# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Franc Meyer' _publ_contact_author_email FRANC.MEYER@CHEMIE.UNI-GOETTINGEN.DE _publ_section_title ; Highly Preorganized Pyrazolate-Bridged Palladium(II) and Nickel(II) Complexes in Bimetallic Norbornene Polymerization ; loop_ _publ_author_name 'Franc Meyer' 'Venita Daebel' 'Sebastian Dechert' 'Serhiy Demeshko' 'Adam Lange' 'Anna Sachse' # Attachment 'Dalton_B925535D_cif.cif' #============================================================================== data_3-as3 _database_code_depnum_ccdc_archive 'CCDC 743828' #TrackingRef 'Dalton_B925535D_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Cl3 N4 Pd2, C3 H6 O' _chemical_formula_sum 'C38 H47 Cl3 N4 O Pd2' _chemical_formula_weight 894.95 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0887(6) _cell_length_b 30.3130(16) _cell_length_c 13.8048(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.161(5) _cell_angle_gamma 90.00 _cell_volume 4221.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 25842 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 24.79 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8369 _exptl_absorpt_correction_T_max 0.9506 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25842 _diffrn_reflns_av_R_equivalents 0.1057 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.79 _reflns_number_total 6973 _reflns_number_gt 4171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _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^)+(0.0130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6973 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.54269(5) 0.836799(16) 0.50236(4) 0.03201(13) Uani 1 1 d . . . Pd2 Pd 0.45944(5) 0.716521(17) 0.51107(4) 0.03376(14) Uani 1 1 d . . . Cl1 Cl 0.52503(18) 0.88878(6) 0.38327(12) 0.0440(5) Uani 1 1 d . . . Cl2 Cl 0.42871(15) 0.78061(6) 0.41312(10) 0.0334(4) Uani 1 1 d . . . Cl3 Cl 0.3940(2) 0.66605(7) 0.39699(13) 0.0535(5) Uani 1 1 d . . . N1 N 0.5719(5) 0.79506(18) 0.6049(3) 0.0303(13) Uani 1 1 d . . . N2 N 0.5385(5) 0.75352(18) 0.6085(4) 0.0329(13) Uani 1 1 d . . . N3 N 0.6435(5) 0.87369(18) 0.6026(4) 0.0312(13) Uani 1 1 d . . . N4 N 0.4889(5) 0.67343(18) 0.6220(4) 0.0360(14) Uani 1 1 d . . . C1 C 0.6640(6) 0.7677(2) 0.7405(4) 0.0312(15) Uani 1 1 d . . . C2 C 0.6490(5) 0.8059(2) 0.6843(5) 0.0321(15) Uani 1 1 d . . . C3 C 0.5934(6) 0.7348(2) 0.6901(4) 0.0304(15) Uani 1 1 d . . . C4 C 0.7366(6) 0.7619(2) 0.8320(4) 0.0330(15) Uani 1 1 d . . . C5 C 0.7508(6) 0.7966(2) 0.8971(4) 0.0404(17) Uani 1 1 d . . . H5 H 0.7156 0.8241 0.8816 0.080 Uiso 1 1 calc R . . C6 C 0.8164(6) 0.7911(3) 0.9843(5) 0.0490(19) Uani 1 1 d . . . H6 H 0.8250 0.8147 1.0270 0.080 Uiso 1 1 calc R . . C7 C 0.8691(7) 0.7505(3) 1.0079(5) 0.053(2) Uani 1 1 d . . . H7 H 0.9130 0.7466 1.0667 0.080 Uiso 1 1 calc R . . C8 C 0.8570(7) 0.7160(3) 0.9453(5) 0.0522(19) Uani 1 1 d . . . H8 H 0.8928 0.6887 0.9613 0.080 Uiso 1 1 calc R . . C9 C 0.7906(7) 0.7216(3) 0.8569(5) 0.0463(18) Uani 1 1 d . . . H9 H 0.7829 0.6980 0.8144 0.080 Uiso 1 1 calc R . . C10 C 0.6844(6) 0.8517(2) 0.6788(5) 0.0338(16) Uani 1 1 d . . . H10 H 0.7341 0.8652 0.7273 0.080 Uiso 1 1 calc R . . C11 C 0.6565(6) 0.9213(2) 0.6025(4) 0.0355(16) Uani 1 1 d . . . C12 C 0.5629(6) 0.9467(2) 0.6531(5) 0.0413(17) Uani 1 1 d . . . C13 C 0.5800(8) 0.9921(2) 0.6507(5) 0.049(2) Uani 1 1 d . . . H13 H 0.5198 1.0100 0.6831 0.080 Uiso 1 1 calc R . . C14 C 0.6848(9) 1.0117(3) 0.6012(6) 0.062(2) Uani 1 1 d . . . H14 H 0.6966 1.0421 0.6033 0.080 Uiso 1 1 calc R . . C15 C 0.7700(7) 0.9858(3) 0.5496(6) 0.055(2) Uani 1 1 d . . . H15 H 0.8378 0.9993 0.5149 0.080 Uiso 1 1 calc R . . C16 C 0.7593(5) 0.9408(3) 0.5471(5) 0.0418(15) Uani 1 1 d . . . C17 C 0.4466(6) 0.9262(2) 0.7058(5) 0.0454(18) Uani 1 1 d . . . H17 H 0.4743 0.8972 0.7296 0.080 Uiso 1 1 calc R . . C18 C 0.3333(7) 0.9194(3) 0.6354(6) 0.065(2) Uani 1 1 d . . . H18A H 0.3060 0.9474 0.6095 0.080 Uiso 1 1 calc R . . H18B H 0.2601 0.9059 0.6684 0.080 Uiso 1 1 calc R . . H18C H 0.3617 0.9006 0.5835 0.080 Uiso 1 1 calc R . . C19 C 0.3989(7) 0.9531(3) 0.7926(5) 0.064(2) Uani 1 1 d . . . H19A H 0.4707 0.9571 0.8375 0.080 Uiso 1 1 calc R . . H19B H 0.3276 0.9378 0.8240 0.080 Uiso 1 1 calc R . . H19C H 0.3683 0.9814 0.7708 0.080 Uiso 1 1 calc R . . C20 C 0.8526(6) 0.9131(2) 0.4871(5) 0.0483(18) Uani 1 1 d . . . H20 H 0.8125 0.8839 0.4790 0.080 Uiso 1 1 calc R . . C21 C 0.8714(7) 0.9331(3) 0.3864(5) 0.067(2) Uani 1 1 d . . . H21A H 0.7864 0.9395 0.3584 0.080 Uiso 1 1 calc R . . H21B H 0.9177 0.9125 0.3459 0.080 Uiso 1 1 calc R . . H21C H 0.9221 0.9598 0.3916 0.080 Uiso 1 1 calc R . . C22 C 0.9845(6) 0.9071(3) 0.5366(6) 0.061(2) Uani 1 1 d . . . H22A H 1.0242 0.9354 0.5479 0.080 Uiso 1 1 calc R . . H22B H 1.0416 0.8898 0.4961 0.080 Uiso 1 1 calc R . . H22C H 0.9719 0.8922 0.5973 0.080 Uiso 1 1 calc R . . C23 C 0.5533(6) 0.6890(2) 0.6978(5) 0.0349(16) Uani 1 1 d . . . H23 H 0.5716 0.6719 0.7521 0.080 Uiso 1 1 calc R . . C24 C 0.4346(7) 0.6295(2) 0.6257(5) 0.0392(17) Uani 1 1 d . . . C25 C 0.3069(7) 0.6229(3) 0.6615(5) 0.051(2) Uani 1 1 d . . . C26 C 0.2574(8) 0.5809(3) 0.6586(6) 0.063(2) Uani 1 1 d . . . H26 H 0.1718 0.5761 0.6811 0.080 Uiso 1 1 calc R . . C27 C 0.3255(9) 0.5468(3) 0.6253(7) 0.075(3) Uani 1 1 d . . . H27 H 0.2884 0.5187 0.6262 0.080 Uiso 1 1 calc R . . C28 C 0.4538(9) 0.5531(3) 0.5885(6) 0.068(2) Uani 1 1 d . . . H28 H 0.5014 0.5293 0.5641 0.080 Uiso 1 1 calc R . . C29 C 0.5091(7) 0.5950(2) 0.5889(5) 0.0460(18) Uani 1 1 d . . . C30 C 0.2231(6) 0.6607(3) 0.7004(5) 0.0478(18) Uani 1 1 d . . . H30 H 0.2810 0.6865 0.7071 0.080 Uiso 1 1 calc R . . C31 C 0.1135(8) 0.6729(3) 0.6318(6) 0.083(3) Uani 1 1 d . . . H31A H 0.1507 0.6847 0.5733 0.080 Uiso 1 1 calc R . . H31B H 0.0575 0.6946 0.6613 0.080 Uiso 1 1 calc R . . H31C H 0.0622 0.6471 0.6167 0.080 Uiso 1 1 calc R . . C32 C 0.1681(7) 0.6502(3) 0.7998(6) 0.064(2) Uani 1 1 d . . . H32A H 0.1085 0.6256 0.7951 0.080 Uiso 1 1 calc R . . H32B H 0.1213 0.6754 0.8243 0.080 Uiso 1 1 calc R . . H32C H 0.2396 0.6429 0.8429 0.080 Uiso 1 1 calc R . . C33 C 0.6500(8) 0.6027(3) 0.5520(5) 0.060(2) Uani 1 1 d . . . H33 H 0.6587 0.6344 0.5402 0.080 Uiso 1 1 calc R . . C34 C 0.6828(10) 0.5799(4) 0.4584(7) 0.097(3) Uani 1 1 d . . . H34A H 0.6947 0.5489 0.4701 0.080 Uiso 1 1 calc R . . H34B H 0.7630 0.5920 0.4324 0.080 Uiso 1 1 calc R . . H34C H 0.6117 0.5841 0.4130 0.080 Uiso 1 1 calc R . . C35 C 0.7513(8) 0.5907(3) 0.6308(6) 0.077(3) Uani 1 1 d . . . H35A H 0.7552 0.5593 0.6378 0.080 Uiso 1 1 calc R . . H35B H 0.7251 0.6038 0.6911 0.080 Uiso 1 1 calc R . . H35C H 0.8371 0.6017 0.6127 0.080 Uiso 1 1 calc R . . O1 O -0.0162(6) 0.8169(3) 0.6856(5) 0.104(2) Uani 1 1 d . . . C36 C 0.1051(9) 0.7826(4) 0.8090(7) 0.093(3) Uani 1 1 d . . . H36A H 0.0193 0.7753 0.8343 0.080 Uiso 1 1 calc R . . H36B H 0.1482 0.8031 0.8517 0.080 Uiso 1 1 calc R . . H36C H 0.1576 0.7563 0.8037 0.080 Uiso 1 1 calc R . . C37 C 0.0900(8) 0.8025(3) 0.7142(7) 0.063(2) Uani 1 1 d . . . C38 C 0.2067(9) 0.8006(3) 0.6507(7) 0.104(4) Uani 1 1 d . . . H38A H 0.2186 0.7710 0.6277 0.080 Uiso 1 1 calc R . . H38B H 0.2839 0.8096 0.6863 0.080 Uiso 1 1 calc R . . H38C H 0.1937 0.8200 0.5965 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0372(3) 0.0245(3) 0.0343(3) -0.0009(2) -0.0017(2) 0.0018(3) Pd2 0.0407(3) 0.0274(3) 0.0331(3) -0.0028(3) -0.0056(2) -0.0018(3) Cl1 0.0629(12) 0.0291(12) 0.0399(10) 0.0013(7) -0.0059(8) 0.0052(8) Cl2 0.0424(9) 0.0273(10) 0.0305(8) -0.0007(7) -0.0045(7) 0.0004(8) Cl3 0.0737(13) 0.0376(13) 0.0493(11) -0.0089(9) -0.0179(9) -0.0019(10) N1 0.029(3) 0.032(4) 0.030(3) 0.000(2) -0.005(2) -0.001(2) N2 0.038(3) 0.022(4) 0.039(3) 0.005(2) 0.002(2) -0.004(2) N3 0.035(3) 0.028(4) 0.031(3) -0.004(2) -0.002(2) 0.001(2) N4 0.048(3) 0.023(4) 0.038(3) 0.000(2) -0.007(3) -0.002(2) C1 0.033(3) 0.026(4) 0.035(4) -0.008(3) 0.002(3) -0.003(3) C2 0.028(3) 0.021(4) 0.047(4) -0.007(3) 0.008(3) -0.003(3) C3 0.040(4) 0.029(4) 0.023(3) 0.003(3) 0.002(3) 0.003(3) C4 0.033(4) 0.031(4) 0.034(4) -0.001(3) 0.001(3) -0.005(3) C5 0.036(4) 0.047(5) 0.039(4) -0.003(3) 0.005(3) -0.003(3) C6 0.048(4) 0.065(6) 0.034(4) -0.003(3) -0.009(3) -0.004(4) C7 0.044(4) 0.072(7) 0.044(4) 0.009(4) -0.009(3) -0.014(4) C8 0.055(4) 0.045(5) 0.057(5) 0.014(4) -0.016(4) -0.007(4) C9 0.049(4) 0.038(5) 0.052(4) 0.005(4) -0.006(4) -0.015(3) C10 0.028(3) 0.032(5) 0.042(4) -0.008(3) 0.002(3) -0.004(3) C11 0.048(4) 0.020(4) 0.039(4) -0.001(3) -0.002(3) 0.003(3) C12 0.043(4) 0.035(5) 0.046(4) -0.001(3) -0.003(3) 0.000(3) C13 0.063(5) 0.031(5) 0.052(5) -0.006(3) 0.002(4) 0.005(4) C14 0.081(7) 0.032(6) 0.074(6) -0.004(4) 0.005(5) -0.002(5) C15 0.055(5) 0.034(6) 0.077(6) 0.012(4) 0.010(4) -0.005(4) C16 0.040(3) 0.029(4) 0.056(4) 0.002(4) 0.005(3) 0.001(4) C17 0.042(4) 0.033(5) 0.061(5) -0.003(3) 0.009(3) 0.005(3) C18 0.051(5) 0.070(7) 0.075(6) -0.014(5) 0.009(4) -0.008(4) C19 0.059(5) 0.074(8) 0.058(5) -0.012(4) 0.015(4) 0.004(4) C20 0.037(4) 0.043(5) 0.065(5) -0.002(4) 0.012(3) -0.001(3) C21 0.058(5) 0.078(7) 0.064(5) 0.002(5) 0.009(4) 0.012(5) C22 0.049(5) 0.050(6) 0.082(6) 0.023(4) 0.010(4) 0.011(4) C23 0.030(3) 0.027(4) 0.047(4) -0.006(3) 0.003(3) -0.002(3) C24 0.055(4) 0.021(4) 0.042(4) -0.001(3) -0.022(3) -0.009(3) C25 0.053(5) 0.038(5) 0.062(5) 0.002(4) -0.016(4) -0.019(4) C26 0.072(6) 0.031(6) 0.084(6) 0.005(4) -0.006(5) -0.017(4) C27 0.088(7) 0.039(7) 0.097(7) 0.001(5) -0.023(6) -0.031(5) C28 0.096(7) 0.028(6) 0.081(6) -0.011(4) -0.014(5) 0.005(5) C29 0.065(5) 0.032(5) 0.040(4) 0.002(3) -0.011(3) -0.004(4) C30 0.043(4) 0.039(5) 0.062(5) 0.006(4) -0.003(3) -0.007(3) C31 0.085(6) 0.069(7) 0.094(7) 0.016(5) -0.030(5) 0.007(5) C32 0.038(4) 0.066(7) 0.088(6) 0.008(4) -0.003(4) -0.006(4) C33 0.082(6) 0.045(6) 0.053(5) -0.009(4) -0.006(4) 0.013(4) C34 0.106(8) 0.094(9) 0.090(7) -0.041(6) 0.004(6) 0.026(6) C35 0.065(6) 0.091(8) 0.075(6) 0.001(5) -0.002(5) 0.000(5) O1 0.077(4) 0.104(6) 0.130(6) 0.040(5) 0.012(4) 0.007(4) C36 0.063(6) 0.123(10) 0.094(7) 0.015(7) -0.002(5) -0.006(6) C37 0.043(5) 0.061(6) 0.084(7) -0.002(5) 0.005(4) 0.002(4) C38 0.093(8) 0.092(10) 0.126(9) -0.003(7) 0.054(7) 0.008(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 N1 1.921(5) . ? Pd1 N3 2.048(5) . ? Pd1 Cl1 2.2838(18) . ? Pd1 Cl2 2.3943(17) . ? Pd2 N2 1.923(5) . ? Pd2 N4 2.034(5) . ? Pd2 Cl3 2.2914(19) . ? Pd2 Cl2 2.3867(17) . ? N1 N2 1.305(7) . ? N1 C2 1.381(7) . ? N2 C3 1.376(7) . ? N3 C10 1.311(8) . ? N3 C11 1.448(8) . ? N4 C23 1.317(7) . ? N4 C24 1.441(8) . ? C1 C2 1.400(8) . ? C1 C3 1.408(8) . ? C1 C4 1.469(8) . ? C2 C10 1.437(8) . ? C3 C23 1.451(9) . ? C4 C9 1.380(9) . ? C4 C5 1.391(8) . ? C5 C6 1.383(8) . ? C6 C7 1.380(10) . ? C7 C8 1.361(10) . ? C8 C9 1.401(9) . ? C11 C12 1.406(9) . ? C11 C16 1.420(9) . ? C12 C13 1.387(10) . ? C12 C17 1.516(9) . ? C13 C14 1.393(11) . ? C14 C15 1.365(11) . ? C15 C16 1.371(10) . ? C16 C20 1.510(9) . ? C17 C18 1.513(9) . ? C17 C19 1.528(9) . ? C20 C22 1.505(9) . ? C20 C21 1.529(10) . ? C24 C29 1.386(10) . ? C24 C25 1.395(9) . ? C25 C26 1.368(10) . ? C25 C30 1.524(10) . ? C26 C27 1.324(11) . ? C27 C28 1.405(11) . ? C28 C29 1.386(10) . ? C29 C33 1.530(10) . ? C30 C31 1.500(9) . ? C30 C32 1.515(10) . ? C33 C34 1.502(10) . ? C33 C35 1.533(10) . ? O1 C37 1.222(9) . ? C36 C37 1.448(11) . ? C37 C38 1.471(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N3 77.7(2) . . ? N1 Pd1 Cl1 175.21(16) . . ? N3 Pd1 Cl1 98.48(16) . . ? N1 Pd1 Cl2 89.04(16) . . ? N3 Pd1 Cl2 166.70(16) . . ? Cl1 Pd1 Cl2 94.82(6) . . ? N2 Pd2 N4 77.8(2) . . ? N2 Pd2 Cl3 171.24(16) . . ? N4 Pd2 Cl3 97.45(15) . . ? N2 Pd2 Cl2 88.54(16) . . ? N4 Pd2 Cl2 165.42(16) . . ? Cl3 Pd2 Cl2 96.75(7) . . ? Pd2 Cl2 Pd1 103.07(5) . . ? N2 N1 C2 110.1(5) . . ? N2 N1 Pd1 128.7(4) . . ? C2 N1 Pd1 120.9(4) . . ? N1 N2 C3 109.0(5) . . ? N1 N2 Pd2 130.0(4) . . ? C3 N2 Pd2 119.9(4) . . ? C10 N3 C11 118.6(5) . . ? C10 N3 Pd1 114.8(4) . . ? C11 N3 Pd1 126.0(4) . . ? C23 N4 C24 119.3(5) . . ? C23 N4 Pd2 116.0(5) . . ? C24 N4 Pd2 124.4(4) . . ? C2 C1 C3 104.9(5) . . ? C2 C1 C4 128.9(5) . . ? C3 C1 C4 126.1(6) . . ? N1 C2 C1 107.7(5) . . ? N1 C2 C10 109.1(6) . . ? C1 C2 C10 143.2(6) . . ? N2 C3 C1 108.3(6) . . ? N2 C3 C23 110.0(5) . . ? C1 C3 C23 141.5(6) . . ? C9 C4 C5 118.0(6) . . ? C9 C4 C1 121.0(6) . . ? C5 C4 C1 121.0(6) . . ? C6 C5 C4 121.2(7) . . ? C7 C6 C5 119.9(7) . . ? C8 C7 C6 120.1(7) . . ? C7 C8 C9 120.1(7) . . ? C4 C9 C8 120.8(7) . . ? N3 C10 C2 117.1(6) . . ? C12 C11 C16 122.1(6) . . ? C12 C11 N3 119.0(6) . . ? C16 C11 N3 118.8(6) . . ? C13 C12 C11 116.7(6) . . ? C13 C12 C17 120.9(6) . . ? C11 C12 C17 122.4(7) . . ? C12 C13 C14 121.9(7) . . ? C15 C14 C13 119.5(8) . . ? C14 C15 C16 122.3(7) . . ? C15 C16 C11 117.3(6) . . ? C15 C16 C20 121.2(6) . . ? C11 C16 C20 121.4(7) . . ? C18 C17 C12 109.4(6) . . ? C18 C17 C19 109.7(6) . . ? C12 C17 C19 113.8(6) . . ? C22 C20 C16 111.8(6) . . ? C22 C20 C21 110.4(6) . . ? C16 C20 C21 110.9(6) . . ? N4 C23 C3 115.0(6) . . ? C29 C24 C25 121.5(6) . . ? C29 C24 N4 118.6(6) . . ? C25 C24 N4 119.8(6) . . ? C26 C25 C24 117.4(7) . . ? C26 C25 C30 120.5(7) . . ? C24 C25 C30 122.1(6) . . ? C27 C26 C25 123.1(8) . . ? C26 C27 C28 120.0(8) . . ? C29 C28 C27 119.6(8) . . ? C28 C29 C24 118.3(7) . . ? C28 C29 C33 120.9(7) . . ? C24 C29 C33 120.8(7) . . ? C31 C30 C32 110.7(6) . . ? C31 C30 C25 111.8(7) . . ? C32 C30 C25 111.5(6) . . ? C34 C33 C29 115.0(7) . . ? C34 C33 C35 110.7(7) . . ? C29 C33 C35 110.2(6) . . ? O1 C37 C36 122.0(8) . . ? O1 C37 C38 121.6(9) . . ? C36 C37 C38 116.1(8) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 24.79 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.598 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.106 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 -0.000 -0.000 -0.000 267 67 ' ' 2 -0.000 0.500 0.500 267 67 ' ' _platon_squeeze_details ; ; #===END data_4-as6 _database_code_depnum_ccdc_archive 'CCDC 743829' #TrackingRef 'Dalton_B925535D_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H49 Cl3 N4 Pd2, 2.5(C H Cl3)' _chemical_formula_sum 'C49.50 H51.50 Cl10.50 N4 Pd2' _chemical_formula_weight 1287.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.082(3) _cell_length_b 12.8094(6) _cell_length_c 28.7200(19) _cell_angle_alpha 90.00 _cell_angle_beta 124.805(5) _cell_angle_gamma 90.00 _cell_volume 10899.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 31067 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 24.71 _exptl_crystal_description block _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5176 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8468 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31067 _diffrn_reflns_av_R_equivalents 0.0898 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8805 _reflns_number_gt 5604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _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^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8805 _refine_ls_number_parameters 626 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.636136(15) 0.26384(3) 0.368261(19) 0.02866(11) Uani 1 1 d . . . Pd2 Pd 0.618859(15) 0.41811(3) 0.464638(19) 0.02899(11) Uani 1 1 d . . . Cl1 Cl 0.65160(5) 0.09280(9) 0.36653(6) 0.0435(4) Uani 1 1 d . . . Cl2 Cl 0.62769(5) 0.24347(9) 0.44410(6) 0.0396(4) Uani 1 1 d . . . Cl3 Cl 0.61372(6) 0.37108(9) 0.53753(6) 0.0432(4) Uani 1 1 d . . . Cl4 Cl 0.73362(7) 0.38793(16) 0.48519(10) 0.1001(8) Uani 1 1 d . . . Cl5 Cl 0.77836(7) 0.49695(13) 0.44429(8) 0.0722(6) Uani 1 1 d . . . Cl6 Cl 0.74955(7) 0.60990(14) 0.50403(9) 0.0798(6) Uani 1 1 d . . . Cl7 Cl 0.62149(8) -0.01207(13) 0.56557(9) 0.0745(6) Uani 1 1 d . . . Cl8 Cl 0.61229(6) 0.15173(11) 0.62634(8) 0.0565(5) Uani 1 1 d . . . Cl9 Cl 0.54077(9) 0.1088(2) 0.51029(12) 0.1438(13) Uani 1 1 d . . . C51 C 0.4898(7) 0.4211(7) 0.2398(6) 0.085(8) Uani 0.50 1 d PD A -1 H51 H 0.4584 0.3978 0.2141 0.080 Uiso 0.50 1 calc PR A -1 Cl10 Cl 0.4942(4) 0.5148(8) 0.2871(5) 0.125(3) Uani 0.50 1 d PD A -1 Cl11 Cl 0.52392(14) 0.3182(3) 0.28391(19) 0.0842(13) Uani 0.50 1 d PD A -1 Cl12 Cl 0.5094(5) 0.4745(7) 0.2014(5) 0.096(3) Uani 0.50 1 d PD A -1 N1 N 0.62710(15) 0.4108(3) 0.36878(18) 0.0279(10) Uani 1 1 d . . . N2 N 0.62095(15) 0.4650(3) 0.40266(19) 0.0299(11) Uani 1 1 d . . . N3 N 0.63982(15) 0.3163(3) 0.30337(19) 0.0274(10) Uani 1 1 d . . . N4 N 0.61267(14) 0.5774(3) 0.46705(18) 0.0270(10) Uani 1 1 d . . . C1 C 0.62521(16) 0.5804(3) 0.3469(2) 0.0244(11) Uani 1 1 d . . . C2 C 0.63078(17) 0.4770(3) 0.3344(2) 0.0227(12) Uani 1 1 d . . . C3 C 0.61914(17) 0.5680(3) 0.3905(2) 0.0279(12) Uani 1 1 d . . . C4 C 0.62776(19) 0.6803(4) 0.3226(2) 0.0294(13) Uani 1 1 d . . . C5 C 0.5991(2) 0.7012(4) 0.2655(3) 0.0440(16) Uani 1 1 d . . . H5 H 0.5781 0.6513 0.2413 0.080 Uiso 1 1 calc R . . C6 C 0.6013(3) 0.7975(4) 0.2435(3) 0.057(2) Uani 1 1 d . . . H6 H 0.5813 0.8128 0.2051 0.080 Uiso 1 1 calc R . . C7 C 0.6343(2) 0.8695(4) 0.2808(3) 0.0513(18) Uani 1 1 d . . . H7 H 0.6370 0.9329 0.2671 0.080 Uiso 1 1 calc R . . C8 C 0.6626(2) 0.8470(4) 0.3372(3) 0.0418(16) Uani 1 1 d . . . H8 H 0.6842 0.8958 0.3615 0.080 Uiso 1 1 calc R . . C9 C 0.66003(18) 0.7540(4) 0.3593(2) 0.0326(13) Uani 1 1 d . . . H9 H 0.6794 0.7404 0.3979 0.080 Uiso 1 1 calc R . . C10 C 0.63901(16) 0.4185(3) 0.2973(2) 0.0233(11) Uani 1 1 d . . . C12 C 0.62453(18) 0.4532(3) 0.2026(2) 0.0247(12) Uani 1 1 d . . . H12 H 0.6039 0.3985 0.1872 0.080 Uiso 1 1 calc R . . C13 C 0.63146(19) 0.5127(4) 0.1673(2) 0.0335(14) Uani 1 1 d . . . H13 H 0.6151 0.4990 0.1286 0.080 Uiso 1 1 calc R . . C14 C 0.66331(19) 0.5927(4) 0.1910(2) 0.0356(13) Uani 1 1 d . . . H14 H 0.6686 0.6321 0.1682 0.080 Uiso 1 1 calc R . . C15 C 0.6868(2) 0.6135(4) 0.2479(3) 0.0370(14) Uani 1 1 d . . . H15 H 0.7079 0.6672 0.2633 0.080 Uiso 1 1 calc R . . C16 C 0.67961(18) 0.5556(3) 0.2829(2) 0.0293(13) Uani 1 1 d . . . H16 H 0.6957 0.5705 0.3215 0.080 Uiso 1 1 calc R . . C17 C 0.64773(18) 0.4746(3) 0.2595(2) 0.0242(12) Uani 1 1 d . . . C18 C 0.64854(17) 0.2462(3) 0.2707(2) 0.0250(11) Uani 1 1 d . . . C19 C 0.61291(18) 0.1841(3) 0.2289(2) 0.0256(12) Uani 1 1 d . . . C20 C 0.62229(19) 0.1138(3) 0.2000(2) 0.0310(13) Uani 1 1 d . . . H20 H 0.5991 0.0735 0.1710 0.080 Uiso 1 1 calc R . . C21 C 0.6657(2) 0.1032(4) 0.2140(2) 0.0385(14) Uani 1 1 d . . . H21 H 0.6714 0.0552 0.1945 0.080 Uiso 1 1 calc R . . C22 C 0.7005(2) 0.1626(4) 0.2564(2) 0.0342(14) Uani 1 1 d . . . H22 H 0.7295 0.1538 0.2654 0.080 Uiso 1 1 calc R . . C23 C 0.69286(18) 0.2361(4) 0.2861(2) 0.0307(12) Uani 1 1 d . . . C24 C 0.56473(19) 0.1912(4) 0.2133(2) 0.0360(14) Uani 1 1 d . . . H24 H 0.5645 0.2450 0.2374 0.080 Uiso 1 1 calc R . . C25 C 0.5493(2) 0.0893(4) 0.2244(3) 0.0563(17) Uani 1 1 d . . . H25A H 0.5200 0.0988 0.2171 0.080 Uiso 1 1 calc R . . H25B H 0.5704 0.0689 0.2632 0.080 Uiso 1 1 calc R . . H25C H 0.5477 0.0358 0.1999 0.080 Uiso 1 1 calc R . . C26 C 0.5300(2) 0.2227(5) 0.1515(3) 0.0535(17) Uani 1 1 d . . . H26A H 0.5288 0.1702 0.1268 0.080 Uiso 1 1 calc R . . H26B H 0.5385 0.2883 0.1441 0.080 Uiso 1 1 calc R . . H26C H 0.5008 0.2292 0.1448 0.080 Uiso 1 1 calc R . . C27 C 0.73220(19) 0.2978(4) 0.3335(3) 0.0391(15) Uani 1 1 d . . . H27 H 0.7202 0.3512 0.3460 0.080 Uiso 1 1 calc R . . C28 C 0.7630(2) 0.2265(4) 0.3835(3) 0.065(2) Uani 1 1 d . . . H28A H 0.7457 0.1905 0.3943 0.080 Uiso 1 1 calc R . . H28B H 0.7861 0.2674 0.4148 0.080 Uiso 1 1 calc R . . H28C H 0.7768 0.1766 0.3729 0.080 Uiso 1 1 calc R . . C29 C 0.7584(2) 0.3531(5) 0.3134(3) 0.062(2) Uani 1 1 d . . . H29A H 0.7727 0.3020 0.3041 0.080 Uiso 1 1 calc R . . H29B H 0.7810 0.3976 0.3430 0.080 Uiso 1 1 calc R . . H29C H 0.7380 0.3943 0.2804 0.080 Uiso 1 1 calc R . . C30 C 0.61075(17) 0.6305(4) 0.4265(2) 0.0258(12) Uani 1 1 d . . . C31 C 0.59767(17) 0.7425(3) 0.4122(2) 0.0263(12) Uani 1 1 d . . . C32 C 0.5626(2) 0.7649(4) 0.3567(3) 0.0428(15) Uani 1 1 d . . . H32 H 0.5484 0.7107 0.3307 0.080 Uiso 1 1 calc R . . C33 C 0.5485(2) 0.8667(5) 0.3393(3) 0.0552(18) Uani 1 1 d . . . H33 H 0.5248 0.8810 0.3020 0.080 Uiso 1 1 calc R . . C34 C 0.5700(2) 0.9468(4) 0.3782(3) 0.0516(17) Uani 1 1 d . . . H34 H 0.5608 1.0155 0.3670 0.080 Uiso 1 1 calc R . . C35 C 0.6049(2) 0.9255(4) 0.4332(3) 0.0446(15) Uani 1 1 d . . . H35 H 0.6194 0.9801 0.4589 0.080 Uiso 1 1 calc R . . C36 C 0.6190(2) 0.8231(4) 0.4510(3) 0.0373(15) Uani 1 1 d . . . H36 H 0.6424 0.8090 0.4884 0.080 Uiso 1 1 calc R . . C37 C 0.60325(19) 0.6291(3) 0.5047(2) 0.0264(12) Uani 1 1 d . . . C38 C 0.55790(18) 0.6402(4) 0.4852(2) 0.0315(13) Uani 1 1 d . . . C39 C 0.5499(2) 0.6874(4) 0.5222(3) 0.0379(14) Uani 1 1 d . . . H39 H 0.5203 0.6964 0.5112 0.080 Uiso 1 1 calc R . . C40 C 0.5853(2) 0.7214(4) 0.5753(2) 0.0358(14) Uani 1 1 d . . . H40 H 0.5792 0.7538 0.5993 0.080 Uiso 1 1 calc R . . C41 C 0.6288(2) 0.7078(4) 0.5926(2) 0.0343(14) Uani 1 1 d . . . H41 H 0.6520 0.7305 0.6286 0.080 Uiso 1 1 calc R . . C42 C 0.63959(19) 0.6605(3) 0.5579(2) 0.0305(13) Uani 1 1 d . B . C43 C 0.5187(2) 0.6022(5) 0.4275(3) 0.0473(16) Uani 1 1 d . . . H43 H 0.5305 0.5870 0.4049 0.080 Uiso 1 1 calc R . . C44 C 0.4987(2) 0.5021(5) 0.4322(3) 0.071(2) Uani 1 1 d . . . H44A H 0.4848 0.5158 0.4518 0.080 Uiso 1 1 calc R . . H44B H 0.5222 0.4512 0.4530 0.080 Uiso 1 1 calc R . . H44C H 0.4765 0.4759 0.3950 0.080 Uiso 1 1 calc R . . C45 C 0.4829(2) 0.6844(6) 0.3967(3) 0.074(2) Uani 1 1 d . . . H45A H 0.4704 0.7004 0.4177 0.080 Uiso 1 1 calc R . . H45B H 0.4595 0.6590 0.3597 0.080 Uiso 1 1 calc R . . H45C H 0.4960 0.7462 0.3928 0.080 Uiso 1 1 calc R . . C46 C 0.6884(2) 0.6472(4) 0.5790(3) 0.0441(15) Uani 1 1 d D . . C47A C 0.7096(4) 0.5549(7) 0.6181(5) 0.086(4) Uani 0.871(19) 1 d PD B 2 H47A H 0.7139 0.5706 0.6536 0.080 Uiso 0.871(19) 1 calc PR B 2 H47B H 0.7382 0.5398 0.6245 0.080 Uiso 0.871(19) 1 calc PR B 2 H47C H 0.6901 0.4954 0.6012 0.080 Uiso 0.871(19) 1 calc PR B 2 C48A C 0.7164(3) 0.7434(5) 0.6098(5) 0.064(3) Uani 0.871(19) 1 d PD B 2 H48A H 0.7024 0.8037 0.5860 0.080 Uiso 0.871(19) 1 calc PR B 2 H48B H 0.7462 0.7349 0.6183 0.080 Uiso 0.871(19) 1 calc PR B 2 H48C H 0.7185 0.7527 0.6443 0.080 Uiso 0.871(19) 1 calc PR B 2 H46A H 0.6894 0.6348 0.5462 0.080 Uiso 0.871(19) 1 d P B 2 C47B C 0.715(2) 0.583(6) 0.633(2) 0.086(4) Uani 0.129(19) 1 d PD B 3 H47D H 0.7181 0.6216 0.6635 0.080 Uiso 0.129(19) 1 calc PR B 3 H47E H 0.7439 0.5669 0.6410 0.080 Uiso 0.129(19) 1 calc PR B 3 H47F H 0.6987 0.5192 0.6274 0.080 Uiso 0.129(19) 1 calc PR B 3 C48B C 0.7201(16) 0.724(4) 0.579(3) 0.064(3) Uani 0.129(19) 1 d PD B 3 H48D H 0.7032 0.7713 0.5480 0.080 Uiso 0.129(19) 1 calc PR B 3 H48E H 0.7418 0.6875 0.5763 0.080 Uiso 0.129(19) 1 calc PR B 3 H48F H 0.7355 0.7632 0.6142 0.080 Uiso 0.129(19) 1 calc PR B 3 H46B H 0.6853 0.5965 0.5515 0.080 Uiso 0.129(19) 1 d P B 3 C49 C 0.7702(2) 0.4893(4) 0.4988(3) 0.0447(15) Uani 1 1 d . . . H49 H 0.7993 0.4754 0.5346 0.080 Uiso 1 1 calc R . . C50 C 0.5989(2) 0.1107(4) 0.5603(3) 0.0515(17) Uani 1 1 d . . . H50 H 0.6122 0.1603 0.5476 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0448(3) 0.02018(19) 0.0258(3) 0.00037(17) 0.0230(2) 0.00032(19) Pd2 0.0441(3) 0.02438(19) 0.0276(3) 0.00074(18) 0.0258(2) -0.00069(19) Cl1 0.0732(11) 0.0225(6) 0.0343(10) 0.0038(6) 0.0304(9) 0.0075(7) Cl2 0.0715(11) 0.0250(6) 0.0374(10) 0.0006(6) 0.0399(9) -0.0025(7) Cl3 0.0739(11) 0.0344(7) 0.0397(10) 0.0020(6) 0.0432(9) -0.0028(7) Cl4 0.0756(15) 0.0940(15) 0.0854(17) 0.0233(12) 0.0192(12) -0.0397(12) Cl5 0.0999(16) 0.0716(11) 0.0500(14) -0.0110(9) 0.0457(12) -0.0113(10) Cl6 0.0813(14) 0.0839(13) 0.0608(14) -0.0053(10) 0.0326(12) 0.0215(11) Cl7 0.1118(17) 0.0601(10) 0.0598(14) 0.0002(9) 0.0539(13) 0.0241(10) Cl8 0.0701(13) 0.0464(9) 0.0624(13) -0.0026(7) 0.0434(11) 0.0052(8) Cl9 0.0781(18) 0.123(2) 0.119(2) -0.0444(17) -0.0093(16) 0.0159(15) C51 0.11(2) 0.086(8) 0.014(14) -0.012(8) 0.008(16) -0.031(12) Cl10 0.097(5) 0.175(9) 0.105(8) -0.073(7) 0.058(5) -0.021(7) Cl11 0.080(3) 0.102(3) 0.098(4) 0.027(2) 0.067(3) 0.025(2) Cl12 0.134(6) 0.086(4) 0.069(5) 0.019(3) 0.059(4) 0.032(4) N1 0.040(3) 0.029(2) 0.022(3) -0.0014(19) 0.022(2) -0.001(2) N2 0.041(3) 0.023(2) 0.031(3) 0.0012(19) 0.024(3) 0.0047(19) N3 0.036(3) 0.023(2) 0.026(3) -0.0028(18) 0.019(2) 0.0018(19) N4 0.033(3) 0.031(2) 0.020(3) -0.0020(19) 0.017(2) 0.001(2) C1 0.032(3) 0.021(2) 0.019(3) 0.001(2) 0.014(3) 0.003(2) C2 0.029(3) 0.028(3) 0.015(3) -0.004(2) 0.015(3) 0.001(2) C3 0.035(3) 0.023(3) 0.026(4) 0.003(2) 0.017(3) 0.006(2) C4 0.045(4) 0.025(3) 0.028(4) 0.005(2) 0.026(3) 0.007(2) C5 0.075(5) 0.029(3) 0.032(4) 0.003(2) 0.032(4) 0.003(3) C6 0.100(6) 0.036(3) 0.039(5) 0.012(3) 0.042(4) 0.014(3) C7 0.092(6) 0.026(3) 0.049(5) 0.010(3) 0.048(5) 0.005(3) C8 0.057(4) 0.026(3) 0.056(5) -0.003(3) 0.041(4) -0.003(3) C9 0.043(3) 0.027(3) 0.031(4) -0.002(2) 0.024(3) -0.003(2) C10 0.024(3) 0.023(2) 0.019(3) -0.003(2) 0.010(2) 0.001(2) C12 0.031(3) 0.025(2) 0.022(4) -0.002(2) 0.017(3) -0.001(2) C13 0.047(4) 0.032(3) 0.026(4) 0.002(2) 0.023(3) 0.007(3) C14 0.051(4) 0.029(3) 0.043(4) 0.004(3) 0.037(3) 0.000(3) C15 0.045(4) 0.035(3) 0.038(4) -0.002(2) 0.027(3) -0.007(2) C16 0.036(3) 0.032(3) 0.024(4) -0.001(2) 0.020(3) -0.003(2) C17 0.036(3) 0.022(2) 0.024(4) -0.002(2) 0.023(3) 0.003(2) C18 0.030(3) 0.025(3) 0.022(3) 0.003(2) 0.016(3) 0.006(2) C19 0.037(3) 0.023(2) 0.019(3) 0.001(2) 0.018(3) -0.002(2) C20 0.047(4) 0.023(2) 0.025(4) -0.001(2) 0.021(3) 0.003(2) C21 0.061(4) 0.025(3) 0.032(4) -0.001(2) 0.028(3) 0.007(3) C22 0.042(4) 0.034(3) 0.036(4) 0.000(2) 0.028(3) 0.010(3) C23 0.043(3) 0.029(3) 0.020(3) 0.003(2) 0.017(3) 0.006(2) C24 0.038(4) 0.037(3) 0.030(4) -0.008(2) 0.018(3) -0.010(2) C25 0.056(4) 0.060(4) 0.053(5) 0.007(3) 0.032(4) -0.017(3) C26 0.041(4) 0.065(4) 0.056(5) 0.008(3) 0.028(4) -0.002(3) C27 0.036(4) 0.036(3) 0.036(4) -0.006(2) 0.015(3) 0.006(2) C28 0.057(5) 0.045(3) 0.054(5) -0.014(3) 0.007(4) 0.015(3) C29 0.054(5) 0.064(4) 0.080(6) -0.022(4) 0.045(5) -0.011(3) C30 0.026(3) 0.030(3) 0.021(4) 0.000(2) 0.013(3) 0.001(2) C31 0.036(3) 0.024(2) 0.025(3) 0.005(2) 0.021(3) 0.008(2) C32 0.047(4) 0.037(3) 0.035(4) 0.000(3) 0.018(3) 0.011(3) C33 0.065(5) 0.054(4) 0.033(4) 0.014(3) 0.020(4) 0.025(3) C34 0.073(5) 0.035(3) 0.052(5) 0.011(3) 0.039(4) 0.020(3) C35 0.073(5) 0.034(3) 0.034(4) 0.004(3) 0.035(4) 0.008(3) C36 0.055(4) 0.031(3) 0.029(4) -0.001(2) 0.026(3) 0.003(3) C37 0.042(4) 0.025(2) 0.019(4) 0.001(2) 0.021(3) -0.001(2) C38 0.028(3) 0.040(3) 0.027(4) -0.006(2) 0.017(3) 0.000(2) C39 0.041(4) 0.048(3) 0.032(4) 0.003(3) 0.026(3) 0.012(3) C40 0.052(4) 0.035(3) 0.027(4) -0.001(2) 0.026(3) 0.002(3) C41 0.044(4) 0.038(3) 0.027(4) -0.004(2) 0.024(3) -0.007(3) C42 0.041(4) 0.028(3) 0.030(4) -0.001(2) 0.025(3) -0.005(2) C43 0.038(4) 0.070(4) 0.033(4) -0.007(3) 0.020(3) 0.003(3) C44 0.052(5) 0.079(5) 0.062(6) -0.028(4) 0.021(4) -0.022(4) C45 0.054(5) 0.099(5) 0.042(5) -0.004(4) 0.011(4) 0.008(4) C46 0.039(4) 0.053(4) 0.045(5) -0.008(3) 0.026(3) -0.011(3) C47A 0.050(5) 0.037(6) 0.177(11) 0.036(6) 0.069(6) 0.020(4) C48A 0.035(4) 0.047(4) 0.084(8) 0.016(4) 0.019(5) -0.005(3) C47B 0.050(5) 0.037(6) 0.177(11) 0.036(6) 0.069(6) 0.020(4) C48B 0.035(4) 0.047(4) 0.084(8) 0.016(4) 0.019(5) -0.005(3) C49 0.046(4) 0.048(3) 0.040(4) 0.003(3) 0.024(4) -0.005(3) C50 0.062(5) 0.041(3) 0.041(5) -0.001(3) 0.023(4) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 1.911(4) . ? Pd1 N3 2.056(4) . ? Pd1 Cl1 2.2685(12) . ? Pd1 Cl2 2.3797(13) . ? Pd2 N2 1.921(4) . ? Pd2 N4 2.058(4) . ? Pd2 Cl3 2.2854(14) . ? Pd2 Cl2 2.3809(13) . ? Pd1 Pd2 3.7316(6) . ? Cl4 C49 1.729(6) . ? Cl5 C49 1.754(6) . ? Cl6 C49 1.758(6) . ? Cl7 C50 1.737(6) . ? Cl8 C50 1.751(7) . ? Cl9 C50 1.740(7) . ? C51 Cl10 1.751(9) . ? C51 Cl12 1.753(10) . ? C51 Cl11 1.754(10) . ? N1 N2 1.314(5) . ? N1 C2 1.366(6) . ? N2 C3 1.356(5) . ? N3 C10 1.319(5) . ? N3 C18 1.458(6) . ? N4 C30 1.315(6) . ? N4 C37 1.464(6) . ? C1 C3 1.396(7) . ? C1 C2 1.417(6) . ? C1 C4 1.484(6) . ? C2 C10 1.463(6) . ? C3 C30 1.471(7) . ? C4 C5 1.377(8) . ? C4 C9 1.398(7) . ? C5 C6 1.410(7) . ? C6 C7 1.401(9) . ? C7 C8 1.365(8) . ? C8 C9 1.377(7) . ? C10 C17 1.477(6) . ? C12 C17 1.375(7) . ? C12 C13 1.400(7) . ? C13 C14 1.393(7) . ? C14 C15 1.370(7) . ? C15 C16 1.388(7) . ? C16 C17 1.404(7) . ? C18 C23 1.400(7) . ? C18 C19 1.401(7) . ? C19 C20 1.390(7) . ? C19 C24 1.530(7) . ? C20 C21 1.383(7) . ? C21 C22 1.377(7) . ? C22 C23 1.399(6) . ? C23 C27 1.512(7) . ? C24 C25 1.523(7) . ? C24 C26 1.532(8) . ? C27 C28 1.519(8) . ? C27 C29 1.534(8) . ? C30 C31 1.493(6) . ? C31 C36 1.385(7) . ? C31 C32 1.386(7) . ? C32 C33 1.387(7) . ? C33 C34 1.383(8) . ? C34 C35 1.373(8) . ? C35 C36 1.395(7) . ? C37 C42 1.388(7) . ? C37 C38 1.402(7) . ? C38 C39 1.391(7) . ? C38 C43 1.518(8) . ? C39 C40 1.387(8) . ? C40 C41 1.360(7) . ? C41 C42 1.400(7) . ? C42 C46 1.508(8) . ? C43 C45 1.500(8) . ? C43 C44 1.514(8) . ? C46 C47A 1.505(7) . ? C46 C48B 1.506(10) . ? C46 C47B 1.510(10) . ? C46 C48A 1.517(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 N1 Pd1 N3 77.57(16) . . ? N1 Pd1 Cl1 175.05(13) . . ? N3 Pd1 Cl1 98.74(11) . . ? N1 Pd1 Cl2 89.39(12) . . ? N3 Pd1 Cl2 166.91(11) . . ? Cl1 Pd1 Cl2 94.35(5) . . ? N2 Pd2 N4 77.49(16) . . ? N2 Pd2 Cl3 176.48(12) . . ? N4 Pd2 Cl3 99.40(11) . . ? N2 Pd2 Cl2 89.01(11) . . ? N4 Pd2 Cl2 166.49(11) . . ? Cl3 Pd2 Cl2 94.10(5) . . ? Pd1 Cl2 Pd2 103.23(5) . . ? Cl10 C51 Cl12 109.3(8) . . ? Cl10 C51 Cl11 103.9(8) . . ? Cl12 C51 Cl11 112.2(11) . . ? N2 N1 C2 109.6(4) . . ? N2 N1 Pd1 128.9(3) . . ? C2 N1 Pd1 121.3(3) . . ? N1 N2 C3 109.1(4) . . ? N1 N2 Pd2 129.3(3) . . ? C3 N2 Pd2 121.5(3) . . ? C10 N3 C18 121.6(4) . . ? C10 N3 Pd1 115.8(3) . . ? C18 N3 Pd1 122.1(3) . . ? C30 N4 C37 120.2(4) . . ? C30 N4 Pd2 115.8(3) . . ? C37 N4 Pd2 123.3(3) . . ? C3 C1 C2 103.8(4) . . ? C3 C1 C4 127.1(4) . . ? C2 C1 C4 129.0(4) . . ? N1 C2 C1 108.1(4) . . ? N1 C2 C10 110.6(4) . . ? C1 C2 C10 141.4(4) . . ? N2 C3 C1 109.5(4) . . ? N2 C3 C30 110.3(4) . . ? C1 C3 C30 140.3(4) . . ? C5 C4 C9 120.1(5) . . ? C5 C4 C1 121.4(5) . . ? C9 C4 C1 118.4(5) . . ? C4 C5 C6 120.6(6) . . ? C7 C6 C5 118.3(6) . . ? C8 C7 C6 120.1(5) . . ? C7 C8 C9 121.9(6) . . ? C8 C9 C4 118.9(5) . . ? N3 C10 C2 114.3(4) . . ? N3 C10 C17 125.5(4) . . ? C2 C10 C17 120.1(4) . . ? C17 C12 C13 121.0(5) . . ? C14 C13 C12 119.0(5) . . ? C15 C14 C13 120.2(5) . . ? C14 C15 C16 121.1(5) . . ? C15 C16 C17 119.3(5) . . ? C12 C17 C16 119.5(4) . . ? C12 C17 C10 122.5(4) . . ? C16 C17 C10 117.9(5) . . ? C23 C18 C19 122.9(4) . . ? C23 C18 N3 118.7(4) . . ? C19 C18 N3 118.1(4) . . ? C20 C19 C18 117.5(5) . . ? C20 C19 C24 119.1(5) . . ? C18 C19 C24 123.4(4) . . ? C21 C20 C19 120.8(5) . . ? C22 C21 C20 120.8(5) . . ? C21 C22 C23 120.9(5) . . ? C22 C23 C18 117.1(5) . . ? C22 C23 C27 119.4(5) . . ? C18 C23 C27 123.5(4) . . ? C25 C24 C19 112.2(4) . . ? C25 C24 C26 108.2(5) . . ? C19 C24 C26 113.4(4) . . ? C23 C27 C28 109.9(4) . . ? C23 C27 C29 111.5(5) . . ? C28 C27 C29 110.9(5) . . ? N4 C30 C3 114.4(4) . . ? N4 C30 C31 126.1(4) . . ? C3 C30 C31 119.3(4) . . ? C36 C31 C32 119.6(5) . . ? C36 C31 C30 123.5(5) . . ? C32 C31 C30 116.9(4) . . ? C31 C32 C33 121.0(5) . . ? C34 C33 C32 119.0(6) . . ? C35 C34 C33 120.3(5) . . ? C34 C35 C36 120.8(5) . . ? C31 C36 C35 119.2(6) . . ? C42 C37 C38 124.4(5) . . ? C42 C37 N4 118.2(5) . . ? C38 C37 N4 117.4(5) . . ? C39 C38 C37 116.3(5) . . ? C39 C38 C43 120.2(5) . . ? C37 C38 C43 123.6(5) . . ? C40 C39 C38 121.0(5) . . ? C41 C40 C39 120.4(5) . . ? C40 C41 C42 121.9(6) . . ? C37 C42 C41 115.9(5) . . ? C37 C42 C46 124.2(5) . . ? C41 C42 C46 119.9(5) . . ? C45 C43 C44 110.7(6) . . ? C45 C43 C38 111.8(5) . . ? C44 C43 C38 111.6(5) . . ? C47A C46 C48B 117(2) . . ? C47A C46 C42 111.6(6) . . ? C48B C46 C42 129(2) . . ? C48B C46 C47B 108.5(15) . . ? C42 C46 C47B 112(4) . . ? C47A C46 C48A 108.6(6) . . ? C42 C46 C48A 112.4(5) . . ? C47B C46 C48A 92(3) . . ? Cl4 C49 Cl5 109.6(3) . . ? Cl4 C49 Cl6 112.0(3) . . ? Cl5 C49 Cl6 108.8(3) . . ? Cl7 C50 Cl9 110.1(3) . . ? Cl7 C50 Cl8 110.6(3) . . ? Cl9 C50 Cl8 110.7(4) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.504 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.086 #===END data_5-as31 _database_code_depnum_ccdc_archive 'CCDC 743830' #TrackingRef 'Dalton_B925535D_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H94 Br6 N8 Ni4 O4, C4 H8 O' _chemical_formula_sum 'C72 H102 Br6 N8 Ni4 O5' _chemical_formula_weight 1873.92 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.278(3) _cell_length_b 39.172(8) _cell_length_c 16.131(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.19(3) _cell_angle_gamma 90.00 _cell_volume 9060(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 83278 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 26.75 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3808 _exptl_absorpt_coefficient_mu 3.509 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3417 _exptl_absorpt_correction_T_max 0.6423 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83278 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.75 _reflns_number_total 19235 _reflns_number_gt 14421 _reflns_threshold_expression >2sigma(I) _puting_data_collection 'X-AREA (Stoe & Cie, 2007)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2007)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _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^)+(0.0630P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19235 _refine_ls_number_parameters 869 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.006 _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 Ni1 Ni 0.53383(4) 0.097129(13) 0.74761(4) 0.02072(11) Uani 1 1 d . . . Ni2 Ni 0.77709(4) 0.108986(13) 0.69746(4) 0.02345(12) Uani 1 1 d . . . Ni3 Ni 0.65531(4) 0.172028(13) 0.53263(4) 0.02173(12) Uani 1 1 d . . . Ni4 Ni 0.41066(4) 0.151005(13) 0.56422(4) 0.02049(11) Uani 1 1 d . . . Br1 Br 0.37170(3) 0.121316(10) 0.68087(3) 0.02419(10) Uani 1 1 d . . . Br2 Br 0.81559(3) 0.158731(11) 0.80502(3) 0.03122(11) Uani 1 1 d . . . Br3 Br 0.68492(3) 0.065051(11) 0.57659(3) 0.03060(11) Uani 1 1 d . . . Br4 Br 0.81009(3) 0.143771(11) 0.58340(3) 0.02816(10) Uani 1 1 d . . . Br5 Br 0.58453(3) 0.142732(11) 0.65445(3) 0.02554(10) Uani 1 1 d . . . Br6 Br 0.39387(3) 0.106399(11) 0.45457(3) 0.02893(10) Uani 1 1 d . . . O4 O 0.6007(2) 0.12998(8) 0.4525(2) 0.0283(7) Uani 1 1 d . . . O1 O 0.5062(2) 0.06459(7) 0.6382(2) 0.0262(6) Uani 1 1 d . . . O3 O 0.7089(2) 0.20751(7) 0.6319(2) 0.0266(6) Uani 1 1 d . . . N1 N 0.6595(3) 0.07560(9) 0.7938(2) 0.0225(7) Uani 1 1 d . . . N2 N 0.7386(2) 0.08015(9) 0.7798(2) 0.0217(7) Uani 1 1 d . . . N3 N 0.5099(3) 0.05752(8) 0.8255(2) 0.0219(7) Uani 1 1 d . . . N4 N 0.8965(3) 0.07919(9) 0.7511(3) 0.0244(8) Uani 1 1 d . . . N5 N 0.5289(3) 0.19296(9) 0.4858(2) 0.0214(7) Uani 1 1 d . . . N6 N 0.4500(2) 0.18726(9) 0.4999(2) 0.0207(7) Uani 1 1 d . . . N7 N 0.6677(2) 0.20371(8) 0.4315(2) 0.0202(7) Uani 1 1 d . . . N8 N 0.2850(2) 0.17692(9) 0.5030(2) 0.0212(7) Uani 1 1 d . . . C1 C 0.7570(3) 0.03373(11) 0.8661(3) 0.0272(9) Uani 1 1 d . . . C2 C 0.6672(3) 0.04767(10) 0.8449(3) 0.0236(9) Uani 1 1 d . . . C3 C 0.7996(3) 0.05555(11) 0.8221(3) 0.0260(9) Uani 1 1 d . . . C4 C 0.7980(4) 0.00296(14) 0.9217(4) 0.0447(14) Uani 1 1 d . . . H4A H 0.8612 -0.0002 0.9240 0.067 Uiso 1 1 calc R . . H4B H 0.7619 -0.0169 0.8961 0.067 Uiso 1 1 calc R . . H4C H 0.7972 0.0063 0.9803 0.067 Uiso 1 1 calc R . . C5 C 0.5823(3) 0.03816(10) 0.8627(3) 0.0220(8) Uani 1 1 d . . . C6 C 0.5824(4) 0.00725(11) 0.9161(3) 0.0319(10) Uani 1 1 d . . . H6A H 0.5221 0.0046 0.9215 0.048 Uiso 1 1 calc R . . H6B H 0.6288 0.0097 0.9738 0.048 Uiso 1 1 calc R . . H6C H 0.5962 -0.0125 0.8875 0.048 Uiso 1 1 calc R . . C7 C 0.4227(3) 0.04896(10) 0.8367(3) 0.0226(8) Uani 1 1 d . . . C8 C 0.3624(3) 0.02552(11) 0.7794(3) 0.0277(9) Uani 1 1 d . . . C9 C 0.2790(4) 0.01771(12) 0.7939(3) 0.0339(11) Uani 1 1 d . . . H9 H 0.2377 0.0022 0.7568 0.041 Uiso 1 1 calc R . . C10 C 0.2567(4) 0.03251(13) 0.8619(4) 0.0363(11) Uani 1 1 d . . . H10 H 0.2016 0.0266 0.8708 0.044 Uiso 1 1 calc R . . C11 C 0.3168(4) 0.05610(12) 0.9167(3) 0.0326(10) Uani 1 1 d . . . H11 H 0.3015 0.0661 0.9622 0.039 Uiso 1 1 calc R . . C12 C 0.4000(3) 0.06508(11) 0.9047(3) 0.0258(9) Uani 1 1 d . . . C13 C 0.3811(4) 0.00914(12) 0.7020(3) 0.0323(10) Uani 1 1 d . . . H13 H 0.4435 0.0161 0.7043 0.039 Uiso 1 1 calc R . . C14 C 0.3108(4) 0.02205(13) 0.6150(3) 0.0397(12) Uani 1 1 d . . . H14A H 0.3231 0.0116 0.5664 0.060 Uiso 1 1 calc R . . H14B H 0.3162 0.0464 0.6117 0.060 Uiso 1 1 calc R . . H14C H 0.2488 0.0163 0.6124 0.060 Uiso 1 1 calc R . . C15 C 0.3795(5) -0.02988(13) 0.7067(4) 0.0477(14) Uani 1 1 d . . . H15A H 0.3920 -0.0393 0.6570 0.072 Uiso 1 1 calc R . . H15B H 0.3193 -0.0373 0.7057 0.072 Uiso 1 1 calc R . . H15C H 0.4264 -0.0375 0.7603 0.072 Uiso 1 1 calc R . . C16 C 0.4638(4) 0.09153(11) 0.9649(3) 0.0301(10) Uani 1 1 d . . . H16 H 0.5081 0.0990 0.9369 0.036 Uiso 1 1 calc R . . C17 C 0.4112(5) 0.12279(14) 0.9771(4) 0.0479(14) Uani 1 1 d . . . H17A H 0.3765 0.1323 0.9204 0.072 Uiso 1 1 calc R . . H17B H 0.4547 0.1394 1.0117 0.072 Uiso 1 1 calc R . . H17C H 0.3691 0.1164 1.0070 0.072 Uiso 1 1 calc R . . C18 C 0.5199(4) 0.07627(14) 1.0545(4) 0.0463(14) Uani 1 1 d . . . H18A H 0.5595 0.0935 1.0909 0.069 Uiso 1 1 calc R . . H18B H 0.5575 0.0578 1.0464 0.069 Uiso 1 1 calc R . . H18C H 0.4781 0.0679 1.0826 0.069 Uiso 1 1 calc R . . C19 C 0.8889(3) 0.05630(12) 0.8064(3) 0.0296(10) Uani 1 1 d . . . C20 C 0.9644(4) 0.03161(14) 0.8534(4) 0.0466(14) Uani 1 1 d . . . H20A H 1.0178 0.0355 0.8362 0.070 Uiso 1 1 calc R . . H20B H 0.9424 0.0087 0.8381 0.070 Uiso 1 1 calc R . . H20C H 0.9816 0.0347 0.9160 0.070 Uiso 1 1 calc R . . C21 C 0.9815(3) 0.08208(11) 0.7315(3) 0.0266(9) Uani 1 1 d . . . C22 C 1.0527(3) 0.10409(12) 0.7819(3) 0.0316(10) Uani 1 1 d . . . C23 C 1.1330(4) 0.10660(14) 0.7593(4) 0.0394(12) Uani 1 1 d . . . H23 H 1.1805 0.1212 0.7917 0.047 Uiso 1 1 calc R . . C24 C 1.1443(4) 0.08824(14) 0.6911(4) 0.0419(13) Uani 1 1 d . . . H24 H 1.1990 0.0901 0.6784 0.050 Uiso 1 1 calc R . . C25 C 1.0730(4) 0.06705(13) 0.6417(4) 0.0384(12) Uani 1 1 d . . . H25 H 1.0797 0.0548 0.5948 0.046 Uiso 1 1 calc R . . C26 C 0.9915(3) 0.06368(12) 0.6611(3) 0.0322(10) Uani 1 1 d . . . C27 C 1.0454(4) 0.12499(14) 0.8588(4) 0.0417(12) Uani 1 1 d . . . H27 H 0.9834 0.1213 0.8625 0.050 Uiso 1 1 calc R . . C28 C 1.0553(5) 0.16316(15) 0.8415(5) 0.0540(16) Uani 1 1 d . . . H28A H 1.0497 0.1763 0.8897 0.081 Uiso 1 1 calc R . . H28B H 1.0072 0.1698 0.7876 0.081 Uiso 1 1 calc R . . H28C H 1.1152 0.1672 0.8364 0.081 Uiso 1 1 calc R . . C29 C 1.1186(5) 0.1137(2) 0.9462(5) 0.0645(19) Uani 1 1 d . . . H29A H 1.1124 0.1271 0.9937 0.097 Uiso 1 1 calc R . . H29B H 1.1798 0.1168 0.9434 0.097 Uiso 1 1 calc R . . H29C H 1.1094 0.0900 0.9564 0.097 Uiso 1 1 calc R . . C30 C 0.9169(4) 0.03977(13) 0.6032(4) 0.0407(12) Uani 1 1 d . . . H30 H 0.8636 0.0406 0.6237 0.049 Uiso 1 1 calc R . . C31 C 0.9514(5) 0.00269(14) 0.6112(5) 0.0578(18) Uani 1 1 d . . . H31A H 0.9027 -0.0117 0.5743 0.087 Uiso 1 1 calc R . . H31B H 0.9685 -0.0046 0.6715 0.087 Uiso 1 1 calc R . . H31C H 1.0048 0.0012 0.5928 0.087 Uiso 1 1 calc R . . C32 C 0.8833(4) 0.05167(16) 0.5066(4) 0.0485(14) Uani 1 1 d . . . H32A H 0.8359 0.0364 0.4713 0.073 Uiso 1 1 calc R . . H32B H 0.9348 0.0517 0.4854 0.073 Uiso 1 1 calc R . . H32C H 0.8582 0.0743 0.5027 0.073 Uiso 1 1 calc R . . C101 C 0.4179(3) 0.22432(10) 0.3865(3) 0.0240(9) Uani 1 1 d . . . C102 C 0.5123(3) 0.21478(10) 0.4166(3) 0.0219(8) Uani 1 1 d . . . C103 C 0.3809(3) 0.20538(10) 0.4407(3) 0.0207(8) Uani 1 1 d . . . C104 C 0.3660(4) 0.24850(14) 0.3140(3) 0.0372(12) Uani 1 1 d . . . H10A H 0.4082 0.2579 0.2876 0.056 Uiso 1 1 calc R . . H10B H 0.3399 0.2666 0.3381 0.056 Uiso 1 1 calc R . . H10C H 0.3169 0.2365 0.2701 0.056 Uiso 1 1 calc R . . C105 C 0.5933(3) 0.22051(10) 0.3891(3) 0.0217(8) Uani 1 1 d . . . C106 C 0.5844(4) 0.24361(13) 0.3129(3) 0.0337(11) Uani 1 1 d . . . H10D H 0.6429 0.2446 0.3031 0.051 Uiso 1 1 calc R . . H10E H 0.5676 0.2661 0.3256 0.051 Uiso 1 1 calc R . . H10F H 0.5371 0.2350 0.2608 0.051 Uiso 1 1 calc R . . C107 C 0.7496(3) 0.20507(10) 0.4060(3) 0.0222(8) Uani 1 1 d . . . C108 C 0.7568(4) 0.18204(11) 0.3421(3) 0.0294(10) Uani 1 1 d . . . C109 C 0.8371(4) 0.18308(13) 0.3202(3) 0.0358(11) Uani 1 1 d . . . H109 H 0.8430 0.1682 0.2775 0.043 Uiso 1 1 calc R . . C110 C 0.9090(4) 0.20593(13) 0.3608(4) 0.0386(12) Uani 1 1 d . . . H110 H 0.9625 0.2061 0.3458 0.046 Uiso 1 1 calc R . . C111 C 0.9003(3) 0.22839(13) 0.4236(3) 0.0321(10) Uani 1 1 d . . . H111 H 0.9482 0.2437 0.4503 0.039 Uiso 1 1 calc R . . C112 C 0.8210(3) 0.22852(11) 0.4474(3) 0.0251(9) Uani 1 1 d . . . C113 C 0.6813(4) 0.15639(12) 0.2965(3) 0.0356(11) Uani 1 1 d . . . H113 H 0.6317 0.1589 0.3217 0.043 Uiso 1 1 calc R . . C114 C 0.6385(5) 0.16389(16) 0.1971(4) 0.0514(16) Uani 1 1 d . . . H11A H 0.5907 0.1474 0.1698 0.077 Uiso 1 1 calc R . . H11B H 0.6861 0.1626 0.1710 0.077 Uiso 1 1 calc R . . H11C H 0.6118 0.1864 0.1885 0.077 Uiso 1 1 calc R . . C115 C 0.7176(6) 0.11989(14) 0.3142(5) 0.0576(18) Uani 1 1 d . . . H11D H 0.6683 0.1043 0.2847 0.086 Uiso 1 1 calc R . . H11E H 0.7393 0.1155 0.3766 0.086 Uiso 1 1 calc R . . H11F H 0.7682 0.1169 0.2923 0.086 Uiso 1 1 calc R . . C116 C 0.8132(3) 0.25367(12) 0.5157(3) 0.0283(9) Uani 1 1 d . . . H116 H 0.7590 0.2472 0.5314 0.034 Uiso 1 1 calc R . . C117 C 0.8975(5) 0.25265(18) 0.5985(4) 0.0546(16) Uani 1 1 d . . . H11G H 0.8901 0.2689 0.6402 0.082 Uiso 1 1 calc R . . H11H H 0.9520 0.2583 0.5846 0.082 Uiso 1 1 calc R . . H11I H 0.9042 0.2302 0.6235 0.082 Uiso 1 1 calc R . . C118 C 0.7968(5) 0.28998(14) 0.4786(4) 0.0524(16) Uani 1 1 d . . . H11J H 0.7427 0.2903 0.4259 0.079 Uiso 1 1 calc R . . H11K H 0.8502 0.2974 0.4651 0.079 Uiso 1 1 calc R . . H11L H 0.7872 0.3050 0.5217 0.079 Uiso 1 1 calc R . . C119 C 0.2886(3) 0.20025(10) 0.4473(3) 0.0216(8) Uani 1 1 d . . . C120 C 0.2080(3) 0.22164(13) 0.3927(4) 0.0359(11) Uani 1 1 d . . . H12A H 0.1530 0.2152 0.4047 0.054 Uiso 1 1 calc R . . H12B H 0.1980 0.2182 0.3312 0.054 Uiso 1 1 calc R . . H12C H 0.2214 0.2453 0.4072 0.054 Uiso 1 1 calc R . . C121 C 0.2003(3) 0.17154(11) 0.5222(3) 0.0279(9) Uani 1 1 d . . . C122 C 0.1884(3) 0.18917(13) 0.5925(3) 0.0319(10) Uani 1 1 d . . . C123 C 0.1074(4) 0.18340(16) 0.6121(4) 0.0470(14) Uani 1 1 d . . . H123 H 0.0983 0.1951 0.6586 0.056 Uiso 1 1 calc R . . C124 C 0.0418(4) 0.16085(17) 0.5640(5) 0.0543(17) Uani 1 1 d . . . H124 H -0.0121 0.1576 0.5775 0.065 Uiso 1 1 calc R . . C125 C 0.0542(4) 0.14300(16) 0.4963(5) 0.0495(15) Uani 1 1 d . . . H125 H 0.0091 0.1274 0.4650 0.059 Uiso 1 1 calc R . . C126 C 0.1339(3) 0.14776(12) 0.4725(4) 0.0346(11) Uani 1 1 d . . . C127 C 0.2593(4) 0.21484(15) 0.6475(4) 0.0426(13) Uani 1 1 d . . . H127 H 0.3151 0.2130 0.6309 0.051 Uiso 1 1 calc R . . C128 C 0.2223(5) 0.25122(16) 0.6279(4) 0.0561(17) Uani 1 1 d . . . H12D H 0.2686 0.2670 0.6629 0.084 Uiso 1 1 calc R . . H12E H 0.1666 0.2535 0.6423 0.084 Uiso 1 1 calc R . . H12F H 0.2085 0.2561 0.5664 0.084 Uiso 1 1 calc R . . C129 C 0.2881(5) 0.20755(17) 0.7460(4) 0.0574(17) Uani 1 1 d . . . H12G H 0.3333 0.2241 0.7783 0.086 Uiso 1 1 calc R . . H12H H 0.3147 0.1851 0.7581 0.086 Uiso 1 1 calc R . . H12I H 0.2343 0.2088 0.7638 0.086 Uiso 1 1 calc R . . C130 C 0.1455(4) 0.12745(13) 0.3974(4) 0.0445(13) Uani 1 1 d . . . H130 H 0.2070 0.1330 0.3946 0.053 Uiso 1 1 calc R . . C131 C 0.1441(5) 0.08916(15) 0.4150(6) 0.072(2) Uani 1 1 d . . . H13A H 0.1519 0.0767 0.3668 0.108 Uiso 1 1 calc R . . H13B H 0.0855 0.0831 0.4207 0.108 Uiso 1 1 calc R . . H13C H 0.1939 0.0836 0.4687 0.108 Uiso 1 1 calc R . . C132 C 0.0721(5) 0.13729(19) 0.3080(5) 0.0650(19) Uani 1 1 d . . . H13D H 0.0749 0.1614 0.2990 0.098 Uiso 1 1 calc R . . H13E H 0.0112 0.1313 0.3079 0.098 Uiso 1 1 calc R . . H13F H 0.0846 0.1253 0.2614 0.098 Uiso 1 1 calc R . . O2 O 0.5701(2) 0.13453(8) 0.8501(2) 0.0311(7) Uani 1 1 d . C . C999 C 0.6583(4) 0.13442(14) 0.9230(4) 0.0424(12) Uani 1 1 d . C . H99D H 0.7087 0.1282 0.9022 0.051 Uiso 1 1 calc R . . H99E H 0.6567 0.1181 0.9676 0.051 Uiso 1 1 calc R . . C201 C 0.6726(5) 0.16989(18) 0.9604(5) 0.0633(19) Uani 1 1 d . . . H99F H 0.6547 0.1713 1.0125 0.076 Uiso 1 1 calc R A 1 H99G H 0.7372 0.1769 0.9759 0.076 Uiso 1 1 calc R A 1 C203 C 0.5315(5) 0.16893(12) 0.8416(4) 0.0450(13) Uani 1 1 d . . . H99H H 0.4840 0.1703 0.8688 0.054 Uiso 1 1 calc R B 1 H99I H 0.5038 0.1752 0.7799 0.054 Uiso 1 1 calc R B 1 C20A C 0.6102(8) 0.1915(2) 0.8872(9) 0.056(4) Uani 0.66(2) 1 d P C 1 H2AF H 0.5893 0.2115 0.9103 0.067 Uiso 0.66(2) 1 calc PR C 1 H2AG H 0.6422 0.1987 0.8476 0.067 Uiso 0.66(2) 1 calc PR C 1 C20B C 0.5856(14) 0.1862(4) 0.9338(14) 0.045(6) Uani 0.34(2) 1 d P C 2 H2BH H 0.5921 0.2106 0.9275 0.054 Uiso 0.34(2) 1 calc PR C 2 H2BI H 0.5540 0.1821 0.9757 0.054 Uiso 0.34(2) 1 calc PR C 2 O5 O 0.5998(3) 0.25877(11) 0.6585(3) 0.0554(11) Uani 1 1 d . . . C303 C 0.5096(5) 0.25495(17) 0.6653(5) 0.0567(16) Uani 1 1 d . . . H30A H 0.5132 0.2582 0.7260 0.068 Uiso 1 1 calc R . . H30B H 0.4855 0.2323 0.6466 0.068 Uiso 1 1 calc R . . C300 C 0.5931(6) 0.28414(17) 0.5913(6) 0.074(2) Uani 1 1 d . . . H30C H 0.6467 0.2992 0.6107 0.089 Uiso 1 1 calc R . . H30D H 0.5917 0.2731 0.5370 0.089 Uiso 1 1 calc R . . C302 C 0.4474(5) 0.2812(2) 0.6073(6) 0.075(2) Uani 1 1 d . . . H30E H 0.4002 0.2705 0.5575 0.090 Uiso 1 1 calc R . . H30F H 0.4167 0.2945 0.6400 0.090 Uiso 1 1 calc R . . C301 C 0.5089(7) 0.3033(3) 0.5764(7) 0.093(3) Uani 1 1 d . . . H30G H 0.4796 0.3086 0.5141 0.112 Uiso 1 1 calc R . . H30H H 0.5222 0.3246 0.6094 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0183(3) 0.0223(2) 0.0232(3) 0.0036(2) 0.0091(2) 0.0002(2) Ni2 0.0198(3) 0.0249(3) 0.0283(3) 0.0051(2) 0.0118(2) 0.0009(2) Ni3 0.0187(3) 0.0257(3) 0.0225(3) 0.0040(2) 0.0094(2) 0.0002(2) Ni4 0.0180(3) 0.0232(2) 0.0224(3) 0.0036(2) 0.0098(2) 0.0008(2) Br1 0.0194(2) 0.0287(2) 0.0278(2) 0.00619(16) 0.01239(18) 0.00118(16) Br2 0.0280(2) 0.0295(2) 0.0332(2) 0.00168(18) 0.0069(2) -0.00048(18) Br3 0.0297(2) 0.0311(2) 0.0353(2) 0.00011(18) 0.0167(2) 0.00088(18) Br4 0.0210(2) 0.0327(2) 0.0355(2) 0.00873(18) 0.01582(19) 0.00232(17) Br5 0.0211(2) 0.0298(2) 0.0266(2) 0.00647(16) 0.00937(18) -0.00069(17) Br6 0.0270(2) 0.0319(2) 0.0279(2) -0.00240(17) 0.00956(19) 0.00023(18) O4 0.0283(17) 0.0317(16) 0.0272(16) 0.0031(13) 0.0125(14) -0.0016(13) O1 0.0257(17) 0.0251(14) 0.0308(17) 0.0002(12) 0.0137(14) -0.0025(12) O3 0.0263(17) 0.0279(15) 0.0247(16) -0.0001(12) 0.0076(14) -0.0026(13) N1 0.0204(18) 0.0253(17) 0.0243(18) 0.0056(14) 0.0111(15) -0.0005(14) N2 0.0139(17) 0.0274(17) 0.0241(18) 0.0009(14) 0.0067(15) -0.0004(14) N3 0.0207(19) 0.0237(16) 0.0228(18) 0.0034(13) 0.0096(15) -0.0039(14) N4 0.0171(18) 0.0249(17) 0.032(2) 0.0011(15) 0.0101(16) -0.0012(14) N5 0.0193(18) 0.0255(17) 0.0221(17) 0.0054(14) 0.0107(15) -0.0026(14) N6 0.0147(17) 0.0251(17) 0.0223(18) 0.0028(13) 0.0064(15) 0.0017(13) N7 0.0197(18) 0.0242(16) 0.0196(17) 0.0001(13) 0.0106(15) -0.0043(14) N8 0.0158(17) 0.0252(17) 0.0224(17) -0.0009(14) 0.0063(15) -0.0011(14) C1 0.025(2) 0.027(2) 0.032(2) 0.0091(18) 0.013(2) 0.0048(18) C2 0.023(2) 0.0230(19) 0.026(2) 0.0077(16) 0.0101(18) 0.0038(17) C3 0.022(2) 0.027(2) 0.030(2) 0.0062(17) 0.0109(19) 0.0031(17) C4 0.035(3) 0.043(3) 0.063(4) 0.029(3) 0.026(3) 0.014(2) C5 0.026(2) 0.0187(18) 0.024(2) 0.0004(15) 0.0113(18) -0.0006(16) C6 0.028(2) 0.029(2) 0.042(3) 0.013(2) 0.016(2) 0.0038(19) C7 0.020(2) 0.026(2) 0.024(2) 0.0071(16) 0.0095(18) 0.0010(16) C8 0.029(2) 0.025(2) 0.030(2) 0.0077(17) 0.011(2) -0.0039(18) C9 0.028(3) 0.037(2) 0.036(3) 0.006(2) 0.008(2) -0.009(2) C10 0.024(2) 0.045(3) 0.041(3) 0.013(2) 0.013(2) -0.001(2) C11 0.030(3) 0.038(2) 0.035(3) 0.011(2) 0.018(2) 0.007(2) C12 0.023(2) 0.029(2) 0.029(2) 0.0078(17) 0.0137(19) 0.0017(18) C13 0.033(3) 0.032(2) 0.035(3) -0.0024(19) 0.014(2) -0.010(2) C14 0.046(3) 0.039(3) 0.035(3) -0.002(2) 0.014(3) -0.006(2) C15 0.059(4) 0.031(3) 0.053(4) -0.003(2) 0.019(3) -0.006(3) C16 0.039(3) 0.028(2) 0.028(2) -0.0018(18) 0.018(2) -0.002(2) C17 0.052(4) 0.035(3) 0.055(4) -0.003(2) 0.015(3) 0.004(3) C18 0.048(4) 0.035(3) 0.045(3) -0.003(2) 0.003(3) -0.001(2) C19 0.024(2) 0.034(2) 0.032(2) 0.0043(19) 0.011(2) 0.0037(19) C20 0.033(3) 0.048(3) 0.067(4) 0.027(3) 0.028(3) 0.016(2) C21 0.016(2) 0.030(2) 0.037(3) 0.0074(18) 0.0135(19) 0.0052(17) C22 0.019(2) 0.036(2) 0.040(3) 0.002(2) 0.011(2) -0.0051(19) C23 0.022(2) 0.041(3) 0.052(3) 0.006(2) 0.008(2) -0.003(2) C24 0.023(2) 0.054(3) 0.054(3) 0.013(3) 0.021(2) 0.004(2) C25 0.030(3) 0.046(3) 0.047(3) 0.006(2) 0.023(2) 0.005(2) C26 0.026(2) 0.035(2) 0.042(3) 0.008(2) 0.019(2) 0.006(2) C27 0.029(3) 0.044(3) 0.052(3) -0.008(2) 0.013(3) -0.004(2) C28 0.044(4) 0.046(3) 0.077(5) -0.017(3) 0.028(3) -0.016(3) C29 0.035(3) 0.098(5) 0.052(4) -0.013(4) 0.003(3) 0.011(3) C30 0.039(3) 0.038(3) 0.055(3) -0.011(2) 0.029(3) -0.001(2) C31 0.062(4) 0.038(3) 0.086(5) -0.007(3) 0.043(4) -0.002(3) C32 0.042(3) 0.055(3) 0.050(3) -0.016(3) 0.018(3) -0.004(3) C101 0.022(2) 0.024(2) 0.027(2) 0.0036(16) 0.0101(19) 0.0000(17) C102 0.024(2) 0.0232(19) 0.019(2) 0.0012(15) 0.0076(18) -0.0016(16) C103 0.017(2) 0.0237(19) 0.020(2) 0.0034(15) 0.0051(17) 0.0034(16) C104 0.031(3) 0.047(3) 0.038(3) 0.022(2) 0.018(2) 0.009(2) C105 0.026(2) 0.0218(19) 0.019(2) -0.0006(15) 0.0095(18) -0.0047(17) C106 0.026(2) 0.043(3) 0.034(3) 0.015(2) 0.014(2) 0.002(2) C107 0.022(2) 0.027(2) 0.022(2) 0.0064(16) 0.0135(18) 0.0003(17) C108 0.041(3) 0.027(2) 0.026(2) 0.0069(17) 0.020(2) 0.0017(19) C109 0.041(3) 0.040(3) 0.038(3) 0.004(2) 0.029(2) 0.008(2) C110 0.032(3) 0.047(3) 0.047(3) 0.008(2) 0.026(3) 0.009(2) C111 0.021(2) 0.041(3) 0.036(3) 0.011(2) 0.012(2) -0.0011(19) C112 0.021(2) 0.031(2) 0.024(2) 0.0080(17) 0.0091(18) 0.0004(17) C113 0.050(3) 0.033(2) 0.033(3) -0.006(2) 0.026(3) -0.007(2) C114 0.070(4) 0.053(3) 0.035(3) -0.012(2) 0.022(3) -0.022(3) C115 0.085(5) 0.031(3) 0.071(4) -0.004(3) 0.045(4) -0.002(3) C116 0.022(2) 0.034(2) 0.028(2) -0.0004(18) 0.0085(19) -0.0064(18) C117 0.048(4) 0.076(4) 0.029(3) -0.010(3) -0.002(3) 0.009(3) C118 0.080(5) 0.037(3) 0.041(3) -0.002(2) 0.022(3) 0.001(3) C119 0.020(2) 0.0219(19) 0.026(2) 0.0010(16) 0.0116(18) 0.0034(16) C120 0.023(2) 0.042(3) 0.043(3) 0.018(2) 0.010(2) 0.007(2) C121 0.020(2) 0.030(2) 0.036(2) 0.0103(19) 0.014(2) 0.0031(18) C122 0.028(3) 0.043(3) 0.030(2) 0.010(2) 0.017(2) 0.010(2) C123 0.036(3) 0.067(4) 0.051(3) 0.022(3) 0.030(3) 0.015(3) C124 0.029(3) 0.076(4) 0.069(4) 0.030(3) 0.031(3) 0.009(3) C125 0.019(3) 0.054(3) 0.070(4) 0.021(3) 0.008(3) -0.005(2) C126 0.019(2) 0.034(2) 0.045(3) 0.011(2) 0.005(2) 0.0008(19) C127 0.039(3) 0.060(3) 0.036(3) -0.009(2) 0.022(3) 0.006(3) C128 0.077(5) 0.051(3) 0.048(4) 0.001(3) 0.031(4) 0.002(3) C129 0.066(4) 0.061(4) 0.047(4) -0.010(3) 0.021(3) 0.022(3) C130 0.031(3) 0.037(3) 0.058(4) -0.009(2) 0.006(3) -0.005(2) C131 0.053(4) 0.037(3) 0.123(7) -0.013(4) 0.024(5) -0.011(3) C132 0.051(4) 0.072(4) 0.055(4) -0.020(3) -0.005(3) 0.000(3) O2 0.0349(19) 0.0283(16) 0.0280(17) 0.0013(13) 0.0082(15) -0.0021(14) C999 0.038(3) 0.051(3) 0.036(3) -0.001(2) 0.010(2) -0.007(2) C201 0.059(4) 0.073(4) 0.050(4) -0.031(3) 0.008(3) -0.006(4) C203 0.059(4) 0.030(2) 0.046(3) -0.006(2) 0.018(3) 0.001(2) C20A 0.065(7) 0.041(5) 0.064(8) -0.014(5) 0.026(6) -0.010(5) C20B 0.052(12) 0.042(9) 0.039(11) -0.014(7) 0.014(9) -0.013(8) O5 0.046(3) 0.053(2) 0.071(3) -0.008(2) 0.025(2) 0.007(2) C303 0.054(4) 0.063(4) 0.060(4) -0.013(3) 0.030(3) -0.005(3) C300 0.077(6) 0.044(3) 0.117(7) -0.002(4) 0.054(5) -0.005(3) C302 0.041(4) 0.089(5) 0.091(6) -0.011(5) 0.019(4) 0.010(4) C301 0.089(7) 0.104(7) 0.098(7) 0.028(6) 0.047(6) 0.033(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 Ni1 N1 1.991(4) . ? Ni1 O1 2.098(3) . ? Ni1 N3 2.107(3) . ? Ni1 O2 2.135(3) . ? Ni1 Br1 2.5202(10) . ? Ni1 Br5 2.6178(7) . ? Ni2 N2 1.981(3) . ? Ni2 N4 2.086(4) . ? Ni2 Br4 2.4771(8) . ? Ni2 Br2 2.5395(8) . ? Ni2 Br3 2.6175(10) . ? Ni3 N5 1.991(4) . ? Ni3 O3 2.064(3) . ? Ni3 O4 2.082(3) . ? Ni3 N7 2.110(3) . ? Ni3 Br4 2.4802(9) . ? Ni3 Br5 2.7953(8) . ? Ni4 N6 1.971(3) . ? Ni4 N8 2.093(4) . ? Ni4 Br6 2.4360(8) . ? Ni4 Br1 2.4537(7) . ? Ni4 Br5 2.5713(11) . ? N1 N2 1.316(5) . ? N1 C2 1.350(5) . ? N2 C3 1.350(6) . ? N3 C5 1.304(6) . ? N3 C7 1.445(5) . ? N4 C19 1.299(6) . ? N4 C21 1.443(5) . ? N5 N6 1.322(5) . ? N5 C102 1.358(5) . ? N6 C103 1.355(5) . ? N7 C105 1.286(6) . ? N7 C107 1.446(5) . ? N8 C119 1.296(5) . ? N8 C121 1.447(5) . ? C1 C2 1.405(6) . ? C1 C3 1.406(6) . ? C1 C4 1.504(6) . ? C2 C5 1.471(6) . ? C3 C19 1.472(6) . ? C5 C6 1.485(6) . ? C7 C8 1.400(6) . ? C7 C12 1.408(6) . ? C8 C9 1.406(6) . ? C8 C13 1.516(7) . ? C9 C10 1.383(7) . ? C10 C11 1.385(8) . ? C11 C12 1.396(6) . ? C12 C16 1.520(7) . ? C13 C15 1.531(7) . ? C13 C14 1.529(7) . ? C16 C17 1.515(7) . ? C16 C18 1.526(7) . ? C19 C20 1.495(7) . ? C21 C26 1.397(7) . ? C21 C22 1.406(7) . ? C22 C23 1.399(7) . ? C22 C27 1.522(7) . ? C23 C24 1.374(8) . ? C24 C25 1.382(8) . ? C25 C26 1.391(6) . ? C26 C30 1.521(8) . ? C27 C29 1.533(9) . ? C27 C28 1.538(8) . ? C30 C32 1.535(9) . ? C30 C31 1.535(8) . ? C101 C102 1.404(6) . ? C101 C103 1.405(6) . ? C101 C104 1.501(6) . ? C102 C105 1.469(6) . ? C103 C119 1.464(6) . ? C105 C106 1.495(6) . ? C107 C108 1.402(6) . ? C107 C112 1.406(6) . ? C108 C109 1.391(7) . ? C108 C113 1.515(7) . ? C109 C110 1.392(8) . ? C110 C111 1.382(7) . ? C111 C112 1.392(6) . ? C112 C116 1.512(6) . ? C113 C115 1.524(7) . ? C113 C114 1.537(8) . ? C116 C117 1.502(7) . ? C116 C118 1.530(7) . ? C119 C120 1.498(6) . ? C121 C122 1.392(7) . ? C121 C126 1.406(7) . ? C122 C123 1.396(7) . ? C122 C127 1.520(8) . ? C123 C124 1.361(9) . ? C124 C125 1.365(10) . ? C125 C126 1.409(7) . ? C126 C130 1.510(8) . ? C127 C128 1.525(8) . ? C127 C129 1.523(8) . ? C130 C131 1.528(8) . ? C130 C132 1.539(9) . ? O2 C999 1.450(7) . ? O2 C203 1.459(6) . ? C999 C201 1.501(8) . ? C201 C20B 1.40(2) . ? C201 C20A 1.498(14) . ? C203 C20A 1.469(11) . ? C203 C20B 1.582(18) . ? O5 C303 1.427(8) . ? O5 C300 1.447(9) . ? C303 C302 1.492(10) . ? C300 C301 1.436(11) . ? C302 C301 1.486(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O1 86.90(14) . . ? N1 Ni1 N3 78.95(14) . . ? O1 Ni1 N3 91.63(13) . . ? N1 Ni1 O2 92.38(15) . . ? O1 Ni1 O2 172.59(12) . . ? N3 Ni1 O2 95.47(13) . . ? N1 Ni1 Br1 176.06(11) . . ? O1 Ni1 Br1 89.20(9) . . ? N3 Ni1 Br1 100.62(10) . . ? O2 Ni1 Br1 91.55(10) . . ? N1 Ni1 Br5 93.77(10) . . ? O1 Ni1 Br5 86.86(8) . . ? N3 Ni1 Br5 172.64(10) . . ? O2 Ni1 Br5 85.83(9) . . ? Br1 Ni1 Br5 86.57(3) . . ? N2 Ni2 N4 79.78(14) . . ? N2 Ni2 Br4 174.36(11) . . ? N4 Ni2 Br4 104.04(10) . . ? N2 Ni2 Br2 91.83(11) . . ? N4 Ni2 Br2 100.53(11) . . ? Br4 Ni2 Br2 91.54(3) . . ? N2 Ni2 Br3 85.21(11) . . ? N4 Ni2 Br3 96.31(11) . . ? Br4 Ni2 Br3 90.20(3) . . ? Br2 Ni2 Br3 162.11(3) . . ? N5 Ni3 O3 95.17(14) . . ? N5 Ni3 O4 87.79(14) . . ? O3 Ni3 O4 168.74(12) . . ? N5 Ni3 N7 78.34(14) . . ? O3 Ni3 N7 94.98(13) . . ? O4 Ni3 N7 96.26(13) . . ? N5 Ni3 Br4 176.68(11) . . ? O3 Ni3 Br4 88.10(10) . . ? O4 Ni3 Br4 89.11(10) . . ? N7 Ni3 Br4 100.86(10) . . ? N5 Ni3 Br5 82.89(10) . . ? O3 Ni3 Br5 82.93(9) . . ? O4 Ni3 Br5 86.67(9) . . ? N7 Ni3 Br5 160.86(10) . . ? Br4 Ni3 Br5 98.09(3) . . ? N6 Ni4 N8 78.39(14) . . ? N6 Ni4 Br6 96.27(10) . . ? N8 Ni4 Br6 98.97(10) . . ? N6 Ni4 Br1 160.74(11) . . ? N8 Ni4 Br1 99.55(10) . . ? Br6 Ni4 Br1 102.96(3) . . ? N6 Ni4 Br5 86.90(11) . . ? N8 Ni4 Br5 158.15(10) . . ? Br6 Ni4 Br5 98.62(3) . . ? Br1 Ni4 Br5 89.02(3) . . ? Ni4 Br1 Ni1 92.46(3) . . ? Ni2 Br4 Ni3 94.33(3) . . ? Ni4 Br5 Ni1 87.61(3) . . ? Ni4 Br5 Ni3 97.19(3) . . ? Ni1 Br5 Ni3 161.18(2) . . ? N2 N1 C2 108.8(3) . . ? N2 N1 Ni1 134.6(3) . . ? C2 N1 Ni1 116.2(3) . . ? N1 N2 C3 109.3(3) . . ? N1 N2 Ni2 134.0(3) . . ? C3 N2 Ni2 115.7(3) . . ? C5 N3 C7 118.7(3) . . ? C5 N3 Ni1 114.1(3) . . ? C7 N3 Ni1 127.1(3) . . ? C19 N4 C21 120.4(4) . . ? C19 N4 Ni2 113.5(3) . . ? C21 N4 Ni2 126.1(3) . . ? N6 N5 C102 108.9(3) . . ? N6 N5 Ni3 133.5(3) . . ? C102 N5 Ni3 117.0(3) . . ? N5 N6 C103 109.0(3) . . ? N5 N6 Ni4 132.4(3) . . ? C103 N6 Ni4 116.4(3) . . ? C105 N7 C107 121.5(3) . . ? C105 N7 Ni3 114.4(3) . . ? C107 N7 Ni3 123.9(3) . . ? C119 N8 C121 120.4(4) . . ? C119 N8 Ni4 114.7(3) . . ? C121 N8 Ni4 124.8(3) . . ? C2 C1 C3 102.9(4) . . ? C2 C1 C4 128.9(4) . . ? C3 C1 C4 128.2(4) . . ? N1 C2 C1 109.6(4) . . ? N1 C2 C5 115.3(4) . . ? C1 C2 C5 135.0(4) . . ? N2 C3 C1 109.3(4) . . ? N2 C3 C19 114.7(4) . . ? C1 C3 C19 135.8(4) . . ? N3 C5 C2 115.3(4) . . ? N3 C5 C6 124.9(4) . . ? C2 C5 C6 119.7(4) . . ? C8 C7 C12 121.8(4) . . ? C8 C7 N3 119.7(4) . . ? C12 C7 N3 118.6(4) . . ? C7 C8 C9 117.4(4) . . ? C7 C8 C13 123.6(4) . . ? C9 C8 C13 119.0(4) . . ? C10 C9 C8 121.7(5) . . ? C9 C10 C11 119.7(5) . . ? C10 C11 C12 121.0(5) . . ? C11 C12 C7 118.4(4) . . ? C11 C12 C16 119.8(4) . . ? C7 C12 C16 121.8(4) . . ? C8 C13 C15 111.8(4) . . ? C8 C13 C14 110.0(4) . . ? C15 C13 C14 110.9(4) . . ? C17 C16 C12 112.5(4) . . ? C17 C16 C18 110.1(4) . . ? C12 C16 C18 111.4(4) . . ? N4 C19 C3 116.1(4) . . ? N4 C19 C20 123.9(4) . . ? C3 C19 C20 120.0(4) . . ? C26 C21 C22 120.5(4) . . ? C26 C21 N4 119.8(4) . . ? C22 C21 N4 119.7(4) . . ? C23 C22 C21 117.7(5) . . ? C23 C22 C27 119.4(5) . . ? C21 C22 C27 122.8(4) . . ? C24 C23 C22 122.3(5) . . ? C23 C24 C25 119.0(5) . . ? C24 C25 C26 121.1(5) . . ? C25 C26 C21 119.4(5) . . ? C25 C26 C30 117.4(5) . . ? C21 C26 C30 123.2(4) . . ? C22 C27 C29 111.0(5) . . ? C22 C27 C28 109.6(5) . . ? C29 C27 C28 111.2(5) . . ? C26 C30 C32 110.7(4) . . ? C26 C30 C31 111.6(5) . . ? C32 C30 C31 111.0(5) . . ? C102 C101 C103 103.4(4) . . ? C102 C101 C104 129.8(4) . . ? C103 C101 C104 126.9(4) . . ? N5 C102 C101 109.3(4) . . ? N5 C102 C105 113.9(4) . . ? C101 C102 C105 136.7(4) . . ? N6 C103 C101 109.4(4) . . ? N6 C103 C119 114.4(3) . . ? C101 C103 C119 136.3(4) . . ? N7 C105 C102 116.3(4) . . ? N7 C105 C106 124.0(4) . . ? C102 C105 C106 119.6(4) . . ? C108 C107 C112 121.6(4) . . ? C108 C107 N7 118.7(4) . . ? C112 C107 N7 119.7(4) . . ? C109 C108 C107 118.0(5) . . ? C109 C108 C113 119.1(4) . . ? C107 C108 C113 122.9(4) . . ? C108 C109 C110 121.3(5) . . ? C111 C110 C109 119.7(4) . . ? C110 C111 C112 121.2(5) . . ? C111 C112 C107 118.2(4) . . ? C111 C112 C116 119.9(4) . . ? C107 C112 C116 121.9(4) . . ? C108 C113 C115 111.4(5) . . ? C108 C113 C114 111.0(4) . . ? C115 C113 C114 111.8(5) . . ? C117 C116 C112 111.8(4) . . ? C117 C116 C118 110.3(5) . . ? C112 C116 C118 111.4(4) . . ? N8 C119 C103 114.8(4) . . ? N8 C119 C120 125.4(4) . . ? C103 C119 C120 119.8(4) . . ? C122 C121 C126 121.4(4) . . ? C122 C121 N8 118.7(4) . . ? C126 C121 N8 119.8(4) . . ? C121 C122 C123 118.6(5) . . ? C121 C122 C127 122.4(4) . . ? C123 C122 C127 119.0(5) . . ? C124 C123 C122 120.8(6) . . ? C123 C124 C125 120.6(5) . . ? C124 C125 C126 121.5(6) . . ? C121 C126 C125 117.0(5) . . ? C121 C126 C130 123.1(5) . . ? C125 C126 C130 120.0(5) . . ? C122 C127 C128 111.0(5) . . ? C122 C127 C129 112.1(5) . . ? C128 C127 C129 110.1(5) . . ? C126 C130 C131 110.8(6) . . ? C126 C130 C132 111.8(5) . . ? C131 C130 C132 111.6(5) . . ? C999 O2 C203 108.2(4) . . ? C999 O2 Ni1 123.1(3) . . ? C203 O2 Ni1 124.9(3) . . ? O2 C999 C201 106.8(5) . . ? C20B C201 C999 107.9(8) . . ? C20A C201 C999 104.0(6) . . ? O2 C203 C20A 105.9(6) . . ? O2 C203 C20B 104.0(8) . . ? C203 C20A C201 104.0(7) . . ? C201 C20B C203 103.2(12) . . ? C303 O5 C300 108.0(5) . . ? O5 C303 C302 107.6(6) . . ? C301 C300 O5 108.3(7) . . ? C301 C302 C303 105.8(6) . . ? C300 C301 C302 105.7(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.525 _refine_diff_density_min -1.373 _refine_diff_density_rms 0.119 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.500 772 182 2 0.000 0.500 1.000 772 181 _platon_squeeze_details ; ? ; #===END data_7-as58 _database_code_depnum_ccdc_archive 'CCDC 743831' #TrackingRef 'Dalton_B925535D_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H86 N8 Ni' _chemical_formula_sum 'C64 H86 N8 Ni' _chemical_formula_weight 1026.12 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8126(13) _cell_length_b 11.8060(16) _cell_length_c 14.793(2) _cell_angle_alpha 73.936(11) _cell_angle_beta 89.425(11) _cell_angle_gamma 86.727(11) _cell_volume 1476.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 13134 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 27.12 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 554 _exptl_absorpt_coefficient_mu 0.374 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7824 _exptl_absorpt_correction_T_max 0.9397 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2007)' _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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13134 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.12 _reflns_number_total 6369 _reflns_number_gt 4061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _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^)+(0.0598P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6369 _refine_ls_number_parameters 327 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.002 _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 Ni1 Ni 1.0000 0.5000 1.0000 0.02364(17) Uani 1 2 d S . . N1 N 0.8793(3) 0.5276(2) 0.89046(17) 0.0296(6) Uani 1 1 d . . . N2 N 0.7891(3) 0.6174(2) 0.84016(17) 0.0316(6) Uani 1 1 d . . . N3 N 0.6225(3) 0.6461(2) 0.61365(17) 0.0336(6) Uani 1 1 d . . . N4 N 1.0474(3) 0.3486(2) 0.97336(16) 0.0279(6) Uani 1 1 d . . . C1 C 0.8069(4) 0.4736(3) 0.7630(2) 0.0305(7) Uani 1 1 d . . . C2 C 0.8915(4) 0.4389(3) 0.8466(2) 0.0289(7) Uani 1 1 d . . . C3 C 0.7438(4) 0.5862(3) 0.76207(19) 0.0288(7) Uani 1 1 d . . . C4 C 0.7895(5) 0.4077(3) 0.6905(2) 0.0485(10) Uani 1 1 d . . . H4A H 0.7240 0.4538 0.6407 0.073 Uiso 1 1 calc R . . H4B H 0.7459 0.3336 0.7191 0.073 Uiso 1 1 calc R . . H4C H 0.8873 0.3937 0.6652 0.073 Uiso 1 1 calc R . . C5 C 0.9819(4) 0.3377(3) 0.8971(2) 0.0316(7) Uani 1 1 d . . . C6 C 0.9938(5) 0.2277(3) 0.8651(3) 0.0486(10) Uani 1 1 d . . . H6A H 1.0591 0.1692 0.9073 0.073 Uiso 1 1 calc R . . H6B H 1.0353 0.2453 0.8028 0.073 Uiso 1 1 calc R . . H6C H 0.8947 0.1981 0.8647 0.073 Uiso 1 1 calc R . . C7 C 1.1377(4) 0.2467(2) 1.0285(2) 0.0299(7) Uani 1 1 d . A . C8 C 1.0672(4) 0.1650(3) 1.1021(2) 0.0382(8) Uani 1 1 d . . . C9 C 1.1532(5) 0.0633(3) 1.1494(3) 0.0495(10) Uani 1 1 d . . . H9 H 1.1097 0.0082 1.1988 0.059 Uiso 1 1 calc R . . C10 C 1.2991(5) 0.0428(3) 1.1249(3) 0.0533(11) Uani 1 1 d . . . H10 H 1.3534 -0.0264 1.1566 0.064 Uiso 1 1 calc R . . C11 C 1.3667(5) 0.1244(3) 1.0531(3) 0.0540(10) Uani 1 1 d . A . H11 H 1.4669 0.1097 1.0374 0.065 Uiso 1 1 calc R . . C12 C 1.2880(5) 0.2288(3) 1.0035(3) 0.0449(9) Uani 1 1 d D . . C13 C 0.9055(5) 0.1853(3) 1.1313(3) 0.0593(11) Uani 1 1 d . . . H13 H 0.8655 0.2614 1.0907 0.071 Uiso 1 1 calc R . . C14 C 0.9005(8) 0.1926(7) 1.2323(5) 0.115(3) Uani 1 1 d . . . H14A H 0.7971 0.2058 1.2496 0.172 Uiso 1 1 calc R . . H14B H 0.9589 0.2566 1.2378 0.172 Uiso 1 1 calc R . . H14C H 0.9425 0.1199 1.2733 0.172 Uiso 1 1 calc R . . C15 C 0.8026(6) 0.0908(6) 1.1204(4) 0.0879(16) Uani 1 1 d . . . H15A H 0.7012 0.1082 1.1389 0.132 Uiso 1 1 calc R . . H15B H 0.8397 0.0152 1.1594 0.132 Uiso 1 1 calc R . . H15C H 0.8019 0.0892 1.0559 0.132 Uiso 1 1 calc R . . C16A C 1.3541(10) 0.3099(6) 0.9137(6) 0.050(2) Uiso 0.534(13) 1 d PD A 1 H16A H 1.2682 0.3507 0.8741 0.060 Uiso 0.534(13) 1 calc PR A 1 C17A C 1.4346(17) 0.4015(11) 0.9456(9) 0.102(4) Uiso 0.534(13) 1 d PD A 1 H17A H 1.3657 0.4385 0.9809 0.153 Uiso 0.534(13) 1 calc PR A 1 H17B H 1.4694 0.4600 0.8917 0.153 Uiso 0.534(13) 1 calc PR A 1 H17C H 1.5200 0.3643 0.9846 0.153 Uiso 0.534(13) 1 calc PR A 1 C18A C 1.4534(12) 0.2501(9) 0.8550(6) 0.068(3) Uiso 0.534(13) 1 d PD A 1 H18A H 1.4868 0.3082 0.8004 0.102 Uiso 0.534(13) 1 calc PR A 1 H18B H 1.3965 0.1937 0.8358 0.102 Uiso 0.534(13) 1 calc PR A 1 H18C H 1.5401 0.2105 0.8914 0.102 Uiso 0.534(13) 1 calc PR A 1 C16B C 1.3785(11) 0.3286(9) 0.9419(7) 0.053(3) Uiso 0.466(13) 1 d PD A 2 H16B H 1.3135 0.4012 0.9319 0.064 Uiso 0.466(13) 1 calc PR A 2 C17B C 1.5256(12) 0.3524(10) 0.9796(7) 0.066(3) Uiso 0.466(13) 1 d PD A 2 H17D H 1.5712 0.4157 0.9343 0.099 Uiso 0.466(13) 1 calc PR A 2 H17E H 1.5924 0.2827 0.9920 0.099 Uiso 0.466(13) 1 calc PR A 2 H17F H 1.5080 0.3742 1.0369 0.099 Uiso 0.466(13) 1 calc PR A 2 C18B C 1.408(3) 0.311(2) 0.8469(11) 0.137(7) Uiso 0.466(13) 1 d PD A 2 H18D H 1.3146 0.2943 0.8212 0.205 Uiso 0.466(13) 1 calc PR A 2 H18E H 1.4805 0.2452 0.8526 0.205 Uiso 0.466(13) 1 calc PR A 2 H18F H 1.4472 0.3806 0.8060 0.205 Uiso 0.466(13) 1 calc PR A 2 C19 C 0.6438(4) 0.6687(3) 0.6922(2) 0.0326(7) Uani 1 1 d . . . C20 C 0.5731(6) 0.7744(4) 0.7185(3) 0.0605(13) Uani 1 1 d . . . H20A H 0.5112 0.8216 0.6673 0.091 Uiso 1 1 calc R . . H20B H 0.6519 0.8207 0.7316 0.091 Uiso 1 1 calc R . . H20C H 0.5113 0.7484 0.7733 0.091 Uiso 1 1 calc R . . C21 C 0.5268(4) 0.7191(3) 0.5412(2) 0.0340(8) Uani 1 1 d . B . C22 C 0.5941(5) 0.8027(3) 0.4675(2) 0.0431(9) Uani 1 1 d D . . C23 C 0.5002(6) 0.8674(3) 0.3926(3) 0.0601(12) Uani 1 1 d . B . H23 H 0.5419 0.9239 0.3434 0.072 Uiso 1 1 calc R . . C24 C 0.3491(6) 0.8488(4) 0.3907(3) 0.0667(13) Uani 1 1 d . . . H24 H 0.2890 0.8929 0.3406 0.080 Uiso 1 1 calc R B . C25 C 0.2846(5) 0.7648(4) 0.4629(3) 0.0587(12) Uani 1 1 d . B . H25 H 0.1814 0.7533 0.4606 0.070 Uiso 1 1 calc R . . C26 C 0.3717(4) 0.6969(3) 0.5392(2) 0.0409(8) Uani 1 1 d . . . C27A C 0.7698(8) 0.8107(8) 0.4648(5) 0.045(2) Uiso 0.609(19) 1 d PD B 3 H27A H 0.8098 0.7367 0.5083 0.054 Uiso 0.609(19) 1 calc PR B 3 C28A C 0.8123(13) 0.9078(11) 0.5090(8) 0.086(4) Uiso 0.609(19) 1 d PD B 3 H28A H 0.7578 0.8998 0.5668 0.129 Uiso 0.609(19) 1 calc PR B 3 H28B H 0.7862 0.9838 0.4664 0.129 Uiso 0.609(19) 1 calc PR B 3 H28C H 0.9196 0.9007 0.5216 0.129 Uiso 0.609(19) 1 calc PR B 3 C29A C 0.8420(15) 0.8139(12) 0.3726(7) 0.072(3) Uiso 0.609(19) 1 d PD B 3 H29A H 0.9498 0.8192 0.3775 0.108 Uiso 0.609(19) 1 calc PR B 3 H29B H 0.8008 0.8814 0.3252 0.108 Uiso 0.609(19) 1 calc PR B 3 H29C H 0.8219 0.7433 0.3558 0.108 Uiso 0.609(19) 1 calc PR B 3 C27B C 0.7503(13) 0.8383(11) 0.4705(8) 0.044(3) Uiso 0.391(19) 1 d PD B 4 H27B H 0.8053 0.7868 0.5252 0.053 Uiso 0.391(19) 1 calc PR B 4 C28B C 0.766(2) 0.9657(13) 0.4653(12) 0.080(5) Uiso 0.391(19) 1 d PD B 4 H28D H 0.8720 0.9804 0.4673 0.121 Uiso 0.391(19) 1 calc PR B 4 H28E H 0.7151 0.9837 0.5177 0.121 Uiso 0.391(19) 1 calc PR B 4 H28F H 0.7219 1.0145 0.4076 0.121 Uiso 0.391(19) 1 calc PR B 4 C29B C 0.837(3) 0.842(2) 0.3794(13) 0.101(8) Uiso 0.391(19) 1 d PD B 4 H29D H 0.9389 0.8651 0.3849 0.152 Uiso 0.391(19) 1 calc PR B 4 H29E H 0.7865 0.8984 0.3275 0.152 Uiso 0.391(19) 1 calc PR B 4 H29F H 0.8413 0.7655 0.3687 0.152 Uiso 0.391(19) 1 calc PR B 4 C30 C 0.3041(5) 0.5988(4) 0.6143(3) 0.0549(11) Uani 1 1 d . B . H30 H 0.3450 0.6002 0.6753 0.066 Uiso 1 1 calc R . . C31 C 0.1293(6) 0.6128(6) 0.6185(4) 0.101(2) Uani 1 1 d . . . H31A H 0.0923 0.5488 0.6675 0.151 Uiso 1 1 calc R B . H31B H 0.0866 0.6120 0.5593 0.151 Uiso 1 1 calc R . . H31C H 0.1001 0.6863 0.6314 0.151 Uiso 1 1 calc R . . C32 C 0.3507(7) 0.4798(4) 0.5989(3) 0.0779(15) Uani 1 1 d . . . H32A H 0.3074 0.4183 0.6471 0.117 Uiso 1 1 calc R B . H32B H 0.4595 0.4685 0.6013 0.117 Uiso 1 1 calc R . . H32C H 0.3147 0.4773 0.5384 0.117 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0294(4) 0.0205(3) 0.0219(3) -0.0084(2) -0.0070(2) 0.0047(3) N1 0.0371(17) 0.0254(13) 0.0267(12) -0.0089(10) -0.0082(11) 0.0051(12) N2 0.0398(18) 0.0254(13) 0.0293(13) -0.0083(11) -0.0121(12) 0.0061(12) N3 0.0389(18) 0.0321(14) 0.0278(13) -0.0050(11) -0.0069(12) -0.0013(12) N4 0.0322(16) 0.0238(12) 0.0268(12) -0.0071(10) -0.0046(11) 0.0076(11) C1 0.034(2) 0.0336(16) 0.0263(15) -0.0129(13) -0.0050(13) 0.0027(14) C2 0.0345(19) 0.0270(15) 0.0265(14) -0.0102(12) -0.0055(13) 0.0040(14) C3 0.0329(19) 0.0322(16) 0.0213(14) -0.0078(12) -0.0061(13) 0.0003(14) C4 0.063(3) 0.050(2) 0.0390(18) -0.0257(17) -0.0164(18) 0.0136(19) C5 0.039(2) 0.0287(15) 0.0282(15) -0.0111(13) -0.0042(14) 0.0041(14) C6 0.069(3) 0.0332(18) 0.048(2) -0.0216(16) -0.0186(19) 0.0131(18) C7 0.038(2) 0.0224(14) 0.0303(15) -0.0103(12) -0.0072(14) 0.0066(14) C8 0.050(2) 0.0273(15) 0.0353(17) -0.0054(13) -0.0063(16) 0.0014(15) C9 0.069(3) 0.0277(17) 0.046(2) -0.0016(15) -0.010(2) 0.0015(18) C10 0.069(3) 0.0324(18) 0.055(2) -0.0088(17) -0.020(2) 0.015(2) C11 0.042(2) 0.050(2) 0.070(3) -0.021(2) -0.012(2) 0.0178(19) C12 0.040(2) 0.0429(19) 0.047(2) -0.0078(16) -0.0002(17) 0.0113(17) C13 0.053(3) 0.040(2) 0.073(3) 0.0028(19) 0.019(2) 0.0008(19) C14 0.098(5) 0.159(6) 0.126(5) -0.096(5) 0.061(4) -0.058(4) C15 0.056(3) 0.119(5) 0.094(4) -0.035(3) -0.004(3) -0.018(3) C19 0.034(2) 0.0339(16) 0.0293(15) -0.0087(13) -0.0087(14) 0.0013(15) C20 0.079(3) 0.057(2) 0.050(2) -0.0289(19) -0.028(2) 0.033(2) C21 0.043(2) 0.0323(16) 0.0265(15) -0.0098(13) -0.0118(14) 0.0067(15) C22 0.059(3) 0.0351(17) 0.0326(17) -0.0046(14) -0.0113(17) -0.0001(17) C23 0.086(4) 0.043(2) 0.043(2) 0.0003(17) -0.020(2) -0.001(2) C24 0.078(4) 0.062(3) 0.055(3) -0.012(2) -0.035(3) 0.019(3) C25 0.051(3) 0.073(3) 0.058(2) -0.031(2) -0.025(2) 0.013(2) C26 0.041(2) 0.050(2) 0.0363(17) -0.0205(16) -0.0096(16) 0.0041(17) C30 0.049(3) 0.079(3) 0.0399(19) -0.020(2) 0.0013(18) -0.020(2) C31 0.057(4) 0.155(6) 0.100(4) -0.047(4) 0.014(3) -0.030(4) C32 0.102(5) 0.060(3) 0.067(3) -0.006(2) -0.007(3) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.889(2) 2_767 ? Ni1 N1 1.889(2) . ? Ni1 N4 1.956(2) 2_767 ? Ni1 N4 1.956(2) . ? N1 N2 1.337(3) . ? N1 C2 1.375(4) . ? N2 C3 1.376(3) . ? N3 C19 1.280(4) . ? N3 C21 1.424(4) . ? N4 C5 1.313(4) . ? N4 C7 1.452(4) . ? C1 C2 1.400(4) . ? C1 C3 1.408(4) . ? C1 C4 1.502(4) . ? C2 C5 1.424(4) . ? C3 C19 1.468(4) . ? C5 C6 1.499(4) . ? C7 C12 1.392(5) . ? C7 C8 1.404(5) . ? C8 C9 1.396(5) . ? C8 C13 1.510(6) . ? C9 C10 1.359(6) . ? C10 C11 1.377(6) . ? C11 C12 1.397(5) . ? C12 C16B 1.534(9) . ? C12 C16A 1.538(8) . ? C13 C14 1.520(7) . ? C13 C15 1.521(7) . ? C16A C18A 1.507(10) . ? C16A C17A 1.507(11) . ? C16B C17B 1.487(11) . ? C16B C18B 1.497(13) . ? C19 C20 1.508(5) . ? C21 C22 1.404(5) . ? C21 C26 1.408(5) . ? C22 C23 1.404(5) . ? C22 C27B 1.467(11) . ? C22 C27A 1.556(8) . ? C23 C24 1.364(7) . ? C24 C25 1.382(7) . ? C25 C26 1.397(5) . ? C26 C30 1.512(6) . ? C27A C29A 1.492(9) . ? C27A C28A 1.534(10) . ? C27B C28B 1.499(12) . ? C27B C29B 1.536(13) . ? C30 C32 1.518(6) . ? C30 C31 1.542(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 N1 Ni1 N1 180.000(1) 2_767 . ? N1 Ni1 N4 82.36(10) 2_767 2_767 ? N1 Ni1 N4 97.64(10) . 2_767 ? N1 Ni1 N4 97.64(10) 2_767 . ? N1 Ni1 N4 82.36(10) . . ? N4 Ni1 N4 180.000(1) 2_767 . ? N2 N1 C2 110.0(2) . . ? N2 N1 Ni1 135.34(19) . . ? C2 N1 Ni1 114.5(2) . . ? N1 N2 C3 106.7(2) . . ? C19 N3 C21 122.9(3) . . ? C5 N4 C7 116.8(2) . . ? C5 N4 Ni1 114.3(2) . . ? C7 N4 Ni1 128.81(18) . . ? C2 C1 C3 103.4(2) . . ? C2 C1 C4 128.5(3) . . ? C3 C1 C4 128.1(3) . . ? N1 C2 C1 109.1(3) . . ? N1 C2 C5 113.8(2) . . ? C1 C2 C5 137.1(3) . . ? N2 C3 C1 110.8(3) . . ? N2 C3 C19 119.4(3) . . ? C1 C3 C19 129.8(3) . . ? N4 C5 C2 114.7(3) . . ? N4 C5 C6 124.2(3) . . ? C2 C5 C6 121.0(3) . . ? C12 C7 C8 122.0(3) . . ? C12 C7 N4 119.3(3) . . ? C8 C7 N4 118.6(3) . . ? C9 C8 C7 117.5(4) . . ? C9 C8 C13 120.3(3) . . ? C7 C8 C13 122.3(3) . . ? C10 C9 C8 121.6(4) . . ? C9 C10 C11 120.1(3) . . ? C10 C11 C12 121.4(4) . . ? C7 C12 C11 117.5(4) . . ? C7 C12 C16B 122.3(5) . . ? C11 C12 C16B 118.6(5) . . ? C7 C12 C16A 120.5(4) . . ? C11 C12 C16A 121.2(4) . . ? C8 C13 C14 110.6(4) . . ? C8 C13 C15 112.7(4) . . ? C14 C13 C15 109.7(4) . . ? C18A C16A C17A 112.8(8) . . ? C18A C16A C12 116.2(6) . . ? C17A C16A C12 105.4(7) . . ? C17B C16B C18B 107.8(11) . . ? C17B C16B C12 117.7(7) . . ? C18B C16B C12 111.0(10) . . ? N3 C19 C3 118.1(3) . . ? N3 C19 C20 124.6(3) . . ? C3 C19 C20 117.3(3) . . ? C22 C21 C26 121.6(3) . . ? C22 C21 N3 118.4(3) . . ? C26 C21 N3 119.6(3) . . ? C23 C22 C21 117.8(4) . . ? C23 C22 C27B 117.8(6) . . ? C21 C22 C27B 123.7(5) . . ? C23 C22 C27A 121.9(4) . . ? C21 C22 C27A 119.9(4) . . ? C24 C23 C22 121.2(4) . . ? C23 C24 C25 120.4(4) . . ? C24 C25 C26 121.2(4) . . ? C25 C26 C21 117.6(4) . . ? C25 C26 C30 121.2(4) . . ? C21 C26 C30 121.0(3) . . ? C29A C27A C28A 115.7(8) . . ? C29A C27A C22 115.3(7) . . ? C28A C27A C22 109.1(6) . . ? C22 C27B C28B 115.7(10) . . ? C22 C27B C29B 112.5(13) . . ? C28B C27B C29B 95.4(13) . . ? C26 C30 C32 110.3(3) . . ? C26 C30 C31 112.8(4) . . ? C32 C30 C31 109.5(4) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.351 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.062 #===END data_8-as33 _database_code_depnum_ccdc_archive 'CCDC 743832' #TrackingRef 'Dalton_B925535D_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H98 N8 Ni' _chemical_formula_sum 'C94 H98 N8 Ni' _chemical_formula_weight 1398.51 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7920(6) _cell_length_b 14.7660(9) _cell_length_c 27.8400(16) _cell_angle_alpha 83.335(5) _cell_angle_beta 80.671(5) _cell_angle_gamma 86.048(5) _cell_volume 3940.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 37618 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.03 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37618 _diffrn_reflns_av_R_equivalents 0.1101 _diffrn_reflns_av_sigmaI/netI 0.1900 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.03 _reflns_number_total 17062 _reflns_number_gt 6680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _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^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17062 _refine_ls_number_parameters 800 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1940 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.882 _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 Ni1 Ni 1.0000 0.5000 1.0000 0.0336(2) Uani 1 2 d S . . Ni2 Ni 0.5000 0.5000 0.5000 0.0363(3) Uani 1 2 d S . . N1 N 0.9841(4) 0.4006(3) 0.96447(12) 0.0339(10) Uani 1 1 d . . . N2 N 1.0371(4) 0.3771(2) 0.91965(12) 0.0345(10) Uani 1 1 d . . . N3 N 0.8735(4) 0.4308(3) 1.04913(12) 0.0399(11) Uani 1 1 d . A . N4 N 1.1208(4) 0.1719(3) 0.87707(12) 0.0364(9) Uani 1 1 d . A . N11 N 0.5200(4) 0.6072(3) 0.52845(12) 0.0350(10) Uani 1 1 d . . . N12 N 0.4708(4) 0.6397(2) 0.57160(12) 0.0347(10) Uani 1 1 d . . . N13 N 0.6342(5) 0.5559(3) 0.44800(13) 0.0412(11) Uani 1 1 d . B . N14 N 0.6231(4) 0.7849(3) 0.63022(12) 0.0413(10) Uani 1 1 d . B . C1 C 0.9153(5) 0.2584(3) 0.96153(15) 0.0352(11) Uani 1 1 d D . . C2 C 0.9078(5) 0.3310(3) 0.99023(15) 0.0328(11) Uani 1 1 d . A . C3 C 0.9973(5) 0.2915(3) 0.91787(14) 0.0317(11) Uani 1 1 d . A . C4A C 0.8724(6) 0.1585(3) 0.97802(18) 0.0219(19) Uiso 0.466(5) 1 d PGD A 1 C5A C 0.9016(6) 0.1114(4) 1.02171(18) 0.032(2) Uiso 0.466(5) 1 d PG A 1 H5A H 0.9584 0.1363 1.0400 0.039 Uiso 0.466(5) 1 calc PR A 1 C6A C 0.8458(6) 0.0273(3) 1.03812(17) 0.038(2) Uiso 0.466(5) 1 d PG A 1 H6A H 0.8653 -0.0042 1.0674 0.046 Uiso 0.466(5) 1 calc PR A 1 C7A C 0.7609(7) -0.0099(3) 1.0109(2) 0.043(2) Uiso 0.466(5) 1 d PG A 1 H7A H 0.7236 -0.0662 1.0218 0.052 Uiso 0.466(5) 1 calc PR A 1 C8A C 0.7317(6) 0.0372(4) 0.9672(2) 0.042(2) Uiso 0.466(5) 1 d PG A 1 H8A H 0.6749 0.0123 0.9489 0.050 Uiso 0.466(5) 1 calc PR A 1 C9A C 0.7875(7) 0.1213(4) 0.95075(16) 0.036(2) Uiso 0.466(5) 1 d PG A 1 H9A H 0.7680 0.1528 0.9215 0.043 Uiso 0.466(5) 1 calc PR A 1 C4B C 0.8220(5) 0.1812(3) 0.9703(2) 0.0305(19) Uiso 0.534(5) 1 d PGD A 2 C5B C 0.8878(4) 0.0952(4) 0.9668(2) 0.038(2) Uiso 0.534(5) 1 d PG A 2 H5B H 0.9833 0.0895 0.9574 0.046 Uiso 0.534(5) 1 calc PR A 2 C6B C 0.8109(6) 0.0177(3) 0.9775(2) 0.053(2) Uiso 0.534(5) 1 d PG A 2 H6B H 0.8549 -0.0398 0.9752 0.063 Uiso 0.534(5) 1 calc PR A 2 C7B C 0.6682(6) 0.0262(3) 0.9916(2) 0.056(3) Uiso 0.534(5) 1 d PG A 2 H7B H 0.6167 -0.0256 0.9988 0.068 Uiso 0.534(5) 1 calc PR A 2 C8B C 0.6024(4) 0.1122(4) 0.9951(2) 0.048(2) Uiso 0.534(5) 1 d PG A 2 H8B H 0.5069 0.1179 1.0045 0.058 Uiso 0.534(5) 1 calc PR A 2 C9B C 0.6793(5) 0.1897(3) 0.9844(2) 0.042(2) Uiso 0.534(5) 1 d PG A 2 H9B H 0.6353 0.2473 0.9867 0.050 Uiso 0.534(5) 1 calc PR A 2 C10 C 0.8429(5) 0.3513(3) 1.03831(16) 0.0333(10) Uiso 1 1 d D . . C11A C 0.7501(5) 0.2902(3) 1.0719(2) 0.034(5) Uiso 0.539(5) 1 d PGD A 3 C12A C 0.6112(5) 0.3098(3) 1.0892(2) 0.039(2) Uiso 0.539(5) 1 d PG A 3 H12A H 0.5705 0.3670 1.0808 0.047 Uiso 0.539(5) 1 calc PR A 3 C13A C 0.5330(4) 0.2438(3) 1.1190(2) 0.039(2) Uiso 0.539(5) 1 d PG A 3 H13A H 0.4400 0.2569 1.1306 0.047 Uiso 0.539(5) 1 calc PR A 3 C14A C 0.5937(5) 0.1583(3) 1.13152(19) 0.042(2) Uiso 0.539(5) 1 d PG A 3 H14A H 0.5414 0.1141 1.1515 0.051 Uiso 0.539(5) 1 calc PR A 3 C15A C 0.7327(5) 0.1387(3) 1.11425(19) 0.044(2) Uiso 0.539(5) 1 d PG A 3 H15A H 0.7733 0.0815 1.1226 0.080 Uiso 0.539(5) 1 calc PR A 3 C16A C 0.8109(4) 0.2047(3) 1.08446(19) 0.0346(19) Uiso 0.539(5) 1 d PG A 3 H16A H 0.9039 0.1916 1.0729 0.041 Uiso 0.539(5) 1 calc PR A 3 C11B C 0.7438(6) 0.2854(4) 1.0679(2) 0.027(5) Uiso 0.461(5) 1 d PGD A 4 C12B C 0.6369(7) 0.2663(5) 1.04398(18) 0.043(3) Uiso 0.461(5) 1 d PG A 4 H12B H 0.6349 0.2908 1.0118 0.052 Uiso 0.461(5) 1 calc PR A 4 C13B C 0.5329(6) 0.2105(5) 1.0682(2) 0.054(3) Uiso 0.461(5) 1 d PG A 4 H13B H 0.4613 0.1977 1.0521 0.065 Uiso 0.461(5) 1 calc PR A 4 C14B C 0.5359(6) 0.1739(4) 1.1163(2) 0.045(3) Uiso 0.461(5) 1 d PG A 4 H14B H 0.4663 0.1366 1.1325 0.054 Uiso 0.461(5) 1 calc PR A 4 C15B C 0.6428(7) 0.1930(4) 1.14026(17) 0.040(2) Uiso 0.461(5) 1 d PG A 4 H15B H 0.6448 0.1684 1.1725 0.080 Uiso 0.461(5) 1 calc PR A 4 C16B C 0.7468(6) 0.2487(4) 1.1161(2) 0.046(3) Uiso 0.461(5) 1 d PG A 4 H16B H 0.8184 0.2615 1.1321 0.055 Uiso 0.461(5) 1 calc PR A 4 C17 C 0.8143(6) 0.4611(4) 1.09613(15) 0.0458(15) Uani 1 1 d . . . C18 C 0.6958(6) 0.5199(5) 1.09856(19) 0.0625(19) Uani 1 1 d D A . C19 C 0.6473(7) 0.5546(5) 1.1429(2) 0.078(2) Uani 1 1 d . . . H19 H 0.5674 0.5927 1.1461 0.094 Uiso 1 1 calc R A . C20 C 0.7170(9) 0.5328(5) 1.1819(2) 0.080(3) Uani 1 1 d . A . H20 H 0.6853 0.5583 1.2110 0.096 Uiso 1 1 calc R . . C21 C 0.8331(9) 0.4740(4) 1.17921(19) 0.079(2) Uani 1 1 d . . . H21 H 0.8764 0.4594 1.2067 0.094 Uiso 1 1 calc R A . C22 C 0.8871(7) 0.4359(4) 1.13580(17) 0.0598(19) Uani 1 1 d D A . C23A C 0.6255(9) 0.5637(9) 1.0523(3) 0.047(3) Uiso 0.590(14) 1 d PD A 5 H23A H 0.6591 0.5248 1.0262 0.057 Uiso 0.590(14) 1 calc PR A 5 C24A C 0.6629(13) 0.6625(9) 1.0303(4) 0.068(3) Uiso 0.590(14) 1 d PD A 5 H24A H 0.7617 0.6667 1.0251 0.102 Uiso 0.590(14) 1 calc PR A 5 H24B H 0.6211 0.7051 1.0527 0.102 Uiso 0.590(14) 1 calc PR A 5 H24C H 0.6289 0.6766 0.9997 0.102 Uiso 0.590(14) 1 calc PR A 5 C25A C 0.4653(10) 0.5646(9) 1.0588(4) 0.069(4) Uiso 0.590(14) 1 d PD A 5 H25A H 0.4350 0.5050 1.0720 0.104 Uiso 0.590(14) 1 calc PR A 5 H25B H 0.4354 0.5809 1.0276 0.104 Uiso 0.590(14) 1 calc PR A 5 H25C H 0.4263 0.6083 1.0808 0.104 Uiso 0.590(14) 1 calc PR A 5 C23B C 0.6177(11) 0.5208(10) 1.0601(4) 0.040(3) Uiso 0.410(14) 1 d PD A 6 H23B H 0.6582 0.4754 1.0381 0.047 Uiso 0.410(14) 1 calc PR A 6 C24B C 0.6448(17) 0.6160(12) 1.0352(5) 0.056(4) Uiso 0.410(14) 1 d PD A 6 H24D H 0.5966 0.6276 1.0076 0.084 Uiso 0.410(14) 1 calc PR A 6 H24E H 0.7425 0.6210 1.0244 0.084 Uiso 0.410(14) 1 calc PR A 6 H24F H 0.6126 0.6599 1.0580 0.084 Uiso 0.410(14) 1 calc PR A 6 C25B C 0.4678(14) 0.5029(12) 1.0783(6) 0.071(5) Uiso 0.410(14) 1 d PD A 6 H25D H 0.4187 0.5052 1.0510 0.106 Uiso 0.410(14) 1 calc PR A 6 H25E H 0.4279 0.5485 1.0991 0.106 Uiso 0.410(14) 1 calc PR A 6 H25F H 0.4611 0.4436 1.0965 0.106 Uiso 0.410(14) 1 calc PR A 6 C26A C 1.0322(13) 0.3777(8) 1.1286(5) 0.058(4) Uiso 0.53(2) 1 d PD A 7 H26A H 1.0298 0.3434 1.1007 0.069 Uiso 0.53(2) 1 calc PR A 7 C27A C 1.0568(19) 0.3039(8) 1.1723(4) 0.078(5) Uiso 0.53(2) 1 d PD A 7 H27A H 0.9755 0.2694 1.1824 0.117 Uiso 0.53(2) 1 calc PR A 7 H27B H 1.0755 0.3336 1.1992 0.117 Uiso 0.53(2) 1 calc PR A 7 H27C H 1.1344 0.2636 1.1618 0.117 Uiso 0.53(2) 1 calc PR A 7 C28A C 1.1671(14) 0.4290(8) 1.1161(5) 0.060(4) Uiso 0.53(2) 1 d PD A 7 H28A H 1.2450 0.3857 1.1132 0.090 Uiso 0.53(2) 1 calc PR A 7 H28B H 1.1733 0.4663 1.1416 0.090 Uiso 0.53(2) 1 calc PR A 7 H28C H 1.1672 0.4669 1.0856 0.090 Uiso 0.53(2) 1 calc PR A 7 C26B C 0.9948(14) 0.3713(7) 1.1361(5) 0.047(4) Uiso 0.47(2) 1 d PD A 8 H26B H 1.0065 0.3418 1.1058 0.057 Uiso 0.47(2) 1 calc PR A 8 C27B C 0.9633(18) 0.2999(8) 1.1791(4) 0.061(4) Uiso 0.47(2) 1 d PD A 8 H27D H 1.0386 0.2547 1.1790 0.092 Uiso 0.47(2) 1 calc PR A 8 H27E H 0.8798 0.2714 1.1768 0.092 Uiso 0.47(2) 1 calc PR A 8 H27F H 0.9514 0.3283 1.2090 0.092 Uiso 0.47(2) 1 calc PR A 8 C28B C 1.1208(17) 0.4285(9) 1.1353(6) 0.069(4) Uiso 0.47(2) 1 d PD A 8 H28D H 1.2028 0.3889 1.1353 0.103 Uiso 0.47(2) 1 calc PR A 8 H28E H 1.1073 0.4609 1.1638 0.103 Uiso 0.47(2) 1 calc PR A 8 H28F H 1.1311 0.4713 1.1064 0.103 Uiso 0.47(2) 1 calc PR A 8 C29 C 1.0494(5) 0.2475(3) 0.87249(14) 0.0319(10) Uani 1 1 d . . . C30 C 1.0133(5) 0.2966(3) 0.82597(14) 0.0362(11) Uani 1 1 d . A . C31 C 0.8825(5) 0.3388(3) 0.82563(16) 0.0434(12) Uani 1 1 d . . . H31 H 0.8204 0.3382 0.8547 0.052 Uiso 1 1 calc R A . C32 C 0.8425(7) 0.3817(4) 0.78298(19) 0.0582(15) Uani 1 1 d . A . H32 H 0.7532 0.4078 0.7834 0.070 Uiso 1 1 calc R . . C33 C 0.9349(7) 0.3862(4) 0.7395(2) 0.0584(16) Uani 1 1 d . . . H33 H 0.9084 0.4156 0.7108 0.070 Uiso 1 1 calc R A . C34 C 1.0657(6) 0.3468(3) 0.73932(17) 0.0501(14) Uani 1 1 d . A . H34 H 1.1282 0.3502 0.7103 0.060 Uiso 1 1 calc R . . C35 C 1.1066(5) 0.3020(3) 0.78178(14) 0.0411(11) Uani 1 1 d . . . H35 H 1.1958 0.2756 0.7810 0.049 Uiso 1 1 calc R A . C36 C 1.1800(5) 0.1230(3) 0.83670(14) 0.0390(11) Uani 1 1 d . . . C37 C 1.3266(5) 0.1208(4) 0.82467(17) 0.0512(13) Uani 1 1 d D A . C38 C 1.3877(6) 0.0691(4) 0.78698(19) 0.0663(17) Uani 1 1 d . . . H38 H 1.4835 0.0679 0.7780 0.080 Uiso 1 1 calc R A . C40 C 1.3104(6) 0.0199(4) 0.76267(18) 0.0581(15) Uani 1 1 d . A . H40 H 1.3537 -0.0137 0.7377 0.070 Uiso 1 1 calc R . . C41 C 1.1689(6) 0.0212(3) 0.77588(17) 0.0523(14) Uani 1 1 d . . . H41 H 1.1170 -0.0124 0.7598 0.063 Uiso 1 1 calc R A . C42 C 1.1005(5) 0.0723(3) 0.81319(16) 0.0391(11) Uani 1 1 d . A . C43A C 1.4050(12) 0.1797(7) 0.8534(4) 0.076(5) Uiso 0.707(14) 1 d PD A 9 H43A H 1.3451 0.2157 0.8767 0.091 Uiso 0.707(14) 1 calc PR A 9 C44A C 1.5026(10) 0.0969(6) 0.8786(4) 0.080(3) Uiso 0.707(14) 1 d PD A 9 H44A H 1.4442 0.0519 0.8977 0.119 Uiso 0.707(14) 1 calc PR A 9 H44B H 1.5560 0.1220 0.8995 0.119 Uiso 0.707(14) 1 calc PR A 9 H44C H 1.5639 0.0690 0.8534 0.119 Uiso 0.707(14) 1 calc PR A 9 C45A C 1.5229(12) 0.2316(8) 0.8210(4) 0.075(4) Uiso 0.707(14) 1 d PD A 9 H45A H 1.5653 0.2675 0.8406 0.112 Uiso 0.707(14) 1 calc PR A 9 H45B H 1.4862 0.2711 0.7957 0.112 Uiso 0.707(14) 1 calc PR A 9 H45C H 1.5908 0.1888 0.8064 0.112 Uiso 0.707(14) 1 calc PR A 9 C43B C 1.4234(18) 0.1601(13) 0.8488(5) 0.026(5) Uiso 0.293(14) 1 d PD A 10 H43B H 1.4938 0.1115 0.8407 0.032 Uiso 0.293(14) 1 calc PR A 10 C44B C 1.426(3) 0.1361(16) 0.9042(6) 0.080(8) Uiso 0.293(14) 1 d PD A 10 H44D H 1.4986 0.1679 0.9136 0.120 Uiso 0.293(14) 1 calc PR A 10 H44E H 1.4439 0.0715 0.9110 0.120 Uiso 0.293(14) 1 calc PR A 10 H44F H 1.3388 0.1541 0.9223 0.120 Uiso 0.293(14) 1 calc PR A 10 C45B C 1.502(2) 0.2304(12) 0.8085(7) 0.036(5) Uiso 0.293(14) 1 d PD A 10 H45D H 1.5700 0.2586 0.8222 0.054 Uiso 0.293(14) 1 calc PR A 10 H45E H 1.4366 0.2765 0.7974 0.054 Uiso 0.293(14) 1 calc PR A 10 H45F H 1.5467 0.1991 0.7814 0.054 Uiso 0.293(14) 1 calc PR A 10 C46 C 0.9441(5) 0.0697(3) 0.82586(17) 0.0423(12) Uani 1 1 d . . . H46 H 0.9130 0.1124 0.8503 0.051 Uiso 1 1 calc R A . C47 C 0.8726(6) 0.1001(3) 0.78152(18) 0.0526(13) Uani 1 1 d . A . H47A H 0.7741 0.0974 0.7910 0.079 Uiso 1 1 calc R . . H47B H 0.9035 0.0604 0.7565 0.079 Uiso 1 1 calc R . . H47C H 0.8951 0.1616 0.7692 0.079 Uiso 1 1 calc R . . C48 C 0.9050(6) -0.0263(3) 0.84931(19) 0.0589(15) Uani 1 1 d . A . H48A H 0.8060 -0.0279 0.8575 0.088 Uiso 1 1 calc R . . H48B H 0.9462 -0.0411 0.8784 0.088 Uiso 1 1 calc R . . H48C H 0.9382 -0.0701 0.8266 0.088 Uiso 1 1 calc R . . C101 C 0.6206(5) 0.7408(3) 0.52673(15) 0.0330(11) Uani 1 1 d D . . C102 C 0.6109(5) 0.6672(3) 0.50083(15) 0.0353(12) Uani 1 1 d . B . C103 C 0.5315(5) 0.7198(3) 0.57069(15) 0.0335(11) Uani 1 1 d . B . C51A C 0.7007(5) 0.8230(3) 0.5090(2) 0.037(6) Uiso 0.719(10) 1 d PGD B 11 C52A C 0.6310(4) 0.9060(4) 0.4976(2) 0.062(2) Uiso 0.719(10) 1 d PG B 11 H52A H 0.5347 0.9110 0.5040 0.074 Uiso 0.719(10) 1 calc PR B 11 C53A C 0.7053(7) 0.9814(3) 0.4767(3) 0.089(3) Uiso 0.719(10) 1 d PG B 11 H53A H 0.6587 1.0370 0.4691 0.107 Uiso 0.719(10) 1 calc PR B 11 C54A C 0.8492(7) 0.9739(3) 0.4672(2) 0.111(5) Uiso 0.719(10) 1 d PG B 11 H54A H 0.8988 1.0244 0.4532 0.133 Uiso 0.719(10) 1 calc PR B 11 C55A C 0.9188(5) 0.8909(4) 0.4786(3) 0.076(3) Uiso 0.719(10) 1 d PG B 11 H55A H 1.0151 0.8859 0.4722 0.091 Uiso 0.719(10) 1 calc PR B 11 C56A C 0.8446(5) 0.8155(3) 0.4995(2) 0.047(2) Uiso 0.719(10) 1 d PG B 11 H56A H 0.8912 0.7599 0.5071 0.057 Uiso 0.719(10) 1 calc PR B 11 C51B C 0.7031(14) 0.8200(8) 0.5119(5) 0.044(19) Uiso 0.281(10) 1 d PGD B 12 C52B C 0.6670(14) 0.8881(10) 0.4768(6) 0.060(6) Uiso 0.281(10) 1 d PG B 12 H52B H 0.5837 0.8867 0.4649 0.072 Uiso 0.281(10) 1 calc PR B 12 C53B C 0.7553(16) 0.9584(9) 0.4593(5) 0.075(7) Uiso 0.281(10) 1 d PG B 12 H53B H 0.7311 1.0040 0.4357 0.090 Uiso 0.281(10) 1 calc PR B 12 C54B C 0.8798(13) 0.9605(8) 0.4769(5) 0.037(4) Uiso 0.281(10) 1 d PG B 12 H54B H 0.9389 1.0075 0.4652 0.045 Uiso 0.281(10) 1 calc PR B 12 C55B C 0.9159(13) 0.8923(10) 0.5121(6) 0.096(9) Uiso 0.281(10) 1 d PG B 12 H55B H 0.9992 0.8938 0.5240 0.115 Uiso 0.281(10) 1 calc PR B 12 C56B C 0.8276(17) 0.8221(9) 0.5296(6) 0.074(7) Uiso 0.281(10) 1 d PG B 12 H56B H 0.8518 0.7765 0.5532 0.089 Uiso 0.281(10) 1 calc PR B 12 C110 C 0.6712(5) 0.6367(3) 0.45485(15) 0.0367(12) Uani 1 1 d D . . C31A C 0.7710(4) 0.6920(3) 0.41844(14) 0.032(3) Uiso 0.736(8) 1 d PGD B 13 C32A C 0.9118(5) 0.6689(2) 0.40766(16) 0.0410(17) Uiso 0.736(8) 1 d PG B 13 H32A H 0.9483 0.6146 0.4221 0.049 Uiso 0.736(8) 1 calc PR B 13 C33A C 0.9979(4) 0.7270(3) 0.37531(17) 0.0469(18) Uiso 0.736(8) 1 d PG B 13 H33A H 1.0921 0.7115 0.3681 0.056 Uiso 0.736(8) 1 calc PR B 13 C34A C 0.9433(4) 0.8082(3) 0.35375(15) 0.0513(13) Uiso 0.736(8) 1 d PG B 13 H34D H 1.0010 0.8470 0.3321 0.062 Uiso 0.736(8) 1 calc PR B 13 C35A C 0.8025(5) 0.8313(3) 0.36453(17) 0.0534(19) Uiso 0.736(8) 1 d PG B 13 H35D H 0.7660 0.8856 0.3501 0.064 Uiso 0.736(8) 1 calc PR B 13 C36A C 0.7164(4) 0.7732(3) 0.39688(18) 0.0423(17) Uiso 0.736(8) 1 d PG B 13 H36A H 0.6222 0.7887 0.4041 0.051 Uiso 0.736(8) 1 calc PR B 13 C31B C 0.7561(12) 0.6993(8) 0.4198(4) 0.027(9) Uiso 0.264(8) 1 d PGD B 14 C32B C 0.8884(14) 0.7038(9) 0.4312(4) 0.060(6) Uiso 0.264(8) 1 d PG B 14 H32B H 0.9128 0.6705 0.4592 0.072 Uiso 0.264(8) 1 calc PR B 14 C33B C 0.9841(11) 0.7581(9) 0.4006(5) 0.058(6) Uiso 0.264(8) 1 d PG B 14 H33B H 1.0726 0.7611 0.4082 0.069 Uiso 0.264(8) 1 calc PR B 14 C34B C 0.9475(10) 0.8078(8) 0.3586(4) 0.0513(13) Uiso 0.264(8) 1 d PG B 14 H34E H 1.0116 0.8441 0.3381 0.062 Uiso 0.264(8) 1 calc PR B 14 C35B C 0.8152(12) 0.8033(7) 0.3473(3) 0.028(4) Uiso 0.264(8) 1 d PG B 14 H35E H 0.7908 0.8366 0.3192 0.034 Uiso 0.264(8) 1 calc PR B 14 C36B C 0.7195(10) 0.7490(8) 0.3779(4) 0.029(4) Uiso 0.264(8) 1 d PG B 14 H36B H 0.6310 0.7460 0.3702 0.035 Uiso 0.264(8) 1 calc PR B 14 C117 C 0.6919(6) 0.5162(3) 0.40345(16) 0.0451(15) Uani 1 1 d . . . C118 C 0.8096(6) 0.4568(4) 0.40412(17) 0.0476(15) Uani 1 1 d . B . C119 C 0.8556(6) 0.4136(4) 0.36238(18) 0.0532(16) Uani 1 1 d . . . H119 H 0.9338 0.3740 0.3614 0.064 Uiso 1 1 calc R B . C120 C 0.7872(7) 0.4285(4) 0.32239(18) 0.0539(16) Uani 1 1 d . B . H120 H 0.8180 0.3973 0.2952 0.065 Uiso 1 1 calc R . . C121 C 0.6747(7) 0.4885(4) 0.32229(16) 0.0547(16) Uani 1 1 d . . . H121 H 0.6317 0.4992 0.2946 0.066 Uiso 1 1 calc R B . C122 C 0.6234(6) 0.5341(3) 0.36311(18) 0.0487(14) Uani 1 1 d . B . C123 C 0.8825(6) 0.4359(5) 0.4496(2) 0.0595(17) Uani 1 1 d . . . H123 H 0.8579 0.4864 0.4698 0.071 Uiso 1 1 calc R B . C124 C 1.0411(6) 0.4302(5) 0.4357(3) 0.086(2) Uani 1 1 d . B . H12D H 1.0708 0.4852 0.4161 0.128 Uiso 1 1 calc R . . H12E H 1.0687 0.3789 0.4174 0.128 Uiso 1 1 calc R . . H12F H 1.0829 0.4228 0.4649 0.128 Uiso 1 1 calc R . . C125 C 0.8330(6) 0.3486(4) 0.4804(2) 0.0670(17) Uani 1 1 d . B . H12G H 0.8801 0.3377 0.5084 0.101 Uiso 1 1 calc R . . H12H H 0.8529 0.2981 0.4611 0.101 Uiso 1 1 calc R . . H12I H 0.7350 0.3551 0.4912 0.101 Uiso 1 1 calc R . . C127 C 0.4975(8) 0.5986(4) 0.36328(18) 0.0649(18) Uani 1 1 d . . . H127 H 0.4981 0.6375 0.3895 0.078 Uiso 1 1 calc R B . C128 C 0.3616(8) 0.5474(5) 0.3756(3) 0.098(2) Uani 1 1 d . B . H12J H 0.2838 0.5906 0.3753 0.147 Uiso 1 1 calc R . . H12K H 0.3569 0.5140 0.4075 0.147 Uiso 1 1 calc R . . H12L H 0.3596 0.5057 0.3518 0.147 Uiso 1 1 calc R . . C129 C 0.4932(10) 0.6623(5) 0.3157(2) 0.107(3) Uani 1 1 d . B . H12M H 0.4096 0.7006 0.3189 0.161 Uiso 1 1 calc R . . H12N H 0.4955 0.6265 0.2889 0.161 Uiso 1 1 calc R . . H12O H 0.5719 0.6997 0.3097 0.161 Uiso 1 1 calc R . . C130 C 0.5105(5) 0.7671(3) 0.61612(15) 0.0360(11) Uani 1 1 d . . . C131 C 0.3638(5) 0.7893(3) 0.63828(17) 0.0397(12) Uani 1 1 d . B . C132 C 0.3234(5) 0.7951(3) 0.68833(17) 0.0532(15) Uani 1 1 d . . . H132 H 0.3880 0.7839 0.7097 0.064 Uiso 1 1 calc R B . C133 C 0.1840(6) 0.8180(4) 0.7061(2) 0.0621(17) Uani 1 1 d . B . H133 H 0.1576 0.8231 0.7394 0.075 Uiso 1 1 calc R . . C134 C 0.0869(6) 0.8328(4) 0.6760(2) 0.0639(17) Uani 1 1 d . . . H134 H -0.0050 0.8468 0.6886 0.077 Uiso 1 1 calc R B . C135 C 0.1252(6) 0.8271(4) 0.6266(2) 0.0638(16) Uani 1 1 d . B . H135 H 0.0598 0.8383 0.6055 0.077 Uiso 1 1 calc R . . C136 C 0.2643(5) 0.8042(3) 0.60820(19) 0.0515(14) Uani 1 1 d . . . H136 H 0.2896 0.7991 0.5749 0.062 Uiso 1 1 calc R B . C137 C 0.6343(5) 0.8261(3) 0.67283(16) 0.0404(12) Uani 1 1 d . . . C138 C 0.6440(5) 0.7682(3) 0.71679(16) 0.0445(12) Uani 1 1 d . B . C139 C 0.6711(5) 0.8076(3) 0.75684(17) 0.0478(13) Uani 1 1 d . . . H139 H 0.6776 0.7709 0.7859 0.057 Uiso 1 1 calc R B . C140 C 0.6887(5) 0.8997(4) 0.75462(18) 0.0522(14) Uani 1 1 d . B . H140 H 0.7053 0.9247 0.7821 0.063 Uiso 1 1 calc R . . C141 C 0.6817(5) 0.9548(4) 0.71139(18) 0.0510(14) Uani 1 1 d . . . H141 H 0.6947 1.0169 0.7101 0.061 Uiso 1 1 calc R B . C142 C 0.6557(5) 0.9198(3) 0.66990(16) 0.0441(12) Uani 1 1 d . B . C143 C 0.6351(6) 0.6655(3) 0.71831(18) 0.0507(14) Uani 1 1 d . . . H143 H 0.5729 0.6550 0.6955 0.061 Uiso 1 1 calc R B . C144 C 0.5760(7) 0.6191(4) 0.7681(2) 0.0672(19) Uani 1 1 d . B . H14C H 0.5730 0.5548 0.7663 0.101 Uiso 1 1 calc R . . H14D H 0.4840 0.6442 0.7780 0.101 Uiso 1 1 calc R . . H14E H 0.6337 0.6291 0.7916 0.101 Uiso 1 1 calc R . . C145 C 0.7768(7) 0.6231(4) 0.6996(2) 0.0731(18) Uani 1 1 d . B . H14F H 0.7712 0.5583 0.7006 0.110 Uiso 1 1 calc R . . H14G H 0.8420 0.6357 0.7200 0.110 Uiso 1 1 calc R . . H14H H 0.8068 0.6485 0.6666 0.110 Uiso 1 1 calc R . . C146 C 0.6504(6) 0.9799(3) 0.62252(18) 0.0552(15) Uani 1 1 d D . . H146 H 0.6667 0.9403 0.5960 0.066 Uiso 1 1 calc R B 15 C47A C 0.7647(9) 1.0486(6) 0.6124(3) 0.072(2) Uiso 0.721(6) 1 d PD B 15 H47D H 0.8534 1.0164 0.6121 0.108 Uiso 0.721(6) 1 calc PR B 15 H47E H 0.7509 1.0890 0.6375 0.108 Uiso 0.721(6) 1 calc PR B 15 H47F H 0.7613 1.0832 0.5812 0.108 Uiso 0.721(6) 1 calc PR B 15 C48A C 0.5088(9) 1.0236(6) 0.6230(3) 0.075(2) Uiso 0.721(6) 1 d PD B 15 H48D H 0.5047 1.0614 0.5928 0.112 Uiso 0.721(6) 1 calc PR B 15 H48E H 0.4876 1.0603 0.6498 0.112 Uiso 0.721(6) 1 calc PR B 15 H48F H 0.4427 0.9772 0.6268 0.112 Uiso 0.721(6) 1 calc PR B 15 C48B C 0.7911(18) 0.9814(16) 0.5911(7) 0.075(2) Uiso 0.279(6) 1 d PD B 16 H48G H 0.7853 1.0194 0.5610 0.112 Uiso 0.279(6) 1 calc PR B 16 H48H H 0.8216 0.9205 0.5841 0.112 Uiso 0.279(6) 1 calc PR B 16 H48I H 0.8559 1.0054 0.6081 0.112 Uiso 0.279(6) 1 calc PR B 16 C47B C 0.590(2) 1.0795(10) 0.6284(8) 0.072(2) Uiso 0.279(6) 1 d PD B 16 H47G H 0.5910 1.1129 0.5967 0.108 Uiso 0.279(6) 1 calc PR B 16 H47H H 0.6465 1.1089 0.6467 0.108 Uiso 0.279(6) 1 calc PR B 16 H47I H 0.4972 1.0780 0.6456 0.108 Uiso 0.279(6) 1 calc PR B 16 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 Ni1 0.0350(6) 0.0430(5) 0.0231(4) -0.0047(4) 0.0010(4) -0.0156(4) Ni2 0.0448(6) 0.0402(5) 0.0236(4) -0.0090(4) 0.0069(4) -0.0190(5) N1 0.035(2) 0.040(2) 0.0262(18) -0.0024(16) -0.0002(17) -0.0080(18) N2 0.037(2) 0.040(2) 0.0250(17) -0.0095(16) 0.0049(17) -0.0068(18) N3 0.045(3) 0.054(2) 0.0203(17) -0.0114(17) 0.0047(18) -0.013(2) N4 0.035(2) 0.044(2) 0.0296(18) -0.0047(16) -0.0004(16) -0.0044(19) N11 0.040(3) 0.041(2) 0.0224(17) -0.0086(16) 0.0068(17) -0.0135(19) N12 0.042(3) 0.038(2) 0.0249(17) -0.0085(15) 0.0037(17) -0.0139(19) N13 0.049(3) 0.046(2) 0.0292(19) -0.0123(17) 0.0028(19) -0.017(2) N14 0.040(2) 0.049(2) 0.0363(19) -0.0174(17) 0.0020(17) -0.0109(19) C1 0.036(3) 0.041(2) 0.028(2) -0.0046(19) 0.003(2) -0.015(2) C2 0.029(3) 0.042(3) 0.027(2) -0.0024(19) -0.0034(19) -0.008(2) C3 0.027(2) 0.043(2) 0.025(2) -0.0030(18) 0.0001(18) -0.009(2) C17 0.060(4) 0.058(3) 0.020(2) -0.009(2) 0.009(2) -0.036(3) C18 0.038(4) 0.108(5) 0.046(3) -0.036(3) 0.012(3) -0.032(3) C19 0.060(4) 0.120(6) 0.059(4) -0.049(4) 0.024(3) -0.047(4) C20 0.117(6) 0.082(5) 0.040(3) -0.029(3) 0.029(4) -0.059(5) C21 0.155(8) 0.058(4) 0.027(3) -0.002(3) -0.007(3) -0.048(5) C22 0.110(5) 0.046(3) 0.028(2) -0.005(2) -0.009(3) -0.039(3) C29 0.030(3) 0.038(2) 0.027(2) -0.0005(18) -0.0028(19) -0.014(2) C30 0.041(3) 0.039(2) 0.030(2) -0.0052(18) -0.0050(19) -0.008(2) C31 0.048(3) 0.044(3) 0.039(2) -0.008(2) -0.008(2) -0.002(2) C32 0.067(4) 0.057(3) 0.054(3) -0.006(3) -0.023(3) 0.012(3) C33 0.079(5) 0.057(3) 0.040(3) -0.004(2) -0.017(3) 0.005(3) C34 0.067(4) 0.046(3) 0.038(2) -0.003(2) -0.007(3) -0.010(3) C35 0.048(3) 0.046(3) 0.029(2) -0.0049(19) -0.003(2) -0.007(2) C36 0.034(3) 0.051(3) 0.029(2) -0.003(2) 0.0001(19) 0.000(2) C37 0.036(3) 0.072(4) 0.040(3) -0.001(2) 0.002(2) 0.005(3) C38 0.040(3) 0.104(5) 0.048(3) -0.002(3) 0.004(3) 0.010(3) C40 0.048(4) 0.077(4) 0.044(3) -0.014(3) 0.006(3) 0.017(3) C41 0.059(4) 0.053(3) 0.045(3) -0.014(2) -0.004(3) 0.005(3) C42 0.034(3) 0.040(2) 0.040(2) -0.0030(19) 0.002(2) 0.001(2) C46 0.043(3) 0.038(2) 0.047(3) -0.014(2) -0.002(2) -0.005(2) C47 0.041(3) 0.054(3) 0.065(3) -0.011(3) -0.013(3) -0.004(3) C48 0.062(4) 0.057(3) 0.056(3) -0.008(3) 0.002(3) -0.017(3) C101 0.027(3) 0.038(2) 0.035(2) -0.0098(19) 0.0025(19) -0.011(2) C102 0.040(3) 0.040(3) 0.025(2) -0.0068(19) 0.006(2) -0.015(2) C103 0.036(3) 0.036(2) 0.029(2) -0.0069(18) 0.002(2) -0.012(2) C110 0.039(3) 0.049(3) 0.023(2) -0.0071(19) -0.0007(19) -0.014(2) C117 0.062(4) 0.051(3) 0.023(2) -0.010(2) 0.009(2) -0.031(3) C118 0.047(4) 0.058(3) 0.037(3) -0.016(2) 0.010(3) -0.021(3) C119 0.053(4) 0.064(3) 0.042(3) -0.019(2) 0.013(3) -0.027(3) C120 0.079(4) 0.048(3) 0.034(3) -0.009(2) 0.007(3) -0.026(3) C121 0.093(5) 0.048(3) 0.024(2) 0.000(2) -0.007(3) -0.024(3) C122 0.065(4) 0.041(3) 0.038(3) -0.005(2) 0.004(3) -0.018(3) C123 0.033(3) 0.099(5) 0.054(3) -0.032(3) -0.006(2) -0.015(3) C124 0.041(4) 0.127(6) 0.097(5) -0.035(4) -0.012(3) -0.029(4) C125 0.043(3) 0.101(5) 0.060(3) -0.004(3) -0.016(3) -0.012(3) C127 0.105(6) 0.059(4) 0.031(3) 0.008(2) -0.013(3) -0.017(4) C128 0.071(5) 0.098(6) 0.125(6) 0.003(5) -0.028(5) -0.007(5) C129 0.164(9) 0.088(5) 0.054(4) 0.024(4) 0.001(5) 0.005(5) C130 0.036(3) 0.036(2) 0.035(2) -0.0086(19) 0.002(2) -0.009(2) C131 0.037(3) 0.039(3) 0.043(3) -0.012(2) 0.004(2) -0.010(2) C132 0.045(3) 0.069(3) 0.047(3) -0.028(3) 0.010(2) -0.022(3) C133 0.050(4) 0.069(4) 0.066(3) -0.031(3) 0.018(3) -0.017(3) C134 0.042(4) 0.064(4) 0.083(4) -0.029(3) 0.013(3) -0.006(3) C135 0.035(3) 0.076(4) 0.080(4) -0.012(3) -0.005(3) -0.005(3) C136 0.044(3) 0.054(3) 0.053(3) -0.010(2) 0.008(3) -0.011(3) C137 0.029(3) 0.051(3) 0.043(2) -0.021(2) 0.007(2) -0.010(2) C138 0.038(3) 0.054(3) 0.042(3) -0.015(2) 0.001(2) -0.007(2) C139 0.045(3) 0.060(3) 0.041(2) -0.014(2) -0.006(2) -0.006(3) C140 0.047(3) 0.064(3) 0.051(3) -0.028(3) -0.003(2) -0.014(3) C141 0.041(3) 0.060(3) 0.054(3) -0.024(3) 0.005(2) -0.014(3) C142 0.039(3) 0.051(3) 0.043(3) -0.018(2) 0.003(2) -0.009(2) C143 0.052(3) 0.057(3) 0.045(3) -0.013(2) -0.004(2) -0.009(3) C144 0.090(5) 0.056(4) 0.054(3) 0.001(3) -0.002(3) -0.022(4) C145 0.072(5) 0.067(4) 0.079(4) -0.021(3) -0.005(4) 0.009(3) C146 0.063(4) 0.052(3) 0.052(3) -0.019(2) 0.001(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.890(4) . ? Ni1 N1 1.891(4) 2_767 ? Ni1 N3 1.936(4) 2_767 ? Ni1 N3 1.937(4) . ? Ni2 N11 1.885(3) 2_666 ? Ni2 N11 1.885(4) . ? Ni2 N13 1.939(4) . ? Ni2 N13 1.939(4) 2_666 ? N1 N2 1.347(5) . ? N1 C2 1.375(5) . ? N2 C3 1.356(5) . ? N3 C10 1.311(6) . ? N3 C17 1.449(5) . ? N4 C29 1.281(6) . ? N4 C36 1.428(5) . ? N11 N12 1.349(5) . ? N11 C102 1.378(5) . ? N12 C103 1.356(5) . ? N13 C110 1.314(5) . ? N13 C117 1.448(5) . ? N14 C130 1.282(6) . ? N14 C137 1.418(5) . ? C1 C2 1.401(6) . ? C1 C3 1.401(5) . ? C1 C4B 1.482(5) . ? C1 C4A 1.558(6) . ? C2 C10 1.441(6) . ? C3 C29 1.488(6) . ? C4A C5A 1.3900 . ? C4A C9A 1.3900 . ? C5A C6A 1.3900 . ? C6A C7A 1.3900 . ? C7A C8A 1.3900 . ? C8A C9A 1.3900 . ? C4B C5B 1.3900 . ? C4B C9B 1.3900 . ? C5B C6B 1.3900 . ? C6B C7B 1.3900 . ? C7B C8B 1.3900 . ? C8B C9B 1.3900 . ? C10 C11A 1.469(5) . ? C10 C11B 1.501(6) . ? C11A C12A 1.3900 . ? C11A C16A 1.3900 . ? C12A C13A 1.3900 . ? C13A C14A 1.3900 . ? C14A C15A 1.3900 . ? C15A C16A 1.3900 . ? C11B C12B 1.3900 . ? C11B C16B 1.3900 . ? C12B C13B 1.3900 . ? C13B C14B 1.3900 . ? C14B C15B 1.3900 . ? C15B C16B 1.3900 . ? C17 C18 1.399(9) . ? C17 C22 1.410(8) . ? C18 C19 1.392(7) . ? C18 C23B 1.412(12) . ? C18 C23A 1.606(11) . ? C19 C20 1.370(10) . ? C20 C21 1.379(10) . ? C21 C22 1.403(7) . ? C22 C26B 1.373(13) . ? C22 C26A 1.605(13) . ? C23A C25A 1.549(11) . ? C23A C24A 1.560(11) . ? C23B C25B 1.504(13) . ? C23B C24B 1.515(13) . ? C26A C28A 1.539(12) . ? C26A C27A 1.573(12) . ? C26B C27B 1.507(12) . ? C26B C28B 1.538(13) . ? C29 C30 1.491(6) . ? C30 C31 1.386(7) . ? C30 C35 1.407(5) . ? C31 C32 1.381(7) . ? C32 C33 1.387(7) . ? C33 C34 1.368(8) . ? C34 C35 1.390(7) . ? C36 C42 1.399(6) . ? C36 C37 1.419(7) . ? C37 C38 1.400(7) . ? C37 C43B 1.435(13) . ? C37 C43A 1.562(11) . ? C38 C40 1.384(8) . ? C40 C41 1.375(8) . ? C41 C42 1.408(6) . ? C42 C46 1.517(7) . ? C43A C45A 1.536(10) . ? C43A C44A 1.661(12) . ? C43B C44B 1.547(14) . ? C43B C45B 1.577(13) . ? C46 C47 1.524(7) . ? C46 C48 1.537(6) . ? C101 C102 1.388(6) . ? C101 C103 1.399(5) . ? C101 C51B 1.449(9) . ? C101 C51A 1.483(5) . ? C102 C110 1.429(6) . ? C103 C130 1.493(6) . ? C51A C52A 1.3900 . ? C51A C56A 1.3900 . ? C52A C53A 1.3900 . ? C53A C54A 1.3900 . ? C54A C55A 1.3900 . ? C55A C56A 1.3900 . ? C51B C52B 1.3900 . ? C51B C56B 1.3900 . ? C52B C53B 1.3900 . ? C53B C54B 1.3900 . ? C54B C55B 1.3900 . ? C55B C56B 1.3900 . ? C110 C31B 1.459(8) . ? C110 C31A 1.498(5) . ? C31A C32A 1.3900 . ? C31A C36A 1.3900 . ? C32A C33A 1.3900 . ? C33A C34A 1.3900 . ? C34A C35A 1.3900 . ? C35A C36A 1.3900 . ? C31B C32B 1.3900 . ? C31B C36B 1.3900 . ? C32B C33B 1.3900 . ? C33B C34B 1.3900 . ? C34B C35B 1.3900 . ? C35B C36B 1.3900 . ? C117 C122 1.390(8) . ? C117 C118 1.400(8) . ? C118 C119 1.387(6) . ? C118 C123 1.543(8) . ? C119 C120 1.379(8) . ? C120 C121 1.366(8) . ? C121 C122 1.394(7) . ? C122 C127 1.505(9) . ? C123 C125 1.525(8) . ? C123 C124 1.537(8) . ? C127 C129 1.537(7) . ? C127 C128 1.546(9) . ? C130 C131 1.498(6) . ? C131 C136 1.375(7) . ? C131 C132 1.396(6) . ? C132 C133 1.407(7) . ? C133 C134 1.358(8) . ? C134 C135 1.376(8) . ? C135 C136 1.409(7) . ? C137 C142 1.404(6) . ? C137 C138 1.422(7) . ? C138 C139 1.386(6) . ? C138 C143 1.520(7) . ? C139 C140 1.375(7) . ? C140 C141 1.381(7) . ? C141 C142 1.385(6) . ? C142 C146 1.508(7) . ? C143 C144 1.517(7) . ? C143 C145 1.520(8) . ? C146 C48A 1.487(9) . ? C146 C48B 1.508(14) . ? C146 C47A 1.532(8) . ? C146 C47B 1.562(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 179.999(1) . 2_767 ? N1 Ni1 N3 98.23(15) . 2_767 ? N1 Ni1 N3 81.77(15) 2_767 2_767 ? N1 Ni1 N3 81.77(15) . . ? N1 Ni1 N3 98.23(15) 2_767 . ? N3 Ni1 N3 179.998(1) 2_767 . ? N11 Ni2 N11 180.00(17) 2_666 . ? N11 Ni2 N13 97.96(14) 2_666 . ? N11 Ni2 N13 82.05(14) . . ? N11 Ni2 N13 82.05(14) 2_666 2_666 ? N11 Ni2 N13 97.95(14) . 2_666 ? N13 Ni2 N13 179.998(1) . 2_666 ? N2 N1 C2 109.3(3) . . ? N2 N1 Ni1 135.5(3) . . ? C2 N1 Ni1 115.1(3) . . ? N1 N2 C3 106.6(3) . . ? C10 N3 C17 119.5(4) . . ? C10 N3 Ni1 116.3(3) . . ? C17 N3 Ni1 124.2(3) . . ? C29 N4 C36 123.4(4) . . ? N12 N11 C102 109.3(3) . . ? N12 N11 Ni2 135.4(3) . . ? C102 N11 Ni2 115.3(3) . . ? N11 N12 C103 106.3(3) . . ? C110 N13 C117 119.6(4) . . ? C110 N13 Ni2 115.3(3) . . ? C117 N13 Ni2 125.1(3) . . ? C130 N14 C137 126.4(4) . . ? C2 C1 C3 102.8(4) . . ? C2 C1 C4B 125.9(4) . . ? C3 C1 C4B 128.6(4) . . ? C2 C1 C4A 128.1(4) . . ? C3 C1 C4A 127.8(4) . . ? N1 C2 C1 109.3(3) . . ? N1 C2 C10 113.3(4) . . ? C1 C2 C10 137.4(4) . . ? N2 C3 C1 111.9(4) . . ? N2 C3 C29 117.2(3) . . ? C1 C3 C29 130.8(4) . . ? C5A C4A C9A 120.0 . . ? C5A C4A C1 122.0(4) . . ? C9A C4A C1 117.5(4) . . ? C4A C5A C6A 120.0 . . ? C5A C6A C7A 120.0 . . ? C8A C7A C6A 120.0 . . ? C7A C8A C9A 120.0 . . ? C8A C9A C4A 120.0 . . ? C5B C4B C9B 120.0 . . ? C5B C4B C1 115.3(4) . . ? C9B C4B C1 124.5(4) . . ? C4B C5B C6B 120.0 . . ? C7B C6B C5B 120.0 . . ? C6B C7B C8B 120.0 . . ? C7B C8B C9B 120.0 . . ? C8B C9B C4B 120.0 . . ? N3 C10 C2 113.3(4) . . ? N3 C10 C11A 122.9(4) . . ? C2 C10 C11A 123.8(4) . . ? N3 C10 C11B 128.1(4) . . ? C2 C10 C11B 118.5(4) . . ? C12A C11A C16A 120.0 . . ? C12A C11A C10 125.8(4) . . ? C16A C11A C10 114.1(4) . . ? C11A C12A C13A 120.0 . . ? C14A C13A C12A 120.0 . . ? C15A C14A C13A 120.0 . . ? C14A C15A C16A 120.0 . . ? C15A C16A C11A 120.0 . . ? C12B C11B C16B 120.0 . . ? C12B C11B C10 113.8(5) . . ? C16B C11B C10 126.1(5) . . ? C11B C12B C13B 120.0 . . ? C14B C13B C12B 120.0 . . ? C13B C14B C15B 120.0 . . ? C16B C15B C14B 120.0 . . ? C15B C16B C11B 120.0 . . ? C18 C17 C22 123.7(5) . . ? C18 C17 N3 118.3(5) . . ? C22 C17 N3 117.7(5) . . ? C19 C18 C17 117.6(6) . . ? C19 C18 C23B 124.5(8) . . ? C17 C18 C23B 116.0(7) . . ? C19 C18 C23A 116.6(7) . . ? C17 C18 C23A 125.0(5) . . ? C20 C19 C18 120.2(7) . . ? C19 C20 C21 121.7(6) . . ? C20 C21 C22 121.2(7) . . ? C26B C22 C21 119.1(8) . . ? C26B C22 C17 125.0(7) . . ? C21 C22 C17 115.6(7) . . ? C21 C22 C26A 123.1(7) . . ? C17 C22 C26A 120.9(6) . . ? C25A C23A C24A 105.0(9) . . ? C25A C23A C18 116.3(8) . . ? C24A C23A C18 117.4(8) . . ? C18 C23B C25B 112.5(10) . . ? C18 C23B C24B 99.3(9) . . ? C25B C23B C24B 115.2(12) . . ? C28A C26A C27A 104.8(10) . . ? C28A C26A C22 118.7(9) . . ? C27A C26A C22 115.6(9) . . ? C22 C26B C27B 109.9(10) . . ? C22 C26B C28B 103.1(10) . . ? C27B C26B C28B 116.7(11) . . ? N4 C29 C3 117.2(4) . . ? N4 C29 C30 126.5(4) . . ? C3 C29 C30 116.3(4) . . ? C31 C30 C35 117.9(4) . . ? C31 C30 C29 119.4(4) . . ? C35 C30 C29 122.7(4) . . ? C32 C31 C30 121.4(5) . . ? C31 C32 C33 120.3(6) . . ? C34 C33 C32 119.1(5) . . ? C33 C34 C35 121.2(5) . . ? C34 C35 C30 120.1(5) . . ? C42 C36 C37 121.1(4) . . ? C42 C36 N4 122.3(4) . . ? C37 C36 N4 116.3(4) . . ? C38 C37 C36 117.4(5) . . ? C38 C37 C43B 114.4(10) . . ? C36 C37 C43B 128.0(9) . . ? C38 C37 C43A 125.8(7) . . ? C36 C37 C43A 116.7(6) . . ? C40 C38 C37 122.2(5) . . ? C41 C40 C38 119.2(5) . . ? C40 C41 C42 121.6(5) . . ? C36 C42 C41 118.4(4) . . ? C36 C42 C46 123.2(4) . . ? C41 C42 C46 118.4(4) . . ? C45A C43A C37 113.5(8) . . ? C45A C43A C44A 97.5(9) . . ? C37 C43A C44A 98.7(7) . . ? C37 C43B C44B 121.3(12) . . ? C37 C43B C45B 105.2(11) . . ? C44B C43B C45B 133.3(14) . . ? C42 C46 C47 112.0(4) . . ? C42 C46 C48 109.5(4) . . ? C47 C46 C48 112.0(4) . . ? C102 C101 C103 103.1(4) . . ? C102 C101 C51B 128.5(7) . . ? C103 C101 C51B 128.4(7) . . ? C102 C101 C51A 126.6(4) . . ? C103 C101 C51A 130.2(4) . . ? N11 C102 C101 109.4(3) . . ? N11 C102 C110 113.0(4) . . ? C101 C102 C110 137.6(4) . . ? N12 C103 C101 111.9(4) . . ? N12 C103 C130 118.8(3) . . ? C101 C103 C130 128.8(4) . . ? C52A C51A C56A 120.0 . . ? C52A C51A C101 119.6(4) . . ? C56A C51A C101 120.1(4) . . ? C53A C52A C51A 120.0 . . ? C52A C53A C54A 120.0 . . ? C55A C54A C53A 120.0 . . ? C56A C55A C54A 120.0 . . ? C55A C56A C51A 120.0 . . ? C52B C51B C56B 120.0 . . ? C52B C51B C101 120.9(11) . . ? C56B C51B C101 118.7(11) . . ? C51B C52B C53B 120.0 . . ? C52B C53B C54B 120.0 . . ? C53B C54B C55B 120.0 . . ? C56B C55B C54B 120.0 . . ? C55B C56B C51B 120.0 . . ? N13 C110 C102 114.4(4) . . ? N13 C110 C31B 127.3(6) . . ? C102 C110 C31B 118.1(6) . . ? N13 C110 C31A 123.4(4) . . ? C102 C110 C31A 122.2(4) . . ? C32A C31A C36A 120.0 . . ? C32A C31A C110 124.0(4) . . ? C36A C31A C110 115.9(4) . . ? C33A C32A C31A 120.0 . . ? C32A C33A C34A 120.0 . . ? C35A C34A C33A 120.0 . . ? C34A C35A C36A 120.0 . . ? C35A C36A C31A 120.0 . . ? C32B C31B C36B 120.0 . . ? C32B C31B C110 112.6(8) . . ? C36B C31B C110 127.4(8) . . ? C31B C32B C33B 120.0 . . ? C34B C33B C32B 120.0 . . ? C33B C34B C35B 120.0 . . ? C36B C35B C34B 120.0 . . ? C35B C36B C31B 120.0 . . ? C122 C117 C118 123.0(4) . . ? C122 C117 N13 118.7(5) . . ? C118 C117 N13 118.1(5) . . ? C119 C118 C117 117.0(5) . . ? C119 C118 C123 120.5(6) . . ? C117 C118 C123 122.5(4) . . ? C120 C119 C118 121.0(6) . . ? C121 C120 C119 120.7(5) . . ? C120 C121 C122 120.9(5) . . ? C117 C122 C121 117.3(6) . . ? C117 C122 C127 122.0(5) . . ? C121 C122 C127 120.8(6) . . ? C125 C123 C124 110.3(6) . . ? C125 C123 C118 111.6(4) . . ? C124 C123 C118 111.9(5) . . ? C122 C127 C129 115.0(5) . . ? C122 C127 C128 111.9(5) . . ? C129 C127 C128 108.6(6) . . ? N14 C130 C103 114.2(4) . . ? N14 C130 C131 128.8(4) . . ? C103 C130 C131 117.0(4) . . ? C136 C131 C132 118.4(5) . . ? C136 C131 C130 118.8(4) . . ? C132 C131 C130 122.8(5) . . ? C131 C132 C133 119.3(6) . . ? C134 C133 C132 121.7(5) . . ? C133 C134 C135 119.6(5) . . ? C134 C135 C136 119.4(6) . . ? C131 C136 C135 121.6(5) . . ? C142 C137 N14 120.6(4) . . ? C142 C137 C138 120.8(4) . . ? N14 C137 C138 118.0(4) . . ? C139 C138 C137 117.8(4) . . ? C139 C138 C143 121.4(5) . . ? C137 C138 C143 120.6(4) . . ? C140 C139 C138 121.7(5) . . ? C139 C140 C141 119.8(4) . . ? C140 C141 C142 121.5(5) . . ? C141 C142 C137 118.3(5) . . ? C141 C142 C146 121.4(4) . . ? C137 C142 C146 120.3(4) . . ? C144 C143 C138 114.1(4) . . ? C144 C143 C145 111.2(5) . . ? C138 C143 C145 109.4(4) . . ? C48A C146 C48B 139.9(11) . . ? C48A C146 C142 109.2(5) . . ? C48B C146 C142 110.8(10) . . ? C48A C146 C47A 113.4(6) . . ? C48B C146 C47A 46.7(9) . . ? C142 C146 C47A 111.8(5) . . ? C48A C146 C47B 47.4(9) . . ? C48B C146 C47B 110.1(13) . . ? C142 C146 C47B 114.9(9) . . ? C47A C146 C47B 68.2(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.360 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.054 # start Validation Reply Form _vrf_PLAT201_8-as33 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 36 RESPONSE: Atoms of the disordered parts were refined isotropically (see article for details). ;