# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address A.F.Dalebrook ; Department of Chemistry The University of Auckland Private Bag 92019 Auckland New Zealand ; Kim.Meyer ; Department of Chemistry The University of Auckland Private Bag 92019 Auckland New Zealand ; L.J.Wright ; Department of Chemistry The University of Auckland Private Bag 92019 Auckland New Zealand ; _publ_contact_author_address ; School of Chemical Sciences The University of Auckland Private Bag 92019 Auckland New Zealand ; _publ_contact_author_email lj.wright@auckland.ac.nz _publ_contact_author_fax '0064 9 3737422' _publ_contact_author_phone '0064 9 3737599 Ext 88257' _publ_contact_author_name 'L. J. Wright' #TrackingRef '- Combined Structures.cif' _publ_contact_letter ; Please consider this CIF for publication. I certify that this contibution is the original work of those listed as authors; that it has not been published before (in any language or medium) and is not being considered for publication elsewhere; that all authors concur with and are aware of the submission; that all workers involved in the study are listed as authors or given proper credit in the acknowledgements; that I have obtained permission for and acknowledged the source of any excerpts from other copyright works; and that to the best of my knowledge the paper contains no statements which are libellous, unlawful or in any way actionable. All coauthors have made significant scientific contributions to the work reported, including the ideas and their execution, and share responsibility and accountability for the results. ; data_2 _database_code_depnum_ccdc_archive 'CCDC 893433' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H31 N11 O4, 4(C H4 O), H2 O' _chemical_formula_sum 'C41 H49 N11 O9' _chemical_formula_weight 839.91 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' _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 11.353(5) _cell_length_b 13.359(5) _cell_length_c 14.031(5) _cell_angle_alpha 90.767(5) _cell_angle_beta 93.754(5) _cell_angle_gamma 105.809(5) _cell_volume 2042.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9987 _cell_measurement_theta_min 4.373 _cell_measurement_theta_max 55.812 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.981 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48885 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.95 _reflns_number_total 9683 _reflns_number_gt 7457 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0908P)^2^+1.4527P] 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 9683 _refine_ls_number_parameters 566 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.188 _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 C1 C 0.6710(2) 0.54997(17) 0.69112(16) 0.0217(4) Uani 1 1 d . . . C2 C 0.7099(2) 0.59700(16) 0.79032(15) 0.0197(4) Uani 1 1 d . . . C3 C 0.6410(2) 0.65525(18) 0.83288(17) 0.0241(5) Uani 1 1 d . . . H3 H 0.5652 0.6600 0.8030 0.029 Uiso 1 1 calc R . . C4 C 0.6864(2) 0.70578(19) 0.91966(17) 0.0271(5) Uani 1 1 d . . . H4 H 0.6411 0.7450 0.9511 0.033 Uiso 1 1 calc R . . C5 C 0.7983(2) 0.69903(18) 0.96069(16) 0.0238(5) Uani 1 1 d . . . H5 H 0.8318 0.7344 1.0196 0.029 Uiso 1 1 calc R . . C6 C 0.8600(2) 0.63892(16) 0.91306(15) 0.0186(4) Uani 1 1 d . . . C7 C 0.9850(2) 0.63376(16) 0.95234(15) 0.0188(4) Uani 1 1 d . . . C8 C 0.7561(2) 0.46324(16) 0.56507(15) 0.0190(4) Uani 1 1 d . . . C9 C 0.6799(2) 0.47599(17) 0.48673(16) 0.0214(4) Uani 1 1 d . . . H9 H 0.6135 0.5054 0.4938 0.026 Uiso 1 1 calc R . . C10 C 0.7057(2) 0.44365(17) 0.39778(16) 0.0228(5) Uani 1 1 d . . . H10 H 0.6559 0.4510 0.3426 0.027 Uiso 1 1 calc R . . C11 C 0.8026(2) 0.40099(17) 0.38819(15) 0.0220(4) Uani 1 1 d . . . H11 H 0.8223 0.3809 0.3273 0.026 Uiso 1 1 calc R . . C12 C 0.8703(2) 0.38874(15) 0.47207(15) 0.0190(4) Uani 1 1 d . . . C13 C 1.15143(19) 0.55625(16) 0.90986(15) 0.0184(4) Uani 1 1 d . . . C14 C 1.2411(2) 0.60442(17) 0.98095(16) 0.0220(4) Uani 1 1 d . . . H14 H 1.2274 0.6529 1.0261 0.026 Uiso 1 1 calc R . . C15 C 1.3515(2) 0.57831(18) 0.98278(16) 0.0244(5) Uani 1 1 d . . . H15 H 1.4151 0.6097 1.0300 0.029 Uiso 1 1 calc R . . C16 C 1.3702(2) 0.50721(17) 0.91688(16) 0.0215(4) Uani 1 1 d . . . H16 H 1.4456 0.4891 0.9177 0.026 Uiso 1 1 calc R . . C17 C 1.27348(19) 0.46318(16) 0.84910(15) 0.0179(4) Uani 1 1 d . . . C18 C 1.0123(2) 0.30079(16) 0.40278(16) 0.0211(4) Uani 1 1 d . . . C19 C 1.1115(2) 0.24905(17) 0.43578(17) 0.0237(5) Uani 1 1 d . . . H19A H 1.1858 0.3034 0.4605 0.028 Uiso 1 1 calc R . . H19B H 1.0823 0.2028 0.4889 0.028 Uiso 1 1 calc R . . C20 C 1.1454(2) 0.18587(17) 0.35656(17) 0.0241(5) Uani 1 1 d . . . H20A H 1.1568 0.2278 0.2985 0.029 Uiso 1 1 calc R . . H20B H 1.2249 0.1723 0.3760 0.029 Uiso 1 1 calc R . . C21 C 1.3746(2) 0.35545(16) 0.75381(15) 0.0201(4) Uani 1 1 d . . . C22 C 1.3477(2) 0.28762(17) 0.66247(16) 0.0221(4) Uani 1 1 d . . . H22A H 1.2763 0.2270 0.6701 0.026 Uiso 1 1 calc R . . H22B H 1.3261 0.3282 0.6088 0.026 Uiso 1 1 calc R . . C23 C 1.4567(2) 0.24954(18) 0.63902(17) 0.0254(5) Uani 1 1 d . . . H23A H 1.5288 0.3102 0.6335 0.030 Uiso 1 1 calc R . . H23B H 1.4767 0.2072 0.6919 0.030 Uiso 1 1 calc R . . C24 C 1.0490(2) -0.00484(17) 0.37714(17) 0.0249(5) Uani 1 1 d . . . H24 H 1.0956 -0.0084 0.4351 0.030 Uiso 1 1 calc R . . C25 C 0.9758(2) 0.06034(17) 0.25068(16) 0.0230(5) Uani 1 1 d . . . C26 C 0.9467(2) 0.12007(19) 0.17619(18) 0.0291(5) Uani 1 1 d . . . H26 H 0.9795 0.1935 0.1768 0.035 Uiso 1 1 calc R . . C27 C 0.8683(3) 0.0670(2) 0.10203(19) 0.0358(6) Uani 1 1 d . . . H27 H 0.8464 0.1049 0.0501 0.043 Uiso 1 1 calc R . . C28 C 0.8198(3) -0.0416(2) 0.1010(2) 0.0395(6) Uani 1 1 d . . . H28 H 0.7668 -0.0755 0.0480 0.047 Uiso 1 1 calc R . . C29 C 0.8472(3) -0.1003(2) 0.17493(19) 0.0346(6) Uani 1 1 d . . . H29 H 0.8130 -0.1736 0.1743 0.041 Uiso 1 1 calc R . . C30 C 0.9271(2) -0.04807(18) 0.25088(17) 0.0260(5) Uani 1 1 d . . . C31 C 1.4753(2) 0.21860(18) 0.46324(17) 0.0262(5) Uani 1 1 d . . . H31 H 1.5192 0.2884 0.4520 0.031 Uiso 1 1 calc R . . C32 C 1.3739(2) 0.08172(17) 0.53818(16) 0.0211(4) Uani 1 1 d . . . C33 C 1.3129(2) 0.00870(18) 0.60131(17) 0.0248(5) Uani 1 1 d . . . H33 H 1.3047 0.0271 0.6657 0.030 Uiso 1 1 calc R . . C34 C 1.2651(2) -0.09199(18) 0.56471(18) 0.0274(5) Uani 1 1 d . . . H34 H 1.2218 -0.1440 0.6049 0.033 Uiso 1 1 calc R . . C35 C 1.2787(2) -0.11948(18) 0.46993(18) 0.0275(5) Uani 1 1 d . . . H35 H 1.2456 -0.1898 0.4480 0.033 Uiso 1 1 calc R . . C36 C 1.3392(2) -0.04687(18) 0.40775(17) 0.0250(5) Uani 1 1 d . . . H36 H 1.3483 -0.0660 0.3438 0.030 Uiso 1 1 calc R . . C37 C 1.3863(2) 0.05573(17) 0.44260(16) 0.0218(4) Uani 1 1 d . . . C38 C 0.7737(3) 0.2851(2) 0.7760(2) 0.0409(6) Uani 1 1 d . . . H38A H 0.7767 0.2227 0.8108 0.061 Uiso 1 1 calc R . . H38B H 0.7501 0.2662 0.7083 0.061 Uiso 1 1 calc R . . H38C H 0.7132 0.3158 0.8025 0.061 Uiso 1 1 calc R . . C39 C 0.5137(4) 0.1420(4) 0.9077(3) 0.0691(11) Uani 1 1 d . . . H39A H 0.5939 0.1659 0.9434 0.104 Uiso 1 1 calc R . . H39B H 0.4584 0.0890 0.9438 0.104 Uiso 1 1 calc R . . H39C H 0.4789 0.2010 0.8980 0.104 Uiso 1 1 calc R . . C40 C 0.3684(3) 0.8235(3) 0.8069(2) 0.0487(8) Uani 1 1 d . . . H40A H 0.3517 0.8008 0.8720 0.073 Uiso 1 1 calc R . . H40B H 0.3100 0.7760 0.7610 0.073 Uiso 1 1 calc R . . H40C H 0.3596 0.8941 0.8002 0.073 Uiso 1 1 calc R . . C41 C 0.7786(4) 0.9758(3) 0.8434(3) 0.0615(10) Uani 1 1 d . . . H41A H 0.8352 1.0436 0.8628 0.092 Uiso 1 1 calc R . . H41B H 0.7661 0.9704 0.7735 0.092 Uiso 1 1 calc R . . H41C H 0.8134 0.9203 0.8664 0.092 Uiso 1 1 calc R . . N1 N 0.74840(17) 0.49751(14) 0.65858(13) 0.0211(4) Uani 1 1 d . . . H1 H 0.8005 0.4832 0.7020 0.025 Uiso 1 1 calc R . . N2 N 0.81649(16) 0.58800(13) 0.82982(12) 0.0180(4) Uani 1 1 d . . . N3 N 1.03541(17) 0.57473(15) 0.89725(13) 0.0206(4) Uani 1 1 d . . . H3A H 0.9893 0.5437 0.8467 0.025 Uiso 1 1 calc R . . N4 N 0.84788(17) 0.41931(13) 0.55857(13) 0.0192(4) Uani 1 1 d . . . N5 N 1.16626(16) 0.48705(14) 0.84519(12) 0.0184(4) Uani 1 1 d . . . N6 N 0.96600(17) 0.34088(14) 0.47707(13) 0.0205(4) Uani 1 1 d . . . H6 H 0.9999 0.3362 0.5344 0.025 Uiso 1 1 calc RD . . N7 N 1.27708(16) 0.38984(14) 0.77729(13) 0.0189(4) Uani 1 1 d . . . H7 H 1.2076 0.3626 0.7431 0.023 Uiso 1 1 calc R . . N8 N 1.05414(18) 0.08601(14) 0.33254(14) 0.0221(4) Uani 1 1 d . . . N9 N 0.9736(2) -0.08737(15) 0.33245(15) 0.0283(4) Uani 1 1 d . . . N10 N 1.43309(17) 0.18688(14) 0.54968(14) 0.0229(4) Uani 1 1 d . . . N11 N 1.44991(18) 0.14425(15) 0.39702(14) 0.0256(4) Uani 1 1 d . . . O1 O 0.58156(16) 0.56357(14) 0.64500(12) 0.0309(4) Uani 1 1 d . . . O2 O 1.03321(15) 0.68126(13) 1.02651(11) 0.0245(3) Uani 1 1 d . . . O3 O 0.98164(16) 0.30616(13) 0.31854(11) 0.0278(4) Uani 1 1 d . . . O4 O 1.47422(15) 0.37659(14) 0.79929(12) 0.0287(4) Uani 1 1 d . . . O5 O 1.05063(15) 0.30290(12) 0.66453(11) 0.0225(3) Uani 1 1 d D . . O7 O 0.5275(3) 0.0995(2) 0.8194(2) 0.0714(8) Uani 1 1 d D . . O8 O 0.4860(3) 0.8231(3) 0.78932(18) 0.0833(11) Uani 1 1 d D . . O9 O 0.6643(3) 0.9660(3) 0.8832(2) 0.0775(9) Uani 1 1 d D . . O6 O 0.89017(17) 0.35790(14) 0.78496(12) 0.0304(4) Uani 1 1 d D . . H5B H 1.034(3) 0.2378(16) 0.667(2) 0.046 Uiso 1 1 d D . . H5C H 0.989(3) 0.315(3) 0.705(2) 0.046 Uiso 1 1 d . . . H7A H 0.5710 0.0433 0.8408 0.046 Uiso 1 1 d D . . H8A H 0.4993 0.8366 0.7234 0.046 Uiso 1 1 d D . . H9A H 0.609(3) 0.916(2) 0.844(2) 0.046 Uiso 1 1 d D . . H6A H 0.921(3) 0.350(3) 0.8429(16) 0.046 Uiso 1 1 d 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 C1 0.0195(10) 0.0228(10) 0.0232(11) 0.0007(8) -0.0004(8) 0.0070(8) C2 0.0192(10) 0.0187(10) 0.0213(10) 0.0017(8) 0.0019(8) 0.0050(8) C3 0.0202(11) 0.0256(11) 0.0285(12) -0.0002(9) 0.0017(9) 0.0097(9) C4 0.0276(12) 0.0286(12) 0.0291(12) -0.0029(9) 0.0056(9) 0.0140(10) C5 0.0268(12) 0.0251(11) 0.0212(11) -0.0029(8) 0.0019(9) 0.0101(9) C6 0.0199(10) 0.0178(9) 0.0182(10) 0.0009(8) 0.0018(8) 0.0052(8) C7 0.0208(10) 0.0194(10) 0.0167(10) 0.0011(8) 0.0013(8) 0.0062(8) C8 0.0189(10) 0.0164(9) 0.0202(10) -0.0006(8) -0.0019(8) 0.0029(8) C9 0.0199(10) 0.0209(10) 0.0230(11) 0.0022(8) -0.0032(8) 0.0060(8) C10 0.0239(11) 0.0228(10) 0.0193(10) 0.0046(8) -0.0041(8) 0.0038(9) C11 0.0253(11) 0.0227(10) 0.0169(10) 0.0024(8) -0.0004(8) 0.0048(9) C12 0.0200(10) 0.0138(9) 0.0214(10) 0.0012(8) -0.0002(8) 0.0022(8) C13 0.0184(10) 0.0211(10) 0.0163(9) 0.0011(8) 0.0000(8) 0.0066(8) C14 0.0235(11) 0.0236(10) 0.0190(10) -0.0055(8) -0.0015(8) 0.0074(9) C15 0.0205(11) 0.0294(12) 0.0218(11) -0.0068(9) -0.0061(8) 0.0063(9) C16 0.0187(10) 0.0235(10) 0.0225(11) -0.0019(8) -0.0023(8) 0.0070(8) C17 0.0193(10) 0.0176(9) 0.0165(10) 0.0001(7) 0.0010(8) 0.0044(8) C18 0.0214(11) 0.0177(10) 0.0228(11) -0.0005(8) 0.0004(8) 0.0031(8) C19 0.0242(11) 0.0211(10) 0.0256(11) -0.0017(9) -0.0009(9) 0.0067(9) C20 0.0204(11) 0.0225(11) 0.0292(12) -0.0005(9) 0.0033(9) 0.0052(9) C21 0.0227(11) 0.0183(10) 0.0197(10) -0.0001(8) 0.0016(8) 0.0061(8) C22 0.0219(11) 0.0227(10) 0.0226(11) -0.0042(8) -0.0009(8) 0.0085(9) C23 0.0218(11) 0.0261(11) 0.0278(12) -0.0097(9) -0.0002(9) 0.0070(9) C24 0.0303(12) 0.0226(11) 0.0244(11) 0.0020(9) 0.0057(9) 0.0106(9) C25 0.0248(11) 0.0223(11) 0.0220(11) -0.0026(8) 0.0037(9) 0.0063(9) C26 0.0350(13) 0.0241(11) 0.0285(12) 0.0023(9) 0.0028(10) 0.0081(10) C27 0.0465(16) 0.0333(13) 0.0280(13) 0.0015(10) -0.0029(11) 0.0129(12) C28 0.0471(17) 0.0371(14) 0.0286(13) -0.0069(11) -0.0038(12) 0.0038(12) C29 0.0450(16) 0.0239(12) 0.0303(13) -0.0043(10) 0.0041(11) 0.0017(11) C30 0.0312(13) 0.0216(11) 0.0249(11) -0.0008(9) 0.0066(9) 0.0059(9) C31 0.0231(11) 0.0230(11) 0.0318(12) -0.0013(9) 0.0068(9) 0.0040(9) C32 0.0184(10) 0.0218(10) 0.0239(11) -0.0034(8) 0.0013(8) 0.0072(8) C33 0.0243(11) 0.0277(11) 0.0232(11) -0.0004(9) 0.0027(9) 0.0083(9) C34 0.0274(12) 0.0243(11) 0.0294(12) 0.0046(9) 0.0010(9) 0.0051(9) C35 0.0299(13) 0.0199(11) 0.0318(13) -0.0028(9) -0.0023(10) 0.0067(9) C36 0.0278(12) 0.0247(11) 0.0241(11) -0.0041(9) -0.0013(9) 0.0105(9) C37 0.0205(11) 0.0233(11) 0.0235(11) -0.0014(8) 0.0023(8) 0.0092(9) C38 0.0410(16) 0.0422(15) 0.0353(15) -0.0001(12) -0.0005(12) 0.0049(12) C39 0.078(3) 0.078(3) 0.050(2) -0.0011(19) 0.0079(19) 0.018(2) C40 0.0515(19) 0.063(2) 0.0310(15) 0.0087(14) 0.0103(13) 0.0123(16) C41 0.070(2) 0.085(3) 0.0448(19) 0.0144(18) 0.0193(17) 0.044(2) N1 0.0213(9) 0.0247(9) 0.0186(9) -0.0021(7) -0.0051(7) 0.0101(7) N2 0.0190(9) 0.0178(8) 0.0176(8) 0.0013(7) 0.0008(7) 0.0057(7) N3 0.0189(9) 0.0269(9) 0.0168(9) -0.0063(7) -0.0042(7) 0.0092(7) N4 0.0205(9) 0.0168(8) 0.0196(9) 0.0000(7) -0.0022(7) 0.0052(7) N5 0.0185(9) 0.0207(8) 0.0165(8) -0.0012(7) -0.0005(7) 0.0066(7) N6 0.0225(9) 0.0209(9) 0.0184(9) -0.0004(7) -0.0023(7) 0.0077(7) N7 0.0169(9) 0.0208(9) 0.0190(9) -0.0041(7) -0.0025(7) 0.0062(7) N8 0.0234(10) 0.0191(9) 0.0245(9) 0.0001(7) 0.0042(7) 0.0064(7) N9 0.0383(12) 0.0208(9) 0.0263(10) 0.0007(8) 0.0065(9) 0.0081(8) N10 0.0201(9) 0.0216(9) 0.0267(10) -0.0054(7) 0.0045(7) 0.0051(7) N11 0.0247(10) 0.0237(9) 0.0285(10) -0.0005(8) 0.0071(8) 0.0056(8) O1 0.0257(9) 0.0429(10) 0.0279(9) -0.0044(7) -0.0078(7) 0.0186(8) O2 0.0268(9) 0.0285(8) 0.0191(8) -0.0051(6) -0.0025(6) 0.0102(7) O3 0.0327(9) 0.0341(9) 0.0200(8) 0.0007(7) 0.0008(7) 0.0151(7) O4 0.0217(8) 0.0360(9) 0.0298(9) -0.0110(7) -0.0057(7) 0.0123(7) O5 0.0248(8) 0.0215(8) 0.0223(8) -0.0025(6) -0.0027(6) 0.0092(6) O7 0.093(2) 0.0682(17) 0.0569(16) 0.0084(13) 0.0102(15) 0.0271(16) O8 0.081(2) 0.161(3) 0.0384(13) 0.0309(16) 0.0233(13) 0.079(2) O9 0.074(2) 0.117(3) 0.0578(17) -0.0068(16) 0.0171(14) 0.0515(19) O6 0.0317(9) 0.0364(10) 0.0235(9) -0.0017(7) -0.0030(7) 0.0111(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.225(3) . ? C1 N1 1.361(3) . ? C1 C2 1.507(3) . ? C2 N2 1.334(3) . ? C2 C3 1.398(3) . ? C3 C4 1.382(3) . ? C4 C5 1.386(3) . ? C5 C6 1.391(3) . ? C6 N2 1.338(3) . ? C6 C7 1.508(3) . ? C7 O2 1.226(3) . ? C7 N3 1.355(3) . ? C8 N4 1.335(3) . ? C8 C9 1.395(3) . ? C8 N1 1.400(3) . ? C9 C10 1.390(3) . ? C10 C11 1.383(3) . ? C11 C12 1.400(3) . ? C12 N4 1.337(3) . ? C12 N6 1.401(3) . ? C13 N5 1.337(3) . ? C13 C14 1.393(3) . ? C13 N3 1.405(3) . ? C14 C15 1.388(3) . ? C15 C16 1.384(3) . ? C16 C17 1.397(3) . ? C17 N5 1.338(3) . ? C17 N7 1.406(3) . ? C18 O3 1.219(3) . ? C18 N6 1.364(3) . ? C18 C19 1.525(3) . ? C19 C20 1.518(3) . ? C20 N8 1.468(3) . ? C21 O4 1.222(3) . ? C21 N7 1.366(3) . ? C21 C22 1.524(3) . ? C22 C23 1.514(3) . ? C23 N10 1.466(3) . ? C24 N9 1.319(3) . ? C24 N8 1.362(3) . ? C25 N8 1.385(3) . ? C25 C26 1.400(3) . ? C25 C30 1.403(3) . ? C26 C27 1.376(4) . ? C27 C28 1.405(4) . ? C28 C29 1.379(4) . ? C29 C30 1.397(4) . ? C30 N9 1.397(3) . ? C31 N11 1.310(3) . ? C31 N10 1.364(3) . ? C32 N10 1.384(3) . ? C32 C33 1.397(3) . ? C32 C37 1.407(3) . ? C33 C34 1.384(3) . ? C34 C35 1.404(4) . ? C35 C36 1.383(3) . ? C36 C37 1.397(3) . ? C37 N11 1.394(3) . ? C38 O6 1.409(3) . ? C39 O7 1.392(5) . ? C40 O8 1.375(4) . ? C41 O9 1.421(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 O1 C1 N1 125.2(2) . . ? O1 C1 C2 121.7(2) . . ? N1 C1 C2 113.07(19) . . ? N2 C2 C3 123.0(2) . . ? N2 C2 C1 116.87(19) . . ? C3 C2 C1 119.9(2) . . ? C4 C3 C2 118.0(2) . . ? C3 C4 C5 119.7(2) . . ? C4 C5 C6 118.1(2) . . ? N2 C6 C5 123.1(2) . . ? N2 C6 C7 116.91(18) . . ? C5 C6 C7 119.9(2) . . ? O2 C7 N3 125.6(2) . . ? O2 C7 C6 120.98(19) . . ? N3 C7 C6 113.45(18) . . ? N4 C8 C9 123.5(2) . . ? N4 C8 N1 112.08(18) . . ? C9 C8 N1 124.4(2) . . ? C10 C9 C8 116.8(2) . . ? C11 C10 C9 121.1(2) . . ? C10 C11 C12 117.1(2) . . ? N4 C12 C11 123.1(2) . . ? N4 C12 N6 111.71(18) . . ? C11 C12 N6 125.1(2) . . ? N5 C13 C14 123.6(2) . . ? N5 C13 N3 112.13(18) . . ? C14 C13 N3 124.2(2) . . ? C15 C14 C13 116.9(2) . . ? C16 C15 C14 121.0(2) . . ? C15 C16 C17 117.1(2) . . ? N5 C17 C16 123.3(2) . . ? N5 C17 N7 112.24(18) . . ? C16 C17 N7 124.50(19) . . ? O3 C18 N6 125.2(2) . . ? O3 C18 C19 122.2(2) . . ? N6 C18 C19 112.56(19) . . ? C20 C19 C18 112.85(19) . . ? N8 C20 C19 114.17(18) . . ? O4 C21 N7 124.8(2) . . ? O4 C21 C22 122.3(2) . . ? N7 C21 C22 112.90(19) . . ? C23 C22 C21 111.67(19) . . ? N10 C23 C22 112.08(19) . . ? N9 C24 N8 113.9(2) . . ? N8 C25 C26 132.3(2) . . ? N8 C25 C30 105.5(2) . . ? C26 C25 C30 122.1(2) . . ? C27 C26 C25 116.6(2) . . ? C26 C27 C28 121.8(2) . . ? C29 C28 C27 121.5(3) . . ? C28 C29 C30 117.7(2) . . ? N9 C30 C29 129.9(2) . . ? N9 C30 C25 109.8(2) . . ? C29 C30 C25 120.2(2) . . ? N11 C31 N10 114.0(2) . . ? N10 C32 C33 132.1(2) . . ? N10 C32 C37 105.37(19) . . ? C33 C32 C37 122.6(2) . . ? C34 C33 C32 116.2(2) . . ? C33 C34 C35 121.9(2) . . ? C36 C35 C34 121.7(2) . . ? C35 C36 C37 117.5(2) . . ? N11 C37 C36 130.1(2) . . ? N11 C37 C32 109.65(19) . . ? C36 C37 C32 120.2(2) . . ? C1 N1 C8 128.51(18) . . ? C2 N2 C6 118.12(19) . . ? C7 N3 C13 128.81(19) . . ? C8 N4 C12 118.31(18) . . ? C18 N6 C12 127.15(19) . . ? C13 N5 C17 117.99(18) . . ? C21 N7 C17 128.34(19) . . ? C24 N8 C25 106.45(19) . . ? C24 N8 C20 125.2(2) . . ? C25 N8 C20 127.10(19) . . ? C24 N9 C30 104.35(19) . . ? C31 N10 C32 106.34(18) . . ? C31 N10 C23 126.5(2) . . ? C32 N10 C23 126.92(19) . . ? C31 N11 C37 104.66(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.125 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.064 #===END data_[HgL2][HgBr4] _database_code_depnum_ccdc_archive 'CCDC 893434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 Hg N12 O4, Br4 Hg, 2(H2 O)' _chemical_formula_sum 'C44 H40 Br4 Hg2 N12 O6' _chemical_formula_weight 1553.70 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' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -4.2923 7.6849 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/a _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.1125(12) _cell_length_b 22.6846(9) _cell_length_c 17.6153(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.727(8) _cell_angle_gamma 90.00 _cell_volume 5684.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2484 _cell_measurement_theta_min 6.12 _cell_measurement_theta_max 70.16 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 13.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.079 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58453 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 6.52 _diffrn_reflns_theta_max 72.10 _reflns_number_total 10893 _reflns_number_gt 8422 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^+0.1904P] 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 10893 _refine_ls_number_parameters 620 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1257 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 C1 C 0.2244(5) 0.1061(3) -0.1314(4) 0.0547(17) Uani 1 1 d . . . C2 C 0.2216(4) 0.0404(3) -0.1190(4) 0.0501(16) Uani 1 1 d . . . C3 C 0.1476(5) 0.0086(3) -0.1706(4) 0.0564(18) Uani 1 1 d . . . H3 H 0.1005 0.0275 -0.2137 0.068 Uiso 1 1 calc R . . C4 C 0.1438(4) -0.0499(3) -0.1581(4) 0.0585(18) Uani 1 1 d . . . H4 H 0.0933 -0.0727 -0.1924 0.070 Uiso 1 1 calc R . . C5 C 0.2129(4) -0.0764(3) -0.0960(4) 0.0596(18) Uani 1 1 d . . . H5 H 0.2118 -0.1176 -0.0864 0.072 Uiso 1 1 calc R . . C6 C 0.2859(4) -0.0403(3) -0.0469(3) 0.0469(15) Uani 1 1 d . . . C7 C 0.3619(4) -0.0695(3) 0.0220(4) 0.0502(16) Uani 1 1 d . . . C8 C 0.3292(5) 0.1929(3) -0.0799(4) 0.0507(16) Uani 1 1 d . . . C9 C 0.2688(5) 0.2377(4) -0.1235(4) 0.069(2) Uani 1 1 d . . . H9 H 0.2052 0.2300 -0.1550 0.083 Uiso 1 1 calc R . . C10 C 0.3078(6) 0.2940(3) -0.1179(5) 0.069(2) Uani 1 1 d . . . H10 H 0.2698 0.3260 -0.1451 0.083 Uiso 1 1 calc R . . C11 C 0.3975(5) 0.3032(3) -0.0748(4) 0.0600(19) Uani 1 1 d . . . H11 H 0.4238 0.3416 -0.0712 0.072 Uiso 1 1 calc R . . C12 C 0.4519(5) 0.2565(3) -0.0354(4) 0.0496(16) Uani 1 1 d . . . C13 C 0.5082(4) -0.0474(3) 0.1318(3) 0.0461(15) Uani 1 1 d . . . C14 C 0.5335(5) -0.1055(2) 0.1547(4) 0.0500(16) Uani 1 1 d . . . H14 H 0.4974 -0.1376 0.1257 0.060 Uiso 1 1 calc R . . C15 C 0.6131(5) -0.1145(3) 0.2209(4) 0.0511(16) Uani 1 1 d . . . H15 H 0.6321 -0.1536 0.2383 0.061 Uiso 1 1 calc R . . C16 C 0.6662(4) -0.0670(2) 0.2628(4) 0.0466(15) Uani 1 1 d . . . H16 H 0.7218 -0.0730 0.3077 0.056 Uiso 1 1 calc R . . C17 C 0.6348(4) -0.0113(2) 0.2365(3) 0.0423(14) Uani 1 1 d . . . C18 C 0.6098(5) 0.3030(3) 0.0093(4) 0.0593(19) Uani 1 1 d . . . C19 C 0.7097(5) 0.2910(3) 0.0627(4) 0.0565(19) Uani 1 1 d . . . H19A H 0.7442 0.2728 0.0299 0.068 Uiso 1 1 calc R . . H19B H 0.7090 0.2622 0.1048 0.068 Uiso 1 1 calc R . . C20 C 0.7620(5) 0.3456(3) 0.1033(4) 0.0549(17) Uani 1 1 d . A . H20A H 0.8267 0.3347 0.1372 0.066 Uiso 1 1 calc R . . H20B H 0.7662 0.3738 0.0617 0.066 Uiso 1 1 calc R . . C21 C 0.7654(4) 0.0464(2) 0.3294(3) 0.0409(14) Uani 1 1 d . . . C22 C 0.7910(4) 0.1070(2) 0.3682(3) 0.0425(14) Uani 1 1 d . . . H22A H 0.8136 0.1029 0.4277 0.051 Uiso 1 1 calc R . . H22B H 0.7344 0.1324 0.3524 0.051 Uiso 1 1 calc R . . C23 C 0.8676(4) 0.1361(2) 0.3419(3) 0.0407(14) Uani 1 1 d . . . H23A H 0.9144 0.1061 0.3399 0.049 Uiso 1 1 calc R . . H23B H 0.8392 0.1530 0.2872 0.049 Uiso 1 1 calc R . . C24 C 0.7144(4) 0.3544(3) 0.2260(4) 0.0448(15) Uani 1 1 d . A . C25 C 0.6531(11) 0.4202(6) 0.1253(8) 0.049(4) Uiso 0.510(15) 1 d PD A 1 C26 C 0.6304(11) 0.4561(6) 0.0572(8) 0.056(4) Uiso 0.510(15) 1 d PD A 1 H26 H 0.6490 0.4463 0.0123 0.067 Uiso 0.510(15) 1 calc PR A 1 C27 C 0.5808(10) 0.5056(6) 0.0580(8) 0.057(4) Uiso 0.510(15) 1 d PD A 1 H27 H 0.5637 0.5304 0.0119 0.069 Uiso 0.510(15) 1 calc PR A 1 C28 C 0.5533(11) 0.5222(6) 0.1236(8) 0.062(4) Uiso 0.510(15) 1 d PD A 1 H28 H 0.5180 0.5572 0.1213 0.074 Uiso 0.510(15) 1 calc PR A 1 C29 C 0.5791(10) 0.4860(6) 0.1931(8) 0.048(3) Uiso 0.510(15) 1 d PD A 1 H29 H 0.5626 0.4963 0.2390 0.057 Uiso 0.510(15) 1 calc PR A 1 C30 C 0.6291(11) 0.4351(6) 0.1918(8) 0.045(4) Uiso 0.510(15) 1 d PD A 1 C25A C 0.6751(10) 0.4342(6) 0.1475(8) 0.044(4) Uiso 0.490(15) 1 d PD A 2 C26A C 0.6691(10) 0.4748(5) 0.0854(8) 0.044(3) Uiso 0.490(15) 1 d PD A 2 H26A H 0.6937 0.4673 0.0433 0.053 Uiso 0.490(15) 1 calc PR A 2 C27A C 0.6235(12) 0.5274(6) 0.0920(9) 0.063(5) Uiso 0.490(15) 1 d PD A 2 H27A H 0.6123 0.5558 0.0501 0.075 Uiso 0.490(15) 1 calc PR A 2 C28A C 0.5934(12) 0.5401(6) 0.1576(8) 0.062(4) Uiso 0.490(15) 1 d PD A 2 H28A H 0.5648 0.5771 0.1596 0.075 Uiso 0.490(15) 1 calc PR A 2 C29A C 0.6049(11) 0.4992(6) 0.2204(8) 0.050(4) Uiso 0.490(15) 1 d PD A 2 H29A H 0.5844 0.5067 0.2649 0.060 Uiso 0.490(15) 1 calc PR A 2 C30A C 0.6476(10) 0.4482(6) 0.2120(8) 0.038(3) Uiso 0.490(15) 1 d P A 2 C31 C 0.8983(4) 0.2417(2) 0.3915(3) 0.0374(13) Uani 1 1 d . A . C32 C 0.9825(4) 0.1708(2) 0.4740(3) 0.0400(13) Uani 1 1 d D . . C33 C 1.0245(4) 0.1185(2) 0.5059(4) 0.0486(16) Uani 1 1 d D . . H33 H 1.0079 0.0821 0.4781 0.058 Uiso 1 1 calc R . . C34 C 1.0933(4) 0.1225(3) 0.5822(4) 0.0581(18) Uani 1 1 d D . . H34 H 1.1251 0.0877 0.6070 0.070 Uiso 1 1 calc R . . C35 C 1.1168(5) 0.1761(3) 0.6232(4) 0.0589(18) Uani 1 1 d D . . H35 H 1.1627 0.1766 0.6756 0.071 Uiso 1 1 calc R . . C36 C 1.0742(4) 0.2292(3) 0.5886(3) 0.0427(14) Uani 1 1 d D . . H36 H 1.0913 0.2660 0.6153 0.051 Uiso 1 1 calc R . . C37 C 1.0057(4) 0.2248(2) 0.5131(3) 0.0359(12) Uani 1 1 d D . . C38 C 0.6486(4) 0.3887(3) 0.3313(4) 0.0455(15) Uani 1 1 d . A . H38A H 0.6223 0.3492 0.3343 0.055 Uiso 1 1 calc R . . H38B H 0.6002 0.4182 0.3308 0.055 Uiso 1 1 calc R . . C39 C 0.7337(4) 0.3981(3) 0.4058(4) 0.0459(15) Uani 1 1 d . . . C40 C 0.7357(6) 0.4382(3) 0.4653(5) 0.074(2) Uani 1 1 d . . . H40 H 0.6824 0.4621 0.4604 0.088 Uiso 1 1 calc R . . C41 C 0.8170(6) 0.4433(4) 0.5326(5) 0.091(3) Uani 1 1 d . . . H41 H 0.8218 0.4724 0.5726 0.109 Uiso 1 1 calc R . . C42 C 0.8897(6) 0.4052(3) 0.5399(4) 0.070(2) Uani 1 1 d . . . H42 H 0.9438 0.4053 0.5872 0.084 Uiso 1 1 calc R . . C43 C 0.8838(5) 0.3663(2) 0.4773(4) 0.0465(15) Uani 1 1 d . . . C44 C 0.9685(4) 0.3312(2) 0.4767(3) 0.0403(14) Uani 1 1 d . . . H44A H 0.9918 0.3480 0.4352 0.048 Uiso 1 1 calc R . . H44B H 1.0188 0.3363 0.5296 0.048 Uiso 1 1 calc R . . N1 N 0.3006(4) 0.1337(2) -0.0775(3) 0.0497(13) Uani 1 1 d . . . H1 H 0.3357 0.1122 -0.0369 0.060 Uiso 1 1 calc R . . N2 N 0.2905(4) 0.0168(2) -0.0579(3) 0.0506(13) Uani 1 1 d . . . N3 N 0.4308(3) -0.0316(2) 0.0656(3) 0.0482(13) Uani 1 1 d . . . H3A H 0.4258 0.0056 0.0506 0.058 Uiso 1 1 calc R . . N4 N 0.4184(4) 0.2027(2) -0.0363(3) 0.0456(13) Uani 1 1 d . . . N5 N 0.5578(3) -0.00036(19) 0.1720(3) 0.0387(11) Uani 1 1 d . . . N6 N 0.5484(4) 0.2605(2) 0.0098(3) 0.0514(14) Uani 1 1 d . . . H6 H 0.5716 0.2309 0.0430 0.062 Uiso 1 1 calc R . . N7 N 0.6780(3) 0.04062(19) 0.2769(3) 0.0442(12) Uani 1 1 d . . . H7 H 0.6434 0.0728 0.2663 0.053 Uiso 1 1 calc R . . N8 N 0.7140(4) 0.3737(2) 0.1535(3) 0.0523(14) Uani 1 1 d . . . N9 N 0.6681(4) 0.3932(2) 0.2560(3) 0.0496(13) Uani 1 1 d . . . N10 N 0.9146(3) 0.18324(19) 0.3994(3) 0.0375(11) Uani 1 1 d . . . N11 N 0.9524(3) 0.26697(19) 0.4608(3) 0.0392(11) Uani 1 1 d . . . N12 N 0.8070(3) 0.36372(19) 0.4123(3) 0.0403(11) Uani 1 1 d . A . O1 O 0.1626(3) 0.1308(2) -0.1883(3) 0.0643(13) Uani 1 1 d . . . O2 O 0.3582(3) -0.12136(19) 0.0357(3) 0.0742(15) Uani 1 1 d . . . O3 O 0.5891(4) 0.3494(3) -0.0298(4) 0.103(2) Uani 1 1 d . . . O4 O 0.8227(3) 0.00671(16) 0.3484(3) 0.0546(11) Uani 1 1 d . . . O5 O 0.4605(4) 0.0948(2) 0.0604(3) 0.0641(13) Uani 1 1 d D . . O6 O 0.5179(3) 0.49661(19) 0.3704(3) 0.0591(12) Uani 1 1 d D . . Br1 Br 0.43516(6) 0.29079(3) 0.18288(4) 0.0587(2) Uani 1 1 d . . . Br2 Br 0.65879(5) 0.23938(3) 0.40548(4) 0.04621(17) Uani 1 1 d . . . Br3 Br 0.65262(5) 0.17482(3) 0.18118(4) 0.04604(17) Uani 1 1 d . . . Br4 Br 0.46318(5) 0.11260(3) 0.28323(4) 0.05409(19) Uani 1 1 d . . . Hg1 Hg 0.800392(18) 0.290352(10) 0.301239(14) 0.04134(10) Uani 1 1 d . . . Hg2 Hg 0.54487(2) 0.210698(11) 0.262592(16) 0.05012(11) Uani 1 1 d . . . H5A H 0.476(5) 0.1292(15) 0.051(4) 0.075 Uiso 1 1 d D . . H5B H 0.466(5) 0.101(3) 0.1084(18) 0.075 Uiso 1 1 d D . . H6B H 0.523(5) 0.5334(10) 0.373(4) 0.075 Uiso 1 1 d D . . H6A H 0.463(3) 0.500(3) 0.376(4) 0.075 Uiso 1 1 d 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 C1 0.037(4) 0.071(5) 0.052(3) 0.004(3) 0.010(3) 0.005(3) C2 0.034(4) 0.063(4) 0.048(3) -0.004(3) 0.008(3) 0.011(3) C3 0.033(4) 0.073(5) 0.051(3) -0.011(3) -0.001(3) 0.006(3) C4 0.028(4) 0.073(5) 0.061(4) -0.013(4) -0.003(3) -0.010(3) C5 0.036(4) 0.063(4) 0.071(4) -0.025(4) 0.005(3) -0.001(3) C6 0.030(4) 0.057(4) 0.047(3) -0.007(3) 0.005(3) 0.003(3) C7 0.031(4) 0.060(4) 0.052(3) -0.010(3) 0.004(3) -0.004(3) C8 0.045(4) 0.051(4) 0.052(3) 0.009(3) 0.011(3) 0.011(3) C9 0.042(5) 0.088(6) 0.066(4) 0.025(4) 0.002(4) 0.019(4) C10 0.054(5) 0.056(4) 0.086(5) 0.030(4) 0.007(4) 0.010(4) C11 0.043(5) 0.054(4) 0.073(4) 0.018(3) 0.007(4) 0.007(3) C12 0.048(4) 0.049(4) 0.047(3) 0.009(3) 0.009(3) 0.003(3) C13 0.036(4) 0.047(3) 0.049(3) 0.002(3) 0.006(3) 0.002(3) C14 0.043(4) 0.031(3) 0.066(4) 0.000(3) 0.006(3) -0.002(3) C15 0.045(4) 0.031(3) 0.068(4) 0.003(3) 0.008(3) -0.004(3) C16 0.038(4) 0.038(3) 0.054(3) 0.006(3) 0.002(3) 0.002(3) C17 0.037(4) 0.032(3) 0.051(3) 0.001(3) 0.006(3) -0.006(3) C18 0.055(5) 0.060(4) 0.059(4) 0.019(4) 0.013(4) 0.001(4) C19 0.050(5) 0.064(4) 0.051(4) 0.021(3) 0.011(3) 0.000(3) C20 0.053(5) 0.052(4) 0.056(4) 0.007(3) 0.014(3) 0.006(3) C21 0.037(4) 0.028(3) 0.049(3) 0.007(2) 0.004(3) 0.000(3) C22 0.040(4) 0.030(3) 0.048(3) 0.004(2) 0.003(3) -0.001(3) C23 0.036(4) 0.029(3) 0.049(3) -0.002(2) 0.003(3) -0.003(2) C24 0.028(4) 0.044(3) 0.059(4) 0.012(3) 0.010(3) 0.004(3) C31 0.024(3) 0.031(3) 0.050(3) 0.002(2) 0.003(3) -0.002(2) C32 0.024(3) 0.035(3) 0.054(3) 0.005(3) 0.004(3) -0.002(2) C33 0.029(4) 0.034(3) 0.070(4) 0.009(3) 0.000(3) 0.006(3) C34 0.039(4) 0.041(3) 0.074(4) 0.018(3) -0.007(3) 0.005(3) C35 0.048(4) 0.052(4) 0.055(4) 0.013(3) -0.011(3) -0.001(3) C36 0.033(4) 0.037(3) 0.054(3) 0.004(3) 0.009(3) -0.001(3) C37 0.020(3) 0.040(3) 0.046(3) 0.006(3) 0.009(3) 0.004(2) C38 0.027(4) 0.046(3) 0.066(4) 0.014(3) 0.020(3) 0.004(3) C39 0.030(4) 0.045(3) 0.062(4) 0.004(3) 0.014(3) 0.005(3) C40 0.066(6) 0.081(5) 0.076(5) -0.007(4) 0.028(4) 0.030(4) C41 0.082(7) 0.102(6) 0.073(5) -0.027(5) 0.005(5) 0.050(5) C42 0.071(6) 0.076(5) 0.053(4) -0.011(4) 0.006(4) 0.035(4) C43 0.044(4) 0.038(3) 0.056(3) 0.001(3) 0.016(3) 0.001(3) C44 0.030(3) 0.031(3) 0.053(3) -0.007(3) 0.005(3) -0.004(2) N1 0.032(3) 0.059(3) 0.048(3) 0.012(3) 0.001(2) 0.005(3) N2 0.046(3) 0.052(3) 0.049(3) -0.007(3) 0.009(3) 0.002(3) N3 0.033(3) 0.038(3) 0.062(3) 0.004(2) 0.002(3) -0.001(2) N4 0.034(3) 0.048(3) 0.049(3) 0.002(2) 0.006(3) 0.008(2) N5 0.028(3) 0.034(2) 0.046(2) 0.002(2) 0.002(2) 0.000(2) N6 0.050(4) 0.045(3) 0.049(3) 0.007(2) 0.003(3) 0.006(3) N7 0.033(3) 0.028(2) 0.057(3) -0.004(2) -0.004(2) 0.001(2) N8 0.049(4) 0.048(3) 0.058(3) 0.018(3) 0.015(3) 0.007(3) N9 0.042(3) 0.037(3) 0.070(3) 0.022(3) 0.019(3) 0.010(2) N10 0.028(3) 0.034(2) 0.046(2) 0.002(2) 0.006(2) -0.001(2) N11 0.030(3) 0.032(2) 0.052(3) 0.000(2) 0.009(2) 0.000(2) N12 0.035(3) 0.035(2) 0.051(3) 0.003(2) 0.013(2) 0.005(2) O1 0.040(3) 0.085(3) 0.054(3) 0.007(2) -0.003(2) 0.015(2) O2 0.060(3) 0.043(3) 0.090(3) -0.004(2) -0.013(3) -0.009(2) O3 0.060(4) 0.109(4) 0.122(5) 0.077(4) 0.006(3) -0.006(3) O4 0.034(3) 0.032(2) 0.082(3) 0.006(2) -0.002(2) 0.0009(18) O5 0.069(3) 0.044(2) 0.058(3) 0.001(2) -0.007(3) -0.009(2) O6 0.048(3) 0.039(2) 0.089(3) -0.002(2) 0.021(3) 0.009(2) Br1 0.0524(5) 0.0534(4) 0.0614(4) 0.0015(3) 0.0075(4) 0.0200(3) Br2 0.0380(4) 0.0421(3) 0.0547(3) 0.0008(3) 0.0106(3) 0.0021(3) Br3 0.0404(4) 0.0427(3) 0.0508(3) 0.0089(3) 0.0098(3) 0.0075(3) Br4 0.0496(5) 0.0462(4) 0.0671(4) -0.0003(3) 0.0205(4) 0.0008(3) Hg1 0.03437(19) 0.03523(15) 0.04694(15) 0.00570(10) 0.00390(12) 0.00391(10) Hg2 0.0397(2) 0.04588(17) 0.05963(18) 0.00191(11) 0.01003(15) 0.00642(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.248(7) . ? C1 N1 1.373(8) . ? C1 C2 1.509(9) . ? C2 N2 1.331(7) . ? C2 C3 1.382(8) . ? C3 C4 1.350(9) . ? C4 C5 1.371(9) . ? C5 C6 1.412(8) . ? C6 N2 1.316(7) . ? C6 C7 1.513(8) . ? C7 O2 1.207(7) . ? C7 N3 1.368(7) . ? C8 N4 1.325(8) . ? C8 C9 1.408(8) . ? C8 N1 1.415(8) . ? C9 C10 1.396(9) . ? C10 C11 1.327(9) . ? C11 C12 1.377(8) . ? C12 N4 1.320(7) . ? C12 N6 1.409(7) . ? C13 N5 1.357(7) . ? C13 N3 1.391(7) . ? C13 C14 1.394(8) . ? C14 C15 1.380(8) . ? C15 C16 1.396(8) . ? C16 C17 1.375(7) . ? C17 N5 1.347(7) . ? C17 N7 1.416(6) . ? C18 O3 1.240(7) . ? C18 N6 1.340(8) . ? C18 C19 1.510(9) . ? C19 C20 1.512(8) . ? C20 N8 1.465(8) . ? C21 O4 1.215(6) . ? C21 N7 1.339(7) . ? C21 C22 1.527(7) . ? C22 C23 1.534(8) . ? C23 N10 1.480(6) . ? C24 N9 1.340(7) . ? C24 N8 1.350(7) . ? C24 Hg1 2.095(6) . ? C25 N8 1.378(13) . ? C25 C30 1.380(14) . ? C25 C26 1.393(13) . ? C26 C27 1.352(13) . ? C27 C28 1.404(13) . ? C28 C29 1.415(13) . ? C29 C30 1.386(14) . ? C30 N9 1.441(12) . ? C25A C30A 1.373(18) . ? C25A C26A 1.409(13) . ? C25A N8 1.482(13) . ? C26A C27A 1.401(13) . ? C27A C28A 1.408(13) . ? C28A C29A 1.408(14) . ? C29A C30A 1.357(18) . ? C30A N9 1.446(13) . ? C31 N11 1.347(7) . ? C31 N10 1.347(7) . ? C31 Hg1 2.085(5) . ? C32 C33 1.372(7) . ? C32 C37 1.390(7) . ? C32 N10 1.397(6) . ? C33 C34 1.397(7) . ? C34 C35 1.397(8) . ? C35 C36 1.405(7) . ? C36 C37 1.386(7) . ? C37 N11 1.382(6) . ? C38 N9 1.455(7) . ? C38 C39 1.511(8) . ? C39 N12 1.329(7) . ? C39 C40 1.379(9) . ? C40 C41 1.395(10) . ? C41 C42 1.370(9) . ? C42 C43 1.391(8) . ? C43 N12 1.328(7) . ? C43 C44 1.511(8) . ? C44 N11 1.488(6) . ? N12 Hg1 2.545(5) . ? Br1 Hg2 2.5396(7) . ? Br2 Hg2 2.6071(7) . ? Br3 Hg2 2.6357(7) . ? Br4 Hg2 2.6288(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 125.2(6) . . ? O1 C1 C2 120.7(6) . . ? N1 C1 C2 114.1(6) . . ? N2 C2 C3 124.1(6) . . ? N2 C2 C1 117.5(6) . . ? C3 C2 C1 118.4(6) . . ? C4 C3 C2 118.4(6) . . ? C3 C4 C5 119.9(6) . . ? C4 C5 C6 117.5(7) . . ? N2 C6 C5 123.4(6) . . ? N2 C6 C7 119.0(5) . . ? C5 C6 C7 117.5(6) . . ? O2 C7 N3 125.3(6) . . ? O2 C7 C6 120.8(6) . . ? N3 C7 C6 113.8(6) . . ? N4 C8 C9 122.7(7) . . ? N4 C8 N1 113.8(5) . . ? C9 C8 N1 123.5(6) . . ? C10 C9 C8 116.2(7) . . ? C11 C10 C9 120.7(7) . . ? C10 C11 C12 119.2(7) . . ? N4 C12 C11 123.0(7) . . ? N4 C12 N6 112.7(5) . . ? C11 C12 N6 124.4(6) . . ? N5 C13 N3 113.3(5) . . ? N5 C13 C14 122.9(5) . . ? N3 C13 C14 123.8(5) . . ? C15 C14 C13 117.5(5) . . ? C14 C15 C16 120.9(5) . . ? C17 C16 C15 117.4(5) . . ? N5 C17 C16 123.7(5) . . ? N5 C17 N7 113.0(5) . . ? C16 C17 N7 123.2(5) . . ? O3 C18 N6 124.7(7) . . ? O3 C18 C19 120.8(7) . . ? N6 C18 C19 114.6(6) . . ? C18 C19 C20 113.6(6) . . ? N8 C20 C19 110.9(6) . . ? O4 C21 N7 124.2(5) . . ? O4 C21 C22 119.7(5) . . ? N7 C21 C22 116.1(5) . . ? C21 C22 C23 110.7(5) . . ? N10 C23 C22 109.9(5) . . ? N9 C24 N8 108.8(5) . . ? N9 C24 Hg1 120.1(4) . . ? N8 C24 Hg1 128.9(5) . . ? N8 C25 C30 102.5(10) . . ? N8 C25 C26 134.3(11) . . ? C30 C25 C26 122.0(11) . . ? C27 C26 C25 116.9(11) . . ? C26 C27 C28 123.4(11) . . ? C27 C28 C29 119.0(11) . . ? C30 C29 C28 117.4(11) . . ? C25 C30 C29 121.3(11) . . ? C25 C30 N9 110.6(10) . . ? C29 C30 N9 128.0(10) . . ? C30A C25A C26A 122.2(11) . . ? C30A C25A N8 112.3(9) . . ? C26A C25A N8 125.5(10) . . ? C27A C26A C25A 113.4(11) . . ? C26A C27A C28A 123.1(11) . . ? C27A C28A C29A 121.5(12) . . ? C30A C29A C28A 114.3(12) . . ? C29A C30A C25A 125.2(12) . . ? C29A C30A N9 134.4(11) . . ? C25A C30A N9 100.0(10) . . ? N11 C31 N10 106.9(4) . . ? N11 C31 Hg1 121.6(4) . . ? N10 C31 Hg1 131.1(4) . . ? C33 C32 C37 123.6(5) . . ? C33 C32 N10 130.7(5) . . ? C37 C32 N10 105.7(5) . . ? C32 C33 C34 115.5(5) . . ? C33 C34 C35 122.0(5) . . ? C34 C35 C36 121.5(6) . . ? C37 C36 C35 116.0(5) . . ? N11 C37 C36 131.8(5) . . ? N11 C37 C32 106.7(5) . . ? C36 C37 C32 121.4(5) . . ? N9 C38 C39 114.0(5) . . ? N12 C39 C40 121.2(6) . . ? N12 C39 C38 115.6(5) . . ? C40 C39 C38 123.2(6) . . ? C39 C40 C41 119.2(6) . . ? C42 C41 C40 118.4(7) . . ? C41 C42 C43 119.4(7) . . ? N12 C43 C42 121.0(6) . . ? N12 C43 C44 117.8(5) . . ? C42 C43 C44 120.7(6) . . ? N11 C44 C43 115.6(5) . . ? C1 N1 C8 127.3(5) . . ? C6 N2 C2 116.7(6) . . ? C7 N3 C13 125.1(5) . . ? C12 N4 C8 118.3(6) . . ? C17 N5 C13 117.6(5) . . ? C18 N6 C12 129.0(5) . . ? C21 N7 C17 127.5(5) . . ? C24 N8 C25 112.3(7) . . ? C24 N8 C20 125.8(5) . . ? C25 N8 C20 121.5(7) . . ? C24 N8 C25A 104.1(6) . . ? C25 N8 C25A 20.8(7) . . ? C20 N8 C25A 128.7(6) . . ? C24 N9 C30 104.7(7) . . ? C24 N9 C30A 113.7(7) . . ? C30 N9 C30A 19.0(7) . . ? C24 N9 C38 127.3(5) . . ? C30 N9 C38 127.4(7) . . ? C30A N9 C38 118.5(7) . . ? C31 N10 C32 110.3(4) . . ? C31 N10 C23 127.7(4) . . ? C32 N10 C23 121.9(4) . . ? C31 N11 C37 110.4(4) . . ? C31 N11 C44 126.7(5) . . ? C37 N11 C44 122.1(5) . . ? C43 N12 C39 120.6(5) . . ? C43 N12 Hg1 119.2(4) . . ? C39 N12 Hg1 120.2(4) . . ? C31 Hg1 C24 168.0(2) . . ? C31 Hg1 N12 85.76(19) . . ? C24 Hg1 N12 83.6(2) . . ? Br1 Hg2 Br2 116.77(2) . . ? Br1 Hg2 Br4 115.63(3) . . ? Br2 Hg2 Br4 105.41(2) . . ? Br1 Hg2 Br3 109.15(2) . . ? Br2 Hg2 Br3 105.93(2) . . ? Br4 Hg2 Br3 102.65(2) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 72.10 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.495 _refine_diff_density_min -1.587 _refine_diff_density_rms 0.142 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.220 0.716 0.500 1155 222 ' ' _platon_squeeze_details ; ; #===END data_[PdClL2][PF6] _database_code_depnum_ccdc_archive 'CCDC 893435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64.59 H43.91 Cl F6 N12 O8.81 P Pd 1.05' _chemical_formula_weight 1410.02 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 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 10.9057(8) _cell_length_b 17.4282(13) _cell_length_c 20.758(2) _cell_angle_alpha 109.393(6) _cell_angle_beta 102.088(6) _cell_angle_gamma 102.117(4) _cell_volume 3468.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 4.365 _cell_measurement_theta_max 53.169 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1442 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86684 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 30.36 _reflns_number_total 20443 _reflns_number_gt 13795 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1260P)^2^+0.6478P] 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 20443 _refine_ls_number_parameters 878 _refine_ls_number_restraints 281 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.2142 _refine_ls_wR_factor_gt 0.1818 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.098 _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 C1 C 1.1909(5) 1.2965(3) 1.1096(2) 0.0545(11) Uani 1 1 d . . . C2 C 1.1366(4) 1.3705(2) 1.1291(2) 0.0477(10) Uani 1 1 d . B . C3 C 1.1761(5) 1.4292(3) 1.1989(2) 0.0537(11) Uani 1 1 d . . . H3 H 1.2388 1.4238 1.2352 0.064 Uiso 1 1 calc R B . C4 C 1.1230(5) 1.4959(3) 1.2149(2) 0.0595(12) Uani 1 1 d . B . H4 H 1.1482 1.5372 1.2626 0.071 Uiso 1 1 calc R . . C5 C 1.0333(5) 1.5015(3) 1.1610(2) 0.0604(12) Uani 1 1 d . . . H5 H 0.9959 1.5471 1.1708 0.072 Uiso 1 1 calc R B . C6 C 0.9977(4) 1.4400(3) 1.0920(2) 0.0490(10) Uani 1 1 d . B . C7 C 0.8989(5) 1.4431(3) 1.0315(2) 0.0542(11) Uani 1 1 d . . . C8 C 1.1336(4) 1.1539(3) 1.0124(2) 0.0485(10) Uani 1 1 d . . . C9 C 1.2519(5) 1.1359(3) 1.0261(2) 0.0580(12) Uani 1 1 d . B . H9 H 1.3294 1.1772 1.0613 0.070 Uiso 1 1 calc R . . C10 C 1.2508(5) 1.0555(3) 0.9861(3) 0.0649(13) Uani 1 1 d . . . H10 H 1.3299 1.0405 0.9935 0.078 Uiso 1 1 calc R B . C11 C 1.1385(5) 0.9960(3) 0.9357(3) 0.0591(12) Uani 1 1 d . B . H11 H 1.1382 0.9400 0.9086 0.071 Uiso 1 1 calc R . . C12 C 1.0253(4) 1.0206(2) 0.9256(2) 0.0440(9) Uani 1 1 d . . . C13 C 0.7949(5) 1.3635(3) 0.9004(2) 0.0492(10) Uani 1 1 d . . . C14 C 0.6910(5) 1.3965(3) 0.8917(2) 0.0624(13) Uani 1 1 d . B . H14 H 0.6789 1.4384 0.9309 0.075 Uiso 1 1 calc R . . C15 C 0.6046(5) 1.3653(3) 0.8224(3) 0.0621(13) Uani 1 1 d . . . H15 H 0.5294 1.3843 0.8141 0.075 Uiso 1 1 calc R B . C16 C 0.6274(5) 1.3071(3) 0.7659(2) 0.0538(11) Uani 1 1 d . B . H16 H 0.5698 1.2860 0.7184 0.065 Uiso 1 1 calc R . . C17 C 0.7377(4) 1.2807(2) 0.78080(19) 0.0406(8) Uani 1 1 d . . . C18 C 0.8720(4) 0.8871(2) 0.8294(2) 0.0456(9) Uani 1 1 d . . . C19 C 0.7291(4) 0.8493(2) 0.78339(19) 0.0374(7) Uani 1 1 d . B . H19A H 0.6950 0.8944 0.7747 0.045 Uiso 1 1 calc R . . H19B H 0.6751 0.8234 0.8080 0.045 Uiso 1 1 calc R . . C20 C 0.7219(3) 0.7816(2) 0.71279(18) 0.0333(7) Uani 1 1 d . . . H20A H 0.7873 0.8060 0.6927 0.040 Uiso 1 1 calc R B . H20B H 0.7448 0.7332 0.7216 0.040 Uiso 1 1 calc R . . C21 C 0.7097(4) 1.1825(2) 0.65727(18) 0.0368(7) Uani 1 1 d . . . C22 C 0.7794(4) 1.1273(2) 0.61600(19) 0.0370(8) Uani 1 1 d . B . H22A H 0.8317 1.1062 0.6476 0.044 Uiso 1 1 calc R . . H22B H 0.8405 1.1614 0.5994 0.044 Uiso 1 1 calc R . . C23 C 0.6802(4) 1.0525(2) 0.55229(19) 0.0418(8) Uani 1 1 d . . . H23A H 0.6157 1.0216 0.5693 0.050 Uiso 1 1 calc R B . H23B H 0.6318 1.0744 0.5199 0.050 Uiso 1 1 calc R . . C24 C 0.5607(3) 0.76839(19) 0.60248(18) 0.0290(6) Uani 1 1 d . . . C25 C 0.4833(3) 0.68991(19) 0.65974(17) 0.0294(6) Uani 1 1 d . . . C26 C 0.4669(4) 0.6498(2) 0.70585(19) 0.0381(8) Uani 1 1 d . B . H26 H 0.5354 0.6613 0.7477 0.046 Uiso 1 1 calc R . . C27 C 0.3426(4) 0.5910(2) 0.6870(2) 0.0470(9) Uani 1 1 d . . . H27 H 0.3267 0.5613 0.7168 0.056 Uiso 1 1 calc R B . C28 C 0.2431(4) 0.5750(2) 0.6268(2) 0.0450(9) Uani 1 1 d . B . H28 H 0.1605 0.5351 0.6170 0.054 Uiso 1 1 calc R . . C29 C 0.2584(3) 0.6144(2) 0.5801(2) 0.0371(7) Uani 1 1 d . . . H29 H 0.1891 0.6034 0.5388 0.045 Uiso 1 1 calc R B . C30 C 0.3822(3) 0.6712(2) 0.59781(18) 0.0300(6) Uani 1 1 d . B . C31 C 0.7288(4) 0.9152(2) 0.51135(19) 0.0377(8) Uani 1 1 d . . . C32 C 0.7925(19) 1.0106(10) 0.4623(8) 0.039(3) Uani 0.64(5) 1 d P A 1 C33 C 0.824(2) 1.0808(7) 0.4453(7) 0.051(4) Uani 0.64(5) 1 d P A 1 H33 H 0.8018 1.1312 0.4672 0.061 Uiso 0.64(5) 1 calc PR A 1 C34 C 0.889(3) 1.0726(9) 0.3943(9) 0.071(5) Uani 0.64(5) 1 d P A 1 H34 H 0.9083 1.1179 0.3786 0.085 Uiso 0.64(5) 1 calc PR A 1 C35 C 0.927(3) 1.0015(10) 0.3652(8) 0.064(5) Uani 0.64(5) 1 d P A 1 H35 H 0.9767 1.0014 0.3326 0.077 Uiso 0.64(5) 1 calc PR A 1 C36 C 0.897(2) 0.9313(11) 0.3811(9) 0.050(4) Uani 0.64(5) 1 d P A 1 H36 H 0.9209 0.8814 0.3601 0.060 Uiso 0.64(5) 1 calc PR A 1 C37 C 0.8283(18) 0.9400(11) 0.4314(8) 0.040(3) Uani 0.64(5) 1 d P A 1 C32A C 0.832(2) 1.0034(13) 0.4716(12) 0.023(4) Uani 0.36(5) 1 d P A 2 C33A C 0.874(2) 1.0728(10) 0.4545(9) 0.030(4) Uani 0.36(5) 1 d P A 2 H33A H 0.8553 1.1245 0.4759 0.035 Uiso 0.36(5) 1 calc PR A 2 C34A C 0.944(2) 1.0655(12) 0.4061(9) 0.037(4) Uani 0.36(5) 1 d P A 2 H34A H 0.9734 1.1122 0.3934 0.045 Uiso 0.36(5) 1 calc PR A 2 C35A C 0.9723(16) 0.9865(13) 0.3746(9) 0.033(4) Uani 0.36(5) 1 d P A 2 H35A H 1.0223 0.9826 0.3419 0.039 Uiso 0.36(5) 1 calc PR A 2 C36A C 0.928(2) 0.9157(15) 0.3905(13) 0.032(4) Uani 0.36(5) 1 d P A 2 H36A H 0.9476 0.8639 0.3699 0.038 Uiso 0.36(5) 1 calc PR A 2 C37A C 0.854(2) 0.9258(12) 0.4395(11) 0.022(3) Uani 0.36(5) 1 d P A 2 C38 C 0.3748(3) 0.7155(3) 0.49248(19) 0.0384(8) Uani 1 1 d . . . H38A H 0.3635 0.7712 0.4951 0.046 Uiso 1 1 calc R B . H38B H 0.2867 0.6724 0.4716 0.046 Uiso 1 1 calc R . . C39 C 0.4601(3) 0.6905(2) 0.44534(18) 0.0325(7) Uani 1 1 d . B . C40 C 0.4164(4) 0.6157(2) 0.3857(2) 0.0422(9) Uani 1 1 d . . . H40 H 0.3316 0.5769 0.3737 0.051 Uiso 1 1 calc R B . C41 C 0.4968(4) 0.5972(2) 0.3435(2) 0.0421(8) Uani 1 1 d . B . H41 H 0.4685 0.5455 0.3021 0.050 Uiso 1 1 calc R . . C42 C 0.6194(3) 0.6549(2) 0.36211(19) 0.0360(7) Uani 1 1 d . . . H42 H 0.6755 0.6441 0.3330 0.043 Uiso 1 1 calc R B . C43 C 0.6592(3) 0.7282(2) 0.42340(19) 0.0320(7) Uani 1 1 d . B . C44 C 0.7941(4) 0.7912(2) 0.4473(2) 0.0431(9) Uani 1 1 d . . . H44A H 0.8492 0.7883 0.4904 0.052 Uiso 1 1 calc R B . H44B H 0.8362 0.7757 0.4089 0.052 Uiso 1 1 calc R . . N1 N 1.1177(4) 1.2329(2) 1.04558(18) 0.0555(10) Uani 1 1 d . B 1 H1 H 1.0507 1.2433 1.0217 0.067 Uiso 0.9554(12) 1 calc PR C 1 N3 N 0.8845(4) 1.3833(2) 0.96764(17) 0.0522(9) Uani 1 1 d . B 1 H3A H 0.9383 1.3520 0.9677 0.063 Uiso 0.9554(12) 1 calc PR C 1 Pd2 Pd 0.9630(5) 1.2921(3) 0.9890(3) 0.0274(18) Uani 0.0446(12) 1 d P B 2 N2 N 1.0468(4) 1.3750(2) 1.07591(16) 0.0453(8) Uani 1 1 d . . . N4 N 1.0225(4) 1.0983(2) 0.96291(17) 0.0456(8) Uani 1 1 d . B . N5 N 0.8186(3) 1.3071(2) 0.84648(16) 0.0425(7) Uani 1 1 d . B . N6 N 0.9035(3) 0.96869(19) 0.87601(17) 0.0432(7) Uani 1 1 d . B . H6 H 0.8394 0.9921 0.8750 0.052 Uiso 1 1 calc R . . N7 N 0.7729(3) 1.22291(19) 0.72933(15) 0.0380(7) Uani 1 1 d . B . H7 H 0.8448 1.2107 0.7449 0.046 Uiso 1 1 calc R . . N8 N 0.5899(3) 0.74997(17) 0.66018(14) 0.0291(5) Uani 1 1 d . B . N9 N 0.4353(3) 0.72135(18) 0.56422(15) 0.0312(6) Uani 1 1 d . B . N10 N 0.7388(4) 0.99304(19) 0.51202(16) 0.0451(8) Uani 1 1 d . A . N11 N 0.7879(3) 0.87780(19) 0.46376(17) 0.0443(8) Uani 1 1 d . A . N12 N 0.5807(3) 0.74500(17) 0.46485(15) 0.0283(5) Uani 1 1 d . . . O1 O 1.2906(4) 1.2958(2) 1.14814(17) 0.0722(11) Uani 1 1 d . B . O2 O 0.8396(4) 1.4957(3) 1.04189(19) 0.0819(12) Uani 1 1 d . B . O3 O 0.9487(3) 0.8458(2) 0.8234(2) 0.0744(11) Uani 1 1 d . B . O4 O 0.6069(3) 1.18888(19) 0.62776(14) 0.0496(7) Uani 1 1 d . B . F1 F 0.0616(2) 0.58071(14) 0.41425(13) 0.0461(5) Uani 1 1 d . . . F2 F 0.0815(2) 0.72079(13) 0.45403(12) 0.0478(5) Uani 1 1 d . . . F3 F -0.0518(2) 0.70150(16) 0.34695(14) 0.0515(6) Uani 1 1 d . . . F4 F -0.1198(2) 0.62446(14) 0.40840(12) 0.0439(5) Uani 1 1 d . . . F5 F -0.0726(2) 0.55983(16) 0.30763(12) 0.0548(6) Uani 1 1 d . . . F6 F 0.1298(2) 0.65782(14) 0.35338(13) 0.0478(5) Uani 1 1 d . . . P P 0.00418(8) 0.64048(5) 0.38026(5) 0.03071(18) Uani 1 1 d . . . Cl Cl 0.73621(12) 0.95860(5) 0.67240(5) 0.0493(3) Uani 1 1 d . . . Pd1 Pd 0.65133(2) 0.846321(15) 0.561661(14) 0.03132(9) Uani 1 1 d . B . O5 O 0.7540(3) 0.57671(19) 0.63713(15) 0.0522(7) Uani 1 1 d D . . C45 C 0.8893(5) 0.6158(3) 0.6457(3) 0.0603(12) Uani 1 1 d D . . H45A H 0.9445 0.5821 0.6598 0.072 Uiso 1 1 calc R . . H45B H 0.9214 0.6743 0.6834 0.072 Uiso 1 1 calc R . . C46 C 0.8963(5) 0.6183(4) 0.5751(3) 0.0690(14) Uani 1 1 d D . . H46A H 0.9166 0.5677 0.5457 0.083 Uiso 1 1 calc R . . H46B H 0.9632 0.6707 0.5816 0.083 Uiso 1 1 calc R . . C47 C 0.7577(5) 0.6181(3) 0.5413(3) 0.0615(13) Uani 1 1 d D . . H47A H 0.7486 0.6762 0.5584 0.074 Uiso 1 1 calc R . . H47B H 0.7335 0.5941 0.4884 0.074 Uiso 1 1 calc R . . C48 C 0.6761(4) 0.5610(3) 0.5677(2) 0.0505(10) Uani 1 1 d D . . H48A H 0.5931 0.5749 0.5696 0.061 Uiso 1 1 calc R . . H48B H 0.6545 0.5003 0.5356 0.061 Uiso 1 1 calc R . . O6 O 0.4695(9) 0.5005(6) 0.9043(5) 0.118(4) Uiso 0.592(10) 1 d PD D 1 C49 C 0.5624(11) 0.5783(7) 0.9581(6) 0.096(4) Uiso 0.592(10) 1 d PD D 1 C50 C 0.4946(12) 0.6463(8) 0.9672(7) 0.099(4) Uiso 0.592(10) 1 d PD D 1 C51 C 0.3982(15) 0.6178(9) 0.8907(7) 0.110(5) Uiso 0.592(10) 1 d PD D 1 C52 C 0.379(2) 0.5192(11) 0.8545(10) 0.152(7) Uiso 0.592(10) 1 d PD D 1 O6A O 0.4266(12) 0.5020(8) 0.8274(7) 0.099(4) Uiso 0.408(10) 1 d PD D 2 C49A C 0.3146(18) 0.5048(15) 0.8552(12) 0.119(8) Uiso 0.408(10) 1 d PD D 2 C50A C 0.336(4) 0.600(2) 0.892(3) 0.48(6) Uiso 0.408(10) 1 d PD D 2 C51A C 0.485(4) 0.630(3) 0.936(2) 0.37(4) Uiso 0.408(10) 1 d PD D 2 C52A C 0.5395(18) 0.5650(15) 0.8861(12) 0.136(9) Uiso 0.408(10) 1 d PD D 2 O7 O 0.2230(14) 0.7873(9) 0.7812(7) 0.199(6) Uiso 0.623(4) 1 d PD E 1 C53 C 0.1698(13) 0.7310(8) 0.8138(7) 0.121(4) Uiso 0.623(4) 1 d PD E 1 C54 C 0.2190(12) 0.7745(8) 0.8902(7) 0.111(4) Uiso 0.623(4) 1 d PD E 1 C55 C 0.3482(12) 0.8409(8) 0.9012(7) 0.111(4) Uiso 0.623(4) 1 d PD E 1 C56 C 0.3655(15) 0.8267(12) 0.8309(8) 0.164(7) Uiso 0.623(4) 1 d PD E 1 O8 O 0.4051(14) 0.9343(8) 0.6187(7) 0.045(4) Uiso 0.182(6) 1 d PD F 2 C57 C 0.381(3) 0.9067(11) 0.6747(10) 0.057(7) Uiso 0.182(6) 1 d PD F 2 C58 C 0.364(2) 0.9778(11) 0.7329(10) 0.044(5) Uiso 0.182(6) 1 d PD F 2 C59 C 0.3939(18) 1.0552(9) 0.7116(9) 0.035(4) Uiso 0.182(6) 1 d PD F 2 C60 C 0.4583(17) 1.0265(9) 0.6517(9) 0.035(4) Uiso 0.182(6) 1 d PD F 2 C57B C 0.4500 1.0502 0.6914 0.075(8) Uiso 0.195(6) 1 d P G 3 C58B C 0.3548 0.9002 0.6835 0.071(9) Uiso 0.195(6) 1 d P G 3 C59B C 0.3671 0.9886 0.7096 0.059(6) Uiso 0.195(6) 1 d P G 3 C60B C 0.2891 1.0134 0.7530 0.054(6) Uiso 0.195(6) 1 d P G 3 C61B C 0.2020 0.9574 0.7690 0.059(6) Uiso 0.195(6) 1 d P G 3 C62B C 0.1903 0.8707 0.7451 0.069(7) Uiso 0.195(6) 1 d P G 3 C63B C 0.2702 0.8454 0.7018 0.101(11) Uiso 0.195(6) 1 d P G 3 O9 O 0.6777 1.0423 0.8665 0.067(2) Uiso 0.591(12) 1 d PD H 1 C61 C 0.6306 1.0793 0.8147 0.228(12) Uiso 0.591(12) 1 d PD H 1 C62 C 0.5326 1.1207 0.8391 0.153(7) Uiso 0.591(12) 1 d PD H 1 C63 C 0.5885 1.1509 0.9229 0.188(9) Uiso 0.591(12) 1 d PD H 1 C64 C 0.6322 1.0652 0.9334 0.289(18) Uiso 0.591(12) 1 d PD H 1 O9A O 0.7089(13) 1.0498(7) 0.8887(8) 0.094(4) Uiso 0.409(12) 1 d PD H 2 C61A C 0.575(2) 1.0241(15) 0.890(2) 0.236(18) Uiso 0.409(12) 1 d PD H 2 C62A C 0.546(2) 1.1067(15) 0.9259(14) 0.148(9) Uiso 0.409(12) 1 d PD H 2 C63A C 0.6347(19) 1.1735(10) 0.9061(11) 0.109(7) Uiso 0.409(12) 1 d PD H 2 C64A C 0.7211(14) 1.1238(9) 0.8688(8) 0.081(5) Uiso 0.409(12) 1 d PD H 2 O10 O 1.0289(3) 1.2004(2) 0.77425(19) 0.0657(9) Uiso 1 1 d D I 1 C65 C 1.0495(7) 1.1539(4) 0.8209(4) 0.0895(18) Uiso 1 1 d D I 1 C66 C 1.1925(11) 1.1632(9) 0.8409(8) 0.101(5) Uiso 0.594(19) 1 d PD I 1 C67 C 1.2518(11) 1.2511(9) 0.8375(8) 0.111(5) Uiso 0.594(19) 1 d PD I 1 C68 C 1.1313(7) 1.2785(4) 0.8031(4) 0.096(2) Uiso 1 1 d D I 1 C66A C 1.194(2) 1.2175(16) 0.8767(13) 0.107(7) Uiso 0.406(19) 1 d P I 2 C67A C 1.223(2) 1.3028(15) 0.8743(13) 0.116(8) Uiso 0.406(19) 1 d P I 2 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 C1 0.081(3) 0.036(2) 0.0298(19) 0.0097(16) -0.0053(19) 0.011(2) C2 0.068(3) 0.0351(19) 0.0240(17) 0.0053(15) -0.0019(17) 0.0094(18) C3 0.068(3) 0.050(2) 0.0251(18) 0.0061(17) -0.0010(18) 0.011(2) C4 0.067(3) 0.060(3) 0.027(2) -0.0048(19) 0.0048(19) 0.015(2) C5 0.067(3) 0.056(3) 0.039(2) -0.004(2) 0.009(2) 0.025(2) C6 0.056(2) 0.053(2) 0.0272(18) 0.0051(17) 0.0071(16) 0.019(2) C7 0.071(3) 0.055(3) 0.031(2) 0.0052(18) 0.0121(19) 0.031(2) C8 0.067(3) 0.0354(19) 0.0293(19) 0.0093(16) -0.0040(17) 0.0121(18) C9 0.065(3) 0.046(2) 0.039(2) 0.0095(19) -0.0115(19) 0.007(2) C10 0.064(3) 0.053(3) 0.056(3) 0.011(2) -0.011(2) 0.020(2) C11 0.058(3) 0.042(2) 0.054(3) 0.006(2) -0.006(2) 0.015(2) C12 0.059(2) 0.0308(17) 0.0295(18) 0.0077(15) -0.0042(16) 0.0126(17) C13 0.071(3) 0.053(2) 0.0308(19) 0.0155(18) 0.0131(18) 0.037(2) C14 0.080(3) 0.076(3) 0.036(2) 0.014(2) 0.013(2) 0.052(3) C15 0.075(3) 0.077(3) 0.047(3) 0.024(2) 0.017(2) 0.052(3) C16 0.069(3) 0.065(3) 0.033(2) 0.019(2) 0.0101(19) 0.038(2) C17 0.059(2) 0.0380(19) 0.0286(17) 0.0132(15) 0.0107(16) 0.0238(17) C18 0.052(2) 0.0336(18) 0.037(2) 0.0053(16) -0.0037(16) 0.0156(17) C19 0.0438(18) 0.0283(16) 0.0320(18) 0.0067(14) 0.0020(14) 0.0128(14) C20 0.0332(15) 0.0278(15) 0.0303(17) 0.0050(13) 0.0013(13) 0.0108(13) C21 0.055(2) 0.0262(15) 0.0281(17) 0.0125(14) 0.0078(15) 0.0107(15) C22 0.052(2) 0.0252(15) 0.0287(17) 0.0092(13) 0.0110(15) 0.0052(14) C23 0.064(2) 0.0261(16) 0.0299(18) 0.0097(14) 0.0122(16) 0.0077(16) C24 0.0291(14) 0.0247(14) 0.0341(17) 0.0138(13) 0.0089(12) 0.0074(12) C25 0.0352(15) 0.0214(13) 0.0295(16) 0.0092(12) 0.0097(13) 0.0057(12) C26 0.052(2) 0.0330(17) 0.0275(17) 0.0126(14) 0.0103(15) 0.0103(15) C27 0.064(2) 0.0353(19) 0.046(2) 0.0230(18) 0.0233(19) 0.0065(18) C28 0.051(2) 0.0319(17) 0.046(2) 0.0138(17) 0.0187(18) -0.0018(16) C29 0.0349(16) 0.0336(17) 0.0380(19) 0.0125(15) 0.0104(14) 0.0038(14) C30 0.0332(15) 0.0267(15) 0.0328(17) 0.0144(13) 0.0118(13) 0.0081(12) C31 0.0483(19) 0.0251(15) 0.0334(18) 0.0074(14) 0.0168(15) 0.0009(14) C32 0.048(7) 0.032(4) 0.027(4) 0.010(3) 0.006(5) 0.002(4) C33 0.067(9) 0.033(4) 0.039(5) 0.012(3) 0.015(6) -0.003(5) C34 0.087(12) 0.057(6) 0.051(6) 0.023(5) 0.022(8) -0.017(7) C35 0.071(10) 0.058(6) 0.053(6) 0.014(5) 0.037(7) -0.006(7) C36 0.057(8) 0.042(6) 0.038(6) 0.004(4) 0.022(6) 0.001(5) C37 0.051(6) 0.032(5) 0.040(5) 0.021(4) 0.018(4) 0.005(4) C32A 0.034(9) 0.017(5) 0.021(7) 0.012(4) 0.010(7) 0.005(6) C33A 0.034(8) 0.022(5) 0.029(6) 0.011(4) 0.003(5) 0.004(5) C34A 0.036(8) 0.038(7) 0.021(6) 0.012(5) 0.000(5) -0.015(6) C35A 0.022(6) 0.044(7) 0.028(6) 0.010(5) 0.009(5) 0.007(5) C36A 0.030(7) 0.032(7) 0.034(7) 0.014(5) 0.009(6) 0.005(5) C37A 0.040(7) 0.007(5) 0.017(6) 0.005(4) 0.004(5) 0.007(4) C38 0.0275(15) 0.051(2) 0.042(2) 0.0308(18) 0.0053(14) 0.0087(15) C39 0.0280(14) 0.0361(17) 0.0348(17) 0.0229(15) 0.0013(13) 0.0063(13) C40 0.0358(17) 0.0398(19) 0.0374(19) 0.0184(16) -0.0068(15) -0.0033(15) C41 0.0455(19) 0.0319(17) 0.0320(18) 0.0060(15) -0.0059(15) 0.0067(15) C42 0.0358(16) 0.0287(16) 0.0356(18) 0.0075(14) 0.0026(14) 0.0110(14) C43 0.0307(15) 0.0263(15) 0.0363(18) 0.0110(14) 0.0058(13) 0.0097(12) C44 0.0354(17) 0.0346(18) 0.048(2) 0.0042(16) 0.0170(16) 0.0032(15) N1 0.078(2) 0.0333(16) 0.0306(17) 0.0018(14) -0.0131(16) 0.0158(17) N3 0.071(2) 0.059(2) 0.0253(16) 0.0071(15) 0.0059(15) 0.0414(19) Pd2 0.039(3) 0.019(3) 0.018(3) 0.0053(19) 0.000(2) 0.008(2) N2 0.060(2) 0.0410(17) 0.0242(15) 0.0070(13) 0.0027(14) 0.0141(15) N4 0.063(2) 0.0297(15) 0.0289(15) 0.0070(13) -0.0075(14) 0.0122(15) N5 0.0574(19) 0.0449(18) 0.0287(15) 0.0132(14) 0.0090(14) 0.0283(16) N6 0.0487(17) 0.0295(15) 0.0378(17) 0.0052(13) -0.0022(14) 0.0134(13) N7 0.0505(17) 0.0383(16) 0.0268(14) 0.0131(13) 0.0078(13) 0.0196(14) N8 0.0313(13) 0.0235(12) 0.0280(13) 0.0083(11) 0.0058(11) 0.0053(10) N9 0.0277(12) 0.0334(14) 0.0345(15) 0.0199(12) 0.0060(11) 0.0054(11) N10 0.073(2) 0.0251(14) 0.0294(15) 0.0060(12) 0.0219(15) -0.0006(14) N11 0.0500(17) 0.0298(15) 0.0400(17) 0.0037(13) 0.0218(14) -0.0058(13) N12 0.0289(12) 0.0254(12) 0.0332(14) 0.0170(11) 0.0047(11) 0.0088(10) O1 0.099(3) 0.0465(17) 0.0382(17) 0.0041(14) -0.0234(17) 0.0223(18) O2 0.099(3) 0.087(3) 0.051(2) 0.0022(19) 0.0075(19) 0.065(2) O3 0.0623(19) 0.0473(18) 0.072(2) -0.0119(16) -0.0201(17) 0.0311(16) O4 0.0657(18) 0.0485(16) 0.0308(14) 0.0146(13) 0.0036(13) 0.0222(14) F1 0.0399(11) 0.0364(11) 0.0616(15) 0.0250(11) 0.0042(10) 0.0125(9) F2 0.0514(13) 0.0309(11) 0.0442(13) 0.0017(10) 0.0107(10) 0.0040(10) F3 0.0602(14) 0.0598(15) 0.0614(15) 0.0436(13) 0.0272(12) 0.0308(12) F4 0.0383(10) 0.0494(13) 0.0552(14) 0.0296(11) 0.0214(10) 0.0140(10) F5 0.0561(14) 0.0460(13) 0.0364(12) 0.0029(11) -0.0008(10) 0.0005(11) F6 0.0451(12) 0.0398(12) 0.0613(15) 0.0157(11) 0.0295(11) 0.0119(10) P 0.0292(4) 0.0262(4) 0.0352(5) 0.0122(4) 0.0083(3) 0.0064(3) Cl 0.0843(7) 0.0242(4) 0.0376(5) 0.0124(4) 0.0302(5) 0.0009(4) Pd1 0.03515(14) 0.02430(13) 0.03436(15) 0.01261(11) 0.01257(10) 0.00488(10) O5 0.0632(18) 0.0471(16) 0.0382(15) 0.0166(13) 0.0094(13) 0.0072(14) C45 0.062(3) 0.044(2) 0.069(3) 0.018(2) 0.012(2) 0.021(2) C46 0.076(3) 0.065(3) 0.079(4) 0.033(3) 0.039(3) 0.025(3) C47 0.097(4) 0.066(3) 0.054(3) 0.037(2) 0.039(3) 0.049(3) C48 0.060(2) 0.052(2) 0.036(2) 0.0108(19) 0.0132(18) 0.022(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.213(6) . ? C1 N1 1.355(5) . ? C1 C2 1.501(6) . ? C2 N2 1.350(5) . ? C2 C3 1.378(5) . ? C3 C4 1.380(7) . ? C4 C5 1.369(7) . ? C5 C6 1.387(6) . ? C6 N2 1.326(6) . ? C6 C7 1.499(6) . ? C6 Pd2 2.637(7) . ? C7 O2 1.217(5) . ? C7 N3 1.340(5) . ? C8 N4 1.337(5) . ? C8 C9 1.385(7) . ? C8 N1 1.387(5) . ? C9 C10 1.368(7) . ? C10 C11 1.372(6) . ? C11 C12 1.388(6) . ? C12 N4 1.329(5) . ? C12 N6 1.395(5) . ? C13 N5 1.335(5) . ? C13 C14 1.381(6) . ? C13 N3 1.411(5) . ? C14 C15 1.396(6) . ? C15 C16 1.381(6) . ? C16 C17 1.388(6) . ? C17 N5 1.326(5) . ? C17 N7 1.386(5) . ? C18 O3 1.211(5) . ? C18 N6 1.349(5) . ? C18 C19 1.518(5) . ? C19 C20 1.519(5) . ? C20 N8 1.475(4) . ? C21 O4 1.206(5) . ? C21 N7 1.369(4) . ? C21 C22 1.507(5) . ? C22 C23 1.511(5) . ? C23 N10 1.452(5) . ? C24 N8 1.333(4) . ? C24 N9 1.347(4) . ? C24 Pd1 2.023(3) . ? C25 C26 1.378(4) . ? C25 N8 1.388(4) . ? C25 C30 1.397(5) . ? C26 C27 1.403(5) . ? C27 C28 1.374(6) . ? C28 C29 1.378(5) . ? C29 C30 1.389(4) . ? C30 N9 1.395(4) . ? C31 N10 1.334(5) . ? C31 N11 1.353(5) . ? C31 Pd1 2.005(3) . ? C32 C37 1.364(17) . ? C32 N10 1.375(14) . ? C32 C33 1.378(16) . ? C33 C34 1.382(17) . ? C34 C35 1.379(19) . ? C35 C36 1.362(16) . ? C36 C37 1.40(2) . ? C37 N11 1.492(16) . ? C32A C33A 1.39(2) . ? C32A C37A 1.39(2) . ? C32A N10 1.46(2) . ? C33A C34A 1.37(2) . ? C34A C35A 1.44(3) . ? C35A C36A 1.40(3) . ? C36A C37A 1.42(3) . ? C37A N11 1.28(2) . ? C38 N9 1.457(4) . ? C38 C39 1.510(5) . ? C39 N12 1.339(4) . ? C39 C40 1.372(5) . ? C40 C41 1.376(6) . ? C41 C42 1.381(5) . ? C42 C43 1.377(5) . ? C43 N12 1.344(4) . ? C43 C44 1.507(5) . ? C44 N11 1.453(5) . ? Pd2 N2 1.790(6) . ? N12 Pd1 2.043(3) . ? F1 P 1.597(2) . ? F2 P 1.598(2) . ? F3 P 1.602(2) . ? F4 P 1.590(2) . ? F5 P 1.587(2) . ? F6 P 1.593(2) . ? Cl Pd1 2.3090(10) . ? O5 C48 1.414(5) . ? O5 C45 1.435(5) . ? C45 C46 1.500(7) . ? C46 C47 1.525(7) . ? C47 C48 1.508(6) . ? O6 C49 1.434(11) . ? O6 C52 1.440(13) . ? C49 C50 1.505(12) . ? C50 C51 1.559(13) . ? C51 C52 1.578(14) . ? O6A C52A 1.457(14) . ? O6A C49A 1.459(14) . ? C49A C50A 1.526(17) . ? C50A C51A 1.566(17) . ? C51A C52A 1.576(16) . ? O7 C53 1.457(12) . ? O7 C56 1.537(13) . ? C53 C54 1.434(12) . ? C54 C55 1.544(12) . ? C55 C56 1.455(13) . ? O8 C57 1.447(14) . ? O8 C60 1.449(13) . ? C57 C58 1.496(15) . ? C58 C59 1.548(14) . ? C59 C60 1.546(14) . ? C57B C59B 1.45585(10) . ? C58B C63B 1.3876 . ? C58B C59B 1.41871(13) . ? C59B C60B 1.3936 . ? C60B C61B 1.3863 . ? C61B C62B 1.39280(13) . ? C62B C63B 1.41041(10) . ? O9 C61 1.4839 . ? O9 C64 1.52938(17) . ? C61 C62 1.49317(10) . ? C62 C63 1.57738(17) . ? C63 C64 1.72528(13) . ? O9A C61A 1.444(15) . ? O9A C64A 1.468(12) . ? C61A C62A 1.518(16) . ? C62A C63A 1.573(15) . ? C63A C64A 1.563(14) . ? O10 C68 1.414(7) . ? O10 C65 1.466(7) . ? C65 C66 1.486(11) . ? C66 C67 1.563(12) . ? C67 C68 1.602(12) . ? C66A C67A 1.47(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 124.9(4) . . ? O1 C1 C2 122.0(4) . . ? N1 C1 C2 113.0(4) . . ? N2 C2 C3 122.7(4) . . ? N2 C2 C1 116.9(3) . . ? C3 C2 C1 120.4(4) . . ? C2 C3 C4 118.7(4) . . ? C5 C4 C3 118.9(4) . . ? C4 C5 C6 119.3(4) . . ? N2 C6 C5 122.6(4) . . ? N2 C6 C7 116.3(3) . . ? C5 C6 C7 121.1(4) . . ? N2 C6 Pd2 38.0(2) . . ? C5 C6 Pd2 158.6(4) . . ? C7 C6 Pd2 78.9(3) . . ? O2 C7 N3 125.5(4) . . ? O2 C7 C6 121.3(4) . . ? N3 C7 C6 113.2(4) . . ? N4 C8 C9 124.0(4) . . ? N4 C8 N1 111.8(4) . . ? C9 C8 N1 124.1(4) . . ? C10 C9 C8 116.3(4) . . ? C11 C10 C9 121.7(5) . . ? C10 C11 C12 117.6(4) . . ? N4 C12 C11 122.6(4) . . ? N4 C12 N6 112.3(4) . . ? C11 C12 N6 125.0(4) . . ? N5 C13 C14 123.7(4) . . ? N5 C13 N3 112.7(4) . . ? C14 C13 N3 123.5(4) . . ? C13 C14 C15 116.7(4) . . ? C16 C15 C14 120.5(4) . . ? C15 C16 C17 117.6(4) . . ? N5 C17 C16 123.0(4) . . ? N5 C17 N7 113.2(3) . . ? C16 C17 N7 123.8(4) . . ? O3 C18 N6 124.4(4) . . ? O3 C18 C19 121.5(3) . . ? N6 C18 C19 114.1(3) . . ? C18 C19 C20 108.0(3) . . ? N8 C20 C19 112.1(3) . . ? O4 C21 N7 124.5(4) . . ? O4 C21 C22 121.4(3) . . ? N7 C21 C22 114.1(3) . . ? C21 C22 C23 109.9(3) . . ? N10 C23 C22 113.5(4) . . ? N8 C24 N9 107.0(3) . . ? N8 C24 Pd1 137.3(2) . . ? N9 C24 Pd1 115.7(2) . . ? C26 C25 N8 132.1(3) . . ? C26 C25 C30 121.3(3) . . ? N8 C25 C30 106.5(3) . . ? C25 C26 C27 115.6(3) . . ? C28 C27 C26 122.3(3) . . ? C27 C28 C29 122.6(3) . . ? C28 C29 C30 115.2(3) . . ? C29 C30 N9 132.1(3) . . ? C29 C30 C25 122.8(3) . . ? N9 C30 C25 105.1(3) . . ? N10 C31 N11 107.0(3) . . ? N10 C31 Pd1 136.0(3) . . ? N11 C31 Pd1 117.0(3) . . ? C37 C32 N10 103.8(11) . . ? C37 C32 C33 121.0(13) . . ? N10 C32 C33 134.9(13) . . ? C32 C33 C34 115.2(12) . . ? C35 C34 C33 122.7(11) . . ? C34 C35 C36 123.1(11) . . ? C35 C36 C37 113.3(11) . . ? C32 C37 C36 124.7(11) . . ? C32 C37 N11 108.2(11) . . ? C36 C37 N11 127.1(11) . . ? C33A C32A C37A 122.2(18) . . ? C33A C32A N10 127.2(15) . . ? C37A C32A N10 109.6(15) . . ? C34A C33A C32A 118.8(16) . . ? C33A C34A C35A 119.7(15) . . ? C36A C35A C34A 122.1(16) . . ? C35A C36A C37A 116.1(17) . . ? N11 C37A C32A 102.2(17) . . ? N11 C37A C36A 136.7(16) . . ? C32A C37A C36A 121.0(17) . . ? N9 C38 C39 110.0(3) . . ? N12 C39 C40 121.6(3) . . ? N12 C39 C38 116.6(3) . . ? C40 C39 C38 121.7(3) . . ? C39 C40 C41 119.3(3) . . ? C40 C41 C42 119.1(3) . . ? C43 C42 C41 119.2(3) . . ? N12 C43 C42 121.3(3) . . ? N12 C43 C44 117.7(3) . . ? C42 C43 C44 120.9(3) . . ? N11 C44 C43 111.6(3) . . ? C1 N1 C8 129.1(4) . . ? C7 N3 C13 128.8(4) . . ? N2 Pd2 C6 27.16(17) . . ? C6 N2 C2 117.8(3) . . ? C6 N2 Pd2 114.8(3) . . ? C2 N2 Pd2 126.3(3) . . ? C12 N4 C8 117.9(4) . . ? C18 N6 C12 127.9(4) . . ? C17 N5 C13 118.5(3) . . ? C21 N7 C17 128.1(3) . . ? C24 N8 C25 110.7(3) . . ? C24 N8 C20 124.4(3) . . ? C25 N8 C20 124.5(3) . . ? C24 N9 C30 110.8(3) . . ? C24 N9 C38 122.6(3) . . ? C30 N9 C38 125.9(3) . . ? C31 N10 C32 115.0(9) . . ? C31 N10 C23 124.9(3) . . ? C32 N10 C23 119.3(9) . . ? C31 N10 C32A 103.2(9) . . ? C32 N10 C32A 19.6(6) . . ? C23 N10 C32A 131.5(9) . . ? C37A N11 C31 116.8(10) . . ? C37A N11 C44 119.7(10) . . ? C31 N11 C44 123.0(3) . . ? C37A N11 C37 16.6(10) . . ? C31 N11 C37 105.7(8) . . ? C44 N11 C37 131.1(8) . . ? C39 N12 C43 119.5(3) . . ? C39 N12 Pd1 120.1(2) . . ? C43 N12 Pd1 120.1(2) . . ? F5 P F4 89.89(13) . . ? F5 P F6 91.09(14) . . ? F4 P F6 179.02(15) . . ? F5 P F1 89.84(13) . . ? F4 P F1 90.26(12) . . ? F6 P F1 89.65(13) . . ? F5 P F2 179.15(14) . . ? F4 P F2 89.74(13) . . ? F6 P F2 89.28(12) . . ? F1 P F2 89.40(13) . . ? F5 P F3 90.87(14) . . ? F4 P F3 90.03(12) . . ? F6 P F3 90.04(13) . . ? F1 P F3 179.23(15) . . ? F2 P F3 89.89(14) . . ? C31 Pd1 C24 174.16(14) . . ? C31 Pd1 N12 87.04(12) . . ? C24 Pd1 N12 87.47(12) . . ? C31 Pd1 Cl 93.62(10) . . ? C24 Pd1 Cl 91.93(10) . . ? N12 Pd1 Cl 178.04(8) . . ? C48 O5 C45 109.4(3) . . ? O5 C45 C46 107.2(4) . . ? C45 C46 C47 102.1(4) . . ? C48 C47 C46 101.6(4) . . ? O5 C48 C47 105.9(4) . . ? C49 O6 C52 110.0(10) . . ? O6 C49 C50 107.1(9) . . ? C49 C50 C51 103.0(9) . . ? C52 C51 C50 104.0(9) . . ? O6 C52 C51 106.1(10) . . ? C52A O6A C49A 104.9(12) . . ? O6A C49A C50A 103.0(17) . . ? C49A C50A C51A 99.8(18) . . ? C52A C51A C50A 102.0(15) . . ? O6A C52A C51A 106.9(13) . . ? C53 O7 C56 99.9(10) . . ? C54 C53 O7 109.2(10) . . ? C53 C54 C55 102.4(9) . . ? C56 C55 C54 107.5(10) . . ? C55 C56 O7 102.4(11) . . ? C57 O8 C60 106.5(11) . . ? O8 C57 C58 109.9(12) . . ? C57 C58 C59 104.5(11) . . ? C60 C59 C58 104.0(11) . . ? O8 C60 C59 105.4(10) . . ? C63B C58B C59B 120.308(5) . . ? C60B C59B C58B 114.996(4) . . ? C60B C59B C57B 120.879(5) . . ? C58B C59B C57B 124.087(5) . . ? C61B C60B C59B 123.982(5) . . ? C60B C61B C62B 121.888(5) . . ? C61B C62B C63B 114.321(5) . . ? C58B C63B C62B 124.440(5) . . ? C61 O9 C64 115.807(6) . . ? O9 C61 C62 107.195(6) . . ? C61 C62 C63 101.141(6) . . ? C62 C63 C64 103.704(6) . . ? O9 C64 C63 93.969(5) . . ? C61A O9A C64A 105.6(13) . . ? O9A C61A C62A 105.4(14) . . ? C61A C62A C63A 103.8(12) . . ? C64A C63A C62A 103.9(11) . . ? O9A C64A C63A 104.8(10) . . ? C68 O10 C65 109.1(5) . . ? O10 C65 C66 106.0(6) . . ? C65 C66 C67 101.5(8) . . ? C68 C67 C66 107.2(8) . . ? O10 C68 C67 100.7(6) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 30.36 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.503 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.122