data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Andreas Danopoulos' 'Sandra Freeman' 'David Pugh' 'Joseph A. Wright' _publ_contact_author_name 'Andreas Danopoulos' _publ_contact_author_address ; School of Chemistry University of Southampton Highfield Southampton Hampshire SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email AD1@SOTON.AC.UK _publ_section_title ; Manuscript Title: 'Pincer' dicarbene complexes of some early transition metals and uranium ; _publ_requested_category FM data_1a _database_code_depnum_ccdc_archive 'CCDC 282396' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H49 Cl2 N5 O V, 2(C4 H8 O)' _chemical_formula_sum 'C47 H65 Cl2 N5 O3 V' _chemical_formula_weight 869.88 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' Cl Cl 0.1484 0.1585 '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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' 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' _cell_length_a 10.306(3) _cell_length_b 32.019(11) _cell_length_c 13.807(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4556(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 33852 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 24.11 _exptl_crystal_description plate _exptl_crystal_colour 'blue green' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 0.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.955 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'Sortav (Blessing, 1997)' _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 KappaCCD area detector' _diffrn_measurement_method 'Phi and Omega scans to fill asymmetric unit' _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 21996 _diffrn_reflns_av_R_equivalents 0.1892 _diffrn_reflns_av_sigmaI/netI 0.2288 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 24.20 _reflns_number_total 6436 _reflns_number_gt 3002 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998) ; _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 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^)+(0.0285P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2774 Friedel pairs' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 6436 _refine_ls_number_parameters 531 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1917 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7959(8) 0.1638(3) 0.5064(6) 0.045(2) Uani 1 1 d . . . H1A H 0.8401 0.1598 0.4434 0.054 Uiso 1 1 calc R . . H1B H 0.8627 0.1660 0.5576 0.054 Uiso 1 1 calc R . . C2 C 0.7156(10) 0.2020(3) 0.5040(9) 0.082(4) Uani 1 1 d . . . H2A H 0.7158 0.2143 0.4382 0.099 Uiso 1 1 calc R . . H2B H 0.7497 0.2230 0.5501 0.099 Uiso 1 1 calc R . . C3 C 0.5828(10) 0.1893(3) 0.5317(10) 0.095(5) Uani 1 1 d . . . H3A H 0.5644 0.1972 0.5997 0.114 Uiso 1 1 calc R . . H3B H 0.5178 0.2028 0.4892 0.114 Uiso 1 1 calc R . . C4 C 0.5792(8) 0.1440(3) 0.5201(7) 0.049(3) Uani 1 1 d . . . H4A H 0.5260 0.1312 0.5719 0.059 Uiso 1 1 calc R . . H4B H 0.5408 0.1365 0.4567 0.059 Uiso 1 1 calc R . . C5 C 0.9230(8) 0.0012(3) 0.6687(6) 0.035(2) Uani 1 1 d . . . C6 C 0.9123(8) 0.0760(3) 0.6811(6) 0.030(2) Uani 1 1 d . . . C7 C 1.0424(8) 0.0819(3) 0.8153(6) 0.037(2) Uani 1 1 d . . . H7 H 1.0876 0.0944 0.8678 0.045 Uiso 1 1 calc R . . C8 C 1.0388(8) 0.0418(3) 0.7940(6) 0.038(2) Uani 1 1 d . . . H8 H 1.0814 0.0200 0.8280 0.046 Uiso 1 1 calc R . . C9 C 0.9546(9) 0.1469(3) 0.7434(6) 0.037(2) Uani 1 1 d . . . C10 C 1.0492(8) 0.1692(3) 0.6975(6) 0.040(2) Uani 1 1 d . . . C11 C 1.0394(9) 0.2129(3) 0.6970(6) 0.047(3) Uani 1 1 d . . . H11 H 1.1046 0.2291 0.6662 0.056 Uiso 1 1 calc R . . C12 C 0.9356(10) 0.2324(3) 0.7407(7) 0.055(3) Uani 1 1 d . . . H12 H 0.9293 0.2620 0.7407 0.067 Uiso 1 1 calc R . . C13 C 0.8391(10) 0.2081(4) 0.7853(7) 0.058(3) Uani 1 1 d . . . H13 H 0.7666 0.2213 0.8148 0.069 Uiso 1 1 calc R . . C14 C 0.8492(8) 0.1656(3) 0.7866(6) 0.041(2) Uani 1 1 d . . . C15 C 0.7471(9) 0.1392(3) 0.8393(6) 0.047(3) Uani 1 1 d . . . H15 H 0.7506 0.1103 0.8120 0.057 Uiso 1 1 calc R . . C16 C 0.7820(10) 0.1367(3) 0.9459(7) 0.073(3) Uani 1 1 d . . . H16A H 0.8670 0.1234 0.9531 0.109 Uiso 1 1 calc R . . H16B H 0.7163 0.1203 0.9802 0.109 Uiso 1 1 calc R . . H16C H 0.7851 0.1650 0.9732 0.109 Uiso 1 1 calc R . . C17 C 0.6072(9) 0.1556(3) 0.8273(7) 0.075(3) Uani 1 1 d . . . H17A H 0.6017 0.1842 0.8526 0.112 Uiso 1 1 calc R . . H17B H 0.5473 0.1376 0.8633 0.112 Uiso 1 1 calc R . . H17C H 0.5836 0.1555 0.7586 0.112 Uiso 1 1 calc R . . C18 C 1.1676(9) 0.1489(3) 0.6497(7) 0.053(3) Uani 1 1 d . . . H18 H 1.1462 0.1188 0.6389 0.063 Uiso 1 1 calc R . . C19 C 1.2845(9) 0.1505(3) 0.7188(7) 0.075(3) Uani 1 1 d . . . H19A H 1.3555 0.1337 0.6922 0.113 Uiso 1 1 calc R . . H19B H 1.2593 0.1394 0.7821 0.113 Uiso 1 1 calc R . . H19C H 1.3132 0.1795 0.7261 0.113 Uiso 1 1 calc R . . C20 C 1.2012(9) 0.1676(3) 0.5521(8) 0.071(3) Uani 1 1 d . . . H20A H 1.1259 0.1655 0.5090 0.107 Uiso 1 1 calc R . . H20B H 1.2743 0.1523 0.5238 0.107 Uiso 1 1 calc R . . H20C H 1.2250 0.1970 0.5604 0.107 Uiso 1 1 calc R . . C21 C 0.9654(8) -0.0386(3) 0.6935(6) 0.038(2) Uani 1 1 d . . . H21 H 1.0248 -0.0426 0.7453 0.046 Uiso 1 1 calc R . . C22 C 0.9192(7) -0.0720(3) 0.6409(6) 0.039(2) Uani 1 1 d . . . H22 H 0.9474 -0.0993 0.6572 0.046 Uiso 1 1 calc R . . C23 C 0.8331(6) -0.0669(3) 0.5653(7) 0.040(2) Uani 1 1 d . . . H23 H 0.8011 -0.0899 0.5290 0.048 Uiso 1 1 calc R . . C24 C 0.7964(7) -0.0267(3) 0.5455(6) 0.032(2) Uani 1 1 d . . . C25 C 0.6667(7) 0.0260(3) 0.4659(6) 0.030(2) Uani 1 1 d . . . C26 C 0.5617(8) -0.0184(3) 0.3613(7) 0.042(2) Uani 1 1 d . . . H26 H 0.5032 -0.0279 0.3129 0.051 Uiso 1 1 calc R . . C27 C 0.6453(8) -0.0421(3) 0.4106(7) 0.041(2) Uani 1 1 d . . . H27 H 0.6595 -0.0713 0.4039 0.049 Uiso 1 1 calc R . . C28 C 0.4900(8) 0.0555(3) 0.3648(6) 0.034(2) Uani 1 1 d . . . C29 C 0.3652(7) 0.0577(3) 0.4028(6) 0.036(2) Uani 1 1 d . . . C30 C 0.2851(9) 0.0896(3) 0.3726(7) 0.047(3) Uani 1 1 d . . . H30 H 0.2000 0.0919 0.3986 0.056 Uiso 1 1 calc R . . C31 C 0.3269(8) 0.1183(3) 0.3052(7) 0.048(3) Uani 1 1 d . . . H31 H 0.2703 0.1400 0.2850 0.058 Uiso 1 1 calc R . . C32 C 0.4481(8) 0.1159(3) 0.2674(6) 0.046(3) Uani 1 1 d . . . H32 H 0.4756 0.1362 0.2216 0.055 Uiso 1 1 calc R . . C33 C 0.5323(8) 0.0844(3) 0.2946(7) 0.042(2) Uani 1 1 d . . . C34 C 0.6599(8) 0.0787(3) 0.2443(6) 0.049(3) Uani 1 1 d . . . H34 H 0.7157 0.0602 0.2851 0.059 Uiso 1 1 calc R . . C35 C 0.6384(10) 0.0573(3) 0.1463(7) 0.079(4) Uani 1 1 d . . . H35A H 0.6084 0.0287 0.1568 0.118 Uiso 1 1 calc R . . H35B H 0.7202 0.0569 0.1101 0.118 Uiso 1 1 calc R . . H35C H 0.5730 0.0728 0.1093 0.118 Uiso 1 1 calc R . . C36 C 0.7298(9) 0.1191(3) 0.2292(7) 0.067(3) Uani 1 1 d . . . H36A H 0.6808 0.1365 0.1836 0.100 Uiso 1 1 calc R . . H36B H 0.8164 0.1136 0.2028 0.100 Uiso 1 1 calc R . . H36C H 0.7380 0.1338 0.2912 0.100 Uiso 1 1 calc R . . C37 C 0.3175(7) 0.0250(3) 0.4747(6) 0.040(2) Uani 1 1 d . . . H37 H 0.3935 0.0081 0.4968 0.048 Uiso 1 1 calc R . . C38 C 0.2209(8) -0.0041(2) 0.4249(6) 0.046(2) Uani 1 1 d . . . H38A H 0.1969 -0.0267 0.4694 0.069 Uiso 1 1 calc R . . H38B H 0.2608 -0.0160 0.3667 0.069 Uiso 1 1 calc R . . H38C H 0.1432 0.0117 0.4068 0.069 Uiso 1 1 calc R . . C39 C 0.2542(7) 0.0449(2) 0.5628(7) 0.049(2) Uani 1 1 d . . . H39A H 0.1780 0.0609 0.5423 0.073 Uiso 1 1 calc R . . H39B H 0.3164 0.0636 0.5945 0.073 Uiso 1 1 calc R . . H39C H 0.2275 0.0230 0.6082 0.073 Uiso 1 1 calc R . . C40 C 0.8967(13) 0.2114(5) 0.2237(12) 0.120(5) Uani 1 1 d . . . H40A H 0.8730 0.2000 0.1594 0.144 Uiso 1 1 calc R . . H40B H 0.8241 0.2063 0.2692 0.144 Uiso 1 1 calc R . . C41 C 1.0181(10) 0.1915(3) 0.2599(8) 0.075(4) Uani 1 1 d . . . H41A H 0.9988 0.1667 0.3001 0.090 Uiso 1 1 calc R . . H41B H 1.0755 0.1832 0.2057 0.090 Uiso 1 1 calc R . . C42 C 1.0267(17) 0.2632(4) 0.2721(13) 0.136(7) Uani 1 1 d . . . H42A H 1.0016 0.2837 0.3224 0.163 Uiso 1 1 calc R . . H42B H 1.0950 0.2759 0.2313 0.163 Uiso 1 1 calc R . . C43 C 1.0773(14) 0.2253(4) 0.3186(10) 0.132(6) Uani 1 1 d . . . H43A H 1.0497 0.2236 0.3871 0.159 Uiso 1 1 calc R . . H43B H 1.1732 0.2243 0.3153 0.159 Uiso 1 1 calc R . . C44 C 0.6811(11) 0.8298(4) 0.5167(9) 0.094(4) Uani 1 1 d . . . H44A H 0.6087 0.8455 0.4866 0.113 Uiso 1 1 calc R . . H44B H 0.6796 0.8349 0.5874 0.113 Uiso 1 1 calc R . . C45 C 0.6678(14) 0.7839(4) 0.4959(9) 0.091(4) Uani 1 1 d . . . H45A H 0.6093 0.7700 0.5428 0.110 Uiso 1 1 calc R . . H45B H 0.6362 0.7787 0.4292 0.110 Uiso 1 1 calc R . . C46 C 0.8061(12) 0.7701(4) 0.5084(9) 0.086(4) Uani 1 1 d . . . H46A H 0.8265 0.7648 0.5774 0.104 Uiso 1 1 calc R . . H46B H 0.8245 0.7446 0.4704 0.104 Uiso 1 1 calc R . . C47 C 0.8802(12) 0.8065(5) 0.4705(10) 0.102(4) Uani 1 1 d . . . H47A H 0.9603 0.8107 0.5089 0.122 Uiso 1 1 calc R . . H47B H 0.9050 0.8017 0.4022 0.122 Uiso 1 1 calc R . . Cl1 Cl 0.93500(19) 0.07535(7) 0.43100(15) 0.0428(6) Uani 1 1 d . . . Cl2 Cl 0.60017(19) 0.06341(8) 0.67642(15) 0.0451(7) Uani 1 1 d . . . N1 N 0.8393(6) 0.0073(2) 0.5936(5) 0.0292(18) Uani 1 1 d . . . N2 N 0.9611(6) 0.0374(2) 0.7126(5) 0.0309(18) Uani 1 1 d . . . N3 N 0.9665(6) 0.1027(2) 0.7455(5) 0.0334(18) Uani 1 1 d . . . N4 N 0.7068(6) -0.0150(2) 0.4737(5) 0.0325(18) Uani 1 1 d . . . N5 N 0.5750(6) 0.0231(2) 0.3933(5) 0.0346(19) Uani 1 1 d . . . O1 O 0.7111(5) 0.12927(17) 0.5258(4) 0.0437(18) Uani 1 1 d . . . O2 O 0.9232(12) 0.2538(4) 0.2172(10) 0.175(5) Uani 1 1 d . . . O3 O 0.7986(11) 0.8425(3) 0.4778(6) 0.122(4) Uani 1 1 d . . . V1 V 0.77477(12) 0.06722(4) 0.56000(12) 0.0310(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 0.041(6) 0.052(7) 0.040(6) 0.009(5) -0.007(5) -0.008(5) C2 0.075(8) 0.047(8) 0.125(10) 0.019(7) 0.005(8) 0.021(7) C3 0.058(7) 0.044(8) 0.183(15) -0.001(8) 0.008(9) 0.017(6) C4 0.033(5) 0.050(7) 0.063(7) -0.006(5) 0.003(5) 0.008(4) C5 0.022(5) 0.052(7) 0.030(6) 0.000(6) 0.003(5) -0.002(5) C6 0.033(5) 0.025(6) 0.031(5) -0.004(5) 0.008(5) -0.013(4) C7 0.030(5) 0.048(7) 0.034(6) -0.004(5) -0.010(5) -0.003(5) C8 0.024(5) 0.061(8) 0.029(6) 0.008(5) -0.003(5) 0.000(5) C9 0.033(6) 0.036(7) 0.043(6) 0.004(5) -0.009(5) -0.004(5) C10 0.042(6) 0.046(7) 0.033(6) 0.002(5) -0.001(5) -0.003(5) C11 0.058(7) 0.041(7) 0.040(6) -0.001(5) 0.003(5) -0.013(5) C12 0.069(8) 0.040(7) 0.057(7) -0.006(6) -0.001(6) 0.000(6) C13 0.051(7) 0.075(10) 0.047(7) -0.017(7) 0.002(6) -0.001(6) C14 0.040(6) 0.048(8) 0.036(6) 0.002(5) -0.011(5) 0.005(5) C15 0.044(6) 0.057(7) 0.041(6) -0.009(5) 0.016(5) -0.009(5) C16 0.065(7) 0.092(9) 0.062(8) 0.018(6) -0.003(6) 0.000(6) C17 0.054(7) 0.114(10) 0.057(7) -0.023(7) 0.018(6) -0.001(7) C18 0.039(6) 0.061(7) 0.058(7) -0.004(6) -0.005(6) -0.011(5) C19 0.046(6) 0.104(10) 0.076(8) 0.008(7) 0.013(7) -0.006(6) C20 0.065(7) 0.090(8) 0.058(7) 0.004(8) 0.013(7) 0.003(6) C21 0.029(5) 0.043(7) 0.043(6) 0.006(5) -0.003(5) 0.004(5) C22 0.034(5) 0.025(6) 0.057(6) 0.015(5) -0.003(5) 0.011(5) C23 0.025(4) 0.037(6) 0.057(6) -0.014(6) -0.003(6) -0.007(4) C24 0.023(5) 0.051(7) 0.024(6) -0.002(6) 0.013(5) -0.007(5) C25 0.018(5) 0.043(7) 0.029(5) 0.003(5) 0.001(4) 0.002(4) C26 0.029(5) 0.052(7) 0.046(6) -0.024(6) -0.005(5) -0.002(5) C27 0.035(5) 0.038(6) 0.049(6) -0.009(6) -0.002(5) 0.006(5) C28 0.037(6) 0.042(7) 0.025(5) -0.008(5) -0.015(5) -0.002(5) C29 0.022(5) 0.046(7) 0.041(6) -0.008(5) -0.004(5) -0.002(4) C30 0.031(5) 0.052(7) 0.057(7) -0.001(6) 0.004(5) 0.014(5) C31 0.024(5) 0.072(8) 0.048(6) 0.015(6) -0.002(5) 0.012(5) C32 0.043(6) 0.057(7) 0.037(6) 0.010(5) -0.004(5) 0.005(6) C33 0.031(6) 0.058(7) 0.039(6) -0.008(6) -0.011(5) 0.009(5) C34 0.035(6) 0.070(8) 0.041(6) 0.013(6) 0.014(5) 0.000(5) C35 0.101(9) 0.070(9) 0.065(8) -0.019(7) 0.027(7) 0.004(7) C36 0.034(6) 0.114(10) 0.053(7) 0.000(7) 0.007(6) 0.018(7) C37 0.024(5) 0.045(6) 0.051(6) -0.001(5) -0.001(5) 0.010(4) C38 0.041(5) 0.049(6) 0.048(6) 0.000(5) 0.012(5) -0.005(5) C39 0.027(5) 0.066(6) 0.054(5) -0.008(7) 0.000(6) 0.001(4) C40 0.105(12) 0.073(11) 0.181(16) 0.011(10) 0.012(11) -0.015(9) C41 0.050(7) 0.070(9) 0.104(10) 0.005(8) -0.011(7) 0.003(7) C42 0.170(17) 0.054(10) 0.183(17) -0.009(11) -0.084(14) 0.007(11) C43 0.169(15) 0.071(11) 0.157(14) -0.034(10) -0.104(13) -0.001(10) C44 0.072(9) 0.111(12) 0.100(10) -0.051(9) -0.010(8) 0.022(8) C45 0.112(12) 0.083(11) 0.079(9) -0.007(8) -0.011(8) -0.008(9) C46 0.105(12) 0.080(10) 0.074(9) 0.002(7) -0.015(9) -0.018(9) C47 0.089(10) 0.108(12) 0.107(11) -0.022(9) 0.036(8) 0.002(10) Cl1 0.0293(12) 0.0638(18) 0.0354(13) 0.0001(14) 0.0049(12) 0.0026(11) Cl2 0.0367(12) 0.0621(17) 0.0364(15) 0.0073(14) 0.0057(11) -0.0040(12) N1 0.023(4) 0.037(5) 0.028(5) 0.002(4) 0.000(4) 0.002(3) N2 0.022(4) 0.039(5) 0.032(5) 0.005(4) -0.004(4) -0.006(4) N3 0.025(4) 0.040(5) 0.035(5) 0.006(4) 0.004(4) -0.002(4) N4 0.023(4) 0.047(6) 0.028(4) -0.011(4) -0.006(4) -0.009(4) N5 0.025(4) 0.049(6) 0.030(5) 0.001(4) 0.007(4) 0.010(4) O1 0.027(3) 0.037(4) 0.067(5) 0.016(3) 0.006(3) 0.006(3) O2 0.158(10) 0.115(10) 0.252(16) 0.039(10) -0.085(10) 0.000(8) O3 0.154(10) 0.080(7) 0.133(8) -0.032(6) 0.077(7) -0.033(7) V1 0.0234(7) 0.0398(9) 0.0299(8) -0.0004(9) 0.0016(8) 0.0001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.434(8) . ? C1 C2 1.478(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.478(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.459(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O1 1.441(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.363(9) . ? C5 N2 1.365(10) . ? C5 C21 1.388(10) . ? C6 N3 1.354(9) . ? C6 N2 1.405(9) . ? C6 V1 2.209(9) . ? C7 C8 1.316(11) . ? C7 N3 1.409(10) . ? C7 H7 0.9500 . ? C8 N2 1.387(9) . ? C8 H8 0.9500 . ? C9 C10 1.366(11) . ? C9 C14 1.377(11) . ? C9 N3 1.420(10) . ? C10 C11 1.401(11) . ? C10 C18 1.533(12) . ? C11 C12 1.378(12) . ? C11 H11 0.9500 . ? C12 C13 1.405(12) . ? C12 H12 0.9500 . ? C13 C14 1.364(12) . ? C13 H13 0.9500 . ? C14 C15 1.533(12) . ? C15 C16 1.517(12) . ? C15 C17 1.544(12) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.514(12) . ? C18 C19 1.537(12) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.377(11) . ? C21 H21 0.9500 . ? C22 C23 1.380(11) . ? C22 H22 0.9500 . ? C23 C24 1.369(11) . ? C23 H23 0.9500 . ? C24 N1 1.348(9) . ? C24 N4 1.405(9) . ? C25 N4 1.378(10) . ? C25 N5 1.381(9) . ? C25 V1 2.162(9) . ? C26 C27 1.336(11) . ? C26 N5 1.406(10) . ? C26 H26 0.9500 . ? C27 N4 1.384(9) . ? C27 H27 0.9500 . ? C28 C29 1.392(11) . ? C28 C33 1.409(11) . ? C28 N5 1.414(10) . ? C29 C30 1.378(11) . ? C29 C37 1.525(11) . ? C30 C31 1.376(11) . ? C30 H30 0.9500 . ? C31 C32 1.356(11) . ? C31 H31 0.9500 . ? C32 C33 1.383(11) . ? C32 H32 0.9500 . ? C33 C34 1.498(11) . ? C34 C36 1.496(12) . ? C34 C35 1.533(12) . ? C34 H34 1.0000 . ? 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 C39 1.520(11) . ? C37 C38 1.527(10) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 O2 1.390(13) . ? C40 C41 1.490(14) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C43 1.483(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O2 1.343(15) . ? C42 C43 1.467(15) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O3 1.386(12) . ? C44 C45 1.504(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.502(14) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.489(14) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 O3 1.428(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? Cl1 V1 2.443(3) . ? Cl2 V1 2.416(3) . ? N1 V1 2.084(7) . ? O1 V1 2.145(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 107.5(7) . . ? O1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? O1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? C1 C2 C3 106.5(8) . . ? C1 C2 H2A 110.4 . . ? C3 C2 H2A 110.4 . . ? C1 C2 H2B 110.4 . . ? C3 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? C4 C3 C2 105.6(8) . . ? C4 C3 H3A 110.6 . . ? C2 C3 H3A 110.6 . . ? C4 C3 H3B 110.6 . . ? C2 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O1 C4 C3 107.2(7) . . ? O1 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O1 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? N1 C5 N2 113.4(8) . . ? N1 C5 C21 121.2(8) . . ? N2 C5 C21 125.3(8) . . ? N3 C6 N2 101.8(7) . . ? N3 C6 V1 147.3(7) . . ? N2 C6 V1 110.6(5) . . ? C8 C7 N3 107.0(8) . . ? C8 C7 H7 126.5 . . ? N3 C7 H7 126.5 . . ? C7 C8 N2 107.4(8) . . ? C7 C8 H8 126.3 . . ? N2 C8 H8 126.3 . . ? C10 C9 C14 122.4(9) . . ? C10 C9 N3 118.1(9) . . ? C14 C9 N3 119.5(8) . . ? C9 C10 C11 118.3(9) . . ? C9 C10 C18 123.0(9) . . ? C11 C10 C18 118.6(8) . . ? C12 C11 C10 120.4(9) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.4(9) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 120.3(9) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 119.3(9) . . ? C13 C14 C15 120.3(9) . . ? C9 C14 C15 120.4(9) . . ? C16 C15 C14 109.1(7) . . ? C16 C15 C17 110.0(8) . . ? C14 C15 C17 113.7(8) . . ? C16 C15 H15 108.0 . . ? C14 C15 H15 108.0 . . ? C17 C15 H15 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C10 113.4(8) . . ? C20 C18 C19 111.1(8) . . ? C10 C18 C19 110.0(8) . . ? C20 C18 H18 107.4 . . ? C10 C18 H18 107.4 . . ? C19 C18 H18 107.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C5 118.2(8) . . ? C22 C21 H21 120.9 . . ? C5 C21 H21 120.9 . . ? C21 C22 C23 122.0(8) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C24 C23 C22 116.0(8) . . ? C24 C23 H23 122.0 . . ? C22 C23 H23 122.0 . . ? N1 C24 C23 124.7(8) . . ? N1 C24 N4 110.4(8) . . ? C23 C24 N4 124.9(8) . . ? N4 C25 N5 101.5(7) . . ? N4 C25 V1 112.3(6) . . ? N5 C25 V1 146.1(7) . . ? C27 C26 N5 108.3(8) . . ? C27 C26 H26 125.9 . . ? N5 C26 H26 125.9 . . ? C26 C27 N4 105.1(8) . . ? C26 C27 H27 127.5 . . ? N4 C27 H27 127.5 . . ? C29 C28 C33 120.8(8) . . ? C29 C28 N5 120.3(8) . . ? C33 C28 N5 118.8(8) . . ? C30 C29 C28 118.5(8) . . ? C30 C29 C37 120.9(8) . . ? C28 C29 C37 120.6(8) . . ? C31 C30 C29 120.8(8) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 120.7(9) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 121.0(9) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C28 118.1(8) . . ? C32 C33 C34 120.9(9) . . ? C28 C33 C34 120.8(8) . . ? C36 C34 C33 112.5(8) . . ? C36 C34 C35 109.4(8) . . ? C33 C34 C35 109.7(8) . . ? C36 C34 H34 108.4 . . ? C33 C34 H34 108.4 . . ? C35 C34 H34 108.4 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C29 111.8(7) . . ? C39 C37 C38 109.7(6) . . ? C29 C37 C38 109.7(7) . . ? C39 C37 H37 108.6 . . ? C29 C37 H37 108.6 . . ? C38 C37 H37 108.6 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O2 C40 C41 105.9(11) . . ? O2 C40 H40A 110.5 . . ? C41 C40 H40A 110.5 . . ? O2 C40 H40B 110.5 . . ? C41 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? C43 C41 C40 102.5(10) . . ? C43 C41 H41A 111.3 . . ? C40 C41 H41A 111.3 . . ? C43 C41 H41B 111.3 . . ? C40 C41 H41B 111.3 . . ? H41A C41 H41B 109.2 . . ? O2 C42 C43 110.2(12) . . ? O2 C42 H42A 109.6 . . ? C43 C42 H42A 109.6 . . ? O2 C42 H42B 109.6 . . ? C43 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C42 C43 C41 102.6(10) . . ? C42 C43 H43A 111.2 . . ? C41 C43 H43A 111.2 . . ? C42 C43 H43B 111.2 . . ? C41 C43 H43B 111.2 . . ? H43A C43 H43B 109.2 . . ? O3 C44 C45 106.9(10) . . ? O3 C44 H44A 110.3 . . ? C45 C44 H44A 110.3 . . ? O3 C44 H44B 110.3 . . ? C45 C44 H44B 110.3 . . ? H44A C44 H44B 108.6 . . ? C46 C45 C44 100.3(10) . . ? C46 C45 H45A 111.7 . . ? C44 C45 H45A 111.7 . . ? C46 C45 H45B 111.7 . . ? C44 C45 H45B 111.7 . . ? H45A C45 H45B 109.5 . . ? C47 C46 C45 102.5(10) . . ? C47 C46 H46A 111.3 . . ? C45 C46 H46A 111.3 . . ? C47 C46 H46B 111.3 . . ? C45 C46 H46B 111.3 . . ? H46A C46 H46B 109.2 . . ? O3 C47 C46 107.7(10) . . ? O3 C47 H47A 110.2 . . ? C46 C47 H47A 110.2 . . ? O3 C47 H47B 110.2 . . ? C46 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? C24 N1 C5 117.8(8) . . ? C24 N1 V1 121.9(6) . . ? C5 N1 V1 120.2(6) . . ? C5 N2 C8 127.8(8) . . ? C5 N2 C6 120.5(7) . . ? C8 N2 C6 111.5(7) . . ? C6 N3 C7 112.3(7) . . ? C6 N3 C9 125.4(8) . . ? C7 N3 C9 122.2(8) . . ? C25 N4 C27 114.2(7) . . ? C25 N4 C24 120.4(7) . . ? C27 N4 C24 125.2(8) . . ? C25 N5 C26 111.0(7) . . ? C25 N5 C28 125.2(7) . . ? C26 N5 C28 123.1(7) . . ? C1 O1 C4 108.2(6) . . ? C1 O1 V1 124.6(4) . . ? C4 O1 V1 127.2(5) . . ? C42 O2 C40 109.7(12) . . ? C44 O3 C47 107.8(9) . . ? N1 V1 O1 179.2(3) . . ? N1 V1 C25 74.7(3) . . ? O1 V1 C25 106.0(3) . . ? N1 V1 C6 75.2(3) . . ? O1 V1 C6 104.2(3) . . ? C25 V1 C6 149.6(3) . . ? N1 V1 Cl2 92.47(17) . . ? O1 V1 Cl2 88.00(16) . . ? C25 V1 Cl2 89.2(2) . . ? C6 V1 Cl2 88.9(2) . . ? N1 V1 Cl1 92.56(17) . . ? O1 V1 Cl1 87.02(16) . . ? C25 V1 Cl1 88.6(2) . . ? C6 V1 Cl1 96.0(2) . . ? Cl2 V1 Cl1 173.73(10) . . ? 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 O1 C1 C2 C3 5.1(12) . . . . ? C1 C2 C3 C4 -17.0(13) . . . . ? C2 C3 C4 O1 22.8(12) . . . . ? N3 C7 C8 N2 -0.5(9) . . . . ? C14 C9 C10 C11 1.7(13) . . . . ? N3 C9 C10 C11 -178.7(7) . . . . ? C14 C9 C10 C18 179.6(8) . . . . ? N3 C9 C10 C18 -0.8(13) . . . . ? C9 C10 C11 C12 -0.8(13) . . . . ? C18 C10 C11 C12 -178.8(8) . . . . ? C10 C11 C12 C13 -0.5(14) . . . . ? C11 C12 C13 C14 1.0(15) . . . . ? C12 C13 C14 C9 -0.2(14) . . . . ? C12 C13 C14 C15 177.2(8) . . . . ? C10 C9 C14 C13 -1.2(14) . . . . ? N3 C9 C14 C13 179.2(8) . . . . ? C10 C9 C14 C15 -178.6(8) . . . . ? N3 C9 C14 C15 1.8(12) . . . . ? C13 C14 C15 C16 -84.2(10) . . . . ? C9 C14 C15 C16 93.2(10) . . . . ? C13 C14 C15 C17 39.0(12) . . . . ? C9 C14 C15 C17 -143.6(8) . . . . ? C9 C10 C18 C20 137.4(9) . . . . ? C11 C10 C18 C20 -44.7(11) . . . . ? C9 C10 C18 C19 -97.5(10) . . . . ? C11 C10 C18 C19 80.4(10) . . . . ? N1 C5 C21 C22 -0.9(11) . . . . ? N2 C5 C21 C22 -179.0(7) . . . . ? C5 C21 C22 C23 0.1(11) . . . . ? C21 C22 C23 C24 0.0(11) . . . . ? C22 C23 C24 N1 0.7(11) . . . . ? C22 C23 C24 N4 -177.9(6) . . . . ? N5 C26 C27 N4 1.2(9) . . . . ? C33 C28 C29 C30 -2.1(12) . . . . ? N5 C28 C29 C30 -179.5(7) . . . . ? C33 C28 C29 C37 176.7(7) . . . . ? N5 C28 C29 C37 -0.8(12) . . . . ? C28 C29 C30 C31 1.0(12) . . . . ? C37 C29 C30 C31 -177.8(8) . . . . ? C29 C30 C31 C32 -0.3(14) . . . . ? C30 C31 C32 C33 0.7(14) . . . . ? C31 C32 C33 C28 -1.8(13) . . . . ? C31 C32 C33 C34 172.6(9) . . . . ? C29 C28 C33 C32 2.5(12) . . . . ? N5 C28 C33 C32 179.9(7) . . . . ? C29 C28 C33 C34 -171.9(8) . . . . ? N5 C28 C33 C34 5.6(12) . . . . ? C32 C33 C34 C36 44.7(12) . . . . ? C28 C33 C34 C36 -141.0(8) . . . . ? C32 C33 C34 C35 -77.3(11) . . . . ? C28 C33 C34 C35 96.9(10) . . . . ? C30 C29 C37 C39 -49.6(10) . . . . ? C28 C29 C37 C39 131.6(8) . . . . ? C30 C29 C37 C38 72.2(10) . . . . ? C28 C29 C37 C38 -106.5(8) . . . . ? O2 C40 C41 C43 29.2(16) . . . . ? O2 C42 C43 C41 17.6(19) . . . . ? C40 C41 C43 C42 -27.5(16) . . . . ? O3 C44 C45 C46 37.0(13) . . . . ? C44 C45 C46 C47 -35.3(12) . . . . ? C45 C46 C47 O3 23.5(14) . . . . ? C23 C24 N1 C5 -1.5(10) . . . . ? N4 C24 N1 C5 177.3(6) . . . . ? C23 C24 N1 V1 -178.7(6) . . . . ? N4 C24 N1 V1 0.1(8) . . . . ? N2 C5 N1 C24 179.9(6) . . . . ? C21 C5 N1 C24 1.6(10) . . . . ? N2 C5 N1 V1 -2.9(8) . . . . ? C21 C5 N1 V1 178.8(6) . . . . ? N1 C5 N2 C8 175.8(6) . . . . ? C21 C5 N2 C8 -6.0(12) . . . . ? N1 C5 N2 C6 1.4(9) . . . . ? C21 C5 N2 C6 179.6(7) . . . . ? C7 C8 N2 C5 -175.3(7) . . . . ? C7 C8 N2 C6 -0.5(9) . . . . ? N3 C6 N2 C5 176.5(6) . . . . ? V1 C6 N2 C5 0.5(8) . . . . ? N3 C6 N2 C8 1.2(8) . . . . ? V1 C6 N2 C8 -174.7(5) . . . . ? N2 C6 N3 C7 -1.5(8) . . . . ? V1 C6 N3 C7 171.5(8) . . . . ? N2 C6 N3 C9 176.2(7) . . . . ? V1 C6 N3 C9 -10.8(15) . . . . ? C8 C7 N3 C6 1.3(9) . . . . ? C8 C7 N3 C9 -176.5(7) . . . . ? C10 C9 N3 C6 -93.8(10) . . . . ? C14 C9 N3 C6 85.8(10) . . . . ? C10 C9 N3 C7 83.7(10) . . . . ? C14 C9 N3 C7 -96.7(9) . . . . ? N5 C25 N4 C27 0.0(8) . . . . ? V1 C25 N4 C27 -176.5(5) . . . . ? N5 C25 N4 C24 -175.9(6) . . . . ? V1 C25 N4 C24 7.6(8) . . . . ? C26 C27 N4 C25 -0.8(9) . . . . ? C26 C27 N4 C24 174.9(7) . . . . ? N1 C24 N4 C25 -5.3(9) . . . . ? C23 C24 N4 C25 173.5(7) . . . . ? N1 C24 N4 C27 179.3(7) . . . . ? C23 C24 N4 C27 -2.0(12) . . . . ? N4 C25 N5 C26 0.8(8) . . . . ? V1 C25 N5 C26 174.9(7) . . . . ? N4 C25 N5 C28 171.1(7) . . . . ? V1 C25 N5 C28 -14.7(13) . . . . ? C27 C26 N5 C25 -1.3(9) . . . . ? C27 C26 N5 C28 -171.9(8) . . . . ? C29 C28 N5 C25 -95.2(9) . . . . ? C33 C28 N5 C25 87.3(9) . . . . ? C29 C28 N5 C26 74.0(10) . . . . ? C33 C28 N5 C26 -103.5(9) . . . . ? C2 C1 O1 C4 9.1(10) . . . . ? C2 C1 O1 V1 -169.8(6) . . . . ? C3 C4 O1 C1 -20.0(10) . . . . ? C3 C4 O1 V1 158.8(7) . . . . ? C43 C42 O2 C40 1(2) . . . . ? C41 C40 O2 C42 -19.3(18) . . . . ? C45 C44 O3 C47 -23.3(14) . . . . ? C46 C47 O3 C44 -0.4(14) . . . . ? C24 N1 V1 C25 2.9(5) . . . . ? C5 N1 V1 C25 -174.2(5) . . . . ? C24 N1 V1 C6 179.6(6) . . . . ? C5 N1 V1 C6 2.4(5) . . . . ? C24 N1 V1 Cl2 91.4(5) . . . . ? C5 N1 V1 Cl2 -85.8(5) . . . . ? C24 N1 V1 Cl1 -84.9(5) . . . . ? C5 N1 V1 Cl1 98.0(5) . . . . ? C1 O1 V1 C25 -130.6(6) . . . . ? C4 O1 V1 C25 50.6(7) . . . . ? C1 O1 V1 C6 52.4(6) . . . . ? C4 O1 V1 C6 -126.3(6) . . . . ? C1 O1 V1 Cl2 140.8(6) . . . . ? C4 O1 V1 Cl2 -37.9(6) . . . . ? C1 O1 V1 Cl1 -43.0(6) . . . . ? C4 O1 V1 Cl1 138.3(6) . . . . ? N4 C25 V1 N1 -5.2(5) . . . . ? N5 C25 V1 N1 -179.0(9) . . . . ? N4 C25 V1 O1 174.3(5) . . . . ? N5 C25 V1 O1 0.5(9) . . . . ? N4 C25 V1 C6 -11.7(9) . . . . ? N5 C25 V1 C6 174.5(8) . . . . ? N4 C25 V1 Cl2 -98.0(5) . . . . ? N5 C25 V1 Cl2 88.2(9) . . . . ? N4 C25 V1 Cl1 87.8(5) . . . . ? N5 C25 V1 Cl1 -86.0(9) . . . . ? N3 C6 V1 N1 -174.1(11) . . . . ? N2 C6 V1 N1 -1.5(5) . . . . ? N3 C6 V1 O1 6.4(11) . . . . ? N2 C6 V1 O1 179.0(5) . . . . ? N3 C6 V1 C25 -167.7(8) . . . . ? N2 C6 V1 C25 4.9(9) . . . . ? N3 C6 V1 Cl2 -81.3(10) . . . . ? N2 C6 V1 Cl2 91.4(5) . . . . ? N3 C6 V1 Cl1 94.8(10) . . . . ? N2 C6 V1 Cl1 -92.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 24.20 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.301 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.064 #==END data_1b _database_code_depnum_ccdc_archive 'CCDC 282397' _audit_creation_date 2004-10-14T10:30:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H49 Br2 N5 O V' _chemical_formula_sum 'C39 H49 Br2 N5 O V' _chemical_formula_weight 814.59 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6919(15) _cell_length_b 14.6332(15) _cell_length_c 17.1157(12) _cell_angle_alpha 90 _cell_angle_beta 102.828(7) _cell_angle_gamma 90 _cell_volume 3832.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8854 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _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_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_unetI/netI 0.1035 _diffrn_reflns_number 36118 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 27.64 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 8801 _reflns_number_gt 5321 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _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-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 2004) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0650P)^2^+14.5625P] 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_number_reflns 8801 _refine_ls_number_parameters 445 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1398 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.772 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.117 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.3674(4) 0.4140(4) 0.3455(4) 0.0424(17) Uani 0.31(4) 1 d PD A 1 H1A1 H 0.3994 0.3748 0.3145 0.051 Uiso 0.31(4) 1 calc PR A 1 H1A2 H 0.3305 0.3747 0.3715 0.051 Uiso 0.31(4) 1 calc PR A 1 C2A C 0.430(3) 0.4679(17) 0.4068(18) 0.062(5) Uani 0.31(4) 1 d PD A 1 H2A1 H 0.4878 0.4373 0.4208 0.075 Uiso 0.31(4) 1 calc PR A 1 H2A2 H 0.4078 0.4755 0.4562 0.075 Uiso 0.31(4) 1 calc PR A 1 C3A C 0.4371(6) 0.5584(5) 0.3679(5) 0.072(3) Uani 0.31(4) 1 d PD A 1 H3A1 H 0.4366 0.6086 0.4066 0.086 Uiso 0.31(4) 1 calc PR A 1 H3A2 H 0.4923 0.5619 0.349 0.086 Uiso 0.31(4) 1 calc PR A 1 C1B C 0.3674(4) 0.4140(4) 0.3455(4) 0.0424(17) Uani 0.69(4) 1 d PD A 2 H1B1 H 0.3754 0.3585 0.3148 0.051 Uiso 0.69(4) 1 calc PR A 2 H1B2 H 0.339 0.3963 0.3894 0.051 Uiso 0.69(4) 1 calc PR A 2 C2B C 0.4550(10) 0.4586(8) 0.3793(14) 0.062(5) Uani 0.69(4) 1 d PD A 2 H2B1 H 0.4759 0.4437 0.4368 0.075 Uiso 0.69(4) 1 calc PR A 2 H2B2 H 0.4993 0.4385 0.3499 0.075 Uiso 0.69(4) 1 calc PR A 2 C3B C 0.4371(6) 0.5584(5) 0.3679(5) 0.072(3) Uani 0.69(4) 1 d PD A 2 H3B1 H 0.4885 0.5904 0.3562 0.086 Uiso 0.69(4) 1 calc PR A 2 H3B2 H 0.4235 0.5855 0.4167 0.086 Uiso 0.69(4) 1 calc PR A 2 C4 C 0.3604(4) 0.5667(4) 0.2987(4) 0.0372(15) Uani 1 1 d . . . H4A H 0.322 0.6174 0.3077 0.045 Uiso 1 1 calc R A 1 H4B H 0.3802 0.5787 0.2486 0.045 Uiso 1 1 calc R A 1 C5 C 0.0155(4) 0.4542(4) 0.1090(4) 0.0344(15) Uani 1 1 d . . . C6 C 0.1031(4) 0.5468(4) 0.2137(4) 0.0300(14) Uani 1 1 d . A . C7 C -0.0039(5) 0.6431(5) 0.2320(5) 0.0472(19) Uani 1 1 d . . . H7 H -0.0316 0.6919 0.2533 0.057 Uiso 1 1 calc R . . C8 C -0.0423(4) 0.5851(5) 0.1767(5) 0.0458(19) Uani 1 1 d . . . H8 H -0.1023 0.5841 0.1501 0.055 Uiso 1 1 calc R . . C9 C 0.1457(4) 0.6765(4) 0.3094(4) 0.0353(15) Uani 1 1 d . . . C10 C 0.1672(4) 0.7608(4) 0.2833(4) 0.0317(14) Uani 1 1 d . . . C11 C 0.2226(4) 0.8165(5) 0.3382(4) 0.0378(16) Uani 1 1 d . . . H11 H 0.2383 0.8748 0.3214 0.045 Uiso 1 1 calc R . . C12 C 0.2550(5) 0.7895(5) 0.4154(4) 0.0484(19) Uani 1 1 d . . . H12 H 0.2917 0.8292 0.452 0.058 Uiso 1 1 calc R . . C13 C 0.2346(5) 0.7061(5) 0.4395(4) 0.053(2) Uani 1 1 d . . . H13 H 0.2594 0.6873 0.4928 0.064 Uiso 1 1 calc R . . C14 C 0.1784(6) 0.6462(5) 0.3890(4) 0.051(2) Uani 1 1 d . . . C15 C 0.1507(8) 0.5564(5) 0.4161(5) 0.082(4) Uani 1 1 d . . . H15 H 0.1443 0.5132 0.3699 0.098 Uiso 1 1 calc R . . C16A C 0.0635(8) 0.5648(7) 0.4360(6) 0.110(5) Uani 1 1 d . . . H16A H 0.0649 0.6144 0.4747 0.165 Uiso 1 1 calc R . . H16B H 0.0488 0.5073 0.4592 0.165 Uiso 1 1 calc R . . H16C H 0.0194 0.5783 0.3872 0.165 Uiso 1 1 calc R . . C17 C 0.2170(10) 0.5146(6) 0.4859(5) 0.129(6) Uani 1 1 d . . . H17A H 0.272 0.5031 0.4695 0.193 Uiso 1 1 calc R . . H17B H 0.194 0.4569 0.5018 0.193 Uiso 1 1 calc R . . H17C H 0.2275 0.557 0.5314 0.193 Uiso 1 1 calc R . . C18 C 0.1352(4) 0.7928(4) 0.1974(4) 0.0348(15) Uani 1 1 d . . . H18 H 0.0924 0.7466 0.1687 0.042 Uiso 1 1 calc R . . C19 C 0.2120(4) 0.7968(5) 0.1558(4) 0.0412(16) Uani 1 1 d . . . H19A H 0.2525 0.8451 0.1802 0.062 Uiso 1 1 calc R . . H19B H 0.1901 0.81 0.0987 0.062 Uiso 1 1 calc R . . H19C H 0.2425 0.7379 0.1618 0.062 Uiso 1 1 calc R . . C20 C 0.0886(4) 0.8852(5) 0.1924(4) 0.0455(18) Uani 1 1 d . . . H20A H 0.0378 0.8802 0.2168 0.068 Uiso 1 1 calc R . . H20B H 0.0692 0.9033 0.1362 0.068 Uiso 1 1 calc R . . H20C H 0.1289 0.9313 0.2213 0.068 Uiso 1 1 calc R . . C21 C -0.0610(4) 0.4316(5) 0.0550(5) 0.0433(18) Uani 1 1 d . . . H21 H -0.1142 0.4627 0.0549 0.052 Uiso 1 1 calc R . . C22 C -0.0574(4) 0.3627(5) 0.0015(4) 0.0457(19) Uani 1 1 d . . . H22 H -0.109 0.3463 -0.0366 0.055 Uiso 1 1 calc R . . C23 C 0.0196(4) 0.3163(4) 0.0016(4) 0.0437(17) Uani 1 1 d . . . H23 H 0.0222 0.2682 -0.0351 0.052 Uiso 1 1 calc R . . C24 C 0.0930(4) 0.3445(4) 0.0586(4) 0.0305(14) Uani 1 1 d . . . C25 C 0.2407(3) 0.3240(4) 0.1345(3) 0.0230(12) Uani 1 1 d . A . C26 C 0.2838(4) 0.2159(4) 0.0553(3) 0.0308(14) Uani 1 1 d . . . H26 H 0.32 0.1729 0.0366 0.037 Uiso 1 1 calc R . . C27 C 0.2024(4) 0.2382(4) 0.0195(4) 0.0323(14) Uani 1 1 d . . . H27 H 0.1692 0.2145 -0.0296 0.039 Uiso 1 1 calc R . . C28 C 0.3878(4) 0.2573(3) 0.1837(3) 0.0220(12) Uani 1 1 d . . . C29 C 0.4609(4) 0.3011(4) 0.1697(3) 0.0272(13) Uani 1 1 d . . . C30 C 0.5397(4) 0.2877(4) 0.2267(4) 0.0332(14) Uani 1 1 d . . . H30 H 0.5917 0.3164 0.2194 0.04 Uiso 1 1 calc R . . C31 C 0.5422(4) 0.2337(4) 0.2924(4) 0.0318(14) Uani 1 1 d . . . H31 H 0.5956 0.2266 0.3309 0.038 Uiso 1 1 calc R . . C32 C 0.4683(4) 0.1896(4) 0.3034(3) 0.0301(14) Uani 1 1 d . . . H32 H 0.4718 0.1516 0.349 0.036 Uiso 1 1 calc R . . C33 C 0.3886(4) 0.1996(4) 0.2492(3) 0.0280(13) Uani 1 1 d . . . C34 C 0.3078(4) 0.1499(5) 0.2606(4) 0.0438(18) Uani 1 1 d . . . H34 H 0.256 0.1882 0.2362 0.053 Uiso 1 1 calc R . . C35 C 0.3058(5) 0.1340(5) 0.3479(5) 0.056(2) Uani 1 1 d . . . H35A H 0.3541 0.0937 0.3727 0.084 Uiso 1 1 calc R . . H35B H 0.2501 0.1056 0.3512 0.084 Uiso 1 1 calc R . . H35C H 0.3118 0.1927 0.3763 0.084 Uiso 1 1 calc R . . C36 C 0.2992(6) 0.0592(5) 0.2153(5) 0.070(3) Uani 1 1 d . . . H36A H 0.295 0.0709 0.1582 0.105 Uiso 1 1 calc R . . H36B H 0.2466 0.0272 0.2223 0.105 Uiso 1 1 calc R . . H36C H 0.3507 0.0212 0.2363 0.105 Uiso 1 1 calc R . . C37 C 0.4585(4) 0.3593(4) 0.0965(3) 0.0317(14) Uani 1 1 d . . . H37 H 0.3959 0.3726 0.0713 0.038 Uiso 1 1 calc R . . C38 C 0.4974(5) 0.3065(5) 0.0361(4) 0.0467(18) Uani 1 1 d . . . H38A H 0.5559 0.2848 0.0621 0.07 Uiso 1 1 calc R . . H38B H 0.5014 0.3466 -0.0088 0.07 Uiso 1 1 calc R . . H38C H 0.4599 0.2541 0.0162 0.07 Uiso 1 1 calc R . . C39 C 0.5054(5) 0.4498(5) 0.1169(4) 0.0477(18) Uani 1 1 d . . . H39A H 0.4874 0.4774 0.1629 0.072 Uiso 1 1 calc R . . H39B H 0.4903 0.491 0.0707 0.072 Uiso 1 1 calc R . . H39C H 0.5686 0.4395 0.1302 0.072 Uiso 1 1 calc R . . Br1 Br 0.26676(4) 0.53996(4) 0.09635(4) 0.03691(19) Uani 1 1 d . A . Br2 Br 0.15079(5) 0.33707(4) 0.30024(4) 0.0417(2) Uani 1 1 d . A . N1 N 0.0914(3) 0.4105(3) 0.1107(3) 0.0260(11) Uani 1 1 d . A . N2 N 0.0230(3) 0.5249(3) 0.1649(3) 0.0350(13) Uani 1 1 d . . . N3 N 0.0835(3) 0.6210(3) 0.2537(3) 0.0371(13) Uani 1 1 d . . . N4 N 0.1754(3) 0.3031(3) 0.0680(3) 0.0261(11) Uani 1 1 d . . . N5 N 0.3062(3) 0.2678(3) 0.1259(3) 0.0223(10) Uani 1 1 d . . . O1 O 0.3141(3) 0.4801(3) 0.2934(2) 0.0302(9) Uani 1 1 d . A . V1 V 0.20312(6) 0.44408(6) 0.19903(6) 0.0239(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 C1A 0.042(4) 0.031(4) 0.045(4) 0.006(3) -0.011(3) 0.006(3) C2A 0.058(9) 0.049(6) 0.063(11) -0.009(6) -0.023(7) 0.004(6) C3A 0.071(6) 0.045(5) 0.081(6) 0.010(4) -0.020(5) -0.025(4) C1B 0.042(4) 0.031(4) 0.045(4) 0.006(3) -0.011(3) 0.006(3) C2B 0.058(9) 0.049(6) 0.063(11) -0.009(6) -0.023(7) 0.004(6) C3B 0.071(6) 0.045(5) 0.081(6) 0.010(4) -0.020(5) -0.025(4) C4 0.045(4) 0.017(3) 0.045(4) 0.003(3) 0.002(3) -0.002(3) C5 0.020(3) 0.027(3) 0.056(4) 0.024(3) 0.007(3) -0.001(3) C6 0.039(4) 0.016(3) 0.041(4) 0.009(3) 0.020(3) -0.003(3) C7 0.040(4) 0.029(4) 0.086(6) 0.012(4) 0.041(4) 0.002(3) C8 0.028(4) 0.034(4) 0.083(6) 0.024(4) 0.030(4) 0.007(3) C9 0.039(4) 0.022(3) 0.053(4) 0.004(3) 0.029(3) 0.009(3) C10 0.027(3) 0.030(3) 0.041(4) 0.007(3) 0.014(3) 0.009(3) C11 0.031(4) 0.042(4) 0.044(4) 0.006(3) 0.017(3) 0.003(3) C12 0.061(5) 0.049(5) 0.039(4) -0.006(3) 0.020(4) 0.017(4) C13 0.081(6) 0.053(5) 0.033(4) -0.004(4) 0.027(4) 0.021(4) C14 0.087(6) 0.031(4) 0.046(4) 0.012(3) 0.038(4) 0.024(4) C15 0.193(12) 0.023(4) 0.044(5) 0.001(3) 0.060(6) -0.002(5) C16A 0.171(12) 0.101(8) 0.073(7) -0.018(6) 0.060(7) -0.103(8) C17 0.306(19) 0.037(5) 0.057(6) 0.022(4) 0.069(9) 0.062(8) C18 0.034(4) 0.023(3) 0.047(4) 0.010(3) 0.008(3) -0.003(3) C19 0.047(4) 0.039(4) 0.041(4) 0.011(3) 0.016(3) 0.005(3) C20 0.034(4) 0.041(4) 0.064(5) 0.018(3) 0.015(3) 0.010(3) C21 0.019(3) 0.032(4) 0.077(5) 0.025(4) 0.005(3) 0.001(3) C22 0.020(3) 0.039(4) 0.065(5) 0.022(4) -0.018(3) -0.009(3) C23 0.041(4) 0.027(3) 0.053(4) 0.008(3) -0.011(3) -0.006(3) C24 0.024(3) 0.021(3) 0.040(4) 0.011(3) -0.007(3) -0.005(2) C25 0.019(3) 0.018(3) 0.030(3) 0.002(2) -0.001(2) -0.004(2) C26 0.039(4) 0.023(3) 0.030(3) -0.007(2) 0.007(3) -0.005(3) C27 0.033(4) 0.025(3) 0.033(3) -0.003(3) -0.004(3) -0.010(3) C28 0.028(3) 0.014(3) 0.024(3) -0.002(2) 0.004(2) 0.004(2) C29 0.030(3) 0.020(3) 0.032(3) 0.000(2) 0.009(3) 0.001(2) C30 0.026(3) 0.033(3) 0.042(4) -0.001(3) 0.008(3) -0.004(3) C31 0.022(3) 0.035(3) 0.034(3) 0.002(3) -0.004(3) 0.005(3) C32 0.034(4) 0.028(3) 0.028(3) 0.005(2) 0.006(3) 0.009(3) C33 0.027(3) 0.019(3) 0.038(3) 0.002(2) 0.008(3) 0.001(2) C34 0.023(3) 0.047(4) 0.059(5) 0.027(3) 0.003(3) 0.002(3) C35 0.040(4) 0.056(5) 0.078(6) 0.036(4) 0.028(4) 0.018(4) C36 0.079(6) 0.054(5) 0.067(5) 0.020(4) -0.006(5) -0.038(5) C37 0.032(3) 0.036(4) 0.026(3) 0.006(3) 0.004(3) -0.007(3) C38 0.062(5) 0.049(4) 0.030(4) 0.005(3) 0.013(3) -0.004(4) C39 0.059(5) 0.039(4) 0.043(4) 0.009(3) 0.009(4) -0.013(4) Br1 0.0338(4) 0.0326(4) 0.0421(4) 0.0098(3) 0.0035(3) 0.0000(3) Br2 0.0452(4) 0.0276(3) 0.0550(4) 0.0056(3) 0.0170(3) -0.0025(3) N1 0.017(2) 0.019(2) 0.039(3) 0.011(2) 0.000(2) -0.0026(19) N2 0.028(3) 0.018(3) 0.063(4) 0.016(2) 0.019(3) 0.002(2) N3 0.034(3) 0.025(3) 0.062(4) 0.014(3) 0.032(3) 0.006(2) N4 0.024(3) 0.020(2) 0.028(3) -0.001(2) -0.007(2) -0.005(2) N5 0.023(3) 0.016(2) 0.026(2) -0.0018(18) 0.002(2) -0.0034(19) O1 0.033(2) 0.023(2) 0.032(2) 0.0054(17) 0.0010(18) -0.0021(17) V1 0.0225(5) 0.0170(5) 0.0307(5) 0.0044(4) 0.0028(4) 0.0003(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 1.448(7) . ? C1A C2A 1.495(18) . ? C1A H1A1 0.99 . ? C1A H1A2 0.99 . ? C2A C3A 1.497(19) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C3A C4 1.494(10) . ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? C4 O1 1.453(7) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 N1 1.347(7) . ? C5 C21 1.383(9) . ? C5 N2 1.396(8) . ? C6 N3 1.355(8) . ? C6 N2 1.383(8) . ? C6 V1 2.227(6) . ? C7 C8 1.314(10) . ? C7 N3 1.378(8) . ? C7 H7 0.95 . ? C8 N2 1.399(8) . ? C8 H8 0.95 . ? C9 C10 1.378(8) . ? C9 C14 1.418(9) . ? C9 N3 1.452(8) . ? C10 C11 1.394(9) . ? C10 C18 1.518(8) . ? C11 C12 1.365(9) . ? C11 H11 0.95 . ? C12 C13 1.349(10) . ? C12 H12 0.95 . ? C13 C14 1.397(11) . ? C13 H13 0.95 . ? C14 C15 1.489(10) . ? C15 C16A 1.487(15) . ? C15 C17 1.528(14) . ? C15 H15 1 . ? C16A H16A 0.98 . ? C16A H16B 0.98 . ? C16A H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.531(8) . ? C18 C20 1.532(9) . ? C18 H18 1 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.372(10) . ? C21 H21 0.95 . ? C22 C23 1.384(10) . ? C22 H22 0.95 . ? C23 C24 1.398(8) . ? C23 H23 0.95 . ? C24 N1 1.319(8) . ? C24 N4 1.403(7) . ? C25 N5 1.350(7) . ? C25 N4 1.386(7) . ? C25 V1 2.224(6) . ? C26 C27 1.329(8) . ? C26 N5 1.404(7) . ? C26 H26 0.95 . ? C27 N4 1.389(8) . ? C27 H27 0.95 . ? C28 C29 1.380(8) . ? C28 C33 1.401(8) . ? C28 N5 1.443(7) . ? C29 C30 1.408(8) . ? C29 C37 1.510(8) . ? C30 C31 1.368(8) . ? C30 H30 0.95 . ? C31 C32 1.376(8) . ? C31 H31 0.95 . ? C32 C33 1.389(8) . ? C32 H32 0.95 . ? C33 C34 1.512(8) . ? C34 C35 1.520(9) . ? C34 C36 1.528(11) . ? C34 H34 1 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 C39 1.517(9) . ? C37 C38 1.523(9) . ? C37 H37 1 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? Br1 V1 2.6142(11) . ? Br2 V1 2.5997(11) . ? N1 V1 2.103(5) . ? O1 V1 2.162(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 O1 C1A C2A 106.3(12) . . ? O1 C1A H1A1 110.5 . . ? C2A C1A H1A1 110.5 . . ? O1 C1A H1A2 110.5 . . ? C2A C1A H1A2 110.5 . . ? H1A1 C1A H1A2 108.7 . . ? C1A C2A C3A 104.8(14) . . ? C1A C2A H2A1 110.8 . . ? C3A C2A H2A1 110.8 . . ? C1A C2A H2A2 110.8 . . ? C3A C2A H2A2 110.8 . . ? H2A1 C2A H2A2 108.9 . . ? C4 C3A C2A 107.4(11) . . ? C4 C3A H3A1 110.2 . . ? C2A C3A H3A1 110.2 . . ? C4 C3A H3A2 110.2 . . ? C2A C3A H3A2 110.2 . . ? H3A1 C3A H3A2 108.5 . . ? H2B1 C2B H2B2 109 . . ? O1 C4 C3A 106.4(5) . . ? O1 C4 H4A 110.4 . . ? C3A C4 H4A 110.4 . . ? O1 C4 H4B 110.4 . . ? C3A C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? N1 C5 C21 122.2(6) . . ? N1 C5 N2 113.4(5) . . ? C21 C5 N2 124.3(6) . . ? N3 C6 N2 102.3(5) . . ? N3 C6 V1 147.4(5) . . ? N2 C6 V1 110.2(4) . . ? C8 C7 N3 108.2(6) . . ? C8 C7 H7 125.9 . . ? N3 C7 H7 125.9 . . ? C7 C8 N2 106.1(6) . . ? C7 C8 H8 127 . . ? N2 C8 H8 127 . . ? C10 C9 C14 122.0(7) . . ? C10 C9 N3 117.7(6) . . ? C14 C9 N3 120.2(6) . . ? C9 C10 C11 117.8(6) . . ? C9 C10 C18 122.5(6) . . ? C11 C10 C18 119.7(5) . . ? C12 C11 C10 121.7(7) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C11 119.7(7) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 122.5(7) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C13 C14 C9 116.2(6) . . ? C13 C14 C15 123.3(7) . . ? C9 C14 C15 120.5(8) . . ? C16A C15 C14 110.2(7) . . ? C16A C15 C17 110.8(8) . . ? C14 C15 C17 113.7(10) . . ? C16A C15 H15 107.3 . . ? C14 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C15 C16A H16A 109.5 . . ? C15 C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15 C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 C19 109.7(5) . . ? C10 C18 C20 112.1(5) . . ? C19 C18 C20 110.8(5) . . ? C10 C18 H18 108 . . ? C19 C18 H18 108 . . ? C20 C18 H18 108 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C5 117.6(6) . . ? C22 C21 H21 121.2 . . ? C5 C21 H21 121.2 . . ? C21 C22 C23 121.7(6) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C24 116.1(7) . . ? C22 C23 H23 121.9 . . ? C24 C23 H23 121.9 . . ? N1 C24 C23 123.5(6) . . ? N1 C24 N4 113.2(5) . . ? C23 C24 N4 123.3(6) . . ? N5 C25 N4 102.6(5) . . ? N5 C25 V1 145.9(4) . . ? N4 C25 V1 110.6(4) . . ? C27 C26 N5 107.2(5) . . ? C27 C26 H26 126.4 . . ? N5 C26 H26 126.4 . . ? C26 C27 N4 106.4(5) . . ? C26 C27 H27 126.8 . . ? N4 C27 H27 126.8 . . ? C29 C28 C33 124.0(5) . . ? C29 C28 N5 118.5(5) . . ? C33 C28 N5 117.5(5) . . ? C28 C29 C30 116.8(5) . . ? C28 C29 C37 122.5(5) . . ? C30 C29 C37 120.7(5) . . ? C31 C30 C29 120.6(6) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 120.8(6) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C31 C32 C33 121.4(5) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C32 C33 C28 116.3(5) . . ? C32 C33 C34 121.3(5) . . ? C28 C33 C34 122.3(5) . . ? C33 C34 C35 113.7(6) . . ? C33 C34 C36 109.5(6) . . ? C35 C34 C36 110.4(6) . . ? C33 C34 H34 107.7 . . ? C35 C34 H34 107.7 . . ? C36 C34 H34 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C29 C37 C39 112.4(5) . . ? C29 C37 C38 109.7(5) . . ? C39 C37 C38 110.6(5) . . ? C29 C37 H37 108 . . ? C39 C37 H37 108 . . ? C38 C37 H37 108 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C24 N1 C5 118.9(5) . . ? C24 N1 V1 121.2(4) . . ? C5 N1 V1 119.8(4) . . ? C6 N2 C5 120.8(5) . . ? C6 N2 C8 111.4(6) . . ? C5 N2 C8 127.7(6) . . ? C6 N3 C7 112.1(6) . . ? C6 N3 C9 125.9(5) . . ? C7 N3 C9 122.0(5) . . ? C25 N4 C27 111.9(5) . . ? C25 N4 C24 119.6(5) . . ? C27 N4 C24 128.5(5) . . ? C25 N5 C26 111.8(5) . . ? C25 N5 C28 124.8(4) . . ? C26 N5 C28 123.2(5) . . ? C1A O1 C4 109.3(4) . . ? C1A O1 V1 123.8(3) . . ? C4 O1 V1 124.6(3) . . ? N1 V1 O1 177.41(18) . . ? N1 V1 C25 74.28(19) . . ? O1 V1 C25 107.79(18) . . ? N1 V1 C6 75.1(2) . . ? O1 V1 C6 102.8(2) . . ? C25 V1 C6 149.4(2) . . ? N1 V1 Br2 90.13(12) . . ? O1 V1 Br2 88.31(11) . . ? C25 V1 Br2 90.74(14) . . ? C6 V1 Br2 89.83(14) . . ? N1 V1 Br1 91.37(12) . . ? O1 V1 Br1 90.38(11) . . ? C25 V1 Br1 84.67(14) . . ? C6 V1 Br1 95.57(14) . . ? Br2 V1 Br1 174.60(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 O1 C1A C2A C3A -24(4) . . . . ? C1A C2A C3A C4 18(4) . . . . ? C2A C3A C4 O1 -5(2) . . . . ? N3 C7 C8 N2 0.8(7) . . . . ? C14 C9 C10 C11 -0.2(9) . . . . ? N3 C9 C10 C11 176.1(5) . . . . ? C14 C9 C10 C18 177.8(6) . . . . ? N3 C9 C10 C18 -5.9(8) . . . . ? C9 C10 C11 C12 0.0(9) . . . . ? C18 C10 C11 C12 -178.1(6) . . . . ? C10 C11 C12 C13 1.3(10) . . . . ? C11 C12 C13 C14 -2.4(11) . . . . ? C12 C13 C14 C9 2.1(10) . . . . ? C12 C13 C14 C15 -176.0(7) . . . . ? C10 C9 C14 C13 -0.7(9) . . . . ? N3 C9 C14 C13 -177.0(6) . . . . ? C10 C9 C14 C15 177.3(7) . . . . ? N3 C9 C14 C15 1.1(10) . . . . ? C13 C14 C15 C16A 97.6(10) . . . . ? C9 C14 C15 C16A -80.4(9) . . . . ? C13 C14 C15 C17 -27.5(11) . . . . ? C9 C14 C15 C17 154.6(7) . . . . ? C9 C10 C18 C19 -110.6(6) . . . . ? C11 C10 C18 C19 67.4(7) . . . . ? C9 C10 C18 C20 125.9(6) . . . . ? C11 C10 C18 C20 -56.2(7) . . . . ? N1 C5 C21 C22 -0.6(9) . . . . ? N2 C5 C21 C22 177.5(6) . . . . ? C5 C21 C22 C23 0.6(10) . . . . ? C21 C22 C23 C24 -0.5(10) . . . . ? C22 C23 C24 N1 0.5(9) . . . . ? C22 C23 C24 N4 178.3(6) . . . . ? N5 C26 C27 N4 -0.1(6) . . . . ? C33 C28 C29 C30 -1.7(8) . . . . ? N5 C28 C29 C30 -178.7(5) . . . . ? C33 C28 C29 C37 177.1(5) . . . . ? N5 C28 C29 C37 0.1(8) . . . . ? C28 C29 C30 C31 -0.2(9) . . . . ? C37 C29 C30 C31 -179.0(6) . . . . ? C29 C30 C31 C32 1.6(9) . . . . ? C30 C31 C32 C33 -1.2(9) . . . . ? C31 C32 C33 C28 -0.6(8) . . . . ? C31 C32 C33 C34 179.0(6) . . . . ? C29 C28 C33 C32 2.1(8) . . . . ? N5 C28 C33 C32 179.1(5) . . . . ? C29 C28 C33 C34 -177.5(6) . . . . ? N5 C28 C33 C34 -0.5(8) . . . . ? C32 C33 C34 C35 31.2(9) . . . . ? C28 C33 C34 C35 -149.3(6) . . . . ? C32 C33 C34 C36 -92.8(7) . . . . ? C28 C33 C34 C36 86.7(7) . . . . ? C28 C29 C37 C39 133.8(6) . . . . ? C30 C29 C37 C39 -47.5(8) . . . . ? C28 C29 C37 C38 -102.7(7) . . . . ? C30 C29 C37 C38 76.0(7) . . . . ? C23 C24 N1 C5 -0.5(8) . . . . ? N4 C24 N1 C5 -178.5(5) . . . . ? C23 C24 N1 V1 176.5(4) . . . . ? N4 C24 N1 V1 -1.4(6) . . . . ? C21 C5 N1 C24 0.6(8) . . . . ? N2 C5 N1 C24 -177.7(5) . . . . ? C21 C5 N1 V1 -176.5(4) . . . . ? N2 C5 N1 V1 5.2(6) . . . . ? N3 C6 N2 C5 175.8(5) . . . . ? V1 C6 N2 C5 -7.6(6) . . . . ? N3 C6 N2 C8 -0.3(6) . . . . ? V1 C6 N2 C8 176.2(4) . . . . ? N1 C5 N2 C6 2.2(7) . . . . ? C21 C5 N2 C6 -176.0(5) . . . . ? N1 C5 N2 C8 177.7(5) . . . . ? C21 C5 N2 C8 -0.6(9) . . . . ? C7 C8 N2 C6 -0.3(7) . . . . ? C7 C8 N2 C5 -176.1(6) . . . . ? N2 C6 N3 C7 0.8(6) . . . . ? V1 C6 N3 C7 -173.1(6) . . . . ? N2 C6 N3 C9 -175.2(5) . . . . ? V1 C6 N3 C9 10.8(11) . . . . ? C8 C7 N3 C6 -1.1(7) . . . . ? C8 C7 N3 C9 175.2(5) . . . . ? C10 C9 N3 C6 104.6(7) . . . . ? C14 C9 N3 C6 -79.0(8) . . . . ? C10 C9 N3 C7 -71.1(7) . . . . ? C14 C9 N3 C7 105.3(7) . . . . ? N5 C25 N4 C27 -2.0(6) . . . . ? V1 C25 N4 C27 170.4(4) . . . . ? N5 C25 N4 C24 175.8(5) . . . . ? V1 C25 N4 C24 -11.8(6) . . . . ? C26 C27 N4 C25 1.4(7) . . . . ? C26 C27 N4 C24 -176.3(5) . . . . ? N1 C24 N4 C25 9.2(7) . . . . ? C23 C24 N4 C25 -168.7(5) . . . . ? N1 C24 N4 C27 -173.3(5) . . . . ? C23 C24 N4 C27 8.7(9) . . . . ? N4 C25 N5 C26 1.9(6) . . . . ? V1 C25 N5 C26 -165.3(6) . . . . ? N4 C25 N5 C28 -174.6(5) . . . . ? V1 C25 N5 C28 18.2(10) . . . . ? C27 C26 N5 C25 -1.2(7) . . . . ? C27 C26 N5 C28 175.4(5) . . . . ? C29 C28 N5 C25 -101.7(6) . . . . ? C33 C28 N5 C25 81.1(7) . . . . ? C29 C28 N5 C26 82.1(7) . . . . ? C33 C28 N5 C26 -95.1(6) . . . . ? C2A C1A O1 C4 22(2) . . . . ? C2A C1A O1 V1 -174(2) . . . . ? C3A C4 O1 C1A -11.0(8) . . . . ? C3A C4 O1 V1 -174.5(5) . . . . ? C24 N1 V1 C25 -3.6(4) . . . . ? C5 N1 V1 C25 173.5(4) . . . . ? C24 N1 V1 C6 175.9(5) . . . . ? C5 N1 V1 C6 -7.0(4) . . . . ? C24 N1 V1 Br2 -94.3(4) . . . . ? C5 N1 V1 Br2 82.7(4) . . . . ? C24 N1 V1 Br1 80.5(4) . . . . ? C5 N1 V1 Br1 -102.5(4) . . . . ? C1A O1 V1 C25 -43.7(5) . . . . ? C4 O1 V1 C25 117.5(5) . . . . ? C1A O1 V1 C6 136.0(5) . . . . ? C4 O1 V1 C6 -62.8(5) . . . . ? C1A O1 V1 Br2 46.6(4) . . . . ? C4 O1 V1 Br2 -152.2(4) . . . . ? C1A O1 V1 Br1 -128.2(4) . . . . ? C4 O1 V1 Br1 33.0(4) . . . . ? N5 C25 V1 N1 174.3(7) . . . . ? N4 C25 V1 N1 7.7(3) . . . . ? N5 C25 V1 O1 -7.3(7) . . . . ? N4 C25 V1 O1 -173.9(3) . . . . ? N5 C25 V1 C6 173.4(6) . . . . ? N4 C25 V1 C6 6.7(6) . . . . ? N5 C25 V1 Br2 -95.7(7) . . . . ? N4 C25 V1 Br2 97.6(4) . . . . ? N5 C25 V1 Br1 81.4(7) . . . . ? N4 C25 V1 Br1 -85.2(4) . . . . ? N3 C6 V1 N1 -179.0(8) . . . . ? N2 C6 V1 N1 7.3(4) . . . . ? N3 C6 V1 O1 2.6(8) . . . . ? N2 C6 V1 O1 -171.1(4) . . . . ? N3 C6 V1 C25 -178.0(6) . . . . ? N2 C6 V1 C25 8.3(6) . . . . ? N3 C6 V1 Br2 90.8(7) . . . . ? N2 C6 V1 Br2 -82.9(4) . . . . ? N3 C6 V1 Br1 -89.1(7) . . . . ? N2 C6 V1 Br1 97.2(4) . . . . ? #==END data_(C-N-C)VCl3 _database_code_depnum_ccdc_archive 'CCDC 282398' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Cl3 N5 V, C4 H8 O' _chemical_formula_sum 'C39 H49 Cl3 N5 O V' _chemical_formula_weight 761.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8934(12) _cell_length_b 18.7259(17) _cell_length_c 18.381(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.051(8) _cell_angle_gamma 90.00 _cell_volume 3740.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6270 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8196 _exptl_absorpt_correction_T_max 0.9796 _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 19040 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.1185 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.62 _reflns_number_total 8522 _reflns_number_gt 4813 _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-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 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^)+(0.0497P)^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 8522 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0974(3) 0.30976(13) 0.56784(16) 0.0191(7) Uani 1 1 d . . . C2 C 0.2325(3) 0.24749(13) 0.49334(15) 0.0187(7) Uani 1 1 d . . . C3 C 0.3460(3) 0.18752(14) 0.58096(15) 0.0220(7) Uani 1 1 d . . . H3 H 0.4073 0.1570 0.6033 0.026 Uiso 1 1 calc R . . C4 C 0.2638(3) 0.22488(14) 0.61533(16) 0.0223(7) Uani 1 1 d . . . H4 H 0.2546 0.2263 0.6663 0.027 Uiso 1 1 calc R . . C5 C 0.3954(3) 0.16600(14) 0.45247(15) 0.0206(7) Uani 1 1 d . . . C6 C 0.5036(3) 0.19747(14) 0.43209(16) 0.0251(7) Uani 1 1 d . . . C7 C 0.5716(3) 0.15959(16) 0.38411(18) 0.0357(9) Uani 1 1 d . . . H7 H 0.6474 0.1787 0.3703 0.043 Uiso 1 1 calc R . . C8 C 0.5314(4) 0.09491(18) 0.35621(19) 0.0429(10) Uani 1 1 d . . . H8 H 0.5786 0.0703 0.3226 0.051 Uiso 1 1 calc R . . C9 C 0.4233(3) 0.06554(16) 0.37660(19) 0.0377(9) Uani 1 1 d . . . H9 H 0.3963 0.0210 0.3566 0.045 Uiso 1 1 calc R . . C10 C 0.3529(3) 0.09996(15) 0.42592(16) 0.0255(7) Uani 1 1 d . . . C11 C 0.2369(3) 0.06554(15) 0.44792(18) 0.0307(8) Uani 1 1 d . . . H11 H 0.1963 0.0995 0.4807 0.037 Uiso 1 1 calc R . . C12 C 0.1477(4) 0.05130(16) 0.3821(2) 0.0489(11) Uani 1 1 d . . . H12A H 0.1346 0.0954 0.3539 0.073 Uiso 1 1 calc R . . H12B H 0.0690 0.0346 0.3985 0.073 Uiso 1 1 calc R . . H12C H 0.1821 0.0147 0.3513 0.073 Uiso 1 1 calc R . . C13 C 0.2651(3) -0.00362(16) 0.49110(19) 0.0423(10) Uani 1 1 d . . . H13A H 0.3053 -0.0379 0.4602 0.064 Uiso 1 1 calc R . . H13B H 0.1882 -0.0242 0.5062 0.064 Uiso 1 1 calc R . . H13C H 0.3197 0.0071 0.5344 0.064 Uiso 1 1 calc R . . C14 C 0.5503(3) 0.26869(15) 0.46182(18) 0.0304(8) Uani 1 1 d . . . H14 H 0.4842 0.2911 0.4892 0.037 Uiso 1 1 calc R . . C15 C 0.6628(3) 0.25688(17) 0.51475(19) 0.0435(10) Uani 1 1 d . . . H15A H 0.6411 0.2248 0.5540 0.065 Uiso 1 1 calc R . . H15B H 0.6905 0.3028 0.5356 0.065 Uiso 1 1 calc R . . H15C H 0.7291 0.2355 0.4887 0.065 Uiso 1 1 calc R . . C16 C 0.5809(3) 0.31920(17) 0.4007(2) 0.0468(10) Uani 1 1 d . . . H16A H 0.6526 0.3010 0.3771 0.070 Uiso 1 1 calc R . . H16B H 0.5996 0.3667 0.4210 0.070 Uiso 1 1 calc R . . H16C H 0.5104 0.3224 0.3647 0.070 Uiso 1 1 calc R . . C17 C 0.0468(3) 0.32769(14) 0.63158(16) 0.0244(7) Uani 1 1 d . . . H17 H 0.0743 0.3064 0.6767 0.029 Uiso 1 1 calc R . . C18 C -0.0461(3) 0.37808(14) 0.62726(17) 0.0265(8) Uani 1 1 d . . . H18 H -0.0841 0.3913 0.6702 0.032 Uiso 1 1 calc R . . C19 C -0.0848(3) 0.40952(14) 0.56173(17) 0.0248(7) Uani 1 1 d . . . H19 H -0.1473 0.4450 0.5588 0.030 Uiso 1 1 calc R . . C20 C -0.0293(3) 0.38746(14) 0.50097(16) 0.0197(7) Uani 1 1 d . . . C21 C 0.0033(3) 0.38395(13) 0.37402(16) 0.0174(7) Uani 1 1 d . . . C22 C -0.1342(3) 0.46779(14) 0.33309(17) 0.0230(7) Uani 1 1 d . . . H22 H -0.1812 0.4981 0.3004 0.028 Uiso 1 1 calc R . . C23 C -0.1408(3) 0.46445(14) 0.40540(17) 0.0255(8) Uani 1 1 d . . . H23 H -0.1927 0.4918 0.4341 0.031 Uiso 1 1 calc R . . C24 C -0.0266(3) 0.40051(13) 0.23929(16) 0.0198(7) Uani 1 1 d . . . C25 C 0.0738(3) 0.42864(13) 0.20626(16) 0.0199(7) Uani 1 1 d . . . C26 C 0.0823(3) 0.41254(14) 0.13292(16) 0.0228(7) Uani 1 1 d . . . H26 H 0.1495 0.4310 0.1085 0.027 Uiso 1 1 calc R . . C27 C -0.0040(3) 0.37056(14) 0.09453(16) 0.0243(7) Uani 1 1 d . . . H27 H 0.0036 0.3605 0.0444 0.029 Uiso 1 1 calc R . . C28 C -0.1010(3) 0.34353(14) 0.12980(16) 0.0237(7) Uani 1 1 d . . . H28 H -0.1603 0.3147 0.1032 0.028 Uiso 1 1 calc R . . C29 C -0.1153(3) 0.35702(13) 0.20308(16) 0.0203(7) Uani 1 1 d . . . C30 C -0.2240(3) 0.32657(14) 0.23947(17) 0.0255(7) Uani 1 1 d . . . H30 H -0.2110 0.3367 0.2929 0.031 Uiso 1 1 calc R . . C31 C -0.3445(3) 0.36278(16) 0.21166(19) 0.0365(9) Uani 1 1 d . . . H31A H -0.3420 0.4133 0.2255 0.055 Uiso 1 1 calc R . . H31B H -0.4137 0.3394 0.2333 0.055 Uiso 1 1 calc R . . H31C H -0.3547 0.3587 0.1584 0.055 Uiso 1 1 calc R . . C32 C -0.2309(3) 0.24529(14) 0.22998(17) 0.0324(8) Uani 1 1 d . . . H32A H -0.2408 0.2336 0.1779 0.049 Uiso 1 1 calc R . . H32B H -0.3013 0.2267 0.2545 0.049 Uiso 1 1 calc R . . H32C H -0.1549 0.2236 0.2515 0.049 Uiso 1 1 calc R . . C33 C 0.1708(3) 0.47639(14) 0.24394(16) 0.0225(7) Uani 1 1 d . . . H33 H 0.1535 0.4804 0.2965 0.027 Uiso 1 1 calc R . . C34 C 0.3000(3) 0.44530(14) 0.23988(17) 0.0269(8) Uani 1 1 d . . . H34A H 0.3026 0.3971 0.2606 0.040 Uiso 1 1 calc R . . H34B H 0.3598 0.4757 0.2676 0.040 Uiso 1 1 calc R . . H34C H 0.3204 0.4433 0.1888 0.040 Uiso 1 1 calc R . . C35 C 0.1643(3) 0.55173(13) 0.21025(17) 0.0275(8) Uani 1 1 d . . . H35A H 0.1859 0.5493 0.1595 0.041 Uiso 1 1 calc R . . H35B H 0.2222 0.5833 0.2379 0.041 Uiso 1 1 calc R . . H35C H 0.0806 0.5705 0.2119 0.041 Uiso 1 1 calc R . . C36 C 0.4668(3) 0.01599(18) 0.1120(2) 0.0500(11) Uani 1 1 d . . . H36A H 0.4112 0.0122 0.0672 0.060 Uiso 1 1 calc R . . H36B H 0.5117 -0.0297 0.1194 0.060 Uiso 1 1 calc R . . C37 C 0.5555(3) 0.07661(17) 0.1058(2) 0.0492(11) Uani 1 1 d . . . H37A H 0.5595 0.0916 0.0543 0.059 Uiso 1 1 calc R . . H37B H 0.6391 0.0632 0.1258 0.059 Uiso 1 1 calc R . . C38 C 0.5014(4) 0.13597(17) 0.1512(2) 0.0541(12) Uani 1 1 d . . . H38A H 0.5552 0.1460 0.1957 0.065 Uiso 1 1 calc R . . H38B H 0.4899 0.1805 0.1225 0.065 Uiso 1 1 calc R . . C39 C 0.3802(3) 0.10606(16) 0.1702(2) 0.0495(11) Uani 1 1 d . . . H39A H 0.3572 0.1249 0.2177 0.059 Uiso 1 1 calc R . . H39B H 0.3145 0.1184 0.1323 0.059 Uiso 1 1 calc R . . Cl1 Cl -0.02449(8) 0.21805(4) 0.39870(4) 0.0311(2) Uani 1 1 d . . . Cl2 Cl 0.27479(7) 0.40129(4) 0.43112(4) 0.0286(2) Uani 1 1 d . . . Cl3 Cl 0.22373(8) 0.25965(4) 0.30571(4) 0.0366(2) Uani 1 1 d . . . N1 N 0.0589(2) 0.33782(11) 0.50341(12) 0.0177(6) Uani 1 1 d . . . N2 N 0.1947(2) 0.26117(11) 0.56135(12) 0.0188(6) Uani 1 1 d . . . N3 N 0.3261(2) 0.20108(11) 0.50603(12) 0.0176(5) Uani 1 1 d . . . N4 N -0.0567(2) 0.41314(11) 0.42983(13) 0.0194(6) Uani 1 1 d . . . N5 N -0.0455(2) 0.41858(11) 0.31455(13) 0.0180(6) Uani 1 1 d . . . O1 O 0.3981(2) 0.03171(12) 0.17375(16) 0.0594(8) Uani 1 1 d . . . V1 V 0.13618(5) 0.30269(2) 0.40445(3) 0.01994(14) 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 0.0200(18) 0.0154(15) 0.0221(16) -0.0025(13) 0.0036(15) -0.0055(13) C2 0.0201(18) 0.0173(15) 0.0192(16) -0.0029(12) 0.0055(14) -0.0010(13) C3 0.0232(19) 0.0251(16) 0.0172(16) 0.0017(13) -0.0025(15) -0.0016(14) C4 0.0266(19) 0.0260(16) 0.0144(15) 0.0039(13) 0.0018(15) -0.0054(14) C5 0.0191(18) 0.0262(16) 0.0167(15) -0.0014(13) 0.0019(14) 0.0093(14) C6 0.026(2) 0.0264(17) 0.0229(17) 0.0049(14) 0.0044(15) 0.0078(15) C7 0.033(2) 0.037(2) 0.039(2) 0.0075(17) 0.0185(18) 0.0110(17) C8 0.048(3) 0.043(2) 0.040(2) -0.0045(18) 0.014(2) 0.0163(19) C9 0.043(3) 0.0316(19) 0.039(2) -0.0045(16) 0.010(2) 0.0073(17) C10 0.026(2) 0.0271(17) 0.0233(17) -0.0025(14) 0.0022(16) 0.0070(15) C11 0.028(2) 0.0271(17) 0.037(2) -0.0127(15) 0.0032(17) 0.0002(15) C12 0.053(3) 0.0327(19) 0.058(3) -0.0040(18) -0.014(2) -0.0054(18) C13 0.050(3) 0.038(2) 0.039(2) -0.0006(17) 0.007(2) -0.0048(18) C14 0.027(2) 0.0319(18) 0.0338(19) 0.0055(15) 0.0094(17) -0.0002(15) C15 0.033(2) 0.051(2) 0.046(2) -0.0002(18) -0.002(2) 0.0013(18) C16 0.049(3) 0.039(2) 0.054(3) 0.0105(18) 0.018(2) -0.0009(18) C17 0.030(2) 0.0248(16) 0.0194(16) 0.0003(14) 0.0074(16) -0.0027(15) C18 0.031(2) 0.0260(17) 0.0237(17) -0.0075(14) 0.0133(16) -0.0052(15) C19 0.0230(19) 0.0207(15) 0.0317(19) -0.0068(14) 0.0099(16) -0.0006(14) C20 0.0182(18) 0.0174(15) 0.0240(17) -0.0031(13) 0.0042(15) -0.0044(13) C21 0.0140(17) 0.0176(15) 0.0206(16) 0.0008(12) 0.0018(14) -0.0047(12) C22 0.0207(18) 0.0175(15) 0.0310(18) 0.0000(14) 0.0021(16) 0.0049(13) C23 0.0222(19) 0.0212(16) 0.0343(19) -0.0037(14) 0.0106(16) 0.0029(14) C24 0.0215(18) 0.0170(15) 0.0211(16) 0.0004(13) 0.0028(15) 0.0050(13) C25 0.0201(18) 0.0144(14) 0.0254(17) 0.0031(13) 0.0029(15) 0.0016(13) C26 0.0241(19) 0.0186(15) 0.0262(17) 0.0014(13) 0.0054(15) 0.0028(14) C27 0.030(2) 0.0237(16) 0.0197(16) 0.0004(13) 0.0027(16) 0.0036(15) C28 0.0227(19) 0.0211(16) 0.0265(17) -0.0010(13) -0.0034(16) 0.0002(14) C29 0.0214(19) 0.0160(15) 0.0237(17) 0.0027(13) 0.0036(15) 0.0030(13) C30 0.0245(19) 0.0262(16) 0.0260(17) 0.0006(14) 0.0023(16) -0.0056(14) C31 0.027(2) 0.0405(19) 0.042(2) 0.0043(17) 0.0061(18) -0.0013(16) C32 0.036(2) 0.0310(18) 0.0302(19) 0.0028(14) 0.0008(17) -0.0096(15) C33 0.0234(19) 0.0214(15) 0.0231(17) 0.0017(13) 0.0053(15) -0.0003(14) C34 0.0224(19) 0.0244(16) 0.0336(19) -0.0005(14) 0.0005(16) -0.0001(14) C35 0.032(2) 0.0223(16) 0.0280(18) -0.0032(13) 0.0046(17) -0.0022(14) C36 0.035(2) 0.052(2) 0.062(3) -0.013(2) 0.002(2) 0.001(2) C37 0.040(3) 0.042(2) 0.068(3) 0.016(2) 0.015(2) 0.0002(19) C38 0.064(3) 0.034(2) 0.066(3) -0.0012(19) 0.015(3) -0.021(2) C39 0.043(3) 0.029(2) 0.077(3) 0.0078(19) 0.008(2) 0.0074(18) Cl1 0.0315(5) 0.0265(4) 0.0346(5) -0.0006(3) -0.0025(4) -0.0056(4) Cl2 0.0255(5) 0.0297(4) 0.0311(4) 0.0012(3) 0.0041(4) -0.0052(3) Cl3 0.0490(6) 0.0385(5) 0.0237(4) 0.0006(4) 0.0116(4) 0.0080(4) N1 0.0164(14) 0.0182(12) 0.0191(13) -0.0034(10) 0.0047(12) -0.0008(11) N2 0.0227(15) 0.0179(12) 0.0162(13) -0.0016(10) 0.0040(12) 0.0004(11) N3 0.0186(14) 0.0172(12) 0.0172(13) -0.0015(10) 0.0031(11) -0.0013(11) N4 0.0191(15) 0.0165(12) 0.0234(14) -0.0022(11) 0.0062(12) 0.0009(11) N5 0.0162(15) 0.0158(12) 0.0224(14) -0.0016(11) 0.0040(12) 0.0017(10) O1 0.0440(18) 0.0416(15) 0.094(2) 0.0032(15) 0.0140(17) -0.0074(13) V1 0.0224(3) 0.0209(3) 0.0168(3) -0.0015(2) 0.0032(2) 0.0035(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 N1 1.336(3) . ? C1 C17 1.372(4) . ? C1 N2 1.408(3) . ? C2 N3 1.348(3) . ? C2 N2 1.368(3) . ? C2 V1 2.144(3) . ? C3 C4 1.330(4) . ? C3 N3 1.402(3) . ? C3 H3 0.9500 . ? C4 N2 1.381(3) . ? C4 H4 0.9500 . ? C5 C6 1.392(4) . ? C5 C10 1.396(4) . ? C5 N3 1.441(3) . ? C6 C7 1.387(4) . ? C6 C14 1.516(4) . ? C7 C8 1.375(4) . ? C7 H7 0.9500 . ? C8 C9 1.376(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C10 C11 1.500(4) . ? C11 C12 1.521(4) . ? C11 C13 1.539(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.523(4) . ? C14 C15 1.526(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C18 C19 1.380(4) . ? C18 H18 0.9500 . ? C19 C20 1.371(4) . ? C19 H19 0.9500 . ? C20 N1 1.335(3) . ? C20 N4 1.405(4) . ? C21 N5 1.348(3) . ? C21 N4 1.368(3) . ? C21 V1 2.147(3) . ? C22 C23 1.338(4) . ? C22 N5 1.395(3) . ? C22 H22 0.9500 . ? C23 N4 1.381(4) . ? C23 H23 0.9500 . ? C24 C25 1.392(4) . ? C24 C29 1.396(4) . ? C24 N5 1.453(3) . ? C25 C26 1.391(4) . ? C25 C33 1.514(4) . ? C26 C27 1.380(4) . ? C26 H26 0.9500 . ? C27 C28 1.375(4) . ? C27 H27 0.9500 . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 C30 1.512(4) . ? C30 C31 1.532(4) . ? C30 C32 1.533(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 1.530(4) . ? C33 C35 1.540(3) . ? 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 O1 1.434(4) . ? C36 C37 1.500(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.533(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.498(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O1 1.407(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? Cl1 V1 2.3580(9) . ? Cl2 V1 2.4134(9) . ? Cl3 V1 2.2578(9) . ? N1 V1 2.160(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C17 122.7(3) . . ? N1 C1 N2 111.7(2) . . ? C17 C1 N2 125.5(3) . . ? N3 C2 N2 103.6(2) . . ? N3 C2 V1 140.0(2) . . ? N2 C2 V1 116.36(19) . . ? C4 C3 N3 108.0(3) . . ? C4 C3 H3 126.0 . . ? N3 C3 H3 126.0 . . ? C3 C4 N2 105.6(3) . . ? C3 C4 H4 127.2 . . ? N2 C4 H4 127.2 . . ? C6 C5 C10 123.1(3) . . ? C6 C5 N3 119.0(2) . . ? C10 C5 N3 117.8(3) . . ? C7 C6 C5 117.1(3) . . ? C7 C6 C14 119.9(3) . . ? C5 C6 C14 123.0(3) . . ? C8 C7 C6 121.2(3) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 120.4(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C5 117.1(3) . . ? C9 C10 C11 119.5(3) . . ? C5 C10 C11 123.5(3) . . ? C10 C11 C12 111.3(3) . . ? C10 C11 C13 111.1(3) . . ? C12 C11 C13 110.9(3) . . ? C10 C11 H11 107.8 . . ? C12 C11 H11 107.8 . . ? C13 C11 H11 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 C16 111.5(3) . . ? C6 C14 C15 109.7(2) . . ? C16 C14 C15 110.6(3) . . ? C6 C14 H14 108.3 . . ? C16 C14 H14 108.3 . . ? C15 C14 H14 108.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C17 C18 117.1(3) . . ? C1 C17 H17 121.5 . . ? C18 C17 H17 121.5 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 117.2(3) . . ? C20 C19 H19 121.4 . . ? C18 C19 H19 121.4 . . ? N1 C20 C19 122.7(3) . . ? N1 C20 N4 112.0(2) . . ? C19 C20 N4 125.3(3) . . ? N5 C21 N4 103.5(2) . . ? N5 C21 V1 140.6(2) . . ? N4 C21 V1 115.9(2) . . ? C23 C22 N5 107.4(3) . . ? C23 C22 H22 126.3 . . ? N5 C22 H22 126.3 . . ? C22 C23 N4 106.0(3) . . ? C22 C23 H23 127.0 . . ? N4 C23 H23 127.0 . . ? C25 C24 C29 123.5(3) . . ? C25 C24 N5 119.7(3) . . ? C29 C24 N5 116.7(3) . . ? C26 C25 C24 116.7(3) . . ? C26 C25 C33 118.7(3) . . ? C24 C25 C33 124.7(3) . . ? C27 C26 C25 122.0(3) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C28 C27 C26 119.1(3) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 122.2(3) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C28 C29 C24 116.6(3) . . ? C28 C29 C30 120.3(3) . . ? C24 C29 C30 123.1(3) . . ? C29 C30 C31 111.4(2) . . ? C29 C30 C32 110.9(2) . . ? C31 C30 C32 111.6(3) . . ? C29 C30 H30 107.6 . . ? C31 C30 H30 107.6 . . ? C32 C30 H30 107.6 . . ? 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 . . ? C25 C33 C34 111.6(2) . . ? C25 C33 C35 110.2(2) . . ? C34 C33 C35 110.2(2) . . ? C25 C33 H33 108.2 . . ? C34 C33 H33 108.2 . . ? C35 C33 H33 108.2 . . ? 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 . . ? O1 C36 C37 106.3(3) . . ? O1 C36 H36A 110.5 . . ? C37 C36 H36A 110.5 . . ? O1 C36 H36B 110.5 . . ? C37 C36 H36B 110.5 . . ? H36A C36 H36B 108.7 . . ? C36 C37 C38 103.4(3) . . ? C36 C37 H37A 111.1 . . ? C38 C37 H37A 111.1 . . ? C36 C37 H37B 111.1 . . ? C38 C37 H37B 111.1 . . ? H37A C37 H37B 109.0 . . ? C39 C38 C37 103.6(3) . . ? C39 C38 H38A 111.0 . . ? C37 C38 H38A 111.0 . . ? C39 C38 H38B 111.0 . . ? C37 C38 H38B 111.0 . . ? H38A C38 H38B 109.0 . . ? O1 C39 C38 105.0(3) . . ? O1 C39 H39A 110.7 . . ? C38 C39 H39A 110.7 . . ? O1 C39 H39B 110.7 . . ? C38 C39 H39B 110.7 . . ? H39A C39 H39B 108.8 . . ? C20 N1 C1 118.9(2) . . ? C20 N1 V1 120.40(19) . . ? C1 N1 V1 120.66(18) . . ? C2 N2 C4 112.4(2) . . ? C2 N2 C1 118.4(2) . . ? C4 N2 C1 129.2(2) . . ? C2 N3 C3 110.4(2) . . ? C2 N3 C5 127.1(2) . . ? C3 N3 C5 122.4(2) . . ? C21 N4 C23 112.0(2) . . ? C21 N4 C20 118.7(2) . . ? C23 N4 C20 129.3(2) . . ? C21 N5 C22 111.1(2) . . ? C21 N5 C24 125.9(2) . . ? C22 N5 C24 122.3(2) . . ? C39 O1 C36 104.2(3) . . ? C2 V1 C21 145.57(11) . . ? C2 V1 N1 72.77(10) . . ? C21 V1 N1 73.01(10) . . ? C2 V1 Cl3 103.23(8) . . ? C21 V1 Cl3 111.03(8) . . ? N1 V1 Cl3 175.91(7) . . ? C2 V1 Cl1 91.82(8) . . ? C21 V1 Cl1 88.85(8) . . ? N1 V1 Cl1 84.85(6) . . ? Cl3 V1 Cl1 94.50(3) . . ? C2 V1 Cl2 87.06(8) . . ? C21 V1 Cl2 84.91(8) . . ? N1 V1 Cl2 82.61(6) . . ? Cl3 V1 Cl2 98.20(3) . . ? Cl1 V1 Cl2 167.17(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.643 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.081 #==END data_(C-N-C)TiCl3 _database_code_depnum_ccdc_archive 'CCDC 282399' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31.20 H39.20 Cl2.40 N4 O0.80 Ti0.80' _chemical_formula_sum 'C31.20 H39.20 Cl2.40 N4 O0.80 Ti0.80' _chemical_formula_weight 606.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8984(8) _cell_length_b 18.7455(11) _cell_length_c 18.6503(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.343(3) _cell_angle_gamma 90.00 _cell_volume 3803.7(5) _cell_formula_units_Z 5 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8607 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour 'light purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8948 _exptl_absorpt_correction_T_max 0.9906 _exptl_absorpt_process_details Sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30658 _diffrn_reflns_av_R_equivalents 0.1943 _diffrn_reflns_av_sigmaI/netI 0.1864 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8607 _reflns_number_gt 4392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski and Minor 1997)' _computing_data_reduction 'Denzo.a Scalepack (Otwinowski and Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0547P)^2^+4.2873P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8607 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1847 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.1964 _refine_ls_wR_factor_gt 0.1615 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4982(4) 0.1154(2) 0.6277(3) 0.0216(11) Uani 1 1 d . . . C2 C 0.6377(4) 0.0309(2) 0.6660(3) 0.0257(12) Uani 1 1 d . . . H2 H 0.6855 0.0009 0.6978 0.031 Uiso 1 1 calc R . . C3 C 0.6425(4) 0.0341(3) 0.5935(3) 0.0270(12) Uani 1 1 d . . . H3 H 0.6935 0.0067 0.5644 0.032 Uiso 1 1 calc R . . C4 C 0.2667(4) 0.2529(2) 0.5074(2) 0.0217(11) Uani 1 1 d . . . C5 C 0.1568(4) 0.3121(3) 0.4180(3) 0.0262(12) Uani 1 1 d . . . H5 H 0.0969 0.3427 0.3951 0.031 Uiso 1 1 calc R . . C6 C 0.2413(4) 0.2734(3) 0.3856(3) 0.0250(11) Uani 1 1 d . . . H6 H 0.2533 0.2711 0.3357 0.030 Uiso 1 1 calc R . . C7 C 0.4042(4) 0.1887(2) 0.4345(3) 0.0228(11) Uani 1 1 d . . . C8 C 0.5299(4) 0.1115(3) 0.5002(3) 0.0261(12) Uani 1 1 d . . . C9 C 0.5879(4) 0.0884(3) 0.4403(3) 0.0280(12) Uani 1 1 d . . . H9 H 0.6497 0.0526 0.4431 0.034 Uiso 1 1 calc R . . C10 C 0.5507(5) 0.1207(3) 0.3760(3) 0.0325(13) Uani 1 1 d . . . H10 H 0.5902 0.1081 0.3338 0.039 Uiso 1 1 calc R . . C11 C 0.4579(4) 0.1708(3) 0.3714(3) 0.0273(12) Uani 1 1 d . . . H11 H 0.4319 0.1920 0.3269 0.033 Uiso 1 1 calc R . . C12 C 0.6195(4) 0.1421(3) 0.7946(3) 0.0245(11) Uani 1 1 d . . . C13 C 0.5308(4) 0.0989(2) 0.7595(3) 0.0234(11) Uani 1 1 d . . . C14 C 0.6038(4) 0.1568(3) 0.8666(3) 0.0279(12) Uani 1 1 d . . . H14 H 0.6619 0.1867 0.8918 0.033 Uiso 1 1 calc R . . C15 C 0.5072(4) 0.1297(3) 0.9029(3) 0.0291(12) Uani 1 1 d . . . H15 H 0.5000 0.1398 0.9524 0.035 Uiso 1 1 calc R . . C16 C 0.4212(4) 0.0874(3) 0.8657(3) 0.0278(12) Uani 1 1 d . . . H16 H 0.3541 0.0691 0.8903 0.033 Uiso 1 1 calc R . . C17 C 0.4293(4) 0.0707(2) 0.7936(3) 0.0230(11) Uani 1 1 d . . . C18 C 0.1437(4) 0.3999(3) 0.5721(3) 0.0286(12) Uani 1 1 d . . . C19 C 0.1019(4) 0.3346(3) 0.5449(3) 0.0241(11) Uani 1 1 d . . . C20 C -0.0078(5) 0.3025(3) 0.5637(3) 0.0284(12) Uani 1 1 d . . . C21 C -0.0769(5) 0.3395(3) 0.6119(3) 0.0386(15) Uani 1 1 d . . . H21 H -0.1524 0.3198 0.6256 0.046 Uiso 1 1 calc R . . C22 C -0.0381(6) 0.4042(3) 0.6403(3) 0.0475(16) Uani 1 1 d . . . H22 H -0.0868 0.4285 0.6732 0.057 Uiso 1 1 calc R . . C23 C 0.3327(4) 0.0227(2) 0.7569(3) 0.0267(12) Uani 1 1 d . . . H23 H 0.3499 0.0192 0.7049 0.032 Uiso 1 1 calc R . . C24 C 0.2026(4) 0.0529(3) 0.7621(3) 0.0307(13) Uani 1 1 d . . . H24A H 0.1822 0.0544 0.8126 0.046 Uiso 1 1 calc R . . H24B H 0.1435 0.0223 0.7350 0.046 Uiso 1 1 calc R . . H24C H 0.1990 0.1012 0.7421 0.046 Uiso 1 1 calc R . . C25 C 0.3410(5) -0.0526(3) 0.7893(3) 0.0325(13) Uani 1 1 d . . . H25A H 0.4238 -0.0717 0.7845 0.049 Uiso 1 1 calc R . . H25B H 0.2807 -0.0837 0.7638 0.049 Uiso 1 1 calc R . . H25C H 0.3237 -0.0504 0.8402 0.049 Uiso 1 1 calc R . . C26 C 0.7276(4) 0.1729(3) 0.7577(3) 0.0299(12) Uani 1 1 d . . . H26 H 0.7149 0.1626 0.7052 0.036 Uiso 1 1 calc R . . C27 C 0.8469(4) 0.1363(3) 0.7848(3) 0.0405(14) Uani 1 1 d . . . H27A H 0.8552 0.1392 0.8374 0.061 Uiso 1 1 calc R . . H27B H 0.9169 0.1601 0.7644 0.061 Uiso 1 1 calc R . . H27C H 0.8449 0.0861 0.7701 0.061 Uiso 1 1 calc R . . C28 C 0.7347(5) 0.2536(3) 0.7667(3) 0.0356(13) Uani 1 1 d . . . H28A H 0.6579 0.2752 0.7472 0.053 Uiso 1 1 calc R . . H28B H 0.8036 0.2722 0.7408 0.053 Uiso 1 1 calc R . . H28C H 0.7471 0.2654 0.8178 0.053 Uiso 1 1 calc R . . C29 C 0.2621(5) 0.4347(3) 0.5518(3) 0.0365(14) Uani 1 1 d . . . H29 H 0.3042 0.4009 0.5198 0.044 Uiso 1 1 calc R . . C30 C 0.2364(5) 0.5040(3) 0.5092(3) 0.0463(16) Uani 1 1 d . . . H30A H 0.1845 0.4934 0.4658 0.069 Uiso 1 1 calc R . . H30B H 0.3143 0.5247 0.4956 0.069 Uiso 1 1 calc R . . H30C H 0.1940 0.5380 0.5390 0.069 Uiso 1 1 calc R . . C31 C 0.3471(6) 0.4479(3) 0.6172(4) 0.0522(17) Uani 1 1 d . . . H31A H 0.3111 0.4840 0.6476 0.078 Uiso 1 1 calc R . . H31B H 0.4267 0.4649 0.6021 0.078 Uiso 1 1 calc R . . H31C H 0.3589 0.4034 0.6443 0.078 Uiso 1 1 calc R . . C32 C -0.0533(5) 0.2321(3) 0.5334(3) 0.0325(13) Uani 1 1 d . . . H32 H 0.0141 0.2102 0.5066 0.039 Uiso 1 1 calc R . . C33 C -0.0873(6) 0.1799(3) 0.5925(3) 0.0513(17) Uani 1 1 d . . . H33A H -0.0164 0.1733 0.6266 0.077 Uiso 1 1 calc R . . H33B H -0.1110 0.1339 0.5709 0.077 Uiso 1 1 calc R . . H33C H -0.1563 0.1993 0.6178 0.077 Uiso 1 1 calc R . . C34 C -0.1640(5) 0.2438(3) 0.4805(3) 0.0448(15) Uani 1 1 d . . . H34A H -0.2309 0.2658 0.5057 0.067 Uiso 1 1 calc R . . H34B H -0.1915 0.1979 0.4603 0.067 Uiso 1 1 calc R . . H34C H -0.1406 0.2754 0.4417 0.067 Uiso 1 1 calc R . . C35 C 0.0707(5) 0.4336(3) 0.6213(3) 0.0430(15) Uani 1 1 d . . . H35 H 0.0970 0.4778 0.6419 0.052 Uiso 1 1 calc R . . C36 C 0.8824(5) 0.8931(3) 0.6770(4) 0.0523(18) Uani 1 1 d . . . H36A H 0.8140 0.8812 0.6418 0.063 Uiso 1 1 calc R . . H36B H 0.8634 0.8738 0.7245 0.063 Uiso 1 1 calc R . . C37 C 0.9655(6) 0.9837(4) 0.6193(4) 0.061(2) Uani 1 1 d . . . H37A H 1.0103 1.0294 0.6264 0.073 Uiso 1 1 calc R . . H37B H 0.9082 0.9881 0.5764 0.073 Uiso 1 1 calc R . . C38 C 1.0545(6) 0.9235(3) 0.6099(4) 0.0533(18) Uani 1 1 d . . . H38A H 1.1382 0.9363 0.6289 0.064 Uiso 1 1 calc R . . H38B H 1.0574 0.9100 0.5587 0.064 Uiso 1 1 calc R . . C39 C 1.0008(6) 0.8632(3) 0.6537(4) 0.068(2) Uani 1 1 d . . . H39A H 0.9862 0.8200 0.6239 0.082 Uiso 1 1 calc R . . H39B H 1.0565 0.8509 0.6957 0.082 Uiso 1 1 calc R . . N1 N 0.5487(3) 0.08027(19) 0.6851(2) 0.0229(9) Uani 1 1 d . . . N2 N 0.5572(3) 0.08581(19) 0.5707(2) 0.0206(9) Uani 1 1 d . . . N3 N 0.4415(3) 0.1605(2) 0.4983(2) 0.0228(9) Uani 1 1 d . . . N4 N 0.3075(3) 0.2373(2) 0.4405(2) 0.0214(9) Uani 1 1 d . . . N5 N 0.1741(3) 0.29884(19) 0.4923(2) 0.0210(9) Uani 1 1 d . . . Cl1 Cl 0.52657(12) 0.28123(7) 0.60036(7) 0.0341(3) Uani 1 1 d . . . Cl2 Cl 0.26394(13) 0.24395(7) 0.69560(7) 0.0388(4) Uani 1 1 d . . . Cl3 Cl 0.22601(11) 0.09562(7) 0.57059(7) 0.0319(3) Uani 1 1 d . . . Ti1 Ti 0.35921(8) 0.19808(4) 0.59922(5) 0.0222(2) Uani 1 1 d . . . O1 O 0.9000(4) 0.9672(2) 0.6809(3) 0.0679(14) 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 0.027(2) 0.017(3) 0.021(3) 0.002(2) 0.003(2) -0.002(2) C2 0.022(2) 0.023(3) 0.032(3) 0.003(2) 0.001(2) 0.008(2) C3 0.025(3) 0.024(3) 0.033(3) 0.000(2) 0.007(2) 0.006(2) C4 0.028(3) 0.021(3) 0.016(3) -0.005(2) 0.005(2) -0.004(2) C5 0.033(3) 0.028(3) 0.017(3) 0.002(2) -0.004(2) -0.001(2) C6 0.031(3) 0.030(3) 0.013(3) 0.000(2) -0.001(2) -0.009(2) C7 0.027(3) 0.025(3) 0.016(3) -0.002(2) 0.003(2) -0.006(2) C8 0.029(3) 0.027(3) 0.023(3) -0.006(2) 0.007(2) -0.008(2) C9 0.030(3) 0.027(3) 0.027(3) -0.010(2) 0.010(2) -0.001(2) C10 0.043(3) 0.036(3) 0.021(3) -0.007(2) 0.015(3) -0.005(3) C11 0.034(3) 0.033(3) 0.016(3) -0.003(2) 0.005(2) -0.003(2) C12 0.022(2) 0.028(3) 0.024(3) 0.003(2) 0.000(2) 0.007(2) C13 0.028(3) 0.023(3) 0.019(3) -0.001(2) 0.000(2) 0.006(2) C14 0.032(3) 0.023(3) 0.028(3) 0.001(2) -0.003(2) -0.003(2) C15 0.036(3) 0.033(3) 0.018(3) 0.001(2) -0.002(2) 0.006(2) C16 0.028(3) 0.031(3) 0.025(3) 0.010(2) 0.001(2) 0.005(2) C17 0.027(3) 0.017(3) 0.024(3) 0.003(2) 0.002(2) 0.002(2) C18 0.033(3) 0.030(3) 0.022(3) -0.003(2) -0.005(2) 0.005(2) C19 0.032(3) 0.023(3) 0.018(3) 0.006(2) 0.002(2) 0.009(2) C20 0.036(3) 0.031(3) 0.018(3) 0.006(2) 0.003(2) 0.008(2) C21 0.041(3) 0.041(4) 0.035(3) 0.010(3) 0.017(3) 0.015(3) C22 0.058(4) 0.053(4) 0.032(4) -0.003(3) 0.016(3) 0.020(3) C23 0.034(3) 0.026(3) 0.020(3) 0.002(2) 0.007(2) 0.001(2) C24 0.032(3) 0.024(3) 0.036(3) 0.003(2) 0.004(2) -0.006(2) C25 0.036(3) 0.031(3) 0.030(3) 0.000(2) 0.006(3) 0.000(2) C26 0.032(3) 0.036(3) 0.021(3) -0.002(2) -0.001(2) -0.006(2) C27 0.033(3) 0.048(4) 0.041(4) 0.000(3) 0.006(3) -0.005(3) C28 0.038(3) 0.037(3) 0.030(3) 0.001(3) -0.005(3) -0.011(3) C29 0.039(3) 0.036(3) 0.035(3) -0.013(3) -0.001(3) -0.001(3) C30 0.059(4) 0.045(4) 0.035(4) -0.005(3) 0.003(3) -0.012(3) C31 0.056(4) 0.038(4) 0.059(5) -0.007(3) -0.023(3) -0.004(3) C32 0.031(3) 0.036(3) 0.031(3) 0.008(3) 0.010(2) 0.004(2) C33 0.062(4) 0.044(4) 0.049(4) 0.015(3) 0.017(3) -0.003(3) C34 0.038(3) 0.053(4) 0.044(4) 0.005(3) 0.001(3) 0.004(3) C35 0.057(4) 0.040(4) 0.032(3) -0.009(3) 0.006(3) 0.008(3) C36 0.043(3) 0.028(3) 0.086(5) -0.008(3) 0.009(3) -0.008(3) C37 0.046(4) 0.063(5) 0.074(5) 0.024(4) 0.003(4) -0.004(3) C38 0.059(4) 0.045(4) 0.057(5) -0.011(3) 0.010(4) -0.004(3) C39 0.082(5) 0.042(4) 0.084(6) 0.003(4) 0.024(4) 0.021(4) N1 0.028(2) 0.017(2) 0.023(2) 0.0004(18) 0.0038(18) 0.0018(17) N2 0.028(2) 0.020(2) 0.015(2) -0.0024(17) 0.0060(17) -0.0005(18) N3 0.026(2) 0.028(2) 0.015(2) -0.0039(18) 0.0040(18) -0.0018(19) N4 0.026(2) 0.024(2) 0.014(2) 0.0009(18) 0.0023(17) -0.0002(18) N5 0.031(2) 0.021(2) 0.011(2) 0.0016(17) 0.0030(17) -0.0009(18) Cl1 0.0397(7) 0.0291(7) 0.0329(8) -0.0030(6) -0.0021(6) -0.0046(6) Cl2 0.0605(9) 0.0381(8) 0.0192(7) -0.0019(6) 0.0154(7) 0.0122(7) Cl3 0.0312(7) 0.0339(7) 0.0310(8) -0.0010(6) 0.0053(6) -0.0053(6) Ti1 0.0282(5) 0.0242(5) 0.0144(5) -0.0016(4) 0.0040(4) 0.0052(4) O1 0.054(3) 0.047(3) 0.104(4) -0.001(3) 0.013(3) 0.005(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 N1 1.347(6) . ? C1 N2 1.388(5) . ? C1 Ti1 2.211(5) . ? C2 C3 1.358(7) . ? C2 N1 1.401(6) . ? C3 N2 1.392(6) . ? C4 N5 1.345(6) . ? C4 N4 1.380(5) . ? C4 Ti1 2.191(5) . ? C5 C6 1.343(6) . ? C5 N5 1.410(6) . ? C6 N4 1.393(6) . ? C7 N3 1.343(6) . ? C7 C11 1.385(6) . ? C7 N4 1.403(6) . ? C8 N3 1.330(6) . ? C8 C9 1.386(6) . ? C8 N2 1.416(6) . ? C9 C10 1.382(7) . ? C10 C11 1.378(7) . ? C12 C14 1.392(7) . ? C12 C13 1.394(6) . ? C12 C26 1.513(6) . ? C13 C17 1.410(6) . ? C13 N1 1.455(6) . ? C14 C15 1.382(7) . ? C15 C16 1.383(7) . ? C16 C17 1.389(7) . ? C17 C23 1.517(7) . ? C18 C19 1.391(7) . ? C18 C35 1.400(7) . ? C18 C29 1.514(7) . ? C19 C20 1.401(7) . ? C19 N5 1.456(6) . ? C20 C21 1.390(7) . ? C20 C32 1.509(7) . ? C21 C22 1.381(8) . ? C22 C35 1.372(8) . ? C23 C24 1.536(6) . ? C23 C25 1.536(6) . ? C26 C28 1.523(7) . ? C26 C27 1.530(7) . ? C29 C31 1.508(8) . ? C29 C30 1.540(7) . ? C32 C34 1.529(7) . ? C32 C33 1.535(7) . ? C36 O1 1.403(6) . ? C36 C39 1.494(8) . ? C37 O1 1.421(7) . ? C37 C38 1.506(8) . ? C38 C39 1.531(8) . ? N3 Ti1 2.246(4) . ? Cl1 Ti1 2.3984(15) . ? Cl2 Ti1 2.2948(14) . ? Cl3 Ti1 2.4476(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 N1 C1 N2 103.2(4) . . ? N1 C1 Ti1 140.9(3) . . ? N2 C1 Ti1 115.9(3) . . ? C3 C2 N1 107.0(4) . . ? C2 C3 N2 105.7(4) . . ? N5 C4 N4 102.9(4) . . ? N5 C4 Ti1 140.4(3) . . ? N4 C4 Ti1 116.7(3) . . ? C6 C5 N5 106.9(4) . . ? C5 C6 N4 105.8(4) . . ? N3 C7 C11 122.4(4) . . ? N3 C7 N4 112.0(4) . . ? C11 C7 N4 125.6(5) . . ? N3 C8 C9 123.9(5) . . ? N3 C8 N2 111.9(4) . . ? C9 C8 N2 124.3(5) . . ? C10 C9 C8 116.0(5) . . ? C11 C10 C9 122.0(5) . . ? C10 C11 C7 117.2(5) . . ? C14 C12 C13 116.5(4) . . ? C14 C12 C26 120.4(4) . . ? C13 C12 C26 123.1(4) . . ? C12 C13 C17 123.2(4) . . ? C12 C13 N1 117.3(4) . . ? C17 C13 N1 119.5(4) . . ? C15 C14 C12 122.8(5) . . ? C14 C15 C16 118.5(5) . . ? C15 C16 C17 122.4(5) . . ? C16 C17 C13 116.6(4) . . ? C16 C17 C23 119.3(4) . . ? C13 C17 C23 124.1(4) . . ? C19 C18 C35 116.7(5) . . ? C19 C18 C29 123.7(4) . . ? C35 C18 C29 119.6(5) . . ? C18 C19 C20 123.5(4) . . ? C18 C19 N5 118.2(4) . . ? C20 C19 N5 118.3(4) . . ? C21 C20 C19 116.8(5) . . ? C21 C20 C32 120.0(5) . . ? C19 C20 C32 123.2(4) . . ? C22 C21 C20 121.4(5) . . ? C35 C22 C21 120.2(5) . . ? C17 C23 C24 111.8(4) . . ? C17 C23 C25 110.2(4) . . ? C24 C23 C25 110.3(4) . . ? C12 C26 C28 111.4(4) . . ? C12 C26 C27 110.4(4) . . ? C28 C26 C27 111.9(4) . . ? C31 C29 C18 111.2(5) . . ? C31 C29 C30 111.3(5) . . ? C18 C29 C30 111.1(4) . . ? C20 C32 C34 110.2(4) . . ? C20 C32 C33 112.0(5) . . ? C34 C32 C33 109.9(5) . . ? C22 C35 C18 121.4(5) . . ? O1 C36 C39 105.6(5) . . ? O1 C37 C38 106.8(5) . . ? C37 C38 C39 102.9(5) . . ? C36 C39 C38 104.0(5) . . ? C1 N1 C2 112.1(4) . . ? C1 N1 C13 124.7(4) . . ? C2 N1 C13 122.3(4) . . ? C1 N2 C3 112.0(4) . . ? C1 N2 C8 119.6(4) . . ? C3 N2 C8 128.3(4) . . ? C8 N3 C7 118.5(4) . . ? C8 N3 Ti1 121.2(3) . . ? C7 N3 Ti1 120.2(3) . . ? C4 N4 C6 112.4(4) . . ? C4 N4 C7 119.6(4) . . ? C6 N4 C7 128.0(4) . . ? C4 N5 C5 112.0(4) . . ? C4 N5 C19 125.6(4) . . ? C5 N5 C19 122.3(4) . . ? C4 Ti1 C1 142.56(17) . . ? C4 Ti1 N3 71.35(15) . . ? C1 Ti1 N3 71.30(16) . . ? C4 Ti1 Cl2 103.17(12) . . ? C1 Ti1 Cl2 114.19(13) . . ? N3 Ti1 Cl2 174.51(12) . . ? C4 Ti1 Cl1 90.99(12) . . ? C1 Ti1 Cl1 86.76(12) . . ? N3 Ti1 Cl1 82.57(10) . . ? Cl2 Ti1 Cl1 97.36(6) . . ? C4 Ti1 Cl3 87.56(12) . . ? C1 Ti1 Cl3 83.77(12) . . ? N3 Ti1 Cl3 80.31(10) . . ? Cl2 Ti1 Cl3 100.09(5) . . ? Cl1 Ti1 Cl3 162.36(6) . . ? C36 O1 C37 104.3(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.629 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.097 #==END data_2b _database_code_depnum_ccdc_archive 'CCDC 282400' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H106 Br4 Cl0 Cr2 N10 O3' _chemical_formula_sum 'C82 H106 Br4 Cl0 Cr2 N10 O3' _chemical_formula_weight 1703.41 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' Cr Cr 0.3209 0.6236 '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 trigonal _symmetry_space_group_name_H-M '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 34.5630(7) _cell_length_b 34.5630(7) _cell_length_c 41.0813(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 42501(2) _cell_formula_units_Z 18 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16012 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 24.7 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15840 _exptl_absorpt_coefficient_mu 1.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6943 _exptl_absorpt_correction_T_max 0.9254 _exptl_absorpt_process_details Sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82975 _diffrn_reflns_av_R_equivalents 0.1702 _diffrn_reflns_av_sigmaI/netI 0.1797 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 24.69 _reflns_number_total 15994 _reflns_number_gt 8432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski and Minor 1997)' _computing_data_reduction 'Denzo.a Scalepack (Otwinowski and Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0827P)^2^+763.8233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15994 _refine_ls_number_parameters 885 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2029 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.2395 _refine_ls_wR_factor_gt 0.1998 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.1906(4) 0.3874(4) 0.3098(3) 0.057(3) Uani 1 1 d . . . H2A H 0.1598 0.3682 0.3172 0.085 Uiso 1 1 calc R . . H2B H 0.2108 0.3965 0.3285 0.085 Uiso 1 1 calc R . . H2C H 0.1985 0.3710 0.2943 0.085 Uiso 1 1 calc R . . C3 C 0.1804(4) 0.4547(4) 0.3162(3) 0.068(4) Uani 1 1 d . . . H3A H 0.1499 0.4344 0.3238 0.102 Uiso 1 1 calc R . . H3B H 0.1813 0.4801 0.3048 0.102 Uiso 1 1 calc R . . H3C H 0.2008 0.4656 0.3348 0.102 Uiso 1 1 calc R . . C1 C 0.1170(3) 0.4181(3) 0.1827(2) 0.025(2) Uani 1 1 d . . . C4 C 0.2491(3) 0.4836(3) 0.2512(2) 0.027(2) Uani 1 1 d . . . C5 C 0.0820(3) 0.4224(3) 0.1706(2) 0.030(2) Uani 1 1 d . . . H5 H 0.0799 0.4483 0.1750 0.037 Uiso 1 1 calc R . . C6 C 0.0499(3) 0.3876(3) 0.1519(2) 0.031(2) Uani 1 1 d . . . H6 H 0.0258 0.3900 0.1429 0.037 Uiso 1 1 calc R . . C7 C 0.1561(3) 0.4880(3) 0.2163(2) 0.028(2) Uani 1 1 d . . . H7 H 0.1370 0.5001 0.2131 0.034 Uiso 1 1 calc R . . C8 C 0.1925(3) 0.5051(3) 0.2348(2) 0.029(2) Uani 1 1 d . . . H8 H 0.2047 0.5319 0.2471 0.035 Uiso 1 1 calc R . . C9 C 0.0008(3) 0.3375(3) 0.0225(2) 0.034(2) Uani 1 1 d . . . C10 C -0.0900(4) 0.3072(3) -0.0651(2) 0.039(3) Uani 1 1 d . . . H10 H -0.0848 0.3126 -0.0877 0.047 Uiso 1 1 calc R . . C11 C 0.1843(3) 0.4402(3) 0.2129(2) 0.028(2) Uani 1 1 d . . . C12 C -0.1178(4) 0.2791(4) 0.0372(3) 0.052(3) Uani 1 1 d . . . H12 H -0.0904 0.3001 0.0496 0.062 Uiso 1 1 calc R . . C13 C 0.0344(4) 0.1737(4) 0.0022(3) 0.045(3) Uani 1 1 d . . . C14 C 0.0129(3) 0.4042(3) 0.0443(2) 0.038(3) Uani 1 1 d . . . H14 H 0.0259 0.4314 0.0562 0.046 Uiso 1 1 calc R . . C15 C 0.0676(3) 0.3774(3) 0.0557(2) 0.031(2) Uani 1 1 d . . . C16 C 0.0899(3) 0.2470(4) 0.1491(2) 0.040(3) Uani 1 1 d . . . H16 H 0.0801 0.2173 0.1423 0.048 Uiso 1 1 calc R . . C17 C -0.0244(3) 0.3870(3) 0.0261(2) 0.042(3) Uani 1 1 d . . . H17 H -0.0429 0.3996 0.0228 0.051 Uiso 1 1 calc R . . C18 C 0.2409(3) 0.4609(3) 0.2806(2) 0.033(2) Uani 1 1 d . . . C19 C 0.1336(3) 0.4089(3) 0.0861(2) 0.039(3) Uani 1 1 d . . . H19 H 0.1545 0.4314 0.1002 0.047 Uiso 1 1 calc R . . C20 C 0.1887(4) 0.2585(3) 0.1603(2) 0.040(3) Uani 1 1 d . . . C21 C 0.2910(3) 0.5156(3) 0.2403(2) 0.030(2) Uani 1 1 d . . . C22 C 0.0966(3) 0.4112(3) 0.0761(2) 0.029(2) Uani 1 1 d . . . H22 H 0.0915 0.4345 0.0828 0.035 Uiso 1 1 calc R . . C23 C 0.1144(4) 0.2415(4) 0.2340(3) 0.062(3) Uani 1 1 d . . . H23 H 0.0990 0.2550 0.2218 0.074 Uiso 1 1 calc R . . C24 C -0.1320(4) 0.2759(4) -0.0544(3) 0.046(3) Uani 1 1 d . . . H24 H -0.1551 0.2606 -0.0699 0.055 Uiso 1 1 calc R . . C25 C 0.1107(3) 0.3438(3) 0.0552(3) 0.038(3) Uani 1 1 d . . . C26 C 0.0770(3) 0.2777(3) 0.0218(2) 0.039(3) Uani 1 1 d . . . C27 C -0.1413(4) 0.2663(3) -0.0221(3) 0.044(3) Uani 1 1 d . . . H27 H -0.1704 0.2440 -0.0154 0.053 Uiso 1 1 calc R . . C28 C 0.1348(3) 0.2631(4) 0.0211(3) 0.045(3) Uani 1 1 d . . . H28 H 0.1516 0.2490 0.0161 0.054 Uiso 1 1 calc R . . C29 C 0.2192(5) 0.2480(4) 0.1740(3) 0.070(4) Uani 1 1 d . . . H29 H 0.2425 0.2493 0.1610 0.084 Uiso 1 1 calc R . . C30 C 0.1479(3) 0.2990(3) 0.0402(3) 0.038(3) Uani 1 1 d . . . H30 H 0.1757 0.3153 0.0511 0.046 Uiso 1 1 calc R . . C31 C 0.1525(4) 0.2459(4) 0.2134(3) 0.045(3) Uani 1 1 d . . . C32 C 0.0885(3) 0.3483(3) 0.1592(2) 0.027(2) Uani 1 1 d . . . C33 C 0.1580(3) 0.2597(3) 0.1808(2) 0.037(3) Uani 1 1 d . . . C34 C 0.1411(3) 0.3747(3) 0.0761(2) 0.038(3) Uani 1 1 d . . . H34 H 0.1662 0.3729 0.0835 0.046 Uiso 1 1 calc R . . C35 C -0.1282(4) 0.2319(4) 0.0452(3) 0.068(4) Uani 1 1 d . . . H35A H -0.1339 0.2265 0.0686 0.102 Uiso 1 1 calc R . . H35B H -0.1028 0.2284 0.0391 0.102 Uiso 1 1 calc R . . H35C H -0.1548 0.2104 0.0331 0.102 Uiso 1 1 calc R . . C36 C 0.2781(4) 0.4715(3) 0.2996(2) 0.042(3) Uani 1 1 d . . . H36 H 0.2744 0.4569 0.3199 0.050 Uiso 1 1 calc R . . C37 C 0.0698(4) 0.2704(3) 0.1423(2) 0.042(3) Uani 1 1 d . . . H37 H 0.0430 0.2609 0.1303 0.050 Uiso 1 1 calc R . . C38 C -0.0557(3) 0.3307(3) -0.0437(2) 0.037(3) Uani 1 1 d . . . C39 C 0.3312(4) 0.5352(4) 0.1878(3) 0.069(4) Uani 1 1 d . . . H39A H 0.3349 0.5505 0.1670 0.103 Uiso 1 1 calc R . . H39B H 0.3204 0.5034 0.1838 0.103 Uiso 1 1 calc R . . H39C H 0.3601 0.5485 0.1991 0.103 Uiso 1 1 calc R . . C40 C 0.0250(3) 0.1693(4) 0.0375(3) 0.049(3) Uani 1 1 d . . . H40 H 0.0344 0.2000 0.0458 0.059 Uiso 1 1 calc R . . C41 C 0.0102(4) 0.1377(4) -0.0189(3) 0.055(3) Uani 1 1 d . . . H41 H -0.0122 0.1097 -0.0106 0.066 Uiso 1 1 calc R . . C42 C -0.1075(4) 0.2895(3) 0.0014(2) 0.038(3) Uani 1 1 d . . . C43 C 0.3207(4) 0.5032(4) 0.2894(3) 0.046(3) Uani 1 1 d . . . H43 H 0.3461 0.5099 0.3024 0.055 Uiso 1 1 calc R . . C44 C 0.0666(3) 0.2134(3) -0.0121(3) 0.041(3) Uani 1 1 d . . . C45 C 0.0525(3) 0.3494(3) 0.1460(2) 0.031(2) Uani 1 1 d . . . H45 H 0.0306 0.3253 0.1335 0.037 Uiso 1 1 calc R . . C46 C 0.1328(3) 0.3142(3) 0.1730(2) 0.031(2) Uani 1 1 d . . . C47 C 0.0750(3) 0.2204(3) -0.0450(3) 0.042(3) Uani 1 1 d . . . C48 C 0.2985(3) 0.5399(4) 0.2082(2) 0.045(3) Uani 1 1 d . . . H48 H 0.2694 0.5258 0.1963 0.054 Uiso 1 1 calc R . . C49 C 0.3131(4) 0.5894(4) 0.2136(3) 0.065(4) Uani 1 1 d . . . H49A H 0.3169 0.6040 0.1925 0.098 Uiso 1 1 calc R . . H49B H 0.3416 0.6040 0.2255 0.098 Uiso 1 1 calc R . . H49C H 0.2903 0.5916 0.2263 0.098 Uiso 1 1 calc R . . C50 C 0.2361(4) 0.3077(4) 0.1147(3) 0.076(4) Uani 1 1 d . . . H50A H 0.2363 0.3141 0.0915 0.114 Uiso 1 1 calc R . . H50B H 0.2590 0.2996 0.1193 0.114 Uiso 1 1 calc R . . H50C H 0.2424 0.3343 0.1274 0.114 Uiso 1 1 calc R . . C51 C -0.0654(3) 0.3211(3) -0.0104(2) 0.032(2) Uani 1 1 d . . . C52 C -0.0097(4) 0.3634(3) -0.0552(2) 0.042(3) Uani 1 1 d . . . H52 H 0.0101 0.3757 -0.0357 0.050 Uiso 1 1 calc R . . C53 C 0.0504(4) 0.1835(4) -0.0652(3) 0.052(3) Uani 1 1 d . . . H53 H 0.0552 0.1863 -0.0880 0.063 Uiso 1 1 calc R . . C54 C 0.0191(4) 0.1432(4) -0.0520(3) 0.057(3) Uani 1 1 d . . . H54 H 0.0032 0.1183 -0.0660 0.069 Uiso 1 1 calc R . . C55 C 0.0521(4) 0.1539(5) 0.0550(3) 0.086(4) Uani 1 1 d . . . H55A H 0.0456 0.1521 0.0783 0.129 Uiso 1 1 calc R . . H55B H 0.0839 0.1750 0.0513 0.129 Uiso 1 1 calc R . . H55C H 0.0448 0.1243 0.0469 0.129 Uiso 1 1 calc R . . C56 C 0.1912(4) 0.2698(4) 0.1240(2) 0.046(3) Uani 1 1 d . . . H56 H 0.1689 0.2796 0.1198 0.055 Uiso 1 1 calc R . . C57 C -0.0238(4) 0.1404(4) 0.0458(3) 0.073(4) Uani 1 1 d . . . H57A H -0.0275 0.1398 0.0695 0.110 Uiso 1 1 calc R . . H57B H -0.0345 0.1100 0.0379 0.110 Uiso 1 1 calc R . . H57C H -0.0409 0.1526 0.0356 0.110 Uiso 1 1 calc R . . C58 C 0.1835(5) 0.2355(5) 0.2257(3) 0.076(4) Uani 1 1 d . . . H58 H 0.1823 0.2280 0.2480 0.091 Uiso 1 1 calc R . . C59 C 0.1305(5) 0.2660(5) 0.2662(3) 0.084(4) Uani 1 1 d . . . H59A H 0.1049 0.2632 0.2785 0.126 Uiso 1 1 calc R . . H59B H 0.1516 0.2977 0.2620 0.126 Uiso 1 1 calc R . . H59C H 0.1453 0.2531 0.2787 0.126 Uiso 1 1 calc R . . C60 C 0.1777(4) 0.2284(4) 0.1036(3) 0.064(4) Uani 1 1 d . . . H60A H 0.1795 0.2361 0.0805 0.097 Uiso 1 1 calc R . . H60B H 0.1469 0.2056 0.1089 0.097 Uiso 1 1 calc R . . H60C H 0.1977 0.2167 0.1082 0.097 Uiso 1 1 calc R . . C61 C -0.1558(4) 0.2866(4) 0.0486(3) 0.067(4) Uani 1 1 d . . . H61A H -0.1611 0.2799 0.0719 0.101 Uiso 1 1 calc R . . H61B H -0.1831 0.2669 0.0364 0.101 Uiso 1 1 calc R . . H61C H -0.1475 0.3178 0.0448 0.101 Uiso 1 1 calc R . . C62 C 0.2159(5) 0.2359(5) 0.2061(3) 0.080(4) Uani 1 1 d . . . H62 H 0.2362 0.2277 0.2148 0.096 Uiso 1 1 calc R . . C63 C 0.1947(3) 0.4297(4) 0.2929(2) 0.043(3) Uani 1 1 d . . . H63 H 0.1739 0.4196 0.2738 0.051 Uiso 1 1 calc R . . C64 C 0.0095(5) 0.3424(4) -0.0773(4) 0.097(5) Uani 1 1 d . . . H64A H 0.0396 0.3651 -0.0842 0.145 Uiso 1 1 calc R . . H64B H -0.0097 0.3299 -0.0965 0.145 Uiso 1 1 calc R . . H64C H 0.0110 0.3185 -0.0656 0.145 Uiso 1 1 calc R . . C65 C -0.0082(4) 0.4032(4) -0.0741(4) 0.091(5) Uani 1 1 d . . . H65A H 0.0226 0.4240 -0.0808 0.136 Uiso 1 1 calc R . . H65B H -0.0190 0.4187 -0.0600 0.136 Uiso 1 1 calc R . . H65C H -0.0273 0.3919 -0.0935 0.136 Uiso 1 1 calc R . . C66 C 0.1085(4) 0.2650(4) -0.0598(3) 0.051(3) Uani 1 1 d . . . H66 H 0.1294 0.2834 -0.0420 0.062 Uiso 1 1 calc R . . C67 C 0.3256(3) 0.5244(3) 0.2605(2) 0.034(2) Uani 1 1 d . . . H67 H 0.3548 0.5466 0.2541 0.041 Uiso 1 1 calc R . . C68 C 0.1366(4) 0.2630(4) -0.0871(3) 0.076(4) Uani 1 1 d . . . H68A H 0.1580 0.2934 -0.0942 0.114 Uiso 1 1 calc R . . H68B H 0.1173 0.2461 -0.1053 0.114 Uiso 1 1 calc R . . H68C H 0.1528 0.2483 -0.0793 0.114 Uiso 1 1 calc R . . C69 C 0.0848(5) 0.2895(5) -0.0713(4) 0.110(6) Uani 1 1 d . . . H69A H 0.1068 0.3187 -0.0801 0.165 Uiso 1 1 calc R . . H69B H 0.0692 0.2937 -0.0529 0.165 Uiso 1 1 calc R . . H69C H 0.0631 0.2719 -0.0882 0.165 Uiso 1 1 calc R . . C70 C 0.0805(6) 0.1925(6) 0.2402(5) 0.154(9) Uani 1 1 d . . . H70A H 0.0559 0.1902 0.2535 0.231 Uiso 1 1 calc R . . H70B H 0.0951 0.1784 0.2518 0.231 Uiso 1 1 calc R . . H70C H 0.0688 0.1772 0.2194 0.231 Uiso 1 1 calc R . . C71 C 0.3687(6) 0.4487(5) 0.3594(4) 0.116(6) Uani 1 1 d . . . H71A H 0.3428 0.4345 0.3444 0.140 Uiso 1 1 calc R . . H71B H 0.3771 0.4262 0.3657 0.140 Uiso 1 1 calc R . . C72 C 0.4065(5) 0.4877(5) 0.3440(4) 0.085(4) Uani 1 1 d . . . H72A H 0.4352 0.4908 0.3515 0.102 Uiso 1 1 calc R . . H72B H 0.4049 0.4843 0.3200 0.102 Uiso 1 1 calc R . . C73 C 0.3587(9) 0.4662(7) 0.3871(5) 0.177(11) Uani 1 1 d . . . H73A H 0.3259 0.4513 0.3903 0.212 Uiso 1 1 calc R . . H73B H 0.3723 0.4614 0.4067 0.212 Uiso 1 1 calc R . . C74 C 0.3764(8) 0.5126(7) 0.3815(5) 0.165(10) Uani 1 1 d . . . H74A H 0.3517 0.5190 0.3787 0.198 Uiso 1 1 calc R . . H74B H 0.3944 0.5297 0.4005 0.198 Uiso 1 1 calc R . . C75 C 0.2727(5) 0.5892(5) 0.3059(4) 0.094(5) Uani 1 1 d . . . H75A H 0.2978 0.6184 0.2989 0.113 Uiso 1 1 calc R . . H75B H 0.2798 0.5656 0.3003 0.113 Uiso 1 1 calc R . . C76 C 0.2654(6) 0.5894(6) 0.3415(4) 0.117(6) Uani 1 1 d . . . H76A H 0.2611 0.5615 0.3516 0.141 Uiso 1 1 calc R . . H76B H 0.2914 0.6151 0.3519 0.141 Uiso 1 1 calc R . . C77 C 0.2253(6) 0.5931(8) 0.3454(5) 0.164(11) Uani 1 1 d . . . H77A H 0.2051 0.5716 0.3619 0.196 Uiso 1 1 calc R . . H77B H 0.2333 0.6236 0.3522 0.196 Uiso 1 1 calc R . . C78 C 0.2045(6) 0.5831(5) 0.3144(4) 0.098(5) Uani 1 1 d . . . H78A H 0.1973 0.6065 0.3083 0.118 Uiso 1 1 calc R . . H78B H 0.1763 0.5542 0.3154 0.118 Uiso 1 1 calc R . . C79 C 0.9394(8) 0.2653(7) 0.1703(5) 0.153(8) Uiso 1 1 d . . . H79A H 0.9409 0.2850 0.1884 0.184 Uiso 1 1 calc R . . H79B H 0.9537 0.2843 0.1510 0.184 Uiso 1 1 calc R . . C80 C 0.9312(12) 0.2033(11) 0.1922(8) 0.225(13) Uiso 1 1 d . . . H80A H 0.9382 0.1791 0.1888 0.270 Uiso 1 1 calc R . . H80B H 0.9294 0.2069 0.2159 0.270 Uiso 1 1 calc R . . C81 C 0.8926(11) 0.1911(11) 0.1796(8) 0.232(13) Uiso 1 1 d . . . H81A H 0.8693 0.1782 0.1966 0.278 Uiso 1 1 calc R . . H81B H 0.8856 0.1678 0.1629 0.278 Uiso 1 1 calc R . . C82 C 0.8929(10) 0.2342(10) 0.1629(7) 0.216(12) Uiso 1 1 d . . . H82A H 0.8868 0.2304 0.1393 0.260 Uiso 1 1 calc R . . H82B H 0.8722 0.2421 0.1738 0.260 Uiso 1 1 calc R . . N1 N 0.0914(3) 0.2502(3) 0.0098(2) 0.040(2) Uani 1 1 d . . . N2 N 0.1125(3) 0.3078(3) 0.0408(2) 0.038(2) Uani 1 1 d . . . N3 N 0.0736(3) 0.3440(2) 0.04569(18) 0.0309(19) Uani 1 1 d . . . N4 N 0.0285(3) 0.3745(2) 0.04233(18) 0.032(2) Uani 1 1 d . . . N5 N -0.0306(2) 0.3470(2) 0.01311(18) 0.0310(19) Uani 1 1 d . . . N6 N 0.1203(2) 0.3818(2) 0.17684(17) 0.0262(18) Uani 1 1 d . . . N7 N 0.1512(2) 0.4490(2) 0.20265(17) 0.0253(18) Uani 1 1 d . . . N8 N 0.0965(2) 0.3120(2) 0.15681(17) 0.0294(19) Uani 1 1 d . . . N9 N 0.2095(2) 0.4757(2) 0.23261(17) 0.0267(18) Uani 1 1 d . . . N10 N 0.1274(3) 0.2733(3) 0.16768(19) 0.038(2) Uani 1 1 d . . . O1 O 0.2335(3) 0.5810(3) 0.2904(2) 0.088(3) Uani 1 1 d . . . O2 O 0.4035(3) 0.5259(3) 0.3534(2) 0.082(3) Uani 1 1 d . . . O3 O 0.9657(8) 0.2422(9) 0.1799(6) 0.255(9) Uiso 1 1 d . . . Cr1 Cr 0.02265(5) 0.28996(5) 0.02153(4) 0.0343(4) Uani 1 1 d . . . Cr2 Cr 0.17627(5) 0.38018(5) 0.19206(3) 0.0281(4) Uani 1 1 d . . . Br1 Br -0.02771(4) 0.23748(4) -0.01955(3) 0.0466(3) Uani 1 1 d . . . Br2 Br -0.01246(4) 0.25598(4) 0.07930(3) 0.0503(3) Uani 1 1 d . . . Br3 Br 0.22046(3) 0.41893(4) 0.13849(2) 0.0399(3) Uani 1 1 d . . . Br4 Br 0.23180(4) 0.37032(4) 0.22197(3) 0.0469(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 C2 0.080(9) 0.058(8) 0.040(7) 0.009(6) 0.021(6) 0.040(7) C3 0.052(8) 0.058(8) 0.094(10) 0.035(7) 0.030(7) 0.028(7) C1 0.012(5) 0.033(6) 0.026(5) 0.005(4) 0.005(4) 0.008(5) C4 0.034(6) 0.026(5) 0.023(5) -0.004(4) -0.006(5) 0.015(5) C5 0.026(6) 0.033(6) 0.033(6) -0.006(5) 0.004(5) 0.015(5) C6 0.028(6) 0.029(6) 0.034(6) 0.010(5) -0.001(5) 0.012(5) C7 0.028(6) 0.036(6) 0.025(5) 0.002(5) 0.000(4) 0.019(5) C8 0.035(6) 0.020(5) 0.031(5) -0.006(4) -0.004(5) 0.014(5) C9 0.041(6) 0.047(7) 0.022(5) 0.007(5) 0.005(5) 0.027(6) C10 0.046(7) 0.042(7) 0.029(6) 0.001(5) -0.010(5) 0.021(6) C11 0.026(5) 0.037(6) 0.017(5) 0.003(5) 0.006(4) 0.014(5) C12 0.041(7) 0.054(8) 0.041(7) -0.007(6) -0.025(6) 0.010(6) C13 0.036(7) 0.057(8) 0.050(7) -0.017(6) -0.007(6) 0.030(6) C14 0.048(7) 0.031(6) 0.042(6) -0.009(5) -0.014(5) 0.025(6) C15 0.032(6) 0.036(6) 0.019(5) 0.000(5) -0.009(4) 0.013(5) C16 0.036(6) 0.036(6) 0.041(6) -0.011(5) -0.011(5) 0.012(6) C17 0.048(7) 0.040(7) 0.043(6) -0.020(5) -0.022(6) 0.025(6) C18 0.028(6) 0.032(6) 0.033(6) -0.002(5) -0.004(5) 0.011(5) C19 0.043(7) 0.032(6) 0.030(6) 0.000(5) -0.007(5) 0.008(5) C20 0.066(8) 0.051(7) 0.030(6) -0.002(5) 0.003(5) 0.049(6) C21 0.025(6) 0.034(6) 0.028(5) 0.002(5) 0.000(5) 0.012(5) C22 0.039(6) 0.027(6) 0.023(5) -0.003(4) -0.005(5) 0.017(5) C23 0.090(10) 0.076(9) 0.040(7) 0.013(7) 0.008(7) 0.057(9) C24 0.067(9) 0.041(7) 0.040(7) -0.016(5) -0.029(6) 0.035(7) C25 0.027(6) 0.034(6) 0.050(7) 0.000(5) -0.011(5) 0.013(5) C26 0.041(7) 0.038(6) 0.044(6) -0.013(5) -0.013(5) 0.024(6) C27 0.049(7) 0.032(6) 0.050(7) -0.006(5) -0.013(6) 0.020(6) C28 0.032(6) 0.047(7) 0.064(8) -0.012(6) -0.013(6) 0.026(6) C29 0.101(11) 0.087(10) 0.060(9) 0.018(7) 0.026(8) 0.075(9) C30 0.024(6) 0.034(6) 0.059(7) 0.002(6) -0.010(5) 0.016(5) C31 0.066(8) 0.057(8) 0.035(6) 0.005(5) 0.009(6) 0.048(7) C32 0.027(6) 0.024(6) 0.030(5) 0.005(4) -0.003(5) 0.011(5) C33 0.046(7) 0.037(6) 0.038(6) -0.004(5) -0.004(5) 0.029(6) C34 0.031(6) 0.035(6) 0.040(6) -0.001(5) -0.012(5) 0.009(5) C35 0.074(9) 0.080(10) 0.052(8) 0.016(7) -0.012(7) 0.039(8) C36 0.048(7) 0.044(7) 0.031(6) 0.007(5) -0.009(5) 0.021(6) C37 0.042(7) 0.041(7) 0.043(7) -0.010(5) -0.010(5) 0.022(6) C38 0.042(7) 0.032(6) 0.045(7) -0.006(5) -0.016(5) 0.025(6) C39 0.075(9) 0.080(9) 0.045(7) 0.003(7) 0.024(7) 0.034(8) C40 0.035(7) 0.047(7) 0.076(9) 0.003(6) -0.002(6) 0.028(6) C41 0.049(8) 0.053(8) 0.069(9) -0.003(7) 0.007(7) 0.030(7) C42 0.049(7) 0.049(7) 0.030(6) -0.010(5) -0.015(5) 0.034(6) C43 0.041(7) 0.046(7) 0.048(7) -0.006(6) -0.023(6) 0.021(6) C44 0.031(6) 0.033(7) 0.057(8) -0.012(6) -0.013(6) 0.015(6) C45 0.025(6) 0.024(6) 0.036(6) 0.004(5) -0.004(5) 0.006(5) C46 0.037(6) 0.047(7) 0.022(5) 0.007(5) 0.000(5) 0.031(5) C47 0.039(7) 0.041(7) 0.049(7) -0.007(6) -0.003(6) 0.024(6) C48 0.032(6) 0.057(8) 0.037(6) 0.009(5) 0.007(5) 0.016(6) C49 0.084(10) 0.054(8) 0.060(8) 0.005(7) 0.008(7) 0.036(7) C50 0.084(10) 0.063(9) 0.061(9) 0.011(7) 0.002(8) 0.022(8) C51 0.038(6) 0.029(6) 0.036(6) -0.007(5) -0.014(5) 0.022(5) C52 0.051(7) 0.042(7) 0.032(6) -0.003(5) -0.009(5) 0.024(6) C53 0.041(7) 0.059(8) 0.056(8) -0.013(7) 0.001(6) 0.025(7) C54 0.044(8) 0.037(7) 0.088(10) -0.025(7) -0.006(7) 0.017(6) C55 0.070(10) 0.107(12) 0.088(11) 0.012(9) 0.017(8) 0.049(9) C56 0.060(8) 0.059(8) 0.038(6) 0.010(6) 0.006(6) 0.045(7) C57 0.042(8) 0.092(10) 0.083(10) 0.001(8) 0.000(7) 0.031(8) C58 0.111(12) 0.104(11) 0.049(8) 0.021(8) 0.003(8) 0.080(10) C59 0.104(12) 0.104(12) 0.065(9) 0.001(8) 0.022(8) 0.068(10) C60 0.082(10) 0.067(9) 0.042(7) 0.006(6) 0.006(7) 0.035(8) C61 0.065(9) 0.074(9) 0.058(8) -0.011(7) -0.007(7) 0.031(8) C62 0.116(12) 0.125(13) 0.058(9) 0.025(8) 0.011(9) 0.105(11) C63 0.040(7) 0.054(7) 0.032(6) 0.006(5) -0.004(5) 0.022(6) C64 0.088(11) 0.066(10) 0.134(14) 0.001(9) 0.052(10) 0.037(9) C65 0.051(9) 0.072(10) 0.142(14) 0.026(10) -0.006(9) 0.025(8) C66 0.050(7) 0.043(7) 0.052(7) -0.002(6) 0.001(6) 0.017(6) C67 0.025(6) 0.031(6) 0.040(6) -0.007(5) 0.000(5) 0.009(5) C68 0.064(9) 0.082(10) 0.080(10) 0.002(8) 0.021(8) 0.034(8) C69 0.090(11) 0.088(11) 0.178(17) 0.068(11) 0.081(12) 0.064(10) C70 0.107(14) 0.116(16) 0.17(2) -0.017(14) 0.086(14) 0.007(12) C71 0.144(16) 0.066(11) 0.122(15) -0.014(10) 0.038(13) 0.040(12) C72 0.069(10) 0.074(11) 0.113(13) -0.021(10) -0.007(9) 0.036(9) C73 0.30(3) 0.117(17) 0.16(2) 0.048(15) 0.13(2) 0.13(2) C74 0.25(3) 0.127(17) 0.136(17) 0.056(14) 0.140(19) 0.111(18) C75 0.042(9) 0.072(10) 0.137(16) -0.028(10) 0.006(10) 0.005(8) C76 0.114(16) 0.139(16) 0.068(12) -0.018(11) -0.010(11) 0.040(13) C77 0.065(12) 0.22(2) 0.129(19) -0.074(17) 0.026(12) 0.008(14) C78 0.134(15) 0.086(12) 0.105(13) 0.013(10) 0.025(13) 0.077(12) N1 0.037(5) 0.044(5) 0.044(5) -0.008(4) -0.018(4) 0.023(5) N2 0.036(5) 0.034(5) 0.047(5) -0.007(4) -0.013(4) 0.019(4) N3 0.031(5) 0.021(5) 0.030(5) -0.005(4) -0.007(4) 0.005(4) N4 0.038(5) 0.030(5) 0.028(4) -0.014(4) -0.013(4) 0.017(4) N5 0.031(5) 0.032(5) 0.031(5) -0.012(4) -0.018(4) 0.017(4) N6 0.019(4) 0.030(5) 0.030(4) -0.002(4) -0.001(4) 0.012(4) N7 0.027(5) 0.028(5) 0.024(4) -0.004(4) -0.004(4) 0.016(4) N8 0.034(5) 0.029(5) 0.024(4) 0.001(4) -0.002(4) 0.015(4) N9 0.031(5) 0.028(5) 0.021(4) 0.010(4) 0.010(4) 0.015(4) N10 0.052(6) 0.036(5) 0.034(5) 0.004(4) 0.001(4) 0.028(5) O1 0.078(7) 0.083(7) 0.083(7) -0.029(6) -0.004(6) 0.026(6) O2 0.097(7) 0.071(6) 0.075(7) -0.005(5) -0.007(6) 0.041(6) Cr1 0.0315(9) 0.0313(9) 0.0414(10) -0.0107(8) -0.0163(8) 0.0166(8) Cr2 0.0272(9) 0.0355(9) 0.0254(8) 0.0013(7) 0.0001(7) 0.0185(8) Br1 0.0403(7) 0.0424(7) 0.0532(7) -0.0178(5) -0.0165(5) 0.0179(6) Br2 0.0464(7) 0.0464(7) 0.0456(7) -0.0003(5) -0.0129(5) 0.0139(6) Br3 0.0258(6) 0.0634(8) 0.0257(5) 0.0067(5) 0.0001(4) 0.0187(5) Br4 0.0451(7) 0.0723(8) 0.0371(6) 0.0044(6) -0.0020(5) 0.0397(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 C2 C63 1.559(14) . ? C3 C63 1.526(15) . ? C1 N6 1.339(11) . ? C1 C5 1.384(12) . ? C1 N7 1.396(11) . ? C4 C21 1.384(12) . ? C4 C18 1.393(12) . ? C4 N9 1.466(11) . ? C5 C6 1.392(12) . ? C6 C45 1.389(12) . ? C7 C8 1.330(12) . ? C7 N7 1.391(11) . ? C8 N9 1.408(11) . ? C9 N5 1.340(11) . ? C9 N4 1.409(12) . ? C9 Cr1 2.125(10) . ? C10 C38 1.369(13) . ? C10 C24 1.377(14) . ? C11 N9 1.361(11) . ? C11 N7 1.386(11) . ? C11 Cr2 2.129(9) . ? C12 C42 1.512(14) . ? C12 C35 1.520(15) . ? C12 C61 1.534(15) . ? C13 C44 1.392(14) . ? C13 C41 1.400(15) . ? C13 C40 1.475(15) . ? C14 C17 1.343(13) . ? C14 N4 1.380(11) . ? C15 N3 1.336(11) . ? C15 C22 1.377(12) . ? C15 N4 1.417(11) . ? C16 C37 1.334(13) . ? C16 N10 1.382(12) . ? C17 N5 1.392(11) . ? C18 C36 1.387(13) . ? C18 C63 1.499(13) . ? C19 C22 1.382(13) . ? C19 C34 1.394(13) . ? C20 C33 1.371(13) . ? C20 C29 1.394(15) . ? C20 C56 1.532(13) . ? C21 C67 1.359(13) . ? C21 C48 1.516(13) . ? C23 C31 1.509(15) . ? C23 C59 1.515(16) . ? C23 C70 1.525(19) . ? C24 C27 1.368(14) . ? C25 N3 1.343(11) . ? C25 C34 1.363(13) . ? C25 N2 1.407(12) . ? C26 N1 1.367(12) . ? C26 N2 1.387(12) . ? C26 Cr1 2.122(10) . ? C27 C42 1.415(13) . ? C28 C30 1.339(13) . ? C28 N1 1.410(12) . ? C29 C62 1.370(16) . ? C30 N2 1.401(12) . ? C31 C58 1.384(15) . ? C31 C33 1.404(13) . ? C32 N6 1.342(11) . ? C32 C45 1.375(12) . ? C32 N8 1.415(11) . ? C33 N10 1.455(12) . ? C36 C43 1.389(14) . ? C37 N8 1.394(12) . ? C38 C51 1.409(13) . ? C38 C52 1.492(14) . ? C39 C48 1.482(14) . ? C40 C55 1.477(15) . ? C40 C57 1.507(15) . ? C41 C54 1.387(16) . ? C42 C51 1.399(13) . ? C43 C67 1.360(13) . ? C44 C47 1.378(14) . ? C44 N1 1.440(12) . ? C46 N10 1.348(11) . ? C46 N8 1.391(11) . ? C46 Cr2 2.156(10) . ? C47 C53 1.397(14) . ? C47 C66 1.518(14) . ? C48 C49 1.537(15) . ? C50 C56 1.495(15) . ? C51 N5 1.452(11) . ? C52 C64 1.509(15) . ? C52 C65 1.557(15) . ? C53 C54 1.378(15) . ? C56 C60 1.516(15) . ? C58 C62 1.375(17) . ? C66 C68 1.508(15) . ? C66 C69 1.516(16) . ? C71 C73 1.41(2) . ? C71 C72 1.472(19) . ? C72 O2 1.430(15) . ? C73 C74 1.42(2) . ? C74 O2 1.410(16) . ? C75 O1 1.389(16) . ? C75 C76 1.48(2) . ? C76 C77 1.46(2) . ? C77 C78 1.41(2) . ? C78 O1 1.434(16) . ? C79 C82 1.45(3) . ? C79 O3 1.53(3) . ? C80 C81 1.29(3) . ? C80 O3 1.37(3) . ? C81 C82 1.63(3) . ? N3 Cr1 2.070(7) . ? N6 Cr2 2.059(7) . ? Cr1 Br1 2.4516(18) . ? Cr1 Br2 2.657(2) . ? Cr2 Br4 2.4421(17) . ? Cr2 Br3 2.6312(17) . ? 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 N6 C1 C5 121.8(8) . . ? N6 C1 N7 112.7(7) . . ? C5 C1 N7 125.5(9) . . ? C21 C4 C18 124.3(8) . . ? C21 C4 N9 119.3(8) . . ? C18 C4 N9 116.1(8) . . ? C1 C5 C6 117.8(9) . . ? C45 C6 C5 121.0(9) . . ? C8 C7 N7 106.8(8) . . ? C7 C8 N9 106.7(8) . . ? N5 C9 N4 102.1(8) . . ? N5 C9 Cr1 146.0(7) . . ? N4 C9 Cr1 111.7(6) . . ? C38 C10 C24 121.6(10) . . ? N9 C11 N7 102.1(7) . . ? N9 C11 Cr2 146.0(7) . . ? N7 C11 Cr2 111.9(6) . . ? C42 C12 C35 111.6(9) . . ? C42 C12 C61 112.1(9) . . ? C35 C12 C61 110.6(10) . . ? C44 C13 C41 116.2(10) . . ? C44 C13 C40 122.9(10) . . ? C41 C13 C40 120.9(11) . . ? C17 C14 N4 106.4(9) . . ? N3 C15 C22 124.0(9) . . ? N3 C15 N4 111.9(8) . . ? C22 C15 N4 124.1(9) . . ? C37 C16 N10 108.7(9) . . ? C14 C17 N5 107.0(9) . . ? C36 C18 C4 116.1(9) . . ? C36 C18 C63 121.0(9) . . ? C4 C18 C63 122.7(8) . . ? C22 C19 C34 122.1(9) . . ? C33 C20 C29 117.2(9) . . ? C33 C20 C56 122.4(9) . . ? C29 C20 C56 120.4(9) . . ? C67 C21 C4 115.9(8) . . ? C67 C21 C48 121.2(9) . . ? C4 C21 C48 122.9(8) . . ? C15 C22 C19 115.7(9) . . ? C31 C23 C59 112.0(11) . . ? C31 C23 C70 110.6(11) . . ? C59 C23 C70 109.9(12) . . ? C27 C24 C10 121.9(10) . . ? N3 C25 C34 122.9(9) . . ? N3 C25 N2 110.3(8) . . ? C34 C25 N2 126.8(9) . . ? N1 C26 N2 103.4(8) . . ? N1 C26 Cr1 143.6(7) . . ? N2 C26 Cr1 113.0(7) . . ? C24 C27 C42 119.8(10) . . ? C30 C28 N1 107.5(9) . . ? C62 C29 C20 120.7(11) . . ? C28 C30 N2 106.5(9) . . ? C58 C31 C33 116.4(10) . . ? C58 C31 C23 121.3(10) . . ? C33 C31 C23 122.3(9) . . ? N6 C32 C45 123.5(8) . . ? N6 C32 N8 111.3(8) . . ? C45 C32 N8 125.2(8) . . ? C20 C33 C31 123.5(9) . . ? C20 C33 N10 118.7(9) . . ? C31 C33 N10 117.7(9) . . ? C25 C34 C19 116.9(10) . . ? C18 C36 C43 121.0(9) . . ? C16 C37 N8 105.0(9) . . ? C10 C38 C51 116.5(10) . . ? C10 C38 C52 121.8(10) . . ? C51 C38 C52 121.6(9) . . ? C13 C40 C55 111.5(9) . . ? C13 C40 C57 114.2(10) . . ? C55 C40 C57 110.5(10) . . ? C54 C41 C13 119.6(11) . . ? C51 C42 C27 116.5(9) . . ? C51 C42 C12 123.6(9) . . ? C27 C42 C12 119.9(10) . . ? C67 C43 C36 119.1(9) . . ? C47 C44 C13 125.6(10) . . ? C47 C44 N1 118.5(10) . . ? C13 C44 N1 115.8(10) . . ? C32 C45 C6 116.6(9) . . ? N10 C46 N8 102.7(8) . . ? N10 C46 Cr2 145.8(7) . . ? N8 C46 Cr2 111.2(6) . . ? C44 C47 C53 116.3(10) . . ? C44 C47 C66 123.9(10) . . ? C53 C47 C66 119.8(10) . . ? C39 C48 C21 111.1(9) . . ? C39 C48 C49 111.1(9) . . ? C21 C48 C49 111.3(9) . . ? C42 C51 C38 123.7(9) . . ? C42 C51 N5 117.8(8) . . ? C38 C51 N5 118.3(9) . . ? C38 C52 C64 112.5(9) . . ? C38 C52 C65 112.3(9) . . ? C64 C52 C65 107.2(10) . . ? C54 C53 C47 120.1(11) . . ? C53 C54 C41 122.1(11) . . ? C50 C56 C60 112.5(10) . . ? C50 C56 C20 111.9(10) . . ? C60 C56 C20 110.2(9) . . ? C62 C58 C31 121.1(11) . . ? C29 C62 C58 120.6(11) . . ? C18 C63 C3 109.5(9) . . ? C18 C63 C2 112.9(9) . . ? C3 C63 C2 110.4(8) . . ? C68 C66 C47 115.6(10) . . ? C68 C66 C69 109.6(11) . . ? C47 C66 C69 110.0(9) . . ? C21 C67 C43 123.5(9) . . ? C73 C71 C72 104.5(14) . . ? O2 C72 C71 106.7(12) . . ? C74 C73 C71 107.1(16) . . ? O2 C74 C73 110.1(15) . . ? O1 C75 C76 107.5(13) . . ? C77 C76 C75 106.1(15) . . ? C78 C77 C76 105.6(15) . . ? C77 C78 O1 110.4(15) . . ? C82 C79 O3 113(2) . . ? C81 C80 O3 115(3) . . ? C80 C81 C82 110(3) . . ? C79 C82 C81 95(2) . . ? C26 N1 C28 111.1(8) . . ? C26 N1 C44 125.1(8) . . ? C28 N1 C44 123.8(8) . . ? C26 N2 C30 111.5(8) . . ? C26 N2 C25 119.2(8) . . ? C30 N2 C25 129.0(8) . . ? C15 N3 C25 118.4(8) . . ? C15 N3 Cr1 119.9(6) . . ? C25 N3 Cr1 121.2(6) . . ? C14 N4 C9 111.6(8) . . ? C14 N4 C15 129.6(8) . . ? C9 N4 C15 118.7(8) . . ? C9 N5 C17 112.9(8) . . ? C9 N5 C51 124.4(8) . . ? C17 N5 C51 122.6(8) . . ? C1 N6 C32 119.2(8) . . ? C1 N6 Cr2 119.5(6) . . ? C32 N6 Cr2 121.1(6) . . ? C11 N7 C7 112.2(7) . . ? C11 N7 C1 119.1(7) . . ? C7 N7 C1 128.6(8) . . ? C46 N8 C37 111.9(8) . . ? C46 N8 C32 119.4(8) . . ? C37 N8 C32 128.4(8) . . ? C11 N9 C8 112.2(7) . . ? C11 N9 C4 126.6(7) . . ? C8 N9 C4 121.1(7) . . ? C46 N10 C16 111.7(8) . . ? C46 N10 C33 122.4(8) . . ? C16 N10 C33 125.9(8) . . ? C75 O1 C78 108.0(12) . . ? C74 O2 C72 105.2(12) . . ? C80 O3 C79 99(2) . . ? N3 Cr1 C26 74.9(4) . . ? N3 Cr1 C9 76.3(4) . . ? C26 Cr1 C9 147.9(4) . . ? N3 Cr1 Br1 165.1(2) . . ? C26 Cr1 Br1 103.1(3) . . ? C9 Cr1 Br1 101.0(3) . . ? N3 Cr1 Br2 88.0(2) . . ? C26 Cr1 Br2 99.3(3) . . ? C9 Cr1 Br2 93.7(2) . . ? Br1 Cr1 Br2 106.82(7) . . ? N6 Cr2 C11 76.2(3) . . ? N6 Cr2 C46 75.6(3) . . ? C11 Cr2 C46 149.2(3) . . ? N6 Cr2 Br4 166.1(2) . . ? C11 Cr2 Br4 101.9(3) . . ? C46 Cr2 Br4 102.4(2) . . ? N6 Cr2 Br3 92.7(2) . . ? C11 Cr2 Br3 94.6(2) . . ? C46 Cr2 Br3 98.9(2) . . ? Br4 Cr2 Br3 101.26(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.669 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.122 #==END data_3 _database_code_depnum_ccdc_archive 'CCDC 282401' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Br2 Mn, C4 H8 O' _chemical_formula_sum 'C39 H49 Br2 Mn N5 O' _chemical_formula_weight 818.59 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6948(8) _cell_length_b 18.7188(14) _cell_length_c 19.2039(19) _cell_angle_alpha 90.00 _cell_angle_beta 93.796(9) _cell_angle_gamma 90.00 _cell_volume 3836.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used 8393 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1684 _exptl_absorpt_coefficient_mu 2.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5779 _exptl_absorpt_correction_T_max 0.5779 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(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 26916 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6754 _reflns_number_gt 4385 _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 diffraction pattern clearly shows discontinuous planes of diffuse scattering at h+0.5kl indicating significant disorder of the molecules within the crystal. From initial refinements it was obvious that the manganese and bromine sites were split over 2 positions and to retain chemically sensible geometry around the core it was necessary to refine the structure with whole molecule disorder. This entailed the use of geometrical and thermal parameter restraints, but some less than ideal features remain and the refinement would not fully converge. As the model clearly does not account for the diffuse scattering some imperfections in the refinement are inevitable. ; _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^)+(0.0921P)^2^+25.8973P] 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 6754 _refine_ls_number_parameters 415 _refine_ls_number_restraints 1413 _refine_ls_R_factor_all 0.1373 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2333 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.006 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 O1A O 0.8290(4) 0.57864(18) 0.1033(2) 0.0600(9) Uani 0.5027(19) 1 d PU A 1 C41A C 1.0469(5) 0.6081(3) 0.1011(2) 0.0680(7) Uani 0.5027(19) 1 d PDU A 1 H41A H 1.1145 0.5719 0.1037 0.082 Uiso 0.5027(19) 1 calc PR A 1 H41B H 1.0789 0.6524 0.0805 0.082 Uiso 0.5027(19) 1 calc PR A 1 C40A C 1.0004(5) 0.6230(3) 0.1745(3) 0.0680(7) Uani 0.5027(19) 1 d PDU A 1 H40A H 0.9590 0.6700 0.1778 0.082 Uiso 0.5027(19) 1 calc PR A 1 H40B H 1.0671 0.6174 0.2124 0.082 Uiso 0.5027(19) 1 calc PR A 1 C43A C 0.9017(6) 0.5565(3) 0.1701(4) 0.0680(7) Uani 0.5027(19) 1 d PU A 1 H43A H 0.9440 0.5099 0.1655 0.082 Uiso 0.5027(19) 1 calc PR A 1 H43B H 0.8486 0.5554 0.2104 0.082 Uiso 0.5027(19) 1 calc PR A 1 C42A C 0.9289(5) 0.5797(3) 0.0568(4) 0.0680(7) Uani 0.5027(19) 1 d PU A 1 H42A H 0.9077 0.6117 0.0167 0.082 Uiso 0.5027(19) 1 calc PR A 1 H42B H 0.9445 0.5312 0.0390 0.082 Uiso 0.5027(19) 1 calc PR A 1 O1B O 0.8849(4) 0.59630(19) 0.1715(2) 0.0600(9) Uani 0.4973(19) 1 d PU A 2 C41B C 1.0729(4) 0.5714(2) 0.1035(3) 0.0680(7) Uani 0.4973(19) 1 d PDU A 2 H41C H 1.0898 0.5797 0.0541 0.082 Uiso 0.4973(19) 1 calc PR A 2 H41D H 1.1530 0.5643 0.1315 0.082 Uiso 0.4973(19) 1 calc PR A 2 C40B C 0.9942(5) 0.6328(3) 0.1331(3) 0.0680(7) Uani 0.4973(19) 1 d PDU A 2 H40C H 0.9595 0.6638 0.0948 0.082 Uiso 0.4973(19) 1 calc PR A 2 H40D H 1.0469 0.6623 0.1662 0.082 Uiso 0.4973(19) 1 calc PR A 2 C43B C 0.9275(5) 0.5228(3) 0.1793(3) 0.0680(7) Uani 0.4973(19) 1 d PDU A 2 H43C H 0.8568 0.4899 0.1859 0.082 Uiso 0.4973(19) 1 calc PR A 2 H43D H 0.9908 0.5177 0.2190 0.082 Uiso 0.4973(19) 1 calc PR A 2 C42B C 0.9836(5) 0.5098(3) 0.1114(3) 0.0680(7) Uani 0.4973(19) 1 d PDU A 2 H42C H 0.9179 0.5092 0.0725 0.082 Uiso 0.4973(19) 1 calc PR A 2 H42D H 1.0289 0.4637 0.1121 0.082 Uiso 0.4973(19) 1 calc PR A 2 Mn1A Mn 0.33394(5) 0.31540(3) 0.09909(3) 0.01994(11) Uani 0.5131(2) 1 d PDU B 3 Br1A Br 0.30778(4) 0.23775(2) 0.20598(2) 0.02917(6) Uani 0.5131(2) 1 d PDU B 3 Br2A Br 0.19558(4) 0.42363(2) 0.06430(2) 0.02917(6) Uani 0.5131(2) 1 d PD B 3 N1A N 0.55073(16) 0.41772(8) 0.19360(8) 0.0263(2) Uani 0.5131(2) 1 d PGU B 3 C14A C 0.6368(2) 0.46752(12) 0.16803(10) 0.0307(3) Uani 0.5131(2) 1 d PGU B 3 H14A H 0.6827 0.5025 0.1949 0.037 Uiso 0.5131(2) 1 calc PR B 3 C15A C 0.6420(3) 0.45592(16) 0.09521(10) 0.0307(3) Uani 0.5131(2) 1 d PGU B 3 H15A H 0.6921 0.4817 0.0648 0.037 Uiso 0.5131(2) 1 calc PR B 3 N2A N 0.5593(3) 0.39894(14) 0.07578(8) 0.0263(2) Uani 0.5131(2) 1 d PGDU B 3 C13A C 0.5028(2) 0.37534(11) 0.13658(9) 0.0275(4) Uani 0.5131(2) 1 d PGU B 3 N3A N 0.43249(14) 0.34187(8) 0.00196(7) 0.0263(2) Uani 0.5131(2) 1 d PGDU B 3 C16A C 0.52116(18) 0.39626(10) 0.00617(9) 0.0281(3) Uani 0.5131(2) 1 d PGDU B 3 C17A C 0.5784(2) 0.41773(13) -0.05326(12) 0.0281(3) Uani 0.5131(2) 1 d PGU B 3 H17A H 0.6390 0.4549 -0.0504 0.034 Uiso 0.5131(2) 1 calc PR B 3 C18A C 0.5470(2) 0.38482(15) -0.11691(10) 0.0281(3) Uani 0.5131(2) 1 d PGU B 3 H18A H 0.5862 0.3995 -0.1575 0.034 Uiso 0.5131(2) 1 calc PR B 3 C19A C 0.4584(2) 0.33043(14) -0.12113(7) 0.0281(3) Uani 0.5131(2) 1 d PGU B 3 H19A H 0.4369 0.3079 -0.1646 0.034 Uiso 0.5131(2) 1 calc PR B 3 C20A C 0.40109(18) 0.30896(10) -0.06169(8) 0.0281(3) Uani 0.5131(2) 1 d PGDU B 3 C1A C 0.54441(14) 0.39534(8) 0.25459(8) 0.0198(4) Uani 0.5131(2) 1 d PGU B 3 C2A C 0.44394(16) 0.42338(12) 0.28797(9) 0.0198(4) Uani 0.5131(2) 1 d PGU B 3 C3A C 0.4316(2) 0.40893(15) 0.35817(10) 0.0178(9) Uani 0.5131(2) 1 d PGU B 3 H3A H 0.3629 0.4281 0.3810 0.021 Uiso 0.5131(2) 1 calc PR B 3 C5A C 0.5196(3) 0.36643(15) 0.39500(8) 0.0206(10) Uani 0.5131(2) 1 d PGU B 3 H5A H 0.5112 0.3566 0.4430 0.025 Uiso 0.5131(2) 1 calc PR B 3 C4A C 0.6201(2) 0.33840(13) 0.36162(10) 0.0254(11) Uani 0.5131(2) 1 d PGU B 3 H4A H 0.6803 0.3094 0.3868 0.030 Uiso 0.5131(2) 1 calc PR B 3 C6A C 0.63250(18) 0.35285(11) 0.29141(9) 0.0198(4) Uani 0.5131(2) 1 d PGU B 3 N4A N 0.29749(15) 0.27122(8) -0.05186(9) 0.0263(2) Uani 0.5131(2) 1 d PGDU B 3 C22A C 0.2274(2) 0.23493(11) -0.10639(10) 0.0307(3) Uani 0.5131(2) 1 d PGU B 3 H22A H 0.2375 0.2399 -0.1549 0.037 Uiso 0.5131(2) 1 calc PR B 3 C23A C 0.1396(2) 0.18984(12) -0.07564(16) 0.0307(3) Uani 0.5131(2) 1 d PGU B 3 H23A H 0.0806 0.1594 -0.1000 0.037 Uiso 0.5131(2) 1 calc PR B 3 N5A N 0.1554(2) 0.19827(13) -0.00210(15) 0.0263(2) Uani 0.5131(2) 1 d PGU B 3 C21A C 0.2530(2) 0.24856(12) 0.01260(10) 0.0275(4) Uani 0.5131(2) 1 d PGU B 3 C24A C 0.10438(8) 0.15763(2) 0.04618(5) 0.0338(11) Uani 0.5131(2) 1 d PGU B 3 C25A C 0.14879(9) 0.09296(3) 0.07344(6) 0.0347(12) Uani 0.5131(2) 1 d PGU B 3 C26A C 0.08570(12) 0.05867(4) 0.12490(7) 0.0430(13) Uani 0.5131(2) 1 d PGU B 3 H26A H 0.1161 0.0145 0.1435 0.052 Uiso 0.5131(2) 1 calc PR B 3 C27A C -0.02180(12) 0.08906(6) 0.14911(7) 0.0391(12) Uani 0.5131(2) 1 d PGU B 3 H27A H -0.0649 0.0656 0.1843 0.047 Uiso 0.5131(2) 1 calc PR B 3 C28A C -0.06621(10) 0.15373(6) 0.12185(7) 0.0485(14) Uani 0.5131(2) 1 d PGU B 3 H28A H -0.1397 0.1745 0.1384 0.058 Uiso 0.5131(2) 1 calc PR B 3 C29A C -0.00312(9) 0.18801(3) 0.07039(6) 0.0399(12) Uani 0.5131(2) 1 d PGDU B 3 C7A C 0.7399(4) 0.3164(2) 0.2557(2) 0.0384(4) Uani 0.5131(2) 1 d PU B 3 H7A H 0.7292 0.3301 0.2054 0.046 Uiso 0.5131(2) 1 calc PR B 3 C11A C 0.3388(4) 0.5436(2) 0.2800(2) 0.0318(4) Uani 0.5131(2) 1 d PU B 3 H11A H 0.3164 0.5440 0.3286 0.048 Uiso 0.5131(2) 1 calc PR B 3 H11B H 0.2777 0.5720 0.2515 0.048 Uiso 0.5131(2) 1 calc PR B 3 H11C H 0.4225 0.5642 0.2771 0.048 Uiso 0.5131(2) 1 calc PR B 3 C12A C 0.2106(4) 0.4374(2) 0.2535(2) 0.0318(4) Uani 0.5131(2) 1 d PU B 3 H12A H 0.1832 0.4386 0.3012 0.048 Uiso 0.5131(2) 1 calc PR B 3 H12B H 0.2099 0.3879 0.2367 0.048 Uiso 0.5131(2) 1 calc PR B 3 H12C H 0.1535 0.4662 0.2230 0.048 Uiso 0.5131(2) 1 calc PR B 3 C10A C 0.3381(4) 0.4663(2) 0.2529(2) 0.0384(4) Uani 0.5131(2) 1 d PU B 3 H10A H 0.3566 0.4696 0.2026 0.046 Uiso 0.5131(2) 1 calc PR B 3 C9A C 0.8644(4) 0.3504(2) 0.2842(2) 0.0318(4) Uani 0.5131(2) 1 d PU B 3 H9A1 H 0.8809 0.3374 0.3333 0.048 Uiso 0.5131(2) 1 calc PR B 3 H9A2 H 0.8586 0.4025 0.2800 0.048 Uiso 0.5131(2) 1 calc PR B 3 H9A3 H 0.9329 0.3330 0.2572 0.048 Uiso 0.5131(2) 1 calc PR B 3 C8A C 0.7333(4) 0.2382(2) 0.2576(2) 0.0318(4) Uani 0.5131(2) 1 d PU B 3 H8A1 H 0.7491 0.2217 0.3058 0.048 Uiso 0.5131(2) 1 calc PR B 3 H8A2 H 0.7967 0.2181 0.2286 0.048 Uiso 0.5131(2) 1 calc PR B 3 H8A3 H 0.6499 0.2226 0.2397 0.048 Uiso 0.5131(2) 1 calc PR B 3 C30A C 0.2571(4) 0.0589(2) 0.0512(2) 0.0367(12) Uani 0.5131(2) 1 d PU B 3 H30A H 0.3013 0.0962 0.0249 0.044 Uiso 0.5131(2) 1 calc PR B 3 C31A C 0.2559(4) -0.0044(3) 0.0071(2) 0.0419(14) Uani 0.5131(2) 1 d PU B 3 H31A H 0.2172 -0.0442 0.0310 0.063 Uiso 0.5131(2) 1 calc PR B 3 H31B H 0.3421 -0.0171 -0.0023 0.063 Uiso 0.5131(2) 1 calc PR B 3 H31C H 0.2077 0.0055 -0.0370 0.063 Uiso 0.5131(2) 1 calc PR B 3 C32A C 0.3564(4) 0.0372(3) 0.1179(2) 0.0472(15) Uani 0.5131(2) 1 d PU B 3 H32A H 0.3715 0.0789 0.1481 0.071 Uiso 0.5131(2) 1 calc PR B 3 H32B H 0.4358 0.0213 0.1003 0.071 Uiso 0.5131(2) 1 calc PR B 3 H32C H 0.3207 -0.0015 0.1447 0.071 Uiso 0.5131(2) 1 calc PR B 3 C33A C -0.05977(3) 0.257656(18) 0.03945(2) 0.0384(4) Uani 0.5131(2) 1 d PDU B 3 H33A H -0.0055 0.2763 0.0031 0.046 Uiso 0.5131(2) 1 calc PR B 3 C34A C -0.0680(2) 0.31372(3) 0.09765(3) 0.08822(17) Uani 0.5131(2) 1 d PDU B 3 H34A H -0.1243 0.3524 0.0812 0.132 Uiso 0.5131(2) 1 calc PR B 3 H34B H 0.0156 0.3332 0.1100 0.132 Uiso 0.5131(2) 1 calc PR B 3 H34C H -0.1007 0.2912 0.1388 0.132 Uiso 0.5131(2) 1 calc PR B 3 C35A C -0.19276(3) 0.24402(10) 0.00643(5) 0.08822(17) Uani 0.5131(2) 1 d PDU B 3 H35A H -0.2480 0.2302 0.0429 0.132 Uiso 0.5131(2) 1 calc PR B 3 H35B H -0.1902 0.2055 -0.0280 0.132 Uiso 0.5131(2) 1 calc PR B 3 H35C H -0.2248 0.2877 -0.0166 0.132 Uiso 0.5131(2) 1 calc PR B 3 Mn1B Mn 0.37477(5) 0.27146(3) 0.11024(3) 0.01994(11) Uani 0.4869(2) 1 d PDU B 4 Br1B Br 0.25096(4) 0.23618(2) 0.21151(2) 0.02917(6) Uani 0.4869(2) 1 d PDU B 4 Br2B Br 0.56385(4) 0.19385(2) 0.09742(2) 0.02917(6) Uani 0.4869(2) 1 d PD B 4 N1B N 0.54929(18) 0.40200(9) 0.19479(8) 0.0263(2) Uani 0.4869(2) 1 d PGU B 4 C14B C 0.6396(2) 0.45483(13) 0.18094(11) 0.0307(3) Uani 0.4869(2) 1 d PGU B 4 H14B H 0.6919 0.4796 0.2148 0.037 Uiso 0.4869(2) 1 calc PR B 4 C15B C 0.6381(3) 0.46420(15) 0.10751(12) 0.0307(3) Uani 0.4869(2) 1 d PGU B 4 H15B H 0.6892 0.4963 0.0837 0.037 Uiso 0.4869(2) 1 calc PR B 4 N2B N 0.5469(3) 0.41715(14) 0.07598(9) 0.0263(2) Uani 0.4869(2) 1 d PGDU B 4 C13B C 0.4920(2) 0.37871(12) 0.12993(9) 0.0275(4) Uani 0.4869(2) 1 d PGU B 4 N3B N 0.42700(16) 0.33317(8) 0.01114(8) 0.0263(2) Uani 0.4869(2) 1 d PGDU B 4 C16B C 0.52989(19) 0.37869(11) 0.01576(10) 0.0281(3) Uani 0.4869(2) 1 d PGDU B 4 C17B C 0.5828(2) 0.40160(15) -0.04455(13) 0.0281(3) Uani 0.4869(2) 1 d PGU B 4 H17B H 0.6531 0.4327 -0.0414 0.034 Uiso 0.4869(2) 1 calc PR B 4 C18B C 0.5328(3) 0.37898(16) -0.10949(11) 0.0281(3) Uani 0.4869(2) 1 d PGU B 4 H18B H 0.5689 0.3946 -0.1507 0.034 Uiso 0.4869(2) 1 calc PR B 4 C19B C 0.4299(3) 0.33346(14) -0.11411(8) 0.0281(3) Uani 0.4869(2) 1 d PGU B 4 H19B H 0.3957 0.3180 -0.1585 0.034 Uiso 0.4869(2) 1 calc PR B 4 C20B C 0.37699(19) 0.31055(10) -0.05380(8) 0.0281(3) Uani 0.4869(2) 1 d PGDU B 4 C1B C 0.51880(16) 0.38907(10) 0.26670(9) 0.0198(4) Uani 0.4869(2) 1 d PGU B 4 C2B C 0.41793(18) 0.41727(13) 0.29961(11) 0.0198(4) Uani 0.4869(2) 1 d PGU B 4 C3B C 0.4050(2) 0.40333(17) 0.36986(11) 0.0225(11) Uani 0.4869(2) 1 d PGU B 4 H3B H 0.3361 0.4226 0.3923 0.027 Uiso 0.4869(2) 1 calc PR B 4 C4B C 0.4929(3) 0.36118(17) 0.40721(9) 0.0283(12) Uani 0.4869(2) 1 d PGU B 4 H4B H 0.4841 0.3517 0.4552 0.034 Uiso 0.4869(2) 1 calc PR B 4 C5B C 0.5938(3) 0.33298(15) 0.37430(11) 0.0236(11) Uani 0.4869(2) 1 d PGU B 4 H5B H 0.6539 0.3042 0.3998 0.028 Uiso 0.4869(2) 1 calc PR B 4 C6B C 0.6067(2) 0.34692(13) 0.30405(10) 0.0198(4) Uani 0.4869(2) 1 d PGU B 4 N4B N 0.29753(17) 0.25569(8) -0.05282(10) 0.0263(2) Uani 0.4869(2) 1 d PGDU B 4 C22B C 0.2230(2) 0.21983(12) -0.10586(12) 0.0307(3) Uani 0.4869(2) 1 d PGU B 4 H22B H 0.2300 0.2245 -0.1547 0.037 Uiso 0.4869(2) 1 calc PR B 4 C23B C 0.1361(2) 0.17581(13) -0.07307(18) 0.0307(3) Uani 0.4869(2) 1 d PGU B 4 H23B H 0.0748 0.1458 -0.0961 0.037 Uiso 0.4869(2) 1 calc PR B 4 N5B N 0.1570(3) 0.18446(14) 0.00024(17) 0.0263(2) Uani 0.4869(2) 1 d PGU B 4 C21B C 0.2567(2) 0.23383(12) 0.01276(11) 0.0275(4) Uani 0.4869(2) 1 d PGU B 4 C7B C 0.7208(4) 0.3152(3) 0.2695(2) 0.0384(4) Uani 0.4869(2) 1 d PU B 4 H7B H 0.7127 0.3253 0.2182 0.046 Uiso 0.4869(2) 1 calc PR B 4 C11B C 0.3404(4) 0.5439(3) 0.2800(2) 0.0318(4) Uani 0.4869(2) 1 d PU B 4 H11D H 0.2786 0.5746 0.2547 0.048 Uiso 0.4869(2) 1 calc PR B 4 H11E H 0.4250 0.5594 0.2704 0.048 Uiso 0.4869(2) 1 calc PR B 4 H11F H 0.3299 0.5472 0.3302 0.048 Uiso 0.4869(2) 1 calc PR B 4 C24B C 0.09121(10) 0.15476(2) 0.04777(7) 0.0266(11) Uani 0.4869(2) 1 d PGU B 4 C25B C 0.14100(10) 0.08945(3) 0.07011(8) 0.0330(12) Uani 0.4869(2) 1 d PGU B 4 C26B C 0.07679(13) 0.04702(4) 0.11523(9) 0.0392(13) Uani 0.4869(2) 1 d PGU B 4 H26B H 0.1108 0.0024 0.1305 0.047 Uiso 0.4869(2) 1 calc PR B 4 C27B C -0.03722(15) 0.06990(6) 0.13801(9) 0.0399(13) Uani 0.4869(2) 1 d PGU B 4 H27B H -0.0811 0.0409 0.1689 0.048 Uiso 0.4869(2) 1 calc PR B 4 C28B C -0.08701(13) 0.13522(5) 0.11567(9) 0.0414(13) Uani 0.4869(2) 1 d PGU B 4 H28B H -0.1649 0.1509 0.1312 0.050 Uiso 0.4869(2) 1 calc PR B 4 C29B C -0.02279(10) 0.17765(3) 0.07055(8) 0.0402(13) Uani 0.4869(2) 1 d PGDU B 4 C12B C 0.1907(4) 0.4358(3) 0.2691(2) 0.0318(4) Uani 0.4869(2) 1 d PU B 4 H12D H 0.1832 0.3883 0.2479 0.048 Uiso 0.4869(2) 1 calc PR B 4 H12E H 0.1250 0.4670 0.2481 0.048 Uiso 0.4869(2) 1 calc PR B 4 H12F H 0.1815 0.4320 0.3194 0.048 Uiso 0.4869(2) 1 calc PR B 4 C10B C 0.3212(5) 0.4677(3) 0.2563(3) 0.0384(4) Uani 0.4869(2) 1 d PU B 4 H10B H 0.3360 0.4641 0.2056 0.046 Uiso 0.4869(2) 1 calc PR B 4 C9B C 0.8416(4) 0.3425(3) 0.2989(2) 0.0318(4) Uani 0.4869(2) 1 d PU B 4 H9B1 H 0.8517 0.3923 0.2845 0.048 Uiso 0.4869(2) 1 calc PR B 4 H9B2 H 0.9096 0.3136 0.2818 0.048 Uiso 0.4869(2) 1 calc PR B 4 H9B3 H 0.8442 0.3398 0.3499 0.048 Uiso 0.4869(2) 1 calc PR B 4 C8B C 0.7217(4) 0.2304(2) 0.2817(2) 0.0318(4) Uani 0.4869(2) 1 d PU B 4 H8B1 H 0.7803 0.2080 0.2512 0.048 Uiso 0.4869(2) 1 calc PR B 4 H8B2 H 0.6373 0.2113 0.2709 0.048 Uiso 0.4869(2) 1 calc PR B 4 H8B3 H 0.7480 0.2201 0.3305 0.048 Uiso 0.4869(2) 1 calc PR B 4 C30B C 0.2728(4) 0.0604(3) 0.0410(3) 0.0329(13) Uani 0.4869(2) 1 d PU B 4 H30B H 0.2976 0.0931 0.0032 0.039 Uiso 0.4869(2) 1 calc PR B 4 C31B C 0.2279(5) -0.0157(2) 0.0059(3) 0.0424(15) Uani 0.4869(2) 1 d PU B 4 H31D H 0.2999 -0.0397 -0.0128 0.064 Uiso 0.4869(2) 1 calc PR B 4 H31E H 0.1636 -0.0070 -0.0319 0.064 Uiso 0.4869(2) 1 calc PR B 4 H31F H 0.1931 -0.0461 0.0415 0.064 Uiso 0.4869(2) 1 calc PR B 4 C32B C 0.3705(5) 0.0606(2) 0.0962(3) 0.0438(15) Uani 0.4869(2) 1 d PU B 4 H32D H 0.3831 0.1094 0.1138 0.066 Uiso 0.4869(2) 1 calc PR B 4 H32E H 0.4484 0.0430 0.0783 0.066 Uiso 0.4869(2) 1 calc PR B 4 H32F H 0.3465 0.0295 0.1342 0.066 Uiso 0.4869(2) 1 calc PR B 4 C33B C -0.06741(12) 0.25351(2) 0.05022(9) 0.0384(4) Uani 0.4869(2) 1 d PDU B 4 H33B H 0.0123 0.2698 0.0308 0.046 Uiso 0.4869(2) 1 calc PR B 4 C34B C -0.0739(6) 0.3070(3) 0.09972(18) 0.08822(17) Uani 0.4869(2) 1 d PDU B 4 H34D H -0.0922 0.3527 0.0763 0.132 Uiso 0.4869(2) 1 calc PR B 4 H34E H 0.0065 0.3104 0.1272 0.132 Uiso 0.4869(2) 1 calc PR B 4 H34F H -0.1404 0.2959 0.1307 0.132 Uiso 0.4869(2) 1 calc PR B 4 C35B C -0.1490(5) 0.2592(3) -0.01703(17) 0.08822(17) Uani 0.4869(2) 1 d PDU B 4 H35D H -0.2351 0.2455 -0.0085 0.132 Uiso 0.4869(2) 1 calc PR B 4 H35E H -0.1167 0.2273 -0.0521 0.132 Uiso 0.4869(2) 1 calc PR B 4 H35F H -0.1481 0.3086 -0.0341 0.132 Uiso 0.4869(2) 1 calc PR B 4 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 O1A 0.0620(15) 0.0385(13) 0.0786(18) 0.0162(13) -0.0032(14) 0.0048(12) C41A 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) C40A 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) C43A 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) C42A 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) O1B 0.0620(15) 0.0385(13) 0.0786(18) 0.0162(13) -0.0032(14) 0.0048(12) C41B 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) C40B 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) C43B 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) C42B 0.0617(11) 0.0603(13) 0.0824(14) 0.0089(13) 0.0090(11) -0.0093(10) Mn1A 0.0236(2) 0.0216(2) 0.01444(19) -0.0005(2) -0.00006(16) -0.00101(18) Br1A 0.03223(12) 0.03162(10) 0.02304(9) -0.00026(8) -0.00277(9) 0.00038(10) Br2A 0.03223(12) 0.03162(10) 0.02304(9) -0.00026(8) -0.00277(9) 0.00038(10) N1A 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C14A 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) C15A 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) N2A 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C13A 0.0348(7) 0.0224(8) 0.0234(7) -0.0089(6) -0.0118(6) 0.0181(7) N3A 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C16A 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C17A 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C18A 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C19A 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C20A 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C1A 0.0234(7) 0.0215(6) 0.0146(6) -0.0016(5) 0.0019(5) -0.0017(5) C2A 0.0234(7) 0.0215(6) 0.0146(6) -0.0016(5) 0.0019(5) -0.0017(5) C3A 0.0193(16) 0.0121(16) 0.0232(18) -0.0067(15) 0.0105(14) -0.0066(14) C5A 0.0279(17) 0.0220(18) 0.0119(17) 0.0037(15) 0.0019(15) -0.0145(15) C4A 0.0299(19) 0.0209(18) 0.0246(19) -0.0027(16) -0.0039(17) 0.0029(17) C6A 0.0234(7) 0.0215(6) 0.0146(6) -0.0016(5) 0.0019(5) -0.0017(5) N4A 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C22A 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) C23A 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) N5A 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C21A 0.0348(7) 0.0224(8) 0.0234(7) -0.0089(6) -0.0118(6) 0.0181(7) C24A 0.041(2) 0.044(2) 0.0144(18) 0.0015(18) -0.0134(17) -0.0088(19) C25A 0.0240(18) 0.044(2) 0.034(2) -0.0036(19) -0.0111(17) -0.0003(18) C26A 0.052(2) 0.047(2) 0.028(2) -0.002(2) -0.0154(19) -0.023(2) C27A 0.043(2) 0.060(2) 0.0141(18) -0.0159(18) -0.0021(17) -0.0326(19) C28A 0.036(2) 0.079(3) 0.030(2) -0.011(2) 0.0032(19) -0.014(2) C29A 0.038(2) 0.061(3) 0.0204(19) -0.002(2) -0.0010(18) -0.002(2) C7A 0.0447(7) 0.0481(8) 0.0225(7) -0.0012(6) 0.0023(6) 0.0188(7) C11A 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C12A 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C10A 0.0447(7) 0.0481(8) 0.0225(7) -0.0012(6) 0.0023(6) 0.0188(7) C9A 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C8A 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C30A 0.039(2) 0.033(2) 0.036(2) 0.0040(19) -0.0035(19) -0.0172(19) C31A 0.039(2) 0.052(3) 0.033(2) -0.008(2) -0.014(2) -0.019(2) C32A 0.049(3) 0.043(3) 0.046(3) 0.022(2) -0.027(2) -0.003(2) C33A 0.0447(7) 0.0481(8) 0.0225(7) -0.0012(6) 0.0023(6) 0.0188(7) C34A 0.0885(3) 0.0878(3) 0.0882(3) -0.0001(2) 0.0049(2) -0.0003(2) C35A 0.0885(3) 0.0878(3) 0.0882(3) -0.0001(2) 0.0049(2) -0.0003(2) Mn1B 0.0236(2) 0.0216(2) 0.01444(19) -0.0005(2) -0.00006(16) -0.00101(18) Br1B 0.03223(12) 0.03162(10) 0.02304(9) -0.00026(8) -0.00277(9) 0.00038(10) Br2B 0.03223(12) 0.03162(10) 0.02304(9) -0.00026(8) -0.00277(9) 0.00038(10) N1B 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C14B 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) C15B 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) N2B 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C13B 0.0348(7) 0.0224(8) 0.0234(7) -0.0089(6) -0.0118(6) 0.0181(7) N3B 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C16B 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C17B 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C18B 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C19B 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C20B 0.0382(5) 0.0177(5) 0.0279(5) 0.0020(4) -0.0015(5) 0.0094(4) C1B 0.0234(7) 0.0215(6) 0.0146(6) -0.0016(5) 0.0019(5) -0.0017(5) C2B 0.0234(7) 0.0215(6) 0.0146(6) -0.0016(5) 0.0019(5) -0.0017(5) C3B 0.0258(18) 0.031(2) 0.0119(18) 0.0072(16) 0.0088(15) -0.0102(17) C4B 0.034(2) 0.030(2) 0.022(2) 0.0045(18) 0.0084(18) -0.0106(19) C5B 0.0252(19) 0.033(2) 0.0124(18) 0.0120(17) 0.0011(16) -0.0097(18) C6B 0.0234(7) 0.0215(6) 0.0146(6) -0.0016(5) 0.0019(5) -0.0017(5) N4B 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C22B 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) C23B 0.0537(6) 0.0125(6) 0.0237(6) -0.0042(5) -0.0135(5) 0.0070(5) N5B 0.0440(4) 0.0094(4) 0.0234(4) -0.0039(3) -0.0124(4) 0.0098(4) C21B 0.0348(7) 0.0224(8) 0.0234(7) -0.0089(6) -0.0118(6) 0.0181(7) C7B 0.0447(7) 0.0481(8) 0.0225(7) -0.0012(6) 0.0023(6) 0.0188(7) C11B 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C24B 0.0139(17) 0.039(2) 0.027(2) -0.0036(19) 0.0037(16) -0.0039(18) C25B 0.035(2) 0.030(2) 0.033(2) -0.0105(19) -0.0073(19) -0.0137(19) C26B 0.035(2) 0.044(2) 0.036(2) -0.016(2) -0.0129(19) -0.019(2) C27B 0.042(2) 0.046(2) 0.030(2) -0.0271(19) -0.0110(19) -0.015(2) C28B 0.040(2) 0.055(3) 0.029(2) -0.026(2) 0.006(2) 0.007(2) C29B 0.030(2) 0.068(3) 0.021(2) -0.013(2) -0.0034(18) 0.022(2) C12B 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C10B 0.0447(7) 0.0481(8) 0.0225(7) -0.0012(6) 0.0023(6) 0.0188(7) C9B 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C8B 0.0369(6) 0.0360(6) 0.0232(7) 0.0018(6) 0.0078(6) 0.0012(6) C30B 0.0212(19) 0.037(2) 0.041(2) -0.006(2) 0.0059(19) 0.0115(19) C31B 0.056(3) 0.014(2) 0.054(3) -0.010(2) -0.015(3) -0.007(2) C32B 0.063(3) 0.020(2) 0.047(3) 0.008(2) -0.006(3) 0.021(2) C33B 0.0447(7) 0.0481(8) 0.0225(7) -0.0012(6) 0.0023(6) 0.0188(7) C34B 0.0885(3) 0.0878(3) 0.0882(3) -0.0001(2) 0.0049(2) -0.0003(2) C35B 0.0885(3) 0.0878(3) 0.0882(3) -0.0001(2) 0.0049(2) -0.0003(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 O1A C42A 1.437(7) . ? O1A C43A 1.513(7) . ? C41A C40A 1.549(7) . ? C41A C42A 1.567(8) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C40A C43A 1.630(8) . ? C40A H40A 0.9900 . ? C40A H40B 0.9900 . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? O1B C43B 1.454(7) . ? O1B C40B 1.579(7) . ? C41B C42B 1.512(6) . ? C41B C40B 1.553(7) . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C40B H40C 0.9900 . ? C40B H40D 0.9900 . ? C43B C42B 1.491(7) . ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? Mn1A C13A 2.206(2) . ? Mn1A C21A 2.210(2) . ? Mn1A N3A 2.2574(16) . ? Mn1A Br1A 2.5458(7) . ? Mn1A Br2A 2.5708(7) . ? N1A C1A 1.250(2) . ? N1A C14A 1.4200 . ? N1A C13A 1.4200 . ? C14A C15A 1.4200 . ? C14A H14A 0.9500 . ? C15A N2A 1.4200 . ? C15A H15A 0.9500 . ? N2A C16A 1.372(2) . ? N2A C13A 1.4200 . ? N3A C16A 1.3900 . ? N3A C20A 1.3900 . ? C16A C17A 1.3900 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A C19A 1.3900 . ? C18A H18A 0.9500 . ? C19A C20A 1.3900 . ? C19A H19A 0.9500 . ? C20A N4A 1.338(2) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A C10A 1.510(5) . ? C3A C5A 1.3900 . ? C3A H3A 0.9500 . ? C5A C4A 1.3900 . ? C5A H5A 0.9500 . ? C4A C6A 1.3900 . ? C4A H4A 0.9500 . ? C6A C7A 1.536(5) . ? N4A C22A 1.4200 . ? N4A C21A 1.4200 . ? C22A C23A 1.4200 . ? C22A H22A 0.9500 . ? C23A N5A 1.4200 . ? C23A H23A 0.9500 . ? N5A C24A 1.343(2) . ? N5A C21A 1.4200 . ? C24A C25A 1.3900 . ? C24A C29A 1.3900 . ? C25A C26A 1.3900 . ? C25A C30A 1.413(5) . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A C29A 1.3900 . ? C28A H28A 0.9500 . ? C29A C33A 1.5401 . ? C7A C8A 1.465(6) . ? C7A C9A 1.543(6) . ? C7A H7A 1.0000 . ? C11A C10A 1.537(6) . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A C10A 1.469(6) . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C10A H10A 1.0000 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C30A C31A 1.456(6) . ? C30A C32A 1.660(6) . ? C30A H30A 1.0000 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33A C35A 1.5398(6) . ? C33A C34A 1.5399(6) . ? C33A H33A 1.0000 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? Mn1B C21B 2.298(2) . ? Mn1B N3B 2.3257(16) . ? Mn1B C13B 2.384(2) . ? Mn1B Br1B 2.5126(8) . ? Mn1B Br2B 2.5151(7) . ? N1B C13B 1.4200 . ? N1B C14B 1.4200 . ? N1B C1B 1.460(2) . ? C14B C15B 1.4200 . ? C14B H14B 0.9500 . ? C15B N2B 1.4200 . ? C15B H15B 0.9500 . ? N2B C16B 1.364(3) . ? N2B C13B 1.4200 . ? N3B C16B 1.3900 . ? N3B C20B 1.3900 . ? C16B C17B 1.3900 . ? C17B C18B 1.3900 . ? C17B H17B 0.9500 . ? C18B C19B 1.3900 . ? C18B H18B 0.9500 . ? C19B C20B 1.3900 . ? C19B H19B 0.9500 . ? C20B N4B 1.334(2) . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C2B C10B 1.593(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 C7B 1.546(5) . ? N4B C22B 1.4200 . ? N4B C21B 1.4200 . ? C22B C23B 1.4200 . ? C22B H22B 0.9500 . ? C23B N5B 1.4200 . ? C23B H23B 0.9500 . ? N5B C24B 1.312(2) . ? N5B C21B 1.4200 . ? C7B C9B 1.467(6) . ? C7B C8B 1.604(7) . ? C7B H7B 1.0000 . ? C11B C10B 1.507(7) . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C24B C25B 1.3900 . ? C24B C29B 1.3900 . ? C25B C26B 1.3900 . ? C25B C30B 1.643(5) . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B H27B 0.9500 . ? C28B C29B 1.3900 . ? C28B H28B 0.9500 . ? C29B C33B 1.5401 . ? C12B C10B 1.553(7) . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C10B H10B 1.0000 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C30B C32B 1.439(7) . ? C30B C31B 1.635(7) . ? C30B H30B 1.0000 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B C34B 1.386(5) . ? C33B C35B 1.514(4) . ? C33B H33B 1.0000 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 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 C42A O1A C43A 99.7(4) . . ? C40A C41A C42A 105.0(5) . . ? C40A C41A H41A 110.7 . . ? C42A C41A H41A 110.7 . . ? C40A C41A H41B 110.7 . . ? C42A C41A H41B 110.7 . . ? H41A C41A H41B 108.8 . . ? C41A C40A C43A 93.6(4) . . ? C41A C40A H40A 113.0 . . ? C43A C40A H40A 113.0 . . ? C41A C40A H40B 113.0 . . ? C43A C40A H40B 113.0 . . ? H40A C40A H40B 110.4 . . ? O1A C43A C40A 97.5(4) . . ? O1A C43A H43A 112.3 . . ? C40A C43A H43A 112.3 . . ? O1A C43A H43B 112.3 . . ? C40A C43A H43B 112.3 . . ? H43A C43A H43B 109.9 . . ? O1A C42A C41A 105.8(5) . . ? O1A C42A H42A 110.6 . . ? C41A C42A H42A 110.6 . . ? O1A C42A H42B 110.6 . . ? C41A C42A H42B 110.6 . . ? H42A C42A H42B 108.7 . . ? C43B O1B C40B 102.7(4) . . ? C42B C41B C40B 99.6(4) . . ? C42B C41B H41C 111.8 . . ? C40B C41B H41C 111.8 . . ? C42B C41B H41D 111.8 . . ? C40B C41B H41D 111.8 . . ? H41C C41B H41D 109.6 . . ? C41B C40B O1B 106.7(4) . . ? C41B C40B H40C 110.4 . . ? O1B C40B H40C 110.4 . . ? C41B C40B H40D 110.4 . . ? O1B C40B H40D 110.4 . . ? H40C C40B H40D 108.6 . . ? O1B C43B C42B 101.9(4) . . ? O1B C43B H43C 111.4 . . ? C42B C43B H43C 111.4 . . ? O1B C43B H43D 111.4 . . ? C42B C43B H43D 111.4 . . ? H43C C43B H43D 109.3 . . ? C43B C42B C41B 104.8(4) . . ? C43B C42B H42C 110.8 . . ? C41B C42B H42C 110.8 . . ? C43B C42B H42D 110.8 . . ? C41B C42B H42D 110.8 . . ? H42C C42B H42D 108.9 . . ? C13A Mn1A C21A 143.58(8) . . ? C13A Mn1A N3A 74.99(7) . . ? C21A Mn1A N3A 71.60(6) . . ? C13A Mn1A Br1A 99.12(6) . . ? C21A Mn1A Br1A 102.96(5) . . ? N3A Mn1A Br1A 150.91(5) . . ? C13A Mn1A Br2A 97.41(6) . . ? C21A Mn1A Br2A 93.48(6) . . ? N3A Mn1A Br2A 84.52(4) . . ? Br1A Mn1A Br2A 124.57(3) . . ? C1A N1A C14A 128.35(12) . . ? C1A N1A C13A 119.75(12) . . ? C14A N1A C13A 108.0 . . ? N1A C14A C15A 108.0 . . ? N1A C14A H14A 126.0 . . ? C15A C14A H14A 126.0 . . ? N2A C15A C14A 108.0 . . ? N2A C15A H15A 126.0 . . ? C14A C15A H15A 126.0 . . ? C16A N2A C15A 115.05(17) . . ? C16A N2A C13A 132.42(18) . . ? C15A N2A C13A 108.0 . . ? N2A C13A N1A 108.0 . . ? N2A C13A Mn1A 105.86(10) . . ? N1A C13A Mn1A 141.39(11) . . ? C16A N3A C20A 120.0 . . ? C16A N3A Mn1A 117.82(7) . . ? C20A N3A Mn1A 122.04(7) . . ? N2A C16A N3A 103.95(15) . . ? N2A C16A C17A 132.11(15) . . ? N3A C16A C17A 120.0 . . ? C18A C17A C16A 120.0 . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C19A C18A C17A 120.0 . . ? C19A C18A H18A 120.0 . . ? C17A C18A H18A 120.0 . . ? C18A C19A C20A 120.0 . . ? C18A C19A H19A 120.0 . . ? C20A C19A H19A 120.0 . . ? N4A C20A C19A 133.05(12) . . ? N4A C20A N3A 105.31(12) . . ? C19A C20A N3A 120.0 . . ? N1A C1A C2A 113.39(12) . . ? N1A C1A C6A 126.28(12) . . ? C2A C1A C6A 120.0 . . ? C3A C2A C1A 120.0 . . ? C3A C2A C10A 114.8(2) . . ? C1A C2A C10A 125.1(2) . . ? C2A C3A C5A 120.0 . . ? C2A C3A H3A 120.0 . . ? C5A C3A H3A 120.0 . . ? C4A C5A C3A 120.0 . . ? C4A C5A H5A 120.0 . . ? C3A C5A H5A 120.0 . . ? C5A C4A C6A 120.0 . . ? C5A C4A H4A 120.0 . . ? C6A C4A H4A 120.0 . . ? C4A C6A C1A 120.0 . . ? C4A C6A C7A 117.93(19) . . ? C1A C6A C7A 121.94(19) . . ? C20A N4A C22A 123.38(12) . . ? C20A N4A C21A 127.53(12) . . ? C22A N4A C21A 108.0 . . ? C23A C22A N4A 108.0 . . ? C23A C22A H22A 126.0 . . ? N4A C22A H22A 126.0 . . ? N5A C23A C22A 108.0 . . ? N5A C23A H23A 126.0 . . ? C22A C23A H23A 126.0 . . ? C24A N5A C23A 126.63(19) . . ? C24A N5A C21A 124.42(19) . . ? C23A N5A C21A 108.0 . . ? N5A C21A N4A 108.0 . . ? N5A C21A Mn1A 140.44(10) . . ? N4A C21A Mn1A 110.42(10) . . ? N5A C24A C25A 127.52(13) . . ? N5A C24A C29A 112.46(13) . . ? C25A C24A C29A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A C30A 116.90(19) . . ? C24A C25A C30A 123.10(19) . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C29A C28A C27A 120.0 . . ? C29A C28A H28A 120.0 . . ? C27A C28A H28A 120.0 . . ? C28A C29A C24A 120.0 . . ? C28A C29A C33A 117.90(5) . . ? C24A C29A C33A 122.03(5) . . ? C8A C7A C6A 113.2(4) . . ? C8A C7A C9A 116.4(4) . . ? C6A C7A C9A 108.2(3) . . ? C8A C7A H7A 106.1 . . ? C6A C7A H7A 106.1 . . ? C9A C7A H7A 106.1 . . ? C12A C10A C2A 118.0(4) . . ? C12A C10A C11A 109.2(4) . . ? C2A C10A C11A 111.4(3) . . ? C12A C10A H10A 105.8 . . ? C2A C10A H10A 105.8 . . ? C11A C10A H10A 105.8 . . ? C25A C30A C31A 124.6(4) . . ? C25A C30A C32A 111.9(3) . . ? C31A C30A C32A 103.3(4) . . ? C25A C30A H30A 105.1 . . ? C31A C30A H30A 105.1 . . ? C32A C30A H30A 105.1 . . ? C35A C33A C34A 108.42(11) . . ? C35A C33A C29A 110.34(8) . . ? C34A C33A C29A 109.69(6) . . ? C35A C33A H33A 109.5 . . ? C34A C33A H33A 109.5 . . ? C29A C33A H33A 109.5 . . ? C21B Mn1B N3B 68.56(6) . . ? C21B Mn1B C13B 129.95(7) . . ? N3B Mn1B C13B 63.85(6) . . ? C21B Mn1B Br1B 105.11(6) . . ? N3B Mn1B Br1B 158.65(5) . . ? C13B Mn1B Br1B 113.40(6) . . ? C21B Mn1B Br2B 98.34(7) . . ? N3B Mn1B Br2B 88.20(5) . . ? C13B Mn1B Br2B 94.84(7) . . ? Br1B Mn1B Br2B 113.10(3) . . ? C13B N1B C14B 108.0 . . ? C13B N1B C1B 131.94(12) . . ? C14B N1B C1B 119.34(12) . . ? C15B C14B N1B 108.0 . . ? C15B C14B H14B 126.0 . . ? N1B C14B H14B 126.0 . . ? N2B C15B C14B 108.0 . . ? N2B C15B H15B 126.0 . . ? C14B C15B H15B 126.0 . . ? C16B N2B C15B 137.55(19) . . ? C16B N2B C13B 108.23(17) . . ? C15B N2B C13B 108.0 . . ? N2B C13B N1B 108.0 . . ? N2B C13B Mn1B 123.34(9) . . ? N1B C13B Mn1B 126.13(9) . . ? C16B N3B C20B 120.0 . . ? C16B N3B Mn1B 118.96(7) . . ? C20B N3B Mn1B 118.94(7) . . ? N2B C16B N3B 115.98(16) . . ? N2B C16B C17B 120.33(15) . . ? N3B C16B C17B 120.0 . . ? C16B C17B C18B 120.0 . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C17B C18B C19B 120.0 . . ? C17B C18B H18B 120.0 . . ? C19B C18B H18B 120.0 . . ? C20B C19B C18B 120.0 . . ? C20B C19B H19B 120.0 . . ? C18B C19B H19B 120.0 . . ? N4B C20B C19B 122.96(13) . . ? N4B C20B N3B 115.43(13) . . ? C19B C20B N3B 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B N1B 126.56(12) . . ? C6B C1B N1B 113.35(12) . . ? C1B C2B C3B 120.0 . . ? C1B C2B C10B 119.0(2) . . ? C3B C2B C10B 121.0(2) . . ? C2B C3B C4B 120.0 . . ? C2B C3B H3B 120.0 . . ? C4B C3B H3B 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B C7B 118.5(2) . . ? C1B C6B C7B 121.5(2) . . ? C20B N4B C22B 132.98(13) . . ? C20B N4B C21B 117.90(14) . . ? C22B N4B C21B 108.0 . . ? C23B C22B N4B 108.0 . . ? C23B C22B H22B 126.0 . . ? N4B C22B H22B 126.0 . . ? N5B C23B C22B 108.0 . . ? N5B C23B H23B 126.0 . . ? C22B C23B H23B 126.0 . . ? C24B N5B C23B 125.8(2) . . ? C24B N5B C21B 126.1(2) . . ? C23B N5B C21B 108.0 . . ? N5B C21B N4B 108.0 . . ? N5B C21B Mn1B 134.70(11) . . ? N4B C21B Mn1B 116.72(11) . . ? C9B C7B C6B 113.6(4) . . ? C9B C7B C8B 107.0(4) . . ? C6B C7B C8B 108.3(3) . . ? C9B C7B H7B 109.3 . . ? C6B C7B H7B 109.3 . . ? C8B C7B H7B 109.3 . . ? N5B C24B C25B 112.04(14) . . ? N5B C24B C29B 127.60(14) . . ? C25B C24B C29B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B C30B 119.54(18) . . ? C24B C25B C30B 120.42(18) . . ? C27B C26B C25B 120.0 . . ? C27B C26B H26B 120.0 . . ? C25B C26B H26B 120.0 . . ? C28B C27B C26B 120.0 . . ? C28B C27B H27B 120.0 . . ? C26B C27B H27B 120.0 . . ? C27B C28B C29B 120.0 . . ? C27B C28B H28B 120.0 . . ? C29B C28B H28B 120.0 . . ? C28B C29B C24B 120.0 . . ? C28B C29B C33B 121.82(8) . . ? C24B C29B C33B 117.90(8) . . ? C11B C10B C12B 115.0(4) . . ? C11B C10B C2B 109.5(3) . . ? C12B C10B C2B 104.4(3) . . ? C11B C10B H10B 109.3 . . ? C12B C10B H10B 109.3 . . ? C2B C10B H10B 109.3 . . ? C32B C30B C31B 119.0(4) . . ? C32B C30B C25B 110.3(4) . . ? C31B C30B C25B 101.2(3) . . ? C32B C30B H30B 108.6 . . ? C31B C30B H30B 108.6 . . ? C25B C30B H30B 108.6 . . ? C34B C33B C35B 118.8(3) . . ? C34B C33B C29B 121.4(2) . . ? C35B C33B C29B 115.7(2) . . ? C34B C33B H33B 96.8 . . ? C35B C33B H33B 96.8 . . ? C29B C33B H33B 96.8 . . ? 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 C42A C41A C40A C43A 34.1(5) . . . . ? C42A O1A C43A C40A 58.8(5) . . . . ? C41A C40A C43A O1A -56.1(5) . . . . ? C43A O1A C42A C41A -36.4(5) . . . . ? C40A C41A C42A O1A -0.8(6) . . . . ? C42B C41B C40B O1B 13.9(5) . . . . ? C43B O1B C40B C41B 15.8(5) . . . . ? C40B O1B C43B C42B -39.5(5) . . . . ? O1B C43B C42B C41B 51.5(5) . . . . ? C40B C41B C42B C43B -38.9(5) . . . . ? C1A N1A C14A C15A 157.27(16) . . . . ? C13A N1A C14A C15A 0.0 . . . . ? N1A C14A C15A N2A 0.0 . . . . ? C14A C15A N2A C16A 159.2(2) . . . . ? C14A C15A N2A C13A 0.0 . . . . ? C16A N2A C13A N1A -154.1(2) . . . . ? C15A N2A C13A N1A 0.0 . . . . ? C16A N2A C13A Mn1A 7.0(2) . . . . ? C15A N2A C13A Mn1A 161.16(15) . . . . ? C1A N1A C13A N2A -159.57(15) . . . . ? C14A N1A C13A N2A 0.0 . . . . ? C1A N1A C13A Mn1A 50.3(2) . . . . ? C14A N1A C13A Mn1A -150.1(2) . . . . ? C21A Mn1A C13A N2A 29.89(17) . . . . ? N3A Mn1A C13A N2A 5.94(9) . . . . ? Br1A Mn1A C13A N2A 156.78(8) . . . . ? Br2A Mn1A C13A N2A -76.33(9) . . . . ? C21A Mn1A C13A N1A -179.59(14) . . . . ? N3A Mn1A C13A N1A 156.46(19) . . . . ? Br1A Mn1A C13A N1A -52.71(18) . . . . ? Br2A Mn1A C13A N1A 74.19(17) . . . . ? C13A Mn1A N3A C16A -18.26(10) . . . . ? C21A Mn1A N3A C16A 176.46(10) . . . . ? Br1A Mn1A N3A C16A -99.97(11) . . . . ? Br2A Mn1A N3A C16A 80.94(8) . . . . ? C13A Mn1A N3A C20A 166.05(10) . . . . ? C21A Mn1A N3A C20A 0.76(9) . . . . ? Br1A Mn1A N3A C20A 84.34(11) . . . . ? Br2A Mn1A N3A C20A -94.76(7) . . . . ? C15A N2A C16A N3A -173.92(13) . . . . ? C13A N2A C16A N3A -21.2(2) . . . . ? C15A N2A C16A C17A 29.3(2) . . . . ? C13A N2A C16A C17A -177.95(12) . . . . ? C20A N3A C16A N2A -160.27(16) . . . . ? Mn1A N3A C16A N2A 23.95(17) . . . . ? C20A N3A C16A C17A 0.0 . . . . ? Mn1A N3A C16A C17A -175.79(8) . . . . ? N2A C16A C17A C18A 153.8(2) . . . . ? N3A C16A C17A C18A 0.0 . . . . ? C16A C17A C18A C19A 0.0 . . . . ? C17A C18A C19A C20A 0.0 . . . . ? C18A C19A C20A N4A 163.05(19) . . . . ? C18A C19A C20A N3A 0.0 . . . . ? C16A N3A C20A N4A -167.24(14) . . . . ? Mn1A N3A C20A N4A 8.37(13) . . . . ? C16A N3A C20A C19A 0.0 . . . . ? Mn1A N3A C20A C19A 175.60(8) . . . . ? C14A N1A C1A C2A 106.43(17) . . . . ? C13A N1A C1A C2A -98.61(14) . . . . ? C14A N1A C1A C6A -66.9(2) . . . . ? C13A N1A C1A C6A 88.09(16) . . . . ? N1A C1A C2A C3A -173.76(13) . . . . ? C6A C1A C2A C3A 0.0 . . . . ? N1A C1A C2A C10A 10.2(3) . . . . ? C6A C1A C2A C10A -176.1(3) . . . . ? C1A C2A C3A C5A 0.0 . . . . ? C10A C2A C3A C5A 176.4(3) . . . . ? C2A C3A C5A C4A 0.0 . . . . ? C3A C5A C4A C6A 0.0 . . . . ? C5A C4A C6A C1A 0.0 . . . . ? C5A C4A C6A C7A -175.8(3) . . . . ? N1A C1A C6A C4A 172.90(14) . . . . ? C2A C1A C6A C4A 0.0 . . . . ? N1A C1A C6A C7A -11.5(3) . . . . ? C2A C1A C6A C7A 175.7(3) . . . . ? C19A C20A N4A C22A 8.8(2) . . . . ? N3A C20A N4A C22A 173.59(10) . . . . ? C19A C20A N4A C21A 175.36(12) . . . . ? N3A C20A N4A C21A -19.82(17) . . . . ? C20A N4A C22A C23A 168.85(15) . . . . ? C21A N4A C22A C23A 0.0 . . . . ? N4A C22A C23A N5A 0.0 . . . . ? C22A C23A N5A C24A -169.2(2) . . . . ? C22A C23A N5A C21A 0.0 . . . . ? C24A N5A C21A N4A 169.5(2) . . . . ? C23A N5A C21A N4A 0.0 . . . . ? C24A N5A C21A Mn1A -24.7(2) . . . . ? C23A N5A C21A Mn1A 165.80(17) . . . . ? C20A N4A C21A N5A -168.25(16) . . . . ? C22A N4A C21A N5A 0.0 . . . . ? C20A N4A C21A Mn1A 21.35(17) . . . . ? C22A N4A C21A Mn1A -170.40(11) . . . . ? C13A Mn1A C21A N5A 160.64(14) . . . . ? N3A Mn1A C21A N5A -174.95(13) . . . . ? Br1A Mn1A C21A N5A 34.78(12) . . . . ? Br2A Mn1A C21A N5A -91.90(11) . . . . ? C13A Mn1A C21A N4A -33.77(19) . . . . ? N3A Mn1A C21A N4A -9.36(9) . . . . ? Br1A Mn1A C21A N4A -159.64(8) . . . . ? Br2A Mn1A C21A N4A 73.68(9) . . . . ? C23A N5A C24A C25A 83.66(19) . . . . ? C21A N5A C24A C25A -83.85(19) . . . . ? C23A N5A C24A C29A -98.01(15) . . . . ? C21A N5A C24A C29A 94.48(15) . . . . ? N5A C24A C25A C26A 178.22(17) . . . . ? C29A C24A C25A C26A 0.0 . . . . ? N5A C24A C25A C30A -2.0(3) . . . . ? C29A C24A C25A C30A 179.8(2) . . . . ? C24A C25A C26A C27A 0.0 . . . . ? C30A C25A C26A C27A -179.8(2) . . . . ? C25A C26A C27A C28A 0.0 . . . . ? C26A C27A C28A C29A 0.0 . . . . ? C27A C28A C29A C24A 0.0 . . . . ? C27A C28A C29A C33A 177.10(6) . . . . ? N5A C24A C29A C28A -178.48(14) . . . . ? C25A C24A C29A C28A 0.0 . . . . ? N5A C24A C29A C33A 4.54(15) . . . . ? C25A C24A C29A C33A -176.98(6) . . . . ? C4A C6A C7A C8A 59.6(4) . . . . ? C1A C6A C7A C8A -116.1(3) . . . . ? C4A C6A C7A C9A -71.0(3) . . . . ? C1A C6A C7A C9A 113.3(3) . . . . ? C3A C2A C10A C12A -58.1(4) . . . . ? C1A C2A C10A C12A 118.2(3) . . . . ? C3A C2A C10A C11A 69.3(4) . . . . ? C1A C2A C10A C11A -114.5(3) . . . . ? C26A C25A C30A C31A 73.8(4) . . . . ? C24A C25A C30A C31A -106.0(4) . . . . ? C26A C25A C30A C32A -51.6(3) . . . . ? C24A C25A C30A C32A 128.7(3) . . . . ? C28A C29A C33A C35A -59.14(6) . . . . ? C24A C29A C33A C35A 117.90(6) . . . . ? C28A C29A C33A C34A 60.24(11) . . . . ? C24A C29A C33A C34A -122.72(11) . . . . ? C13B N1B C14B C15B 0.0 . . . . ? C1B N1B C14B C15B -171.43(14) . . . . ? N1B C14B C15B N2B 0.0 . . . . ? C14B C15B N2B C16B -147.4(3) . . . . ? C14B C15B N2B C13B 0.0 . . . . ? C16B N2B C13B N1B 157.5(2) . . . . ? C15B N2B C13B N1B 0.0 . . . . ? C16B N2B C13B Mn1B -5.4(2) . . . . ? C15B N2B C13B Mn1B -162.91(18) . . . . ? C14B N1B C13B N2B 0.0 . . . . ? C1B N1B C13B N2B 169.94(16) . . . . ? C14B N1B C13B Mn1B 162.31(18) . . . . ? C1B N1B C13B Mn1B -27.8(2) . . . . ? C21B Mn1B C13B N2B -28.95(17) . . . . ? N3B Mn1B C13B N2B -9.44(11) . . . . ? Br1B Mn1B C13B N2B -166.09(10) . . . . ? Br2B Mn1B C13B N2B 76.16(12) . . . . ? C21B Mn1B C13B N1B 171.29(12) . . . . ? N3B Mn1B C13B N1B -169.19(16) . . . . ? Br1B Mn1B C13B N1B 34.15(15) . . . . ? Br2B Mn1B C13B N1B -83.59(13) . . . . ? C21B Mn1B N3B C16B -172.21(11) . . . . ? C13B Mn1B N3B C16B 23.76(11) . . . . ? Br1B Mn1B N3B C16B 111.41(14) . . . . ? Br2B Mn1B N3B C16B -72.52(9) . . . . ? C21B Mn1B N3B C20B -8.67(10) . . . . ? C13B Mn1B N3B C20B -172.70(11) . . . . ? Br1B Mn1B N3B C20B -85.05(14) . . . . ? Br2B Mn1B N3B C20B 91.02(7) . . . . ? C15B N2B C16B N3B 173.72(16) . . . . ? C13B N2B C16B N3B 26.4(2) . . . . ? C15B N2B C16B C17B -27.9(3) . . . . ? C13B N2B C16B C17B -175.27(10) . . . . ? C20B N3B C16B N2B 158.43(19) . . . . ? Mn1B N3B C16B N2B -38.2(2) . . . . ? C20B N3B C16B C17B 0.0 . . . . ? Mn1B N3B C16B C17B 163.36(9) . . . . ? N2B C16B C17B C18B -157.5(2) . . . . ? N3B C16B C17B C18B 0.0 . . . . ? C16B C17B C18B C19B 0.0 . . . . ? C17B C18B C19B C20B 0.0 . . . . ? C18B C19B C20B N4B -164.88(19) . . . . ? C18B C19B C20B N3B 0.0 . . . . ? C16B N3B C20B N4B 165.98(17) . . . . ? Mn1B N3B C20B N4B 2.61(16) . . . . ? C16B N3B C20B C19B 0.0 . . . . ? Mn1B N3B C20B C19B -163.36(9) . . . . ? C13B N1B C1B C2B -71.88(19) . . . . ? C14B N1B C1B C2B 97.13(18) . . . . ? C13B N1B C1B C6B 111.63(16) . . . . ? C14B N1B C1B C6B -79.36(17) . . . . ? C6B C1B C2B C3B 0.0 . . . . ? N1B C1B C2B C3B -176.28(14) . . . . ? C6B C1B C2B C10B 177.8(3) . . . . ? N1B C1B C2B C10B 1.5(3) . . . . ? C1B C2B C3B C4B 0.0 . . . . ? C10B C2B C3B C4B -177.8(3) . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C4B C5B C6B C1B 0.0 . . . . ? C4B C5B C6B C7B 179.4(3) . . . . ? C2B C1B C6B C5B 0.0 . . . . ? N1B C1B C6B C5B 176.75(12) . . . . ? C2B C1B C6B C7B -179.4(3) . . . . ? N1B C1B C6B C7B -2.7(3) . . . . ? C19B C20B N4B C22B -18.3(2) . . . . ? N3B C20B N4B C22B 176.18(12) . . . . ? C19B C20B N4B C21B 175.44(11) . . . . ? N3B C20B N4B C21B 9.92(18) . . . . ? C20B N4B C22B C23B -167.25(19) . . . . ? C21B N4B C22B C23B 0.0 . . . . ? N4B C22B C23B N5B 0.0 . . . . ? C22B C23B N5B C24B 176.8(2) . . . . ? C22B C23B N5B C21B 0.0 . . . . ? C24B N5B C21B N4B -176.8(2) . . . . ? C23B N5B C21B N4B 0.0 . . . . ? C24B N5B C21B Mn1B 12.5(2) . . . . ? C23B N5B C21B Mn1B -170.64(17) . . . . ? C20B N4B C21B N5B 169.47(15) . . . . ? C22B N4B C21B N5B 0.0 . . . . ? C20B N4B C21B Mn1B -17.97(17) . . . . ? C22B N4B C21B Mn1B 172.56(13) . . . . ? N3B Mn1B C21B N5B -176.64(13) . . . . ? C13B Mn1B C21B N5B -157.85(12) . . . . ? Br1B Mn1B C21B N5B -18.14(12) . . . . ? Br2B Mn1B C21B N5B 98.62(11) . . . . ? N3B Mn1B C21B N4B 13.33(10) . . . . ? C13B Mn1B C21B N4B 32.12(17) . . . . ? Br1B Mn1B C21B N4B 171.83(10) . . . . ? Br2B Mn1B C21B N4B -71.41(11) . . . . ? C5B C6B C7B C9B -63.6(4) . . . . ? C1B C6B C7B C9B 115.8(3) . . . . ? C5B C6B C7B C8B 55.1(4) . . . . ? C1B C6B C7B C8B -125.5(3) . . . . ? C23B N5B C24B C25B 91.37(17) . . . . ? C21B N5B C24B C25B -92.36(17) . . . . ? C23B N5B C24B C29B -81.6(2) . . . . ? C21B N5B C24B C29B 94.6(2) . . . . ? N5B C24B C25B C26B -173.61(16) . . . . ? C29B C24B C25B C26B 0.0 . . . . ? N5B C24B C25B C30B 3.9(3) . . . . ? C29B C24B C25B C30B 177.5(2) . . . . ? C24B C25B C26B C27B 0.0 . . . . ? C30B C25B C26B C27B -177.5(2) . . . . ? C25B C26B C27B C28B 0.0 . . . . ? C26B C27B C28B C29B 0.0 . . . . ? C27B C28B C29B C24B 0.0 . . . . ? C27B C28B C29B C33B -173.78(9) . . . . ? N5B C24B C29B C28B 172.52(19) . . . . ? C25B C24B C29B C28B 0.0 . . . . ? N5B C24B C29B C33B -13.5(2) . . . . ? C25B C24B C29B C33B 174.02(9) . . . . ? C1B C2B C10B C11B -107.0(3) . . . . ? C3B C2B C10B C11B 70.8(4) . . . . ? C1B C2B C10B C12B 129.4(3) . . . . ? C3B C2B C10B C12B -52.8(4) . . . . ? C26B C25B C30B C32B -71.1(4) . . . . ? C24B C25B C30B C32B 111.3(3) . . . . ? C26B C25B C30B C31B 55.8(3) . . . . ? C24B C25B C30B C31B -121.8(3) . . . . ? C28B C29B C33B C34B 62.2(3) . . . . ? C24B C29B C33B C34B -111.7(3) . . . . ? C28B C29B C33B C35B -94.7(3) . . . . ? C24B C29B C33B C35B 91.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.097 _refine_diff_density_min -1.073 _refine_diff_density_rms 0.130 #==END data_4 _database_code_depnum_ccdc_archive 'CCDC 282402' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Cl3 N5 Nb, C4 H8 O' _chemical_formula_sum 'C39 H49 Cl3 N5 Nb O' _chemical_formula_weight 803.09 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' Cl Cl 0.1484 0.1585 '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' Nb Nb -2.0727 0.6215 '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/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.803(7) _cell_length_b 18.707(11) _cell_length_c 18.838(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.61(6) _cell_angle_gamma 90.00 _cell_volume 3803(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8081 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6249 _exptl_absorpt_correction_T_max 0.9944 _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 26634 _diffrn_reflns_av_R_equivalents 0.1325 _diffrn_reflns_av_sigmaI/netI 0.1954 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8730 _reflns_number_gt 4281 _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 'SIR92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 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^)+(0.0444P)^2^+5.6157P] 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 8730 _refine_ls_number_parameters 460 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1973 _refine_ls_R_factor_gt 0.0902 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1446 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4103(5) 0.1845(3) -0.0613(4) 0.0326(15) Uani 1 1 d . . . C2 C 0.2707(5) 0.2503(3) 0.0075(3) 0.0272(14) Uani 1 1 d . . . C3 C 0.1594(6) 0.3075(3) -0.0796(4) 0.0376(16) Uani 1 1 d . . . H3 H 0.0986 0.3373 -0.1025 0.045 Uiso 1 1 calc R . . C4 C 0.2439(6) 0.2688(3) -0.1114(4) 0.0350(16) Uani 1 1 d . . . H4 H 0.2550 0.2657 -0.1611 0.042 Uiso 1 1 calc R . . C5 C 0.1022(5) 0.3315(3) 0.0459(3) 0.0328(15) Uani 1 1 d . . . C6 C -0.0102(5) 0.2993(3) 0.0619(3) 0.0376(16) Uani 1 1 d . . . C7 C -0.0833(7) 0.3366(4) 0.1090(4) 0.053(2) Uani 1 1 d . . . H7 H -0.1607 0.3172 0.1214 0.064 Uiso 1 1 calc R . . C8 C -0.0447(7) 0.4006(4) 0.1375(4) 0.062(2) Uani 1 1 d . . . H8 H -0.0954 0.4251 0.1694 0.074 Uiso 1 1 calc R . . C9 C 0.0666(7) 0.4298(3) 0.1203(4) 0.053(2) Uani 1 1 d . . . H9 H 0.0922 0.4737 0.1416 0.064 Uiso 1 1 calc R . . C10 C 0.1428(6) 0.3970(3) 0.0725(4) 0.0427(17) Uani 1 1 d . . . C11 C 0.2624(6) 0.4325(3) 0.0529(4) 0.0466(19) Uani 1 1 d . . . H11 H 0.3097 0.3980 0.0241 0.056 Uiso 1 1 calc R . . C12 C 0.3419(7) 0.4515(4) 0.1189(5) 0.062(2) Uani 1 1 d . . . H12A H 0.3010 0.4891 0.1454 0.094 Uiso 1 1 calc R . . H12B H 0.4230 0.4686 0.1048 0.094 Uiso 1 1 calc R . . H12C H 0.3530 0.4090 0.1490 0.094 Uiso 1 1 calc R . . C13 C 0.2348(7) 0.4990(3) 0.0073(4) 0.057(2) Uani 1 1 d . . . H13A H 0.1885 0.4850 -0.0364 0.086 Uiso 1 1 calc R . . H13B H 0.3129 0.5217 -0.0046 0.086 Uiso 1 1 calc R . . H13C H 0.1853 0.5328 0.0339 0.086 Uiso 1 1 calc R . . C14 C -0.0558(6) 0.2300(3) 0.0302(4) 0.0401(17) Uani 1 1 d . . . H14 H 0.0137 0.2072 0.0051 0.048 Uiso 1 1 calc R . . C15 C -0.0990(7) 0.1780(4) 0.0860(5) 0.065(2) Uani 1 1 d . . . H15A H -0.0333 0.1719 0.1231 0.098 Uiso 1 1 calc R . . H15B H -0.1180 0.1318 0.0637 0.098 Uiso 1 1 calc R . . H15C H -0.1735 0.1970 0.1071 0.098 Uiso 1 1 calc R . . C16 C -0.1604(7) 0.2454(4) -0.0241(4) 0.059(2) Uani 1 1 d . . . H16A H -0.2284 0.2690 -0.0006 0.089 Uiso 1 1 calc R . . H16B H -0.1902 0.2004 -0.0454 0.089 Uiso 1 1 calc R . . H16C H -0.1303 0.2767 -0.0612 0.089 Uiso 1 1 calc R . . C17 C 0.4630(6) 0.1661(3) -0.1245(4) 0.0386(17) Uani 1 1 d . . . H17 H 0.4363 0.1867 -0.1687 0.046 Uiso 1 1 calc R . . C18 C 0.5575(6) 0.1156(3) -0.1192(4) 0.0453(19) Uani 1 1 d . . . H18 H 0.5981 0.1016 -0.1607 0.054 Uiso 1 1 calc R . . C19 C 0.5931(6) 0.0858(3) -0.0551(4) 0.0408(18) Uani 1 1 d . . . H19 H 0.6562 0.0504 -0.0517 0.049 Uiso 1 1 calc R . . C20 C 0.5342(5) 0.1087(3) 0.0043(4) 0.0338(16) Uani 1 1 d . . . C21 C 0.4999(5) 0.1156(3) 0.1275(4) 0.0307(15) Uani 1 1 d . . . C22 C 0.6347(5) 0.0307(3) 0.1674(4) 0.0363(16) Uani 1 1 d . . . H22 H 0.6802 0.0001 0.1993 0.044 Uiso 1 1 calc R . . C23 C 0.6425(5) 0.0320(3) 0.0979(4) 0.0356(17) Uani 1 1 d . . . H23 H 0.6944 0.0030 0.0704 0.043 Uiso 1 1 calc R . . C24 C 0.5302(5) 0.1013(3) 0.2595(3) 0.0316(15) Uani 1 1 d . . . C25 C 0.4281(5) 0.0743(3) 0.2946(4) 0.0339(16) Uani 1 1 d . . . C26 C 0.4205(6) 0.0908(3) 0.3654(4) 0.0396(17) Uani 1 1 d . . . H26 H 0.3533 0.0726 0.3907 0.048 Uiso 1 1 calc R . . C27 C 0.5070(6) 0.1329(3) 0.4006(4) 0.0386(17) Uani 1 1 d . . . H27 H 0.4993 0.1437 0.4495 0.046 Uiso 1 1 calc R . . C28 C 0.6064(6) 0.1596(3) 0.3643(4) 0.0383(17) Uani 1 1 d . . . H28 H 0.6664 0.1886 0.3889 0.046 Uiso 1 1 calc R . . C29 C 0.6197(5) 0.1448(3) 0.2930(4) 0.0332(16) Uani 1 1 d . . . C30 C 0.7298(6) 0.1740(3) 0.2549(4) 0.0411(17) Uani 1 1 d . . . H30 H 0.7167 0.1639 0.2030 0.049 Uiso 1 1 calc R . . C31 C 0.7407(6) 0.2551(3) 0.2651(4) 0.0495(19) Uani 1 1 d . . . H31A H 0.6677 0.2786 0.2429 0.074 Uiso 1 1 calc R . . H31B H 0.8155 0.2724 0.2430 0.074 Uiso 1 1 calc R . . H31C H 0.7460 0.2663 0.3160 0.074 Uiso 1 1 calc R . . C32 C 0.8498(6) 0.1364(4) 0.2819(4) 0.052(2) Uani 1 1 d . . . H32A H 0.8588 0.1408 0.3337 0.078 Uiso 1 1 calc R . . H32B H 0.9211 0.1587 0.2604 0.078 Uiso 1 1 calc R . . H32C H 0.8460 0.0857 0.2689 0.078 Uiso 1 1 calc R . . C33 C 0.3312(5) 0.0259(3) 0.2590(4) 0.0326(16) Uani 1 1 d . . . H33 H 0.3455 0.0246 0.2069 0.039 Uiso 1 1 calc R . . C34 C 0.3459(6) -0.0498(3) 0.2884(4) 0.0391(17) Uani 1 1 d . . . H34A H 0.4294 -0.0674 0.2799 0.059 Uiso 1 1 calc R . . H34B H 0.2845 -0.0812 0.2645 0.059 Uiso 1 1 calc R . . H34C H 0.3332 -0.0494 0.3395 0.059 Uiso 1 1 calc R . . C35 C 0.1991(5) 0.0536(3) 0.2691(4) 0.0424(18) Uani 1 1 d . . . H35A H 0.1831 0.0546 0.3199 0.064 Uiso 1 1 calc R . . H35B H 0.1392 0.0219 0.2444 0.064 Uiso 1 1 calc R . . H35C H 0.1908 0.1020 0.2495 0.064 Uiso 1 1 calc R . . C36A C 0.104(2) 0.404(2) 0.3054(14) 0.047(4) Uani 0.363(6) 1 d PD A 1 H36A H 0.1540 0.3724 0.2756 0.056 Uiso 0.363(6) 1 calc PR A 1 H36B H 0.0791 0.4480 0.2794 0.056 Uiso 0.363(6) 1 calc PR A 1 C37A C -0.0018(9) 0.3661(4) 0.3390(6) 0.098(4) Uani 0.363(6) 1 d PD A 1 H37A H -0.0643 0.3496 0.3026 0.117 Uiso 0.363(6) 1 calc PR A 1 H37B H 0.0280 0.3247 0.3677 0.117 Uiso 0.363(6) 1 calc PR A 1 C38A C -0.0535(7) 0.4229(4) 0.3849(5) 0.070(3) Uani 0.363(6) 1 d PD A 1 H38A H -0.0983 0.4601 0.3565 0.084 Uiso 0.363(6) 1 calc PR A 1 H38B H -0.1086 0.4028 0.4204 0.084 Uiso 0.363(6) 1 calc PR A 1 C39A C 0.0645(14) 0.4501(11) 0.4182(13) 0.062(4) Uani 0.363(6) 1 d PD A 1 H39A H 0.0684 0.5029 0.4151 0.074 Uiso 0.363(6) 1 calc PR A 1 H39B H 0.0732 0.4358 0.4687 0.074 Uiso 0.363(6) 1 calc PR A 1 C36B C 0.1246(12) 0.3894(8) 0.3207(9) 0.047(4) Uani 0.637(6) 1 d PD A 2 H36C H 0.1865 0.3790 0.3597 0.056 Uiso 0.637(6) 1 calc PR A 2 H36D H 0.1506 0.3663 0.2765 0.056 Uiso 0.637(6) 1 calc PR A 2 C37B C -0.0018(9) 0.3661(4) 0.3390(6) 0.098(4) Uani 0.637(6) 1 d PD A 2 H37C H 0.0024 0.3200 0.3648 0.117 Uiso 0.637(6) 1 calc PR A 2 H37D H -0.0551 0.3599 0.2953 0.117 Uiso 0.637(6) 1 calc PR A 2 C38B C -0.0535(7) 0.4229(4) 0.3849(5) 0.070(3) Uani 0.637(6) 1 d PD A 2 H38C H -0.0504 0.4084 0.4355 0.084 Uiso 0.637(6) 1 calc PR A 2 H38D H -0.1400 0.4348 0.3696 0.084 Uiso 0.637(6) 1 calc PR A 2 C39B C 0.0358(10) 0.4862(6) 0.3718(7) 0.062(4) Uani 0.637(6) 1 d PD A 2 H39C H -0.0116 0.5305 0.3612 0.074 Uiso 0.637(6) 1 calc PR A 2 H39D H 0.0916 0.4945 0.4141 0.074 Uiso 0.637(6) 1 calc PR A 2 Cl1 Cl 0.21143(14) 0.09663(9) 0.08219(11) 0.0529(5) Uani 1 1 d . . . Cl2 Cl 0.52601(15) 0.29054(8) 0.10871(11) 0.0487(5) Uani 1 1 d . . . Cl3 Cl 0.2635(2) 0.24579(11) 0.20005(12) 0.0814(8) Uani 1 1 d . . . N1 N 0.4454(4) 0.1592(2) 0.0023(3) 0.0302(12) Uani 1 1 d . . . N2 N 0.3126(4) 0.2340(2) -0.0580(3) 0.0312(12) Uani 1 1 d . . . N3 N 0.1759(4) 0.2965(2) -0.0070(3) 0.0305(12) Uani 1 1 d . . . N4 N 0.5596(4) 0.0844(2) 0.0725(3) 0.0325(13) Uani 1 1 d . . . N5 N 0.5478(4) 0.0821(2) 0.1865(3) 0.0307(13) Uani 1 1 d . . . Nb1 Nb 0.36084(5) 0.19892(3) 0.10177(3) 0.03293(19) Uani 1 1 d . . . O1A O 0.1608(12) 0.4171(7) 0.3771(10) 0.066(2) Uani 0.363(6) 1 d PD A 1 O1B O 0.1064(7) 0.4653(4) 0.3113(5) 0.066(2) Uani 0.637(6) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(3) 0.029(3) 0.041(5) -0.007(3) 0.009(3) -0.008(3) C2 0.024(3) 0.024(3) 0.034(4) 0.001(3) 0.002(3) -0.005(2) C3 0.040(4) 0.035(3) 0.037(5) 0.003(3) -0.005(3) -0.001(3) C4 0.035(3) 0.039(3) 0.032(4) -0.001(3) 0.005(3) 0.002(3) C5 0.029(3) 0.034(3) 0.036(4) -0.001(3) 0.000(3) 0.012(3) C6 0.032(3) 0.044(4) 0.038(4) 0.011(3) 0.002(3) 0.017(3) C7 0.045(4) 0.053(4) 0.064(6) 0.007(4) 0.024(4) 0.021(4) C8 0.061(5) 0.069(5) 0.057(6) -0.010(4) 0.023(5) 0.024(4) C9 0.059(5) 0.038(4) 0.063(6) -0.016(4) 0.008(4) 0.008(4) C10 0.049(4) 0.036(4) 0.042(5) -0.009(3) -0.006(4) 0.012(3) C11 0.039(4) 0.040(4) 0.060(6) -0.014(4) -0.003(4) 0.006(3) C12 0.061(5) 0.039(4) 0.086(7) -0.013(4) -0.012(5) 0.002(4) C13 0.059(5) 0.048(4) 0.064(6) -0.010(4) 0.002(4) 0.004(4) C14 0.033(3) 0.041(4) 0.047(5) 0.005(3) 0.009(3) 0.004(3) C15 0.060(5) 0.056(5) 0.080(7) 0.014(4) 0.024(5) 0.000(4) C16 0.046(4) 0.063(5) 0.068(6) 0.001(4) 0.000(4) -0.004(4) C17 0.042(4) 0.043(4) 0.031(4) -0.002(3) 0.009(3) -0.008(3) C18 0.045(4) 0.038(4) 0.055(6) -0.018(4) 0.017(4) -0.002(3) C19 0.030(3) 0.034(3) 0.059(6) -0.006(4) 0.011(4) 0.001(3) C20 0.030(3) 0.028(3) 0.045(5) -0.001(3) 0.013(3) -0.004(3) C21 0.025(3) 0.031(3) 0.036(4) -0.003(3) 0.003(3) -0.008(3) C22 0.026(3) 0.030(3) 0.053(5) 0.001(3) 0.002(3) 0.002(3) C23 0.024(3) 0.029(3) 0.054(5) 0.002(3) 0.005(3) 0.003(3) C24 0.029(3) 0.026(3) 0.039(5) 0.003(3) 0.001(3) 0.008(3) C25 0.030(3) 0.025(3) 0.048(5) 0.005(3) 0.007(3) 0.010(3) C26 0.029(3) 0.033(3) 0.057(5) 0.003(3) 0.001(4) 0.002(3) C27 0.036(4) 0.040(4) 0.041(5) -0.001(3) 0.004(3) 0.007(3) C28 0.032(3) 0.033(3) 0.050(5) -0.003(3) 0.000(3) -0.002(3) C29 0.028(3) 0.028(3) 0.043(5) 0.002(3) -0.002(3) -0.001(3) C30 0.034(3) 0.050(4) 0.040(5) 0.001(3) -0.005(3) -0.011(3) C31 0.046(4) 0.047(4) 0.055(5) 0.002(4) -0.001(4) -0.018(3) C32 0.036(4) 0.065(5) 0.055(5) 0.001(4) 0.008(4) -0.005(4) C33 0.033(3) 0.026(3) 0.040(4) 0.004(3) 0.011(3) 0.000(3) C34 0.041(4) 0.036(3) 0.041(5) 0.000(3) 0.008(3) -0.001(3) C35 0.030(3) 0.034(3) 0.064(5) 0.005(3) 0.003(3) -0.002(3) C36A 0.053(7) 0.035(9) 0.052(9) 0.007(6) -0.010(6) 0.005(6) C37A 0.100(7) 0.054(5) 0.142(10) -0.019(6) 0.040(7) -0.033(5) C38A 0.063(5) 0.054(5) 0.093(8) 0.017(5) 0.017(5) -0.006(4) C39A 0.043(6) 0.051(7) 0.090(12) -0.013(6) -0.008(7) 0.005(5) C36B 0.053(7) 0.035(9) 0.052(9) 0.007(6) -0.010(6) 0.005(6) C37B 0.100(7) 0.054(5) 0.142(10) -0.019(6) 0.040(7) -0.033(5) C38B 0.063(5) 0.054(5) 0.093(8) 0.017(5) 0.017(5) -0.006(4) C39B 0.043(6) 0.051(7) 0.090(12) -0.013(6) -0.008(7) 0.005(5) Cl1 0.0294(8) 0.0521(10) 0.0769(15) 0.0240(10) -0.0024(9) -0.0077(8) Cl2 0.0466(9) 0.0291(8) 0.0689(14) -0.0057(8) -0.0151(9) -0.0036(7) Cl3 0.124(2) 0.0703(13) 0.0527(15) 0.0108(11) 0.0361(14) 0.0395(13) N1 0.029(3) 0.029(3) 0.033(4) -0.003(2) 0.008(3) -0.001(2) N2 0.032(3) 0.027(2) 0.035(4) -0.005(2) 0.006(3) -0.005(2) N3 0.028(3) 0.027(2) 0.037(4) -0.006(3) 0.003(2) -0.002(2) N4 0.025(3) 0.026(3) 0.047(4) 0.000(3) 0.009(3) -0.002(2) N5 0.024(3) 0.027(3) 0.041(4) -0.001(2) 0.005(3) 0.001(2) Nb1 0.0304(3) 0.0319(3) 0.0367(4) -0.0006(3) 0.0048(3) 0.0081(3) O1A 0.052(4) 0.039(4) 0.108(7) -0.001(4) 0.011(5) -0.002(3) O1B 0.052(4) 0.039(4) 0.108(7) -0.001(4) 0.011(5) -0.002(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 N1 1.329(8) . ? C1 C17 1.386(8) . ? C1 N2 1.406(7) . ? C2 N3 1.359(7) . ? C2 N2 1.370(7) . ? C2 Nb1 2.206(6) . ? C3 C4 1.329(8) . ? C3 N3 1.387(8) . ? C3 H3 0.9500 . ? C4 N2 1.386(8) . ? C4 H4 0.9500 . ? C5 C10 1.387(8) . ? C5 C6 1.401(8) . ? C5 N3 1.458(7) . ? C6 C7 1.401(8) . ? C6 C14 1.501(9) . ? C7 C8 1.370(10) . ? C7 H7 0.9500 . ? C8 C9 1.372(10) . ? C8 H8 0.9500 . ? C9 C10 1.390(9) . ? C9 H9 0.9500 . ? C10 C11 1.514(9) . ? C11 C12 1.520(11) . ? C11 C13 1.532(10) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.516(10) . ? C14 C15 1.521(9) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.391(9) . ? C17 H17 0.9500 . ? C18 C19 1.369(10) . ? C18 H18 0.9500 . ? C19 C20 1.381(8) . ? C19 H19 0.9500 . ? C20 N1 1.345(7) . ? C20 N4 1.378(8) . ? C21 N5 1.358(8) . ? C21 N4 1.376(7) . ? C21 Nb1 2.203(6) . ? C22 C23 1.316(9) . ? C22 N5 1.402(7) . ? C22 H22 0.9500 . ? C23 N4 1.398(7) . ? C23 H23 0.9500 . ? C24 C29 1.394(8) . ? C24 C25 1.406(8) . ? C24 N5 1.442(8) . ? C25 C26 1.375(9) . ? C25 C33 1.517(9) . ? C26 C27 1.370(9) . ? C26 H26 0.9500 . ? C27 C28 1.392(8) . ? C27 H27 0.9500 . ? C28 C29 1.384(9) . ? C28 H28 0.9500 . ? C29 C30 1.518(8) . ? C30 C31 1.535(8) . ? C30 C32 1.541(9) . ? 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 1.527(8) . ? C33 C35 1.539(8) . ? 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 . ? C36A O1A 1.48(2) . ? C36A C37A 1.508(19) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A C38A 1.493(11) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C38A C39A 1.485(15) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C39A O1A 1.462(16) . ? C39A H39A 0.9900 . ? C39A H39B 0.9900 . ? C36B O1B 1.444(15) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C39B O1B 1.454(11) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? Cl1 Nb1 2.520(2) . ? Cl2 Nb1 2.473(2) . ? Cl3 Nb1 2.341(3) . ? N1 Nb1 2.248(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C17 125.1(6) . . ? N1 C1 N2 112.2(5) . . ? C17 C1 N2 122.7(6) . . ? N3 C2 N2 103.8(5) . . ? N3 C2 Nb1 137.8(4) . . ? N2 C2 Nb1 118.4(4) . . ? C4 C3 N3 107.8(6) . . ? C4 C3 H3 126.1 . . ? N3 C3 H3 126.1 . . ? C3 C4 N2 106.5(6) . . ? C3 C4 H4 126.7 . . ? N2 C4 H4 126.7 . . ? C10 C5 C6 124.4(6) . . ? C10 C5 N3 118.0(5) . . ? C6 C5 N3 117.4(5) . . ? C5 C6 C7 116.2(6) . . ? C5 C6 C14 123.9(5) . . ? C7 C6 C14 119.9(6) . . ? C8 C7 C6 120.8(7) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.7(6) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 121.9(7) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C5 C10 C9 116.0(6) . . ? C5 C10 C11 124.0(6) . . ? C9 C10 C11 120.0(6) . . ? C10 C11 C12 111.1(6) . . ? C10 C11 C13 110.3(6) . . ? C12 C11 C13 110.9(6) . . ? C10 C11 H11 108.1 . . ? C12 C11 H11 108.1 . . ? C13 C11 H11 108.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 C16 109.0(5) . . ? C6 C14 C15 112.4(6) . . ? C16 C14 C15 110.2(6) . . ? C6 C14 H14 108.4 . . ? C16 C14 H14 108.4 . . ? C15 C14 H14 108.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C17 C18 115.9(7) . . ? C1 C17 H17 122.1 . . ? C18 C17 H17 122.1 . . ? C19 C18 C17 121.0(6) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 117.9(6) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? N1 C20 N4 111.7(5) . . ? N1 C20 C19 123.3(7) . . ? N4 C20 C19 125.0(6) . . ? N5 C21 N4 104.3(5) . . ? N5 C21 Nb1 137.5(4) . . ? N4 C21 Nb1 118.2(5) . . ? C23 C22 N5 108.5(6) . . ? C23 C22 H22 125.8 . . ? N5 C22 H22 125.8 . . ? C22 C23 N4 106.5(5) . . ? C22 C23 H23 126.7 . . ? N4 C23 H23 126.7 . . ? C29 C24 C25 122.6(6) . . ? C29 C24 N5 117.4(5) . . ? C25 C24 N5 120.0(6) . . ? C26 C25 C24 117.3(6) . . ? C26 C25 C33 119.6(5) . . ? C24 C25 C33 123.1(6) . . ? C27 C26 C25 122.0(6) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 119.5(7) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 121.5(6) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C24 117.1(5) . . ? C28 C29 C30 120.4(6) . . ? C24 C29 C30 122.5(6) . . ? C29 C30 C31 110.7(5) . . ? C29 C30 C32 110.2(5) . . ? C31 C30 C32 110.6(6) . . ? C29 C30 H30 108.4 . . ? C31 C30 H30 108.4 . . ? C32 C30 H30 108.4 . . ? 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 . . ? C25 C33 C34 109.6(5) . . ? C25 C33 C35 111.7(5) . . ? C34 C33 C35 110.4(5) . . ? C25 C33 H33 108.4 . . ? C34 C33 H33 108.4 . . ? C35 C33 H33 108.4 . . ? 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 . . ? O1A C36A C37A 89.2(14) . . ? O1A C36A H36A 113.8 . . ? C37A C36A H36A 113.8 . . ? O1A C36A H36B 113.8 . . ? C37A C36A H36B 113.8 . . ? H36A C36A H36B 111.0 . . ? C38A C37A C36A 102.8(16) . . ? C38A C37A H37A 111.2 . . ? C36A C37A H37A 111.2 . . ? C38A C37A H37B 111.2 . . ? C36A C37A H37B 111.2 . . ? H37A C37A H37B 109.1 . . ? C39A C38A C37A 98.7(9) . . ? C39A C38A H38A 112.0 . . ? C37A C38A H38A 112.0 . . ? C39A C38A H38B 112.0 . . ? C37A C38A H38B 112.0 . . ? H38A C38A H38B 109.7 . . ? O1A C39A C38A 104.4(13) . . ? O1A C39A H39A 110.9 . . ? C38A C39A H39A 110.9 . . ? O1A C39A H39B 110.9 . . ? C38A C39A H39B 110.9 . . ? H39A C39A H39B 108.9 . . ? O1B C36B H36C 111.5 . . ? O1B C36B H36D 111.5 . . ? H36C C36B H36D 109.3 . . ? O1B C39B H39C 110.6 . . ? O1B C39B H39D 110.6 . . ? H39C C39B H39D 108.7 . . ? C1 N1 C20 116.7(5) . . ? C1 N1 Nb1 121.6(4) . . ? C20 N1 Nb1 121.7(5) . . ? C2 N2 C4 111.2(5) . . ? C2 N2 C1 117.8(5) . . ? C4 N2 C1 131.0(5) . . ? C2 N3 C3 110.7(5) . . ? C2 N3 C5 125.3(5) . . ? C3 N3 C5 124.0(5) . . ? C21 N4 C20 118.8(5) . . ? C21 N4 C23 110.7(6) . . ? C20 N4 C23 130.4(5) . . ? C21 N5 C22 110.0(5) . . ? C21 N5 C24 127.1(5) . . ? C22 N5 C24 122.3(6) . . ? C21 Nb1 C2 139.2(2) . . ? C21 Nb1 N1 69.5(2) . . ? C2 Nb1 N1 69.8(2) . . ? C21 Nb1 Cl3 114.66(18) . . ? C2 Nb1 Cl3 105.98(16) . . ? N1 Nb1 Cl3 175.79(15) . . ? C21 Nb1 Cl2 89.73(15) . . ? C2 Nb1 Cl2 91.79(15) . . ? N1 Nb1 Cl2 87.35(13) . . ? Cl3 Nb1 Cl2 92.73(9) . . ? C21 Nb1 Cl1 85.47(15) . . ? C2 Nb1 Cl1 87.54(15) . . ? N1 Nb1 Cl1 84.75(13) . . ? Cl3 Nb1 Cl1 95.30(9) . . ? Cl2 Nb1 Cl1 171.81(6) . . ? C39A O1A C36A 106.2(19) . . ? C36B O1B C39B 104.0(10) . . ? 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 N3 C3 C4 N2 0.0(7) . . . . ? C10 C5 C6 C7 -1.2(10) . . . . ? N3 C5 C6 C7 -175.5(6) . . . . ? C10 C5 C6 C14 177.0(6) . . . . ? N3 C5 C6 C14 2.7(9) . . . . ? C5 C6 C7 C8 -0.4(10) . . . . ? C14 C6 C7 C8 -178.7(7) . . . . ? C6 C7 C8 C9 0.2(12) . . . . ? C7 C8 C9 C10 1.5(13) . . . . ? C6 C5 C10 C9 2.7(10) . . . . ? N3 C5 C10 C9 177.1(6) . . . . ? C6 C5 C10 C11 -177.8(7) . . . . ? N3 C5 C10 C11 -3.5(10) . . . . ? C8 C9 C10 C5 -2.9(11) . . . . ? C8 C9 C10 C11 177.6(7) . . . . ? C5 C10 C11 C12 -126.2(7) . . . . ? C9 C10 C11 C12 53.2(9) . . . . ? C5 C10 C11 C13 110.4(7) . . . . ? C9 C10 C11 C13 -70.2(9) . . . . ? C5 C6 C14 C16 -106.2(7) . . . . ? C7 C6 C14 C16 71.9(8) . . . . ? C5 C6 C14 C15 131.3(7) . . . . ? C7 C6 C14 C15 -50.5(8) . . . . ? N1 C1 C17 C18 1.8(9) . . . . ? N2 C1 C17 C18 -179.0(5) . . . . ? C1 C17 C18 C19 1.1(9) . . . . ? C17 C18 C19 C20 -1.6(9) . . . . ? C18 C19 C20 N1 -0.7(9) . . . . ? C18 C19 C20 N4 -179.6(6) . . . . ? N5 C22 C23 N4 -0.2(6) . . . . ? C29 C24 C25 C26 -1.8(9) . . . . ? N5 C24 C25 C26 176.0(5) . . . . ? C29 C24 C25 C33 -179.0(5) . . . . ? N5 C24 C25 C33 -1.2(8) . . . . ? C24 C25 C26 C27 1.1(9) . . . . ? C33 C25 C26 C27 178.4(5) . . . . ? C25 C26 C27 C28 -0.4(9) . . . . ? C26 C27 C28 C29 0.2(9) . . . . ? C27 C28 C29 C24 -0.8(9) . . . . ? C27 C28 C29 C30 -179.3(6) . . . . ? C25 C24 C29 C28 1.6(9) . . . . ? N5 C24 C29 C28 -176.2(5) . . . . ? C25 C24 C29 C30 -179.9(5) . . . . ? N5 C24 C29 C30 2.3(8) . . . . ? C28 C29 C30 C31 -52.9(8) . . . . ? C24 C29 C30 C31 128.7(6) . . . . ? C28 C29 C30 C32 69.7(7) . . . . ? C24 C29 C30 C32 -108.7(7) . . . . ? C26 C25 C33 C34 -68.6(7) . . . . ? C24 C25 C33 C34 108.5(6) . . . . ? C26 C25 C33 C35 54.0(7) . . . . ? C24 C25 C33 C35 -128.8(6) . . . . ? O1A C36A C37A C38A 60(2) . . . . ? C36A C37A C38A C39A -46.0(17) . . . . ? C37A C38A C39A O1A 11.3(17) . . . . ? C17 C1 N1 C20 -4.0(8) . . . . ? N2 C1 N1 C20 176.8(4) . . . . ? C17 C1 N1 Nb1 175.8(4) . . . . ? N2 C1 N1 Nb1 -3.5(6) . . . . ? N4 C20 N1 C1 -177.6(5) . . . . ? C19 C20 N1 C1 3.4(8) . . . . ? N4 C20 N1 Nb1 2.7(6) . . . . ? C19 C20 N1 Nb1 -176.4(4) . . . . ? N3 C2 N2 C4 -0.6(6) . . . . ? Nb1 C2 N2 C4 178.1(4) . . . . ? N3 C2 N2 C1 -178.1(4) . . . . ? Nb1 C2 N2 C1 0.6(6) . . . . ? C3 C4 N2 C2 0.4(7) . . . . ? C3 C4 N2 C1 177.4(5) . . . . ? N1 C1 N2 C2 1.8(7) . . . . ? C17 C1 N2 C2 -177.5(5) . . . . ? N1 C1 N2 C4 -175.1(5) . . . . ? C17 C1 N2 C4 5.6(9) . . . . ? N2 C2 N3 C3 0.6(6) . . . . ? Nb1 C2 N3 C3 -177.7(4) . . . . ? N2 C2 N3 C5 -178.1(5) . . . . ? Nb1 C2 N3 C5 3.5(8) . . . . ? C4 C3 N3 C2 -0.4(7) . . . . ? C4 C3 N3 C5 178.4(5) . . . . ? C10 C5 N3 C2 89.6(7) . . . . ? C6 C5 N3 C2 -95.7(7) . . . . ? C10 C5 N3 C3 -89.0(7) . . . . ? C6 C5 N3 C3 85.7(7) . . . . ? N5 C21 N4 C20 -177.9(5) . . . . ? Nb1 C21 N4 C20 3.0(7) . . . . ? N5 C21 N4 C23 0.3(6) . . . . ? Nb1 C21 N4 C23 -178.8(4) . . . . ? N1 C20 N4 C21 -3.6(7) . . . . ? C19 C20 N4 C21 175.4(5) . . . . ? N1 C20 N4 C23 178.6(5) . . . . ? C19 C20 N4 C23 -2.3(10) . . . . ? C22 C23 N4 C21 -0.1(6) . . . . ? C22 C23 N4 C20 177.9(6) . . . . ? N4 C21 N5 C22 -0.5(6) . . . . ? Nb1 C21 N5 C22 178.4(4) . . . . ? N4 C21 N5 C24 170.5(5) . . . . ? Nb1 C21 N5 C24 -10.6(9) . . . . ? C23 C22 N5 C21 0.5(7) . . . . ? C23 C22 N5 C24 -171.0(5) . . . . ? C29 C24 N5 C21 -94.4(7) . . . . ? C25 C24 N5 C21 87.7(7) . . . . ? C29 C24 N5 C22 75.5(7) . . . . ? C25 C24 N5 C22 -102.3(6) . . . . ? N5 C21 Nb1 C2 -174.7(5) . . . . ? N4 C21 Nb1 C2 4.1(6) . . . . ? N5 C21 Nb1 N1 -179.9(6) . . . . ? N4 C21 Nb1 N1 -1.1(4) . . . . ? N5 C21 Nb1 Cl3 0.0(6) . . . . ? N4 C21 Nb1 Cl3 178.8(3) . . . . ? N5 C21 Nb1 Cl2 92.9(6) . . . . ? N4 C21 Nb1 Cl2 -88.4(4) . . . . ? N5 C21 Nb1 Cl1 -93.8(6) . . . . ? N4 C21 Nb1 Cl1 85.0(4) . . . . ? N3 C2 Nb1 C21 171.3(5) . . . . ? N2 C2 Nb1 C21 -6.9(6) . . . . ? N3 C2 Nb1 N1 176.4(6) . . . . ? N2 C2 Nb1 N1 -1.7(4) . . . . ? N3 C2 Nb1 Cl3 -3.7(6) . . . . ? N2 C2 Nb1 Cl3 178.2(4) . . . . ? N3 C2 Nb1 Cl2 -97.1(5) . . . . ? N2 C2 Nb1 Cl2 84.8(4) . . . . ? N3 C2 Nb1 Cl1 91.1(5) . . . . ? N2 C2 Nb1 Cl1 -87.0(4) . . . . ? C1 N1 Nb1 C21 179.3(5) . . . . ? C20 N1 Nb1 C21 -0.9(4) . . . . ? C1 N1 Nb1 C2 2.9(4) . . . . ? C20 N1 Nb1 C2 -177.3(5) . . . . ? C1 N1 Nb1 Cl2 -90.0(4) . . . . ? C20 N1 Nb1 Cl2 89.8(4) . . . . ? C1 N1 Nb1 Cl1 92.2(4) . . . . ? C20 N1 Nb1 Cl1 -88.0(4) . . . . ? C38A C39A O1A C36A 27(2) . . . . ? C37A C36A O1A C39A -52(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.069 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.099 #==END data_5 _database_code_depnum_ccdc_archive 'CCDC 282403' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Cl4 N5 U, C4 H8 O' _chemical_formula_sum 'C39 H49 Cl4 N5 O U' _chemical_formula_weight 983.66 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' Cl Cl 0.1484 0.1585 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7146(8) _cell_length_b 18.384(2) _cell_length_c 20.229(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.628(10) _cell_angle_gamma 90.00 _cell_volume 3976.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6319 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 4.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2835 _exptl_absorpt_correction_T_max 0.4171 _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 37286 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.15 _reflns_number_total 7713 _reflns_number_gt 6186 _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-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 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^)+(0.0206P)^2^+21.0719P] 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 7713 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9415(5) 0.1763(3) 0.5447(2) 0.0207(11) Uani 1 1 d . . . C2 C 0.7811(5) 0.2512(3) 0.4862(2) 0.0181(11) Uani 1 1 d . . . C3 C 0.6981(5) 0.3004(3) 0.5754(2) 0.0238(12) Uani 1 1 d . . . H3 H 0.6442 0.3286 0.6008 0.029 Uiso 1 1 calc R . . C4 C 0.7920(5) 0.2584(3) 0.5995(3) 0.0237(12) Uani 1 1 d . . . H4 H 0.8186 0.2509 0.6446 0.028 Uiso 1 1 calc R . . C5 C 0.5980(5) 0.3331(3) 0.4656(2) 0.0230(12) Uani 1 1 d . . . C6 C 0.6284(5) 0.3999(3) 0.4380(3) 0.0264(13) Uani 1 1 d . . . C7 C 0.5320(6) 0.4347(3) 0.3999(3) 0.0360(15) Uani 1 1 d . . . H7 H 0.5480 0.4802 0.3800 0.043 Uiso 1 1 calc R . . C8 C 0.4152(6) 0.4044(3) 0.3909(3) 0.0377(15) Uani 1 1 d . . . H8 H 0.3516 0.4294 0.3652 0.045 Uiso 1 1 calc R . . C9 C 0.3893(5) 0.3383(3) 0.4187(3) 0.0341(14) Uani 1 1 d . . . H9 H 0.3082 0.3178 0.4113 0.041 Uiso 1 1 calc R . . C10 C 0.4802(5) 0.3009(3) 0.4575(3) 0.0259(13) Uani 1 1 d . . . C11 C 0.4503(5) 0.2276(3) 0.4869(3) 0.0296(13) Uani 1 1 d . . . H11 H 0.5293 0.2068 0.5080 0.036 Uiso 1 1 calc R . . C12 C 0.3978(6) 0.1738(3) 0.4339(3) 0.0399(15) Uani 1 1 d . . . H12A H 0.3179 0.1921 0.4142 0.060 Uiso 1 1 calc R . . H12B H 0.3848 0.1263 0.4544 0.060 Uiso 1 1 calc R . . H12C H 0.4573 0.1687 0.3993 0.060 Uiso 1 1 calc R . . C13 C 0.3574(6) 0.2377(4) 0.5405(3) 0.0448(17) Uani 1 1 d . . . H13A H 0.3939 0.2698 0.5752 0.067 Uiso 1 1 calc R . . H13B H 0.3386 0.1904 0.5598 0.067 Uiso 1 1 calc R . . H13C H 0.2801 0.2594 0.5209 0.067 Uiso 1 1 calc R . . C14 C 0.7570(5) 0.4338(3) 0.4457(3) 0.0305(13) Uani 1 1 d . . . H14 H 0.8143 0.3980 0.4694 0.037 Uiso 1 1 calc R . . C15 C 0.7558(6) 0.5027(3) 0.4877(3) 0.0418(16) Uani 1 1 d . . . H15A H 0.7027 0.5394 0.4648 0.063 Uiso 1 1 calc R . . H15B H 0.8411 0.5216 0.4948 0.063 Uiso 1 1 calc R . . H15C H 0.7227 0.4914 0.5306 0.063 Uiso 1 1 calc R . . C16 C 0.8080(6) 0.4489(3) 0.3778(3) 0.0416(16) Uani 1 1 d . . . H16A H 0.7997 0.4051 0.3503 0.062 Uiso 1 1 calc R . . H16B H 0.8964 0.4627 0.3837 0.062 Uiso 1 1 calc R . . H16C H 0.7604 0.4887 0.3560 0.062 Uiso 1 1 calc R . . C17 C 0.9996(5) 0.1516(3) 0.6032(3) 0.0241(12) Uani 1 1 d . . . H17 H 0.9784 0.1703 0.6448 0.029 Uiso 1 1 calc R . . C18 C 1.0893(5) 0.0987(3) 0.5988(3) 0.0282(13) Uani 1 1 d . . . H18 H 1.1305 0.0797 0.6381 0.034 Uiso 1 1 calc R . . C19 C 1.1202(5) 0.0729(3) 0.5375(3) 0.0257(12) Uani 1 1 d . . . H19 H 1.1812 0.0359 0.5338 0.031 Uiso 1 1 calc R . . C20 C 1.0591(5) 0.1031(3) 0.4825(2) 0.0204(11) Uani 1 1 d . . . C21 C 1.0386(5) 0.1172(3) 0.3619(2) 0.0197(11) Uani 1 1 d . . . C22 C 1.1633(5) 0.0234(3) 0.3354(3) 0.0236(12) Uani 1 1 d . . . H22 H 1.2066 -0.0100 0.3093 0.028 Uiso 1 1 calc R . . C23 C 1.1633(5) 0.0236(3) 0.4015(3) 0.0242(12) Uani 1 1 d . . . H23 H 1.2070 -0.0087 0.4314 0.029 Uiso 1 1 calc R . . C24 C 1.0740(5) 0.0985(3) 0.2415(2) 0.0218(12) Uani 1 1 d . . . C25 C 0.9683(5) 0.0732(3) 0.2049(2) 0.0206(11) Uani 1 1 d . . . C26 C 0.9597(5) 0.0907(3) 0.1376(3) 0.0255(12) Uani 1 1 d . . . H26 H 0.8895 0.0741 0.1107 0.031 Uiso 1 1 calc R . . C27 C 1.0494(5) 0.1312(3) 0.1092(3) 0.0283(13) Uani 1 1 d . . . H27 H 1.0408 0.1424 0.0633 0.034 Uiso 1 1 calc R . . C28 C 1.1524(5) 0.1558(3) 0.1474(3) 0.0275(13) Uani 1 1 d . . . H28 H 1.2137 0.1842 0.1274 0.033 Uiso 1 1 calc R . . C29 C 1.1679(5) 0.1396(3) 0.2146(3) 0.0241(12) Uani 1 1 d . . . C30 C 1.2834(5) 0.1662(3) 0.2548(3) 0.0292(13) Uani 1 1 d . . . H30 H 1.2752 0.1515 0.3019 0.035 Uiso 1 1 calc R . . C31 C 1.2949(6) 0.2488(3) 0.2528(3) 0.0419(16) Uani 1 1 d . . . H31A H 1.3017 0.2647 0.2069 0.063 Uiso 1 1 calc R . . H31B H 1.3698 0.2639 0.2796 0.063 Uiso 1 1 calc R . . H31C H 1.2208 0.2708 0.2705 0.063 Uiso 1 1 calc R . . C32 C 1.4021(5) 0.1308(4) 0.2311(3) 0.0430(16) Uani 1 1 d . . . H32A H 1.3952 0.0778 0.2345 0.065 Uiso 1 1 calc R . . H32B H 1.4748 0.1476 0.2588 0.065 Uiso 1 1 calc R . . H32C H 1.4121 0.1444 0.1849 0.065 Uiso 1 1 calc R . . C33 C 0.8677(5) 0.0281(3) 0.2344(3) 0.0252(12) Uani 1 1 d . . . H33 H 0.8797 0.0323 0.2837 0.030 Uiso 1 1 calc R . . C34 C 0.8820(6) -0.0517(3) 0.2165(3) 0.0324(14) Uani 1 1 d . . . H34A H 0.8783 -0.0569 0.1682 0.049 Uiso 1 1 calc R . . H34B H 0.8143 -0.0799 0.2345 0.049 Uiso 1 1 calc R . . H34C H 0.9628 -0.0697 0.2353 0.049 Uiso 1 1 calc R . . C35 C 0.7366(5) 0.0567(3) 0.2139(3) 0.0315(14) Uani 1 1 d . . . H35A H 0.7310 0.1082 0.2258 0.047 Uiso 1 1 calc R . . H35B H 0.6743 0.0289 0.2368 0.047 Uiso 1 1 calc R . . H35C H 0.7206 0.0512 0.1659 0.047 Uiso 1 1 calc R . . C36 C 0.6262(6) 0.3646(3) 0.1808(3) 0.0394(15) Uani 1 1 d . . . H36A H 0.7069 0.3617 0.2073 0.047 Uiso 1 1 calc R . . H36B H 0.5938 0.3146 0.1734 0.047 Uiso 1 1 calc R . . C37 C 0.5349(6) 0.4090(3) 0.2161(3) 0.0408(16) Uani 1 1 d . . . H37A H 0.5758 0.4512 0.2389 0.049 Uiso 1 1 calc R . . H37B H 0.4915 0.3795 0.2486 0.049 Uiso 1 1 calc R . . C38 C 0.4471(7) 0.4325(5) 0.1593(4) 0.061(2) Uani 1 1 d . . . H38A H 0.4057 0.4790 0.1693 0.073 Uiso 1 1 calc R . . H38B H 0.3825 0.3951 0.1488 0.073 Uiso 1 1 calc R . . C39 C 0.5337(6) 0.4414(4) 0.1024(3) 0.0492(18) Uani 1 1 d . . . H39A H 0.4918 0.4239 0.0604 0.059 Uiso 1 1 calc R . . H39B H 0.5562 0.4932 0.0970 0.059 Uiso 1 1 calc R . . Cl1 Cl 1.03593(11) 0.30767(7) 0.42507(6) 0.0193(3) Uani 1 1 d . . . Cl2 Cl 0.74489(11) 0.09022(6) 0.39527(6) 0.0205(3) Uani 1 1 d . . . Cl3 Cl 0.94245(13) 0.26069(7) 0.26127(6) 0.0262(3) Uani 1 1 d . . . Cl4 Cl 0.65203(12) 0.25627(8) 0.32262(7) 0.0279(3) Uani 1 1 d . . . N1 N 0.9707(4) 0.1538(2) 0.48438(19) 0.0174(9) Uani 1 1 d . . . N2 N 0.8429(4) 0.2278(2) 0.54390(19) 0.0184(9) Uani 1 1 d . . . N3 N 0.6930(4) 0.2959(2) 0.5071(2) 0.0196(9) Uani 1 1 d . . . N4 N 1.0856(4) 0.0812(2) 0.4174(2) 0.0184(9) Uani 1 1 d . . . N5 N 1.0885(4) 0.0806(2) 0.3117(2) 0.0185(9) Uani 1 1 d . . . O1 O 0.6426(4) 0.3992(2) 0.1192(2) 0.0419(11) Uani 1 1 d . . . U1 U 0.867082(17) 0.214196(10) 0.375139(9) 0.01797(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 0.018(3) 0.021(3) 0.023(3) 0.004(2) -0.001(2) -0.006(2) C2 0.016(3) 0.018(3) 0.020(3) 0.004(2) 0.002(2) -0.001(2) C3 0.024(3) 0.028(3) 0.020(3) -0.003(2) 0.006(2) 0.000(2) C4 0.025(3) 0.031(3) 0.016(3) -0.001(2) 0.003(2) -0.002(2) C5 0.024(3) 0.026(3) 0.019(3) -0.001(2) 0.000(2) 0.007(2) C6 0.030(3) 0.024(3) 0.025(3) -0.002(2) 0.007(2) 0.007(2) C7 0.047(4) 0.032(3) 0.030(3) 0.003(3) 0.007(3) 0.011(3) C8 0.030(4) 0.042(4) 0.041(4) 0.001(3) 0.002(3) 0.019(3) C9 0.020(3) 0.053(4) 0.029(3) -0.008(3) -0.001(2) 0.004(3) C10 0.020(3) 0.035(3) 0.023(3) -0.003(2) 0.005(2) 0.001(2) C11 0.020(3) 0.041(4) 0.028(3) -0.002(3) 0.003(2) -0.004(3) C12 0.035(4) 0.042(4) 0.043(4) -0.007(3) 0.002(3) -0.009(3) C13 0.038(4) 0.064(5) 0.033(4) 0.002(3) 0.013(3) -0.003(3) C14 0.033(3) 0.020(3) 0.040(3) 0.004(2) 0.007(3) -0.001(3) C15 0.051(4) 0.033(4) 0.042(4) 0.000(3) 0.009(3) -0.003(3) C16 0.045(4) 0.035(4) 0.046(4) 0.001(3) 0.017(3) -0.005(3) C17 0.025(3) 0.029(3) 0.018(3) 0.000(2) 0.002(2) 0.002(2) C18 0.027(3) 0.033(3) 0.024(3) 0.008(2) -0.003(2) 0.004(3) C19 0.024(3) 0.026(3) 0.027(3) 0.005(2) -0.001(2) 0.001(2) C20 0.019(3) 0.020(3) 0.022(3) 0.003(2) -0.001(2) -0.005(2) C21 0.017(3) 0.026(3) 0.016(3) -0.001(2) 0.000(2) -0.004(2) C22 0.021(3) 0.023(3) 0.027(3) -0.003(2) 0.001(2) 0.004(2) C23 0.022(3) 0.020(3) 0.030(3) 0.001(2) -0.002(2) 0.004(2) C24 0.024(3) 0.024(3) 0.017(3) -0.003(2) -0.001(2) 0.006(2) C25 0.022(3) 0.019(3) 0.021(3) -0.005(2) 0.003(2) 0.004(2) C26 0.022(3) 0.028(3) 0.027(3) -0.005(2) -0.001(2) 0.002(2) C27 0.034(3) 0.031(3) 0.021(3) 0.001(2) 0.007(2) 0.004(3) C28 0.023(3) 0.027(3) 0.033(3) 0.002(2) 0.008(2) 0.001(2) C29 0.023(3) 0.022(3) 0.027(3) -0.002(2) 0.004(2) -0.002(2) C30 0.028(3) 0.030(3) 0.030(3) -0.002(3) 0.004(3) -0.005(3) C31 0.031(4) 0.033(4) 0.060(4) -0.006(3) -0.004(3) -0.001(3) C32 0.028(3) 0.042(4) 0.059(4) -0.008(3) -0.004(3) 0.004(3) C33 0.023(3) 0.027(3) 0.025(3) 0.001(2) 0.001(2) -0.003(2) C34 0.036(4) 0.027(3) 0.034(3) -0.002(3) 0.003(3) -0.001(3) C35 0.021(3) 0.039(4) 0.034(3) -0.003(3) 0.003(3) -0.003(3) C36 0.036(4) 0.036(4) 0.046(4) 0.005(3) 0.007(3) 0.004(3) C37 0.046(4) 0.037(4) 0.040(4) -0.001(3) 0.007(3) 0.002(3) C38 0.056(5) 0.068(5) 0.058(5) -0.001(4) -0.001(4) 0.025(4) C39 0.044(4) 0.053(4) 0.049(4) 0.012(4) -0.007(3) -0.004(4) Cl1 0.0179(6) 0.0230(6) 0.0171(6) -0.0007(5) 0.0007(5) -0.0069(5) Cl2 0.0208(6) 0.0134(6) 0.0266(7) 0.0009(5) -0.0038(5) -0.0027(5) Cl3 0.0287(7) 0.0320(7) 0.0182(6) 0.0039(5) 0.0040(5) 0.0015(6) Cl4 0.0193(7) 0.0345(8) 0.0296(7) 0.0030(6) -0.0021(6) 0.0041(6) N1 0.018(2) 0.017(2) 0.017(2) 0.0022(17) 0.0002(17) 0.0028(18) N2 0.021(2) 0.018(2) 0.016(2) 0.0018(17) -0.0005(17) -0.0005(18) N3 0.021(2) 0.019(2) 0.020(2) 0.0010(18) 0.0031(18) 0.0006(18) N4 0.017(2) 0.017(2) 0.021(2) 0.0006(18) -0.0021(18) 0.0022(18) N5 0.015(2) 0.020(2) 0.021(2) -0.0012(18) 0.0005(18) 0.0016(18) O1 0.044(3) 0.039(2) 0.044(3) 0.005(2) 0.009(2) -0.001(2) U1 0.01716(10) 0.02000(10) 0.01669(10) 0.00074(9) 0.00067(7) 0.00113(9) _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 N1 1.344(6) . ? C1 C17 1.380(7) . ? C1 N2 1.417(6) . ? C2 N3 1.340(6) . ? C2 N2 1.375(6) . ? C2 U1 2.573(5) . ? C3 C4 1.336(7) . ? C3 N3 1.382(6) . ? C3 H3 0.9500 . ? C4 N2 1.398(6) . ? C4 H4 0.9500 . ? C5 C10 1.395(7) . ? C5 C6 1.396(7) . ? C5 N3 1.448(6) . ? C6 C7 1.403(8) . ? C6 C14 1.512(8) . ? C7 C8 1.371(9) . ? C7 H7 0.9500 . ? C8 C9 1.375(9) . ? C8 H8 0.9500 . ? C9 C10 1.394(8) . ? C9 H9 0.9500 . ? C10 C11 1.514(8) . ? C11 C13 1.529(8) . ? C11 C12 1.539(8) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.527(8) . ? C14 C16 1.536(8) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.374(7) . ? C17 H17 0.9500 . ? C18 C19 1.388(7) . ? C18 H18 0.9500 . ? C19 C20 1.372(7) . ? C19 H19 0.9500 . ? C20 N1 1.331(6) . ? C20 N4 1.422(6) . ? C21 N5 1.356(6) . ? C21 N4 1.371(6) . ? C21 U1 2.587(5) . ? C22 C23 1.336(7) . ? C22 N5 1.390(6) . ? C22 H22 0.9500 . ? C23 N4 1.397(6) . ? C23 H23 0.9500 . ? C24 C25 1.395(7) . ? C24 C29 1.397(7) . ? C24 N5 1.455(6) . ? C25 C26 1.396(7) . ? C25 C33 1.512(7) . ? C26 C27 1.371(7) . ? C26 H26 0.9500 . ? C27 C28 1.382(8) . ? C27 H27 0.9500 . ? C28 C29 1.391(7) . ? C28 H28 0.9500 . ? C29 C30 1.517(7) . ? C30 C31 1.524(8) . ? C30 C32 1.532(8) . ? 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(7) . ? C33 C35 1.533(7) . ? 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 O1 1.420(7) . ? C36 C37 1.492(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.501(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.533(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O1 1.424(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? Cl1 U1 2.6486(12) . ? Cl2 U1 2.6725(12) . ? Cl3 U1 2.6314(13) . ? Cl4 U1 2.5936(13) . ? N1 U1 2.653(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 N1 C1 C17 124.0(5) . . ? N1 C1 N2 114.4(4) . . ? C17 C1 N2 121.7(5) . . ? N3 C2 N2 103.6(4) . . ? N3 C2 U1 137.4(3) . . ? N2 C2 U1 118.6(3) . . ? C4 C3 N3 108.1(4) . . ? C4 C3 H3 126.0 . . ? N3 C3 H3 126.0 . . ? C3 C4 N2 105.2(4) . . ? C3 C4 H4 127.4 . . ? N2 C4 H4 127.4 . . ? C10 C5 C6 124.0(5) . . ? C10 C5 N3 117.7(5) . . ? C6 C5 N3 118.3(5) . . ? C5 C6 C7 116.0(5) . . ? C5 C6 C14 123.7(5) . . ? C7 C6 C14 120.2(5) . . ? C8 C7 C6 121.5(6) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 120.7(6) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 121.0(6) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C5 116.9(5) . . ? C9 C10 C11 120.2(5) . . ? C5 C10 C11 122.9(5) . . ? C10 C11 C13 109.5(5) . . ? C10 C11 C12 112.0(5) . . ? C13 C11 C12 110.3(5) . . ? C10 C11 H11 108.3 . . ? C13 C11 H11 108.3 . . ? C12 C11 H11 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 C15 111.0(5) . . ? C6 C14 C16 110.9(5) . . ? C15 C14 C16 111.3(5) . . ? C6 C14 H14 107.8 . . ? C15 C14 H14 107.8 . . ? C16 C14 H14 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C1 117.2(5) . . ? C18 C17 H17 121.4 . . ? C1 C17 H17 121.4 . . ? C17 C18 C19 120.5(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 117.3(5) . . ? C20 C19 H19 121.4 . . ? C18 C19 H19 121.4 . . ? N1 C20 C19 124.3(5) . . ? N1 C20 N4 114.1(4) . . ? C19 C20 N4 121.6(5) . . ? N5 C21 N4 103.5(4) . . ? N5 C21 U1 137.4(3) . . ? N4 C21 U1 118.3(3) . . ? C23 C22 N5 107.8(5) . . ? C23 C22 H22 126.1 . . ? N5 C22 H22 126.1 . . ? C22 C23 N4 105.7(5) . . ? C22 C23 H23 127.1 . . ? N4 C23 H23 127.1 . . ? C25 C24 C29 123.6(5) . . ? C25 C24 N5 118.4(4) . . ? C29 C24 N5 117.9(4) . . ? C24 C25 C26 116.3(5) . . ? C24 C25 C33 123.2(5) . . ? C26 C25 C33 120.4(5) . . ? C27 C26 C25 122.0(5) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 119.9(5) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 121.2(5) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C28 C29 C24 116.9(5) . . ? C28 C29 C30 119.9(5) . . ? C24 C29 C30 123.2(5) . . ? C29 C30 C31 111.8(5) . . ? C29 C30 C32 111.1(5) . . ? C31 C30 C32 110.1(5) . . ? C29 C30 H30 107.9 . . ? C31 C30 H30 107.9 . . ? C32 C30 H30 107.9 . . ? 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 . . ? C25 C33 C34 110.5(4) . . ? C25 C33 C35 111.7(4) . . ? C34 C33 C35 111.8(5) . . ? C25 C33 H33 107.6 . . ? C34 C33 H33 107.6 . . ? C35 C33 H33 107.6 . . ? 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 . . ? O1 C36 C37 107.3(5) . . ? O1 C36 H36A 110.3 . . ? C37 C36 H36A 110.3 . . ? O1 C36 H36B 110.3 . . ? C37 C36 H36B 110.3 . . ? H36A C36 H36B 108.5 . . ? C36 C37 C38 100.9(5) . . ? C36 C37 H37A 111.6 . . ? C38 C37 H37A 111.6 . . ? C36 C37 H37B 111.6 . . ? C38 C37 H37B 111.6 . . ? H37A C37 H37B 109.4 . . ? C37 C38 C39 103.1(6) . . ? C37 C38 H38A 111.1 . . ? C39 C38 H38A 111.1 . . ? C37 C38 H38B 111.1 . . ? C39 C38 H38B 111.1 . . ? H38A C38 H38B 109.1 . . ? O1 C39 C38 106.8(5) . . ? 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 . . ? C20 N1 C1 116.7(4) . . ? C20 N1 U1 122.0(3) . . ? C1 N1 U1 121.2(3) . . ? C2 N2 C4 111.5(4) . . ? C2 N2 C1 122.5(4) . . ? C4 N2 C1 126.0(4) . . ? C2 N3 C3 111.6(4) . . ? C2 N3 C5 126.1(4) . . ? C3 N3 C5 122.2(4) . . ? C21 N4 C23 111.7(4) . . ? C21 N4 C20 122.5(4) . . ? C23 N4 C20 125.8(4) . . ? C21 N5 C22 111.2(4) . . ? C21 N5 C24 126.5(4) . . ? C22 N5 C24 122.2(4) . . ? C36 O1 C39 108.0(5) . . ? C2 U1 C21 124.68(15) . . ? C2 U1 Cl4 85.44(11) . . ? C21 U1 Cl4 141.43(11) . . ? C2 U1 Cl3 145.58(11) . . ? C21 U1 Cl3 82.76(11) . . ? Cl4 U1 Cl3 81.86(4) . . ? C2 U1 Cl1 76.65(11) . . ? C21 U1 Cl1 90.81(11) . . ? Cl4 U1 Cl1 122.03(4) . . ? Cl3 U1 Cl1 83.28(4) . . ? C2 U1 N1 62.47(14) . . ? C21 U1 N1 62.30(14) . . ? Cl4 U1 N1 141.27(9) . . ? Cl3 U1 N1 136.87(9) . . ? Cl1 U1 N1 73.40(9) . . ? C2 U1 Cl2 83.50(11) . . ? C21 U1 Cl2 77.64(11) . . ? Cl4 U1 Cl2 83.44(4) . . ? Cl3 U1 Cl2 126.22(4) . . ? Cl1 U1 Cl2 145.55(4) . . ? N1 U1 Cl2 72.50(9) . . ? 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 N3 C3 C4 N2 -0.5(6) . . . . ? C10 C5 C6 C7 -0.3(8) . . . . ? N3 C5 C6 C7 -178.1(4) . . . . ? C10 C5 C6 C14 -178.6(5) . . . . ? N3 C5 C6 C14 3.6(7) . . . . ? C5 C6 C7 C8 0.2(8) . . . . ? C14 C6 C7 C8 178.5(5) . . . . ? C6 C7 C8 C9 -0.6(9) . . . . ? C7 C8 C9 C10 1.0(9) . . . . ? C8 C9 C10 C5 -1.1(8) . . . . ? C8 C9 C10 C11 -179.2(5) . . . . ? C6 C5 C10 C9 0.7(8) . . . . ? N3 C5 C10 C9 178.6(5) . . . . ? C6 C5 C10 C11 178.8(5) . . . . ? N3 C5 C10 C11 -3.4(7) . . . . ? C9 C10 C11 C13 -69.1(7) . . . . ? C5 C10 C11 C13 112.9(6) . . . . ? C9 C10 C11 C12 53.6(7) . . . . ? C5 C10 C11 C12 -124.4(6) . . . . ? C5 C6 C14 C15 -112.6(6) . . . . ? C7 C6 C14 C15 69.3(7) . . . . ? C5 C6 C14 C16 123.1(6) . . . . ? C7 C6 C14 C16 -55.0(7) . . . . ? N1 C1 C17 C18 -2.5(8) . . . . ? N2 C1 C17 C18 176.5(5) . . . . ? C1 C17 C18 C19 1.0(8) . . . . ? C17 C18 C19 C20 0.9(8) . . . . ? C18 C19 C20 N1 -1.7(8) . . . . ? C18 C19 C20 N4 178.9(5) . . . . ? N5 C22 C23 N4 1.0(6) . . . . ? C29 C24 C25 C26 0.3(8) . . . . ? N5 C24 C25 C26 -178.9(4) . . . . ? C29 C24 C25 C33 179.4(5) . . . . ? N5 C24 C25 C33 0.1(7) . . . . ? C24 C25 C26 C27 -0.7(8) . . . . ? C33 C25 C26 C27 -179.7(5) . . . . ? C25 C26 C27 C28 0.2(8) . . . . ? C26 C27 C28 C29 0.6(8) . . . . ? C27 C28 C29 C24 -0.9(8) . . . . ? C27 C28 C29 C30 178.8(5) . . . . ? C25 C24 C29 C28 0.4(8) . . . . ? N5 C24 C29 C28 179.7(4) . . . . ? C25 C24 C29 C30 -179.3(5) . . . . ? N5 C24 C29 C30 0.0(7) . . . . ? C28 C29 C30 C31 58.6(7) . . . . ? C24 C29 C30 C31 -121.7(6) . . . . ? C28 C29 C30 C32 -64.9(7) . . . . ? C24 C29 C30 C32 114.8(6) . . . . ? C24 C25 C33 C34 -102.2(6) . . . . ? C26 C25 C33 C34 76.8(6) . . . . ? C24 C25 C33 C35 132.7(5) . . . . ? C26 C25 C33 C35 -48.3(7) . . . . ? O1 C36 C37 C38 36.9(7) . . . . ? C36 C37 C38 C39 -34.2(7) . . . . ? C37 C38 C39 O1 21.3(8) . . . . ? C19 C20 N1 C1 0.4(7) . . . . ? N4 C20 N1 C1 179.8(4) . . . . ? C19 C20 N1 U1 176.4(4) . . . . ? N4 C20 N1 U1 -4.1(6) . . . . ? C17 C1 N1 C20 1.8(7) . . . . ? N2 C1 N1 C20 -177.2(4) . . . . ? C17 C1 N1 U1 -174.3(4) . . . . ? N2 C1 N1 U1 6.7(6) . . . . ? N3 C2 N2 C4 0.0(5) . . . . ? U1 C2 N2 C4 174.0(3) . . . . ? N3 C2 N2 C1 177.2(4) . . . . ? U1 C2 N2 C1 -8.8(6) . . . . ? C3 C4 N2 C2 0.3(6) . . . . ? C3 C4 N2 C1 -176.7(5) . . . . ? N1 C1 N2 C2 1.3(7) . . . . ? C17 C1 N2 C2 -177.7(5) . . . . ? N1 C1 N2 C4 178.1(4) . . . . ? C17 C1 N2 C4 -1.0(8) . . . . ? N2 C2 N3 C3 -0.3(5) . . . . ? U1 C2 N3 C3 -172.6(4) . . . . ? N2 C2 N3 C5 -177.3(4) . . . . ? U1 C2 N3 C5 10.5(8) . . . . ? C4 C3 N3 C2 0.5(6) . . . . ? C4 C3 N3 C5 177.6(5) . . . . ? C10 C5 N3 C2 96.3(6) . . . . ? C6 C5 N3 C2 -85.7(6) . . . . ? C10 C5 N3 C3 -80.3(6) . . . . ? C6 C5 N3 C3 97.6(6) . . . . ? N5 C21 N4 C23 0.1(5) . . . . ? U1 C21 N4 C23 171.3(3) . . . . ? N5 C21 N4 C20 178.4(4) . . . . ? U1 C21 N4 C20 -10.5(6) . . . . ? C22 C23 N4 C21 -0.7(6) . . . . ? C22 C23 N4 C20 -178.9(5) . . . . ? N1 C20 N4 C21 9.7(7) . . . . ? C19 C20 N4 C21 -170.9(5) . . . . ? N1 C20 N4 C23 -172.3(4) . . . . ? C19 C20 N4 C23 7.2(8) . . . . ? N4 C21 N5 C22 0.5(5) . . . . ? U1 C21 N5 C22 -167.9(4) . . . . ? N4 C21 N5 C24 -176.7(4) . . . . ? U1 C21 N5 C24 14.9(8) . . . . ? C23 C22 N5 C21 -1.0(6) . . . . ? C23 C22 N5 C24 176.4(4) . . . . ? C25 C24 N5 C21 -84.7(6) . . . . ? C29 C24 N5 C21 96.0(6) . . . . ? C25 C24 N5 C22 98.4(6) . . . . ? C29 C24 N5 C22 -80.9(6) . . . . ? C37 C36 O1 C39 -24.4(7) . . . . ? C38 C39 O1 C36 1.5(7) . . . . ? N3 C2 U1 C21 -177.1(5) . . . . ? N2 C2 U1 C21 11.5(4) . . . . ? N3 C2 U1 Cl4 -23.1(5) . . . . ? N2 C2 U1 Cl4 165.5(4) . . . . ? N3 C2 U1 Cl3 45.3(6) . . . . ? N2 C2 U1 Cl3 -126.1(3) . . . . ? N3 C2 U1 Cl1 101.4(5) . . . . ? N2 C2 U1 Cl1 -70.1(3) . . . . ? N3 C2 U1 N1 179.4(6) . . . . ? N2 C2 U1 N1 8.0(3) . . . . ? N3 C2 U1 Cl2 -107.0(5) . . . . ? N2 C2 U1 Cl2 81.6(3) . . . . ? N5 C21 U1 C2 169.0(5) . . . . ? N4 C21 U1 C2 1.8(4) . . . . ? N5 C21 U1 Cl4 33.5(6) . . . . ? N4 C21 U1 Cl4 -133.7(3) . . . . ? N5 C21 U1 Cl3 -33.6(5) . . . . ? N4 C21 U1 Cl3 159.2(4) . . . . ? N5 C21 U1 Cl1 -116.7(5) . . . . ? N4 C21 U1 Cl1 76.0(4) . . . . ? N5 C21 U1 N1 172.5(6) . . . . ? N4 C21 U1 N1 5.3(3) . . . . ? N5 C21 U1 Cl2 96.0(5) . . . . ? N4 C21 U1 Cl2 -71.2(3) . . . . ? C20 N1 U1 C2 176.3(4) . . . . ? C1 N1 U1 C2 -7.9(3) . . . . ? C20 N1 U1 C21 -0.4(4) . . . . ? C1 N1 U1 C21 175.4(4) . . . . ? C20 N1 U1 Cl4 138.7(3) . . . . ? C1 N1 U1 Cl4 -45.4(4) . . . . ? C20 N1 U1 Cl3 -40.2(4) . . . . ? C1 N1 U1 Cl3 135.7(3) . . . . ? C20 N1 U1 Cl1 -100.4(4) . . . . ? C1 N1 U1 Cl1 75.5(4) . . . . ? C20 N1 U1 Cl2 84.5(4) . . . . ? C1 N1 U1 Cl2 -99.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.15 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.052 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.137 #==END data_6 _database_code_depnum_ccdc_archive 'CCDC 282404' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 Cl2 N5 O V' _chemical_formula_sum 'C35 H41 Cl2 N5 O V' _chemical_formula_weight 669.57 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' Cl Cl 0.1484 0.1585 '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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 16.699(5) _cell_length_b 19.125(5) _cell_length_c 22.226(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.012(4) _cell_angle_gamma 90.00 _cell_volume 7045(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2061 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 17.02 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.621243 _exptl_absorpt_correction_T_max 0.9861 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6868 _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 34114 _diffrn_reflns_av_R_equivalents 0.1383 _diffrn_reflns_av_sigmaI/netI 0.1286 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 20.08 _reflns_number_total 7369 _reflns_number_gt 4130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) ENCIFER (Allen, 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^)+(0.1074P)^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 7369 _refine_ls_number_parameters 809 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1342 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2073 _refine_ls_wR_factor_gt 0.1795 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5734(6) 0.1586(5) 0.2868(4) 0.052(2) Uani 1 1 d . . . C2 C 0.5008(5) 0.2059(5) 0.3654(4) 0.050(2) Uani 1 1 d . . . C3 C 0.4758(5) 0.2650(5) 0.4627(4) 0.055(3) Uani 1 1 d . . . C4 C 0.4651(5) 0.2195(5) 0.5106(4) 0.057(3) Uani 1 1 d . . . C5 C 0.4920(6) 0.1429(5) 0.5118(4) 0.061(3) Uani 1 1 d . . . H5 H 0.5062 0.1311 0.4706 0.073 Uiso 1 1 calc R . . C6 C 0.5662(6) 0.1302(5) 0.5566(5) 0.076(3) Uani 1 1 d . . . H6A H 0.6112 0.1579 0.5451 0.114 Uiso 1 1 calc R . . H6B H 0.5803 0.0804 0.5566 0.114 Uiso 1 1 calc R . . H6C H 0.5552 0.1439 0.5973 0.114 Uiso 1 1 calc R . . C7 C 0.4232(6) 0.0945(6) 0.5245(5) 0.078(3) Uani 1 1 d . . . H7A H 0.4414 0.0458 0.5242 0.116 Uiso 1 1 calc R . . H7B H 0.3772 0.1010 0.4931 0.116 Uiso 1 1 calc R . . H7C H 0.4068 0.1056 0.5642 0.116 Uiso 1 1 calc R . . C8 C 0.4316(6) 0.2481(6) 0.5594(5) 0.070(3) Uani 1 1 d . . . H8 H 0.4253 0.2196 0.5936 0.084 Uiso 1 1 calc R . . C9 C 0.4077(6) 0.3165(6) 0.5591(5) 0.066(3) Uani 1 1 d . . . H9 H 0.3859 0.3348 0.5934 0.079 Uiso 1 1 calc R . . C10 C 0.4143(6) 0.3589(6) 0.5109(5) 0.076(3) Uani 1 1 d . . . H10 H 0.3954 0.4058 0.5109 0.091 Uiso 1 1 calc R . . C11 C 0.4494(6) 0.3328(6) 0.4610(5) 0.063(3) Uani 1 1 d . . . C12 C 0.4570(6) 0.3815(6) 0.4072(5) 0.075(3) Uani 1 1 d . . . H12 H 0.4928 0.3573 0.3809 0.090 Uiso 1 1 calc R . . C13 C 0.4948(7) 0.4524(5) 0.4231(5) 0.079(3) Uani 1 1 d . . . H13A H 0.4594 0.4795 0.4463 0.119 Uiso 1 1 calc R . . H13B H 0.5022 0.4776 0.3858 0.119 Uiso 1 1 calc R . . H13C H 0.5473 0.4459 0.4474 0.119 Uiso 1 1 calc R . . C14 C 0.3737(7) 0.3893(6) 0.3692(5) 0.098(4) Uani 1 1 d . . . H14A H 0.3356 0.4101 0.3942 0.146 Uiso 1 1 calc R . . H14B H 0.3541 0.3431 0.3550 0.146 Uiso 1 1 calc R . . H14C H 0.3787 0.4195 0.3342 0.146 Uiso 1 1 calc R . . C15 C 0.6077(5) 0.2566(5) 0.4236(5) 0.061(3) Uani 1 1 d . . . H15 H 0.6374 0.2809 0.4563 0.073 Uiso 1 1 calc R . . C16 C 0.6360(6) 0.2293(5) 0.3746(5) 0.063(3) Uani 1 1 d . . . H16 H 0.6902 0.2308 0.3657 0.076 Uiso 1 1 calc R . . C17 C 0.6412(5) 0.1470(6) 0.2566(5) 0.068(3) Uani 1 1 d . . . H17 H 0.6921 0.1678 0.2697 0.082 Uiso 1 1 calc R . . C18 C 0.6295(6) 0.1036(6) 0.2067(5) 0.062(3) Uani 1 1 d . . . H18 H 0.6736 0.0942 0.1846 0.074 Uiso 1 1 calc R . . C19 C 0.5572(6) 0.0741(5) 0.1881(4) 0.065(3) Uani 1 1 d . . . H19 H 0.5502 0.0439 0.1540 0.078 Uiso 1 1 calc R . . C20 C 0.4932(6) 0.0894(5) 0.2207(5) 0.054(3) Uani 1 1 d . . . C21 C 0.3546(6) 0.0888(5) 0.2416(4) 0.057(3) Uani 1 1 d . . . C22 C 0.3060(6) 0.0111(5) 0.1690(4) 0.052(2) Uani 1 1 d . . . H22 H 0.2692 -0.0188 0.1452 0.062 Uiso 1 1 calc R . . C23 C 0.3849(6) 0.0179(5) 0.1632(4) 0.059(3) Uani 1 1 d . . . H23 H 0.4145 -0.0046 0.1349 0.070 Uiso 1 1 calc R . . C24 C 0.2060(5) 0.0706(5) 0.2279(4) 0.049(2) Uani 1 1 d . . . C25 C 0.1762(5) 0.0386(5) 0.2768(4) 0.052(2) Uani 1 1 d . . . C26 C 0.2263(6) -0.0089(5) 0.3233(4) 0.063(3) Uani 1 1 d . . . H26 H 0.2814 -0.0144 0.3107 0.075 Uiso 1 1 calc R . . C27 C 0.1868(6) -0.0825(5) 0.3244(5) 0.077(3) Uani 1 1 d . . . H27A H 0.1355 -0.0788 0.3414 0.116 Uiso 1 1 calc R . . H27B H 0.2231 -0.1141 0.3495 0.116 Uiso 1 1 calc R . . H27C H 0.1769 -0.1009 0.2830 0.116 Uiso 1 1 calc R . . C28 C 0.2344(6) 0.0233(5) 0.3862(4) 0.065(3) Uani 1 1 d . . . H28A H 0.2522 0.0720 0.3840 0.097 Uiso 1 1 calc R . . H28B H 0.2742 -0.0030 0.4133 0.097 Uiso 1 1 calc R . . H28C H 0.1821 0.0219 0.4020 0.097 Uiso 1 1 calc R . . C29 C 0.0958(6) 0.0505(5) 0.2842(5) 0.070(3) Uani 1 1 d . . . H29 H 0.0730 0.0295 0.3169 0.084 Uiso 1 1 calc R . . C30 C 0.0500(6) 0.0926(5) 0.2440(5) 0.067(3) Uani 1 1 d . . . H30 H -0.0049 0.1000 0.2494 0.080 Uiso 1 1 calc R . . C31 C 0.0797(6) 0.1245(5) 0.1967(5) 0.069(3) Uani 1 1 d . . . H31 H 0.0465 0.1544 0.1703 0.083 Uiso 1 1 calc R . . C32 C 0.1604(6) 0.1124(5) 0.1877(4) 0.054(2) Uani 1 1 d . . . C33 C 0.1924(5) 0.1471(5) 0.1329(4) 0.056(3) Uani 1 1 d . . . H33 H 0.2518 0.1382 0.1374 0.067 Uiso 1 1 calc R . . C34 C 0.1576(7) 0.1134(6) 0.0739(5) 0.092(4) Uani 1 1 d . . . H34A H 0.0991 0.1208 0.0676 0.138 Uiso 1 1 calc R . . H34B H 0.1691 0.0632 0.0755 0.138 Uiso 1 1 calc R . . H34C H 0.1821 0.1345 0.0403 0.138 Uiso 1 1 calc R . . C35 C 0.1819(6) 0.2248(5) 0.1331(5) 0.081(3) Uani 1 1 d . . . H35A H 0.1247 0.2361 0.1330 0.122 Uiso 1 1 calc R . . H35B H 0.2014 0.2447 0.0969 0.122 Uiso 1 1 calc R . . H35C H 0.2129 0.2445 0.1694 0.122 Uiso 1 1 calc R . . C36 C 1.0199(6) 0.3638(5) 0.2567(4) 0.053(2) Uani 1 1 d . . . C37 C 0.8802(6) 0.3677(5) 0.2646(4) 0.052(2) Uani 1 1 d . . . C38 C 0.8423(6) 0.4545(5) 0.1964(4) 0.059(3) Uani 1 1 d . . . H38 H 0.8090 0.4870 0.1726 0.070 Uiso 1 1 calc R . . C39 C 0.9207(7) 0.4462(5) 0.1979(4) 0.059(3) Uani 1 1 d . . . H39 H 0.9551 0.4711 0.1743 0.071 Uiso 1 1 calc R . . C40 C 0.7333(5) 0.3885(5) 0.2421(4) 0.056(3) Uani 1 1 d . . . C41 C 0.6944(5) 0.4144(5) 0.2895(4) 0.051(2) Uani 1 1 d . . . C42 C 0.7338(5) 0.4616(4) 0.3382(4) 0.051(2) Uani 1 1 d . . . H42 H 0.7912 0.4697 0.3312 0.062 Uiso 1 1 calc R . . C43 C 0.7324(6) 0.4269(5) 0.4012(4) 0.070(3) Uani 1 1 d . . . H43A H 0.6764 0.4211 0.4092 0.105 Uiso 1 1 calc R . . H43B H 0.7613 0.4565 0.4326 0.105 Uiso 1 1 calc R . . H43C H 0.7586 0.3810 0.4014 0.105 Uiso 1 1 calc R . . C44 C 0.6895(6) 0.5332(5) 0.3372(5) 0.075(3) Uani 1 1 d . . . H44A H 0.6917 0.5559 0.2979 0.113 Uiso 1 1 calc R . . H44B H 0.7158 0.5631 0.3696 0.113 Uiso 1 1 calc R . . H44C H 0.6331 0.5257 0.3435 0.113 Uiso 1 1 calc R . . C45 C 0.6117(6) 0.3940(6) 0.2885(5) 0.063(3) Uani 1 1 d . . . H45 H 0.5814 0.4112 0.3188 0.076 Uiso 1 1 calc R . . C46 C 0.5761(6) 0.3507(5) 0.2453(5) 0.061(3) Uani 1 1 d . . . H46 H 0.5213 0.3379 0.2463 0.073 Uiso 1 1 calc R . . C47 C 0.6157(6) 0.3251(5) 0.2011(5) 0.062(3) Uani 1 1 d . . . H47 H 0.5887 0.2945 0.1716 0.074 Uiso 1 1 calc R . . C48 C 0.6966(6) 0.3430(5) 0.1979(5) 0.063(3) Uani 1 1 d . . . C49 C 0.7415(6) 0.3147(5) 0.1452(4) 0.062(3) Uani 1 1 d . . . H49 H 0.8007 0.3209 0.1574 0.075 Uiso 1 1 calc R . . C50 C 0.7189(6) 0.3561(5) 0.0876(4) 0.072(3) Uani 1 1 d . . . H50A H 0.7447 0.3353 0.0546 0.108 Uiso 1 1 calc R . . H50B H 0.7371 0.4046 0.0939 0.108 Uiso 1 1 calc R . . H50C H 0.6602 0.3554 0.0771 0.108 Uiso 1 1 calc R . . C51 C 0.7257(6) 0.2367(5) 0.1342(5) 0.072(3) Uani 1 1 d . . . H51A H 0.6681 0.2292 0.1213 0.108 Uiso 1 1 calc R . . H51B H 0.7419 0.2108 0.1717 0.108 Uiso 1 1 calc R . . H51C H 0.7570 0.2202 0.1024 0.108 Uiso 1 1 calc R . . C52 C 1.0918(6) 0.3807(5) 0.2329(4) 0.057(3) Uani 1 1 d . . . H52 H 1.0932 0.4154 0.2025 0.069 Uiso 1 1 calc R . . C53 C 1.1589(6) 0.3451(5) 0.2555(4) 0.060(3) Uani 1 1 d . . . H53 H 1.2086 0.3565 0.2412 0.073 Uiso 1 1 calc R . . C54 C 1.1584(5) 0.2923(5) 0.2990(4) 0.061(3) Uani 1 1 d . . . H54 H 1.2051 0.2663 0.3138 0.073 Uiso 1 1 calc R . . C55 C 1.0832(6) 0.2812(5) 0.3189(4) 0.055(3) Uani 1 1 d . . . C56 C 0.9903(6) 0.2294(5) 0.3810(5) 0.061(3) Uani 1 1 d . . . C57 C 1.0774(6) 0.1587(5) 0.4404(4) 0.057(3) Uani 1 1 d . . . H57 H 1.0964 0.1254 0.4705 0.068 Uiso 1 1 calc R . . C58 C 1.1213(6) 0.1910(5) 0.4030(5) 0.063(3) Uani 1 1 d . . . H58 H 1.1776 0.1855 0.4016 0.075 Uiso 1 1 calc R . . C59 C 0.9319(6) 0.1565(6) 0.4528(4) 0.060(3) Uani 1 1 d . . . C60 C 0.9009(6) 0.0926(6) 0.4327(5) 0.064(3) Uani 1 1 d . . . C61 C 0.9373(6) 0.0489(6) 0.3861(5) 0.070(3) Uani 1 1 d . . . H61 H 0.9792 0.0782 0.3697 0.084 Uiso 1 1 calc R . . C62 C 0.9797(6) -0.0170(6) 0.4138(5) 0.084(4) Uani 1 1 d . . . H62A H 1.0296 -0.0036 0.4391 0.126 Uiso 1 1 calc R . . H62B H 0.9926 -0.0481 0.3813 0.126 Uiso 1 1 calc R . . H62C H 0.9440 -0.0413 0.4388 0.126 Uiso 1 1 calc R . . C63 C 0.8758(7) 0.0279(6) 0.3327(5) 0.080(3) Uani 1 1 d . . . H63A H 0.8382 -0.0064 0.3461 0.120 Uiso 1 1 calc R . . H63B H 0.9039 0.0073 0.3007 0.120 Uiso 1 1 calc R . . H63C H 0.8459 0.0694 0.3168 0.120 Uiso 1 1 calc R . . C64 C 0.8311(7) 0.0666(6) 0.4565(5) 0.080(3) Uani 1 1 d . . . H64 H 0.8088 0.0226 0.4436 0.095 Uiso 1 1 calc R . . C65 C 0.7960(7) 0.1063(6) 0.4989(5) 0.074(3) Uani 1 1 d . . . H65 H 0.7496 0.0888 0.5148 0.089 Uiso 1 1 calc R . . C66 C 0.8267(7) 0.1699(7) 0.5182(5) 0.080(3) Uani 1 1 d . . . H66 H 0.8016 0.1957 0.5472 0.096 Uiso 1 1 calc R . . C67 C 0.8936(6) 0.1969(6) 0.4960(4) 0.064(3) Uani 1 1 d . . . C68 C 0.9295(7) 0.2660(6) 0.5183(5) 0.074(3) Uani 1 1 d . . . H68 H 0.9626 0.2845 0.4873 0.089 Uiso 1 1 calc R . . C69 C 0.8640(7) 0.3207(6) 0.5277(6) 0.100(4) Uani 1 1 d . . . H69A H 0.8245 0.3229 0.4913 0.150 Uiso 1 1 calc R . . H69B H 0.8891 0.3667 0.5352 0.150 Uiso 1 1 calc R . . H69C H 0.8367 0.3072 0.5625 0.150 Uiso 1 1 calc R . . C70 C 0.9859(7) 0.2530(6) 0.5774(5) 0.093(4) Uani 1 1 d . . . H70A H 0.9550 0.2327 0.6079 0.140 Uiso 1 1 calc R . . H70B H 1.0098 0.2974 0.5925 0.140 Uiso 1 1 calc R . . H70C H 1.0289 0.2206 0.5695 0.140 Uiso 1 1 calc R . . Cl1 Cl 0.37920(12) 0.25193(11) 0.24580(10) 0.0514(6) Uani 1 1 d . . . Cl2 Cl 0.43826(13) 0.05075(11) 0.36927(9) 0.0463(6) Uani 1 1 d . . . Cl3 Cl 0.88259(13) 0.20641(12) 0.25469(10) 0.0534(6) Uani 1 1 d . . . Cl4 Cl 0.94550(14) 0.39410(12) 0.39471(10) 0.0553(7) Uani 1 1 d . . . N1 N 0.5007(4) 0.1314(4) 0.2675(3) 0.0480(19) Uani 1 1 d . . . N2 N 0.5716(4) 0.1988(4) 0.3400(4) 0.052(2) Uani 1 1 d . . . N3 N 0.5245(4) 0.2415(4) 0.4163(4) 0.053(2) Uani 1 1 d . . . N4 N 0.4138(5) 0.0659(4) 0.2088(3) 0.052(2) Uani 1 1 d . . . N5 N 0.2869(5) 0.0551(4) 0.2157(3) 0.055(2) Uani 1 1 d . . . N6 N 1.0175(5) 0.3150(4) 0.2979(3) 0.0496(19) Uani 1 1 d . . . N7 N 0.9440(4) 0.3945(4) 0.2399(3) 0.053(2) Uani 1 1 d . . . N8 N 0.8177(5) 0.4048(4) 0.2381(3) 0.051(2) Uani 1 1 d . . . N9 N 1.0691(4) 0.2345(4) 0.3661(3) 0.053(2) Uani 1 1 d . . . N10 N 0.9981(4) 0.1824(4) 0.4275(3) 0.055(2) Uani 1 1 d . . . O1 O 0.3196(3) 0.1772(3) 0.3539(3) 0.0575(17) Uani 1 1 d . . . O2 O 0.8182(3) 0.2760(3) 0.3639(3) 0.0643(18) Uani 1 1 d . . . V1 V 0.39373(9) 0.15788(8) 0.31765(7) 0.0510(5) Uani 1 1 d . . . V2 V 0.89899(9) 0.29130(9) 0.33402(7) 0.0555(5) 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 0.051(7) 0.045(6) 0.062(7) 0.017(5) 0.011(6) 0.005(5) C2 0.043(6) 0.065(7) 0.044(6) 0.016(5) 0.018(5) 0.004(5) C3 0.040(6) 0.066(7) 0.058(7) 0.009(6) 0.004(5) -0.001(5) C4 0.053(6) 0.070(7) 0.048(6) 0.006(6) 0.009(5) 0.000(5) C5 0.062(7) 0.071(8) 0.051(6) 0.002(5) 0.012(5) -0.004(6) C6 0.088(8) 0.060(7) 0.079(8) -0.006(6) 0.004(7) 0.004(6) C7 0.091(8) 0.083(8) 0.061(7) 0.010(6) 0.018(6) -0.001(7) C8 0.055(6) 0.091(9) 0.066(8) 0.004(6) 0.014(6) -0.004(6) C9 0.078(7) 0.066(8) 0.057(7) -0.002(6) 0.014(6) 0.022(6) C10 0.071(7) 0.081(8) 0.077(8) 0.016(7) 0.015(6) 0.028(6) C11 0.051(6) 0.072(8) 0.069(7) 0.003(6) 0.023(6) -0.004(6) C12 0.078(8) 0.075(8) 0.074(8) 0.011(6) 0.021(7) 0.018(6) C13 0.095(8) 0.059(7) 0.091(8) 0.016(6) 0.037(7) 0.003(6) C14 0.095(9) 0.105(10) 0.093(9) 0.008(8) 0.014(8) 0.016(8) C15 0.044(7) 0.055(7) 0.082(8) 0.009(6) 0.001(6) -0.007(5) C16 0.054(7) 0.077(8) 0.063(7) 0.011(6) 0.029(6) 0.007(6) C17 0.036(6) 0.084(8) 0.090(9) 0.026(7) 0.025(6) 0.006(5) C18 0.047(7) 0.079(8) 0.063(7) -0.001(6) 0.023(6) 0.003(6) C19 0.060(7) 0.090(8) 0.049(6) 0.018(6) 0.023(6) 0.006(6) C20 0.045(7) 0.061(7) 0.054(7) 0.018(6) 0.004(6) 0.006(5) C21 0.070(7) 0.058(7) 0.048(6) 0.023(5) 0.027(6) 0.021(6) C22 0.071(7) 0.055(6) 0.031(5) -0.001(5) 0.016(5) 0.004(5) C23 0.068(7) 0.068(7) 0.046(6) 0.003(6) 0.029(6) 0.008(6) C24 0.048(6) 0.052(6) 0.050(6) 0.005(5) 0.020(5) 0.003(5) C25 0.050(6) 0.056(6) 0.055(6) 0.003(5) 0.024(5) -0.004(5) C26 0.070(7) 0.055(7) 0.071(7) 0.004(6) 0.041(6) -0.001(6) C27 0.076(7) 0.072(8) 0.088(8) 0.002(6) 0.026(6) 0.019(6) C28 0.082(7) 0.068(7) 0.047(6) 0.007(5) 0.021(5) -0.014(6) C29 0.070(8) 0.072(8) 0.075(8) 0.019(6) 0.032(6) -0.006(6) C30 0.057(6) 0.073(8) 0.075(8) 0.005(6) 0.028(6) 0.011(6) C31 0.054(7) 0.077(8) 0.079(8) 0.008(6) 0.020(6) 0.002(6) C32 0.059(7) 0.053(6) 0.049(6) 0.013(5) 0.005(5) 0.001(5) C33 0.040(5) 0.079(8) 0.049(6) 0.001(5) 0.005(5) -0.006(5) C34 0.087(8) 0.122(10) 0.067(8) 0.015(7) 0.008(7) -0.025(8) C35 0.083(8) 0.067(8) 0.100(9) 0.021(6) 0.033(7) 0.005(6) C36 0.058(7) 0.062(7) 0.040(6) -0.006(5) 0.010(5) -0.008(6) C37 0.046(6) 0.065(7) 0.044(6) -0.009(5) 0.005(5) -0.007(6) C38 0.058(7) 0.054(7) 0.067(7) -0.003(5) 0.021(6) 0.003(5) C39 0.072(8) 0.050(7) 0.059(7) -0.005(6) 0.017(6) -0.003(6) C40 0.049(6) 0.070(7) 0.051(6) 0.006(6) 0.014(5) -0.003(5) C41 0.063(7) 0.053(6) 0.040(6) 0.002(5) 0.017(5) 0.000(5) C42 0.053(6) 0.043(6) 0.058(6) -0.001(5) 0.006(5) -0.002(5) C43 0.084(8) 0.071(7) 0.059(7) 0.009(6) 0.022(6) -0.004(6) C44 0.077(7) 0.083(8) 0.071(7) 0.000(6) 0.031(6) -0.003(6) C45 0.045(6) 0.075(8) 0.076(8) 0.029(7) 0.034(6) 0.004(6) C46 0.049(6) 0.064(7) 0.072(7) -0.003(6) 0.014(6) -0.007(6) C47 0.055(7) 0.071(7) 0.059(7) -0.005(5) 0.006(6) -0.004(6) C48 0.062(7) 0.064(7) 0.064(7) 0.010(6) 0.007(6) -0.006(6) C49 0.060(6) 0.073(8) 0.057(7) -0.008(6) 0.019(5) 0.005(6) C50 0.072(7) 0.079(8) 0.066(7) -0.005(6) 0.008(6) -0.010(6) C51 0.078(7) 0.070(8) 0.066(7) -0.011(6) 0.003(6) 0.007(6) C52 0.044(6) 0.064(7) 0.064(7) -0.005(5) 0.007(6) -0.004(5) C53 0.070(8) 0.066(7) 0.048(6) 0.007(6) 0.019(6) -0.014(6) C54 0.039(6) 0.082(8) 0.064(7) -0.023(6) 0.021(5) -0.014(5) C55 0.068(7) 0.051(6) 0.048(6) -0.011(5) 0.009(6) -0.007(6) C56 0.057(7) 0.059(7) 0.074(8) -0.001(6) 0.036(6) -0.008(5) C57 0.053(7) 0.072(7) 0.045(6) -0.006(5) 0.004(5) 0.005(6) C58 0.049(6) 0.079(8) 0.061(7) -0.008(6) 0.008(6) 0.002(6) C59 0.067(7) 0.066(8) 0.047(6) 0.008(6) 0.008(6) 0.006(6) C60 0.053(6) 0.073(8) 0.072(7) 0.027(6) 0.035(6) 0.006(6) C61 0.063(7) 0.089(8) 0.060(7) 0.006(6) 0.016(6) -0.006(6) C62 0.065(7) 0.101(9) 0.094(9) -0.003(7) 0.040(7) -0.003(7) C63 0.098(9) 0.078(8) 0.067(8) 0.008(6) 0.028(7) -0.012(7) C64 0.095(9) 0.069(8) 0.079(8) 0.003(6) 0.027(7) 0.003(7) C65 0.084(8) 0.069(8) 0.079(8) 0.025(7) 0.047(7) 0.000(7) C66 0.094(9) 0.096(10) 0.058(7) 0.027(7) 0.043(7) 0.018(8) C67 0.068(7) 0.076(8) 0.052(6) 0.016(6) 0.024(6) 0.011(6) C68 0.085(8) 0.081(9) 0.057(7) 0.005(6) 0.011(6) 0.009(7) C69 0.083(8) 0.119(10) 0.103(9) 0.005(8) 0.034(7) 0.041(8) C70 0.097(9) 0.100(10) 0.078(9) 0.000(7) -0.005(7) 0.021(7) Cl1 0.0379(12) 0.0496(14) 0.0674(16) 0.0189(12) 0.0086(11) 0.0003(11) Cl2 0.0541(14) 0.0456(13) 0.0426(13) 0.0010(11) 0.0192(11) 0.0093(11) Cl3 0.0565(14) 0.0500(15) 0.0531(14) -0.0034(12) 0.0039(12) 0.0014(12) Cl4 0.0597(15) 0.0628(16) 0.0459(14) 0.0039(12) 0.0160(12) 0.0042(13) N1 0.048(5) 0.050(5) 0.045(5) 0.006(4) 0.004(4) -0.010(4) N2 0.030(4) 0.059(5) 0.067(6) 0.004(5) 0.010(5) -0.007(4) N3 0.047(5) 0.064(5) 0.052(5) 0.005(4) 0.017(4) 0.009(4) N4 0.053(6) 0.071(6) 0.034(5) 0.007(4) 0.013(4) 0.009(4) N5 0.041(5) 0.071(6) 0.052(5) 0.001(4) 0.004(4) 0.001(4) N6 0.052(5) 0.056(5) 0.043(5) -0.009(4) 0.012(4) 0.001(4) N7 0.037(5) 0.070(6) 0.056(5) -0.002(5) 0.017(4) -0.002(5) N8 0.055(5) 0.056(5) 0.045(5) -0.002(4) 0.019(4) -0.012(5) N9 0.043(5) 0.062(6) 0.055(5) -0.008(5) 0.008(4) 0.000(4) N10 0.046(5) 0.067(6) 0.054(5) 0.003(4) 0.020(4) 0.005(4) O1 0.045(4) 0.062(4) 0.069(4) 0.002(3) 0.022(3) 0.005(3) O2 0.052(4) 0.075(5) 0.070(4) 0.006(4) 0.025(3) 0.008(3) V1 0.0454(9) 0.0576(11) 0.0526(10) 0.0063(8) 0.0169(8) 0.0042(8) V2 0.0474(10) 0.0711(12) 0.0503(10) -0.0006(9) 0.0152(8) -0.0013(9) _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 N1 1.342(11) . ? C1 C17 1.402(12) . ? C1 N2 1.414(11) . ? C2 N3 1.337(11) . ? C2 N2 1.378(10) . ? C2 V1 2.169(10) . ? C3 C11 1.369(13) . ? C3 C4 1.404(12) . ? C3 N3 1.459(12) . ? C4 C8 1.392(13) . ? C4 C5 1.532(13) . ? C5 C6 1.511(13) . ? C5 C7 1.528(12) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.368(13) . ? C8 H8 0.9500 . ? C9 C10 1.360(13) . ? C9 H9 0.9500 . ? C10 C11 1.407(13) . ? C10 H10 0.9500 . ? C11 C12 1.533(14) . ? C12 C13 1.519(14) . ? C12 C14 1.543(14) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.345(13) . ? C15 N3 1.409(11) . ? C15 H15 0.9500 . ? C16 N2 1.374(12) . ? C16 H16 0.9500 . ? C17 C18 1.381(13) . ? C17 H17 0.9500 . ? C18 C19 1.351(12) . ? C18 H18 0.9500 . ? C19 C20 1.393(12) . ? C19 H19 0.9500 . ? C20 N1 1.307(11) . ? C20 N4 1.395(11) . ? C21 N4 1.371(10) . ? C21 N5 1.366(11) . ? C21 V1 2.182(11) . ? C22 C23 1.346(12) . ? C22 N5 1.403(11) . ? C22 H22 0.9500 . ? C23 N4 1.407(11) . ? C23 H23 0.9500 . ? C24 C32 1.361(12) . ? C24 C25 1.393(12) . ? C24 N5 1.441(10) . ? C25 C29 1.390(12) . ? C25 C26 1.543(13) . ? C26 C28 1.520(12) . ? C26 C27 1.555(13) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.365(13) . ? C29 H29 0.9500 . ? C30 C31 1.360(13) . ? C30 H30 0.9500 . ? C31 C32 1.405(12) . ? C31 H31 0.9500 . ? C32 C33 1.539(12) . ? C33 C35 1.497(13) . ? C33 C34 1.512(13) . ? 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 N6 1.312(11) . ? C36 N7 1.406(11) . ? C36 C52 1.407(12) . ? C37 N8 1.338(11) . ? C37 N7 1.357(10) . ? C37 V2 2.120(10) . ? C38 C39 1.316(12) . ? C38 N8 1.423(11) . ? C38 H38 0.9500 . ? C39 N7 1.382(11) . ? C39 H39 0.9500 . ? C40 C41 1.395(12) . ? C40 C48 1.397(13) . ? C40 N8 1.456(11) . ? C41 C45 1.433(12) . ? C41 C42 1.498(12) . ? C42 C43 1.553(12) . ? C42 C44 1.554(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 C46 1.350(13) . ? C45 H45 0.9500 . ? C46 C47 1.343(12) . ? C46 H46 0.9500 . ? C47 C48 1.402(12) . ? C47 H47 0.9500 . ? C48 C49 1.564(13) . ? C49 C50 1.513(13) . ? C49 C51 1.528(13) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.355(12) . ? C52 H52 0.9500 . ? C53 C54 1.399(13) . ? C53 H53 0.9500 . ? C54 C55 1.397(12) . ? C54 H54 0.9500 . ? C55 N6 1.309(11) . ? C55 N9 1.419(11) . ? C56 N10 1.365(11) . ? C56 N9 1.398(10) . ? C56 V2 2.104(11) . ? C57 C58 1.326(12) . ? C57 N10 1.395(11) . ? C57 H57 0.9500 . ? C58 N9 1.396(11) . ? C58 H58 0.9500 . ? C59 C60 1.380(13) . ? C59 N10 1.392(12) . ? C59 C67 1.441(13) . ? C60 C64 1.426(13) . ? C60 C61 1.515(14) . ? C61 C63 1.525(13) . ? C61 C62 1.538(14) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.394(14) . ? C64 H64 0.9500 . ? C65 C66 1.369(14) . ? C65 H65 0.9500 . ? C66 C67 1.374(13) . ? C66 H66 0.9500 . ? C67 C68 1.510(14) . ? C68 C70 1.540(14) . ? C68 C69 1.546(13) . ? 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 . ? Cl1 V1 2.398(3) . ? Cl2 V1 2.421(3) . ? Cl3 V2 2.388(3) . ? Cl4 V2 2.456(3) . ? N1 V1 2.275(7) . ? N6 V2 2.270(7) . ? O1 V1 1.600(5) . ? O2 V2 1.602(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C17 122.6(10) . . ? N1 C1 N2 111.5(8) . . ? C17 C1 N2 125.9(10) . . ? N3 C2 N2 102.6(8) . . ? N3 C2 V1 140.4(6) . . ? N2 C2 V1 117.0(7) . . ? C11 C3 C4 122.5(9) . . ? C11 C3 N3 118.6(8) . . ? C4 C3 N3 118.5(9) . . ? C8 C4 C3 116.7(10) . . ? C8 C4 C5 120.4(9) . . ? C3 C4 C5 122.8(9) . . ? C6 C5 C7 110.8(8) . . ? C6 C5 C4 112.4(8) . . ? C7 C5 C4 110.9(8) . . ? C6 C5 H5 107.5 . . ? C7 C5 H5 107.5 . . ? C4 C5 H5 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C4 121.1(10) . . ? C9 C8 H8 119.5 . . ? C4 C8 H8 119.5 . . ? C10 C9 C8 121.6(10) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 119.4(10) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C3 C11 C10 118.6(9) . . ? C3 C11 C12 122.7(9) . . ? C10 C11 C12 118.7(10) . . ? C13 C12 C11 115.6(9) . . ? C13 C12 C14 111.3(9) . . ? C11 C12 C14 109.3(9) . . ? C13 C12 H12 106.7 . . ? C11 C12 H12 106.7 . . ? C14 C12 H12 106.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N3 105.5(9) . . ? C16 C15 H15 127.3 . . ? N3 C15 H15 127.3 . . ? C15 C16 N2 106.8(8) . . ? C15 C16 H16 126.6 . . ? N2 C16 H16 126.6 . . ? C18 C17 C1 115.8(9) . . ? C18 C17 H17 122.1 . . ? C1 C17 H17 122.1 . . ? C19 C18 C17 122.0(9) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 117.9(10) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? N1 C20 N4 110.3(8) . . ? N1 C20 C19 122.5(9) . . ? N4 C20 C19 127.2(10) . . ? N4 C21 N5 103.7(8) . . ? N4 C21 V1 116.0(7) . . ? N5 C21 V1 140.1(7) . . ? C23 C22 N5 109.0(9) . . ? C23 C22 H22 125.5 . . ? N5 C22 H22 125.5 . . ? C22 C23 N4 104.4(8) . . ? C22 C23 H23 127.8 . . ? N4 C23 H23 127.8 . . ? C32 C24 C25 123.2(8) . . ? C32 C24 N5 117.4(8) . . ? C25 C24 N5 119.3(8) . . ? C29 C25 C24 117.5(9) . . ? C29 C25 C26 118.0(8) . . ? C24 C25 C26 124.5(8) . . ? C28 C26 C25 110.9(8) . . ? C28 C26 C27 110.1(8) . . ? C25 C26 C27 110.3(8) . . ? C28 C26 H26 108.5 . . ? C25 C26 H26 108.5 . . ? C27 C26 H26 108.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C25 119.5(9) . . ? C30 C29 H29 120.3 . . ? C25 C29 H29 120.3 . . ? C31 C30 C29 122.8(9) . . ? C31 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C30 C31 C32 118.9(10) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C24 C32 C31 118.2(8) . . ? C24 C32 C33 123.5(8) . . ? C31 C32 C33 118.3(9) . . ? C35 C33 C34 113.1(9) . . ? C35 C33 C32 112.0(8) . . ? C34 C33 C32 111.6(8) . . ? C35 C33 H33 106.5 . . ? C34 C33 H33 106.5 . . ? C32 C33 H33 106.5 . . ? 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 . . ? N6 C36 N7 112.3(8) . . ? N6 C36 C52 121.7(9) . . ? N7 C36 C52 126.0(9) . . ? N8 C37 N7 103.3(8) . . ? N8 C37 V2 136.4(7) . . ? N7 C37 V2 120.1(7) . . ? C39 C38 N8 105.6(9) . . ? C39 C38 H38 127.2 . . ? N8 C38 H38 127.2 . . ? C38 C39 N7 107.4(9) . . ? C38 C39 H39 126.3 . . ? N7 C39 H39 126.3 . . ? C41 C40 C48 123.2(9) . . ? C41 C40 N8 120.9(9) . . ? C48 C40 N8 115.8(8) . . ? C40 C41 C45 115.3(9) . . ? C40 C41 C42 123.8(8) . . ? C45 C41 C42 120.9(9) . . ? C41 C42 C43 109.8(7) . . ? C41 C42 C44 110.7(8) . . ? C43 C42 C44 109.3(8) . . ? C41 C42 H42 109.0 . . ? C43 C42 H42 109.0 . . ? C44 C42 H42 109.0 . . ? 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 . . ? C46 C45 C41 121.2(9) . . ? C46 C45 H45 119.4 . . ? C41 C45 H45 119.4 . . ? C47 C46 C45 122.1(9) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C46 C47 C48 120.7(10) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C40 C48 C47 117.4(9) . . ? C40 C48 C49 122.2(9) . . ? C47 C48 C49 120.4(10) . . ? C50 C49 C51 110.8(8) . . ? C50 C49 C48 111.1(8) . . ? C51 C49 C48 111.6(8) . . ? C50 C49 H49 107.7 . . ? C51 C49 H49 107.7 . . ? C48 C49 H49 107.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C36 116.8(9) . . ? C53 C52 H52 121.6 . . ? C36 C52 H52 121.6 . . ? C52 C53 C54 123.0(9) . . ? C52 C53 H53 118.5 . . ? C54 C53 H53 118.5 . . ? C55 C54 C53 114.2(10) . . ? C55 C54 H54 122.9 . . ? C53 C54 H54 122.9 . . ? N6 C55 C54 123.9(9) . . ? N6 C55 N9 111.6(8) . . ? C54 C55 N9 124.4(10) . . ? N10 C56 N9 102.7(8) . . ? N10 C56 V2 137.9(6) . . ? N9 C56 V2 119.4(7) . . ? C58 C57 N10 107.7(9) . . ? C58 C57 H57 126.2 . . ? N10 C57 H57 126.2 . . ? C57 C58 N9 107.0(8) . . ? C57 C58 H58 126.5 . . ? N9 C58 H58 126.5 . . ? C60 C59 N10 118.0(9) . . ? C60 C59 C67 120.7(9) . . ? N10 C59 C67 121.2(10) . . ? C59 C60 C64 118.7(10) . . ? C59 C60 C61 123.0(8) . . ? C64 C60 C61 118.4(10) . . ? C60 C61 C63 113.0(9) . . ? C60 C61 C62 112.4(8) . . ? C63 C61 C62 109.3(9) . . ? C60 C61 H61 107.3 . . ? C63 C61 H61 107.3 . . ? C62 C61 H61 107.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C60 119.4(11) . . ? C65 C64 H64 120.3 . . ? C60 C64 H64 120.3 . . ? C66 C65 C64 121.5(10) . . ? C66 C65 H65 119.3 . . ? C64 C65 H65 119.3 . . ? C65 C66 C67 120.8(10) . . ? C65 C66 H66 119.6 . . ? C67 C66 H66 119.6 . . ? C66 C67 C59 118.9(11) . . ? C66 C67 C68 121.3(10) . . ? C59 C67 C68 119.8(9) . . ? C67 C68 C70 108.4(9) . . ? C67 C68 C69 112.1(9) . . ? C70 C68 C69 111.3(9) . . ? C67 C68 H68 108.3 . . ? C70 C68 H68 108.3 . . ? C69 C68 H68 108.3 . . ? 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 . . ? C20 N1 C1 119.1(8) . . ? C20 N1 V1 121.4(6) . . ? C1 N1 V1 119.4(6) . . ? C16 N2 C2 112.3(8) . . ? C16 N2 C1 127.2(8) . . ? C2 N2 C1 120.3(8) . . ? C2 N3 C15 112.8(8) . . ? C2 N3 C3 128.4(8) . . ? C15 N3 C3 118.8(8) . . ? C21 N4 C20 121.7(9) . . ? C21 N4 C23 112.7(8) . . ? C20 N4 C23 125.6(8) . . ? C21 N5 C22 110.1(7) . . ? C21 N5 C24 124.7(8) . . ? C22 N5 C24 124.5(8) . . ? C55 N6 C36 120.3(8) . . ? C55 N6 V2 120.2(6) . . ? C36 N6 V2 119.4(7) . . ? C37 N7 C39 112.0(8) . . ? C37 N7 C36 117.5(9) . . ? C39 N7 C36 130.4(8) . . ? C37 N8 C38 111.7(7) . . ? C37 N8 C40 124.6(8) . . ? C38 N8 C40 122.8(8) . . ? C56 N9 C58 111.0(8) . . ? C56 N9 C55 117.6(9) . . ? C58 N9 C55 131.4(8) . . ? C56 N10 C59 122.3(8) . . ? C56 N10 C57 111.7(8) . . ? C59 N10 C57 125.6(8) . . ? O1 V1 C2 107.3(3) . . ? O1 V1 C21 110.6(3) . . ? C2 V1 C21 141.9(4) . . ? O1 V1 N1 178.9(3) . . ? C2 V1 N1 71.6(3) . . ? C21 V1 N1 70.4(3) . . ? O1 V1 Cl1 98.1(2) . . ? C2 V1 Cl1 91.1(2) . . ? C21 V1 Cl1 86.7(2) . . ? N1 V1 Cl1 82.10(18) . . ? O1 V1 Cl2 99.7(2) . . ? C2 V1 Cl2 86.5(2) . . ? C21 V1 Cl2 84.3(2) . . ? N1 V1 Cl2 80.18(18) . . ? Cl1 V1 Cl2 161.97(10) . . ? O2 V2 C56 106.7(3) . . ? O2 V2 C37 111.7(3) . . ? C56 V2 C37 141.5(4) . . ? O2 V2 N6 176.2(3) . . ? C56 V2 N6 71.2(3) . . ? C37 V2 N6 70.3(3) . . ? O2 V2 Cl3 99.0(2) . . ? C56 V2 Cl3 89.7(3) . . ? C37 V2 Cl3 86.4(2) . . ? N6 V2 Cl3 84.32(18) . . ? O2 V2 Cl4 98.3(2) . . ? C56 V2 Cl4 90.9(3) . . ? C37 V2 Cl4 81.8(2) . . ? N6 V2 Cl4 78.66(18) . . ? Cl3 V2 Cl4 161.78(10) . . ? 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 C11 C3 C4 C8 -4.9(14) . . . . ? N3 C3 C4 C8 168.2(8) . . . . ? C11 C3 C4 C5 178.0(9) . . . . ? N3 C3 C4 C5 -8.9(13) . . . . ? C8 C4 C5 C6 -70.3(11) . . . . ? C3 C4 C5 C6 106.7(10) . . . . ? C8 C4 C5 C7 54.4(12) . . . . ? C3 C4 C5 C7 -128.6(9) . . . . ? C3 C4 C8 C9 2.5(14) . . . . ? C5 C4 C8 C9 179.7(9) . . . . ? C4 C8 C9 C10 1.1(16) . . . . ? C8 C9 C10 C11 -2.4(16) . . . . ? C4 C3 C11 C10 3.7(14) . . . . ? N3 C3 C11 C10 -169.5(8) . . . . ? C4 C3 C11 C12 -176.7(9) . . . . ? N3 C3 C11 C12 10.1(14) . . . . ? C9 C10 C11 C3 0.1(15) . . . . ? C9 C10 C11 C12 -179.5(9) . . . . ? C3 C11 C12 C13 -129.5(10) . . . . ? C10 C11 C12 C13 50.1(13) . . . . ? C3 C11 C12 C14 104.0(11) . . . . ? C10 C11 C12 C14 -76.4(12) . . . . ? N3 C15 C16 N2 -0.4(10) . . . . ? N1 C1 C17 C18 -2.1(13) . . . . ? N2 C1 C17 C18 177.5(8) . . . . ? C1 C17 C18 C19 -0.1(14) . . . . ? C17 C18 C19 C20 0.8(15) . . . . ? C18 C19 C20 N1 0.7(14) . . . . ? C18 C19 C20 N4 178.7(9) . . . . ? N5 C22 C23 N4 1.5(10) . . . . ? C32 C24 C25 C29 0.0(14) . . . . ? N5 C24 C25 C29 -174.9(8) . . . . ? C32 C24 C25 C26 -179.8(9) . . . . ? N5 C24 C25 C26 5.2(13) . . . . ? C29 C25 C26 C28 -63.8(11) . . . . ? C24 C25 C26 C28 116.0(10) . . . . ? C29 C25 C26 C27 58.4(11) . . . . ? C24 C25 C26 C27 -121.7(9) . . . . ? C24 C25 C29 C30 -0.3(14) . . . . ? C26 C25 C29 C30 179.6(9) . . . . ? C25 C29 C30 C31 -0.6(16) . . . . ? C29 C30 C31 C32 1.6(16) . . . . ? C25 C24 C32 C31 1.0(14) . . . . ? N5 C24 C32 C31 176.1(8) . . . . ? C25 C24 C32 C33 -179.1(8) . . . . ? N5 C24 C32 C33 -4.0(13) . . . . ? C30 C31 C32 C24 -1.8(14) . . . . ? C30 C31 C32 C33 178.3(9) . . . . ? C24 C32 C33 C35 -123.9(10) . . . . ? C31 C32 C33 C35 56.0(12) . . . . ? C24 C32 C33 C34 108.1(11) . . . . ? C31 C32 C33 C34 -71.9(12) . . . . ? N8 C38 C39 N7 -1.4(10) . . . . ? C48 C40 C41 C45 -3.0(13) . . . . ? N8 C40 C41 C45 -179.4(8) . . . . ? C48 C40 C41 C42 178.2(9) . . . . ? N8 C40 C41 C42 1.8(13) . . . . ? C40 C41 C42 C43 -120.8(9) . . . . ? C45 C41 C42 C43 60.5(11) . . . . ? C40 C41 C42 C44 118.4(10) . . . . ? C45 C41 C42 C44 -60.3(11) . . . . ? C40 C41 C45 C46 2.1(13) . . . . ? C42 C41 C45 C46 -179.1(9) . . . . ? C41 C45 C46 C47 -0.5(15) . . . . ? C45 C46 C47 C48 -0.3(15) . . . . ? C41 C40 C48 C47 2.3(14) . . . . ? N8 C40 C48 C47 178.9(8) . . . . ? C41 C40 C48 C49 179.9(8) . . . . ? N8 C40 C48 C49 -3.5(13) . . . . ? C46 C47 C48 C40 -0.5(14) . . . . ? C46 C47 C48 C49 -178.2(9) . . . . ? C40 C48 C49 C50 -98.7(11) . . . . ? C47 C48 C49 C50 78.9(11) . . . . ? C40 C48 C49 C51 137.1(9) . . . . ? C47 C48 C49 C51 -45.3(12) . . . . ? N6 C36 C52 C53 -1.3(13) . . . . ? N7 C36 C52 C53 179.7(8) . . . . ? C36 C52 C53 C54 1.9(14) . . . . ? C52 C53 C54 C55 -2.3(13) . . . . ? C53 C54 C55 N6 2.1(13) . . . . ? C53 C54 C55 N9 -174.8(8) . . . . ? N10 C57 C58 N9 -0.6(10) . . . . ? N10 C59 C60 C64 -177.6(9) . . . . ? C67 C59 C60 C64 -1.2(14) . . . . ? N10 C59 C60 C61 1.8(14) . . . . ? C67 C59 C60 C61 178.2(9) . . . . ? C59 C60 C61 C63 -126.7(10) . . . . ? C64 C60 C61 C63 52.8(12) . . . . ? C59 C60 C61 C62 109.0(11) . . . . ? C64 C60 C61 C62 -71.5(12) . . . . ? C59 C60 C64 C65 0.3(15) . . . . ? C61 C60 C64 C65 -179.2(9) . . . . ? C60 C64 C65 C66 0.2(16) . . . . ? C64 C65 C66 C67 0.2(17) . . . . ? C65 C66 C67 C59 -1.1(15) . . . . ? C65 C66 C67 C68 -178.1(10) . . . . ? C60 C59 C67 C66 1.6(14) . . . . ? N10 C59 C67 C66 177.9(9) . . . . ? C60 C59 C67 C68 178.7(9) . . . . ? N10 C59 C67 C68 -5.0(14) . . . . ? C66 C67 C68 C70 83.5(12) . . . . ? C59 C67 C68 C70 -93.5(11) . . . . ? C66 C67 C68 C69 -39.8(13) . . . . ? C59 C67 C68 C69 143.2(10) . . . . ? N4 C20 N1 C1 178.9(7) . . . . ? C19 C20 N1 C1 -2.9(13) . . . . ? N4 C20 N1 V1 -0.3(10) . . . . ? C19 C20 N1 V1 178.0(6) . . . . ? C17 C1 N1 C20 3.6(12) . . . . ? N2 C1 N1 C20 -176.1(7) . . . . ? C17 C1 N1 V1 -177.2(6) . . . . ? N2 C1 N1 V1 3.1(9) . . . . ? C15 C16 N2 C2 0.3(11) . . . . ? C15 C16 N2 C1 -174.4(8) . . . . ? N3 C2 N2 C16 -0.1(10) . . . . ? V1 C2 N2 C16 -178.2(6) . . . . ? N3 C2 N2 C1 175.0(7) . . . . ? V1 C2 N2 C1 -3.1(10) . . . . ? N1 C1 N2 C16 174.3(8) . . . . ? C17 C1 N2 C16 -5.4(14) . . . . ? N1 C1 N2 C2 -0.1(11) . . . . ? C17 C1 N2 C2 -179.7(8) . . . . ? N2 C2 N3 C15 -0.2(9) . . . . ? V1 C2 N3 C15 177.2(8) . . . . ? N2 C2 N3 C3 179.8(8) . . . . ? V1 C2 N3 C3 -2.8(16) . . . . ? C16 C15 N3 C2 0.4(10) . . . . ? C16 C15 N3 C3 -179.6(8) . . . . ? C11 C3 N3 C2 -98.4(12) . . . . ? C4 C3 N3 C2 88.2(12) . . . . ? C11 C3 N3 C15 81.6(11) . . . . ? C4 C3 N3 C15 -91.8(10) . . . . ? N5 C21 N4 C20 178.9(7) . . . . ? V1 C21 N4 C20 -4.4(10) . . . . ? N5 C21 N4 C23 -0.7(9) . . . . ? V1 C21 N4 C23 175.9(6) . . . . ? N1 C20 N4 C21 3.1(11) . . . . ? C19 C20 N4 C21 -175.1(9) . . . . ? N1 C20 N4 C23 -177.3(8) . . . . ? C19 C20 N4 C23 4.5(14) . . . . ? C22 C23 N4 C21 -0.5(10) . . . . ? C22 C23 N4 C20 179.9(8) . . . . ? N4 C21 N5 C22 1.6(9) . . . . ? V1 C21 N5 C22 -173.6(7) . . . . ? N4 C21 N5 C24 -169.4(8) . . . . ? V1 C21 N5 C24 15.4(14) . . . . ? C23 C22 N5 C21 -2.1(10) . . . . ? C23 C22 N5 C24 169.0(8) . . . . ? C32 C24 N5 C21 98.4(11) . . . . ? C25 C24 N5 C21 -86.4(11) . . . . ? C32 C24 N5 C22 -71.4(11) . . . . ? C25 C24 N5 C22 103.9(10) . . . . ? C54 C55 N6 C36 -1.6(13) . . . . ? N9 C55 N6 C36 175.6(7) . . . . ? C54 C55 N6 V2 179.7(7) . . . . ? N9 C55 N6 V2 -3.1(10) . . . . ? N7 C36 N6 C55 -179.7(7) . . . . ? C52 C36 N6 C55 1.1(13) . . . . ? N7 C36 N6 V2 -1.0(10) . . . . ? C52 C36 N6 V2 179.8(6) . . . . ? N8 C37 N7 C39 -1.3(10) . . . . ? V2 C37 N7 C39 -176.6(6) . . . . ? N8 C37 N7 C36 -177.1(7) . . . . ? V2 C37 N7 C36 7.6(10) . . . . ? C38 C39 N7 C37 1.8(11) . . . . ? C38 C39 N7 C36 176.9(9) . . . . ? N6 C36 N7 C37 -3.9(11) . . . . ? C52 C36 N7 C37 175.2(8) . . . . ? N6 C36 N7 C39 -178.8(8) . . . . ? C52 C36 N7 C39 0.3(15) . . . . ? N7 C37 N8 C38 0.4(9) . . . . ? V2 C37 N8 C38 174.5(7) . . . . ? N7 C37 N8 C40 169.7(8) . . . . ? V2 C37 N8 C40 -16.2(14) . . . . ? C39 C38 N8 C37 0.7(10) . . . . ? C39 C38 N8 C40 -168.9(8) . . . . ? C41 C40 N8 C37 87.9(11) . . . . ? C48 C40 N8 C37 -88.8(11) . . . . ? C41 C40 N8 C38 -103.9(10) . . . . ? C48 C40 N8 C38 79.4(11) . . . . ? N10 C56 N9 C58 0.4(10) . . . . ? V2 C56 N9 C58 178.5(6) . . . . ? N10 C56 N9 C55 -178.9(7) . . . . ? V2 C56 N9 C55 -0.8(10) . . . . ? C57 C58 N9 C56 0.1(10) . . . . ? C57 C58 N9 C55 179.4(8) . . . . ? N6 C55 N9 C56 2.5(11) . . . . ? C54 C55 N9 C56 179.7(8) . . . . ? N6 C55 N9 C58 -176.7(8) . . . . ? C54 C55 N9 C58 0.5(15) . . . . ? N9 C56 N10 C59 -173.8(8) . . . . ? V2 C56 N10 C59 8.7(15) . . . . ? N9 C56 N10 C57 -0.8(10) . . . . ? V2 C56 N10 C57 -178.3(8) . . . . ? C60 C59 N10 C56 97.0(11) . . . . ? C67 C59 N10 C56 -79.4(12) . . . . ? C60 C59 N10 C57 -75.0(12) . . . . ? C67 C59 N10 C57 108.6(11) . . . . ? C58 C57 N10 C56 0.9(11) . . . . ? C58 C57 N10 C59 173.7(9) . . . . ? N3 C2 V1 O1 6.0(11) . . . . ? N2 C2 V1 O1 -176.8(6) . . . . ? N3 C2 V1 C21 -169.2(8) . . . . ? N2 C2 V1 C21 8.0(9) . . . . ? N3 C2 V1 N1 -173.9(11) . . . . ? N2 C2 V1 N1 3.3(6) . . . . ? N3 C2 V1 Cl1 104.8(10) . . . . ? N2 C2 V1 Cl1 -78.0(6) . . . . ? N3 C2 V1 Cl2 -93.1(10) . . . . ? N2 C2 V1 Cl2 84.1(6) . . . . ? N4 C21 V1 O1 -177.0(6) . . . . ? N5 C21 V1 O1 -2.1(10) . . . . ? N4 C21 V1 C2 -1.9(9) . . . . ? N5 C21 V1 C2 173.0(8) . . . . ? N4 C21 V1 N1 2.8(5) . . . . ? N5 C21 V1 N1 177.7(10) . . . . ? N4 C21 V1 Cl1 85.6(6) . . . . ? N5 C21 V1 Cl1 -99.5(10) . . . . ? N4 C21 V1 Cl2 -78.8(6) . . . . ? N5 C21 V1 Cl2 96.1(10) . . . . ? C20 N1 V1 C2 175.5(7) . . . . ? C1 N1 V1 C2 -3.6(6) . . . . ? C20 N1 V1 C21 -1.4(6) . . . . ? C1 N1 V1 C21 179.4(7) . . . . ? C20 N1 V1 Cl1 -90.7(7) . . . . ? C1 N1 V1 Cl1 90.1(6) . . . . ? C20 N1 V1 Cl2 86.0(7) . . . . ? C1 N1 V1 Cl2 -93.2(6) . . . . ? N10 C56 V2 O2 0.1(11) . . . . ? N9 C56 V2 O2 -177.2(7) . . . . ? N10 C56 V2 C37 177.0(8) . . . . ? N9 C56 V2 C37 -0.3(11) . . . . ? N10 C56 V2 N6 176.7(11) . . . . ? N9 C56 V2 N6 -0.6(6) . . . . ? N10 C56 V2 Cl3 -99.2(10) . . . . ? N9 C56 V2 Cl3 83.6(7) . . . . ? N10 C56 V2 Cl4 99.0(10) . . . . ? N9 C56 V2 Cl4 -78.2(7) . . . . ? N8 C37 V2 O2 -2.6(10) . . . . ? N7 C37 V2 O2 170.8(6) . . . . ? N8 C37 V2 C56 -179.4(8) . . . . ? N7 C37 V2 C56 -6.0(10) . . . . ? N8 C37 V2 N6 -179.1(10) . . . . ? N7 C37 V2 N6 -5.7(6) . . . . ? N8 C37 V2 Cl3 95.6(9) . . . . ? N7 C37 V2 Cl3 -91.0(7) . . . . ? N8 C37 V2 Cl4 -98.3(9) . . . . ? N7 C37 V2 Cl4 75.1(7) . . . . ? C55 N6 V2 C56 2.1(7) . . . . ? C36 N6 V2 C56 -176.6(7) . . . . ? C55 N6 V2 C37 -177.7(7) . . . . ? C36 N6 V2 C37 3.6(6) . . . . ? C55 N6 V2 Cl3 -89.5(6) . . . . ? C36 N6 V2 Cl3 91.8(6) . . . . ? C55 N6 V2 Cl4 97.0(6) . . . . ? C36 N6 V2 Cl4 -81.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.320 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.074 # 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 0.500 0.500 255.7 35.4 2 0.134 0.438 0.919 20.9 2.5 3 0.500 1.000 0.000 255.6 35.4 4 0.365 0.938 0.581 20.8 2.5 5 0.634 0.062 0.419 20.9 2.5 6 0.865 0.562 0.081 20.8 2.5 _platon_squeeze_details ; One disordered molecule of water was removed using the SQUEEZE method ; #==END data_7 _database_code_depnum_ccdc_archive 'CCDC 282405' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H47 B2 F8 N7 O V (C2 H3 N)' _chemical_formula_sum 'C41 H50 B2 F8 N8 O V' _chemical_formula_weight 895.45 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' B B 0.0013 0.0007 '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' 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' V V 0.3005 0.5294 '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 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 16.851(3) _cell_length_b 12.707(4) _cell_length_c 21.564(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.152(13) _cell_angle_gamma 90.00 _cell_volume 4545.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10762 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 0.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8634 _exptl_absorpt_correction_T_max 0.9942 _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 'BrukerNonius 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 66201 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.65 _reflns_number_total 10463 _reflns_number_gt 7469 _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 'DIRDIF-99 (Beurskens, 1999)' _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^)+(0.0629P)^2^+6.4833P] 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 10463 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.24920(2) 0.02121(3) 0.112028(19) 0.01929(11) Uani 1 1 d . . . F4 F 0.45680(16) 0.0578(2) 0.39823(10) 0.0814(8) Uani 1 1 d . . . F3 F 0.54267(10) 0.05319(14) 0.33006(9) 0.0458(5) Uani 1 1 d . . . F8 F 0.66229(17) 0.21236(19) 0.13799(11) 0.0812(8) Uani 1 1 d . . . O1 O 0.15881(11) 0.06174(15) 0.09317(9) 0.0303(4) Uani 1 1 d . . . F2 F 0.43809(12) -0.05980(15) 0.31840(12) 0.0603(6) Uani 1 1 d . . . F1 F 0.41478(11) 0.11191(15) 0.29967(9) 0.0498(5) Uani 1 1 d . . . N4 N 0.40550(12) 0.13852(17) 0.15724(9) 0.0217(4) Uani 1 1 d . . . N7 N 0.28480(13) 0.02452(18) 0.02394(10) 0.0258(5) Uani 1 1 d . . . C36 C 0.25571(16) -0.0120(2) 0.26076(13) 0.0264(6) Uani 1 1 d . . . C38 C 0.31316(17) 0.0234(2) -0.01999(13) 0.0299(6) Uani 1 1 d . . . N5 N 0.31711(12) 0.26037(16) 0.13715(10) 0.0217(4) Uani 1 1 d . . . F5 F 0.71207(17) 0.09068(18) 0.21108(12) 0.0851(9) Uani 1 1 d . . . N2 N 0.32086(13) -0.19753(16) 0.12457(10) 0.0230(5) Uani 1 1 d . . . F7 F 0.75977(15) 0.2559(2) 0.21844(14) 0.0939(10) Uani 1 1 d . . . N6 N 0.24986(12) 0.00055(16) 0.20811(10) 0.0229(5) Uani 1 1 d . . . C25 C 0.18573(16) 0.3244(2) 0.15539(13) 0.0281(6) Uani 1 1 d . . . F6 F 0.63613(16) 0.2209(2) 0.23391(12) 0.0868(8) Uani 1 1 d . . . C26 C 0.11526(17) 0.3803(2) 0.13265(15) 0.0338(6) Uani 1 1 d . . . H26 H 0.0757 0.3886 0.1587 0.041 Uiso 1 1 calc R . . C40 C 0.5120(2) 0.2247(3) 0.02392(16) 0.0443(8) Uani 1 1 d . . . C8 C -0.02315(17) -0.1938(3) 0.08668(14) 0.0358(7) Uani 1 1 d . . . H8 H -0.0604 -0.1964 0.1149 0.043 Uiso 1 1 calc R . . N3 N 0.37574(12) -0.03483(16) 0.14313(9) 0.0208(4) Uani 1 1 d . . . C17 C 0.46760(16) -0.1776(2) 0.16688(12) 0.0263(6) Uani 1 1 d . . . H17 H 0.4780 -0.2511 0.1685 0.032 Uiso 1 1 calc R . . C2 C 0.31145(17) -0.3054(2) 0.12085(13) 0.0292(6) Uani 1 1 d . . . H2 H 0.3521 -0.3572 0.1321 0.035 Uiso 1 1 calc R . . N1 N 0.19583(13) -0.22350(17) 0.08873(10) 0.0232(5) Uani 1 1 d . . . C6 C 0.00193(17) -0.1724(2) -0.01824(14) 0.0340(7) Uani 1 1 d . . . H6 H -0.0181 -0.1592 -0.0615 0.041 Uiso 1 1 calc R . . C34 C 0.3322(2) 0.4539(3) 0.00455(15) 0.0418(8) Uani 1 1 d . . . H34A H 0.2912 0.5048 -0.0141 0.063 Uiso 1 1 calc R . . H34B H 0.3725 0.4461 -0.0228 0.063 Uiso 1 1 calc R . . H34C H 0.3585 0.4789 0.0461 0.063 Uiso 1 1 calc R . . C22 C 0.44657(16) 0.2325(2) 0.17138(12) 0.0250(5) Uani 1 1 d . . . H22 H 0.5026 0.2410 0.1869 0.030 Uiso 1 1 calc R . . C37 C 0.26098(19) -0.0243(3) 0.32841(13) 0.0373(7) Uani 1 1 d . . . H37A H 0.2843 0.0394 0.3499 0.056 Uiso 1 1 calc R . . H37B H 0.2952 -0.0849 0.3429 0.056 Uiso 1 1 calc R . . H37C H 0.2069 -0.0357 0.3380 0.056 Uiso 1 1 calc R . . C29 C 0.22986(16) 0.3577(2) 0.05428(13) 0.0265(6) Uani 1 1 d . . . C7 C -0.05103(18) -0.1752(3) 0.02378(15) 0.0380(7) Uani 1 1 d . . . H7 H -0.1070 -0.1643 0.0092 0.046 Uiso 1 1 calc R . . C28 C 0.15832(17) 0.4120(2) 0.03409(14) 0.0329(6) Uani 1 1 d . . . H28 H 0.1480 0.4415 -0.0070 0.039 Uiso 1 1 calc R . . C21 C 0.32489(15) 0.1553(2) 0.13597(11) 0.0206(5) Uani 1 1 d . . . C27 C 0.10196(17) 0.4237(2) 0.07316(15) 0.0358(7) Uani 1 1 d . . . H27 H 0.0538 0.4619 0.0588 0.043 Uiso 1 1 calc R . . C24 C 0.24216(15) 0.3156(2) 0.11533(12) 0.0241(5) Uani 1 1 d . . . C10 C 0.08882(17) -0.2265(3) 0.17975(13) 0.0345(7) Uani 1 1 d . . . H10 H 0.1490 -0.2234 0.1871 0.041 Uiso 1 1 calc R . . C23 C 0.39135(16) 0.3089(2) 0.15865(12) 0.0264(6) Uani 1 1 d . . . H23 H 0.4008 0.3824 0.1634 0.032 Uiso 1 1 calc R . . C16 C 0.39142(15) -0.1373(2) 0.14593(11) 0.0221(5) Uani 1 1 d . . . C5 C 0.08442(16) -0.1887(2) 0.00172(13) 0.0271(6) Uani 1 1 d . . . C39 C 0.3499(2) 0.0213(3) -0.07620(14) 0.0446(8) Uani 1 1 d . . . H39A H 0.4014 -0.0163 -0.0671 0.067 Uiso 1 1 calc R . . H39B H 0.3592 0.0935 -0.0892 0.067 Uiso 1 1 calc R . . H39C H 0.3138 -0.0147 -0.1102 0.067 Uiso 1 1 calc R . . C30 C 0.19836(18) 0.2766(2) 0.22090(13) 0.0325(6) Uani 1 1 d . . . H30 H 0.2487 0.2334 0.2266 0.039 Uiso 1 1 calc R . . C9 C 0.05877(16) -0.2088(2) 0.10989(13) 0.0290(6) Uani 1 1 d . . . C18 C 0.52808(16) -0.1039(2) 0.18546(12) 0.0281(6) Uani 1 1 d . . . H18 H 0.5815 -0.1281 0.1998 0.034 Uiso 1 1 calc R . . C12 C 0.0594(2) -0.1393(3) 0.21917(15) 0.0433(8) Uani 1 1 d . . . H12A H 0.0762 -0.0707 0.2052 0.065 Uiso 1 1 calc R . . H12B H 0.0828 -0.1497 0.2637 0.065 Uiso 1 1 calc R . . H12C H 0.0005 -0.1417 0.2139 0.065 Uiso 1 1 calc R . . C15 C 0.1242(2) -0.0995(3) -0.09350(16) 0.0478(8) Uani 1 1 d . . . H15A H 0.0712 -0.1103 -0.1199 0.072 Uiso 1 1 calc R . . H15B H 0.1658 -0.0988 -0.1200 0.072 Uiso 1 1 calc R . . H15C H 0.1245 -0.0322 -0.0713 0.072 Uiso 1 1 calc R . . C19 C 0.51338(15) 0.0034(2) 0.18383(12) 0.0244(6) Uani 1 1 d . . . H19 H 0.5551 0.0531 0.1969 0.029 Uiso 1 1 calc R . . C20 C 0.43444(15) 0.0340(2) 0.16213(11) 0.0217(5) Uani 1 1 d . . . C32 C 0.12815(19) 0.2040(3) 0.22869(16) 0.0418(8) Uani 1 1 d . . . H32A H 0.0782 0.2450 0.2239 0.063 Uiso 1 1 calc R . . H32B H 0.1388 0.1718 0.2706 0.063 Uiso 1 1 calc R . . H32C H 0.1226 0.1487 0.1965 0.063 Uiso 1 1 calc R . . C1 C 0.24911(15) -0.1460(2) 0.10546(11) 0.0209(5) Uani 1 1 d . . . N8 N 0.4747(2) 0.1500(3) 0.02384(16) 0.0624(9) Uani 1 1 d . . . C11 C 0.0650(2) -0.3353(3) 0.19999(16) 0.0478(8) Uani 1 1 d . . . H11A H 0.0061 -0.3414 0.1923 0.072 Uiso 1 1 calc R . . H11B H 0.0858 -0.3452 0.2450 0.072 Uiso 1 1 calc R . . H11C H 0.0877 -0.3892 0.1757 0.072 Uiso 1 1 calc R . . C31 C 0.2096(2) 0.3628(3) 0.27141(16) 0.0509(9) Uani 1 1 d . . . H31A H 0.2561 0.4065 0.2668 0.076 Uiso 1 1 calc R . . H31B H 0.2186 0.3304 0.3133 0.076 Uiso 1 1 calc R . . H31C H 0.1611 0.4068 0.2664 0.076 Uiso 1 1 calc R . . C33 C 0.29221(18) 0.3473(2) 0.01156(13) 0.0309(6) Uani 1 1 d . . . H33 H 0.3349 0.2976 0.0321 0.037 Uiso 1 1 calc R . . C13 C 0.14120(18) -0.1886(2) -0.04565(13) 0.0319(6) Uani 1 1 d . . . H13 H 0.1972 -0.1788 -0.0218 0.038 Uiso 1 1 calc R . . C4 C 0.11042(15) -0.2069(2) 0.06597(12) 0.0244(5) Uani 1 1 d . . . C3 C 0.23256(17) -0.3220(2) 0.09792(13) 0.0289(6) Uani 1 1 d . . . H3 H 0.2069 -0.3883 0.0896 0.035 Uiso 1 1 calc R . . C35 C 0.2552(2) 0.3014(3) -0.05291(14) 0.0392(7) Uani 1 1 d . . . H35A H 0.2309 0.2329 -0.0471 0.059 Uiso 1 1 calc R . . H35B H 0.2975 0.2926 -0.0785 0.059 Uiso 1 1 calc R . . H35C H 0.2138 0.3494 -0.0744 0.059 Uiso 1 1 calc R . . C41 C 0.5582(2) 0.3204(3) 0.02470(19) 0.0583(10) Uani 1 1 d . . . H41A H 0.5369 0.3627 -0.0125 0.087 Uiso 1 1 calc R . . H41B H 0.6148 0.3029 0.0243 0.087 Uiso 1 1 calc R . . H41C H 0.5544 0.3605 0.0629 0.087 Uiso 1 1 calc R . . C14 C 0.1381(3) -0.2946(3) -0.07920(19) 0.0596(10) Uani 1 1 d . . . H14A H 0.1501 -0.3509 -0.0479 0.089 Uiso 1 1 calc R . . H14B H 0.1780 -0.2955 -0.1072 0.089 Uiso 1 1 calc R . . H14C H 0.0841 -0.3053 -0.1040 0.089 Uiso 1 1 calc R . . B1 B 0.4624(2) 0.0407(3) 0.33721(16) 0.0310(7) Uani 1 1 d . . . B2 B 0.6950(2) 0.1946(3) 0.20087(16) 0.0317(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 V1 0.0196(2) 0.0199(2) 0.0179(2) 0.00060(17) 0.00205(15) 0.00120(17) F4 0.0921(18) 0.123(2) 0.0319(11) -0.0040(13) 0.0184(11) 0.0014(16) F3 0.0319(9) 0.0390(10) 0.0667(13) -0.0093(9) 0.0090(9) -0.0100(8) F8 0.112(2) 0.0639(15) 0.0515(14) -0.0064(11) -0.0305(13) 0.0139(14) O1 0.0265(10) 0.0313(10) 0.0318(10) 0.0006(8) 0.0012(8) 0.0048(8) F2 0.0425(11) 0.0341(10) 0.1056(18) -0.0072(11) 0.0164(11) -0.0113(9) F1 0.0459(11) 0.0443(11) 0.0548(12) 0.0111(9) -0.0029(9) -0.0009(9) N4 0.0213(11) 0.0246(11) 0.0195(10) 0.0001(8) 0.0040(8) -0.0012(9) N7 0.0322(12) 0.0261(11) 0.0189(11) 0.0000(9) 0.0037(9) -0.0018(10) C36 0.0265(13) 0.0256(13) 0.0272(14) -0.0025(11) 0.0052(11) -0.0025(11) C38 0.0367(15) 0.0286(14) 0.0232(13) 0.0001(11) 0.0020(11) -0.0007(12) N5 0.0238(11) 0.0205(11) 0.0211(11) 0.0000(8) 0.0048(9) -0.0014(9) F5 0.115(2) 0.0388(12) 0.0854(18) -0.0059(12) -0.0280(15) 0.0223(13) N2 0.0236(11) 0.0203(11) 0.0239(11) -0.0006(9) 0.0009(9) 0.0023(9) F7 0.0638(16) 0.091(2) 0.110(2) 0.0355(17) -0.0327(15) -0.0361(14) N6 0.0225(11) 0.0231(12) 0.0227(11) -0.0002(9) 0.0033(8) -0.0025(8) C25 0.0286(14) 0.0241(14) 0.0324(15) -0.0023(11) 0.0077(11) -0.0018(11) F6 0.0758(17) 0.118(2) 0.0720(17) 0.0129(16) 0.0272(14) 0.0352(16) C26 0.0290(15) 0.0304(15) 0.0428(17) -0.0036(13) 0.0085(13) 0.0001(12) C40 0.0454(19) 0.049(2) 0.0382(18) -0.0053(15) 0.0061(15) -0.0050(16) C8 0.0251(14) 0.0446(18) 0.0377(16) 0.0016(14) 0.0054(12) -0.0003(13) N3 0.0205(10) 0.0228(11) 0.0190(10) 0.0001(8) 0.0031(8) 0.0001(8) C17 0.0261(14) 0.0275(14) 0.0251(13) 0.0031(11) 0.0036(11) 0.0051(11) C2 0.0312(15) 0.0211(13) 0.0337(15) -0.0010(11) 0.0010(12) 0.0031(11) N1 0.0235(11) 0.0215(11) 0.0233(11) -0.0016(9) 0.0009(9) 0.0008(9) C6 0.0351(16) 0.0340(16) 0.0290(15) 0.0007(12) -0.0049(12) 0.0012(12) C34 0.0476(19) 0.0435(19) 0.0359(17) -0.0023(14) 0.0117(14) -0.0109(15) C22 0.0278(14) 0.0258(14) 0.0209(13) 0.0009(10) 0.0030(10) -0.0048(11) C37 0.0419(17) 0.0483(18) 0.0234(14) 0.0012(13) 0.0105(12) -0.0076(15) C29 0.0305(14) 0.0196(13) 0.0282(14) -0.0016(10) 0.0022(11) -0.0027(11) C7 0.0239(14) 0.0462(18) 0.0406(17) 0.0018(14) -0.0030(12) -0.0004(13) C28 0.0381(16) 0.0249(14) 0.0332(15) 0.0024(12) -0.0003(12) 0.0018(12) C21 0.0225(12) 0.0240(13) 0.0157(11) 0.0013(9) 0.0045(9) 0.0005(10) C27 0.0289(15) 0.0281(15) 0.0474(18) -0.0015(13) -0.0014(13) 0.0052(12) C24 0.0255(13) 0.0179(12) 0.0282(13) -0.0013(10) 0.0026(10) -0.0008(10) C10 0.0277(15) 0.0482(18) 0.0276(15) 0.0031(13) 0.0051(12) -0.0007(13) C23 0.0305(14) 0.0254(14) 0.0233(13) -0.0005(11) 0.0046(11) -0.0070(11) C16 0.0214(12) 0.0254(13) 0.0191(12) 0.0001(10) 0.0026(10) 0.0004(10) C5 0.0291(14) 0.0231(13) 0.0270(14) -0.0038(11) -0.0007(11) -0.0010(11) C39 0.059(2) 0.052(2) 0.0266(15) -0.0030(14) 0.0166(14) 0.0009(17) C30 0.0377(16) 0.0301(15) 0.0329(15) 0.0009(12) 0.0147(13) 0.0010(12) C9 0.0273(14) 0.0296(15) 0.0287(14) 0.0000(11) 0.0013(11) -0.0018(11) C18 0.0207(13) 0.0406(16) 0.0227(13) 0.0066(12) 0.0029(10) 0.0053(11) C12 0.0401(18) 0.057(2) 0.0341(17) -0.0058(15) 0.0095(14) -0.0087(15) C15 0.054(2) 0.053(2) 0.0358(17) 0.0117(16) 0.0068(15) 0.0035(17) C19 0.0215(12) 0.0312(15) 0.0203(12) 0.0030(10) 0.0027(10) -0.0012(10) C20 0.0256(13) 0.0242(13) 0.0160(11) 0.0012(10) 0.0061(10) -0.0004(10) C32 0.0445(18) 0.0378(18) 0.0495(19) 0.0056(15) 0.0256(15) 0.0038(14) C1 0.0219(12) 0.0237(13) 0.0165(11) -0.0002(10) 0.0021(9) 0.0012(10) N8 0.067(2) 0.064(2) 0.059(2) -0.0148(17) 0.0168(17) -0.0223(18) C11 0.056(2) 0.052(2) 0.0380(18) 0.0106(15) 0.0143(16) 0.0056(17) C31 0.073(2) 0.046(2) 0.0345(18) -0.0075(15) 0.0110(17) -0.0042(18) C33 0.0383(16) 0.0298(15) 0.0249(14) 0.0024(11) 0.0066(12) 0.0018(12) C13 0.0339(15) 0.0362(16) 0.0246(14) -0.0032(12) 0.0026(11) 0.0018(12) C4 0.0228(13) 0.0223(13) 0.0261(13) -0.0029(10) -0.0013(10) -0.0011(10) C3 0.0328(15) 0.0185(13) 0.0330(15) -0.0027(11) -0.0007(11) 0.0019(11) C35 0.0513(19) 0.0391(18) 0.0281(15) -0.0003(13) 0.0095(13) -0.0018(15) C41 0.064(2) 0.048(2) 0.058(2) 0.0104(18) -0.0043(19) -0.0133(18) C14 0.078(3) 0.048(2) 0.060(2) -0.0173(18) 0.031(2) -0.003(2) B1 0.0331(17) 0.0297(17) 0.0311(17) 0.0002(13) 0.0079(13) -0.0037(13) B2 0.0297(17) 0.0322(17) 0.0324(17) -0.0045(14) 0.0033(13) -0.0012(13) _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 V1 O1 1.5913(19) . ? V1 N6 2.087(2) . ? V1 N7 2.091(2) . ? V1 C1 2.129(3) . ? V1 C21 2.136(3) . ? V1 N3 2.236(2) . ? F4 B1 1.354(4) . ? F3 B1 1.397(4) . ? F8 B2 1.389(4) . ? F2 B1 1.380(4) . ? F1 B1 1.375(4) . ? N4 C21 1.372(3) . ? N4 C22 1.387(3) . ? N4 C20 1.413(3) . ? N7 C38 1.134(3) . ? C36 N6 1.133(3) . ? C36 C37 1.454(4) . ? C38 C39 1.455(4) . ? N5 C21 1.342(3) . ? N5 C23 1.399(3) . ? N5 C24 1.449(3) . ? F5 B2 1.362(4) . ? N2 C1 1.373(3) . ? N2 C2 1.380(3) . ? N2 C16 1.420(3) . ? F7 B2 1.341(4) . ? C25 C26 1.396(4) . ? C25 C24 1.397(4) . ? C25 C30 1.518(4) . ? F6 B2 1.360(4) . ? C26 C27 1.378(4) . ? C26 H26 0.9500 . ? C40 N8 1.138(4) . ? C40 C41 1.442(5) . ? C8 C7 1.375(4) . ? C8 C9 1.396(4) . ? C8 H8 0.9500 . ? N3 C16 1.328(3) . ? N3 C20 1.329(3) . ? C17 C16 1.382(4) . ? C17 C18 1.389(4) . ? C17 H17 0.9500 . ? C2 C3 1.351(4) . ? C2 H2 0.9500 . ? N1 C1 1.339(3) . ? N1 C3 1.395(3) . ? N1 C4 1.452(3) . ? C6 C7 1.380(4) . ? C6 C5 1.396(4) . ? C6 H6 0.9500 . ? C34 C33 1.532(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C22 C23 1.339(4) . ? C22 H22 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C29 C28 1.391(4) . ? C29 C24 1.402(4) . ? C29 C33 1.520(4) . ? C7 H7 0.9500 . ? C28 C27 1.384(4) . ? C28 H28 0.9500 . ? C27 H27 0.9500 . ? C10 C9 1.519(4) . ? C10 C11 1.524(5) . ? C10 C12 1.531(4) . ? C10 H10 1.0000 . ? C23 H23 0.9500 . ? C5 C4 1.397(4) . ? C5 C13 1.518(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C30 C32 1.533(4) . ? C30 C31 1.533(4) . ? C30 H30 1.0000 . ? C9 C4 1.395(4) . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C15 C13 1.524(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C19 C20 1.386(4) . ? C19 H19 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 C35 1.535(4) . ? C33 H33 1.0000 . ? C13 C14 1.525(4) . ? C13 H13 1.0000 . ? C3 H3 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 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 O1 V1 N6 97.58(9) . . ? O1 V1 N7 100.15(9) . . ? N6 V1 N7 162.27(9) . . ? O1 V1 C1 108.46(10) . . ? N6 V1 C1 86.58(9) . . ? N7 V1 C1 87.51(9) . . ? O1 V1 C21 107.91(10) . . ? N6 V1 C21 87.82(9) . . ? N7 V1 C21 87.06(9) . . ? C1 V1 C21 143.63(10) . . ? O1 V1 N3 177.39(9) . . ? N6 V1 N3 79.87(8) . . ? N7 V1 N3 82.40(8) . . ? C1 V1 N3 72.04(9) . . ? C21 V1 N3 71.59(9) . . ? C21 N4 C22 111.5(2) . . ? C21 N4 C20 118.7(2) . . ? C22 N4 C20 129.9(2) . . ? C38 N7 V1 171.7(2) . . ? N6 C36 C37 177.6(3) . . ? N7 C38 C39 179.6(4) . . ? C21 N5 C23 111.1(2) . . ? C21 N5 C24 123.9(2) . . ? C23 N5 C24 124.9(2) . . ? C1 N2 C2 111.7(2) . . ? C1 N2 C16 118.9(2) . . ? C2 N2 C16 129.4(2) . . ? C36 N6 V1 175.3(2) . . ? C26 C25 C24 116.9(3) . . ? C26 C25 C30 120.1(3) . . ? C24 C25 C30 123.0(2) . . ? C27 C26 C25 121.3(3) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? N8 C40 C41 178.9(4) . . ? C7 C8 C9 121.4(3) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C16 N3 C20 120.0(2) . . ? C16 N3 V1 119.82(16) . . ? C20 N3 V1 120.10(17) . . ? C16 C17 C18 115.9(3) . . ? C16 C17 H17 122.0 . . ? C18 C17 H17 122.0 . . ? C3 C2 N2 105.8(2) . . ? C3 C2 H2 127.1 . . ? N2 C2 H2 127.1 . . ? C1 N1 C3 111.2(2) . . ? C1 N1 C4 124.2(2) . . ? C3 N1 C4 124.5(2) . . ? C7 C6 C5 121.2(3) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? 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 . . ? C23 C22 N4 106.1(2) . . ? C23 C22 H22 127.0 . . ? N4 C22 H22 127.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C28 C29 C24 117.4(3) . . ? C28 C29 C33 120.5(2) . . ? C24 C29 C33 122.2(2) . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C27 C28 C29 120.8(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? N5 C21 N4 104.0(2) . . ? N5 C21 V1 137.87(18) . . ? N4 C21 V1 118.09(17) . . ? C26 C27 C28 120.5(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C25 C24 C29 123.1(2) . . ? C25 C24 N5 119.1(2) . . ? C29 C24 N5 117.8(2) . . ? C9 C10 C11 111.1(3) . . ? C9 C10 C12 111.0(3) . . ? C11 C10 C12 111.7(3) . . ? C9 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C22 C23 N5 107.3(2) . . ? C22 C23 H23 126.4 . . ? N5 C23 H23 126.4 . . ? N3 C16 C17 122.9(2) . . ? N3 C16 N2 111.4(2) . . ? C17 C16 N2 125.7(2) . . ? C4 C5 C6 116.8(3) . . ? C4 C5 C13 122.9(2) . . ? C6 C5 C13 120.3(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C25 C30 C32 111.0(3) . . ? C25 C30 C31 110.8(3) . . ? C32 C30 C31 110.7(3) . . ? C25 C30 H30 108.1 . . ? C32 C30 H30 108.1 . . ? C31 C30 H30 108.1 . . ? C4 C9 C8 116.7(3) . . ? C4 C9 C10 122.5(2) . . ? C8 C9 C10 120.8(3) . . ? C19 C18 C17 122.5(2) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? 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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C19 C20 116.2(2) . . ? C18 C19 H19 121.9 . . ? C20 C19 H19 121.9 . . ? N3 C20 C19 122.5(2) . . ? N3 C20 N4 111.5(2) . . ? C19 C20 N4 126.0(2) . . ? 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 . . ? N1 C1 N2 104.1(2) . . ? N1 C1 V1 138.13(18) . . ? N2 C1 V1 117.77(17) . . ? 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 . . ? 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 . . ? C29 C33 C34 110.2(2) . . ? C29 C33 C35 111.6(2) . . ? C34 C33 C35 111.2(2) . . ? C29 C33 H33 107.9 . . ? C34 C33 H33 107.9 . . ? C35 C33 H33 107.9 . . ? C5 C13 C14 110.2(3) . . ? C5 C13 C15 113.0(3) . . ? C14 C13 C15 110.4(3) . . ? C5 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C9 C4 C5 123.5(2) . . ? C9 C4 N1 117.9(2) . . ? C5 C4 N1 118.6(2) . . ? C2 C3 N1 107.2(2) . . ? C2 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? 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 . . ? 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 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? F4 B1 F1 109.4(3) . . ? F4 B1 F2 111.5(3) . . ? F1 B1 F2 108.9(3) . . ? F4 B1 F3 108.9(3) . . ? F1 B1 F3 109.6(2) . . ? F2 B1 F3 108.4(3) . . ? F7 B2 F6 110.0(3) . . ? F7 B2 F5 112.3(3) . . ? F6 B2 F5 107.8(3) . . ? F7 B2 F8 110.1(3) . . ? F6 B2 F8 105.8(3) . . ? F5 B2 F8 110.6(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 O1 V1 N7 C38 173.5(16) . . . . ? N6 V1 N7 C38 -7.6(17) . . . . ? C1 V1 N7 C38 -78.2(16) . . . . ? C21 V1 N7 C38 65.8(16) . . . . ? N3 V1 N7 C38 -6.0(16) . . . . ? V1 N7 C38 C39 42(62) . . . . ? C37 C36 N6 V1 139(6) . . . . ? O1 V1 N6 C36 -172(3) . . . . ? N7 V1 N6 C36 9(3) . . . . ? C1 V1 N6 C36 79(3) . . . . ? C21 V1 N6 C36 -65(3) . . . . ? N3 V1 N6 C36 7(3) . . . . ? C24 C25 C26 C27 0.7(4) . . . . ? C30 C25 C26 C27 -179.4(3) . . . . ? O1 V1 N3 C16 99(2) . . . . ? N6 V1 N3 C16 86.84(19) . . . . ? N7 V1 N3 C16 -92.67(19) . . . . ? C1 V1 N3 C16 -2.83(18) . . . . ? C21 V1 N3 C16 177.9(2) . . . . ? O1 V1 N3 C20 -78(2) . . . . ? N6 V1 N3 C20 -89.42(18) . . . . ? N7 V1 N3 C20 91.07(19) . . . . ? C1 V1 N3 C20 -179.1(2) . . . . ? C21 V1 N3 C20 1.65(17) . . . . ? C1 N2 C2 C3 1.1(3) . . . . ? C16 N2 C2 C3 179.5(2) . . . . ? C21 N4 C22 C23 -0.2(3) . . . . ? C20 N4 C22 C23 -179.8(2) . . . . ? C9 C8 C7 C6 0.9(5) . . . . ? C5 C6 C7 C8 0.3(5) . . . . ? C24 C29 C28 C27 0.1(4) . . . . ? C33 C29 C28 C27 -178.7(3) . . . . ? C23 N5 C21 N4 0.1(3) . . . . ? C24 N5 C21 N4 176.7(2) . . . . ? C23 N5 C21 V1 179.5(2) . . . . ? C24 N5 C21 V1 -3.9(4) . . . . ? C22 N4 C21 N5 0.1(3) . . . . ? C20 N4 C21 N5 179.7(2) . . . . ? C22 N4 C21 V1 -179.44(16) . . . . ? C20 N4 C21 V1 0.1(3) . . . . ? O1 V1 C21 N5 -2.9(3) . . . . ? N6 V1 C21 N5 -100.1(3) . . . . ? N7 V1 C21 N5 96.9(3) . . . . ? C1 V1 C21 N5 178.6(2) . . . . ? N3 V1 C21 N5 179.8(3) . . . . ? O1 V1 C21 N4 176.44(17) . . . . ? N6 V1 C21 N4 79.18(18) . . . . ? N7 V1 C21 N4 -83.83(18) . . . . ? C1 V1 C21 N4 -2.1(3) . . . . ? N3 V1 C21 N4 -0.87(17) . . . . ? C25 C26 C27 C28 0.5(4) . . . . ? C29 C28 C27 C26 -0.9(4) . . . . ? C26 C25 C24 C29 -1.5(4) . . . . ? C30 C25 C24 C29 178.5(2) . . . . ? C26 C25 C24 N5 178.7(2) . . . . ? C30 C25 C24 N5 -1.3(4) . . . . ? C28 C29 C24 C25 1.2(4) . . . . ? C33 C29 C24 C25 179.9(2) . . . . ? C28 C29 C24 N5 -179.0(2) . . . . ? C33 C29 C24 N5 -0.3(4) . . . . ? C21 N5 C24 C25 82.0(3) . . . . ? C23 N5 C24 C25 -101.9(3) . . . . ? C21 N5 C24 C29 -97.8(3) . . . . ? C23 N5 C24 C29 78.3(3) . . . . ? N4 C22 C23 N5 0.3(3) . . . . ? C21 N5 C23 C22 -0.2(3) . . . . ? C24 N5 C23 C22 -176.8(2) . . . . ? C20 N3 C16 C17 -1.3(4) . . . . ? V1 N3 C16 C17 -177.58(19) . . . . ? C20 N3 C16 N2 179.0(2) . . . . ? V1 N3 C16 N2 2.8(3) . . . . ? C18 C17 C16 N3 0.2(4) . . . . ? C18 C17 C16 N2 179.8(2) . . . . ? C1 N2 C16 N3 -0.7(3) . . . . ? C2 N2 C16 N3 -179.1(2) . . . . ? C1 N2 C16 C17 179.6(2) . . . . ? C2 N2 C16 C17 1.3(4) . . . . ? C7 C6 C5 C4 -0.5(4) . . . . ? C7 C6 C5 C13 178.1(3) . . . . ? C26 C25 C30 C32 55.3(3) . . . . ? C24 C25 C30 C32 -124.8(3) . . . . ? C26 C25 C30 C31 -68.1(4) . . . . ? C24 C25 C30 C31 111.8(3) . . . . ? C7 C8 C9 C4 -1.7(4) . . . . ? C7 C8 C9 C10 178.5(3) . . . . ? C11 C10 C9 C4 -108.1(3) . . . . ? C12 C10 C9 C4 126.9(3) . . . . ? C11 C10 C9 C8 71.7(4) . . . . ? C12 C10 C9 C8 -53.3(4) . . . . ? C16 C17 C18 C19 0.6(4) . . . . ? C17 C18 C19 C20 -0.4(4) . . . . ? C16 N3 C20 C19 1.6(4) . . . . ? V1 N3 C20 C19 177.83(18) . . . . ? C16 N3 C20 N4 -178.3(2) . . . . ? V1 N3 C20 N4 -2.0(3) . . . . ? C18 C19 C20 N3 -0.7(4) . . . . ? C18 C19 C20 N4 179.1(2) . . . . ? C21 N4 C20 N3 1.2(3) . . . . ? C22 N4 C20 N3 -179.3(2) . . . . ? C21 N4 C20 C19 -178.6(2) . . . . ? C22 N4 C20 C19 0.9(4) . . . . ? C3 N1 C1 N2 0.9(3) . . . . ? C4 N1 C1 N2 179.0(2) . . . . ? C3 N1 C1 V1 -176.6(2) . . . . ? C4 N1 C1 V1 1.5(4) . . . . ? C2 N2 C1 N1 -1.2(3) . . . . ? C16 N2 C1 N1 -179.9(2) . . . . ? C2 N2 C1 V1 176.92(18) . . . . ? C16 N2 C1 V1 -1.7(3) . . . . ? O1 V1 C1 N1 2.3(3) . . . . ? N6 V1 C1 N1 99.1(3) . . . . ? N7 V1 C1 N1 -97.6(3) . . . . ? C21 V1 C1 N1 -179.3(2) . . . . ? N3 V1 C1 N1 179.6(3) . . . . ? O1 V1 C1 N2 -175.06(18) . . . . ? N6 V1 C1 N2 -78.21(19) . . . . ? N7 V1 C1 N2 85.06(19) . . . . ? C21 V1 C1 N2 3.4(3) . . . . ? N3 V1 C1 N2 2.25(17) . . . . ? C28 C29 C33 C34 70.3(3) . . . . ? C24 C29 C33 C34 -108.4(3) . . . . ? C28 C29 C33 C35 -53.8(3) . . . . ? C24 C29 C33 C35 127.5(3) . . . . ? C4 C5 C13 C14 98.4(3) . . . . ? C6 C5 C13 C14 -80.1(4) . . . . ? C4 C5 C13 C15 -137.6(3) . . . . ? C6 C5 C13 C15 43.8(4) . . . . ? C8 C9 C4 C5 1.5(4) . . . . ? C10 C9 C4 C5 -178.7(3) . . . . ? C8 C9 C4 N1 -179.3(2) . . . . ? C10 C9 C4 N1 0.5(4) . . . . ? C6 C5 C4 C9 -0.4(4) . . . . ? C13 C5 C4 C9 -179.0(3) . . . . ? C6 C5 C4 N1 -179.6(2) . . . . ? C13 C5 C4 N1 1.8(4) . . . . ? C1 N1 C4 C9 -92.8(3) . . . . ? C3 N1 C4 C9 85.0(3) . . . . ? C1 N1 C4 C5 86.4(3) . . . . ? C3 N1 C4 C5 -95.7(3) . . . . ? N2 C2 C3 N1 -0.5(3) . . . . ? C1 N1 C3 C2 -0.3(3) . . . . ? C4 N1 C3 C2 -178.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.651 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.065 #==END data_9 _database_code_depnum_ccdc_archive 'CCDC 282406' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H49 Cl2 N6 Ti' _chemical_formula_sum 'C39 H49 Cl2 N6 O0 Ti' _chemical_formula_weight 720.64 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' Cl Cl 0.1484 0.1585 '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' Ti Ti 0.2776 0.4457 '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 Orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 10.802(9) _cell_length_b 13.630(13) _cell_length_c 32.45(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4778(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6000 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9389 _exptl_absorpt_correction_T_max 0.9873 _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 33304 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_sigmaI/netI 0.1938 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10871 _reflns_number_gt 5519 _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 'DIRDIF-99 (Beurskens, 1999)' _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 THF - 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^)+(0.1016P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(5) _refine_ls_number_reflns 10871 _refine_ls_number_parameters 477 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.1728 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.2221 _refine_ls_wR_factor_gt 0.1944 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.007 _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 Ti1 Ti 0.76731(9) 0.87609(7) 0.82365(3) 0.0269(3) Uani 1 1 d . . . Cl2 Cl 0.62972(15) 0.74301(12) 0.80586(5) 0.0494(5) Uani 1 1 d . . . Cl1 Cl 0.92655(14) 1.00175(11) 0.81862(5) 0.0428(4) Uani 1 1 d . . . C7 C 0.3174(6) 0.9585(5) 0.77813(19) 0.0394(16) Uani 1 1 d . . . H7 H 0.3880 0.9364 0.7605 0.047 Uiso 1 1 calc R . . N4 N 0.9676(4) 0.7295(3) 0.78850(13) 0.0279(11) Uani 1 1 d . . . N3 N 0.8391(4) 0.8399(3) 0.75759(13) 0.0278(11) Uani 1 1 d . . . N5 N 0.9828(5) 0.7008(4) 0.85296(15) 0.0404(13) Uani 1 1 d . . . N2 N 0.6983(4) 0.9540(4) 0.73637(13) 0.0352(13) Uani 1 1 d . . . C3 C 0.2894(6) 1.0738(5) 0.83766(19) 0.0497(18) Uani 1 1 d . . . H3 H 0.2056 1.0531 0.8394 0.060 Uiso 1 1 calc R . . C19 C 0.9629(5) 0.7433(4) 0.71253(16) 0.0306(14) Uani 1 1 d . . . H19 H 1.0238 0.6938 0.7088 0.037 Uiso 1 1 calc R . . C2 C 0.3657(6) 1.0326(4) 0.80767(18) 0.0387(15) Uani 1 1 d . . . C22 C 1.0564(5) 0.6554(4) 0.79263(18) 0.0350(15) Uani 1 1 d . . . H22 H 1.1004 0.6237 0.7711 0.042 Uiso 1 1 calc R . . C9 C 0.2657(7) 0.8682(5) 0.80051(19) 0.0551(18) Uani 1 1 d . . . H9A H 0.3320 0.8366 0.8163 0.083 Uiso 1 1 calc R . . H9B H 0.2326 0.8218 0.7803 0.083 Uiso 1 1 calc R . . H9C H 0.1995 0.8885 0.8193 0.083 Uiso 1 1 calc R . . C6 C 0.5349(5) 1.1423(5) 0.83236(18) 0.0416(16) Uani 1 1 d . . . N1 N 0.5692(5) 1.0338(3) 0.77286(14) 0.0376(12) Uani 1 1 d . . . C5 C 0.4550(6) 1.1794(5) 0.8615(2) 0.0488(18) Uani 1 1 d . . . H5 H 0.4828 1.2295 0.8796 0.059 Uiso 1 1 calc R . . C36 C 0.6377(5) 0.8899(4) 0.90991(16) 0.0378(15) Uani 1 1 d D . . C8 C 0.2196(6) 1.0049(5) 0.74985(19) 0.0505(18) Uani 1 1 d . . . H8A H 0.1495 1.0276 0.7665 0.076 Uiso 1 1 calc R . . H8B H 0.1908 0.9559 0.7299 0.076 Uiso 1 1 calc R . . H8C H 0.2560 1.0606 0.7351 0.076 Uiso 1 1 calc R . . N6 N 0.7102(4) 0.8931(3) 0.87118(13) 0.0337(12) Uani 1 1 d . C . C14 C 0.5507(6) 1.0630(5) 0.73209(18) 0.0458(18) Uani 1 1 d . . . H14 H 0.4906 1.1085 0.7225 0.055 Uiso 1 1 calc R . . C1 C 0.4878(6) 1.0701(5) 0.80615(18) 0.0380(16) Uani 1 1 d . . . C12 C 0.7353(8) 1.1872(6) 0.8678(2) 0.070(2) Uani 1 1 d . . . H12A H 0.6938 1.2309 0.8873 0.106 Uiso 1 1 calc R . . H12B H 0.8188 1.2119 0.8621 0.106 Uiso 1 1 calc R . . H12C H 0.7408 1.1211 0.8796 0.106 Uiso 1 1 calc R . . C17 C 0.8233(5) 0.8615(5) 0.68519(17) 0.0394(15) Uani 1 1 d . . . H17 H 0.7874 0.8949 0.6624 0.047 Uiso 1 1 calc R . . C4 C 0.3321(6) 1.1442(5) 0.8650(2) 0.0526(19) Uani 1 1 d . . . H4 H 0.2792 1.1687 0.8860 0.063 Uiso 1 1 calc R . . C20 C 0.9239(5) 0.7721(4) 0.75149(17) 0.0312(14) Uani 1 1 d . . . C23 C 1.0665(5) 0.6386(5) 0.83264(17) 0.0406(16) Uani 1 1 d . . . H23 H 1.1206 0.5927 0.8453 0.049 Uiso 1 1 calc R . . C24 C 0.9533(6) 0.6925(5) 0.89623(19) 0.0464(18) Uani 1 1 d . A . C10 C 0.6620(6) 1.1834(5) 0.8280(2) 0.0464(17) Uani 1 1 d . . . H10 H 0.7077 1.1373 0.8094 0.056 Uiso 1 1 calc R . . C16 C 0.7897(5) 0.8842(5) 0.72537(16) 0.0338(14) Uani 1 1 d . . . C13 C 0.6580(5) 0.9656(4) 0.77673(17) 0.0339(14) Uani 1 1 d . . . C25 C 0.8820(7) 0.6136(5) 0.90970(19) 0.0520(19) Uani 1 1 d . . . C21 C 0.9182(5) 0.7587(4) 0.82664(17) 0.0348(14) Uani 1 1 d . . . C33A C 1.0892(7) 0.8480(6) 0.9087(3) 0.077(2) Uani 0.442(9) 1 d PDU A 1 H33A H 1.0653 0.8719 0.8807 0.092 Uiso 0.442(9) 1 calc PR A 1 C35A C 1.2157(13) 0.7895(14) 0.9091(6) 0.078(3) Uani 0.442(9) 1 d PDU A 1 H35A H 1.2748 0.8215 0.8906 0.116 Uiso 0.442(9) 1 calc PR A 1 H35B H 1.2013 0.7220 0.8999 0.116 Uiso 0.442(9) 1 calc PR A 1 H35C H 1.2493 0.7887 0.9372 0.116 Uiso 0.442(9) 1 calc PR A 1 C34A C 1.109(2) 0.9302(12) 0.9396(5) 0.085(4) Uani 0.442(9) 1 d PDU A 1 H34A H 1.0372 0.9741 0.9394 0.128 Uiso 0.442(9) 1 calc PR A 1 H34B H 1.1835 0.9674 0.9321 0.128 Uiso 0.442(9) 1 calc PR A 1 H34C H 1.1195 0.9024 0.9673 0.128 Uiso 0.442(9) 1 calc PR A 1 C33B C 1.0892(7) 0.8480(6) 0.9087(3) 0.077(2) Uani 0.558(9) 1 d PU A 2 C35B C 1.2209(10) 0.8696(13) 0.9226(4) 0.078(3) Uani 0.558(9) 1 d PDU A 2 H35D H 1.2242 0.8711 0.9528 0.116 Uiso 0.558(9) 1 calc PR A 2 H35E H 1.2469 0.9333 0.9117 0.116 Uiso 0.558(9) 1 calc PR A 2 H35F H 1.2764 0.8183 0.9123 0.116 Uiso 0.558(9) 1 calc PR A 2 C34B C 1.0255(16) 0.9468(9) 0.9226(5) 0.085(4) Uani 0.558(9) 1 d PDU A 2 H34D H 1.0163 0.9474 0.9526 0.128 Uiso 0.558(9) 1 calc PR A 2 H34E H 0.9438 0.9520 0.9096 0.128 Uiso 0.558(9) 1 calc PR A 2 H34F H 1.0769 1.0025 0.9140 0.128 Uiso 0.558(9) 1 calc PR A 2 C28 C 0.9873(8) 0.7416(8) 0.9658(2) 0.086(3) Uani 1 1 d . A . H28 H 1.0211 0.7841 0.9861 0.104 Uiso 1 1 calc R . . C15 C 0.6326(6) 1.0153(5) 0.7093(2) 0.0485(18) Uani 1 1 d . . . H15 H 0.6445 1.0213 0.6804 0.058 Uiso 1 1 calc R . . C27 C 0.9186(9) 0.6624(7) 0.9782(2) 0.080(3) Uani 1 1 d . . . H27 H 0.9076 0.6503 1.0068 0.097 Uiso 1 1 calc R B . C29 C 1.0090(6) 0.7616(6) 0.9240(2) 0.056(2) Uani 1 1 d . . . C26 C 0.8667(8) 0.6018(6) 0.9508(2) 0.069(2) Uani 1 1 d . B . H26 H 0.8175 0.5488 0.9605 0.083 Uiso 1 1 calc R . . C30A C 0.8280(7) 0.5398(6) 0.8790(3) 0.071(2) Uani 0.46(3) 1 d PDU B 3 H30A H 0.8388 0.5751 0.8522 0.085 Uiso 0.46(3) 1 calc PR B 3 C31A C 0.6868(12) 0.526(4) 0.8807(11) 0.093(4) Uani 0.46(3) 1 d PDU B 3 H31A H 0.6614 0.5131 0.9092 0.139 Uiso 0.46(3) 1 calc PR B 3 H31B H 0.6630 0.4705 0.8633 0.139 Uiso 0.46(3) 1 calc PR B 3 H31C H 0.6459 0.5857 0.8708 0.139 Uiso 0.46(3) 1 calc PR B 3 C32A C 0.878(2) 0.4382(9) 0.8687(9) 0.068(3) Uani 0.46(3) 1 d PDU B 3 H32A H 0.9653 0.4432 0.8611 0.101 Uiso 0.46(3) 1 calc PR B 3 H32B H 0.8308 0.4108 0.8456 0.101 Uiso 0.46(3) 1 calc PR B 3 H32C H 0.8691 0.3953 0.8928 0.101 Uiso 0.46(3) 1 calc PR B 3 C30B C 0.8280(7) 0.5398(6) 0.8790(3) 0.071(2) Uani 0.54(3) 1 d PU B 4 C31B C 0.6902(11) 0.528(4) 0.8893(9) 0.093(4) Uani 0.54(3) 1 d PDU B 4 H31D H 0.6780 0.4675 0.9051 0.139 Uiso 0.54(3) 1 calc PR B 4 H31E H 0.6424 0.5244 0.8636 0.139 Uiso 0.54(3) 1 calc PR B 4 H31F H 0.6622 0.5842 0.9056 0.139 Uiso 0.54(3) 1 calc PR B 4 C32B C 0.9031(15) 0.4446(10) 0.8881(8) 0.068(3) Uani 0.54(3) 1 d PDU B 4 H32D H 0.9491 0.4252 0.8634 0.101 Uiso 0.54(3) 1 calc PR B 4 H32E H 0.8462 0.3919 0.8960 0.101 Uiso 0.54(3) 1 calc PR B 4 H32F H 0.9614 0.4569 0.9107 0.101 Uiso 0.54(3) 1 calc PR B 4 C11 C 0.6562(8) 1.2810(6) 0.8051(2) 0.079(3) Uani 1 1 d . . . H11A H 0.6100 1.2726 0.7793 0.119 Uiso 1 1 calc R . . H11B H 0.7404 1.3033 0.7989 0.119 Uiso 1 1 calc R . . H11C H 0.6146 1.3299 0.8224 0.119 Uiso 1 1 calc R . . C18 C 0.9083(5) 0.7905(5) 0.67964(18) 0.0371(15) Uani 1 1 d . . . H18 H 0.9313 0.7726 0.6524 0.045 Uiso 1 1 calc R . . C37A C 0.5277(8) 0.9602(7) 0.9080(3) 0.053(2) Uani 0.723(6) 1 d PDU C 5 H37A H 0.5577 1.0280 0.9091 0.079 Uiso 0.723(6) 1 calc PR C 5 H37B H 0.4725 0.9479 0.9313 0.079 Uiso 0.723(6) 1 calc PR C 5 H37C H 0.4825 0.9499 0.8821 0.079 Uiso 0.723(6) 1 calc PR C 5 C39A C 0.5938(9) 0.7828(6) 0.9162(3) 0.056(3) Uani 0.723(6) 1 d PDU C 5 H39A H 0.5424 0.7629 0.8928 0.085 Uiso 0.723(6) 1 calc PR C 5 H39B H 0.5454 0.7784 0.9417 0.085 Uiso 0.723(6) 1 calc PR C 5 H39C H 0.6660 0.7395 0.9181 0.085 Uiso 0.723(6) 1 calc PR C 5 C38A C 0.7215(10) 0.9186(9) 0.9465(2) 0.067(3) Uani 0.723(6) 1 d PDU C 5 H38A H 0.7956 0.8771 0.9465 0.100 Uiso 0.723(6) 1 calc PR C 5 H38B H 0.6761 0.9094 0.9724 0.100 Uiso 0.723(6) 1 calc PR C 5 H38C H 0.7460 0.9875 0.9438 0.100 Uiso 0.723(6) 1 calc PR C 5 C37B C 0.5029(11) 0.879(2) 0.8950(6) 0.053(2) Uani 0.277(6) 1 d PDU C 6 H37D H 0.4858 0.9273 0.8735 0.079 Uiso 0.277(6) 1 calc PR C 6 H37E H 0.4464 0.8888 0.9182 0.079 Uiso 0.277(6) 1 calc PR C 6 H37F H 0.4909 0.8125 0.8838 0.079 Uiso 0.277(6) 1 calc PR C 6 C39B C 0.700(2) 0.8192(17) 0.9406(6) 0.056(3) Uani 0.277(6) 1 d PDU C 6 H39D H 0.7737 0.8507 0.9523 0.085 Uiso 0.277(6) 1 calc PR C 6 H39E H 0.7245 0.7590 0.9262 0.085 Uiso 0.277(6) 1 calc PR C 6 H39F H 0.6419 0.8031 0.9627 0.085 Uiso 0.277(6) 1 calc PR C 6 C38B C 0.653(3) 0.9865(13) 0.9336(7) 0.067(3) Uani 0.277(6) 1 d PD C 6 H38D H 0.7397 0.9933 0.9424 0.100 Uiso 0.277(6) 1 calc PR C 6 H38E H 0.5993 0.9863 0.9578 0.100 Uiso 0.277(6) 1 calc PR C 6 H38F H 0.6312 1.0416 0.9157 0.100 Uiso 0.277(6) 1 calc PR C 6 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 Ti1 0.0231(5) 0.0291(5) 0.0286(5) 0.0013(5) -0.0004(4) 0.0003(5) Cl2 0.0386(9) 0.0451(10) 0.0643(11) -0.0148(9) 0.0064(8) -0.0168(8) Cl1 0.0305(8) 0.0382(8) 0.0599(10) -0.0012(8) 0.0085(8) -0.0061(7) C7 0.030(4) 0.045(4) 0.043(4) 0.003(3) -0.006(3) 0.006(3) N4 0.019(3) 0.033(3) 0.031(3) 0.002(2) 0.000(2) -0.001(2) N3 0.024(3) 0.032(3) 0.027(2) -0.003(2) -0.005(2) 0.002(2) N5 0.040(3) 0.041(3) 0.040(3) 0.002(3) -0.008(2) 0.011(3) N2 0.035(3) 0.041(3) 0.030(3) 0.014(2) -0.001(2) 0.006(3) C3 0.027(4) 0.071(5) 0.051(4) -0.004(4) -0.008(3) 0.010(3) C19 0.034(4) 0.030(3) 0.028(3) -0.008(3) 0.003(3) 0.002(3) C2 0.039(4) 0.039(4) 0.038(3) 0.005(3) 0.005(3) 0.013(3) C22 0.023(3) 0.037(3) 0.045(4) 0.001(3) -0.005(3) 0.010(3) C9 0.051(4) 0.058(4) 0.056(4) -0.003(4) 0.001(4) 0.005(4) C6 0.029(3) 0.051(4) 0.044(4) -0.006(3) -0.003(3) 0.014(3) N1 0.034(3) 0.038(3) 0.040(3) 0.000(2) 0.000(2) 0.011(3) C5 0.038(4) 0.055(4) 0.054(4) -0.015(4) 0.000(3) 0.002(4) C36 0.037(4) 0.043(4) 0.034(3) -0.002(3) 0.008(3) 0.011(3) C8 0.048(4) 0.054(4) 0.050(4) -0.007(4) 0.003(3) 0.005(4) N6 0.036(3) 0.033(3) 0.032(2) 0.005(2) -0.003(2) -0.003(2) C14 0.041(4) 0.055(4) 0.041(4) 0.018(3) -0.006(3) 0.013(4) C1 0.050(4) 0.035(3) 0.029(3) 0.003(3) 0.011(3) 0.006(3) C12 0.066(6) 0.079(6) 0.066(5) 0.001(4) 0.010(5) -0.013(5) C17 0.030(3) 0.054(4) 0.034(3) 0.015(3) -0.005(3) 0.010(3) C4 0.039(4) 0.054(5) 0.064(4) -0.021(4) 0.003(3) 0.027(4) C20 0.023(3) 0.026(3) 0.045(4) 0.005(3) 0.005(3) -0.003(3) C23 0.030(3) 0.047(4) 0.045(4) 0.013(3) 0.003(3) 0.014(3) C24 0.038(4) 0.062(5) 0.039(4) 0.003(4) -0.011(3) 0.018(4) C10 0.045(4) 0.042(4) 0.052(4) -0.007(3) 0.017(4) -0.010(3) C16 0.028(3) 0.045(4) 0.028(3) 0.003(3) -0.003(3) 0.001(3) C13 0.030(4) 0.041(4) 0.030(3) 0.002(3) -0.005(3) 0.003(3) C25 0.076(5) 0.035(4) 0.046(4) 0.018(3) 0.013(4) 0.019(4) C21 0.027(3) 0.045(4) 0.033(3) -0.005(3) 0.004(3) -0.005(3) C33A 0.077(2) 0.077(2) 0.077(2) 0.0002(7) 0.0002(7) -0.0006(7) C35A 0.078(4) 0.078(4) 0.078(3) 0.0001(7) -0.0003(7) -0.0002(7) C34A 0.085(4) 0.085(4) 0.085(4) 0.0000(7) 0.0000(7) -0.0002(7) C33B 0.077(2) 0.077(2) 0.077(2) 0.0002(7) 0.0002(7) -0.0006(7) C35B 0.078(4) 0.078(4) 0.078(3) 0.0001(7) -0.0003(7) -0.0002(7) C34B 0.085(4) 0.085(4) 0.085(4) 0.0000(7) 0.0000(7) -0.0002(7) C28 0.066(6) 0.158(10) 0.035(4) 0.004(6) -0.014(4) 0.020(7) C15 0.043(4) 0.060(5) 0.042(4) 0.016(4) 0.013(3) 0.016(4) C27 0.107(8) 0.089(7) 0.046(5) 0.048(5) 0.010(5) 0.005(6) C29 0.033(4) 0.095(6) 0.041(4) -0.002(4) -0.005(3) 0.009(4) C26 0.104(7) 0.054(5) 0.050(5) 0.012(4) 0.012(5) 0.026(5) C30A 0.071(2) 0.071(2) 0.071(2) 0.0000(7) 0.0008(7) -0.0002(7) C31A 0.093(4) 0.093(4) 0.093(4) 0.0001(7) 0.0000(7) -0.0001(7) C32A 0.068(4) 0.068(3) 0.068(4) -0.0003(7) 0.0002(7) -0.0002(7) C30B 0.071(2) 0.071(2) 0.071(2) 0.0000(7) 0.0008(7) -0.0002(7) C31B 0.093(4) 0.093(4) 0.093(4) 0.0001(7) 0.0000(7) -0.0001(7) C32B 0.068(4) 0.068(3) 0.068(4) -0.0003(7) 0.0002(7) -0.0002(7) C11 0.099(7) 0.064(5) 0.074(5) 0.013(5) -0.002(5) -0.014(5) C18 0.027(3) 0.057(4) 0.028(3) -0.011(3) 0.009(3) -0.001(3) C37A 0.053(4) 0.056(4) 0.049(4) 0.007(4) 0.027(4) 0.006(4) C39A 0.063(5) 0.053(5) 0.053(5) 0.005(4) 0.023(4) 0.004(4) C38A 0.078(7) 0.081(7) 0.040(5) -0.004(5) -0.002(5) -0.015(5) C37B 0.053(4) 0.056(4) 0.049(4) 0.007(4) 0.027(4) 0.006(4) C39B 0.063(5) 0.053(5) 0.053(5) 0.005(4) 0.023(4) 0.004(4) C38B 0.078(7) 0.081(7) 0.040(5) -0.004(5) -0.002(5) -0.015(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 Ti1 N6 1.677(5) . ? Ti1 C13 2.281(6) . ? Ti1 C21 2.286(6) . ? Ti1 N3 2.332(5) . ? Ti1 Cl2 2.415(2) . ? Ti1 Cl1 2.433(2) . ? C7 C2 1.486(9) . ? C7 C9 1.535(9) . ? C7 C8 1.536(8) . ? C7 H7 1.0000 . ? N4 C22 1.398(7) . ? N4 C21 1.406(7) . ? N4 C20 1.416(7) . ? N3 C20 1.316(7) . ? N3 C16 1.320(7) . ? N5 C21 1.356(7) . ? N5 C23 1.403(7) . ? N5 C24 1.444(8) . ? N2 C13 1.389(7) . ? N2 C15 1.405(7) . ? N2 C16 1.416(7) . ? C3 C4 1.385(9) . ? C3 C2 1.394(9) . ? C3 H3 0.9500 . ? C19 C18 1.379(8) . ? C19 C20 1.390(7) . ? C19 H19 0.9500 . ? C2 C1 1.416(9) . ? C22 C23 1.323(7) . ? C22 H22 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C6 C5 1.376(8) . ? C6 C1 1.397(8) . ? C6 C10 1.490(8) . ? N1 C13 1.342(7) . ? N1 C14 1.396(7) . ? N1 C1 1.477(7) . ? C5 C4 1.416(9) . ? C5 H5 0.9500 . ? C36 N6 1.481(7) . ? C36 C37A 1.528(7) . ? C36 C38B 1.534(10) . ? C36 C39B 1.540(10) . ? C36 C37B 1.541(10) . ? C36 C38A 1.543(8) . ? C36 C39A 1.547(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C14 C15 1.324(9) . ? C14 H14 0.9500 . ? C12 C10 1.516(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C17 C18 1.347(8) . ? C17 C16 1.388(8) . ? C17 H17 0.9500 . ? C4 H4 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.394(9) . ? C24 C29 1.435(10) . ? C10 C11 1.525(9) . ? C10 H10 1.0000 . ? C25 C26 1.355(9) . ? C25 C30A 1.530(10) . ? C33A C34A 1.520(9) . ? C33A C29 1.544(11) . ? C33A C35A 1.581(9) . ? C33A H33A 1.0000 . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C28 C27 1.370(12) . ? C28 C29 1.404(9) . ? C28 H28 0.9500 . ? C15 H15 0.9500 . ? C27 C26 1.336(11) . ? C27 H27 0.9500 . ? C26 H26 0.9500 . ? C30A C32A 1.523(9) . ? C30A C31A 1.538(10) . ? C30A H30A 1.0000 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C18 H18 0.9500 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C39B H39D 0.9800 . ? C39B H39E 0.9800 . ? C39B H39F 0.9800 . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 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 N6 Ti1 C13 110.5(2) . . ? N6 Ti1 C21 108.7(2) . . ? C13 Ti1 C21 140.5(2) . . ? N6 Ti1 N3 175.3(2) . . ? C13 Ti1 N3 70.82(19) . . ? C21 Ti1 N3 69.77(18) . . ? N6 Ti1 Cl2 95.56(17) . . ? C13 Ti1 Cl2 85.62(17) . . ? C21 Ti1 Cl2 85.59(17) . . ? N3 Ti1 Cl2 79.99(12) . . ? N6 Ti1 Cl1 102.99(17) . . ? C13 Ti1 Cl1 86.82(17) . . ? C21 Ti1 Cl1 89.53(16) . . ? N3 Ti1 Cl1 81.49(12) . . ? Cl2 Ti1 Cl1 161.42(7) . . ? C2 C7 C9 111.5(5) . . ? C2 C7 C8 110.3(5) . . ? C9 C7 C8 111.2(6) . . ? C2 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C22 N4 C21 112.4(5) . . ? C22 N4 C20 127.4(5) . . ? C21 N4 C20 120.2(5) . . ? C20 N3 C16 118.9(5) . . ? C20 N3 Ti1 121.2(4) . . ? C16 N3 Ti1 119.8(4) . . ? C21 N5 C23 112.8(5) . . ? C21 N5 C24 123.0(5) . . ? C23 N5 C24 123.5(5) . . ? C13 N2 C15 111.3(5) . . ? C13 N2 C16 122.2(5) . . ? C15 N2 C16 126.4(5) . . ? C4 C3 C2 121.9(7) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C18 C19 C20 116.2(5) . . ? C18 C19 H19 121.9 . . ? C20 C19 H19 121.9 . . ? C3 C2 C1 115.5(6) . . ? C3 C2 C7 121.1(6) . . ? C1 C2 C7 123.3(6) . . ? C23 C22 N4 106.0(5) . . ? C23 C22 H22 127.0 . . ? N4 C22 H22 127.0 . . ? 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 . . ? C5 C6 C1 116.7(6) . . ? C5 C6 C10 120.4(6) . . ? C1 C6 C10 122.8(6) . . ? C13 N1 C14 112.8(5) . . ? C13 N1 C1 126.1(5) . . ? C14 N1 C1 120.8(5) . . ? C6 C5 C4 121.2(6) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? N6 C36 C37A 110.9(5) . . ? N6 C36 C38B 110.0(11) . . ? C37A C36 C38B 64.4(12) . . ? N6 C36 C39B 109.6(10) . . ? C37A C36 C39B 139.4(11) . . ? C38B C36 C39B 99.5(15) . . ? N6 C36 C37B 103.7(9) . . ? C37A C36 C37B 46.8(10) . . ? C38B C36 C37B 110.3(16) . . ? C39B C36 C37B 123.6(15) . . ? N6 C36 C38A 109.6(6) . . ? C37A C36 C38A 109.2(7) . . ? C38B C36 C38A 48.1(11) . . ? C39B C36 C38A 53.5(11) . . ? C37B C36 C38A 145.1(10) . . ? N6 C36 C39A 107.5(5) . . ? C37A C36 C39A 111.0(6) . . ? C38B C36 C39A 141.0(11) . . ? C39B C36 C39A 57.3(11) . . ? C37B C36 C39A 70.0(11) . . ? C38A C36 C39A 108.5(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 . . ? C36 N6 Ti1 166.1(4) . . ? C15 C14 N1 107.1(6) . . ? C15 C14 H14 126.4 . . ? N1 C14 H14 126.4 . . ? C6 C1 C2 124.9(6) . . ? C6 C1 N1 117.7(6) . . ? C2 C1 N1 117.3(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 . . ? C18 C17 C16 117.6(5) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C3 C4 C5 119.7(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N3 C20 C19 123.2(5) . . ? N3 C20 N4 113.2(5) . . ? C19 C20 N4 123.6(5) . . ? C22 C23 N5 107.7(5) . . ? C22 C23 H23 126.2 . . ? N5 C23 H23 126.2 . . ? C25 C24 C29 122.8(6) . . ? C25 C24 N5 119.2(6) . . ? C29 C24 N5 117.8(6) . . ? C6 C10 C12 114.4(6) . . ? C6 C10 C11 109.7(6) . . ? C12 C10 C11 114.0(6) . . ? C6 C10 H10 106.0 . . ? C12 C10 H10 106.0 . . ? C11 C10 H10 106.0 . . ? N3 C16 C17 122.5(5) . . ? N3 C16 N2 112.9(5) . . ? C17 C16 N2 124.6(5) . . ? N1 C13 N2 102.4(5) . . ? N1 C13 Ti1 143.4(4) . . ? N2 C13 Ti1 114.0(4) . . ? C26 C25 C24 117.9(7) . . ? C26 C25 C30A 121.1(7) . . ? C24 C25 C30A 120.9(6) . . ? N5 C21 N4 101.2(5) . . ? N5 C21 Ti1 143.2(4) . . ? N4 C21 Ti1 115.6(4) . . ? C34A C33A C29 115.5(10) . . ? C34A C33A C35A 104.2(12) . . ? C29 C33A C35A 95.6(9) . . ? C34A C33A H33A 113.3 . . ? C29 C33A H33A 113.3 . . ? C35A C33A H33A 113.3 . . ? H35D C35B H35E 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? H34D C34B H34E 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C27 C28 C29 121.7(9) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C14 C15 N2 106.3(6) . . ? C14 C15 H15 126.9 . . ? N2 C15 H15 126.9 . . ? C26 C27 C28 121.3(7) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C28 C29 C24 114.2(8) . . ? C28 C29 C33A 123.5(8) . . ? C24 C29 C33A 122.3(6) . . ? C27 C26 C25 122.0(8) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C32A C30A C25 127.3(13) . . ? C32A C30A C31A 104(3) . . ? C25 C30A C31A 116(2) . . ? C32A C30A H30A 101.8 . . ? C25 C30A H30A 101.8 . . ? C31A C30A H30A 101.8 . . ? 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 . . ? C17 C18 C19 121.6(5) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C36 C37A H37A 109.5 . . ? C36 C37A H37B 109.5 . . ? C36 C37A H37C 109.5 . . ? C36 C39A H39A 109.5 . . ? C36 C39A H39B 109.5 . . ? C36 C39A H39C 109.5 . . ? C36 C38A H38A 109.5 . . ? C36 C38A H38B 109.5 . . ? C36 C38A H38C 109.5 . . ? C36 C37B H37D 109.5 . . ? C36 C37B H37E 109.5 . . ? C36 C37B H37F 109.5 . . ? C36 C39B H39D 109.5 . . ? C36 C39B H39E 109.5 . . ? C36 C39B H39F 109.5 . . ? C36 C38B H38D 109.5 . . ? C36 C38B H38E 109.5 . . ? C36 C38B H38F 109.5 . . ? 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 N6 Ti1 N3 C20 -69(3) . . . . ? C13 Ti1 N3 C20 -175.8(5) . . . . ? C21 Ti1 N3 C20 2.0(4) . . . . ? Cl2 Ti1 N3 C20 -86.9(4) . . . . ? Cl1 Ti1 N3 C20 94.7(4) . . . . ? N6 Ti1 N3 C16 107(2) . . . . ? C13 Ti1 N3 C16 0.7(4) . . . . ? C21 Ti1 N3 C16 178.4(5) . . . . ? Cl2 Ti1 N3 C16 89.5(4) . . . . ? Cl1 Ti1 N3 C16 -88.9(4) . . . . ? C4 C3 C2 C1 -2.2(9) . . . . ? C4 C3 C2 C7 -178.9(6) . . . . ? C9 C7 C2 C3 -58.9(8) . . . . ? C8 C7 C2 C3 65.3(7) . . . . ? C9 C7 C2 C1 124.8(6) . . . . ? C8 C7 C2 C1 -111.0(7) . . . . ? C21 N4 C22 C23 -1.5(7) . . . . ? C20 N4 C22 C23 -179.4(5) . . . . ? C1 C6 C5 C4 1.2(9) . . . . ? C10 C6 C5 C4 177.3(6) . . . . ? C37A C36 N6 Ti1 -86.9(17) . . . . ? C38B C36 N6 Ti1 -156.2(19) . . . . ? C39B C36 N6 Ti1 95(2) . . . . ? C37B C36 N6 Ti1 -38(2) . . . . ? C38A C36 N6 Ti1 152.5(15) . . . . ? C39A C36 N6 Ti1 34.7(18) . . . . ? C13 Ti1 N6 C36 82.2(16) . . . . ? C21 Ti1 N6 C36 -92.4(16) . . . . ? N3 Ti1 N6 C36 -23(4) . . . . ? Cl2 Ti1 N6 C36 -5.2(16) . . . . ? Cl1 Ti1 N6 C36 173.6(16) . . . . ? C13 N1 C14 C15 -2.4(8) . . . . ? C1 N1 C14 C15 -176.9(6) . . . . ? C5 C6 C1 C2 -0.4(9) . . . . ? C10 C6 C1 C2 -176.4(6) . . . . ? C5 C6 C1 N1 176.1(5) . . . . ? C10 C6 C1 N1 0.1(9) . . . . ? C3 C2 C1 C6 0.9(9) . . . . ? C7 C2 C1 C6 177.4(5) . . . . ? C3 C2 C1 N1 -175.6(5) . . . . ? C7 C2 C1 N1 1.0(9) . . . . ? C13 N1 C1 C6 81.8(7) . . . . ? C14 N1 C1 C6 -104.5(7) . . . . ? C13 N1 C1 C2 -101.5(7) . . . . ? C14 N1 C1 C2 72.2(7) . . . . ? C2 C3 C4 C5 3.1(10) . . . . ? C6 C5 C4 C3 -2.5(10) . . . . ? C16 N3 C20 C19 -1.2(8) . . . . ? Ti1 N3 C20 C19 175.3(4) . . . . ? C16 N3 C20 N4 -179.1(5) . . . . ? Ti1 N3 C20 N4 -2.6(6) . . . . ? C18 C19 C20 N3 0.5(8) . . . . ? C18 C19 C20 N4 178.2(5) . . . . ? C22 N4 C20 N3 179.5(5) . . . . ? C21 N4 C20 N3 1.7(7) . . . . ? C22 N4 C20 C19 1.6(9) . . . . ? C21 N4 C20 C19 -176.2(5) . . . . ? N4 C22 C23 N5 1.0(7) . . . . ? C21 N5 C23 C22 -0.3(7) . . . . ? C24 N5 C23 C22 169.8(6) . . . . ? C21 N5 C24 C25 97.5(8) . . . . ? C23 N5 C24 C25 -71.5(8) . . . . ? C21 N5 C24 C29 -88.1(8) . . . . ? C23 N5 C24 C29 102.9(7) . . . . ? C5 C6 C10 C12 52.4(9) . . . . ? C1 C6 C10 C12 -131.7(7) . . . . ? C5 C6 C10 C11 -77.0(8) . . . . ? C1 C6 C10 C11 98.8(7) . . . . ? C20 N3 C16 C17 0.5(8) . . . . ? Ti1 N3 C16 C17 -176.0(4) . . . . ? C20 N3 C16 N2 178.8(5) . . . . ? Ti1 N3 C16 N2 2.3(6) . . . . ? C18 C17 C16 N3 0.9(9) . . . . ? C18 C17 C16 N2 -177.3(5) . . . . ? C13 N2 C16 N3 -6.1(8) . . . . ? C15 N2 C16 N3 177.5(6) . . . . ? C13 N2 C16 C17 172.2(6) . . . . ? C15 N2 C16 C17 -4.2(10) . . . . ? C14 N1 C13 N2 1.5(6) . . . . ? C1 N1 C13 N2 175.6(5) . . . . ? C14 N1 C13 Ti1 175.8(6) . . . . ? C1 N1 C13 Ti1 -10.1(11) . . . . ? C15 N2 C13 N1 -0.1(7) . . . . ? C16 N2 C13 N1 -177.0(5) . . . . ? C15 N2 C13 Ti1 -176.4(4) . . . . ? C16 N2 C13 Ti1 6.7(7) . . . . ? N6 Ti1 C13 N1 7.2(8) . . . . ? C21 Ti1 C13 N1 179.2(6) . . . . ? N3 Ti1 C13 N1 -177.5(8) . . . . ? Cl2 Ti1 C13 N1 101.6(7) . . . . ? Cl1 Ti1 C13 N1 -95.4(7) . . . . ? N6 Ti1 C13 N2 -178.8(4) . . . . ? C21 Ti1 C13 N2 -6.9(6) . . . . ? N3 Ti1 C13 N2 -3.6(4) . . . . ? Cl2 Ti1 C13 N2 -84.5(4) . . . . ? Cl1 Ti1 C13 N2 78.5(4) . . . . ? C29 C24 C25 C26 -0.9(10) . . . . ? N5 C24 C25 C26 173.1(6) . . . . ? C29 C24 C25 C30A -178.0(6) . . . . ? N5 C24 C25 C30A -3.9(9) . . . . ? C23 N5 C21 N4 -0.6(6) . . . . ? C24 N5 C21 N4 -170.7(6) . . . . ? C23 N5 C21 Ti1 178.4(5) . . . . ? C24 N5 C21 Ti1 8.3(11) . . . . ? C22 N4 C21 N5 1.2(6) . . . . ? C20 N4 C21 N5 179.3(5) . . . . ? C22 N4 C21 Ti1 -178.1(3) . . . . ? C20 N4 C21 Ti1 0.0(6) . . . . ? N6 Ti1 C21 N5 -4.5(8) . . . . ? C13 Ti1 C21 N5 -176.5(6) . . . . ? N3 Ti1 C21 N5 -179.8(8) . . . . ? Cl2 Ti1 C21 N5 -98.9(7) . . . . ? Cl1 Ti1 C21 N5 99.0(7) . . . . ? N6 Ti1 C21 N4 174.4(4) . . . . ? C13 Ti1 C21 N4 2.4(6) . . . . ? N3 Ti1 C21 N4 -0.9(4) . . . . ? Cl2 Ti1 C21 N4 80.0(4) . . . . ? Cl1 Ti1 C21 N4 -82.0(4) . . . . ? N1 C14 C15 N2 2.1(8) . . . . ? C13 N2 C15 C14 -1.3(8) . . . . ? C16 N2 C15 C14 175.4(6) . . . . ? C29 C28 C27 C26 -1.6(13) . . . . ? C27 C28 C29 C24 0.0(11) . . . . ? C27 C28 C29 C33A -177.9(8) . . . . ? C25 C24 C29 C28 1.2(10) . . . . ? N5 C24 C29 C28 -172.9(6) . . . . ? C25 C24 C29 C33A 179.2(6) . . . . ? N5 C24 C29 C33A 5.1(10) . . . . ? C34A C33A C29 C28 -19.7(14) . . . . ? C35A C33A C29 C28 88.9(10) . . . . ? C34A C33A C29 C24 162.5(11) . . . . ? C35A C33A C29 C24 -88.9(10) . . . . ? C28 C27 C26 C25 2.0(14) . . . . ? C24 C25 C26 C27 -0.7(12) . . . . ? C30A C25 C26 C27 176.3(8) . . . . ? C26 C25 C30A C32A -76.3(14) . . . . ? C24 C25 C30A C32A 100.7(12) . . . . ? C26 C25 C30A C31A 59(2) . . . . ? C24 C25 C30A C31A -124(2) . . . . ? C16 C17 C18 C19 -1.5(9) . . . . ? C20 C19 C18 C17 0.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.414 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.079 #==END