# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 N3 Cl Pt, Cl O4, H2 O' _chemical_formula_sum 'C15 H13 Cl2 N3 O5 Pt' _chemical_formula_weight 581.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6710(6) _cell_length_b 10.2403(9) _cell_length_c 13.3874(14) _cell_angle_alpha 103.816(5) _cell_angle_beta 102.813(5) _cell_angle_gamma 90.485(5) _cell_volume 864.14(14) _cell_formula_units_Z 2 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 2600 _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 65.48 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 18.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5368 _exptl_absorpt_correction_T_max 0.7004 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick)' _exptl_special_details ; A suitable crystal was mounted in a Cryo-loop with paratone-N and transferred immediately to the goniostat bathed in a cold stream. ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART6000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6655 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 66.95 _reflns_number_total 2879 _reflns_number_gt 2441 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART v5.632' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. The O-atoms of the anion (O1-O4) are disordered. A disorder model consisting of 2 components is presented. The refined occupancies for O1 and O4 have the major component 78 and 77%, respectively. The occupancy of the major component for O2 and O3 is 51 and 50%, respectively. The O-atoms of the anion were refined isotropically; the water oxygen (O5) was refined anisotropically. ; _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^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2879 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Pt Pt 0.75458(7) 0.50323(4) 0.51446(4) 0.03421(19) Uani 1 1 d . . . Cl1 Cl 0.7439(4) 0.7176(3) 0.4861(2) 0.0453(7) Uani 1 1 d . . . N1 N 0.7993(14) 0.5518(9) 0.6735(8) 0.042(2) Uani 1 1 d . . . N2 N 0.7628(15) 0.3234(9) 0.5366(7) 0.042(2) Uani 1 1 d . . . N3 N 0.7130(14) 0.3923(11) 0.3615(7) 0.044(2) Uani 1 1 d . . . C1 C 0.8179(18) 0.6765(12) 0.7403(10) 0.047(3) Uani 1 1 d . . . H1 H 0.8130 0.7525 0.7122 0.057 Uiso 1 1 calc R . . C2 C 0.844(2) 0.6948(13) 0.8465(11) 0.057(4) Uani 1 1 d . . . H2 H 0.8549 0.7820 0.8909 0.068 Uiso 1 1 calc R . . C3 C 0.852(2) 0.5839(15) 0.8878(10) 0.060(4) Uani 1 1 d . . . H3 H 0.8680 0.5956 0.9610 0.072 Uiso 1 1 calc R . . C4 C 0.8386(19) 0.4551(13) 0.8231(10) 0.051(3) Uani 1 1 d . . . H4 H 0.8471 0.3794 0.8517 0.061 Uiso 1 1 calc R . . C5 C 0.8123(17) 0.4399(12) 0.7160(9) 0.040(3) Uani 1 1 d . . . C6 C 0.7930(16) 0.3107(11) 0.6376(9) 0.036(2) Uani 1 1 d . . . C7 C 0.801(2) 0.1848(14) 0.6550(11) 0.055(3) Uani 1 1 d . . . H7 H 0.8257 0.1736 0.7243 0.066 Uiso 1 1 calc R . . C8 C 0.774(2) 0.0736(12) 0.5700(11) 0.054(3) Uani 1 1 d . . . H8 H 0.7766 -0.0131 0.5821 0.065 Uiso 1 1 calc R . . C9 C 0.7419(18) 0.0872(12) 0.4669(11) 0.051(3) Uani 1 1 d . . . H9 H 0.7228 0.0115 0.4091 0.061 Uiso 1 1 calc R . . C10 C 0.7396(17) 0.2162(11) 0.4529(9) 0.042(3) Uani 1 1 d . . . C11 C 0.7094(17) 0.2587(12) 0.3526(9) 0.042(3) Uani 1 1 d . . . C12 C 0.6827(19) 0.1693(13) 0.2541(10) 0.050(3) Uani 1 1 d . . . H12 H 0.6810 0.0759 0.2479 0.060 Uiso 1 1 calc R . . C13 C 0.659(2) 0.2189(16) 0.1656(10) 0.061(4) Uani 1 1 d . . . H13 H 0.6413 0.1593 0.0985 0.073 Uiso 1 1 calc R . . C14 C 0.660(2) 0.3561(15) 0.1752(10) 0.055(3) Uani 1 1 d . . . H14 H 0.6427 0.3902 0.1149 0.066 Uiso 1 1 calc R . . C15 C 0.6870(18) 0.4429(15) 0.2743(10) 0.053(3) Uani 1 1 d . . . H15 H 0.6875 0.5365 0.2816 0.063 Uiso 1 1 calc R . . Cl2 Cl 0.3906(6) 0.2250(3) 0.8668(2) 0.0573(8) Uani 1 1 d . . . O1A O 0.303(3) 0.1425(19) 0.9205(14) 0.085(7) Uiso 0.78(5) 1 d P A 1 O2A O 0.403(10) 0.167(3) 0.7608(19) 0.075(11) Uiso 0.51(11) 1 d P A 1 O3A O 0.308(7) 0.354(3) 0.881(2) 0.084(12) Uiso 0.50(7) 1 d P A 1 O4A O 0.606(3) 0.227(2) 0.9124(13) 0.102(7) Uiso 0.77(3) 1 d P . 1 O1B O 0.210(11) 0.184(6) 0.888(5) 0.08(2) Uiso 0.22(5) 1 d P A 2 O2B O 0.313(11) 0.183(3) 0.755(2) 0.081(12) Uiso 0.49(11) 1 d P A 2 O3B O 0.422(8) 0.362(3) 0.913(3) 0.094(12) Uiso 0.50(7) 1 d P A 2 O4B O 0.491(10) 0.120(7) 0.906(4) 0.10(2) Uiso 0.23(3) 1 d P . 2 O5 O 0.874(3) 0.0070(16) 0.8489(16) 0.151(7) Uani 1 1 d . . . H51 H 0.9914 0.0596 0.8783 0.227 Uiso 1 1 d . . . H52 H 0.8162 0.0774 0.8806 0.227 Uiso 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 Pt 0.0282(3) 0.0299(3) 0.0466(3) 0.01133(18) 0.01081(19) 0.00273(18) Cl1 0.0399(16) 0.0291(14) 0.0715(19) 0.0181(12) 0.0160(13) 0.0039(12) N1 0.026(5) 0.038(5) 0.066(6) 0.014(4) 0.014(4) -0.001(4) N2 0.037(6) 0.034(5) 0.052(6) 0.006(4) 0.011(4) 0.009(4) N3 0.029(5) 0.058(7) 0.045(6) 0.016(5) 0.010(4) 0.007(5) C1 0.033(7) 0.039(7) 0.064(8) 0.005(5) 0.009(6) -0.006(5) C2 0.052(8) 0.042(7) 0.070(9) -0.001(6) 0.017(7) 0.005(6) C3 0.051(8) 0.079(10) 0.049(7) 0.011(7) 0.016(6) 0.020(8) C4 0.045(8) 0.046(7) 0.066(8) 0.014(6) 0.020(6) 0.004(6) C5 0.027(6) 0.040(6) 0.054(7) 0.016(5) 0.010(5) 0.006(5) C6 0.020(5) 0.039(6) 0.051(7) 0.012(5) 0.010(5) 0.007(5) C7 0.044(8) 0.054(8) 0.074(9) 0.027(7) 0.015(6) 0.005(7) C8 0.055(8) 0.031(6) 0.082(9) 0.022(6) 0.019(7) 0.008(6) C9 0.034(7) 0.037(7) 0.083(9) 0.009(6) 0.023(6) 0.016(6) C10 0.023(6) 0.036(6) 0.065(8) 0.010(5) 0.011(5) 0.003(5) C11 0.023(6) 0.048(7) 0.051(7) 0.010(5) 0.000(5) 0.003(5) C12 0.045(8) 0.040(7) 0.061(8) 0.002(5) 0.015(6) 0.002(6) C13 0.060(9) 0.071(10) 0.043(7) -0.001(6) 0.008(6) -0.001(8) C14 0.043(8) 0.069(10) 0.051(7) 0.014(6) 0.009(6) 0.003(7) C15 0.032(7) 0.068(9) 0.054(8) 0.011(6) 0.007(5) 0.009(6) Cl2 0.079(2) 0.0441(17) 0.0514(17) 0.0106(13) 0.0222(16) 0.0029(17) O5 0.124(14) 0.094(11) 0.25(2) 0.069(13) 0.052(13) 0.020(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 Pt N2 1.933(9) . ? Pt N1 2.020(10) . ? Pt N3 2.048(9) . ? Pt Cl1 2.314(3) . ? N1 C1 1.359(15) . ? N1 C5 1.391(14) . ? N2 C10 1.347(15) . ? N2 C6 1.360(14) . ? N3 C11 1.344(16) . ? N3 C15 1.363(16) . ? C1 C2 1.360(18) . ? C1 H1 0.9400 . ? C2 C3 1.373(19) . ? C2 H2 0.9400 . ? C3 C4 1.384(18) . ? C3 H3 0.9400 . ? C4 C5 1.375(17) . ? C4 H4 0.9400 . ? C5 C6 1.464(16) . ? C6 C7 1.364(17) . ? C7 C8 1.382(19) . ? C7 H7 0.9400 . ? C8 C9 1.389(19) . ? C8 H8 0.9400 . ? C9 C10 1.378(17) . ? C9 H9 0.9400 . ? C10 C11 1.482(16) . ? C11 C12 1.388(16) . ? C12 C13 1.375(19) . ? C12 H12 0.9400 . ? C13 C14 1.38(2) . ? C13 H13 0.9400 . ? C14 C15 1.383(18) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? Cl2 O3B 1.38(3) . ? Cl2 O1B 1.39(6) . ? Cl2 O3A 1.42(3) . ? Cl2 O4B 1.42(6) . ? Cl2 O2A 1.42(3) . ? Cl2 O2B 1.43(3) . ? Cl2 O1A 1.427(18) . ? Cl2 O4A 1.430(19) . ? O5 H51 0.9004 . ? O5 H52 0.8839 . ? 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 Pt N1 81.3(4) . . ? N2 Pt N3 80.0(4) . . ? N1 Pt N3 161.3(4) . . ? N2 Pt Cl1 179.4(3) . . ? N1 Pt Cl1 99.3(3) . . ? N3 Pt Cl1 99.4(3) . . ? C1 N1 C5 118.6(10) . . ? C1 N1 Pt 128.3(9) . . ? C5 N1 Pt 113.2(7) . . ? C10 N2 C6 122.6(10) . . ? C10 N2 Pt 119.6(8) . . ? C6 N2 Pt 117.8(7) . . ? C11 N3 C15 121.0(11) . . ? C11 N3 Pt 113.1(7) . . ? C15 N3 Pt 125.9(9) . . ? N1 C1 C2 122.1(12) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 119.0(12) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 120.8(12) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.7(12) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 N1 120.7(11) . . ? C4 C5 C6 125.1(11) . . ? N1 C5 C6 114.2(10) . . ? N2 C6 C7 118.8(11) . . ? N2 C6 C5 113.5(10) . . ? C7 C6 C5 127.8(11) . . ? C6 C7 C8 119.5(12) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 121.5(12) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C8 117.2(12) . . ? C10 C9 H9 121.4 . . ? C8 C9 H9 121.4 . . ? N2 C10 C9 120.5(11) . . ? N2 C10 C11 111.3(10) . . ? C9 C10 C11 128.2(11) . . ? N3 C11 C12 120.4(11) . . ? N3 C11 C10 116.0(10) . . ? C12 C11 C10 123.6(12) . . ? C13 C12 C11 119.2(13) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.1(12) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 119.5(13) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N3 C15 C14 119.8(14) . . ? N3 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? O3B Cl2 O1B 106(3) . . ? O3B Cl2 O4B 127(3) . . ? O1B Cl2 O4B 89(4) . . ? O3A Cl2 O2A 113(2) . . ? O3B Cl2 O2B 118(2) . . ? O1B Cl2 O2B 93(3) . . ? O4B Cl2 O2B 111(3) . . ? O3A Cl2 O1A 111.1(14) . . ? O2A Cl2 O1A 117.7(13) . . ? O3A Cl2 O4A 115(2) . . ? O2A Cl2 O4A 96(3) . . ? O1A Cl2 O4A 102.3(13) . . ? H51 O5 H52 83.7 . . ? 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 Pt N1 C1 179.6(10) . . . . ? N3 Pt N1 C1 179.2(10) . . . . ? Cl1 Pt N1 C1 -0.4(10) . . . . ? N2 Pt N1 C5 -0.1(8) . . . . ? N3 Pt N1 C5 -0.5(15) . . . . ? Cl1 Pt N1 C5 179.8(7) . . . . ? N1 Pt N2 C10 179.8(9) . . . . ? N3 Pt N2 C10 -0.3(9) . . . . ? Cl1 Pt N2 C10 4(29) . . . . ? N1 Pt N2 C6 -0.4(8) . . . . ? N3 Pt N2 C6 179.5(9) . . . . ? Cl1 Pt N2 C6 -176(100) . . . . ? N2 Pt N3 C11 0.8(8) . . . . ? N1 Pt N3 C11 1.2(16) . . . . ? Cl1 Pt N3 C11 -179.2(7) . . . . ? N2 Pt N3 C15 179.7(10) . . . . ? N1 Pt N3 C15 -179.9(10) . . . . ? Cl1 Pt N3 C15 -0.3(10) . . . . ? C5 N1 C1 C2 -1.7(17) . . . . ? Pt N1 C1 C2 178.6(9) . . . . ? N1 C1 C2 C3 1(2) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 N1 -0.1(18) . . . . ? C3 C4 C5 C6 -179.3(12) . . . . ? C1 N1 C5 C4 1.5(17) . . . . ? Pt N1 C5 C4 -178.7(9) . . . . ? C1 N1 C5 C6 -179.2(9) . . . . ? Pt N1 C5 C6 0.5(12) . . . . ? C10 N2 C6 C7 0.5(17) . . . . ? Pt N2 C6 C7 -179.3(9) . . . . ? C10 N2 C6 C5 -179.4(10) . . . . ? Pt N2 C6 C5 0.8(13) . . . . ? C4 C5 C6 N2 178.4(11) . . . . ? N1 C5 C6 N2 -0.9(14) . . . . ? C4 C5 C6 C7 -1(2) . . . . ? N1 C5 C6 C7 179.3(11) . . . . ? N2 C6 C7 C8 -1.7(19) . . . . ? C5 C6 C7 C8 178.1(11) . . . . ? C6 C7 C8 C9 1(2) . . . . ? C7 C8 C9 C10 0(2) . . . . ? C6 N2 C10 C9 1.2(17) . . . . ? Pt N2 C10 C9 -179.0(8) . . . . ? C6 N2 C10 C11 -179.9(9) . . . . ? Pt N2 C10 C11 -0.1(13) . . . . ? C8 C9 C10 N2 -1.4(18) . . . . ? C8 C9 C10 C11 179.9(11) . . . . ? C15 N3 C11 C12 1.1(17) . . . . ? Pt N3 C11 C12 -179.9(9) . . . . ? C15 N3 C11 C10 180.0(10) . . . . ? Pt N3 C11 C10 -1.1(13) . . . . ? N2 C10 C11 N3 0.8(15) . . . . ? C9 C10 C11 N3 179.6(11) . . . . ? N2 C10 C11 C12 179.6(11) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? N3 C11 C12 C13 -0.4(19) . . . . ? C10 C11 C12 C13 -179.1(11) . . . . ? C11 C12 C13 C14 0(2) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C11 N3 C15 C14 -1.1(18) . . . . ? Pt N3 C15 C14 -179.9(9) . . . . ? C13 C14 C15 N3 0(2) . . . . ? 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 O5 H51 O1A 0.90 2.14 3.02(2) 164 1_655 O5 H51 O1B 0.90 1.88 2.74(6) 158 1_655 O5 H52 O4A 0.88 2.12 2.97(2) 162 1_555 O5 H52 O4B 0.88 2.30 2.99(6) 135 1_555 _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 66.95 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 2.019 _refine_diff_density_min -1.290 _refine_diff_density_rms 0.219 _iucr_refine_instructions_details ; TITL 1 in P-1 CELL 1.54178 6.6710 10.2403 13.3874 103.816 102.813 90.485 ZERR 2.00 0.0006 0.0009 0.0014 0.005 0.005 0.005 LATT 1 SFAC C H N O CL PT UNIT 30 26 6 10 4 2 TEMP -43.0 omit 1 5 0 L.S. 5 acta bond $h conf mpla 6 n1 c1 c2 c3 c4 c5 mpla 6 n2 c6 c7 c8 c9 c10 pt mpla 6 n2 c6 c7 c8 c9 c10 pt mpla 6 n3 c11 c12 c13 c14 c15 htab 2.5 eqiv $1 x+1, y, z htab o5 o1a_$1 htab o5 o1b_$1 eqiv $2 x, y, z htab o5 o4a_$2 htab o5 o4b_$2 size 0.18 0.03 0.02 FMAP 2 PLAN 5 WGHT 0.075900 FVAR 0.28170 0.78135 0.51216 0.50433 0.77066 PT 6 0.754581 0.503228 0.514459 11.00000 0.02817 0.02986 = 0.04665 0.01133 0.01081 0.00273 CL1 5 0.743900 0.717576 0.486119 11.00000 0.03986 0.02914 = 0.07149 0.01813 0.01597 0.00390 N1 3 0.799289 0.551808 0.673495 11.00000 0.02577 0.03761 = 0.06589 0.01417 0.01384 -0.00136 N2 3 0.762830 0.323360 0.536582 11.00000 0.03689 0.03392 = 0.05244 0.00561 0.01109 0.00859 N3 3 0.712953 0.392346 0.361461 11.00000 0.02901 0.05816 = 0.04542 0.01562 0.00962 0.00715 C1 1 0.817934 0.676462 0.740313 11.00000 0.03299 0.03923 = 0.06423 0.00532 0.00928 -0.00635 AFIX 43 H1 2 0.812986 0.752492 0.712212 11.00000 -1.20000 AFIX 0 C2 1 0.843507 0.694759 0.846468 11.00000 0.05210 0.04248 = 0.06964 -0.00122 0.01707 0.00550 AFIX 43 H2 2 0.854936 0.782049 0.890918 11.00000 -1.20000 AFIX 0 C3 1 0.852400 0.583874 0.887820 11.00000 0.05112 0.07873 = 0.04906 0.01108 0.01577 0.01966 AFIX 43 H3 2 0.868049 0.595585 0.961009 11.00000 -1.20000 AFIX 0 C4 1 0.838604 0.455088 0.823060 11.00000 0.04547 0.04561 = 0.06561 0.01394 0.02005 0.00361 AFIX 43 H4 2 0.847088 0.379446 0.851729 11.00000 -1.20000 AFIX 0 C5 1 0.812255 0.439891 0.716004 11.00000 0.02727 0.03999 = 0.05434 0.01573 0.01048 0.00596 C6 1 0.792956 0.310717 0.637575 11.00000 0.01972 0.03900 = 0.05111 0.01183 0.00988 0.00674 C7 1 0.801357 0.184752 0.655021 11.00000 0.04396 0.05442 = 0.07417 0.02655 0.01509 0.00496 AFIX 43 H7 2 0.825698 0.173647 0.724309 11.00000 -1.20000 AFIX 0 C8 1 0.773782 0.073576 0.569978 11.00000 0.05483 0.03145 = 0.08244 0.02188 0.01893 0.00831 AFIX 43 H8 2 0.776639 -0.013149 0.582146 11.00000 -1.20000 AFIX 0 C9 1 0.741936 0.087155 0.466909 11.00000 0.03396 0.03725 = 0.08345 0.00886 0.02287 0.01572 AFIX 43 H9 2 0.722811 0.011467 0.409126 11.00000 -1.20000 AFIX 0 C10 1 0.739557 0.216225 0.452927 11.00000 0.02332 0.03559 = 0.06529 0.01020 0.01056 0.00273 C11 1 0.709394 0.258730 0.352556 11.00000 0.02325 0.04825 = 0.05063 0.01045 0.00006 0.00268 C12 1 0.682684 0.169296 0.254058 11.00000 0.04533 0.03959 = 0.06077 0.00205 0.01469 0.00158 AFIX 43 H12 2 0.681042 0.075882 0.247867 11.00000 -1.20000 AFIX 0 C13 1 0.658651 0.218942 0.165634 11.00000 0.06035 0.07056 = 0.04281 -0.00121 0.00777 -0.00077 AFIX 43 H13 2 0.641273 0.159331 0.098540 11.00000 -1.20000 AFIX 0 C14 1 0.660003 0.356059 0.175238 11.00000 0.04285 0.06925 = 0.05138 0.01428 0.00867 0.00310 AFIX 43 H14 2 0.642698 0.390234 0.114858 11.00000 -1.20000 AFIX 0 C15 1 0.687003 0.442898 0.274344 11.00000 0.03235 0.06775 = 0.05446 0.01125 0.00745 0.00922 AFIX 43 H15 2 0.687467 0.536510 0.281636 11.00000 -1.20000 AFIX 0 CL2 5 0.390601 0.225033 0.866827 11.00000 0.07940 0.04406 = 0.05136 0.01062 0.02221 0.00286 PART 1 O1A 4 0.303261 0.142460 0.920452 21.00000 0.08493 O2A 4 0.402529 0.166826 0.760816 31.00000 0.07471 O3A 4 0.307550 0.353569 0.880804 41.00000 0.08406 O4A 4 0.606068 0.226796 0.912421 51.00000 0.10247 PART 2 O1B 4 0.209780 0.183626 0.888477 -21.00000 0.07859 O2B 4 0.312737 0.182959 0.755184 -31.00000 0.08080 O3B 4 0.422413 0.361545 0.912880 -41.00000 0.09381 O4B 4 0.490716 0.119587 0.906138 -51.00000 0.10049 PART 0 O5 4 0.874236 0.006969 0.848930 11.00000 0.12425 0.09400 = 0.25389 0.06862 0.05198 0.01998 AFIX 1 H51 2 0.991360 0.059570 0.878280 11.00000 -1.50000 H52 2 0.816200 0.077400 0.880600 11.00000 -1.50000 HKLF 4 REM 07199f in P-1 (CRYSTAL 3) REM R1 = 0.0534 for 2441 Fo > 4sig(Fo) and 0.0658 for all 2879 data REM 235 parameters refined using 0 restraints END WGHT 0.0760 0.0000 REM Highest difference peak 2.019, deepest hole -1.290, 1-sigma level 0.219 Q1 1 0.7969 0.5367 0.4592 11.00000 0.05 2.02 Q2 1 0.7257 0.4277 0.4562 11.00000 0.05 1.91 Q3 1 0.6815 0.5207 0.4478 11.00000 0.05 1.83 Q4 1 0.7616 0.5791 0.5412 11.00000 0.05 1.77 Q5 1 0.7796 0.5247 0.5967 11.00000 0.05 1.75 ; _database_code_depnum_ccdc_archive 'CCDC 948313' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 N3 Cl Pt, Cl O4' _chemical_formula_sum 'C15 H11 Cl2 N3 O4 Pt' _chemical_formula_weight 563.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0027 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N -0.0031 0.0054 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' O O -0.0042 0.0099 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' Cl Cl 0.1687 0.2462 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' Pt Pt -6.9210 11.8937 'L. Kissel & R.H. Pratt, Acta Cryst A (1990), A46, 170-175' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 7.0189(3) _cell_length_b 16.8805(8) _cell_length_c 26.8979(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.336(3) _cell_angle_gamma 90.00 _cell_volume 3186.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5242 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 33.16 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.005 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 15.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5675 _exptl_absorpt_correction_T_max 0.9244 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop mount with paratone ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.88560 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'Si-<111> channel cut crystal' _diffrn_measurement_device_type 'Bruker AXS APEXII CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41902 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 33.67 _reflns_number_total 6536 _reflns_number_gt 4625 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 v2010.3.0' _computing_cell_refinement 'Bruker SAINT v7.60A' _computing_data_reduction 'Bruker SAINT v7.60A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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^)+(0.0001P)^2^+0.9677P] 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 6536 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.45966(3) 0.219395(15) 0.059104(10) 0.02133(8) Uani 1 1 d . . . Cl1 Cl 0.3718(2) 0.09324(9) 0.03603(6) 0.0282(4) Uani 1 1 d . . . N1A N 0.4456(7) 0.2057(3) 0.13342(18) 0.0216(11) Uani 1 1 d . . . N2A N 0.5448(7) 0.3241(3) 0.07868(19) 0.0206(11) Uani 1 1 d . . . N3A N 0.5047(7) 0.2649(3) -0.0093(2) 0.0247(12) Uani 1 1 d . . . C1A C 0.3926(8) 0.1420(4) 0.1590(2) 0.0274(15) Uani 1 1 d . . . H2 H 0.3538 0.0959 0.1413 0.033 Uiso 1 1 calc R . . C2A C 0.3921(9) 0.1406(4) 0.2103(2) 0.0333(16) Uani 1 1 d . . . H9 H 0.3573 0.0937 0.2274 0.040 Uiso 1 1 calc R . . C3A C 0.4422(10) 0.2078(4) 0.2366(3) 0.0373(17) Uani 1 1 d . . . H6 H 0.4398 0.2082 0.2719 0.045 Uiso 1 1 calc R . . C4A C 0.4961(9) 0.2745(4) 0.2102(3) 0.0311(16) Uani 1 1 d . . . H13 H 0.5334 0.3211 0.2276 0.037 Uiso 1 1 calc R . . C5A C 0.4958(8) 0.2736(4) 0.1588(2) 0.0255(15) Uani 1 1 d . . . C6A C 0.5551(8) 0.3401(4) 0.1280(3) 0.0259(15) Uani 1 1 d . . . C7A C 0.6132(9) 0.4156(4) 0.1429(3) 0.0353(18) Uani 1 1 d . . . H1 H 0.6163 0.4301 0.1770 0.042 Uiso 1 1 calc R . . C8A C 0.6665(9) 0.4686(4) 0.1060(3) 0.0387(19) Uani 1 1 d . . . H12 H 0.7078 0.5201 0.1154 0.046 Uiso 1 1 calc R . . C9A C 0.6617(9) 0.4492(4) 0.0561(3) 0.0352(18) Uani 1 1 d . . . H11 H 0.7015 0.4861 0.0316 0.042 Uiso 1 1 calc R . . C10A C 0.5977(9) 0.3749(4) 0.0427(3) 0.0275(16) Uani 1 1 d . . . C11A C 0.5761(9) 0.3415(4) -0.0077(3) 0.0300(16) Uani 1 1 d . . . C12A C 0.6213(10) 0.3810(4) -0.0502(3) 0.0357(18) Uani 1 1 d . . . H12B H 0.6754 0.4326 -0.0488 0.043 Uiso 1 1 calc R . . C13A C 0.5865(10) 0.3440(5) -0.0961(3) 0.045(2) Uani 1 1 d . . . H13B H 0.6154 0.3707 -0.1262 0.053 Uiso 1 1 calc R . . C14A C 0.5103(10) 0.2689(5) -0.0974(3) 0.0413(19) Uani 1 1 d . . . H14B H 0.4828 0.2437 -0.1282 0.050 Uiso 1 1 calc R . . C15A C 0.4749(9) 0.2310(4) -0.0530(3) 0.0312(16) Uani 1 1 d . . . H15A H 0.4270 0.1784 -0.0538 0.037 Uiso 1 1 calc R . . Pt2 Pt 1.02916(3) 0.287816(15) 0.068226(10) 0.02254(8) Uani 1 1 d . . . Cl2 Cl 1.1185(2) 0.39925(9) 0.02451(7) 0.0312(4) Uani 1 1 d . . . N1B N 0.9719(7) 0.2150(3) 0.0103(2) 0.0265(12) Uani 1 1 d . . . N2B N 0.9480(7) 0.1956(3) 0.10476(19) 0.0225(12) Uani 1 1 d . . . N3B N 1.0516(7) 0.3320(3) 0.1382(2) 0.0259(12) Uani 1 1 d . . . C1B C 0.9903(9) 0.2304(4) -0.0383(3) 0.0317(16) Uani 1 1 d . . . H14 H 1.0373 0.2805 -0.0486 0.038 Uiso 1 1 calc R . . C2B C 0.9420(9) 0.1744(4) -0.0740(3) 0.0352(17) Uani 1 1 d . . . H3 H 0.9556 0.1863 -0.1083 0.042 Uiso 1 1 calc R . . C3B C 0.8738(10) 0.1008(4) -0.0594(3) 0.0375(18) Uani 1 1 d . . . H8 H 0.8423 0.0617 -0.0836 0.045 Uiso 1 1 calc R . . C4B C 0.8521(9) 0.0850(4) -0.0088(3) 0.0301(16) Uani 1 1 d . . . H5 H 0.8010 0.0357 0.0018 0.036 Uiso 1 1 calc R . . C5B C 0.9049(8) 0.1408(4) 0.0251(2) 0.0255(14) Uani 1 1 d . . . C6B C 0.8909(8) 0.1314(4) 0.0793(2) 0.0231(14) Uani 1 1 d . . . C7B C 0.8314(9) 0.0648(4) 0.1051(3) 0.0300(16) Uani 1 1 d . . . H4 H 0.7917 0.0185 0.0878 0.036 Uiso 1 1 calc R . . C8B C 0.8307(9) 0.0669(4) 0.1571(3) 0.0349(17) Uani 1 1 d . . . H10 H 0.7919 0.0213 0.1751 0.042 Uiso 1 1 calc R . . C9B C 0.8858(9) 0.1345(4) 0.1828(3) 0.0346(17) Uani 1 1 d . . . H7 H 0.8842 0.1356 0.2181 0.042 Uiso 1 1 calc R . . C10B C 0.9433(8) 0.2006(4) 0.1559(2) 0.0253(15) Uani 1 1 d . . . C11B C 0.9983(8) 0.2795(4) 0.1740(3) 0.0276(15) Uani 1 1 d . . . C12B C 0.9977(10) 0.3001(4) 0.2236(3) 0.0378(18) Uani 1 1 d . . . H12A H 0.9606 0.2628 0.2482 0.045 Uiso 1 1 calc R . . C13B C 1.0522(10) 0.3762(4) 0.2370(3) 0.0405(19) Uani 1 1 d . . . H13A H 1.0517 0.3919 0.2709 0.049 Uiso 1 1 calc R . . C14B C 1.1069(10) 0.4285(5) 0.2008(3) 0.0417(19) Uani 1 1 d . . . H14A H 1.1463 0.4804 0.2097 0.050 Uiso 1 1 calc R . . C15B C 1.1051(9) 0.4060(4) 0.1509(3) 0.0345(17) Uani 1 1 d . . . H15B H 1.1414 0.4428 0.1260 0.041 Uiso 1 1 calc R . . Cl3 Cl 0.0481(3) 0.14041(11) 0.33255(7) 0.0414(4) Uani 1 1 d . . . O1 O 0.1134(9) 0.2210(3) 0.3320(2) 0.0641(17) Uani 1 1 d . . . O2 O 0.0158(8) 0.1152(3) 0.38256(18) 0.0570(16) Uani 1 1 d . . . O3 O 0.1895(8) 0.0909(3) 0.3101(2) 0.0604(16) Uani 1 1 d . . . O4 O -0.1281(8) 0.1351(3) 0.30492(19) 0.0530(15) Uani 1 1 d . . . Cl4 Cl 0.6101(3) 0.41892(10) 0.31824(7) 0.0377(4) Uani 1 1 d . . . O5 O 0.6723(7) 0.3379(3) 0.31152(18) 0.0448(13) Uani 1 1 d . . . O6 O 0.7750(7) 0.4677(3) 0.3273(2) 0.0467(14) Uani 1 1 d . . . O7 O 0.4862(8) 0.4232(3) 0.3604(2) 0.0577(16) Uani 1 1 d . . . O8 O 0.5102(8) 0.4456(3) 0.2744(2) 0.0549(16) 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 0.01760(14) 0.01953(13) 0.02685(15) -0.00001(12) 0.00072(11) 0.00034(11) Cl1 0.0283(9) 0.0201(8) 0.0362(10) -0.0057(7) -0.0010(7) -0.0023(6) N1A 0.020(3) 0.020(3) 0.025(3) -0.003(2) -0.002(2) 0.000(2) N2A 0.019(3) 0.016(3) 0.027(3) 0.001(2) 0.003(2) 0.007(2) N3A 0.019(3) 0.025(3) 0.030(3) 0.004(2) 0.002(2) 0.005(2) C1A 0.022(3) 0.028(4) 0.032(4) -0.005(3) 0.003(3) -0.002(3) C2A 0.036(4) 0.037(4) 0.028(4) 0.006(3) 0.006(3) 0.004(3) C3A 0.041(4) 0.050(5) 0.021(4) 0.004(4) 0.001(3) 0.008(4) C4A 0.027(4) 0.027(4) 0.039(4) -0.004(3) 0.002(3) 0.000(3) C5A 0.017(3) 0.029(4) 0.030(4) 0.001(3) -0.006(3) 0.000(3) C6A 0.018(3) 0.023(3) 0.037(4) -0.006(3) -0.004(3) 0.005(3) C7A 0.027(4) 0.025(4) 0.053(5) -0.012(3) -0.007(3) 0.000(3) C8A 0.026(4) 0.023(4) 0.068(6) -0.009(4) -0.004(4) -0.002(3) C9A 0.025(4) 0.020(4) 0.061(6) 0.002(3) 0.006(3) 0.001(3) C10A 0.018(3) 0.021(3) 0.043(4) 0.007(3) 0.002(3) 0.005(3) C11A 0.026(4) 0.025(4) 0.039(4) 0.010(3) 0.011(3) 0.010(3) C12A 0.034(4) 0.033(4) 0.040(5) 0.008(3) 0.014(3) 0.006(3) C13A 0.040(5) 0.050(5) 0.043(5) 0.016(4) 0.009(4) 0.014(4) C14A 0.035(4) 0.060(6) 0.029(4) 0.001(4) 0.006(3) 0.014(4) C15A 0.032(4) 0.032(4) 0.030(4) 0.006(3) 0.001(3) 0.007(3) Pt2 0.01707(14) 0.02148(14) 0.02908(16) 0.00227(12) 0.00028(11) 0.00043(11) Cl2 0.0256(9) 0.0249(8) 0.0430(10) 0.0095(7) 0.0049(7) -0.0005(7) N1B 0.022(3) 0.028(3) 0.029(3) 0.008(3) -0.001(2) 0.004(2) N2B 0.015(3) 0.027(3) 0.025(3) 0.004(2) -0.001(2) 0.000(2) N3B 0.019(3) 0.025(3) 0.034(3) -0.001(3) 0.003(2) 0.000(2) C1B 0.027(4) 0.035(4) 0.033(4) 0.002(3) 0.000(3) 0.002(3) C2B 0.032(4) 0.049(5) 0.024(4) -0.001(3) -0.008(3) 0.007(3) C3B 0.034(4) 0.044(5) 0.034(4) -0.012(4) -0.004(3) 0.005(3) C4B 0.021(4) 0.032(4) 0.038(4) -0.002(3) -0.005(3) 0.003(3) C5B 0.018(3) 0.026(3) 0.032(4) 0.002(3) -0.001(3) -0.001(3) C6B 0.013(3) 0.023(3) 0.033(4) 0.000(3) -0.001(3) 0.008(3) C7B 0.027(4) 0.021(3) 0.042(4) 0.008(3) -0.002(3) 0.000(3) C8B 0.029(4) 0.034(4) 0.042(5) 0.013(3) -0.001(3) 0.002(3) C9B 0.033(4) 0.037(4) 0.034(4) 0.006(3) 0.000(3) 0.003(3) C10B 0.013(3) 0.030(4) 0.033(4) 0.001(3) 0.001(3) 0.004(3) C11B 0.016(3) 0.031(4) 0.035(4) -0.007(3) -0.001(3) -0.001(3) C12B 0.037(4) 0.040(4) 0.037(4) 0.000(4) -0.006(3) -0.002(3) C13B 0.036(4) 0.049(5) 0.037(5) -0.018(4) -0.002(4) 0.002(4) C14B 0.038(4) 0.038(4) 0.049(5) -0.012(4) -0.004(4) -0.003(3) C15B 0.025(4) 0.032(4) 0.046(5) -0.003(3) -0.007(3) 0.003(3) Cl3 0.0506(12) 0.0426(11) 0.0312(10) 0.0028(8) 0.0053(9) 0.0108(9) O1 0.077(4) 0.049(4) 0.065(4) -0.002(3) -0.009(3) -0.003(3) O2 0.067(4) 0.078(4) 0.026(3) 0.010(3) 0.008(3) 0.025(3) O3 0.070(4) 0.062(4) 0.049(4) 0.009(3) 0.028(3) 0.021(3) O4 0.054(4) 0.066(4) 0.039(3) 0.006(3) -0.003(3) -0.002(3) Cl4 0.0474(11) 0.0318(9) 0.0339(10) -0.0038(8) -0.0034(9) 0.0054(8) O5 0.061(3) 0.030(3) 0.043(3) -0.005(2) 0.000(3) 0.015(2) O6 0.044(3) 0.042(3) 0.054(4) -0.007(3) -0.016(3) -0.001(3) O7 0.054(4) 0.068(4) 0.051(4) -0.005(3) 0.016(3) 0.015(3) O8 0.079(4) 0.036(3) 0.049(4) -0.005(3) -0.035(3) 0.008(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 N2A 1.937(5) . ? Pt1 N1A 2.015(5) . ? Pt1 N3A 2.020(5) . ? Pt1 Cl1 2.3013(15) . ? N1A C1A 1.331(7) . ? N1A C5A 1.380(7) . ? N2A C10A 1.348(8) . ? N2A C6A 1.356(8) . ? N3A C15A 1.324(8) . ? N3A C11A 1.386(8) . ? C1A C2A 1.380(9) . ? C1A H2 0.9500 . ? C2A C3A 1.381(9) . ? C2A H9 0.9500 . ? C3A C4A 1.385(9) . ? C3A H6 0.9500 . ? C4A C5A 1.383(9) . ? C4A H13 0.9500 . ? C5A C6A 1.458(9) . ? C6A C7A 1.395(9) . ? C7A C8A 1.389(10) . ? C7A H1 0.9500 . ? C8A C9A 1.383(10) . ? C8A H12 0.9500 . ? C9A C10A 1.378(8) . ? C9A H11 0.9500 . ? C10A C11A 1.474(9) . ? C11A C12A 1.365(9) . ? C12A C13A 1.405(10) . ? C12A H12B 0.9500 . ? C13A C14A 1.376(10) . ? C13A H13B 0.9500 . ? C14A C15A 1.379(9) . ? C14A H14B 0.9500 . ? C15A H15A 0.9500 . ? Pt2 N2B 1.928(5) . ? Pt2 N1B 2.022(5) . ? Pt2 N3B 2.029(5) . ? Pt2 Cl2 2.3071(15) . ? N1B C1B 1.342(8) . ? N1B C5B 1.396(8) . ? N2B C6B 1.343(7) . ? N2B C10B 1.378(8) . ? N3B C15B 1.349(8) . ? N3B C11B 1.362(8) . ? C1B C2B 1.387(9) . ? C1B H14 0.9500 . ? C2B C3B 1.389(10) . ? C2B H3 0.9500 . ? C3B C4B 1.396(9) . ? C3B H8 0.9500 . ? C4B C5B 1.362(9) . ? C4B H5 0.9500 . ? C5B C6B 1.470(9) . ? C6B C7B 1.388(8) . ? C7B C8B 1.399(9) . ? C7B H4 0.9500 . ? C8B C9B 1.387(9) . ? C8B H10 0.9500 . ? C9B C10B 1.391(9) . ? C9B H7 0.9500 . ? C10B C11B 1.469(9) . ? C11B C12B 1.380(9) . ? C12B C13B 1.388(9) . ? C12B H12A 0.9500 . ? C13B C14B 1.372(10) . ? C13B H13A 0.9500 . ? C14B C15B 1.393(10) . ? C14B H14A 0.9500 . ? C15B H15B 0.9500 . ? Cl3 O2 1.430(5) . ? Cl3 O3 1.434(5) . ? Cl3 O1 1.436(6) . ? Cl3 O4 1.442(5) . ? Cl4 O7 1.435(5) . ? Cl4 O6 1.440(5) . ? Cl4 O8 1.441(5) . ? Cl4 O5 1.448(5) . ? 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 N2A Pt1 N1A 81.5(2) . . ? N2A Pt1 N3A 81.4(2) . . ? N1A Pt1 N3A 162.9(2) . . ? N2A Pt1 Cl1 177.56(14) . . ? N1A Pt1 Cl1 98.43(14) . . ? N3A Pt1 Cl1 98.61(16) . . ? C1A N1A C5A 119.2(5) . . ? C1A N1A Pt1 128.4(4) . . ? C5A N1A Pt1 112.5(4) . . ? C10A N2A C6A 124.2(5) . . ? C10A N2A Pt1 118.2(4) . . ? C6A N2A Pt1 117.6(4) . . ? C15A N3A C11A 119.1(6) . . ? C15A N3A Pt1 128.3(4) . . ? C11A N3A Pt1 112.6(4) . . ? N1A C1A C2A 122.2(6) . . ? N1A C1A H2 118.9 . . ? C2A C1A H2 118.9 . . ? C1A C2A C3A 119.8(6) . . ? C1A C2A H9 120.1 . . ? C3A C2A H9 120.1 . . ? C2A C3A C4A 118.3(6) . . ? C2A C3A H6 120.8 . . ? C4A C3A H6 120.8 . . ? C5A C4A C3A 120.3(6) . . ? C5A C4A H13 119.9 . . ? C3A C4A H13 119.9 . . ? N1A C5A C4A 120.2(6) . . ? N1A C5A C6A 115.6(6) . . ? C4A C5A C6A 124.2(6) . . ? N2A C6A C7A 118.5(6) . . ? N2A C6A C5A 112.9(5) . . ? C7A C6A C5A 128.6(7) . . ? C8A C7A C6A 117.6(7) . . ? C8A C7A H1 121.2 . . ? C6A C7A H1 121.2 . . ? C9A C8A C7A 122.3(6) . . ? C9A C8A H12 118.8 . . ? C7A C8A H12 118.8 . . ? C10A C9A C8A 118.4(7) . . ? C10A C9A H11 120.8 . . ? C8A C9A H11 120.8 . . ? N2A C10A C9A 118.9(7) . . ? N2A C10A C11A 112.8(6) . . ? C9A C10A C11A 128.3(6) . . ? C12A C11A N3A 121.0(7) . . ? C12A C11A C10A 124.1(6) . . ? N3A C11A C10A 114.9(6) . . ? C11A C12A C13A 118.7(7) . . ? C11A C12A H12B 120.7 . . ? C13A C12A H12B 120.7 . . ? C14A C13A C12A 119.9(7) . . ? C14A C13A H13B 120.1 . . ? C12A C13A H13B 120.1 . . ? C13A C14A C15A 118.5(7) . . ? C13A C14A H14B 120.7 . . ? C15A C14A H14B 120.7 . . ? N3A C15A C14A 122.7(7) . . ? N3A C15A H15A 118.6 . . ? C14A C15A H15A 118.6 . . ? N2B Pt2 N1B 81.0(2) . . ? N2B Pt2 N3B 81.1(2) . . ? N1B Pt2 N3B 162.0(2) . . ? N2B Pt2 Cl2 178.56(14) . . ? N1B Pt2 Cl2 98.99(15) . . ? N3B Pt2 Cl2 98.83(15) . . ? C1B N1B C5B 119.1(6) . . ? C1B N1B Pt2 127.9(5) . . ? C5B N1B Pt2 113.1(4) . . ? C6B N2B C10B 123.3(5) . . ? C6B N2B Pt2 118.7(4) . . ? C10B N2B Pt2 118.0(4) . . ? C15B N3B C11B 120.1(6) . . ? C15B N3B Pt2 126.5(5) . . ? C11B N3B Pt2 113.3(4) . . ? N1B C1B C2B 121.2(7) . . ? N1B C1B H14 119.4 . . ? C2B C1B H14 119.4 . . ? C1B C2B C3B 119.9(7) . . ? C1B C2B H3 120.0 . . ? C3B C2B H3 120.0 . . ? C2B C3B C4B 119.0(7) . . ? C2B C3B H8 120.5 . . ? C4B C3B H8 120.5 . . ? C5B C4B C3B 119.3(7) . . ? C5B C4B H5 120.3 . . ? C3B C4B H5 120.3 . . ? C4B C5B N1B 121.4(6) . . ? C4B C5B C6B 124.7(6) . . ? N1B C5B C6B 113.8(5) . . ? N2B C6B C7B 119.2(6) . . ? N2B C6B C5B 113.4(5) . . ? C7B C6B C5B 127.4(6) . . ? C6B C7B C8B 118.9(6) . . ? C6B C7B H4 120.6 . . ? C8B C7B H4 120.6 . . ? C9B C8B C7B 121.1(6) . . ? C9B C8B H10 119.5 . . ? C7B C8B H10 119.5 . . ? C8B C9B C10B 118.8(7) . . ? C8B C9B H7 120.6 . . ? C10B C9B H7 120.6 . . ? N2B C10B C9B 118.6(6) . . ? N2B C10B C11B 112.2(5) . . ? C9B C10B C11B 129.2(6) . . ? N3B C11B C12B 121.5(6) . . ? N3B C11B C10B 115.4(6) . . ? C12B C11B C10B 123.2(6) . . ? C11B C12B C13B 118.8(7) . . ? C11B C12B H12A 120.6 . . ? C13B C12B H12A 120.6 . . ? C14B C13B C12B 119.3(7) . . ? C14B C13B H13A 120.4 . . ? C12B C13B H13A 120.4 . . ? C13B C14B C15B 120.5(7) . . ? C13B C14B H14A 119.7 . . ? C15B C14B H14A 119.7 . . ? N3B C15B C14B 119.8(7) . . ? N3B C15B H15B 120.1 . . ? C14B C15B H15B 120.1 . . ? O2 Cl3 O3 109.7(3) . . ? O2 Cl3 O1 110.1(4) . . ? O3 Cl3 O1 109.0(4) . . ? O2 Cl3 O4 109.1(3) . . ? O3 Cl3 O4 109.9(4) . . ? O1 Cl3 O4 109.0(3) . . ? O7 Cl4 O6 109.1(3) . . ? O7 Cl4 O8 109.7(4) . . ? O6 Cl4 O8 110.3(3) . . ? O7 Cl4 O5 109.3(3) . . ? O6 Cl4 O5 108.6(3) . . ? O8 Cl4 O5 109.8(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 N2A Pt1 N1A C1A -179.9(5) . . . . ? N3A Pt1 N1A C1A -176.6(6) . . . . ? Cl1 Pt1 N1A C1A -2.4(5) . . . . ? N2A Pt1 N1A C5A 1.4(4) . . . . ? N3A Pt1 N1A C5A 4.7(9) . . . . ? Cl1 Pt1 N1A C5A 178.9(4) . . . . ? N1A Pt1 N2A C10A 176.9(4) . . . . ? N3A Pt1 N2A C10A -2.2(4) . . . . ? Cl1 Pt1 N2A C10A 89(4) . . . . ? N1A Pt1 N2A C6A -0.3(4) . . . . ? N3A Pt1 N2A C6A -179.4(4) . . . . ? Cl1 Pt1 N2A C6A -89(4) . . . . ? N2A Pt1 N3A C15A -177.7(5) . . . . ? N1A Pt1 N3A C15A 179.0(6) . . . . ? Cl1 Pt1 N3A C15A 4.7(5) . . . . ? N2A Pt1 N3A C11A 2.3(4) . . . . ? N1A Pt1 N3A C11A -1.0(9) . . . . ? Cl1 Pt1 N3A C11A -175.2(4) . . . . ? C5A N1A C1A C2A -2.2(9) . . . . ? Pt1 N1A C1A C2A 179.2(4) . . . . ? N1A C1A C2A C3A 2.0(10) . . . . ? C1A C2A C3A C4A -1.4(10) . . . . ? C2A C3A C4A C5A 1.1(10) . . . . ? C1A N1A C5A C4A 1.8(8) . . . . ? Pt1 N1A C5A C4A -179.3(5) . . . . ? C1A N1A C5A C6A 179.0(5) . . . . ? Pt1 N1A C5A C6A -2.1(6) . . . . ? C3A C4A C5A N1A -1.3(9) . . . . ? C3A C4A C5A C6A -178.3(6) . . . . ? C10A N2A C6A C7A 4.0(9) . . . . ? Pt1 N2A C6A C7A -179.0(4) . . . . ? C10A N2A C6A C5A -177.7(5) . . . . ? Pt1 N2A C6A C5A -0.7(6) . . . . ? N1A C5A C6A N2A 1.9(7) . . . . ? C4A C5A C6A N2A 178.9(6) . . . . ? N1A C5A C6A C7A -180.0(6) . . . . ? C4A C5A C6A C7A -2.9(10) . . . . ? N2A C6A C7A C8A -3.2(9) . . . . ? C5A C6A C7A C8A 178.8(6) . . . . ? C6A C7A C8A C9A 0.6(10) . . . . ? C7A C8A C9A C10A 1.4(10) . . . . ? C6A N2A C10A C9A -1.9(9) . . . . ? Pt1 N2A C10A C9A -178.9(4) . . . . ? C6A N2A C10A C11A 178.5(5) . . . . ? Pt1 N2A C10A C11A 1.5(7) . . . . ? C8A C9A C10A N2A -0.8(9) . . . . ? C8A C9A C10A C11A 178.6(6) . . . . ? C15A N3A C11A C12A -2.1(9) . . . . ? Pt1 N3A C11A C12A 177.8(5) . . . . ? C15A N3A C11A C10A 177.9(5) . . . . ? Pt1 N3A C11A C10A -2.2(6) . . . . ? N2A C10A C11A C12A -179.5(6) . . . . ? C9A C10A C11A C12A 1.0(10) . . . . ? N2A C10A C11A N3A 0.5(7) . . . . ? C9A C10A C11A N3A -179.0(6) . . . . ? N3A C11A C12A C13A 2.8(10) . . . . ? C10A C11A C12A C13A -177.3(6) . . . . ? C11A C12A C13A C14A -0.8(10) . . . . ? C12A C13A C14A C15A -1.7(10) . . . . ? C11A N3A C15A C14A -0.5(9) . . . . ? Pt1 N3A C15A C14A 179.5(5) . . . . ? C13A C14A C15A N3A 2.4(10) . . . . ? N2B Pt2 N1B C1B -179.4(5) . . . . ? N3B Pt2 N1B C1B 174.8(6) . . . . ? Cl2 Pt2 N1B C1B 2.0(5) . . . . ? N2B Pt2 N1B C5B 0.8(4) . . . . ? N3B Pt2 N1B C5B -4.9(9) . . . . ? Cl2 Pt2 N1B C5B -177.7(4) . . . . ? N1B Pt2 N2B C6B -1.5(4) . . . . ? N3B Pt2 N2B C6B 176.7(5) . . . . ? Cl2 Pt2 N2B C6B 90(6) . . . . ? N1B Pt2 N2B C10B -178.5(4) . . . . ? N3B Pt2 N2B C10B -0.3(4) . . . . ? Cl2 Pt2 N2B C10B -87(6) . . . . ? N2B Pt2 N3B C15B -178.7(5) . . . . ? N1B Pt2 N3B C15B -172.9(6) . . . . ? Cl2 Pt2 N3B C15B -0.1(5) . . . . ? N2B Pt2 N3B C11B -1.3(4) . . . . ? N1B Pt2 N3B C11B 4.5(9) . . . . ? Cl2 Pt2 N3B C11B 177.2(4) . . . . ? C5B N1B C1B C2B 0.7(9) . . . . ? Pt2 N1B C1B C2B -179.0(5) . . . . ? N1B C1B C2B C3B -0.2(10) . . . . ? C1B C2B C3B C4B 1.0(10) . . . . ? C2B C3B C4B C5B -2.4(10) . . . . ? C3B C4B C5B N1B 3.0(9) . . . . ? C3B C4B C5B C6B -179.5(6) . . . . ? C1B N1B C5B C4B -2.2(9) . . . . ? Pt2 N1B C5B C4B 177.5(5) . . . . ? C1B N1B C5B C6B -179.9(5) . . . . ? Pt2 N1B C5B C6B -0.2(6) . . . . ? C10B N2B C6B C7B -2.9(8) . . . . ? Pt2 N2B C6B C7B -179.7(4) . . . . ? C10B N2B C6B C5B 178.6(5) . . . . ? Pt2 N2B C6B C5B 1.7(6) . . . . ? C4B C5B C6B N2B -178.6(6) . . . . ? N1B C5B C6B N2B -0.9(7) . . . . ? C4B C5B C6B C7B 3.0(10) . . . . ? N1B C5B C6B C7B -179.3(6) . . . . ? N2B C6B C7B C8B 0.7(9) . . . . ? C5B C6B C7B C8B 179.0(6) . . . . ? C6B C7B C8B C9B 0.9(9) . . . . ? C7B C8B C9B C10B -0.4(10) . . . . ? C6B N2B C10B C9B 3.4(8) . . . . ? Pt2 N2B C10B C9B -179.8(4) . . . . ? C6B N2B C10B C11B -175.2(5) . . . . ? Pt2 N2B C10B C11B 1.7(6) . . . . ? C8B C9B C10B N2B -1.6(9) . . . . ? C8B C9B C10B C11B 176.6(6) . . . . ? C15B N3B C11B C12B -0.1(9) . . . . ? Pt2 N3B C11B C12B -177.7(5) . . . . ? C15B N3B C11B C10B -179.9(5) . . . . ? Pt2 N3B C11B C10B 2.6(7) . . . . ? N2B C10B C11B N3B -2.8(7) . . . . ? C9B C10B C11B N3B 178.9(6) . . . . ? N2B C10B C11B C12B 177.5(6) . . . . ? C9B C10B C11B C12B -0.9(10) . . . . ? N3B C11B C12B C13B 0.2(10) . . . . ? C10B C11B C12B C13B 180.0(6) . . . . ? C11B C12B C13B C14B -0.6(10) . . . . ? C12B C13B C14B C15B 1.0(11) . . . . ? C11B N3B C15B C14B 0.4(9) . . . . ? Pt2 N3B C15B C14B 177.6(5) . . . . ? C13B C14B C15B N3B -0.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.67 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.789 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.150 _iucr_refine_instructions_details ; TITL 2 in P2(1)/c CELL 0.88560 7.0189 16.8805 26.8979 90.000 90.336 90.000 ZERR 8.00 0.0003 0.0008 0.0013 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Cl Pt DISP C -0.00203 0.00267 18.57 DISP H 0.00000 0.00000 0.67 DISP N -0.00309 0.00541 33.78 DISP O -0.00423 0.00986 57.86 DISP Cl 0.16873 0.24621 1264.58 DISP Pt -6.92097 11.89369 60478.44 UNIT 120 88 24 32 16 8 TEMP -123.000 omit 0 0 2 omit 0 1 2 omit 0 1 1 L.S. 5 acta size 0.04 0.005 0.005 rem orange needle, als, apex2 bond $h conf mpla 6 n1a c1a c2a c3a c4a c5a mpla 6 n2a c6a c7a c8a c9a c10a mpla 6 n2a c6a c7a c8a c9a c10a mpla 6 n3a C11a C12a C13a C14a C15a mpla 6 n1b c1b c2b c3b c4b c5b mpla 6 n2b c6b c7b c8b c9b c10b mpla 6 n2b c6b c7b c8b c9b c10b mpla 6 n3b C11b C12b C13b C14b C15b FMAP 2 PLAN 5 WGHT 0.000100 0.967700 FVAR 0.03765 PT1 6 0.459659 0.219395 0.059104 11.00000 0.01760 0.01953 = 0.02685 -0.00001 0.00072 0.00034 CL1 5 0.371762 0.093244 0.036035 11.00000 0.02831 0.02008 = 0.03615 -0.00565 -0.00101 -0.00228 N1A 3 0.445616 0.205693 0.133416 11.00000 0.02011 0.01955 = 0.02505 -0.00325 -0.00197 0.00033 N2A 3 0.544795 0.324058 0.078678 11.00000 0.01865 0.01617 = 0.02707 0.00095 0.00294 0.00723 N3A 3 0.504739 0.264922 -0.009275 11.00000 0.01885 0.02547 = 0.02993 0.00400 0.00174 0.00548 C1A 1 0.392568 0.141991 0.158976 11.00000 0.02165 0.02799 = 0.03245 -0.00466 0.00334 -0.00192 AFIX 43 H2 2 0.353772 0.095929 0.141330 11.00000 -1.20000 AFIX 0 C2A 1 0.392056 0.140636 0.210288 11.00000 0.03550 0.03673 = 0.02772 0.00629 0.00565 0.00385 AFIX 43 H9 2 0.357294 0.093658 0.227437 11.00000 -1.20000 AFIX 0 C3A 1 0.442224 0.207772 0.236615 11.00000 0.04082 0.05008 = 0.02095 0.00404 0.00144 0.00755 AFIX 43 H6 2 0.439844 0.208169 0.271924 11.00000 -1.20000 AFIX 0 C4A 1 0.496104 0.274521 0.210249 11.00000 0.02746 0.02692 = 0.03896 -0.00377 0.00206 -0.00036 AFIX 43 H13 2 0.533398 0.321115 0.227560 11.00000 -1.20000 AFIX 0 C5A 1 0.495848 0.273634 0.158825 11.00000 0.01701 0.02902 = 0.03038 0.00106 -0.00620 0.00003 C6A 1 0.555052 0.340146 0.128002 11.00000 0.01784 0.02270 = 0.03709 -0.00617 -0.00373 0.00477 C7A 1 0.613230 0.415561 0.142868 11.00000 0.02746 0.02495 = 0.05344 -0.01221 -0.00694 0.00009 AFIX 43 H1 2 0.616301 0.430110 0.176982 11.00000 -1.20000 AFIX 0 C8A 1 0.666527 0.468645 0.106012 11.00000 0.02573 0.02256 = 0.06776 -0.00947 -0.00402 -0.00210 AFIX 43 H12 2 0.707758 0.520129 0.115439 11.00000 -1.20000 AFIX 0 C9A 1 0.661663 0.449162 0.056070 11.00000 0.02458 0.01972 = 0.06130 0.00186 0.00562 0.00070 AFIX 43 H11 2 0.701464 0.486069 0.031574 11.00000 -1.20000 AFIX 0 C10A 1 0.597697 0.374933 0.042701 11.00000 0.01844 0.02121 = 0.04295 0.00654 0.00214 0.00537 C11A 1 0.576083 0.341471 -0.007652 11.00000 0.02606 0.02532 = 0.03885 0.01037 0.01068 0.00968 C12A 1 0.621348 0.381022 -0.050222 11.00000 0.03421 0.03349 = 0.03971 0.00827 0.01393 0.00644 AFIX 43 H12B 2 0.675353 0.432584 -0.048832 11.00000 -1.20000 AFIX 0 C13A 1 0.586488 0.343963 -0.096140 11.00000 0.03999 0.05038 = 0.04331 0.01591 0.00911 0.01366 AFIX 43 H13B 2 0.615414 0.370684 -0.126249 11.00000 -1.20000 AFIX 0 C14A 1 0.510339 0.268863 -0.097412 11.00000 0.03544 0.05952 = 0.02910 0.00121 0.00646 0.01362 AFIX 43 H14B 2 0.482829 0.243671 -0.128210 11.00000 -1.20000 AFIX 0 C15A 1 0.474853 0.230989 -0.053016 11.00000 0.03151 0.03202 = 0.02995 0.00572 0.00117 0.00659 AFIX 43 H15A 2 0.426973 0.178363 -0.053835 11.00000 -1.20000 AFIX 0 PT2 6 1.029162 0.287816 0.068226 11.00000 0.01707 0.02148 = 0.02908 0.00227 0.00028 0.00043 CL2 5 1.118490 0.399247 0.024508 11.00000 0.02560 0.02494 = 0.04300 0.00947 0.00494 -0.00053 N1B 3 0.971894 0.215012 0.010322 11.00000 0.02221 0.02780 = 0.02938 0.00791 -0.00096 0.00354 N2B 3 0.948015 0.195647 0.104765 11.00000 0.01490 0.02737 = 0.02510 0.00411 -0.00106 0.00028 N3B 3 1.051622 0.331953 0.138198 11.00000 0.01890 0.02484 = 0.03389 -0.00112 0.00330 0.00040 C1B 1 0.990328 0.230391 -0.038348 11.00000 0.02692 0.03520 = 0.03308 0.00215 -0.00003 0.00183 AFIX 43 H14 2 1.037291 0.280546 -0.048596 11.00000 -1.20000 AFIX 0 C2B 1 0.942037 0.174364 -0.073961 11.00000 0.03228 0.04918 = 0.02417 -0.00130 -0.00821 0.00725 AFIX 43 H3 2 0.955640 0.186326 -0.108269 11.00000 -1.20000 AFIX 0 C3B 1 0.873783 0.100766 -0.059427 11.00000 0.03400 0.04416 = 0.03415 -0.01229 -0.00421 0.00455 AFIX 43 H8 2 0.842309 0.061742 -0.083562 11.00000 -1.20000 AFIX 0 C4B 1 0.852090 0.084954 -0.008847 11.00000 0.02072 0.03168 = 0.03795 -0.00177 -0.00511 0.00323 AFIX 43 H5 2 0.801038 0.035721 0.001811 11.00000 -1.20000 AFIX 0 C5B 1 0.904860 0.140833 0.025093 11.00000 0.01814 0.02637 = 0.03210 0.00201 -0.00091 -0.00059 C6B 1 0.890907 0.131389 0.079265 11.00000 0.01338 0.02270 = 0.03332 -0.00012 -0.00141 0.00812 C7B 1 0.831375 0.064772 0.105127 11.00000 0.02682 0.02103 = 0.04217 0.00759 -0.00249 -0.00028 AFIX 43 H4 2 0.791748 0.018509 0.087817 11.00000 -1.20000 AFIX 0 C8B 1 0.830719 0.066916 0.157112 11.00000 0.02871 0.03375 = 0.04230 0.01278 -0.00119 0.00152 AFIX 43 H10 2 0.791950 0.021346 0.175141 11.00000 -1.20000 AFIX 0 C9B 1 0.885764 0.134508 0.182759 11.00000 0.03276 0.03670 = 0.03438 0.00615 0.00035 0.00334 AFIX 43 H7 2 0.884185 0.135644 0.218066 11.00000 -1.20000 AFIX 0 C10B 1 0.943304 0.200579 0.155867 11.00000 0.01346 0.02968 = 0.03280 0.00100 0.00111 0.00433 C11B 1 0.998285 0.279460 0.173964 11.00000 0.01616 0.03142 = 0.03516 -0.00683 -0.00123 -0.00083 C12B 1 0.997695 0.300057 0.223624 11.00000 0.03667 0.03967 = 0.03707 -0.00014 -0.00565 -0.00186 AFIX 43 H12A 2 0.960607 0.262783 0.248196 11.00000 -1.20000 AFIX 0 C13B 1 1.052237 0.376173 0.237024 11.00000 0.03560 0.04913 = 0.03679 -0.01825 -0.00199 0.00159 AFIX 43 H13A 2 1.051735 0.391892 0.270936 11.00000 -1.20000 AFIX 0 C14B 1 1.106880 0.428467 0.200773 11.00000 0.03764 0.03785 = 0.04944 -0.01222 -0.00394 -0.00253 AFIX 43 H14A 2 1.146259 0.480412 0.209728 11.00000 -1.20000 AFIX 0 C15B 1 1.105101 0.406020 0.150919 11.00000 0.02539 0.03169 = 0.04620 -0.00255 -0.00665 0.00318 AFIX 43 H15B 2 1.141444 0.442769 0.125963 11.00000 -1.20000 AFIX 0 CL3 5 0.048060 0.140411 0.332550 11.00000 0.05062 0.04261 = 0.03116 0.00275 0.00533 0.01081 O1 4 0.113444 0.221013 0.331979 11.00000 0.07740 0.04935 = 0.06548 -0.00236 -0.00946 -0.00293 O2 4 0.015850 0.115214 0.382556 11.00000 0.06689 0.07849 = 0.02563 0.01014 0.00761 0.02537 O3 4 0.189467 0.090886 0.310068 11.00000 0.07035 0.06206 = 0.04903 0.00857 0.02765 0.02078 O4 4 -0.128077 0.135131 0.304917 11.00000 0.05380 0.06609 = 0.03896 0.00584 -0.00270 -0.00219 CL4 5 0.610098 0.418923 0.318237 11.00000 0.04743 0.03184 = 0.03393 -0.00378 -0.00342 0.00543 O5 4 0.672261 0.337850 0.311518 11.00000 0.06127 0.03046 = 0.04264 -0.00462 -0.00007 0.01500 O6 4 0.774977 0.467665 0.327298 11.00000 0.04436 0.04152 = 0.05389 -0.00661 -0.01571 -0.00122 O7 4 0.486225 0.423222 0.360409 11.00000 0.05424 0.06762 = 0.05140 -0.00544 0.01583 0.01487 O8 4 0.510180 0.445557 0.274384 11.00000 0.07855 0.03635 = 0.04929 -0.00492 -0.03457 0.00759 HKLF 4 REM uc11067b in P2(1)/c REM R1 = 0.0332 for 4625 Fo > 4sig(Fo) and 0.0633 for all 6536 data REM 451 parameters refined using 0 restraints END WGHT 0.0001 0.9718 REM Highest difference peak 0.789, deepest hole -0.700, 1-sigma level 0.150 Q1 1 0.9029 0.2845 0.0682 11.00000 0.05 0.79 Q2 1 0.5738 0.3436 0.0587 11.00000 0.05 0.60 Q3 1 1.1301 0.4043 0.0009 11.00000 0.05 0.60 Q4 1 -0.2243 0.1009 0.2888 11.00000 0.05 0.59 Q5 1 1.1973 0.4011 0.0385 11.00000 0.05 0.58 ; #eof data_2 =============================================== #eof ====================================================== _database_code_depnum_ccdc_archive 'CCDC 948314'