# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nyy134907a _audit_creation_date 2013-04-12 _audit_creation_method ; Olex2 1.2 (compiled Apr 9 2013 14:06:00, GUI svn.r4456) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '3(Mo8 O26), 4(C18 H21 N6), 4(H2 O), 0.6(O)' _chemical_formula_sum 'C72 H93.20 Mo24 N24 O82.60' _chemical_formula_weight 4919.07 _chemical_melting_point ? _chemical_oxdiff_formula C20H20N4O4Mo1Fe1 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' Mo Mo -1.6832 0.6857 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.3022(3) _cell_length_b 12.5187(4) _cell_length_c 25.8195(11) _cell_angle_alpha 101.016(3) _cell_angle_beta 92.618(3) _cell_angle_gamma 96.446(3) _cell_volume 3240.2(2) _cell_formula_units_Z 1 _cell_measurement_reflns_used 8846 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 29.2259 _cell_measurement_theta_min 2.9404 _exptl_absorpt_coefficient_mu 2.347 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 2.521 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2362 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_unetI/netI 0.0593 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 26832 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.95 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -11.00 25.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 -99.0000 -150.0000 36 #__ type_ start__ end____ width___ exp.time_ 2 omega -76.00 -25.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 128.0000 -101.0000 51 #__ type_ start__ end____ width___ exp.time_ 3 omega -80.00 -34.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 141.0000 69.0000 46 #__ type_ start__ end____ width___ exp.time_ 4 omega -24.00 35.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 -57.0000 30.0000 59 #__ type_ start__ end____ width___ exp.time_ 5 omega -26.00 20.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 -57.0000 -150.0000 46 #__ type_ start__ end____ width___ exp.time_ 6 omega -52.00 93.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 0.0000 60.0000 145 #__ type_ start__ end____ width___ exp.time_ 7 omega -6.00 49.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 37.0000 -180.0000 55 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0255299000 _diffrn_orient_matrix_UB_12 0.0215075000 _diffrn_orient_matrix_UB_13 -0.0212906000 _diffrn_orient_matrix_UB_21 0.0269614000 _diffrn_orient_matrix_UB_22 -0.0400773000 _diffrn_orient_matrix_UB_23 -0.0182149000 _diffrn_orient_matrix_UB_31 -0.0586929000 _diffrn_orient_matrix_UB_32 -0.0362583000 _diffrn_orient_matrix_UB_33 -0.0013913000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9602 _reflns_number_total 13242 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.663 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.133 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 923 _refine_ls_number_reflns 13242 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0378 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.0708 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C16) = Uanis(C17) 3. Others Fixed Sof: O42(0.3) 4.a Free rotating group: O40(H40A,H40B), O41(H41A,H41B) 4.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C25(H25A,H25B), C27(H27A,H27B), C7(H7A,H7B), C26(H26A,H26B), C9(H9A,H9B) 4.c Aromatic/amide H refined with riding coordinates: N4(H4), C15(H15), C30(H30), C20(H20), C14(H14), C35(H35), C24(H24), C31(H31), C13(H13), C22(H22), N2(H2), N12(H12A), C2(H2A), C11(H11), C29(H29), C10(H10), N10(H10A), C32(H32), C36(H36), C12(H12), C4(H4A), C28(H28), C33(H33), C6(H6), C34(H34), N6(H6A), C18(H18), C16(H16), C17(H17) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Mo4 Mo 0.44720(4) 0.85538(3) 0.105578(17) 0.01946(10) Uani 1 1 d . . . Mo5 Mo 0.40163(4) 0.71547(3) 0.210236(18) 0.02428(11) Uani 1 1 d . . . Mo6 Mo 0.51447(4) 0.97147(3) 0.243284(17) 0.01930(10) Uani 1 1 d . . . Mo8 Mo 0.69815(4) 0.78814(3) 0.166149(18) 0.02086(11) Uani 1 1 d . . . Mo2 Mo 0.25935(4) 1.03576(3) 0.184212(18) 0.02333(11) Uani 1 1 d . . . Mo1 Mo 0.14311(4) 0.77770(3) 0.150194(18) 0.02403(11) Uani 1 1 d . . . Mo3 Mo 0.55127(4) 1.11273(3) 0.137123(18) 0.02444(11) Uani 1 1 d . . . Mo7 Mo 0.80974(4) 1.04641(3) 0.193432(18) 0.02257(11) Uani 1 1 d . . . Mo9 Mo 0.84070(4) 0.54407(3) 0.494475(18) 0.02237(11) Uani 1 1 d . . . Mo11 Mo 0.80045(4) 0.39711(4) 0.595516(19) 0.02795(12) Uani 1 1 d . . . Mo12 Mo 0.94950(4) 0.41355(4) 0.388292(19) 0.02623(12) Uani 1 1 d . . . Mo10 Mo 0.90954(4) 0.26920(3) 0.486975(19) 0.02538(11) Uani 1 1 d . . . O28 O 0.7563(3) 0.6167(3) 0.45958(15) 0.0332(9) Uani 1 1 d . . . O16 O 0.3304(3) 0.7330(3) 0.26855(15) 0.0369(10) Uani 1 1 d . . . O36 O 0.8966(4) 0.3264(3) 0.62953(15) 0.0375(10) Uani 1 1 d . . . O24 O 0.7605(3) 0.7751(3) 0.10558(14) 0.0297(9) Uani 1 1 d . . . O33 O 0.9978(3) 0.1962(3) 0.52177(15) 0.0382(10) Uani 1 1 d . . . O3 O 0.2543(3) 0.6689(2) 0.16106(14) 0.0276(9) Uani 1 1 d . . . O1 O 0.0664(3) 0.7856(3) 0.20735(14) 0.0328(9) Uani 1 1 d . . . O26 O 0.2915(3) 0.7855(3) 0.08581(13) 0.0272(9) Uani 1 1 d . . . O5 O 0.1969(3) 1.0382(3) 0.24423(14) 0.0334(9) Uani 1 1 d . . . O38 O 0.9231(3) 0.2846(3) 0.35100(14) 0.0360(10) Uani 1 1 d . . . O23 O 0.8181(3) 0.9015(2) 0.20779(13) 0.0251(8) Uani 1 1 d . . . O12 O 0.6995(3) 1.1588(2) 0.18629(13) 0.0242(8) Uani 1 1 d . . . O21 O 0.8710(3) 1.0325(3) 0.13278(15) 0.0358(10) Uani 1 1 d . . . O20 O 0.6718(3) 1.0387(2) 0.26151(13) 0.0248(8) Uani 1 1 d . . . O39 O 0.8658(3) 0.4887(3) 0.35347(15) 0.0386(10) Uani 1 1 d . . . O31 O 0.8289(3) 0.4028(2) 0.44534(13) 0.0246(8) Uani 1 1 d . . . O18 O 0.5617(3) 0.8215(2) 0.23386(13) 0.0202(8) Uani 1 1 d . . . O7 O 0.3563(3) 0.8762(2) 0.18933(13) 0.0216(8) Uani 1 1 d . . . O2 O 0.0315(3) 0.7041(3) 0.10253(14) 0.0357(10) Uani 1 1 d . . . O11 O 0.6242(3) 1.0875(3) 0.07927(14) 0.0385(10) Uani 1 1 d . . . O9 O 0.4458(3) 1.0850(2) 0.21211(13) 0.0214(8) Uani 1 1 d . . . O8 O 0.3942(3) 1.0025(2) 0.11428(13) 0.0202(8) Uani 1 1 d . . . O27 O 0.9435(3) 0.6605(2) 0.54652(13) 0.0242(8) Uani 1 1 d . . . O13 O 0.6023(3) 0.9464(2) 0.15892(13) 0.0203(8) Uani 1 1 d . . . O34 O 0.7671(3) 0.2914(3) 0.53017(14) 0.0297(9) Uani 1 1 d . . . O4 O 0.1420(3) 0.9242(3) 0.13928(14) 0.0274(8) Uani 1 1 d . . . O19 O 0.4393(3) 0.9790(3) 0.30057(14) 0.0307(9) Uani 1 1 d . . . O15 O 0.5131(3) 0.7388(2) 0.13541(13) 0.0215(8) Uani 1 1 d . . . O6 O 0.2217(3) 1.1520(3) 0.16603(15) 0.0346(9) Uani 1 1 d . . . O14 O 0.5275(3) 0.8473(3) 0.04939(14) 0.0309(9) Uani 1 1 d . . . O32 O 0.8342(3) 0.1739(3) 0.43557(14) 0.0339(10) Uani 1 1 d . . . O29 O 1.0231(3) 0.5579(2) 0.45928(13) 0.0219(8) Uani 1 1 d . . . O10 O 0.4883(3) 1.2333(3) 0.13804(16) 0.0396(10) Uani 1 1 d . . . O30 O 0.7293(3) 0.5005(3) 0.53792(14) 0.0277(9) Uani 1 1 d . . . O22 O 0.9316(3) 1.1195(3) 0.23594(15) 0.0350(10) Uani 1 1 d . . . O17 O 0.4649(3) 0.5929(3) 0.20407(16) 0.0396(10) Uani 1 1 d . . . O25 O 0.7350(3) 0.6770(3) 0.18953(15) 0.0327(9) Uani 1 1 d . . . O35 O 0.6533(3) 0.3885(3) 0.62196(16) 0.0427(11) Uani 1 1 d . . . O37 O 0.8757(3) 0.5431(3) 0.62752(14) 0.0304(9) Uani 1 1 d . . . N3 N 0.1355(4) -0.0486(3) 0.36831(17) 0.0278(11) Uani 1 1 d . . . N9 N 0.7051(4) 0.5578(3) -0.02179(18) 0.0284(10) Uani 1 1 d . . . N4 N -0.0089(4) -0.0648(4) 0.30425(19) 0.0361(12) Uani 1 1 d . . . H4 H -0.0519 -0.0881 0.2741 0.043 Uiso 1 1 calc R . . N7 N 1.0075(4) 0.1472(3) 0.01424(18) 0.0275(10) Uani 1 1 d . . . N1 N 0.5123(4) 0.3072(3) 0.3953(2) 0.0335(12) Uani 1 1 d . . . N11 N 0.9051(5) 0.4438(4) 0.21366(18) 0.0385(13) Uani 1 1 d . . . C8 C 0.2471(5) -0.0732(4) 0.3997(2) 0.0336(14) Uani 1 1 d . . . H8A H 0.3115 -0.1000 0.3759 0.040 Uiso 1 1 calc R . . H8B H 0.2168 -0.1316 0.4177 0.040 Uiso 1 1 calc R . . O40 O 0.8220(4) 0.7501(3) 0.6945(2) 0.0618(14) Uani 1 1 d GU . . H40A H 0.8933 0.7604 0.6799 0.093 Uiso 1 1 d G . . H40B H 0.8010 0.8114 0.7098 0.093 Uiso 1 1 d G . . C15 C 0.0973(5) -0.1007(4) 0.3201(2) 0.0315(14) Uani 1 1 d . . . H15 H 0.1394 -0.1549 0.3002 0.038 Uiso 1 1 calc R . . N5 N 0.3161(4) 0.1814(4) 0.61945(18) 0.0335(11) Uani 1 1 d . . . C25 C 0.8685(5) 0.1647(4) 0.0176(2) 0.0279(13) Uani 1 1 d . . . H25A H 0.8255 0.1128 0.0368 0.034 Uiso 1 1 calc R . . H25B H 0.8264 0.1499 -0.0179 0.034 Uiso 1 1 calc R . . C23 C 0.8058(5) 0.4061(4) 0.1232(2) 0.0276(13) Uani 1 1 d . . . C27 C 0.7826(6) 0.4276(4) 0.1815(2) 0.0384(15) Uani 1 1 d . . . H27A H 0.7381 0.4924 0.1901 0.046 Uiso 1 1 calc R . . H27B H 0.7266 0.3660 0.1894 0.046 Uiso 1 1 calc R . . C1 C 0.4350(5) 0.2037(4) 0.4636(2) 0.0297(13) Uani 1 1 d . . . C30 C 1.0671(6) 0.1240(4) -0.0297(2) 0.0340(14) Uani 1 1 d . . . H30 H 1.0292 0.1167 -0.0637 0.041 Uiso 1 1 calc R . . N8 N 1.1888(5) 0.1129(4) -0.0174(2) 0.0435(15) Uani 1 1 d . . . C21 C 0.8278(5) 0.4680(4) 0.0410(2) 0.0254(12) Uani 1 1 d . . . C20 C 0.8483(4) 0.3627(4) 0.0166(2) 0.0234(12) Uani 1 1 d . . . H20 H 0.8612 0.3479 -0.0193 0.028 Uiso 1 1 calc R . . C14 C -0.0401(6) 0.0159(5) 0.3435(2) 0.0404(15) Uani 1 1 d . . . H14 H -0.1100 0.0566 0.3423 0.048 Uiso 1 1 calc R . . C35 C 1.0985(7) 0.5146(6) 0.2514(3) 0.065(2) Uani 1 1 d . . . H35 H 1.1731 0.5629 0.2647 0.078 Uiso 1 1 calc R . . C24 C 0.8289(5) 0.3014(4) 0.0980(2) 0.0294(13) Uani 1 1 d . . . H24 H 0.8300 0.2457 0.1172 0.035 Uiso 1 1 calc R . . C3 C 0.3126(5) 0.0223(4) 0.4401(2) 0.0266(12) Uani 1 1 d . . . C31 C 0.6130(6) 0.6275(5) -0.0089(3) 0.0423(16) Uani 1 1 d . . . H31 H 0.6140 0.6798 0.0221 0.051 Uiso 1 1 calc R . . C13 C 0.0488(5) 0.0253(4) 0.3838(2) 0.0386(15) Uani 1 1 d . . . H13 H 0.0515 0.0729 0.4164 0.046 Uiso 1 1 calc R . . C22 C 0.8071(5) 0.4884(4) 0.0942(2) 0.0276(13) Uani 1 1 d . . . H22 H 0.7938 0.5586 0.1108 0.033 Uiso 1 1 calc R . . N2 N 0.4785(5) 0.3329(4) 0.3158(2) 0.0553(15) Uani 1 1 d . . . H2 H 0.4443 0.3539 0.2891 0.066 Uiso 1 1 calc R . . N12 N 1.0747(5) 0.4069(5) 0.2550(2) 0.0591(16) Uani 1 1 d . . . H12A H 1.1282 0.3709 0.2692 0.071 Uiso 1 1 calc R . . C7 C 0.4978(5) 0.3095(4) 0.4511(2) 0.0391(15) Uani 1 1 d . . . H7A H 0.4457 0.3673 0.4645 0.047 Uiso 1 1 calc R . . H7B H 0.5837 0.3279 0.4698 0.047 Uiso 1 1 calc R . . C2 C 0.3710(5) 0.1171(4) 0.4252(2) 0.0305(13) Uani 1 1 d . . . H2A H 0.3673 0.1227 0.3898 0.037 Uiso 1 1 calc R . . C11 C 0.5830(6) 0.2740(5) 0.3158(3) 0.0439(17) Uani 1 1 d . . . H11 H 0.6304 0.2502 0.2869 0.053 Uiso 1 1 calc R . . C19 C 0.8499(5) 0.2802(4) 0.0448(2) 0.0238(12) Uani 1 1 d . . . C29 C 1.2091(6) 0.1270(5) 0.0360(3) 0.0514(18) Uani 1 1 d . . . H29 H 1.2866 0.1228 0.0551 0.062 Uiso 1 1 calc R . . C26 C 0.8284(5) 0.5588(4) 0.0096(2) 0.0299(13) Uani 1 1 d . . . H26A H 0.8470 0.6288 0.0339 0.036 Uiso 1 1 calc R . . H26B H 0.8988 0.5528 -0.0141 0.036 Uiso 1 1 calc R . . C10 C 0.6041(5) 0.2572(4) 0.3647(3) 0.0397(16) Uani 1 1 d . . . H10 H 0.6685 0.2190 0.3762 0.048 Uiso 1 1 calc R . . N10 N 0.5563(6) 0.5232(5) -0.0854(2) 0.0643(17) Uani 1 1 d . . . H10A H 0.5125 0.4934 -0.1147 0.077 Uiso 1 1 calc R . . O41 O 0.6213(6) 0.6156(4) 0.7757(2) 0.0830(17) Uani 1 1 d G . . H41A H 0.6250 0.6713 0.8007 0.124 Uiso 1 1 d G . . H41B H 0.5485 0.5758 0.7750 0.124 Uiso 1 1 d G . . C32 C 0.5219(6) 0.6065(5) -0.0489(3) 0.0507(18) Uani 1 1 d . . . H32 H 0.4482 0.6423 -0.0513 0.061 Uiso 1 1 calc R . . C36 C 0.9571(7) 0.3672(5) 0.2334(2) 0.0465(17) Uani 1 1 d . . . H36 H 0.9167 0.2964 0.2323 0.056 Uiso 1 1 calc R . . C5 C 0.3775(5) 0.1011(5) 0.5313(2) 0.0358(14) Uani 1 1 d . . . C12 C 0.4396(7) 0.3518(5) 0.3649(3) 0.0532(18) Uani 1 1 d . . . H12 H 0.3708 0.3909 0.3758 0.064 Uiso 1 1 calc R . . C4 C 0.3160(5) 0.0173(4) 0.4927(2) 0.0353(14) Uani 1 1 d . . . H4A H 0.2752 -0.0451 0.5026 0.042 Uiso 1 1 calc R . . C28 C 1.0945(5) 0.1481(5) 0.0555(2) 0.0450(16) Uani 1 1 d . . . H28 H 1.0774 0.1612 0.0910 0.054 Uiso 1 1 calc R . . C9 C 0.3791(6) 0.0927(5) 0.5889(2) 0.0490(17) Uani 1 1 d . . . H9A H 0.3334 0.0225 0.5922 0.059 Uiso 1 1 calc R . . H9B H 0.4689 0.0968 0.6030 0.059 Uiso 1 1 calc R . . C33 C 0.6667(6) 0.4957(5) -0.0686(3) 0.0544(19) Uani 1 1 d . . . H33 H 0.7114 0.4412 -0.0867 0.065 Uiso 1 1 calc R . . C6 C 0.4377(5) 0.1942(4) 0.5160(2) 0.0349(14) Uani 1 1 d . . . H6 H 0.4806 0.2513 0.5416 0.042 Uiso 1 1 calc R . . C34 C 0.9942(7) 0.5367(5) 0.2252(3) 0.058(2) Uani 1 1 d . . . H34 H 0.9833 0.6038 0.2161 0.069 Uiso 1 1 calc R . . N6 N 0.1722(6) 0.2863(5) 0.6436(3) 0.073(2) Uani 1 1 d . . . H6A H 0.0985 0.3122 0.6464 0.088 Uiso 1 1 calc R . . C18 C 0.1966(6) 0.2022(6) 0.6099(3) 0.0516(18) Uani 1 1 d . . . H18 H 0.1380 0.1622 0.5827 0.062 Uiso 1 1 calc R . . C16 C 0.3745(9) 0.2598(7) 0.6600(3) 0.0870(19) Uani 1 1 d . . . H16 H 0.4594 0.2657 0.6751 0.104 Uiso 1 1 calc R . . C17 C 0.2847(9) 0.3261(7) 0.6738(3) 0.0870(19) Uani 1 1 d U . . H17 H 0.2969 0.3895 0.6998 0.104 Uiso 1 1 calc R . . H8 H 1.244(6) 0.102(5) -0.034(2) 0.05(2) Uiso 1 1 d . . . O42 O 0.167(2) 0.393(2) 0.1287(9) 0.152(11) Uani 0.30 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo4 0.0186(2) 0.0224(2) 0.0170(2) 0.00239(18) 0.00115(18) 0.00360(18) Mo5 0.0256(2) 0.0214(2) 0.0260(3) 0.0076(2) 0.0014(2) -0.00114(19) Mo6 0.0226(2) 0.0187(2) 0.0165(2) 0.00267(18) 0.00245(18) 0.00363(18) Mo8 0.0199(2) 0.0181(2) 0.0238(3) 0.00069(19) 0.00147(19) 0.00514(17) Mo2 0.0200(2) 0.0229(2) 0.0272(3) 0.0032(2) 0.00314(19) 0.00572(18) Mo1 0.0198(2) 0.0270(2) 0.0228(3) 0.0001(2) 0.00205(19) 0.00034(19) Mo3 0.0231(2) 0.0247(2) 0.0276(3) 0.0114(2) 0.0021(2) 0.00149(19) Mo7 0.0197(2) 0.0205(2) 0.0269(3) 0.00414(19) 0.00077(19) 0.00144(18) Mo9 0.0220(2) 0.0214(2) 0.0243(3) 0.00363(19) 0.00360(19) 0.00601(18) Mo11 0.0322(3) 0.0254(2) 0.0265(3) 0.0053(2) 0.0070(2) 0.0026(2) Mo12 0.0311(3) 0.0253(2) 0.0221(3) 0.0032(2) 0.0035(2) 0.0042(2) Mo10 0.0303(3) 0.0194(2) 0.0267(3) 0.0046(2) 0.0037(2) 0.00354(19) O28 0.031(2) 0.035(2) 0.037(2) 0.0116(18) 0.0000(17) 0.0137(16) O16 0.037(2) 0.041(2) 0.033(2) 0.0144(19) 0.0044(18) -0.0030(18) O36 0.053(2) 0.030(2) 0.032(2) 0.0108(18) 0.0070(19) 0.0046(18) O24 0.0266(19) 0.034(2) 0.029(2) 0.0037(17) 0.0053(16) 0.0086(16) O33 0.044(2) 0.033(2) 0.041(3) 0.0137(19) -0.0025(19) 0.0080(18) O3 0.0257(19) 0.0192(18) 0.035(2) -0.0002(16) 0.0029(16) -0.0006(15) O1 0.032(2) 0.033(2) 0.033(2) 0.0049(18) 0.0099(17) 0.0026(16) O26 0.0230(19) 0.032(2) 0.023(2) -0.0003(16) 0.0006(15) -0.0018(15) O5 0.029(2) 0.037(2) 0.034(2) 0.0032(18) 0.0108(17) 0.0061(17) O38 0.043(2) 0.032(2) 0.030(2) -0.0006(18) 0.0058(18) 0.0032(17) O23 0.0215(18) 0.0207(18) 0.032(2) 0.0029(16) -0.0016(15) 0.0036(14) O12 0.0260(19) 0.0200(17) 0.027(2) 0.0063(15) 0.0016(16) -0.0002(14) O21 0.035(2) 0.041(2) 0.035(2) 0.0110(19) 0.0124(18) 0.0096(17) O20 0.0254(19) 0.0222(18) 0.025(2) 0.0007(16) -0.0017(15) 0.0035(14) O39 0.044(2) 0.042(2) 0.033(2) 0.0129(19) 0.0010(19) 0.0111(18) O31 0.0267(19) 0.0218(18) 0.025(2) 0.0042(16) 0.0010(15) 0.0012(15) O18 0.0212(17) 0.0184(17) 0.021(2) 0.0043(15) -0.0015(14) 0.0020(14) O7 0.0199(18) 0.0201(17) 0.024(2) 0.0026(15) 0.0057(15) 0.0026(14) O2 0.026(2) 0.043(2) 0.032(2) -0.0036(19) -0.0004(17) -0.0030(17) O11 0.038(2) 0.050(2) 0.028(2) 0.0128(19) 0.0066(18) -0.0064(19) O9 0.0194(17) 0.0174(17) 0.028(2) 0.0057(15) 0.0031(15) 0.0010(14) O8 0.0189(17) 0.0212(17) 0.022(2) 0.0080(15) 0.0015(14) 0.0043(14) O27 0.0270(19) 0.0204(17) 0.025(2) 0.0006(15) 0.0069(15) 0.0052(14) O13 0.0215(18) 0.0191(17) 0.021(2) 0.0055(15) 0.0038(15) 0.0034(14) O34 0.026(2) 0.0286(19) 0.033(2) 0.0052(17) 0.0064(17) -0.0022(15) O4 0.0205(18) 0.033(2) 0.029(2) 0.0067(17) -0.0017(15) 0.0073(15) O19 0.040(2) 0.031(2) 0.022(2) 0.0045(16) 0.0092(17) 0.0052(16) O15 0.0225(18) 0.0187(17) 0.022(2) 0.0011(15) 0.0017(15) 0.0010(14) O6 0.031(2) 0.029(2) 0.046(3) 0.0099(18) 0.0017(18) 0.0110(16) O14 0.033(2) 0.037(2) 0.023(2) 0.0060(17) 0.0081(17) 0.0059(17) O32 0.038(2) 0.0256(19) 0.036(2) 0.0034(17) 0.0043(18) 0.0002(16) O29 0.0255(18) 0.0199(17) 0.022(2) 0.0058(15) 0.0026(15) 0.0064(14) O10 0.034(2) 0.031(2) 0.059(3) 0.021(2) 0.002(2) 0.0070(17) O30 0.0262(19) 0.0281(19) 0.031(2) 0.0073(17) 0.0080(16) 0.0081(15) O22 0.030(2) 0.0261(19) 0.046(3) 0.0059(18) -0.0045(18) -0.0005(16) O17 0.041(2) 0.0183(19) 0.061(3) 0.0141(19) 0.002(2) 0.0029(16) O25 0.035(2) 0.0226(19) 0.044(3) 0.0089(17) 0.0038(18) 0.0123(16) O35 0.038(2) 0.046(2) 0.045(3) 0.009(2) 0.017(2) 0.0033(19) O37 0.037(2) 0.0263(19) 0.028(2) 0.0015(17) 0.0117(17) 0.0041(16) N3 0.033(3) 0.024(2) 0.024(3) 0.001(2) 0.002(2) 0.0036(19) N9 0.036(3) 0.023(2) 0.028(3) 0.008(2) -0.002(2) 0.006(2) N4 0.038(3) 0.039(3) 0.030(3) 0.007(2) -0.005(2) 0.004(2) N7 0.029(2) 0.028(2) 0.028(3) 0.005(2) 0.007(2) 0.0110(19) N1 0.027(3) 0.025(2) 0.047(3) 0.007(2) 0.007(2) 0.001(2) N11 0.066(4) 0.028(3) 0.017(3) 0.003(2) -0.001(2) -0.007(3) C8 0.035(3) 0.027(3) 0.037(4) 0.003(3) 0.002(3) 0.003(2) O40 0.052(3) 0.049(3) 0.074(4) -0.016(3) 0.014(3) 0.009(2) C15 0.045(4) 0.027(3) 0.022(3) 0.002(2) 0.007(3) 0.003(3) N5 0.038(3) 0.040(3) 0.025(3) 0.011(2) -0.005(2) 0.009(2) C25 0.025(3) 0.023(3) 0.035(3) 0.004(2) 0.008(2) 0.003(2) C23 0.030(3) 0.027(3) 0.024(3) 0.003(2) 0.006(2) -0.001(2) C27 0.061(4) 0.028(3) 0.027(4) 0.005(3) 0.012(3) 0.009(3) C1 0.024(3) 0.029(3) 0.034(4) 0.003(3) 0.001(2) 0.003(2) C30 0.044(4) 0.036(3) 0.029(4) 0.016(3) 0.013(3) 0.017(3) N8 0.042(4) 0.048(3) 0.050(4) 0.020(3) 0.025(3) 0.016(3) C21 0.023(3) 0.024(3) 0.029(3) 0.007(2) -0.002(2) -0.001(2) C20 0.020(3) 0.029(3) 0.019(3) 0.001(2) -0.002(2) 0.002(2) C14 0.041(4) 0.041(3) 0.041(4) 0.006(3) 0.006(3) 0.017(3) C35 0.068(5) 0.079(6) 0.036(5) 0.008(4) -0.006(4) -0.033(5) C24 0.029(3) 0.028(3) 0.034(4) 0.012(3) 0.006(3) 0.001(2) C3 0.026(3) 0.029(3) 0.026(3) 0.007(2) 0.004(2) 0.005(2) C31 0.045(4) 0.036(3) 0.042(4) -0.003(3) 0.002(3) 0.006(3) C13 0.044(4) 0.040(3) 0.030(4) -0.005(3) 0.001(3) 0.017(3) C22 0.032(3) 0.022(3) 0.027(3) 0.002(2) 0.001(2) 0.004(2) N2 0.070(4) 0.057(4) 0.046(4) 0.024(3) 0.000(3) 0.018(3) N12 0.065(4) 0.073(4) 0.035(4) 0.009(3) -0.010(3) -0.002(3) C7 0.036(3) 0.033(3) 0.044(4) 0.001(3) 0.000(3) 0.000(3) C2 0.031(3) 0.039(3) 0.020(3) 0.003(3) 0.003(2) 0.004(3) C11 0.046(4) 0.043(4) 0.044(4) 0.009(3) 0.014(3) 0.003(3) C19 0.024(3) 0.022(3) 0.025(3) 0.003(2) 0.001(2) 0.004(2) C29 0.034(4) 0.073(5) 0.047(5) 0.011(4) -0.003(3) 0.013(3) C26 0.028(3) 0.030(3) 0.033(3) 0.008(3) -0.004(2) 0.005(2) C10 0.026(3) 0.038(3) 0.058(5) 0.012(3) 0.006(3) 0.007(3) N10 0.073(4) 0.065(4) 0.049(4) 0.004(3) -0.030(3) 0.009(3) O41 0.139(5) 0.054(3) 0.059(4) 0.018(3) 0.009(4) 0.014(3) C32 0.046(4) 0.045(4) 0.063(5) 0.017(4) -0.008(4) 0.007(3) C36 0.071(5) 0.035(4) 0.030(4) 0.002(3) 0.002(3) -0.002(3) C5 0.042(3) 0.045(4) 0.025(3) 0.011(3) 0.002(3) 0.015(3) C12 0.064(5) 0.054(4) 0.047(5) 0.008(4) 0.010(4) 0.028(3) C4 0.036(3) 0.033(3) 0.042(4) 0.017(3) 0.008(3) 0.006(3) C28 0.039(4) 0.067(4) 0.029(4) 0.004(3) -0.003(3) 0.019(3) C9 0.066(4) 0.054(4) 0.031(4) 0.010(3) 0.001(3) 0.023(3) C33 0.065(5) 0.050(4) 0.041(4) -0.013(3) -0.014(3) 0.021(3) C6 0.036(3) 0.037(3) 0.028(4) -0.004(3) -0.007(3) 0.009(3) C34 0.094(6) 0.035(4) 0.039(4) 0.010(3) 0.002(4) -0.022(4) N6 0.081(5) 0.094(5) 0.073(5) 0.051(4) 0.037(4) 0.061(4) C18 0.045(4) 0.058(4) 0.059(5) 0.028(4) -0.006(3) 0.010(3) C16 0.111(5) 0.096(4) 0.052(4) -0.006(3) -0.008(3) 0.040(3) C17 0.111(5) 0.096(4) 0.052(4) -0.006(3) -0.008(3) 0.040(3) O42 0.132(19) 0.20(2) 0.11(2) 0.023(18) 0.031(16) -0.047(18) _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 Mo4 Mo3 3.2146(6) . ? Mo4 O26 1.743(3) . ? Mo4 O7 2.376(3) . ? Mo4 O8 1.954(3) . ? Mo4 O13 2.130(3) . ? Mo4 O15 1.946(3) . ? Mo4 O14 1.694(3) . ? Mo5 O16 1.693(3) . ? Mo5 O3 1.897(3) . ? Mo5 O18 1.990(3) . ? Mo5 O7 2.272(3) . ? Mo5 O15 2.341(3) . ? Mo5 O17 1.716(4) . ? Mo6 O20 1.740(3) . ? Mo6 O18 1.965(3) . ? Mo6 O7 2.177(3) . ? Mo6 O9 1.944(3) . ? Mo6 O13 2.376(3) . ? Mo6 O19 1.692(3) . ? Mo8 O24 1.704(3) . ? Mo8 O23 1.897(3) . ? Mo8 O18 2.299(3) . ? Mo8 O13 2.345(3) . ? Mo8 O15 2.014(3) . ? Mo8 O25 1.692(4) . ? Mo2 O5 1.701(3) . ? Mo2 O7 2.354(3) . ? Mo2 O9 2.007(3) . ? Mo2 O8 2.331(3) . ? Mo2 O4 1.906(3) . ? Mo2 O6 1.691(4) . ? Mo1 O3 1.927(4) . ? Mo1 O1 1.697(3) . ? Mo1 O26 2.317(3) . ? Mo1 O7 2.466(3) . ? Mo1 O2 1.699(3) . ? Mo1 O4 1.909(3) . ? Mo3 O12 1.903(3) . ? Mo3 O11 1.695(3) . ? Mo3 O9 2.327(3) . ? Mo3 O8 1.993(3) . ? Mo3 O13 2.366(3) . ? Mo3 O10 1.705(4) . ? Mo7 O23 1.930(3) . ? Mo7 O12 1.934(3) . ? Mo7 O21 1.700(3) . ? Mo7 O20 2.320(3) . ? Mo7 O13 2.393(3) . ? Mo7 O22 1.689(3) . ? Mo9 O28 1.677(4) . ? Mo9 O31 1.957(3) . ? Mo9 O27 1.956(3) . ? Mo9 O29 2.128(3) . ? Mo9 O29 2.420(3) 2_766 ? Mo9 O30 1.756(3) . ? Mo11 O36 1.718(4) . ? Mo11 O34 1.925(3) . ? Mo11 O29 2.436(3) 2_766 ? Mo11 O30 2.297(4) . ? Mo11 O35 1.691(3) . ? Mo11 O37 1.916(3) . ? Mo12 O38 1.701(3) . ? Mo12 O39 1.694(4) . ? Mo12 O31 1.984(3) . ? Mo12 O27 2.359(4) 2_766 ? Mo12 O29 2.345(3) . ? Mo12 O37 1.907(3) 2_766 ? Mo10 O33 1.701(4) . ? Mo10 O31 2.358(4) . ? Mo10 O27 1.982(3) 2_766 ? Mo10 O34 1.897(3) . ? Mo10 O32 1.697(3) . ? Mo10 O29 2.349(3) 2_766 ? O27 Mo12 2.359(4) 2_766 ? O27 Mo10 1.982(3) 2_766 ? O29 Mo9 2.420(3) 2_766 ? O29 Mo11 2.436(3) 2_766 ? O29 Mo10 2.349(3) 2_766 ? O37 Mo12 1.907(3) 2_766 ? N3 C8 1.471(7) . ? N3 C15 1.311(6) . ? N3 C13 1.375(6) . ? N9 C31 1.370(7) . ? N9 C26 1.473(6) . ? N9 C33 1.323(7) . ? N4 H4 0.8600 . ? N4 C15 1.306(7) . ? N4 C14 1.364(6) . ? N7 C25 1.476(6) . ? N7 C30 1.314(6) . ? N7 C28 1.357(7) . ? N1 C7 1.452(7) . ? N1 C10 1.386(6) . ? N1 C12 1.303(8) . ? N11 C27 1.451(7) . ? N11 C36 1.320(8) . ? N11 C34 1.374(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C3 1.499(7) . ? O40 H40A 0.8499 . ? O40 H40B 0.8499 . ? C15 H15 0.9300 . ? N5 C9 1.467(7) . ? N5 C18 1.310(7) . ? N5 C16 1.356(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 C19 1.520(6) . ? C23 C27 1.512(7) . ? C23 C24 1.398(7) . ? C23 C22 1.385(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C1 C7 1.506(7) . ? C1 C2 1.401(7) . ? C1 C6 1.378(8) . ? C30 H30 0.9300 . ? C30 N8 1.308(8) . ? N8 C29 1.361(8) . ? N8 H8 0.74(5) . ? C21 C20 1.392(6) . ? C21 C22 1.379(7) . ? C21 C26 1.517(7) . ? C20 H20 0.9300 . ? C20 C19 1.374(7) . ? C14 H14 0.9300 . ? C14 C13 1.334(8) . ? C35 H35 0.9300 . ? C35 N12 1.364(8) . ? C35 C34 1.328(10) . ? C24 H24 0.9300 . ? C24 C19 1.380(7) . ? C3 C2 1.398(6) . ? C3 C4 1.370(7) . ? C31 H31 0.9300 . ? C31 C32 1.329(8) . ? C13 H13 0.9300 . ? C22 H22 0.9300 . ? N2 H2 0.8600 . ? N2 C11 1.372(8) . ? N2 C12 1.332(8) . ? N12 H12A 0.8600 . ? N12 C36 1.313(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C2 H2A 0.9300 . ? C11 H11 0.9300 . ? C11 C10 1.332(8) . ? C29 H29 0.9300 . ? C29 C28 1.339(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C10 H10 0.9300 . ? N10 H10A 0.8600 . ? N10 C32 1.356(8) . ? N10 C33 1.304(8) . ? O41 H41A 0.8500 . ? O41 H41B 0.8500 . ? C32 H32 0.9300 . ? C36 H36 0.9300 . ? C5 C4 1.376(7) . ? C5 C9 1.511(8) . ? C5 C6 1.391(7) . ? C12 H12 0.9300 . ? C4 H4A 0.9300 . ? C28 H28 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C33 H33 0.9300 . ? C6 H6 0.9300 . ? C34 H34 0.9300 . ? N6 H6A 0.8600 . ? N6 C18 1.287(8) . ? N6 C17 1.356(9) . ? C18 H18 0.9300 . ? C16 H16 0.9300 . ? C16 C17 1.327(10) . ? C17 H17 0.9300 . ? 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 O26 Mo4 Mo3 131.78(12) . . ? O26 Mo4 O7 80.99(13) . . ? O26 Mo4 O8 95.90(14) . . ? O26 Mo4 O13 157.11(13) . . ? O26 Mo4 O15 95.79(14) . . ? O7 Mo4 Mo3 86.53(7) . . ? O8 Mo4 Mo3 35.88(8) . . ? O8 Mo4 O7 77.84(12) . . ? O8 Mo4 O13 79.51(12) . . ? O13 Mo4 Mo3 47.38(9) . . ? O13 Mo4 O7 76.12(11) . . ? O15 Mo4 Mo3 126.56(9) . . ? O15 Mo4 O7 77.42(12) . . ? O15 Mo4 O8 150.52(13) . . ? O15 Mo4 O13 79.22(12) . . ? O14 Mo4 Mo3 89.58(11) . . ? O14 Mo4 O26 105.19(16) . . ? O14 Mo4 O7 173.80(14) . . ? O14 Mo4 O8 101.71(15) . . ? O14 Mo4 O13 97.70(14) . . ? O14 Mo4 O15 101.17(15) . . ? O16 Mo5 O3 101.74(15) . . ? O16 Mo5 O18 97.35(14) . . ? O16 Mo5 O7 95.86(15) . . ? O16 Mo5 O15 165.64(13) . . ? O16 Mo5 O17 106.00(19) . . ? O3 Mo5 O18 147.66(14) . . ? O3 Mo5 O7 78.01(13) . . ? O3 Mo5 O15 84.15(12) . . ? O18 Mo5 O7 74.26(12) . . ? O18 Mo5 O15 71.91(11) . . ? O7 Mo5 O15 72.36(11) . . ? O17 Mo5 O3 98.39(16) . . ? O17 Mo5 O18 101.12(15) . . ? O17 Mo5 O7 158.10(15) . . ? O17 Mo5 O15 85.82(15) . . ? O20 Mo6 O18 96.65(14) . . ? O20 Mo6 O7 155.93(13) . . ? O20 Mo6 O9 97.53(14) . . ? O20 Mo6 O13 80.69(13) . . ? O18 Mo6 O7 76.96(12) . . ? O18 Mo6 O13 77.25(12) . . ? O7 Mo6 O13 75.27(10) . . ? O9 Mo6 O18 148.46(13) . . ? O9 Mo6 O7 78.64(12) . . ? O9 Mo6 O13 77.45(12) . . ? O19 Mo6 O20 105.00(16) . . ? O19 Mo6 O18 100.18(15) . . ? O19 Mo6 O7 98.99(14) . . ? O19 Mo6 O9 103.11(15) . . ? O19 Mo6 O13 174.07(13) . . ? O24 Mo8 O23 102.22(14) . . ? O24 Mo8 O18 162.40(15) . . ? O24 Mo8 O13 94.38(14) . . ? O24 Mo8 O15 93.27(14) . . ? O23 Mo8 O18 85.91(12) . . ? O23 Mo8 O13 77.34(13) . . ? O23 Mo8 O15 147.32(13) . . ? O18 Mo8 O13 71.96(11) . . ? O15 Mo8 O18 72.42(11) . . ? O15 Mo8 O13 72.88(11) . . ? O25 Mo8 O24 105.15(17) . . ? O25 Mo8 O23 101.76(16) . . ? O25 Mo8 O18 88.13(14) . . ? O25 Mo8 O13 160.09(14) . . ? O25 Mo8 O15 101.66(14) . . ? O5 Mo2 O7 91.77(15) . . ? O5 Mo2 O9 96.13(15) . . ? O5 Mo2 O8 161.34(16) . . ? O5 Mo2 O4 102.24(15) . . ? O9 Mo2 O7 73.27(11) . . ? O9 Mo2 O8 71.46(12) . . ? O8 Mo2 O7 71.57(11) . . ? O4 Mo2 O7 77.57(13) . . ? O4 Mo2 O9 145.83(13) . . ? O4 Mo2 O8 82.79(12) . . ? O6 Mo2 O5 104.93(17) . . ? O6 Mo2 O7 162.59(14) . . ? O6 Mo2 O9 99.58(14) . . ? O6 Mo2 O8 91.16(14) . . ? O6 Mo2 O4 103.09(16) . . ? O3 Mo1 O26 77.04(13) . . ? O3 Mo1 O7 72.71(11) . . ? O1 Mo1 O3 97.87(16) . . ? O1 Mo1 O26 166.19(14) . . ? O1 Mo1 O7 97.10(13) . . ? O1 Mo1 O2 105.10(16) . . ? O1 Mo1 O4 100.38(15) . . ? O26 Mo1 O7 69.17(10) . . ? O2 Mo1 O3 101.54(16) . . ? O2 Mo1 O26 88.57(13) . . ? O2 Mo1 O7 157.68(13) . . ? O2 Mo1 O4 102.98(17) . . ? O4 Mo1 O3 144.25(12) . . ? O4 Mo1 O26 77.98(13) . . ? O4 Mo1 O7 74.71(12) . . ? O12 Mo3 Mo4 118.48(10) . . ? O12 Mo3 O9 83.16(12) . . ? O12 Mo3 O8 145.89(14) . . ? O12 Mo3 O13 77.00(12) . . ? O11 Mo3 Mo4 83.16(11) . . ? O11 Mo3 O12 101.15(16) . . ? O11 Mo3 O9 161.14(14) . . ? O11 Mo3 O8 96.12(14) . . ? O11 Mo3 O13 91.96(15) . . ? O11 Mo3 O10 105.31(19) . . ? O9 Mo3 Mo4 78.72(7) . . ? O9 Mo3 O13 70.95(11) . . ? O8 Mo3 Mo4 35.08(9) . . ? O8 Mo3 O9 71.79(11) . . ? O8 Mo3 O13 73.19(12) . . ? O13 Mo3 Mo4 41.49(7) . . ? O10 Mo3 Mo4 137.06(12) . . ? O10 Mo3 O12 101.38(16) . . ? O10 Mo3 O9 91.62(15) . . ? O10 Mo3 O8 102.09(15) . . ? O10 Mo3 O13 162.57(15) . . ? O23 Mo7 O12 146.33(12) . . ? O23 Mo7 O20 76.46(12) . . ? O23 Mo7 O13 75.54(12) . . ? O12 Mo7 O20 77.51(13) . . ? O12 Mo7 O13 75.76(11) . . ? O21 Mo7 O23 100.79(15) . . ? O21 Mo7 O12 97.97(16) . . ? O21 Mo7 O20 163.18(14) . . ? O21 Mo7 O13 93.08(14) . . ? O20 Mo7 O13 70.13(11) . . ? O22 Mo7 O23 100.74(16) . . ? O22 Mo7 O12 100.92(15) . . ? O22 Mo7 O21 105.31(17) . . ? O22 Mo7 O20 91.48(14) . . ? O22 Mo7 O13 161.61(14) . . ? O28 Mo9 O31 101.58(16) . . ? O28 Mo9 O27 101.56(16) . . ? O28 Mo9 O29 175.48(13) . 2_766 ? O28 Mo9 O29 99.73(15) . . ? O28 Mo9 O30 104.47(16) . . ? O31 Mo9 O29 77.63(13) . 2_766 ? O31 Mo9 O29 78.47(11) . . ? O27 Mo9 O31 149.65(14) . . ? O27 Mo9 O29 78.50(12) . . ? O27 Mo9 O29 77.75(12) . 2_766 ? O29 Mo9 O29 75.76(13) . 2_766 ? O30 Mo9 O31 96.16(13) . . ? O30 Mo9 O27 96.78(14) . . ? O30 Mo9 O29 80.04(14) . 2_766 ? O30 Mo9 O29 155.79(16) . . ? O36 Mo11 O34 98.89(16) . . ? O36 Mo11 O29 92.27(14) . 2_766 ? O36 Mo11 O30 162.74(13) . . ? O36 Mo11 O37 98.49(16) . . ? O34 Mo11 O29 74.53(11) . 2_766 ? O34 Mo11 O30 77.59(14) . . ? O30 Mo11 O29 70.48(11) . 2_766 ? O35 Mo11 O36 105.60(18) . . ? O35 Mo11 O34 102.17(16) . . ? O35 Mo11 O29 162.13(17) . 2_766 ? O35 Mo11 O30 91.65(17) . . ? O35 Mo11 O37 102.04(15) . . ? O37 Mo11 O34 145.01(14) . . ? O37 Mo11 O29 74.65(11) . 2_766 ? O37 Mo11 O30 76.84(14) . . ? O38 Mo12 O31 101.96(14) . . ? O38 Mo12 O27 87.64(15) . 2_766 ? O38 Mo12 O29 159.79(16) . . ? O38 Mo12 O37 100.34(15) . 2_766 ? O39 Mo12 O38 104.05(19) . . ? O39 Mo12 O31 99.28(15) . . ? O39 Mo12 O27 166.86(14) . 2_766 ? O39 Mo12 O29 96.11(15) . . ? O39 Mo12 O37 100.48(16) . 2_766 ? O31 Mo12 O27 71.99(13) . 2_766 ? O31 Mo12 O29 72.87(11) . . ? O29 Mo12 O27 72.16(11) . 2_766 ? O37 Mo12 O31 145.46(14) 2_766 . ? O37 Mo12 O27 82.98(14) 2_766 2_766 ? O37 Mo12 O29 77.08(12) 2_766 . ? O33 Mo10 O31 166.51(13) . . ? O33 Mo10 O27 97.97(15) . 2_766 ? O33 Mo10 O34 100.80(17) . . ? O33 Mo10 O29 96.67(15) . 2_766 ? O27 Mo10 O31 72.04(13) 2_766 . ? O27 Mo10 O29 72.81(11) 2_766 2_766 ? O34 Mo10 O31 84.12(13) . . ? O34 Mo10 O27 146.12(13) . 2_766 ? O34 Mo10 O29 77.18(11) . 2_766 ? O32 Mo10 O33 104.15(17) . . ? O32 Mo10 O31 87.12(15) . . ? O32 Mo10 O27 102.21(14) . 2_766 ? O32 Mo10 O34 100.20(15) . . ? O32 Mo10 O29 159.10(16) . 2_766 ? O29 Mo10 O31 72.01(11) 2_766 . ? Mo5 O3 Mo1 117.18(15) . . ? Mo4 O26 Mo1 117.66(16) . . ? Mo8 O23 Mo7 115.64(18) . . ? Mo3 O12 Mo7 115.20(15) . . ? Mo6 O20 Mo7 116.15(16) . . ? Mo9 O31 Mo12 109.99(13) . . ? Mo9 O31 Mo10 110.90(15) . . ? Mo12 O31 Mo10 103.07(14) . . ? Mo5 O18 Mo8 104.55(13) . . ? Mo6 O18 Mo5 109.09(15) . . ? Mo6 O18 Mo8 111.02(13) . . ? Mo4 O7 Mo1 92.14(11) . . ? Mo5 O7 Mo4 98.12(11) . . ? Mo5 O7 Mo2 163.06(14) . . ? Mo5 O7 Mo1 86.99(9) . . ? Mo6 O7 Mo4 103.56(11) . . ? Mo6 O7 Mo5 92.77(13) . . ? Mo6 O7 Mo2 91.00(10) . . ? Mo6 O7 Mo1 164.16(14) . . ? Mo2 O7 Mo4 97.03(12) . . ? Mo2 O7 Mo1 84.91(11) . . ? Mo6 O9 Mo2 109.87(13) . . ? Mo6 O9 Mo3 112.00(13) . . ? Mo2 O9 Mo3 103.25(14) . . ? Mo4 O8 Mo2 111.23(13) . . ? Mo4 O8 Mo3 109.04(15) . . ? Mo3 O8 Mo2 103.55(13) . . ? Mo9 O27 Mo12 110.68(14) . 2_766 ? Mo9 O27 Mo10 110.16(15) . 2_766 ? Mo10 O27 Mo12 103.15(14) 2_766 2_766 ? Mo4 O13 Mo6 105.03(11) . . ? Mo4 O13 Mo8 92.45(10) . . ? Mo4 O13 Mo3 91.13(12) . . ? Mo4 O13 Mo7 161.95(15) . . ? Mo6 O13 Mo7 93.00(11) . . ? Mo8 O13 Mo6 96.42(12) . . ? Mo8 O13 Mo3 164.87(14) . . ? Mo8 O13 Mo7 86.25(11) . . ? Mo3 O13 Mo6 96.84(11) . . ? Mo3 O13 Mo7 85.80(9) . . ? Mo10 O34 Mo11 117.34(15) . . ? Mo2 O4 Mo1 117.10(18) . . ? Mo4 O15 Mo5 109.66(13) . . ? Mo4 O15 Mo8 109.49(13) . . ? Mo8 O15 Mo5 102.30(14) . . ? Mo9 O29 Mo9 104.24(13) . 2_766 ? Mo9 O29 Mo11 164.13(17) . 2_766 ? Mo9 O29 Mo11 91.62(11) 2_766 2_766 ? Mo9 O29 Mo12 92.27(10) . . ? Mo9 O29 Mo10 92.15(11) . 2_766 ? Mo12 O29 Mo9 96.53(11) . 2_766 ? Mo12 O29 Mo11 85.72(10) . 2_766 ? Mo12 O29 Mo10 164.65(16) . 2_766 ? Mo10 O29 Mo9 96.62(12) 2_766 2_766 ? Mo10 O29 Mo11 86.02(9) 2_766 2_766 ? Mo9 O30 Mo11 117.85(16) . . ? Mo12 O37 Mo11 116.64(16) 2_766 . ? C15 N3 C8 124.2(5) . . ? C15 N3 C13 107.7(5) . . ? C13 N3 C8 128.0(5) . . ? C31 N9 C26 125.4(5) . . ? C33 N9 C31 107.5(5) . . ? C33 N9 C26 127.0(5) . . ? C15 N4 H4 125.7 . . ? C15 N4 C14 108.7(5) . . ? C14 N4 H4 125.7 . . ? C30 N7 C25 125.6(5) . . ? C30 N7 C28 108.1(5) . . ? C28 N7 C25 126.3(5) . . ? C10 N1 C7 126.7(6) . . ? C12 N1 C7 125.5(5) . . ? C12 N1 C10 107.8(5) . . ? C36 N11 C27 125.5(5) . . ? C36 N11 C34 107.0(6) . . ? C34 N11 C27 127.2(6) . . ? N3 C8 H8A 108.6 . . ? N3 C8 H8B 108.6 . . ? N3 C8 C3 114.6(4) . . ? H8A C8 H8B 107.6 . . ? C3 C8 H8A 108.6 . . ? C3 C8 H8B 108.6 . . ? H40A O40 H40B 109.5 . . ? N3 C15 H15 125.2 . . ? N4 C15 N3 109.5(5) . . ? N4 C15 H15 125.2 . . ? C18 N5 C9 125.5(5) . . ? C18 N5 C16 108.6(6) . . ? C16 N5 C9 125.7(6) . . ? N7 C25 H25A 108.9 . . ? N7 C25 H25B 108.9 . . ? N7 C25 C19 113.2(4) . . ? H25A C25 H25B 107.8 . . ? C19 C25 H25A 108.9 . . ? C19 C25 H25B 108.9 . . ? C24 C23 C27 119.6(5) . . ? C22 C23 C27 121.5(5) . . ? C22 C23 C24 118.9(5) . . ? N11 C27 C23 111.2(4) . . ? N11 C27 H27A 109.4 . . ? N11 C27 H27B 109.4 . . ? C23 C27 H27A 109.4 . . ? C23 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C2 C1 C7 123.5(5) . . ? C6 C1 C7 117.5(5) . . ? C6 C1 C2 119.0(5) . . ? N7 C30 H30 125.7 . . ? N8 C30 N7 108.6(6) . . ? N8 C30 H30 125.7 . . ? C30 N8 C29 109.6(5) . . ? C30 N8 H8 131(5) . . ? C29 N8 H8 120(5) . . ? C20 C21 C26 120.5(5) . . ? C22 C21 C20 118.9(5) . . ? C22 C21 C26 120.6(5) . . ? C21 C20 H20 119.5 . . ? C19 C20 C21 121.0(5) . . ? C19 C20 H20 119.5 . . ? N4 C14 H14 126.6 . . ? C13 C14 N4 106.9(5) . . ? C13 C14 H14 126.6 . . ? N12 C35 H35 126.8 . . ? C34 C35 H35 126.8 . . ? C34 C35 N12 106.4(6) . . ? C23 C24 H24 119.8 . . ? C19 C24 C23 120.4(5) . . ? C19 C24 H24 119.8 . . ? C2 C3 C8 121.3(5) . . ? C4 C3 C8 119.9(5) . . ? C4 C3 C2 118.8(5) . . ? N9 C31 H31 126.4 . . ? C32 C31 N9 107.2(5) . . ? C32 C31 H31 126.4 . . ? N3 C13 H13 126.4 . . ? C14 C13 N3 107.2(5) . . ? C14 C13 H13 126.4 . . ? C23 C22 H22 119.4 . . ? C21 C22 C23 121.1(5) . . ? C21 C22 H22 119.4 . . ? C11 N2 H2 126.2 . . ? C12 N2 H2 126.2 . . ? C12 N2 C11 107.6(6) . . ? C35 N12 H12A 125.5 . . ? C36 N12 C35 109.0(7) . . ? C36 N12 H12A 125.5 . . ? N1 C7 C1 114.6(4) . . ? N1 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C1 C7 H7A 108.6 . . ? C1 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C1 C2 H2A 120.0 . . ? C3 C2 C1 120.1(5) . . ? C3 C2 H2A 120.0 . . ? N2 C11 H11 126.3 . . ? C10 C11 N2 107.4(5) . . ? C10 C11 H11 126.3 . . ? C20 C19 C25 120.7(5) . . ? C20 C19 C24 119.7(5) . . ? C24 C19 C25 119.6(5) . . ? N8 C29 H29 127.1 . . ? C28 C29 N8 105.7(6) . . ? C28 C29 H29 127.1 . . ? N9 C26 C21 114.5(4) . . ? N9 C26 H26A 108.6 . . ? N9 C26 H26B 108.6 . . ? C21 C26 H26A 108.6 . . ? C21 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? N1 C10 H10 126.3 . . ? C11 C10 N1 107.3(6) . . ? C11 C10 H10 126.3 . . ? C32 N10 H10A 125.7 . . ? C33 N10 H10A 125.7 . . ? C33 N10 C32 108.7(6) . . ? H41A O41 H41B 109.5 . . ? C31 C32 N10 107.4(6) . . ? C31 C32 H32 126.3 . . ? N10 C32 H32 126.3 . . ? N11 C36 H36 125.4 . . ? N12 C36 N11 109.2(5) . . ? N12 C36 H36 125.4 . . ? C4 C5 C9 120.9(5) . . ? C4 C5 C6 118.2(5) . . ? C6 C5 C9 120.9(5) . . ? N1 C12 N2 109.8(6) . . ? N1 C12 H12 125.1 . . ? N2 C12 H12 125.1 . . ? C3 C4 C5 122.5(5) . . ? C3 C4 H4A 118.8 . . ? C5 C4 H4A 118.8 . . ? N7 C28 H28 126.0 . . ? C29 C28 N7 108.1(6) . . ? C29 C28 H28 126.0 . . ? N5 C9 C5 110.5(5) . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N9 C33 H33 125.4 . . ? N10 C33 N9 109.2(6) . . ? N10 C33 H33 125.4 . . ? C1 C6 C5 121.4(5) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? N11 C34 H34 125.8 . . ? C35 C34 N11 108.4(7) . . ? C35 C34 H34 125.8 . . ? C18 N6 H6A 126.5 . . ? C18 N6 C17 107.1(7) . . ? C17 N6 H6A 126.5 . . ? N5 C18 H18 125.1 . . ? N6 C18 N5 109.9(6) . . ? N6 C18 H18 125.1 . . ? N5 C16 H16 127.3 . . ? C17 C16 N5 105.4(8) . . ? C17 C16 H16 127.3 . . ? N6 C17 H17 125.6 . . ? C16 C17 N6 108.9(8) . . ? C16 C17 H17 125.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O41 0.86 1.90 2.752(9) 172.2 2_666 N12 H12A O40 0.86 2.03 2.830(8) 155.1 2_766 O41 H41B O17 0.85 2.27 2.814(6) 122.0 2_666 _database_code_depnum_ccdc_archive 'CCDC 938667' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nyy2013031804 _audit_creation_date 2013-03-22 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Cu H4 Mo16 O54, 2(C18 H20 N6), 2(H2 O)' _chemical_formula_sum 'C36 H48 Cu Mo16 N12 O56' _chemical_formula_weight 3143.44 _chemical_melting_point ? _chemical_oxdiff_formula C20H20N4O4Mo8Cu1 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' Cu Cu 0.3201 1.2651 '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' 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.6510(6) _cell_length_b 10.4093(7) _cell_length_c 20.4141(12) _cell_angle_alpha 75.506(5) _cell_angle_beta 79.777(5) _cell_angle_gamma 78.407(5) _cell_volume 1927.5(2) _cell_formula_units_Z 1 _cell_measurement_reflns_used 7355 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 26.3154 _cell_measurement_theta_min 2.9399 _exptl_absorpt_coefficient_mu 2.889 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 2.708 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1497 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_unetI/netI 0.0397 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 15880 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.95 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -11.00 20.00 1.0000 1.6000 omega____ theta____ kappa____ phi______ frames - -17.1323 -108.0000 -7.0000 31 #__ type_ start__ end____ width___ exp.time_ 2 omega -13.00 24.00 1.0000 1.6000 omega____ theta____ kappa____ phi______ frames - -17.1323 -99.0000 90.0000 37 #__ type_ start__ end____ width___ exp.time_ 3 omega -36.00 38.00 1.0000 1.6000 omega____ theta____ kappa____ phi______ frames - 19.7104 -57.0000 -180.0000 74 #__ type_ start__ end____ width___ exp.time_ 4 omega 44.00 95.00 1.0000 1.6000 omega____ theta____ kappa____ phi______ frames - 19.7104 -178.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 5 omega -3.00 92.00 1.0000 1.6000 omega____ theta____ kappa____ phi______ frames - 19.7104 37.0000 120.0000 95 #__ type_ start__ end____ width___ exp.time_ 6 omega -47.00 46.00 1.0000 1.6000 omega____ theta____ kappa____ phi______ frames - 19.7104 -37.0000 -60.0000 93 #__ type_ start__ end____ width___ exp.time_ 7 omega -24.00 30.00 1.0000 1.6000 omega____ theta____ kappa____ phi______ frames - 19.7104 19.0000 -30.0000 54 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0035886000 _diffrn_orient_matrix_UB_12 0.0342346000 _diffrn_orient_matrix_UB_13 0.0263967000 _diffrn_orient_matrix_UB_21 0.0161545000 _diffrn_orient_matrix_UB_22 -0.0625126000 _diffrn_orient_matrix_UB_23 0.0231923000 _diffrn_orient_matrix_UB_31 0.0738786000 _diffrn_orient_matrix_UB_32 0.0033200000 _diffrn_orient_matrix_UB_33 -0.0087662000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6257 _reflns_number_total 7842 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.109 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.146 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 551 _refine_ls_number_reflns 7842 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0323 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+1.1202P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.0730 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: {H15A,H15B} of C15, H2 of C2, H10 of C10, {H11A,H11B} of C11, H16 of C16, H12 of C12, H18 of C18, H13 of C13, H4A of C4, H14 of C14, H9 of C9, H6 of C6, H4 of N4, {H7A,H7B} of C7, H17 of C17, H8 of C8, H6A of N6 At 1.5 times of: {H28A,H28B} of O28, {H27A,H27B} of O27 2.a Free rotating group: O28(H28A,H28B) 2.b Rotating group: O27(H27A,H27B) 2.c Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C7(H7A,H7B), C15(H15A,H15B) 2.d Aromatic/amide H refined with riding coordinates: N4(H4), C2(H2), C4(H4A), C6(H6), C14(H14), N6(H6A), C12(H12), C18(H18), C16(H16), C13(H13), C17(H17), C8(H8), C9(H9), C10(H10) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap 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 Mo5 Mo 0.00852(4) 0.85806(4) 0.310026(18) 0.01380(9) Uani 1 1 d . . . Mo6 Mo 0.05463(4) 0.77062(5) 0.154433(18) 0.01649(10) Uani 1 1 d . . . Mo4 Mo 0.29575(4) 0.62837(4) 0.257179(17) 0.01186(9) Uani 1 1 d . . . Mo1 Mo 0.25469(4) 0.74862(4) 0.407592(17) 0.01201(9) Uani 1 1 d . . . Cu1 Cu 0.5000 0.5000 0.5000 0.01728(18) Uani 1 2 d S . . O5 O 0.2286(3) 0.8432(3) 0.30061(13) 0.0139(7) Uani 1 1 d . . . O4 O 0.0790(3) 0.7231(3) 0.39738(13) 0.0163(7) Uani 1 1 d . . . O20 O 0.0864(3) 0.6295(4) 0.12420(17) 0.0360(10) Uani 1 1 d . . . O19 O 0.1000(3) 0.6643(3) 0.26393(14) 0.0167(7) Uani 1 1 d . . . O18 O 0.0090(3) 0.9222(3) 0.22211(14) 0.0197(7) Uani 1 1 d . . . O9 O 0.3272(3) 0.5774(3) 0.34296(13) 0.0164(7) Uani 1 1 d . . . O17 O -0.1587(3) 0.7847(3) 0.33331(14) 0.0204(8) Uani 1 1 d . . . O14 O 0.2535(3) 0.7733(3) 0.16456(13) 0.0178(7) Uani 1 1 d . . . Mo7 Mo -0.31370(4) 0.69998(4) 0.212336(18) 0.01334(9) Uani 1 1 d . . . Mo8 Mo -0.35805(4) 0.79275(4) 0.363350(17) 0.01271(9) Uani 1 1 d . . . Mo3 Mo 0.44241(4) 0.81130(4) 0.113614(17) 0.01384(10) Uani 1 1 d . . . Mo2 Mo 0.40033(4) 0.93321(4) 0.263054(17) 0.01189(9) Uani 1 1 d . . . O3 O 0.4396(3) 0.7938(3) 0.35663(13) 0.0146(7) Uani 1 1 d . . . O2 O 0.2130(3) 0.8829(4) 0.44436(15) 0.0245(8) Uani 1 1 d . . . O15 O 0.3463(3) 0.4878(3) 0.22605(15) 0.0230(8) Uani 1 1 d . . . O7 O 0.5991(3) 0.8942(3) 0.25826(13) 0.0148(7) Uani 1 1 d . . . O16 O -0.0364(3) 0.9959(4) 0.34228(16) 0.0265(8) Uani 1 1 d . . . O25 O -0.3826(3) 0.9384(4) 0.39038(16) 0.0261(8) Uani 1 1 d . . . O24 O -0.3205(3) 0.6381(3) 0.30116(14) 0.0173(7) Uani 1 1 d . . . O11 O 0.6230(3) 0.8342(3) 0.12511(13) 0.0157(7) Uani 1 1 d . . . O23 O -0.2786(3) 0.5602(4) 0.18091(15) 0.0250(8) Uani 1 1 d . . . O10 O 0.4638(3) 0.7217(3) 0.22274(13) 0.0134(7) Uani 1 1 d . . . O22 O -0.1441(3) 0.7650(4) 0.19029(15) 0.0248(8) Uani 1 1 d . . . O13 O 0.3867(3) 0.9338(3) 0.04517(14) 0.0208(7) Uani 1 1 d . . . O1 O 0.3223(3) 0.6146(3) 0.47164(14) 0.0197(7) Uani 1 1 d . . . O8 O 0.3740(3) 0.9823(3) 0.17714(14) 0.0168(7) Uani 1 1 d . . . O26 O -0.3592(3) 0.6689(3) 0.43691(14) 0.0212(8) Uani 1 1 d . . . O12 O 0.4844(3) 0.6689(4) 0.08310(15) 0.0238(8) Uani 1 1 d . . . O6 O 0.3540(3) 1.0767(3) 0.29104(15) 0.0238(8) Uani 1 1 d . . . O27 O 0.5226(3) 0.4189(4) 0.42228(14) 0.0234(8) Uani 1 1 d . . . H27A H 0.4522 0.4520 0.3983 0.035 Uiso 1 1 d R . . H27B H 0.5248 0.3323 0.4357 0.035 Uiso 1 1 d R . . O21 O 0.0385(3) 0.8981(4) 0.08432(16) 0.0347(10) Uani 1 1 d . . . N3 N -0.0107(4) 0.6559(5) 0.58950(18) 0.0240(9) Uani 1 1 d . . . N5 N 0.3421(4) 0.7885(5) 0.8396(2) 0.0282(10) Uani 1 1 d . . . C11 C 0.1026(5) 0.5839(6) 0.6320(2) 0.0291(13) Uani 1 1 d . . . H11A H 0.1955 0.5911 0.6052 0.035 Uiso 1 1 calc R . . H11B H 0.0943 0.4893 0.6467 0.035 Uiso 1 1 calc R . . N1 N -0.1811(4) 0.7060(5) 0.9120(2) 0.0319(11) Uani 1 1 d . . . N4 N -0.1784(5) 0.6898(6) 0.5287(2) 0.0453(14) Uani 1 1 d . . . H4 H -0.2408 0.6758 0.5072 0.054 Uiso 1 1 calc R . . C2 C -0.0341(5) 0.6476(5) 0.7397(2) 0.0233(11) Uani 1 1 d . . . H2 H -0.1110 0.6140 0.7323 0.028 Uiso 1 1 calc R . . C1 C -0.0460(5) 0.7006(5) 0.7957(2) 0.0219(11) Uani 1 1 d . . . C4 C 0.2035(5) 0.6947(5) 0.7053(2) 0.0245(11) Uani 1 1 d . . . H4A H 0.2869 0.6935 0.6745 0.029 Uiso 1 1 calc R . . C5 C 0.1945(5) 0.7474(5) 0.7610(2) 0.0252(11) Uani 1 1 d . . . C3 C 0.0901(5) 0.6427(5) 0.6936(2) 0.0235(11) Uani 1 1 d . . . C6 C 0.0684(5) 0.7520(5) 0.8065(2) 0.0260(12) Uani 1 1 d . . . H6 H 0.0607 0.7895 0.8441 0.031 Uiso 1 1 calc R . . C7 C -0.1881(5) 0.7087(6) 0.8406(2) 0.0314(13) Uani 1 1 d . . . H7A H -0.2489 0.7911 0.8217 0.038 Uiso 1 1 calc R . . H7B H -0.2328 0.6340 0.8393 0.038 Uiso 1 1 calc R . . C14 C -0.0908(5) 0.5960(6) 0.5644(2) 0.0317(13) Uani 1 1 d . . . H14 H -0.0861 0.5037 0.5707 0.038 Uiso 1 1 calc R . . N6 N 0.3614(6) 0.8269(6) 0.9352(2) 0.0525(15) Uani 1 1 d . . . H6A H 0.3590 0.8683 0.9671 0.063 Uiso 1 1 calc R . . C12 C -0.0496(6) 0.7917(6) 0.5695(3) 0.0428(15) Uani 1 1 d . . . H12 H -0.0104 0.8571 0.5803 0.051 Uiso 1 1 calc R . . N2 N -0.1943(7) 0.7637(8) 1.0060(3) 0.085(2) Uani 1 1 d . . . C18 C 0.3252(6) 0.8824(6) 0.8744(3) 0.0389(14) Uani 1 1 d . . . H18 H 0.2928 0.9734 0.8583 0.047 Uiso 1 1 calc R . . C15 C 0.3167(6) 0.8095(7) 0.7688(2) 0.0491(19) Uani 1 1 d . . . H15A H 0.4028 0.7720 0.7428 0.059 Uiso 1 1 calc R . . H15B H 0.2979 0.9054 0.7495 0.059 Uiso 1 1 calc R . . C16 C 0.3920(7) 0.6681(7) 0.8798(3) 0.0532(18) Uani 1 1 d . . . H16 H 0.4137 0.5850 0.8679 0.064 Uiso 1 1 calc R . . O28 O 0.5670(8) 0.1542(6) 0.4563(3) 0.110(2) Uani 1 1 d G . . H28A H 0.5288 0.1226 0.4965 0.164 Uiso 1 1 d G . . H28B H 0.5176 0.1463 0.4274 0.164 Uiso 1 1 d G . . C13 C -0.1544(7) 0.8131(7) 0.5315(3) 0.0525(18) Uani 1 1 d . . . H13 H -0.2021 0.8961 0.5108 0.063 Uiso 1 1 calc R . . C17 C 0.4036(8) 0.6923(8) 0.9396(3) 0.065(2) Uani 1 1 d . . . H17 H 0.4348 0.6290 0.9773 0.078 Uiso 1 1 calc R . . C8 C -0.1581(8) 0.5949(8) 0.9619(3) 0.064(2) Uani 1 1 d . . . H8 H -0.1410 0.5062 0.9573 0.077 Uiso 1 1 calc R . . C9 C -0.1645(8) 0.6368(11) 1.0196(3) 0.080(3) Uani 1 1 d . . . H9 H -0.1495 0.5820 1.0622 0.097 Uiso 1 1 calc R . . C10 C -0.2024(9) 0.8093(9) 0.9391(4) 0.087(3) Uani 1 1 d . . . H10 H -0.2202 0.8990 0.9162 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo5 0.00808(18) 0.0179(2) 0.01602(18) -0.00409(17) -0.00390(14) -0.00100(16) Mo6 0.01026(19) 0.0271(3) 0.01362(18) -0.00457(18) -0.00344(14) -0.00497(17) Mo4 0.00936(18) 0.0146(2) 0.01234(17) -0.00260(16) -0.00226(14) -0.00337(15) Mo1 0.00930(18) 0.0161(2) 0.01038(16) -0.00198(16) -0.00200(14) -0.00201(15) Cu1 0.0163(4) 0.0208(5) 0.0140(3) -0.0034(3) -0.0059(3) 0.0012(3) O5 0.0096(14) 0.0174(19) 0.0143(14) 0.0009(13) -0.0055(11) -0.0032(13) O4 0.0118(15) 0.023(2) 0.0148(14) -0.0032(14) -0.0020(12) -0.0052(13) O20 0.031(2) 0.047(3) 0.039(2) -0.024(2) -0.0076(16) -0.0068(18) O19 0.0134(15) 0.020(2) 0.0187(15) -0.0049(14) -0.0030(12) -0.0065(13) O18 0.0162(16) 0.022(2) 0.0204(15) -0.0041(15) -0.0041(13) 0.0001(14) O9 0.0170(15) 0.019(2) 0.0134(14) -0.0032(14) -0.0036(12) -0.0018(13) O17 0.0108(15) 0.030(2) 0.0209(15) -0.0037(15) -0.0039(12) -0.0060(14) O14 0.0144(15) 0.028(2) 0.0109(14) -0.0006(14) -0.0032(12) -0.0067(14) Mo7 0.00827(18) 0.0194(2) 0.01351(17) -0.00563(17) -0.00243(14) -0.00156(16) Mo8 0.00942(18) 0.0187(2) 0.01118(17) -0.00360(16) -0.00269(14) -0.00349(16) Mo3 0.01122(19) 0.0209(2) 0.01044(17) -0.00320(16) -0.00180(14) -0.00497(16) Mo2 0.00985(18) 0.0134(2) 0.01236(17) -0.00139(16) -0.00261(14) -0.00275(15) O3 0.0116(14) 0.0187(19) 0.0121(13) 0.0015(13) -0.0039(11) -0.0033(13) O2 0.0239(17) 0.027(2) 0.0269(17) -0.0142(16) -0.0030(14) -0.0034(15) O15 0.0217(17) 0.023(2) 0.0268(17) -0.0119(16) -0.0021(14) -0.0021(15) O7 0.0121(15) 0.0183(19) 0.0148(14) -0.0036(14) -0.0013(12) -0.0047(13) O16 0.0259(18) 0.025(2) 0.0301(17) -0.0108(17) -0.0081(14) 0.0026(15) O25 0.0273(18) 0.028(2) 0.0289(17) -0.0165(17) -0.0049(14) -0.0050(16) O24 0.0137(15) 0.023(2) 0.0157(14) -0.0055(14) -0.0057(12) -0.0005(13) O11 0.0117(15) 0.020(2) 0.0145(14) -0.0021(14) -0.0003(12) -0.0052(13) O23 0.0294(18) 0.023(2) 0.0241(16) -0.0116(16) -0.0067(14) 0.0020(15) O10 0.0091(14) 0.0206(19) 0.0118(13) -0.0032(13) -0.0037(11) -0.0039(13) O22 0.0114(15) 0.041(2) 0.0242(16) -0.0095(17) -0.0034(13) -0.0063(15) O13 0.0234(17) 0.026(2) 0.0129(14) -0.0012(14) -0.0048(13) -0.0061(15) O1 0.0161(16) 0.027(2) 0.0133(14) -0.0005(14) -0.0038(12) 0.0003(14) O8 0.0161(15) 0.0169(19) 0.0158(14) -0.0007(14) -0.0026(12) -0.0023(13) O26 0.0220(17) 0.027(2) 0.0143(14) -0.0002(15) -0.0054(13) -0.0069(15) O12 0.0240(17) 0.026(2) 0.0255(16) -0.0121(16) -0.0045(14) -0.0050(15) O6 0.0228(17) 0.022(2) 0.0281(17) -0.0095(16) -0.0041(14) -0.0004(15) O27 0.0290(19) 0.021(2) 0.0198(16) -0.0053(15) -0.0089(14) 0.0015(15) O21 0.034(2) 0.047(3) 0.0217(16) 0.0048(18) -0.0107(15) -0.0113(18) N3 0.027(2) 0.029(3) 0.0201(19) -0.0076(19) -0.0078(17) -0.0069(19) N5 0.037(2) 0.029(3) 0.026(2) -0.010(2) -0.0078(19) -0.017(2) C11 0.023(3) 0.043(4) 0.026(2) -0.017(3) -0.007(2) -0.002(2) N1 0.027(2) 0.041(3) 0.026(2) -0.013(2) -0.0061(18) 0.007(2) N4 0.045(3) 0.058(4) 0.040(3) -0.007(3) -0.022(2) -0.014(3) C2 0.021(2) 0.026(3) 0.024(2) -0.005(2) -0.009(2) -0.005(2) C1 0.027(3) 0.018(3) 0.019(2) -0.004(2) -0.004(2) 0.001(2) C4 0.026(3) 0.027(3) 0.021(2) -0.005(2) -0.002(2) -0.007(2) C5 0.035(3) 0.019(3) 0.024(2) 0.001(2) -0.011(2) -0.010(2) C3 0.027(3) 0.022(3) 0.025(2) -0.009(2) -0.009(2) -0.003(2) C6 0.043(3) 0.023(3) 0.016(2) -0.005(2) -0.009(2) -0.010(2) C7 0.031(3) 0.040(4) 0.023(2) -0.009(3) -0.009(2) 0.001(3) C14 0.034(3) 0.045(4) 0.022(2) -0.007(3) -0.006(2) -0.018(3) N6 0.081(4) 0.058(4) 0.032(3) -0.023(3) -0.007(3) -0.029(3) C12 0.064(4) 0.025(4) 0.044(3) -0.012(3) -0.015(3) -0.008(3) N2 0.098(5) 0.096(6) 0.062(4) -0.055(4) -0.034(4) 0.048(5) C18 0.054(4) 0.033(4) 0.035(3) -0.005(3) -0.009(3) -0.017(3) C15 0.064(4) 0.078(6) 0.019(3) -0.009(3) -0.004(3) -0.047(4) C16 0.071(4) 0.043(5) 0.052(4) -0.015(3) -0.029(3) 0.001(4) O28 0.225(7) 0.041(4) 0.057(3) -0.012(3) -0.034(4) 0.005(4) C13 0.067(4) 0.037(5) 0.048(4) 0.000(3) -0.027(3) 0.009(3) C17 0.102(6) 0.054(6) 0.049(4) -0.009(4) -0.047(4) -0.006(4) C8 0.103(6) 0.056(5) 0.027(3) -0.003(3) -0.006(3) -0.007(4) C9 0.086(6) 0.118(9) 0.026(3) -0.018(5) -0.003(3) 0.010(6) C10 0.126(7) 0.070(7) 0.067(5) -0.046(5) -0.057(5) 0.059(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 Mo5 Mo1 3.2195(5) . ? Mo5 O5 2.076(3) . ? Mo5 O4 2.100(3) . ? Mo5 O19 2.381(3) . ? Mo5 O18 1.751(3) . ? Mo5 O17 1.859(3) . ? Mo5 O16 1.674(3) . ? Mo6 O20 1.684(4) . ? Mo6 O19 2.308(3) . ? Mo6 O18 2.278(3) . ? Mo6 O14 1.973(3) . ? Mo6 O22 1.935(3) . ? Mo6 O21 1.697(3) . ? Mo4 O19 1.838(3) . ? Mo4 O9 1.760(3) . ? Mo4 O14 2.149(3) . ? Mo4 O15 1.689(3) . ? Mo4 O10 1.989(3) . ? Mo1 O5 2.196(3) . ? Mo1 O4 1.824(3) . ? Mo1 O9 2.399(3) . ? Mo1 O3 1.980(3) . ? Mo1 O2 1.694(3) . ? Mo1 O1 1.762(3) . ? Cu1 O1 1.971(3) 2_666 ? Cu1 O1 1.971(3) . ? Cu1 O26 2.409(3) 1_655 ? Cu1 O26 2.409(3) 2_566 ? Cu1 O27 1.937(3) 2_666 ? Cu1 O27 1.937(3) . ? O5 Mo2 2.007(3) . ? O17 Mo8 1.904(3) . ? O14 Mo3 1.993(3) . ? Mo7 Mo3 3.2192(5) 1_455 ? Mo7 O7 2.379(3) 1_455 ? Mo7 O24 1.760(3) . ? Mo7 O11 2.072(3) 1_455 ? Mo7 O23 1.683(3) . ? Mo7 O10 2.091(3) 1_455 ? Mo7 O22 1.836(3) . ? Mo8 O3 1.980(3) 1_455 ? Mo8 O7 2.212(3) 1_455 ? Mo8 O25 1.699(3) . ? Mo8 O24 2.227(3) . ? Mo8 O26 1.717(3) . ? Mo3 Mo7 3.2191(5) 1_655 ? Mo3 O11 1.868(3) . ? Mo3 O10 2.218(3) . ? Mo3 O13 1.723(3) . ? Mo3 O8 2.380(3) . ? Mo3 O12 1.698(3) . ? Mo2 O3 2.132(3) . ? Mo2 O7 1.870(3) . ? Mo2 O10 2.467(3) . ? Mo2 O8 1.749(3) . ? Mo2 O6 1.681(3) . ? O3 Mo8 1.980(3) 1_655 ? O7 Mo7 2.379(3) 1_655 ? O7 Mo8 2.212(3) 1_655 ? O11 Mo7 2.072(3) 1_655 ? O10 Mo7 2.091(3) 1_655 ? O26 Cu1 2.409(3) 1_455 ? O27 H27A 0.8706 . ? O27 H27B 0.8709 . ? N3 C11 1.481(6) . ? N3 C14 1.321(6) . ? N3 C12 1.363(7) . ? N5 C18 1.314(7) . ? N5 C15 1.464(6) . ? N5 C16 1.363(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C3 1.507(6) . ? N1 C7 1.465(6) . ? N1 C8 1.346(7) . ? N1 C10 1.292(8) . ? N4 H4 0.8600 . ? N4 C14 1.314(7) . ? N4 C13 1.365(8) . ? C2 H2 0.9300 . ? C2 C1 1.367(6) . ? C2 C3 1.387(6) . ? C1 C6 1.392(6) . ? C1 C7 1.508(6) . ? C4 H4A 0.9300 . ? C4 C5 1.364(6) . ? C4 C3 1.394(6) . ? C5 C6 1.393(6) . ? C5 C15 1.504(7) . ? C6 H6 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C14 H14 0.9300 . ? N6 H6A 0.8600 . ? N6 C18 1.309(7) . ? N6 C17 1.363(9) . ? C12 H12 0.9300 . ? C12 C13 1.333(8) . ? N2 C9 1.264(11) . ? N2 C10 1.340(9) . ? C18 H18 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16 0.9300 . ? C16 C17 1.334(8) . ? O28 H28A 0.8502 . ? O28 H28B 0.8496 . ? C13 H13 0.9300 . ? C17 H17 0.9300 . ? C8 H8 0.9300 . ? C8 C9 1.343(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? 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 O5 Mo5 Mo1 42.51(7) . . ? O5 Mo5 O4 72.03(10) . . ? O5 Mo5 O19 75.62(11) . . ? O4 Mo5 Mo1 32.14(7) . . ? O4 Mo5 O19 80.47(11) . . ? O19 Mo5 Mo1 86.01(7) . . ? O18 Mo5 Mo1 134.02(9) . . ? O18 Mo5 O5 91.63(12) . . ? O18 Mo5 O4 155.00(13) . . ? O18 Mo5 O19 77.12(13) . . ? O18 Mo5 O17 101.53(13) . . ? O17 Mo5 Mo1 118.97(9) . . ? O17 Mo5 O5 152.55(14) . . ? O17 Mo5 O4 86.86(12) . . ? O17 Mo5 O19 83.90(12) . . ? O16 Mo5 Mo1 89.11(11) . . ? O16 Mo5 O5 97.84(14) . . ? O16 Mo5 O4 97.64(14) . . ? O16 Mo5 O19 173.45(12) . . ? O16 Mo5 O18 103.37(16) . . ? O16 Mo5 O17 102.31(15) . . ? O20 Mo6 O19 95.83(15) . . ? O20 Mo6 O18 165.00(15) . . ? O20 Mo6 O14 97.34(15) . . ? O20 Mo6 O22 97.07(15) . . ? O20 Mo6 O21 104.71(18) . . ? O18 Mo6 O19 69.76(11) . . ? O14 Mo6 O19 69.65(10) . . ? O14 Mo6 O18 81.85(12) . . ? O22 Mo6 O19 85.60(11) . . ? O22 Mo6 O18 78.19(12) . . ? O22 Mo6 O14 152.43(12) . . ? O21 Mo6 O19 157.51(15) . . ? O21 Mo6 O18 90.21(15) . . ? O21 Mo6 O14 98.27(14) . . ? O21 Mo6 O22 100.62(15) . . ? O19 Mo4 O14 75.78(11) . . ? O19 Mo4 O10 140.03(14) . . ? O9 Mo4 O19 103.23(12) . . ? O9 Mo4 O14 154.59(14) . . ? O9 Mo4 O10 96.28(12) . . ? O15 Mo4 O19 105.88(14) . . ? O15 Mo4 O9 104.99(15) . . ? O15 Mo4 O14 99.56(14) . . ? O15 Mo4 O10 102.14(13) . . ? O10 Mo4 O14 71.90(11) . . ? O5 Mo1 Mo5 39.71(7) . . ? O5 Mo1 O9 72.14(11) . . ? O4 Mo1 Mo5 37.77(9) . . ? O4 Mo1 O5 74.66(11) . . ? O4 Mo1 O9 80.99(12) . . ? O4 Mo1 O3 143.38(12) . . ? O9 Mo1 Mo5 84.29(7) . . ? O3 Mo1 Mo5 109.91(8) . . ? O3 Mo1 O5 70.43(10) . . ? O3 Mo1 O9 78.19(11) . . ? O2 Mo1 Mo5 93.83(11) . . ? O2 Mo1 O5 101.92(14) . . ? O2 Mo1 O4 101.87(14) . . ? O2 Mo1 O9 172.65(13) . . ? O2 Mo1 O3 95.85(14) . . ? O2 Mo1 O1 104.48(15) . . ? O1 Mo1 Mo5 144.88(10) . . ? O1 Mo1 O5 152.11(13) . . ? O1 Mo1 O4 108.11(14) . . ? O1 Mo1 O9 80.80(12) . . ? O1 Mo1 O3 97.91(12) . . ? O1 Cu1 O1 179.998(1) . 2_666 ? O1 Cu1 O26 91.89(12) 2_666 2_566 ? O1 Cu1 O26 88.11(12) . 2_566 ? O1 Cu1 O26 88.12(12) 2_666 1_655 ? O1 Cu1 O26 91.88(12) . 1_655 ? O26 Cu1 O26 180.0 1_655 2_566 ? O27 Cu1 O1 90.14(13) . . ? O27 Cu1 O1 89.86(13) 2_666 . ? O27 Cu1 O1 90.14(13) 2_666 2_666 ? O27 Cu1 O1 89.86(13) . 2_666 ? O27 Cu1 O26 91.94(12) . 1_655 ? O27 Cu1 O26 91.94(12) 2_666 2_566 ? O27 Cu1 O26 88.06(12) . 2_566 ? O27 Cu1 O26 88.06(12) 2_666 1_655 ? O27 Cu1 O27 179.999(1) 2_666 . ? Mo5 O5 Mo1 97.78(10) . . ? Mo2 O5 Mo5 147.43(16) . . ? Mo2 O5 Mo1 105.14(11) . . ? Mo1 O4 Mo5 110.10(13) . . ? Mo6 O19 Mo5 94.69(11) . . ? Mo4 O19 Mo5 110.62(13) . . ? Mo4 O19 Mo6 104.31(12) . . ? Mo5 O18 Mo6 117.18(16) . . ? Mo4 O9 Mo1 115.14(15) . . ? Mo5 O17 Mo8 153.0(2) . . ? Mo6 O14 Mo4 105.67(12) . . ? Mo6 O14 Mo3 144.06(15) . . ? Mo3 O14 Mo4 106.60(13) . . ? O7 Mo7 Mo3 86.68(7) 1_455 1_455 ? O24 Mo7 Mo3 132.68(9) . 1_455 ? O24 Mo7 O7 75.91(13) . 1_455 ? O24 Mo7 O11 154.20(13) . 1_455 ? O24 Mo7 O10 89.54(11) . 1_455 ? O24 Mo7 O22 101.93(13) . . ? O11 Mo7 Mo3 33.17(7) 1_455 1_455 ? O11 Mo7 O7 80.95(11) 1_455 1_455 ? O11 Mo7 O10 73.26(10) 1_455 1_455 ? O23 Mo7 Mo3 87.13(11) . 1_455 ? O23 Mo7 O7 171.18(12) . 1_455 ? O23 Mo7 O24 103.93(16) . . ? O23 Mo7 O11 97.19(14) . 1_455 ? O23 Mo7 O10 96.63(14) . 1_455 ? O23 Mo7 O22 103.70(15) . . ? O10 Mo7 Mo3 43.19(7) 1_455 1_455 ? O10 Mo7 O7 74.57(11) 1_455 1_455 ? O22 Mo7 Mo3 120.16(10) . 1_455 ? O22 Mo7 O7 84.86(13) . 1_455 ? O22 Mo7 O11 87.04(12) . 1_455 ? O22 Mo7 O10 153.31(15) . 1_455 ? O17 Mo8 O3 156.99(12) . 1_455 ? O17 Mo8 O7 89.42(11) . 1_455 ? O17 Mo8 O24 79.34(12) . . ? O3 Mo8 O7 71.24(10) 1_455 1_455 ? O3 Mo8 O24 82.64(11) 1_455 . ? O7 Mo8 O24 71.45(11) 1_455 . ? O25 Mo8 O17 96.43(15) . . ? O25 Mo8 O3 97.31(14) . 1_455 ? O25 Mo8 O7 94.25(14) . 1_455 ? O25 Mo8 O24 165.00(13) . . ? O25 Mo8 O26 104.64(16) . . ? O26 Mo8 O17 101.49(13) . . ? O26 Mo8 O3 92.78(12) . 1_455 ? O26 Mo8 O7 156.81(13) . 1_455 ? O26 Mo8 O24 90.34(13) . . ? O14 Mo3 Mo7 110.23(8) . 1_655 ? O14 Mo3 O10 70.34(10) . . ? O14 Mo3 O8 77.30(12) . . ? O11 Mo3 O14 142.88(12) . . ? O11 Mo3 Mo7 37.36(9) . 1_655 ? O11 Mo3 O10 74.31(10) . . ? O11 Mo3 O8 80.62(12) . . ? O10 Mo3 Mo7 40.18(7) . 1_655 ? O10 Mo3 O8 70.45(11) . . ? O13 Mo3 O14 99.69(13) . . ? O13 Mo3 Mo7 145.30(10) . 1_655 ? O13 Mo3 O11 108.18(13) . . ? O13 Mo3 O10 155.82(14) . . ? O13 Mo3 O8 86.05(13) . . ? O8 Mo3 Mo7 83.86(7) . 1_655 ? O12 Mo3 O14 95.72(14) . . ? O12 Mo3 Mo7 90.65(11) . 1_655 ? O12 Mo3 O11 100.78(14) . . ? O12 Mo3 O10 99.21(14) . . ? O12 Mo3 O13 103.76(15) . . ? O12 Mo3 O8 168.92(13) . . ? O5 Mo2 O3 71.30(10) . . ? O5 Mo2 O10 76.81(11) . . ? O3 Mo2 O10 80.06(11) . . ? O7 Mo2 O5 139.82(13) . . ? O7 Mo2 O3 75.12(11) . . ? O7 Mo2 O10 76.23(11) . . ? O8 Mo2 O5 98.75(12) . . ? O8 Mo2 O3 155.65(14) . . ? O8 Mo2 O7 102.95(12) . . ? O8 Mo2 O10 75.98(12) . . ? O6 Mo2 O5 102.14(13) . . ? O6 Mo2 O3 99.77(14) . . ? O6 Mo2 O7 104.74(14) . . ? O6 Mo2 O10 178.95(12) . . ? O6 Mo2 O8 104.10(15) . . ? Mo1 O3 Mo2 108.51(12) . . ? Mo8 O3 Mo1 145.22(14) 1_655 . ? Mo8 O3 Mo2 104.58(11) 1_655 . ? Mo8 O7 Mo7 95.02(11) 1_655 1_655 ? Mo2 O7 Mo7 109.56(13) . 1_655 ? Mo2 O7 Mo8 105.45(11) . 1_655 ? Mo7 O24 Mo8 115.84(16) . . ? Mo3 O11 Mo7 109.47(13) . 1_655 ? Mo4 O10 Mo7 145.22(17) . 1_655 ? Mo4 O10 Mo3 104.15(11) . . ? Mo4 O10 Mo2 105.25(11) . . ? Mo7 O10 Mo3 96.62(10) 1_655 . ? Mo7 O10 Mo2 99.36(11) 1_655 . ? Mo3 O10 Mo2 97.18(11) . . ? Mo7 O22 Mo6 157.9(2) . . ? Mo1 O1 Cu1 143.03(16) . . ? Mo2 O8 Mo3 115.99(15) . . ? Mo8 O26 Cu1 139.17(15) . 1_455 ? Cu1 O27 H27A 111.0 . . ? Cu1 O27 H27B 110.6 . . ? H27A O27 H27B 108.0 . . ? C14 N3 C11 124.3(5) . . ? C14 N3 C12 108.8(5) . . ? C12 N3 C11 126.9(5) . . ? C18 N5 C15 126.0(5) . . ? C18 N5 C16 108.6(5) . . ? C16 N5 C15 125.4(5) . . ? N3 C11 H11A 109.6 . . ? N3 C11 H11B 109.6 . . ? N3 C11 C3 110.3(4) . . ? H11A C11 H11B 108.1 . . ? C3 C11 H11A 109.6 . . ? C3 C11 H11B 109.6 . . ? C8 N1 C7 125.9(5) . . ? C10 N1 C7 126.2(6) . . ? C10 N1 C8 107.8(6) . . ? C14 N4 H4 125.5 . . ? C14 N4 C13 109.1(5) . . ? C13 N4 H4 125.5 . . ? C1 C2 H2 119.3 . . ? C1 C2 C3 121.4(4) . . ? C3 C2 H2 119.3 . . ? C2 C1 C6 119.4(4) . . ? C2 C1 C7 117.5(4) . . ? C6 C1 C7 122.9(4) . . ? C5 C4 H4A 119.3 . . ? C5 C4 C3 121.3(4) . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 119.4(4) . . ? C4 C5 C15 119.0(4) . . ? C6 C5 C15 121.4(5) . . ? C2 C3 C11 121.2(4) . . ? C2 C3 C4 118.3(4) . . ? C4 C3 C11 120.5(4) . . ? C1 C6 C5 120.1(4) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? N1 C7 C1 115.0(4) . . ? N1 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C1 C7 H7A 108.5 . . ? C1 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? N3 C14 H14 126.0 . . ? N4 C14 N3 108.0(5) . . ? N4 C14 H14 126.0 . . ? C18 N6 H6A 125.8 . . ? C18 N6 C17 108.4(5) . . ? C17 N6 H6A 125.8 . . ? N3 C12 H12 126.4 . . ? C13 C12 N3 107.1(5) . . ? C13 C12 H12 126.4 . . ? C9 N2 C10 109.7(7) . . ? N5 C18 H18 125.6 . . ? N6 C18 N5 108.9(6) . . ? N6 C18 H18 125.6 . . ? N5 C15 C5 113.9(4) . . ? N5 C15 H15A 108.8 . . ? N5 C15 H15B 108.8 . . ? C5 C15 H15A 108.8 . . ? C5 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N5 C16 H16 126.6 . . ? C17 C16 N5 106.8(6) . . ? C17 C16 H16 126.6 . . ? H28A O28 H28B 109.5 . . ? N4 C13 H13 126.5 . . ? C12 C13 N4 107.0(6) . . ? C12 C13 H13 126.5 . . ? N6 C17 H17 126.3 . . ? C16 C17 N6 107.3(6) . . ? C16 C17 H17 126.3 . . ? N1 C8 H8 126.6 . . ? C9 C8 N1 106.7(7) . . ? C9 C8 H8 126.6 . . ? N2 C9 C8 108.1(7) . . ? N2 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? N1 C10 N2 107.6(7) . . ? N1 C10 H10 126.2 . . ? N2 C10 H10 126.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O27 H27A O9 0.87 1.88 2.720(4) 160.2 . O27 H27B O28 0.87 1.77 2.632(7) 168.2 . N4 H4 O26 0.86 2.01 2.850(5) 165.9 . N6 H6A O13 0.86 1.96 2.809(6) 168.2 1_556 O28 H28B O25 0.85 2.43 2.817(7) 108.5 1_645 _database_code_depnum_ccdc_archive 'CCDC 938668' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nyy2013031803 _audit_creation_date 2013-03-22 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Mo8 O26, C36 H38 Cu N12, 4(H2 O)' _chemical_formula_sum 'C36 H46 Cu Mo8 N12 O30' _chemical_formula_weight 1957.91 _chemical_melting_point ? _chemical_oxdiff_formula C20H20N4O4Mo8Cu1 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' Cu Cu 0.3201 1.2651 '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' 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.5513(7) _cell_length_b 12.9013(5) _cell_length_c 13.0406(6) _cell_angle_alpha 65.070(4) _cell_angle_beta 71.264(5) _cell_angle_gamma 68.809(5) _cell_volume 1470.68(13) _cell_formula_units_Z 1 _cell_measurement_reflns_used 6037 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 26.3137 _cell_measurement_theta_min 2.9168 _exptl_absorpt_coefficient_mu 2.097 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 2.211 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 951 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_unetI/netI 0.0572 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 12140 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.92 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -76.00 -32.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 128.0000 -36.0000 44 #__ type_ start__ end____ width___ exp.time_ 2 omega -19.00 12.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 -99.0000 -180.0000 31 #__ type_ start__ end____ width___ exp.time_ 3 omega -4.00 62.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.6323 -99.0000 -90.0000 66 #__ type_ start__ end____ width___ exp.time_ 4 omega 36.00 64.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.6323 178.0000 60.0000 28 #__ type_ start__ end____ width___ exp.time_ 5 omega -5.00 70.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.6323 37.0000 -150.0000 75 #__ type_ start__ end____ width___ exp.time_ 6 omega -53.00 64.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.6323 -19.0000 0.0000 117 #__ type_ start__ end____ width___ exp.time_ 7 omega -6.00 70.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.6323 37.0000 60.0000 76 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0603569000 _diffrn_orient_matrix_UB_12 -0.0065931000 _diffrn_orient_matrix_UB_13 0.0175368000 _diffrn_orient_matrix_UB_21 0.0348079000 _diffrn_orient_matrix_UB_22 0.0172778000 _diffrn_orient_matrix_UB_23 -0.0585496000 _diffrn_orient_matrix_UB_31 -0.0236567000 _diffrn_orient_matrix_UB_32 0.0600628000 _diffrn_orient_matrix_UB_33 -0.0033859000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4804 _reflns_number_total 6016 _reflns_odcompleteness_completeness 99.87 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.754 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.101 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 400 _refine_ls_number_reflns 6016 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0325 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0541 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: H16 of C16, {H15A,H15B} of C15, H14 of C14, H2 of C2, H13 of C13, H10 of C10, {H7A,H7B} of C7, H18 of C18, H12 of C12, H6 of N6, H17 of C17, {H11A, H11B} of C11, H8 of C8, H6A of C6, H9 of C9, H4 of C4 At 1.5 times of: {H14A,H14B} of O14, {H15C,H15D} of O15 2.a Free rotating group: O14(H14A,H14B), O15(H15C,H15D) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C11(H11A,H11B), C15(H15A,H15B) 2.c Aromatic/amide H refined with riding coordinates: N6(H6), C2(H2), C4(H4), C6(H6A), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap 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 Mo1 Mo 0.65395(4) 0.24099(3) 0.46643(3) 0.02628(9) Uani 1 1 d . . . Mo2 Mo 0.61662(4) 0.48879(3) 0.24061(3) 0.02381(9) Uani 1 1 d . . . Mo3 Mo 0.34512(3) 0.47685(3) 0.49360(3) 0.02154(9) Uani 1 1 d . . . Mo4 Mo 0.52523(4) 0.22084(3) 0.75452(3) 0.03535(11) Uani 1 1 d . . . Cu3 Cu 1.0000 0.5000 0.0000 0.02819(18) Uani 1 2 d S . . O1 O 0.6209(3) 0.1122(2) 0.4944(2) 0.0452(8) Uani 1 1 d . . . O2 O 0.8286(3) 0.2183(2) 0.4193(2) 0.0447(8) Uani 1 1 d . . . O3 O 0.6582(3) 0.2231(2) 0.6230(2) 0.0327(7) Uani 1 1 d . . . O4 O 0.6274(3) 0.44190(19) 0.4328(2) 0.0302(7) Uani 1 1 d . . . O5 O 0.5926(3) 0.33408(19) 0.3233(2) 0.0270(6) Uani 1 1 d . . . O6 O 0.7903(3) 0.4571(2) 0.1847(2) 0.0342(7) Uani 1 1 d . . . O7 O 0.5432(3) 0.5336(2) 0.1259(2) 0.0348(7) Uani 1 1 d . . . O8 O 0.3918(3) 0.5430(2) 0.3436(2) 0.0312(7) Uani 1 1 d . . . O9 O 0.1713(3) 0.4920(2) 0.5250(3) 0.0415(8) Uani 1 1 d . . . O10 O 0.4278(3) 0.32152(19) 0.5384(2) 0.0311(7) Uani 1 1 d . . . O11 O 0.3881(3) 0.35735(19) 0.7577(2) 0.0319(7) Uani 1 1 d . . . O12 O 0.4475(4) 0.1128(2) 0.7908(3) 0.0712(12) Uani 1 1 d . . . O13 O 0.6135(4) 0.1809(3) 0.8595(3) 0.0694(11) Uani 1 1 d . . . O14 O 0.2942(4) 0.1639(3) 0.5217(4) 0.0683(11) Uani 1 1 d G . . H14A H 0.2198 0.1888 0.4964 0.102 Uiso 1 1 d G . . H14B H 0.3141 0.2221 0.5219 0.102 Uiso 1 1 d G . . O15 O 0.0542(4) 0.3103(3) 0.4216(4) 0.0876(13) Uani 1 1 d G . . H15C H -0.0072 0.3703 0.4341 0.131 Uiso 1 1 d G . . H15D H 0.1308 0.3282 0.3873 0.131 Uiso 1 1 d G . . N1 N 1.0697(3) 0.6301(2) 0.2106(3) 0.0267(8) Uani 1 1 d . . . N2 N 1.0658(4) 0.5557(2) 0.0892(3) 0.0299(8) Uani 1 1 d . . . N3 N 1.1342(3) 1.1498(2) 0.1943(3) 0.0250(8) Uani 1 1 d . . . N4 N 1.1068(3) 1.3321(2) 0.0729(3) 0.0271(8) Uani 1 1 d . . . N5 N 0.6134(4) 1.1345(3) 0.1617(3) 0.0361(9) Uani 1 1 d . . . N6 N 0.4518(4) 1.1574(3) 0.3074(4) 0.0507(11) Uani 1 1 d . . . H6 H 0.4040 1.1444 0.3767 0.061 Uiso 1 1 calc R . . C1 C 0.9868(4) 0.8155(3) 0.2566(3) 0.0276(10) Uani 1 1 d . . . C2 C 1.0534(4) 0.8695(3) 0.2878(3) 0.0260(9) Uani 1 1 d . . . H2 H 1.1206 0.8230 0.3325 0.031 Uiso 1 1 calc R . . C3 C 1.0211(4) 0.9921(3) 0.2532(3) 0.0268(9) Uani 1 1 d . . . C4 C 0.9206(4) 1.0585(3) 0.1881(4) 0.0345(11) Uani 1 1 d . . . H4 H 0.8977 1.1406 0.1651 0.041 Uiso 1 1 calc R . . C5 C 0.8522(4) 1.0071(3) 0.1556(4) 0.0340(10) Uani 1 1 d . . . C6 C 0.8869(4) 0.8851(3) 0.1907(4) 0.0335(10) Uani 1 1 d . . . H6A H 0.8421 0.8492 0.1695 0.040 Uiso 1 1 calc R . . C7 C 1.0207(5) 0.6807(3) 0.3027(3) 0.0332(11) Uani 1 1 d . . . H7A H 1.0915 0.6493 0.3484 0.040 Uiso 1 1 calc R . . H7B H 0.9384 0.6564 0.3531 0.040 Uiso 1 1 calc R . . C8 C 1.2004(4) 0.6089(3) 0.1482(4) 0.0382(11) Uani 1 1 d . . . H8 H 1.2767 0.6234 0.1553 0.046 Uiso 1 1 calc R . . C9 C 1.1981(4) 0.5623(3) 0.0735(4) 0.0379(11) Uani 1 1 d . . . H9 H 1.2740 0.5386 0.0200 0.045 Uiso 1 1 calc R . . C10 C 0.9916(4) 0.5963(3) 0.1730(4) 0.0306(10) Uani 1 1 d . . . H10 H 0.8977 0.6010 0.2025 0.037 Uiso 1 1 calc R . . C11 C 1.0950(4) 1.0475(3) 0.2905(3) 0.0286(10) Uani 1 1 d . . . H11A H 1.0346 1.0726 0.3543 0.034 Uiso 1 1 calc R . . H11B H 1.1775 0.9892 0.3168 0.034 Uiso 1 1 calc R . . C12 C 1.2337(4) 1.1471(3) 0.0986(4) 0.0385(12) Uani 1 1 d . . . H12 H 1.3007 1.0807 0.0863 0.046 Uiso 1 1 calc R . . C13 C 1.2164(5) 1.2599(3) 0.0244(4) 0.0445(12) Uani 1 1 d . . . H13 H 1.2710 1.2845 -0.0486 0.053 Uiso 1 1 calc R . . C14 C 1.0596(4) 1.2627(3) 0.1749(3) 0.0261(9) Uani 1 1 d . . . H14 H 0.9839 1.2885 0.2273 0.031 Uiso 1 1 calc R . . C15 C 0.7377(5) 1.0818(4) 0.0895(4) 0.0438(12) Uani 1 1 d . . . H15A H 0.7697 1.1444 0.0227 0.053 Uiso 1 1 calc R . . H15B H 0.7139 1.0332 0.0622 0.053 Uiso 1 1 calc R . . C16 C 0.5167(5) 1.2385(4) 0.1225(5) 0.0553(14) Uani 1 1 d . . . H16 H 0.5194 1.2897 0.0464 0.066 Uiso 1 1 calc R . . C17 C 0.4174(6) 1.2532(4) 0.2138(5) 0.0643(17) Uani 1 1 d . . . H17 H 0.3395 1.3172 0.2130 0.077 Uiso 1 1 calc R . . C18 C 0.5709(5) 1.0875(4) 0.2743(4) 0.0437(12) Uani 1 1 d . . . H18 H 0.6175 1.0164 0.3225 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0308(2) 0.02210(17) 0.0223(2) -0.00793(16) -0.00651(18) -0.00157(15) Mo2 0.0237(2) 0.02344(17) 0.0201(2) -0.00730(16) -0.00243(17) -0.00347(14) Mo3 0.01999(19) 0.02307(17) 0.0211(2) -0.00706(15) -0.00343(16) -0.00645(14) Mo4 0.0308(2) 0.0309(2) 0.0332(2) -0.01141(19) -0.0005(2) -0.00045(16) Cu3 0.0428(5) 0.0161(3) 0.0301(4) -0.0067(3) -0.0176(4) -0.0052(3) O1 0.067(2) 0.0271(15) 0.039(2) -0.0052(14) -0.0191(19) -0.0106(15) O2 0.0334(19) 0.0478(17) 0.037(2) -0.0132(16) -0.0067(16) 0.0046(14) O3 0.0317(17) 0.0338(15) 0.0269(17) -0.0102(13) -0.0132(15) 0.0038(13) O4 0.0395(18) 0.0238(13) 0.0268(17) -0.0079(13) -0.0115(15) -0.0048(12) O5 0.0340(17) 0.0247(13) 0.0227(16) -0.0087(12) -0.0064(14) -0.0069(12) O6 0.0275(17) 0.0314(14) 0.0395(19) -0.0146(14) -0.0022(15) -0.0042(12) O7 0.0321(17) 0.0392(15) 0.0252(17) -0.0072(14) -0.0067(15) -0.0047(13) O8 0.0269(16) 0.0348(15) 0.0258(17) -0.0113(13) -0.0061(14) 0.0003(12) O9 0.0256(17) 0.0435(16) 0.046(2) -0.0079(15) -0.0010(16) -0.0137(13) O10 0.0331(17) 0.0278(14) 0.0255(17) -0.0053(13) -0.0025(14) -0.0079(12) O11 0.0313(17) 0.0265(14) 0.0346(18) -0.0079(13) -0.0021(15) -0.0109(12) O12 0.076(3) 0.0349(17) 0.086(3) -0.0219(19) 0.014(2) -0.0218(17) O13 0.069(3) 0.084(2) 0.034(2) -0.0215(19) -0.020(2) 0.013(2) O14 0.054(3) 0.070(2) 0.083(3) -0.034(2) -0.009(2) -0.0144(19) O15 0.065(3) 0.099(3) 0.088(4) -0.049(3) -0.016(3) 0.011(2) N1 0.033(2) 0.0224(16) 0.028(2) -0.0085(16) -0.0111(18) -0.0069(15) N2 0.038(2) 0.0201(16) 0.034(2) -0.0102(16) -0.0143(19) -0.0029(15) N3 0.0263(19) 0.0169(16) 0.030(2) -0.0075(15) -0.0078(17) -0.0020(14) N4 0.034(2) 0.0187(16) 0.028(2) -0.0063(16) -0.0088(18) -0.0061(15) N5 0.037(2) 0.0324(19) 0.038(2) -0.0058(19) -0.023(2) -0.0028(17) N6 0.049(3) 0.057(3) 0.050(3) -0.026(2) -0.012(2) -0.008(2) C1 0.034(3) 0.028(2) 0.022(2) -0.0089(19) -0.003(2) -0.0105(18) C2 0.027(2) 0.024(2) 0.024(2) -0.0057(18) -0.009(2) -0.0037(17) C3 0.029(2) 0.023(2) 0.025(2) -0.0048(18) -0.007(2) -0.0065(17) C4 0.039(3) 0.022(2) 0.038(3) -0.005(2) -0.016(2) -0.0020(19) C5 0.031(3) 0.037(2) 0.031(3) -0.008(2) -0.014(2) -0.0038(19) C6 0.038(3) 0.038(2) 0.031(3) -0.012(2) -0.011(2) -0.014(2) C7 0.055(3) 0.028(2) 0.023(2) -0.0079(19) -0.011(2) -0.015(2) C8 0.029(3) 0.048(3) 0.045(3) -0.021(2) -0.011(2) -0.008(2) C9 0.027(3) 0.046(3) 0.038(3) -0.022(2) -0.004(2) 0.000(2) C10 0.030(2) 0.033(2) 0.037(3) -0.015(2) -0.006(2) -0.0136(19) C11 0.034(2) 0.0169(18) 0.031(3) -0.0002(18) -0.013(2) -0.0061(17) C12 0.034(3) 0.024(2) 0.044(3) -0.014(2) 0.003(2) 0.0011(19) C13 0.040(3) 0.033(2) 0.042(3) -0.007(2) 0.005(3) -0.007(2) C14 0.031(2) 0.0204(19) 0.027(3) -0.0108(19) -0.007(2) -0.0031(18) C15 0.046(3) 0.048(3) 0.036(3) -0.008(2) -0.019(3) -0.009(2) C16 0.059(4) 0.045(3) 0.050(4) -0.002(3) -0.032(3) 0.001(3) C17 0.059(4) 0.055(3) 0.069(4) -0.015(3) -0.040(4) 0.011(3) C18 0.053(3) 0.035(3) 0.039(3) -0.009(2) -0.014(3) -0.008(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 Mo1 O1 1.685(2) . ? Mo1 O2 1.701(3) . ? Mo1 O3 1.969(3) . ? Mo1 O4 2.363(2) . ? Mo1 O5 1.915(2) . ? Mo1 O10 2.290(3) . ? Mo2 O4 2.348(3) . ? Mo2 O5 1.894(2) . ? Mo2 O6 1.705(3) . ? Mo2 O7 1.692(3) . ? Mo2 O8 2.338(3) . ? Mo2 O11 1.977(2) 2_666 ? Mo3 O4 1.831(2) 2_666 ? Mo3 O8 1.753(3) . ? Mo3 O9 1.702(3) . ? Mo3 O10 1.787(2) . ? Mo4 O3 1.831(3) . ? Mo4 O11 1.838(2) . ? Mo4 O12 1.692(3) . ? Mo4 O13 1.698(3) . ? Cu3 N2 1.984(3) . ? Cu3 N2 1.984(3) 2_765 ? Cu3 N4 2.014(3) 1_545 ? Cu3 N4 2.014(3) 2_775 ? O4 Mo3 1.831(2) 2_666 ? O11 Mo2 1.977(2) 2_666 ? O14 H14A 0.8502 . ? O14 H14B 0.8505 . ? O15 H15C 0.8495 . ? O15 H15D 0.8500 . ? N1 C7 1.469(4) . ? N1 C8 1.353(5) . ? N1 C10 1.345(4) . ? N2 C9 1.373(5) . ? N2 C10 1.310(5) . ? N3 C11 1.468(4) . ? N3 C12 1.352(5) . ? N3 C14 1.339(4) . ? N4 Cu3 2.014(3) 1_565 ? N4 C13 1.361(5) . ? N4 C14 1.308(5) . ? N5 C15 1.473(5) . ? N5 C16 1.367(5) . ? N5 C18 1.322(5) . ? N6 H6 0.8600 . ? N6 C17 1.356(6) . ? N6 C18 1.318(5) . ? C1 C2 1.385(5) . ? C1 C6 1.380(5) . ? C1 C7 1.523(5) . ? C2 H2 0.9300 . ? C2 C3 1.390(4) . ? C3 C4 1.374(5) . ? C3 C11 1.515(5) . ? C4 H4 0.9300 . ? C4 C5 1.384(5) . ? C5 C6 1.380(5) . ? C5 C15 1.503(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9300 . ? C8 C9 1.352(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12 0.9300 . ? C12 C13 1.349(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16 0.9300 . ? C16 C17 1.340(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 O2 105.79(14) . . ? O1 Mo1 O3 99.92(12) . . ? O1 Mo1 O4 162.81(12) . . ? O1 Mo1 O5 100.52(12) . . ? O1 Mo1 O10 91.97(12) . . ? O2 Mo1 O3 94.36(12) . . ? O2 Mo1 O4 91.00(11) . . ? O2 Mo1 O5 100.38(13) . . ? O2 Mo1 O10 161.37(11) . . ? O3 Mo1 O4 82.08(9) . . ? O3 Mo1 O10 76.70(10) . . ? O5 Mo1 O3 150.40(9) . . ? O5 Mo1 O4 72.21(9) . . ? O5 Mo1 O10 81.43(10) . . ? O10 Mo1 O4 71.76(9) . . ? O5 Mo2 O4 72.91(9) . . ? O5 Mo2 O8 82.76(10) . . ? O5 Mo2 O11 148.94(11) . 2_666 ? O6 Mo2 O4 98.40(11) . . ? O6 Mo2 O5 100.64(11) . . ? O6 Mo2 O8 167.93(11) . . ? O6 Mo2 O11 93.17(11) . 2_666 ? O7 Mo2 O4 157.82(11) . . ? O7 Mo2 O5 102.44(11) . . ? O7 Mo2 O6 103.77(13) . . ? O7 Mo2 O8 86.61(11) . . ? O7 Mo2 O11 101.04(11) . 2_666 ? O8 Mo2 O4 71.36(9) . . ? O11 Mo2 O4 77.65(9) 2_666 . ? O11 Mo2 O8 78.62(10) 2_666 . ? O8 Mo3 O4 110.32(11) . 2_666 ? O8 Mo3 O10 110.61(11) . . ? O9 Mo3 O4 106.33(12) . 2_666 ? O9 Mo3 O8 106.83(13) . . ? O9 Mo3 O10 107.02(12) . . ? O10 Mo3 O4 115.24(11) . 2_666 ? O3 Mo4 O11 118.96(11) . . ? O12 Mo4 O3 109.58(14) . . ? O12 Mo4 O11 107.73(14) . . ? O12 Mo4 O13 107.04(18) . . ? O13 Mo4 O3 105.20(14) . . ? O13 Mo4 O11 107.74(13) . . ? N2 Cu3 N2 180.0 . 2_765 ? N2 Cu3 N4 90.89(12) . 1_545 ? N2 Cu3 N4 89.11(12) 2_765 1_545 ? N2 Cu3 N4 89.11(12) . 2_775 ? N2 Cu3 N4 90.89(12) 2_765 2_775 ? N4 Cu3 N4 180.000(1) 1_545 2_775 ? Mo4 O3 Mo1 133.37(15) . . ? Mo2 O4 Mo1 89.20(8) . . ? Mo3 O4 Mo1 135.93(13) 2_666 . ? Mo3 O4 Mo2 132.71(12) 2_666 . ? Mo2 O5 Mo1 120.59(12) . . ? Mo3 O8 Mo2 122.40(12) . . ? Mo3 O10 Mo1 123.88(13) . . ? Mo4 O11 Mo2 134.35(15) . 2_666 ? H14A O14 H14B 109.4 . . ? H15C O15 H15D 109.5 . . ? C8 N1 C7 126.7(3) . . ? C10 N1 C7 125.7(4) . . ? C10 N1 C8 107.6(3) . . ? C9 N2 Cu3 126.8(3) . . ? C10 N2 Cu3 127.1(3) . . ? C10 N2 C9 106.0(3) . . ? C12 N3 C11 126.7(3) . . ? C14 N3 C11 125.1(3) . . ? C14 N3 C12 107.0(3) . . ? C13 N4 Cu3 130.0(3) . 1_565 ? C14 N4 Cu3 122.7(3) . 1_565 ? C14 N4 C13 105.6(3) . . ? C16 N5 C15 125.7(4) . . ? C18 N5 C15 126.6(4) . . ? C18 N5 C16 107.6(4) . . ? C17 N6 H6 125.8 . . ? C18 N6 H6 125.8 . . ? C18 N6 C17 108.5(4) . . ? C2 C1 C7 118.5(3) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 C7 122.3(3) . . ? C1 C2 H2 119.6 . . ? C1 C2 C3 120.9(4) . . ? C3 C2 H2 119.6 . . ? C2 C3 C11 119.2(3) . . ? C4 C3 C2 118.3(3) . . ? C4 C3 C11 122.6(3) . . ? C3 C4 H4 118.9 . . ? C3 C4 C5 122.2(3) . . ? C5 C4 H4 118.9 . . ? C4 C5 C15 120.9(3) . . ? C6 C5 C4 118.3(4) . . ? C6 C5 C15 120.7(4) . . ? C1 C6 C5 121.2(4) . . ? C1 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? N1 C7 C1 112.8(3) . . ? N1 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C1 C7 H7A 109.0 . . ? C1 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C8 H8 126.7 . . ? C9 C8 N1 106.5(4) . . ? C9 C8 H8 126.7 . . ? N2 C9 H9 125.5 . . ? C8 C9 N2 109.1(4) . . ? C8 C9 H9 125.5 . . ? N1 C10 H10 124.6 . . ? N2 C10 N1 110.8(4) . . ? N2 C10 H10 124.6 . . ? N3 C11 C3 110.4(3) . . ? N3 C11 H11A 109.6 . . ? N3 C11 H11B 109.6 . . ? C3 C11 H11A 109.6 . . ? C3 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N3 C12 H12 126.8 . . ? C13 C12 N3 106.4(3) . . ? C13 C12 H12 126.8 . . ? N4 C13 H13 125.2 . . ? C12 C13 N4 109.5(4) . . ? C12 C13 H13 125.2 . . ? N3 C14 H14 124.3 . . ? N4 C14 N3 111.4(4) . . ? N4 C14 H14 124.3 . . ? N5 C15 C5 111.4(3) . . ? N5 C15 H15A 109.4 . . ? N5 C15 H15B 109.4 . . ? C5 C15 H15A 109.4 . . ? C5 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N5 C16 H16 126.3 . . ? C17 C16 N5 107.5(5) . . ? C17 C16 H16 126.3 . . ? N6 C17 H17 126.4 . . ? C16 C17 N6 107.2(4) . . ? C16 C17 H17 126.4 . . ? N5 C18 H18 125.4 . . ? N6 C18 N5 109.2(4) . . ? N6 C18 H18 125.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14A O15 0.85 2.07 2.876(6) 157.8 . O14 H14B O10 0.85 2.15 2.969(5) 160.2 . O15 H15C O9 0.85 2.10 2.949(4) 174.6 2_566 N6 H6 O14 0.86 1.94 2.774(6) 162.9 1_565 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu3 N2 C9 C8 177.7(3) . . . . ? Cu3 N2 C10 N1 -177.7(2) . . . . ? Cu3 N4 C13 C12 -165.3(3) 1_565 . . . ? Cu3 N4 C14 N3 167.1(2) 1_565 . . . ? O1 Mo1 O3 Mo4 -68.4(2) . . . . ? O1 Mo1 O4 Mo2 -81.4(4) . . . . ? O1 Mo1 O4 Mo3 114.7(4) . . . 2_666 ? O1 Mo1 O5 Mo2 -175.28(15) . . . . ? O1 Mo1 O10 Mo3 -153.07(17) . . . . ? O2 Mo1 O3 Mo4 -175.32(18) . . . . ? O2 Mo1 O4 Mo2 86.31(12) . . . . ? O2 Mo1 O4 Mo3 -77.6(2) . . . 2_666 ? O2 Mo1 O5 Mo2 -66.90(16) . . . . ? O2 Mo1 O10 Mo3 44.4(4) . . . . ? O3 Mo1 O4 Mo2 -179.42(11) . . . . ? O3 Mo1 O4 Mo3 16.7(2) . . . 2_666 ? O3 Mo1 O5 Mo2 51.7(3) . . . . ? O3 Mo1 O10 Mo3 107.20(16) . . . . ? O3 Mo4 O11 Mo2 -69.8(2) . . . 2_666 ? O4 Mo1 O3 Mo4 94.28(18) . . . . ? O4 Mo1 O5 Mo2 20.80(13) . . . . ? O4 Mo1 O10 Mo3 21.28(14) . . . . ? O4 Mo2 O5 Mo1 -20.86(13) . . . . ? O4 Mo2 O8 Mo3 -24.21(13) . . . . ? O4 Mo3 O8 Mo2 89.70(15) 2_666 . . . ? O4 Mo3 O10 Mo1 -84.44(17) 2_666 . . . ? O5 Mo1 O3 Mo4 64.7(3) . . . . ? O5 Mo1 O4 Mo2 -14.28(9) . . . . ? O5 Mo1 O4 Mo3 -178.2(2) . . . 2_666 ? O5 Mo1 O10 Mo3 -52.72(15) . . . . ? O5 Mo2 O4 Mo1 14.39(9) . . . . ? O5 Mo2 O4 Mo3 179.2(2) . . . 2_666 ? O5 Mo2 O8 Mo3 50.14(15) . . . . ? O6 Mo2 O4 Mo1 -84.24(11) . . . . ? O6 Mo2 O4 Mo3 80.55(19) . . . 2_666 ? O6 Mo2 O5 Mo1 74.75(16) . . . . ? O6 Mo2 O8 Mo3 -57.1(6) . . . . ? O7 Mo2 O4 Mo1 95.4(3) . . . . ? O7 Mo2 O4 Mo3 -99.8(3) . . . 2_666 ? O7 Mo2 O5 Mo1 -178.42(14) . . . . ? O7 Mo2 O8 Mo3 153.15(16) . . . . ? O8 Mo2 O4 Mo1 102.35(10) . . . . ? O8 Mo2 O4 Mo3 -92.86(18) . . . 2_666 ? O8 Mo2 O5 Mo1 -93.52(14) . . . . ? O8 Mo3 O10 Mo1 41.55(18) . . . . ? O9 Mo3 O8 Mo2 -155.12(14) . . . . ? O9 Mo3 O10 Mo1 157.57(15) . . . . ? O10 Mo1 O3 Mo4 21.24(16) . . . . ? O10 Mo1 O4 Mo2 -100.89(10) . . . . ? O10 Mo1 O4 Mo3 95.2(2) . . . 2_666 ? O10 Mo1 O5 Mo2 94.31(14) . . . . ? O10 Mo3 O8 Mo2 -38.99(18) . . . . ? O11 Mo2 O4 Mo1 -175.66(11) 2_666 . . . ? O11 Mo2 O4 Mo3 -10.87(18) 2_666 . . 2_666 ? O11 Mo2 O5 Mo1 -40.1(3) 2_666 . . . ? O11 Mo2 O8 Mo3 -104.87(16) 2_666 . . . ? O11 Mo4 O3 Mo1 -67.6(2) . . . . ? O12 Mo4 O3 Mo1 56.9(2) . . . . ? O12 Mo4 O11 Mo2 164.9(2) . . . 2_666 ? O13 Mo4 O3 Mo1 171.66(18) . . . . ? O13 Mo4 O11 Mo2 49.7(3) . . . 2_666 ? N1 C8 C9 N2 0.5(5) . . . . ? N2 Cu3 N2 C9 126(9) 2_765 . . . ? N2 Cu3 N2 C10 -55(9) 2_765 . . . ? N3 C12 C13 N4 -0.4(5) . . . . ? N4 Cu3 N2 C9 70.6(3) 1_545 . . . ? N4 Cu3 N2 C9 -109.4(3) 2_775 . . . ? N4 Cu3 N2 C10 -111.1(3) 1_545 . . . ? N4 Cu3 N2 C10 68.9(3) 2_775 . . . ? N5 C16 C17 N6 -1.4(6) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C1 C2 C3 C11 179.2(4) . . . . ? C2 C1 C6 C5 -0.1(6) . . . . ? C2 C1 C7 N1 -123.5(4) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C2 C3 C11 N3 137.5(4) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? C3 C4 C5 C15 176.9(4) . . . . ? C4 C3 C11 N3 -43.9(5) . . . . ? C4 C5 C6 C1 0.1(6) . . . . ? C4 C5 C15 N5 -69.4(5) . . . . ? C6 C1 C2 C3 -0.3(6) . . . . ? C6 C1 C7 N1 60.3(5) . . . . ? C6 C5 C15 N5 107.2(4) . . . . ? C7 N1 C8 C9 -179.9(3) . . . . ? C7 N1 C10 N2 179.4(3) . . . . ? C7 C1 C2 C3 -176.6(4) . . . . ? C7 C1 C6 C5 176.1(4) . . . . ? C8 N1 C7 C1 82.5(5) . . . . ? C8 N1 C10 N2 -0.6(4) . . . . ? C9 N2 C10 N1 0.9(4) . . . . ? C10 N1 C7 C1 -97.5(4) . . . . ? C10 N1 C8 C9 0.0(4) . . . . ? C10 N2 C9 C8 -0.8(5) . . . . ? C11 N3 C12 C13 168.5(4) . . . . ? C11 N3 C14 N4 -168.7(3) . . . . ? C11 C3 C4 C5 -179.1(4) . . . . ? C12 N3 C11 C3 -70.6(5) . . . . ? C12 N3 C14 N4 -0.6(4) . . . . ? C13 N4 C14 N3 0.4(4) . . . . ? C14 N3 C11 C3 95.2(4) . . . . ? C14 N3 C12 C13 0.6(5) . . . . ? C14 N4 C13 C12 0.0(5) . . . . ? C15 N5 C16 C17 177.5(4) . . . . ? C15 N5 C18 N6 -176.5(4) . . . . ? C15 C5 C6 C1 -176.6(4) . . . . ? C16 N5 C15 C5 152.1(4) . . . . ? C16 N5 C18 N6 0.0(5) . . . . ? C17 N6 C18 N5 -0.9(5) . . . . ? C18 N5 C15 C5 -32.0(6) . . . . ? C18 N5 C16 C17 0.9(5) . . . . ? C18 N6 C17 C16 1.5(6) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 938669' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nyy2013031802 _audit_creation_date 2013-03-25 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C72 H72 Cu4 Mo16 N24 O56), O' _chemical_formula_sum 'C36 H42 Cu2 Mo8 N12 O29' _chemical_formula_weight 2001.42 _chemical_melting_point ? _chemical_oxdiff_formula C20H20N4O4Mo8Cu1 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' Cu Cu 0.3201 1.2651 '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' 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 11.4044(6) _cell_length_b 22.5801(8) _cell_length_c 11.8951(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.844(6) _cell_angle_gamma 90.00 _cell_volume 2756.8(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5444 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 26.3104 _cell_measurement_theta_min 3.2879 _exptl_absorpt_coefficient_mu 2.610 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 2.411 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0519 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12576 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.31 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -12.00 25.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 -99.0000 -30.0000 37 #__ type_ start__ end____ width___ exp.time_ 2 omega -62.00 -25.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 124.0000 105.0000 37 #__ type_ start__ end____ width___ exp.time_ 3 omega -42.00 39.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 -57.0000 90.0000 81 #__ type_ start__ end____ width___ exp.time_ 4 omega -11.00 57.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 0.0000 90.0000 68 #__ type_ start__ end____ width___ exp.time_ 5 omega -6.00 19.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 19.7104 37.0000 150.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0626573000 _diffrn_orient_matrix_UB_12 0.0126499000 _diffrn_orient_matrix_UB_13 0.0185481000 _diffrn_orient_matrix_UB_21 0.0267327000 _diffrn_orient_matrix_UB_22 -0.0286481000 _diffrn_orient_matrix_UB_23 0.0032234000 _diffrn_orient_matrix_UB_31 -0.0118212000 _diffrn_orient_matrix_UB_32 0.0022309000 _diffrn_orient_matrix_UB_33 -0.0635453000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4614 _reflns_number_total 5626 _reflns_odcompleteness_completeness 99.74 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.647 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.132 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 401 _refine_ls_number_reflns 5626 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0355 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+2.6434P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.0715 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: H1 of C1, H18 of C18, H17 of C17, {H7A,H7B} of C7, {H2A,H2B} of C2, H15 of C15, H8 of C8, {H11A,H11B} of C11, H9 of C9, H16 of C16, H4 of C4, H14 of C14, H12 of C12, H6 of C6, H13 of C13 2. Restrained distances Cu1-O14A 2.1 with sigma of 0.02 Cu1-O14 2.2 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O14) ~ Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008 Uanis(O14) = Uanis(O14A) 4. Others Sof(O14)=1-Sof(O14A) Fixed Sof: O15(0.5) 5.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C7(H7A,H7B), C11(H11A,H11B) 5.b Aromatic/amide H refined with riding coordinates: C1(H1), C4(H4), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Mo1 Mo -0.05627(4) 0.386869(19) 0.23105(4) 0.01905(11) Uani 1 1 d . . . Mo2 Mo 0.21504(4) 0.401741(19) 0.48722(4) 0.01977(11) Uani 1 1 d . . . Mo3 Mo 0.00817(4) 0.524694(18) 0.36080(3) 0.01387(10) Uani 1 1 d . . . Mo4 Mo 0.27339(4) 0.519738(18) 0.66031(3) 0.01508(10) Uani 1 1 d . . . Cu1 Cu 0.24877(6) 0.64070(3) 0.52074(6) 0.02523(16) Uani 1 1 d D . . O1 O -0.1907(4) 0.34398(16) 0.1883(3) 0.0320(9) Uani 1 1 d . . . O2 O 0.0324(4) 0.35505(17) 0.1628(3) 0.0348(10) Uani 1 1 d . . . O3 O 0.0462(3) 0.36446(14) 0.4002(3) 0.0205(8) Uani 1 1 d . . . O4 O 0.0939(3) 0.46422(14) 0.3229(3) 0.0190(7) Uani 1 1 d . . . O5 O 0.2980(4) 0.37634(17) 0.4078(3) 0.0358(10) Uani 1 1 d . . . O6 O 0.2704(4) 0.35941(16) 0.6183(3) 0.0329(9) Uani 1 1 d . . . O7 O 0.3206(3) 0.47423(15) 0.5512(3) 0.0221(8) Uani 1 1 d . . . O8 O 0.1087(3) 0.46371(14) 0.5593(3) 0.0158(7) Uani 1 1 d . . . O9 O -0.0530(3) 0.56799(15) 0.2327(3) 0.0234(8) Uani 1 1 d . . . O10 O 0.1406(3) 0.56859(14) 0.4693(3) 0.0194(7) Uani 1 1 d . A . O11 O 0.1365(3) 0.54247(14) 0.7069(3) 0.0161(7) Uani 1 1 d . . . O12 O 0.3722(3) 0.48636(15) 0.7962(3) 0.0229(8) Uani 1 1 d . . . O13 O 0.3478(3) 0.58893(15) 0.6689(3) 0.0234(8) Uani 1 1 d . A . O14 O 0.4197(13) 0.6254(8) 0.4594(14) 0.056(3) Uani 0.54(2) 1 d PDU A 1 O15 O 0.4259(11) 0.5218(7) 0.4023(10) 0.110(5) Uani 0.50 1 d P . . N1 N -0.1358(4) 0.44325(18) 0.0627(3) 0.0208(9) Uani 1 1 d . . . N2 N -0.2456(4) 0.50884(18) -0.0809(3) 0.0210(9) Uani 1 1 d . . . N3 N 0.1407(4) 0.67954(19) 0.3599(4) 0.0269(10) Uani 1 1 d . A . N4 N -0.0222(4) 0.71759(19) 0.1965(4) 0.0266(10) Uani 1 1 d . A . N5 N -0.5802(4) 0.69731(19) 0.1442(4) 0.0249(10) Uani 1 1 d . . . N6 N -0.6622(4) 0.78725(19) 0.1092(4) 0.0288(11) Uani 1 1 d . . . C1 C -0.2490(5) 0.6497(2) -0.0178(4) 0.0251(12) Uani 1 1 d . . . H1 H -0.1849 0.6520 -0.0461 0.030 Uiso 1 1 calc R . . C2 C -0.5425(5) 0.6391(2) 0.1165(5) 0.0242(12) Uani 1 1 d . . . H2A H -0.6191 0.6191 0.0556 0.029 Uiso 1 1 calc R . . H2B H -0.5076 0.6154 0.1921 0.029 Uiso 1 1 calc R . . C3 C -0.2530(5) 0.6915(2) 0.0653(4) 0.0232(11) Uani 1 1 d . . . C4 C -0.3490(5) 0.6884(2) 0.1061(4) 0.0250(12) Uani 1 1 d . . . H4 H -0.3515 0.7168 0.1615 0.030 Uiso 1 1 calc R . . C5 C -0.4417(5) 0.6438(2) 0.0663(4) 0.0199(11) Uani 1 1 d . . . C6 C -0.4372(5) 0.6015(2) -0.0173(4) 0.0195(11) Uani 1 1 d . . . H6 H -0.4989 0.5714 -0.0450 0.023 Uiso 1 1 calc R . . C7 C -0.3353(5) 0.5576(2) -0.1483(4) 0.0265(12) Uani 1 1 d . . . H7A H -0.4219 0.5416 -0.1966 0.032 Uiso 1 1 calc R . . H7B H -0.3065 0.5757 -0.2060 0.032 Uiso 1 1 calc R . . C8 C -0.1745(6) 0.4759(3) -0.1262(5) 0.0366(15) Uani 1 1 d . . . H8 H -0.1734 0.4804 -0.2035 0.044 Uiso 1 1 calc R . . C9 C -0.1070(6) 0.4362(3) -0.0381(5) 0.0379(15) Uani 1 1 d . . . H9 H -0.0499 0.4082 -0.0438 0.046 Uiso 1 1 calc R . . C10 C -0.3407(5) 0.6041(2) -0.0596(4) 0.0223(11) Uani 1 1 d . . . C11 C -0.1521(5) 0.7403(2) 0.1129(5) 0.0318(13) Uani 1 1 d . . . H11A H -0.1477 0.7601 0.0425 0.038 Uiso 1 1 calc R . . H11B H -0.1786 0.7693 0.1575 0.038 Uiso 1 1 calc R . . C12 C 0.0785(6) 0.7099(3) 0.1659(5) 0.0405(16) Uani 1 1 d . A . H12 H 0.0785 0.7186 0.0895 0.049 Uiso 1 1 calc R . . C13 C 0.1784(6) 0.6872(3) 0.2672(5) 0.0415(15) Uani 1 1 d . . . H13 H 0.2603 0.6782 0.2727 0.050 Uiso 1 1 calc R A . C14 C 0.0194(5) 0.6982(2) 0.3140(5) 0.0303(13) Uani 1 1 d . . . H14 H -0.0312 0.6981 0.3578 0.036 Uiso 1 1 calc R A . C15 C -0.2205(5) 0.4879(2) 0.0325(4) 0.0231(12) Uani 1 1 d . . . H15 H -0.2570 0.5025 0.0833 0.028 Uiso 1 1 calc R . . C16 C -0.5248(5) 0.7273(2) 0.2570(5) 0.0301(13) Uani 1 1 d . . . H16 H -0.4637 0.7126 0.3331 0.036 Uiso 1 1 calc R . . C17 C -0.6617(5) 0.7353(2) 0.0586(5) 0.0269(12) Uani 1 1 d . . . H17 H -0.7112 0.7261 -0.0253 0.032 Uiso 1 1 calc R . . C18 C -0.5777(5) 0.7826(2) 0.2339(5) 0.0308(13) Uani 1 1 d . . . H18 H -0.5597 0.8125 0.2930 0.037 Uiso 1 1 calc R . . O14A O 0.3990(16) 0.5995(9) 0.4550(17) 0.056(3) Uani 0.46(2) 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 Mo1 0.0244(3) 0.0138(2) 0.0165(2) -0.00238(18) 0.00659(18) 0.00256(19) Mo2 0.0193(2) 0.0156(2) 0.0216(2) -0.00148(18) 0.00627(18) 0.00484(19) Mo3 0.0160(2) 0.0111(2) 0.01468(19) 0.00000(17) 0.00692(16) -0.00078(17) Mo4 0.0147(2) 0.0127(2) 0.0160(2) 0.00051(17) 0.00511(16) -0.00107(17) Cu1 0.0263(4) 0.0169(3) 0.0262(3) 0.0027(3) 0.0057(3) -0.0052(3) O1 0.039(2) 0.021(2) 0.0304(19) -0.0029(17) 0.0090(17) -0.0056(18) O2 0.045(3) 0.034(2) 0.0273(19) 0.0023(18) 0.0177(18) 0.019(2) O3 0.024(2) 0.0145(18) 0.0212(17) -0.0022(14) 0.0084(15) 0.0030(15) O4 0.025(2) 0.0176(19) 0.0179(16) 0.0008(14) 0.0123(15) 0.0028(15) O5 0.033(2) 0.036(2) 0.043(2) -0.013(2) 0.0213(19) 0.0022(19) O6 0.033(2) 0.024(2) 0.0285(19) 0.0021(17) 0.0019(16) 0.0047(18) O7 0.0163(19) 0.024(2) 0.0281(18) -0.0034(16) 0.0119(15) -0.0003(16) O8 0.0164(18) 0.0134(17) 0.0174(16) -0.0031(14) 0.0071(14) -0.0019(14) O9 0.027(2) 0.0201(19) 0.0201(17) 0.0011(15) 0.0075(15) -0.0007(16) O10 0.0174(19) 0.0153(18) 0.0222(17) 0.0005(15) 0.0055(14) -0.0030(15) O11 0.0184(19) 0.0120(17) 0.0168(16) -0.0045(14) 0.0066(14) -0.0012(14) O12 0.022(2) 0.0198(19) 0.0223(17) 0.0046(15) 0.0057(15) -0.0004(16) O13 0.022(2) 0.021(2) 0.0223(17) 0.0012(15) 0.0057(15) -0.0055(16) O14 0.040(4) 0.077(7) 0.055(3) 0.025(6) 0.027(3) -0.005(5) O15 0.072(9) 0.176(16) 0.079(8) 0.007(9) 0.032(7) -0.026(9) N1 0.026(2) 0.022(2) 0.0134(19) -0.0006(18) 0.0084(18) 0.002(2) N2 0.024(2) 0.021(2) 0.017(2) -0.0022(18) 0.0081(18) -0.0002(19) N3 0.027(3) 0.020(2) 0.027(2) 0.005(2) 0.007(2) -0.004(2) N4 0.025(3) 0.018(2) 0.030(2) 0.001(2) 0.006(2) -0.004(2) N5 0.025(3) 0.018(2) 0.030(2) -0.004(2) 0.010(2) 0.003(2) N6 0.030(3) 0.017(2) 0.027(2) -0.003(2) 0.001(2) 0.006(2) C1 0.023(3) 0.020(3) 0.030(3) 0.006(2) 0.009(2) 0.001(2) C2 0.026(3) 0.012(3) 0.034(3) -0.001(2) 0.012(2) 0.004(2) C3 0.018(3) 0.013(3) 0.029(3) 0.006(2) 0.001(2) 0.000(2) C4 0.028(3) 0.014(3) 0.025(3) 0.001(2) 0.005(2) 0.002(2) C5 0.019(3) 0.015(3) 0.019(2) 0.002(2) 0.003(2) 0.002(2) C6 0.019(3) 0.014(3) 0.019(2) 0.002(2) 0.002(2) 0.002(2) C7 0.028(3) 0.027(3) 0.021(3) 0.006(2) 0.008(2) 0.009(3) C8 0.051(4) 0.042(4) 0.027(3) 0.011(3) 0.026(3) 0.020(3) C9 0.055(4) 0.038(4) 0.031(3) 0.006(3) 0.028(3) 0.016(3) C10 0.027(3) 0.017(3) 0.017(2) 0.006(2) 0.003(2) 0.007(2) C11 0.024(3) 0.023(3) 0.040(3) 0.002(3) 0.006(2) -0.003(3) C12 0.030(4) 0.060(5) 0.030(3) 0.015(3) 0.012(3) 0.001(3) C13 0.031(4) 0.051(4) 0.045(3) 0.009(3) 0.018(3) -0.001(3) C14 0.029(3) 0.029(3) 0.034(3) 0.003(3) 0.015(3) -0.002(3) C15 0.026(3) 0.026(3) 0.014(2) -0.003(2) 0.005(2) 0.004(2) C16 0.031(3) 0.028(3) 0.023(3) -0.002(2) 0.005(2) 0.006(3) C17 0.024(3) 0.022(3) 0.027(3) -0.006(2) 0.003(2) 0.005(2) C18 0.035(4) 0.028(3) 0.025(3) -0.009(2) 0.008(2) 0.004(3) O14A 0.040(4) 0.077(7) 0.055(3) 0.025(6) 0.027(3) -0.005(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 Mo1 O1 1.694(4) . ? Mo1 O2 1.707(3) . ? Mo1 O3 1.903(3) . ? Mo1 O4 2.355(3) . ? Mo1 O11 2.125(3) 3_566 ? Mo1 N1 2.207(4) . ? Mo2 O3 1.936(3) . ? Mo2 O4 2.316(3) . ? Mo2 O5 1.702(3) . ? Mo2 O6 1.699(3) . ? Mo2 O7 1.977(3) . ? Mo2 O8 2.251(3) . ? Mo3 O4 1.846(3) . ? Mo3 O8 1.964(3) 3_566 ? Mo3 O9 1.685(3) . ? Mo3 O10 1.797(3) . ? Mo3 O11 2.124(3) 3_566 ? Mo4 O7 1.908(3) . ? Mo4 O8 2.146(3) . ? Mo4 O10 2.382(3) . ? Mo4 O11 1.940(3) . ? Mo4 O12 1.692(3) . ? Mo4 O13 1.760(3) . ? Cu1 O10 1.972(3) . ? Cu1 O13 2.003(3) . ? Cu1 O14 2.385(11) . ? Cu1 N3 1.973(4) . ? Cu1 N6 1.963(4) 4_676 ? Cu1 O14A 2.362(13) . ? O8 Mo3 1.963(3) 3_566 ? O11 Mo1 2.125(3) 3_566 ? O11 Mo3 2.124(3) 3_566 ? N1 C9 1.383(6) . ? N1 C15 1.332(6) . ? N2 C7 1.478(6) . ? N2 C8 1.372(6) . ? N2 C15 1.338(5) . ? N3 C13 1.358(6) . ? N3 C14 1.316(6) . ? N4 C11 1.470(6) . ? N4 C12 1.359(7) . ? N4 C14 1.339(6) . ? N5 C2 1.464(6) . ? N5 C16 1.385(6) . ? N5 C17 1.346(6) . ? N6 Cu1 1.963(4) 4_475 ? N6 C17 1.320(6) . ? N6 C18 1.376(6) . ? C1 H1 0.9300 . ? C1 C3 1.382(7) . ? C1 C10 1.396(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C5 1.513(6) . ? C3 C4 1.379(7) . ? C3 C11 1.513(7) . ? C4 H4 0.9300 . ? C4 C5 1.386(7) . ? C5 C6 1.395(6) . ? C6 H6 0.9300 . ? C6 C10 1.397(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C10 1.510(7) . ? C8 H8 0.9300 . ? C8 C9 1.340(7) . ? C9 H9 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12 0.9300 . ? C12 C13 1.347(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C16 C18 1.363(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 O2 105.27(18) . . ? O1 Mo1 O3 102.91(15) . . ? O1 Mo1 O4 160.65(14) . . ? O1 Mo1 O11 93.60(15) . 3_566 ? O1 Mo1 N1 95.59(16) . . ? O2 Mo1 O3 99.97(15) . . ? O2 Mo1 O4 94.07(16) . . ? O2 Mo1 O11 156.23(16) . 3_566 ? O2 Mo1 N1 84.57(15) . . ? O3 Mo1 O4 73.71(12) . . ? O3 Mo1 O11 89.50(12) . 3_566 ? O3 Mo1 N1 158.92(15) . . ? O11 Mo1 O4 67.56(11) 3_566 . ? O11 Mo1 N1 79.24(13) 3_566 . ? N1 Mo1 O4 85.48(13) . . ? O3 Mo2 O4 74.08(12) . . ? O3 Mo2 O7 149.59(13) . . ? O3 Mo2 O8 84.18(12) . . ? O5 Mo2 O3 102.76(16) . . ? O5 Mo2 O4 90.47(15) . . ? O5 Mo2 O7 95.73(16) . . ? O5 Mo2 O8 160.54(16) . . ? O6 Mo2 O3 97.51(16) . . ? O6 Mo2 O4 164.50(14) . . ? O6 Mo2 O5 104.24(18) . . ? O6 Mo2 O7 101.10(15) . . ? O6 Mo2 O8 92.66(14) . . ? O7 Mo2 O4 81.92(13) . . ? O7 Mo2 O8 71.20(12) . . ? O8 Mo2 O4 73.78(10) . . ? O4 Mo3 O8 139.52(13) . 3_566 ? O4 Mo3 O11 77.64(13) . 3_566 ? O8 Mo3 O11 72.53(12) 3_566 3_566 ? O9 Mo3 O4 105.24(14) . . ? O9 Mo3 O8 105.05(14) . 3_566 ? O9 Mo3 O10 102.51(15) . . ? O9 Mo3 O11 97.14(14) . 3_566 ? O10 Mo3 O4 102.39(14) . . ? O10 Mo3 O8 96.56(13) . 3_566 ? O10 Mo3 O11 159.52(12) . 3_566 ? O7 Mo4 O8 74.87(12) . . ? O7 Mo4 O10 81.42(12) . . ? O7 Mo4 O11 146.92(14) . . ? O8 Mo4 O10 72.63(11) . . ? O11 Mo4 O8 72.49(12) . . ? O11 Mo4 O10 83.91(11) . . ? O12 Mo4 O7 98.17(15) . . ? O12 Mo4 O8 109.18(14) . . ? O12 Mo4 O10 178.01(14) . . ? O12 Mo4 O11 97.41(14) . . ? O12 Mo4 O13 103.68(15) . . ? O13 Mo4 O7 104.21(15) . . ? O13 Mo4 O8 146.95(13) . . ? O13 Mo4 O10 74.58(13) . . ? O13 Mo4 O11 100.17(14) . . ? O10 Cu1 O13 80.09(13) . . ? O10 Cu1 O14 105.7(5) . . ? O10 Cu1 N3 91.38(15) . . ? O10 Cu1 O14A 91.0(5) . . ? O13 Cu1 O14 87.8(4) . . ? O13 Cu1 O14A 81.3(4) . . ? N3 Cu1 O13 170.69(16) . . ? N3 Cu1 O14 90.9(4) . . ? N3 Cu1 O14A 95.2(5) . . ? N6 Cu1 O10 163.33(15) 4_676 . ? N6 Cu1 O13 92.90(15) 4_676 . ? N6 Cu1 O14 89.0(5) 4_676 . ? N6 Cu1 N3 96.31(17) 4_676 . ? N6 Cu1 O14A 102.9(6) 4_676 . ? O14A Cu1 O14 15.1(4) . . ? Mo1 O3 Mo2 117.30(16) . . ? Mo2 O4 Mo1 89.16(11) . . ? Mo3 O4 Mo1 107.84(14) . . ? Mo3 O4 Mo2 115.39(13) . . ? Mo4 O7 Mo2 113.73(15) . . ? Mo3 O8 Mo2 149.24(16) 3_566 . ? Mo3 O8 Mo4 105.26(13) 3_566 . ? Mo4 O8 Mo2 95.43(12) . . ? Mo3 O10 Mo4 114.54(15) . . ? Mo3 O10 Cu1 153.45(18) . . ? Cu1 O10 Mo4 91.98(12) . . ? Mo3 O11 Mo1 106.67(13) 3_566 3_566 ? Mo4 O11 Mo1 145.07(17) . 3_566 ? Mo4 O11 Mo3 106.96(13) . 3_566 ? Mo4 O13 Cu1 113.24(16) . . ? C9 N1 Mo1 124.1(3) . . ? C15 N1 Mo1 130.0(3) . . ? C15 N1 C9 105.8(4) . . ? C8 N2 C7 125.3(4) . . ? C15 N2 C7 127.2(4) . . ? C15 N2 C8 107.6(4) . . ? C13 N3 Cu1 124.0(4) . . ? C14 N3 Cu1 130.1(4) . . ? C14 N3 C13 105.7(4) . . ? C12 N4 C11 125.7(4) . . ? C14 N4 C11 127.8(5) . . ? C14 N4 C12 106.4(4) . . ? C16 N5 C2 127.0(4) . . ? C17 N5 C2 125.1(4) . . ? C17 N5 C16 107.1(4) . . ? C17 N6 Cu1 126.6(3) . 4_475 ? C17 N6 C18 106.5(4) . . ? C18 N6 Cu1 126.6(4) . 4_475 ? C3 C1 H1 119.8 . . ? C3 C1 C10 120.4(5) . . ? C10 C1 H1 119.8 . . ? N5 C2 H2A 109.2 . . ? N5 C2 H2B 109.2 . . ? N5 C2 C5 111.9(4) . . ? H2A C2 H2B 107.9 . . ? C5 C2 H2A 109.2 . . ? C5 C2 H2B 109.2 . . ? C1 C3 C11 120.5(5) . . ? C4 C3 C1 119.7(5) . . ? C4 C3 C11 119.8(5) . . ? C3 C4 H4 119.3 . . ? C3 C4 C5 121.5(5) . . ? C5 C4 H4 119.3 . . ? C4 C5 C2 121.0(4) . . ? C4 C5 C6 118.7(5) . . ? C6 C5 C2 120.3(4) . . ? C5 C6 H6 119.7 . . ? C5 C6 C10 120.5(5) . . ? C10 C6 H6 119.7 . . ? N2 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? N2 C7 C10 111.6(4) . . ? H7A C7 H7B 108.0 . . ? C10 C7 H7A 109.3 . . ? C10 C7 H7B 109.3 . . ? N2 C8 H8 126.5 . . ? C9 C8 N2 107.0(4) . . ? C9 C8 H8 126.5 . . ? N1 C9 H9 125.4 . . ? C8 C9 N1 109.1(5) . . ? C8 C9 H9 125.4 . . ? C1 C10 C6 119.2(4) . . ? C1 C10 C7 120.6(5) . . ? C6 C10 C7 120.1(5) . . ? N4 C11 C3 112.2(4) . . ? N4 C11 H11A 109.2 . . ? N4 C11 H11B 109.2 . . ? C3 C11 H11A 109.2 . . ? C3 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N4 C12 H12 126.5 . . ? C13 C12 N4 107.0(5) . . ? C13 C12 H12 126.5 . . ? N3 C13 H13 125.3 . . ? C12 C13 N3 109.3(5) . . ? C12 C13 H13 125.3 . . ? N3 C14 N4 111.5(5) . . ? N3 C14 H14 124.2 . . ? N4 C14 H14 124.2 . . ? N1 C15 N2 110.5(4) . . ? N1 C15 H15 124.7 . . ? N2 C15 H15 124.7 . . ? N5 C16 H16 126.9 . . ? C18 C16 N5 106.1(4) . . ? C18 C16 H16 126.9 . . ? N5 C17 H17 124.5 . . ? N6 C17 N5 111.1(4) . . ? N6 C17 H17 124.5 . . ? N6 C18 H18 125.4 . . ? C16 C18 N6 109.1(5) . . ? C16 C18 H18 125.4 . . ? _database_code_depnum_ccdc_archive 'CCDC 938670' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nyy134901 _audit_creation_date 2013-04-12 _audit_creation_method ; Olex2 1.2 (compiled Mar 21 2013 11:16:32, GUI svn.r4446) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Co H4 Mo16 O54, 2(O), 2(C18 H21 N6)' _chemical_formula_sum 'C36 H50 Co Mo16 N12 O56' _chemical_formula_weight 3140.85 _chemical_melting_point ? _chemical_oxdiff_formula C20H20N4O4Mo4Co1 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' Co Co 0.3494 0.9721 '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' 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.6394(4) _cell_length_b 10.3809(4) _cell_length_c 20.3352(8) _cell_angle_alpha 104.412(4) _cell_angle_beta 95.009(3) _cell_angle_gamma 101.078(3) _cell_volume 1914.46(13) _cell_formula_units_Z 1 _cell_measurement_reflns_used 7800 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 26.3149 _cell_measurement_theta_min 3.1285 _exptl_absorpt_coefficient_mu 2.847 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 2.724 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1497 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_unetI/netI 0.0352 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 15733 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.13 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -9.00 29.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - -17.1323 -113.0000 2.0000 38 #__ type_ start__ end____ width___ exp.time_ 2 omega 0.00 37.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 19.7104 57.0000 -60.0000 37 #__ type_ start__ end____ width___ exp.time_ 3 omega 39.00 79.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 19.7104 178.0000 90.0000 40 #__ type_ start__ end____ width___ exp.time_ 4 omega -50.00 45.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 19.7104 -77.0000 90.0000 95 #__ type_ start__ end____ width___ exp.time_ 5 omega -40.00 39.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 19.7104 -57.0000 -60.0000 79 #__ type_ start__ end____ width___ exp.time_ 6 omega 3.00 89.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 19.7104 57.0000 -150.0000 86 #__ type_ start__ end____ width___ exp.time_ 7 omega 35.00 94.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 19.7104 178.0000 -60.0000 59 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0246616000 _diffrn_orient_matrix_UB_12 0.0651695000 _diffrn_orient_matrix_UB_13 0.0237627000 _diffrn_orient_matrix_UB_21 0.0232496000 _diffrn_orient_matrix_UB_22 0.0274818000 _diffrn_orient_matrix_UB_23 -0.0268130000 _diffrn_orient_matrix_UB_31 -0.0677446000 _diffrn_orient_matrix_UB_32 0.0152241000 _diffrn_orient_matrix_UB_33 -0.0063354000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6480 _reflns_number_total 7794 _reflns_odcompleteness_completeness 99.77 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.839 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.136 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 552 _refine_ls_number_reflns 7794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0291 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+1.5604P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.0676 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O28) = Uanis(O28A) 3. Others Sof(O28)=1-Sof(O28A) 4.a Rotating group: O1(H1A,H1B) 4.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B) 4.c Aromatic/amide H refined with riding coordinates: N2(H2), N4(H4), N6(H6), C2(H2A), C4(H4A), C6(H6A), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Mo1 Mo 1.13192(3) 0.34980(3) 0.135257(16) 0.01242(8) Uani 1 1 d . . . Mo2 Mo 1.17758(3) 0.59155(3) 0.286193(17) 0.01351(8) Uani 1 1 d . . . Mo3 Mo 0.93753(3) 0.57540(3) 0.385675(16) 0.01411(8) Uani 1 1 d . . . Mo4 Mo 0.89366(3) 0.30568(3) 0.235699(16) 0.01205(8) Uani 1 1 d . . . Mo5 Mo 0.74302(3) 0.34584(3) 0.090469(16) 0.01245(8) Uani 1 1 d . . . Mo6 Mo 0.78587(3) 0.61604(3) 0.241670(16) 0.01235(8) Uani 1 1 d . . . Mo7 Mo 0.54795(3) 0.57651(4) 0.344302(17) 0.01685(9) Uani 1 1 d . . . Mo8 Mo 0.49927(3) 0.33544(3) 0.188076(17) 0.01377(8) Uani 1 1 d . . . Co1 Co 1.0000 0.5000 0.0000 0.01699(17) Uani 1 2 d S . . O1 O 1.0178(3) 0.6659(3) 0.08039(14) 0.0261(7) Uani 1 1 d . . . H1A H 1.0204 0.7359 0.0651 0.039 Uiso 1 1 d R . . H1B H 1.0949 0.6782 0.1077 0.039 Uiso 1 1 d R . . O2 O 1.1181(3) 0.4029(3) 0.06116(13) 0.0196(6) Uani 1 1 d . . . O3 O 1.1095(3) 0.1784(3) 0.10714(15) 0.0256(7) Uani 1 1 d . . . O4 O 1.3315(3) 0.3882(3) 0.16337(14) 0.0209(6) Uani 1 1 d . . . O5 O 0.9277(2) 0.3524(3) 0.14236(13) 0.0147(6) Uani 1 1 d . . . O6 O 1.0933(3) 0.3497(3) 0.23914(13) 0.0158(6) Uani 1 1 d . . . O7 O 1.1670(3) 0.5664(3) 0.19677(13) 0.0186(6) Uani 1 1 d . . . O8 O 1.3490(3) 0.5504(3) 0.30817(15) 0.0266(7) Uani 1 1 d . . . O9 O 1.2094(3) 0.7617(3) 0.31743(14) 0.0259(7) Uani 1 1 d . . . O10 O 1.1188(3) 0.5429(3) 0.37429(13) 0.0158(6) Uani 1 1 d . . . O11 O 0.9558(2) 0.5565(3) 0.27603(13) 0.0139(6) Uani 1 1 d . . . O12 O 0.9773(3) 0.7481(3) 0.41603(14) 0.0236(7) Uani 1 1 d . . . O13 O 0.8857(3) 0.5200(3) 0.45443(13) 0.0209(6) Uani 1 1 d . . . O14 O 0.7461(3) 0.5617(3) 0.33459(13) 0.0171(6) Uani 1 1 d . . . O15 O 0.8726(3) 0.3412(3) 0.32209(13) 0.0184(6) Uani 1 1 d . . . O16 O 0.8506(3) 0.1346(3) 0.20786(15) 0.0238(7) Uani 1 1 d . . . O17 O 0.7186(3) 0.3565(3) 0.19928(13) 0.0150(6) Uani 1 1 d . . . O18 O 0.8153(3) 0.5814(3) 0.15592(13) 0.0170(6) Uani 1 1 d . . . O19 O 0.8068(3) 0.4146(3) 0.02638(13) 0.0208(6) Uani 1 1 d . . . O20 O 0.7013(3) 0.1752(3) 0.05424(15) 0.0253(7) Uani 1 1 d . . . O21 O 0.5673(3) 0.3840(3) 0.10151(13) 0.0166(6) Uani 1 1 d . . . O22 O 0.8366(3) 0.7872(3) 0.27230(14) 0.0236(7) Uani 1 1 d . . . O23 O 0.5897(3) 0.5745(3) 0.23490(13) 0.0165(6) Uani 1 1 d . . . O24 O 0.5802(3) 0.7478(3) 0.37520(16) 0.0352(8) Uani 1 1 d . . . O25 O 0.5317(3) 0.5175(4) 0.41408(15) 0.0364(8) Uani 1 1 d . . . O26 O 0.4985(3) 0.3577(3) 0.27625(14) 0.0208(6) Uani 1 1 d . . . O27 O 0.4530(3) 0.1655(3) 0.15568(15) 0.0278(7) Uani 1 1 d . . . O28 O 1.0680(8) 0.8979(5) 0.0430(3) 0.093(2) Uani 0.823(6) 1 d P A 1 O28A O 0.965(4) 0.922(2) 0.1040(13) 0.093(2) Uani 0.177(6) 1 d P A 2 N1 N 0.6799(4) 0.1191(4) 0.41212(19) 0.0312(9) Uani 1 1 d . . . N2 N 0.6963(6) 0.2667(6) 0.5073(3) 0.086(2) Uani 1 1 d . . . H2 H 0.7101 0.3450 0.5367 0.103 Uiso 1 1 calc R . . N3 N 0.1540(4) 0.1295(4) 0.33846(19) 0.0297(9) Uani 1 1 d . . . N4 N 0.1367(5) 0.2631(5) 0.4342(2) 0.0503(13) Uani 1 1 d . . . H4 H 0.1415 0.3360 0.4665 0.060 Uiso 1 1 calc R . . N5 N 0.5125(4) -0.2459(4) 0.08897(18) 0.0254(8) Uani 1 1 d . . . N6 N 0.6803(5) -0.2798(6) 0.0291(2) 0.0564(14) Uani 1 1 d . . . H6 H 0.7413 -0.3176 0.0075 0.068 Uiso 1 1 calc R . . C1 C 0.5444(4) 0.0012(4) 0.2955(2) 0.0218(9) Uani 1 1 d . . . C2 C 0.4291(5) 0.0617(4) 0.3066(2) 0.0264(10) Uani 1 1 d . . . H2A H 0.4359 0.1350 0.3448 0.032 Uiso 1 1 calc R . . C3 C 0.3037(5) 0.0131(5) 0.2607(2) 0.0254(10) Uani 1 1 d . . . C4 C 0.2940(4) -0.0945(4) 0.2038(2) 0.0250(10) Uani 1 1 d . . . H4A H 0.2098 -0.1268 0.1730 0.030 Uiso 1 1 calc R . . C5 C 0.4087(4) -0.1551(4) 0.1921(2) 0.0241(10) Uani 1 1 d . . . C6 C 0.5331(4) -0.1071(4) 0.2385(2) 0.0241(10) Uani 1 1 d . . . H6A H 0.6100 -0.1485 0.2312 0.029 Uiso 1 1 calc R . . C7 C 0.6865(5) 0.0527(5) 0.3409(2) 0.0314(11) Uani 1 1 d . . . H7A H 0.7316 -0.0237 0.3395 0.038 Uiso 1 1 calc R . . H7B H 0.7470 0.1167 0.3223 0.038 Uiso 1 1 calc R . . C8 C 0.1789(6) 0.0812(6) 0.2679(2) 0.0476(15) Uani 1 1 d . . . H8A H 0.1956 0.1580 0.2482 0.057 Uiso 1 1 calc R . . H8B H 0.0935 0.0171 0.2417 0.057 Uiso 1 1 calc R . . C9 C 0.3974(5) -0.2740(5) 0.1296(2) 0.0322(11) Uani 1 1 d . . . H9A H 0.4027 -0.3554 0.1440 0.039 Uiso 1 1 calc R . . H9B H 0.3057 -0.2907 0.1015 0.039 Uiso 1 1 calc R . . C10 C 0.6584(7) 0.0559(7) 0.4622(3) 0.0672(19) Uani 1 1 d . . . H10 H 0.6410 -0.0378 0.4564 0.081 Uiso 1 1 calc R . . C11 C 0.6662(8) 0.1501(8) 0.5212(3) 0.080(2) Uani 1 1 d . . . H11 H 0.6528 0.1353 0.5636 0.096 Uiso 1 1 calc R . . C12 C 0.7025(8) 0.2464(6) 0.4402(3) 0.085(3) Uani 1 1 d . . . H12 H 0.7203 0.3145 0.4177 0.102 Uiso 1 1 calc R . . C13 C 0.1028(6) 0.0501(6) 0.3784(3) 0.0519(16) Uani 1 1 d . . . H13 H 0.0804 -0.0447 0.3664 0.062 Uiso 1 1 calc R . . C14 C 0.0902(7) 0.1332(6) 0.4384(3) 0.0617(18) Uani 1 1 d . . . H14 H 0.0564 0.1073 0.4757 0.074 Uiso 1 1 calc R . . C15 C 0.1727(5) 0.2593(5) 0.3734(2) 0.0357(12) Uani 1 1 d . . . H15 H 0.2057 0.3345 0.3574 0.043 Uiso 1 1 calc R . . C16 C 0.6616(6) -0.1486(7) 0.0337(3) 0.0610(18) Uani 1 1 d . . . H16 H 0.7132 -0.0857 0.0144 0.073 Uiso 1 1 calc R . . C17 C 0.5584(6) -0.1295(5) 0.0701(3) 0.0469(14) Uani 1 1 d . . . H17 H 0.5227 -0.0509 0.0811 0.056 Uiso 1 1 calc R . . C18 C 0.5897(5) -0.3351(5) 0.0631(2) 0.0337(12) Uani 1 1 d . . . H18 H 0.5801 -0.4226 0.0685 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00978(15) 0.01722(18) 0.01068(16) 0.00275(13) 0.00268(13) 0.00477(13) Mo2 0.00862(15) 0.01671(18) 0.01357(17) 0.00094(14) 0.00242(13) 0.00267(13) Mo3 0.01150(15) 0.02011(19) 0.01018(16) 0.00161(14) 0.00144(13) 0.00551(14) Mo4 0.01057(15) 0.01473(18) 0.01188(17) 0.00441(13) 0.00214(13) 0.00394(13) Mo5 0.00948(15) 0.01725(18) 0.01027(16) 0.00306(13) 0.00158(13) 0.00293(13) Mo6 0.00974(15) 0.01528(18) 0.01258(17) 0.00358(13) 0.00182(13) 0.00423(13) Mo7 0.01013(16) 0.0262(2) 0.01337(17) 0.00183(15) 0.00284(13) 0.00618(14) Mo8 0.00865(15) 0.01765(18) 0.01500(17) 0.00406(14) 0.00318(13) 0.00273(13) Co1 0.0163(4) 0.0206(4) 0.0140(4) 0.0047(3) 0.0041(3) 0.0030(3) O1 0.0297(16) 0.0253(17) 0.0197(16) 0.0038(13) -0.0001(13) 0.0022(13) O2 0.0163(13) 0.0305(17) 0.0130(14) 0.0064(12) 0.0021(11) 0.0068(12) O3 0.0257(15) 0.0216(16) 0.0283(17) 0.0024(13) 0.0052(13) 0.0077(13) O4 0.0115(13) 0.0311(17) 0.0185(15) 0.0032(13) 0.0028(12) 0.0052(12) O5 0.0105(12) 0.0234(15) 0.0135(13) 0.0091(11) 0.0044(11) 0.0053(11) O6 0.0117(12) 0.0212(15) 0.0154(14) 0.0058(12) 0.0008(11) 0.0050(11) O7 0.0164(13) 0.0206(15) 0.0175(14) 0.0021(12) 0.0041(12) 0.0042(12) O8 0.0125(13) 0.0415(19) 0.0249(16) 0.0033(14) 0.0040(12) 0.0106(13) O9 0.0326(16) 0.0187(16) 0.0211(16) 0.0003(13) 0.0065(14) -0.0012(13) O10 0.0112(12) 0.0236(15) 0.0122(13) 0.0031(12) 0.0013(11) 0.0054(11) O11 0.0100(12) 0.0169(14) 0.0137(13) 0.0020(11) 0.0015(11) 0.0031(11) O12 0.0249(15) 0.0204(16) 0.0231(16) -0.0003(13) 0.0046(13) 0.0067(13) O13 0.0210(14) 0.0290(17) 0.0128(14) 0.0053(12) 0.0036(12) 0.0063(13) O14 0.0127(13) 0.0276(16) 0.0147(14) 0.0084(12) 0.0037(11) 0.0089(12) O15 0.0172(13) 0.0219(16) 0.0156(14) 0.0048(12) 0.0028(12) 0.0030(12) O16 0.0265(15) 0.0177(16) 0.0267(16) 0.0054(13) 0.0047(13) 0.0044(13) O17 0.0107(12) 0.0210(15) 0.0145(14) 0.0061(12) 0.0019(11) 0.0044(11) O18 0.0184(13) 0.0192(15) 0.0151(14) 0.0070(12) 0.0032(11) 0.0048(12) O19 0.0158(13) 0.0284(17) 0.0173(15) 0.0077(12) 0.0035(12) 0.0001(12) O20 0.0238(15) 0.0217(16) 0.0255(16) -0.0012(13) 0.0021(13) 0.0037(13) O21 0.0121(12) 0.0239(16) 0.0154(14) 0.0069(12) 0.0020(11) 0.0058(11) O22 0.0222(15) 0.0177(16) 0.0265(16) 0.0002(13) 0.0010(13) 0.0025(12) O23 0.0125(13) 0.0188(15) 0.0181(14) 0.0027(12) 0.0001(11) 0.0070(11) O24 0.0296(17) 0.0327(19) 0.0369(19) -0.0060(15) 0.0049(15) 0.0120(15) O25 0.0354(18) 0.058(2) 0.0205(16) 0.0159(16) 0.0096(15) 0.0124(17) O26 0.0190(14) 0.0245(16) 0.0187(15) 0.0063(12) 0.0044(12) 0.0033(12) O27 0.0279(16) 0.0192(16) 0.0327(18) 0.0019(14) 0.0095(14) 0.0010(13) O28 0.189(7) 0.029(3) 0.053(3) 0.011(2) 0.019(4) 0.008(3) O28A 0.189(7) 0.029(3) 0.053(3) 0.011(2) 0.019(4) 0.008(3) N1 0.030(2) 0.027(2) 0.025(2) -0.0032(17) 0.0013(17) -0.0061(17) N2 0.098(5) 0.059(4) 0.057(4) -0.036(3) 0.037(3) -0.032(3) N3 0.036(2) 0.033(2) 0.023(2) 0.0018(17) 0.0071(17) 0.0213(18) N4 0.076(3) 0.040(3) 0.033(3) -0.007(2) 0.010(2) 0.030(3) N5 0.0279(19) 0.028(2) 0.0195(19) 0.0025(16) 0.0022(16) 0.0095(17) N6 0.045(3) 0.083(4) 0.042(3) 0.009(3) 0.018(2) 0.023(3) C1 0.024(2) 0.023(2) 0.019(2) 0.0083(18) 0.0057(18) 0.0027(18) C2 0.041(3) 0.023(2) 0.015(2) 0.0000(18) 0.008(2) 0.010(2) C3 0.031(2) 0.033(3) 0.020(2) 0.0107(19) 0.0097(19) 0.017(2) C4 0.025(2) 0.033(3) 0.020(2) 0.0067(19) 0.0061(19) 0.012(2) C5 0.028(2) 0.020(2) 0.022(2) 0.0012(18) 0.0066(19) 0.0054(18) C6 0.024(2) 0.021(2) 0.028(2) 0.0041(19) 0.0055(19) 0.0094(18) C7 0.032(2) 0.037(3) 0.020(2) 0.001(2) 0.007(2) 0.001(2) C8 0.062(4) 0.072(4) 0.022(3) 0.008(3) 0.009(3) 0.051(3) C9 0.028(2) 0.025(3) 0.034(3) -0.008(2) 0.006(2) 0.003(2) C10 0.109(6) 0.059(4) 0.027(3) 0.008(3) 0.004(3) 0.010(4) C11 0.099(6) 0.090(6) 0.028(3) 0.001(4) 0.005(4) -0.014(5) C12 0.130(6) 0.034(4) 0.070(5) -0.005(3) 0.060(5) -0.027(4) C13 0.077(4) 0.030(3) 0.049(4) 0.004(3) 0.029(3) 0.013(3) C14 0.100(5) 0.054(4) 0.048(4) 0.022(3) 0.046(4) 0.030(4) C15 0.046(3) 0.031(3) 0.035(3) 0.011(2) 0.004(2) 0.019(2) C16 0.057(4) 0.078(5) 0.046(4) 0.030(4) 0.015(3) -0.010(3) C17 0.062(4) 0.033(3) 0.050(3) 0.017(3) 0.005(3) 0.012(3) C18 0.037(3) 0.042(3) 0.024(2) 0.003(2) 0.005(2) 0.022(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 Mo1 O2 1.732(3) . ? Mo1 O3 1.692(3) . ? Mo1 O4 1.894(3) . ? Mo1 O5 1.991(2) . ? Mo1 O6 2.177(3) . ? Mo1 O7 2.229(3) . ? Mo2 Mo3 3.2113(4) . ? Mo2 O6 2.401(3) . ? Mo2 O7 1.762(3) . ? Mo2 O8 1.831(3) . ? Mo2 O9 1.679(3) . ? Mo2 O10 2.074(3) . ? Mo2 O11 2.082(2) . ? Mo3 O10 1.865(2) . ? Mo3 O11 2.215(3) . ? Mo3 O12 1.699(3) . ? Mo3 O13 1.717(3) . ? Mo3 O14 1.999(3) . ? Mo3 O15 2.384(3) . ? Mo4 O5 2.110(3) . ? Mo4 O6 1.881(2) . ? Mo4 O11 2.463(3) . ? Mo4 O15 1.741(3) . ? Mo4 O16 1.680(3) . ? Mo4 O17 1.998(2) . ? Mo5 Mo8 3.2086(4) . ? Mo5 O5 1.969(2) . ? Mo5 O17 2.223(3) . ? Mo5 O18 2.408(3) . ? Mo5 O19 1.738(3) . ? Mo5 O20 1.693(3) . ? Mo5 O21 1.832(2) . ? Mo6 O11 1.989(2) . ? Mo6 O14 2.147(3) . ? Mo6 O18 1.750(3) . ? Mo6 O22 1.687(3) . ? Mo6 O23 1.842(2) . ? Mo7 O8 1.935(3) 1_455 ? Mo7 O14 1.969(2) . ? Mo7 O23 2.291(3) . ? Mo7 O24 1.688(3) . ? Mo7 O25 1.688(3) . ? Mo7 O26 2.281(3) . ? Mo8 O4 1.872(3) 1_455 ? Mo8 O17 2.070(2) . ? Mo8 O21 2.074(3) . ? Mo8 O23 2.381(3) . ? Mo8 O26 1.751(3) . ? Mo8 O27 1.677(3) . ? Co1 O1 2.026(3) 2_765 ? Co1 O1 2.026(3) . ? Co1 O2 2.162(3) 2_765 ? Co1 O2 2.162(3) . ? Co1 O19 2.078(2) . ? Co1 O19 2.078(2) 2_765 ? O1 H1A 0.8547 . ? O1 H1B 0.8559 . ? O4 Mo8 1.872(3) 1_655 ? O8 Mo7 1.935(3) 1_655 ? N1 C7 1.453(5) . ? N1 C10 1.351(7) . ? N1 C12 1.270(7) . ? N2 H2 0.8600 . ? N2 C11 1.295(9) . ? N2 C12 1.336(8) . ? N3 C8 1.455(5) . ? N3 C13 1.354(6) . ? N3 C15 1.327(6) . ? N4 H4 0.8600 . ? N4 C14 1.363(7) . ? N4 C15 1.308(6) . ? N5 C9 1.468(5) . ? N5 C17 1.363(6) . ? N5 C18 1.334(5) . ? N6 H6 0.8600 . ? N6 C16 1.389(8) . ? N6 C18 1.296(6) . ? C1 C2 1.387(6) . ? C1 C6 1.378(5) . ? C1 C7 1.507(6) . ? C2 H2A 0.9300 . ? C2 C3 1.386(6) . ? C3 C4 1.376(6) . ? C3 C8 1.508(6) . ? C4 H4A 0.9300 . ? C4 C5 1.383(5) . ? C5 C6 1.384(6) . ? C5 C9 1.515(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10 0.9300 . ? C10 C11 1.331(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C13 C14 1.336(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C16 C17 1.307(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 O2 Mo1 O4 103.42(12) . . ? O2 Mo1 O5 89.97(11) . . ? O2 Mo1 O6 154.74(11) . . ? O2 Mo1 O7 89.08(11) . . ? O3 Mo1 O2 104.56(13) . . ? O3 Mo1 O4 96.46(13) . . ? O3 Mo1 O5 96.91(12) . . ? O3 Mo1 O6 94.61(12) . . ? O3 Mo1 O7 166.36(13) . . ? O4 Mo1 O5 158.03(11) . . ? O4 Mo1 O6 90.36(10) . . ? O4 Mo1 O7 79.97(11) . . ? O5 Mo1 O6 71.25(10) . . ? O5 Mo1 O7 82.95(10) . . ? O6 Mo1 O7 72.36(10) . . ? O6 Mo2 Mo3 87.04(6) . . ? O7 Mo2 Mo3 132.35(8) . . ? O7 Mo2 O6 75.61(11) . . ? O7 Mo2 O8 102.39(12) . . ? O7 Mo2 O10 154.24(11) . . ? O7 Mo2 O11 89.15(11) . . ? O8 Mo2 Mo3 120.15(9) . . ? O8 Mo2 O6 85.03(11) . . ? O8 Mo2 O10 86.91(11) . . ? O8 Mo2 O11 153.12(13) . . ? O9 Mo2 Mo3 86.97(9) . . ? O9 Mo2 O6 171.01(12) . . ? O9 Mo2 O7 103.73(14) . . ? O9 Mo2 O8 103.79(14) . . ? O9 Mo2 O10 97.10(12) . . ? O9 Mo2 O11 96.74(12) . . ? O10 Mo2 Mo3 33.30(7) . . ? O10 Mo2 O6 81.44(9) . . ? O10 Mo2 O11 73.34(10) . . ? O11 Mo2 Mo3 43.24(7) . . ? O11 Mo2 O6 74.32(9) . . ? O10 Mo3 Mo2 37.62(8) . . ? O10 Mo3 O11 74.39(10) . . ? O10 Mo3 O14 143.11(11) . . ? O10 Mo3 O15 80.46(10) . . ? O11 Mo3 Mo2 40.08(6) . . ? O11 Mo3 O15 70.14(9) . . ? O12 Mo3 Mo2 90.53(9) . . ? O12 Mo3 O10 100.66(12) . . ? O12 Mo3 O11 99.43(12) . . ? O12 Mo3 O13 103.89(13) . . ? O12 Mo3 O14 95.71(12) . . ? O12 Mo3 O15 168.93(12) . . ? O13 Mo3 Mo2 145.23(9) . . ? O13 Mo3 O10 107.86(12) . . ? O13 Mo3 O11 155.58(11) . . ? O13 Mo3 O14 99.82(12) . . ? O13 Mo3 O15 86.06(11) . . ? O14 Mo3 Mo2 110.17(7) . . ? O14 Mo3 O11 70.43(9) . . ? O14 Mo3 O15 77.57(10) . . ? O15 Mo3 Mo2 83.70(6) . . ? O5 Mo4 O11 80.14(9) . . ? O6 Mo4 O5 74.86(10) . . ? O6 Mo4 O11 76.23(10) . . ? O6 Mo4 O17 140.36(12) . . ? O15 Mo4 O5 155.69(11) . . ? O15 Mo4 O6 102.67(12) . . ? O15 Mo4 O11 75.85(11) . . ? O15 Mo4 O17 98.93(11) . . ? O16 Mo4 O5 99.67(12) . . ? O16 Mo4 O6 103.96(12) . . ? O16 Mo4 O11 179.70(13) . . ? O16 Mo4 O15 104.32(13) . . ? O16 Mo4 O17 102.31(12) . . ? O17 Mo4 O5 71.87(10) . . ? O17 Mo4 O11 77.41(9) . . ? O5 Mo5 Mo8 109.66(7) . . ? O5 Mo5 O17 69.96(9) . . ? O5 Mo5 O18 77.46(10) . . ? O17 Mo5 Mo8 39.85(6) . . ? O17 Mo5 O18 71.97(9) . . ? O18 Mo5 Mo8 83.77(6) . . ? O19 Mo5 Mo8 144.42(9) . . ? O19 Mo5 O5 98.45(11) . . ? O19 Mo5 O17 152.66(11) . . ? O19 Mo5 O18 81.48(11) . . ? O19 Mo5 O21 107.96(12) . . ? O20 Mo5 Mo8 93.82(9) . . ? O20 Mo5 O5 96.43(12) . . ? O20 Mo5 O17 101.43(12) . . ? O20 Mo5 O18 172.14(12) . . ? O20 Mo5 O19 104.50(13) . . ? O20 Mo5 O21 102.33(12) . . ? O21 Mo5 Mo8 37.30(8) . . ? O21 Mo5 O5 142.24(11) . . ? O21 Mo5 O17 74.33(10) . . ? O21 Mo5 O18 80.27(10) . . ? O11 Mo6 O14 72.06(10) . . ? O18 Mo6 O11 95.91(11) . . ? O18 Mo6 O14 153.99(11) . . ? O18 Mo6 O23 103.13(12) . . ? O22 Mo6 O11 101.95(12) . . ? O22 Mo6 O14 100.12(12) . . ? O22 Mo6 O18 104.99(13) . . ? O22 Mo6 O23 105.97(12) . . ? O23 Mo6 O11 140.49(12) . . ? O23 Mo6 O14 75.92(11) . . ? O8 Mo7 O14 152.69(11) 1_455 . ? O8 Mo7 O23 85.06(10) 1_455 . ? O8 Mo7 O26 78.04(11) 1_455 . ? O14 Mo7 O23 70.27(10) . . ? O14 Mo7 O26 82.48(10) . . ? O24 Mo7 O8 96.60(14) . 1_455 ? O24 Mo7 O14 97.52(13) . . ? O24 Mo7 O23 96.24(13) . . ? O24 Mo7 O26 165.33(14) . . ? O25 Mo7 O8 100.56(14) . 1_455 ? O25 Mo7 O14 98.32(13) . . ? O25 Mo7 O23 157.51(13) . . ? O25 Mo7 O24 104.61(16) . . ? O25 Mo7 O26 89.85(13) . . ? O26 Mo7 O23 69.86(9) . . ? O4 Mo8 Mo5 118.33(8) 1_455 . ? O4 Mo8 O17 152.85(12) 1_455 . ? O4 Mo8 O21 86.00(11) 1_455 . ? O4 Mo8 O23 83.50(10) 1_455 . ? O17 Mo8 Mo5 43.48(7) . . ? O17 Mo8 O21 73.16(10) . . ? O17 Mo8 O23 76.24(9) . . ? O21 Mo8 Mo5 32.37(7) . . ? O21 Mo8 O23 80.72(10) . . ? O23 Mo8 Mo5 86.68(6) . . ? O26 Mo8 Mo5 134.81(9) . . ? O26 Mo8 O4 101.47(12) . 1_455 ? O26 Mo8 O17 91.46(11) . . ? O26 Mo8 O21 155.39(12) . . ? O26 Mo8 O23 76.94(11) . . ? O27 Mo8 Mo5 89.16(9) . . ? O27 Mo8 O4 102.11(13) . 1_455 ? O27 Mo8 O17 97.91(12) . . ? O27 Mo8 O21 97.90(13) . . ? O27 Mo8 O23 174.15(11) . . ? O27 Mo8 O26 103.27(14) . . ? O1 Co1 O1 180.0 . 2_765 ? O1 Co1 O2 92.04(11) 2_765 2_765 ? O1 Co1 O2 87.96(11) . 2_765 ? O1 Co1 O2 92.04(11) . . ? O1 Co1 O2 87.96(11) 2_765 . ? O1 Co1 O19 89.11(11) . . ? O1 Co1 O19 90.89(11) 2_765 . ? O1 Co1 O19 89.11(11) 2_765 2_765 ? O1 Co1 O19 90.89(11) . 2_765 ? O2 Co1 O2 180.0 2_765 . ? O19 Co1 O2 92.14(11) . . ? O19 Co1 O2 87.86(11) 2_765 . ? O19 Co1 O2 92.14(11) 2_765 2_765 ? O19 Co1 O2 87.86(11) . 2_765 ? O19 Co1 O19 179.998(1) . 2_765 ? Co1 O1 H1A 108.6 . . ? Co1 O1 H1B 110.2 . . ? H1A O1 H1B 108.9 . . ? Mo1 O2 Co1 146.22(14) . . ? Mo8 O4 Mo1 151.72(17) 1_655 . ? Mo1 O5 Mo4 104.63(11) . . ? Mo5 O5 Mo1 144.31(14) . . ? Mo5 O5 Mo4 109.48(11) . . ? Mo1 O6 Mo2 95.01(10) . . ? Mo4 O6 Mo1 106.00(12) . . ? Mo4 O6 Mo2 108.85(11) . . ? Mo2 O7 Mo1 115.18(14) . . ? Mo2 O8 Mo7 159.56(18) . 1_655 ? Mo3 O10 Mo2 109.08(13) . . ? Mo2 O11 Mo3 96.68(10) . . ? Mo2 O11 Mo4 100.25(9) . . ? Mo3 O11 Mo4 97.48(10) . . ? Mo6 O11 Mo2 144.47(14) . . ? Mo6 O11 Mo3 104.02(10) . . ? Mo6 O11 Mo4 105.20(10) . . ? Mo3 O14 Mo6 106.19(11) . . ? Mo7 O14 Mo3 144.54(14) . . ? Mo7 O14 Mo6 105.09(12) . . ? Mo4 O15 Mo3 116.27(13) . . ? Mo4 O17 Mo5 104.12(10) . . ? Mo4 O17 Mo8 150.05(14) . . ? Mo8 O17 Mo5 96.67(10) . . ? Mo6 O18 Mo5 115.79(13) . . ? Mo5 O19 Co1 139.37(15) . . ? Mo5 O21 Mo8 110.33(13) . . ? Mo6 O23 Mo7 104.01(12) . . ? Mo6 O23 Mo8 110.28(11) . . ? Mo7 O23 Mo8 95.20(10) . . ? Mo8 O26 Mo7 117.08(14) . . ? C10 N1 C7 125.8(4) . . ? C12 N1 C7 127.1(5) . . ? C12 N1 C10 107.0(5) . . ? C11 N2 H2 125.2 . . ? C11 N2 C12 109.5(5) . . ? C12 N2 H2 125.2 . . ? C13 N3 C8 125.9(4) . . ? C15 N3 C8 125.4(5) . . ? C15 N3 C13 108.7(4) . . ? C14 N4 H4 125.4 . . ? C15 N4 H4 125.4 . . ? C15 N4 C14 109.2(4) . . ? C17 N5 C9 127.7(4) . . ? C18 N5 C9 124.2(4) . . ? C18 N5 C17 108.1(4) . . ? C16 N6 H6 126.0 . . ? C18 N6 H6 126.0 . . ? C18 N6 C16 107.9(4) . . ? C2 C1 C7 123.1(4) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 C7 117.3(4) . . ? C1 C2 H2A 120.0 . . ? C3 C2 C1 120.0(4) . . ? C3 C2 H2A 120.0 . . ? C2 C3 C8 122.0(4) . . ? C4 C3 C2 120.0(4) . . ? C4 C3 C8 117.8(4) . . ? C3 C4 H4A 119.8 . . ? C3 C4 C5 120.4(4) . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 119.4(4) . . ? C4 C5 C9 120.2(4) . . ? C6 C5 C9 120.4(4) . . ? C1 C6 C5 120.7(4) . . ? C1 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? N1 C7 C1 115.0(3) . . ? N1 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C1 C7 H7A 108.5 . . ? C1 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? N3 C8 C3 113.7(4) . . ? N3 C8 H8A 108.8 . . ? N3 C8 H8B 108.8 . . ? C3 C8 H8A 108.8 . . ? C3 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N5 C9 C5 110.9(4) . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N1 C10 H10 125.7 . . ? C11 C10 N1 108.7(6) . . ? C11 C10 H10 125.7 . . ? N2 C11 C10 105.9(6) . . ? N2 C11 H11 127.0 . . ? C10 C11 H11 127.0 . . ? N1 C12 N2 108.8(6) . . ? N1 C12 H12 125.6 . . ? N2 C12 H12 125.6 . . ? N3 C13 H13 126.3 . . ? C14 C13 N3 107.3(5) . . ? C14 C13 H13 126.3 . . ? N4 C14 H14 126.6 . . ? C13 C14 N4 106.7(5) . . ? C13 C14 H14 126.6 . . ? N3 C15 H15 126.0 . . ? N4 C15 N3 108.0(5) . . ? N4 C15 H15 126.0 . . ? N6 C16 H16 126.2 . . ? C17 C16 N6 107.7(5) . . ? C17 C16 H16 126.2 . . ? N5 C17 H17 126.2 . . ? C16 C17 N5 107.5(5) . . ? C16 C17 H17 126.2 . . ? N5 C18 H18 125.6 . . ? N6 C18 N5 108.8(5) . . ? N6 C18 H18 125.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O28 0.85 1.83 2.672(6) 166.8 . O1 H1A O28A 0.85 2.09 2.74(2) 132.2 . O1 H1B O7 0.86 2.50 3.152(4) 133.6 . N2 H2 O10 0.86 2.25 2.900(6) 132.9 2_766 N4 H4 O13 0.86 1.98 2.824(5) 167.4 2_666 N6 H6 O2 0.86 2.18 3.031(5) 170.7 2_755 _database_code_depnum_ccdc_archive 'CCDC 938671' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nyy13050701 _audit_creation_date 2013-05-09 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H18 Mo1 N6 O4 Zn1, 3(H2 O)' _chemical_formula_sum 'C18 H24 Mo N6 O7 Zn' _chemical_formula_weight 597.74 _chemical_melting_point ? _chemical_oxdiff_formula C20H20N4O4Mo1 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' Mo Mo -1.6832 0.6857 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 147 _space_group_name_H-M_alt 'P -3' _space_group_name_Hall '-P 3' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x-y, z' 3 '-x+y, -x, z' 4 '-x, -y, -z' 5 'y, -x+y, -z' 6 'x-y, x, -z' _cell_length_a 11.8441(5) _cell_length_b 11.8441(5) _cell_length_c 9.2064(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1118.47(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1106 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 26.2090 _cell_measurement_theta_min 3.9690 _exptl_absorpt_coefficient_mu 1.686 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2458 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 2.97 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -21.00 54.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -99.0000 0.0000 75 #__ type_ start__ end____ width___ exp.time_ 2 omega 34.00 73.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -178.0000 150.0000 39 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0582784000 _diffrn_orient_matrix_UB_12 -0.0031167000 _diffrn_orient_matrix_UB_13 -0.0004740000 _diffrn_orient_matrix_UB_21 -0.0343734000 _diffrn_orient_matrix_UB_22 -0.0641009000 _diffrn_orient_matrix_UB_23 0.0285610000 _diffrn_orient_matrix_UB_31 -0.0140627000 _diffrn_orient_matrix_UB_32 -0.0255446000 _diffrn_orient_matrix_UB_33 -0.0716331000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1211 _reflns_number_total 1542 _reflns_odcompleteness_completeness 99.74 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.716 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.088 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0489 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1428 _refine_ls_wR_factor_ref 0.1576 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Mo1 \\sim O1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 3.a Riding coordinates: O3(H3A,H3B) 3.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B) 3.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C6(H6) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Mo1 Mo 0.3333 0.6667 -0.39501(8) 0.0520(3) Uani 1 3 d S . . Zn1 Zn 0.3333 0.6667 -0.00130(10) 0.0416(3) Uani 1 3 d S . . O1 O 0.3333 0.6667 -0.2095(6) 0.081(2) Uani 1 3 d S . . O2 O 0.4772(6) 0.6927(9) -0.4611(7) 0.180(4) Uani 1 1 d . . . O3 O 0.3873(6) 0.4212(5) 0.3626(6) 0.1181(19) Uani 1 1 d . . . H3A H 0.4302 0.3861 0.3933 0.177 Uiso 1 1 d R . . H3B H 0.3428 0.4239 0.4335 0.177 Uiso 1 1 d R . . N1 N 0.4997(3) 0.6800(3) 0.0640(4) 0.0410(8) Uani 1 1 d . . . N2 N 0.6722(3) 0.7226(4) 0.1893(4) 0.0468(10) Uani 1 1 d . . . C1 C 0.5863(5) 0.6678(4) -0.0256(5) 0.0492(12) Uani 1 1 d . . . H1 H 0.5735 0.6459 -0.1236 0.059 Uiso 1 1 calc R . . C2 C 0.6902(5) 0.6924(5) 0.0509(6) 0.0572(14) Uani 1 1 d . . . H2 H 0.7628 0.6897 0.0169 0.069 Uiso 1 1 calc R . . C3 C 0.5565(4) 0.7131(4) 0.1906(5) 0.0474(11) Uani 1 1 d . . . H3 H 0.5197 0.7283 0.2722 0.057 Uiso 1 1 calc R . . C4 C 0.7588(5) 0.7525(5) 0.3140(6) 0.0646(15) Uani 1 1 d . . . H4A H 0.7790 0.6831 0.3259 0.078 Uiso 1 1 calc R . . H4B H 0.7135 0.7548 0.4008 0.078 Uiso 1 1 calc R . . C5 C 0.8852(5) 0.8813(4) 0.2998(5) 0.0474(11) Uani 1 1 d . . . C6 C 1.0023(4) 0.8850(4) 0.2979(5) 0.0480(11) Uani 1 1 d . . . H6 H 1.0044 0.8076 0.2952 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0586(4) 0.0586(4) 0.0388(4) 0.000 0.000 0.02929(19) Zn1 0.0419(4) 0.0419(4) 0.0410(5) 0.000 0.000 0.02093(19) O1 0.104(4) 0.104(4) 0.037(4) 0.000 0.000 0.0519(19) O2 0.127(5) 0.341(12) 0.104(5) -0.008(6) 0.029(4) 0.140(7) O3 0.139(5) 0.110(4) 0.098(4) -0.021(3) 0.003(3) 0.057(4) N1 0.0378(18) 0.0357(18) 0.049(2) -0.0021(16) 0.0041(17) 0.0177(15) N2 0.038(2) 0.039(2) 0.057(2) 0.0091(18) -0.0016(18) 0.0144(16) C1 0.050(3) 0.045(3) 0.053(3) -0.012(2) 0.005(2) 0.024(2) C2 0.051(3) 0.050(3) 0.078(4) -0.010(3) 0.005(3) 0.031(2) C3 0.040(2) 0.046(3) 0.045(3) 0.004(2) 0.010(2) 0.014(2) C4 0.052(3) 0.054(3) 0.072(4) 0.019(3) -0.012(3) 0.015(2) C5 0.048(2) 0.043(2) 0.048(3) 0.011(2) -0.010(2) 0.020(2) C6 0.053(3) 0.045(2) 0.048(3) -0.007(2) -0.014(2) 0.026(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 Mo1 O1 1.708(6) . ? Mo1 O2 1.686(6) 3_565 ? Mo1 O2 1.686(6) 2_665 ? Mo1 O2 1.686(6) . ? Zn1 O1 1.917(6) . ? Zn1 N1 1.990(4) 2_665 ? Zn1 N1 1.990(4) 3_565 ? Zn1 N1 1.990(4) . ? O3 H3A 0.8495 . ? O3 H3B 0.8500 . ? N1 C1 1.379(6) . ? N1 C3 1.304(6) . ? N2 C2 1.368(6) . ? N2 C3 1.318(6) . ? N2 C4 1.460(6) . ? C1 H1 0.9300 . ? C1 C2 1.318(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C5 1.517(7) . ? C5 C6 1.365(6) . ? C5 C6 1.394(6) 3_675 ? C6 C5 1.394(6) 2_765 ? C6 H6 0.9300 . ? 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 O2 Mo1 O1 111.1(2) . . ? O2 Mo1 O1 111.1(2) 3_565 . ? O2 Mo1 O1 111.1(2) 2_665 . ? O2 Mo1 O2 107.8(3) 3_565 . ? O2 Mo1 O2 107.8(3) 2_665 . ? O2 Mo1 O2 107.8(3) 2_665 3_565 ? O1 Zn1 N1 107.59(11) . 2_665 ? O1 Zn1 N1 107.59(11) . 3_565 ? O1 Zn1 N1 107.59(11) . . ? N1 Zn1 N1 111.28(10) 2_665 3_565 ? N1 Zn1 N1 111.28(10) 2_665 . ? N1 Zn1 N1 111.28(10) 3_565 . ? Mo1 O1 Zn1 180.0 . . ? H3A O3 H3B 107.3 . . ? C1 N1 Zn1 124.7(3) . . ? C3 N1 Zn1 129.4(3) . . ? C3 N1 C1 105.5(4) . . ? C2 N2 C4 127.8(4) . . ? C3 N2 C2 106.1(4) . . ? C3 N2 C4 126.0(4) . . ? N1 C1 H1 125.7 . . ? C2 C1 N1 108.6(4) . . ? C2 C1 H1 125.7 . . ? N2 C2 H2 126.1 . . ? C1 C2 N2 107.8(4) . . ? C1 C2 H2 126.1 . . ? N1 C3 N2 112.0(4) . . ? N1 C3 H3 124.0 . . ? N2 C3 H3 124.0 . . ? N2 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? N2 C4 C5 113.4(4) . . ? H4A C4 H4B 107.7 . . ? C5 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C6 C5 C4 119.8(5) 3_675 . ? C6 C5 C4 120.6(4) . . ? C6 C5 C6 119.4(5) . 3_675 ? C5 C6 C5 120.5(5) . 2_765 ? C5 C6 H6 119.7 . . ? C5 C6 H6 119.7 2_765 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O2 0.85 1.87 2.716(10) 179.4 4_665 O3 H3B O2 0.85 2.52 3.268(11) 147.1 3_566 _database_code_depnum_ccdc_archive 'CCDC 938672'