Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' # SUBMISSION DETAILS _journal_coden_cambridge 0222 _audit_creation_method SHELXL _publ_contact_author ; Dr. James P. Donahue Department of Chemistry Tulane University 6400 Freret Street New Orleans, LA 70118-5698 ; _publ_contact_author_email donahue@tulane.edu _publ_contact_author_fax 504-865-5596 _publ_contact_author_phone 504-862-3562 _publ_contact_letter ; This CIF is being submitted with the request for a deposition number. The deposition number is required prior to the formal submission of the manuscript to the journal. ; # TITLE AND AUTHOR LIST _publ_section_title ; An Unusual Trigonal D~3~ Assembly Composed of Molybdate Anions and Multiply Bonded Dimolybdenum Units ; loop_ _publ_author_name _publ_author_address J.P.Donahue ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, LA 70118-5698 ; C.A.Murillo ; Department of Chemistry Texas A&M University PO Box 30012 College Station, TX 77842-3012 ; _publ_contact_author_name 'Dr. James P. Donahue' #################################################################### data_Manuscript _database_code_depnum_ccdc_archive 'CCDC 661903' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; [[[(H3 C O C6 H4 N)2 C H]3 Mo2]3 (Mo O4)2][P F6]2 . (C H2 Cl2)2 ; _chemical_formula_structural ; [[Mo2(DAniF)3]3(mu(3)-MoO4)2][PF6]2.2(CH2Cl2) ; _chemical_formula_analytical 'not measured' _chemical_formula_sum 'C137 H139 Cl4 F12 Mo8 N18 O26 P2' _chemical_formula_weight 3652.92 _chemical_melting_point 'not measured' _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.7246(14) _cell_length_b 18.0560(14) _cell_length_c 28.435(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.772(2) _cell_angle_gamma 90.00 _cell_volume 14740.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 9104 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method none _exptl_crystal_F_000 7348 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.928 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method omega-scans _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51271 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.53 _reflns_number_total 16673 _reflns_number_observed 12494 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V. 5.059' _computing_cell_refinement 'SAINT V. 6.02' _computing_data_reduction 'SAINT V. 6.02' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL V. 5.03 (Siemens, 1994)' _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+77.1929P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 16672 _refine_ls_number_parameters 935 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_obs 0.0450 _refine_ls_wR_factor_all 0.1140 _refine_ls_wR_factor_obs 0.0994 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max -0.059 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.040513(12) 0.38624(2) 0.365928(12) 0.02577(8) Uani 1 d . . Mo2 Mo -0.031397(12) 0.41708(2) 0.355733(12) 0.02516(8) Uani 1 d . . Mo3 Mo 0.034564(12) 0.09904(2) 0.236699(13) 0.02729(9) Uani 1 d . . Mo4 Mo 0.070640(11) 0.29926(2) 0.248781(12) 0.02304(8) Uani 1 d . . C70A C 0.2659(4) -0.2386(8) 0.2237(6) 0.065(3) Uani 0.541(4) d P 1 H70A H 0.2431(4) -0.2778(8) 0.2266(6) 0.078 Uiso 0.541(4) calc PR 1 H70B H 0.2949(4) -0.2569(8) 0.2377(6) 0.078 Uiso 0.541(4) calc PR 1 Cl1A Cl 0.2485(2) -0.1672(3) 0.2568(2) 0.114(2) Uani 0.541(4) d P 1 Cl2A Cl 0.2748(3) -0.2258(4) 0.1634(3) 0.133(2) Uani 0.541(4) d P 1 C70B C 0.2305(4) -0.2277(7) 0.1822(5) 0.065(3) Uani 0.459(4) d P 2 H70C H 0.2081(4) -0.1883(7) 0.1761(5) 0.078 Uiso 0.459(4) calc PR 2 H70D H 0.2132(4) -0.2738(7) 0.1834(5) 0.078 Uiso 0.459(4) calc PR 2 Cl1B Cl 0.2564(2) -0.2129(4) 0.2356(3) 0.114(2) Uani 0.459(4) d P 2 Cl2B Cl 0.2689(3) -0.2320(5) 0.1340(3) 0.133(2) Uani 0.459(4) d P 2 P1A P 0.0488(8) 0.2267(12) -0.0992(5) 0.059(2) Uani 0.559(4) d P 1 F1A F -0.0054(3) 0.2280(4) -0.0895(3) 0.0741(15) Uiso 0.559(4) d P 1 F2A F 0.0447(3) 0.1404(5) -0.1015(3) 0.092(2) Uiso 0.559(4) d P 1 F3A F 0.0490(3) 0.3152(4) -0.0989(3) 0.085(2) Uiso 0.559(4) d P 1 F4A F 0.0402(3) 0.2270(5) -0.1539(3) 0.112(2) Uiso 0.559(4) d P 1 F5A F 0.0556(4) 0.2201(6) -0.0425(4) 0.121(3) Uiso 0.559(4) d P 1 F6A F 0.1032(3) 0.2258(5) -0.1017(4) 0.115(2) Uiso 0.559(4) d P 1 P1B P 0.0520(10) 0.2321(16) -0.0875(7) 0.059(2) Uani 0.441(4) d P 2 F1B F -0.0029(3) 0.2344(6) -0.1088(3) 0.0741(15) Uiso 0.441(4) d P 2 F2B F 0.0653(4) 0.1573(6) -0.1164(4) 0.092(2) Uiso 0.441(4) d P 2 F3B F 0.0420(3) 0.3031(5) -0.0572(3) 0.085(2) Uiso 0.441(4) d P 2 F4B F 0.0618(4) 0.2797(7) -0.1326(4) 0.112(2) Uiso 0.441(4) d P 2 F5B F 0.0381(5) 0.1818(8) -0.0447(5) 0.121(3) Uiso 0.441(4) d P 2 F6B F 0.1006(4) 0.2344(7) -0.0675(5) 0.115(2) Uiso 0.441(4) d P 2 O1 O 0.05309(11) 0.3254(2) 0.30595(10) 0.0356(7) Uani 1 d . . O2 O 0.04989(12) 0.2093(2) 0.23328(11) 0.0430(8) Uani 1 d . . O3 O 0.05166(11) 0.3658(2) 0.20615(10) 0.0350(7) Uani 1 d . . O4 O 0.12955(11) 0.2960(2) 0.24958(13) 0.0500(9) Uani 1 d . . O5 O 0.16497(12) 0.1118(2) 0.47933(13) 0.0533(9) Uani 1 d . . O6 O -0.24126(11) 0.2726(2) 0.43689(13) 0.0515(9) Uani 1 d . . O7 O 0.23261(11) 0.5193(2) 0.46925(14) 0.0523(9) Uani 1 d . . O8 O -0.18732(12) 0.6584(2) 0.4381(2) 0.0694(12) Uani 1 d . . O9 O 0.25347(11) 0.5586(2) 0.32025(14) 0.0566(10) Uani 1 d . . O10 O -0.14513(12) 0.7182(2) 0.25214(14) 0.0540(9) Uani 1 d . . O11 O 0.24139(12) -0.0298(2) 0.33557(15) 0.0650(11) Uani 1 d . . O12 O 0.15811(14) -0.1194(2) 0.1006(2) 0.0715(13) Uani 1 d . . O13 O 0.13406(13) 0.0817(2) 0.01826(13) 0.0571(10) Uani 1 d . . N1 N 0.02240(12) 0.2896(2) 0.40335(12) 0.0298(7) Uani 1 d . . N2 N -0.05477(11) 0.3228(2) 0.39401(12) 0.0283(7) Uani 1 d . . N3 N 0.04670(12) 0.4512(2) 0.42732(11) 0.0291(7) Uani 1 d . . N4 N -0.02990(11) 0.4826(2) 0.41647(12) 0.0292(7) Uani 1 d . . N5 N 0.06511(12) 0.4820(2) 0.33095(12) 0.0298(7) Uani 1 d . . N6 N -0.01211(11) 0.5146(2) 0.31936(12) 0.0285(7) Uani 1 d . . N7 N 0.06403(12) 0.0910(2) 0.30581(12) 0.0319(8) Uani 1 d . . N8 N 0.03546(11) -0.0170(2) 0.23299(12) 0.0298(7) Uani 1 d . . N9 N 0.00999(12) 0.0975(2) 0.16519(12) 0.0310(8) Uani 1 d . . C1 C -0.02245(14) 0.2766(2) 0.41090(14) 0.0284(8) Uani 1 d . . H1A H -0.03108 0.2351 0.42800 0.034 Uiso 1 calc R . C2 C 0.05689(14) 0.2400(2) 0.42235(14) 0.0293(9) Uani 1 d . . C3 C 0.0545(2) 0.2089(3) 0.4664(2) 0.0372(10) Uani 1 d . . H3A H 0.0285 0.2173 0.4844 0.045 Uiso 1 calc R . C4 C 0.0910(2) 0.1648(3) 0.4842(2) 0.0454(12) Uani 1 d . . H4B H 0.0888 0.1429 0.5137 0.054 Uiso 1 calc R . C5 C 0.1304(2) 0.1534(3) 0.4582(2) 0.0390(10) Uani 1 d . . C6 C 0.1328(2) 0.1837(3) 0.4137(2) 0.0381(10) Uani 1 d . . H6A H 0.1588 0.1753 0.3956 0.046 Uiso 1 calc R . C7 C 0.09611(14) 0.2270(2) 0.3962(2) 0.0333(9) Uani 1 d . . H7A H 0.09788 0.2476 0.3663 0.040 Uiso 1 calc R . C8 C 0.2057(2) 0.0985(4) 0.4530(2) 0.064(2) Uani 1 d . . H8A H 0.2273 0.0689 0.4714 0.096 Uiso 1 calc R . H8B H 0.2200 0.1448 0.4454 0.096 Uiso 1 calc R . H8C H 0.1972 0.0726 0.4245 0.096 Uiso 1 calc R . C9 C -0.10243(14) 0.3087(2) 0.40486(14) 0.0289(8) Uani 1 d . . C10 C -0.1155(2) 0.2845(2) 0.4491(2) 0.0346(10) Uani 1 d . . H10A H -0.0929 0.2761 0.4725 0.041 Uiso 1 calc R . C11 C -0.1618(2) 0.2729(2) 0.4585(2) 0.0381(10) Uani 1 d . . H11A H -0.1700 0.2561 0.4881 0.046 Uiso 1 calc R . C12 C -0.1962(2) 0.2861(2) 0.4243(2) 0.0376(10) Uani 1 d . . C13 C -0.18402(15) 0.3115(3) 0.3806(2) 0.0374(10) Uani 1 d . . H13A H -0.20693 0.3213 0.3576 0.045 Uiso 1 calc R . C14 C -0.13707(14) 0.3223(2) 0.3711(2) 0.0325(9) Uani 1 d . . H14A H -0.12896 0.3390 0.3415 0.039 Uiso 1 calc R . C15 C -0.2778(2) 0.2999(4) 0.4067(2) 0.062(2) Uani 1 d . . H15A H -0.3073 0.2868 0.4194 0.093 Uiso 1 calc R . H15B H -0.2753 0.2784 0.3760 0.093 Uiso 1 calc R . H15C H -0.2755 0.3528 0.4045 0.093 Uiso 1 calc R . C16 C 0.01071(15) 0.4917(2) 0.43903(14) 0.0326(9) Uani 1 d . . H16A H 0.01382 0.5266 0.46301 0.039 Uiso 1 calc R . C17 C 0.09274(14) 0.4705(2) 0.44368(14) 0.0306(9) Uani 1 d . . C18 C 0.1058(2) 0.5433(2) 0.4524(2) 0.0361(10) Uani 1 d . . H18A H 0.0834 0.5805 0.4517 0.043 Uiso 1 calc R . C19 C 0.1523(2) 0.5611(3) 0.4620(2) 0.0386(10) Uani 1 d . . H19A H 0.1607 0.6098 0.4686 0.046 Uiso 1 calc R . C20 C 0.18586(15) 0.5066(3) 0.4619(2) 0.0357(10) Uani 1 d . . C21 C 0.1728(2) 0.4338(3) 0.4537(2) 0.0427(11) Uani 1 d . . H21A H 0.1953 0.3968 0.4538 0.051 Uiso 1 calc R . C22 C 0.1266(2) 0.4157(3) 0.4454(2) 0.0389(10) Uani 1 d . . H22A H 0.1181 0.3664 0.4408 0.047 Uiso 1 calc R . C23 C 0.2471(2) 0.5931(3) 0.4758(3) 0.076(2) Uani 1 d . . H23A H 0.2803 0.5946 0.4806 0.114 Uiso 1 calc R . H23B H 0.2325 0.6135 0.5028 0.114 Uiso 1 calc R . H23C H 0.2384 0.6217 0.4484 0.114 Uiso 1 calc R . C24 C -0.06832(14) 0.5307(2) 0.42449(14) 0.0294(9) Uani 1 d . . C25 C -0.0635(2) 0.6064(3) 0.4285(2) 0.0422(11) Uani 1 d . . H25A H -0.0341 0.6279 0.4279 0.051 Uiso 1 calc R . C26 C -0.1028(2) 0.6507(3) 0.4336(2) 0.0548(14) Uani 1 d . . H26A H -0.0994 0.7016 0.4371 0.066 Uiso 1 calc R . C27 C -0.1468(2) 0.6194(3) 0.4333(2) 0.0463(12) Uani 1 d . . C28 C -0.1518(2) 0.5444(3) 0.4281(2) 0.0393(10) Uani 1 d . . H28A H -0.1813 0.5233 0.4271 0.047 Uiso 1 calc R . C29 C -0.11314(15) 0.5001(2) 0.4243(2) 0.0360(10) Uani 1 d . . H29A H -0.11681 0.4491 0.4216 0.043 Uiso 1 calc R . C30 C -0.1834(2) 0.7316(4) 0.4557(4) 0.128(4) Uani 1 d . . H30A H -0.2139 0.7531 0.4574 0.193 Uiso 1 calc R . H30B H -0.1650 0.7606 0.4350 0.193 Uiso 1 calc R . H30C H -0.1688 0.7307 0.4865 0.193 Uiso 1 calc R . C31 C 0.03315(14) 0.5285(2) 0.31450(14) 0.0295(9) Uani 1 d . . H31A H 0.04225 0.5716 0.29935 0.035 Uiso 1 calc R . C32 C 0.11298(14) 0.5041(2) 0.32928(14) 0.0299(9) Uani 1 d . . C33 C 0.14663(15) 0.4522(2) 0.3178(2) 0.0370(10) Uani 1 d . . H33A H 0.13778 0.4036 0.3115 0.044 Uiso 1 calc R . C34 C 0.1930(2) 0.4720(3) 0.3155(2) 0.0426(11) Uani 1 d . . H34A H 0.2151 0.4367 0.3078 0.051 Uiso 1 calc R . C35 C 0.20650(15) 0.5443(3) 0.3247(2) 0.0388(10) Uani 1 d . . C36 C 0.1738(2) 0.5963(3) 0.3379(2) 0.0404(11) Uani 1 d . . H36A H 0.1829 0.6444 0.3454 0.048 Uiso 1 calc R . C37 C 0.1274(2) 0.5755(2) 0.3400(2) 0.0360(10) Uani 1 d . . H37A H 0.1054 0.6104 0.3488 0.043 Uiso 1 calc R . C38 C 0.2691(2) 0.6319(4) 0.3284(3) 0.073(2) Uani 1 d . . H38A H 0.3021 0.6344 0.3242 0.110 Uiso 1 calc R . H38B H 0.2623 0.6464 0.3599 0.110 Uiso 1 calc R . H38C H 0.2536 0.6648 0.3065 0.110 Uiso 1 calc R . C39 C -0.04501(14) 0.5696(2) 0.30358(14) 0.0293(9) Uani 1 d . . C40 C -0.0346(2) 0.6447(2) 0.3026(2) 0.0374(10) Uani 1 d . . H40A H -0.0055 0.6609 0.3134 0.045 Uiso 1 calc R . C41 C -0.0670(2) 0.6956(2) 0.2858(2) 0.0440(11) Uani 1 d . . H41A H -0.0593 0.7456 0.2848 0.053 Uiso 1 calc R . C42 C -0.1109(2) 0.6725(2) 0.2705(2) 0.0382(10) Uani 1 d . . C43 C -0.12240(15) 0.5981(2) 0.2739(2) 0.0362(10) Uani 1 d . . H43A H -0.15231 0.5824 0.2654 0.043 Uiso 1 calc R . C44 C -0.08964(14) 0.5475(2) 0.28976(15) 0.0314(9) Uani 1 d . . H44A H -0.09759 0.4977 0.29125 0.038 Uiso 1 calc R . C45 C -0.1308(2) 0.7894(3) 0.2367(3) 0.074(2) Uani 1 d . . H45A H -0.1574 0.8163 0.2246 0.112 Uiso 1 calc R . H45B H -0.1086 0.7838 0.2123 0.112 Uiso 1 calc R . H45C H -0.1167 0.8160 0.2626 0.112 Uiso 1 calc R . C46 C 0.11024(14) 0.0644(2) 0.31496(15) 0.0313(9) Uani 1 d . . C47 C 0.1170(2) -0.0035(3) 0.3371(2) 0.0409(11) Uani 1 d . . H47A H 0.0914 -0.0294 0.3478 0.049 Uiso 1 calc R . C48 C 0.1605(2) -0.0330(3) 0.3435(2) 0.0481(12) Uani 1 d . . H48A H 0.1643 -0.0784 0.3585 0.058 Uiso 1 calc R . C49 C 0.1990(2) 0.0049(3) 0.3274(2) 0.0458(12) Uani 1 d . . C50 C 0.1932(2) 0.0724(3) 0.3049(2) 0.0423(11) Uani 1 d . . H50A H 0.2189 0.0979 0.2940 0.051 Uiso 1 calc R . C51 C 0.1487(2) 0.1020(2) 0.2985(2) 0.0361(10) Uani 1 d . . H51A H 0.1447 0.1471 0.2832 0.043 Uiso 1 calc R . C52 C 0.2812(2) 0.0057(4) 0.3177(2) 0.072(2) Uani 1 d . . H52A H 0.3085 -0.0232 0.3254 0.109 Uiso 1 calc R . H52B H 0.2845 0.0540 0.3315 0.109 Uiso 1 calc R . H52C H 0.2777 0.0102 0.2842 0.109 Uiso 1 calc R . C53 C 0.0000 -0.0547(3) 0.2500 0.0298(12) Uani 1 d S . H53A H 0.0000 -0.1062 0.2500 0.036 Uiso 1 calc SR . C54 C 0.06799(14) -0.0513(2) 0.2027(2) 0.0305(9) Uani 1 d . . C55 C 0.11387(15) -0.0266(2) 0.2046(2) 0.0344(10) Uani 1 d . . H55A H 0.12372 0.0050 0.2287 0.041 Uiso 1 calc R . C56 C 0.1451(2) -0.0483(3) 0.1712(2) 0.0388(10) Uani 1 d . . H56A H 0.1755 -0.0305 0.1725 0.047 Uiso 1 calc R . C57 C 0.1306(2) -0.0966(3) 0.1360(2) 0.0442(11) Uani 1 d . . C58 C 0.0857(2) -0.1249(3) 0.1357(2) 0.0502(13) Uani 1 d . . H58A H 0.0766 -0.1600 0.1133 0.060 Uiso 1 calc R . C59 C 0.0541(2) -0.1014(3) 0.1684(2) 0.0395(10) Uani 1 d . . H59A H 0.0238 -0.1193 0.1673 0.047 Uiso 1 calc R . C60 C 0.1971(2) -0.0749(3) 0.0904(2) 0.0554(14) Uani 1 d . . H60A H 0.2136 -0.0967 0.0650 0.083 Uiso 1 calc R . H60B H 0.2174 -0.0716 0.1178 0.083 Uiso 1 calc R . H60C H 0.1867 -0.0262 0.0815 0.083 Uiso 1 calc R . C61 C -0.0357(2) 0.0904(2) 0.1581(2) 0.0343(9) Uani 1 d . . H61A H -0.0480 0.0849 0.1276 0.041 Uiso 1 calc R . C62 C 0.03964(15) 0.0917(2) 0.1259(2) 0.0331(9) Uani 1 d . . C63 C 0.0278(2) 0.0538(3) 0.0851(2) 0.0486(13) Uani 1 d . . H63A H -0.0009 0.0301 0.0823 0.058 Uiso 1 calc R . C64 C 0.0582(2) 0.0504(3) 0.0483(2) 0.0526(13) Uani 1 d . . H64A H 0.0492 0.0262 0.0206 0.063 Uiso 1 calc R . C65 C 0.1016(2) 0.0827(3) 0.0524(2) 0.0406(11) Uani 1 d . . C66 C 0.1145(2) 0.1178(3) 0.0939(2) 0.0398(11) Uani 1 d . . H66A H 0.1442 0.1379 0.0976 0.048 Uiso 1 calc R . C67 C 0.0836(2) 0.1233(2) 0.1300(2) 0.0354(10) Uani 1 d . . H67A H 0.0924 0.1484 0.1574 0.043 Uiso 1 calc R . C68 C 0.1201(2) 0.0547(4) -0.0269(2) 0.067(2) Uani 1 d . . H68A H 0.1460 0.0570 -0.0474 0.101 Uiso 1 calc R . H68B H 0.0951 0.0846 -0.0395 0.101 Uiso 1 calc R . H68C H 0.1098 0.0043 -0.0242 0.101 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0267(2) 0.0261(2) 0.0246(2) -0.00120(13) 0.00111(13) 0.00094(13) Mo2 0.0261(2) 0.0246(2) 0.0247(2) -0.00212(13) -0.00002(13) -0.00015(13) Mo3 0.0306(2) 0.0204(2) 0.0312(2) -0.00080(13) 0.00509(14) -0.00244(13) Mo4 0.0249(2) 0.0209(2) 0.0233(2) 0.00041(13) 0.00070(13) 0.00054(12) C70A 0.042(5) 0.056(5) 0.095(8) -0.003(5) -0.026(5) 0.023(4) Cl1A 0.091(2) 0.113(4) 0.140(4) 0.034(3) 0.023(2) -0.003(3) Cl2A 0.139(3) 0.117(3) 0.141(6) -0.021(4) -0.019(5) 0.033(2) C70B 0.042(5) 0.056(5) 0.095(8) -0.003(5) -0.026(5) 0.023(4) Cl1B 0.091(2) 0.113(4) 0.140(4) 0.034(3) 0.023(2) -0.003(3) Cl2B 0.139(3) 0.117(3) 0.141(6) -0.021(4) -0.019(5) 0.033(2) P1A 0.056(3) 0.050(3) 0.069(7) 0.000(5) -0.019(5) -0.001(2) P1B 0.056(3) 0.050(3) 0.069(7) 0.000(5) -0.019(5) -0.001(2) O1 0.051(2) 0.031(2) 0.0256(15) -0.0039(12) 0.0039(13) 0.0067(14) O2 0.063(2) 0.025(2) 0.041(2) -0.0011(13) 0.009(2) -0.0116(15) O3 0.046(2) 0.030(2) 0.028(2) 0.0056(12) -0.0047(13) 0.0015(13) O4 0.028(2) 0.067(2) 0.055(2) -0.005(2) -0.0002(15) 0.005(2) O5 0.044(2) 0.066(2) 0.050(2) 0.012(2) -0.004(2) 0.019(2) O6 0.033(2) 0.054(2) 0.069(2) 0.014(2) 0.011(2) 0.000(2) O7 0.028(2) 0.051(2) 0.078(3) -0.005(2) -0.005(2) -0.0005(15) O8 0.037(2) 0.043(2) 0.129(4) -0.011(2) 0.008(2) 0.008(2) O9 0.032(2) 0.058(2) 0.080(3) -0.001(2) 0.003(2) -0.009(2) O10 0.045(2) 0.034(2) 0.082(3) 0.006(2) -0.011(2) 0.0109(15) O11 0.038(2) 0.086(3) 0.071(3) 0.026(2) 0.006(2) 0.011(2) O12 0.062(2) 0.079(3) 0.076(3) -0.041(2) 0.041(2) -0.027(2) O13 0.049(2) 0.079(3) 0.045(2) 0.005(2) 0.018(2) 0.009(2) N1 0.030(2) 0.030(2) 0.029(2) 0.0005(14) -0.0003(14) 0.0028(14) N2 0.025(2) 0.029(2) 0.030(2) -0.0005(14) -0.0005(14) -0.0001(13) N3 0.031(2) 0.033(2) 0.023(2) -0.0030(14) -0.0017(14) 0.0003(14) N4 0.028(2) 0.035(2) 0.025(2) -0.0052(14) 0.0047(14) -0.0016(14) N5 0.029(2) 0.029(2) 0.031(2) 0.0005(14) 0.0018(14) 0.0007(14) N6 0.029(2) 0.030(2) 0.027(2) -0.0018(14) -0.0003(14) 0.0008(14) N7 0.035(2) 0.029(2) 0.032(2) 0.0010(15) 0.003(2) -0.0045(15) N8 0.030(2) 0.024(2) 0.037(2) -0.0013(14) 0.0062(15) 0.0009(14) N9 0.034(2) 0.027(2) 0.033(2) -0.0025(14) 0.0062(15) -0.0012(14) C1 0.034(2) 0.025(2) 0.027(2) 0.000(2) 0.000(2) -0.002(2) C2 0.031(2) 0.027(2) 0.030(2) -0.001(2) -0.002(2) 0.000(2) C3 0.035(2) 0.040(3) 0.036(2) 0.004(2) 0.004(2) 0.005(2) C4 0.047(3) 0.052(3) 0.037(3) 0.013(2) 0.001(2) 0.006(2) C5 0.038(2) 0.040(3) 0.039(3) 0.002(2) -0.004(2) 0.005(2) C6 0.034(2) 0.041(3) 0.039(3) -0.004(2) -0.001(2) 0.005(2) C7 0.033(2) 0.039(2) 0.028(2) 0.002(2) -0.001(2) 0.001(2) C8 0.042(3) 0.084(4) 0.066(4) 0.007(3) -0.005(3) 0.027(3) C9 0.030(2) 0.026(2) 0.031(2) 0.000(2) 0.003(2) 0.000(2) C10 0.039(2) 0.030(2) 0.034(2) 0.003(2) -0.002(2) 0.003(2) C11 0.043(3) 0.037(2) 0.035(2) 0.006(2) 0.011(2) 0.002(2) C12 0.033(2) 0.031(2) 0.049(3) 0.002(2) 0.006(2) 0.001(2) C13 0.032(2) 0.040(3) 0.039(3) -0.001(2) -0.002(2) 0.001(2) C14 0.034(2) 0.033(2) 0.031(2) 0.002(2) 0.002(2) -0.001(2) C15 0.032(3) 0.078(4) 0.077(4) 0.012(3) 0.007(3) 0.001(3) C16 0.037(2) 0.036(2) 0.025(2) -0.005(2) 0.001(2) -0.003(2) C17 0.030(2) 0.038(2) 0.023(2) -0.001(2) -0.003(2) -0.001(2) C18 0.034(2) 0.035(2) 0.039(3) -0.006(2) 0.000(2) 0.005(2) C19 0.042(3) 0.032(2) 0.041(3) -0.003(2) -0.004(2) -0.002(2) C20 0.030(2) 0.042(3) 0.035(2) 0.000(2) -0.002(2) -0.001(2) C21 0.035(2) 0.037(3) 0.056(3) -0.005(2) -0.006(2) 0.008(2) C22 0.040(2) 0.032(2) 0.044(3) -0.003(2) -0.006(2) 0.002(2) C23 0.037(3) 0.061(4) 0.130(6) -0.018(4) -0.005(3) -0.012(3) C24 0.027(2) 0.039(2) 0.022(2) -0.004(2) 0.005(2) 0.000(2) C25 0.035(2) 0.034(2) 0.058(3) -0.003(2) 0.004(2) -0.007(2) C26 0.042(3) 0.030(2) 0.094(4) -0.003(3) 0.010(3) 0.002(2) C27 0.036(3) 0.040(3) 0.063(3) -0.005(2) 0.007(2) 0.006(2) C28 0.029(2) 0.044(3) 0.045(3) -0.007(2) 0.002(2) -0.004(2) C29 0.036(2) 0.033(2) 0.039(3) -0.010(2) 0.006(2) -0.004(2) C30 0.055(4) 0.044(4) 0.287(14) -0.031(6) 0.021(6) 0.012(3) C31 0.033(2) 0.028(2) 0.027(2) 0.000(2) 0.003(2) -0.001(2) C32 0.031(2) 0.032(2) 0.027(2) 0.005(2) 0.001(2) -0.002(2) C33 0.035(2) 0.030(2) 0.046(3) 0.001(2) -0.001(2) 0.001(2) C34 0.034(2) 0.040(3) 0.054(3) -0.001(2) 0.000(2) 0.006(2) C35 0.027(2) 0.047(3) 0.042(3) 0.005(2) -0.002(2) 0.000(2) C36 0.040(2) 0.037(2) 0.044(3) -0.002(2) -0.004(2) -0.005(2) C37 0.036(2) 0.031(2) 0.041(3) -0.001(2) 0.006(2) 0.003(2) C38 0.041(3) 0.074(4) 0.104(5) 0.002(4) 0.003(3) -0.023(3) C39 0.033(2) 0.028(2) 0.027(2) -0.001(2) 0.003(2) 0.000(2) C40 0.033(2) 0.032(2) 0.047(3) -0.009(2) -0.002(2) -0.001(2) C41 0.047(3) 0.023(2) 0.061(3) -0.002(2) -0.002(2) -0.002(2) C42 0.036(2) 0.033(2) 0.045(3) -0.001(2) -0.003(2) 0.009(2) C43 0.028(2) 0.036(2) 0.044(3) 0.000(2) -0.001(2) 0.000(2) C44 0.032(2) 0.025(2) 0.037(2) 0.003(2) 0.001(2) -0.003(2) C45 0.074(4) 0.041(3) 0.108(6) 0.019(3) -0.013(4) 0.010(3) C46 0.032(2) 0.034(2) 0.028(2) -0.004(2) 0.002(2) -0.003(2) C47 0.037(2) 0.045(3) 0.041(3) 0.008(2) 0.007(2) -0.004(2) C48 0.044(3) 0.054(3) 0.047(3) 0.015(2) 0.005(2) 0.004(2) C49 0.034(2) 0.062(3) 0.042(3) 0.005(2) -0.002(2) 0.007(2) C50 0.032(2) 0.053(3) 0.042(3) 0.002(2) 0.005(2) -0.008(2) C51 0.038(2) 0.034(2) 0.035(2) 0.002(2) 0.001(2) -0.006(2) C52 0.035(3) 0.105(5) 0.077(4) 0.017(4) 0.003(3) 0.003(3) C53 0.031(3) 0.020(3) 0.038(3) 0.000 0.006(3) 0.000 C54 0.031(2) 0.022(2) 0.040(2) 0.003(2) 0.006(2) 0.000(2) C55 0.037(2) 0.027(2) 0.040(2) -0.006(2) 0.004(2) -0.003(2) C56 0.030(2) 0.036(2) 0.050(3) -0.004(2) 0.008(2) -0.004(2) C57 0.043(3) 0.042(3) 0.049(3) -0.011(2) 0.018(2) -0.004(2) C58 0.051(3) 0.049(3) 0.050(3) -0.023(2) 0.012(2) -0.013(2) C59 0.034(2) 0.038(2) 0.047(3) -0.008(2) 0.005(2) -0.007(2) C60 0.045(3) 0.073(4) 0.050(3) -0.011(3) 0.019(2) -0.007(3) C61 0.039(2) 0.031(2) 0.034(2) -0.002(2) 0.001(2) 0.001(2) C62 0.037(2) 0.029(2) 0.034(2) 0.004(2) 0.004(2) 0.002(2) C63 0.038(3) 0.065(3) 0.043(3) -0.015(2) 0.007(2) -0.011(2) C64 0.047(3) 0.073(4) 0.038(3) -0.017(3) 0.005(2) 0.001(3) C65 0.038(2) 0.045(3) 0.039(3) 0.007(2) 0.011(2) 0.011(2) C66 0.034(2) 0.042(3) 0.043(3) 0.007(2) 0.005(2) -0.001(2) C67 0.041(2) 0.035(2) 0.031(2) 0.001(2) -0.001(2) -0.002(2) C68 0.075(4) 0.082(4) 0.046(3) 0.004(3) 0.021(3) 0.022(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 Mo1 O1 2.070(3) . Y Mo1 N3 2.106(3) . Y Mo1 N1 2.118(3) . Y Mo1 N5 2.127(3) . Y Mo1 Mo2 2.1503(5) . Y Mo2 O3 2.056(3) 2 Y Mo2 N4 2.093(3) . Y Mo2 N6 2.124(3) . Y Mo2 N2 2.140(3) . Y Mo3 O2 2.041(3) . Y Mo3 N8 2.099(3) . Y Mo3 N7 2.121(4) . Y Mo3 N9 2.132(4) . Y Mo3 Mo3 2.1467(7) 2 Y Mo4 O4 1.693(3) . Y Mo4 O1 1.780(3) . Y Mo4 O3 1.780(3) . Y Mo4 O2 1.782(3) . Y C70A Cl1A 1.682(14) . N C70A Cl2A 1.76(2) . N C70B Cl1B 1.691(15) . N C70B Cl2B 1.79(2) . N P1A F2A 1.56(2) . N P1A F6A 1.57(2) . N P1A F4A 1.57(2) . N P1A F1A 1.59(2) . N P1A F3A 1.60(2) . N P1A F5A 1.62(2) . N P1B F6B 1.49(3) . N P1B F3B 1.58(3) . N P1B F4B 1.58(3) . N P1B F5B 1.58(3) . N P1B F2B 1.63(3) . N P1B F1B 1.67(3) . N O3 Mo2 2.056(3) 2 Y O5 C5 1.369(5) . N O5 C8 1.429(6) . N O6 C12 1.374(5) . N O6 C15 1.423(6) . N O7 C20 1.372(5) . N O7 C23 1.407(6) . N O8 C27 1.369(6) . N O8 C30 1.417(8) . N O9 C35 1.383(5) . N O9 C38 1.415(7) . N O10 C42 1.374(5) . N O10 C45 1.423(6) . N O11 C49 1.381(6) . N O11 C52 1.419(7) . N O12 C57 1.362(6) . N O12 C60 1.415(6) . N O13 C65 1.367(5) . N O13 C68 1.418(7) . N N1 C1 1.333(5) . Y N1 C2 1.428(5) . Y N2 C1 1.327(5) . Y N2 C9 1.435(5) . Y N3 C16 1.317(5) . Y N3 C17 1.431(5) . Y N4 C16 1.324(5) . Y N4 C24 1.428(5) . Y N5 C31 1.319(5) . Y N5 C32 1.434(5) . Y N6 C31 1.336(5) . Y N6 C39 1.433(5) . Y N7 C61 1.330(6) 2 Y N7 C46 1.428(5) . Y N8 C53 1.328(4) . Y N8 C54 1.430(5) . Y N9 C61 1.328(5) . Y N9 C62 1.429(5) . Y C2 C3 1.378(6) . N C2 C7 1.389(6) . N C3 C4 1.399(6) . N C4 C5 1.387(7) . N C5 C6 1.383(6) . N C6 C7 1.392(6) . N C9 C14 1.384(6) . N C9 C10 1.395(6) . N C10 C11 1.379(6) . N C11 C12 1.386(6) . N C12 C13 1.380(6) . N C13 C14 1.398(6) . N C17 C22 1.387(6) . N C17 C18 1.387(6) . N C18 C19 1.393(6) . N C19 C20 1.376(6) . N C20 C21 1.385(6) . N C21 C22 1.379(6) . N C24 C25 1.378(6) . N C24 C29 1.401(6) . N C25 C26 1.394(6) . N C26 C27 1.386(7) . N C27 C28 1.370(7) . N C28 C29 1.374(6) . N C32 C37 1.385(6) . N C32 C33 1.393(6) . N C33 C34 1.381(6) . N C34 C35 1.385(7) . N C35 C36 1.388(6) . N C36 C37 1.389(6) . N C39 C44 1.387(6) . N C39 C40 1.389(6) . N C40 C41 1.383(6) . N C41 C42 1.387(6) . N C42 C43 1.387(6) . N C43 C44 1.378(6) . N C46 C47 1.390(6) . N C46 C51 1.390(6) . N C47 C48 1.365(7) . N C48 C49 1.391(7) . N C49 C50 1.386(7) . N C50 C51 1.390(6) . N C53 N8 1.329(4) 2 Y C54 C59 1.380(6) . N C54 C55 1.391(6) . N C55 C56 1.381(6) . N C56 C57 1.383(7) . N C57 C58 1.389(7) . N C58 C59 1.386(7) . N C61 N7 1.330(6) 2 Y C62 C63 1.382(6) . N C62 C67 1.387(6) . N C63 C64 1.384(7) . N C64 C65 1.380(7) . N C65 C66 1.380(7) . N C66 C67 1.380(6) . N 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 Mo1 N3 165.06(13) . . Y O1 Mo1 N1 91.62(12) . . Y N3 Mo1 N1 93.35(13) . . Y O1 Mo1 N5 88.70(13) . . Y N3 Mo1 N5 85.06(13) . . Y N1 Mo1 N5 174.68(13) . . Y O1 Mo1 Mo2 102.58(9) . . Y N3 Mo1 Mo2 91.35(9) . . Y N1 Mo1 Mo2 91.79(9) . . Y N5 Mo1 Mo2 93.33(9) . . Y O3 Mo2 N4 163.47(13) 2 . Y O3 Mo2 N6 91.58(12) 2 . Y N4 Mo2 N6 86.23(13) . . Y O3 Mo2 N2 89.55(12) 2 . Y N4 Mo2 N2 91.65(13) . . Y N6 Mo2 N2 176.17(13) . . Y O3 Mo2 Mo1 104.13(9) 2 . Y N4 Mo2 Mo1 92.29(9) . . Y N6 Mo2 Mo1 90.94(9) . . Y N2 Mo2 Mo1 92.33(9) . . Y O2 Mo3 N8 165.52(13) . . Y O2 Mo3 N7 91.75(13) . . Y N8 Mo3 N7 88.45(13) . . Y O2 Mo3 N9 91.87(13) . . Y N8 Mo3 N9 86.76(13) . . Y N7 Mo3 N9 173.69(13) . . Y O2 Mo3 Mo3 102.71(10) . 2 Y N8 Mo3 Mo3 91.75(9) . 2 Y N7 Mo3 Mo3 91.18(10) . 2 Y N9 Mo3 Mo3 93.06(9) . 2 Y O4 Mo4 O1 108.0(2) . . Y O4 Mo4 O3 108.5(2) . . Y O1 Mo4 O3 110.69(14) . . Y O4 Mo4 O2 107.3(2) . . Y O1 Mo4 O2 111.45(14) . . Y O3 Mo4 O2 110.74(14) . . Y Cl1A C70A Cl2A 120.0(9) . . N Cl1B C70B Cl2B 115.4(8) . . N F2A P1A F6A 93.6(13) . . N F2A P1A F4A 87.4(8) . . N F6A P1A F4A 94.7(13) . . N F2A P1A F1A 87.0(12) . . N F6A P1A F1A 172.5(11) . . N F4A P1A F1A 92.8(9) . . N F2A P1A F3A 175.5(13) . . N F6A P1A F3A 90.4(12) . . N F4A P1A F3A 90.2(12) . . N F1A P1A F3A 89.3(12) . . N F2A P1A F5A 88.5(12) . . N F6A P1A F5A 87.3(9) . . N F4A P1A F5A 175.5(17) . . N F1A P1A F5A 85.2(12) . . N F3A P1A F5A 93.9(9) . . N F6B P1B F3B 87.4(11) . . N F6B P1B F4B 96.0(19) . . N F3B P1B F4B 92.4(17) . . N F6B P1B F5B 88.8(14) . . N F3B P1B F5B 89.5(14) . . N F4B P1B F5B 174.9(17) . . N F6B P1B F2B 89.0(17) . . N F3B P1B F2B 176.1(16) . . N F4B P1B F2B 89.5(14) . . N F5B P1B F2B 88.9(16) . . N F6B P1B F1B 176.8(20) . . N F3B P1B F1B 89.6(16) . . N F4B P1B F1B 83.3(12) . . N F5B P1B F1B 92.0(17) . . N F2B P1B F1B 94.0(11) . . N Mo4 O1 Mo1 162.6(2) . . Y Mo4 O2 Mo3 161.5(2) . . Y Mo4 O3 Mo2 163.5(2) . 2 Y C5 O5 C8 117.2(4) . . N C12 O6 C15 117.7(4) . . N C20 O7 C23 117.6(4) . . N C27 O8 C30 117.2(4) . . N C35 O9 C38 117.8(4) . . N C42 O10 C45 116.7(4) . . N C49 O11 C52 116.9(4) . . N C57 O12 C60 117.3(4) . . N C65 O13 C68 117.9(4) . . N C1 N1 C2 119.4(3) . . Y C1 N1 Mo1 118.7(3) . . Y C2 N1 Mo1 121.9(3) . . Y C1 N2 C9 118.1(3) . . Y C1 N2 Mo2 117.2(3) . . Y C9 N2 Mo2 124.5(3) . . Y C16 N3 C17 120.5(3) . . Y C16 N3 Mo1 118.2(3) . . Y C17 N3 Mo1 117.3(3) . . Y C16 N4 C24 121.4(3) . . Y C16 N4 Mo2 117.7(3) . . Y C24 N4 Mo2 118.6(3) . . Y C31 N5 C32 117.9(3) . . Y C31 N5 Mo1 116.5(3) . . Y C32 N5 Mo1 125.1(3) . . Y C31 N6 C39 118.1(3) . . Y C31 N6 Mo2 118.4(3) . . Y C39 N6 Mo2 123.2(3) . . Y C61 N7 C46 116.4(4) 2 . Y C61 N7 Mo3 118.7(3) 2 . Y C46 N7 Mo3 122.3(3) . . Y C53 N8 C54 121.3(3) . . Y C53 N8 Mo3 118.9(3) . . Y C54 N8 Mo3 118.1(3) . . Y C61 N9 C62 119.0(4) . . Y C61 N9 Mo3 116.3(3) . . Y C62 N9 Mo3 123.9(3) . . Y N2 C1 N1 120.0(4) . . Y C3 C2 C7 118.9(4) . . N C3 C2 N1 123.1(4) . . N C7 C2 N1 117.9(4) . . N C2 C3 C4 120.2(4) . . N C5 C4 C3 120.5(4) . . N O5 C5 C6 124.2(4) . . N O5 C5 C4 116.2(4) . . N C6 C5 C4 119.6(4) . . N C5 C6 C7 119.4(4) . . N C2 C7 C6 121.5(4) . . N C14 C9 C10 118.3(4) . . N C14 C9 N2 119.3(4) . . N C10 C9 N2 122.4(4) . . N C11 C10 C9 120.7(4) . . N C10 C11 C12 120.6(4) . . N O6 C12 C13 124.1(4) . . N O6 C12 C11 116.4(4) . . N C13 C12 C11 119.5(4) . . N C12 C13 C14 119.7(4) . . N C9 C14 C13 121.1(4) . . N N3 C16 N4 119.7(4) . . Y C22 C17 C18 119.0(4) . . N C22 C17 N3 118.6(4) . . N C18 C17 N3 122.0(4) . . N C17 C18 C19 120.4(4) . . N C20 C19 C18 120.2(4) . . N O7 C20 C19 124.2(4) . . N O7 C20 C21 116.3(4) . . N C19 C20 C21 119.5(4) . . N C22 C21 C20 120.6(4) . . N C21 C22 C17 120.4(4) . . N C25 C24 C29 118.8(4) . . N C25 C24 N4 122.7(4) . . N C29 C24 N4 118.3(4) . . N C24 C25 C26 119.8(4) . . N C27 C26 C25 120.6(5) . . N O8 C27 C28 115.7(4) . . N O8 C27 C26 124.7(5) . . N C28 C27 C26 119.6(4) . . N C27 C28 C29 120.2(4) . . N C28 C29 C24 120.9(4) . . N N5 C31 N6 120.8(4) . . Y C37 C32 C33 118.3(4) . . N C37 C32 N5 122.1(4) . . N C33 C32 N5 119.6(4) . . N C34 C33 C32 120.9(4) . . N C33 C34 C35 120.0(4) . . N O9 C35 C34 115.4(4) . . N O9 C35 C36 124.6(4) . . N C34 C35 C36 120.1(4) . . N C35 C36 C37 119.2(4) . . N C32 C37 C36 121.5(4) . . N C44 C39 C40 118.2(4) . . N C44 C39 N6 119.0(4) . . N C40 C39 N6 122.8(4) . . N C41 C40 C39 120.9(4) . . N C40 C41 C42 120.3(4) . . N O10 C42 C41 124.9(4) . . N O10 C42 C43 116.1(4) . . N C41 C42 C43 119.1(4) . . N C44 C43 C42 120.2(4) . . N C43 C44 C39 121.2(4) . . N C47 C46 C51 118.9(4) . . N C47 C46 N7 119.7(4) . . N C51 C46 N7 121.2(4) . . N C48 C47 C46 121.2(4) . . N C47 C48 C49 120.0(5) . . N O11 C49 C50 124.8(5) . . N O11 C49 C48 115.4(5) . . N C50 C49 C48 119.9(4) . . N C49 C50 C51 119.7(4) . . N C46 C51 C50 120.4(4) . . N N8 C53 N8 118.4(5) . 2 Y C59 C54 C55 119.3(4) . . N C59 C54 N8 122.0(4) . . N C55 C54 N8 118.3(4) . . N C56 C55 C54 121.2(4) . . N C55 C56 C57 119.3(4) . . N O12 C57 C56 124.0(4) . . N O12 C57 C58 116.4(4) . . N C56 C57 C58 119.7(4) . . N C59 C58 C57 120.7(4) . . N C54 C59 C58 119.7(4) . . N N9 C61 N7 120.4(4) . 2 Y C63 C62 C67 118.2(4) . . N C63 C62 N9 123.8(4) . . N C67 C62 N9 118.0(4) . . N C62 C63 C64 120.9(5) . . N C65 C64 C63 120.4(5) . . N O13 C65 C66 116.4(4) . . N O13 C65 C64 124.6(5) . . N C66 C65 C64 119.0(4) . . N C67 C66 C65 120.5(4) . . N C66 C67 C62 120.9(4) . . N _refine_diff_density_max 1.260 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.101