?
C3 C2 N2 120.5(5) . . ?
C2 N2 Pd1 121.6(4) . . ?
C2 N2 Pd2 118.5(4) . 2_776 ?
Pd1 N2 Pd2 89.5(2) . 2_776 ?
C2 N2 N2' 110.7(3) . . ?
Pd1 N2 N2' 106.8(2) . . ?
Pd2 N2 N2' 107.3(2) 2_776 . ?
C2 N2 H2 100.7(49) . . ?
Pd1 N2 H2 112.5(48) . . ?
Pd2 N2 H2 114.9(47) 2_776 . ?
N2' N2 H2 10.1(48) . . ?
C4 C3 C2 119.6(6) . . ?
C4 C3 H3 120.2(4) . . ?
C2 C3 H3 120.2(4) . . ?
C3 C4 C5 119.5(6) . . ?
C3 C4 H4 120.3(4) . . ?
C5 C4 H4 120.3(4) . . ?
C6 C5 C4 119.1(6) . . ?
C6 C5 H5 120.5(4) . . ?
C4 C5 H5 120.5(4) . . ?
C5 C6 N1 122.2(6) . . ?
C5 C6 H6 118.9(4) . . ?
N1 C6 H6 118.9(3) . . ?
C2' N1' C6' 117.6(5) . . ?
C2' N1' Pt1 127.6(4) . . ?
C6' N1' Pt1 114.7(4) . . ?
N1' C2' C3' 121.0(5) . . ?
N1' C2' N2' 119.1(5) . . ?
C3' C2' N2' 119.8(5) . . ?
C2' N2' Pd1 120.1(4) . 2_776 ?
C2' N2' Pd2 117.8(4) . . ?
Pd1 N2' Pd2 89.0(2) 2_776 . ?
C2' N2' N2 109.5(3) . . ?
Pd1 N2' N2 109.1(2) 2_776 . ?
Pd2 N2' N2 109.7(2) . . ?
C2' N2' H2' 108.2(46) . . ?
Pd1 N2' H2' 111.5(44) 2_776 . ?
Pd2 N2' H2' 108.8(44) . . ?
N2 N2' H2' 2.5(42) . . ?
C4' C3' C2' 120.4(6) . . ?
C4' C3' H3' 119.8(4) . . ?
C2' C3' H3' 119.8(4) . . ?
C3' C4' C5' 118.6(6) . . ?
C3' C4' H4' 120.7(4) . . ?
C5' C4' H4' 120.7(4) . . ?
C6' C5' C4' 118.9(6) . . ?
C6' C5' H5' 120.6(4) . . ?
C4' C5' H5' 120.6(4) . . ?
C5' C6' N1' 123.5(6) . . ?
C5' C6' H6' 118.2(4) . . ?
N1' C6' H6' 118.2(4) . . ?
O13 N10 O11 121.0(6) . . ?
O13 N10 O12 118.5(6) . . ?
O11 N10 O12 120.5(6) . . ?
O21 N20 O23 124.9(9) . . ?
O21 N20 O22 116.7(8) . . ?
O23 N20 O22 118.3(9) . . ?
O31 N30 O32A 137.5(12) . . ?
O31 N30 O32 117.7(10) . . ?
O31 N30 O33 122.0(13) . . ?
O32 N30 O33 119.8(13) . . ?
O31 N30 O33A 105.5(14) . . ?
O32A N30 O33A 98.9(17) . . ?
O42 N40 O41 121.1(6) . . ?
O42 N40 O43 119.1(6) . . ?
O41 N40 O43 119.8(7) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Pt1 N7 C7 -129.6(5) . . . . ?
N1' Pt1 N7 C7 43.0(5) . . . . ?
N7' Pt1 N7 C7 -91.4(43) . . . . ?
N1 Pt1 N7 N7' 95.59(15) . . . 2_776 ?
N1' Pt1 N7 N7' -91.85(15) . . . 2_776 ?
N7' Pt1 N7 N7' 133.8(42) . . . 2_776 ?
N1 Pt1 N7' C7' 90.7(6) . . . . ?
N1' Pt1 N7' C7' -81.9(6) . . . . ?
N7 Pt1 N7' C7' 52.5(44) . . . . ?
N2 Pd1 N11 C11 160.0(5) . . . . ?
N12 Pd1 N11 C11 -16.5(5) . . . . ?
N2' Pd1 N11 C11 -172.6(50) 2_776 . . . ?
Pd2 Pd1 N11 C11 -165.6(4) 2_776 . . . ?
Pd1 N11 C11 C12 41.5(8) . . . . ?
N11 C11 C12 N12 -52.5(10) . . . . ?
C11 C12 N12 Pd1 37.5(9) . . . . ?
N11 Pd1 N12 C12 -11.5(5) . . . . ?
N2 Pd1 N12 C12 -112.2(31) . . . . ?
N2' Pd1 N12 C12 167.6(5) 2_776 . . . ?
Pd2 Pd1 N12 C12 135.3(5) 2_776 . . . ?
N22 Pd2 N21 C21 8.1(7) . . . . ?
N2 Pd2 N21 C21 160.7(78) 2_776 . . . ?
N2' Pd2 N21 C21 -171.9(6) . . . . ?
Pd1 Pd2 N21 C21 153.5(6) 2_776 . . . ?
Pd2 N21 C21 C22 -1.1(14) . . . . ?
N21 C21 C22 N22 -10.3(17) . . . . ?
C21 C22 N22 Pd2 16.6(13) . . . . ?
N21 Pd2 N22 C22 -13.1(6) . . . . ?
N2 Pd2 N22 C22 167.7(6) 2_776 . . . ?
N2' Pd2 N22 C22 167.3(100) . . . . ?
Pd1 Pd2 N22 C22 -158.4(5) 2_776 . . . ?
N1' Pt1 N1 C2 -174.7(12) . . . . ?
N7' Pt1 N1 C2 94.7(5) . . . . ?
N7 Pt1 N1 C2 -87.1(5) . . . . ?
N1' Pt1 N1 C6 2.0(16) . . . . ?
N7' Pt1 N1 C6 -88.7(4) . . . . ?
N7 Pt1 N1 C6 89.6(4) . . . . ?
C6 N1 C2 C3 0.4(7) . . . . ?
Pt1 N1 C2 C3 176.9(4) . . . . ?
C6 N1 C2 N2 -178.7(5) . . . . ?
Pt1 N1 C2 N2 -2.1(7) . . . . ?
N1 C2 N2 Pd1 -123.1(5) . . . . ?
C3 C2 N2 Pd1 57.8(6) . . . . ?
N1 C2 N2 Pd2 128.1(4) . . . 2_776 ?
C3 C2 N2 Pd2 -51.0(6) . . . 2_776 ?
N1 C2 N2 N2' 3.5(5) . . . . ?
C3 C2 N2 N2' -175.6(4) . . . . ?
N11 Pd1 N2 C2 20.3(5) . . . . ?
N12 Pd1 N2 C2 120.5(31) . . . . ?
N2' Pd1 N2 C2 -158.7(5) 2_776 . . . ?
Pd2 Pd1 N2 C2 -123.7(5) 2_776 . . . ?
N11 Pd1 N2 Pd2 144.0(2) . . . 2_776 ?
N12 Pd1 N2 Pd2 -115.8(31) . . . 2_776 ?
N2' Pd1 N2 Pd2 -34.9(2) 2_776 . . 2_776 ?
Pd2 Pd1 N2 Pd2 0.0 2_776 . . 2_776 ?
N11 Pd1 N2 N2' -108.0(2) . . . . ?
N12 Pd1 N2 N2' -7.8(32) . . . . ?
N2' Pd1 N2 N2' 73.0(2) 2_776 . . . ?
Pd2 Pd1 N2 N2' 108.0(2) 2_776 . . . ?
N1 C2 C3 C4 -0.7(8) . . . . ?
N2 C2 C3 C4 178.3(5) . . . . ?
C2 C3 C4 C5 0.1(9) . . . . ?
C3 C4 C5 C6 0.7(9) . . . . ?
C4 C5 C6 N1 -1.1(9) . . . . ?
C2 N1 C6 C5 0.5(8) . . . . ?
Pt1 N1 C6 C5 -176.4(4) . . . . ?
N1 Pt1 N1' C2' 171.6(12) . . . . ?
N7' Pt1 N1' C2' -97.8(5) . . . . ?
N7 Pt1 N1' C2' 84.3(5) . . . . ?
N1 Pt1 N1' C6' -6.2(16) . . . . ?
N7' Pt1 N1' C6' 84.5(4) . . . . ?
N7 Pt1 N1' C6' -93.5(4) . . . . ?
C6' N1' C2' C3' 0.3(8) . . . . ?
Pt1 N1' C2' C3' -177.4(4) . . . . ?
C6' N1' C2' N2' -179.1(5) . . . . ?
Pt1 N1' C2' N2' 3.2(7) . . . . ?
N1' C2' N2' Pd1 -129.1(5) . . . 2_776 ?
C3' C2' N2' Pd1 51.5(7) . . . 2_776 ?
N1' C2' N2' Pd2 124.5(5) . . . . ?
C3' C2' N2' Pd2 -55.0(6) . . . . ?
N1' C2' N2' N2 -1.8(6) . . . . ?
C3' C2' N2' N2 178.8(4) . . . . ?
N22 Pd2 N2' C2' 159.0(100) . . . . ?
N21 Pd2 N2' C2' -20.7(5) . . . . ?
N2 Pd2 N2' C2' 158.6(4) 2_776 . . . ?
Pd1 Pd2 N2' C2' 123.9(5) 2_776 . . . ?
N22 Pd2 N2' Pd1 35.0(103) . . . 2_776 ?
N21 Pd2 N2' Pd1 -144.6(2) . . . 2_776 ?
N2 Pd2 N2' Pd1 34.7(2) 2_776 . . 2_776 ?
Pd1 Pd2 N2' Pd1 0.000(1) 2_776 . . 2_776 ?
N22 Pd2 N2' N2 -74.9(102) . . . . ?
N21 Pd2 N2' N2 105.5(2) . . . . ?
N2 Pd2 N2' N2 -75.3(2) 2_776 . . . ?
Pd1 Pd2 N2' N2 -109.9(2) 2_776 . . . ?
C2 N2 N2' C2' -3.0(5) . . . . ?
Pd1 N2 N2' C2' 131.3(3) . . . . ?
Pd2 N2 N2' C2' -133.8(4) 2_776 . . . ?
C2 N2 N2' Pd1 130.3(3) . . . 2_776 ?
Pd1 N2 N2' Pd1 -95.4(2) . . . 2_776 ?
Pd2 N2 N2' Pd1 -0.5(3) 2_776 . . 2_776 ?
C2 N2 N2' Pd2 -133.7(3) . . . . ?
Pd1 N2 N2' Pd2 0.7(2) . . . . ?
Pd2 N2 N2' Pd2 95.5(2) 2_776 . . . ?
N1' C2' C3' C4' -0.4(9) . . . . ?
N2' C2' C3' C4' 179.0(6) . . . . ?
C2' C3' C4' C5' 0.4(9) . . . . ?
C3' C4' C5' C6' -0.3(10) . . . . ?
C4' C5' C6' N1' 0.1(10) . . . . ?
C2' N1' C6' C5' -0.2(9) . . . . ?
Pt1 N1' C6' C5' 177.8(5) . . . . ?
_refine_diff_density_max 0.617
_refine_diff_density_min -1.271
_refine_diff_density_rms 0.123
#===END