Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;'Pincer' pyridine dicarbene complexes of nickel and their derivatives. Unusual ring opening of a coordinated imidazol-2-ylidene ; _publ_requested_category FO _publ_contact_author_name 'Andreas Danopoulos' _publ_contact_author_email AD1@SOTON.AC.UK loop_ _publ_author_name 'Andreas Danopoulos' 'Aimee Boyle' 'David Pugh' # Attachment 'CombinedCIF.cif' data_1MeBr2 _database_code_depnum_ccdc_archive 'CCDC 663954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H47 N5, 2(Br)' _chemical_formula_sum 'C37 H47 Br2 N5' _chemical_formula_weight 721.62 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 52.1838(13) _cell_length_b 52.1838(13) _cell_length_c 9.4150(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 22203.5(11) _cell_formula_units_Z 18 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 64208 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6732 _exptl_absorpt_coefficient_mu 1.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6805 _exptl_absorpt_correction_T_max 0.7217 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60773 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -62 _diffrn_reflns_limit_h_max 62 _diffrn_reflns_limit_k_min -61 _diffrn_reflns_limit_k_max 62 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8591 _reflns_number_gt 5739 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains highly disordered molecules of DCM and Et2O - attempts to satisfactorily model this failed. As a result it was removed using the squeeze algorithm ( P. v.d. Sluis and A. L. Spek, Acta Crystallogr., Sect A 1990, 46, 194-201.). This treatment explains the following checkCIF alerts: PLAT602_ALERT_4_C, PLAT601_ALERT_2_A. ; _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^)+(0.1778P)^2^+188.3305P] 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 8591 _refine_ls_number_parameters 407 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.3094 _refine_ls_wR_factor_gt 0.2847 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3621(2) 0.0679(2) 0.8788(10) 0.064(2) Uani 1 1 d . . . C2 C 0.3651(2) 0.0431(2) 0.8513(10) 0.063(2) Uani 1 1 d . . . C3 C 0.3396(2) 0.0156(2) 0.8667(11) 0.070(3) Uani 1 1 d . . . H3 H 0.3401 -0.0020 0.8482 0.084 Uiso 1 1 calc R . . C4 C 0.3131(2) 0.0142(2) 0.9101(11) 0.072(3) Uani 1 1 d . . . H4 H 0.2958 -0.0047 0.9192 0.086 Uiso 1 1 calc R . . C5 C 0.3112(3) 0.0390(2) 0.9399(12) 0.084(3) Uani 1 1 d . . . H5 H 0.2931 0.0373 0.9721 0.101 Uiso 1 1 calc R . . C6 C 0.3365(2) 0.0670(3) 0.9216(11) 0.079(3) Uani 1 1 d . . . C7 C 0.3941(2) 0.0451(2) 0.8025(11) 0.066(3) Uani 1 1 d . . . H7 H 0.4108 0.0646 0.8351 0.079 Uiso 1 1 calc R . . C8 C 0.3996(4) 0.0211(4) 0.8592(18) 0.144(6) Uani 1 1 d U . . H8A H 0.3838 0.0017 0.8265 0.217 Uiso 1 1 calc R . . H8B H 0.3997 0.0216 0.9632 0.217 Uiso 1 1 calc R . . H8C H 0.4187 0.0244 0.8245 0.217 Uiso 1 1 calc R . . C9 C 0.3964(3) 0.0436(3) 0.6472(12) 0.092(3) Uani 1 1 d . . . H9A H 0.4157 0.0459 0.6227 0.138 Uiso 1 1 calc R . . H9B H 0.3944 0.0595 0.6026 0.138 Uiso 1 1 calc R . . H9C H 0.3807 0.0244 0.6128 0.138 Uiso 1 1 calc R . . C10 C 0.3344(2) 0.0951(2) 0.9506(11) 0.077(3) Uani 1 1 d . . . H10 H 0.3540 0.1127 0.9266 0.093 Uiso 1 1 calc R . . C11 C 0.3108(4) 0.0956(3) 0.8546(15) 0.124(5) Uani 1 1 d . . . H11A H 0.3148 0.0932 0.7553 0.186 Uiso 1 1 calc R . . H11B H 0.3113 0.1145 0.8659 0.186 Uiso 1 1 calc R . . H11C H 0.2912 0.0794 0.8815 0.186 Uiso 1 1 calc R . . C12 C 0.3281(3) 0.0973(3) 1.1062(13) 0.091(3) Uani 1 1 d . . . H12A H 0.3208 0.1112 1.1169 0.136 Uiso 1 1 calc R . . H12B H 0.3463 0.1042 1.1614 0.136 Uiso 1 1 calc R . . H12C H 0.3131 0.0777 1.1407 0.136 Uiso 1 1 calc R . . C13 C 0.4097(2) 0.1109(2) 0.9642(10) 0.062(2) Uani 1 1 d . . . H13 H 0.4088 0.1047 1.0599 0.075 Uiso 1 1 calc R . . C14 C 0.3984(2) 0.1125(2) 0.7371(10) 0.063(2) Uani 1 1 d . . . H14 H 0.3881 0.1071 0.6491 0.075 Uiso 1 1 calc R . . C15 C 0.4245(2) 0.1370(2) 0.7634(10) 0.065(2) Uani 1 1 d . . . H15 H 0.4358 0.1525 0.6979 0.078 Uiso 1 1 calc R . . C16 C 0.4580(2) 0.1575(2) 0.9762(9) 0.057(2) Uani 1 1 d . . . C17 C 0.47355(19) 0.15044(19) 1.0672(10) 0.059(2) Uani 1 1 d . . . C18 C 0.4984(2) 0.1740(2) 1.1329(11) 0.066(2) Uani 1 1 d . . . H18 H 0.5102 0.1701 1.1965 0.079 Uiso 1 1 calc R . . C19 C 0.5056(2) 0.20299(19) 1.1045(9) 0.057(2) Uani 1 1 d . . . C20 C 0.4875(2) 0.2067(2) 1.0070(10) 0.065(2) Uani 1 1 d . . . C21 C 0.4975(2) 0.25772(18) 1.0554(9) 0.055(2) Uani 1 1 d . . . H21 H 0.4991 0.2574 1.1558 0.066 Uiso 1 1 calc R . . C22 C 0.4911(2) 0.2441(2) 0.8301(10) 0.073(3) Uani 1 1 d . . . H22 H 0.4874 0.2327 0.7462 0.088 Uiso 1 1 calc R . . C23 C 0.4958(2) 0.2723(2) 0.8400(10) 0.061(2) Uani 1 1 d . . . H23 H 0.4964 0.2844 0.7634 0.073 Uiso 1 1 calc R . . C24 C 0.5047(2) 0.3081(2) 1.0428(10) 0.062(2) Uani 1 1 d . . . C25 C 0.4802(2) 0.3096(2) 1.0888(9) 0.059(2) Uani 1 1 d . . . C26 C 0.4862(3) 0.3358(2) 1.1498(11) 0.076(3) Uani 1 1 d . . . H26 H 0.4701 0.3376 1.1845 0.091 Uiso 1 1 calc R . . C27 C 0.5143(2) 0.3595(2) 1.1635(10) 0.071(3) Uani 1 1 d . . . H27 H 0.5173 0.3774 1.2055 0.086 Uiso 1 1 calc R . . C28 C 0.5379(2) 0.3571(2) 1.1156(11) 0.072(3) Uani 1 1 d . . . H28 H 0.5573 0.3735 1.1259 0.086 Uiso 1 1 calc R . . C29 C 0.5341(2) 0.3312(2) 1.0524(10) 0.063(2) Uani 1 1 d . . . C30 C 0.4492(2) 0.2838(2) 1.0712(11) 0.074(3) Uani 1 1 d . . . H30 H 0.4509 0.2659 1.0509 0.089 Uiso 1 1 calc R . . C31 C 0.4302(3) 0.2773(3) 1.2145(14) 0.113(5) Uani 1 1 d . . . H31A H 0.4238 0.2920 1.2249 0.170 Uiso 1 1 calc R . . H31B H 0.4424 0.2785 1.2963 0.170 Uiso 1 1 calc R . . H31C H 0.4127 0.2575 1.2098 0.170 Uiso 1 1 calc R . . C32 C 0.4331(3) 0.2874(4) 0.9517(14) 0.126(5) Uani 1 1 d . . . H32A H 0.4291 0.3035 0.9730 0.189 Uiso 1 1 calc R . . H32B H 0.4144 0.2690 0.9371 0.189 Uiso 1 1 calc R . . H32C H 0.4451 0.2923 0.8653 0.189 Uiso 1 1 calc R . . C33 C 0.5606(2) 0.3284(2) 1.0124(11) 0.077(3) Uani 1 1 d . . . H33 H 0.5527 0.3088 0.9643 0.092 Uiso 1 1 calc R . . C34 C 0.5773(3) 0.3276(4) 1.1432(15) 0.120(5) Uani 1 1 d . . . H34A H 0.5848 0.3462 1.1958 0.179 Uiso 1 1 calc R . . H34B H 0.5938 0.3250 1.1140 0.179 Uiso 1 1 calc R . . H34C H 0.5639 0.3111 1.2042 0.179 Uiso 1 1 calc R . . C35 C 0.5793(4) 0.3524(3) 0.8994(16) 0.128(5) Uani 1 1 d U . . H35A H 0.5685 0.3474 0.8090 0.191 Uiso 1 1 calc R . . H35B H 0.5983 0.3532 0.8863 0.191 Uiso 1 1 calc R . . H35C H 0.5827 0.3718 0.9319 0.191 Uiso 1 1 calc R . . C36 C 0.4675(2) 0.1188(2) 1.0986(11) 0.076(3) Uani 1 1 d . . . H36A H 0.4860 0.1196 1.1242 0.114 Uiso 1 1 calc R . . H36B H 0.4591 0.1065 1.0139 0.114 Uiso 1 1 calc R . . H36C H 0.4534 0.1104 1.1775 0.114 Uiso 1 1 calc R . . C37 C 0.5331(2) 0.2286(2) 1.1763(11) 0.074(3) Uani 1 1 d . . . H37A H 0.5456 0.2212 1.2150 0.111 Uiso 1 1 calc R . . H37B H 0.5267 0.2368 1.2534 0.111 Uiso 1 1 calc R . . H37C H 0.5443 0.2441 1.1061 0.111 Uiso 1 1 calc R . . N1 N 0.38936(17) 0.09683(17) 0.8632(8) 0.063(2) Uani 1 1 d . . . N2 N 0.43193(17) 0.13561(16) 0.9036(8) 0.0626(19) Uani 1 1 d . . . N3 N 0.46432(16) 0.18482(16) 0.9406(8) 0.0586(18) Uani 1 1 d . . . N4 N 0.49290(16) 0.23569(16) 0.9675(8) 0.0597(19) Uani 1 1 d . . . N5 N 0.49947(17) 0.27971(16) 0.9807(8) 0.0618(19) Uani 1 1 d . . . Br1 Br 0.401022(16) 0.107129(16) 0.34771(7) 0.0410(3) Uani 1 1 d . . . Br2 Br 0.603730(19) 0.433577(19) 1.22224(8) 0.0639(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.061(6) 0.057(6) 0.069(6) 0.003(5) 0.004(5) 0.025(5) C2 0.066(6) 0.059(6) 0.065(6) 0.006(5) -0.002(5) 0.032(5) C3 0.062(6) 0.064(6) 0.080(7) 0.006(5) 0.008(5) 0.029(5) C4 0.071(7) 0.060(6) 0.078(7) 0.005(5) 0.003(5) 0.028(5) C5 0.083(8) 0.068(7) 0.084(8) 0.015(6) -0.008(6) 0.026(6) C6 0.062(6) 0.098(8) 0.075(7) 0.004(6) 0.007(5) 0.040(6) C7 0.060(6) 0.062(6) 0.081(7) 0.005(5) -0.005(5) 0.034(5) C8 0.144(6) 0.144(6) 0.145(6) 0.0004(10) 0.0000(10) 0.072(3) C9 0.094(8) 0.112(9) 0.081(8) 0.003(7) 0.005(6) 0.058(8) C10 0.088(7) 0.079(7) 0.076(7) 0.004(6) 0.013(6) 0.050(6) C11 0.190(16) 0.114(11) 0.111(11) 0.003(8) -0.024(10) 0.109(12) C12 0.090(8) 0.080(7) 0.111(10) -0.025(7) -0.015(7) 0.050(7) C13 0.058(5) 0.058(6) 0.059(6) -0.006(5) -0.009(5) 0.021(5) C14 0.059(6) 0.056(5) 0.059(6) 0.000(4) -0.013(4) 0.018(5) C15 0.065(6) 0.075(6) 0.058(6) 0.012(5) 0.002(5) 0.037(5) C16 0.066(6) 0.062(6) 0.045(5) -0.002(4) -0.009(4) 0.033(5) C17 0.053(5) 0.053(5) 0.064(6) 0.003(4) 0.008(4) 0.021(4) C18 0.060(6) 0.055(6) 0.080(7) 0.001(5) 0.001(5) 0.027(5) C19 0.063(5) 0.056(5) 0.047(5) -0.006(4) -0.006(4) 0.026(4) C20 0.072(6) 0.067(6) 0.064(6) 0.016(5) 0.012(5) 0.041(5) C21 0.083(6) 0.045(5) 0.031(4) -0.001(4) 0.009(4) 0.028(4) C22 0.094(8) 0.090(8) 0.041(5) -0.013(5) -0.009(5) 0.050(6) C23 0.078(6) 0.067(6) 0.046(5) -0.003(4) -0.004(4) 0.042(5) C24 0.067(6) 0.058(5) 0.057(6) -0.002(4) -0.002(5) 0.029(5) C25 0.068(6) 0.062(6) 0.053(5) -0.002(4) -0.007(4) 0.037(5) C26 0.084(8) 0.080(7) 0.077(7) 0.001(6) -0.002(6) 0.051(7) C27 0.084(8) 0.077(7) 0.067(7) 0.009(5) -0.001(5) 0.050(6) C28 0.082(7) 0.052(6) 0.074(7) 0.002(5) -0.015(5) 0.027(5) C29 0.065(6) 0.062(6) 0.061(6) 0.002(5) 0.011(5) 0.031(5) C30 0.066(6) 0.092(7) 0.067(7) 0.001(5) 0.003(5) 0.041(6) C31 0.081(8) 0.125(11) 0.124(11) 0.002(9) 0.041(8) 0.044(8) C32 0.074(8) 0.196(16) 0.104(10) 0.023(10) -0.020(7) 0.064(10) C33 0.063(6) 0.075(7) 0.074(7) 0.009(5) 0.006(5) 0.021(5) C34 0.106(10) 0.154(13) 0.107(10) -0.018(9) -0.032(8) 0.071(10) C35 0.128(5) 0.128(5) 0.128(5) 0.0002(10) 0.0004(10) 0.064(3) C36 0.084(7) 0.056(6) 0.087(7) 0.011(5) 0.007(6) 0.035(5) C37 0.064(6) 0.079(7) 0.069(7) -0.015(5) -0.005(5) 0.028(5) N1 0.059(5) 0.058(4) 0.058(5) 0.001(4) 0.007(4) 0.019(4) N2 0.067(5) 0.056(4) 0.057(5) 0.009(4) -0.002(4) 0.025(4) N3 0.055(4) 0.055(5) 0.063(5) -0.003(4) -0.001(4) 0.025(4) N4 0.062(5) 0.058(4) 0.061(5) 0.010(4) 0.003(4) 0.031(4) N5 0.073(5) 0.057(4) 0.056(5) 0.000(4) 0.000(4) 0.034(4) Br1 0.0437(5) 0.0493(5) 0.0295(5) -0.0027(3) 0.0000(3) 0.0227(4) Br2 0.0622(6) 0.0510(5) 0.0256(5) 0.0014(3) -0.0015(3) -0.0115(4) _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 C1 C6 1.375(13) . ? C1 C2 1.405(13) . ? C1 N1 1.474(11) . ? C2 C3 1.391(13) . ? C2 C7 1.536(13) . ? C3 C4 1.412(13) . ? C3 H3 0.9500 . ? C4 C5 1.376(15) . ? C4 H4 0.9500 . ? C5 C6 1.407(15) . ? C5 H5 0.9500 . ? C6 C10 1.547(15) . ? C7 C9 1.473(14) . ? C7 C8 1.513(18) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.518(14) . ? C10 C11 1.540(16) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.339(12) . ? C13 N2 1.356(11) . ? C13 H13 0.9500 . ? C14 C15 1.347(12) . ? C14 N1 1.385(11) . ? C14 H14 0.9500 . ? C15 N2 1.388(11) . ? C15 H15 0.9500 . ? C16 N3 1.335(11) . ? C16 C17 1.351(12) . ? C16 N2 1.440(11) . ? C17 C18 1.408(12) . ? C17 C36 1.545(12) . ? C18 C19 1.390(13) . ? C18 H18 0.9500 . ? C19 C20 1.400(13) . ? C19 C37 1.543(12) . ? C20 N3 1.332(12) . ? C20 N4 1.443(11) . ? C21 N5 1.306(11) . ? C21 N4 1.337(10) . ? C21 H21 0.9500 . ? C22 C23 1.365(13) . ? C22 N4 1.385(11) . ? C22 H22 0.9500 . ? C23 N5 1.367(11) . ? C23 H23 0.9500 . ? C24 C25 1.388(12) . ? C24 C29 1.401(13) . ? C24 N5 1.486(11) . ? C25 C26 1.369(13) . ? C25 C30 1.510(13) . ? C26 C27 1.371(14) . ? C26 H26 0.9500 . ? C27 C28 1.377(14) . ? C27 H27 0.9500 . ? C28 C29 1.396(13) . ? C28 H28 0.9500 . ? C29 C33 1.507(14) . ? C30 C32 1.473(14) . ? C30 C31 1.608(14) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.521(16) . ? C33 C35 1.559(17) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? 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 C6 C1 C2 125.2(9) . . ? C6 C1 N1 119.2(9) . . ? C2 C1 N1 115.6(8) . . ? C3 C2 C1 116.3(9) . . ? C3 C2 C7 120.2(8) . . ? C1 C2 C7 123.5(8) . . ? C2 C3 C4 119.4(9) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 122.7(10) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C4 C5 C6 118.7(11) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C1 C6 C5 117.6(11) . . ? C1 C6 C10 123.2(10) . . ? C5 C6 C10 119.2(10) . . ? C9 C7 C8 104.6(10) . . ? C9 C7 C2 113.4(8) . . ? C8 C7 C2 115.1(10) . . ? C9 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C2 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.1(10) . . ? C12 C10 C6 111.2(9) . . ? C11 C10 C6 110.4(9) . . ? C12 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? C6 C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 106.8(8) . . ? N1 C13 H13 126.6 . . ? N2 C13 H13 126.6 . . ? C15 C14 N1 106.7(8) . . ? C15 C14 H14 126.7 . . ? N1 C14 H14 126.7 . . ? C14 C15 N2 107.5(8) . . ? C14 C15 H15 126.2 . . ? N2 C15 H15 126.2 . . ? N3 C16 C17 126.2(8) . . ? N3 C16 N2 111.0(7) . . ? C17 C16 N2 122.8(8) . . ? C16 C17 C18 117.1(8) . . ? C16 C17 C36 125.6(9) . . ? C18 C17 C36 117.1(9) . . ? C19 C18 C17 119.8(9) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 116.2(8) . . ? C18 C19 C37 119.3(9) . . ? C20 C19 C37 124.5(8) . . ? N3 C20 C19 125.3(8) . . ? N3 C20 N4 113.3(8) . . ? C19 C20 N4 121.5(9) . . ? N5 C21 N4 108.9(7) . . ? N5 C21 H21 125.6 . . ? N4 C21 H21 125.6 . . ? C23 C22 N4 105.9(8) . . ? C23 C22 H22 127.0 . . ? N4 C22 H22 127.0 . . ? C22 C23 N5 107.2(8) . . ? C22 C23 H23 126.4 . . ? N5 C23 H23 126.4 . . ? C25 C24 C29 125.1(9) . . ? C25 C24 N5 117.4(8) . . ? C29 C24 N5 117.5(8) . . ? C26 C25 C24 115.4(9) . . ? C26 C25 C30 123.0(9) . . ? C24 C25 C30 121.7(8) . . ? C25 C26 C27 123.4(10) . . ? C25 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? C26 C27 C28 119.0(10) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C27 C28 C29 122.0(10) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C24 115.1(9) . . ? C28 C29 C33 120.5(9) . . ? C24 C29 C33 124.1(9) . . ? C32 C30 C25 113.3(10) . . ? C32 C30 C31 109.7(10) . . ? C25 C30 C31 111.7(9) . . ? C32 C30 H30 107.3 . . ? C25 C30 H30 107.3 . . ? C31 C30 H30 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C34 111.4(9) . . ? C29 C33 C35 109.1(10) . . ? C34 C33 C35 116.0(10) . . ? C29 C33 H33 106.6 . . ? C34 C33 H33 106.6 . . ? C35 C33 H33 106.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C19 C37 H37A 109.5 . . ? C19 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C19 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C13 N1 C14 110.1(8) . . ? C13 N1 C1 125.8(8) . . ? C14 N1 C1 124.0(8) . . ? C13 N2 C15 108.8(8) . . ? C13 N2 C16 125.1(8) . . ? C15 N2 C16 126.0(7) . . ? C20 N3 C16 115.4(8) . . ? C21 N4 C22 108.5(7) . . ? C21 N4 C20 126.8(8) . . ? C22 N4 C20 124.5(8) . . ? C21 N5 C23 109.5(8) . . ? C21 N5 C24 124.0(7) . . ? C23 N5 C24 126.5(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.3(15) . . . . ? N1 C1 C2 C3 179.5(8) . . . . ? C6 C1 C2 C7 179.5(10) . . . . ? N1 C1 C2 C7 -2.3(13) . . . . ? C1 C2 C3 C4 -1.0(14) . . . . ? C7 C2 C3 C4 -179.3(9) . . . . ? C2 C3 C4 C5 -0.7(16) . . . . ? C3 C4 C5 C6 2.2(16) . . . . ? C2 C1 C6 C5 0.2(16) . . . . ? N1 C1 C6 C5 -177.9(9) . . . . ? C2 C1 C6 C10 179.9(10) . . . . ? N1 C1 C6 C10 1.8(15) . . . . ? C4 C5 C6 C1 -1.9(16) . . . . ? C4 C5 C6 C10 178.3(10) . . . . ? C3 C2 C7 C9 83.5(12) . . . . ? C1 C2 C7 C9 -94.7(12) . . . . ? C3 C2 C7 C8 -36.9(15) . . . . ? C1 C2 C7 C8 144.9(11) . . . . ? C1 C6 C10 C12 -114.7(12) . . . . ? C5 C6 C10 C12 65.0(13) . . . . ? C1 C6 C10 C11 121.5(12) . . . . ? C5 C6 C10 C11 -58.7(14) . . . . ? N1 C14 C15 N2 2.3(11) . . . . ? N3 C16 C17 C18 1.3(14) . . . . ? N2 C16 C17 C18 -179.0(8) . . . . ? N3 C16 C17 C36 -174.9(9) . . . . ? N2 C16 C17 C36 4.8(15) . . . . ? C16 C17 C18 C19 1.1(13) . . . . ? C36 C17 C18 C19 177.6(9) . . . . ? C17 C18 C19 C20 -1.5(13) . . . . ? C17 C18 C19 C37 -179.5(8) . . . . ? C18 C19 C20 N3 -0.3(14) . . . . ? C37 C19 C20 N3 177.6(9) . . . . ? C18 C19 C20 N4 -179.3(8) . . . . ? C37 C19 C20 N4 -1.4(14) . . . . ? N4 C22 C23 N5 -1.5(11) . . . . ? C29 C24 C25 C26 -1.2(14) . . . . ? N5 C24 C25 C26 177.7(8) . . . . ? C29 C24 C25 C30 178.5(9) . . . . ? N5 C24 C25 C30 -2.6(13) . . . . ? C24 C25 C26 C27 1.2(14) . . . . ? C30 C25 C26 C27 -178.5(9) . . . . ? C25 C26 C27 C28 -0.9(15) . . . . ? C26 C27 C28 C29 0.6(14) . . . . ? C27 C28 C29 C24 -0.5(14) . . . . ? C27 C28 C29 C33 -174.8(9) . . . . ? C25 C24 C29 C28 0.9(14) . . . . ? N5 C24 C29 C28 -178.0(8) . . . . ? C25 C24 C29 C33 175.0(9) . . . . ? N5 C24 C29 C33 -4.0(14) . . . . ? C26 C25 C30 C32 77.7(13) . . . . ? C24 C25 C30 C32 -101.9(12) . . . . ? C26 C25 C30 C31 -46.7(13) . . . . ? C24 C25 C30 C31 133.6(10) . . . . ? C28 C29 C33 C34 67.3(13) . . . . ? C24 C29 C33 C34 -106.5(12) . . . . ? C28 C29 C33 C35 -62.1(13) . . . . ? C24 C29 C33 C35 124.2(11) . . . . ? N2 C13 N1 C14 -0.2(10) . . . . ? N2 C13 N1 C1 176.2(8) . . . . ? C15 C14 N1 C13 -1.3(11) . . . . ? C15 C14 N1 C1 -177.8(8) . . . . ? C6 C1 N1 C13 91.4(12) . . . . ? C2 C1 N1 C13 -86.9(12) . . . . ? C6 C1 N1 C14 -92.7(12) . . . . ? C2 C1 N1 C14 89.0(11) . . . . ? N1 C13 N2 C15 1.6(10) . . . . ? N1 C13 N2 C16 178.4(8) . . . . ? C14 C15 N2 C13 -2.5(11) . . . . ? C14 C15 N2 C16 -179.2(9) . . . . ? N3 C16 N2 C13 -136.3(9) . . . . ? C17 C16 N2 C13 43.9(14) . . . . ? N3 C16 N2 C15 39.9(12) . . . . ? C17 C16 N2 C15 -139.9(10) . . . . ? C19 C20 N3 C16 2.4(13) . . . . ? N4 C20 N3 C16 -178.6(8) . . . . ? C17 C16 N3 C20 -2.9(14) . . . . ? N2 C16 N3 C20 177.3(8) . . . . ? N5 C21 N4 C22 -1.6(11) . . . . ? N5 C21 N4 C20 -175.5(8) . . . . ? C23 C22 N4 C21 1.9(11) . . . . ? C23 C22 N4 C20 176.0(8) . . . . ? N3 C20 N4 C21 131.4(9) . . . . ? C19 C20 N4 C21 -49.5(13) . . . . ? N3 C20 N4 C22 -41.5(12) . . . . ? C19 C20 N4 C22 137.6(10) . . . . ? N4 C21 N5 C23 0.6(11) . . . . ? N4 C21 N5 C24 -179.6(8) . . . . ? C22 C23 N5 C21 0.6(11) . . . . ? C22 C23 N5 C24 -179.1(9) . . . . ? C25 C24 N5 C21 -86.3(11) . . . . ? C29 C24 N5 C21 92.6(11) . . . . ? C25 C24 N5 C23 93.3(11) . . . . ? C29 C24 N5 C23 -87.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 3.818 _refine_diff_density_min -1.838 _refine_diff_density_rms 0.135 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.006 472.3 10.0 2 0.000 0.500 0.790 587.8 7.3 3 0.167 0.333 0.944 591.7 7.2 4 0.167 0.833 0.367 591.5 6.9 5 0.333 0.167 0.016 591.0 7.3 6 0.333 0.667 0.789 474.0 10.1 7 0.500 1.000 0.611 587.2 7.4 8 0.500 0.500 0.034 587.2 7.3 9 0.667 0.833 0.683 591.1 7.2 10 0.667 0.333 0.456 474.1 10.0 11 0.833 0.667 0.278 591.7 7.2 12 0.833 0.167 0.700 591.5 7.1 _platon_squeeze_details ; ; #==END data_1MeI2 _database_code_depnum_ccdc_archive 'CCDC 663955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H47 N5, C H Cl3, 0.67(C H Cl3), 2(I)' _chemical_formula_sum 'C38.67 H48.67 Cl5 I2 N5' _chemical_formula_weight 1014.54 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 52.325(4) _cell_length_b 52.325(4) _cell_length_c 9.4345(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 22370(3) _cell_formula_units_Z 18 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10814 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9120 _exptl_absorpt_coefficient_mu 1.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6031 _exptl_absorpt_correction_T_max 0.7881 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40406 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.0986 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 67 _diffrn_reflns_limit_k_min -67 _diffrn_reflns_limit_k_max 66 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.63 _reflns_number_total 11431 _reflns_number_gt 6384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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. There is a partially occupied chloroform molecule which was fixed at 0.6667 occupancy. ; _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^)+(0.0575P)^2^+268.5240P] 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 11431 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1396 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1754 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.63044(16) 0.03180(15) 0.7891(6) 0.0404(16) Uani 1 1 d . . . C2 C 0.60506(16) 0.00629(16) 0.7443(7) 0.0449(17) Uani 1 1 d . . . C3 C 0.60690(16) -0.01915(16) 0.7299(7) 0.0458(17) Uani 1 1 d . . . H3 H 0.5903 -0.0368 0.6968 0.055 Uiso 1 1 calc R . . C4 C 0.63297(17) -0.01913(16) 0.7638(7) 0.0460(18) Uani 1 1 d . . . H4 H 0.6339 -0.0368 0.7571 0.055 Uiso 1 1 calc R . . C5 C 0.65751(15) 0.00699(15) 0.8071(7) 0.0401(16) Uani 1 1 d . . . H5 H 0.6752 0.0070 0.8280 0.048 Uiso 1 1 calc R . . C6 C 0.65700(15) 0.03322(14) 0.8209(6) 0.0376(15) Uani 1 1 d . . . C7 C 0.57613(17) 0.00567(19) 0.7135(8) 0.056(2) Uani 1 1 d . . . H7 H 0.5802 0.0265 0.7208 0.067 Uiso 1 1 calc R . . C8 C 0.5648(2) -0.0049(2) 0.5645(9) 0.0758(9) Uani 1 1 d . . . H8A H 0.5598 -0.0255 0.5542 0.114 Uiso 1 1 calc R . . H8B H 0.5802 0.0073 0.4957 0.114 Uiso 1 1 calc R . . H8C H 0.5472 -0.0032 0.5474 0.114 Uiso 1 1 calc R . . C9 C 0.5532(2) -0.0118(2) 0.8214(9) 0.0758(9) Uani 1 1 d . . . H9A H 0.5465 -0.0328 0.8087 0.114 Uiso 1 1 calc R . . H9B H 0.5365 -0.0086 0.8100 0.114 Uiso 1 1 calc R . . H9C H 0.5616 -0.0056 0.9165 0.114 Uiso 1 1 calc R . . C10 C 0.68434(15) 0.06145(15) 0.8677(7) 0.0431(17) Uani 1 1 d . . . H10 H 0.6820 0.0787 0.8405 0.052 Uiso 1 1 calc R . . C11 C 0.6890(2) 0.0622(2) 1.0253(9) 0.0758(9) Uani 1 1 d . . . H11A H 0.6712 0.0591 1.0744 0.114 Uiso 1 1 calc R . . H11B H 0.7057 0.0814 1.0523 0.114 Uiso 1 1 calc R . . H11C H 0.6932 0.0466 1.0519 0.114 Uiso 1 1 calc R . . C12 C 0.7130(2) 0.0653(2) 0.7993(9) 0.0758(9) Uani 1 1 d . . . H12A H 0.7299 0.0837 0.8326 0.114 Uiso 1 1 calc R . . H12B H 0.7116 0.0659 0.6959 0.114 Uiso 1 1 calc R . . H12C H 0.7156 0.0487 0.8262 0.114 Uiso 1 1 calc R . . C13 C 0.63499(15) 0.07884(15) 0.7071(6) 0.0400(16) Uani 1 1 d . . . H13 H 0.6402 0.0779 0.6116 0.048 Uiso 1 1 calc R . . C14 C 0.62240(16) 0.06781(16) 0.9312(7) 0.0446(17) Uani 1 1 d . . . H14 H 0.6175 0.0576 1.0190 0.054 Uiso 1 1 calc R . . C15 C 0.62429(16) 0.09363(16) 0.9071(7) 0.0454(17) Uani 1 1 d . . . H15 H 0.6207 0.1051 0.9734 0.054 Uiso 1 1 calc R . . C16 C 0.63574(15) 0.12623(14) 0.6917(6) 0.0377(15) Uani 1 1 d . . . C17 C 0.65898(14) 0.14271(14) 0.5979(6) 0.0367(15) Uani 1 1 d . . . C18 C 0.65802(14) 0.16572(15) 0.5343(7) 0.0398(16) Uani 1 1 d . . . H18 H 0.6731 0.1774 0.4682 0.048 Uiso 1 1 calc R . . C19 C 0.63645(14) 0.17299(14) 0.5604(6) 0.0357(15) Uani 1 1 d . . . C20 C 0.61479(14) 0.15436(14) 0.6579(6) 0.0345(15) Uani 1 1 d . . . C21 C 0.57366(14) 0.16313(14) 0.6068(7) 0.0359(15) Uani 1 1 d . . . H21 H 0.5762 0.1652 0.5069 0.043 Uiso 1 1 calc R . . C22 C 0.57965(15) 0.15634(15) 0.8329(7) 0.0407(16) Uani 1 1 d . . . H22 H 0.5873 0.1529 0.9175 0.049 Uiso 1 1 calc R . . C23 C 0.55620(15) 0.16018(15) 0.8220(6) 0.0407(16) Uani 1 1 d . . . H23 H 0.5442 0.1600 0.8980 0.049 Uiso 1 1 calc R . . C24 C 0.52980(15) 0.16901(16) 0.6198(6) 0.0393(16) Uani 1 1 d . . . C25 C 0.50428(15) 0.14457(16) 0.5704(7) 0.0419(16) Uani 1 1 d . . . C26 C 0.48320(16) 0.14964(19) 0.5087(7) 0.0511(19) Uani 1 1 d . . . H26 H 0.4656 0.1336 0.4722 0.061 Uiso 1 1 calc R . . C27 C 0.48772(17) 0.1781(2) 0.5000(7) 0.051(2) Uani 1 1 d . . . H27 H 0.4728 0.1812 0.4601 0.061 Uiso 1 1 calc R . . C28 C 0.51315(17) 0.20161(18) 0.5476(7) 0.0493(19) Uani 1 1 d . . . H28 H 0.5158 0.2209 0.5382 0.059 Uiso 1 1 calc R . . C29 C 0.53558(16) 0.19818(16) 0.6102(7) 0.0427(17) Uani 1 1 d . . . C30 C 0.49907(15) 0.11354(16) 0.5826(7) 0.0475(18) Uani 1 1 d . . . H30 H 0.5181 0.1148 0.6104 0.057 Uiso 1 1 calc R . . C31 C 0.4769(2) 0.0975(2) 0.6993(9) 0.0758(9) Uani 1 1 d . . . H31A H 0.4838 0.1088 0.7876 0.114 Uiso 1 1 calc R . . H31B H 0.4747 0.0779 0.7129 0.114 Uiso 1 1 calc R . . H31C H 0.4578 0.0954 0.6729 0.114 Uiso 1 1 calc R . . C32 C 0.4887(2) 0.0961(2) 0.4448(9) 0.0758(9) Uani 1 1 d . . . H32A H 0.4697 0.0940 0.4170 0.114 Uiso 1 1 calc R . . H32B H 0.4864 0.0765 0.4588 0.114 Uiso 1 1 calc R . . H32C H 0.5032 0.1065 0.3701 0.114 Uiso 1 1 calc R . . C33 C 0.56380(16) 0.22435(16) 0.6566(8) 0.0493(18) Uani 1 1 d . . . H33 H 0.5758 0.2167 0.7034 0.059 Uiso 1 1 calc R . . C34 C 0.5811(2) 0.2423(2) 0.5299(9) 0.0758(9) Uani 1 1 d . . . H34A H 0.5822 0.2292 0.4587 0.114 Uiso 1 1 calc R . . H34B H 0.6011 0.2569 0.5597 0.114 Uiso 1 1 calc R . . H34C H 0.5713 0.2524 0.4889 0.114 Uiso 1 1 calc R . . C35 C 0.5590(2) 0.2427(2) 0.7643(9) 0.0758(9) Uani 1 1 d . . . H35A H 0.5461 0.2494 0.7243 0.114 Uiso 1 1 calc R . . H35B H 0.5781 0.2598 0.7898 0.114 Uiso 1 1 calc R . . H35C H 0.5498 0.2308 0.8492 0.114 Uiso 1 1 calc R . . C36 C 0.68360(15) 0.13645(17) 0.5673(8) 0.0484(18) Uani 1 1 d . . . H36A H 0.6778 0.1222 0.4895 0.073 Uiso 1 1 calc R . . H36B H 0.6877 0.1283 0.6522 0.073 Uiso 1 1 calc R . . H36C H 0.7014 0.1548 0.5403 0.073 Uiso 1 1 calc R . . C37 C 0.63734(15) 0.19931(15) 0.4933(7) 0.0443(17) Uani 1 1 d . . . H37A H 0.6577 0.2135 0.4659 0.067 Uiso 1 1 calc R . . H37B H 0.6302 0.2085 0.5610 0.067 Uiso 1 1 calc R . . H37C H 0.6247 0.1931 0.4089 0.067 Uiso 1 1 calc R . . C38 C 0.1093(2) 0.2673(2) 0.9093(11) 0.080(3) Uani 1 1 d . . . H38 H 0.0927 0.2701 0.9432 0.096 Uiso 1 1 calc R . . C39 C 0.1844(3) 0.3842(3) 0.3252(13) 0.062(3) Uani 0.67 1 d P . . H39 H 0.1766 0.3732 0.4162 0.074 Uiso 0.67 1 calc PR . . N1 N 0.62882(13) 0.05842(12) 0.8075(5) 0.0404(14) Uani 1 1 d . . . N2 N 0.63258(12) 0.10073(12) 0.7655(5) 0.0376(13) Uani 1 1 d . . . N3 N 0.61420(11) 0.13183(11) 0.7243(5) 0.0326(12) Uani 1 1 d . . . N4 N 0.59059(12) 0.15845(11) 0.6968(5) 0.0352(12) Uani 1 1 d . . . N5 N 0.55267(12) 0.16446(12) 0.6805(5) 0.0363(12) Uani 1 1 d . . . I1 I 0.628975(11) 0.067810(11) 0.32367(5) 0.04747(16) Uani 1 1 d . . . I2 I 0.099632(11) 0.164328(13) 0.11597(5) 0.05107(17) Uani 1 1 d . . . Cl1 Cl 0.10445(6) 0.23369(6) 0.9787(3) 0.0904(8) Uani 1 1 d . . . Cl2 Cl 0.10850(6) 0.26598(6) 0.7226(3) 0.0950(8) Uani 1 1 d . . . Cl3 Cl 0.14243(7) 0.29730(6) 0.9643(4) 0.1108(10) Uani 1 1 d . . . Cl4 Cl 0.21969(9) 0.39098(12) 0.3099(5) 0.1126(16) Uani 0.67 1 d P . . Cl5 Cl 0.18220(13) 0.41571(11) 0.3403(6) 0.1240(18) Uani 0.67 1 d P . . Cl6 Cl 0.16129(9) 0.36109(10) 0.1915(4) 0.0929(12) Uani 0.67 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.061(5) 0.042(4) 0.026(3) 0.001(3) 0.000(3) 0.031(4) C2 0.044(4) 0.053(5) 0.044(4) -0.010(3) -0.008(3) 0.029(4) C3 0.043(4) 0.043(4) 0.041(4) -0.003(3) -0.002(3) 0.014(4) C4 0.062(5) 0.045(4) 0.039(4) -0.002(3) 0.003(3) 0.032(4) C5 0.041(4) 0.043(4) 0.036(3) -0.003(3) 0.000(3) 0.021(3) C6 0.047(4) 0.035(4) 0.032(3) 0.000(3) -0.002(3) 0.021(3) C7 0.046(5) 0.064(5) 0.060(5) -0.015(4) -0.012(4) 0.028(4) C8 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C9 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C10 0.045(4) 0.041(4) 0.037(4) -0.001(3) -0.001(3) 0.017(3) C11 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C12 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C13 0.048(4) 0.051(4) 0.026(3) -0.001(3) -0.006(3) 0.028(4) C14 0.057(5) 0.050(5) 0.033(4) 0.002(3) -0.007(3) 0.031(4) C15 0.058(5) 0.054(5) 0.030(3) -0.009(3) -0.006(3) 0.032(4) C16 0.050(4) 0.037(4) 0.032(3) -0.006(3) -0.010(3) 0.027(4) C17 0.035(4) 0.039(4) 0.032(3) -0.003(3) -0.004(3) 0.016(3) C18 0.032(4) 0.042(4) 0.037(4) -0.007(3) -0.003(3) 0.012(3) C19 0.035(4) 0.040(4) 0.027(3) -0.003(3) -0.002(3) 0.014(3) C20 0.034(4) 0.037(4) 0.033(3) -0.005(3) -0.002(3) 0.017(3) C21 0.041(4) 0.036(4) 0.031(3) 0.006(3) 0.004(3) 0.020(3) C22 0.043(4) 0.048(4) 0.030(3) 0.000(3) -0.002(3) 0.022(4) C23 0.041(4) 0.051(4) 0.027(3) -0.003(3) 0.000(3) 0.021(4) C24 0.035(4) 0.054(5) 0.031(3) 0.000(3) 0.002(3) 0.024(4) C25 0.037(4) 0.053(5) 0.035(3) 0.009(3) 0.008(3) 0.022(4) C26 0.038(4) 0.071(6) 0.047(4) 0.007(4) 0.006(3) 0.029(4) C27 0.045(5) 0.089(6) 0.036(4) 0.009(4) 0.005(3) 0.046(5) C28 0.062(5) 0.067(5) 0.038(4) 0.008(4) 0.009(4) 0.046(5) C29 0.048(4) 0.059(5) 0.032(3) 0.005(3) 0.007(3) 0.034(4) C30 0.033(4) 0.048(4) 0.050(4) 0.007(3) -0.003(3) 0.012(3) C31 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C32 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C33 0.049(5) 0.052(5) 0.051(4) -0.006(4) 0.002(4) 0.028(4) C34 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C35 0.068(2) 0.083(2) 0.065(2) -0.0076(17) 0.0014(16) 0.0298(19) C36 0.037(4) 0.055(5) 0.056(4) -0.006(4) -0.003(3) 0.025(4) C37 0.038(4) 0.048(4) 0.044(4) 0.009(3) 0.001(3) 0.019(4) C38 0.064(6) 0.062(6) 0.116(8) -0.016(5) -0.027(6) 0.034(5) C39 0.046(7) 0.077(9) 0.061(7) -0.016(6) -0.001(6) 0.031(7) N1 0.055(4) 0.047(3) 0.028(3) -0.004(2) -0.005(2) 0.032(3) N2 0.047(3) 0.042(3) 0.029(3) -0.006(2) -0.009(2) 0.026(3) N3 0.038(3) 0.031(3) 0.029(3) -0.004(2) -0.004(2) 0.018(3) N4 0.038(3) 0.037(3) 0.029(3) 0.003(2) 0.000(2) 0.018(3) N5 0.032(3) 0.045(3) 0.033(3) 0.005(2) 0.002(2) 0.021(3) I1 0.0579(3) 0.0495(3) 0.0333(2) -0.0018(2) -0.0016(2) 0.0255(3) I2 0.0477(3) 0.0856(4) 0.0322(2) -0.0026(2) -0.0018(2) 0.0425(3) Cl1 0.0789(17) 0.0789(18) 0.122(2) 0.0085(15) 0.0013(15) 0.0461(15) Cl2 0.094(2) 0.0873(19) 0.099(2) -0.0119(15) -0.0163(16) 0.0415(16) Cl3 0.093(2) 0.0824(19) 0.136(3) -0.0132(17) -0.0505(19) 0.0277(16) Cl4 0.068(3) 0.153(4) 0.115(3) -0.035(3) 0.007(2) 0.053(3) Cl5 0.166(5) 0.089(3) 0.140(4) -0.013(3) -0.028(4) 0.080(4) Cl6 0.067(2) 0.099(3) 0.089(3) -0.023(2) 0.007(2) 0.024(2) _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 C1 C6 1.387(9) . ? C1 C2 1.397(10) . ? C1 N1 1.448(8) . ? C2 C3 1.389(10) . ? C2 C7 1.526(10) . ? C3 C4 1.400(10) . ? C3 H3 0.9500 . ? C4 C5 1.389(10) . ? C4 H4 0.9500 . ? C5 C6 1.392(9) . ? C5 H5 0.9500 . ? C6 C10 1.520(9) . ? C7 C9 1.487(11) . ? C7 C8 1.518(11) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.505(10) . ? C10 C12 1.551(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.333(8) . ? C13 N1 1.341(8) . ? C13 H13 0.9500 . ? C14 C15 1.324(9) . ? C14 N1 1.371(8) . ? C14 H14 0.9500 . ? C15 N2 1.396(8) . ? C15 H15 0.9500 . ? C16 N3 1.335(8) . ? C16 C17 1.399(9) . ? C16 N2 1.439(8) . ? C17 C18 1.368(9) . ? C17 C36 1.507(9) . ? C18 C19 1.381(9) . ? C18 H18 0.9500 . ? C19 C20 1.406(9) . ? C19 C37 1.496(9) . ? C20 N3 1.321(8) . ? C20 N4 1.433(8) . ? C21 N5 1.331(8) . ? C21 N4 1.335(8) . ? C21 H21 0.9500 . ? C22 C23 1.343(9) . ? C22 N4 1.388(8) . ? C22 H22 0.9500 . ? C23 N5 1.382(8) . ? C23 H23 0.9500 . ? C24 C25 1.389(9) . ? C24 C29 1.403(10) . ? C24 N5 1.449(8) . ? C25 C26 1.385(9) . ? C25 C30 1.511(10) . ? C26 C27 1.390(11) . ? C26 H26 0.9500 . ? C27 C28 1.359(11) . ? C27 H27 0.9500 . ? C28 C29 1.403(10) . ? C28 H28 0.9500 . ? C29 C33 1.492(10) . ? C30 C31 1.513(11) . ? C30 C32 1.525(11) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.502(11) . ? C33 C34 1.511(11) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Cl3 1.737(9) . ? C38 Cl2 1.762(11) . ? C38 Cl1 1.774(10) . ? C38 H38 1.0000 . ? C39 Cl4 1.705(12) . ? C39 Cl5 1.714(13) . ? C39 Cl6 1.747(12) . ? C39 H39 1.0000 . ? 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 C6 C1 C2 124.4(6) . . ? C6 C1 N1 117.5(6) . . ? C2 C1 N1 118.0(6) . . ? C3 C2 C1 117.2(6) . . ? C3 C2 C7 120.3(7) . . ? C1 C2 C7 122.5(7) . . ? C2 C3 C4 120.8(7) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.3(7) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.3(7) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C1 C6 C5 116.1(6) . . ? C1 C6 C10 123.1(6) . . ? C5 C6 C10 120.9(6) . . ? C9 C7 C8 111.3(7) . . ? C9 C7 C2 111.6(7) . . ? C8 C7 C2 112.8(7) . . ? C9 C7 H7 107.0 . . ? C8 C7 H7 107.0 . . ? C2 C7 H7 107.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 112.0(6) . . ? C11 C10 C12 105.8(6) . . ? C6 C10 C12 112.6(6) . . ? C11 C10 H10 108.8 . . ? C6 C10 H10 108.8 . . ? C12 C10 H10 108.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 N1 107.7(5) . . ? N2 C13 H13 126.1 . . ? N1 C13 H13 126.1 . . ? C15 C14 N1 108.2(6) . . ? C15 C14 H14 125.9 . . ? N1 C14 H14 125.9 . . ? C14 C15 N2 106.9(6) . . ? C14 C15 H15 126.5 . . ? N2 C15 H15 126.5 . . ? N3 C16 C17 125.4(6) . . ? N3 C16 N2 112.0(6) . . ? C17 C16 N2 122.6(6) . . ? C18 C17 C16 114.6(6) . . ? C18 C17 C36 121.3(6) . . ? C16 C17 C36 124.1(6) . . ? C17 C18 C19 124.0(6) . . ? C17 C18 H18 118.0 . . ? C19 C18 H18 118.0 . . ? C18 C19 C20 114.4(6) . . ? C18 C19 C37 121.6(6) . . ? C20 C19 C37 124.0(6) . . ? N3 C20 C19 125.4(6) . . ? N3 C20 N4 112.6(5) . . ? C19 C20 N4 122.0(6) . . ? N5 C21 N4 108.6(5) . . ? N5 C21 H21 125.7 . . ? N4 C21 H21 125.7 . . ? C23 C22 N4 106.8(6) . . ? C23 C22 H22 126.6 . . ? N4 C22 H22 126.6 . . ? C22 C23 N5 107.7(6) . . ? C22 C23 H23 126.1 . . ? N5 C23 H23 126.1 . . ? C25 C24 C29 124.4(6) . . ? C25 C24 N5 118.3(6) . . ? C29 C24 N5 117.2(6) . . ? C26 C25 C24 117.2(7) . . ? C26 C25 C30 120.3(7) . . ? C24 C25 C30 122.5(6) . . ? C25 C26 C27 120.4(7) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 121.0(7) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 121.8(7) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C24 115.3(7) . . ? C28 C29 C33 120.9(7) . . ? C24 C29 C33 123.7(6) . . ? C25 C30 C31 109.2(7) . . ? C25 C30 C32 113.5(6) . . ? C31 C30 C32 110.0(7) . . ? C25 C30 H30 108.0 . . ? C31 C30 H30 108.0 . . ? C32 C30 H30 108.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 112.4(6) . . ? C29 C33 C34 110.4(6) . . ? C35 C33 C34 112.2(7) . . ? C29 C33 H33 107.2 . . ? C35 C33 H33 107.2 . . ? C34 C33 H33 107.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C19 C37 H37A 109.5 . . ? C19 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C19 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Cl3 C38 Cl2 109.1(6) . . ? Cl3 C38 Cl1 111.6(5) . . ? Cl2 C38 Cl1 109.9(5) . . ? Cl3 C38 H38 108.7 . . ? Cl2 C38 H38 108.7 . . ? Cl1 C38 H38 108.7 . . ? Cl4 C39 Cl5 113.1(8) . . ? Cl4 C39 Cl6 112.6(7) . . ? Cl5 C39 Cl6 111.8(7) . . ? Cl4 C39 H39 106.2 . . ? Cl5 C39 H39 106.2 . . ? Cl6 C39 H39 106.2 . . ? C13 N1 C14 108.7(6) . . ? C13 N1 C1 125.1(5) . . ? C14 N1 C1 126.1(5) . . ? C13 N2 C15 108.5(5) . . ? C13 N2 C16 125.5(5) . . ? C15 N2 C16 125.9(5) . . ? C20 N3 C16 116.2(5) . . ? C21 N4 C22 108.5(5) . . ? C21 N4 C20 125.6(5) . . ? C22 N4 C20 125.8(5) . . ? C21 N5 C23 108.4(5) . . ? C21 N5 C24 125.0(5) . . ? C23 N5 C24 126.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.5(10) . . . . ? N1 C1 C2 C3 -178.8(6) . . . . ? C6 C1 C2 C7 178.7(6) . . . . ? N1 C1 C2 C7 0.4(10) . . . . ? C1 C2 C3 C4 2.0(10) . . . . ? C7 C2 C3 C4 -177.2(6) . . . . ? C2 C3 C4 C5 -2.4(10) . . . . ? C3 C4 C5 C6 1.3(10) . . . . ? C2 C1 C6 C5 -0.5(10) . . . . ? N1 C1 C6 C5 177.7(5) . . . . ? C2 C1 C6 C10 179.2(6) . . . . ? N1 C1 C6 C10 -2.5(9) . . . . ? C4 C5 C6 C1 0.2(9) . . . . ? C4 C5 C6 C10 -179.6(6) . . . . ? C3 C2 C7 C9 68.9(9) . . . . ? C1 C2 C7 C9 -110.3(8) . . . . ? C3 C2 C7 C8 -57.1(10) . . . . ? C1 C2 C7 C8 123.7(8) . . . . ? C1 C6 C10 C11 101.6(8) . . . . ? C5 C6 C10 C11 -78.6(8) . . . . ? C1 C6 C10 C12 -139.2(7) . . . . ? C5 C6 C10 C12 40.5(9) . . . . ? N1 C14 C15 N2 -1.0(8) . . . . ? N3 C16 C17 C18 -1.9(9) . . . . ? N2 C16 C17 C18 178.3(5) . . . . ? N3 C16 C17 C36 177.7(6) . . . . ? N2 C16 C17 C36 -2.2(10) . . . . ? C16 C17 C18 C19 1.2(9) . . . . ? C36 C17 C18 C19 -178.4(6) . . . . ? C17 C18 C19 C20 -0.8(9) . . . . ? C17 C18 C19 C37 176.9(6) . . . . ? C18 C19 C20 N3 1.2(9) . . . . ? C37 C19 C20 N3 -176.5(6) . . . . ? C18 C19 C20 N4 -179.4(5) . . . . ? C37 C19 C20 N4 2.9(9) . . . . ? N4 C22 C23 N5 0.3(8) . . . . ? C29 C24 C25 C26 -0.6(10) . . . . ? N5 C24 C25 C26 -178.0(6) . . . . ? C29 C24 C25 C30 179.7(6) . . . . ? N5 C24 C25 C30 2.4(9) . . . . ? C24 C25 C26 C27 -0.9(10) . . . . ? C30 C25 C26 C27 178.7(6) . . . . ? C25 C26 C27 C28 2.0(10) . . . . ? C26 C27 C28 C29 -1.4(10) . . . . ? C27 C28 C29 C24 -0.1(9) . . . . ? C27 C28 C29 C33 177.6(6) . . . . ? C25 C24 C29 C28 1.1(9) . . . . ? N5 C24 C29 C28 178.5(5) . . . . ? C25 C24 C29 C33 -176.5(6) . . . . ? N5 C24 C29 C33 0.9(9) . . . . ? C26 C25 C30 C31 -74.5(8) . . . . ? C24 C25 C30 C31 105.1(8) . . . . ? C26 C25 C30 C32 48.6(9) . . . . ? C24 C25 C30 C32 -131.8(7) . . . . ? C28 C29 C33 C35 58.9(9) . . . . ? C24 C29 C33 C35 -123.6(8) . . . . ? C28 C29 C33 C34 -67.2(9) . . . . ? C24 C29 C33 C34 110.2(8) . . . . ? N2 C13 N1 C14 0.0(8) . . . . ? N2 C13 N1 C1 -176.6(6) . . . . ? C15 C14 N1 C13 0.6(8) . . . . ? C15 C14 N1 C1 177.3(7) . . . . ? C6 C1 N1 C13 90.7(8) . . . . ? C2 C1 N1 C13 -91.0(8) . . . . ? C6 C1 N1 C14 -85.4(8) . . . . ? C2 C1 N1 C14 93.0(8) . . . . ? N1 C13 N2 C15 -0.7(7) . . . . ? N1 C13 N2 C16 -176.2(6) . . . . ? C14 C15 N2 C13 1.1(8) . . . . ? C14 C15 N2 C16 176.6(6) . . . . ? N3 C16 N2 C13 133.5(6) . . . . ? C17 C16 N2 C13 -46.6(9) . . . . ? N3 C16 N2 C15 -41.2(8) . . . . ? C17 C16 N2 C15 138.6(7) . . . . ? C19 C20 N3 C16 -1.8(9) . . . . ? N4 C20 N3 C16 178.8(5) . . . . ? C17 C16 N3 C20 2.2(9) . . . . ? N2 C16 N3 C20 -178.0(5) . . . . ? N5 C21 N4 C22 0.8(7) . . . . ? N5 C21 N4 C20 177.1(6) . . . . ? C23 C22 N4 C21 -0.7(7) . . . . ? C23 C22 N4 C20 -176.9(6) . . . . ? N3 C20 N4 C21 -133.8(6) . . . . ? C19 C20 N4 C21 46.7(9) . . . . ? N3 C20 N4 C22 41.8(8) . . . . ? C19 C20 N4 C22 -137.7(6) . . . . ? N4 C21 N5 C23 -0.6(7) . . . . ? N4 C21 N5 C24 -179.4(6) . . . . ? C22 C23 N5 C21 0.2(8) . . . . ? C22 C23 N5 C24 178.9(6) . . . . ? C25 C24 N5 C21 85.5(8) . . . . ? C29 C24 N5 C21 -92.1(8) . . . . ? C25 C24 N5 C23 -93.0(8) . . . . ? C29 C24 N5 C23 89.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.194 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.117 #==END data_2Me _database_code_depnum_ccdc_archive 'CCDC 663956' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H45 N5' _chemical_formula_sum 'C37 H45 N5' _chemical_formula_weight 559.78 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.058(3) _cell_length_b 24.920(6) _cell_length_c 10.967(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.360(3) _cell_angle_gamma 90.00 _cell_volume 4114.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 837 _cell_measurement_theta_min 4.83 _cell_measurement_theta_max 22.66 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9947 _exptl_absorpt_correction_T_max 0.9947 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.7848 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2smx' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 22457 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.63 _diffrn_reflns_theta_max 26.34 _reflns_number_total 5879 _reflns_number_gt 3714 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains one highly disordered molecule of isohexane - attempts to satisfactorily model this failed. As a result it was removed using the squeeze algorithm ( P. v.d. Sluis and A. L. Spek, Acta Crystallogr., Sect A 1990, 46, 194-201.). This treatment explains the following checkCIF alerts: PLAT602_ALERT_4_C, PLAT601_ALERT_2_A. ; _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^)+(0.1410P)^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 5879 _refine_ls_number_parameters 448 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2125 _refine_ls_wR_factor_gt 0.1937 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 C1A C 0.1915(11) 0.9021(4) 0.4761(12) 0.0489(14) Uani 0.277(7) 1 d PGD A 1 C2A C 0.2331(10) 0.8907(5) 0.3673(12) 0.101(8) Uani 0.277(7) 1 d PGD A 1 C3A C 0.2160(10) 0.8425(5) 0.3073(11) 0.0689(17) Uani 0.277(7) 1 d PG A 1 H3A H 0.2444 0.8348 0.2330 0.083 Uiso 0.277(7) 1 calc PR A 1 C4A C 0.1571(9) 0.8058(4) 0.3560(14) 0.094(8) Uani 0.277(7) 1 d PG A 1 H4A H 0.1454 0.7729 0.3149 0.113 Uiso 0.277(7) 1 calc PR A 1 C5A C 0.1154(8) 0.8172(4) 0.4647(14) 0.075(5) Uani 0.277(7) 1 d PG A 1 H5A H 0.0752 0.7921 0.4980 0.090 Uiso 0.277(7) 1 calc PR A 1 C6A C 0.1326(9) 0.8653(4) 0.5248(11) 0.0516(14) Uani 0.277(7) 1 d PGD A 1 C7A C 0.3050(10) 0.9290(6) 0.3236(15) 0.0587(15) Uani 0.277(7) 1 d PD A 1 H7A H 0.3241 0.9515 0.3951 0.070 Uiso 0.277(7) 1 calc PR A 1 C8A C 0.264(3) 0.9670(9) 0.228(2) 0.135(12) Uani 0.277(7) 1 d PD A 1 H8A1 H 0.1996 0.9603 0.2203 0.203 Uiso 0.277(7) 1 calc PR A 1 H8A2 H 0.2909 0.9606 0.1486 0.203 Uiso 0.277(7) 1 calc PR A 1 H8A3 H 0.2740 1.0043 0.2526 0.203 Uiso 0.277(7) 1 calc PR A 1 C9A C 0.3885(14) 0.9005(10) 0.277(2) 0.121(8) Uani 0.277(7) 1 d PD A 1 H9A1 H 0.4254 0.8887 0.3471 0.181 Uiso 0.277(7) 1 calc PR A 1 H9A2 H 0.4224 0.9255 0.2273 0.181 Uiso 0.277(7) 1 calc PR A 1 H9A3 H 0.3707 0.8693 0.2282 0.181 Uiso 0.277(7) 1 calc PR A 1 C10A C 0.0893(15) 0.8770(7) 0.6479(15) 0.079(7) Uani 0.277(7) 1 d PD A 1 H10A H 0.1298 0.9002 0.6988 0.095 Uiso 0.277(7) 1 calc PR A 1 C11A C 0.0654(14) 0.8261(6) 0.720(2) 0.086(6) Uani 0.277(7) 1 d PD A 1 H11A H 0.0110 0.8103 0.6850 0.129 Uiso 0.277(7) 1 calc PR A 1 H11B H 0.0558 0.8357 0.8055 0.129 Uiso 0.277(7) 1 calc PR A 1 H11C H 0.1141 0.8002 0.7158 0.129 Uiso 0.277(7) 1 calc PR A 1 C12A C -0.0028(18) 0.9076(11) 0.623(3) 0.101(3) Uani 0.277(7) 1 d P A 1 H12A H 0.0084 0.9419 0.5828 0.152 Uiso 0.277(7) 1 calc PR A 1 H12B H -0.0317 0.9141 0.7010 0.152 Uiso 0.277(7) 1 calc PR A 1 H12C H -0.0417 0.8854 0.5709 0.152 Uiso 0.277(7) 1 calc PR A 1 C1B C 0.2081(3) 0.90905(14) 0.4434(3) 0.0489(14) Uani 0.723(7) 1 d PGD A 2 C2B C 0.2591(3) 0.90778(14) 0.3394(3) 0.0478(16) Uani 0.723(7) 1 d PGD A 2 C3B C 0.2509(3) 0.86513(16) 0.2582(3) 0.0689(17) Uani 0.723(7) 1 d PG A 2 H3B H 0.2857 0.8643 0.1872 0.083 Uiso 0.723(7) 1 calc PR A 2 C4B C 0.1916(3) 0.82375(14) 0.2810(4) 0.078(2) Uani 0.723(7) 1 d PG A 2 H4B H 0.1860 0.7946 0.2256 0.094 Uiso 0.723(7) 1 calc PR A 2 C5B C 0.1407(3) 0.82502(12) 0.3850(5) 0.068(2) Uani 0.723(7) 1 d PG A 2 H5B H 0.1002 0.7967 0.4006 0.081 Uiso 0.723(7) 1 calc PR A 2 C6B C 0.1489(3) 0.86766(14) 0.4662(4) 0.0516(14) Uani 0.723(7) 1 d PGD A 2 C7B C 0.3231(4) 0.9546(2) 0.3100(5) 0.0587(15) Uani 0.723(7) 1 d PD A 2 H7B H 0.3332 0.9755 0.3869 0.070 Uiso 0.723(7) 1 calc PR A 2 C8B C 0.2780(7) 0.9925(3) 0.2157(7) 0.078(2) Uani 0.723(7) 1 d P A 2 H8B1 H 0.2667 0.9731 0.1393 0.117 Uiso 0.723(7) 1 calc PR A 2 H8B2 H 0.3172 1.0231 0.2005 0.117 Uiso 0.723(7) 1 calc PR A 2 H8B3 H 0.2217 1.0055 0.2476 0.117 Uiso 0.723(7) 1 calc PR A 2 C9B C 0.4135(5) 0.9342(3) 0.2699(6) 0.078(2) Uani 0.723(7) 1 d P A 2 H9B1 H 0.4388 0.9104 0.3328 0.117 Uiso 0.723(7) 1 calc PR A 2 H9B2 H 0.4534 0.9647 0.2581 0.117 Uiso 0.723(7) 1 calc PR A 2 H9B3 H 0.4062 0.9144 0.1931 0.117 Uiso 0.723(7) 1 calc PR A 2 C10B C 0.0927(6) 0.8691(3) 0.5804(7) 0.068(2) Uani 0.723(7) 1 d PD A 2 H10B H 0.1276 0.8886 0.6453 0.082 Uiso 0.723(7) 1 calc PR A 2 C11B C 0.0698(5) 0.8134(3) 0.6303(8) 0.088(2) Uani 0.723(7) 1 d P A 2 H11D H 0.0458 0.8171 0.7121 0.132 Uiso 0.723(7) 1 calc PR A 2 H11E H 0.1235 0.7913 0.6343 0.132 Uiso 0.723(7) 1 calc PR A 2 H11F H 0.0254 0.7964 0.5762 0.132 Uiso 0.723(7) 1 calc PR A 2 C12B C 0.0077(6) 0.9000(3) 0.5568(9) 0.101(3) Uani 0.723(7) 1 d P A 2 H12D H 0.0214 0.9380 0.5447 0.152 Uiso 0.723(7) 1 calc PR A 2 H12E H -0.0311 0.8961 0.6268 0.152 Uiso 0.723(7) 1 calc PR A 2 H12F H -0.0226 0.8858 0.4835 0.152 Uiso 0.723(7) 1 calc PR A 2 C13 C 0.2736(2) 0.95563(11) 0.6225(3) 0.0475(8) Uani 1 1 d . A . C14 C 0.1697(2) 1.00181(11) 0.5067(3) 0.0486(8) Uani 1 1 d . A . H14 H 0.1258 1.0091 0.4452 0.058 Uiso 1 1 calc R . . C15 C 0.2015(2) 1.03603(11) 0.5906(3) 0.0473(8) Uani 1 1 d . A . H15 H 0.1848 1.0725 0.6005 0.057 Uiso 1 1 calc R . . C16 C 0.3158(2) 1.03178(10) 0.7571(3) 0.0433(7) Uani 1 1 d . A . C17 C 0.3418(2) 1.00369(11) 0.8616(3) 0.0530(9) Uani 1 1 d . . . C18 C 0.3903(3) 1.03402(12) 0.9469(3) 0.0573(9) Uani 1 1 d . . . H18 H 0.4101 1.0166 1.0196 0.069 Uiso 1 1 calc R . . C19 C 0.4117(2) 1.08779(11) 0.9331(3) 0.0503(8) Uani 1 1 d . . . C20 C 0.3801(2) 1.11062(10) 0.8229(2) 0.0411(7) Uani 1 1 d . A . C21 C 0.4061(2) 1.20757(10) 0.8672(2) 0.0409(7) Uani 1 1 d . A . C22 C 0.4007(2) 1.18012(11) 0.6658(2) 0.0428(7) Uani 1 1 d . A . H22 H 0.3956 1.1573 0.5966 0.051 Uiso 1 1 calc R . . C23 C 0.4129(2) 1.23325(11) 0.6658(2) 0.0423(7) Uani 1 1 d . A . H23 H 0.4184 1.2558 0.5965 0.051 Uiso 1 1 calc R . . C24 C 0.4300(2) 1.30415(10) 0.8254(2) 0.0383(7) Uani 1 1 d . A . C25 C 0.3552(2) 1.33746(11) 0.8372(3) 0.0443(8) Uani 1 1 d . . . C26 C 0.3713(2) 1.39043(11) 0.8733(3) 0.0492(8) Uani 1 1 d . . . H26 H 0.3226 1.4141 0.8837 0.059 Uiso 1 1 calc R . . C27 C 0.4563(2) 1.40893(11) 0.8941(3) 0.0470(8) Uani 1 1 d . . . H27 H 0.4655 1.4452 0.9180 0.056 Uiso 1 1 calc R . . C28 C 0.5282(2) 1.37546(10) 0.8806(2) 0.0441(8) Uani 1 1 d . . . H28 H 0.5864 1.3891 0.8950 0.053 Uiso 1 1 calc R . . C29 C 0.5171(2) 1.32200(10) 0.8462(2) 0.0395(7) Uani 1 1 d . . . C30 C 0.2619(2) 1.31696(13) 0.8142(3) 0.0551(9) Uani 1 1 d . . . H30 H 0.2668 1.2807 0.7761 0.066 Uiso 1 1 calc R . . C31 C 0.2090(4) 1.3513(2) 0.7278(5) 0.1222(18) Uani 1 1 d U . . H31A H 0.1509 1.3347 0.7118 0.183 Uiso 1 1 calc R . . H31B H 0.2406 1.3548 0.6512 0.183 Uiso 1 1 calc R . . H31C H 0.2008 1.3868 0.7638 0.183 Uiso 1 1 calc R . . C32 C 0.2127(3) 1.31008(19) 0.9327(4) 0.0920(14) Uani 1 1 d . . . H32A H 0.2080 1.3449 0.9737 0.138 Uiso 1 1 calc R . . H32B H 0.2453 1.2849 0.9859 0.138 Uiso 1 1 calc R . . H32C H 0.1530 1.2960 0.9150 0.138 Uiso 1 1 calc R . . C33 C 0.5964(2) 1.28487(11) 0.8343(3) 0.0478(8) Uani 1 1 d . . . H33 H 0.5752 1.2514 0.7928 0.057 Uiso 1 1 calc R . . C34 C 0.6683(2) 1.30979(12) 0.7556(3) 0.0529(8) Uani 1 1 d . . . H34A H 0.6424 1.3200 0.6761 0.079 Uiso 1 1 calc R . . H34B H 0.7160 1.2836 0.7439 0.079 Uiso 1 1 calc R . . H34C H 0.6927 1.3417 0.7964 0.079 Uiso 1 1 calc R . . C35 C 0.6342(2) 1.26920(14) 0.9594(3) 0.0684(10) Uani 1 1 d . . . H35A H 0.6544 1.3015 1.0030 0.103 Uiso 1 1 calc R . . H35B H 0.6845 1.2447 0.9496 0.103 Uiso 1 1 calc R . . H35C H 0.5881 1.2513 1.0062 0.103 Uiso 1 1 calc R . . C36 C 0.3193(3) 0.94577(12) 0.8855(3) 0.0757(12) Uani 1 1 d . . . H36A H 0.2550 0.9407 0.8770 0.114 Uiso 1 1 calc R . . H36B H 0.3390 0.9361 0.9684 0.114 Uiso 1 1 calc R . . H36C H 0.3494 0.9229 0.8266 0.114 Uiso 1 1 calc R . . C37 C 0.4641(3) 1.11696(13) 1.0299(3) 0.0640(10) Uani 1 1 d . . . H37A H 0.4253 1.1422 1.0718 0.096 Uiso 1 1 calc R . . H37B H 0.5127 1.1367 0.9925 0.096 Uiso 1 1 calc R . . H37C H 0.4887 1.0911 1.0889 0.096 Uiso 1 1 calc R . . N1 N 0.21357(16) 0.95345(8) 0.5275(2) 0.0456(6) Uani 1 1 d D . . N2 N 0.26437(16) 1.00774(8) 0.6612(2) 0.0418(6) Uani 1 1 d . . . N3 N 0.33369(16) 1.08334(8) 0.7386(2) 0.0399(6) Uani 1 1 d . . . N4 N 0.39704(16) 1.16486(8) 0.78858(19) 0.0396(6) Uani 1 1 d . . . N5 N 0.41592(16) 1.24893(8) 0.78732(19) 0.0385(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.050(3) 0.031(2) 0.065(4) -0.011(2) -0.005(3) 0.0053(18) C2A 0.124(19) 0.056(12) 0.123(18) 0.002(12) -0.024(14) -0.056(11) C3A 0.078(4) 0.049(3) 0.080(4) -0.033(3) 0.009(3) 0.000(3) C4A 0.085(14) 0.056(13) 0.14(2) -0.024(13) -0.022(13) 0.019(11) C5A 0.075(11) 0.050(9) 0.100(13) 0.002(9) 0.012(9) 0.000(7) C6A 0.050(3) 0.032(2) 0.073(4) 0.004(3) 0.006(3) -0.0010(19) C7A 0.079(4) 0.049(4) 0.048(3) -0.014(3) 0.019(2) -0.011(3) C8A 0.21(3) 0.056(16) 0.15(2) 0.005(17) 0.07(2) 0.03(2) C9A 0.14(2) 0.122(19) 0.106(15) -0.013(16) 0.018(14) -0.005(16) C10A 0.063(11) 0.043(9) 0.130(19) 0.006(12) -0.023(14) 0.010(8) C11A 0.089(12) 0.051(9) 0.118(15) 0.016(11) 0.010(13) -0.008(8) C12A 0.067(4) 0.067(4) 0.172(10) 0.043(6) 0.052(6) 0.015(3) C1B 0.050(3) 0.031(2) 0.065(4) -0.011(2) -0.005(3) 0.0053(18) C2B 0.055(4) 0.032(3) 0.056(3) -0.020(3) -0.003(3) -0.002(3) C3B 0.078(4) 0.049(3) 0.080(4) -0.033(3) 0.009(3) 0.000(3) C4B 0.089(5) 0.037(3) 0.107(5) -0.031(3) -0.025(4) 0.007(3) C5B 0.063(4) 0.021(3) 0.117(6) -0.005(4) -0.020(4) 0.000(3) C6B 0.050(3) 0.032(2) 0.073(4) 0.004(3) 0.006(3) -0.0010(19) C7B 0.079(4) 0.049(4) 0.048(3) -0.014(3) 0.019(2) -0.011(3) C8B 0.128(6) 0.049(5) 0.057(4) -0.008(3) 0.008(4) 0.002(4) C9B 0.089(5) 0.095(5) 0.051(3) -0.017(4) 0.018(3) -0.004(4) C10B 0.063(4) 0.039(3) 0.102(6) 0.014(4) -0.003(5) -0.017(3) C11B 0.077(4) 0.062(4) 0.125(7) 0.035(4) -0.004(5) 0.002(3) C12B 0.067(4) 0.067(4) 0.172(10) 0.043(6) 0.052(6) 0.015(3) C13 0.057(2) 0.0292(16) 0.056(2) -0.0044(13) 0.0074(16) -0.0017(14) C14 0.056(2) 0.0271(16) 0.063(2) -0.0002(15) 0.0019(15) 0.0040(14) C15 0.062(2) 0.0238(15) 0.0563(19) 0.0033(14) 0.0074(16) 0.0069(14) C16 0.062(2) 0.0261(16) 0.0421(17) -0.0029(13) 0.0116(15) 0.0017(14) C17 0.091(3) 0.0285(16) 0.0398(18) 0.0037(14) 0.0088(17) 0.0006(16) C18 0.106(3) 0.0314(17) 0.0345(17) 0.0035(14) 0.0072(17) 0.0029(17) C19 0.081(2) 0.0330(17) 0.0377(17) -0.0039(13) 0.0123(15) 0.0007(15) C20 0.066(2) 0.0261(15) 0.0324(16) 0.0003(13) 0.0160(14) 0.0013(14) C21 0.0559(19) 0.0297(15) 0.0375(16) -0.0008(13) 0.0098(13) -0.0018(13) C22 0.065(2) 0.0357(17) 0.0284(16) -0.0020(12) 0.0094(13) -0.0032(14) C23 0.063(2) 0.0328(16) 0.0317(16) -0.0020(12) 0.0106(13) -0.0050(14) C24 0.058(2) 0.0251(14) 0.0321(15) 0.0013(11) 0.0065(13) -0.0022(14) C25 0.060(2) 0.0343(17) 0.0386(17) -0.0003(13) 0.0071(14) 0.0013(14) C26 0.065(2) 0.0330(17) 0.0501(19) 0.0013(14) 0.0061(15) 0.0086(15) C27 0.073(2) 0.0235(15) 0.0443(18) 0.0007(12) 0.0044(15) -0.0001(15) C28 0.061(2) 0.0286(16) 0.0433(18) 0.0004(13) 0.0045(14) -0.0043(14) C29 0.055(2) 0.0264(15) 0.0370(16) 0.0040(12) 0.0060(13) -0.0027(13) C30 0.055(2) 0.0453(19) 0.065(2) -0.0015(16) 0.0008(17) 0.0054(15) C31 0.120(2) 0.123(2) 0.123(2) 0.0047(10) -0.0004(10) -0.0019(10) C32 0.080(3) 0.110(3) 0.088(3) -0.022(2) 0.028(2) -0.023(3) C33 0.056(2) 0.0279(15) 0.059(2) 0.0020(14) 0.0062(15) -0.0027(14) C34 0.060(2) 0.0377(17) 0.062(2) -0.0055(15) 0.0136(16) -0.0016(15) C35 0.068(2) 0.068(2) 0.070(2) 0.0208(19) 0.0069(19) 0.0158(19) C36 0.145(4) 0.0325(18) 0.050(2) 0.0062(15) 0.006(2) -0.013(2) C37 0.104(3) 0.0417(19) 0.046(2) -0.0006(15) -0.0050(18) -0.0002(18) N1 0.0500(16) 0.0269(13) 0.0599(17) -0.0058(11) 0.0030(13) 0.0010(11) N2 0.0588(16) 0.0220(12) 0.0451(14) 0.0008(11) 0.0103(12) 0.0008(11) N3 0.0573(16) 0.0247(13) 0.0380(14) 0.0004(10) 0.0099(11) -0.0001(11) N4 0.0593(16) 0.0273(12) 0.0328(13) -0.0016(10) 0.0095(11) -0.0039(11) N5 0.0564(16) 0.0269(12) 0.0327(13) -0.0010(10) 0.0076(11) -0.0031(11) _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 C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C1A N1 1.435(6) . ? C2A C3A 1.3900 . ? C2A C7A 1.529(9) . ? C3A C4A 1.3900 . ? C3A H3A 0.9500 . ? C4A C5A 1.3900 . ? C4A H4A 0.9500 . ? C5A C6A 1.3900 . ? C5A H5A 0.9500 . ? C6A C10A 1.541(10) . ? C7A C8A 1.538(10) . ? C7A C9A 1.539(10) . ? C7A H7A 1.0000 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A C11A 1.542(10) . ? C10A C12A 1.60(4) . ? C10A H10A 1.0000 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B N1 1.441(3) . ? C2B C3B 1.3900 . ? C2B C7B 1.552(5) . ? C3B C4B 1.3900 . ? C3B H3B 0.9500 . ? C4B C5B 1.3900 . ? C4B H4B 0.9500 . ? C5B C6B 1.3900 . ? C5B H5B 0.9500 . ? C6B C10B 1.529(7) . ? C7B C9B 1.527(8) . ? C7B C8B 1.547(9) . ? C7B H7B 1.0000 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B C12B 1.510(12) . ? C10B C11B 1.535(8) . ? C10B H10B 1.0000 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13 N1 1.364(4) . ? C13 N2 1.374(3) . ? C14 C15 1.336(4) . ? C14 N1 1.391(3) . ? C14 H14 0.9500 . ? C15 N2 1.398(4) . ? C15 H15 0.9500 . ? C16 N3 1.329(3) . ? C16 C17 1.391(4) . ? C16 N2 1.424(4) . ? C17 C18 1.396(4) . ? C17 C36 1.507(4) . ? C18 C19 1.387(4) . ? C18 H18 0.9500 . ? C19 C20 1.409(4) . ? C19 C37 1.497(4) . ? C20 N3 1.332(3) . ? C20 N4 1.428(3) . ? C21 N5 1.363(3) . ? C21 N4 1.375(3) . ? C22 C23 1.336(4) . ? C22 N4 1.402(3) . ? C22 H22 0.9500 . ? C23 N5 1.389(3) . ? C23 H23 0.9500 . ? C24 C29 1.399(4) . ? C24 C25 1.407(4) . ? C24 N5 1.452(3) . ? C25 C26 1.398(4) . ? C25 C30 1.511(4) . ? C26 C27 1.373(4) . ? C26 H26 0.9500 . ? C27 C28 1.378(4) . ? C27 H27 0.9500 . ? C28 C29 1.394(4) . ? C28 H28 0.9500 . ? C29 C33 1.519(4) . ? C30 C31 1.492(6) . ? C30 C32 1.521(5) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.524(4) . ? C33 C34 1.532(4) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? 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 C2A C1A C6A 120.0 . . ? C2A C1A N1 114.5(8) . . ? C6A C1A N1 125.5(8) . . ? C1A C2A C3A 120.0 . . ? C1A C2A C7A 118.6(10) . . ? C3A C2A C7A 121.0(10) . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A C10A 120.0(10) . . ? C1A C6A C10A 119.9(10) . . ? C2A C7A C8A 108.7(16) . . ? C2A C7A C9A 113.9(15) . . ? C8A C7A C9A 112(2) . . ? C2A C7A H7A 107.2 . . ? C8A C7A H7A 107.2 . . ? C9A C7A H7A 107.2 . . ? C6A C10A C11A 113.8(14) . . ? C6A C10A C12A 109.0(16) . . ? C11A C10A C12A 105.4(17) . . ? C6A C10A H10A 109.5 . . ? C11A C10A H10A 109.5 . . ? C12A C10A H10A 109.5 . . ? C2B C1B C6B 120.0 . . ? C2B C1B N1 121.2(2) . . ? C6B C1B N1 118.8(2) . . ? C3B C2B C1B 120.0 . . ? C3B C2B C7B 119.2(3) . . ? C1B C2B C7B 120.8(3) . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B H4B 120.0 . . ? C5B C4B H4B 120.0 . . ? C4B C5B C6B 120.0 . . ? C4B C5B H5B 120.0 . . ? C6B C5B H5B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B C10B 120.0(3) . . ? C1B C6B C10B 120.0(3) . . ? C9B C7B C8B 113.0(6) . . ? C9B C7B C2B 111.9(4) . . ? C8B C7B C2B 109.5(5) . . ? C9B C7B H7B 107.4 . . ? C8B C7B H7B 107.4 . . ? C2B C7B H7B 107.4 . . ? C7B C8B H8B1 109.5 . . ? C7B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7B C9B H9B1 109.5 . . ? C7B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C12B C10B C6B 110.8(6) . . ? C12B C10B C11B 108.9(6) . . ? C6B C10B C11B 113.8(5) . . ? C12B C10B H10B 107.7 . . ? C6B C10B H10B 107.7 . . ? C11B C10B H10B 107.7 . . ? C10B C11B H11D 109.5 . . ? C10B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C10B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C10B C12B H12D 109.5 . . ? C10B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C10B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? N1 C13 N2 101.7(2) . . ? C15 C14 N1 106.2(3) . . ? C15 C14 H14 126.9 . . ? N1 C14 H14 126.9 . . ? C14 C15 N2 106.7(2) . . ? C14 C15 H15 126.7 . . ? N2 C15 H15 126.7 . . ? N3 C16 C17 123.9(3) . . ? N3 C16 N2 113.7(2) . . ? C17 C16 N2 122.3(2) . . ? C16 C17 C18 114.4(3) . . ? C16 C17 C36 124.4(3) . . ? C18 C17 C36 121.2(3) . . ? C19 C18 C17 124.7(3) . . ? C19 C18 H18 117.7 . . ? C17 C18 H18 117.7 . . ? C18 C19 C20 114.2(3) . . ? C18 C19 C37 120.8(3) . . ? C20 C19 C37 125.1(3) . . ? N3 C20 C19 123.4(2) . . ? N3 C20 N4 113.2(2) . . ? C19 C20 N4 123.3(3) . . ? N5 C21 N4 101.1(2) . . ? C23 C22 N4 106.1(2) . . ? C23 C22 H22 126.9 . . ? N4 C22 H22 126.9 . . ? C22 C23 N5 106.3(2) . . ? C22 C23 H23 126.9 . . ? N5 C23 H23 126.9 . . ? C29 C24 C25 123.2(2) . . ? C29 C24 N5 118.5(2) . . ? C25 C24 N5 118.3(3) . . ? C26 C25 C24 116.7(3) . . ? C26 C25 C30 121.4(3) . . ? C24 C25 C30 121.9(2) . . ? C27 C26 C25 121.2(3) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 120.7(3) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 121.2(3) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C28 C29 C24 117.0(3) . . ? C28 C29 C33 121.1(3) . . ? C24 C29 C33 121.9(2) . . ? C31 C30 C25 113.1(3) . . ? C31 C30 C32 110.1(4) . . ? C25 C30 C32 111.5(3) . . ? C31 C30 H30 107.3 . . ? C25 C30 H30 107.3 . . ? C32 C30 H30 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 110.9(2) . . ? C29 C33 C34 111.7(2) . . ? C35 C33 C34 110.9(3) . . ? C29 C33 H33 107.7 . . ? C35 C33 H33 107.7 . . ? C34 C33 H33 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C19 C37 H37A 109.5 . . ? C19 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C19 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C13 N1 C14 113.2(2) . . ? C13 N1 C1A 118.6(7) . . ? C14 N1 C1A 127.2(8) . . ? C13 N1 C1B 123.1(3) . . ? C14 N1 C1B 122.7(3) . . ? C13 N2 C15 112.2(3) . . ? C13 N2 C16 124.7(2) . . ? C15 N2 C16 123.1(2) . . ? C16 N3 C20 119.5(2) . . ? C21 N4 C22 112.8(2) . . ? C21 N4 C20 125.7(2) . . ? C22 N4 C20 121.4(2) . . ? C21 N5 C23 113.7(2) . . ? C21 N5 C24 123.3(2) . . ? C23 N5 C24 123.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A C1A C2A C3A 0.0 . . . . ? N1 C1A C2A C3A -178.8(14) . . . . ? C6A C1A C2A C7A -173.3(16) . . . . ? N1 C1A C2A C7A 7.8(14) . . . . ? C1A C2A C3A C4A 0.0 . . . . ? C7A C2A C3A C4A 173.1(16) . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C1A 0.0 . . . . ? C4A C5A C6A C10A -177.6(16) . . . . ? C2A C1A C6A C5A 0.0 . . . . ? N1 C1A C6A C5A 178.7(15) . . . . ? C2A C1A C6A C10A 177.6(16) . . . . ? N1 C1A C6A C10A -3.7(16) . . . . ? C1A C2A C7A C8A -98.6(16) . . . . ? C3A C2A C7A C8A 88.2(18) . . . . ? C1A C2A C7A C9A 135.4(16) . . . . ? C3A C2A C7A C9A -38(2) . . . . ? C5A C6A C10A C11A 26(2) . . . . ? C1A C6A C10A C11A -151.5(15) . . . . ? C5A C6A C10A C12A -91.2(17) . . . . ? C1A C6A C10A C12A 91.2(17) . . . . ? C6B C1B C2B C3B 0.0 . . . . ? N1 C1B C2B C3B -178.3(5) . . . . ? C6B C1B C2B C7B 177.8(5) . . . . ? N1 C1B C2B C7B -0.5(5) . . . . ? C1B C2B C3B C4B 0.0 . . . . ? C7B C2B C3B C4B -177.9(5) . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C4B C5B C6B C1B 0.0 . . . . ? C4B C5B C6B C10B 179.9(5) . . . . ? C2B C1B C6B C5B 0.0 . . . . ? N1 C1B C6B C5B 178.4(5) . . . . ? C2B C1B C6B C10B -179.9(5) . . . . ? N1 C1B C6B C10B -1.5(6) . . . . ? C3B C2B C7B C9B -46.9(6) . . . . ? C1B C2B C7B C9B 135.3(4) . . . . ? C3B C2B C7B C8B 79.2(5) . . . . ? C1B C2B C7B C8B -98.6(5) . . . . ? C5B C6B C10B C12B -92.7(6) . . . . ? C1B C6B C10B C12B 87.2(6) . . . . ? C5B C6B C10B C11B 30.4(8) . . . . ? C1B C6B C10B C11B -149.7(5) . . . . ? N1 C14 C15 N2 0.0(3) . . . . ? N3 C16 C17 C18 -0.8(5) . . . . ? N2 C16 C17 C18 -178.8(3) . . . . ? N3 C16 C17 C36 177.9(3) . . . . ? N2 C16 C17 C36 -0.1(5) . . . . ? C16 C17 C18 C19 0.5(5) . . . . ? C36 C17 C18 C19 -178.3(3) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C17 C18 C19 C37 -180.0(3) . . . . ? C18 C19 C20 N3 0.0(4) . . . . ? C37 C19 C20 N3 179.9(3) . . . . ? C18 C19 C20 N4 -177.9(3) . . . . ? C37 C19 C20 N4 2.0(5) . . . . ? N4 C22 C23 N5 -0.2(3) . . . . ? C29 C24 C25 C26 -1.0(4) . . . . ? N5 C24 C25 C26 -179.6(2) . . . . ? C29 C24 C25 C30 -179.9(3) . . . . ? N5 C24 C25 C30 1.4(4) . . . . ? C24 C25 C26 C27 1.1(4) . . . . ? C30 C25 C26 C27 -180.0(3) . . . . ? C25 C26 C27 C28 -0.4(4) . . . . ? C26 C27 C28 C29 -0.3(4) . . . . ? C27 C28 C29 C24 0.4(4) . . . . ? C27 C28 C29 C33 -178.5(3) . . . . ? C25 C24 C29 C28 0.3(4) . . . . ? N5 C24 C29 C28 178.9(2) . . . . ? C25 C24 C29 C33 179.2(2) . . . . ? N5 C24 C29 C33 -2.2(4) . . . . ? C26 C25 C30 C31 52.4(4) . . . . ? C24 C25 C30 C31 -128.7(4) . . . . ? C26 C25 C30 C32 -72.3(4) . . . . ? C24 C25 C30 C32 106.6(3) . . . . ? C28 C29 C33 C35 73.9(3) . . . . ? C24 C29 C33 C35 -105.0(3) . . . . ? C28 C29 C33 C34 -50.4(4) . . . . ? C24 C29 C33 C34 130.7(3) . . . . ? N2 C13 N1 C14 0.6(3) . . . . ? N2 C13 N1 C1A -168.7(6) . . . . ? N2 C13 N1 C1B 169.7(3) . . . . ? C15 C14 N1 C13 -0.3(4) . . . . ? C15 C14 N1 C1A 167.8(7) . . . . ? C15 C14 N1 C1B -169.5(3) . . . . ? C2A C1A N1 C13 -101.6(8) . . . . ? C6A C1A N1 C13 79.6(12) . . . . ? C2A C1A N1 C14 90.7(9) . . . . ? C6A C1A N1 C14 -88.0(11) . . . . ? C2A C1A N1 C1B 7(2) . . . . ? C6A C1A N1 C1B -171(4) . . . . ? C2B C1B N1 C13 -88.1(4) . . . . ? C6B C1B N1 C13 93.5(4) . . . . ? C2B C1B N1 C14 80.0(4) . . . . ? C6B C1B N1 C14 -98.4(4) . . . . ? C2B C1B N1 C1A -170(3) . . . . ? C6B C1B N1 C1A 11(3) . . . . ? N1 C13 N2 C15 -0.6(3) . . . . ? N1 C13 N2 C16 -177.2(2) . . . . ? C14 C15 N2 C13 0.4(3) . . . . ? C14 C15 N2 C16 177.1(3) . . . . ? N3 C16 N2 C13 144.8(3) . . . . ? C17 C16 N2 C13 -37.1(4) . . . . ? N3 C16 N2 C15 -31.5(4) . . . . ? C17 C16 N2 C15 146.6(3) . . . . ? C17 C16 N3 C20 0.8(4) . . . . ? N2 C16 N3 C20 178.8(2) . . . . ? C19 C20 N3 C16 -0.3(4) . . . . ? N4 C20 N3 C16 177.8(2) . . . . ? N5 C21 N4 C22 -0.4(3) . . . . ? N5 C21 N4 C20 -176.6(3) . . . . ? C23 C22 N4 C21 0.4(3) . . . . ? C23 C22 N4 C20 176.9(3) . . . . ? N3 C20 N4 C21 149.5(3) . . . . ? C19 C20 N4 C21 -32.4(4) . . . . ? N3 C20 N4 C22 -26.5(4) . . . . ? C19 C20 N4 C22 151.6(3) . . . . ? N4 C21 N5 C23 0.2(3) . . . . ? N4 C21 N5 C24 -178.7(2) . . . . ? C22 C23 N5 C21 0.0(3) . . . . ? C22 C23 N5 C24 178.9(3) . . . . ? C29 C24 N5 C21 89.2(3) . . . . ? C25 C24 N5 C21 -92.1(3) . . . . ? C29 C24 N5 C23 -89.6(3) . . . . ? C25 C24 N5 C23 89.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.427 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.050 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.005 -0.037 1008.2 -8.4 _platon_squeeze_details ; ; #==END data_3BrBr _database_code_depnum_ccdc_archive 'CCDC 663957' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Br2 N5 Ni, (C H2 Cl2)' _chemical_formula_sum 'C36 H43 Br2 Cl2 N5 Ni' _chemical_formula_weight 835.18 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7728(5) _cell_length_b 13.6700(5) _cell_length_c 25.2292(10) _cell_angle_alpha 87.286(2) _cell_angle_beta 75.428(2) _cell_angle_gamma 71.776(2) _cell_volume 4047.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16970 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 2.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8180 _exptl_absorpt_correction_T_max 0.9495 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69924 _diffrn_reflns_av_R_equivalents 0.1227 _diffrn_reflns_av_sigmaI/netI 0.1810 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.73 _reflns_number_total 18589 _reflns_number_gt 9474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'enCIFer (2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains one highly disordered molecule of DCM - attempts to satisfactorily model this failed. As a result it was removed using the squeeze algorithm ( P. v.d. Sluis and A. L. Spek, Acta Crystallogr., Sect A 1990, 46, 194-201.). This treatment explains the following checkCIF alerts: PLAT602_ALERT_4_C, PLAT049_ALERT_1_B. ; _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^)+(0.0702P)^2^+6.5178P] 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 18589 _refine_ls_number_parameters 846 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1837 _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7395(6) 0.5068(5) 0.1384(3) 0.0218(16) Uani 1 1 d . . . C2 C 0.7797(6) 0.5928(5) 0.1273(3) 0.0249(17) Uani 1 1 d . . . C3 C 0.7615(6) 0.6593(6) 0.1694(3) 0.0324(19) Uani 1 1 d . . . H3 H 0.7884 0.7173 0.1627 0.039 Uiso 1 1 calc R . . C4 C 0.7036(7) 0.6435(6) 0.2228(3) 0.036(2) Uani 1 1 d . . . H4 H 0.6901 0.6913 0.2518 0.043 Uiso 1 1 calc R . . C5 C 0.6666(6) 0.5582(6) 0.2327(3) 0.0335(19) Uani 1 1 d . . . H5 H 0.6281 0.5475 0.2689 0.040 Uiso 1 1 calc R . . C6 C 0.6846(6) 0.4870(5) 0.1905(3) 0.0291(18) Uani 1 1 d . . . C7 C 0.8410(7) 0.6093(6) 0.0696(3) 0.0322(19) Uani 1 1 d . . . H7 H 0.8376 0.5555 0.0452 0.039 Uiso 1 1 calc R . . C8 C 0.9673(7) 0.5931(6) 0.0660(3) 0.045(2) Uani 1 1 d . . . H8A H 0.9737 0.6446 0.0898 0.068 Uiso 1 1 calc R . . H8B H 1.0067 0.6005 0.0281 0.068 Uiso 1 1 calc R . . H8C H 1.0020 0.5239 0.0779 0.068 Uiso 1 1 calc R . . C9 C 0.7829(7) 0.7145(6) 0.0492(3) 0.039(2) Uani 1 1 d . . . H9A H 0.7026 0.7220 0.0527 0.059 Uiso 1 1 calc R . . H9B H 0.8204 0.7197 0.0106 0.059 Uiso 1 1 calc R . . H9C H 0.7885 0.7691 0.0711 0.059 Uiso 1 1 calc R . . C10 C 0.6472(6) 0.3919(6) 0.2027(3) 0.0295(18) Uani 1 1 d . . . H10 H 0.6719 0.3505 0.1676 0.035 Uiso 1 1 calc R . . C11 C 0.5180(7) 0.4173(6) 0.2223(3) 0.038(2) Uani 1 1 d . . . H11A H 0.4910 0.4547 0.2578 0.057 Uiso 1 1 calc R . . H11B H 0.4979 0.3533 0.2261 0.057 Uiso 1 1 calc R . . H11C H 0.4821 0.4602 0.1955 0.057 Uiso 1 1 calc R . . C12 C 0.7079(7) 0.3254(6) 0.2429(3) 0.045(2) Uani 1 1 d . . . H12A H 0.7896 0.3164 0.2308 0.068 Uiso 1 1 calc R . . H12B H 0.6957 0.2579 0.2444 0.068 Uiso 1 1 calc R . . H12C H 0.6774 0.3592 0.2794 0.068 Uiso 1 1 calc R . . C13 C 0.8359(6) 0.3563(5) 0.0700(3) 0.0205(15) Uani 1 1 d . . . C14 C 0.6655(6) 0.4629(5) 0.0646(3) 0.0270(17) Uani 1 1 d . . . H14 H 0.5964 0.5183 0.0735 0.032 Uiso 1 1 calc R . . C15 C 0.6971(6) 0.3950(5) 0.0230(3) 0.0247(17) Uani 1 1 d . . . H15 H 0.6565 0.3915 -0.0033 0.030 Uiso 1 1 calc R . . C16 C 0.8751(6) 0.2434(5) -0.0040(3) 0.0213(16) Uani 1 1 d . . . C17 C 0.8667(6) 0.2056(5) -0.0513(3) 0.0255(17) Uani 1 1 d . . . H17 H 0.8034 0.2370 -0.0663 0.031 Uiso 1 1 calc R . . C18 C 0.9543(6) 0.1194(6) -0.0769(3) 0.0313(18) Uani 1 1 d . . . H18 H 0.9507 0.0916 -0.1099 0.038 Uiso 1 1 calc R . . C19 C 1.0467(6) 0.0733(6) -0.0549(3) 0.0282(18) Uani 1 1 d . . . H19 H 1.1062 0.0138 -0.0717 0.034 Uiso 1 1 calc R . . C20 C 1.0473(6) 0.1182(5) -0.0078(3) 0.0247(17) Uani 1 1 d . . . C21 C 1.1128(6) 0.1468(5) 0.0681(3) 0.0214(16) Uani 1 1 d . . . C22 C 1.2288(6) 0.0048(6) 0.0148(3) 0.0286(18) Uani 1 1 d . . . H22 H 1.2578 -0.0460 -0.0141 0.034 Uiso 1 1 calc R . . C23 C 1.2750(6) 0.0111(5) 0.0552(3) 0.0303(18) Uani 1 1 d . . . H23 H 1.3436 -0.0353 0.0613 0.036 Uiso 1 1 calc R . . C24 C 1.2348(6) 0.1353(6) 0.1337(3) 0.0280(18) Uani 1 1 d . . . C25 C 1.3120(6) 0.1905(6) 0.1220(3) 0.0300(18) Uani 1 1 d . . . C26 C 1.3444(7) 0.2211(6) 0.1661(3) 0.037(2) Uani 1 1 d . . . H26 H 1.3974 0.2586 0.1600 0.044 Uiso 1 1 calc R . . C27 C 1.2981(7) 0.1958(6) 0.2186(3) 0.043(2) Uani 1 1 d . . . H27 H 1.3201 0.2165 0.2484 0.052 Uiso 1 1 calc R . . C28 C 1.2207(7) 0.1413(6) 0.2289(3) 0.039(2) Uani 1 1 d . . . H28 H 1.1901 0.1259 0.2656 0.046 Uiso 1 1 calc R . . C29 C 1.1874(6) 0.1090(6) 0.1868(3) 0.034(2) Uani 1 1 d . . . C30 C 1.3589(7) 0.2216(6) 0.0643(3) 0.0339(19) Uani 1 1 d . . . H30 H 1.3164 0.2029 0.0401 0.041 Uiso 1 1 calc R . . C31 C 1.4835(8) 0.1619(7) 0.0424(4) 0.056(3) Uani 1 1 d . . . H31A H 1.5252 0.1648 0.0697 0.084 Uiso 1 1 calc R . . H31B H 1.5145 0.1922 0.0085 0.084 Uiso 1 1 calc R . . H31C H 1.4912 0.0899 0.0349 0.084 Uiso 1 1 calc R . . C32 C 1.3384(9) 0.3378(6) 0.0607(4) 0.055(3) Uani 1 1 d . . . H32A H 1.2564 0.3739 0.0698 0.083 Uiso 1 1 calc R . . H32B H 1.3730 0.3538 0.0234 0.083 Uiso 1 1 calc R . . H32C H 1.3728 0.3602 0.0866 0.083 Uiso 1 1 calc R . . C33 C 1.1005(7) 0.0510(6) 0.1982(3) 0.040(2) Uani 1 1 d . . . H33 H 1.0690 0.0567 0.1653 0.048 Uiso 1 1 calc R . . C34 C 1.1559(7) -0.0639(6) 0.2059(4) 0.048(2) Uani 1 1 d . . . H34A H 1.2151 -0.0940 0.1728 0.073 Uiso 1 1 calc R . . H34B H 1.0979 -0.0991 0.2127 0.073 Uiso 1 1 calc R . . H34C H 1.1899 -0.0720 0.2373 0.073 Uiso 1 1 calc R . . C35 C 1.0004(7) 0.0969(7) 0.2475(4) 0.054(3) Uani 1 1 d . . . H35A H 1.0277 0.0877 0.2810 0.081 Uiso 1 1 calc R . . H35B H 0.9431 0.0617 0.2507 0.081 Uiso 1 1 calc R . . H35C H 0.9665 0.1705 0.2425 0.081 Uiso 1 1 calc R . . C36 C 0.4292(7) 0.1598(5) 0.3954(3) 0.0287(18) Uani 1 1 d . . . C37 C 0.5089(7) 0.1460(6) 0.4261(3) 0.038(2) Uani 1 1 d . . . C38 C 0.4648(9) 0.1892(7) 0.4799(4) 0.050(2) Uani 1 1 d . . . H38 H 0.5148 0.1805 0.5032 0.060 Uiso 1 1 calc R . . C39 C 0.3524(10) 0.2431(7) 0.4994(4) 0.057(3) Uani 1 1 d . . . H39 H 0.3256 0.2728 0.5355 0.068 Uiso 1 1 calc R . . C40 C 0.2777(8) 0.2544(7) 0.4667(3) 0.047(2) Uani 1 1 d . . . H40 H 0.1993 0.2906 0.4810 0.057 Uiso 1 1 calc R . . C41 C 0.3147(7) 0.2139(6) 0.4131(3) 0.037(2) Uani 1 1 d . . . C42 C 0.6328(7) 0.0868(7) 0.4049(4) 0.047(2) Uani 1 1 d . . . H42 H 0.6450 0.0645 0.3661 0.056 Uiso 1 1 calc R . . C43 C 0.6647(10) -0.0088(7) 0.4374(4) 0.076(4) Uani 1 1 d . . . H43A H 0.6547 0.0110 0.4756 0.114 Uiso 1 1 calc R . . H43B H 0.7444 -0.0488 0.4217 0.114 Uiso 1 1 calc R . . H43C H 0.6157 -0.0507 0.4359 0.114 Uiso 1 1 calc R . . C44 C 0.7088(9) 0.1556(9) 0.4054(6) 0.102(5) Uani 1 1 d . . . H44A H 0.6834 0.2184 0.3855 0.154 Uiso 1 1 calc R . . H44B H 0.7881 0.1178 0.3876 0.154 Uiso 1 1 calc R . . H44C H 0.7029 0.1740 0.4433 0.154 Uiso 1 1 calc R . . C45 C 0.2340(7) 0.2334(7) 0.3760(3) 0.044(2) Uani 1 1 d . . . H45 H 0.2683 0.1815 0.3447 0.053 Uiso 1 1 calc R . . C46 C 0.1180(8) 0.2227(8) 0.4066(4) 0.066(3) Uani 1 1 d . . . H46A H 0.0791 0.2786 0.4344 0.100 Uiso 1 1 calc R . . H46B H 0.1295 0.1563 0.4245 0.100 Uiso 1 1 calc R . . H46C H 0.0716 0.2265 0.3806 0.100 Uiso 1 1 calc R . . C47 C 0.2171(8) 0.3398(7) 0.3533(4) 0.060(3) Uani 1 1 d . . . H47A H 0.1859 0.3913 0.3836 0.090 Uiso 1 1 calc R . . H47B H 0.1641 0.3520 0.3298 0.090 Uiso 1 1 calc R . . H47C H 0.2904 0.3452 0.3317 0.090 Uiso 1 1 calc R . . C48 C 0.4653(6) 0.0422(6) 0.3125(3) 0.0299(18) Uani 1 1 d . . . C49 C 0.5287(6) 0.1798(6) 0.3001(3) 0.0307(18) Uani 1 1 d . . . H49 H 0.5434 0.2407 0.3082 0.037 Uiso 1 1 calc R . . C50 C 0.5577(6) 0.1331(6) 0.2510(3) 0.0334(19) Uani 1 1 d . . . H50 H 0.5976 0.1536 0.2175 0.040 Uiso 1 1 calc R . . C51 C 0.5162(6) -0.0193(5) 0.2204(3) 0.0249(17) Uani 1 1 d . . . C52 C 0.5553(6) -0.0221(6) 0.1646(3) 0.0303(18) Uani 1 1 d . . . H52 H 0.5920 0.0251 0.1463 0.036 Uiso 1 1 calc R . . C53 C 0.5380(6) -0.0981(6) 0.1363(3) 0.0326(19) Uani 1 1 d . . . H53 H 0.5633 -0.1021 0.0974 0.039 Uiso 1 1 calc R . . C54 C 0.4859(7) -0.1678(6) 0.1620(3) 0.0333(19) Uani 1 1 d . . . H54 H 0.4750 -0.2194 0.1420 0.040 Uiso 1 1 calc R . . C55 C 0.4505(6) -0.1587(5) 0.2184(3) 0.0271(17) Uani 1 1 d . . . C56 C 0.3673(6) -0.1936(6) 0.3096(3) 0.0284(18) Uani 1 1 d . . . C57 C 0.3557(6) -0.2983(5) 0.2445(3) 0.0263(17) Uani 1 1 d . . . H57 H 0.3634 -0.3279 0.2098 0.032 Uiso 1 1 calc R . . C58 C 0.3053(6) -0.3249(6) 0.2934(3) 0.0314(18) Uani 1 1 d . . . H58 H 0.2703 -0.3776 0.3005 0.038 Uiso 1 1 calc R . . C59 C 0.2693(7) -0.2709(6) 0.3908(3) 0.0321(19) Uani 1 1 d . . . C60 C 0.3333(7) -0.3484(6) 0.4182(3) 0.0330(19) Uani 1 1 d . . . C61 C 0.2846(8) -0.3576(7) 0.4740(3) 0.052(2) Uani 1 1 d . . . H61 H 0.3252 -0.4098 0.4941 0.062 Uiso 1 1 calc R . . C62 C 0.1811(8) -0.2938(7) 0.4995(3) 0.051(2) Uani 1 1 d . . . H62 H 0.1505 -0.3017 0.5373 0.061 Uiso 1 1 calc R . . C63 C 0.1194(8) -0.2176(7) 0.4718(3) 0.052(2) Uani 1 1 d . . . H63 H 0.0470 -0.1735 0.4907 0.062 Uiso 1 1 calc R . . C64 C 0.1619(7) -0.2039(6) 0.4158(3) 0.038(2) Uani 1 1 d . . . C65 C 0.4516(7) -0.4174(6) 0.3901(3) 0.042(2) Uani 1 1 d . . . H65 H 0.4627 -0.4068 0.3498 0.050 Uiso 1 1 calc R . . C66 C 0.4653(9) -0.5313(8) 0.3992(4) 0.074(3) Uani 1 1 d . . . H66A H 0.4598 -0.5453 0.4381 0.111 Uiso 1 1 calc R . . H66B H 0.5398 -0.5730 0.3774 0.111 Uiso 1 1 calc R . . H66C H 0.4051 -0.5490 0.3880 0.111 Uiso 1 1 calc R . . C67 C 0.5415(8) -0.3861(8) 0.4078(5) 0.076(3) Uani 1 1 d . . . H67A H 0.5332 -0.3137 0.3995 0.114 Uiso 1 1 calc R . . H67B H 0.6172 -0.4294 0.3881 0.114 Uiso 1 1 calc R . . H67C H 0.5324 -0.3949 0.4473 0.114 Uiso 1 1 calc R . . C68 C 0.0933(7) -0.1213(7) 0.3858(3) 0.048(2) Uani 1 1 d . . . H68 H 0.1489 -0.1015 0.3551 0.058 Uiso 1 1 calc R . . C69 C 0.0204(9) -0.1607(8) 0.3603(4) 0.080(4) Uani 1 1 d . . . H69A H 0.0686 -0.2177 0.3343 0.121 Uiso 1 1 calc R . . H69B H -0.0228 -0.1051 0.3408 0.121 Uiso 1 1 calc R . . H69C H -0.0324 -0.1851 0.3888 0.121 Uiso 1 1 calc R . . C70 C 0.0227(8) -0.0228(7) 0.4209(4) 0.065(3) Uani 1 1 d . . . H70A H -0.0050 0.0330 0.3972 0.098 Uiso 1 1 calc R . . H70B H 0.0703 -0.0031 0.4407 0.098 Uiso 1 1 calc R . . H70C H -0.0423 -0.0354 0.4472 0.098 Uiso 1 1 calc R . . C71 C 0.1676(8) 0.5502(7) 0.1727(4) 0.059(3) Uani 1 1 d . . . H71A H 0.1301 0.5093 0.1571 0.071 Uiso 1 1 calc R . . H71B H 0.2364 0.5526 0.1445 0.071 Uiso 1 1 calc R . . C72 C 0.9150(11) 0.4457(12) 0.2926(5) 0.121(6) Uani 1 1 d . . . H72A H 0.9984 0.4162 0.2779 0.145 Uiso 1 1 calc R . . H72B H 0.8785 0.4528 0.2617 0.145 Uiso 1 1 calc R . . N1 N 0.7493(5) 0.4398(4) 0.0929(2) 0.0251(14) Uani 1 1 d . . . N2 N 0.8024(5) 0.3309(4) 0.0268(2) 0.0210(13) Uani 1 1 d . . . N3 N 0.9656(5) 0.2016(4) 0.0168(2) 0.0225(13) Uani 1 1 d . . . N4 N 1.1311(5) 0.0860(4) 0.0228(2) 0.0237(14) Uani 1 1 d . . . N5 N 1.2037(5) 0.0997(4) 0.0879(2) 0.0268(14) Uani 1 1 d . . . N6 N 0.4728(5) 0.1228(5) 0.3374(2) 0.0312(15) Uani 1 1 d . . . N7 N 0.5190(5) 0.0503(4) 0.2585(2) 0.0262(14) Uani 1 1 d . . . N8 N 0.4651(5) -0.0860(5) 0.2465(2) 0.0252(14) Uani 1 1 d . . . N9 N 0.3940(5) -0.2192(4) 0.2543(2) 0.0264(14) Uani 1 1 d . . . N10 N 0.3140(5) -0.2600(4) 0.3326(2) 0.0269(14) Uani 1 1 d . . . Ni1 Ni 0.97711(8) 0.26237(7) 0.07915(3) 0.0235(2) Uani 1 1 d . . . Ni2 Ni 0.41129(8) -0.07575(7) 0.32289(4) 0.0263(2) Uani 1 1 d . . . Br1 Br 1.00091(7) 0.34521(6) 0.14952(3) 0.0327(2) Uani 1 1 d . . . Br2 Br 0.35197(8) -0.06426(7) 0.41528(3) 0.0396(2) Uani 1 1 d . . . Br3 Br 0.72606(8) 0.15085(6) 0.11426(3) 0.0408(2) Uani 1 1 d . . . Br4 Br 0.39012(7) 0.66165(6) 0.09724(3) 0.0383(2) Uani 1 1 d . . . Cl1 Cl 0.0748(3) 0.6754(2) 0.18839(13) 0.0846(9) Uani 1 1 d . . . Cl2 Cl 0.2079(2) 0.4898(2) 0.22968(12) 0.0721(8) Uani 1 1 d . . . Cl3 Cl 0.8830(5) 0.5659(4) 0.3240(2) 0.173(2) Uani 1 1 d U . . Cl4 Cl 0.8652(4) 0.3642(3) 0.34093(17) 0.1322(15) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.019(4) 0.020(4) 0.028(4) 0.001(3) -0.010(3) -0.003(3) C2 0.014(4) 0.033(4) 0.022(4) 0.005(3) -0.003(3) -0.001(3) C3 0.035(5) 0.032(5) 0.033(4) -0.002(4) -0.009(4) -0.014(4) C4 0.038(5) 0.045(5) 0.030(4) -0.001(4) -0.014(4) -0.015(4) C5 0.033(5) 0.038(5) 0.021(4) -0.006(4) 0.003(3) -0.006(4) C6 0.021(4) 0.026(4) 0.033(4) 0.007(3) -0.003(3) -0.002(3) C7 0.036(5) 0.038(5) 0.030(4) 0.005(4) -0.006(4) -0.025(4) C8 0.035(5) 0.048(5) 0.047(5) 0.015(4) -0.005(4) -0.010(4) C9 0.036(5) 0.030(5) 0.047(5) 0.002(4) -0.009(4) -0.005(4) C10 0.029(4) 0.031(5) 0.024(4) -0.001(3) -0.001(3) -0.007(4) C11 0.036(5) 0.029(5) 0.043(5) 0.008(4) -0.008(4) -0.005(4) C12 0.033(5) 0.047(5) 0.057(6) 0.019(4) -0.013(4) -0.016(4) C13 0.018(4) 0.020(4) 0.024(4) 0.003(3) 0.000(3) -0.009(3) C14 0.020(4) 0.033(5) 0.025(4) 0.005(3) -0.013(3) 0.002(3) C15 0.019(4) 0.035(4) 0.021(4) 0.004(3) -0.010(3) -0.006(3) C16 0.022(4) 0.028(4) 0.016(3) 0.009(3) -0.002(3) -0.015(3) C17 0.013(4) 0.034(4) 0.026(4) 0.007(3) -0.008(3) -0.002(3) C18 0.027(4) 0.048(5) 0.028(4) 0.003(4) -0.012(4) -0.020(4) C19 0.020(4) 0.031(4) 0.028(4) -0.001(3) -0.001(3) -0.004(3) C20 0.022(4) 0.028(4) 0.019(4) 0.002(3) -0.001(3) -0.004(3) C21 0.024(4) 0.026(4) 0.013(3) 0.002(3) -0.005(3) -0.006(3) C22 0.033(5) 0.029(4) 0.020(4) -0.007(3) -0.004(3) -0.005(4) C23 0.024(4) 0.022(4) 0.036(4) 0.003(3) -0.007(4) 0.006(3) C24 0.022(4) 0.033(5) 0.021(4) -0.005(3) -0.006(3) 0.005(4) C25 0.026(4) 0.034(5) 0.026(4) 0.002(3) -0.011(3) -0.001(4) C26 0.044(5) 0.036(5) 0.039(5) 0.004(4) -0.022(4) -0.015(4) C27 0.040(5) 0.055(6) 0.034(5) -0.002(4) -0.029(4) 0.001(4) C28 0.037(5) 0.044(5) 0.031(5) 0.005(4) -0.005(4) -0.010(4) C29 0.024(4) 0.038(5) 0.029(4) -0.004(4) -0.010(4) 0.010(4) C30 0.034(5) 0.040(5) 0.033(4) 0.000(4) -0.017(4) -0.013(4) C31 0.048(6) 0.062(6) 0.040(5) -0.004(5) 0.010(5) -0.007(5) C32 0.072(7) 0.048(6) 0.043(5) 0.006(4) -0.003(5) -0.025(5) C33 0.033(5) 0.049(6) 0.029(4) 0.005(4) -0.005(4) -0.005(4) C34 0.035(5) 0.052(6) 0.056(6) 0.001(5) -0.008(5) -0.012(4) C35 0.037(5) 0.062(6) 0.060(6) 0.009(5) -0.004(5) -0.018(5) C36 0.036(5) 0.028(4) 0.018(4) -0.004(3) -0.004(3) -0.006(4) C37 0.043(5) 0.039(5) 0.034(5) 0.002(4) -0.021(4) -0.010(4) C38 0.064(7) 0.045(6) 0.046(6) -0.007(4) -0.033(5) -0.010(5) C39 0.095(9) 0.043(6) 0.031(5) 0.001(4) -0.027(6) -0.010(6) C40 0.043(6) 0.061(6) 0.029(5) -0.002(4) -0.006(4) -0.005(5) C41 0.035(5) 0.056(6) 0.023(4) 0.005(4) -0.011(4) -0.015(4) C42 0.038(5) 0.062(6) 0.053(6) 0.005(5) -0.031(5) -0.018(5) C43 0.100(9) 0.065(7) 0.041(6) -0.013(5) -0.033(6) 0.020(6) C44 0.040(7) 0.092(9) 0.187(15) -0.023(9) -0.048(8) -0.018(6) C45 0.022(5) 0.061(6) 0.041(5) -0.009(4) -0.001(4) -0.004(4) C46 0.048(6) 0.085(8) 0.063(7) 0.006(6) -0.006(5) -0.023(6) C47 0.055(7) 0.066(7) 0.063(7) 0.016(5) -0.029(5) -0.014(5) C48 0.022(4) 0.037(5) 0.029(4) -0.003(4) -0.013(3) -0.001(4) C49 0.034(5) 0.040(5) 0.021(4) -0.001(4) -0.006(3) -0.015(4) C50 0.032(5) 0.038(5) 0.027(4) 0.001(4) -0.003(4) -0.009(4) C51 0.028(4) 0.026(4) 0.015(4) 0.005(3) -0.001(3) -0.004(3) C52 0.027(4) 0.036(5) 0.028(4) 0.006(4) -0.003(3) -0.013(4) C53 0.034(5) 0.034(5) 0.019(4) 0.002(3) -0.008(4) 0.005(4) C54 0.039(5) 0.039(5) 0.022(4) 0.004(4) -0.006(4) -0.013(4) C55 0.025(4) 0.026(4) 0.031(4) 0.008(3) -0.014(4) -0.004(3) C56 0.024(4) 0.036(5) 0.024(4) 0.006(3) -0.012(3) -0.004(4) C57 0.030(4) 0.022(4) 0.029(4) -0.004(3) -0.008(4) -0.009(3) C58 0.036(5) 0.032(5) 0.031(4) -0.001(4) -0.005(4) -0.020(4) C59 0.031(5) 0.048(5) 0.022(4) 0.005(4) -0.002(4) -0.024(4) C60 0.036(5) 0.042(5) 0.024(4) 0.006(4) -0.006(4) -0.017(4) C61 0.063(7) 0.064(6) 0.026(5) 0.017(4) -0.015(5) -0.017(5) C62 0.058(7) 0.065(7) 0.024(4) 0.013(4) 0.001(5) -0.022(5) C63 0.043(6) 0.069(7) 0.036(5) -0.003(5) -0.002(4) -0.013(5) C64 0.042(5) 0.048(5) 0.031(5) 0.004(4) -0.012(4) -0.024(4) C65 0.044(6) 0.048(6) 0.027(4) 0.011(4) -0.015(4) -0.003(4) C66 0.072(8) 0.072(8) 0.055(7) -0.001(6) 0.006(6) -0.007(6) C67 0.034(6) 0.090(8) 0.093(9) -0.012(7) -0.015(6) -0.004(6) C68 0.036(5) 0.064(6) 0.038(5) 0.001(5) -0.005(4) -0.009(5) C69 0.077(8) 0.083(8) 0.082(8) -0.017(6) -0.043(7) -0.006(7) C70 0.053(7) 0.060(7) 0.076(7) -0.010(6) -0.024(6) 0.000(5) C71 0.059(7) 0.058(6) 0.055(6) -0.003(5) -0.010(5) -0.014(5) C72 0.071(9) 0.176(15) 0.066(8) 0.006(9) -0.013(7) 0.027(9) N1 0.025(3) 0.030(4) 0.024(3) 0.003(3) -0.013(3) -0.009(3) N2 0.019(3) 0.029(3) 0.020(3) -0.003(3) -0.008(3) -0.010(3) N3 0.023(3) 0.030(4) 0.016(3) -0.001(3) -0.005(3) -0.009(3) N4 0.020(3) 0.023(3) 0.023(3) 0.000(3) -0.004(3) 0.000(3) N5 0.029(4) 0.032(4) 0.019(3) 0.006(3) -0.009(3) -0.007(3) N6 0.034(4) 0.039(4) 0.021(3) 0.005(3) -0.004(3) -0.014(3) N7 0.029(4) 0.033(4) 0.018(3) -0.001(3) -0.001(3) -0.015(3) N8 0.016(3) 0.040(4) 0.019(3) 0.002(3) -0.004(3) -0.009(3) N9 0.028(4) 0.025(4) 0.018(3) 0.000(3) -0.004(3) 0.003(3) N10 0.029(4) 0.035(4) 0.019(3) 0.000(3) -0.006(3) -0.014(3) Ni1 0.0210(5) 0.0274(5) 0.0198(5) 0.0009(4) -0.0067(4) -0.0032(4) Ni2 0.0263(5) 0.0362(6) 0.0175(5) 0.0022(4) -0.0066(4) -0.0105(5) Br1 0.0298(4) 0.0363(5) 0.0306(4) -0.0039(3) -0.0132(4) -0.0031(4) Br2 0.0498(6) 0.0534(6) 0.0202(4) 0.0018(4) -0.0074(4) -0.0235(4) Br3 0.0484(6) 0.0350(5) 0.0302(4) -0.0033(4) 0.0089(4) -0.0147(4) Br4 0.0284(5) 0.0531(5) 0.0302(4) -0.0097(4) -0.0136(4) -0.0014(4) Cl1 0.071(2) 0.074(2) 0.090(2) 0.0179(16) -0.0140(17) -0.0022(16) Cl2 0.076(2) 0.0619(17) 0.089(2) 0.0133(15) -0.0424(17) -0.0205(15) Cl3 0.189(5) 0.168(4) 0.156(4) 0.013(3) -0.035(4) -0.053(4) Cl4 0.145(4) 0.167(4) 0.108(3) 0.030(3) -0.072(3) -0.053(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 C1 C6 1.383(9) . ? C1 C2 1.412(10) . ? C1 N1 1.459(8) . ? C2 C3 1.359(9) . ? C2 C7 1.512(9) . ? C3 C4 1.406(10) . ? C3 H3 0.9500 . ? C4 C5 1.380(10) . ? C4 H4 0.9500 . ? C5 C6 1.404(10) . ? C5 H5 0.9500 . ? C6 C10 1.513(10) . ? C7 C9 1.530(10) . ? C7 C8 1.537(10) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.525(10) . ? C10 C11 1.529(10) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.346(8) . ? C13 N2 1.364(8) . ? C13 Ni1 1.920(7) . ? C14 C15 1.331(9) . ? C14 N1 1.381(8) . ? C14 H14 0.9500 . ? C15 N2 1.380(8) . ? C15 H15 0.9500 . ? C16 N3 1.342(8) . ? C16 C17 1.364(9) . ? C16 N2 1.389(8) . ? C17 C18 1.392(10) . ? C17 H17 0.9500 . ? C18 C19 1.388(10) . ? C18 H18 0.9500 . ? C19 C20 1.367(9) . ? C19 H19 0.9500 . ? C20 N3 1.330(8) . ? C20 N4 1.423(9) . ? C21 N5 1.344(8) . ? C21 N4 1.372(8) . ? C21 Ni1 1.914(7) . ? C22 C23 1.319(10) . ? C22 N4 1.362(9) . ? C22 H22 0.9500 . ? C23 N5 1.416(8) . ? C23 H23 0.9500 . ? C24 C25 1.389(10) . ? C24 C29 1.403(10) . ? C24 N5 1.462(9) . ? C25 C26 1.402(10) . ? C25 C30 1.525(10) . ? C26 C27 1.383(11) . ? C26 H26 0.9500 . ? C27 C28 1.383(11) . ? C27 H27 0.9500 . ? C28 C29 1.378(10) . ? C28 H28 0.9500 . ? C29 C33 1.519(11) . ? C30 C31 1.513(11) . ? C30 C32 1.529(11) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.533(11) . ? C33 C34 1.534(11) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C41 1.382(10) . ? C36 C37 1.389(10) . ? C36 N6 1.480(8) . ? C37 C38 1.410(11) . ? C37 C42 1.503(11) . ? C38 C39 1.366(13) . ? C38 H38 0.9500 . ? C39 C40 1.381(12) . ? C39 H39 0.9500 . ? C40 C41 1.394(10) . ? C40 H40 0.9500 . ? C41 C45 1.517(11) . ? C42 C43 1.510(12) . ? C42 C44 1.550(12) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.509(12) . ? C45 C46 1.536(12) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 N6 1.334(9) . ? C48 N7 1.379(9) . ? C48 Ni2 1.927(8) . ? C49 C50 1.332(9) . ? C49 N6 1.394(9) . ? C49 H49 0.9500 . ? C50 N7 1.358(9) . ? C50 H50 0.9500 . ? C51 N8 1.337(9) . ? C51 C52 1.369(9) . ? C51 N7 1.398(8) . ? C52 C53 1.390(10) . ? C52 H52 0.9500 . ? C53 C54 1.376(10) . ? C53 H53 0.9500 . ? C54 C55 1.379(10) . ? C54 H54 0.9500 . ? C55 N8 1.332(9) . ? C55 N9 1.414(9) . ? C56 N10 1.328(9) . ? C56 N9 1.385(8) . ? C56 Ni2 1.932(8) . ? C57 C58 1.333(10) . ? C57 N9 1.374(9) . ? C57 H57 0.9500 . ? C58 N10 1.406(9) . ? C58 H58 0.9500 . ? C59 C60 1.393(10) . ? C59 C64 1.397(11) . ? C59 N10 1.455(9) . ? C60 C61 1.405(10) . ? C60 C65 1.519(11) . ? C61 C62 1.352(12) . ? C61 H61 0.9500 . ? C62 C63 1.375(12) . ? C62 H62 0.9500 . ? C63 C64 1.405(11) . ? C63 H63 0.9500 . ? C64 C68 1.500(11) . ? C65 C67 1.512(12) . ? C65 C66 1.524(12) . ? C65 H65 1.0000 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.490(12) . ? C68 C70 1.538(11) . ? C68 H68 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 Cl2 1.735(10) . ? C71 Cl1 1.746(9) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 Cl3 1.742(15) . ? C72 Cl4 1.748(15) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? N3 Ni1 1.872(5) . ? N8 Ni2 1.873(5) . ? Ni1 Br1 2.2813(11) . ? Ni2 Br2 2.2591(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 C6 C1 C2 122.6(6) . . ? C6 C1 N1 118.3(6) . . ? C2 C1 N1 119.0(6) . . ? C3 C2 C1 118.4(7) . . ? C3 C2 C7 121.4(7) . . ? C1 C2 C7 120.2(6) . . ? C2 C3 C4 120.9(7) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.5(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.4(7) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 117.1(7) . . ? C1 C6 C10 122.4(6) . . ? C5 C6 C10 120.5(7) . . ? C2 C7 C9 111.8(6) . . ? C2 C7 C8 110.5(6) . . ? C9 C7 C8 112.1(6) . . ? C2 C7 H7 107.4 . . ? C9 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 110.4(6) . . ? C6 C10 C11 112.8(6) . . ? C12 C10 C11 111.9(6) . . ? C6 C10 H10 107.1 . . ? C12 C10 H10 107.1 . . ? C11 C10 H10 107.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 103.0(6) . . ? N1 C13 Ni1 143.0(5) . . ? N2 C13 Ni1 113.9(5) . . ? C15 C14 N1 109.1(6) . . ? C15 C14 H14 125.4 . . ? N1 C14 H14 125.4 . . ? C14 C15 N2 104.1(6) . . ? C14 C15 H15 128.0 . . ? N2 C15 H15 128.0 . . ? N3 C16 C17 121.8(6) . . ? N3 C16 N2 110.0(6) . . ? C17 C16 N2 128.0(6) . . ? C16 C17 C18 117.6(6) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? C19 C18 C17 121.3(7) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 116.3(7) . . ? C20 C19 H19 121.9 . . ? C18 C19 H19 121.9 . . ? N3 C20 C19 123.5(7) . . ? N3 C20 N4 109.2(6) . . ? C19 C20 N4 127.3(6) . . ? N5 C21 N4 102.6(6) . . ? N5 C21 Ni1 143.7(5) . . ? N4 C21 Ni1 113.7(5) . . ? C23 C22 N4 106.1(6) . . ? C23 C22 H22 126.9 . . ? N4 C22 H22 126.9 . . ? C22 C23 N5 107.3(6) . . ? C22 C23 H23 126.3 . . ? N5 C23 H23 126.3 . . ? C25 C24 C29 123.9(7) . . ? C25 C24 N5 118.0(6) . . ? C29 C24 N5 118.0(7) . . ? C24 C25 C26 117.6(7) . . ? C24 C25 C30 122.9(6) . . ? C26 C25 C30 119.5(7) . . ? C27 C26 C25 119.0(8) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C28 C27 C26 122.0(7) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C29 C28 C27 120.8(8) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C24 116.6(8) . . ? C28 C29 C33 120.9(7) . . ? C24 C29 C33 122.5(7) . . ? C31 C30 C25 111.5(6) . . ? C31 C30 C32 111.4(7) . . ? C25 C30 C32 112.3(6) . . ? C31 C30 H30 107.1 . . ? C25 C30 H30 107.1 . . ? C32 C30 H30 107.1 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 112.7(7) . . ? C29 C33 C34 111.5(7) . . ? C35 C33 C34 110.0(7) . . ? C29 C33 H33 107.4 . . ? C35 C33 H33 107.4 . . ? C34 C33 H33 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 125.3(7) . . ? C41 C36 N6 117.4(6) . . ? C37 C36 N6 117.0(7) . . ? C36 C37 C38 115.2(7) . . ? C36 C37 C42 123.3(7) . . ? C38 C37 C42 121.6(7) . . ? C39 C38 C37 122.0(8) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 119.9(8) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 121.5(8) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C36 C41 C40 116.1(7) . . ? C36 C41 C45 122.6(7) . . ? C40 C41 C45 121.2(7) . . ? C37 C42 C43 110.3(8) . . ? C37 C42 C44 111.1(8) . . ? C43 C42 C44 111.7(8) . . ? C37 C42 H42 107.9 . . ? C43 C42 H42 107.9 . . ? C44 C42 H42 107.9 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C41 110.1(7) . . ? C47 C45 C46 109.4(7) . . ? C41 C45 C46 111.5(7) . . ? C47 C45 H45 108.6 . . ? C41 C45 H45 108.6 . . ? C46 C45 H45 108.6 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N6 C48 N7 103.3(6) . . ? N6 C48 Ni2 144.7(6) . . ? N7 C48 Ni2 111.9(5) . . ? C50 C49 N6 107.4(7) . . ? C50 C49 H49 126.3 . . ? N6 C49 H49 126.3 . . ? C49 C50 N7 106.2(7) . . ? C49 C50 H50 126.9 . . ? N7 C50 H50 126.9 . . ? N8 C51 C52 122.2(7) . . ? N8 C51 N7 109.7(6) . . ? C52 C51 N7 128.0(7) . . ? C51 C52 C53 116.1(7) . . ? C51 C52 H52 121.9 . . ? C53 C52 H52 121.9 . . ? C54 C53 C52 122.9(7) . . ? C54 C53 H53 118.6 . . ? C52 C53 H53 118.6 . . ? C53 C54 C55 116.4(7) . . ? C53 C54 H54 121.8 . . ? C55 C54 H54 121.8 . . ? N8 C55 C54 121.9(7) . . ? N8 C55 N9 110.4(6) . . ? C54 C55 N9 127.7(7) . . ? N10 C56 N9 102.8(6) . . ? N10 C56 Ni2 144.9(5) . . ? N9 C56 Ni2 112.2(5) . . ? C58 C57 N9 105.9(6) . . ? C58 C57 H57 127.0 . . ? N9 C57 H57 127.0 . . ? C57 C58 N10 107.0(6) . . ? C57 C58 H58 126.5 . . ? N10 C58 H58 126.5 . . ? C60 C59 C64 123.6(7) . . ? C60 C59 N10 119.0(7) . . ? C64 C59 N10 117.4(7) . . ? C59 C60 C61 116.6(7) . . ? C59 C60 C65 122.1(7) . . ? C61 C60 C65 121.2(7) . . ? C62 C61 C60 121.3(8) . . ? C62 C61 H61 119.3 . . ? C60 C61 H61 119.3 . . ? C61 C62 C63 121.1(8) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C62 C63 C64 121.0(8) . . ? C62 C63 H63 119.5 . . ? C64 C63 H63 119.5 . . ? C59 C64 C63 116.3(8) . . ? C59 C64 C68 123.1(7) . . ? C63 C64 C68 120.5(8) . . ? C67 C65 C60 110.6(7) . . ? C67 C65 C66 111.4(8) . . ? C60 C65 C66 112.4(7) . . ? C67 C65 H65 107.4 . . ? C60 C65 H65 107.4 . . ? C66 C65 H65 107.4 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C64 111.5(8) . . ? C69 C68 C70 111.0(8) . . ? C64 C68 C70 113.7(7) . . ? C69 C68 H68 106.7 . . ? C64 C68 H68 106.7 . . ? C70 C68 H68 106.7 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? Cl2 C71 Cl1 112.2(5) . . ? Cl2 C71 H71A 109.2 . . ? Cl1 C71 H71A 109.2 . . ? Cl2 C71 H71B 109.2 . . ? Cl1 C71 H71B 109.2 . . ? H71A C71 H71B 107.9 . . ? Cl3 C72 Cl4 108.9(7) . . ? Cl3 C72 H72A 109.9 . . ? Cl4 C72 H72A 109.9 . . ? Cl3 C72 H72B 109.9 . . ? Cl4 C72 H72B 109.9 . . ? H72A C72 H72B 108.3 . . ? C13 N1 C14 110.6(6) . . ? C13 N1 C1 129.0(6) . . ? C14 N1 C1 120.3(6) . . ? C13 N2 C15 113.2(5) . . ? C13 N2 C16 115.9(6) . . ? C15 N2 C16 130.8(6) . . ? C20 N3 C16 119.5(6) . . ? C20 N3 Ni1 120.6(5) . . ? C16 N3 Ni1 119.9(5) . . ? C22 N4 C21 113.2(6) . . ? C22 N4 C20 131.2(6) . . ? C21 N4 C20 115.6(5) . . ? C21 N5 C23 110.7(6) . . ? C21 N5 C24 127.1(6) . . ? C23 N5 C24 122.0(6) . . ? C48 N6 C49 111.0(6) . . ? C48 N6 C36 130.7(6) . . ? C49 N6 C36 118.3(6) . . ? C50 N7 C48 112.1(6) . . ? C50 N7 C51 130.6(6) . . ? C48 N7 C51 117.0(6) . . ? C55 N8 C51 120.5(6) . . ? C55 N8 Ni2 119.7(5) . . ? C51 N8 Ni2 119.8(5) . . ? C57 N9 C56 112.4(6) . . ? C57 N9 C55 131.5(6) . . ? C56 N9 C55 116.1(6) . . ? C56 N10 C58 112.0(6) . . ? C56 N10 C59 127.2(6) . . ? C58 N10 C59 120.8(6) . . ? N3 Ni1 C21 80.8(3) . . ? N3 Ni1 C13 80.3(3) . . ? C21 Ni1 C13 161.1(3) . . ? N3 Ni1 Br1 174.43(18) . . ? C21 Ni1 Br1 99.1(2) . . ? C13 Ni1 Br1 99.8(2) . . ? N8 Ni2 C48 81.3(3) . . ? N8 Ni2 C56 81.6(3) . . ? C48 Ni2 C56 162.7(3) . . ? N8 Ni2 Br2 178.24(18) . . ? C48 Ni2 Br2 97.9(2) . . ? C56 Ni2 Br2 99.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.2(10) . . . . ? N1 C1 C2 C3 174.6(6) . . . . ? C6 C1 C2 C7 178.9(7) . . . . ? N1 C1 C2 C7 -5.3(10) . . . . ? C1 C2 C3 C4 -0.4(11) . . . . ? C7 C2 C3 C4 179.5(7) . . . . ? C2 C3 C4 C5 1.3(12) . . . . ? C3 C4 C5 C6 -0.6(12) . . . . ? C2 C1 C6 C5 1.8(10) . . . . ? N1 C1 C6 C5 -174.0(6) . . . . ? C2 C1 C6 C10 -176.8(7) . . . . ? N1 C1 C6 C10 7.4(10) . . . . ? C4 C5 C6 C1 -0.9(11) . . . . ? C4 C5 C6 C10 177.7(7) . . . . ? C3 C2 C7 C9 -56.9(9) . . . . ? C1 C2 C7 C9 123.1(7) . . . . ? C3 C2 C7 C8 68.7(9) . . . . ? C1 C2 C7 C8 -111.3(7) . . . . ? C1 C6 C10 C12 118.0(8) . . . . ? C5 C6 C10 C12 -60.6(9) . . . . ? C1 C6 C10 C11 -116.0(8) . . . . ? C5 C6 C10 C11 65.4(9) . . . . ? N1 C14 C15 N2 -0.3(8) . . . . ? N3 C16 C17 C18 1.9(10) . . . . ? N2 C16 C17 C18 176.2(6) . . . . ? C16 C17 C18 C19 0.2(11) . . . . ? C17 C18 C19 C20 -1.0(11) . . . . ? C18 C19 C20 N3 -0.2(11) . . . . ? C18 C19 C20 N4 179.7(7) . . . . ? N4 C22 C23 N5 -1.0(8) . . . . ? C29 C24 C25 C26 0.2(11) . . . . ? N5 C24 C25 C26 -177.7(6) . . . . ? C29 C24 C25 C30 -177.7(7) . . . . ? N5 C24 C25 C30 4.3(10) . . . . ? C24 C25 C26 C27 -0.4(11) . . . . ? C30 C25 C26 C27 177.6(7) . . . . ? C25 C26 C27 C28 0.0(12) . . . . ? C26 C27 C28 C29 0.6(12) . . . . ? C27 C28 C29 C24 -0.7(11) . . . . ? C27 C28 C29 C33 -178.7(7) . . . . ? C25 C24 C29 C28 0.3(11) . . . . ? N5 C24 C29 C28 178.3(6) . . . . ? C25 C24 C29 C33 178.2(7) . . . . ? N5 C24 C29 C33 -3.8(10) . . . . ? C24 C25 C30 C31 -109.8(8) . . . . ? C26 C25 C30 C31 72.3(9) . . . . ? C24 C25 C30 C32 124.3(8) . . . . ? C26 C25 C30 C32 -53.6(9) . . . . ? C28 C29 C33 C35 42.5(10) . . . . ? C24 C29 C33 C35 -135.4(8) . . . . ? C28 C29 C33 C34 -81.9(9) . . . . ? C24 C29 C33 C34 100.2(8) . . . . ? C41 C36 C37 C38 2.1(12) . . . . ? N6 C36 C37 C38 175.5(7) . . . . ? C41 C36 C37 C42 -179.7(8) . . . . ? N6 C36 C37 C42 -6.3(11) . . . . ? C36 C37 C38 C39 -1.8(13) . . . . ? C42 C37 C38 C39 180.0(8) . . . . ? C37 C38 C39 C40 1.6(14) . . . . ? C38 C39 C40 C41 -1.6(14) . . . . ? C37 C36 C41 C40 -2.1(12) . . . . ? N6 C36 C41 C40 -175.5(7) . . . . ? C37 C36 C41 C45 175.0(8) . . . . ? N6 C36 C41 C45 1.6(12) . . . . ? C39 C40 C41 C36 1.7(13) . . . . ? C39 C40 C41 C45 -175.4(8) . . . . ? C36 C37 C42 C43 -114.8(9) . . . . ? C38 C37 C42 C43 63.3(11) . . . . ? C36 C37 C42 C44 120.8(10) . . . . ? C38 C37 C42 C44 -61.1(12) . . . . ? C36 C41 C45 C47 -98.1(9) . . . . ? C40 C41 C45 C47 78.9(10) . . . . ? C36 C41 C45 C46 140.3(8) . . . . ? C40 C41 C45 C46 -42.7(11) . . . . ? N6 C49 C50 N7 0.7(8) . . . . ? N8 C51 C52 C53 0.5(11) . . . . ? N7 C51 C52 C53 -177.8(7) . . . . ? C51 C52 C53 C54 -0.6(11) . . . . ? C52 C53 C54 C55 0.2(11) . . . . ? C53 C54 C55 N8 0.4(11) . . . . ? C53 C54 C55 N9 179.2(7) . . . . ? N9 C57 C58 N10 0.2(8) . . . . ? C64 C59 C60 C61 0.1(12) . . . . ? N10 C59 C60 C61 -178.1(7) . . . . ? C64 C59 C60 C65 -177.9(7) . . . . ? N10 C59 C60 C65 4.0(11) . . . . ? C59 C60 C61 C62 -0.4(13) . . . . ? C65 C60 C61 C62 177.5(8) . . . . ? C60 C61 C62 C63 0.3(15) . . . . ? C61 C62 C63 C64 0.3(14) . . . . ? C60 C59 C64 C63 0.4(12) . . . . ? N10 C59 C64 C63 178.6(7) . . . . ? C60 C59 C64 C68 -179.5(7) . . . . ? N10 C59 C64 C68 -1.3(11) . . . . ? C62 C63 C64 C59 -0.6(12) . . . . ? C62 C63 C64 C68 179.3(8) . . . . ? C59 C60 C65 C67 104.3(9) . . . . ? C61 C60 C65 C67 -73.6(10) . . . . ? C59 C60 C65 C66 -130.5(8) . . . . ? C61 C60 C65 C66 51.7(11) . . . . ? C59 C64 C68 C69 88.4(10) . . . . ? C63 C64 C68 C69 -91.4(10) . . . . ? C59 C64 C68 C70 -145.1(8) . . . . ? C63 C64 C68 C70 35.0(11) . . . . ? N2 C13 N1 C14 0.8(7) . . . . ? Ni1 C13 N1 C14 -174.5(7) . . . . ? N2 C13 N1 C1 -174.9(6) . . . . ? Ni1 C13 N1 C1 9.8(13) . . . . ? C15 C14 N1 C13 -0.3(8) . . . . ? C15 C14 N1 C1 175.8(6) . . . . ? C6 C1 N1 C13 -94.9(9) . . . . ? C2 C1 N1 C13 89.1(8) . . . . ? C6 C1 N1 C14 89.7(8) . . . . ? C2 C1 N1 C14 -86.2(8) . . . . ? N1 C13 N2 C15 -1.1(7) . . . . ? Ni1 C13 N2 C15 175.9(5) . . . . ? N1 C13 N2 C16 -177.9(5) . . . . ? Ni1 C13 N2 C16 -1.0(7) . . . . ? C14 C15 N2 C13 0.9(8) . . . . ? C14 C15 N2 C16 177.1(7) . . . . ? N3 C16 N2 C13 0.3(8) . . . . ? C17 C16 N2 C13 -174.5(7) . . . . ? N3 C16 N2 C15 -175.9(6) . . . . ? C17 C16 N2 C15 9.3(12) . . . . ? C19 C20 N3 C16 2.3(10) . . . . ? N4 C20 N3 C16 -177.6(6) . . . . ? C19 C20 N3 Ni1 -176.7(6) . . . . ? N4 C20 N3 Ni1 3.5(8) . . . . ? C17 C16 N3 C20 -3.2(10) . . . . ? N2 C16 N3 C20 -178.3(6) . . . . ? C17 C16 N3 Ni1 175.8(5) . . . . ? N2 C16 N3 Ni1 0.6(7) . . . . ? C23 C22 N4 C21 0.6(8) . . . . ? C23 C22 N4 C20 179.8(7) . . . . ? N5 C21 N4 C22 0.0(8) . . . . ? Ni1 C21 N4 C22 179.0(5) . . . . ? N5 C21 N4 C20 -179.3(6) . . . . ? Ni1 C21 N4 C20 -0.2(7) . . . . ? N3 C20 N4 C22 179.0(7) . . . . ? C19 C20 N4 C22 -0.9(12) . . . . ? N3 C20 N4 C21 -1.9(8) . . . . ? C19 C20 N4 C21 178.2(7) . . . . ? N4 C21 N5 C23 -0.6(7) . . . . ? Ni1 C21 N5 C23 -179.1(7) . . . . ? N4 C21 N5 C24 174.6(6) . . . . ? Ni1 C21 N5 C24 -3.9(13) . . . . ? C22 C23 N5 C21 1.1(8) . . . . ? C22 C23 N5 C24 -174.4(7) . . . . ? C25 C24 N5 C21 -95.4(9) . . . . ? C29 C24 N5 C21 86.5(9) . . . . ? C25 C24 N5 C23 79.3(9) . . . . ? C29 C24 N5 C23 -98.8(8) . . . . ? N7 C48 N6 C49 0.4(8) . . . . ? Ni2 C48 N6 C49 179.9(7) . . . . ? N7 C48 N6 C36 178.2(7) . . . . ? Ni2 C48 N6 C36 -2.4(15) . . . . ? C50 C49 N6 C48 -0.7(9) . . . . ? C50 C49 N6 C36 -178.8(6) . . . . ? C41 C36 N6 C48 -78.1(10) . . . . ? C37 C36 N6 C48 108.0(9) . . . . ? C41 C36 N6 C49 99.5(8) . . . . ? C37 C36 N6 C49 -74.4(9) . . . . ? C49 C50 N7 C48 -0.4(9) . . . . ? C49 C50 N7 C51 173.0(7) . . . . ? N6 C48 N7 C50 0.0(8) . . . . ? Ni2 C48 N7 C50 -179.7(5) . . . . ? N6 C48 N7 C51 -174.4(6) . . . . ? Ni2 C48 N7 C51 5.9(8) . . . . ? N8 C51 N7 C50 -177.0(7) . . . . ? C52 C51 N7 C50 1.5(13) . . . . ? N8 C51 N7 C48 -3.8(9) . . . . ? C52 C51 N7 C48 174.7(7) . . . . ? C54 C55 N8 C51 -0.6(11) . . . . ? N9 C55 N8 C51 -179.5(6) . . . . ? C54 C55 N8 Ni2 178.3(5) . . . . ? N9 C55 N8 Ni2 -0.6(8) . . . . ? C52 C51 N8 C55 0.1(11) . . . . ? N7 C51 N8 C55 178.7(6) . . . . ? C52 C51 N8 Ni2 -178.8(5) . . . . ? N7 C51 N8 Ni2 -0.2(8) . . . . ? C58 C57 N9 C56 -0.8(8) . . . . ? C58 C57 N9 C55 -177.9(7) . . . . ? N10 C56 N9 C57 1.0(8) . . . . ? Ni2 C56 N9 C57 -175.7(5) . . . . ? N10 C56 N9 C55 178.6(6) . . . . ? Ni2 C56 N9 C55 1.9(7) . . . . ? N8 C55 N9 C57 176.1(7) . . . . ? C54 C55 N9 C57 -2.8(12) . . . . ? N8 C55 N9 C56 -0.9(8) . . . . ? C54 C55 N9 C56 -179.8(7) . . . . ? N9 C56 N10 C58 -0.8(8) . . . . ? Ni2 C56 N10 C58 173.8(7) . . . . ? N9 C56 N10 C59 178.0(6) . . . . ? Ni2 C56 N10 C59 -7.4(14) . . . . ? C57 C58 N10 C56 0.4(9) . . . . ? C57 C58 N10 C59 -178.5(6) . . . . ? C60 C59 N10 C56 -98.9(9) . . . . ? C64 C59 N10 C56 82.9(9) . . . . ? C60 C59 N10 C58 79.9(9) . . . . ? C64 C59 N10 C58 -98.4(8) . . . . ? C20 N3 Ni1 C21 -3.0(5) . . . . ? C16 N3 Ni1 C21 178.1(6) . . . . ? C20 N3 Ni1 C13 178.0(6) . . . . ? C16 N3 Ni1 C13 -0.9(5) . . . . ? C20 N3 Ni1 Br1 87(2) . . . . ? C16 N3 Ni1 Br1 -92.4(19) . . . . ? N5 C21 Ni1 N3 180.0(9) . . . . ? N4 C21 Ni1 N3 1.6(5) . . . . ? N5 C21 Ni1 C13 -176.9(8) . . . . ? N4 C21 Ni1 C13 4.7(12) . . . . ? N5 C21 Ni1 Br1 5.6(9) . . . . ? N4 C21 Ni1 Br1 -172.8(4) . . . . ? N1 C13 Ni1 N3 176.0(9) . . . . ? N2 C13 Ni1 N3 1.0(5) . . . . ? N1 C13 Ni1 C21 172.9(8) . . . . ? N2 C13 Ni1 C21 -2.1(12) . . . . ? N1 C13 Ni1 Br1 -9.6(9) . . . . ? N2 C13 Ni1 Br1 175.3(4) . . . . ? C55 N8 Ni2 C48 -176.2(6) . . . . ? C51 N8 Ni2 C48 2.7(5) . . . . ? C55 N8 Ni2 C56 1.4(5) . . . . ? C51 N8 Ni2 C56 -179.7(6) . . . . ? C55 N8 Ni2 Br2 119(6) . . . . ? C51 N8 Ni2 Br2 -62(7) . . . . ? N6 C48 Ni2 N8 176.1(10) . . . . ? N7 C48 Ni2 N8 -4.5(5) . . . . ? N6 C48 Ni2 C56 167.9(9) . . . . ? N7 C48 Ni2 C56 -12.7(13) . . . . ? N6 C48 Ni2 Br2 -5.6(10) . . . . ? N7 C48 Ni2 Br2 173.9(5) . . . . ? N10 C56 Ni2 N8 -176.1(10) . . . . ? N9 C56 Ni2 N8 -1.7(5) . . . . ? N10 C56 Ni2 C48 -167.9(9) . . . . ? N9 C56 Ni2 C48 6.5(13) . . . . ? N10 C56 Ni2 Br2 5.5(10) . . . . ? N9 C56 Ni2 Br2 179.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.869 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.123 #==END data_3MeAgI2 _database_code_depnum_ccdc_archive 'CCDC 663958' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H45 Br N5 Ni, 0.5(Ag2 I4)' _chemical_formula_sum 'C37 H45 Ag Br I2 N5 Ni' _chemical_formula_weight 1060.07 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 41.413(2) _cell_length_b 8.1837(4) _cell_length_c 23.0900(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.661(2) _cell_angle_gamma 90.00 _cell_volume 7570.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9214 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 3.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3166 _exptl_absorpt_correction_T_max 0.5908 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42239 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.55 _reflns_number_total 8691 _reflns_number_gt 5945 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Shedrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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^)+(0.1130P)^2^+108.2317P] 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 8691 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2119 _refine_ls_wR_factor_gt 0.1858 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.11568(17) 0.5013(9) 0.2303(3) 0.0179(14) Uani 1 1 d . . . C2 C 0.12216(19) 0.6675(10) 0.2359(3) 0.0221(16) Uani 1 1 d . . . C3 C 0.0970(2) 0.7676(10) 0.2460(3) 0.0258(17) Uani 1 1 d . . . H3 H 0.1005 0.8822 0.2503 0.031 Uiso 1 1 calc R . . C4 C 0.06695(19) 0.7011(10) 0.2499(4) 0.0266(17) Uani 1 1 d . . . H4 H 0.0499 0.7711 0.2563 0.032 Uiso 1 1 calc R . . C5 C 0.06136(18) 0.5373(10) 0.2447(3) 0.0222(16) Uani 1 1 d . . . H5 H 0.0404 0.4952 0.2475 0.027 Uiso 1 1 calc R . . C6 C 0.08581(18) 0.4296(9) 0.2354(3) 0.0207(15) Uani 1 1 d . . . C7 C 0.15482(19) 0.7435(10) 0.2290(3) 0.0233(16) Uani 1 1 d . . . H7 H 0.1678 0.6559 0.2149 0.028 Uiso 1 1 calc R . . C8 C 0.1759(2) 0.8075(11) 0.2882(4) 0.0292(18) Uani 1 1 d . . . H8A H 0.1640 0.8966 0.3023 0.044 Uiso 1 1 calc R . . H8B H 0.1972 0.8483 0.2827 0.044 Uiso 1 1 calc R . . H8C H 0.1801 0.7191 0.3177 0.044 Uiso 1 1 calc R . . C9 C 0.1479(2) 0.8781(11) 0.1819(4) 0.036(2) Uani 1 1 d . . . H9A H 0.1326 0.8372 0.1452 0.053 Uiso 1 1 calc R . . H9B H 0.1689 0.9116 0.1732 0.053 Uiso 1 1 calc R . . H9C H 0.1378 0.9720 0.1970 0.053 Uiso 1 1 calc R . . C10 C 0.07989(18) 0.2466(9) 0.2310(4) 0.0228(16) Uani 1 1 d . . . H10 H 0.1010 0.1914 0.2526 0.027 Uiso 1 1 calc R . . C11 C 0.0526(2) 0.1902(11) 0.2587(5) 0.035(2) Uani 1 1 d . . . H11A H 0.0558 0.2393 0.2985 0.053 Uiso 1 1 calc R . . H11B H 0.0533 0.0709 0.2624 0.053 Uiso 1 1 calc R . . H11C H 0.0309 0.2237 0.2333 0.053 Uiso 1 1 calc R . . C12 C 0.0712(2) 0.1870(10) 0.1660(4) 0.0290(18) Uani 1 1 d . . . H12A H 0.0509 0.2425 0.1433 0.043 Uiso 1 1 calc R . . H12B H 0.0673 0.0688 0.1650 0.043 Uiso 1 1 calc R . . H12C H 0.0897 0.2116 0.1480 0.043 Uiso 1 1 calc R . . C13 C 0.14673(17) 0.3684(9) 0.1643(3) 0.0190(15) Uani 1 1 d . . . C14 C 0.16687(17) 0.3319(9) 0.2638(3) 0.0205(15) Uani 1 1 d . . . H14 H 0.1686 0.3368 0.3056 0.025 Uiso 1 1 calc R . . C15 C 0.18846(18) 0.2591(10) 0.2374(4) 0.0237(16) Uani 1 1 d . . . H15 H 0.2086 0.2051 0.2568 0.028 Uiso 1 1 calc R . . C16 C 0.18748(16) 0.2318(9) 0.1273(3) 0.0162(14) Uani 1 1 d . . . C17 C 0.21606(18) 0.1436(10) 0.1270(4) 0.0231(16) Uani 1 1 d . . . C18 C 0.22172(18) 0.1207(9) 0.0703(4) 0.0200(15) Uani 1 1 d . . . H18 H 0.2412 0.0623 0.0681 0.024 Uiso 1 1 calc R . . C19 C 0.20071(17) 0.1775(9) 0.0164(4) 0.0198(15) Uani 1 1 d . . . C20 C 0.17279(16) 0.2631(9) 0.0228(3) 0.0163(14) Uani 1 1 d . . . C21 C 0.12293(17) 0.4154(9) -0.0034(3) 0.0179(14) Uani 1 1 d . . . C22 C 0.1413(2) 0.3290(10) -0.0838(4) 0.0251(17) Uani 1 1 d . . . H22 H 0.1547 0.2784 -0.1067 0.030 Uiso 1 1 calc R . . C23 C 0.11346(18) 0.4122(9) -0.1051(3) 0.0211(15) Uani 1 1 d . . . H23 H 0.1029 0.4319 -0.1461 0.025 Uiso 1 1 calc R . . C24 C 0.07354(18) 0.5711(9) -0.0638(3) 0.0205(15) Uani 1 1 d . . . C25 C 0.0792(2) 0.7395(10) -0.0605(4) 0.0245(16) Uani 1 1 d . . . C26 C 0.05122(19) 0.8392(10) -0.0721(4) 0.0262(17) Uani 1 1 d . . . H26 H 0.0541 0.9544 -0.0702 0.031 Uiso 1 1 calc R . . C27 C 0.0197(2) 0.7767(10) -0.0860(4) 0.0288(18) Uani 1 1 d . . . H27 H 0.0010 0.8480 -0.0938 0.035 Uiso 1 1 calc R . . C28 C 0.01491(19) 0.6068(10) -0.0890(4) 0.0249(17) Uani 1 1 d . . . H28 H -0.0071 0.5641 -0.0985 0.030 Uiso 1 1 calc R . . C29 C 0.04164(17) 0.5008(9) -0.0782(3) 0.0187(15) Uani 1 1 d . . . C30 C 0.1135(2) 0.8132(10) -0.0466(4) 0.033(2) Uani 1 1 d . . . H30 H 0.1298 0.7215 -0.0355 0.040 Uiso 1 1 calc R . . C31 C 0.1199(2) 0.8960(12) -0.1013(5) 0.041(2) Uani 1 1 d . . . H31A H 0.1176 0.8160 -0.1337 0.062 Uiso 1 1 calc R . . H31B H 0.1426 0.9410 -0.0913 0.062 Uiso 1 1 calc R . . H31C H 0.1038 0.9845 -0.1142 0.062 Uiso 1 1 calc R . . C32 C 0.1194(3) 0.9293(14) 0.0075(5) 0.051(3) Uani 1 1 d . . . H32A H 0.1060 1.0282 -0.0036 0.076 Uiso 1 1 calc R . . H32B H 0.1431 0.9590 0.0199 0.076 Uiso 1 1 calc R . . H32C H 0.1131 0.8746 0.0407 0.076 Uiso 1 1 calc R . . C33 C 0.03611(18) 0.3171(9) -0.0803(4) 0.0218(16) Uani 1 1 d . . . H33 H 0.0578 0.2613 -0.0791 0.026 Uiso 1 1 calc R . . C34 C 0.0244(3) 0.2665(12) -0.0257(4) 0.039(2) Uani 1 1 d . . . H34A H 0.0404 0.3053 0.0106 0.059 Uiso 1 1 calc R . . H34B H 0.0229 0.1471 -0.0244 0.059 Uiso 1 1 calc R . . H34C H 0.0025 0.3145 -0.0279 0.059 Uiso 1 1 calc R . . C35 C 0.0105(2) 0.2663(11) -0.1375(4) 0.0318(19) Uani 1 1 d . . . H35A H -0.0120 0.2958 -0.1343 0.048 Uiso 1 1 calc R . . H35B H 0.0117 0.1480 -0.1429 0.048 Uiso 1 1 calc R . . H35C H 0.0152 0.3227 -0.1718 0.048 Uiso 1 1 calc R . . C36 C 0.24002(19) 0.0783(11) 0.1808(4) 0.0283(18) Uani 1 1 d . . . H36A H 0.2500 0.1689 0.2069 0.043 Uiso 1 1 calc R . . H36B H 0.2576 0.0171 0.1687 0.043 Uiso 1 1 calc R . . H36C H 0.2283 0.0056 0.2024 0.043 Uiso 1 1 calc R . . C37 C 0.2100(2) 0.1503(11) -0.0409(4) 0.0276(18) Uani 1 1 d . . . H37A H 0.1938 0.0763 -0.0663 0.041 Uiso 1 1 calc R . . H37B H 0.2323 0.1016 -0.0327 0.041 Uiso 1 1 calc R . . H37C H 0.2100 0.2549 -0.0615 0.041 Uiso 1 1 calc R . . N1 N 0.14151(15) 0.3989(7) 0.2186(3) 0.0179(12) Uani 1 1 d . . . N2 N 0.17573(14) 0.2779(7) 0.1768(3) 0.0165(12) Uani 1 1 d . . . N3 N 0.16658(14) 0.2885(7) 0.0770(3) 0.0163(12) Uani 1 1 d . . . N4 N 0.14735(14) 0.3296(7) -0.0220(3) 0.0155(12) Uani 1 1 d . . . N5 N 0.10235(14) 0.4664(8) -0.0554(3) 0.0176(12) Uani 1 1 d . . . Ni1 Ni 0.12936(2) 0.41097(11) 0.08082(4) 0.0157(2) Uani 1 1 d . . . Br1 Br 0.084119(18) 0.56453(10) 0.08466(3) 0.0231(2) Uani 1 1 d . . . I1 I 0.22766(2) 0.60491(10) 0.15548(3) 0.0551(2) Uani 1 1 d . . . I2 I 0.202370(16) 0.65662(9) -0.05968(3) 0.0486(2) Uani 1 1 d . . . Ag1 Ag 0.23485(2) 0.68680(11) 0.05335(4) 0.0538(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(3) 0.019(4) 0.017(3) 0.002(3) 0.003(3) 0.005(3) C2 0.023(4) 0.023(4) 0.021(4) 0.000(3) 0.008(3) 0.000(3) C3 0.032(4) 0.020(4) 0.025(4) -0.003(3) 0.006(3) -0.001(3) C4 0.017(4) 0.021(4) 0.039(5) -0.002(4) 0.004(3) 0.002(3) C5 0.015(3) 0.024(4) 0.027(4) -0.001(3) 0.004(3) 0.000(3) C6 0.018(3) 0.018(4) 0.024(4) 0.002(3) 0.001(3) 0.003(3) C7 0.023(4) 0.021(4) 0.030(4) -0.001(3) 0.013(3) -0.004(3) C8 0.021(4) 0.037(5) 0.031(4) 0.001(4) 0.008(3) -0.001(3) C9 0.038(5) 0.032(5) 0.036(5) 0.007(4) 0.009(4) -0.013(4) C10 0.018(3) 0.018(4) 0.032(4) 0.000(3) 0.005(3) -0.001(3) C11 0.030(4) 0.025(5) 0.054(6) -0.001(4) 0.018(4) -0.002(4) C12 0.024(4) 0.021(4) 0.036(5) 0.000(4) -0.004(3) 0.001(3) C13 0.012(3) 0.018(4) 0.028(4) -0.001(3) 0.007(3) 0.006(3) C14 0.016(3) 0.020(4) 0.023(4) 0.001(3) 0.000(3) -0.004(3) C15 0.014(3) 0.024(4) 0.030(4) 0.002(3) 0.001(3) 0.000(3) C16 0.012(3) 0.013(3) 0.024(4) -0.004(3) 0.005(3) -0.005(3) C17 0.011(3) 0.021(4) 0.036(4) -0.002(3) 0.003(3) -0.002(3) C18 0.014(3) 0.014(4) 0.035(4) 0.003(3) 0.013(3) 0.003(3) C19 0.013(3) 0.015(4) 0.033(4) 0.000(3) 0.009(3) 0.003(3) C20 0.011(3) 0.013(3) 0.025(4) 0.004(3) 0.004(3) 0.002(3) C21 0.010(3) 0.016(4) 0.028(4) 0.001(3) 0.008(3) 0.001(3) C22 0.025(4) 0.027(4) 0.025(4) -0.001(3) 0.010(3) 0.000(3) C23 0.022(4) 0.022(4) 0.020(4) 0.002(3) 0.006(3) -0.002(3) C24 0.017(3) 0.022(4) 0.024(4) -0.003(3) 0.007(3) 0.003(3) C25 0.027(4) 0.018(4) 0.028(4) 0.006(3) 0.006(3) 0.000(3) C26 0.023(4) 0.021(4) 0.036(4) 0.003(3) 0.009(3) 0.003(3) C27 0.021(4) 0.025(4) 0.040(5) 0.000(4) 0.007(3) 0.009(3) C28 0.015(3) 0.025(4) 0.034(4) -0.002(3) 0.004(3) -0.002(3) C29 0.018(3) 0.013(4) 0.023(4) 0.006(3) 0.002(3) 0.004(3) C30 0.022(4) 0.021(4) 0.050(5) 0.005(4) -0.004(4) 0.001(3) C31 0.020(4) 0.041(6) 0.064(7) 0.008(5) 0.014(4) -0.004(4) C32 0.045(6) 0.049(7) 0.055(6) -0.008(5) 0.007(5) -0.033(5) C33 0.018(3) 0.014(4) 0.032(4) 0.003(3) 0.003(3) 0.000(3) C34 0.055(6) 0.028(5) 0.034(5) 0.003(4) 0.011(4) -0.007(4) C35 0.030(4) 0.027(5) 0.036(5) -0.008(4) 0.004(4) 0.001(4) C36 0.019(4) 0.028(4) 0.037(5) 0.003(4) 0.005(3) 0.005(3) C37 0.023(4) 0.032(5) 0.033(4) -0.001(4) 0.015(3) 0.008(3) N1 0.019(3) 0.014(3) 0.019(3) 0.000(2) 0.002(2) 0.001(2) N2 0.013(3) 0.013(3) 0.022(3) 0.003(2) 0.003(2) 0.000(2) N3 0.011(3) 0.013(3) 0.026(3) 0.001(2) 0.006(2) -0.002(2) N4 0.017(3) 0.012(3) 0.019(3) 0.002(2) 0.007(2) 0.004(2) N5 0.011(3) 0.019(3) 0.023(3) -0.001(3) 0.003(2) 0.001(2) Ni1 0.0116(4) 0.0151(5) 0.0206(5) 0.0007(4) 0.0046(3) 0.0032(3) Br1 0.0187(4) 0.0259(4) 0.0247(4) 0.0006(3) 0.0057(3) 0.0094(3) I1 0.0566(5) 0.0570(5) 0.0551(4) -0.0122(4) 0.0205(4) -0.0239(4) I2 0.0350(4) 0.0462(4) 0.0609(5) -0.0028(3) 0.0054(3) 0.0030(3) Ag1 0.0674(6) 0.0413(5) 0.0558(5) -0.0026(4) 0.0210(4) 0.0193(4) _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 C1 C2 1.386(11) . ? C1 C6 1.401(10) . ? C1 N1 1.437(9) . ? C2 C3 1.390(11) . ? C2 C7 1.533(10) . ? C3 C4 1.383(11) . ? C3 H3 0.9500 . ? C4 C5 1.360(11) . ? C4 H4 0.9500 . ? C5 C6 1.400(10) . ? C5 H5 0.9500 . ? C6 C10 1.517(11) . ? C7 C8 1.517(11) . ? C7 C9 1.522(12) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.507(11) . ? C10 C12 1.531(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.348(10) . ? C13 N2 1.378(9) . ? C13 Ni1 1.911(8) . ? C14 C15 1.342(11) . ? C14 N1 1.392(9) . ? C14 H14 0.9500 . ? C15 N2 1.373(10) . ? C15 H15 0.9500 . ? C16 N3 1.344(9) . ? C16 C17 1.388(10) . ? C16 N2 1.403(9) . ? C17 C18 1.399(11) . ? C17 C36 1.480(11) . ? C18 C19 1.406(11) . ? C18 H18 0.9500 . ? C19 C20 1.392(10) . ? C19 C37 1.485(11) . ? C20 N3 1.354(9) . ? C20 N4 1.388(9) . ? C21 N5 1.351(9) . ? C21 N4 1.386(9) . ? C21 Ni1 1.895(8) . ? C22 C23 1.323(11) . ? C22 N4 1.386(10) . ? C22 H22 0.9500 . ? C23 N5 1.411(9) . ? C23 H23 0.9500 . ? C24 C25 1.397(11) . ? C24 C29 1.401(10) . ? C24 N5 1.442(9) . ? C25 C26 1.387(11) . ? C25 C30 1.500(11) . ? C26 C27 1.363(11) . ? C26 H26 0.9500 . ? C27 C28 1.403(12) . ? C27 H27 0.9500 . ? C28 C29 1.379(10) . ? C28 H28 0.9500 . ? C29 C33 1.520(10) . ? C30 C31 1.515(14) . ? C30 C32 1.539(14) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.519(12) . ? C33 C35 1.526(11) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N3 Ni1 1.860(6) . ? Ni1 Br1 2.2761(11) . ? I1 Ag1 2.5404(12) . ? I2 Ag1 2.6278(12) . ? I2 Ag1 2.8691(13) 7_565 ? Ag1 I2 2.8691(13) 7_565 ? Ag1 Ag1 3.2064(19) 7_565 ? 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 C2 C1 C6 123.9(7) . . ? C2 C1 N1 117.0(6) . . ? C6 C1 N1 119.1(7) . . ? C1 C2 C3 117.3(7) . . ? C1 C2 C7 122.9(7) . . ? C3 C2 C7 119.7(7) . . ? C4 C3 C2 120.2(8) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 121.2(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 121.4(7) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 115.9(7) . . ? C5 C6 C10 121.4(7) . . ? C1 C6 C10 122.6(7) . . ? C8 C7 C9 110.8(7) . . ? C8 C7 C2 111.6(6) . . ? C9 C7 C2 110.9(7) . . ? C8 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C2 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 113.5(7) . . ? C11 C10 C12 107.7(7) . . ? C6 C10 C12 112.0(7) . . ? C11 C10 H10 107.8 . . ? C6 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 103.9(6) . . ? N1 C13 Ni1 142.7(5) . . ? N2 C13 Ni1 113.3(5) . . ? C15 C14 N1 107.3(7) . . ? C15 C14 H14 126.3 . . ? N1 C14 H14 126.3 . . ? C14 C15 N2 106.5(6) . . ? C14 C15 H15 126.7 . . ? N2 C15 H15 126.7 . . ? N3 C16 C17 122.6(7) . . ? N3 C16 N2 109.4(6) . . ? C17 C16 N2 128.0(7) . . ? C16 C17 C18 114.8(7) . . ? C16 C17 C36 125.1(7) . . ? C18 C17 C36 120.1(7) . . ? C17 C18 C19 124.9(7) . . ? C17 C18 H18 117.6 . . ? C19 C18 H18 117.6 . . ? C20 C19 C18 114.6(7) . . ? C20 C19 C37 125.5(7) . . ? C18 C19 C37 119.8(6) . . ? N3 C20 N4 110.1(6) . . ? N3 C20 C19 122.2(6) . . ? N4 C20 C19 127.7(7) . . ? N5 C21 N4 103.1(6) . . ? N5 C21 Ni1 144.2(5) . . ? N4 C21 Ni1 112.6(5) . . ? C23 C22 N4 107.0(7) . . ? C23 C22 H22 126.5 . . ? N4 C22 H22 126.5 . . ? C22 C23 N5 107.1(7) . . ? C22 C23 H23 126.5 . . ? N5 C23 H23 126.5 . . ? C25 C24 C29 123.6(7) . . ? C25 C24 N5 117.2(6) . . ? C29 C24 N5 119.1(7) . . ? C26 C25 C24 116.7(7) . . ? C26 C25 C30 120.2(7) . . ? C24 C25 C30 123.0(7) . . ? C27 C26 C25 121.9(8) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 119.9(7) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 121.2(7) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C24 116.8(7) . . ? C28 C29 C33 120.6(7) . . ? C24 C29 C33 122.6(6) . . ? C25 C30 C31 111.0(7) . . ? C25 C30 C32 111.8(8) . . ? C31 C30 C32 112.0(8) . . ? C25 C30 H30 107.2 . . ? C31 C30 H30 107.2 . . ? C32 C30 H30 107.2 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C29 108.7(7) . . ? C34 C33 C35 110.2(7) . . ? C29 C33 C35 111.3(6) . . ? C34 C33 H33 108.9 . . ? C29 C33 H33 108.9 . . ? C35 C33 H33 108.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C19 C37 H37A 109.5 . . ? C19 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C19 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C13 N1 C14 110.9(6) . . ? C13 N1 C1 125.8(6) . . ? C14 N1 C1 123.0(6) . . ? C15 N2 C13 111.3(6) . . ? C15 N2 C16 132.6(6) . . ? C13 N2 C16 115.9(6) . . ? C16 N3 C20 120.9(6) . . ? C16 N3 Ni1 120.3(5) . . ? C20 N3 Ni1 118.7(5) . . ? C21 N4 C22 111.5(6) . . ? C21 N4 C20 116.3(6) . . ? C22 N4 C20 132.2(6) . . ? C21 N5 C23 111.3(6) . . ? C21 N5 C24 128.1(6) . . ? C23 N5 C24 120.5(6) . . ? N3 Ni1 C21 82.2(3) . . ? N3 Ni1 C13 81.1(3) . . ? C21 Ni1 C13 163.3(3) . . ? N3 Ni1 Br1 178.99(19) . . ? C21 Ni1 Br1 97.2(2) . . ? C13 Ni1 Br1 99.5(2) . . ? Ag1 I2 Ag1 71.21(4) . 7_565 ? I1 Ag1 I2 138.28(5) . . ? I1 Ag1 I2 112.84(4) . 7_565 ? I2 Ag1 I2 108.79(4) . 7_565 ? I1 Ag1 Ag1 163.53(6) . 7_565 ? I2 Ag1 Ag1 57.90(3) . 7_565 ? I2 Ag1 Ag1 50.88(3) 7_565 7_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.3(11) . . . . ? N1 C1 C2 C3 178.7(6) . . . . ? C6 C1 C2 C7 -178.9(7) . . . . ? N1 C1 C2 C7 1.2(10) . . . . ? C1 C2 C3 C4 -0.3(11) . . . . ? C7 C2 C3 C4 177.4(7) . . . . ? C2 C3 C4 C5 0.8(12) . . . . ? C3 C4 C5 C6 0.1(13) . . . . ? C4 C5 C6 C1 -1.6(11) . . . . ? C4 C5 C6 C10 178.7(7) . . . . ? C2 C1 C6 C5 2.2(11) . . . . ? N1 C1 C6 C5 -177.8(6) . . . . ? C2 C1 C6 C10 -178.1(7) . . . . ? N1 C1 C6 C10 1.9(10) . . . . ? C1 C2 C7 C8 -110.7(8) . . . . ? C3 C2 C7 C8 71.8(9) . . . . ? C1 C2 C7 C9 125.2(8) . . . . ? C3 C2 C7 C9 -52.3(10) . . . . ? C5 C6 C10 C11 -21.0(11) . . . . ? C1 C6 C10 C11 159.4(7) . . . . ? C5 C6 C10 C12 101.3(8) . . . . ? C1 C6 C10 C12 -78.4(9) . . . . ? N1 C14 C15 N2 -1.7(8) . . . . ? N3 C16 C17 C18 1.0(11) . . . . ? N2 C16 C17 C18 -178.2(7) . . . . ? N3 C16 C17 C36 179.9(7) . . . . ? N2 C16 C17 C36 0.7(13) . . . . ? C16 C17 C18 C19 -0.9(11) . . . . ? C36 C17 C18 C19 -179.9(7) . . . . ? C17 C18 C19 C20 0.6(11) . . . . ? C17 C18 C19 C37 177.9(7) . . . . ? C18 C19 C20 N3 -0.2(10) . . . . ? C37 C19 C20 N3 -177.4(7) . . . . ? C18 C19 C20 N4 -178.2(7) . . . . ? C37 C19 C20 N4 4.6(13) . . . . ? N4 C22 C23 N5 0.6(9) . . . . ? C29 C24 C25 C26 0.3(12) . . . . ? N5 C24 C25 C26 176.3(7) . . . . ? C29 C24 C25 C30 -178.3(8) . . . . ? N5 C24 C25 C30 -2.3(12) . . . . ? C24 C25 C26 C27 0.0(12) . . . . ? C30 C25 C26 C27 178.6(8) . . . . ? C25 C26 C27 C28 0.1(13) . . . . ? C26 C27 C28 C29 -0.4(13) . . . . ? C27 C28 C29 C24 0.6(12) . . . . ? C27 C28 C29 C33 178.8(8) . . . . ? C25 C24 C29 C28 -0.6(11) . . . . ? N5 C24 C29 C28 -176.6(7) . . . . ? C25 C24 C29 C33 -178.7(7) . . . . ? N5 C24 C29 C33 5.3(11) . . . . ? C26 C25 C30 C31 -69.0(11) . . . . ? C24 C25 C30 C31 109.6(9) . . . . ? C26 C25 C30 C32 56.9(11) . . . . ? C24 C25 C30 C32 -124.6(9) . . . . ? C28 C29 C33 C34 -72.0(9) . . . . ? C24 C29 C33 C34 106.1(9) . . . . ? C28 C29 C33 C35 49.6(10) . . . . ? C24 C29 C33 C35 -132.4(8) . . . . ? N2 C13 N1 C14 1.1(8) . . . . ? Ni1 C13 N1 C14 -176.4(7) . . . . ? N2 C13 N1 C1 174.5(6) . . . . ? Ni1 C13 N1 C1 -2.9(14) . . . . ? C15 C14 N1 C13 0.4(9) . . . . ? C15 C14 N1 C1 -173.3(7) . . . . ? C2 C1 N1 C13 -84.4(9) . . . . ? C6 C1 N1 C13 95.6(9) . . . . ? C2 C1 N1 C14 88.3(9) . . . . ? C6 C1 N1 C14 -91.7(9) . . . . ? C14 C15 N2 C13 2.5(9) . . . . ? C14 C15 N2 C16 178.2(7) . . . . ? N1 C13 N2 C15 -2.2(8) . . . . ? Ni1 C13 N2 C15 176.2(5) . . . . ? N1 C13 N2 C16 -178.7(6) . . . . ? Ni1 C13 N2 C16 -0.3(8) . . . . ? N3 C16 N2 C15 -176.0(7) . . . . ? C17 C16 N2 C15 3.3(13) . . . . ? N3 C16 N2 C13 -0.4(8) . . . . ? C17 C16 N2 C13 178.8(7) . . . . ? C17 C16 N3 C20 -0.7(11) . . . . ? N2 C16 N3 C20 178.6(6) . . . . ? C17 C16 N3 Ni1 -178.2(5) . . . . ? N2 C16 N3 Ni1 1.1(8) . . . . ? N4 C20 N3 C16 178.6(6) . . . . ? C19 C20 N3 C16 0.3(11) . . . . ? N4 C20 N3 Ni1 -3.8(8) . . . . ? C19 C20 N3 Ni1 177.8(5) . . . . ? N5 C21 N4 C22 -0.2(8) . . . . ? Ni1 C21 N4 C22 177.5(5) . . . . ? N5 C21 N4 C20 179.2(6) . . . . ? Ni1 C21 N4 C20 -3.1(8) . . . . ? C23 C22 N4 C21 -0.3(9) . . . . ? C23 C22 N4 C20 -179.6(7) . . . . ? N3 C20 N4 C21 4.4(9) . . . . ? C19 C20 N4 C21 -177.4(7) . . . . ? N3 C20 N4 C22 -176.4(7) . . . . ? C19 C20 N4 C22 1.9(13) . . . . ? N4 C21 N5 C23 0.6(8) . . . . ? Ni1 C21 N5 C23 -175.8(7) . . . . ? N4 C21 N5 C24 -175.5(7) . . . . ? Ni1 C21 N5 C24 8.1(14) . . . . ? C22 C23 N5 C21 -0.8(9) . . . . ? C22 C23 N5 C24 175.6(7) . . . . ? C25 C24 N5 C21 82.9(10) . . . . ? C29 C24 N5 C21 -100.9(9) . . . . ? C25 C24 N5 C23 -92.8(8) . . . . ? C29 C24 N5 C23 83.4(9) . . . . ? C16 N3 Ni1 C21 179.4(6) . . . . ? C20 N3 Ni1 C21 1.8(5) . . . . ? C16 N3 Ni1 C13 -1.0(5) . . . . ? C20 N3 Ni1 C13 -178.6(6) . . . . ? N5 C21 Ni1 N3 176.9(10) . . . . ? N4 C21 Ni1 N3 0.7(5) . . . . ? N5 C21 Ni1 C13 175.4(9) . . . . ? N4 C21 Ni1 C13 -0.8(14) . . . . ? N5 C21 Ni1 Br1 -3.9(10) . . . . ? N4 C21 Ni1 Br1 179.9(5) . . . . ? N1 C13 Ni1 N3 178.0(10) . . . . ? N2 C13 Ni1 N3 0.7(5) . . . . ? N1 C13 Ni1 C21 179.5(9) . . . . ? N2 C13 Ni1 C21 2.2(14) . . . . ? N1 C13 Ni1 Br1 -1.1(10) . . . . ? N2 C13 Ni1 Br1 -178.5(5) . . . . ? Ag1 I2 Ag1 I1 -175.94(8) 7_565 . . . ? Ag1 I2 Ag1 I2 0.0 7_565 . . 7_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.368 _refine_diff_density_min -2.665 _refine_diff_density_rms 0.219 #==END data_3MeOTf _database_code_depnum_ccdc_archive 'CCDC 663959' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H45 Br N5 Ni, C F3 O3 S' _chemical_formula_sum 'C38 H45 Br F3 N5 Ni O3 S' _chemical_formula_weight 847.47 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6147(3) _cell_length_b 14.2268(7) _cell_length_c 16.2224(8) _cell_angle_alpha 101.802(2) _cell_angle_beta 98.787(3) _cell_angle_gamma 96.327(3) _cell_volume 1902.67(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8252 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5400 _exptl_absorpt_correction_T_max 0.9835 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27224 _diffrn_reflns_av_R_equivalents 0.1479 _diffrn_reflns_av_sigmaI/netI 0.1539 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6686 _reflns_number_gt 4135 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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^)+(0.0000P)^2^+25.1678P] 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 6686 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1853 _refine_ls_R_factor_gt 0.1050 _refine_ls_wR_factor_ref 0.2085 _refine_ls_wR_factor_gt 0.1744 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0305(11) 0.0344(7) 0.2558(6) 0.0182(15) Uani 1 1 d . . . C2 C -0.1240(10) 0.0513(7) 0.2653(6) 0.0188(15) Uani 1 1 d . . . C3 C -0.2404(10) 0.0119(7) 0.1956(6) 0.022(2) Uani 1 1 d . . . H3 H -0.3464 0.0232 0.1981 0.027 Uiso 1 1 calc R . . C4 C -0.2079(12) -0.0444(7) 0.1208(7) 0.027(2) Uani 1 1 d . . . H4 H -0.2919 -0.0718 0.0739 0.032 Uiso 1 1 calc R . . C5 C -0.0535(11) -0.0608(7) 0.1144(7) 0.026(2) Uani 1 1 d . . . H5 H -0.0319 -0.0998 0.0637 0.031 Uiso 1 1 calc R . . C6 C 0.0678(10) -0.0199(7) 0.1824(6) 0.0188(15) Uani 1 1 d . . . C7 C -0.1593(11) 0.1147(7) 0.3457(7) 0.026(2) Uani 1 1 d . . . H7 H -0.0722 0.1133 0.3937 0.031 Uiso 1 1 calc R . . C8 C -0.3158(12) 0.0763(8) 0.3700(7) 0.033(3) Uani 1 1 d . . . H8A H -0.4054 0.0883 0.3303 0.050 Uiso 1 1 calc R . . H8B H -0.3205 0.1098 0.4285 0.050 Uiso 1 1 calc R . . H8C H -0.3215 0.0065 0.3667 0.050 Uiso 1 1 calc R . . C9 C -0.1563(13) 0.2199(9) 0.3393(8) 0.042(3) Uani 1 1 d . . . H9A H -0.0530 0.2444 0.3275 0.063 Uiso 1 1 calc R . . H9B H -0.1735 0.2590 0.3935 0.063 Uiso 1 1 calc R . . H9C H -0.2405 0.2243 0.2928 0.063 Uiso 1 1 calc R . . C10 C 0.2404(11) -0.0347(7) 0.1760(6) 0.021(2) Uani 1 1 d . . . H10 H 0.3104 0.0221 0.2163 0.026 Uiso 1 1 calc R . . C11 C 0.2765(12) -0.0343(8) 0.0860(6) 0.029(3) Uani 1 1 d . . . H11A H 0.3914 -0.0295 0.0877 0.044 Uiso 1 1 calc R . . H11B H 0.2380 0.0214 0.0669 0.044 Uiso 1 1 calc R . . H11C H 0.2232 -0.0945 0.0459 0.044 Uiso 1 1 calc R . . C12 C 0.2830(13) -0.1243(8) 0.2047(8) 0.039(3) Uani 1 1 d . . . H12A H 0.2614 -0.1215 0.2626 0.058 Uiso 1 1 calc R . . H12B H 0.3960 -0.1277 0.2046 0.058 Uiso 1 1 calc R . . H12C H 0.2194 -0.1820 0.1654 0.058 Uiso 1 1 calc R . . C13 C 0.2552(10) 0.1581(7) 0.3448(6) 0.0166(15) Uani 1 1 d . . . C14 C 0.1841(10) 0.0291(7) 0.3975(6) 0.021(2) Uani 1 1 d . . . H14 H 0.1289 -0.0312 0.4010 0.025 Uiso 1 1 calc R . . C15 C 0.3016(11) 0.0845(7) 0.4567(6) 0.023(2) Uani 1 1 d . . . H15 H 0.3457 0.0715 0.5098 0.027 Uiso 1 1 calc R . . C16 C 0.4584(10) 0.2478(7) 0.4582(6) 0.016(2) Uani 1 1 d . . . C17 C 0.5560(10) 0.2778(7) 0.5379(6) 0.021(2) Uani 1 1 d . . . C18 C 0.6553(10) 0.3636(7) 0.5525(6) 0.021(2) Uani 1 1 d . . . H18 H 0.7242 0.3844 0.6065 0.026 Uiso 1 1 calc R . . C19 C 0.6634(10) 0.4230(7) 0.4941(6) 0.020(2) Uani 1 1 d . . . C20 C 0.5615(10) 0.3858(7) 0.4155(6) 0.021(2) Uani 1 1 d . . . C21 C 0.4367(10) 0.3726(7) 0.2722(6) 0.0166(15) Uani 1 1 d . . . C22 C 0.6291(10) 0.5063(7) 0.3225(6) 0.017(2) Uani 1 1 d . . . H22 H 0.7105 0.5533 0.3594 0.021 Uiso 1 1 calc R . . C23 C 0.5691(11) 0.5041(7) 0.2415(6) 0.022(2) Uani 1 1 d . . . H23 H 0.6000 0.5501 0.2099 0.027 Uiso 1 1 calc R . . C24 C 0.3605(11) 0.3976(7) 0.1243(6) 0.0182(15) Uani 1 1 d . . . C25 C 0.2165(10) 0.4320(7) 0.1119(6) 0.018(2) Uani 1 1 d . . . C26 C 0.1286(11) 0.4046(7) 0.0278(6) 0.023(2) Uani 1 1 d . . . H26 H 0.0282 0.4254 0.0159 0.028 Uiso 1 1 calc R . . C27 C 0.1855(12) 0.3483(8) -0.0376(7) 0.030(3) Uani 1 1 d . . . H27 H 0.1238 0.3299 -0.0936 0.035 Uiso 1 1 calc R . . C28 C 0.3339(12) 0.3184(7) -0.0211(7) 0.029(2) Uani 1 1 d . . . H28 H 0.3725 0.2804 -0.0668 0.034 Uiso 1 1 calc R . . C29 C 0.4261(11) 0.3426(7) 0.0598(6) 0.021(2) Uani 1 1 d . . . C30 C 0.1535(10) 0.4937(7) 0.1830(6) 0.020(2) Uani 1 1 d . . . H30 H 0.2082 0.4828 0.2385 0.024 Uiso 1 1 calc R . . C31 C -0.0255(11) 0.4678(8) 0.1782(7) 0.031(3) Uani 1 1 d . . . H31A H -0.0826 0.4826 0.1264 0.046 Uiso 1 1 calc R . . H31B H -0.0573 0.5058 0.2287 0.046 Uiso 1 1 calc R . . H31C H -0.0510 0.3985 0.1762 0.046 Uiso 1 1 calc R . . C32 C 0.1944(11) 0.6010(7) 0.1838(7) 0.029(3) Uani 1 1 d . . . H32A H 0.3098 0.6179 0.1910 0.043 Uiso 1 1 calc R . . H32B H 0.1560 0.6403 0.2314 0.043 Uiso 1 1 calc R . . H32C H 0.1437 0.6136 0.1296 0.043 Uiso 1 1 calc R . . C33 C 0.5866(11) 0.3057(8) 0.0792(6) 0.026(2) Uani 1 1 d . . . H33 H 0.6487 0.3505 0.1326 0.032 Uiso 1 1 calc R . . C34 C 0.5639(11) 0.2054(8) 0.0972(8) 0.036(3) Uani 1 1 d . . . H34A H 0.4988 0.2052 0.1417 0.053 Uiso 1 1 calc R . . H34B H 0.6676 0.1875 0.1168 0.053 Uiso 1 1 calc R . . H34C H 0.5106 0.1585 0.0448 0.053 Uiso 1 1 calc R . . C35 C 0.6831(13) 0.3116(10) 0.0074(7) 0.041(3) Uani 1 1 d . . . H35A H 0.6324 0.2628 -0.0444 0.062 Uiso 1 1 calc R . . H35B H 0.7913 0.2992 0.0257 0.062 Uiso 1 1 calc R . . H35C H 0.6871 0.3764 -0.0047 0.062 Uiso 1 1 calc R . . C36 C 0.5593(11) 0.2165(8) 0.6052(7) 0.026(2) Uani 1 1 d . . . H36A H 0.5987 0.1558 0.5839 0.039 Uiso 1 1 calc R . . H36B H 0.4517 0.2020 0.6165 0.039 Uiso 1 1 calc R . . H36C H 0.6295 0.2526 0.6581 0.039 Uiso 1 1 calc R . . C37 C 0.7775(12) 0.5142(8) 0.5148(7) 0.029(3) Uani 1 1 d . . . H37A H 0.8253 0.5291 0.5757 0.044 Uiso 1 1 calc R . . H37B H 0.7217 0.5674 0.5022 0.044 Uiso 1 1 calc R . . H37C H 0.8610 0.5062 0.4802 0.044 Uiso 1 1 calc R . . C38 C 0.1390(11) 0.2284(8) 0.6926(7) 0.029(3) Uani 1 1 d . . . N1 N 0.1570(9) 0.0746(6) 0.3305(5) 0.0198(18) Uani 1 1 d . . . N2 N 0.3462(8) 0.1651(6) 0.4249(5) 0.0193(18) Uani 1 1 d . . . N3 N 0.4630(8) 0.3018(5) 0.3994(5) 0.0130(17) Uani 1 1 d . . . N4 N 0.5481(8) 0.4253(6) 0.3424(5) 0.0184(18) Uani 1 1 d . . . N5 N 0.4532(8) 0.4230(6) 0.2110(5) 0.0206(19) Uani 1 1 d . . . O1 O 0.0115(7) 0.3608(5) 0.6333(4) 0.0292(17) Uani 1 1 d . . . O2 O 0.1789(8) 0.2698(5) 0.5492(5) 0.0336(18) Uani 1 1 d . . . O3 O -0.0813(8) 0.1930(5) 0.5605(5) 0.0339(19) Uani 1 1 d . . . F1 F 0.1861(7) 0.1415(4) 0.6691(4) 0.0391(16) Uani 1 1 d . . . F2 F 0.0376(7) 0.2180(5) 0.7448(4) 0.0398(16) Uani 1 1 d . . . F3 F 0.2666(7) 0.2889(5) 0.7359(4) 0.0436(18) Uani 1 1 d . . . S1 S 0.0507(3) 0.26732(18) 0.59724(16) 0.0230(6) Uani 1 1 d . . . Ni1 Ni 0.32105(13) 0.26162(9) 0.29468(8) 0.0165(3) Uani 1 1 d . . . Br1 Br 0.13901(12) 0.21840(8) 0.17144(7) 0.0274(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(4) 0.007(4) 0.016(4) 0.006(3) 0.004(3) -0.006(3) C2 0.023(3) 0.014(4) 0.021(4) 0.008(3) 0.005(3) -0.001(3) C3 0.014(4) 0.022(6) 0.034(6) 0.010(5) 0.005(4) 0.006(4) C4 0.034(6) 0.015(6) 0.029(6) 0.004(5) 0.005(5) -0.011(4) C5 0.029(5) 0.022(6) 0.025(6) 0.003(5) 0.007(4) 0.005(4) C6 0.023(3) 0.014(4) 0.021(4) 0.008(3) 0.005(3) -0.001(3) C7 0.018(5) 0.026(6) 0.031(6) 0.000(5) 0.001(4) 0.006(4) C8 0.033(6) 0.023(6) 0.046(7) 0.005(5) 0.022(5) 0.003(5) C9 0.035(6) 0.043(8) 0.046(8) 0.002(6) 0.015(6) 0.001(5) C10 0.028(5) 0.024(6) 0.016(5) 0.005(4) 0.014(4) 0.005(4) C11 0.032(6) 0.033(7) 0.023(6) 0.006(5) 0.009(5) 0.005(5) C12 0.034(6) 0.038(7) 0.055(8) 0.026(6) 0.011(6) 0.016(5) C13 0.018(3) 0.011(4) 0.022(4) 0.003(3) 0.008(3) 0.008(3) C14 0.023(5) 0.023(6) 0.021(6) 0.008(5) 0.010(4) 0.002(4) C15 0.024(5) 0.029(6) 0.015(6) 0.006(5) 0.000(4) 0.004(4) C16 0.016(4) 0.019(6) 0.014(5) 0.010(4) -0.002(4) -0.003(4) C17 0.017(5) 0.018(6) 0.029(6) 0.008(5) 0.010(4) 0.002(4) C18 0.013(4) 0.030(6) 0.019(6) -0.001(5) 0.002(4) 0.007(4) C19 0.012(4) 0.027(6) 0.019(6) 0.000(5) -0.001(4) 0.006(4) C20 0.011(4) 0.027(6) 0.028(6) 0.011(5) 0.008(4) 0.006(4) C21 0.018(3) 0.011(4) 0.022(4) 0.003(3) 0.008(3) 0.008(3) C22 0.017(4) 0.018(6) 0.024(6) 0.016(4) 0.004(4) 0.003(4) C23 0.026(5) 0.025(6) 0.013(6) 0.001(4) 0.004(4) -0.004(4) C24 0.030(4) 0.007(4) 0.016(4) 0.006(3) 0.004(3) -0.006(3) C25 0.018(5) 0.019(6) 0.023(6) 0.011(4) 0.009(4) -0.001(4) C26 0.021(5) 0.020(6) 0.028(6) 0.006(5) 0.004(4) 0.002(4) C27 0.037(6) 0.032(7) 0.018(6) 0.006(5) -0.004(5) 0.010(5) C28 0.049(6) 0.013(6) 0.026(6) 0.008(5) 0.011(5) 0.001(5) C29 0.031(5) 0.023(6) 0.016(6) 0.010(4) 0.009(4) 0.008(4) C30 0.026(5) 0.020(6) 0.015(5) 0.008(4) -0.002(4) 0.005(4) C31 0.025(5) 0.040(7) 0.031(7) 0.008(5) 0.016(5) 0.005(5) C32 0.023(5) 0.030(7) 0.030(7) -0.002(5) 0.003(4) 0.006(4) C33 0.028(5) 0.035(7) 0.013(6) -0.004(5) 0.004(4) 0.009(5) C34 0.023(5) 0.037(7) 0.048(8) 0.001(6) 0.015(5) 0.015(5) C35 0.034(6) 0.059(9) 0.030(7) 0.001(6) 0.014(5) 0.010(6) C36 0.025(5) 0.026(6) 0.027(6) 0.009(5) 0.004(4) -0.003(4) C37 0.031(5) 0.029(7) 0.023(6) 0.002(5) -0.005(5) 0.000(5) C38 0.023(5) 0.023(6) 0.039(7) -0.001(5) 0.013(5) 0.002(4) N1 0.025(4) 0.012(5) 0.023(5) 0.008(4) 0.003(4) 0.000(3) N2 0.017(4) 0.026(5) 0.014(4) 0.003(4) 0.002(3) 0.003(3) N3 0.017(4) 0.013(4) 0.008(4) -0.001(3) 0.004(3) 0.000(3) N4 0.020(4) 0.019(5) 0.018(5) 0.005(4) 0.009(3) -0.001(3) N5 0.016(4) 0.021(5) 0.023(5) 0.007(4) -0.003(3) 0.000(3) O1 0.031(4) 0.024(4) 0.032(4) 0.002(3) 0.005(3) 0.008(3) O2 0.036(4) 0.033(5) 0.040(5) 0.014(4) 0.023(3) 0.005(3) O3 0.027(4) 0.034(5) 0.033(5) -0.001(4) 0.001(3) -0.009(3) F1 0.046(4) 0.025(4) 0.052(4) 0.017(3) 0.012(3) 0.010(3) F2 0.044(4) 0.052(4) 0.027(4) 0.013(3) 0.016(3) 0.003(3) F3 0.038(4) 0.036(4) 0.049(4) 0.014(3) -0.013(3) -0.009(3) S1 0.0242(12) 0.0203(15) 0.0233(15) 0.0019(11) 0.0061(10) 0.0005(10) Ni1 0.0167(6) 0.0166(7) 0.0150(7) 0.0049(5) -0.0003(5) -0.0011(5) Br1 0.0297(5) 0.0250(6) 0.0238(6) 0.0103(5) -0.0053(4) -0.0067(4) _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 C1 C6 1.384(13) . ? C1 C2 1.404(13) . ? C1 N1 1.469(11) . ? C2 C3 1.367(13) . ? C2 C7 1.520(14) . ? C3 C4 1.395(14) . ? C3 H3 0.9500 . ? C4 C5 1.391(13) . ? C4 H4 0.9500 . ? C5 C6 1.377(13) . ? C5 H5 0.9500 . ? C6 C10 1.540(12) . ? C7 C9 1.520(16) . ? C7 C8 1.536(13) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.507(14) . ? C10 C11 1.540(13) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.336(11) . ? C13 N2 1.390(12) . ? C13 Ni1 1.897(10) . ? C14 C15 1.336(13) . ? C14 N1 1.379(12) . ? C14 H14 0.9500 . ? C15 N2 1.390(13) . ? C15 H15 0.9500 . ? C16 N3 1.344(11) . ? C16 C17 1.387(13) . ? C16 N2 1.393(11) . ? C17 C18 1.367(13) . ? C17 C36 1.528(14) . ? C18 C19 1.397(14) . ? C18 H18 0.9500 . ? C19 C20 1.399(13) . ? C19 C37 1.484(13) . ? C20 N3 1.341(12) . ? C20 N4 1.407(12) . ? C21 N5 1.354(12) . ? C21 N4 1.392(11) . ? C21 Ni1 1.901(9) . ? C22 C23 1.328(13) . ? C22 N4 1.401(12) . ? C22 H22 0.9500 . ? C23 N5 1.391(12) . ? C23 H23 0.9500 . ? C24 C25 1.384(13) . ? C24 C29 1.404(13) . ? C24 N5 1.460(12) . ? C25 C26 1.409(13) . ? C25 C30 1.510(13) . ? C26 C27 1.380(14) . ? C26 H26 0.9500 . ? C27 C28 1.395(14) . ? C27 H27 0.9500 . ? C28 C29 1.382(14) . ? C28 H28 0.9500 . ? C29 C33 1.543(13) . ? C30 C32 1.525(14) . ? C30 C31 1.531(12) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.512(15) . ? C33 C35 1.541(14) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 F2 1.323(11) . ? C38 F3 1.324(11) . ? C38 F1 1.342(12) . ? C38 S1 1.833(12) . ? N3 Ni1 1.877(7) . ? O1 S1 1.437(7) . ? O2 S1 1.447(7) . ? O3 S1 1.428(7) . ? Ni1 Br1 2.2717(15) . ? 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 C6 C1 C2 124.0(9) . . ? C6 C1 N1 119.2(8) . . ? C2 C1 N1 116.8(8) . . ? C3 C2 C1 115.9(9) . . ? C3 C2 C7 121.7(8) . . ? C1 C2 C7 122.3(8) . . ? C2 C3 C4 121.8(9) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 120.5(9) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 119.4(9) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C1 118.4(9) . . ? C5 C6 C10 120.4(9) . . ? C1 C6 C10 121.3(8) . . ? C2 C7 C9 112.0(9) . . ? C2 C7 C8 112.9(8) . . ? C9 C7 C8 110.6(8) . . ? C2 C7 H7 107.0 . . ? C9 C7 H7 107.0 . . ? C8 C7 H7 107.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.5(9) . . ? C12 C10 C6 112.2(8) . . ? C11 C10 C6 112.1(8) . . ? C12 C10 H10 106.9 . . ? C11 C10 H10 106.9 . . ? C6 C10 H10 106.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 104.2(8) . . ? N1 C13 Ni1 143.6(7) . . ? N2 C13 Ni1 112.0(6) . . ? C15 C14 N1 108.0(9) . . ? C15 C14 H14 126.0 . . ? N1 C14 H14 126.0 . . ? C14 C15 N2 106.2(9) . . ? C14 C15 H15 126.9 . . ? N2 C15 H15 126.9 . . ? N3 C16 C17 120.6(8) . . ? N3 C16 N2 109.4(8) . . ? C17 C16 N2 129.9(9) . . ? C18 C17 C16 116.7(9) . . ? C18 C17 C36 121.0(9) . . ? C16 C17 C36 122.2(8) . . ? C17 C18 C19 125.0(9) . . ? C17 C18 H18 117.5 . . ? C19 C18 H18 117.5 . . ? C18 C19 C20 113.9(9) . . ? C18 C19 C37 121.3(9) . . ? C20 C19 C37 124.8(9) . . ? N3 C20 C19 122.4(9) . . ? N3 C20 N4 110.0(8) . . ? C19 C20 N4 127.6(9) . . ? N5 C21 N4 103.4(8) . . ? N5 C21 Ni1 143.3(7) . . ? N4 C21 Ni1 113.3(7) . . ? C23 C22 N4 106.2(8) . . ? C23 C22 H22 126.9 . . ? N4 C22 H22 126.9 . . ? C22 C23 N5 108.3(9) . . ? C22 C23 H23 125.9 . . ? N5 C23 H23 125.9 . . ? C25 C24 C29 125.1(9) . . ? C25 C24 N5 117.3(8) . . ? C29 C24 N5 117.6(8) . . ? C24 C25 C26 115.9(9) . . ? C24 C25 C30 123.1(9) . . ? C26 C25 C30 121.1(8) . . ? C27 C26 C25 121.4(9) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 119.9(10) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 121.7(10) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C28 C29 C24 116.0(9) . . ? C28 C29 C33 121.9(9) . . ? C24 C29 C33 122.0(9) . . ? C25 C30 C32 110.3(8) . . ? C25 C30 C31 113.3(8) . . ? C32 C30 C31 110.0(8) . . ? C25 C30 H30 107.7 . . ? C32 C30 H30 107.7 . . ? C31 C30 H30 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 112.9(9) . . ? C34 C33 C29 111.3(8) . . ? C35 C33 C29 111.0(9) . . ? C34 C33 H33 107.1 . . ? C35 C33 H33 107.1 . . ? C29 C33 H33 107.1 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C19 C37 H37A 109.5 . . ? C19 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C19 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? F2 C38 F3 108.9(9) . . ? F2 C38 F1 106.7(9) . . ? F3 C38 F1 106.7(8) . . ? F2 C38 S1 112.7(7) . . ? F3 C38 S1 111.9(8) . . ? F1 C38 S1 109.7(7) . . ? C13 N1 C14 111.4(8) . . ? C13 N1 C1 126.6(8) . . ? C14 N1 C1 122.0(8) . . ? C13 N2 C15 110.2(7) . . ? C13 N2 C16 117.1(8) . . ? C15 N2 C16 132.7(8) . . ? C20 N3 C16 121.5(8) . . ? C20 N3 Ni1 119.4(7) . . ? C16 N3 Ni1 119.1(6) . . ? C21 N4 C22 110.9(8) . . ? C21 N4 C20 115.5(8) . . ? C22 N4 C20 133.6(8) . . ? C21 N5 C23 111.3(8) . . ? C21 N5 C24 125.0(8) . . ? C23 N5 C24 123.7(8) . . ? O3 S1 O1 115.5(4) . . ? O3 S1 O2 115.7(4) . . ? O1 S1 O2 114.8(4) . . ? O3 S1 C38 102.7(5) . . ? O1 S1 C38 102.4(4) . . ? O2 S1 C38 102.9(4) . . ? N3 Ni1 C13 82.0(4) . . ? N3 Ni1 C21 81.5(4) . . ? C13 Ni1 C21 163.2(4) . . ? N3 Ni1 Br1 176.6(2) . . ? C13 Ni1 Br1 98.0(3) . . ? C21 Ni1 Br1 98.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.4(14) . . . . ? N1 C1 C2 C3 -178.9(8) . . . . ? C6 C1 C2 C7 -177.6(10) . . . . ? N1 C1 C2 C7 4.8(13) . . . . ? C1 C2 C3 C4 2.2(15) . . . . ? C7 C2 C3 C4 178.4(10) . . . . ? C2 C3 C4 C5 -1.2(16) . . . . ? C3 C4 C5 C6 -0.7(15) . . . . ? C4 C5 C6 C1 1.5(15) . . . . ? C4 C5 C6 C10 -178.3(9) . . . . ? C2 C1 C6 C5 -0.5(15) . . . . ? N1 C1 C6 C5 177.0(9) . . . . ? C2 C1 C6 C10 179.4(9) . . . . ? N1 C1 C6 C10 -3.1(14) . . . . ? C3 C2 C7 C9 -84.7(11) . . . . ? C1 C2 C7 C9 91.3(11) . . . . ? C3 C2 C7 C8 40.9(14) . . . . ? C1 C2 C7 C8 -143.1(9) . . . . ? C5 C6 C10 C12 -89.3(12) . . . . ? C1 C6 C10 C12 90.9(11) . . . . ? C5 C6 C10 C11 37.1(13) . . . . ? C1 C6 C10 C11 -142.7(10) . . . . ? N1 C14 C15 N2 0.1(10) . . . . ? N3 C16 C17 C18 -0.2(13) . . . . ? N2 C16 C17 C18 -179.9(9) . . . . ? N3 C16 C17 C36 -177.4(8) . . . . ? N2 C16 C17 C36 3.0(16) . . . . ? C16 C17 C18 C19 1.1(14) . . . . ? C36 C17 C18 C19 178.3(9) . . . . ? C17 C18 C19 C20 -1.7(13) . . . . ? C17 C18 C19 C37 -178.7(9) . . . . ? C18 C19 C20 N3 1.5(13) . . . . ? C37 C19 C20 N3 178.4(9) . . . . ? C18 C19 C20 N4 -176.2(8) . . . . ? C37 C19 C20 N4 0.7(15) . . . . ? N4 C22 C23 N5 -0.3(10) . . . . ? C29 C24 C25 C26 3.0(14) . . . . ? N5 C24 C25 C26 -178.9(8) . . . . ? C29 C24 C25 C30 -177.9(9) . . . . ? N5 C24 C25 C30 0.3(13) . . . . ? C24 C25 C26 C27 -0.9(14) . . . . ? C30 C25 C26 C27 179.9(10) . . . . ? C25 C26 C27 C28 -0.9(16) . . . . ? C26 C27 C28 C29 0.9(16) . . . . ? C27 C28 C29 C24 1.0(15) . . . . ? C27 C28 C29 C33 177.1(10) . . . . ? C25 C24 C29 C28 -3.0(14) . . . . ? N5 C24 C29 C28 178.8(8) . . . . ? C25 C24 C29 C33 -179.1(9) . . . . ? N5 C24 C29 C33 2.7(14) . . . . ? C24 C25 C30 C32 95.9(11) . . . . ? C26 C25 C30 C32 -85.0(10) . . . . ? C24 C25 C30 C31 -140.2(9) . . . . ? C26 C25 C30 C31 38.9(13) . . . . ? C28 C29 C33 C34 -84.2(12) . . . . ? C24 C29 C33 C34 91.6(11) . . . . ? C28 C29 C33 C35 42.4(13) . . . . ? C24 C29 C33 C35 -141.7(10) . . . . ? N2 C13 N1 C14 -0.6(10) . . . . ? Ni1 C13 N1 C14 173.8(9) . . . . ? N2 C13 N1 C1 177.2(8) . . . . ? Ni1 C13 N1 C1 -8.3(17) . . . . ? C15 C14 N1 C13 0.4(11) . . . . ? C15 C14 N1 C1 -177.6(8) . . . . ? C6 C1 N1 C13 85.1(12) . . . . ? C2 C1 N1 C13 -97.3(11) . . . . ? C6 C1 N1 C14 -97.3(11) . . . . ? C2 C1 N1 C14 80.4(11) . . . . ? N1 C13 N2 C15 0.7(9) . . . . ? Ni1 C13 N2 C15 -175.8(6) . . . . ? N1 C13 N2 C16 -178.4(7) . . . . ? Ni1 C13 N2 C16 5.1(9) . . . . ? C14 C15 N2 C13 -0.5(10) . . . . ? C14 C15 N2 C16 178.4(9) . . . . ? N3 C16 N2 C13 -5.2(11) . . . . ? C17 C16 N2 C13 174.5(9) . . . . ? N3 C16 N2 C15 175.9(9) . . . . ? C17 C16 N2 C15 -4.4(17) . . . . ? C19 C20 N3 C16 -0.8(13) . . . . ? N4 C20 N3 C16 177.3(8) . . . . ? C19 C20 N3 Ni1 176.0(7) . . . . ? N4 C20 N3 Ni1 -6.0(9) . . . . ? C17 C16 N3 C20 0.1(13) . . . . ? N2 C16 N3 C20 179.8(8) . . . . ? C17 C16 N3 Ni1 -176.7(7) . . . . ? N2 C16 N3 Ni1 3.0(10) . . . . ? N5 C21 N4 C22 0.1(9) . . . . ? Ni1 C21 N4 C22 -179.7(6) . . . . ? N5 C21 N4 C20 -177.3(7) . . . . ? Ni1 C21 N4 C20 2.8(9) . . . . ? C23 C22 N4 C21 0.1(10) . . . . ? C23 C22 N4 C20 176.9(9) . . . . ? N3 C20 N4 C21 1.8(10) . . . . ? C19 C20 N4 C21 179.7(9) . . . . ? N3 C20 N4 C22 -174.9(9) . . . . ? C19 C20 N4 C22 3.0(16) . . . . ? N4 C21 N5 C23 -0.3(10) . . . . ? Ni1 C21 N5 C23 179.4(9) . . . . ? N4 C21 N5 C24 -179.4(8) . . . . ? Ni1 C21 N5 C24 0.4(16) . . . . ? C22 C23 N5 C21 0.4(11) . . . . ? C22 C23 N5 C24 179.5(8) . . . . ? C25 C24 N5 C21 86.6(11) . . . . ? C29 C24 N5 C21 -95.1(11) . . . . ? C25 C24 N5 C23 -92.4(11) . . . . ? C29 C24 N5 C23 85.9(11) . . . . ? F2 C38 S1 O3 -57.3(8) . . . . ? F3 C38 S1 O3 179.5(7) . . . . ? F1 C38 S1 O3 61.3(7) . . . . ? F2 C38 S1 O1 62.8(8) . . . . ? F3 C38 S1 O1 -60.4(8) . . . . ? F1 C38 S1 O1 -178.5(6) . . . . ? F2 C38 S1 O2 -177.8(7) . . . . ? F3 C38 S1 O2 59.0(8) . . . . ? F1 C38 S1 O2 -59.2(7) . . . . ? C20 N3 Ni1 C13 -177.1(7) . . . . ? C16 N3 Ni1 C13 -0.3(7) . . . . ? C20 N3 Ni1 C21 6.2(7) . . . . ? C16 N3 Ni1 C21 -177.0(7) . . . . ? N1 C13 Ni1 N3 -176.7(11) . . . . ? N2 C13 Ni1 N3 -2.6(6) . . . . ? N1 C13 Ni1 C21 -165.4(11) . . . . ? N2 C13 Ni1 C21 8.8(16) . . . . ? N1 C13 Ni1 Br1 6.7(11) . . . . ? N2 C13 Ni1 Br1 -179.1(5) . . . . ? N5 C21 Ni1 N3 175.6(11) . . . . ? N4 C21 Ni1 N3 -4.6(6) . . . . ? N5 C21 Ni1 C13 164.3(11) . . . . ? N4 C21 Ni1 C13 -16.0(16) . . . . ? N5 C21 Ni1 Br1 -7.8(11) . . . . ? N4 C21 Ni1 Br1 172.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.654 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.163 #==END data_3PF6 _database_code_depnum_ccdc_archive 'CCDC 663960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Br N5 Ni, F6 P' _chemical_formula_sum 'C35 H41 Br F6 N5 Ni P' _chemical_formula_weight 815.32 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 35.7904(8) _cell_length_b 8.6403(2) _cell_length_c 23.4502(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.3100(10) _cell_angle_gamma 90.00 _cell_volume 7156.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8626 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 1.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8159 _exptl_absorpt_correction_T_max 0.9326 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41758 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8207 _reflns_number_gt 6537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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^)+(0.0150P)^2^+21.0296P] 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 8207 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.11569(7) 0.0738(3) 0.23875(10) 0.0177(5) Uani 1 1 d . . . C2 C 0.11942(7) -0.0872(3) 0.23744(11) 0.0194(6) Uani 1 1 d . . . C3 C 0.08984(7) -0.1739(3) 0.25314(12) 0.0259(6) Uani 1 1 d . . . H3 H 0.0910 -0.2836 0.2521 0.031 Uiso 1 1 calc R . . C4 C 0.05885(7) -0.1026(4) 0.27015(12) 0.0284(7) Uani 1 1 d . . . H4 H 0.0392 -0.1639 0.2812 0.034 Uiso 1 1 calc R . . C5 C 0.05618(7) 0.0564(3) 0.27129(12) 0.0264(6) Uani 1 1 d . . . H5 H 0.0347 0.1034 0.2833 0.032 Uiso 1 1 calc R . . C6 C 0.08450(7) 0.1495(3) 0.25499(11) 0.0197(6) Uani 1 1 d . . . C7 C 0.15385(7) -0.1667(3) 0.22056(12) 0.0245(6) Uani 1 1 d . . . H7 H 0.1683 -0.0877 0.2017 0.029 Uiso 1 1 calc R . . C8 C 0.17974(8) -0.2268(4) 0.27379(15) 0.0448(9) Uani 1 1 d . . . H8A H 0.1867 -0.1413 0.3009 0.067 Uiso 1 1 calc R . . H8B H 0.2026 -0.2709 0.2623 0.067 Uiso 1 1 calc R . . H8C H 0.1665 -0.3068 0.2924 0.067 Uiso 1 1 calc R . . C9 C 0.14325(9) -0.2982(4) 0.17742(14) 0.0363(7) Uani 1 1 d . . . H9A H 0.1321 -0.3836 0.1965 0.054 Uiso 1 1 calc R . . H9B H 0.1660 -0.3347 0.1632 0.054 Uiso 1 1 calc R . . H9C H 0.1248 -0.2606 0.1449 0.054 Uiso 1 1 calc R . . C10 C 0.08088(7) 0.3248(3) 0.25274(11) 0.0227(6) Uani 1 1 d . . . H10 H 0.1070 0.3691 0.2567 0.027 Uiso 1 1 calc R . . C11 C 0.05928(9) 0.3746(4) 0.19392(13) 0.0371(8) Uani 1 1 d . . . H11A H 0.0726 0.3371 0.1633 0.056 Uiso 1 1 calc R . . H11B H 0.0577 0.4878 0.1923 0.056 Uiso 1 1 calc R . . H11C H 0.0337 0.3309 0.1885 0.056 Uiso 1 1 calc R . . C12 C 0.06196(10) 0.3922(4) 0.30104(14) 0.0406(8) Uani 1 1 d . . . H12A H 0.0358 0.3553 0.2969 0.061 Uiso 1 1 calc R . . H12B H 0.0621 0.5055 0.2987 0.061 Uiso 1 1 calc R . . H12C H 0.0759 0.3592 0.3385 0.061 Uiso 1 1 calc R . . C13 C 0.15305(6) 0.2154(3) 0.17318(11) 0.0153(5) Uani 1 1 d . . . C14 C 0.17392(7) 0.2285(3) 0.26948(11) 0.0218(6) Uani 1 1 d . . . H14 H 0.1752 0.2110 0.3097 0.026 Uiso 1 1 calc R . . C15 C 0.19802(7) 0.3143(3) 0.24475(11) 0.0202(6) Uani 1 1 d . . . H15 H 0.2195 0.3696 0.2635 0.024 Uiso 1 1 calc R . . C16 C 0.20062(6) 0.3640(3) 0.13954(11) 0.0155(5) Uani 1 1 d . . . C17 C 0.23264(7) 0.4528(3) 0.14148(11) 0.0184(5) Uani 1 1 d . . . H17 H 0.2473 0.4830 0.1772 0.022 Uiso 1 1 calc R . . C18 C 0.24262(7) 0.4963(3) 0.08900(12) 0.0207(6) Uani 1 1 d . . . H18 H 0.2644 0.5588 0.0887 0.025 Uiso 1 1 calc R . . C19 C 0.22142(7) 0.4502(3) 0.03709(11) 0.0200(6) Uani 1 1 d . . . H19 H 0.2284 0.4788 0.0011 0.024 Uiso 1 1 calc R . . C20 C 0.18988(6) 0.3613(3) 0.03988(11) 0.0163(5) Uani 1 1 d . . . C21 C 0.13509(6) 0.2117(3) 0.00877(11) 0.0160(5) Uani 1 1 d . . . C22 C 0.16335(7) 0.3081(3) -0.06486(11) 0.0214(6) Uani 1 1 d . . . H22 H 0.1805 0.3620 -0.0847 0.026 Uiso 1 1 calc R . . C23 C 0.13299(7) 0.2242(3) -0.08827(11) 0.0215(6) Uani 1 1 d . . . H23 H 0.1246 0.2071 -0.1283 0.026 Uiso 1 1 calc R . . C24 C 0.08290(7) 0.0675(3) -0.05358(10) 0.0176(5) Uani 1 1 d . . . C25 C 0.08822(7) -0.0921(3) -0.04831(11) 0.0191(6) Uani 1 1 d . . . C26 C 0.05623(7) -0.1849(3) -0.06217(11) 0.0241(6) Uani 1 1 d . . . H26 H 0.0586 -0.2943 -0.0596 0.029 Uiso 1 1 calc R . . C27 C 0.02095(7) -0.1193(4) -0.07971(12) 0.0269(6) Uani 1 1 d . . . H27 H -0.0005 -0.1843 -0.0895 0.032 Uiso 1 1 calc R . . C28 C 0.01654(7) 0.0389(4) -0.08316(12) 0.0265(6) Uani 1 1 d . . . H28 H -0.0080 0.0815 -0.0947 0.032 Uiso 1 1 calc R . . C29 C 0.04759(7) 0.1373(3) -0.07003(11) 0.0203(6) Uani 1 1 d . . . C30 C 0.12722(7) -0.1620(3) -0.02778(12) 0.0256(6) Uani 1 1 d . . . H30 H 0.1419 -0.0861 -0.0008 0.031 Uiso 1 1 calc R . . C31 C 0.12540(9) -0.3136(4) 0.00536(14) 0.0387(8) Uani 1 1 d . . . H31A H 0.1096 -0.2991 0.0354 0.058 Uiso 1 1 calc R . . H31B H 0.1510 -0.3439 0.0233 0.058 Uiso 1 1 calc R . . H31C H 0.1144 -0.3948 -0.0214 0.058 Uiso 1 1 calc R . . C32 C 0.14902(9) -0.1869(4) -0.07832(15) 0.0410(8) Uani 1 1 d . . . H32A H 0.1359 -0.2645 -0.1048 0.061 Uiso 1 1 calc R . . H32B H 0.1747 -0.2230 -0.0634 0.061 Uiso 1 1 calc R . . H32C H 0.1504 -0.0891 -0.0990 0.061 Uiso 1 1 calc R . . C33 C 0.04293(7) 0.3127(3) -0.06953(12) 0.0249(6) Uani 1 1 d . . . H33 H 0.0657 0.3599 -0.0823 0.030 Uiso 1 1 calc R . . C34 C 0.04156(8) 0.3687(3) -0.00776(12) 0.0300(7) Uani 1 1 d . . . H34A H 0.0193 0.3247 0.0057 0.045 Uiso 1 1 calc R . . H34B H 0.0400 0.4819 -0.0074 0.045 Uiso 1 1 calc R . . H34C H 0.0645 0.3351 0.0178 0.045 Uiso 1 1 calc R . . C35 C 0.00778(8) 0.3707(4) -0.11018(14) 0.0369(8) Uani 1 1 d . . . H35A H 0.0079 0.3297 -0.1491 0.055 Uiso 1 1 calc R . . H35B H 0.0080 0.4840 -0.1114 0.055 Uiso 1 1 calc R . . H35C H -0.0151 0.3353 -0.0960 0.055 Uiso 1 1 calc R . . N1 N 0.14650(5) 0.1691(2) 0.22552(9) 0.0159(4) Uani 1 1 d . . . N2 N 0.18505(5) 0.3053(2) 0.18613(9) 0.0157(4) Uani 1 1 d . . . N3 N 0.17935(5) 0.3212(2) 0.08998(9) 0.0147(4) Uani 1 1 d . . . N4 N 0.16422(5) 0.2991(2) -0.00598(9) 0.0165(4) Uani 1 1 d . . . N5 N 0.11602(5) 0.1668(3) -0.04276(9) 0.0169(5) Uani 1 1 d . . . F1 F 0.24336(4) 0.10486(18) 0.07933(7) 0.0293(4) Uani 1 1 d . . . F2 F 0.23918(4) 0.04834(18) 0.17240(7) 0.0272(4) Uani 1 1 d . . . F3 F 0.19480(4) -0.0417(2) 0.10035(7) 0.0338(4) Uani 1 1 d . . . F4 F 0.23690(4) -0.20643(18) 0.15140(6) 0.0263(4) Uani 1 1 d . . . F5 F 0.24072(5) -0.15133(19) 0.05768(7) 0.0352(4) Uani 1 1 d . . . F6 F 0.28515(4) -0.06066(19) 0.12944(7) 0.0323(4) Uani 1 1 d . . . P1 P 0.239645(18) -0.05174(8) 0.11478(3) 0.01860(15) Uani 1 1 d . . . Ni1 Ni 0.137216(8) 0.19462(4) 0.091093(13) 0.01389(8) Uani 1 1 d . . . Br1 Br 0.085792(7) 0.04115(3) 0.092960(11) 0.01994(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0153(12) 0.0254(15) 0.0127(12) 0.0049(11) 0.0029(9) -0.0024(11) C2 0.0202(12) 0.0245(15) 0.0135(12) 0.0039(11) 0.0023(10) -0.0005(11) C3 0.0274(14) 0.0252(16) 0.0254(15) 0.0033(13) 0.0051(11) -0.0047(12) C4 0.0203(13) 0.0350(18) 0.0317(16) 0.0056(14) 0.0096(11) -0.0090(12) C5 0.0197(13) 0.0334(18) 0.0281(15) 0.0045(13) 0.0095(11) 0.0012(12) C6 0.0181(12) 0.0257(15) 0.0157(13) 0.0031(11) 0.0037(10) 0.0014(11) C7 0.0256(14) 0.0205(15) 0.0299(15) 0.0049(12) 0.0122(11) 0.0025(12) C8 0.0270(16) 0.058(2) 0.048(2) -0.0047(18) -0.0014(14) 0.0120(16) C9 0.0407(17) 0.0319(18) 0.0367(18) -0.0040(15) 0.0072(14) 0.0104(15) C10 0.0178(12) 0.0285(16) 0.0224(14) 0.0021(12) 0.0052(10) 0.0030(11) C11 0.0438(18) 0.0332(19) 0.0310(17) 0.0026(15) -0.0044(14) 0.0097(15) C12 0.054(2) 0.035(2) 0.0389(19) -0.0001(16) 0.0255(16) 0.0062(16) C13 0.0119(11) 0.0144(13) 0.0203(13) -0.0005(11) 0.0043(9) 0.0010(10) C14 0.0180(12) 0.0311(17) 0.0156(13) -0.0031(12) 0.0006(10) -0.0025(11) C15 0.0182(12) 0.0242(15) 0.0174(13) -0.0043(12) 0.0004(10) -0.0012(11) C16 0.0158(11) 0.0129(13) 0.0187(13) -0.0010(11) 0.0053(9) 0.0018(10) C17 0.0145(11) 0.0168(14) 0.0239(14) -0.0024(11) 0.0031(10) -0.0013(10) C18 0.0155(12) 0.0168(14) 0.0314(15) 0.0006(12) 0.0089(11) -0.0019(10) C19 0.0196(12) 0.0191(14) 0.0233(14) 0.0047(12) 0.0096(10) 0.0001(11) C20 0.0143(11) 0.0159(14) 0.0189(13) 0.0012(11) 0.0036(9) 0.0018(10) C21 0.0105(11) 0.0166(14) 0.0216(13) 0.0025(11) 0.0048(9) 0.0012(10) C22 0.0182(12) 0.0284(16) 0.0189(13) 0.0053(12) 0.0065(10) -0.0014(11) C23 0.0194(12) 0.0314(17) 0.0150(13) 0.0029(12) 0.0067(10) -0.0009(11) C24 0.0154(12) 0.0245(15) 0.0136(12) -0.0004(11) 0.0043(9) -0.0039(10) C25 0.0202(12) 0.0234(15) 0.0144(12) 0.0003(11) 0.0047(10) 0.0009(11) C26 0.0306(14) 0.0232(16) 0.0194(14) -0.0030(12) 0.0067(11) -0.0035(12) C27 0.0224(13) 0.0360(18) 0.0219(14) -0.0019(13) 0.0027(11) -0.0109(13) C28 0.0158(12) 0.0362(18) 0.0271(15) 0.0079(14) 0.0023(11) -0.0011(12) C29 0.0161(12) 0.0289(16) 0.0168(13) 0.0044(12) 0.0051(10) -0.0005(11) C30 0.0242(14) 0.0201(15) 0.0314(16) -0.0056(13) 0.0010(11) 0.0028(12) C31 0.0399(18) 0.0291(18) 0.046(2) 0.0043(16) 0.0044(15) 0.0127(15) C32 0.0333(17) 0.041(2) 0.053(2) -0.0001(17) 0.0197(15) 0.0102(15) C33 0.0178(12) 0.0279(16) 0.0297(15) 0.0111(13) 0.0060(11) 0.0026(11) C34 0.0324(15) 0.0243(17) 0.0346(17) 0.0077(14) 0.0094(13) 0.0089(13) C35 0.0327(16) 0.039(2) 0.0388(18) 0.0143(16) 0.0048(13) 0.0089(14) N1 0.0133(10) 0.0188(12) 0.0162(11) 0.0019(9) 0.0048(8) -0.0006(8) N2 0.0137(9) 0.0184(12) 0.0156(10) -0.0018(9) 0.0041(8) -0.0005(9) N3 0.0141(9) 0.0133(11) 0.0173(11) 0.0012(9) 0.0041(8) 0.0003(8) N4 0.0133(10) 0.0191(12) 0.0182(11) 0.0032(9) 0.0058(8) 0.0002(9) N5 0.0135(9) 0.0224(12) 0.0154(11) 0.0036(9) 0.0045(8) 0.0002(9) F1 0.0393(9) 0.0207(9) 0.0312(9) 0.0094(7) 0.0159(7) 0.0071(7) F2 0.0346(9) 0.0237(9) 0.0252(8) -0.0042(7) 0.0106(7) 0.0025(7) F3 0.0215(8) 0.0441(11) 0.0351(10) 0.0074(9) 0.0021(7) 0.0010(8) F4 0.0387(9) 0.0193(9) 0.0225(8) 0.0046(7) 0.0093(7) -0.0016(7) F5 0.0632(12) 0.0238(9) 0.0217(9) -0.0009(7) 0.0163(8) 0.0034(8) F6 0.0208(8) 0.0357(10) 0.0423(10) 0.0091(8) 0.0109(7) 0.0065(7) P1 0.0203(3) 0.0176(4) 0.0193(3) 0.0026(3) 0.0075(3) 0.0032(3) Ni1 0.01120(14) 0.01702(18) 0.01401(16) 0.00175(14) 0.00370(11) -0.00209(13) Br1 0.01521(12) 0.02686(16) 0.01805(13) 0.00257(11) 0.00356(9) -0.00713(11) _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 C1 C6 1.398(3) . ? C1 C2 1.399(4) . ? C1 N1 1.450(3) . ? C2 C3 1.394(4) . ? C2 C7 1.518(3) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.378(4) . ? C4 H4 0.9500 . ? C5 C6 1.395(4) . ? C5 H5 0.9500 . ? C6 C10 1.521(4) . ? C7 C8 1.521(4) . ? C7 C9 1.528(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.526(4) . ? C10 C11 1.530(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.347(3) . ? C13 N2 1.377(3) . ? C13 Ni1 1.925(2) . ? C14 C15 1.339(4) . ? C14 N1 1.401(3) . ? C14 H14 0.9500 . ? C15 N2 1.380(3) . ? C15 H15 0.9500 . ? C16 N3 1.334(3) . ? C16 C17 1.373(3) . ? C16 N2 1.399(3) . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.376(3) . ? C19 H19 0.9500 . ? C20 N3 1.336(3) . ? C20 N4 1.403(3) . ? C21 N5 1.345(3) . ? C21 N4 1.376(3) . ? C21 Ni1 1.925(2) . ? C22 C23 1.347(4) . ? C22 N4 1.378(3) . ? C22 H22 0.9500 . ? C23 N5 1.401(3) . ? C23 H23 0.9500 . ? C24 C25 1.394(4) . ? C24 C29 1.397(3) . ? C24 N5 1.452(3) . ? C25 C26 1.393(4) . ? C25 C30 1.525(3) . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? C27 C28 1.376(4) . ? C27 H27 0.9500 . ? C28 C29 1.394(4) . ? C28 H28 0.9500 . ? C29 C33 1.525(4) . ? C30 C31 1.530(4) . ? C30 C32 1.536(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.534(4) . ? C33 C34 1.535(4) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N3 Ni1 1.8667(19) . ? F1 P1 1.6047(17) . ? F2 P1 1.6065(16) . ? F3 P1 1.5883(16) . ? F4 P1 1.6003(16) . ? F5 P1 1.5973(17) . ? F6 P1 1.6112(16) . ? Ni1 Br1 2.2746(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 123.6(2) . . ? C6 C1 N1 117.5(2) . . ? C2 C1 N1 118.8(2) . . ? C3 C2 C1 116.7(2) . . ? C3 C2 C7 120.6(2) . . ? C1 C2 C7 122.7(2) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 116.9(3) . . ? C5 C6 C10 121.5(2) . . ? C1 C6 C10 121.6(2) . . ? C2 C7 C8 110.7(2) . . ? C2 C7 C9 112.6(2) . . ? C8 C7 C9 110.0(3) . . ? C2 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 113.6(2) . . ? C6 C10 C11 109.8(2) . . ? C12 C10 C11 110.0(2) . . ? C6 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 103.2(2) . . ? N1 C13 Ni1 144.78(19) . . ? N2 C13 Ni1 111.90(16) . . ? C15 C14 N1 107.9(2) . . ? C15 C14 H14 126.0 . . ? N1 C14 H14 126.0 . . ? C14 C15 N2 105.3(2) . . ? C14 C15 H15 127.3 . . ? N2 C15 H15 127.3 . . ? N3 C16 C17 122.6(2) . . ? N3 C16 N2 109.7(2) . . ? C17 C16 N2 127.7(2) . . ? C16 C17 C18 117.1(2) . . ? C16 C17 H17 121.5 . . ? C18 C17 H17 121.5 . . ? C19 C18 C17 121.2(2) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 117.1(2) . . ? C20 C19 H19 121.4 . . ? C18 C19 H19 121.4 . . ? N3 C20 C19 122.5(2) . . ? N3 C20 N4 109.4(2) . . ? C19 C20 N4 128.2(2) . . ? N5 C21 N4 103.1(2) . . ? N5 C21 Ni1 144.17(18) . . ? N4 C21 Ni1 112.66(17) . . ? C23 C22 N4 105.3(2) . . ? C23 C22 H22 127.3 . . ? N4 C22 H22 127.3 . . ? C22 C23 N5 107.5(2) . . ? C22 C23 H23 126.3 . . ? N5 C23 H23 126.3 . . ? C25 C24 C29 123.8(2) . . ? C25 C24 N5 118.2(2) . . ? C29 C24 N5 118.0(2) . . ? C26 C25 C24 117.0(2) . . ? C26 C25 C30 121.4(2) . . ? C24 C25 C30 121.6(2) . . ? C27 C26 C25 120.6(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 121.0(3) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.9(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C24 116.8(3) . . ? C28 C29 C33 121.6(2) . . ? C24 C29 C33 121.5(2) . . ? C25 C30 C31 112.8(2) . . ? C25 C30 C32 111.4(2) . . ? C31 C30 C32 109.9(2) . . ? C25 C30 H30 107.5 . . ? C31 C30 H30 107.5 . . ? C32 C30 H30 107.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 113.5(2) . . ? C29 C33 C34 109.9(2) . . ? C35 C33 C34 109.6(2) . . ? C29 C33 H33 107.9 . . ? C35 C33 H33 107.9 . . ? C34 C33 H33 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C13 N1 C14 111.0(2) . . ? C13 N1 C1 127.9(2) . . ? C14 N1 C1 121.1(2) . . ? C13 N2 C15 112.7(2) . . ? C13 N2 C16 117.0(2) . . ? C15 N2 C16 130.2(2) . . ? C16 N3 C20 119.4(2) . . ? C16 N3 Ni1 119.90(16) . . ? C20 N3 Ni1 120.51(17) . . ? C21 N4 C22 112.8(2) . . ? C21 N4 C20 116.5(2) . . ? C22 N4 C20 130.7(2) . . ? C21 N5 C23 111.3(2) . . ? C21 N5 C24 127.5(2) . . ? C23 N5 C24 121.2(2) . . ? F3 P1 F5 90.65(10) . . ? F3 P1 F4 90.70(9) . . ? F5 P1 F4 90.68(9) . . ? F3 P1 F1 90.54(9) . . ? F5 P1 F1 90.27(9) . . ? F4 P1 F1 178.44(10) . . ? F3 P1 F2 90.12(9) . . ? F5 P1 F2 179.23(10) . . ? F4 P1 F2 89.33(8) . . ? F1 P1 F2 89.71(9) . . ? F3 P1 F6 179.62(11) . . ? F5 P1 F6 89.58(9) . . ? F4 P1 F6 89.61(9) . . ? F1 P1 F6 89.16(9) . . ? F2 P1 F6 89.65(9) . . ? N3 Ni1 C13 81.46(9) . . ? N3 Ni1 C21 80.92(9) . . ? C13 Ni1 C21 162.36(10) . . ? N3 Ni1 Br1 179.64(7) . . ? C13 Ni1 Br1 98.24(7) . . ? C21 Ni1 Br1 99.38(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.3(4) . . . . ? N1 C1 C2 C3 177.0(2) . . . . ? C6 C1 C2 C7 -179.0(2) . . . . ? N1 C1 C2 C7 -2.3(4) . . . . ? C1 C2 C3 C4 -1.2(4) . . . . ? C7 C2 C3 C4 178.2(3) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C1 -1.2(4) . . . . ? C4 C5 C6 C10 176.5(3) . . . . ? C2 C1 C6 C5 0.8(4) . . . . ? N1 C1 C6 C5 -175.9(2) . . . . ? C2 C1 C6 C10 -176.8(2) . . . . ? N1 C1 C6 C10 6.4(3) . . . . ? C3 C2 C7 C8 -76.2(3) . . . . ? C1 C2 C7 C8 103.1(3) . . . . ? C3 C2 C7 C9 47.4(3) . . . . ? C1 C2 C7 C9 -133.3(3) . . . . ? C5 C6 C10 C12 37.3(4) . . . . ? C1 C6 C10 C12 -145.1(3) . . . . ? C5 C6 C10 C11 -86.3(3) . . . . ? C1 C6 C10 C11 91.2(3) . . . . ? N1 C14 C15 N2 -0.3(3) . . . . ? N3 C16 C17 C18 -0.7(4) . . . . ? N2 C16 C17 C18 179.5(2) . . . . ? C16 C17 C18 C19 -0.8(4) . . . . ? C17 C18 C19 C20 0.8(4) . . . . ? C18 C19 C20 N3 0.8(4) . . . . ? C18 C19 C20 N4 -179.2(2) . . . . ? N4 C22 C23 N5 0.3(3) . . . . ? C29 C24 C25 C26 2.0(4) . . . . ? N5 C24 C25 C26 -176.4(2) . . . . ? C29 C24 C25 C30 -177.4(2) . . . . ? N5 C24 C25 C30 4.1(4) . . . . ? C24 C25 C26 C27 -0.7(4) . . . . ? C30 C25 C26 C27 178.8(2) . . . . ? C25 C26 C27 C28 -0.8(4) . . . . ? C26 C27 C28 C29 1.1(4) . . . . ? C27 C28 C29 C24 0.2(4) . . . . ? C27 C28 C29 C33 -175.7(2) . . . . ? C25 C24 C29 C28 -1.8(4) . . . . ? N5 C24 C29 C28 176.6(2) . . . . ? C25 C24 C29 C33 174.1(2) . . . . ? N5 C24 C29 C33 -7.5(3) . . . . ? C26 C25 C30 C31 -30.6(4) . . . . ? C24 C25 C30 C31 148.9(3) . . . . ? C26 C25 C30 C32 93.6(3) . . . . ? C24 C25 C30 C32 -87.0(3) . . . . ? C28 C29 C33 C35 -27.7(4) . . . . ? C24 C29 C33 C35 156.7(2) . . . . ? C28 C29 C33 C34 95.5(3) . . . . ? C24 C29 C33 C34 -80.2(3) . . . . ? N2 C13 N1 C14 -0.3(3) . . . . ? Ni1 C13 N1 C14 174.4(3) . . . . ? N2 C13 N1 C1 178.5(2) . . . . ? Ni1 C13 N1 C1 -6.8(5) . . . . ? C15 C14 N1 C13 0.4(3) . . . . ? C15 C14 N1 C1 -178.5(2) . . . . ? C6 C1 N1 C13 -97.4(3) . . . . ? C2 C1 N1 C13 85.7(3) . . . . ? C6 C1 N1 C14 81.3(3) . . . . ? C2 C1 N1 C14 -95.6(3) . . . . ? N1 C13 N2 C15 0.1(3) . . . . ? Ni1 C13 N2 C15 -176.58(17) . . . . ? N1 C13 N2 C16 176.2(2) . . . . ? Ni1 C13 N2 C16 -0.5(3) . . . . ? C14 C15 N2 C13 0.1(3) . . . . ? C14 C15 N2 C16 -175.3(2) . . . . ? N3 C16 N2 C13 1.8(3) . . . . ? C17 C16 N2 C13 -178.4(2) . . . . ? N3 C16 N2 C15 177.0(2) . . . . ? C17 C16 N2 C15 -3.2(4) . . . . ? C17 C16 N3 C20 2.1(4) . . . . ? N2 C16 N3 C20 -178.0(2) . . . . ? C17 C16 N3 Ni1 177.83(19) . . . . ? N2 C16 N3 Ni1 -2.3(3) . . . . ? C19 C20 N3 C16 -2.2(4) . . . . ? N4 C20 N3 C16 177.7(2) . . . . ? C19 C20 N3 Ni1 -177.87(19) . . . . ? N4 C20 N3 Ni1 2.1(3) . . . . ? N5 C21 N4 C22 -0.1(3) . . . . ? Ni1 C21 N4 C22 178.39(17) . . . . ? N5 C21 N4 C20 -179.1(2) . . . . ? Ni1 C21 N4 C20 -0.6(3) . . . . ? C23 C22 N4 C21 -0.1(3) . . . . ? C23 C22 N4 C20 178.7(2) . . . . ? N3 C20 N4 C21 -0.9(3) . . . . ? C19 C20 N4 C21 179.1(2) . . . . ? N3 C20 N4 C22 -179.6(2) . . . . ? C19 C20 N4 C22 0.3(4) . . . . ? N4 C21 N5 C23 0.3(3) . . . . ? Ni1 C21 N5 C23 -177.3(3) . . . . ? N4 C21 N5 C24 178.0(2) . . . . ? Ni1 C21 N5 C24 0.4(5) . . . . ? C22 C23 N5 C21 -0.4(3) . . . . ? C22 C23 N5 C24 -178.3(2) . . . . ? C25 C24 N5 C21 -79.7(3) . . . . ? C29 C24 N5 C21 101.8(3) . . . . ? C25 C24 N5 C23 97.8(3) . . . . ? C29 C24 N5 C23 -80.7(3) . . . . ? C16 N3 Ni1 C13 1.69(19) . . . . ? C20 N3 Ni1 C13 177.3(2) . . . . ? C16 N3 Ni1 C21 -177.6(2) . . . . ? C20 N3 Ni1 C21 -1.99(19) . . . . ? N1 C13 Ni1 N3 -175.0(3) . . . . ? N2 C13 Ni1 N3 -0.55(17) . . . . ? N1 C13 Ni1 C21 -172.7(3) . . . . ? N2 C13 Ni1 C21 1.7(4) . . . . ? N1 C13 Ni1 Br1 5.2(3) . . . . ? N2 C13 Ni1 Br1 179.66(16) . . . . ? N5 C21 Ni1 N3 178.8(3) . . . . ? N4 C21 Ni1 N3 1.30(17) . . . . ? N5 C21 Ni1 C13 176.5(3) . . . . ? N4 C21 Ni1 C13 -1.0(5) . . . . ? N5 C21 Ni1 Br1 -1.4(3) . . . . ? N4 C21 Ni1 Br1 -178.91(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.383 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.082 #==END data_5 _database_code_depnum_ccdc_archive 'CCDC 663961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H49 F6 N5 Ni O7 S2, 2(C4 H8 O)' _chemical_formula_sum 'C49 H65 F6 N5 Ni O9 S2' _chemical_formula_weight 1104.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 22.7194(19) _cell_length_b 25.510(3) _cell_length_c 14.1716(13) _cell_angle_alpha 90.00 _cell_angle_beta 125.520(4) _cell_angle_gamma 90.00 _cell_volume 6685.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6193 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8856 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28442 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7590 _reflns_number_gt 4876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'enCIFer (2004)' _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^)+(0.0933P)^2^+16.9459P] 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 7590 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1390 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.2181 _refine_ls_wR_factor_gt 0.1959 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3893(2) 0.18511(16) -0.0705(3) 0.0350(9) Uani 1 1 d . . . C2 C 0.3172(2) 0.19718(18) -0.1141(4) 0.0443(11) Uani 1 1 d . . . C3 C 0.2952(3) 0.2491(2) -0.1523(4) 0.0521(12) Uani 1 1 d . . . H3 H 0.2469 0.2592 -0.1834 0.063 Uiso 1 1 calc R . . C4 C 0.3418(3) 0.2852(2) -0.1454(4) 0.0553(13) Uani 1 1 d . . . H4 H 0.3255 0.3199 -0.1724 0.066 Uiso 1 1 calc R . . C5 C 0.4127(3) 0.27178(19) -0.0995(4) 0.0484(11) Uani 1 1 d . . . H5 H 0.4446 0.2976 -0.0941 0.058 Uiso 1 1 calc R . . C6 C 0.4380(2) 0.22084(17) -0.0611(4) 0.0400(10) Uani 1 1 d . . . C7 C 0.2646(3) 0.1582(2) -0.1208(4) 0.0540(13) Uani 1 1 d . . . H7 H 0.2926 0.1257 -0.0795 0.065 Uiso 1 1 calc R . . C8 C 0.2331(3) 0.1791(2) -0.0571(5) 0.0688(16) Uani 1 1 d . . . H8A H 0.2726 0.1885 0.0226 0.103 Uiso 1 1 calc R . . H8B H 0.2030 0.1520 -0.0559 0.103 Uiso 1 1 calc R . . H8C H 0.2036 0.2102 -0.0974 0.103 Uiso 1 1 calc R . . C9 C 0.2067(3) 0.1432(3) -0.2463(5) 0.0795(18) Uani 1 1 d . . . H9A H 0.1825 0.1749 -0.2917 0.119 Uiso 1 1 calc R . . H9B H 0.1711 0.1201 -0.2494 0.119 Uiso 1 1 calc R . . H9C H 0.2291 0.1248 -0.2786 0.119 Uiso 1 1 calc R . . C10 C 0.5150(2) 0.20496(19) -0.0133(4) 0.0457(11) Uani 1 1 d . . . H10 H 0.5314 0.1803 0.0525 0.055 Uiso 1 1 calc R . . C11 C 0.5693(3) 0.2500(2) 0.0343(5) 0.0593(14) Uani 1 1 d . . . H11A H 0.6183 0.2358 0.0743 0.089 Uiso 1 1 calc R . . H11B H 0.5655 0.2705 0.0890 0.089 Uiso 1 1 calc R . . H11C H 0.5588 0.2725 -0.0297 0.089 Uiso 1 1 calc R . . C12 C 0.5174(3) 0.1752(3) -0.1028(6) 0.0782(19) Uani 1 1 d . . . H12A H 0.4850 0.1449 -0.1293 0.117 Uiso 1 1 calc R . . H12B H 0.5670 0.1631 -0.0685 0.117 Uiso 1 1 calc R . . H12C H 0.5020 0.1982 -0.1688 0.117 Uiso 1 1 calc R . . C13 C 0.4441(2) 0.11126(16) 0.0727(3) 0.0307(9) Uani 1 1 d . . . C14 C 0.3892(2) 0.09030(17) -0.1181(3) 0.0387(10) Uani 1 1 d . . . H14 H 0.3652 0.0945 -0.1992 0.046 Uiso 1 1 calc R . . C15 C 0.4091(2) 0.04486(17) -0.0597(3) 0.0365(9) Uani 1 1 d . . . H15 H 0.4022 0.0106 -0.0908 0.044 Uiso 1 1 calc R . . C16 C 0.4717(2) 0.02345(15) 0.1517(3) 0.0304(9) Uani 1 1 d . . . C17 C 0.4701(2) -0.03031(17) 0.1455(4) 0.0376(10) Uani 1 1 d . . . H17 H 0.4498 -0.0483 0.0743 0.045 Uiso 1 1 calc R . . C18 C 0.5000 -0.0568(2) 0.2500 0.0429(15) Uani 1 2 d S . . H18 H 0.5000 -0.0940 0.2500 0.051 Uiso 1 2 calc SR . . C36 C 0.3036(3) 0.0554(2) 0.1753(4) 0.0519(12) Uani 1 1 d . . . C38 C 0.4361(2) 0.24239(16) 0.1986(4) 0.0397(10) Uani 1 1 d . . . H38A H 0.4112 0.2358 0.2360 0.048 Uiso 1 1 calc R . . H38B H 0.4021 0.2351 0.1146 0.048 Uiso 1 1 calc R . . C39 C 0.4626(3) 0.2979(2) 0.2185(7) 0.087(2) Uani 1 1 d . . . H39A H 0.4414 0.3156 0.1431 0.104 Uiso 1 1 calc R . . H39B H 0.4473 0.3171 0.2616 0.104 Uiso 1 1 calc R . . C42 C 0.2931(4) 0.9021(3) 0.0186(6) 0.100(2) Uani 1 1 d . . . H42A H 0.3227 0.9059 -0.0115 0.120 Uiso 1 1 calc R . . H42B H 0.2841 0.9375 0.0363 0.120 Uiso 1 1 calc R . . C43 C 0.2251(4) 0.8773(4) -0.0677(7) 0.115(3) Uani 1 1 d . . . H43A H 0.2162 0.8785 -0.1449 0.139 Uiso 1 1 calc R . . H43B H 0.1845 0.8949 -0.0727 0.139 Uiso 1 1 calc R . . C44 C 0.2331(6) 0.8231(4) -0.0277(7) 0.155(4) Uani 1 1 d . . . H44A H 0.2332 0.7989 -0.0822 0.186 Uiso 1 1 calc R . . H44B H 0.1922 0.8135 -0.0240 0.186 Uiso 1 1 calc R . . C45 C 0.3038(4) 0.8187(3) 0.0914(6) 0.087(2) Uani 1 1 d . . . H45A H 0.2957 0.8045 0.1481 0.104 Uiso 1 1 calc R . . H45B H 0.3381 0.7956 0.0896 0.104 Uiso 1 1 calc R . . N1 N 0.41090(17) 0.13073(13) -0.0359(3) 0.0348(8) Uani 1 1 d . . . N2 N 0.44196(16) 0.05831(13) 0.0559(3) 0.0307(7) Uani 1 1 d . . . N3 N 0.5000 0.04984(17) 0.2500 0.0305(10) Uani 1 2 d S . . O1 O 0.39503(14) 0.12964(11) 0.2237(2) 0.0363(6) Uani 1 1 d . . . O2 O 0.31025(18) 0.14449(13) 0.2711(3) 0.0533(9) Uani 1 1 d . . . O3 O 0.40780(15) 0.08136(12) 0.3829(2) 0.0421(7) Uani 1 1 d . . . O7 O 0.5000 0.21004(15) 0.2500 0.0411(10) Uani 1 2 d S . . O8 O 0.3306(3) 0.87133(18) 0.1207(4) 0.0868(13) Uani 1 1 d . . . F1 F 0.26587(16) 0.03338(13) 0.2094(3) 0.0725(9) Uani 1 1 d . . . F2 F 0.34418(18) 0.01809(13) 0.1756(3) 0.0778(10) Uani 1 1 d . . . F3 F 0.25771(19) 0.07211(15) 0.0689(3) 0.0933(12) Uani 1 1 d . . . S1 S 0.36018(5) 0.10888(4) 0.27501(9) 0.0356(3) Uani 1 1 d . . . Ni1 Ni 0.5000 0.12891(3) 0.2500 0.0299(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(2) 0.033(2) 0.027(2) 0.0046(16) 0.0181(18) 0.0092(18) C2 0.042(3) 0.050(3) 0.037(2) 0.010(2) 0.021(2) 0.013(2) C3 0.050(3) 0.055(3) 0.052(3) 0.018(2) 0.030(2) 0.021(2) C4 0.074(4) 0.046(3) 0.055(3) 0.018(2) 0.043(3) 0.021(3) C5 0.061(3) 0.043(3) 0.045(3) 0.006(2) 0.033(2) 0.004(2) C6 0.048(3) 0.037(3) 0.035(2) 0.0026(18) 0.023(2) 0.006(2) C7 0.041(3) 0.053(3) 0.065(3) 0.011(2) 0.029(3) 0.009(2) C8 0.048(3) 0.077(4) 0.087(4) 0.020(3) 0.043(3) 0.015(3) C9 0.050(3) 0.085(4) 0.070(4) 0.005(3) 0.016(3) -0.002(3) C10 0.041(2) 0.046(3) 0.049(3) 0.003(2) 0.026(2) 0.000(2) C11 0.060(3) 0.063(4) 0.060(3) -0.009(3) 0.037(3) -0.015(3) C12 0.068(4) 0.084(4) 0.095(5) -0.031(4) 0.054(4) -0.005(3) C13 0.0268(19) 0.033(2) 0.032(2) 0.0007(16) 0.0172(17) -0.0021(16) C14 0.038(2) 0.044(3) 0.027(2) -0.0021(18) 0.0142(18) 0.0002(19) C15 0.039(2) 0.039(3) 0.026(2) -0.0041(17) 0.0161(18) -0.0006(19) C16 0.030(2) 0.032(2) 0.032(2) 0.0005(16) 0.0190(17) -0.0007(16) C17 0.046(2) 0.038(3) 0.035(2) -0.0020(18) 0.026(2) -0.0025(19) C18 0.065(4) 0.028(3) 0.051(4) 0.000 0.042(4) 0.000 C36 0.042(3) 0.052(3) 0.055(3) 0.006(2) 0.024(2) -0.007(2) C38 0.033(2) 0.039(3) 0.043(2) 0.0013(19) 0.020(2) 0.0059(18) C39 0.049(3) 0.037(3) 0.144(6) 0.007(3) 0.039(4) -0.002(2) C42 0.106(6) 0.092(5) 0.066(4) -0.007(4) 0.030(4) -0.011(4) C43 0.094(6) 0.116(7) 0.091(6) -0.009(5) 0.028(5) -0.018(5) C44 0.155(9) 0.125(8) 0.080(6) -0.014(5) 0.008(6) -0.056(7) C45 0.099(5) 0.097(5) 0.073(4) -0.024(4) 0.055(4) -0.026(4) N1 0.0349(18) 0.036(2) 0.0310(17) -0.0001(15) 0.0176(15) 0.0044(15) N2 0.0286(17) 0.0337(19) 0.0303(17) -0.0007(14) 0.0174(15) -0.0006(14) N3 0.031(2) 0.026(3) 0.038(3) 0.000 0.022(2) 0.000 O1 0.0301(14) 0.0423(17) 0.0385(15) 0.0034(13) 0.0210(13) 0.0021(13) O2 0.054(2) 0.049(2) 0.072(2) 0.0119(16) 0.0452(19) 0.0135(16) O3 0.0398(16) 0.0453(18) 0.0382(16) 0.0092(13) 0.0209(14) 0.0034(14) O7 0.030(2) 0.032(2) 0.050(3) 0.000 0.016(2) 0.000 O8 0.102(3) 0.090(3) 0.055(2) -0.019(2) 0.038(2) -0.021(3) F1 0.0535(18) 0.074(2) 0.088(2) 0.0011(17) 0.0401(18) -0.0213(16) F2 0.077(2) 0.064(2) 0.103(3) -0.0387(19) 0.059(2) -0.0236(18) F3 0.079(2) 0.097(3) 0.0477(18) 0.0075(17) 0.0041(17) -0.040(2) S1 0.0321(5) 0.0376(6) 0.0381(6) 0.0041(4) 0.0210(5) 0.0029(4) Ni1 0.0289(4) 0.0305(4) 0.0278(4) 0.000 0.0149(3) 0.000 _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 C1 C6 1.380(6) . ? C1 C2 1.407(6) . ? C1 N1 1.458(5) . ? C2 C3 1.409(6) . ? C2 C7 1.515(7) . ? C3 C4 1.363(7) . ? C3 H3 0.9500 . ? C4 C5 1.384(7) . ? C4 H4 0.9500 . ? C5 C6 1.397(6) . ? C5 H5 0.9500 . ? C6 C10 1.519(6) . ? C7 C9 1.525(7) . ? C7 C8 1.538(7) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.506(7) . ? C10 C11 1.525(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.355(5) . ? C13 N2 1.368(5) . ? C13 Ni1 2.103(4) . ? C14 C15 1.341(6) . ? C14 N1 1.413(5) . ? C14 H14 0.9500 . ? C15 N2 1.392(5) . ? C15 H15 0.9500 . ? C16 N3 1.329(4) . ? C16 C17 1.373(6) . ? C16 N2 1.423(5) . ? C17 C18 1.393(5) . ? C17 H17 0.9500 . ? C18 C17 1.393(5) 2_655 ? C18 H18 0.9500 . ? C36 F3 1.310(5) . ? C36 F2 1.322(6) . ? C36 F1 1.327(5) . ? C36 S1 1.844(5) . ? C38 O7 1.446(4) . ? C38 C39 1.499(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C39 1.388(10) 2_655 ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C42 O8 1.416(8) . ? C42 C43 1.444(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.467(11) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.514(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 O8 1.432(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? N3 C16 1.329(4) 2_655 ? N3 Ni1 2.017(4) . ? O1 S1 1.450(3) . ? O1 Ni1 2.190(3) . ? O2 S1 1.429(3) . ? O3 S1 1.442(3) . ? O7 C38 1.446(4) 2_655 ? O7 Ni1 2.069(4) . ? Ni1 C13 2.103(4) 2_655 ? Ni1 O1 2.190(3) 2_655 ? 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 C6 C1 C2 124.1(4) . . ? C6 C1 N1 120.1(4) . . ? C2 C1 N1 115.8(4) . . ? C1 C2 C3 116.0(4) . . ? C1 C2 C7 123.9(4) . . ? C3 C2 C7 120.2(4) . . ? C4 C3 C2 121.3(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.7(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 121.1(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 116.8(4) . . ? C1 C6 C10 121.3(4) . . ? C5 C6 C10 121.9(4) . . ? C2 C7 C9 110.6(4) . . ? C2 C7 C8 110.8(4) . . ? C9 C7 C8 113.0(4) . . ? C2 C7 H7 107.4 . . ? C9 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C6 110.8(4) . . ? C12 C10 C11 109.7(4) . . ? C6 C10 C11 114.9(4) . . ? C12 C10 H10 107.0 . . ? C6 C10 H10 107.0 . . ? C11 C10 H10 107.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 103.0(3) . . ? N1 C13 Ni1 146.1(3) . . ? N2 C13 Ni1 110.8(3) . . ? C15 C14 N1 107.0(3) . . ? C15 C14 H14 126.5 . . ? N1 C14 H14 126.5 . . ? C14 C15 N2 105.7(4) . . ? C14 C15 H15 127.1 . . ? N2 C15 H15 127.1 . . ? N3 C16 C17 123.5(4) . . ? N3 C16 N2 110.8(3) . . ? C17 C16 N2 125.7(4) . . ? C16 C17 C18 116.0(4) . . ? C16 C17 H17 122.0 . . ? C18 C17 H17 122.0 . . ? C17 C18 C17 121.9(6) 2_655 . ? C17 C18 H18 119.0 2_655 . ? C17 C18 H18 119.0 . . ? F3 C36 F2 109.0(5) . . ? F3 C36 F1 107.8(4) . . ? F2 C36 F1 106.9(4) . . ? F3 C36 S1 112.0(4) . . ? F2 C36 S1 110.8(3) . . ? F1 C36 S1 110.1(4) . . ? O7 C38 C39 105.6(4) . . ? O7 C38 H38A 110.6 . . ? C39 C38 H38A 110.6 . . ? O7 C38 H38B 110.6 . . ? C39 C38 H38B 110.6 . . ? H38A C38 H38B 108.8 . . ? C39 C39 C38 109.2(3) 2_655 . ? C39 C39 H39A 109.8 2_655 . ? C38 C39 H39A 109.8 . . ? C39 C39 H39B 109.8 2_655 . ? C38 C39 H39B 109.8 . . ? H39A C39 H39B 108.3 . . ? O8 C42 C43 109.7(7) . . ? O8 C42 H42A 109.7 . . ? C43 C42 H42A 109.7 . . ? O8 C42 H42B 109.7 . . ? C43 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C42 C43 C44 104.7(7) . . ? C42 C43 H43A 110.8 . . ? C44 C43 H43A 110.8 . . ? C42 C43 H43B 110.8 . . ? C44 C43 H43B 110.8 . . ? H43A C43 H43B 108.9 . . ? C43 C44 C45 108.3(7) . . ? C43 C44 H44A 110.0 . . ? C45 C44 H44A 110.0 . . ? C43 C44 H44B 110.0 . . ? C45 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? O8 C45 C44 104.6(6) . . ? O8 C45 H45A 110.8 . . ? C44 C45 H45A 110.8 . . ? O8 C45 H45B 110.8 . . ? C44 C45 H45B 110.8 . . ? H45A C45 H45B 108.9 . . ? C13 N1 C14 111.5(3) . . ? C13 N1 C1 126.0(3) . . ? C14 N1 C1 122.0(3) . . ? C13 N2 C15 112.9(3) . . ? C13 N2 C16 120.1(3) . . ? C15 N2 C16 127.0(3) . . ? C16 N3 C16 119.1(5) . 2_655 ? C16 N3 Ni1 120.4(2) . . ? C16 N3 Ni1 120.4(2) 2_655 . ? S1 O1 Ni1 140.30(17) . . ? C38 O7 C38 110.4(4) 2_655 . ? C38 O7 Ni1 124.8(2) 2_655 . ? C38 O7 Ni1 124.8(2) . . ? C42 O8 C45 108.7(5) . . ? O2 S1 O3 116.11(19) . . ? O2 S1 O1 113.63(18) . . ? O3 S1 O1 114.66(17) . . ? O2 S1 C36 104.9(2) . . ? O3 S1 C36 102.2(2) . . ? O1 S1 C36 103.1(2) . . ? N3 Ni1 O7 180.0 . . ? N3 Ni1 C13 77.63(11) . . ? O7 Ni1 C13 102.37(11) . . ? N3 Ni1 C13 77.63(11) . 2_655 ? O7 Ni1 C13 102.37(11) . 2_655 ? C13 Ni1 C13 155.3(2) . 2_655 ? N3 Ni1 O1 90.48(8) . . ? O7 Ni1 O1 89.52(8) . . ? C13 Ni1 O1 87.49(12) . . ? C13 Ni1 O1 92.71(12) 2_655 . ? N3 Ni1 O1 90.48(8) . 2_655 ? O7 Ni1 O1 89.52(8) . 2_655 ? C13 Ni1 O1 92.71(12) . 2_655 ? C13 Ni1 O1 87.49(12) 2_655 2_655 ? O1 Ni1 O1 179.03(15) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.6(6) . . . . ? N1 C1 C2 C3 -177.4(4) . . . . ? C6 C1 C2 C7 -178.0(4) . . . . ? N1 C1 C2 C7 3.0(6) . . . . ? C1 C2 C3 C4 -0.8(7) . . . . ? C7 C2 C3 C4 178.9(5) . . . . ? C2 C3 C4 C5 -0.6(8) . . . . ? C3 C4 C5 C6 1.2(7) . . . . ? C2 C1 C6 C5 -1.0(6) . . . . ? N1 C1 C6 C5 177.9(4) . . . . ? C2 C1 C6 C10 -179.9(4) . . . . ? N1 C1 C6 C10 -0.9(6) . . . . ? C4 C5 C6 C1 -0.4(6) . . . . ? C4 C5 C6 C10 178.4(4) . . . . ? C1 C2 C7 C9 -109.3(5) . . . . ? C3 C2 C7 C9 71.1(6) . . . . ? C1 C2 C7 C8 124.5(5) . . . . ? C3 C2 C7 C8 -55.1(6) . . . . ? C1 C6 C10 C12 77.0(5) . . . . ? C5 C6 C10 C12 -101.7(5) . . . . ? C1 C6 C10 C11 -157.9(4) . . . . ? C5 C6 C10 C11 23.4(6) . . . . ? N1 C14 C15 N2 0.2(4) . . . . ? N3 C16 C17 C18 0.3(5) . . . . ? N2 C16 C17 C18 -177.4(3) . . . . ? C16 C17 C18 C17 -0.1(2) . . . 2_655 ? O7 C38 C39 C39 -2.2(10) . . . 2_655 ? O8 C42 C43 C44 -17.2(11) . . . . ? C42 C43 C44 C45 6.9(12) . . . . ? C43 C44 C45 O8 5.4(11) . . . . ? N2 C13 N1 C14 -0.4(4) . . . . ? Ni1 C13 N1 C14 174.6(4) . . . . ? N2 C13 N1 C1 170.7(3) . . . . ? Ni1 C13 N1 C1 -14.2(7) . . . . ? C15 C14 N1 C13 0.1(5) . . . . ? C15 C14 N1 C1 -171.4(4) . . . . ? C6 C1 N1 C13 86.1(5) . . . . ? C2 C1 N1 C13 -94.8(5) . . . . ? C6 C1 N1 C14 -103.6(5) . . . . ? C2 C1 N1 C14 75.5(5) . . . . ? N1 C13 N2 C15 0.6(4) . . . . ? Ni1 C13 N2 C15 -176.5(2) . . . . ? N1 C13 N2 C16 -179.5(3) . . . . ? Ni1 C13 N2 C16 3.4(4) . . . . ? C14 C15 N2 C13 -0.5(5) . . . . ? C14 C15 N2 C16 179.6(4) . . . . ? N3 C16 N2 C13 -1.1(5) . . . . ? C17 C16 N2 C13 176.9(4) . . . . ? N3 C16 N2 C15 178.8(3) . . . . ? C17 C16 N2 C15 -3.2(6) . . . . ? C17 C16 N3 C16 -0.2(3) . . . 2_655 ? N2 C16 N3 C16 177.9(3) . . . 2_655 ? C17 C16 N3 Ni1 179.8(3) . . . . ? N2 C16 N3 Ni1 -2.1(3) . . . . ? C39 C38 O7 C38 0.8(4) . . . 2_655 ? C39 C38 O7 Ni1 -179.2(4) . . . . ? C43 C42 O8 C45 21.6(9) . . . . ? C44 C45 O8 C42 -16.1(8) . . . . ? Ni1 O1 S1 O2 142.7(3) . . . . ? Ni1 O1 S1 O3 5.8(3) . . . . ? Ni1 O1 S1 C36 -104.4(3) . . . . ? F3 C36 S1 O2 61.2(4) . . . . ? F2 C36 S1 O2 -176.8(3) . . . . ? F1 C36 S1 O2 -58.7(4) . . . . ? F3 C36 S1 O3 -177.2(4) . . . . ? F2 C36 S1 O3 -55.2(4) . . . . ? F1 C36 S1 O3 62.9(4) . . . . ? F3 C36 S1 O1 -57.9(4) . . . . ? F2 C36 S1 O1 64.0(4) . . . . ? F1 C36 S1 O1 -177.9(3) . . . . ? C16 N3 Ni1 O7 -82(21) . . . . ? C16 N3 Ni1 O7 98(27) 2_655 . . . ? C16 N3 Ni1 C13 3.1(2) . . . . ? C16 N3 Ni1 C13 -176.9(2) 2_655 . . . ? C16 N3 Ni1 C13 -176.9(2) . . . 2_655 ? C16 N3 Ni1 C13 3.1(2) 2_655 . . 2_655 ? C16 N3 Ni1 O1 90.42(19) . . . . ? C16 N3 Ni1 O1 -89.58(19) 2_655 . . . ? C16 N3 Ni1 O1 -89.58(19) . . . 2_655 ? C16 N3 Ni1 O1 90.42(19) 2_655 . . 2_655 ? C38 O7 Ni1 N3 -30(33) 2_655 . . . ? C38 O7 Ni1 N3 150(100) . . . . ? C38 O7 Ni1 C13 -114.7(2) 2_655 . . . ? C38 O7 Ni1 C13 65.3(2) . . . . ? C38 O7 Ni1 C13 65.3(2) 2_655 . . 2_655 ? C38 O7 Ni1 C13 -114.7(2) . . . 2_655 ? C38 O7 Ni1 O1 158.0(2) 2_655 . . . ? C38 O7 Ni1 O1 -22.0(2) . . . . ? C38 O7 Ni1 O1 -22.0(2) 2_655 . . 2_655 ? C38 O7 Ni1 O1 158.0(2) . . . 2_655 ? N1 C13 Ni1 N3 -178.1(5) . . . . ? N2 C13 Ni1 N3 -3.3(2) . . . . ? N1 C13 Ni1 O7 1.9(5) . . . . ? N2 C13 Ni1 O7 176.7(2) . . . . ? N1 C13 Ni1 C13 -178.1(5) . . . 2_655 ? N2 C13 Ni1 C13 -3.3(2) . . . 2_655 ? N1 C13 Ni1 O1 90.9(5) . . . . ? N2 C13 Ni1 O1 -94.3(3) . . . . ? N1 C13 Ni1 O1 -88.2(5) . . . 2_655 ? N2 C13 Ni1 O1 86.6(3) . . . 2_655 ? S1 O1 Ni1 N3 54.4(3) . . . . ? S1 O1 Ni1 O7 -125.6(3) . . . . ? S1 O1 Ni1 C13 132.0(3) . . . . ? S1 O1 Ni1 C13 -23.2(3) . . . 2_655 ? S1 O1 Ni1 O1 -125.6(3) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.280 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.082 #==END data_6MeAg6I8 _database_code_depnum_ccdc_archive 'CCDC 663962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H90 N10 Ag2, 2(C4 H10 O), Ag6 I8' _chemical_formula_sum 'C82 H110 Ag8 I8 N10 O2' _chemical_formula_weight 3145.96 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.6353(4) _cell_length_b 22.1211(6) _cell_length_c 17.0640(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.0900(10) _cell_angle_gamma 90.00 _cell_volume 5095.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11779 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 3.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7417 _exptl_absorpt_correction_T_max 0.9614 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78859 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.63 _reflns_number_total 11729 _reflns_number_gt 9506 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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^)+(0.0000P)^2^+71.9300P] 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 11729 _refine_ls_number_parameters 508 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6926(5) 0.7547(3) 0.4828(4) 0.0231(15) Uani 1 1 d . . . C2 C 0.7505(5) 0.7548(3) 0.5572(4) 0.0238(15) Uani 1 1 d . . . C3 C 0.7671(6) 0.6992(4) 0.5945(4) 0.0280(16) Uani 1 1 d . . . H3 H 0.8069 0.6974 0.6448 0.034 Uiso 1 1 calc R . . C4 C 0.7272(6) 0.6466(4) 0.5601(5) 0.0314(18) Uani 1 1 d . . . H4 H 0.7415 0.6090 0.5860 0.038 Uiso 1 1 calc R . . C5 C 0.6665(6) 0.6486(3) 0.4881(5) 0.0273(16) Uani 1 1 d . . . H5 H 0.6367 0.6124 0.4660 0.033 Uiso 1 1 calc R . . C6 C 0.6485(5) 0.7031(3) 0.4475(4) 0.0216(14) Uani 1 1 d . . . C7 C 0.7924(6) 0.8136(3) 0.5956(4) 0.0266(16) Uani 1 1 d . . . H7 H 0.7433 0.8465 0.5793 0.032 Uiso 1 1 calc R . . C8 C 0.8074(7) 0.8104(4) 0.6865(5) 0.041(2) Uani 1 1 d . . . H8A H 0.8622 0.7828 0.7046 0.062 Uiso 1 1 calc R . . H8B H 0.7467 0.7956 0.7046 0.062 Uiso 1 1 calc R . . H8C H 0.8230 0.8508 0.7084 0.062 Uiso 1 1 calc R . . C9 C 0.8899(7) 0.8316(4) 0.5684(5) 0.0360(19) Uani 1 1 d . . . H9A H 0.9394 0.8000 0.5834 0.054 Uiso 1 1 calc R . . H9B H 0.9130 0.8698 0.5935 0.054 Uiso 1 1 calc R . . H9C H 0.8800 0.8365 0.5108 0.054 Uiso 1 1 calc R . . C10 C 0.5765(6) 0.7055(3) 0.3698(4) 0.0266(16) Uani 1 1 d . . . H10 H 0.5850 0.7455 0.3442 0.032 Uiso 1 1 calc R . . C11 C 0.4701(6) 0.7018(4) 0.3882(5) 0.039(2) Uani 1 1 d . . . H11A H 0.4240 0.7043 0.3388 0.058 Uiso 1 1 calc R . . H11B H 0.4577 0.7354 0.4229 0.058 Uiso 1 1 calc R . . H11C H 0.4605 0.6634 0.4147 0.058 Uiso 1 1 calc R . . C12 C 0.5973(7) 0.6563(4) 0.3122(5) 0.037(2) Uani 1 1 d . . . H12A H 0.6667 0.6586 0.3034 0.056 Uiso 1 1 calc R . . H12B H 0.5540 0.6619 0.2618 0.056 Uiso 1 1 calc R . . H12C H 0.5845 0.6167 0.3343 0.056 Uiso 1 1 calc R . . C13 C 0.6060(5) 0.8509(3) 0.4373(4) 0.0197(13) Uani 1 1 d . . . C14 C 0.7458(5) 0.8268(3) 0.3851(4) 0.0216(14) Uani 1 1 d . . . H14 H 0.8031 0.8055 0.3748 0.026 Uiso 1 1 calc R . . C15 C 0.7102(5) 0.8790(3) 0.3515(4) 0.0221(14) Uani 1 1 d . . . H15 H 0.7384 0.9020 0.3133 0.026 Uiso 1 1 calc R . . C16 C 0.5672(5) 0.9459(3) 0.3619(4) 0.0204(14) Uani 1 1 d . . . C17 C 0.4661(5) 0.9421(3) 0.3304(4) 0.0223(14) Uani 1 1 d . . . C18 C 0.4213(6) 0.9972(3) 0.3099(4) 0.0255(15) Uani 1 1 d . . . H18 H 0.3532 0.9975 0.2881 0.031 Uiso 1 1 calc R . . C19 C 0.4708(6) 1.0516(3) 0.3198(4) 0.0243(15) Uani 1 1 d . . . C20 C 0.5698(6) 1.0480(3) 0.3526(4) 0.0224(14) Uani 1 1 d . . . C21 C 0.3843(5) 0.8549(3) 0.5816(4) 0.0193(13) Uani 1 1 d . . . C22 C 0.7139(6) 1.1116(3) 0.3305(4) 0.0256(16) Uani 1 1 d . . . H22 H 0.7396 1.0864 0.2932 0.031 Uiso 1 1 calc R . . C23 C 0.2488(6) 0.8353(3) 0.6409(4) 0.0240(15) Uani 1 1 d . . . H23 H 0.1923 0.8152 0.6551 0.029 Uiso 1 1 calc R . . C24 C 0.2955(5) 0.7572(3) 0.5471(4) 0.0225(14) Uani 1 1 d . . . C25 C 0.3434(5) 0.7077(3) 0.5854(4) 0.0215(14) Uani 1 1 d . . . C26 C 0.3232(6) 0.6513(3) 0.5503(5) 0.0273(16) Uani 1 1 d . . . H26 H 0.3544 0.6163 0.5746 0.033 Uiso 1 1 calc R . . C27 C 0.2588(6) 0.6456(3) 0.4812(5) 0.0299(17) Uani 1 1 d . . . H27 H 0.2446 0.6067 0.4589 0.036 Uiso 1 1 calc R . . C28 C 0.2146(6) 0.6961(4) 0.4437(5) 0.0299(17) Uani 1 1 d . . . H28 H 0.1705 0.6913 0.3958 0.036 Uiso 1 1 calc R . . C29 C 0.2333(5) 0.7536(3) 0.4745(4) 0.0230(15) Uani 1 1 d . . . C30 C 0.4172(6) 0.7137(4) 0.6606(4) 0.0266(16) Uani 1 1 d . . . H30 H 0.4130 0.7560 0.6805 0.032 Uiso 1 1 calc R . . C31 C 0.5218(6) 0.7038(5) 0.6419(5) 0.046(2) Uani 1 1 d . . . H31A H 0.5293 0.6617 0.6257 0.068 Uiso 1 1 calc R . . H31B H 0.5695 0.7124 0.6891 0.068 Uiso 1 1 calc R . . H31C H 0.5341 0.7308 0.5988 0.068 Uiso 1 1 calc R . . C32 C 0.3937(7) 0.6707(4) 0.7258(5) 0.040(2) Uani 1 1 d . . . H32A H 0.3257 0.6776 0.7360 0.059 Uiso 1 1 calc R . . H32B H 0.4397 0.6783 0.7743 0.059 Uiso 1 1 calc R . . H32C H 0.4008 0.6288 0.7088 0.059 Uiso 1 1 calc R . . C33 C 0.1869(6) 0.8095(4) 0.4333(4) 0.0278(16) Uani 1 1 d . . . H33 H 0.2316 0.8444 0.4497 0.033 Uiso 1 1 calc R . . C34 C 0.1777(7) 0.8040(4) 0.3439(5) 0.041(2) Uani 1 1 d . . . H34A H 0.2411 0.7909 0.3289 0.061 Uiso 1 1 calc R . . H34B H 0.1595 0.8434 0.3197 0.061 Uiso 1 1 calc R . . H34C H 0.1264 0.7743 0.3252 0.061 Uiso 1 1 calc R . . C35 C 0.0858(7) 0.8230(4) 0.4597(6) 0.039(2) Uani 1 1 d . . . H35A H 0.0427 0.7875 0.4499 0.058 Uiso 1 1 calc R . . H35B H 0.0551 0.8575 0.4297 0.058 Uiso 1 1 calc R . . H35C H 0.0951 0.8326 0.5164 0.058 Uiso 1 1 calc R . . C36 C 0.4094(6) 0.8841(3) 0.3143(4) 0.0258(15) Uani 1 1 d . . . H36A H 0.3800 0.8725 0.3613 0.039 Uiso 1 1 calc R . . H36B H 0.4544 0.8521 0.3016 0.039 Uiso 1 1 calc R . . H36C H 0.3568 0.8898 0.2695 0.039 Uiso 1 1 calc R . . C37 C 0.4207(6) 1.1096(3) 0.2917(5) 0.0287(16) Uani 1 1 d . . . H37A H 0.3622 1.1007 0.2532 0.043 Uiso 1 1 calc R . . H37B H 0.4667 1.1347 0.2667 0.043 Uiso 1 1 calc R . . H37C H 0.4005 1.1313 0.3369 0.043 Uiso 1 1 calc R . . C38 C 0.2322(12) 0.9984(6) 0.4433(7) 0.086(5) Uani 1 1 d . . . H38A H 0.2816 0.9684 0.4326 0.129 Uiso 1 1 calc R . . H38B H 0.2155 0.9921 0.4968 0.129 Uiso 1 1 calc R . . H38C H 0.2594 1.0391 0.4394 0.129 Uiso 1 1 calc R . . C39 C 0.1405(13) 0.9915(6) 0.3839(9) 0.096(5) Uani 1 1 d . . . H39A H 0.1166 0.9492 0.3828 0.115 Uiso 1 1 calc R . . H39B H 0.0873 1.0183 0.3975 0.115 Uiso 1 1 calc R . . C40 C 0.0902(13) 0.9996(8) 0.2425(10) 0.108(6) Uani 1 1 d . . . H40A H 0.0298 1.0209 0.2534 0.129 Uiso 1 1 calc R . . H40B H 0.0748 0.9560 0.2360 0.129 Uiso 1 1 calc R . . C41 C 0.1237(14) 1.0244(9) 0.1679(11) 0.117(6) Uani 1 1 d U . . H41A H 0.1402 1.0673 0.1754 0.176 Uiso 1 1 calc R . . H41B H 0.0702 1.0199 0.1235 0.176 Uiso 1 1 calc R . . H41C H 0.1822 1.0022 0.1566 0.176 Uiso 1 1 calc R . . N1 N 0.6810(4) 0.8108(3) 0.4380(3) 0.0203(12) Uani 1 1 d . . . N2 N 0.6250(4) 0.8927(2) 0.3830(3) 0.0184(11) Uani 1 1 d . . . N3 N 0.6184(5) 0.9969(3) 0.3732(3) 0.0205(12) Uani 1 1 d . . . N4 N 0.6305(5) 1.1010(3) 0.3665(3) 0.0220(12) Uani 1 1 d . . . N5 N 0.3091(5) 0.8155(3) 0.5864(3) 0.0220(12) Uani 1 1 d . . . Ag1 Ag 0.49473(4) 0.85048(2) 0.50910(3) 0.02027(11) Uani 1 1 d . . . Ag2 Ag 0.53996(9) 0.15578(4) 0.96879(5) 0.0734(3) Uani 1 1 d . . . Ag3 Ag 0.60199(6) 0.05253(3) 1.07244(4) 0.04021(17) Uani 1 1 d . . . Ag4 Ag 0.40244(6) 0.07232(3) 0.86613(4) 0.04388(18) Uani 1 1 d . . . I1 I 0.58803(4) 0.17168(2) 1.12459(3) 0.02797(11) Uani 1 1 d . . . I2 I 0.42717(4) 0.19252(2) 0.83550(3) 0.02928(12) Uani 1 1 d . . . I3 I 0.58797(4) 0.01411(2) 0.91013(3) 0.03264(12) Uani 1 1 d . . . I4 I 0.76541(4) -0.00495(2) 1.16442(3) 0.03137(12) Uani 1 1 d . . . O1 O 0.1685(7) 1.0084(4) 0.3066(5) 0.075(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(4) 0.020(3) 0.023(3) 0.006(3) 0.001(3) 0.004(3) C2 0.023(4) 0.022(4) 0.028(4) -0.001(3) 0.009(3) 0.005(3) C3 0.031(4) 0.031(4) 0.022(3) 0.009(3) 0.002(3) 0.005(3) C4 0.029(4) 0.027(4) 0.039(4) 0.015(3) 0.007(3) 0.010(3) C5 0.031(4) 0.021(4) 0.032(4) 0.004(3) 0.011(3) 0.007(3) C6 0.025(4) 0.019(3) 0.023(3) 0.002(3) 0.008(3) 0.005(3) C7 0.026(4) 0.024(4) 0.029(4) 0.002(3) -0.001(3) 0.006(3) C8 0.051(6) 0.041(5) 0.028(4) -0.002(4) -0.008(4) 0.013(4) C9 0.039(5) 0.027(4) 0.041(5) -0.005(4) 0.002(4) -0.006(4) C10 0.031(4) 0.021(4) 0.027(4) -0.002(3) 0.004(3) -0.002(3) C11 0.028(4) 0.055(6) 0.032(4) -0.007(4) 0.003(3) 0.002(4) C12 0.040(5) 0.039(5) 0.034(4) -0.008(4) 0.008(4) 0.007(4) C13 0.020(3) 0.016(3) 0.024(3) 0.002(3) 0.005(3) -0.002(3) C14 0.024(4) 0.022(3) 0.021(3) 0.002(3) 0.008(3) 0.002(3) C15 0.024(4) 0.025(4) 0.019(3) 0.002(3) 0.010(3) -0.001(3) C16 0.024(4) 0.020(3) 0.019(3) 0.002(3) 0.007(3) 0.003(3) C17 0.024(4) 0.025(4) 0.018(3) -0.003(3) 0.002(3) -0.004(3) C18 0.023(4) 0.025(4) 0.028(4) 0.003(3) 0.004(3) 0.002(3) C19 0.033(4) 0.021(3) 0.018(3) -0.001(3) 0.003(3) 0.001(3) C20 0.029(4) 0.022(3) 0.016(3) 0.000(3) 0.005(3) -0.005(3) C21 0.022(4) 0.017(3) 0.020(3) 0.003(3) 0.007(3) -0.001(3) C22 0.030(4) 0.020(3) 0.028(4) -0.007(3) 0.008(3) 0.001(3) C23 0.024(4) 0.023(4) 0.027(4) 0.001(3) 0.011(3) -0.003(3) C24 0.021(4) 0.019(3) 0.029(4) -0.004(3) 0.007(3) -0.001(3) C25 0.024(4) 0.020(3) 0.022(3) -0.001(3) 0.008(3) -0.005(3) C26 0.029(4) 0.019(3) 0.034(4) -0.001(3) 0.005(3) 0.001(3) C27 0.041(5) 0.020(4) 0.029(4) -0.008(3) 0.007(3) 0.001(3) C28 0.025(4) 0.033(4) 0.032(4) -0.004(3) 0.002(3) -0.009(3) C29 0.019(3) 0.026(4) 0.026(4) -0.004(3) 0.008(3) -0.004(3) C30 0.031(4) 0.027(4) 0.022(3) 0.000(3) 0.001(3) -0.004(3) C31 0.027(5) 0.079(7) 0.032(4) 0.008(5) 0.007(4) -0.002(5) C32 0.048(5) 0.044(5) 0.027(4) 0.008(4) 0.007(4) -0.014(4) C33 0.032(4) 0.027(4) 0.023(4) -0.002(3) -0.002(3) -0.004(3) C34 0.049(6) 0.044(5) 0.027(4) 0.005(4) -0.003(4) 0.001(4) C35 0.036(5) 0.034(5) 0.047(5) -0.002(4) 0.009(4) 0.005(4) C36 0.027(4) 0.024(4) 0.027(4) -0.001(3) 0.006(3) -0.005(3) C37 0.034(4) 0.021(4) 0.030(4) 0.001(3) 0.000(3) 0.002(3) C38 0.119(13) 0.073(9) 0.055(7) 0.008(7) -0.023(8) 0.003(9) C39 0.130(14) 0.047(7) 0.101(12) 0.019(7) -0.011(10) -0.010(8) C40 0.089(12) 0.100(12) 0.119(14) 0.016(11) -0.036(10) -0.022(10) C41 0.115(9) 0.139(10) 0.099(9) 0.008(8) 0.019(7) 0.034(8) N1 0.021(3) 0.016(3) 0.026(3) 0.005(2) 0.009(2) -0.001(2) N2 0.021(3) 0.016(3) 0.019(3) 0.003(2) 0.005(2) 0.002(2) N3 0.028(3) 0.015(3) 0.019(3) 0.002(2) 0.003(2) -0.003(2) N4 0.029(3) 0.017(3) 0.019(3) -0.001(2) 0.004(2) 0.002(2) N5 0.025(3) 0.021(3) 0.021(3) 0.000(2) 0.005(2) -0.001(2) Ag1 0.0238(3) 0.0180(2) 0.0200(2) 0.00004(19) 0.0064(2) 0.0004(2) Ag2 0.1122(8) 0.0595(5) 0.0366(4) 0.0175(4) -0.0309(5) -0.0364(5) Ag3 0.0476(4) 0.0244(3) 0.0452(4) -0.0015(3) -0.0055(3) 0.0019(3) Ag4 0.0580(5) 0.0308(3) 0.0408(4) 0.0030(3) -0.0003(3) -0.0131(3) I1 0.0321(3) 0.0240(2) 0.0273(2) -0.00232(19) 0.00238(19) 0.0003(2) I2 0.0334(3) 0.0244(2) 0.0291(2) 0.0026(2) 0.0013(2) 0.0025(2) I3 0.0356(3) 0.0337(3) 0.0285(3) -0.0015(2) 0.0042(2) -0.0062(2) I4 0.0383(3) 0.0222(2) 0.0322(3) -0.0033(2) -0.0001(2) 0.0020(2) O1 0.063(5) 0.090(7) 0.073(6) 0.006(5) 0.012(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.387(10) . ? C1 C2 1.397(10) . ? C1 N1 1.456(8) . ? C2 C3 1.388(10) . ? C2 C7 1.531(10) . ? C3 C4 1.379(12) . ? C3 H3 0.9500 . ? C4 C5 1.383(11) . ? C4 H4 0.9500 . ? C5 C6 1.395(10) . ? C5 H5 0.9500 . ? C6 C10 1.535(10) . ? C7 C9 1.522(11) . ? C7 C8 1.537(11) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.520(10) . ? C10 C11 1.529(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.352(9) . ? C13 N2 1.359(8) . ? C13 Ag1 2.079(7) . ? C14 C15 1.347(10) . ? C14 N1 1.395(8) . ? C14 H14 0.9500 . ? C15 N2 1.381(9) . ? C15 H15 0.9500 . ? C16 N3 1.326(9) . ? C16 C17 1.411(10) . ? C16 N2 1.435(9) . ? C17 C18 1.386(10) . ? C17 C36 1.503(10) . ? C18 C19 1.380(10) . ? C18 H18 0.9500 . ? C19 C20 1.390(10) . ? C19 C37 1.499(10) . ? C20 N3 1.330(9) . ? C20 N4 1.436(9) . ? C21 N4 1.351(9) 3_676 ? C21 N5 1.357(9) . ? C21 Ag1 2.082(7) . ? C22 C23 1.343(10) 3_676 ? C22 N4 1.387(9) . ? C22 H22 0.9500 . ? C23 C22 1.343(10) 3_676 ? C23 N5 1.396(9) . ? C23 H23 0.9500 . ? C24 C25 1.389(10) . ? C24 C29 1.402(10) . ? C24 N5 1.454(9) . ? C25 C26 1.395(10) . ? C25 C30 1.521(10) . ? C26 C27 1.374(11) . ? C26 H26 0.9500 . ? C27 C28 1.382(11) . ? C27 H27 0.9500 . ? C28 C29 1.387(10) . ? C28 H28 0.9500 . ? C29 C33 1.515(11) . ? C30 C31 1.521(11) . ? C30 C32 1.530(10) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.519(10) . ? C33 C35 1.540(11) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.502(19) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O1 1.473(17) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O1 1.430(16) . ? C40 C41 1.51(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N4 C21 1.351(9) 3_676 ? Ag2 I1 2.6704(9) . ? Ag2 I2 2.6861(9) . ? Ag2 Ag3 2.9392(11) . ? Ag2 Ag4 3.0114(11) . ? Ag3 I1 2.7970(8) . ? Ag3 I4 2.8392(9) . ? Ag3 I3 2.8776(9) . ? Ag3 Ag4 2.9576(9) 3_657 ? Ag3 I3 3.0311(9) 3_657 ? Ag4 I4 2.7193(9) 3_657 ? Ag4 I2 2.7399(8) . ? Ag4 I3 2.8437(10) . ? Ag4 Ag3 2.9576(9) 3_657 ? I3 Ag3 3.0311(9) 3_657 ? I4 Ag4 2.7193(9) 3_657 ? 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 C6 C1 C2 123.5(6) . . ? C6 C1 N1 117.7(6) . . ? C2 C1 N1 118.8(6) . . ? C3 C2 C1 116.7(7) . . ? C3 C2 C7 122.0(7) . . ? C1 C2 C7 121.3(6) . . ? C4 C3 C2 121.5(7) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 120.2(7) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.6(7) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 117.3(7) . . ? C1 C6 C10 122.2(6) . . ? C5 C6 C10 120.3(7) . . ? C9 C7 C2 112.4(6) . . ? C9 C7 C8 108.8(7) . . ? C2 C7 C8 112.5(7) . . ? C9 C7 H7 107.7 . . ? C2 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.3(7) . . ? C12 C10 C6 112.3(6) . . ? C11 C10 C6 109.3(6) . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C6 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 103.6(6) . . ? N1 C13 Ag1 127.3(5) . . ? N2 C13 Ag1 129.0(5) . . ? C15 C14 N1 105.6(6) . . ? C15 C14 H14 127.2 . . ? N1 C14 H14 127.2 . . ? C14 C15 N2 107.1(6) . . ? C14 C15 H15 126.4 . . ? N2 C15 H15 126.4 . . ? N3 C16 C17 125.0(6) . . ? N3 C16 N2 113.8(6) . . ? C17 C16 N2 121.2(6) . . ? C18 C17 C16 114.5(7) . . ? C18 C17 C36 120.5(7) . . ? C16 C17 C36 124.9(7) . . ? C19 C18 C17 123.1(7) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C18 C19 C20 115.5(7) . . ? C18 C19 C37 121.0(7) . . ? C20 C19 C37 123.5(7) . . ? N3 C20 C19 125.1(7) . . ? N3 C20 N4 113.4(6) . . ? C19 C20 N4 121.5(7) . . ? N4 C21 N5 103.9(6) 3_676 . ? N4 C21 Ag1 127.7(5) 3_676 . ? N5 C21 Ag1 128.4(5) . . ? C23 C22 N4 106.2(6) 3_676 . ? C23 C22 H22 126.9 3_676 . ? N4 C22 H22 126.9 . . ? C22 C23 N5 106.7(6) 3_676 . ? C22 C23 H23 126.6 3_676 . ? N5 C23 H23 126.6 . . ? C25 C24 C29 123.8(7) . . ? C25 C24 N5 117.5(6) . . ? C29 C24 N5 118.7(6) . . ? C24 C25 C26 116.9(7) . . ? C24 C25 C30 122.7(6) . . ? C26 C25 C30 120.5(7) . . ? C27 C26 C25 121.0(7) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.5(7) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 121.4(7) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C24 116.3(7) . . ? C28 C29 C33 122.0(7) . . ? C24 C29 C33 121.7(6) . . ? C25 C30 C31 109.8(6) . . ? C25 C30 C32 112.2(6) . . ? C31 C30 C32 111.2(7) . . ? C25 C30 H30 107.8 . . ? C31 C30 H30 107.8 . . ? C32 C30 H30 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C34 111.8(7) . . ? C29 C33 C35 110.8(6) . . ? C34 C33 C35 111.0(7) . . ? C29 C33 H33 107.7 . . ? C34 C33 H33 107.7 . . ? C35 C33 H33 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C19 C37 H37A 109.5 . . ? C19 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C19 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O1 C39 C38 106.4(13) . . ? O1 C39 H39A 110.4 . . ? C38 C39 H39A 110.4 . . ? O1 C39 H39B 110.4 . . ? C38 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? O1 C40 C41 108.2(14) . . ? O1 C40 H40A 110.1 . . ? C41 C40 H40A 110.1 . . ? O1 C40 H40B 110.1 . . ? C41 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C13 N1 C14 112.1(6) . . ? C13 N1 C1 126.1(6) . . ? C14 N1 C1 121.7(6) . . ? C13 N2 C15 111.6(6) . . ? C13 N2 C16 125.4(6) . . ? C15 N2 C16 123.0(6) . . ? C16 N3 C20 116.8(6) . . ? C21 N4 C22 112.0(6) 3_676 . ? C21 N4 C20 124.2(6) 3_676 . ? C22 N4 C20 123.7(6) . . ? C21 N5 C23 111.1(6) . . ? C21 N5 C24 126.2(6) . . ? C23 N5 C24 122.5(6) . . ? C13 Ag1 C21 177.0(3) . . ? I1 Ag2 I2 146.54(5) . . ? I1 Ag2 Ag3 59.59(2) . . ? I2 Ag2 Ag3 145.76(4) . . ? I1 Ag2 Ag4 134.86(4) . . ? I2 Ag2 Ag4 57.14(2) . . ? Ag3 Ag2 Ag4 88.66(3) . . ? I1 Ag3 I4 109.23(3) . . ? I1 Ag3 I3 125.89(3) . . ? I4 Ag3 I3 109.90(3) . . ? I1 Ag3 Ag2 55.42(2) . . ? I4 Ag3 Ag2 144.85(4) . . ? I3 Ag3 Ag2 71.08(3) . . ? I1 Ag3 Ag4 139.60(3) . 3_657 ? I4 Ag3 Ag4 55.91(2) . 3_657 ? I3 Ag3 Ag4 93.64(3) . 3_657 ? Ag2 Ag3 Ag4 156.98(3) . 3_657 ? I1 Ag3 I3 109.25(3) . 3_657 ? I4 Ag3 I3 110.06(3) . 3_657 ? I3 Ag3 I3 90.51(2) . 3_657 ? Ag2 Ag3 I3 105.04(3) . 3_657 ? Ag4 Ag3 I3 56.68(2) 3_657 3_657 ? I4 Ag4 I2 128.17(3) 3_657 . ? I4 Ag4 I3 119.73(3) 3_657 . ? I2 Ag4 I3 111.16(3) . . ? I4 Ag4 Ag3 59.84(2) 3_657 3_657 ? I2 Ag4 Ag3 169.43(3) . 3_657 ? I3 Ag4 Ag3 62.96(2) . 3_657 ? I4 Ag4 Ag2 152.36(4) 3_657 . ? I2 Ag4 Ag2 55.44(2) . . ? I3 Ag4 Ag2 70.49(3) . . ? Ag3 Ag4 Ag2 114.11(3) 3_657 . ? Ag2 I1 Ag3 64.99(3) . . ? Ag2 I2 Ag4 67.41(3) . . ? Ag4 I3 Ag3 93.24(3) . . ? Ag4 I3 Ag3 60.35(2) . 3_657 ? Ag3 I3 Ag3 89.49(2) . 3_657 ? Ag4 I4 Ag3 64.25(2) 3_657 . ? C40 O1 C39 113.0(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3.1(11) . . . . ? N1 C1 C2 C3 -174.1(6) . . . . ? C6 C1 C2 C7 -176.3(7) . . . . ? N1 C1 C2 C7 6.5(10) . . . . ? C1 C2 C3 C4 -0.9(11) . . . . ? C7 C2 C3 C4 178.6(7) . . . . ? C2 C3 C4 C5 -2.1(12) . . . . ? C3 C4 C5 C6 3.0(12) . . . . ? C2 C1 C6 C5 -2.2(11) . . . . ? N1 C1 C6 C5 175.0(6) . . . . ? C2 C1 C6 C10 173.4(7) . . . . ? N1 C1 C6 C10 -9.3(10) . . . . ? C4 C5 C6 C1 -0.9(11) . . . . ? C4 C5 C6 C10 -176.6(7) . . . . ? C3 C2 C7 C9 95.6(9) . . . . ? C1 C2 C7 C9 -85.0(9) . . . . ? C3 C2 C7 C8 -27.5(10) . . . . ? C1 C2 C7 C8 151.9(7) . . . . ? C1 C6 C10 C12 135.6(8) . . . . ? C5 C6 C10 C12 -48.9(10) . . . . ? C1 C6 C10 C11 -100.4(8) . . . . ? C5 C6 C10 C11 75.1(9) . . . . ? N1 C14 C15 N2 -1.1(8) . . . . ? N3 C16 C17 C18 0.9(10) . . . . ? N2 C16 C17 C18 -177.6(6) . . . . ? N3 C16 C17 C36 177.2(7) . . . . ? N2 C16 C17 C36 -1.2(11) . . . . ? C16 C17 C18 C19 -0.3(10) . . . . ? C36 C17 C18 C19 -176.9(7) . . . . ? C17 C18 C19 C20 -0.5(11) . . . . ? C17 C18 C19 C37 175.9(7) . . . . ? C18 C19 C20 N3 1.1(11) . . . . ? C37 C19 C20 N3 -175.2(7) . . . . ? C18 C19 C20 N4 -179.9(6) . . . . ? C37 C19 C20 N4 3.8(11) . . . . ? C29 C24 C25 C26 -3.4(11) . . . . ? N5 C24 C25 C26 174.8(6) . . . . ? C29 C24 C25 C30 174.7(7) . . . . ? N5 C24 C25 C30 -7.1(10) . . . . ? C24 C25 C26 C27 0.1(11) . . . . ? C30 C25 C26 C27 -178.1(7) . . . . ? C25 C26 C27 C28 1.7(12) . . . . ? C26 C27 C28 C29 -0.2(12) . . . . ? C27 C28 C29 C24 -2.8(11) . . . . ? C27 C28 C29 C33 178.8(7) . . . . ? C25 C24 C29 C28 4.7(11) . . . . ? N5 C24 C29 C28 -173.4(6) . . . . ? C25 C24 C29 C33 -176.9(7) . . . . ? N5 C24 C29 C33 4.9(10) . . . . ? C24 C25 C30 C31 -106.5(9) . . . . ? C26 C25 C30 C31 71.6(9) . . . . ? C24 C25 C30 C32 129.3(8) . . . . ? C26 C25 C30 C32 -52.6(10) . . . . ? C28 C29 C33 C34 -36.1(10) . . . . ? C24 C29 C33 C34 145.6(7) . . . . ? C28 C29 C33 C35 88.3(9) . . . . ? C24 C29 C33 C35 -90.0(8) . . . . ? N2 C13 N1 C14 -0.2(8) . . . . ? Ag1 C13 N1 C14 -176.3(5) . . . . ? N2 C13 N1 C1 -175.8(6) . . . . ? Ag1 C13 N1 C1 8.0(10) . . . . ? C15 C14 N1 C13 0.9(8) . . . . ? C15 C14 N1 C1 176.7(6) . . . . ? C6 C1 N1 C13 88.4(9) . . . . ? C2 C1 N1 C13 -94.2(9) . . . . ? C6 C1 N1 C14 -86.9(9) . . . . ? C2 C1 N1 C14 90.5(8) . . . . ? N1 C13 N2 C15 -0.6(8) . . . . ? Ag1 C13 N2 C15 175.5(5) . . . . ? N1 C13 N2 C16 -178.4(6) . . . . ? Ag1 C13 N2 C16 -2.3(10) . . . . ? C14 C15 N2 C13 1.1(8) . . . . ? C14 C15 N2 C16 179.0(6) . . . . ? N3 C16 N2 C13 121.7(7) . . . . ? C17 C16 N2 C13 -59.7(9) . . . . ? N3 C16 N2 C15 -55.9(9) . . . . ? C17 C16 N2 C15 122.7(7) . . . . ? C17 C16 N3 C20 -0.4(10) . . . . ? N2 C16 N3 C20 178.1(6) . . . . ? C19 C20 N3 C16 -0.6(10) . . . . ? N4 C20 N3 C16 -179.8(6) . . . . ? C23 C22 N4 C21 -1.6(9) 3_676 . . 3_676 ? C23 C22 N4 C20 -179.0(6) 3_676 . . . ? N3 C20 N4 C21 -115.8(7) . . . 3_676 ? C19 C20 N4 C21 65.0(9) . . . 3_676 ? N3 C20 N4 C22 61.2(9) . . . . ? C19 C20 N4 C22 -118.0(8) . . . . ? N4 C21 N5 C23 0.0(8) 3_676 . . . ? Ag1 C21 N5 C23 -178.4(5) . . . . ? N4 C21 N5 C24 -174.4(6) 3_676 . . . ? Ag1 C21 N5 C24 7.2(10) . . . . ? C22 C23 N5 C21 1.0(8) 3_676 . . . ? C22 C23 N5 C24 175.7(6) 3_676 . . . ? C25 C24 N5 C21 86.2(9) . . . . ? C29 C24 N5 C21 -95.5(9) . . . . ? C25 C24 N5 C23 -87.6(9) . . . . ? C29 C24 N5 C23 90.7(8) . . . . ? I2 Ag2 Ag3 I1 -148.96(10) . . . . ? Ag4 Ag2 Ag3 I1 -146.30(4) . . . . ? I1 Ag2 Ag3 I4 -73.50(6) . . . . ? I2 Ag2 Ag3 I4 137.54(7) . . . . ? Ag4 Ag2 Ag3 I4 140.20(5) . . . . ? I1 Ag2 Ag3 I3 -171.46(4) . . . . ? I2 Ag2 Ag3 I3 39.59(9) . . . . ? Ag4 Ag2 Ag3 I3 42.24(3) . . . . ? I1 Ag2 Ag3 Ag4 137.97(10) . . . 3_657 ? I2 Ag2 Ag3 Ag4 -10.99(18) . . . 3_657 ? Ag4 Ag2 Ag3 Ag4 -8.33(12) . . . 3_657 ? I1 Ag2 Ag3 I3 103.27(3) . . . 3_657 ? I2 Ag2 Ag3 I3 -45.69(10) . . . 3_657 ? Ag4 Ag2 Ag3 I3 -43.03(4) . . . 3_657 ? I1 Ag2 Ag4 I4 31.71(12) . . . 3_657 ? I2 Ag2 Ag4 I4 -107.60(8) . . . 3_657 ? Ag3 Ag2 Ag4 I4 74.17(9) . . . 3_657 ? I1 Ag2 Ag4 I2 139.32(8) . . . . ? Ag3 Ag2 Ag4 I2 -178.22(5) . . . . ? I1 Ag2 Ag4 I3 -85.52(6) . . . . ? I2 Ag2 Ag4 I3 135.16(3) . . . . ? Ag3 Ag2 Ag4 I3 -43.06(3) . . . . ? I1 Ag2 Ag4 Ag3 -38.90(8) . . . 3_657 ? I2 Ag2 Ag4 Ag3 -178.22(4) . . . 3_657 ? Ag3 Ag2 Ag4 Ag3 3.56(5) . . . 3_657 ? I2 Ag2 I1 Ag3 148.25(8) . . . . ? Ag4 Ag2 I1 Ag3 51.50(6) . . . . ? I4 Ag3 I1 Ag2 144.22(4) . . . . ? I3 Ag3 I1 Ag2 9.99(4) . . . . ? Ag4 Ag3 I1 Ag2 -156.17(6) 3_657 . . . ? I3 Ag3 I1 Ag2 -95.34(4) 3_657 . . . ? I1 Ag2 I2 Ag4 -123.08(8) . . . . ? Ag3 Ag2 I2 Ag4 3.16(8) . . . . ? I4 Ag4 I2 Ag2 145.77(5) 3_657 . . . ? I3 Ag4 I2 Ag2 -45.45(4) . . . . ? Ag3 Ag4 I2 Ag2 8.9(2) 3_657 . . . ? I4 Ag4 I3 Ag3 -107.35(3) 3_657 . . . ? I2 Ag4 I3 Ag3 82.80(3) . . . . ? Ag3 Ag4 I3 Ag3 -87.57(2) 3_657 . . . ? Ag2 Ag4 I3 Ag3 44.29(3) . . . . ? I4 Ag4 I3 Ag3 -19.78(3) 3_657 . . 3_657 ? I2 Ag4 I3 Ag3 170.37(4) . . . 3_657 ? Ag2 Ag4 I3 Ag3 131.86(3) . . . 3_657 ? I1 Ag3 I3 Ag4 -54.15(4) . . . . ? I4 Ag3 I3 Ag4 171.86(3) . . . . ? Ag2 Ag3 I3 Ag4 -45.47(3) . . . . ? Ag4 Ag3 I3 Ag4 116.91(2) 3_657 . . . ? I3 Ag3 I3 Ag4 60.27(2) 3_657 . . . ? I1 Ag3 I3 Ag3 -114.42(4) . . . 3_657 ? I4 Ag3 I3 Ag3 111.59(3) . . . 3_657 ? Ag2 Ag3 I3 Ag3 -105.74(3) . . . 3_657 ? Ag4 Ag3 I3 Ag3 56.64(2) 3_657 . . 3_657 ? I3 Ag3 I3 Ag3 0.0 3_657 . . 3_657 ? I1 Ag3 I4 Ag4 137.54(4) . . . 3_657 ? I3 Ag3 I4 Ag4 -80.58(3) . . . 3_657 ? Ag2 Ag3 I4 Ag4 -165.73(7) . . . 3_657 ? I3 Ag3 I4 Ag4 17.60(3) 3_657 . . 3_657 ? C41 C40 O1 C39 174.2(13) . . . . ? C38 C39 O1 C40 175.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.834 _refine_diff_density_min -3.554 _refine_diff_density_rms 0.199 #==END data_6MeOTf2 _database_code_depnum_ccdc_archive 'CCDC 663963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H90 Ag2 N10, 2(C4 H8 O), 2(C F3 O3 S)' _chemical_formula_sum 'C84 H106 Ag2 F6 N10 O8 S2' _chemical_formula_weight 1777.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7012(3) _cell_length_b 13.0999(3) _cell_length_c 13.2765(3) _cell_angle_alpha 89.4130(10) _cell_angle_beta 74.8100(10) _cell_angle_gamma 80.2370(10) _cell_volume 2099.59(8) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 46902 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8714 _exptl_absorpt_correction_T_max 0.8912 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42521 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9617 _reflns_number_gt 8412 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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^)+(0.0391P)^2^+2.4814P] 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 9617 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7082(2) 0.28917(19) 0.27535(18) 0.0180(5) Uani 1 1 d . . . C2 C 0.7129(2) 0.39508(19) 0.26693(19) 0.0218(5) Uani 1 1 d . . . C3 C 0.6978(2) 0.4414(2) 0.1755(2) 0.0273(6) Uani 1 1 d . . . H3 H 0.7012 0.5129 0.1668 0.033 Uiso 1 1 calc R . . C4 C 0.6781(2) 0.3847(2) 0.0974(2) 0.0267(6) Uani 1 1 d . . . H4 H 0.6667 0.4178 0.0362 0.032 Uiso 1 1 calc R . . C5 C 0.6747(2) 0.2796(2) 0.1073(2) 0.0250(6) Uani 1 1 d . . . H5 H 0.6615 0.2416 0.0527 0.030 Uiso 1 1 calc R . . C6 C 0.6906(2) 0.2289(2) 0.19681(19) 0.0204(5) Uani 1 1 d . . . C7 C 0.7316(2) 0.4603(2) 0.3529(2) 0.0271(6) Uani 1 1 d . . . H7 H 0.7270 0.4173 0.4161 0.033 Uiso 1 1 calc R . . C8 C 0.6423(4) 0.5561(3) 0.3823(3) 0.0536(10) Uani 1 1 d . . . H8A H 0.6481 0.6019 0.3230 0.080 Uiso 1 1 calc R . . H8B H 0.6520 0.5928 0.4424 0.080 Uiso 1 1 calc R . . H8C H 0.5692 0.5354 0.4005 0.080 Uiso 1 1 calc R . . C9 C 0.8481(3) 0.4884(3) 0.3196(3) 0.0431(8) Uani 1 1 d . . . H9A H 0.9035 0.4248 0.3051 0.065 Uiso 1 1 calc R . . H9B H 0.8597 0.5292 0.3760 0.065 Uiso 1 1 calc R . . H9C H 0.8554 0.5291 0.2566 0.065 Uiso 1 1 calc R . . C10 C 0.6833(2) 0.1142(2) 0.2064(2) 0.0243(5) Uani 1 1 d . . . H10 H 0.7108 0.0881 0.2676 0.029 Uiso 1 1 calc R . . C11 C 0.5625(3) 0.0988(2) 0.2260(3) 0.0365(7) Uani 1 1 d . . . H11A H 0.5179 0.1361 0.2908 0.055 Uiso 1 1 calc R . . H11B H 0.5589 0.0248 0.2320 0.055 Uiso 1 1 calc R . . H11C H 0.5336 0.1258 0.1675 0.055 Uiso 1 1 calc R . . C12 C 0.7546(3) 0.0504(2) 0.1083(2) 0.0341(7) Uani 1 1 d . . . H12A H 0.7241 0.0702 0.0490 0.051 Uiso 1 1 calc R . . H12B H 0.7546 -0.0235 0.1203 0.051 Uiso 1 1 calc R . . H12C H 0.8307 0.0639 0.0932 0.051 Uiso 1 1 calc R . . C13 C 0.80240(19) 0.21599(17) 0.41115(18) 0.0153(5) Uani 1 1 d . . . C14 C 0.6147(2) 0.2376(2) 0.45199(19) 0.0211(5) Uani 1 1 d . . . H14 H 0.5413 0.2531 0.4446 0.025 Uiso 1 1 calc R . . C15 C 0.6444(2) 0.20600(19) 0.53909(19) 0.0201(5) Uani 1 1 d . . . H15 H 0.5967 0.1943 0.6047 0.024 Uiso 1 1 calc R . . C16 C 0.82125(19) 0.16111(17) 0.58768(17) 0.0143(4) Uani 1 1 d . . . C17 C 0.8918(2) 0.22120(18) 0.61349(18) 0.0177(5) Uani 1 1 d . . . C18 C 0.9438(2) 0.18129(19) 0.68908(19) 0.0196(5) Uani 1 1 d . . . H18 H 0.9956 0.2174 0.7071 0.023 Uiso 1 1 calc R . . C19 C 0.9225(2) 0.09013(19) 0.73914(18) 0.0184(5) Uani 1 1 d . . . C20 C 0.84535(19) 0.04176(17) 0.70880(17) 0.0149(4) Uani 1 1 d . . . C21 C 0.86562(19) -0.14294(18) 0.75753(17) 0.0152(4) Uani 1 1 d . . . C22 C 0.7010(2) -0.03843(19) 0.83074(18) 0.0187(5) Uani 1 1 d . . . H22 H 0.6449 0.0215 0.8467 0.022 Uiso 1 1 calc R . . C23 C 0.6944(2) -0.13358(19) 0.86867(18) 0.0183(5) Uani 1 1 d . . . H23 H 0.6328 -0.1539 0.9174 0.022 Uiso 1 1 calc R . . C24 C 0.81645(19) -0.30638(17) 0.84027(18) 0.0162(5) Uani 1 1 d . . . C25 C 0.7803(2) -0.37316(19) 0.78017(19) 0.0202(5) Uani 1 1 d . . . C26 C 0.7981(2) -0.4783(2) 0.8000(2) 0.0250(6) Uani 1 1 d . . . H26 H 0.7754 -0.5259 0.7599 0.030 Uiso 1 1 calc R . . C27 C 0.8483(2) -0.5146(2) 0.8771(2) 0.0262(6) Uani 1 1 d . . . H27 H 0.8606 -0.5867 0.8892 0.031 Uiso 1 1 calc R . . C28 C 0.8807(2) -0.4462(2) 0.9368(2) 0.0247(6) Uani 1 1 d . . . H28 H 0.9140 -0.4722 0.9903 0.030 Uiso 1 1 calc R . . C29 C 0.8657(2) -0.34021(19) 0.92040(19) 0.0183(5) Uani 1 1 d . . . C30 C 0.7239(2) -0.3335(2) 0.6959(2) 0.0235(5) Uani 1 1 d . . . H30 H 0.6971 -0.2574 0.7096 0.028 Uiso 1 1 calc R . . C31 C 0.8075(3) -0.3485(3) 0.5895(2) 0.0462(8) Uani 1 1 d . . . H31A H 0.8694 -0.3131 0.5899 0.069 Uiso 1 1 calc R . . H31B H 0.7718 -0.3195 0.5360 0.069 Uiso 1 1 calc R . . H31C H 0.8353 -0.4227 0.5739 0.069 Uiso 1 1 calc R . . C32 C 0.6237(3) -0.3838(3) 0.6963(3) 0.0500(9) Uani 1 1 d . . . H32A H 0.6483 -0.4578 0.6776 0.075 Uiso 1 1 calc R . . H32B H 0.5864 -0.3505 0.6455 0.075 Uiso 1 1 calc R . . H32C H 0.5721 -0.3754 0.7662 0.075 Uiso 1 1 calc R . . C33 C 0.9023(2) -0.2656(2) 0.98614(19) 0.0218(5) Uani 1 1 d . . . H33 H 0.8600 -0.1947 0.9817 0.026 Uiso 1 1 calc R . . C34 C 1.0254(2) -0.2621(2) 0.9425(2) 0.0318(6) Uani 1 1 d . . . H34A H 1.0686 -0.3312 0.9445 0.048 Uiso 1 1 calc R . . H34B H 1.0475 -0.2129 0.9848 0.048 Uiso 1 1 calc R . . H34C H 1.0391 -0.2400 0.8702 0.048 Uiso 1 1 calc R . . C35 C 0.8789(2) -0.2927(2) 1.1012(2) 0.0299(6) Uani 1 1 d . . . H35A H 0.8010 -0.2999 1.1274 0.045 Uiso 1 1 calc R . . H35B H 0.8944 -0.2374 1.1414 0.045 Uiso 1 1 calc R . . H35C H 0.9263 -0.3581 1.1084 0.045 Uiso 1 1 calc R . . C36 C 0.9054(2) 0.32608(19) 0.5694(2) 0.0265(6) Uani 1 1 d . . . H36A H 0.9405 0.3630 0.6117 0.040 Uiso 1 1 calc R . . H36B H 0.8325 0.3661 0.5704 0.040 Uiso 1 1 calc R . . H36C H 0.9518 0.3173 0.4973 0.040 Uiso 1 1 calc R . . C37 C 0.9764(3) 0.0494(2) 0.8235(2) 0.0285(6) Uani 1 1 d . . . H37A H 0.9221 0.0225 0.8795 0.043 Uiso 1 1 calc R . . H37B H 1.0035 0.1056 0.8518 0.043 Uiso 1 1 calc R . . H37C H 1.0387 -0.0064 0.7940 0.043 Uiso 1 1 calc R . . C75 C 0.4217(3) 0.6702(2) 0.1670(2) 0.0367(7) Uani 1 1 d . . . C77 C 0.3256(3) 0.0868(2) 0.4638(3) 0.0373(7) Uani 1 1 d . . . H77A H 0.3728 0.0174 0.4508 0.045 Uiso 1 1 calc R . . H77B H 0.3037 0.1073 0.3992 0.045 Uiso 1 1 calc R . . C78 C 0.2237(3) 0.0831(3) 0.5523(3) 0.0523(10) Uani 1 1 d . . . H78A H 0.2171 0.0108 0.5713 0.063 Uiso 1 1 calc R . . H78B H 0.1558 0.1164 0.5334 0.063 Uiso 1 1 calc R . . C79 C 0.2431(4) 0.1434(3) 0.6414(3) 0.0560(11) Uani 1 1 d . . . H79A H 0.2266 0.1064 0.7076 0.067 Uiso 1 1 calc R . . H79B H 0.1976 0.2137 0.6517 0.067 Uiso 1 1 calc R . . C80 C 0.3670(4) 0.1480(3) 0.6021(3) 0.0597(11) Uani 1 1 d . . . H80A H 0.3853 0.2080 0.6347 0.072 Uiso 1 1 calc R . . H80B H 0.4125 0.0837 0.6176 0.072 Uiso 1 1 calc R . . N1 N 0.71168(16) 0.24313(15) 0.37488(15) 0.0164(4) Uani 1 1 d . . . N2 N 0.75940(16) 0.19414(15) 0.51301(15) 0.0150(4) Uani 1 1 d . . . N3 N 0.79642(16) 0.07433(15) 0.63440(15) 0.0147(4) Uani 1 1 d . . . N4 N 0.80660(16) -0.04576(15) 0.76346(15) 0.0147(4) Uani 1 1 d . . . N5 N 0.79536(16) -0.19632(14) 0.82264(15) 0.0149(4) Uani 1 1 d . . . O1 O 0.46793(19) 0.83853(15) 0.22582(15) 0.0354(5) Uani 1 1 d . . . O2 O 0.4802(2) 0.81405(19) 0.04374(16) 0.0432(6) Uani 1 1 d . . . O3 O 0.6177(2) 0.7141(2) 0.1190(3) 0.0720(9) Uani 1 1 d . . . O7 O 0.3848(2) 0.1592(2) 0.4907(2) 0.0549(7) Uani 1 1 d . . . F1 F 0.45207(19) 0.59235(15) 0.09603(17) 0.0536(5) Uani 1 1 d . . . F2 F 0.4256(3) 0.62948(17) 0.25791(17) 0.0793(9) Uani 1 1 d . . . F3 F 0.31622(17) 0.70858(17) 0.17288(19) 0.0583(6) Uani 1 1 d . . . S1 S 0.50788(6) 0.77013(5) 0.13490(5) 0.02555(14) Uani 1 1 d . . . Ag1 Ag 0.968966(14) 0.188501(13) 0.327207(13) 0.01605(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0157(12) 0.0247(12) 0.0131(11) 0.0065(9) -0.0041(9) -0.0017(9) C2 0.0247(13) 0.0228(12) 0.0177(12) 0.0054(10) -0.0059(10) -0.0034(10) C3 0.0352(16) 0.0246(13) 0.0233(13) 0.0099(10) -0.0099(12) -0.0059(11) C4 0.0306(15) 0.0340(14) 0.0182(12) 0.0125(11) -0.0109(11) -0.0071(12) C5 0.0275(14) 0.0337(14) 0.0158(12) 0.0045(10) -0.0086(11) -0.0062(11) C6 0.0166(12) 0.0270(13) 0.0186(12) 0.0061(10) -0.0062(10) -0.0041(10) C7 0.0417(17) 0.0218(13) 0.0198(13) 0.0038(10) -0.0117(12) -0.0053(12) C8 0.074(3) 0.0412(19) 0.045(2) -0.0121(16) -0.0286(19) 0.0151(18) C9 0.057(2) 0.0493(19) 0.0312(16) 0.0044(14) -0.0136(16) -0.0287(17) C10 0.0294(14) 0.0250(13) 0.0215(13) 0.0034(10) -0.0105(11) -0.0072(11) C11 0.0347(17) 0.0375(16) 0.0401(17) 0.0060(13) -0.0087(14) -0.0163(13) C12 0.0420(18) 0.0301(15) 0.0306(15) -0.0020(12) -0.0135(14) -0.0009(13) C13 0.0165(12) 0.0136(10) 0.0142(11) 0.0030(8) -0.0023(9) -0.0016(9) C14 0.0132(12) 0.0309(13) 0.0184(12) 0.0066(10) -0.0035(10) -0.0032(10) C15 0.0130(11) 0.0270(13) 0.0185(12) 0.0052(10) -0.0006(9) -0.0043(10) C16 0.0130(11) 0.0170(11) 0.0111(10) 0.0015(8) -0.0012(9) -0.0003(9) C17 0.0177(12) 0.0170(11) 0.0172(11) 0.0027(9) -0.0019(10) -0.0043(9) C18 0.0205(12) 0.0199(12) 0.0205(12) 0.0018(9) -0.0073(10) -0.0066(10) C19 0.0198(12) 0.0211(12) 0.0152(11) 0.0027(9) -0.0064(10) -0.0033(10) C20 0.0159(11) 0.0145(11) 0.0130(10) 0.0039(8) -0.0021(9) -0.0021(9) C21 0.0136(11) 0.0190(11) 0.0119(10) 0.0027(9) -0.0024(9) -0.0018(9) C22 0.0149(12) 0.0219(12) 0.0175(11) 0.0027(9) -0.0018(9) -0.0017(9) C23 0.0130(11) 0.0232(12) 0.0164(11) 0.0023(9) -0.0007(9) -0.0020(9) C24 0.0144(11) 0.0142(11) 0.0183(11) 0.0059(9) -0.0020(9) -0.0021(9) C25 0.0198(12) 0.0212(12) 0.0194(12) 0.0048(9) -0.0055(10) -0.0023(10) C26 0.0291(14) 0.0207(12) 0.0266(13) 0.0005(10) -0.0094(11) -0.0052(11) C27 0.0306(15) 0.0157(12) 0.0327(14) 0.0071(10) -0.0101(12) -0.0030(10) C28 0.0262(14) 0.0221(12) 0.0282(14) 0.0092(10) -0.0139(12) -0.0011(10) C29 0.0157(12) 0.0211(12) 0.0173(11) 0.0029(9) -0.0028(9) -0.0032(9) C30 0.0294(14) 0.0197(12) 0.0254(13) 0.0038(10) -0.0141(11) -0.0047(10) C31 0.050(2) 0.061(2) 0.0257(16) 0.0064(15) -0.0125(15) -0.0005(17) C32 0.0388(19) 0.062(2) 0.063(2) 0.0273(19) -0.0323(18) -0.0181(17) C33 0.0249(13) 0.0219(12) 0.0216(12) 0.0046(10) -0.0106(11) -0.0056(10) C34 0.0330(16) 0.0443(17) 0.0243(14) 0.0057(12) -0.0111(12) -0.0180(13) C35 0.0321(16) 0.0393(16) 0.0204(13) 0.0019(11) -0.0074(12) -0.0114(13) C36 0.0387(16) 0.0190(12) 0.0265(14) 0.0059(10) -0.0126(12) -0.0120(11) C37 0.0391(16) 0.0293(14) 0.0264(14) 0.0077(11) -0.0210(13) -0.0124(12) C75 0.053(2) 0.0321(15) 0.0286(15) 0.0067(12) -0.0155(15) -0.0100(14) C77 0.0345(17) 0.0349(16) 0.0407(17) -0.0014(13) -0.0020(14) -0.0133(13) C78 0.052(2) 0.062(2) 0.0392(19) -0.0171(17) 0.0047(16) -0.0269(19) C79 0.095(3) 0.0366(18) 0.0249(16) -0.0077(13) 0.0074(18) -0.0154(19) C80 0.070(3) 0.058(2) 0.070(3) 0.014(2) -0.048(2) -0.017(2) N1 0.0154(10) 0.0206(10) 0.0131(9) 0.0048(8) -0.0038(8) -0.0028(8) N2 0.0138(10) 0.0172(9) 0.0134(9) 0.0032(7) -0.0028(8) -0.0020(8) N3 0.0145(10) 0.0159(9) 0.0129(9) 0.0019(7) -0.0025(8) -0.0017(8) N4 0.0146(10) 0.0153(9) 0.0139(9) 0.0040(7) -0.0036(8) -0.0026(7) N5 0.0142(10) 0.0149(9) 0.0140(9) 0.0042(7) -0.0014(8) -0.0018(7) O1 0.0526(14) 0.0297(10) 0.0212(10) 0.0021(8) -0.0021(9) -0.0119(10) O2 0.0541(15) 0.0585(14) 0.0232(10) 0.0152(10) -0.0109(10) -0.0268(12) O3 0.0272(13) 0.0687(19) 0.117(3) -0.0223(18) -0.0247(15) 0.0095(13) O7 0.0530(16) 0.0642(17) 0.0505(15) 0.0044(13) -0.0094(13) -0.0252(13) F1 0.0718(15) 0.0365(10) 0.0583(13) -0.0134(9) -0.0285(11) -0.0063(10) F2 0.167(3) 0.0513(13) 0.0495(13) 0.0309(11) -0.0570(16) -0.0573(16) F3 0.0342(11) 0.0575(13) 0.0780(16) 0.0031(11) 0.0010(11) -0.0186(10) S1 0.0212(3) 0.0299(3) 0.0233(3) -0.0004(3) -0.0043(3) -0.0006(3) Ag1 0.01448(10) 0.01789(9) 0.01423(9) 0.00339(6) -0.00184(7) -0.00176(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 C1 C6 1.399(3) . ? C1 C2 1.401(3) . ? C1 N1 1.455(3) . ? C2 C3 1.395(3) . ? C2 C7 1.523(4) . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.399(3) . ? C5 H5 0.9500 . ? C6 C10 1.524(4) . ? C7 C8 1.519(4) . ? C7 C9 1.536(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.535(4) . ? C10 C12 1.537(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.354(3) . ? C13 N2 1.366(3) . ? C13 Ag1 2.089(2) . ? C14 C15 1.348(3) . ? C14 N1 1.393(3) . ? C14 H14 0.9500 . ? C15 N2 1.392(3) . ? C15 H15 0.9500 . ? C16 N3 1.335(3) . ? C16 C17 1.395(3) . ? C16 N2 1.439(3) . ? C17 C18 1.391(3) . ? C17 C36 1.507(3) . ? C18 C19 1.393(3) . ? C18 H18 0.9500 . ? C19 C20 1.395(3) . ? C19 C37 1.508(3) . ? C20 N3 1.329(3) . ? C20 N4 1.439(3) . ? C21 N5 1.352(3) . ? C21 N4 1.355(3) . ? C21 Ag1 2.094(2) 2_756 ? C22 C23 1.347(3) . ? C22 N4 1.392(3) . ? C22 H22 0.9500 . ? C23 N5 1.391(3) . ? C23 H23 0.9500 . ? C24 C25 1.398(3) . ? C24 C29 1.402(3) . ? C24 N5 1.449(3) . ? C25 C26 1.392(3) . ? C25 C30 1.522(3) . ? C26 C27 1.383(4) . ? C26 H26 0.9500 . ? C27 C28 1.382(4) . ? C27 H27 0.9500 . ? C28 C29 1.392(3) . ? C28 H28 0.9500 . ? C29 C33 1.523(3) . ? C30 C31 1.521(4) . ? C30 C32 1.527(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.526(4) . ? C33 C35 1.528(4) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C75 F2 1.324(3) . ? C75 F3 1.331(4) . ? C75 F1 1.331(4) . ? C75 S1 1.823(3) . ? C77 O7 1.409(4) . ? C77 C78 1.509(5) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.524(5) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.534(6) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 O7 1.446(5) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? O1 S1 1.437(2) . ? O2 S1 1.435(2) . ? O3 S1 1.425(2) . ? Ag1 C21 2.094(2) 2_756 ? 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 C6 C1 C2 123.3(2) . . ? C6 C1 N1 119.1(2) . . ? C2 C1 N1 117.4(2) . . ? C3 C2 C1 117.3(2) . . ? C3 C2 C7 119.7(2) . . ? C1 C2 C7 123.0(2) . . ? C4 C3 C2 120.9(2) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 117.0(2) . . ? C5 C6 C10 119.5(2) . . ? C1 C6 C10 123.5(2) . . ? C8 C7 C2 111.2(2) . . ? C8 C7 C9 111.8(3) . . ? C2 C7 C9 110.1(2) . . ? C8 C7 H7 107.8 . . ? C2 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C11 110.3(2) . . ? C6 C10 C12 111.8(2) . . ? C11 C10 C12 109.5(2) . . ? C6 C10 H10 108.4 . . ? C11 C10 H10 108.4 . . ? C12 C10 H10 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 103.55(19) . . ? N1 C13 Ag1 128.58(17) . . ? N2 C13 Ag1 127.11(16) . . ? C15 C14 N1 107.1(2) . . ? C15 C14 H14 126.4 . . ? N1 C14 H14 126.4 . . ? C14 C15 N2 105.8(2) . . ? C14 C15 H15 127.1 . . ? N2 C15 H15 127.1 . . ? N3 C16 C17 124.8(2) . . ? N3 C16 N2 113.38(19) . . ? C17 C16 N2 121.6(2) . . ? C18 C17 C16 115.5(2) . . ? C18 C17 C36 121.4(2) . . ? C16 C17 C36 123.0(2) . . ? C17 C18 C19 122.1(2) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C18 C19 C20 115.6(2) . . ? C18 C19 C37 121.7(2) . . ? C20 C19 C37 122.6(2) . . ? N3 C20 C19 124.7(2) . . ? N3 C20 N4 114.4(2) . . ? C19 C20 N4 120.7(2) . . ? N5 C21 N4 103.72(19) . . ? N5 C21 Ag1 130.72(16) . 2_756 ? N4 C21 Ag1 125.42(17) . 2_756 ? C23 C22 N4 106.0(2) . . ? C23 C22 H22 127.0 . . ? N4 C22 H22 127.0 . . ? C22 C23 N5 106.6(2) . . ? C22 C23 H23 126.7 . . ? N5 C23 H23 126.7 . . ? C25 C24 C29 123.1(2) . . ? C25 C24 N5 117.9(2) . . ? C29 C24 N5 118.8(2) . . ? C26 C25 C24 117.4(2) . . ? C26 C25 C30 120.7(2) . . ? C24 C25 C30 121.9(2) . . ? C27 C26 C25 120.9(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 120.2(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 121.6(2) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C28 C29 C24 116.7(2) . . ? C28 C29 C33 121.2(2) . . ? C24 C29 C33 122.1(2) . . ? C31 C30 C25 109.8(2) . . ? C31 C30 C32 110.8(3) . . ? C25 C30 C32 113.1(2) . . ? C31 C30 H30 107.7 . . ? C25 C30 H30 107.7 . . ? C32 C30 H30 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C34 110.4(2) . . ? C29 C33 C35 112.8(2) . . ? C34 C33 C35 109.8(2) . . ? C29 C33 H33 107.9 . . ? C34 C33 H33 107.9 . . ? C35 C33 H33 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C19 C37 H37A 109.5 . . ? C19 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C19 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? F2 C75 F3 107.6(3) . . ? F2 C75 F1 107.0(3) . . ? F3 C75 F1 106.6(3) . . ? F2 C75 S1 111.5(2) . . ? F3 C75 S1 111.1(2) . . ? F1 C75 S1 112.7(2) . . ? O7 C77 C78 109.0(3) . . ? O7 C77 H77A 109.9 . . ? C78 C77 H77A 109.9 . . ? O7 C77 H77B 109.9 . . ? C78 C77 H77B 109.9 . . ? H77A C77 H77B 108.3 . . ? C77 C78 C79 103.6(3) . . ? C77 C78 H78A 111.0 . . ? C79 C78 H78A 111.0 . . ? C77 C78 H78B 111.0 . . ? C79 C78 H78B 111.0 . . ? H78A C78 H78B 109.0 . . ? C78 C79 C80 101.9(3) . . ? C78 C79 H79A 111.4 . . ? C80 C79 H79A 111.4 . . ? C78 C79 H79B 111.4 . . ? C80 C79 H79B 111.4 . . ? H79A C79 H79B 109.3 . . ? O7 C80 C79 104.0(3) . . ? O7 C80 H80A 111.0 . . ? C79 C80 H80A 111.0 . . ? O7 C80 H80B 111.0 . . ? C79 C80 H80B 111.0 . . ? H80A C80 H80B 109.0 . . ? C13 N1 C14 111.50(19) . . ? C13 N1 C1 126.7(2) . . ? C14 N1 C1 121.05(19) . . ? C13 N2 C15 112.00(19) . . ? C13 N2 C16 126.33(19) . . ? C15 N2 C16 121.67(19) . . ? C20 N3 C16 117.2(2) . . ? C21 N4 C22 111.95(19) . . ? C21 N4 C20 125.71(19) . . ? C22 N4 C20 122.33(19) . . ? C21 N5 C23 111.69(19) . . ? C21 N5 C24 125.92(19) . . ? C23 N5 C24 122.31(19) . . ? C77 O7 C80 102.7(3) . . ? O3 S1 O2 115.89(18) . . ? O3 S1 O1 115.67(16) . . ? O2 S1 O1 113.56(14) . . ? O3 S1 C75 103.65(17) . . ? O2 S1 C75 102.93(13) . . ? O1 S1 C75 102.62(13) . . ? C13 Ag1 C21 173.42(9) . 2_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.7(4) . . . . ? N1 C1 C2 C3 -173.4(2) . . . . ? C6 C1 C2 C7 179.7(2) . . . . ? N1 C1 C2 C7 5.5(4) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C7 C2 C3 C4 -178.4(3) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? C4 C5 C6 C10 178.4(2) . . . . ? C2 C1 C6 C5 -1.5(4) . . . . ? N1 C1 C6 C5 172.6(2) . . . . ? C2 C1 C6 C10 -178.9(2) . . . . ? N1 C1 C6 C10 -4.8(4) . . . . ? C3 C2 C7 C8 52.1(4) . . . . ? C1 C2 C7 C8 -126.9(3) . . . . ? C3 C2 C7 C9 -72.5(3) . . . . ? C1 C2 C7 C9 108.6(3) . . . . ? C5 C6 C10 C11 -72.2(3) . . . . ? C1 C6 C10 C11 105.1(3) . . . . ? C5 C6 C10 C12 49.8(3) . . . . ? C1 C6 C10 C12 -132.9(3) . . . . ? N1 C14 C15 N2 0.6(3) . . . . ? N3 C16 C17 C18 4.3(3) . . . . ? N2 C16 C17 C18 178.2(2) . . . . ? N3 C16 C17 C36 -171.2(2) . . . . ? N2 C16 C17 C36 2.6(4) . . . . ? C16 C17 C18 C19 -3.0(4) . . . . ? C36 C17 C18 C19 172.6(2) . . . . ? C17 C18 C19 C20 -0.2(4) . . . . ? C17 C18 C19 C37 -177.9(2) . . . . ? C18 C19 C20 N3 2.9(4) . . . . ? C37 C19 C20 N3 -179.4(2) . . . . ? C18 C19 C20 N4 -172.5(2) . . . . ? C37 C19 C20 N4 5.1(4) . . . . ? N4 C22 C23 N5 -0.7(3) . . . . ? C29 C24 C25 C26 -2.1(4) . . . . ? N5 C24 C25 C26 -178.1(2) . . . . ? C29 C24 C25 C30 178.1(2) . . . . ? N5 C24 C25 C30 2.0(3) . . . . ? C24 C25 C26 C27 0.8(4) . . . . ? C30 C25 C26 C27 -179.3(3) . . . . ? C25 C26 C27 C28 0.7(4) . . . . ? C26 C27 C28 C29 -1.0(4) . . . . ? C27 C28 C29 C24 -0.2(4) . . . . ? C27 C28 C29 C33 -179.6(2) . . . . ? C25 C24 C29 C28 1.8(4) . . . . ? N5 C24 C29 C28 177.8(2) . . . . ? C25 C24 C29 C33 -178.8(2) . . . . ? N5 C24 C29 C33 -2.8(3) . . . . ? C26 C25 C30 C31 -81.3(3) . . . . ? C24 C25 C30 C31 98.5(3) . . . . ? C26 C25 C30 C32 42.9(4) . . . . ? C24 C25 C30 C32 -137.2(3) . . . . ? C28 C29 C33 C34 83.5(3) . . . . ? C24 C29 C33 C34 -96.0(3) . . . . ? C28 C29 C33 C35 -39.7(3) . . . . ? C24 C29 C33 C35 140.8(2) . . . . ? O7 C77 C78 C79 -11.5(4) . . . . ? C77 C78 C79 C80 -15.0(4) . . . . ? C78 C79 C80 O7 36.3(4) . . . . ? N2 C13 N1 C14 -0.4(3) . . . . ? Ag1 C13 N1 C14 169.97(17) . . . . ? N2 C13 N1 C1 169.8(2) . . . . ? Ag1 C13 N1 C1 -19.8(3) . . . . ? C15 C14 N1 C13 -0.1(3) . . . . ? C15 C14 N1 C1 -171.0(2) . . . . ? C6 C1 N1 C13 108.1(3) . . . . ? C2 C1 N1 C13 -77.5(3) . . . . ? C6 C1 N1 C14 -82.5(3) . . . . ? C2 C1 N1 C14 91.9(3) . . . . ? N1 C13 N2 C15 0.9(3) . . . . ? Ag1 C13 N2 C15 -169.75(17) . . . . ? N1 C13 N2 C16 -180.0(2) . . . . ? Ag1 C13 N2 C16 9.4(3) . . . . ? C14 C15 N2 C13 -1.0(3) . . . . ? C14 C15 N2 C16 179.8(2) . . . . ? N3 C16 N2 C13 -126.9(2) . . . . ? C17 C16 N2 C13 58.6(3) . . . . ? N3 C16 N2 C15 52.2(3) . . . . ? C17 C16 N2 C15 -122.3(3) . . . . ? C19 C20 N3 C16 -1.8(3) . . . . ? N4 C20 N3 C16 173.84(19) . . . . ? C17 C16 N3 C20 -2.0(3) . . . . ? N2 C16 N3 C20 -176.29(19) . . . . ? N5 C21 N4 C22 -0.3(2) . . . . ? Ag1 C21 N4 C22 -176.43(16) 2_756 . . . ? N5 C21 N4 C20 179.3(2) . . . . ? Ag1 C21 N4 C20 3.2(3) 2_756 . . . ? C23 C22 N4 C21 0.6(3) . . . . ? C23 C22 N4 C20 -179.0(2) . . . . ? N3 C20 N4 C21 111.0(2) . . . . ? C19 C20 N4 C21 -73.2(3) . . . . ? N3 C20 N4 C22 -69.5(3) . . . . ? C19 C20 N4 C22 106.4(3) . . . . ? N4 C21 N5 C23 -0.2(3) . . . . ? Ag1 C21 N5 C23 175.67(17) 2_756 . . . ? N4 C21 N5 C24 176.5(2) . . . . ? Ag1 C21 N5 C24 -7.7(3) 2_756 . . . ? C22 C23 N5 C21 0.6(3) . . . . ? C22 C23 N5 C24 -176.2(2) . . . . ? C25 C24 N5 C21 -93.4(3) . . . . ? C29 C24 N5 C21 90.4(3) . . . . ? C25 C24 N5 C23 83.0(3) . . . . ? C29 C24 N5 C23 -93.2(3) . . . . ? C78 C77 O7 C80 34.7(4) . . . . ? C79 C80 O7 C77 -44.0(4) . . . . ? F2 C75 S1 O3 66.9(3) . . . . ? F3 C75 S1 O3 -173.0(2) . . . . ? F1 C75 S1 O3 -53.4(3) . . . . ? F2 C75 S1 O2 -171.9(3) . . . . ? F3 C75 S1 O2 -51.9(2) . . . . ? F1 C75 S1 O2 67.7(2) . . . . ? F2 C75 S1 O1 -53.8(3) . . . . ? F3 C75 S1 O1 66.2(2) . . . . ? F1 C75 S1 O1 -174.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.357 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.085 #==END data_7 _database_code_depnum_ccdc_archive 'CCDC 663964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H47 N5 Ni (C4 H10 O)' _chemical_formula_sum 'C41 H57 N5 Ni O' _chemical_formula_weight 694.63 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.907(2) _cell_length_b 13.813(3) _cell_length_c 15.330(3) _cell_angle_alpha 111.24(3) _cell_angle_beta 93.82(3) _cell_angle_gamma 99.87(3) _cell_volume 1907.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3772 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.47 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9892 _exptl_absorpt_correction_T_max 0.9946 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6709 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 18662 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 28.33 _reflns_number_total 9332 _reflns_number_gt 6700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'enCIFer (2004)' _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^)+(0.0651P)^2^+0.1496P] 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 9332 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1906(2) 0.18311(18) 0.40855(15) 0.0244(5) Uani 1 1 d . . . C2 C -0.2594(2) 0.24963(18) 0.38038(15) 0.0263(5) Uani 1 1 d . . . C3 C -0.4019(2) 0.2166(2) 0.35499(17) 0.0322(5) Uani 1 1 d . . . H3 H -0.4524 0.2601 0.3363 0.039 Uiso 1 1 calc R . . C4 C -0.4714(2) 0.1220(2) 0.35646(18) 0.0357(6) Uani 1 1 d . . . H4 H -0.5688 0.1007 0.3384 0.043 Uiso 1 1 calc R . . C5 C -0.4002(3) 0.0577(2) 0.38396(18) 0.0363(6) Uani 1 1 d . . . H5 H -0.4494 -0.0072 0.3849 0.044 Uiso 1 1 calc R . . C6 C -0.2578(2) 0.08670(19) 0.41025(17) 0.0303(5) Uani 1 1 d . . . C7 C -0.1830(3) 0.35423(19) 0.37951(18) 0.0330(5) Uani 1 1 d . . . H7 H -0.0828 0.3514 0.3794 0.040 Uiso 1 1 calc R . . C8 C -0.1953(4) 0.4454(2) 0.4693(2) 0.0529(8) Uani 1 1 d . . . H8A H -0.1410 0.5121 0.4699 0.079 Uiso 1 1 calc R . . H8B H -0.1602 0.4325 0.5245 0.079 Uiso 1 1 calc R . . H8C H -0.2926 0.4504 0.4714 0.079 Uiso 1 1 calc R . . C9 C -0.2307(3) 0.3739(2) 0.2921(2) 0.0465(7) Uani 1 1 d . . . H9A H -0.2309 0.3111 0.2354 0.070 Uiso 1 1 calc R . . H9B H -0.1675 0.4355 0.2897 0.070 Uiso 1 1 calc R . . H9C H -0.3244 0.3878 0.2950 0.070 Uiso 1 1 calc R . . C10 C -0.1804(3) 0.0141(2) 0.4384(2) 0.0395(6) Uani 1 1 d . . . H10 H -0.0843 0.0550 0.4673 0.047 Uiso 1 1 calc R . . C11 C -0.2465(4) -0.0218(3) 0.5111(2) 0.0617(10) Uani 1 1 d . . . H11A H -0.3352 -0.0712 0.4815 0.092 Uiso 1 1 calc R . . H11B H -0.2620 0.0401 0.5633 0.092 Uiso 1 1 calc R . . H11C H -0.1850 -0.0575 0.5355 0.092 Uiso 1 1 calc R . . C12 C -0.1701(3) -0.0813(3) 0.3520(2) 0.0516(8) Uani 1 1 d . . . H12A H -0.2628 -0.1251 0.3245 0.077 Uiso 1 1 calc R . . H12B H -0.1120 -0.1233 0.3703 0.077 Uiso 1 1 calc R . . H12C H -0.1290 -0.0569 0.3052 0.077 Uiso 1 1 calc R . . C13 C 0.0275(2) 0.26549(17) 0.52238(16) 0.0239(4) Uani 1 1 d . . . C14 C 0.0484(2) 0.19089(19) 0.36563(16) 0.0278(5) Uani 1 1 d . . . H14 H 0.0227 0.1546 0.2993 0.033 Uiso 1 1 calc R . . C15 C 0.1770(2) 0.22975(18) 0.41173(16) 0.0283(5) Uani 1 1 d . . . H15 H 0.2606 0.2271 0.3848 0.034 Uiso 1 1 calc R . . C16 C 0.2665(2) 0.32176(18) 0.58638(16) 0.0260(5) Uani 1 1 d . . . C17 C 0.4068(2) 0.3356(2) 0.58840(19) 0.0350(6) Uani 1 1 d . . . H17 H 0.4487 0.3149 0.5324 0.042 Uiso 1 1 calc R . . C18 C 0.4847(3) 0.3824(2) 0.67846(19) 0.0393(6) Uani 1 1 d . . . H18 H 0.5828 0.3941 0.6836 0.047 Uiso 1 1 calc R . . C19 C 0.4244(3) 0.4119(2) 0.75945(18) 0.0352(6) Uani 1 1 d . . . H19 H 0.4791 0.4434 0.8200 0.042 Uiso 1 1 calc R . . C20 C 0.2793(2) 0.39393(18) 0.75015(16) 0.0279(5) Uani 1 1 d . . . C21 C 0.0500(2) 0.37984(19) 0.79034(17) 0.0290(5) Uani 1 1 d . . . C22 C 0.2611(3) 0.4618(2) 0.91864(16) 0.0335(5) Uani 1 1 d . . . H22A H 0.2024 0.5072 0.9570 0.040 Uiso 1 1 calc R . . H22B H 0.3527 0.5074 0.9245 0.040 Uiso 1 1 calc R . . C23 C 0.2785(2) 0.3778(2) 0.95637(16) 0.0309(5) Uani 1 1 d . . . H23 H 0.2229 0.3083 0.9256 0.037 Uiso 1 1 calc R . . C24 C 0.3713(2) 0.31272(19) 1.06009(16) 0.0289(5) Uani 1 1 d . . . C25 C 0.4636(2) 0.2460(2) 1.02549(17) 0.0320(5) Uani 1 1 d . . . C26 C 0.4680(3) 0.1650(2) 1.05883(19) 0.0387(6) Uani 1 1 d . . . H26 H 0.5287 0.1180 1.0360 0.046 Uiso 1 1 calc R . . C27 C 0.3851(3) 0.1519(2) 1.12484(19) 0.0427(7) Uani 1 1 d . . . H27 H 0.3881 0.0956 1.1460 0.051 Uiso 1 1 calc R . . C28 C 0.2983(3) 0.2209(2) 1.15972(18) 0.0398(6) Uani 1 1 d . . . H28 H 0.2430 0.2119 1.2056 0.048 Uiso 1 1 calc R . . C29 C 0.2898(3) 0.3029(2) 1.12940(17) 0.0323(5) Uani 1 1 d . . . C30 C 0.5553(2) 0.2595(2) 0.95358(17) 0.0334(5) Uani 1 1 d . . . H30 H 0.5576 0.3322 0.9536 0.040 Uiso 1 1 calc R . . C31 C 0.4967(3) 0.1797(3) 0.85377(19) 0.0478(7) Uani 1 1 d . . . H31A H 0.4949 0.1075 0.8510 0.072 Uiso 1 1 calc R . . H31B H 0.5551 0.1937 0.8088 0.072 Uiso 1 1 calc R . . H31C H 0.4024 0.1867 0.8375 0.072 Uiso 1 1 calc R . . C32 C 0.7034(3) 0.2532(2) 0.9803(2) 0.0446(7) Uani 1 1 d . . . H32A H 0.7367 0.3020 1.0458 0.067 Uiso 1 1 calc R . . H32B H 0.7626 0.2731 0.9382 0.067 Uiso 1 1 calc R . . H32C H 0.7062 0.1805 0.9741 0.067 Uiso 1 1 calc R . . C33 C 0.1933(3) 0.3778(2) 1.16622(17) 0.0350(6) Uani 1 1 d . . . H33 H 0.2308 0.4451 1.1574 0.042 Uiso 1 1 calc R . . C34 C 0.0488(3) 0.3326(2) 1.1098(2) 0.0474(7) Uani 1 1 d . . . H34A H 0.0547 0.3175 1.0428 0.071 Uiso 1 1 calc R . . H34B H -0.0098 0.3844 1.1328 0.071 Uiso 1 1 calc R . . H34C H 0.0087 0.2668 1.1177 0.071 Uiso 1 1 calc R . . C35 C 0.1827(3) 0.4064(2) 1.27091(19) 0.0485(7) Uani 1 1 d . . . H35A H 0.1318 0.3444 1.2804 0.073 Uiso 1 1 calc R . . H35B H 0.1337 0.4649 1.2930 0.073 Uiso 1 1 calc R . . H35C H 0.2759 0.4284 1.3067 0.073 Uiso 1 1 calc R . . C36 C -0.1866(2) 0.2917(2) 0.64912(17) 0.0347(6) Uani 1 1 d . . . H36A H -0.2171 0.2242 0.6567 0.052 Uiso 1 1 calc R . . H36B H -0.2301 0.2870 0.5880 0.052 Uiso 1 1 calc R . . H36C H -0.2135 0.3490 0.7001 0.052 Uiso 1 1 calc R . . C37 C -0.0319(3) 0.3884(2) 0.85746(17) 0.0379(6) Uani 1 1 d . . . H37A H 0.0074 0.4173 0.9221 0.045 Uiso 1 1 calc R . . H37B H -0.1294 0.3655 0.8405 0.045 Uiso 1 1 calc R . . C38 C 0.7810(4) 1.0568(3) 0.1255(2) 0.0592(9) Uani 1 1 d . . . H38A H 0.7467 1.0597 0.1847 0.089 Uiso 1 1 calc R . . H38B H 0.7026 1.0419 0.0768 0.089 Uiso 1 1 calc R . . H38C H 0.8412 1.1251 0.1355 0.089 Uiso 1 1 calc R . . C39 C 0.8604(3) 0.9716(3) 0.0945(2) 0.0545(8) Uani 1 1 d . . . H39A H 0.8005 0.9025 0.0855 0.065 Uiso 1 1 calc R . . H39B H 0.8921 0.9665 0.0334 0.065 Uiso 1 1 calc R . . C40 C 1.0497(3) 0.9129(3) 0.1444(2) 0.0569(9) Uani 1 1 d . . . H40A H 1.0877 0.9018 0.0842 0.068 Uiso 1 1 calc R . . H40B H 0.9872 0.8458 0.1377 0.068 Uiso 1 1 calc R . . C41 C 1.1642(3) 0.9410(3) 0.2221(2) 0.0551(8) Uani 1 1 d . . . H41A H 1.2258 1.0076 0.2287 0.083 Uiso 1 1 calc R . . H41B H 1.2165 0.8843 0.2078 0.083 Uiso 1 1 calc R . . H41C H 1.1263 0.9498 0.2813 0.083 Uiso 1 1 calc R . . N1 N -0.04166(19) 0.21367(14) 0.43353(13) 0.0235(4) Uani 1 1 d . . . N2 N 0.16429(19) 0.27467(15) 0.50652(13) 0.0247(4) Uani 1 1 d . . . N3 N 0.20470(18) 0.34933(14) 0.66385(13) 0.0241(4) Uani 1 1 d . . . N4 N 0.1980(2) 0.41576(15) 0.81984(13) 0.0284(4) Uani 1 1 d . . . N5 N 0.36487(19) 0.39699(16) 1.02766(13) 0.0286(4) Uani 1 1 d . . . Ni1 Ni 0.01137(3) 0.32075(2) 0.65412(2) 0.02417(9) Uani 1 1 d . . . O1 O 0.97519(18) 0.99400(14) 0.16297(12) 0.0396(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0258(11) 0.0248(12) 0.0193(10) 0.0058(9) -0.0020(8) 0.0043(9) C2 0.0305(12) 0.0268(12) 0.0199(10) 0.0068(9) 0.0006(9) 0.0071(10) C3 0.0325(13) 0.0341(14) 0.0296(12) 0.0106(11) -0.0014(10) 0.0116(11) C4 0.0243(12) 0.0409(15) 0.0352(13) 0.0100(12) -0.0035(10) 0.0025(11) C5 0.0341(13) 0.0342(14) 0.0376(14) 0.0154(12) -0.0018(11) -0.0015(11) C6 0.0309(12) 0.0278(12) 0.0305(12) 0.0125(10) -0.0052(10) 0.0020(10) C7 0.0372(13) 0.0279(13) 0.0362(13) 0.0139(11) 0.0022(11) 0.0104(11) C8 0.079(2) 0.0289(15) 0.0415(16) 0.0067(13) 0.0025(15) 0.0045(15) C9 0.066(2) 0.0395(16) 0.0408(16) 0.0222(13) 0.0065(14) 0.0127(14) C10 0.0354(13) 0.0308(14) 0.0525(17) 0.0236(13) -0.0105(12) -0.0035(11) C11 0.110(3) 0.0481(19) 0.0395(17) 0.0241(15) 0.0083(18) 0.0331(19) C12 0.0625(19) 0.0547(19) 0.061(2) 0.0374(17) 0.0219(16) 0.0329(16) C13 0.0248(11) 0.0209(11) 0.0262(11) 0.0090(9) 0.0022(9) 0.0053(9) C14 0.0343(12) 0.0287(12) 0.0215(11) 0.0091(9) 0.0057(9) 0.0099(10) C15 0.0332(12) 0.0299(13) 0.0239(11) 0.0104(10) 0.0087(9) 0.0101(10) C16 0.0274(11) 0.0211(11) 0.0281(11) 0.0089(9) -0.0006(9) 0.0045(9) C17 0.0274(12) 0.0375(14) 0.0365(14) 0.0099(11) 0.0049(10) 0.0070(11) C18 0.0236(12) 0.0422(15) 0.0452(15) 0.0111(13) -0.0025(11) 0.0047(11) C19 0.0313(13) 0.0346(14) 0.0332(13) 0.0092(11) -0.0087(10) 0.0031(11) C20 0.0304(12) 0.0237(12) 0.0290(12) 0.0097(10) -0.0028(9) 0.0074(10) C21 0.0327(12) 0.0251(12) 0.0279(12) 0.0090(10) -0.0006(10) 0.0068(10) C22 0.0416(14) 0.0312(13) 0.0231(11) 0.0071(10) -0.0036(10) 0.0060(11) C23 0.0347(13) 0.0300(13) 0.0235(11) 0.0076(10) -0.0014(10) 0.0027(10) C24 0.0304(12) 0.0306(13) 0.0227(11) 0.0094(10) -0.0017(9) 0.0025(10) C25 0.0301(12) 0.0346(14) 0.0277(12) 0.0097(10) -0.0032(10) 0.0051(10) C26 0.0394(14) 0.0406(15) 0.0375(14) 0.0156(12) 0.0000(11) 0.0125(12) C27 0.0529(17) 0.0440(16) 0.0377(15) 0.0242(13) 0.0012(13) 0.0098(13) C28 0.0480(16) 0.0463(16) 0.0296(13) 0.0199(12) 0.0070(12) 0.0087(13) C29 0.0335(13) 0.0366(14) 0.0247(12) 0.0112(10) 0.0008(10) 0.0039(11) C30 0.0314(12) 0.0357(14) 0.0309(13) 0.0097(11) 0.0037(10) 0.0085(11) C31 0.0456(16) 0.0574(19) 0.0308(14) 0.0074(13) 0.0080(12) 0.0061(14) C32 0.0363(14) 0.0496(17) 0.0516(17) 0.0209(14) 0.0097(13) 0.0138(13) C33 0.0423(14) 0.0349(14) 0.0277(12) 0.0114(11) 0.0115(11) 0.0070(11) C34 0.0422(15) 0.0493(18) 0.0485(17) 0.0143(14) 0.0101(13) 0.0123(13) C35 0.065(2) 0.0482(18) 0.0335(15) 0.0151(13) 0.0174(14) 0.0120(15) C36 0.0266(12) 0.0451(15) 0.0295(12) 0.0099(11) 0.0053(10) 0.0096(11) C37 0.0407(14) 0.0456(16) 0.0240(12) 0.0095(11) 0.0035(11) 0.0096(12) C38 0.061(2) 0.0446(18) 0.068(2) 0.0191(17) -0.0136(17) 0.0137(16) C39 0.0475(17) 0.057(2) 0.0478(18) 0.0076(15) -0.0065(14) 0.0152(15) C40 0.0493(18) 0.055(2) 0.0471(17) -0.0065(15) -0.0040(14) 0.0225(15) C41 0.0492(17) 0.064(2) 0.0423(17) 0.0049(15) -0.0026(14) 0.0227(16) N1 0.0262(9) 0.0225(10) 0.0219(9) 0.0090(8) 0.0003(7) 0.0055(8) N2 0.0247(9) 0.0239(10) 0.0241(9) 0.0082(8) 0.0013(7) 0.0042(8) N3 0.0240(9) 0.0211(9) 0.0249(9) 0.0074(8) -0.0012(7) 0.0039(8) N4 0.0314(10) 0.0290(11) 0.0220(9) 0.0081(8) -0.0040(8) 0.0056(8) N5 0.0280(10) 0.0351(11) 0.0219(9) 0.0101(8) 0.0031(8) 0.0064(9) Ni1 0.02306(15) 0.02673(17) 0.02183(15) 0.00810(12) 0.00131(11) 0.00613(11) O1 0.0387(10) 0.0369(10) 0.0344(10) 0.0045(8) -0.0021(8) 0.0081(8) _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 C1 C6 1.393(3) . ? C1 C2 1.399(3) . ? C1 N1 1.448(3) . ? C2 C3 1.390(3) . ? C2 C7 1.517(3) . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 C10 1.521(3) . ? C7 C9 1.521(3) . ? C7 C8 1.522(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.517(4) . ? C10 C11 1.517(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.356(3) . ? C13 N2 1.386(3) . ? C13 Ni1 1.912(2) . ? C14 C15 1.335(3) . ? C14 N1 1.400(3) . ? C14 H14 0.9500 . ? C15 N2 1.382(3) . ? C15 H15 0.9500 . ? C16 N3 1.334(3) . ? C16 C17 1.367(3) . ? C16 N2 1.407(3) . ? C17 C18 1.400(4) . ? C17 H17 0.9500 . ? C18 C19 1.371(4) . ? C18 H18 0.9500 . ? C19 C20 1.405(3) . ? C19 H19 0.9500 . ? C20 N3 1.342(3) . ? C20 N4 1.359(3) . ? C21 C37 1.337(3) . ? C21 N4 1.449(3) . ? C21 Ni1 1.930(2) . ? C22 N4 1.459(3) . ? C22 C23 1.502(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N5 1.259(3) . ? C23 H23 0.9500 . ? C24 C25 1.402(3) . ? C24 C29 1.408(3) . ? C24 N5 1.431(3) . ? C25 C26 1.394(4) . ? C25 C30 1.516(3) . ? C26 C27 1.387(4) . ? C26 H26 0.9500 . ? C27 C28 1.381(4) . ? C27 H27 0.9500 . ? C28 C29 1.383(4) . ? C28 H28 0.9500 . ? C29 C33 1.514(4) . ? C30 C32 1.523(3) . ? C30 C31 1.528(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.523(3) . ? C33 C34 1.524(4) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 Ni1 1.924(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9500 . ? C37 H37B 0.9500 . ? C38 C39 1.481(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O1 1.405(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O1 1.401(3) . ? C40 C41 1.480(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N3 Ni1 1.8725(19) . ? 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 C6 C1 C2 123.2(2) . . ? C6 C1 N1 118.24(19) . . ? C2 C1 N1 118.5(2) . . ? C3 C2 C1 116.9(2) . . ? C3 C2 C7 121.2(2) . . ? C1 C2 C7 121.8(2) . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.4(2) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 117.4(2) . . ? C5 C6 C10 120.3(2) . . ? C1 C6 C10 122.3(2) . . ? C2 C7 C9 113.1(2) . . ? C2 C7 C8 110.1(2) . . ? C9 C7 C8 111.0(2) . . ? C2 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 110.4(2) . . ? C12 C10 C6 110.5(2) . . ? C11 C10 C6 112.2(2) . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C6 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 102.15(18) . . ? N1 C13 Ni1 145.66(17) . . ? N2 C13 Ni1 112.06(15) . . ? C15 C14 N1 107.1(2) . . ? C15 C14 H14 126.5 . . ? N1 C14 H14 126.5 . . ? C14 C15 N2 106.3(2) . . ? C14 C15 H15 126.9 . . ? N2 C15 H15 126.9 . . ? N3 C16 C17 123.5(2) . . ? N3 C16 N2 108.82(19) . . ? C17 C16 N2 127.6(2) . . ? C16 C17 C18 115.6(2) . . ? C16 C17 H17 122.2 . . ? C18 C17 H17 122.2 . . ? C19 C18 C17 122.3(2) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 117.9(2) . . ? C18 C19 H19 121.0 . . ? C20 C19 H19 121.0 . . ? N3 C20 N4 112.1(2) . . ? N3 C20 C19 119.8(2) . . ? N4 C20 C19 128.1(2) . . ? C37 C21 N4 117.9(2) . . ? C37 C21 Ni1 132.2(2) . . ? N4 C21 Ni1 109.84(16) . . ? N4 C22 C23 111.8(2) . . ? N4 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? N4 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? N5 C23 C22 121.7(2) . . ? N5 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C25 C24 C29 122.1(2) . . ? C25 C24 N5 119.1(2) . . ? C29 C24 N5 118.8(2) . . ? C26 C25 C24 117.7(2) . . ? C26 C25 C30 120.4(2) . . ? C24 C25 C30 121.9(2) . . ? C27 C26 C25 121.0(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 119.9(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 121.6(2) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C28 C29 C24 117.6(2) . . ? C28 C29 C33 121.9(2) . . ? C24 C29 C33 120.4(2) . . ? C25 C30 C32 111.6(2) . . ? C25 C30 C31 111.7(2) . . ? C32 C30 C31 111.0(2) . . ? C25 C30 H30 107.4 . . ? C32 C30 H30 107.4 . . ? C31 C30 H30 107.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 113.6(2) . . ? C29 C33 C34 111.3(2) . . ? C35 C33 C34 109.2(2) . . ? C29 C33 H33 107.5 . . ? C35 C33 H33 107.5 . . ? C34 C33 H33 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Ni1 C36 H36A 109.5 . . ? Ni1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Ni1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C21 C37 H37A 120.0 . . ? C21 C37 H37B 120.0 . . ? H37A C37 H37B 120.0 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O1 C39 C38 109.7(2) . . ? O1 C39 H39A 109.7 . . ? C38 C39 H39A 109.7 . . ? O1 C39 H39B 109.7 . . ? C38 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? O1 C40 C41 110.3(2) . . ? O1 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? O1 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C13 N1 C14 112.06(19) . . ? C13 N1 C1 125.67(18) . . ? C14 N1 C1 122.26(18) . . ? C15 N2 C13 112.47(19) . . ? C15 N2 C16 130.25(19) . . ? C13 N2 C16 117.19(19) . . ? C16 N3 C20 120.9(2) . . ? C16 N3 Ni1 120.41(15) . . ? C20 N3 Ni1 118.68(16) . . ? C20 N4 C21 116.45(19) . . ? C20 N4 C22 119.84(19) . . ? C21 N4 C22 123.3(2) . . ? C23 N5 C24 117.7(2) . . ? N3 Ni1 C13 81.50(9) . . ? N3 Ni1 C36 177.77(10) . . ? C13 Ni1 C36 100.58(11) . . ? N3 Ni1 C21 82.68(10) . . ? C13 Ni1 C21 164.05(10) . . ? C36 Ni1 C21 95.21(11) . . ? C40 O1 C39 114.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.2(3) . . . . ? N1 C1 C2 C3 178.65(19) . . . . ? C6 C1 C2 C7 179.9(2) . . . . ? N1 C1 C2 C7 -2.7(3) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C7 C2 C3 C4 -179.5(2) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C4 C5 C6 C1 0.6(4) . . . . ? C4 C5 C6 C10 -178.7(2) . . . . ? C2 C1 C6 C5 -1.1(4) . . . . ? N1 C1 C6 C5 -178.5(2) . . . . ? C2 C1 C6 C10 178.2(2) . . . . ? N1 C1 C6 C10 0.8(3) . . . . ? C3 C2 C7 C9 -43.7(3) . . . . ? C1 C2 C7 C9 137.6(2) . . . . ? C3 C2 C7 C8 81.0(3) . . . . ? C1 C2 C7 C8 -97.6(3) . . . . ? C5 C6 C10 C12 73.9(3) . . . . ? C1 C6 C10 C12 -105.4(3) . . . . ? C5 C6 C10 C11 -49.8(3) . . . . ? C1 C6 C10 C11 131.0(3) . . . . ? N1 C14 C15 N2 0.5(3) . . . . ? N3 C16 C17 C18 -0.5(4) . . . . ? N2 C16 C17 C18 -178.2(2) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C20 -0.1(4) . . . . ? C18 C19 C20 N3 0.0(4) . . . . ? C18 C19 C20 N4 179.5(2) . . . . ? N4 C22 C23 N5 158.5(2) . . . . ? C29 C24 C25 C26 3.0(4) . . . . ? N5 C24 C25 C26 179.7(2) . . . . ? C29 C24 C25 C30 -177.6(2) . . . . ? N5 C24 C25 C30 -0.9(3) . . . . ? C24 C25 C26 C27 -0.8(4) . . . . ? C30 C25 C26 C27 179.8(2) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C26 C27 C28 C29 1.0(4) . . . . ? C27 C28 C29 C24 1.1(4) . . . . ? C27 C28 C29 C33 179.1(2) . . . . ? C25 C24 C29 C28 -3.1(4) . . . . ? N5 C24 C29 C28 -179.8(2) . . . . ? C25 C24 C29 C33 178.9(2) . . . . ? N5 C24 C29 C33 2.2(3) . . . . ? C26 C25 C30 C32 -46.1(3) . . . . ? C24 C25 C30 C32 134.5(2) . . . . ? C26 C25 C30 C31 78.8(3) . . . . ? C24 C25 C30 C31 -100.5(3) . . . . ? C28 C29 C33 C35 37.8(4) . . . . ? C24 C29 C33 C35 -144.2(2) . . . . ? C28 C29 C33 C34 -85.9(3) . . . . ? C24 C29 C33 C34 92.0(3) . . . . ? N2 C13 N1 C14 0.5(2) . . . . ? Ni1 C13 N1 C14 -174.4(2) . . . . ? N2 C13 N1 C1 -179.99(19) . . . . ? Ni1 C13 N1 C1 5.1(4) . . . . ? C15 C14 N1 C13 -0.6(3) . . . . ? C15 C14 N1 C1 179.83(19) . . . . ? C6 C1 N1 C13 -86.0(3) . . . . ? C2 C1 N1 C13 96.5(3) . . . . ? C6 C1 N1 C14 93.5(3) . . . . ? C2 C1 N1 C14 -84.1(3) . . . . ? C14 C15 N2 C13 -0.2(3) . . . . ? C14 C15 N2 C16 176.3(2) . . . . ? N1 C13 N2 C15 -0.2(2) . . . . ? Ni1 C13 N2 C15 176.72(15) . . . . ? N1 C13 N2 C16 -177.21(18) . . . . ? Ni1 C13 N2 C16 -0.3(2) . . . . ? N3 C16 N2 C15 -176.9(2) . . . . ? C17 C16 N2 C15 1.0(4) . . . . ? N3 C16 N2 C13 -0.5(3) . . . . ? C17 C16 N2 C13 177.4(2) . . . . ? C17 C16 N3 C20 0.4(3) . . . . ? N2 C16 N3 C20 178.45(18) . . . . ? C17 C16 N3 Ni1 -176.83(19) . . . . ? N2 C16 N3 Ni1 1.2(2) . . . . ? N4 C20 N3 C16 -179.7(2) . . . . ? C19 C20 N3 C16 -0.1(3) . . . . ? N4 C20 N3 Ni1 -2.4(3) . . . . ? C19 C20 N3 Ni1 177.18(17) . . . . ? N3 C20 N4 C21 5.1(3) . . . . ? C19 C20 N4 C21 -174.4(2) . . . . ? N3 C20 N4 C22 178.28(19) . . . . ? C19 C20 N4 C22 -1.3(4) . . . . ? C37 C21 N4 C20 172.0(2) . . . . ? Ni1 C21 N4 C20 -5.4(2) . . . . ? C37 C21 N4 C22 -0.9(3) . . . . ? Ni1 C21 N4 C22 -178.32(17) . . . . ? C23 C22 N4 C20 -89.6(3) . . . . ? C23 C22 N4 C21 83.1(3) . . . . ? C22 C23 N5 C24 178.2(2) . . . . ? C25 C24 N5 C23 91.4(3) . . . . ? C29 C24 N5 C23 -91.8(3) . . . . ? C16 N3 Ni1 C13 -1.14(17) . . . . ? C20 N3 Ni1 C13 -178.44(18) . . . . ? C16 N3 Ni1 C36 158(3) . . . . ? C20 N3 Ni1 C36 -19(3) . . . . ? C16 N3 Ni1 C21 176.79(19) . . . . ? C20 N3 Ni1 C21 -0.51(17) . . . . ? N1 C13 Ni1 N3 175.4(3) . . . . ? N2 C13 Ni1 N3 0.71(15) . . . . ? N1 C13 Ni1 C36 -3.8(3) . . . . ? N2 C13 Ni1 C36 -178.47(16) . . . . ? N1 C13 Ni1 C21 167.9(3) . . . . ? N2 C13 Ni1 C21 -6.8(4) . . . . ? C37 C21 Ni1 N3 -173.9(3) . . . . ? N4 C21 Ni1 N3 3.07(15) . . . . ? C37 C21 Ni1 C13 -166.4(3) . . . . ? N4 C21 Ni1 C13 10.6(4) . . . . ? C37 C21 Ni1 C36 5.4(3) . . . . ? N4 C21 Ni1 C36 -177.65(16) . . . . ? C41 C40 O1 C39 -177.3(3) . . . . ? C38 C39 O1 C40 174.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.459 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.062 #==END