# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' #TrackingRef '- PV_revise.cif' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sakai, Ken' _publ_contact_author_email ksakai@chem.kyushu-univ.jp _publ_section_title ; Synthesis, crystal structure, spectroscopic and electrochemical properties, and H2-evolving activity of a new [PtCl(terpyridine)]+ derivative with viologen-like redox properties ; loop_ _publ_author_name M.Kobayashi S.Masaoka K.Sakai # Attachment 'Mepytpy.cif' #===================================================================== data_10722Mepytpy _database_code_depnum_ccdc_archive 'CCDC 854080' #TrackingRef 'web_deposit_cif_file_0_MasayukiKobayashi_1321413732.Mepytpy.cif' #===================================================================== # 5. Chemical Data _chemical_name_systematic ; NONE ; _chemical_name_common ? _chemical_formula_iupac ? _chemical_formula_moiety 'C21 H17 N4, Cl O4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H17 Cl N4 O4' _chemical_formula_weight 424.84 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' #========================================================================== # 6. 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 'x, y, z' '-x, -y, -z' _cell_length_a 7.6458(19) _cell_length_b 8.934(2) _cell_length_c 14.264(4) _cell_angle_alpha 76.092(3) _cell_angle_beta 78.249(3) _cell_angle_gamma 83.803(3) _cell_volume 924.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 4173 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.32 _cell_special_details ; ? # Insert any comments here. ; _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.246 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _exptl_absorpt_correction_T_min 0.6717 _exptl_absorpt_correction_T_max 0.7452 #========================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART APEX CCD-detector diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8932 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.36 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _reflns_number_total 3343 _reflns_number_gt 2951 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'KENX (Sakai, 2002)' _computing_publication_material ; SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976) ; #========================================================================= # 8. Refinement Data _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^)+(0.0176P)^2^+4.1697P] 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_extinction_expression not_refined _refine_ls_number_reflns 3343 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1743 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.313 _refine_ls_restrained_S_all 1.313 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.868 _refine_diff_density_min -0.332 #========================================================================= # 9. Atomic Coordinates and Displacement Parameters 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 Cl1 Cl 0.76404(14) 0.21816(12) 0.49292(7) 0.0172(3) Uani 1 1 d . . . O1 O 0.8093(5) 0.2466(6) 0.5786(3) 0.0501(12) Uani 1 1 d . . . O2 O 0.9253(5) 0.1707(4) 0.4308(3) 0.0305(8) Uani 1 1 d . . . O3 O 0.6830(5) 0.3569(4) 0.4399(3) 0.0381(9) Uani 1 1 d . . . O4 O 0.6394(5) 0.0980(4) 0.5175(3) 0.0418(10) Uani 1 1 d . . . N1 N 0.5654(5) -0.3119(4) -0.0845(3) 0.0196(8) Uani 1 1 d . . . N2 N 0.7437(5) 0.0589(4) -0.1218(3) 0.0164(7) Uani 1 1 d . . . N3 N 0.9230(5) 0.3828(4) -0.0746(3) 0.0208(8) Uani 1 1 d . . . N4 N 0.7463(5) -0.2260(4) 0.3830(3) 0.0189(8) Uani 1 1 d . . . C1 C 0.4907(6) -0.3904(5) -0.1324(3) 0.0243(10) Uani 1 1 d . . . H1 H 0.4487 -0.4863 -0.0989 0.029 Uiso 1 1 calc R . . C2 C 0.4717(6) -0.3371(5) -0.2300(3) 0.0235(10) Uani 1 1 d . . . H2 H 0.4142 -0.3940 -0.2600 0.028 Uiso 1 1 calc R . . C3 C 0.5401(6) -0.1982(5) -0.2810(3) 0.0225(10) Uani 1 1 d . . . H3 H 0.5308 -0.1603 -0.3467 0.027 Uiso 1 1 calc R . . C4 C 0.6225(6) -0.1155(5) -0.2338(3) 0.0190(9) Uani 1 1 d . . . H4 H 0.6729 -0.0230 -0.2675 0.023 Uiso 1 1 calc R . . C5 C 0.6286(6) -0.1741(5) -0.1344(3) 0.0178(9) Uani 1 1 d . . . C6 C 0.6948(5) -0.0838(5) -0.0755(3) 0.0168(9) Uani 1 1 d . . . C7 C 0.6986(6) -0.1445(5) 0.0237(3) 0.0185(9) Uani 1 1 d . . . H7 H 0.6692 -0.2457 0.0529 0.022 Uiso 1 1 calc R . . C8 C 0.7470(5) -0.0511(5) 0.0785(3) 0.0172(9) Uani 1 1 d . . . C9 C 0.7961(5) 0.0973(5) 0.0309(3) 0.0168(9) Uani 1 1 d . . . H9 H 0.8288 0.1625 0.0655 0.020 Uiso 1 1 calc R . . C10 C 0.7958(5) 0.1469(5) -0.0696(3) 0.0170(9) Uani 1 1 d . . . C11 C 0.8563(6) 0.3005(5) -0.1249(3) 0.0171(9) Uani 1 1 d . . . C12 C 0.8510(6) 0.3530(5) -0.2245(3) 0.0192(9) Uani 1 1 d . . . H12 H 0.8023 0.2944 -0.2575 0.023 Uiso 1 1 calc R . . C13 C 0.9190(6) 0.4931(5) -0.2734(3) 0.0222(10) Uani 1 1 d . . . H13 H 0.9177 0.5301 -0.3400 0.027 Uiso 1 1 calc R . . C14 C 0.9892(6) 0.5781(5) -0.2221(3) 0.0231(10) Uani 1 1 d . . . H14 H 1.0366 0.6728 -0.2535 0.028 Uiso 1 1 calc R . . C15 C 0.9873(6) 0.5191(5) -0.1233(3) 0.0240(10) Uani 1 1 d . . . H15 H 1.0330 0.5770 -0.0887 0.029 Uiso 1 1 calc R . . C16 C 0.8409(6) -0.1032(5) 0.3344(3) 0.0208(9) Uani 1 1 d . . . H16 H 0.9059 -0.0580 0.3676 0.025 Uiso 1 1 calc R . . C17 C 0.8420(6) -0.0443(5) 0.2361(3) 0.0178(9) Uani 1 1 d . . . H17 H 0.9080 0.0406 0.2032 0.021 Uiso 1 1 calc R . . C18 C 0.7456(6) -0.1102(5) 0.1851(3) 0.0175(9) Uani 1 1 d . . . C19 C 0.6442(6) -0.2339(5) 0.2396(3) 0.0192(9) Uani 1 1 d . . . H19 H 0.5738 -0.2786 0.2090 0.023 Uiso 1 1 calc R . . C20 C 0.6473(6) -0.2901(5) 0.3373(3) 0.0204(9) Uani 1 1 d . . . H20 H 0.5803 -0.3734 0.3723 0.025 Uiso 1 1 calc R . . C21 C 0.7543(6) -0.2939(6) 0.4874(3) 0.0252(10) Uani 1 1 d . . . H21A H 0.6362 -0.3172 0.5232 0.038 Uiso 1 1 calc R . . H21B H 0.8014 -0.2215 0.5144 0.038 Uiso 1 1 calc R . . H21C H 0.8306 -0.3870 0.4924 0.038 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 Cl1 0.0185(5) 0.0199(5) 0.0128(5) 0.0008(4) -0.0054(4) -0.0046(4) O1 0.039(2) 0.090(3) 0.033(2) -0.031(2) -0.0126(18) 0.000(2) O2 0.0320(19) 0.0310(19) 0.0279(18) -0.0079(15) -0.0027(15) -0.0019(15) O3 0.036(2) 0.0280(19) 0.044(2) 0.0039(17) -0.0080(17) -0.0013(16) O4 0.039(2) 0.029(2) 0.048(2) 0.0060(17) -0.0010(18) -0.0099(17) N1 0.0205(19) 0.0179(18) 0.0193(19) -0.0034(15) -0.0018(15) -0.0023(15) N2 0.0154(17) 0.0174(18) 0.0155(18) -0.0033(14) -0.0012(14) -0.0016(14) N3 0.025(2) 0.0192(19) 0.0180(19) -0.0024(15) -0.0043(15) -0.0045(15) N4 0.0197(19) 0.0203(19) 0.0167(18) -0.0038(15) -0.0048(15) 0.0002(15) C1 0.029(2) 0.020(2) 0.024(2) -0.0051(19) -0.0024(19) -0.0061(19) C2 0.023(2) 0.024(2) 0.027(2) -0.011(2) -0.0072(19) 0.0004(19) C3 0.025(2) 0.023(2) 0.021(2) -0.0075(19) -0.0060(19) 0.0029(19) C4 0.020(2) 0.017(2) 0.017(2) -0.0021(17) -0.0010(17) 0.0006(17) C5 0.017(2) 0.016(2) 0.021(2) -0.0061(17) -0.0027(17) 0.0016(17) C6 0.015(2) 0.016(2) 0.020(2) -0.0059(17) -0.0021(17) 0.0010(16) C7 0.017(2) 0.017(2) 0.020(2) -0.0002(17) -0.0027(17) -0.0011(17) C8 0.013(2) 0.019(2) 0.019(2) -0.0054(17) -0.0015(16) 0.0024(16) C9 0.016(2) 0.017(2) 0.018(2) -0.0040(17) -0.0033(17) -0.0022(17) C10 0.014(2) 0.018(2) 0.018(2) -0.0041(17) -0.0014(16) -0.0001(16) C11 0.017(2) 0.017(2) 0.017(2) -0.0032(17) -0.0028(16) 0.0000(17) C12 0.020(2) 0.019(2) 0.019(2) -0.0054(18) -0.0058(17) 0.0025(17) C13 0.025(2) 0.021(2) 0.018(2) 0.0010(18) -0.0041(18) -0.0005(18) C14 0.024(2) 0.018(2) 0.024(2) 0.0006(18) -0.0019(19) -0.0018(18) C15 0.033(3) 0.019(2) 0.023(2) -0.0044(19) -0.007(2) -0.0067(19) C16 0.020(2) 0.021(2) 0.023(2) -0.0074(18) -0.0058(18) 0.0005(18) C17 0.018(2) 0.016(2) 0.019(2) -0.0039(17) -0.0016(17) -0.0016(17) C18 0.014(2) 0.017(2) 0.020(2) -0.0034(17) -0.0016(17) 0.0013(16) C19 0.024(2) 0.018(2) 0.017(2) -0.0033(17) -0.0073(18) -0.0025(18) C20 0.023(2) 0.020(2) 0.017(2) -0.0017(18) -0.0024(18) -0.0046(18) C21 0.028(2) 0.033(3) 0.016(2) -0.0033(19) -0.0073(18) -0.001(2) #========================================================================= # 10. Molecular Geometry 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 Cl1 O1 1.420(4) . ? Cl1 O3 1.437(4) . ? Cl1 O4 1.445(4) . ? Cl1 O2 1.452(4) . ? N1 C1 1.327(6) . ? N1 C5 1.350(6) . ? N2 C6 1.341(5) . ? N2 C10 1.343(5) . ? N3 C15 1.338(6) . ? N3 C11 1.341(6) . ? N4 C20 1.342(6) . ? N4 C16 1.345(6) . ? N4 C21 1.477(6) . ? C1 C2 1.391(7) . ? C1 H1 0.9300 . ? C2 C3 1.377(7) . ? C2 H2 0.9300 . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C4 C5 1.397(6) . ? C4 H4 0.9300 . ? C5 C6 1.484(6) . ? C6 C7 1.393(6) . ? C7 C8 1.394(6) . ? C7 H7 0.9300 . ? C8 C9 1.389(6) . ? C8 C18 1.483(6) . ? C9 C10 1.395(6) . ? C9 H9 0.9300 . ? C10 C11 1.479(6) . ? C11 C12 1.392(6) . ? C12 C13 1.377(6) . ? C12 H12 0.9300 . ? C13 C14 1.384(7) . ? C13 H13 0.9300 . ? C14 C15 1.378(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.373(6) . ? C16 H16 0.9300 . ? C17 C18 1.392(6) . ? C17 H17 0.9300 . ? C18 C19 1.397(6) . ? C19 C20 1.367(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 O1 Cl1 O3 109.6(3) . . ? O1 Cl1 O4 111.3(3) . . ? O3 Cl1 O4 108.5(2) . . ? O1 Cl1 O2 109.3(2) . . ? O3 Cl1 O2 109.3(2) . . ? O4 Cl1 O2 108.8(2) . . ? C1 N1 C5 117.6(4) . . ? C6 N2 C10 118.2(4) . . ? C15 N3 C11 117.9(4) . . ? C20 N4 C16 120.8(4) . . ? C20 N4 C21 119.3(4) . . ? C16 N4 C21 119.9(4) . . ? N1 C1 C2 123.6(4) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.4(4) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.5(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 122.4(4) . . ? N1 C5 C6 115.7(4) . . ? C4 C5 C6 121.8(4) . . ? N2 C6 C7 122.7(4) . . ? N2 C6 C5 116.6(4) . . ? C7 C6 C5 120.6(4) . . ? C6 C7 C8 118.9(4) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C9 C8 C7 118.5(4) . . ? C9 C8 C18 121.3(4) . . ? C7 C8 C18 120.2(4) . . ? C8 C9 C10 119.0(4) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 122.6(4) . . ? N2 C10 C11 116.2(4) . . ? C9 C10 C11 121.2(4) . . ? N3 C11 C12 122.3(4) . . ? N3 C11 C10 116.1(4) . . ? C12 C11 C10 121.6(4) . . ? C13 C12 C11 118.9(4) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 119.2(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 118.4(4) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? N3 C15 C14 123.4(4) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N4 C16 C17 120.4(4) . . ? N4 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 116.7(4) . . ? C17 C18 C8 122.0(4) . . ? C19 C18 C8 121.2(4) . . ? C20 C19 C18 120.9(4) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? N4 C20 C19 120.4(4) . . ? N4 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _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. Mean-plane data from final SHELXL refinement run:- Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) ; # Attachment 'PV_revise.cif' #===================================================================== data_120123_PV #TrackingRef '- PV_revise.cif' _database_code_depnum_ccdc_archive 'CCDC 854081' #===================================================================== # 5. Chemical Data _chemical_name_systematic ; NONE ; _chemical_name_common NONE _chemical_formula_iupac ? _chemical_formula_moiety 'C21 H17 Cl N4 Pt, 2(Cl O4)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H17 Cl3 N4 O8 Pt' _chemical_formula_weight 754.83 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' #========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/acd _symmetry_space_group_name_Hall '-I 4bd 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 27.302(3) _cell_length_b 27.302(3) _cell_length_c 27.053(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20165(4) _cell_formula_units_Z 32 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9747 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 25.36 _cell_special_details ; ? # Insert any comments here. ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.989 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11648 _exptl_absorpt_coefficient_mu 5.939 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _exptl_absorpt_correction_T_min 0.5730 _exptl_absorpt_correction_T_max 0.7452 #========================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART APEX CCD-detector diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95159 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.38 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 4651 _reflns_number_gt 4030 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'KENX (Sakai, 2002)' _computing_publication_material ; SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976) ; #========================================================================= # 8. Refinement Data _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. High residual electron density comes from a ghost peak around Cl1 with a distance of 0.443 A. A solvent molecule, probably water or methanol, was found disordered around the symmetry centre. Any attempt to locate its atomic coordinates failed. The SQUEEZE routine in PLATON was used to modify the HKL file, resulting in improved refinement parameters for the main residue. ; _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^)+(0.0299P)^2^+129.1080P] 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_extinction_expression not_refined _refine_ls_number_reflns 4651 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.898 _refine_diff_density_min -1.127 #========================================================================= # 9. Atomic Coordinates and Displacement Parameters 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 0.213765(5) 0.510978(6) 0.062897(6) 0.02331(7) Uani 1 1 d . . . Cl1 Cl 0.13635(4) 0.54571(4) 0.06354(4) 0.0289(2) Uani 1 1 d . . . Cl2 Cl 0.49745(5) 0.58329(5) 0.07782(6) 0.0490(3) Uani 1 1 d . . . Cl3A Cl 0.16380(18) 0.75223(16) 0.0457(2) 0.0443(10) Uani 0.552(8) 1 d P . . Cl3B Cl 0.1446(3) 0.7495(2) 0.0541(2) 0.0424(12) Uani 0.448(8) 1 d P . . O1 O 0.45421(15) 0.57185(18) 0.0509(2) 0.0791(15) Uani 1 1 d . . . O2A O 0.5216(12) 0.5401(6) 0.0946(19) 0.30(2) Uani 0.55(2) 1 d P . . O2B O 0.5332(4) 0.5492(6) 0.0619(7) 0.072(5) Uani 0.45(2) 1 d P . . O3A O 0.5283(6) 0.6090(10) 0.0507(4) 0.142(11) Uani 0.55(2) 1 d P . . O3B O 0.5159(6) 0.6280(5) 0.0672(12) 0.153(12) Uani 0.45(2) 1 d P . . O4A O 0.4898(5) 0.6077(8) 0.1225(5) 0.104(6) Uani 0.55(2) 1 d P . . O4B O 0.4858(8) 0.5645(14) 0.1204(7) 0.147(12) Uani 0.45(2) 1 d P . . O5 O 0.1687(2) 0.78972(17) 0.0757(2) 0.0937(18) Uani 1 1 d . . . O6A O 0.1583(6) 0.7021(6) 0.0707(6) 0.044(3) Uani 0.552(8) 1 d P . . O6B O 0.1636(9) 0.7082(9) 0.0597(11) 0.090(9) Uani 0.448(8) 1 d P . . O7 O 0.1254(2) 0.7564(2) 0.0083(2) 0.0898(16) Uani 1 1 d . . . O8A O 0.2080(3) 0.7540(3) 0.0176(3) 0.059(2) Uani 0.552(8) 1 d P . . O8B O 0.1014(4) 0.7562(3) 0.0831(4) 0.071(4) Uani 0.448(8) 1 d P . . N1 N 0.25426(13) 0.57289(13) 0.06191(13) 0.0260(7) Uani 1 1 d . . . N2 N 0.28004(11) 0.48299(11) 0.06235(10) 0.0149(7) Uani 1 1 d . . . N3 N 0.19404(13) 0.43956(13) 0.06320(12) 0.0258(7) Uani 1 1 d . . . N4 N 0.50968(15) 0.37663(16) 0.0582(2) 0.0510(12) Uani 1 1 d . . . C1 C 0.23815(17) 0.61936(17) 0.06218(17) 0.0320(10) Uani 1 1 d . . . H1 H 0.2046 0.6253 0.0634 0.038 Uiso 1 1 calc R . . C2 C 0.27025(18) 0.65867(17) 0.06069(19) 0.0367(11) Uani 1 1 d . . . H2 H 0.2584 0.6906 0.0610 0.044 Uiso 1 1 calc R . . C3 C 0.32009(18) 0.64975(17) 0.05878(19) 0.0381(11) Uani 1 1 d . . . H3 H 0.3421 0.6757 0.0575 0.046 Uiso 1 1 calc R . . C4 C 0.33705(17) 0.60186(17) 0.05878(18) 0.0344(10) Uani 1 1 d . . . H4 H 0.3705 0.5955 0.0576 0.041 Uiso 1 1 calc R . . C5 C 0.30418(16) 0.56414(16) 0.06048(16) 0.0270(9) Uani 1 1 d . . . C6 C 0.31700(15) 0.51145(15) 0.06066(15) 0.0241(9) Uani 1 1 d . . . C7 C 0.36361(16) 0.49207(15) 0.06009(15) 0.0266(9) Uani 1 1 d . . . H7 H 0.3910 0.5124 0.0589 0.032 Uiso 1 1 calc R . . C8 C 0.36875(15) 0.44119(16) 0.06133(16) 0.0255(9) Uani 1 1 d . . . C9 C 0.32730(15) 0.41131(16) 0.06278(16) 0.0273(9) Uani 1 1 d . . . H9 H 0.3305 0.3774 0.0636 0.033 Uiso 1 1 calc R . . C10 C 0.28154(15) 0.43256(16) 0.06297(15) 0.0262(9) Uani 1 1 d . . . C11 C 0.23360(16) 0.40839(16) 0.06334(16) 0.0272(9) Uani 1 1 d . . . C12 C 0.22676(17) 0.35848(17) 0.06377(17) 0.0315(10) Uani 1 1 d . . . H12 H 0.2536 0.3375 0.0645 0.038 Uiso 1 1 calc R . . C13 C 0.17954(17) 0.33953(17) 0.06317(18) 0.0356(11) Uani 1 1 d . . . H13 H 0.1744 0.3059 0.0628 0.043 Uiso 1 1 calc R . . C14 C 0.14016(17) 0.37156(18) 0.06306(18) 0.0367(11) Uani 1 1 d . . . H14 H 0.1083 0.3595 0.0631 0.044 Uiso 1 1 calc R . . C15 C 0.14839(16) 0.42107(18) 0.06296(16) 0.0305(10) Uani 1 1 d . . . H15 H 0.1218 0.4424 0.0627 0.037 Uiso 1 1 calc R . . C16 C 0.50514(18) 0.42472(18) 0.0621(2) 0.0446(13) Uani 1 1 d . . . H16 H 0.5330 0.4442 0.0644 0.053 Uiso 1 1 calc R . . C17 C 0.46080(17) 0.44565(18) 0.0629(2) 0.0417(12) Uani 1 1 d . . . H17 H 0.4586 0.4796 0.0650 0.050 Uiso 1 1 calc R . . C18 C 0.41844(16) 0.41854(16) 0.06049(18) 0.0301(10) Uani 1 1 d . . . C19 C 0.4245(2) 0.3684(2) 0.0562(3) 0.0634(19) Uani 1 1 d . . . H19 H 0.3972 0.3482 0.0544 0.076 Uiso 1 1 calc R . . C20 C 0.4701(2) 0.3485(2) 0.0546(3) 0.079(3) Uani 1 1 d . . . H20 H 0.4737 0.3148 0.0508 0.095 Uiso 1 1 calc R . . C21 C 0.5590(2) 0.3531(2) 0.0564(3) 0.069(2) Uani 1 1 d . . . H21A H 0.5759 0.3589 0.0869 0.104 Uiso 1 1 calc R . . H21B H 0.5775 0.3669 0.0296 0.104 Uiso 1 1 calc R . . H21C H 0.5553 0.3185 0.0514 0.104 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 0.02222(10) 0.02783(10) 0.01987(10) 0.00048(7) 0.00087(6) 0.00400(6) Cl1 0.0234(5) 0.0337(5) 0.0296(5) 0.0007(5) 0.0009(4) 0.0059(4) Cl2 0.0315(7) 0.0472(8) 0.0682(10) -0.0009(7) -0.0007(6) -0.0081(5) Cl3A 0.034(2) 0.0246(15) 0.074(3) 0.0038(15) -0.006(2) 0.0014(16) Cl3B 0.045(3) 0.0260(17) 0.056(2) 0.0053(13) 0.011(3) 0.001(2) O1 0.030(2) 0.076(3) 0.131(4) 0.009(3) -0.016(2) -0.003(2) O2A 0.25(3) 0.048(8) 0.59(6) -0.01(2) -0.33(3) 0.002(14) O2B 0.011(4) 0.066(10) 0.139(13) -0.029(8) 0.007(6) 0.003(4) O3A 0.069(9) 0.31(3) 0.045(6) -0.015(9) 0.010(5) -0.110(13) O3B 0.052(8) 0.030(7) 0.38(4) 0.016(11) 0.035(14) -0.021(5) O4A 0.075(8) 0.177(16) 0.061(7) -0.039(9) 0.016(6) 0.006(9) O4B 0.124(15) 0.25(3) 0.064(10) 0.044(17) 0.034(10) -0.049(19) O5 0.088(4) 0.049(3) 0.144(5) 0.005(3) -0.034(4) -0.023(3) O6A 0.038(6) 0.022(5) 0.072(6) 0.017(5) -0.004(6) -0.011(4) O6B 0.048(8) 0.035(9) 0.19(2) 0.049(9) 0.061(10) 0.012(7) O7 0.086(4) 0.090(4) 0.094(4) 0.026(3) -0.021(3) -0.009(3) O8A 0.053(5) 0.046(4) 0.079(6) 0.011(4) 0.016(4) 0.012(3) O8B 0.075(7) 0.032(5) 0.105(8) 0.002(5) 0.050(6) 0.002(4) N1 0.0253(18) 0.0276(19) 0.0252(18) 0.0034(16) -0.0014(15) 0.0045(15) N2 0.0224(16) 0.0180(16) 0.0045(14) 0.0009(12) 0.0026(13) 0.0076(13) N3 0.0264(18) 0.0308(19) 0.0201(17) -0.0004(16) 0.0012(15) 0.0032(15) N4 0.024(2) 0.040(2) 0.088(4) 0.007(2) -0.007(2) -0.0006(18) C1 0.032(2) 0.034(2) 0.030(2) -0.002(2) 0.000(2) 0.0095(19) C2 0.042(3) 0.025(2) 0.043(3) -0.004(2) 0.003(2) 0.003(2) C3 0.041(3) 0.026(2) 0.047(3) 0.001(2) -0.005(2) -0.001(2) C4 0.029(2) 0.037(3) 0.038(3) 0.000(2) -0.002(2) -0.001(2) C5 0.027(2) 0.029(2) 0.025(2) 0.0002(18) -0.0032(18) 0.0051(18) C6 0.027(2) 0.027(2) 0.018(2) 0.0004(18) -0.0001(18) 0.0045(18) C7 0.026(2) 0.028(2) 0.026(2) 0.0026(19) -0.0007(18) -0.0053(17) C8 0.020(2) 0.034(2) 0.023(2) 0.0008(19) 0.0002(17) 0.0028(17) C9 0.027(2) 0.027(2) 0.027(2) 0.0033(18) 0.0002(19) 0.0047(18) C10 0.027(2) 0.032(2) 0.019(2) 0.0002(18) 0.0001(18) -0.0047(18) C11 0.026(2) 0.032(2) 0.023(2) 0.0013(18) 0.0033(18) 0.0026(18) C12 0.029(2) 0.032(2) 0.033(2) 0.000(2) 0.000(2) -0.0015(19) C13 0.033(2) 0.031(2) 0.043(3) 0.001(2) 0.005(2) -0.005(2) C14 0.026(2) 0.044(3) 0.040(3) 0.000(2) -0.001(2) -0.006(2) C15 0.020(2) 0.044(3) 0.028(2) 0.000(2) 0.0015(18) -0.0001(19) C16 0.029(3) 0.034(3) 0.072(4) 0.007(3) -0.003(3) -0.009(2) C17 0.027(2) 0.032(3) 0.066(4) 0.001(3) -0.001(2) 0.004(2) C18 0.023(2) 0.028(2) 0.039(3) 0.004(2) -0.004(2) -0.0005(17) C19 0.028(3) 0.033(3) 0.129(6) 0.009(3) -0.007(3) -0.005(2) C20 0.032(3) 0.031(3) 0.174(8) 0.016(4) -0.008(4) 0.002(2) C21 0.027(3) 0.042(3) 0.139(7) 0.011(4) -0.009(4) 0.007(2) #========================================================================= # 10. Molecular Geometry 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 N2 1.964(3) . ? Pt1 N1 2.020(4) . ? Pt1 N3 2.023(4) . ? Pt1 Cl1 2.3167(10) . ? Pt1 Pt1 3.8227(6) 15_444 ? Pt1 Pt1 3.9365(6) 5 ? Cl2 O4B 1.302(15) . ? Cl2 O3A 1.320(14) . ? Cl2 O3B 1.352(13) . ? Cl2 O4A 1.397(11) . ? Cl2 O2B 1.417(11) . ? Cl2 O1 1.422(5) . ? Cl2 O2A 1.426(18) . ? Cl3A O5 1.312(7) . ? Cl3A O8A 1.428(9) . ? Cl3A O7 1.462(7) . ? Cl3A O6A 1.533(18) . ? Cl3B O6B 1.25(3) . ? Cl3B O7 1.359(8) . ? Cl3B O5 1.408(8) . ? Cl3B O8B 1.427(11) . ? N1 C1 1.343(6) . ? N1 C5 1.384(6) . ? N2 C6 1.274(5) . ? N2 C10 1.377(5) . ? N3 C15 1.345(6) . ? N3 C11 1.375(6) . ? N4 C16 1.323(7) . ? N4 C20 1.329(7) . ? N4 C21 1.493(7) . ? C1 C2 1.386(7) . ? C1 H1 0.9300 . ? C2 C3 1.383(7) . ? C2 H2 0.9300 . ? C3 C4 1.387(7) . ? C3 H3 0.9300 . ? C4 C5 1.367(6) . ? C4 H4 0.9300 . ? C5 C6 1.481(6) . ? C6 C7 1.378(6) . ? C7 C8 1.397(6) . ? C7 H7 0.9300 . ? C8 C9 1.396(6) . ? C8 C18 1.491(6) . ? C9 C10 1.377(6) . ? C9 H9 0.9300 . ? C10 C11 1.466(6) . ? C11 C12 1.375(6) . ? C12 C13 1.389(6) . ? C12 H12 0.9300 . ? C13 C14 1.386(7) . ? C13 H13 0.9300 . ? C14 C15 1.371(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.339(7) . ? C16 H16 0.9300 . ? C17 C18 1.374(6) . ? C17 H17 0.9300 . ? C18 C19 1.383(7) . ? C19 C20 1.359(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 N2 Pt1 N1 79.70(13) . . ? N2 Pt1 N3 82.54(13) . . ? N1 Pt1 N3 162.24(14) . . ? N2 Pt1 Cl1 178.73(10) . . ? N1 Pt1 Cl1 99.03(10) . . ? N3 Pt1 Cl1 98.73(10) . . ? N2 Pt1 Pt1 64.20(8) . 15_444 ? N1 Pt1 Pt1 96.27(10) . 15_444 ? N3 Pt1 Pt1 76.18(10) . 15_444 ? Cl1 Pt1 Pt1 116.05(3) . 15_444 ? N2 Pt1 Pt1 62.00(8) . 5 ? N1 Pt1 Pt1 73.35(10) . 5 ? N3 Pt1 Pt1 97.89(10) . 5 ? Cl1 Pt1 Pt1 117.71(3) . 5 ? Pt1 Pt1 Pt1 126.185(11) 15_444 5 ? O4B Cl2 O3A 149.2(12) . . ? O4B Cl2 O3B 129.5(16) . . ? O3A Cl2 O3B 33.2(10) . . ? O4B Cl2 O4A 52.1(12) . . ? O3A Cl2 O4A 108.8(9) . . ? O3B Cl2 O4A 78.9(12) . . ? O4B Cl2 O2B 100.3(16) . . ? O3A Cl2 O2B 75.0(12) . . ? O3B Cl2 O2B 105.8(9) . . ? O4A Cl2 O2B 132.8(9) . . ? O4B Cl2 O1 99.4(10) . . ? O3A Cl2 O1 111.3(6) . . ? O3B Cl2 O1 113.6(11) . . ? O4A Cl2 O1 115.1(6) . . ? O2B Cl2 O1 105.8(7) . . ? O4B Cl2 O2A 60.3(17) . . ? O3A Cl2 O2A 108.8(18) . . ? O3B Cl2 O2A 129.9(15) . . ? O4A Cl2 O2A 100.8(17) . . ? O2B Cl2 O2A 40(2) . . ? O1 Cl2 O2A 111.5(7) . . ? O5 Cl3A O8A 102.5(5) . . ? O5 Cl3A O7 116.1(5) . . ? O8A Cl3A O7 103.6(5) . . ? O5 Cl3A O6A 115.7(8) . . ? O8A Cl3A O6A 110.3(9) . . ? O7 Cl3A O6A 107.7(6) . . ? O6B Cl3B O7 113.3(14) . . ? O6B Cl3B O5 117.3(14) . . ? O7 Cl3B O5 116.7(5) . . ? O6B Cl3B O8B 113.2(13) . . ? O7 Cl3B O8B 99.5(7) . . ? O5 Cl3B O8B 93.3(6) . . ? Cl3A O5 Cl3B 24.1(2) . . ? Cl3B O7 Cl3A 23.2(2) . . ? C1 N1 C5 119.1(4) . . ? C1 N1 Pt1 127.7(3) . . ? C5 N1 Pt1 113.3(3) . . ? C6 N2 C10 125.9(3) . . ? C6 N2 Pt1 119.5(3) . . ? C10 N2 Pt1 114.6(3) . . ? C15 N3 C11 119.7(4) . . ? C15 N3 Pt1 127.5(3) . . ? C11 N3 Pt1 112.8(3) . . ? C16 N4 C20 120.2(5) . . ? C16 N4 C21 120.9(4) . . ? C20 N4 C21 118.8(5) . . ? N1 C1 C2 121.6(4) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 N1 121.2(4) . . ? C4 C5 C6 125.2(4) . . ? N1 C5 C6 113.6(4) . . ? N2 C6 C7 119.8(4) . . ? N2 C6 C5 113.9(3) . . ? C7 C6 C5 126.2(4) . . ? C6 C7 C8 118.3(4) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 120.0(4) . . ? C9 C8 C18 119.7(4) . . ? C7 C8 C18 120.2(4) . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 N2 116.6(4) . . ? C9 C10 C11 128.3(4) . . ? N2 C10 C11 115.1(4) . . ? N3 C11 C12 120.4(4) . . ? N3 C11 C10 115.0(4) . . ? C12 C11 C10 124.6(4) . . ? C11 C12 C13 119.7(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.0(4) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? N3 C15 C14 121.5(4) . . ? N3 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? N4 C16 C17 120.6(5) . . ? N4 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 122.0(5) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C19 115.8(4) . . ? C17 C18 C8 122.8(4) . . ? C19 C18 C8 121.4(4) . . ? C20 C19 C18 120.6(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? N4 C20 C19 120.7(5) . . ? N4 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.250 0.125 184.6 63.6 2 0.000 0.250 0.625 184.7 62.9 3 0.000 0.250 0.375 15.0 5.5 4 0.000 0.250 0.875 15.0 5.8 5 0.000 0.750 0.375 184.8 64.8 6 0.000 0.750 0.875 184.7 64.9 7 0.000 0.750 0.125 15.0 4.7 8 0.000 0.750 0.625 15.0 5.1 9 0.500 0.250 0.875 184.8 64.8 10 0.500 0.250 0.375 184.7 64.9 11 0.500 0.750 0.125 184.7 62.9 12 0.500 0.750 0.625 184.6 63.7 13 0.500 0.250 0.125 15.0 5.1 14 0.500 0.250 0.625 15.0 4.7 15 0.500 0.750 0.375 15.0 5.8 16 0.500 0.750 0.875 15.0 5.5 _platon_squeeze_details ; ; #====================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ #========================================================================= # END of CIF #=========================================================================