# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chris Adams' _publ_contact_author_email CHCJA@BRIS.AC.UK loop_ _publ_author_name C.Adams M.F.Haddow R.J.I.Hughes M.A.Kurawa A.Orpen data_8 _database_code_depnum_ccdc_archive 'CCDC 748472' #TrackingRef 'Revised_crystal_structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cl2 N4 Pd' _chemical_formula_weight 313.46 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' Cl Cl 0.1484 0.1585 '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' Pd Pd -0.9988 1.0072 '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 4.0628(5) _cell_length_b 7.2328(7) _cell_length_c 8.3661(8) _cell_angle_alpha 93.805(7) _cell_angle_beta 99.073(6) _cell_angle_gamma 91.601(7) _cell_volume 242.05(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3090 _cell_measurement_theta_min 2.4715 _cell_measurement_theta_max 27.598 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 152 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.405 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3731 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 27.62 _reflns_number_total 1116 _reflns_number_gt 1100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0351P)^2^+0.2033P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1116 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.0000 0.0000 0.01796(12) Uani 1 2 d S . . Cl1 Cl 0.5681(2) -0.26471(8) 0.13939(8) 0.02608(18) Uani 1 1 d . . . N1 N 0.8314(6) 0.1404(3) 0.1760(3) 0.0207(5) Uani 1 1 d . . . N2 N 0.8797(7) 0.3261(3) 0.1840(3) 0.0242(5) Uani 1 1 d . . . H1A H 0.7801 0.3981 0.1120 0.029 Uiso 1 1 calc R . . C1 C 1.0260(8) 0.0848(4) 0.3060(3) 0.0249(6) Uani 1 1 d . . . H2B H 1.0515 -0.0308 0.3305 0.030 Uiso 1 1 d R . . C2 C 1.1984(8) 0.2357(4) 0.3975(4) 0.0279(6) Uani 1 1 d . . . H3A H 1.3519 0.2339 0.4956 0.033 Uiso 1 1 calc R . . C3 C 1.0978(8) 0.3875(4) 0.3149(3) 0.0284(6) Uani 1 1 d . . . H2A H 1.1698 0.5128 0.3451 0.034 Uiso 1 1 calc R . . 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 Pd1 0.02703(19) 0.00954(15) 0.01850(17) 0.00427(10) 0.00561(12) 0.00272(11) Cl1 0.0430(4) 0.0112(3) 0.0235(3) 0.0067(2) 0.0015(3) 0.0002(3) N1 0.0289(13) 0.0119(9) 0.0234(11) 0.0041(8) 0.0092(10) 0.0017(9) N2 0.0376(15) 0.0117(10) 0.0231(11) 0.0040(8) 0.0035(10) -0.0022(9) C1 0.0336(17) 0.0178(12) 0.0239(13) 0.0059(10) 0.0046(12) 0.0015(11) C2 0.0322(17) 0.0250(14) 0.0255(14) 0.0020(11) 0.0022(12) -0.0023(12) C3 0.0375(18) 0.0203(13) 0.0274(14) 0.0009(11) 0.0070(13) -0.0058(12) _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 Pd1 N1 2.028(2) 2_655 ? Pd1 N1 2.028(2) . ? Pd1 Cl1 2.3079(6) . ? Pd1 Cl1 2.3079(6) 2_655 ? N1 C1 1.331(4) . ? N1 N2 1.348(3) . ? N2 C3 1.337(4) . ? N2 H1A 0.8800 . ? C1 C2 1.395(4) . ? C1 H2B 0.8793 . ? C2 C3 1.373(4) . ? C2 H3A 0.9500 . ? C3 H2A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.0 2_655 . ? N1 Pd1 Cl1 90.09(6) 2_655 . ? N1 Pd1 Cl1 89.92(6) . . ? N1 Pd1 Cl1 89.91(6) 2_655 2_655 ? N1 Pd1 Cl1 90.08(6) . 2_655 ? Cl1 Pd1 Cl1 180.00(4) . 2_655 ? C1 N1 N2 105.4(2) . . ? C1 N1 Pd1 131.87(19) . . ? N2 N1 Pd1 122.65(19) . . ? C3 N2 N1 111.6(2) . . ? C3 N2 H1A 124.2 . . ? N1 N2 H1A 124.2 . . ? N1 C1 C2 110.7(3) . . ? N1 C1 H2B 125.7 . . ? C2 C1 H2B 123.5 . . ? C3 C2 C1 104.9(3) . . ? C3 C2 H3A 127.5 . . ? C1 C2 H3A 127.5 . . ? N2 C3 C2 107.3(3) . . ? N2 C3 H2A 126.3 . . ? C2 C3 H2A 126.3 . . ? 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 Cl1 Pd1 N1 C1 6.4(3) . . . . ? Cl1 Pd1 N1 C1 -173.6(3) 2_655 . . . ? Cl1 Pd1 N1 N2 -169.7(2) . . . . ? Cl1 Pd1 N1 N2 10.3(2) 2_655 . . . ? C1 N1 N2 C3 -0.1(3) . . . . ? Pd1 N1 N2 C3 176.88(19) . . . . ? N2 N1 C1 C2 0.2(3) . . . . ? Pd1 N1 C1 C2 -176.4(2) . . . . ? N1 C1 C2 C3 -0.2(4) . . . . ? N1 N2 C3 C2 -0.1(3) . . . . ? C1 C2 C3 N2 0.2(3) . . . . ? 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 N2 H1A Cl1 0.88 2.46 3.012(3) 120.9 2_655 N2 H1A Cl1 0.88 2.62 3.272(3) 132.1 1_565 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.841 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.122 #===END data_beta-11 _database_code_depnum_ccdc_archive 'CCDC 748473' #TrackingRef 'Revised_crystal_structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cl2 N4 Pt' _chemical_formula_weight 402.14 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0643(15) _cell_length_b 13.1094(17) _cell_length_c 14.912(2) _cell_angle_alpha 94.583(8) _cell_angle_beta 98.669(7) _cell_angle_gamma 99.749(8) _cell_volume 2095.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4985 _cell_measurement_theta_min 3.323.32 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 13.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.871 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9564 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9564 _reflns_number_gt 6874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1826P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9564 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.2583 _refine_ls_wR_factor_gt 0.2256 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 Pt1 Pt 0.15225(6) 0.13444(5) 0.53578(4) 0.0204(2) Uani 1 1 d . . . Pt2 Pt 0.84379(6) 0.36878(5) -0.03819(4) 0.0192(2) Uani 1 1 d . . . Pt3 Pt 0.40426(6) 0.33698(5) 0.49856(4) 0.0195(2) Uani 1 1 d . . . Pt4 Pt 0.64460(6) 0.11914(5) -0.03875(4) 0.0174(2) Uani 1 1 d . . . Cl1 Cl 0.3067(4) 0.0368(4) 0.5611(3) 0.0252(9) Uani 1 1 d . . . Cl2 Cl 0.1031(5) 0.0609(4) 0.3865(3) 0.0321(11) Uani 1 1 d . . . Cl3 Cl 1.0207(4) 0.3093(4) 0.0187(3) 0.0269(10) Uani 1 1 d . . . Cl4 Cl 0.8610(4) 0.3095(3) -0.1847(3) 0.0219(8) Uani 1 1 d . . . Cl5 Cl 0.3478(4) 0.4542(4) 0.5999(3) 0.0279(10) Uani 1 1 d . . . Cl6 Cl 0.5403(4) 0.2840(4) 0.6111(3) 0.0248(9) Uani 1 1 d . . . Cl7 Cl 0.4955(4) 0.1995(4) 0.0139(3) 0.0236(9) Uani 1 1 d . . . Cl8 Cl 0.5661(4) 0.1390(3) -0.1869(3) 0.0216(8) Uani 1 1 d . . . N1 N 0.0208(14) 0.2197(12) 0.5142(10) 0.024(3) Uani 1 1 d . . . N2 N -0.1028(17) 0.1758(14) 0.4971(16) 0.051(6) Uani 1 1 d . . . H12A H -0.1320 0.1085 0.4920 0.062 Uiso 1 1 calc R . . N3 N 0.1838(14) 0.1919(12) 0.6696(10) 0.026(3) Uani 1 1 d . . . N4 N 0.3005(14) 0.2178(11) 0.7215(10) 0.023(3) Uani 1 1 d . . . H14A H 0.3709 0.2189 0.7006 0.028 Uiso 1 1 calc R . . N5 N 0.8241(14) 0.4174(10) 0.0890(9) 0.020(3) Uani 1 1 d . . . N6 N 0.9074(18) 0.4955(13) 0.1452(11) 0.039(4) Uani 1 1 d . . . H6A H 0.9737 0.5329 0.1301 0.046 Uiso 1 1 calc R . . N7 N 0.6990(15) 0.4302(12) -0.0846(10) 0.024(3) Uani 1 1 d . . . N8 N 0.6124(14) 0.3953(14) -0.1601(11) 0.033(4) Uani 1 1 d . . . H8A H 0.6078 0.3351 -0.1922 0.040 Uiso 1 1 calc R . . N9 N 0.4501(16) 0.2413(11) 0.4036(10) 0.027(4) Uani 1 1 d . . . N10 N 0.4402(15) 0.1390(13) 0.4036(11) 0.029(4) Uani 1 1 d . . . H16B H 0.4213 0.1048 0.4495 0.035 Uiso 1 1 calc R . . N11 N 0.2901(15) 0.3775(12) 0.3978(11) 0.028(4) Uani 1 1 d . . . N12 N 0.2908(18) 0.4755(14) 0.3792(12) 0.042(5) Uani 1 1 d . . . H10A H 0.3390 0.5298 0.4126 0.050 Uiso 1 1 calc R . . N13 N 0.7174(13) 0.0999(11) 0.0894(10) 0.020(3) Uani 1 1 d . . . N14 N 0.8210(15) 0.1503(14) 0.1414(12) 0.034(4) Uani 1 1 d . . . H4B H 0.8744 0.2000 0.1248 0.041 Uiso 1 1 calc R . . N15 N 0.7687(13) 0.0410(10) -0.0806(9) 0.016(3) Uani 1 1 d . . . C22 C 0.797(2) -0.0516(16) -0.0564(17) 0.044(6) Uani 1 1 d . . . H39A H 0.7617 -0.0918 -0.0135 0.053 Uiso 1 1 calc R . . C1 C -0.173(2) 0.249(2) 0.489(2) 0.063(8) Uani 1 1 d . . . H38A H -0.2609 0.2359 0.4770 0.076 Uiso 1 1 calc R . . C2 C -0.097(2) 0.347(2) 0.5014(17) 0.048(6) Uani 1 1 d . . . H37A H -0.1187 0.4137 0.4982 0.057 Uiso 1 1 calc R . . C3 C 0.0213(18) 0.3184(18) 0.5200(16) 0.039(5) Uani 1 1 d . . . H36A H 0.0960 0.3686 0.5357 0.047 Uiso 1 1 calc R . . C4 C 0.1022(18) 0.2027(14) 0.7229(13) 0.028(4) Uani 1 1 d . . . H4A H 0.0144 0.1917 0.7054 0.033 Uiso 1 1 calc R . . C5 C 0.1699(17) 0.2337(16) 0.8114(13) 0.029(4) Uani 1 1 d . . . H5A H 0.1363 0.2473 0.8651 0.035 Uiso 1 1 calc R . . C6 C 0.2907(17) 0.2404(14) 0.8056(12) 0.025(4) Uani 1 1 d . . . H3A H 0.3578 0.2588 0.8552 0.030 Uiso 1 1 calc R . . C7 C 0.7432(17) 0.3771(16) 0.1384(14) 0.032(5) Uani 1 1 d . . . H33A H 0.6787 0.3185 0.1184 0.038 Uiso 1 1 calc R . . C8 C 0.766(3) 0.4329(16) 0.2238(16) 0.049(7) Uani 1 1 d . . . H20A H 0.7183 0.4226 0.2712 0.058 Uiso 1 1 calc R . . C9 C 0.870(2) 0.5047(18) 0.2267(14) 0.041(6) Uani 1 1 d . . . H21A H 0.9099 0.5534 0.2776 0.049 Uiso 1 1 calc R . . C10 C 0.6730(18) 0.5249(16) -0.0587(14) 0.030(4) Uani 1 1 d . . . H22A H 0.7193 0.5713 -0.0083 0.036 Uiso 1 1 calc R . . C11 C 0.569(2) 0.5453(18) -0.1160(15) 0.046(6) Uani 1 1 d . . . H34A H 0.5310 0.6047 -0.1109 0.055 Uiso 1 1 calc R . . C12 C 0.5343(19) 0.4609(16) -0.1812(14) 0.035(5) Uani 1 1 d . . . H19A H 0.4680 0.4510 -0.2314 0.041 Uiso 1 1 calc R . . C13 C 0.208(2) 0.4825(18) 0.3023(15) 0.040(5) Uani 1 1 d . . . H35A H 0.1954 0.5434 0.2745 0.048 Uiso 1 1 calc R . . C14 C 0.146(2) 0.379(2) 0.2737(14) 0.050(7) Uani 1 1 d . . . H11A H 0.0822 0.3550 0.2227 0.060 Uiso 1 1 calc R . . C15 C 0.1982(19) 0.3199(17) 0.3346(15) 0.039(5) Uani 1 1 d . . . H10B H 0.1727 0.2468 0.3330 0.046 Uiso 1 1 calc R . . C16 C 0.480(2) 0.2592(18) 0.3228(15) 0.043(6) Uani 1 1 d . . . H30A H 0.4920 0.3257 0.3009 0.051 Uiso 1 1 calc R . . C17 C 0.491(2) 0.169(2) 0.2757(14) 0.046(6) Uani 1 1 d . . . H29A H 0.5150 0.1614 0.2174 0.055 Uiso 1 1 calc R . . C18 C 0.462(2) 0.0952(17) 0.3276(13) 0.040(5) Uani 1 1 d . . . H40A H 0.4571 0.0227 0.3123 0.048 Uiso 1 1 calc R . . C19 C 0.6628(17) 0.0311(15) 0.1369(13) 0.029(4) Uani 1 1 d . . . H16A H 0.5872 -0.0164 0.1149 0.034 Uiso 1 1 calc R . . C20 C 0.729(2) 0.0375(19) 0.2214(14) 0.041(5) Uani 1 1 d . . . H15A H 0.7090 -0.0025 0.2692 0.049 Uiso 1 1 calc R . . C21 C 0.8329(18) 0.1136(16) 0.2248(11) 0.028(4) Uani 1 1 d . . . H14B H 0.8988 0.1359 0.2747 0.033 Uiso 1 1 calc R . . N16 N 0.8450(16) 0.0714(11) -0.1402(9) 0.027(4) Uani 1 1 d . . . H2A H 0.8452 0.1292 -0.1663 0.033 Uiso 1 1 calc R . . C23 C 0.8888(18) -0.0768(16) -0.1062(15) 0.036(5) Uani 1 1 d . . . H25A H 0.9231 -0.1385 -0.1060 0.043 Uiso 1 1 calc R . . C24 C 0.918(2) 0.0059(17) -0.1550(15) 0.041(5) Uani 1 1 d . . . H24A H 0.9805 0.0139 -0.1926 0.050 Uiso 1 1 calc R . . 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 0.0218(4) 0.0213(4) 0.0165(3) 0.0004(3) 0.0011(3) 0.0020(3) Pt2 0.0176(4) 0.0200(4) 0.0193(3) 0.0015(3) 0.0019(3) 0.0033(3) Pt3 0.0222(4) 0.0205(4) 0.0148(3) -0.0014(2) 0.0027(3) 0.0029(3) Pt4 0.0179(3) 0.0185(4) 0.0151(3) 0.0001(2) 0.0022(2) 0.0030(3) Cl1 0.026(2) 0.028(2) 0.022(2) -0.0002(17) 0.0032(17) 0.0083(18) Cl2 0.037(3) 0.039(3) 0.018(2) -0.0021(18) -0.0023(18) 0.007(2) Cl3 0.020(2) 0.038(3) 0.024(2) 0.0072(18) 0.0042(17) 0.0089(19) Cl4 0.024(2) 0.020(2) 0.022(2) 0.0022(16) 0.0065(16) 0.0037(16) Cl5 0.034(2) 0.033(2) 0.0171(19) -0.0066(17) 0.0017(17) 0.012(2) Cl6 0.025(2) 0.030(2) 0.0185(19) -0.0008(17) -0.0002(16) 0.0073(18) Cl7 0.020(2) 0.032(2) 0.0190(19) -0.0014(17) 0.0025(16) 0.0083(18) Cl8 0.024(2) 0.022(2) 0.0173(19) -0.0024(15) -0.0014(16) 0.0053(16) N1 0.022(8) 0.022(8) 0.025(8) 0.004(6) 0.000(6) -0.002(6) N2 0.035(11) 0.017(9) 0.099(18) 0.010(10) 0.000(11) 0.004(8) N3 0.025(8) 0.029(8) 0.018(7) -0.003(6) -0.012(6) 0.008(7) N4 0.019(7) 0.018(7) 0.028(8) 0.000(6) -0.003(6) 0.001(6) N5 0.032(8) 0.012(7) 0.013(7) -0.004(5) -0.001(6) 0.000(6) N6 0.051(12) 0.030(9) 0.027(9) -0.005(7) 0.004(8) -0.009(8) N7 0.032(9) 0.020(8) 0.016(7) -0.004(6) 0.000(6) -0.003(6) N8 0.016(8) 0.046(10) 0.034(9) -0.016(8) -0.008(7) 0.016(7) N9 0.046(10) 0.011(7) 0.022(8) 0.003(6) 0.000(7) 0.005(7) N10 0.031(9) 0.032(9) 0.025(8) -0.006(7) 0.007(7) 0.010(7) N11 0.028(9) 0.022(8) 0.032(9) 0.008(7) -0.008(7) 0.013(7) N12 0.062(13) 0.034(10) 0.031(9) -0.012(8) -0.001(9) 0.028(9) N13 0.019(7) 0.017(7) 0.029(8) 0.016(6) 0.011(6) 0.007(6) N14 0.019(8) 0.047(11) 0.034(9) 0.007(8) -0.003(7) 0.011(7) N15 0.017(7) 0.010(6) 0.018(7) 0.005(5) -0.003(5) -0.003(5) C22 0.054(15) 0.021(11) 0.063(16) 0.019(10) 0.020(12) 0.010(10) C1 0.027(12) 0.067(18) 0.10(2) 0.004(16) -0.012(13) 0.038(13) C2 0.035(13) 0.051(15) 0.063(17) 0.015(12) 0.002(11) 0.026(11) C3 0.018(10) 0.044(13) 0.054(14) -0.005(10) 0.016(9) 0.002(9) C4 0.026(10) 0.030(10) 0.032(10) -0.003(8) 0.020(8) 0.009(8) C5 0.023(10) 0.039(12) 0.029(10) 0.011(8) 0.014(8) 0.003(8) C6 0.025(9) 0.030(10) 0.023(9) -0.004(7) 0.005(7) 0.013(8) C7 0.017(9) 0.037(12) 0.041(12) -0.006(9) 0.015(8) -0.002(8) C8 0.082(19) 0.020(10) 0.053(14) -0.001(10) 0.053(14) 0.003(11) C9 0.055(14) 0.050(14) 0.021(10) -0.001(9) -0.008(9) 0.029(11) C10 0.024(10) 0.033(11) 0.032(10) 0.012(8) 0.000(8) 0.003(8) C11 0.054(15) 0.048(14) 0.034(12) -0.008(10) -0.013(10) 0.027(12) C12 0.033(11) 0.036(11) 0.031(10) -0.007(9) -0.010(8) 0.015(9) C13 0.050(14) 0.042(13) 0.038(12) 0.019(10) 0.011(10) 0.025(11) C14 0.042(14) 0.09(2) 0.021(10) 0.007(11) -0.018(10) 0.024(13) C15 0.031(11) 0.031(11) 0.042(12) 0.009(9) -0.012(9) -0.016(9) C16 0.059(15) 0.042(13) 0.041(12) 0.011(10) 0.045(12) 0.016(11) C17 0.056(15) 0.068(17) 0.018(10) -0.002(10) 0.006(9) 0.027(13) C18 0.057(14) 0.036(12) 0.028(10) -0.012(9) -0.004(10) 0.030(11) C19 0.019(9) 0.032(11) 0.028(10) -0.002(8) -0.001(7) -0.010(8) C20 0.040(13) 0.055(15) 0.031(11) 0.018(10) 0.004(10) 0.013(11) C21 0.028(10) 0.048(13) 0.011(8) 0.010(8) 0.003(7) 0.017(9) N16 0.063(11) 0.016(7) 0.012(7) 0.012(6) 0.016(7) 0.020(7) C23 0.027(11) 0.032(11) 0.053(13) 0.013(10) 0.013(9) 0.008(9) C24 0.057(15) 0.034(12) 0.042(12) 0.012(10) 0.030(11) 0.010(10) _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 1.984(16) . ? Pt1 N3 2.032(15) . ? Pt1 Cl2 2.301(4) . ? Pt1 Cl1 2.308(4) 1 ? Pt1 Cl1 2.308(4) . ? Pt2 N7 1.971(16) . ? Pt2 N5 2.007(14) . ? Pt2 Cl3 2.298(4) 1 ? Pt2 Cl3 2.298(4) . ? Pt2 Cl4 2.306(4) 1 ? Pt2 Cl4 2.306(4) . ? Pt3 N11 1.979(14) . ? Pt3 N9 1.996(16) . ? Pt3 Cl5 2.296(4) . ? Pt3 Cl6 2.311(4) 1 ? Pt3 Cl6 2.311(4) . ? Pt4 N15 1.989(15) . ? Pt4 N13 2.012(14) . ? Pt4 Cl8 2.300(4) 1 ? Pt4 Cl8 2.300(4) . ? Pt4 Cl7 2.301(4) . ? N1 C3 1.29(3) . ? N1 N2 1.37(2) . ? N2 C1 1.33(3) . ? N3 C4 1.31(2) . ? N3 N4 1.375(19) . ? N4 C6 1.29(2) . ? N5 C7 1.31(2) . ? N5 N6 1.38(2) . ? N6 C9 1.35(3) . ? N7 N8 1.36(2) . ? N7 C10 1.36(3) . ? N8 C12 1.34(2) . ? N9 C16 1.33(2) . ? N9 N10 1.33(2) . ? N10 C18 1.30(2) . ? N11 N12 1.34(2) . ? N11 C15 1.35(2) . ? N12 C13 1.37(3) . ? N13 C19 1.31(2) . ? N13 N14 1.32(2) . ? N14 C21 1.36(2) . ? N15 N16 1.35(2) . ? N15 C22 1.37(2) . ? C22 C23 1.41(3) . ? C1 C2 1.39(3) . ? C2 C3 1.41(3) . ? C4 C5 1.41(3) . ? C5 C6 1.34(2) . ? C7 C8 1.38(3) . ? C8 C9 1.35(3) . ? C10 C11 1.40(3) . ? C11 C12 1.37(3) . ? C13 C14 1.42(3) . ? C14 C15 1.36(3) . ? C16 C17 1.36(3) . ? C17 C18 1.32(3) . ? C19 C20 1.35(3) . ? C20 C21 1.38(3) . ? N16 C24 1.30(3) . ? C23 C24 1.38(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 N3 88.5(6) . . ? N1 Pt1 Cl2 90.6(5) . . ? N3 Pt1 Cl2 175.5(5) . . ? N1 Pt1 Cl1 179.4(4) . 1 ? N3 Pt1 Cl1 91.3(4) . 1 ? Cl2 Pt1 Cl1 89.67(16) . 1 ? N1 Pt1 Cl1 179.4(4) . . ? N3 Pt1 Cl1 91.3(4) . . ? Cl2 Pt1 Cl1 89.67(16) . . ? N7 Pt2 N5 88.6(6) . . ? N7 Pt2 Cl3 175.8(4) . 1 ? N5 Pt2 Cl3 90.1(4) . 1 ? N7 Pt2 Cl3 175.8(4) . . ? N5 Pt2 Cl3 90.1(4) . . ? N7 Pt2 Cl4 90.8(4) . 1 ? N5 Pt2 Cl4 178.3(4) . 1 ? Cl3 Pt2 Cl4 90.58(15) 1 1 ? Cl3 Pt2 Cl4 90.58(15) . 1 ? N7 Pt2 Cl4 90.8(4) . . ? N5 Pt2 Cl4 178.3(4) . . ? Cl3 Pt2 Cl4 90.58(15) 1 . ? Cl3 Pt2 Cl4 90.58(15) . . ? N11 Pt3 N9 86.2(6) . . ? N11 Pt3 Cl5 90.2(5) . . ? N9 Pt3 Cl5 176.0(4) . . ? N11 Pt3 Cl6 177.2(5) . 1 ? N9 Pt3 Cl6 91.0(4) . 1 ? Cl5 Pt3 Cl6 92.63(15) . 1 ? N11 Pt3 Cl6 177.2(5) . . ? N9 Pt3 Cl6 91.0(4) . . ? Cl5 Pt3 Cl6 92.63(15) . . ? N15 Pt4 N13 87.2(6) . . ? N15 Pt4 Cl8 91.1(4) . 1 ? N13 Pt4 Cl8 178.3(4) . 1 ? N15 Pt4 Cl8 91.1(4) . . ? N13 Pt4 Cl8 178.3(4) . . ? N15 Pt4 Cl7 176.1(4) . . ? N13 Pt4 Cl7 90.9(4) . . ? Cl8 Pt4 Cl7 90.83(15) 1 . ? Cl8 Pt4 Cl7 90.83(15) . . ? C3 N1 N2 104.0(16) . . ? C3 N1 Pt1 133.8(14) . . ? N2 N1 Pt1 121.8(12) . . ? C1 N2 N1 110.7(19) . . ? C4 N3 N4 108.2(15) . . ? C4 N3 Pt1 128.3(13) . . ? N4 N3 Pt1 123.4(12) . . ? C6 N4 N3 109.4(15) . . ? C7 N5 N6 106.8(15) . . ? C7 N5 Pt2 128.9(12) . . ? N6 N5 Pt2 123.9(12) . . ? C9 N6 N5 108.5(18) . . ? N8 N7 C10 103.0(15) . . ? N8 N7 Pt2 127.5(12) . . ? C10 N7 Pt2 128.7(13) . . ? C12 N8 N7 113.9(16) . . ? C16 N9 N10 103.8(16) . . ? C16 N9 Pt3 129.9(13) . . ? N10 N9 Pt3 125.7(12) . . ? C18 N10 N9 112.0(17) . . ? N12 N11 C15 104.6(15) . . ? N12 N11 Pt3 124.0(13) . . ? C15 N11 Pt3 131.4(13) . . ? N11 N12 C13 112.8(18) . . ? C19 N13 N14 107.8(15) . . ? C19 N13 Pt4 122.8(12) . . ? N14 N13 Pt4 129.4(12) . . ? N13 N14 C21 109.7(17) . . ? N16 N15 C22 105.2(15) . . ? N16 N15 Pt4 125.7(10) . . ? C22 N15 Pt4 129.1(14) . . ? N15 C22 C23 108.1(18) . . ? N2 C1 C2 110(2) . . ? C1 C2 C3 100.0(19) . . ? N1 C3 C2 115(2) . . ? N3 C4 C5 106.5(17) . . ? C6 C5 C4 107.3(17) . . ? N4 C6 C5 108.6(17) . . ? N5 C7 C8 109.7(17) . . ? C9 C8 C7 106.6(18) . . ? N6 C9 C8 108.1(19) . . ? N7 C10 C11 111.3(18) . . ? C12 C11 C10 105.3(19) . . ? N8 C12 C11 106.5(17) . . ? N12 C13 C14 104.6(18) . . ? C15 C14 C13 105.5(18) . . ? N11 C15 C14 112.4(19) . . ? N9 C16 C17 110(2) . . ? C18 C17 C16 105.8(19) . . ? N10 C18 C17 107.8(19) . . ? N13 C19 C20 110.3(17) . . ? C19 C20 C21 106.5(18) . . ? N14 C21 C20 105.7(17) . . ? C24 N16 N15 113.0(15) . . ? C24 C23 C22 106.0(19) . . ? N16 C24 C23 107.5(19) . . ? 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 N2 H12A Cl1 0.88 2.46 3.241(18) 148.5 2_556 N4 H14A Cl6 0.88 2.53 3.356(16) 156.1 1 N4 H14A Cl8 0.88 2.92 3.408(15) 116.7 1_556 N8 H8A Cl8 0.88 2.54 3.294(18) 143.7 1 N8 H8A Cl6 0.88 2.91 3.521(16) 128.1 1_554 N10 H16B Cl1 0.88 2.38 3.220(17) 160.0 1 N12 H10A Cl6 0.88 2.65 3.36(2) 138.3 2_666 N14 H4B Cl3 0.88 2.74 3.584(19) 160.2 1 N16 H2A Cl4 0.88 2.38 3.225(14) 160.7 1 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 5.284 _refine_diff_density_min -5.461 _refine_diff_density_rms 0.722 #===END data_[H2Pz]2[PtCl6].2H2O _database_code_depnum_ccdc_archive 'CCDC 748474' #TrackingRef 'Revised_crystal_structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H12 Cl6 N4 O2 Pt' _chemical_formula_weight 579.98 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' 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' O O 0.0106 0.0060 '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 6.8406(2) _cell_length_b 11.1912(4) _cell_length_c 11.2366(4) _cell_angle_alpha 84.322(2) _cell_angle_beta 76.887(2) _cell_angle_gamma 75.824(2) _cell_volume 811.41(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5011 _cell_measurement_theta_min 3.1445 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 9.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.035 _exptl_absorpt_correction_T_max 0.146 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5527 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 33.69 _reflns_number_total 5527 _reflns_number_gt 4709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0165P)^2^+5.7889P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5527 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_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 Pt1 Pt 0.0000 0.0000 1.0000 0.01131(6) Uani 1 2 d S . . Pt2 Pt 0.0000 0.5000 0.5000 0.01170(6) Uani 1 2 d S . . Cl1 Cl 0.1245(2) -0.14638(11) 0.85173(11) 0.0157(2) Uani 1 1 d . . . Cl2 Cl 0.2359(2) 0.11285(12) 0.89788(12) 0.0159(2) Uani 1 1 d . . . Cl3 Cl 0.2345(2) -0.11137(12) 1.11387(12) 0.0159(2) Uani 1 1 d . . . Cl4 Cl 0.3372(2) 0.41732(13) 0.40186(12) 0.0179(3) Uani 1 1 d . . . Cl5 Cl 0.0148(2) 0.33601(11) 0.64394(11) 0.0154(2) Uani 1 1 d . . . Cl6 Cl 0.1143(2) 0.60932(13) 0.62516(13) 0.0175(3) Uani 1 1 d . . . C1 C 0.2264(10) 1.0905(6) 0.4571(6) 0.0194(12) Uani 1 1 d . . . H1B H 0.1928 1.1779 0.4467 0.023 Uiso 1 1 calc R . . C2 C 0.2116(10) 1.0236(6) 0.5672(6) 0.0205(13) Uani 1 1 d . . . H2B H 0.1656 1.0552 0.6467 0.025 Uiso 1 1 calc R . . C3 C 0.2777(10) 0.9012(5) 0.5380(6) 0.0196(12) Uani 1 1 d . . . H3B H 0.2873 0.8327 0.5953 0.024 Uiso 1 1 calc R . . C4 C 0.3286(11) 0.4083(5) 0.9519(6) 0.0194(12) Uani 1 1 d . . . H4A H 0.3951 0.3484 0.8926 0.023 Uiso 1 1 calc R . . C5 C 0.2700(10) 0.5334(6) 0.9287(6) 0.0192(12) Uani 1 1 d . . . H5A H 0.2870 0.5759 0.8510 0.023 Uiso 1 1 calc R . . C6 C 0.1818(11) 0.5851(5) 1.0404(6) 0.0202(12) Uani 1 1 d . . . H6A H 0.1270 0.6704 1.0538 0.024 Uiso 1 1 calc R . . N1 N 0.3262(8) 0.8942(5) 0.4161(5) 0.0185(10) Uani 1 1 d . . . H1A H 0.3695 0.8260 0.3755 0.022 Uiso 1 1 calc R . . N2 N 0.2968(9) 1.0102(5) 0.3667(5) 0.0199(11) Uani 1 1 d . . . H2A H 0.3200 1.0304 0.2879 0.024 Uiso 1 1 calc R . . N3 N 0.1874(9) 0.4932(5) 1.1265(5) 0.0190(10) Uani 1 1 d . . . H3A H 0.1408 0.5020 1.2056 0.023 Uiso 1 1 calc R . . N4 N 0.2753(9) 0.3857(5) 1.0730(5) 0.0194(11) Uani 1 1 d . . . H4B H 0.2948 0.3124 1.1110 0.023 Uiso 1 1 calc R . . O1 O 0.5091(8) 0.6747(4) 0.3184(4) 0.0205(8) Uani 1 1 d . . . O2 O 0.3931(8) 0.1465(4) 1.1486(4) 0.0173(8) Uani 1 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 0.01431(14) 0.00912(11) 0.01025(11) 0.00015(8) -0.00206(11) -0.00293(11) Pt2 0.01456(14) 0.00972(11) 0.00998(11) 0.00021(8) -0.00149(11) -0.00246(11) Cl1 0.0211(7) 0.0120(5) 0.0130(5) -0.0015(4) -0.0022(5) -0.0026(5) Cl2 0.0177(6) 0.0132(5) 0.0165(5) 0.0004(4) -0.0006(5) -0.0060(5) Cl3 0.0189(6) 0.0138(5) 0.0153(5) 0.0009(4) -0.0068(5) -0.0020(5) Cl4 0.0165(6) 0.0168(6) 0.0166(6) 0.0009(4) -0.0001(5) -0.0007(5) Cl5 0.0220(7) 0.0110(5) 0.0115(5) 0.0014(4) -0.0018(5) -0.0033(5) Cl6 0.0237(7) 0.0146(6) 0.0163(6) -0.0010(4) -0.0066(5) -0.0062(5) C1 0.024(3) 0.015(2) 0.019(3) -0.001(2) -0.003(2) -0.005(2) C2 0.028(3) 0.020(3) 0.013(2) -0.003(2) -0.001(2) -0.007(2) C3 0.026(3) 0.015(2) 0.016(3) 0.002(2) -0.002(2) -0.004(2) C4 0.025(3) 0.016(2) 0.017(3) -0.0037(19) -0.003(2) -0.005(2) C5 0.026(3) 0.017(2) 0.017(3) 0.004(2) -0.008(2) -0.008(2) C6 0.026(3) 0.013(2) 0.020(3) 0.003(2) -0.004(2) -0.003(2) N1 0.022(3) 0.014(2) 0.019(2) -0.0023(17) -0.0031(18) -0.0020(17) N2 0.026(3) 0.025(3) 0.009(2) 0.0000(18) -0.0039(17) -0.006(2) N3 0.024(3) 0.016(2) 0.014(2) -0.0010(17) 0.0008(18) -0.0015(18) N4 0.029(3) 0.013(2) 0.016(2) 0.0025(17) -0.0046(19) -0.0047(18) O1 0.027(2) 0.0162(18) 0.0163(18) 0.0009(14) -0.0016(19) -0.0041(19) O2 0.023(2) 0.0154(17) 0.0136(17) -0.0008(13) -0.0062(18) -0.0026(18) _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 Cl2 2.3210(14) . ? Pt1 Cl2 2.3210(14) 2_557 ? Pt1 Cl1 2.3232(12) 2_557 ? Pt1 Cl1 2.3233(12) . ? Pt1 Cl3 2.3241(14) 2_557 ? Pt1 Cl3 2.3241(14) . ? Pt2 Cl5 2.3217(12) . ? Pt2 Cl5 2.3217(12) 2_566 ? Pt2 Cl6 2.3224(14) 2_566 ? Pt2 Cl6 2.3224(14) . ? Pt2 Cl4 2.3227(14) . ? Pt2 Cl4 2.3227(14) 2_566 ? C1 N2 1.349(8) . ? C1 C2 1.377(9) . ? C1 H1B 0.9500 . ? C2 C3 1.381(8) . ? C2 H2B 0.9500 . ? C3 N1 1.340(8) . ? C3 H3B 0.9500 . ? C4 N4 1.342(8) . ? C4 C5 1.374(8) . ? C4 H4A 0.9500 . ? C5 C6 1.379(9) . ? C5 H5A 0.9500 . ? C6 N3 1.340(8) . ? C6 H6A 0.9500 . ? N1 N2 1.347(7) . ? N1 H1A 0.8800 . ? N2 H2A 0.8800 . ? N3 N4 1.340(7) . ? N3 H3A 0.8800 . ? N4 H4B 0.8800 . ? 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 Cl2 Pt1 Cl2 179.999(1) . 2_557 ? Cl2 Pt1 Cl1 89.78(5) . 2_557 ? Cl2 Pt1 Cl1 90.22(5) 2_557 2_557 ? Cl2 Pt1 Cl1 90.22(5) . . ? Cl2 Pt1 Cl1 89.78(5) 2_557 . ? Cl1 Pt1 Cl1 180.0 2_557 . ? Cl2 Pt1 Cl3 88.97(5) . 2_557 ? Cl2 Pt1 Cl3 91.03(5) 2_557 2_557 ? Cl1 Pt1 Cl3 89.88(5) 2_557 2_557 ? Cl1 Pt1 Cl3 90.12(5) . 2_557 ? Cl2 Pt1 Cl3 91.03(5) . . ? Cl2 Pt1 Cl3 88.97(5) 2_557 . ? Cl1 Pt1 Cl3 90.12(5) 2_557 . ? Cl1 Pt1 Cl3 89.88(5) . . ? Cl3 Pt1 Cl3 180.00(6) 2_557 . ? Cl5 Pt2 Cl5 180.0 . 2_566 ? Cl5 Pt2 Cl6 90.50(5) . 2_566 ? Cl5 Pt2 Cl6 89.50(5) 2_566 2_566 ? Cl5 Pt2 Cl6 89.50(5) . . ? Cl5 Pt2 Cl6 90.50(5) 2_566 . ? Cl6 Pt2 Cl6 180.0 2_566 . ? Cl5 Pt2 Cl4 90.41(5) . . ? Cl5 Pt2 Cl4 89.59(5) 2_566 . ? Cl6 Pt2 Cl4 89.07(6) 2_566 . ? Cl6 Pt2 Cl4 90.93(6) . . ? Cl5 Pt2 Cl4 89.59(5) . 2_566 ? Cl5 Pt2 Cl4 90.41(5) 2_566 2_566 ? Cl6 Pt2 Cl4 90.93(6) 2_566 2_566 ? Cl6 Pt2 Cl4 89.07(6) . 2_566 ? Cl4 Pt2 Cl4 180.0 . 2_566 ? N2 C1 C2 108.0(5) . . ? N2 C1 H1B 126.0 . . ? C2 C1 H1B 126.0 . . ? C1 C2 C3 105.8(5) . . ? C1 C2 H2B 127.1 . . ? C3 C2 H2B 127.1 . . ? N1 C3 C2 109.2(5) . . ? N1 C3 H3B 125.4 . . ? C2 C3 H3B 125.4 . . ? N4 C4 C5 108.0(5) . . ? N4 C4 H4A 126.0 . . ? C5 C4 H4A 126.0 . . ? C4 C5 C6 106.6(5) . . ? C4 C5 H5A 126.7 . . ? C6 C5 H5A 126.7 . . ? N3 C6 C5 107.6(5) . . ? N3 C6 H6A 126.2 . . ? C5 C6 H6A 126.2 . . ? C3 N1 N2 107.8(5) . . ? C3 N1 H1A 126.1 . . ? N2 N1 H1A 126.1 . . ? N1 N2 C1 109.2(5) . . ? N1 N2 H2A 125.4 . . ? C1 N2 H2A 125.4 . . ? N4 N3 C6 109.1(5) . . ? N4 N3 H3A 125.4 . . ? C6 N3 H3A 125.4 . . ? N3 N4 C4 108.6(5) . . ? N3 N4 H4B 125.7 . . ? C4 N4 H4B 125.7 . . ? 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 N2 C1 C2 C3 0.5(8) . . . . ? C1 C2 C3 N1 -1.2(8) . . . . ? N4 C4 C5 C6 0.7(8) . . . . ? C4 C5 C6 N3 -0.3(8) . . . . ? C2 C3 N1 N2 1.4(7) . . . . ? C3 N1 N2 C1 -1.1(7) . . . . ? C2 C1 N2 N1 0.3(7) . . . . ? C5 C6 N3 N4 -0.2(8) . . . . ? C6 N3 N4 C4 0.6(7) . . . . ? C5 C4 N4 N3 -0.8(7) . . . . ? 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 N1 H1A O1 0.88 1.83 2.684(6) 164.5 1 N2 H2A O2 0.88 1.99 2.790(7) 151.1 1_564 N2 H2A Cl3 0.88 2.88 3.420(5) 121.7 1_564 N3 H3A Cl5 0.88 2.47 3.206(5) 141.0 2_567 N3 H3A Cl6 0.88 2.70 3.358(5) 132.2 2_567 N3 H3A Cl4 0.88 2.81 3.440(6) 130.2 1_556 N4 H4B O2 0.88 1.86 2.709(6) 163.0 1 _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.082 _refine_diff_density_min -1.985 _refine_diff_density_rms 0.242 # Attachment 'powder_solutions.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 748475' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '2(C3 H5 N2), Cl4 Pt' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum ' C6 H10 Cl4 N4 Pt ' _chemical_formula_weight 475.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source pt 27.00590 1.51293 17.76390 8.81174 15.71310 0.42459 5.78370 38.61030 11.68830 -5.23300 6.92500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 cl 11.46040 0.01040 7.19640 1.16620 6.25560 18.51940 1.64550 47.77840 -9.55740 0.34800 0.70200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x,-y,-z _cell_length_a 7.0225(3) _cell_length_b 7.6375(3) _cell_length_c 6.7148(3) _cell_angle_alpha 110.2813(19) _cell_angle_beta 96.859(2) _cell_angle_gamma 64.110(2) _cell_volume 303.69(2) _cell_formula_units_Z 1 _cell_measurement_temperature ? _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 1746 _pd_meas_2theta_range_min 5.10000 _pd_meas_2theta_range_max 40.00000 _pd_meas_2theta_range_inc 0.020011 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 8.6344 _pd_proc_ls_prof_wR_factor 10.8631 _pd_proc_ls_prof_wR_expected 6.8111 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 16.3119 _pd_proc_ls_prof_cwR_factor 17.2363 _pd_proc_ls_prof_cwR_expected 10.8070 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 2.5438 _pd_proc_ls_prof_echi2 2.7446 # Items related to LS refinement _refine_ls_R_I_factor 6.8426 _refine_ls_number_reflns 126 _refine_ls_number_parameters 24 _refine_ls_number_restraints 0 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5.1885 _pd_proc_2theta_range_max 40.0885 _pd_proc_2theta_range_inc 0.020011 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Pt1 0.00000 0.00000 1.00000 0.01900 1.00000 Uiso Pt Cl1 0.175(2) 0.0577(18) 0.785(2) 0.02533 1.00000 Uiso Cl Cl2 0.322(3) -0.151(2) 1.132(2) 0.02533 1.00000 Uiso Cl N1 0.29640 -0.70420 1.27970 0.03800 1.00000 Uiso N N2 0.22620 -0.39850 1.44540 0.03800 1.00000 Uiso N C1 0.25040 -0.52650 1.26340 0.03800 1.00000 Uiso C C2 0.25780 -0.48910 1.58940 0.03800 1.00000 Uiso C C3 0.30400 -0.68600 1.48250 0.03800 1.00000 Uiso C H1 0.32330 -0.84280 1.15160 0.06333 1.00000 Uiso H H2 0.18490 -0.23830 1.47890 0.06333 1.00000 Uiso H H3 0.23710 -0.49640 1.11870 0.06333 1.00000 Uiso H H4 0.25070 -0.41840 1.75640 0.06333 1.00000 Uiso H H5 0.33790 -0.80420 1.54760 0.06333 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 748476' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '2(C3 H5 N2), Pt Cl4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C6 H10 Cl4 N4 Pt' _chemical_formula_weight ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source pt 27.00590 1.51293 17.76390 8.81174 15.71310 0.42459 5.78370 38.61030 11.68830 -5.23300 6.92500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 cl 11.46040 0.01040 7.19640 1.16620 6.25560 18.51940 1.64550 47.77840 -9.55740 0.34800 0.70200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x,-y,-z _cell_length_a 8.5229(2) _cell_length_b 7.0222(3) _cell_length_c 7.3333(3) _cell_angle_alpha 66.635(3) _cell_angle_beta 127.557(3) _cell_angle_gamma 105.595(3) _cell_volume 319.18(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source ? # Put here: 'rotating-anode X-ray tube' or similar _diffrn_radiation_type 'Cu K\a' _diffrn_source_target ? # Put here the chemical symbol of the anode _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 1775 _pd_meas_2theta_range_min 5.09800 _pd_meas_2theta_range_max 40.01000 _pd_meas_2theta_range_inc 0.019691 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 19.6585 _pd_proc_ls_prof_wR_factor 24.0424 _pd_proc_ls_prof_wR_expected 7.5956 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 33.8945 _pd_proc_ls_prof_cwR_factor 34.4380 _pd_proc_ls_prof_cwR_expected 10.8798 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 10.0192 _pd_proc_ls_prof_echi2 10.2303 # Items related to LS refinement _refine_ls_R_I_factor 19.0857 _refine_ls_number_reflns 130 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5.0980 _pd_proc_2theta_range_max 40.0100 _pd_proc_2theta_range_inc 0.019691 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Pt1 0.50000 0.50000 0.50000 0.00024 1.00000 Uiso Pt Cl1 0.704(4) 0.663(5) 0.769(5) 0.00032 1.00000 Uiso Cl Cl2 0.421(4) 0.831(5) 0.221(5) 0.00032 1.00000 Uiso Cl C4 -0.24335 0.19971 -0.55409 0.00048 1.00000 Uiso C H4A -0.37754 0.17487 -0.60852 0.00080 1.00000 Uiso H C5 -0.09586 0.22819 -0.34067 0.00048 1.00000 Uiso C H5A -0.10831 0.22541 -0.22027 0.00080 1.00000 Uiso H C6 0.07389 0.26165 -0.33599 0.00048 1.00000 Uiso C H6A 0.20034 0.28677 -0.21107 0.00080 1.00000 Uiso H N3 0.02766 0.25217 -0.53967 0.00048 1.00000 Uiso N H3A 0.11035 0.26875 -0.58040 0.00080 1.00000 Uiso H N4 -0.16454 0.21330 -0.67179 0.00048 1.00000 Uiso N H4B -0.22849 0.19913 -0.81257 0.00080 1.00000 Uiso H #===END