Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Miguel Quiros' 'Mohammad Abul Haj' 'Juan M. Salas' _publ_contact_author_name 'Dr Miguel Quiros' _publ_contact_author_address ; Quimica Inorganica Universidad de Granada Facultad de Ciencias Granada 18071 SPAIN ; _publ_contact_author_email 'MQUIROS@UGR.ES' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Coexistence in solution and solid state of head-head and head-tail isomers in dimeric complexes of the type [M2(a-a)2(mu-L-N3,N4)2]2+ with a bridging triazolopyrimidine ligand and chelating bidentate diamines ; data_compound3 _database_code_CSD 190494 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Cl2 N12 O12 Pd2' _chemical_formula_weight 1078.37 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorrombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.468(6) _cell_length_b 20.652(10) _cell_length_c 25.162(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8038(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 63 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 16.0 _exptl_crystal_description 'prismatic' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.317 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4288 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6390 _exptl_absorpt_correction_T_max 0.7230 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 1.05 - 1.20, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7.5 _diffrn_reflns_number 7765 _diffrn_reflns_av_R_equivalents 0.1512 _diffrn_reflns_av_sigmaI/netI 0.2649 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.97 _reflns_number_total 7060 _reflns_number_gt 3251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0600P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7060 _refine_ls_number_parameters 517 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.2782 _refine_ls_R_factor_gt 0.1483 _refine_ls_wR_factor_ref 0.2882 _refine_ls_wR_factor_gt 0.2413 _refine_ls_goodness_of_fit_ref 1.485 _refine_ls_restrained_S_all 1.485 _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 Pd1 Pd 0.51892(9) 0.69469(8) 0.31661(6) 0.0447(5) Uani 1 1 d . . . Pd2 Pd 0.46011(9) 0.69137(8) 0.42962(6) 0.0482(5) Uani 1 1 d . . . N1A N 0.6377(11) 0.8770(9) 0.3420(10) 0.079(7) Uani 1 1 d . . . C2A C 0.6075(13) 0.8276(11) 0.3132(10) 0.062(6) Uani 1 1 d . . . H2A H 0.6123 0.8264 0.2764 0.074 Uiso 1 1 d R . . N3A N 0.5684(9) 0.7772(7) 0.3413(6) 0.045(4) Uani 1 1 d . . . C3AA C 0.5749(12) 0.7952(10) 0.3921(9) 0.046(5) Uani 1 1 d . . . N4A N 0.5429(11) 0.7664(8) 0.4351(7) 0.058(5) Uani 1 1 d . . . C5A C 0.5605(12) 0.7967(11) 0.4805(9) 0.062(6) Uani 1 1 d . . . H5A H 0.5447 0.7777 0.5126 0.075 Uiso 1 1 d R . . C6A C 0.6036(14) 0.8544(13) 0.4796(10) 0.075(8) Uani 1 1 d . . . H6A H 0.6127 0.8724 0.5130 0.090 Uiso 1 1 d R . . C7A C 0.634(2) 0.8919(15) 0.4371(16) 0.118(13) Uani 1 1 d . . . O7A O 0.6670(12) 0.9450(9) 0.4315(10) 0.137(9) Uani 1 1 d . . . N8A N 0.6144(11) 0.8546(10) 0.3971(8) 0.066(6) Uani 1 1 d . . . N1B N 0.2580(14) 0.8247(10) 0.3958(9) 0.095(7) Uani 1 1 d . . . C2B C 0.3125(16) 0.7897(10) 0.4268(9) 0.069(7) Uani 1 1 d . . . H2B H 0.3111 0.7928 0.4637 0.082 Uiso 1 1 d R . . N3B N 0.3703(11) 0.7515(8) 0.4011(7) 0.054(5) Uani 1 1 d . . . C3AB C 0.3607(12) 0.7634(10) 0.3503(9) 0.049(6) Uani 1 1 d . . . N4B N 0.4055(9) 0.7403(7) 0.3090(6) 0.038(4) Uani 1 1 d . . . C5B C 0.3774(13) 0.7655(10) 0.2608(8) 0.050(6) Uani 1 1 d . . . H5B H 0.4054 0.7519 0.2301 0.060 Uiso 1 1 d R . . C6B C 0.3149(14) 0.8069(11) 0.2555(9) 0.063(6) Uani 1 1 d . . . H6B H 0.3008 0.8213 0.2216 0.076 Uiso 1 1 d R . . C7B C 0.2678(17) 0.8310(13) 0.2979(14) 0.093(10) Uani 1 1 d . . . O7B O 0.2084(12) 0.8729(9) 0.2993(8) 0.132(8) Uani 1 1 d . . . N8B N 0.2939(13) 0.8080(10) 0.3440(8) 0.075(6) Uani 1 1 d . . . N1P N 0.4721(11) 0.6070(7) 0.3003(6) 0.045(4) Uani 1 1 d . . . C1AP C 0.5347(12) 0.5614(9) 0.3044(6) 0.037(5) Uani 1 1 d . . . C2P C 0.3913(15) 0.5875(10) 0.2912(7) 0.054(6) Uani 1 1 d . . . H2P H 0.3481 0.6187 0.2887 0.065 Uiso 1 1 d R . . C3P C 0.3674(17) 0.5223(11) 0.2852(7) 0.070(8) Uani 1 1 d . . . H3P H 0.3107 0.5096 0.2788 0.084 Uiso 1 1 d R . . C4P C 0.4358(19) 0.4787(11) 0.2890(9) 0.077(8) Uani 1 1 d . . . H4P H 0.4221 0.4351 0.2857 0.093 Uiso 1 1 d R . . C4AP C 0.5197(16) 0.4951(13) 0.2979(10) 0.075(8) Uani 1 1 d . . . C5P C 0.5896(18) 0.4500(11) 0.3025(9) 0.078(8) Uani 1 1 d . . . H5P H 0.5794 0.4058 0.2992 0.093 Uiso 1 1 d R . . C6P C 0.6704(16) 0.4724(11) 0.3120(8) 0.066(7) Uani 1 1 d . . . H6P H 0.7161 0.4431 0.3134 0.079 Uiso 1 1 d R . . C6AP C 0.6869(14) 0.5396(12) 0.3198(9) 0.063(6) Uani 1 1 d . . . C7P C 0.7690(13) 0.5623(12) 0.3300(8) 0.062(7) Uani 1 1 d . . . H7P H 0.8155 0.5340 0.3330 0.074 Uiso 1 1 d R . . C8P C 0.7815(13) 0.6283(11) 0.3350(8) 0.052(6) Uani 1 1 d . . . H8P H 0.8366 0.6451 0.3406 0.062 Uiso 1 1 d R . . C9P C 0.7104(14) 0.6689(11) 0.3315(8) 0.063(7) Uani 1 1 d . . . H9P H 0.7182 0.7133 0.3352 0.076 Uiso 1 1 d R . . N10P N 0.6303(10) 0.6452(8) 0.3229(6) 0.048(4) Uani 1 1 d . . . C0AP C 0.6203(13) 0.5821(11) 0.3130(7) 0.045(5) Uani 1 1 d . . . N1Q N 0.3836(10) 0.6150(7) 0.4245(6) 0.044(4) Uani 1 1 d . . . C1AQ C 0.4267(13) 0.5567(10) 0.4267(7) 0.046(5) Uani 1 1 d . . . C2Q C 0.2994(16) 0.6100(10) 0.4172(8) 0.060(6) Uani 1 1 d . . . H2Q H 0.2676 0.6482 0.4163 0.072 Uiso 1 1 d R . . C3Q C 0.2527(16) 0.5529(13) 0.4094(8) 0.069(7) Uani 1 1 d . . . H3Q H 0.1929 0.5536 0.4057 0.083 Uiso 1 1 d R . . C4Q C 0.2949(18) 0.4969(12) 0.4090(9) 0.077(8) Uani 1 1 d . . . H4Q H 0.2668 0.4585 0.4004 0.093 Uiso 1 1 d R . . C4AQ C 0.3878(18) 0.4977(12) 0.4210(8) 0.068(7) Uani 1 1 d . . . C5Q C 0.440(2) 0.4410(13) 0.4230(10) 0.097(11) Uani 1 1 d . . . H5Q H 0.4145 0.4006 0.4183 0.116 Uiso 1 1 d R . . C6Q C 0.529(3) 0.4464(17) 0.4323(12) 0.120(14) Uani 1 1 d . . . H6Q H 0.5632 0.4093 0.4328 0.144 Uiso 1 1 d R . . C6AQ C 0.5665(18) 0.5081(14) 0.4399(9) 0.073(8) Uani 1 1 d . . . C7Q C 0.653(2) 0.5120(15) 0.4528(10) 0.091(10) Uani 1 1 d . . . H7Q H 0.6861 0.4749 0.4564 0.109 Uiso 1 1 d R . . C8Q C 0.6878(16) 0.5747(17) 0.4615(10) 0.096(11) Uani 1 1 d . . . H8Q H 0.7467 0.5803 0.4673 0.115 Uiso 1 1 d R . . C9Q C 0.6318(15) 0.6266(14) 0.4589(7) 0.074(8) Uani 1 1 d . . . H9Q H 0.6547 0.6671 0.4667 0.089 Uiso 1 1 d R . . N10Q N 0.5476(11) 0.6235(9) 0.4466(7) 0.055(5) Uani 1 1 d . . . C0AQ C 0.5159(13) 0.5642(11) 0.4385(7) 0.049(5) Uani 1 1 d . . . Cl1 Cl 0.8396(4) 0.7750(3) 0.4280(2) 0.090(2) Uani 1 1 d D . . O1P O 0.8357(13) 0.7946(9) 0.3768(4) 0.169(10) Uiso 1 1 d D . . O2P O 0.7704(10) 0.7359(8) 0.4386(7) 0.162(9) Uiso 1 1 d D . . O3P O 0.9141(10) 0.7443(12) 0.4384(10) 0.37(2) Uiso 1 1 d D . . O4P O 0.8332(17) 0.8283(8) 0.4606(8) 0.280(18) Uiso 1 1 d D . . Cl2 Cl 0.6160(5) 0.6706(4) 0.1776(3) 0.124(3) Uani 1 1 d D . . O5P O 0.6210(11) 0.6798(9) 0.1235(4) 0.130(7) Uiso 1 1 d D . . O6P O 0.5435(11) 0.6357(10) 0.1880(8) 0.235(15) Uiso 1 1 d D . . O7P O 0.6870(11) 0.6403(12) 0.1954(8) 0.276(18) Uiso 1 1 d D . . O8P O 0.6073(17) 0.7297(7) 0.2013(8) 0.286(19) Uiso 1 1 d D . . O1W O 0.435(3) 0.950(2) 0.3442(17) 0.129(15) Uiso 0.50 1 d P . . O1W' O 0.435(2) 0.9158(18) 0.3863(15) 0.107(12) Uiso 0.50 1 d P . . O2W O 0.450(4) 0.933(3) 0.566(3) 0.26(3) Uiso 0.50 1 d P . . O2W' O 0.400(2) 0.9468(18) 0.4933(15) 0.118(13) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0403(8) 0.0441(9) 0.0496(9) -0.0003(9) 0.0002(8) -0.0007(9) Pd2 0.0408(9) 0.0550(10) 0.0487(9) 0.0067(10) 0.0011(8) 0.0032(9) N1A 0.032(10) 0.054(13) 0.15(2) 0.019(14) 0.001(13) -0.010(10) C2A 0.048(14) 0.068(17) 0.069(17) 0.008(14) 0.014(13) 0.005(12) N3A 0.038(10) 0.052(11) 0.045(11) 0.010(9) 0.000(8) -0.011(8) C3AA 0.034(11) 0.050(15) 0.054(14) 0.000(12) -0.025(11) -0.006(10) N4A 0.063(12) 0.071(13) 0.040(11) -0.004(10) -0.004(11) -0.014(10) C5A 0.046(13) 0.086(19) 0.055(14) 0.000(14) -0.002(11) -0.028(13) C6A 0.056(16) 0.10(2) 0.074(18) -0.043(16) 0.016(14) -0.034(15) C7A 0.09(2) 0.08(2) 0.18(4) -0.06(3) -0.02(3) -0.017(19) O7A 0.084(14) 0.076(14) 0.25(3) -0.042(17) 0.010(16) -0.043(11) N8A 0.055(12) 0.067(14) 0.077(15) -0.026(13) -0.014(11) -0.006(11) N1B 0.087(16) 0.093(18) 0.104(18) -0.005(15) 0.029(15) 0.041(14) C2B 0.093(19) 0.055(16) 0.058(16) -0.018(13) 0.017(15) 0.027(14) N3B 0.051(11) 0.055(12) 0.056(12) 0.012(10) -0.014(10) 0.006(9) C3AB 0.030(11) 0.043(14) 0.075(17) 0.027(13) 0.020(12) -0.006(10) N4B 0.031(9) 0.043(10) 0.040(10) 0.011(8) 0.007(8) -0.003(8) C5B 0.056(14) 0.049(14) 0.045(14) -0.010(11) 0.003(12) -0.005(12) C6B 0.050(14) 0.069(16) 0.071(16) 0.007(16) 0.018(13) 0.004(14) C7B 0.059(18) 0.07(2) 0.15(3) 0.04(2) -0.043(19) 0.000(15) O7B 0.102(15) 0.124(17) 0.17(2) -0.028(15) -0.060(14) 0.070(14) N8B 0.084(15) 0.065(13) 0.076(14) 0.011(13) -0.005(12) 0.015(13) N1P 0.052(11) 0.054(11) 0.031(9) 0.007(8) 0.019(9) 0.015(10) C1AP 0.049(13) 0.040(12) 0.022(9) 0.002(9) 0.022(9) 0.008(10) C2P 0.067(15) 0.057(15) 0.038(13) 0.034(11) -0.007(11) -0.008(13) C3P 0.12(2) 0.056(16) 0.035(13) 0.012(12) -0.039(14) -0.050(16) C4P 0.14(3) 0.030(13) 0.064(17) 0.013(12) 0.019(17) 0.021(16) C4AP 0.050(15) 0.08(2) 0.10(2) -0.002(16) -0.001(15) -0.018(15) C5P 0.10(2) 0.036(14) 0.10(2) -0.012(14) -0.006(17) 0.004(15) C6P 0.075(17) 0.073(18) 0.049(15) 0.012(13) 0.012(14) -0.017(15) C6AP 0.052(15) 0.069(17) 0.067(16) -0.002(14) -0.012(13) -0.023(13) C7P 0.045(15) 0.10(2) 0.043(13) -0.020(13) 0.013(10) 0.022(14) C8P 0.031(12) 0.062(16) 0.062(15) -0.004(13) -0.006(10) -0.005(12) C9P 0.067(16) 0.062(16) 0.060(15) 0.025(12) -0.008(13) -0.005(13) N10P 0.043(10) 0.046(11) 0.053(11) -0.008(9) 0.008(9) -0.003(9) C0AP 0.046(13) 0.062(15) 0.027(11) 0.026(11) 0.020(10) -0.003(12) N1Q 0.038(10) 0.042(11) 0.052(11) 0.014(9) 0.009(9) 0.010(8) C1AQ 0.048(13) 0.058(15) 0.033(11) 0.008(11) -0.006(10) -0.010(12) C2Q 0.088(19) 0.034(13) 0.059(16) -0.008(11) 0.007(14) 0.012(13) C3Q 0.058(14) 0.079(18) 0.070(16) 0.009(17) 0.009(15) -0.024(14) C4Q 0.11(2) 0.052(17) 0.070(17) -0.004(14) 0.015(17) -0.014(17) C4AQ 0.10(2) 0.055(16) 0.047(14) 0.021(13) -0.020(14) -0.027(16) C5Q 0.20(4) 0.043(17) 0.049(16) 0.021(13) 0.02(2) 0.01(2) C6Q 0.20(4) 0.09(3) 0.07(2) 0.03(2) 0.05(3) 0.06(3) C6AQ 0.09(2) 0.09(2) 0.044(14) 0.023(14) 0.029(14) 0.069(17) C7Q 0.09(2) 0.12(3) 0.062(18) 0.027(19) 0.033(17) 0.07(2) C8Q 0.040(15) 0.18(3) 0.067(18) 0.06(2) 0.005(13) 0.04(2) C9Q 0.058(16) 0.15(3) 0.013(11) 0.016(14) -0.012(11) -0.005(18) N10Q 0.042(11) 0.061(13) 0.063(13) 0.011(10) 0.004(10) 0.004(10) C0AQ 0.048(13) 0.067(16) 0.031(11) 0.001(11) 0.001(10) 0.009(12) Cl1 0.090(5) 0.117(6) 0.063(4) 0.007(4) -0.004(4) -0.031(4) Cl2 0.108(6) 0.194(10) 0.069(5) 0.008(6) 0.016(5) 0.017(6) _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 N3A 1.968(16) . ? Pd1 N1P 1.994(16) . ? Pd1 N4B 2.001(14) . ? Pd1 N10P 2.009(16) . ? Pd1 Pd2 2.986(2) . ? Pd2 N1Q 1.977(16) . ? Pd2 N10Q 1.995(16) . ? Pd2 N3B 1.996(16) . ? Pd2 N4A 2.015(17) . ? N1A C2A 1.34(3) . ? N1A N8A 1.51(3) . ? C2A N3A 1.40(2) . ? N3A C3AA 1.34(2) . ? C3AA N4A 1.33(2) . ? C3AA N8A 1.38(2) . ? N4A C5A 1.33(2) . ? C5A C6A 1.37(3) . ? C6A C7A 1.40(4) . ? C7A O7A 1.22(3) . ? C7A N8A 1.30(3) . ? N1B C2B 1.36(3) . ? N1B N8B 1.46(2) . ? C2B N3B 1.36(2) . ? N3B C3AB 1.31(2) . ? C3AB N4B 1.34(2) . ? C3AB N8B 1.39(2) . ? N4B C5B 1.39(2) . ? C5B C6B 1.30(3) . ? C6B C7B 1.39(3) . ? C7B O7B 1.26(3) . ? C7B N8B 1.32(3) . ? N1P C2P 1.33(2) . ? N1P C1AP 1.35(2) . ? C1AP C4AP 1.40(3) . ? C1AP C0AP 1.41(2) . ? C2P C3P 1.40(3) . ? C3P C4P 1.39(3) . ? C4P C4AP 1.36(3) . ? C4AP C5P 1.43(3) . ? C5P C6P 1.35(3) . ? C6P C6AP 1.43(3) . ? C6AP C0AP 1.36(3) . ? C6AP C7P 1.38(3) . ? C7P C8P 1.38(3) . ? C8P C9P 1.39(3) . ? C9P N10P 1.35(2) . ? N10P C0AP 1.33(2) . ? N1Q C2Q 1.32(2) . ? N1Q C1AQ 1.38(2) . ? C1AQ C4AQ 1.37(3) . ? C1AQ C0AQ 1.42(3) . ? C2Q C3Q 1.40(3) . ? C3Q C4Q 1.33(3) . ? C4Q C4AQ 1.47(3) . ? C4AQ C5Q 1.42(3) . ? C5Q C6Q 1.40(4) . ? C6Q C6AQ 1.41(4) . ? C6AQ C7Q 1.37(3) . ? C6AQ C0AQ 1.40(3) . ? C7Q C8Q 1.42(3) . ? C8Q C9Q 1.38(3) . ? C9Q N10Q 1.34(2) . ? N10Q C0AQ 1.34(2) . ? Cl1 O3P 1.341(8) . ? Cl1 O1P 1.351(8) . ? Cl1 O2P 1.368(8) . ? Cl1 O4P 1.376(9) . ? Cl2 O7P 1.340(8) . ? Cl2 O6P 1.359(9) . ? Cl2 O8P 1.366(9) . ? Cl2 O5P 1.376(8) . ? O1W O1W' 1.28(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3A Pd1 N1P 173.1(6) . . ? N3A Pd1 N4B 88.0(6) . . ? N1P Pd1 N4B 95.1(6) . . ? N3A Pd1 N10P 94.7(7) . . ? N1P Pd1 N10P 82.3(7) . . ? N4B Pd1 N10P 177.3(6) . . ? N3A Pd1 Pd2 80.6(5) . . ? N1P Pd1 Pd2 93.7(4) . . ? N4B Pd1 Pd2 80.5(4) . . ? N10P Pd1 Pd2 100.1(5) . . ? N1Q Pd2 N10Q 81.9(7) . . ? N1Q Pd2 N3B 93.2(7) . . ? N10Q Pd2 N3B 170.4(7) . . ? N1Q Pd2 N4A 177.3(7) . . ? N10Q Pd2 N4A 95.5(7) . . ? N3B Pd2 N4A 89.3(7) . . ? N1Q Pd2 Pd1 98.0(5) . . ? N10Q Pd2 Pd1 90.8(5) . . ? N3B Pd2 Pd1 81.7(5) . . ? N4A Pd2 Pd1 81.6(5) . . ? C2A N1A N8A 100.4(18) . . ? N1A C2A N3A 117(2) . . ? C3AA N3A C2A 104.2(17) . . ? C3AA N3A Pd1 124.9(14) . . ? C2A N3A Pd1 130.8(15) . . ? N4A C3AA N3A 128.8(19) . . ? N4A C3AA N8A 119(2) . . ? N3A C3AA N8A 111.6(19) . . ? C3AA N4A C5A 114.4(18) . . ? C3AA N4A Pd2 121.7(14) . . ? C5A N4A Pd2 123.3(15) . . ? N4A C5A C6A 120(2) . . ? C5A C6A C7A 131(2) . . ? O7A C7A N8A 123(4) . . ? O7A C7A C6A 137(4) . . ? N8A C7A C6A 100(3) . . ? C7A N8A C3AA 135(3) . . ? C7A N8A N1A 118(3) . . ? C3AA N8A N1A 107.2(17) . . ? C2B N1B N8B 98.7(18) . . ? N3B C2B N1B 116(2) . . ? C3AB N3B C2B 106.3(18) . . ? C3AB N3B Pd2 123.1(16) . . ? C2B N3B Pd2 130.5(16) . . ? N3B C3AB N4B 129(2) . . ? N3B C3AB N8B 108.6(19) . . ? N4B C3AB N8B 122(2) . . ? C3AB N4B C5B 112.5(17) . . ? C3AB N4B Pd1 123.2(14) . . ? C5B N4B Pd1 122.3(13) . . ? C6B C5B N4B 125(2) . . ? C5B C6B C7B 123(2) . . ? O7B C7B N8B 117(3) . . ? O7B C7B C6B 131(3) . . ? N8B C7B C6B 113(2) . . ? C7B N8B C3AB 125(2) . . ? C7B N8B N1B 126(2) . . ? C3AB N8B N1B 109.7(19) . . ? C2P N1P C1AP 118.3(18) . . ? C2P N1P Pd1 130.6(14) . . ? C1AP N1P Pd1 110.8(13) . . ? N1P C1AP C4AP 123(2) . . ? N1P C1AP C0AP 118.3(18) . . ? C4AP C1AP C0AP 118(2) . . ? N1P C2P C3P 124(2) . . ? C4P C3P C2P 114(2) . . ? C4AP C4P C3P 125(2) . . ? C4P C4AP C1AP 115(2) . . ? C4P C4AP C5P 125(2) . . ? C1AP C4AP C5P 120(2) . . ? C6P C5P C4AP 119(2) . . ? C5P C6P C6AP 121(2) . . ? C0AP C6AP C7P 120(2) . . ? C0AP C6AP C6P 118(2) . . ? C7P C6AP C6P 121(2) . . ? C6AP C7P C8P 119(2) . . ? C7P C8P C9P 118.6(19) . . ? N10P C9P C8P 121(2) . . ? C0AP N10P C9P 119.4(18) . . ? C0AP N10P Pd1 112.5(14) . . ? C9P N10P Pd1 128.0(15) . . ? N10P C0AP C6AP 121(2) . . ? N10P C0AP C1AP 115.7(19) . . ? C6AP C0AP C1AP 122(2) . . ? C2Q N1Q C1AQ 114.5(17) . . ? C2Q N1Q Pd2 131.5(14) . . ? C1AQ N1Q Pd2 113.9(13) . . ? C4AQ C1AQ N1Q 124(2) . . ? C4AQ C1AQ C0AQ 123(2) . . ? N1Q C1AQ C0AQ 112.6(19) . . ? N1Q C2Q C3Q 127(2) . . ? C4Q C3Q C2Q 119(2) . . ? C3Q C4Q C4AQ 118(2) . . ? C1AQ C4AQ C5Q 119(3) . . ? C1AQ C4AQ C4Q 118(2) . . ? C5Q C4AQ C4Q 124(3) . . ? C6Q C5Q C4AQ 120(3) . . ? C5Q C6Q C6AQ 120(3) . . ? C7Q C6AQ C0AQ 120(3) . . ? C7Q C6AQ C6Q 119(3) . . ? C0AQ C6AQ C6Q 121(3) . . ? C6AQ C7Q C8Q 118(3) . . ? C9Q C8Q C7Q 117(3) . . ? N10Q C9Q C8Q 126(3) . . ? C0AQ N10Q C9Q 116(2) . . ? C0AQ N10Q Pd2 111.3(14) . . ? C9Q N10Q Pd2 132.4(18) . . ? N10Q C0AQ C6AQ 123(2) . . ? N10Q C0AQ C1AQ 119(2) . . ? C6AQ C0AQ C1AQ 117(2) . . ? O3P Cl1 O1P 111.5(9) . . ? O3P Cl1 O2P 110.8(8) . . ? O1P Cl1 O2P 109.1(8) . . ? O3P Cl1 O4P 108.9(8) . . ? O1P Cl1 O4P 109.0(8) . . ? O2P Cl1 O4P 107.4(8) . . ? O7P Cl2 O6P 111.3(9) . . ? O7P Cl2 O8P 110.7(9) . . ? O6P Cl2 O8P 108.0(8) . . ? O7P Cl2 O5P 110.4(8) . . ? O6P Cl2 O5P 108.1(8) . . ? O8P Cl2 O5P 108.3(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.491 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.194 #===END data_compound6 _database_code_CSD 190495 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H29 Cl3 N16 O19 Pd2' _chemical_formula_weight 1188.80 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P m m n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z' 'x+1/2, -y, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z' '-x-1/2, y, z' _cell_length_a 11.1799(14) _cell_length_b 18.9400(18) _cell_length_c 9.6374(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2040.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description 'prismatic' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5388 _exptl_absorpt_correction_T_max 0.6505 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 1.05 - 1.25, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987) ; _diffrn_detector_area_resol_mean ? _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3.7 _diffrn_reflns_number 3193 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3193 _reflns_number_gt 1900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material ? _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^)+(0.0600P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3193 _refine_ls_number_parameters 162 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1404 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2107 _refine_ls_wR_factor_gt 0.1705 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.115 _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 Pd Pd 0.39204(8) 0.2500 0.53000(8) 0.0569(3) Uani 1 2 d S . . N1 N 0.3916(10) 0.4104(9) 0.8390(17) 0.075(4) Uiso 0.50 1 d PD A -1 C2 C 0.4428(11) 0.3648(11) 0.752(2) 0.069(7) Uiso 0.50 1 d PD A -1 H2 H 0.5283 0.3619 0.7445 0.082 Uiso 0.50 1 d PR A -1 N3 N 0.3718(10) 0.3220(7) 0.6749(14) 0.051(3) Uiso 0.50 1 d PD A -1 C3A C 0.2635(9) 0.3451(5) 0.7167(9) 0.046(2) Uiso 0.50 1 d PD A -1 N4 N 0.1558(10) 0.3287(7) 0.6722(14) 0.048(3) Uiso 0.50 1 d PD . -1 C5 C 0.0559(15) 0.3528(14) 0.738(3) 0.082(8) Uiso 0.50 1 d PD A -1 H5 H -0.0215 0.3345 0.7138 0.098 Uiso 0.50 1 d PR A -1 C6 C 0.0682(14) 0.4025(10) 0.840(2) 0.073(5) Uiso 0.50 1 d PD A -1 H6 H -0.0031 0.4187 0.8855 0.088 Uiso 0.50 1 d PR A -1 C7 C 0.1767(10) 0.4309(8) 0.8837(16) 0.080(5) Uiso 0.50 1 d PD A -1 O7 O 0.2073(10) 0.4767(6) 0.9664(12) 0.096(4) Uiso 0.50 1 d PD A -1 N8 N 0.2726(9) 0.3958(5) 0.8183(9) 0.058(3) Uiso 0.50 1 d PD A -1 N1P N 0.4419(6) 0.3179(4) 0.3814(6) 0.0691(17) Uani 1 1 d . A . C2P C 0.4282(10) 0.3887(6) 0.3823(9) 0.090(3) Uani 1 1 d . . . H2P H 0.3881 0.4104 0.4553 0.107 Uiso 1 1 d R A . C3P C 0.4739(12) 0.4284(6) 0.2738(11) 0.118(4) Uani 1 1 d . A . H3P H 0.4626 0.4770 0.2700 0.142 Uiso 1 1 d R . . C4P C 0.5375(14) 0.3919(9) 0.1737(12) 0.144(6) Uani 1 1 d . . . H4P H 0.5733 0.4180 0.1034 0.173 Uiso 1 1 d R A . N5P N 0.5492(9) 0.3229(6) 0.1714(8) 0.109(3) Uani 1 1 d . A . C6P C 0.4992(8) 0.2887(5) 0.2758(7) 0.081(3) Uani 1 1 d . . . Cl1 Cl 0.2500 0.2500 0.0583(4) 0.0679(10) Uani 1 4 d S . . O1Q O 0.3519(10) 0.2500 -0.0262(9) 0.096(3) Uani 1 2 d S . . O2Q O 0.2500 0.1891(6) 0.1438(11) 0.126(4) Uani 1 2 d S . . Cl2 Cl 0.2500 0.56295(19) 0.5095(4) 0.0891(10) Uani 1 2 d S . . O3Q O 0.3488(9) 0.5628(5) 0.4235(9) 0.147(3) Uani 1 1 d . . . O4Q O 0.2500 0.5034(6) 0.5949(11) 0.123(4) Uani 1 2 d S . . O5Q O 0.2500 0.6234(7) 0.5939(15) 0.170(6) Uani 1 2 d S . . O1W O 0.2500 0.5837(5) 0.1318(10) 0.118(4) Uani 1 2 d S . . O2W O 0.1676(12) 0.7096(6) 0.0628(10) 0.086(3) Uani 0.50 1 d P . -1 O3W O 0.684(3) 0.2500 0.578(3) 0.170(11) Uiso 0.50 2 d SP . . 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 Pd 0.0615(5) 0.0675(5) 0.0418(4) 0.000 -0.0001(4) 0.000 N1P 0.078(4) 0.086(5) 0.044(3) 0.005(3) -0.001(3) -0.014(4) C2P 0.112(8) 0.098(7) 0.059(5) 0.003(5) 0.005(5) -0.027(6) C3P 0.176(12) 0.113(8) 0.066(6) 0.015(6) 0.008(7) -0.058(9) C4P 0.170(13) 0.188(14) 0.073(7) 0.013(9) 0.019(8) -0.107(12) N5P 0.117(7) 0.156(9) 0.054(4) -0.005(6) 0.021(4) -0.051(7) C6P 0.074(5) 0.127(7) 0.042(4) -0.001(4) 0.004(4) -0.022(5) Cl1 0.082(3) 0.076(2) 0.0450(19) 0.000 0.000 0.000 O1Q 0.123(8) 0.092(6) 0.074(5) 0.000 0.034(6) 0.000 O2Q 0.104(8) 0.163(10) 0.111(8) 0.082(8) 0.000 0.000 Cl2 0.120(3) 0.082(2) 0.0647(18) 0.0053(16) 0.000 0.000 O3Q 0.153(7) 0.167(8) 0.122(6) 0.015(6) 0.040(6) -0.015(7) O4Q 0.162(10) 0.112(8) 0.096(7) 0.042(7) 0.000 0.000 O5Q 0.262(18) 0.110(9) 0.138(11) -0.038(9) 0.000 0.000 O1W 0.188(12) 0.088(7) 0.077(6) 0.010(5) 0.000 0.000 O2W 0.101(8) 0.103(8) 0.054(6) 0.004(6) -0.015(6) -0.007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N3 1.964(10) . ? Pd N3 1.964(10) 7_565 ? Pd N1P 2.004(6) 7_565 ? Pd N1P 2.004(6) . ? Pd N4 2.095(11) 8_655 ? Pd N4 2.095(11) 2 ? Pd Pd 3.1760(17) 2 ? N1 C2 1.333(5) . ? N1 N8 1.373(5) . ? C2 N3 1.357(5) . ? N3 C3A 1.349(5) . ? C3A N4 1.315(5) . ? C3A N8 1.375(5) . ? N4 C5 1.362(5) . ? N4 Pd 2.095(11) 2 ? C5 C6 1.368(5) . ? C6 C7 1.393(5) . ? C7 O7 1.227(5) . ? C7 N8 1.410(5) . ? N1P C6P 1.323(10) . ? N1P C2P 1.350(11) . ? C2P C3P 1.385(12) . ? C3P C4P 1.384(18) . ? C4P N5P 1.314(16) . ? N5P C6P 1.321(10) . ? C6P C6P 1.466(19) 7_565 ? Cl1 O1Q 1.400(9) 2 ? Cl1 O1Q 1.400(9) . ? Cl1 O2Q 1.417(10) 2 ? Cl1 O2Q 1.417(10) . ? Cl2 O3Q 1.381(9) . ? Cl2 O3Q 1.381(9) 8_655 ? Cl2 O4Q 1.397(10) . ? Cl2 O5Q 1.404(12) . ? O1W O7 2.622(15) 1_554 ? O1W O2W 2.641(15) . ? O2W O2W 2.39(3) 2_565 ? O2W N5P 2.688(13) 4_465 ? O3W O3W 1.47(6) 2_655 ? O3W O5Q 3.01(2) 5_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd N3 87.9(9) . 7_565 ? N3 Pd N1P 170.2(4) . 7_565 ? N3 Pd N1P 95.4(5) 7_565 7_565 ? N3 Pd N1P 95.4(5) . . ? N3 Pd N1P 170.2(4) 7_565 . ? N1P Pd N1P 79.9(4) 7_565 . ? N3 Pd N4 8.7(6) . 8_655 ? N3 Pd N4 90.0(3) 7_565 8_655 ? N1P Pd N4 174.5(5) 7_565 8_655 ? N1P Pd N4 94.7(5) . 8_655 ? N3 Pd N4 90.0(3) . 2 ? N3 Pd N4 8.7(6) 7_565 2 ? N1P Pd N4 94.7(5) 7_565 2 ? N1P Pd N4 174.5(5) . 2 ? N4 Pd N4 90.8(9) 8_655 2 ? N3 Pd Pd 83.4(3) . 2 ? N3 Pd Pd 83.4(3) 7_565 2 ? N1P Pd Pd 106.2(2) 7_565 2 ? N1P Pd Pd 106.2(2) . 2 ? N4 Pd Pd 75.2(3) 8_655 2 ? N4 Pd Pd 75.2(3) 2 2 ? C2 N1 N8 101.2(11) . . ? N1 C2 N3 118.7(10) . . ? C3A N3 C2 99.6(7) . . ? C3A N3 Pd 122.8(8) . . ? C2 N3 Pd 137.5(8) . . ? N4 C3A N3 130.4(8) . . ? N4 C3A N8 117.6(10) . . ? N3 C3A N8 111.9(8) . . ? C3A N4 C5 121.4(12) . . ? C3A N4 Pd 127.9(9) . 2 ? C5 N4 Pd 109.4(9) . 2 ? N4 C5 C6 118.8(17) . . ? C5 C6 C7 124.8(18) . . ? O7 C7 C6 135.5(12) . . ? O7 C7 N8 114.3(11) . . ? C6 C7 N8 110.2(12) . . ? N1 N8 C3A 108.4(11) . . ? N1 N8 C7 125.2(11) . . ? C3A N8 C7 126.3(10) . . ? C6P N1P C2P 118.4(8) . . ? C6P N1P Pd 114.6(6) . . ? C2P N1P Pd 127.0(6) . . ? N1P C2P C3P 119.5(10) . . ? C4P C3P C2P 116.4(12) . . ? N5P C4P C3P 124.1(11) . . ? C4P N5P C6P 115.6(10) . . ? N5P C6P N1P 125.9(10) . . ? N5P C6P C6P 119.3(6) . 7_565 ? N1P C6P C6P 114.7(5) . 7_565 ? O1Q Cl1 O1Q 108.9(9) 2 . ? O1Q Cl1 O2Q 109.8(3) 2 2 ? O1Q Cl1 O2Q 109.8(3) . 2 ? O1Q Cl1 O2Q 109.8(3) 2 . ? O1Q Cl1 O2Q 109.8(3) . . ? O2Q Cl1 O2Q 108.9(11) 2 . ? O3Q Cl2 O3Q 106.2(9) . 8_655 ? O3Q Cl2 O4Q 110.6(5) . . ? O3Q Cl2 O4Q 110.6(5) 8_655 . ? O3Q Cl2 O5Q 110.5(6) . . ? O3Q Cl2 O5Q 110.5(6) 8_655 . ? O4Q Cl2 O5Q 108.5(8) . . ? O7 O1W O2W 118.8(5) 1_554 . ? O2W O2W O1W 108.0(7) 2_565 . ? O2W O2W N5P 121.7(4) 2_565 4_465 ? O1W O2W N5P 100.1(5) . 4_465 ? O3W O3W O5Q 75.8(5) 2_655 5_666 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.858 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.119 #===END data_compound7 _database_code_CSD 190496 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C26 H30 N18 O14 Pt2' _chemical_formula_weight 1208.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 6/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' _cell_length_a 26.509(2) _cell_length_b 26.509(2) _cell_length_c 10.1184(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6158.0(11) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 10.46 _exptl_crystal_description 'hexagonal blocks' _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3480 _exptl_absorpt_coefficient_mu 6.891 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.3313 _exptl_absorpt_correction_T_max 0.3788 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 8.66 _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_number 6833 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 22.51 _reflns_number_total 2876 _reflns_number_gt 2065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0750P)^2^+60.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2876 _refine_ls_number_parameters 262 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.133 _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 Pt Pt 0.42599(2) 0.13539(2) 0.34379(7) 0.0465(3) Uani 1 1 d . . . N1A N 0.6065(11) 0.2151(12) 0.6729(16) 0.057(6) Uiso 0.50 1 d PD . . C2A C 0.5528(10) 0.1896(17) 0.722(3) 0.056(6) Uiso 0.50 1 d PD . . H2A H 0.5456 0.1847 0.8153 0.068 Uiso 0.50 1 d PR . . N3A N 0.5088(10) 0.1737(12) 0.6346(19) 0.036(3) Uiso 0.50 1 d PD . . C3AA C 0.5369(5) 0.1877(7) 0.5175(18) 0.032(5) Uiso 0.50 1 d PD . . N4A N 0.5155(10) 0.1819(12) 0.3972(19) 0.036(3) Uiso 0.50 1 d PD . . C5A C 0.5550(11) 0.2019(17) 0.297(3) 0.056(6) Uiso 0.50 1 d PD . . H5A H 0.5404 0.1903 0.2088 0.068 Uiso 0.50 1 d PR . . C6A C 0.6141(12) 0.2320(15) 0.314(2) 0.057(6) Uiso 0.50 1 d PD . . H6A H 0.6387 0.2505 0.2395 0.068 Uiso 0.50 1 d PR . . C7A C 0.6387(8) 0.2389(10) 0.4392(19) 0.047(7) Uiso 0.50 1 d PD . . O7A O 0.6909(6) 0.2632(6) 0.472(2) 0.049(5) Uiso 0.50 1 d P . . N8A N 0.5960(5) 0.2142(7) 0.5391(16) 0.039(5) Uiso 0.50 1 d PD . . N1B N 0.432(2) -0.0154(15) 0.6746(16) 0.070(6) Uiso 0.50 1 d PD . . C2B C 0.423(2) 0.0252(17) 0.729(3) 0.060(6) Uiso 0.50 1 d PD . . H2B H 0.4220 0.0313 0.8221 0.072 Uiso 0.50 1 d PR . . N3B N 0.4224(15) 0.0610(13) 0.634(2) 0.040(3) Uiso 0.50 1 d PD . . C3AB C 0.4244(8) 0.0383(6) 0.516(2) 0.033(5) Uiso 0.50 1 d PD . . N4B N 0.4240(15) 0.0561(13) 0.395(2) 0.040(3) Uiso 0.50 1 d PD . . C5B C 0.430(2) 0.0250(17) 0.294(4) 0.060(6) Uiso 0.50 1 d PD . . H5B H 0.4324 0.0393 0.2060 0.072 Uiso 0.50 1 d PR . . C6B C 0.428(2) -0.0270(17) 0.313(3) 0.070(6) Uiso 0.50 1 d PD . . H6B H 0.4254 -0.0498 0.2375 0.084 Uiso 0.50 1 d PR . . C7B C 0.4311(11) -0.0462(9) 0.439(2) 0.048(7) Uiso 0.50 1 d PD . . O7B O 0.4327(7) -0.0907(7) 0.469(2) 0.063(6) Uiso 0.50 1 d P . . N8B N 0.4279(7) -0.0111(6) 0.5395(16) 0.037(5) Uiso 0.50 1 d PD . . N1P N 0.3408(5) 0.0990(5) 0.2934(13) 0.053(3) Uani 1 1 d . . . C2P C 0.3005(6) 0.0443(7) 0.3095(17) 0.065(5) Uani 1 1 d . . . H2P H 0.3081 0.0174 0.3507 0.077 Uiso 1 1 d R . . C3P C 0.2460(8) 0.0293(9) 0.261(2) 0.084(6) Uani 1 1 d . . . H3P H 0.2162 -0.0093 0.2646 0.101 Uiso 1 1 d R . . C4P C 0.2357(8) 0.0683(10) 0.207(2) 0.093(7) Uani 1 1 d . . . H4P H 0.1977 0.0567 0.1819 0.111 Uiso 1 1 d R . . N5P N 0.2766(6) 0.1244(7) 0.1919(16) 0.082(5) Uani 1 1 d . . . C6P C 0.3273(6) 0.1371(7) 0.2395(17) 0.059(4) Uani 1 1 d . . . C7P C 0.3755(7) 0.1989(7) 0.2352(16) 0.056(4) Uani 1 1 d . . . N8P N 0.3643(6) 0.2374(6) 0.1857(15) 0.070(4) Uani 1 1 d . . . C9P C 0.4058(9) 0.2903(9) 0.1882(18) 0.084(6) Uani 1 1 d . . . H9P H 0.3985 0.3184 0.1524 0.101 Uiso 1 1 d R . . C10P C 0.4642(8) 0.3091(8) 0.242(2) 0.083(6) Uani 1 1 d . . . H10P H 0.4941 0.3478 0.2438 0.100 Uiso 1 1 d R . . C11P C 0.4702(8) 0.2625(7) 0.2942(19) 0.071(5) Uani 1 1 d . . . H11P H 0.5053 0.2698 0.3313 0.085 Uiso 1 1 d R . . N12P N 0.4254(5) 0.2078(5) 0.2907(14) 0.053(3) Uani 1 1 d . . . N1N N 0.4482(11) 0.1563(14) 0.0000 0.078(7) Uani 1 2 d S . . O1N O 0.3934(10) 0.1351(9) 0.0000 0.093(6) Uani 1 2 d S . . O2N O 0.4635(11) 0.1188(12) 0.0000 0.120(8) Uani 1 2 d S . . O3N O 0.4815(12) 0.2069(10) 0.0000 0.147(11) Uani 1 2 d S . . N2N N 0.3296(15) 0.2368(17) 0.5000 0.102(9) Uani 1 2 d S . . O4N O 0.3371(14) 0.1970(14) 0.5000 0.162(13) Uani 1 2 d S . . O5N O 0.2759(16) 0.2186(13) 0.5000 0.164(11) Uani 1 2 d S . . O6N O 0.3579(11) 0.2888(12) 0.5000 0.170(14) Uani 1 2 d S . . O1W O 0.2650(9) 0.2095(9) 0.0000 0.105(6) Uiso 1 2 d S . . O2W O 0.3368(10) 0.0066(9) 0.0000 0.118(7) Uiso 1 2 d S . . O3W O 0.5711(17) 0.3222(18) 0.0000 0.191(16) Uiso 0.80 2 d SP . . O4W O 0.5831(17) 0.1359(17) 0.0000 0.181(15) Uiso 0.80 2 d SP . . O5W O 0.1525(15) 0.1163(15) 0.0000 0.159(12) Uiso 0.80 2 d SP . . O6W O 0.1138(16) 0.0844(17) 0.274(4) 0.159(14) Uiso 0.50 1 d P . . O7W O 0.184(2) 0.113(2) 0.5000 0.19(2) Uiso 0.60 2 d SP . . 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 0.0422(4) 0.0478(4) 0.0519(4) 0.0007(3) 0.0027(3) 0.0244(3) N1P 0.037(7) 0.062(8) 0.058(8) 0.000(7) 0.002(6) 0.023(7) C2P 0.039(9) 0.060(10) 0.078(14) 0.001(9) 0.001(8) 0.013(8) C3P 0.072(12) 0.082(13) 0.087(15) -0.003(12) -0.022(12) 0.029(10) C4P 0.057(11) 0.110(17) 0.101(17) -0.013(14) -0.039(12) 0.034(12) N5P 0.066(10) 0.079(11) 0.092(13) 0.011(9) -0.017(9) 0.030(9) C6P 0.048(9) 0.081(12) 0.056(11) -0.012(10) -0.003(9) 0.039(9) C7P 0.067(10) 0.058(10) 0.052(11) 0.002(9) 0.006(9) 0.038(9) N8P 0.070(9) 0.059(9) 0.091(13) 0.003(8) -0.008(8) 0.040(8) C9P 0.123(17) 0.102(16) 0.069(14) 0.019(11) -0.010(12) 0.088(15) C10P 0.096(14) 0.077(12) 0.095(16) 0.015(12) -0.004(13) 0.057(11) C11P 0.070(11) 0.064(11) 0.083(13) 0.012(10) 0.016(10) 0.037(10) N12P 0.049(7) 0.053(7) 0.064(9) -0.002(7) -0.002(7) 0.031(6) N1N 0.068(15) 0.13(2) 0.031(12) 0.000 0.000 0.046(16) O1N 0.113(16) 0.142(17) 0.058(12) 0.000 0.000 0.089(15) O2N 0.124(19) 0.16(2) 0.089(17) 0.000 0.000 0.077(19) O3N 0.15(2) 0.076(14) 0.12(2) 0.000 0.000 -0.008(16) N2N 0.12(2) 0.17(3) 0.074(17) 0.000 0.000 0.12(3) O4N 0.29(4) 0.28(3) 0.068(15) 0.000 0.000 0.26(3) O5N 0.18(3) 0.18(3) 0.18(3) 0.000 0.000 0.13(3) O6N 0.13(2) 0.102(19) 0.24(4) 0.000 0.000 0.022(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 Pt N3A 1.92(2) 10_556 ? Pt N3B 1.94(3) 10_556 ? Pt N12P 2.000(12) . ? Pt N1P 2.027(11) . ? Pt N4A 2.12(2) . ? Pt N4B 2.14(3) . ? Pt Pt 3.1612(14) 10_556 ? N1A C2A 1.329(5) . ? N1A N8A 1.380(5) . ? C2A N3A 1.351(5) . ? N3A C3AA 1.349(5) . ? C3AA N4A 1.319(5) . ? C3AA N8A 1.377(5) . ? N4A C5A 1.361(5) . ? C5A C6A 1.369(5) . ? C6A C7A 1.390(5) . ? C7A O7A 1.25(2) . ? C7A N8A 1.409(5) . ? N1B C2B 1.329(5) . ? N1B N8B 1.380(5) . ? C2B N3B 1.352(5) . ? N3B C3AB 1.348(5) . ? C3AB N4B 1.318(5) . ? C3AB N8B 1.377(5) . ? N4B C5B 1.361(5) . ? C5B C6B 1.368(5) . ? C6B C7B 1.390(5) . ? C7B O7B 1.24(3) . ? C7B N8B 1.409(5) . ? N1P C2P 1.313(18) . ? N1P C6P 1.344(19) . ? C2P C3P 1.38(2) . ? C3P C4P 1.31(3) . ? C4P N5P 1.34(2) . ? N5P C6P 1.304(19) . ? C6P C7P 1.49(2) . ? C7P N8P 1.300(18) . ? C7P N12P 1.345(18) . ? N8P C9P 1.28(2) . ? C9P C10P 1.48(2) . ? C10P C11P 1.42(2) . ? C11P N12P 1.340(19) . ? N1N O3N 1.18(3) . ? N1N O2N 1.25(3) . ? N1N O1N 1.27(3) . ? N2N O4N 1.17(3) . ? N2N O6N 1.19(3) . ? N2N O5N 1.26(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3A Pt N3B 89.2(13) 10_556 10_556 ? N3A Pt N12P 94.5(9) 10_556 . ? N3B Pt N12P 170.6(8) 10_556 . ? N3A Pt N1P 171.7(7) 10_556 . ? N3B Pt N1P 94.0(10) 10_556 . ? N12P Pt N1P 81.2(5) . . ? N3B Pt N4A 91.9(12) 10_556 . ? N12P Pt N4A 93.0(8) . . ? N1P Pt N4A 174.1(8) . . ? N3A Pt N4B 87.2(12) 10_556 . ? N12P Pt N4B 177.7(9) . . ? N1P Pt N4B 96.9(10) . . ? N4A Pt N4B 88.9(12) . . ? C2A N1A N8A 102(2) . . ? N1A C2A N3A 117(3) . . ? C3AA N3A C2A 103(2) . . ? N4A C3AA N3A 129.2(12) . . ? N4A C3AA N8A 121.3(18) . . ? N3A C3AA N8A 109.4(17) . . ? C3AA N4A C5A 116(3) . . ? C3AA N4A Pt 126.4(16) . . ? C5A N4A Pt 117.1(17) . . ? N4A C5A C6A 124(3) . . ? C5A C6A C7A 121(3) . . ? O7A C7A C6A 129.7(19) . . ? O7A C7A N8A 118.2(18) . . ? C6A C7A N8A 112.1(19) . . ? C3AA N8A N1A 109.4(17) . . ? C3AA N8A C7A 124.5(15) . . ? N1A N8A C7A 126.0(15) . . ? C2B N1B N8B 107(3) . . ? N1B C2B N3B 110(3) . . ? C3AB N3B C2B 107(3) . . ? N4B C3AB N3B 131.0(13) . . ? N4B C3AB N8B 121(2) . . ? N3B C3AB N8B 108.0(19) . . ? C3AB N4B C5B 117(3) . . ? C3AB N4B Pt 125.1(19) . . ? C5B N4B Pt 117.2(19) . . ? N4B C5B C6B 123(4) . . ? C5B C6B C7B 121(3) . . ? O7B C7B C6B 128(2) . . ? O7B C7B N8B 120(2) . . ? C6B C7B N8B 112(2) . . ? C3AB N8B N1B 106.8(19) . . ? C3AB N8B C7B 124.0(16) . . ? N1B N8B C7B 129.0(17) . . ? C2P N1P C6P 120.4(13) . . ? C2P N1P Pt 126.3(11) . . ? C6P N1P Pt 113.4(10) . . ? N1P C2P C3P 115.5(16) . . ? C4P C3P C2P 121.3(18) . . ? C3P C4P N5P 123.3(17) . . ? C6P N5P C4P 113.8(16) . . ? N5P C6P N1P 125.6(15) . . ? N5P C6P C7P 118.7(15) . . ? N1P C6P C7P 115.6(13) . . ? N8P C7P N12P 128.0(15) . . ? N8P C7P C6P 117.8(14) . . ? N12P C7P C6P 114.1(13) . . ? C9P N8P C7P 116.4(15) . . ? N8P C9P C10P 124.1(15) . . ? C11P C10P C9P 113.4(17) . . ? N12P C11P C10P 120.5(17) . . ? C11P N12P C7P 117.5(14) . . ? C11P N12P Pt 127.2(11) . . ? C7P N12P Pt 115.0(10) . . ? O3N N1N O2N 123(3) . . ? O3N N1N O1N 123(3) . . ? O2N N1N O1N 114(3) . . ? O4N N2N O6N 139(4) . . ? O4N N2N O5N 109(4) . . ? O6N N2N O5N 112(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.385 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.193