# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Errington, John' _publ_contact_author_name 'Errington, John' _publ_contact_author_email John.Errington@ncl.ac.uk _publ_section_title ; Rational addition of capping groups to the phosphomolybdate Keggin anion [PMo12O40]3- by mild, non-aqueous reductive aggregation ; # Attachment '- cc.cif' data_rje411_salt_of_1 _database_code_depnum_ccdc_archive 'CCDC 857416' #TrackingRef '- cc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C16 H36 N +,C4 H6 Co Mo12 N2 O40 P 3-,C2 H3 N' _chemical_formula_sum 'C54 H117 Co Mo12 N6 O40 P' _chemical_formula_weight 2731.72 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 17.975(4) _cell_length_b 22.382(9) _cell_length_c 44.296(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17821(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 185 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10792 _exptl_absorpt_coefficient_mu 1.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.563 _exptl_absorpt_correction_T_max 0.598 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48140 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7887 _reflns_number_gt 6224 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+186.6674P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7887 _refine_ls_number_parameters 794 _refine_ls_number_restraints 1005 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.59808(2) 0.67471(2) 0.691801(9) 0.01939(11) Uani 1 1 d . . . Mo2 Mo 0.5000 0.76538(3) 0.644355(13) 0.02224(15) Uani 1 2 d S . . Mo3 Mo 0.60253(2) 0.69868(2) 0.580679(10) 0.02411(12) Uani 1 1 d . . . Mo4 Mo 0.60418(2) 0.54737(2) 0.568555(9) 0.02412(12) Uani 1 1 d . . . Mo5 Mo 0.69973(2) 0.60703(2) 0.627670(10) 0.03151(14) Uani 1 1 d . . . Mo6 Mo 0.59753(3) 0.50718(2) 0.679862(10) 0.03671(15) Uani 1 1 d . . . Mo7 Mo 0.5000 0.44852(3) 0.620230(14) 0.0379(2) Uani 1 2 d S . . Co Co 0.5000 0.57989(5) 0.72751(2) 0.0260(2) Uani 1 2 d S . . P P 0.5000 0.60695(8) 0.63073(4) 0.0136(4) Uani 1 2 d S . . O1 O 0.5000 0.4996(2) 0.70176(10) 0.0367(14) Uani 1 2 d S . . O2 O 0.58787(19) 0.58830(16) 0.69681(7) 0.0244(8) Uani 1 1 d . . . O3 O 0.5000 0.6703(2) 0.71375(9) 0.0197(10) Uani 1 2 d S . . O4 O 0.6545(3) 0.4744(2) 0.70530(8) 0.0563(14) Uani 1 1 d . . . O5 O 0.65537(19) 0.69299(18) 0.72055(8) 0.0321(9) Uani 1 1 d . . . O6 O 0.5000 0.8409(2) 0.64387(12) 0.0432(15) Uani 1 2 d S . . O7 O 0.57318(19) 0.74873(15) 0.67613(7) 0.0244(8) Uani 1 1 d . . . O8 O 0.5712(3) 0.44456(17) 0.65511(8) 0.0473(12) Uani 1 1 d . . . O9 O 0.66394(18) 0.65557(16) 0.66034(7) 0.0256(8) Uani 1 1 d . . . O10 O 0.57284(19) 0.74448(15) 0.61399(7) 0.0248(8) Uani 1 1 d . . . O11 O 0.7914(2) 0.6037(2) 0.63437(9) 0.0571(14) Uani 1 1 d . . . O12 O 0.6372(2) 0.75005(17) 0.55671(8) 0.0381(10) Uani 1 1 d . . . O13 O 0.5000 0.6931(2) 0.56895(10) 0.0252(11) Uani 1 2 d S . . O14 O 0.6636(2) 0.54103(17) 0.65254(7) 0.0355(10) Uani 1 1 d . . . O15 O 0.69185(19) 0.67255(18) 0.60078(8) 0.0327(9) Uani 1 1 d . . . O16 O 0.5000 0.3764(3) 0.60989(12) 0.067(2) Uani 1 2 d S . . O17 O 0.6377(2) 0.50726(17) 0.53944(8) 0.0350(9) Uani 1 1 d . . . O18 O 0.6905(2) 0.55465(18) 0.59344(7) 0.0342(9) Uani 1 1 d . . . O19 O 0.5733(2) 0.48226(16) 0.59679(7) 0.0314(9) Uani 1 1 d . . . O20 O 0.5000 0.5505(2) 0.56058(10) 0.0249(11) Uani 1 2 d S . . O21 O 0.61691(18) 0.62576(16) 0.55533(7) 0.0246(8) Uani 1 1 d . . . O24 O 0.5000 0.65774(19) 0.65407(9) 0.0152(10) Uani 1 2 d S . . O22 O 0.5000 0.5456(2) 0.64610(10) 0.0235(11) Uani 1 2 d S . . O23 O 0.57025(17) 0.61247(14) 0.61112(7) 0.0173(7) Uani 1 1 d . . . N5 N 0.4149(3) 0.5726(3) 0.75950(10) 0.0557(16) Uani 1 1 d DU . . C51 C 0.3521(6) 0.5618(8) 0.7695(3) 0.047(3) Uani 0.538(13) 1 d PDU A 5 C52 C 0.2784(7) 0.5576(8) 0.7849(3) 0.057(4) Uani 0.538(13) 1 d PDU A 5 H52A H 0.2499 0.5244 0.7764 0.085 Uiso 0.538(13) 1 calc PR A 5 H52B H 0.2509 0.5950 0.7820 0.085 Uiso 0.538(13) 1 calc PR A 5 H52C H 0.2862 0.5508 0.8066 0.085 Uiso 0.538(13) 1 calc PR A 5 C51A C 0.3719(8) 0.5917(8) 0.7759(3) 0.042(3) Uani 0.462(13) 1 d PDU A 6 C52A C 0.3045(7) 0.6044(8) 0.7929(3) 0.049(4) Uani 0.462(13) 1 d PDU A 6 H52D H 0.3143 0.6366 0.8073 0.073 Uiso 0.462(13) 1 calc PR A 6 H52E H 0.2888 0.5685 0.8038 0.073 Uiso 0.462(13) 1 calc PR A 6 H52F H 0.2650 0.6168 0.7790 0.073 Uiso 0.462(13) 1 calc PR A 6 N1 N 0.5362(4) 0.3307(4) 0.73622(16) 0.0315(16) Uani 0.50 1 d PDU B -1 C1 C 0.5905(6) 0.3265(5) 0.7628(2) 0.037(2) Uani 0.50 1 d PDU B -1 H1A H 0.5635 0.3101 0.7804 0.044 Uiso 0.50 1 calc PR B -1 H1B H 0.6304 0.2979 0.7575 0.044 Uiso 0.50 1 calc PR B -1 C2 C 0.6264(7) 0.3856(6) 0.7720(3) 0.047(3) Uani 0.50 1 d PDU B -1 H2A H 0.5882 0.4125 0.7806 0.056 Uiso 0.50 1 calc PR B -1 H2B H 0.6483 0.4052 0.7541 0.056 Uiso 0.50 1 calc PR B -1 C3 C 0.6873(6) 0.3738(6) 0.7955(3) 0.050(3) Uani 0.50 1 d PDU B -1 H3A H 0.7039 0.4124 0.8041 0.060 Uiso 0.50 1 calc PR B -1 H3B H 0.6660 0.3498 0.8122 0.060 Uiso 0.50 1 calc PR B -1 C4 C 0.7537(7) 0.3414(7) 0.7827(3) 0.061(4) Uani 0.50 1 d PDU B -1 H4A H 0.7902 0.3345 0.7988 0.092 Uiso 0.50 1 calc PR B -1 H4B H 0.7762 0.3656 0.7667 0.092 Uiso 0.50 1 calc PR B -1 H4C H 0.7377 0.3029 0.7744 0.092 Uiso 0.50 1 calc PR B -1 C5 C 0.5774(6) 0.3477(5) 0.7077(2) 0.032(2) Uani 0.50 1 d PDU B -1 H5A H 0.5405 0.3524 0.6912 0.039 Uiso 0.50 1 calc PR B -1 H5B H 0.6010 0.3872 0.7109 0.039 Uiso 0.50 1 calc PR B -1 C6 C 0.6366(6) 0.3044(5) 0.6973(2) 0.040(2) Uani 0.50 1 d PDU B -1 H6A H 0.6143 0.2641 0.6952 0.049 Uiso 0.50 1 calc PR B -1 H6B H 0.6762 0.3021 0.7128 0.049 Uiso 0.50 1 calc PR B -1 C7 C 0.6708(6) 0.3228(5) 0.6672(2) 0.035(2) Uani 0.50 1 d PDU B -1 H7A H 0.6318 0.3230 0.6514 0.042 Uiso 0.50 1 calc PR B -1 H7B H 0.6909 0.3639 0.6690 0.042 Uiso 0.50 1 calc PR B -1 C8 C 0.7324(6) 0.2807(6) 0.6581(3) 0.047(3) Uani 0.50 1 d PDU B -1 H8A H 0.7537 0.2937 0.6388 0.071 Uiso 0.50 1 calc PR B -1 H8B H 0.7123 0.2402 0.6559 0.071 Uiso 0.50 1 calc PR B -1 H8C H 0.7712 0.2807 0.6736 0.071 Uiso 0.50 1 calc PR B -1 C9 C 0.4770(5) 0.3775(5) 0.74238(19) 0.034(2) Uani 0.50 1 d PDU B -1 H9A H 0.4433 0.3791 0.7247 0.041 Uiso 0.50 1 calc PR B -1 H9B H 0.5017 0.4169 0.7440 0.041 Uiso 0.50 1 calc PR B -1 C10 C 0.4298(7) 0.3681(5) 0.7706(2) 0.037(2) Uani 0.50 1 d PDU B -1 H10A H 0.3940 0.3352 0.7669 0.044 Uiso 0.50 1 calc PR B -1 H10B H 0.4624 0.3560 0.7875 0.044 Uiso 0.50 1 calc PR B -1 C11 C 0.3874(7) 0.4241(6) 0.7793(3) 0.042(3) Uani 0.50 1 d PDU B -1 H11A H 0.4233 0.4567 0.7833 0.051 Uiso 0.50 1 calc PR B -1 H11B H 0.3556 0.4366 0.7621 0.051 Uiso 0.50 1 calc PR B -1 C12 C 0.3395(8) 0.4148(7) 0.8067(3) 0.057(4) Uani 0.50 1 d PDU B -1 H12A H 0.3138 0.4522 0.8116 0.085 Uiso 0.50 1 calc PR B -1 H12B H 0.3708 0.4027 0.8238 0.085 Uiso 0.50 1 calc PR B -1 H12C H 0.3028 0.3836 0.8026 0.085 Uiso 0.50 1 calc PR B -1 C13 C 0.5002(12) 0.2696(3) 0.73306(19) 0.0380(18) Uani 0.50 1 d PDU B -1 H13A H 0.5401 0.2392 0.7323 0.046 Uiso 0.50 1 calc PR B -1 H13B H 0.4704 0.2618 0.7514 0.046 Uiso 0.50 1 calc PR B -1 C14 C 0.4507(7) 0.2612(5) 0.7059(2) 0.043(2) Uani 0.50 1 d PDU B -1 H14A H 0.4112 0.2921 0.7061 0.052 Uiso 0.50 1 calc PR B -1 H14B H 0.4804 0.2668 0.6873 0.052 Uiso 0.50 1 calc PR B -1 C15 C 0.4153(8) 0.2005(5) 0.7053(3) 0.055(3) Uani 0.50 1 d PDU B -1 H15A H 0.4549 0.1698 0.7055 0.066 Uiso 0.50 1 calc PR B -1 H15B H 0.3853 0.1954 0.7239 0.066 Uiso 0.50 1 calc PR B -1 C16 C 0.3668(10) 0.1903(7) 0.6787(3) 0.078(5) Uani 0.50 1 d PDU B -1 H16A H 0.3460 0.1499 0.6796 0.117 Uiso 0.50 1 calc PR B -1 H16B H 0.3962 0.1947 0.6602 0.117 Uiso 0.50 1 calc PR B -1 H16C H 0.3263 0.2195 0.6787 0.117 Uiso 0.50 1 calc PR B -1 N2 N 0.1447(4) 0.4235(3) 0.58329(16) 0.0296(16) Uani 0.50 1 d PDU C -2 C17 C 0.1243(7) 0.4826(4) 0.5982(2) 0.038(2) Uani 0.50 1 d PDU C -2 H17A H 0.1706 0.5053 0.6019 0.046 Uiso 0.50 1 calc PR C -2 H17B H 0.0938 0.5061 0.5838 0.046 Uiso 0.50 1 calc PR C -2 C18 C 0.0817(7) 0.4776(5) 0.6278(2) 0.043(2) Uani 0.50 1 d PDU C -2 H18A H 0.0468 0.4435 0.6268 0.051 Uiso 0.50 1 calc PR C -2 H18B H 0.1171 0.4701 0.6445 0.051 Uiso 0.50 1 calc PR C -2 C19 C 0.0388(7) 0.5348(5) 0.6339(2) 0.044(3) Uani 0.50 1 d PDU C -2 H19A H 0.0733 0.5692 0.6324 0.052 Uiso 0.50 1 calc PR C -2 H19B H 0.0002 0.5397 0.6182 0.052 Uiso 0.50 1 calc PR C -2 C20 C 0.002(2) 0.5360(5) 0.6644(2) 0.059(3) Uani 0.50 1 d PDU C -2 H20A H -0.0257 0.5734 0.6667 0.089 Uiso 0.50 1 calc PR C -2 H20B H 0.0402 0.5334 0.6802 0.089 Uiso 0.50 1 calc PR C -2 H20C H -0.0321 0.5021 0.6662 0.089 Uiso 0.50 1 calc PR C -2 C21 C 0.1840(5) 0.3820(4) 0.6056(2) 0.023(2) Uani 0.50 1 d PDU C -2 H21A H 0.1489 0.3731 0.6222 0.028 Uiso 0.50 1 calc PR C -2 H21B H 0.1945 0.3439 0.5951 0.028 Uiso 0.50 1 calc PR C -2 C22 C 0.2560(6) 0.4041(5) 0.6195(3) 0.037(2) Uani 0.50 1 d PDU C -2 H22A H 0.2451 0.4353 0.6347 0.045 Uiso 0.50 1 calc PR C -2 H22B H 0.2879 0.4220 0.6037 0.045 Uiso 0.50 1 calc PR C -2 C23 C 0.2967(6) 0.3522(5) 0.6344(2) 0.042(3) Uani 0.50 1 d PDU C -2 H23A H 0.3354 0.3684 0.6481 0.050 Uiso 0.50 1 calc PR C -2 H23B H 0.2609 0.3294 0.6469 0.050 Uiso 0.50 1 calc PR C -2 C24 C 0.3327(8) 0.3103(6) 0.6125(3) 0.063(4) Uani 0.50 1 d PDU C -2 H24A H 0.3577 0.2782 0.6235 0.095 Uiso 0.50 1 calc PR C -2 H24B H 0.3692 0.3322 0.6003 0.095 Uiso 0.50 1 calc PR C -2 H24C H 0.2946 0.2932 0.5992 0.095 Uiso 0.50 1 calc PR C -2 C25 C 0.0734(5) 0.3916(4) 0.5729(2) 0.031(2) Uani 0.50 1 d PDU C -2 H25A H 0.0872 0.3510 0.5661 0.038 Uiso 0.50 1 calc PR C -2 H25B H 0.0405 0.3870 0.5907 0.038 Uiso 0.50 1 calc PR C -2 C26 C 0.0289(5) 0.4208(5) 0.5481(2) 0.034(2) Uani 0.50 1 d PDU C -2 H26A H 0.0624 0.4312 0.5311 0.041 Uiso 0.50 1 calc PR C -2 H26B H 0.0064 0.4582 0.5557 0.041 Uiso 0.50 1 calc PR C -2 C27 C -0.0323(6) 0.3791(5) 0.5369(3) 0.037(2) Uani 0.50 1 d PDU C -2 H27A H -0.0582 0.3619 0.5546 0.045 Uiso 0.50 1 calc PR C -2 H27B H -0.0691 0.4029 0.5254 0.045 Uiso 0.50 1 calc PR C -2 C28 C -0.006(2) 0.3290(4) 0.5172(2) 0.038(4) Uani 0.50 1 d PDU C -2 H28A H -0.0481 0.3043 0.5111 0.058 Uiso 0.50 1 calc PR C -2 H28B H 0.0300 0.3045 0.5285 0.058 Uiso 0.50 1 calc PR C -2 H28C H 0.0185 0.3454 0.4992 0.058 Uiso 0.50 1 calc PR C -2 C29 C 0.1939(6) 0.4378(5) 0.5564(2) 0.035(2) Uani 0.50 1 d PDU C -2 H29A H 0.1675 0.4669 0.5434 0.042 Uiso 0.50 1 calc PR C -2 H29B H 0.2396 0.4575 0.5639 0.042 Uiso 0.50 1 calc PR C -2 C30 C 0.2163(7) 0.3855(5) 0.5373(2) 0.043(3) Uani 0.50 1 d PDU C -2 H30A H 0.1753 0.3560 0.5372 0.052 Uiso 0.50 1 calc PR C -2 H30B H 0.2603 0.3661 0.5466 0.052 Uiso 0.50 1 calc PR C -2 C31 C 0.2348(15) 0.4021(8) 0.5052(3) 0.049(4) Uani 0.50 1 d PDU C -2 H31A H 0.1935 0.4260 0.4966 0.059 Uiso 0.50 1 calc PR C -2 H31B H 0.2801 0.4273 0.5050 0.059 Uiso 0.50 1 calc PR C -2 C32 C 0.2474(10) 0.3484(8) 0.4857(3) 0.077(5) Uani 0.50 1 d PDU C -2 H32A H 0.2582 0.3612 0.4650 0.116 Uiso 0.50 1 calc PR C -2 H32B H 0.2027 0.3233 0.4858 0.116 Uiso 0.50 1 calc PR C -2 H32C H 0.2896 0.3254 0.4936 0.116 Uiso 0.50 1 calc PR C -2 N3 N 0.6773(4) 0.3407(3) 0.54450(16) 0.0273(16) Uani 0.50 1 d PDU D -3 C33 C 0.6703(6) 0.2768(4) 0.5565(2) 0.028(2) Uani 0.50 1 d PDU D -3 H33A H 0.6527 0.2508 0.5399 0.034 Uiso 0.50 1 calc PR D -3 H33B H 0.7204 0.2627 0.5625 0.034 Uiso 0.50 1 calc PR D -3 C34 C 0.6184(6) 0.2692(5) 0.5831(2) 0.036(2) Uani 0.50 1 d PDU D -3 H34A H 0.6417 0.2868 0.6013 0.043 Uiso 0.50 1 calc PR D -3 H34B H 0.5716 0.2911 0.5791 0.043 Uiso 0.50 1 calc PR D -3 C35 C 0.6006(7) 0.2046(5) 0.5892(3) 0.042(3) Uani 0.50 1 d PDU D -3 H35A H 0.5724 0.1883 0.5719 0.050 Uiso 0.50 1 calc PR D -3 H35B H 0.6478 0.1819 0.5908 0.050 Uiso 0.50 1 calc PR D -3 C36 C 0.5562(7) 0.1948(6) 0.6176(3) 0.046(3) Uani 0.50 1 d PDU D -3 H36A H 0.5466 0.1521 0.6202 0.069 Uiso 0.50 1 calc PR D -3 H36B H 0.5088 0.2162 0.6160 0.069 Uiso 0.50 1 calc PR D -3 H36C H 0.5842 0.2099 0.6350 0.069 Uiso 0.50 1 calc PR D -3 C37 C 0.6021(6) 0.3638(6) 0.5348(3) 0.029(2) Uani 0.50 1 d PDU D -3 H37A H 0.6098 0.4026 0.5245 0.035 Uiso 0.50 1 calc PR D -3 H37B H 0.5726 0.3717 0.5532 0.035 Uiso 0.50 1 calc PR D -3 C38 C 0.5554(6) 0.3250(6) 0.5141(2) 0.040(2) Uani 0.50 1 d PDU D -3 H38A H 0.5462 0.2858 0.5239 0.048 Uiso 0.50 1 calc PR D -3 H38B H 0.5825 0.3178 0.4950 0.048 Uiso 0.50 1 calc PR D -3 C39 C 0.4815(5) 0.3555(7) 0.5074(2) 0.054(3) Uani 0.50 1 d PDU D -3 H39A H 0.4917 0.3962 0.4997 0.065 Uiso 0.50 1 calc PR D -3 H39B H 0.4560 0.3330 0.4911 0.065 Uiso 0.50 1 calc PR D -3 C40 C 0.4294(8) 0.3603(10) 0.5340(4) 0.067(5) Uani 0.50 1 d PDU D -3 H40A H 0.3839 0.3810 0.5277 0.100 Uiso 0.50 1 calc PR D -3 H40B H 0.4536 0.3829 0.5502 0.100 Uiso 0.50 1 calc PR D -3 H40C H 0.4169 0.3202 0.5412 0.100 Uiso 0.50 1 calc PR D -3 C41 C 0.7307(5) 0.3376(4) 0.5178(2) 0.028(2) Uani 0.50 1 d PDU D -3 H41A H 0.7759 0.3159 0.5244 0.033 Uiso 0.50 1 calc PR D -3 H41B H 0.7070 0.3133 0.5018 0.033 Uiso 0.50 1 calc PR D -3 C42 C 0.7549(11) 0.3960(6) 0.5040(3) 0.029(3) Uani 0.50 1 d PDU D -3 H42A H 0.7834 0.4193 0.5191 0.035 Uiso 0.50 1 calc PR D -3 H42B H 0.7104 0.4196 0.4983 0.035 Uiso 0.50 1 calc PR D -3 C43 C 0.8028(6) 0.3857(5) 0.4762(2) 0.031(2) Uani 0.50 1 d PDU D -3 H43A H 0.8438 0.3582 0.4817 0.037 Uiso 0.50 1 calc PR D -3 H43B H 0.7722 0.3654 0.4607 0.037 Uiso 0.50 1 calc PR D -3 C44 C 0.8357(6) 0.4409(5) 0.4625(3) 0.037(3) Uani 0.50 1 d PDU D -3 H44A H 0.8667 0.4298 0.4452 0.056 Uiso 0.50 1 calc PR D -3 H44B H 0.8663 0.4615 0.4776 0.056 Uiso 0.50 1 calc PR D -3 H44C H 0.7957 0.4675 0.4558 0.056 Uiso 0.50 1 calc PR D -3 C45 C 0.7054(5) 0.3822(5) 0.5691(2) 0.033(2) Uani 0.50 1 d PDU D -3 H45A H 0.7041 0.4235 0.5609 0.040 Uiso 0.50 1 calc PR D -3 H45B H 0.6695 0.3806 0.5860 0.040 Uiso 0.50 1 calc PR D -3 C46 C 0.7821(6) 0.3718(6) 0.5820(3) 0.053(3) Uani 0.50 1 d PDU D -3 H46A H 0.8203 0.3753 0.5660 0.064 Uiso 0.50 1 calc PR D -3 H46B H 0.7854 0.3314 0.5910 0.064 Uiso 0.50 1 calc PR D -3 C47 C 0.7937(8) 0.4196(9) 0.6060(4) 0.078(4) Uani 0.50 1 d PDU D -3 H47A H 0.7604 0.4535 0.6012 0.094 Uiso 0.50 1 calc PR D -3 H47B H 0.7771 0.4029 0.6256 0.094 Uiso 0.50 1 calc PR D -3 C48 C 0.8680(10) 0.4431(11) 0.6101(5) 0.112(6) Uani 0.50 1 d PDU D -3 H48A H 0.8673 0.4738 0.6259 0.168 Uiso 0.50 1 calc PR D -3 H48B H 0.8854 0.4607 0.5912 0.168 Uiso 0.50 1 calc PR D -3 H48C H 0.9015 0.4107 0.6161 0.168 Uiso 0.50 1 calc PR D -3 N4 N 0.4397(10) 0.0892(6) 0.5484(4) 0.095(5) Uani 0.50 1 d PDU E -4 C49 C 0.4099(10) 0.1276(7) 0.5613(4) 0.071(4) Uani 0.50 1 d PDU E -4 C50 C 0.3736(9) 0.1756(8) 0.5781(4) 0.071(4) Uani 0.50 1 d PDU E -4 H50A H 0.3269 0.1608 0.5868 0.107 Uiso 0.50 1 calc PR E -4 H50B H 0.3631 0.2090 0.5644 0.107 Uiso 0.50 1 calc PR E -4 H50C H 0.4065 0.1892 0.5943 0.107 Uiso 0.50 1 calc PR E -4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0184(2) 0.0221(2) 0.0177(2) -0.00478(18) -0.00229(17) 0.00055(18) Mo2 0.0333(4) 0.0111(3) 0.0224(3) 0.0008(3) 0.000 0.000 Mo3 0.0273(3) 0.0243(3) 0.0208(2) 0.0013(2) 0.00387(19) -0.00914(19) Mo4 0.0267(2) 0.0278(3) 0.0178(2) -0.0054(2) 0.00047(19) 0.0085(2) Mo5 0.0189(2) 0.0520(3) 0.0237(2) -0.0115(2) -0.00330(19) 0.0118(2) Mo6 0.0700(4) 0.0236(3) 0.0165(2) -0.0015(2) -0.0081(2) 0.0262(3) Mo7 0.0835(6) 0.0123(3) 0.0179(3) -0.0020(3) 0.000 0.000 Co 0.0431(6) 0.0201(6) 0.0148(4) -0.0001(4) 0.000 0.000 P 0.0176(9) 0.0111(9) 0.0122(8) -0.0001(7) 0.000 0.000 O1 0.078(4) 0.019(3) 0.013(2) 0.004(2) 0.000 0.000 O2 0.032(2) 0.024(2) 0.0166(16) -0.0018(15) -0.0050(15) 0.0086(16) O3 0.026(3) 0.018(3) 0.014(2) -0.001(2) 0.000 0.000 O4 0.099(4) 0.048(3) 0.0223(19) 0.0003(19) -0.011(2) 0.050(3) O5 0.026(2) 0.044(2) 0.0255(18) -0.0101(18) -0.0059(16) 0.0001(18) O6 0.082(5) 0.019(3) 0.028(3) 0.000(2) 0.000 0.000 O7 0.0270(19) 0.022(2) 0.0239(17) -0.0017(15) 0.0006(15) -0.0058(16) O8 0.099(3) 0.022(2) 0.0203(18) 0.0001(17) -0.006(2) 0.027(2) O9 0.0152(17) 0.036(2) 0.0255(18) -0.0065(17) -0.0008(15) -0.0002(16) O10 0.031(2) 0.0184(19) 0.0246(17) -0.0003(15) 0.0015(16) -0.0083(16) O11 0.023(2) 0.117(4) 0.031(2) -0.024(3) -0.0079(18) 0.024(2) O12 0.049(3) 0.032(2) 0.033(2) -0.0013(18) 0.0158(19) -0.0170(19) O13 0.032(3) 0.023(3) 0.021(2) 0.006(2) 0.000 0.000 O14 0.047(2) 0.041(2) 0.0189(17) -0.0058(17) -0.0061(17) 0.026(2) O15 0.0215(19) 0.051(3) 0.0257(18) -0.0067(18) 0.0039(16) -0.0093(18) O16 0.164(8) 0.015(3) 0.023(3) -0.002(3) 0.000 0.000 O17 0.040(2) 0.037(2) 0.0272(19) -0.0080(18) 0.0012(18) 0.0106(19) O18 0.026(2) 0.054(3) 0.0221(18) -0.0069(18) -0.0004(16) 0.0182(18) O19 0.052(2) 0.019(2) 0.0228(18) -0.0023(16) -0.0040(18) 0.0128(18) O20 0.029(3) 0.026(3) 0.020(2) -0.003(2) 0.000 0.000 O21 0.0228(19) 0.030(2) 0.0211(17) -0.0027(16) 0.0031(15) -0.0003(16) O24 0.020(2) 0.013(2) 0.013(2) -0.0009(19) 0.000 0.000 O22 0.039(3) 0.015(3) 0.016(2) 0.000(2) 0.000 0.000 O23 0.0145(17) 0.0189(18) 0.0184(16) -0.0014(14) 0.0009(14) 0.0023(14) N5 0.066(3) 0.078(4) 0.023(2) 0.016(3) 0.012(2) 0.040(3) C51 0.057(5) 0.068(7) 0.016(5) 0.001(5) 0.005(4) 0.030(5) C52 0.058(7) 0.082(10) 0.030(6) -0.003(6) 0.021(5) 0.010(7) C51A 0.053(6) 0.056(7) 0.018(5) -0.002(5) 0.002(5) 0.028(5) C52A 0.041(7) 0.073(9) 0.031(6) -0.009(7) 0.007(5) 0.013(7) N1 0.046(4) 0.021(4) 0.027(3) 0.009(3) -0.007(3) 0.001(3) C1 0.049(5) 0.030(5) 0.032(4) 0.008(4) -0.011(4) -0.003(4) C2 0.059(6) 0.043(6) 0.039(5) 0.002(5) -0.016(5) -0.009(5) C3 0.052(6) 0.052(7) 0.045(6) 0.004(6) -0.013(5) -0.011(5) C4 0.044(7) 0.074(10) 0.065(8) 0.001(7) -0.005(7) -0.014(6) C5 0.044(5) 0.023(5) 0.029(4) 0.008(4) -0.007(4) 0.009(4) C6 0.047(5) 0.033(5) 0.042(5) 0.004(5) -0.006(4) 0.014(4) C7 0.043(6) 0.031(6) 0.032(5) -0.001(5) -0.010(4) 0.011(5) C8 0.045(7) 0.042(7) 0.055(7) -0.008(6) -0.009(6) 0.013(6) C9 0.049(6) 0.026(4) 0.027(4) 0.007(4) -0.003(4) 0.002(4) C10 0.052(6) 0.032(6) 0.025(5) 0.010(4) 0.000(4) -0.001(5) C11 0.053(7) 0.042(6) 0.033(5) 0.007(5) 0.000(5) 0.004(5) C12 0.051(8) 0.073(10) 0.047(7) 0.007(7) 0.013(6) 0.010(7) C13 0.053(5) 0.022(4) 0.039(4) 0.005(3) -0.008(6) -0.003(6) C14 0.059(6) 0.029(5) 0.040(5) 0.006(4) -0.010(5) -0.009(5) C15 0.081(7) 0.038(6) 0.045(6) -0.003(5) 0.002(6) -0.025(6) C16 0.114(12) 0.062(10) 0.058(8) 0.004(8) -0.019(8) -0.039(9) N2 0.034(4) 0.023(4) 0.032(4) 0.003(3) 0.001(3) -0.007(3) C17 0.055(6) 0.022(5) 0.038(5) 0.005(4) 0.004(4) -0.008(4) C18 0.057(6) 0.034(5) 0.038(5) -0.003(5) 0.005(5) -0.005(5) C19 0.047(6) 0.040(6) 0.044(5) -0.009(5) 0.007(5) -0.001(5) C20 0.072(7) 0.058(7) 0.048(6) -0.010(5) 0.012(12) -0.001(16) C21 0.017(4) 0.016(4) 0.036(5) 0.002(4) -0.001(4) -0.013(4) C22 0.035(5) 0.041(5) 0.036(5) 0.003(5) -0.013(4) -0.014(4) C23 0.037(6) 0.046(6) 0.043(6) 0.008(5) -0.012(5) -0.013(5) C24 0.050(8) 0.072(9) 0.068(8) 0.002(7) -0.008(7) 0.012(7) C25 0.029(4) 0.024(5) 0.041(5) -0.001(4) -0.002(4) -0.005(4) C26 0.031(5) 0.024(5) 0.047(5) -0.001(4) -0.001(4) -0.004(4) C27 0.031(5) 0.028(5) 0.053(6) -0.005(5) -0.008(4) -0.001(4) C28 0.032(9) 0.044(5) 0.039(5) -0.002(4) -0.008(10) -0.001(10) C29 0.036(5) 0.036(5) 0.033(4) 0.005(4) 0.000(4) -0.009(4) C30 0.045(6) 0.046(6) 0.039(5) -0.004(5) 0.005(5) -0.011(5) C31 0.052(8) 0.060(8) 0.036(6) -0.004(6) 0.008(6) -0.019(7) C32 0.069(9) 0.101(11) 0.062(8) -0.035(8) 0.021(8) -0.022(9) N3 0.028(4) 0.028(4) 0.026(3) 0.000(3) 0.000(3) 0.007(3) C33 0.030(5) 0.028(4) 0.026(4) 0.002(4) 0.000(4) 0.007(4) C34 0.036(5) 0.038(5) 0.033(5) 0.007(4) 0.006(4) 0.002(4) C35 0.044(6) 0.043(6) 0.039(6) 0.009(5) 0.010(5) -0.001(5) C36 0.033(6) 0.056(8) 0.049(7) 0.011(6) 0.014(5) 0.000(6) C37 0.029(5) 0.033(5) 0.025(5) 0.008(4) 0.001(4) 0.009(5) C38 0.033(6) 0.064(7) 0.022(5) 0.006(5) -0.001(4) 0.005(5) C39 0.039(8) 0.085(8) 0.039(5) 0.017(6) -0.013(5) 0.003(6) C40 0.033(8) 0.097(12) 0.071(9) -0.017(9) -0.003(7) 0.005(9) C41 0.026(4) 0.026(5) 0.031(4) -0.002(4) 0.001(4) 0.005(4) C42 0.030(6) 0.029(6) 0.027(5) -0.002(5) 0.000(5) -0.004(5) C43 0.025(5) 0.037(6) 0.031(5) -0.001(4) 0.005(4) 0.000(4) C44 0.030(6) 0.037(7) 0.044(6) 0.004(5) 0.008(5) -0.003(5) C45 0.026(4) 0.036(5) 0.038(5) -0.013(4) 0.005(4) -0.002(4) C46 0.035(5) 0.081(7) 0.043(6) -0.023(5) 0.004(5) -0.002(5) C47 0.065(7) 0.115(9) 0.056(7) -0.041(7) -0.007(6) -0.004(7) C48 0.105(11) 0.134(15) 0.096(12) -0.062(11) 0.035(10) -0.053(11) N4 0.119(12) 0.061(9) 0.106(11) 0.028(8) 0.034(9) 0.008(8) C49 0.079(10) 0.059(9) 0.075(9) 0.030(7) 0.021(8) -0.002(7) C50 0.062(10) 0.086(11) 0.066(10) 0.014(8) 0.009(8) 0.009(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O2 1.955(4) . ? Mo1 O3 2.016(2) . ? Mo1 O5 1.688(3) . ? Mo1 O7 1.851(4) . ? Mo1 O9 1.878(3) . ? Mo1 O24 2.459(3) . ? Mo2 O6 1.689(5) . ? Mo2 O7 1.962(3) . ? Mo2 O7 1.962(3) 12_655 ? Mo2 O10 1.935(3) . ? Mo2 O10 1.935(3) 12_655 ? Mo2 O24 2.447(5) . ? Mo3 O10 1.874(3) . ? Mo3 O12 1.685(4) . ? Mo3 O13 1.9189(14) . ? Mo3 O15 1.927(4) . ? Mo3 O21 1.998(3) . ? Mo3 O23 2.424(3) . ? Mo4 O17 1.683(4) . ? Mo4 O18 1.911(4) . ? Mo4 O19 1.999(4) . ? Mo4 O20 1.9069(10) . ? Mo4 O21 1.864(4) . ? Mo4 O23 2.460(3) . ? Mo5 O9 1.921(3) . ? Mo5 O11 1.677(4) . ? Mo5 O14 1.954(4) . ? Mo5 O15 1.894(4) . ? Mo5 O18 1.924(4) . ? Mo5 O23 2.443(3) . ? Mo6 O1 2.011(2) . ? Mo6 O2 1.972(4) . ? Mo6 O4 1.690(4) . ? Mo6 O8 1.841(4) . ? Mo6 O14 1.857(4) . ? Mo6 O22 2.460(3) . ? Mo7 O8 2.009(4) . ? Mo7 O8 2.009(4) 12_655 ? Mo7 O16 1.678(6) . ? Mo7 O19 1.840(4) . ? Mo7 O19 1.840(4) 12_655 ? Mo7 O22 2.457(5) . ? Co O1 2.128(5) . ? Co O2 2.093(3) . ? Co O2 2.093(3) 12_655 ? Co O3 2.113(5) . ? Co N5 2.092(5) . ? Co N5 2.092(5) 12_655 ? P O24 1.537(5) . ? P O22 1.532(5) . ? P O23 1.538(3) . ? P O23 1.538(3) 12_655 ? O1 Mo6 2.011(2) 12_655 ? O3 Mo1 2.016(2) 12_655 ? O13 Mo3 1.9189(14) 12_655 ? O20 Mo4 1.9069(10) 12_655 ? O24 Mo1 2.459(3) 12_655 ? O22 Mo6 2.460(3) 12_655 ? N5 C51 1.236(11) . ? N5 C51A 1.141(11) . ? C51 C52 1.494(13) . ? C51A C52A 1.456(13) . ? N1 C1 1.531(9) . ? N1 C5 1.514(9) . ? N1 C9 1.518(9) . ? N1 C13 1.518(10) . ? C1 C2 1.527(12) . ? C2 C3 1.534(12) . ? C3 C4 1.507(13) . ? C5 C6 1.512(11) . ? C6 C7 1.524(11) . ? C7 C8 1.510(11) . ? C9 C10 1.524(10) . ? C10 C11 1.516(12) . ? C11 C12 1.503(12) . ? C13 C14 1.509(12) . ? C14 C15 1.500(11) . ? C15 C16 1.484(12) . ? N2 C17 1.522(10) . ? N2 C21 1.530(10) . ? N2 C25 1.536(9) . ? N2 C29 1.518(10) . ? C17 C18 1.524(11) . ? C18 C19 1.519(11) . ? C19 C20 1.502(13) . ? C21 C22 1.517(11) . ? C22 C23 1.525(11) . ? C23 C24 1.496(12) . ? C25 C26 1.509(11) . ? C26 C27 1.527(10) . ? C27 C28 1.497(13) . ? C29 C30 1.499(11) . ? C30 C31 1.509(14) . ? C31 C32 1.498(14) . ? N3 C33 1.531(9) . ? N3 C37 1.510(10) . ? N3 C41 1.525(9) . ? N3 C45 1.517(9) . ? C33 C34 1.513(10) . ? C34 C35 1.504(12) . ? C35 C36 1.504(11) . ? C37 C38 1.515(12) . ? C38 C39 1.523(11) . ? C39 C40 1.507(13) . ? C41 C42 1.508(12) . ? C42 C43 1.521(13) . ? C43 C44 1.499(11) . ? C45 C46 1.511(11) . ? C46 C47 1.524(12) . ? C47 C48 1.446(13) . ? N4 C49 1.162(14) . ? C49 C50 1.461(15) . ? C52 H52A 0.980 . ? C52 H52B 0.980 . ? C52 H52C 0.980 . ? C52A H52D 0.980 . ? C52A H52E 0.980 . ? C52A H52F 0.980 . ? C1 H1A 0.990 . ? C1 H1B 0.990 . ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.990 . ? C5 H5B 0.990 . ? C6 H6A 0.990 . ? C6 H6B 0.990 . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 H28A 0.980 . ? C28 H28B 0.980 . ? C28 H28C 0.980 . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C33 H33A 0.990 . ? C33 H33B 0.990 . ? C34 H34A 0.990 . ? C34 H34B 0.990 . ? C35 H35A 0.990 . ? C35 H35B 0.990 . ? C36 H36A 0.980 . ? C36 H36B 0.980 . ? C36 H36C 0.980 . ? C37 H37A 0.990 . ? C37 H37B 0.990 . ? C38 H38A 0.990 . ? C38 H38B 0.990 . ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? C41 H41A 0.990 . ? C41 H41B 0.990 . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C44 H44A 0.980 . ? C44 H44B 0.980 . ? C44 H44C 0.980 . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C46 H46A 0.990 . ? C46 H46B 0.990 . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C48 H48A 0.980 . ? C48 H48B 0.980 . ? C48 H48C 0.980 . ? C50 H50A 0.980 . ? C50 H50B 0.980 . ? C50 H50C 0.980 . ? 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 O3 79.30(17) . . ? O2 Mo1 O5 102.20(17) . . ? O2 Mo1 O7 154.82(14) . . ? O2 Mo1 O9 85.28(15) . . ? O2 Mo1 O24 81.78(14) . . ? O3 Mo1 O5 100.46(16) . . ? O3 Mo1 O7 90.78(17) . . ? O3 Mo1 O9 153.90(16) . . ? O3 Mo1 O24 72.13(13) . . ? O5 Mo1 O7 102.33(17) . . ? O5 Mo1 O9 103.32(16) . . ? O5 Mo1 O24 170.98(15) . . ? O7 Mo1 O9 94.49(15) . . ? O7 Mo1 O24 73.14(14) . . ? O9 Mo1 O24 84.98(12) . . ? O6 Mo2 O7 101.48(17) . . ? O6 Mo2 O7 101.47(16) . 12_655 ? O6 Mo2 O10 103.48(16) . . ? O6 Mo2 O10 103.47(16) . 12_655 ? O6 Mo2 O24 170.6(2) . . ? O7 Mo2 O7 84.20(19) . 12_655 ? O7 Mo2 O10 89.95(14) . . ? O7 Mo2 O10 155.03(15) . 12_655 ? O7 Mo2 O10 155.03(15) 12_655 . ? O7 Mo2 O10 89.95(14) 12_655 12_655 ? O7 Mo2 O24 71.75(12) . . ? O7 Mo2 O24 71.75(12) 12_655 . ? O10 Mo2 O10 85.2(2) . 12_655 ? O10 Mo2 O24 83.35(12) . . ? O10 Mo2 O24 83.36(12) 12_655 . ? O10 Mo3 O12 103.19(17) . . ? O10 Mo3 O13 88.58(18) . . ? O10 Mo3 O15 92.27(15) . . ? O10 Mo3 O21 157.83(14) . . ? O10 Mo3 O23 85.94(13) . . ? O12 Mo3 O13 103.2(2) . . ? O12 Mo3 O15 100.98(18) . . ? O12 Mo3 O21 98.95(16) . . ? O12 Mo3 O23 169.21(16) . . ? O13 Mo3 O15 154.91(18) . . ? O13 Mo3 O21 85.35(17) . . ? O13 Mo3 O23 82.47(16) . . ? O15 Mo3 O21 84.49(15) . . ? O15 Mo3 O23 72.59(13) . . ? O21 Mo3 O23 72.14(12) . . ? O17 Mo4 O18 101.33(17) . . ? O17 Mo4 O19 100.95(17) . . ? O17 Mo4 O20 103.26(19) . . ? O17 Mo4 O21 102.56(17) . . ? O17 Mo4 O23 172.82(16) . . ? O18 Mo4 O19 85.80(16) . . ? O18 Mo4 O20 154.35(17) . . ? O18 Mo4 O21 90.08(16) . . ? O18 Mo4 O23 73.07(13) . . ? O19 Mo4 O20 82.51(18) . . ? O19 Mo4 O21 156.48(14) . . ? O19 Mo4 O23 83.31(13) . . ? O20 Mo4 O21 91.61(18) . . ? O20 Mo4 O23 82.93(16) . . ? O21 Mo4 O23 73.36(12) . . ? O9 Mo5 O11 102.78(17) . . ? O9 Mo5 O14 83.76(15) . . ? O9 Mo5 O15 90.63(16) . . ? O9 Mo5 O18 155.50(15) . . ? O9 Mo5 O23 83.04(12) . . ? O11 Mo5 O14 101.1(2) . . ? O11 Mo5 O15 102.7(2) . . ? O11 Mo5 O18 101.34(18) . . ? O11 Mo5 O23 172.73(16) . . ? O14 Mo5 O15 156.18(15) . . ? O14 Mo5 O18 87.43(16) . . ? O14 Mo5 O23 83.69(13) . . ? O15 Mo5 O18 88.27(16) . . ? O15 Mo5 O23 72.63(13) . . ? O18 Mo5 O23 73.27(12) . . ? O1 Mo6 O2 79.46(18) . . ? O1 Mo6 O4 99.8(2) . . ? O1 Mo6 O8 90.0(2) . . ? O1 Mo6 O14 154.98(17) . . ? O1 Mo6 O22 72.62(14) . . ? O2 Mo6 O4 101.48(18) . . ? O2 Mo6 O8 154.80(16) . . ? O2 Mo6 O14 85.92(15) . . ? O2 Mo6 O22 81.18(14) . . ? O4 Mo6 O8 102.8(2) . . ? O4 Mo6 O14 103.0(2) . . ? O4 Mo6 O22 171.5(2) . . ? O8 Mo6 O14 94.97(18) . . ? O8 Mo6 O22 73.81(17) . . ? O14 Mo6 O22 85.22(13) . . ? O8 Mo7 O8 79.2(3) . 12_655 ? O8 Mo7 O16 99.65(18) . . ? O8 Mo7 O16 99.65(18) 12_655 . ? O8 Mo7 O19 89.75(18) . . ? O8 Mo7 O19 155.34(16) . 12_655 ? O8 Mo7 O19 89.75(18) 12_655 12_655 ? O8 Mo7 O19 155.34(16) 12_655 . ? O8 Mo7 O22 71.36(13) . . ? O8 Mo7 O22 71.35(13) 12_655 . ? O16 Mo7 O19 103.93(17) . . ? O16 Mo7 O19 103.93(17) . 12_655 ? O16 Mo7 O22 168.0(2) . . ? O19 Mo7 O19 91.5(2) . 12_655 ? O19 Mo7 O22 84.27(13) . . ? O19 Mo7 O22 84.27(13) 12_655 . ? O1 Co O2 74.19(13) . . ? O1 Co O2 74.19(13) . 12_655 ? O1 Co O3 130.82(18) . . ? O1 Co N5 107.3(2) . . ? O1 Co N5 107.3(2) . 12_655 ? O2 Co O2 98.01(18) . 12_655 ? O2 Co O3 74.13(12) . . ? O2 Co O3 74.13(12) 12_655 . ? O2 Co N5 177.8(2) . . ? O2 Co N5 83.99(17) 12_655 . ? O2 Co N5 177.81(19) 12_655 12_655 ? O2 Co N5 83.99(17) . 12_655 ? O3 Co N5 105.65(18) . . ? O3 Co N5 105.65(18) . 12_655 ? N5 Co N5 94.0(3) . 12_655 ? O24 P O22 111.3(3) . . ? O24 P O23 108.70(16) . . ? O24 P O23 108.70(16) . 12_655 ? O22 P O23 108.85(16) . . ? O22 P O23 108.85(16) . 12_655 ? O23 P O23 110.4(2) . 12_655 ? Mo6 O1 Mo6 121.4(2) . 12_655 ? Mo6 O1 Co 100.81(16) . . ? Mo6 O1 Co 100.81(16) 12_655 . ? Mo1 O2 Mo6 149.21(18) . . ? Mo1 O2 Co 103.51(15) . . ? Mo6 O2 Co 103.36(16) . . ? Mo1 O3 Mo1 122.0(2) . 12_655 ? Mo1 O3 Co 100.74(15) . . ? Mo1 O3 Co 100.74(15) 12_655 . ? Mo1 O7 Mo2 126.95(18) . . ? Mo6 O8 Mo7 126.0(2) . . ? Mo1 O9 Mo5 154.1(2) . . ? Mo2 O10 Mo3 150.74(19) . . ? Mo3 O13 Mo3 147.7(3) . 12_655 ? Mo5 O14 Mo6 152.7(2) . . ? Mo3 O15 Mo5 126.00(18) . . ? Mo4 O18 Mo5 125.19(18) . . ? Mo4 O19 Mo7 148.4(2) . . ? Mo4 O20 Mo4 158.3(3) . 12_655 ? Mo3 O21 Mo4 125.22(17) . . ? Mo1 O24 Mo1 91.62(14) . 12_655 ? Mo1 O24 Mo2 88.13(12) . . ? Mo1 O24 Mo2 88.14(12) 12_655 . ? Mo1 O24 P 124.86(14) . . ? Mo1 O24 P 124.86(14) 12_655 . ? Mo2 O24 P 127.6(2) . . ? Mo6 O22 Mo6 90.92(15) . 12_655 ? Mo6 O22 Mo7 88.52(13) . . ? Mo6 O22 Mo7 88.52(13) 12_655 . ? Mo6 O22 P 125.69(15) . . ? Mo6 O22 P 125.69(15) 12_655 . ? Mo7 O22 P 125.8(2) . . ? Mo3 O23 Mo4 89.19(10) . . ? Mo3 O23 Mo5 88.77(10) . . ? Mo3 O23 P 125.08(18) . . ? Mo4 O23 Mo5 87.95(10) . . ? Mo4 O23 P 126.08(18) . . ? Mo5 O23 P 127.51(17) . . ? Co N5 C51 157.7(8) . . ? Co N5 C51A 153.6(11) . . ? N5 C51 C52 170.2(15) . . ? N5 C51A C52A 164.9(18) . . ? C1 N1 C5 110.3(8) . . ? C1 N1 C9 110.5(7) . . ? C1 N1 C13 106.7(7) . . ? C5 N1 C9 108.6(6) . . ? C5 N1 C13 111.0(8) . . ? C9 N1 C13 109.7(10) . . ? N1 C1 C2 115.0(8) . . ? C1 C2 C3 109.6(9) . . ? C2 C3 C4 113.1(10) . . ? N1 C5 C6 115.9(8) . . ? C5 C6 C7 112.1(8) . . ? C6 C7 C8 111.1(9) . . ? N1 C9 C10 116.3(8) . . ? C9 C10 C11 111.9(8) . . ? C10 C11 C12 112.3(10) . . ? N1 C13 C14 116.0(7) . . ? C13 C14 C15 112.2(9) . . ? C14 C15 C16 113.7(10) . . ? C17 N2 C21 111.0(8) . . ? C17 N2 C25 109.4(8) . . ? C17 N2 C29 107.3(7) . . ? C21 N2 C25 107.3(7) . . ? C21 N2 C29 111.4(7) . . ? C25 N2 C29 110.5(7) . . ? N2 C17 C18 115.5(8) . . ? C17 C18 C19 110.3(9) . . ? C18 C19 C20 113.5(11) . . ? N2 C21 C22 117.3(8) . . ? C21 C22 C23 109.7(8) . . ? C22 C23 C24 113.8(10) . . ? N2 C25 C26 117.3(8) . . ? C25 C26 C27 110.7(8) . . ? C26 C27 C28 114.6(15) . . ? N2 C29 C30 115.7(8) . . ? C29 C30 C31 113.5(10) . . ? C30 C31 C32 112.2(13) . . ? C33 N3 C37 110.2(8) . . ? C33 N3 C41 106.2(6) . . ? C33 N3 C45 110.5(7) . . ? C37 N3 C41 111.0(7) . . ? C37 N3 C45 107.1(7) . . ? C41 N3 C45 112.0(7) . . ? N3 C33 C34 115.3(7) . . ? C33 C34 C35 112.3(8) . . ? C34 C35 C36 113.7(10) . . ? N3 C37 C38 118.2(9) . . ? C37 C38 C39 110.1(10) . . ? C38 C39 C40 114.9(10) . . ? N3 C41 C42 117.1(9) . . ? C41 C42 C43 111.0(11) . . ? C42 C43 C44 115.2(9) . . ? N3 C45 C46 118.7(8) . . ? C45 C46 C47 106.3(10) . . ? C46 C47 C48 118.0(13) . . ? N4 C49 C50 179(2) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51A C52A H52D 109.5 . . ? C51A C52A H52E 109.5 . . ? C51A C52A H52F 109.5 . . ? H52D C52A H52E 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? N1 C1 H1A 108.5 . . ? N1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? H1A C1 C2 108.5 . . ? H1B C1 C2 108.5 . . ? C1 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? H2A C2 C3 109.8 . . ? H2B C2 C3 109.8 . . ? C2 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? H3A C3 C4 109.0 . . ? H3B C3 C4 109.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 108.3 . . ? N1 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? H5A C5 C6 108.3 . . ? H5B C5 C6 108.3 . . ? C5 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? H6A C6 C7 109.2 . . ? H6B C6 C7 109.2 . . ? C6 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? H7A C7 C8 109.4 . . ? H7B C7 C8 109.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 108.2 . . ? N1 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? H9A C9 C10 108.2 . . ? H9B C9 C10 108.2 . . ? C9 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? H10A C10 C11 109.2 . . ? H10B C10 C11 109.2 . . ? C10 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? H11A C11 C12 109.1 . . ? H11B C11 C12 109.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 H13A 108.3 . . ? N1 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? H13A C13 C14 108.3 . . ? H13B C13 C14 108.3 . . ? C13 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? H14A C14 C15 109.2 . . ? H14B C14 C15 109.2 . . ? C14 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? H15A C15 C16 108.8 . . ? H15B C15 C16 108.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 108.4 . . ? N2 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? H17A C17 C18 108.4 . . ? H17B C17 C18 108.4 . . ? C17 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? H18A C18 C19 109.6 . . ? H18B C18 C19 109.6 . . ? C18 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? H19A C19 C20 108.9 . . ? H19B C19 C20 108.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 H21A 108.0 . . ? N2 C21 H21B 108.0 . . ? H21A C21 H21B 107.2 . . ? H21A C21 C22 108.0 . . ? H21B C21 C22 108.0 . . ? C21 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? H22A C22 C23 109.7 . . ? H22B C22 C23 109.7 . . ? C22 C23 H23A 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? H23A C23 C24 108.8 . . ? H23B C23 C24 108.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 H25A 108.0 . . ? N2 C25 H25B 108.0 . . ? H25A C25 H25B 107.2 . . ? H25A C25 C26 108.0 . . ? H25B C25 C26 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? H26A C26 C27 109.5 . . ? H26B C26 C27 109.5 . . ? C26 C27 H27A 108.6 . . ? C26 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? H27A C27 C28 108.6 . . ? H27B C27 C28 108.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 H29A 108.3 . . ? N2 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? H29A C29 C30 108.3 . . ? H29B C29 C30 108.3 . . ? C29 C30 H30A 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? H30A C30 C31 108.9 . . ? H30B C30 C31 108.9 . . ? C30 C31 H31A 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? H31A C31 C32 109.2 . . ? H31B C31 C32 109.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 H33A 108.4 . . ? N3 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? H33A C33 C34 108.4 . . ? H33B C33 C34 108.4 . . ? C33 C34 H34A 109.1 . . ? C33 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? H34A C34 C35 109.1 . . ? H34B C34 C35 109.1 . . ? C34 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? H35A C35 C36 108.8 . . ? H35B C35 C36 108.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 H37A 107.8 . . ? N3 C37 H37B 107.8 . . ? H37A C37 H37B 107.1 . . ? H37A C37 C38 107.8 . . ? H37B C37 C38 107.8 . . ? C37 C38 H38A 109.6 . . ? C37 C38 H38B 109.6 . . ? H38A C38 H38B 108.1 . . ? H38A C38 C39 109.6 . . ? H38B C38 C39 109.6 . . ? C38 C39 H39A 108.5 . . ? C38 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? H39A C39 C40 108.5 . . ? H39B C39 C40 108.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 H41A 108.0 . . ? N3 C41 H41B 108.0 . . ? H41A C41 H41B 107.3 . . ? H41A C41 C42 108.0 . . ? H41B C41 C42 108.0 . . ? C41 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? H42A C42 C43 109.4 . . ? H42B C42 C43 109.4 . . ? C42 C43 H43A 108.5 . . ? C42 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? H43A C43 C44 108.5 . . ? H43B C43 C44 108.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 H45A 107.6 . . ? N3 C45 H45B 107.6 . . ? H45A C45 H45B 107.1 . . ? H45A C45 C46 107.6 . . ? H45B C45 C46 107.6 . . ? C45 C46 H46A 110.5 . . ? C45 C46 H46B 110.5 . . ? H46A C46 H46B 108.7 . . ? H46A C46 C47 110.5 . . ? H46B C46 C47 110.5 . . ? C46 C47 H47A 107.8 . . ? C46 C47 H47B 107.8 . . ? H47A C47 H47B 107.1 . . ? H47A C47 C48 107.8 . . ? H47B C47 C48 107.8 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.903 _refine_diff_density_min -1.535 _refine_diff_density_rms 0.127 # Contents of RES file _computing_special_details ; TITL rje411 in Cmca CELL 0.71073 17.975 22.382 44.296 90.000 90.000 90.000 ZERR 8.00 0.004 0.009 0.016 0.000 0.000 0.000 LATT 7 SYMM -X, 0.5-Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM X, -Y, -Z SFAC C H O P MO N Co UNIT 432 936 320 8 96 48 8 REM blue block SIZE 0.34 0.30 0.30 TEMP -123 OMIT -3 50 OMIT 4 2 1 OMIT 1 3 36 OMIT 5 25 3 L.S. 8 ACTA BOND FMAP 2 PLAN 10 SIMU 0.01 $C $N DELU 0.01 $C $N REM EXTI 0.000010 WGHT 0.000000 186.667404 FVAR 0.02151 0.53848 MO1 5 0.598082 0.674713 0.691801 11.00000 0.01841 0.02212 = 0.01765 -0.00478 -0.00229 0.00055 MO2 5 0.500000 0.765379 0.644355 10.50000 0.03328 0.01108 = 0.02237 0.00082 0.00000 0.00000 MO3 5 0.602531 0.698681 0.580679 11.00000 0.02728 0.02427 = 0.02079 0.00135 0.00387 -0.00914 MO4 5 0.604183 0.547369 0.568555 11.00000 0.02674 0.02780 = 0.01783 -0.00537 0.00047 0.00847 MO5 5 0.699729 0.607030 0.627670 11.00000 0.01887 0.05198 = 0.02367 -0.01155 -0.00330 0.01179 MO6 5 0.597534 0.507185 0.679862 11.00000 0.07004 0.02359 = 0.01650 -0.00151 -0.00809 0.02620 MO7 5 0.500000 0.448517 0.620230 10.50000 0.08346 0.01233 = 0.01786 -0.00205 0.00000 0.00000 CO 7 0.500000 0.579889 0.727510 10.50000 0.04306 0.02015 = 0.01481 -0.00006 0.00000 0.00000 P 4 0.500000 0.606946 0.630730 10.50000 0.01762 0.01105 = 0.01218 -0.00008 0.00000 0.00000 O1 3 0.500000 0.499625 0.701761 10.50000 0.07812 0.01892 = 0.01302 0.00429 0.00000 0.00000 O2 3 0.587868 0.588298 0.696810 11.00000 0.03215 0.02442 = 0.01657 -0.00183 -0.00500 0.00864 O3 3 0.500000 0.670274 0.713753 10.50000 0.02615 0.01849 = 0.01446 -0.00119 0.00000 0.00000 O4 3 0.654464 0.474413 0.705302 11.00000 0.09895 0.04767 = 0.02227 0.00035 -0.01143 0.04962 O5 3 0.655374 0.692990 0.720551 11.00000 0.02643 0.04424 = 0.02551 -0.01012 -0.00588 0.00005 O6 3 0.500000 0.840857 0.643875 10.50000 0.08218 0.01941 = 0.02795 -0.00044 0.00000 0.00000 O7 3 0.573183 0.748728 0.676127 11.00000 0.02700 0.02237 = 0.02390 -0.00170 0.00056 -0.00583 O8 3 0.571240 0.444557 0.655108 11.00000 0.09930 0.02232 = 0.02033 0.00012 -0.00598 0.02678 O9 3 0.663945 0.655568 0.660345 11.00000 0.01518 0.03617 = 0.02548 -0.00654 -0.00082 -0.00016 O10 3 0.572837 0.744479 0.613986 11.00000 0.03129 0.01842 = 0.02464 -0.00027 0.00148 -0.00830 O11 3 0.791450 0.603676 0.634374 11.00000 0.02345 0.11661 = 0.03131 -0.02353 -0.00787 0.02426 O12 3 0.637185 0.750052 0.556707 11.00000 0.04942 0.03190 = 0.03300 -0.00130 0.01581 -0.01700 O13 3 0.500000 0.693098 0.568950 10.50000 0.03158 0.02293 = 0.02103 0.00647 0.00000 0.00000 O14 3 0.663584 0.541035 0.652540 11.00000 0.04664 0.04105 = 0.01885 -0.00581 -0.00607 0.02576 O15 3 0.691848 0.672547 0.600782 11.00000 0.02153 0.05078 = 0.02569 -0.00668 0.00385 -0.00927 O16 3 0.500000 0.376384 0.609886 10.50000 0.16373 0.01493 = 0.02340 -0.00240 0.00000 0.00000 O17 3 0.637733 0.507257 0.539442 11.00000 0.04044 0.03729 = 0.02715 -0.00803 0.00115 0.01058 O18 3 0.690544 0.554645 0.593440 11.00000 0.02631 0.05404 = 0.02213 -0.00690 -0.00036 0.01818 O19 3 0.573297 0.482258 0.596788 11.00000 0.05242 0.01896 = 0.02278 -0.00230 -0.00403 0.01280 O20 3 0.500000 0.550467 0.560585 10.50000 0.02863 0.02647 = 0.01967 -0.00315 0.00000 0.00000 O21 3 0.616908 0.625757 0.555335 11.00000 0.02285 0.02981 = 0.02110 -0.00268 0.00314 -0.00027 O24 3 0.500000 0.657739 0.654073 10.50000 0.02002 0.01297 = 0.01273 -0.00093 0.00000 0.00000 O22 3 0.500000 0.545617 0.646099 10.50000 0.03934 0.01530 = 0.01572 -0.00039 0.00000 0.00000 O23 3 0.570255 0.612475 0.611121 11.00000 0.01447 0.01894 = 0.01842 -0.00141 0.00092 0.00229 SAME N5 C51A C52A SAME N4 C49 C50 N5 6 0.414896 0.572635 0.759502 11.00000 0.06551 0.07849 = 0.02323 0.01605 0.01164 0.04048 PART 5 C51 1 0.352059 0.561826 0.769455 21.00000 0.05707 0.06826 = 0.01603 0.00108 0.00476 0.03004 C52 1 0.278437 0.557638 0.784941 21.00000 0.05797 0.08218 = 0.03009 -0.00322 0.02102 0.01017 AFIX 33 H52A 2 0.249942 0.524363 0.776393 21.00000 -1.50000 H52B 2 0.250905 0.594987 0.782022 21.00000 -1.50000 H52C 2 0.286156 0.550818 0.806569 21.00000 -1.50000 AFIX 0 PART 6 C51A 1 0.371945 0.591654 0.775857 -21.00000 0.05303 0.05589 = 0.01785 -0.00165 0.00182 0.02827 C52A 1 0.304494 0.604430 0.792871 -21.00000 0.04144 0.07318 = 0.03141 -0.00940 0.00670 0.01279 AFIX 33 H52D 2 0.314266 0.636642 0.807323 -21.00000 -1.50000 H52E 2 0.288829 0.568480 0.803784 -21.00000 -1.50000 H52F 2 0.264983 0.616769 0.778960 -21.00000 -1.50000 AFIX 0 SAME N2 > C32 SAME N3 > C48 SAME N1 C5 > C16 C1 > C4 SAME N1 C13 > C16 C9 > C12 C5 > C8 C1 > C4 PART -1 N1 6 0.536238 0.330678 0.736223 10.50000 0.04642 0.02134 = 0.02666 0.00875 -0.00690 0.00075 C1 1 0.590468 0.326508 0.762781 10.50000 0.04914 0.02992 = 0.03188 0.00803 -0.01125 -0.00327 AFIX 23 H1A 2 0.563538 0.310051 0.780415 10.50000 -1.20000 H1B 2 0.630353 0.297880 0.757461 10.50000 -1.20000 AFIX 0 C2 1 0.626390 0.385551 0.772006 10.50000 0.05858 0.04272 = 0.03879 0.00222 -0.01571 -0.00943 AFIX 23 H2A 2 0.588234 0.412539 0.780598 10.50000 -1.20000 H2B 2 0.648281 0.405213 0.754065 10.50000 -1.20000 AFIX 0 C3 1 0.687272 0.373774 0.795525 10.50000 0.05167 0.05225 = 0.04542 0.00389 -0.01297 -0.01130 AFIX 23 H3A 2 0.703903 0.412403 0.804069 10.50000 -1.20000 H3B 2 0.666039 0.349767 0.812202 10.50000 -1.20000 AFIX 0 C4 1 0.753666 0.341371 0.782713 10.50000 0.04407 0.07407 = 0.06493 0.00072 -0.00471 -0.01374 AFIX 33 H4A 2 0.790249 0.334544 0.798751 10.50000 -1.50000 H4B 2 0.776195 0.365592 0.766710 10.50000 -1.50000 H4C 2 0.737718 0.302911 0.774351 10.50000 -1.50000 AFIX 0 C5 1 0.577370 0.347730 0.707681 10.50000 0.04384 0.02332 = 0.02949 0.00811 -0.00713 0.00896 AFIX 23 H5A 2 0.540520 0.352381 0.691237 10.50000 -1.20000 H5B 2 0.601006 0.387172 0.710897 10.50000 -1.20000 AFIX 0 C6 1 0.636563 0.304360 0.697287 10.50000 0.04662 0.03254 = 0.04224 0.00409 -0.00577 0.01359 AFIX 23 H6A 2 0.614342 0.264098 0.695209 10.50000 -1.20000 H6B 2 0.676187 0.302058 0.712767 10.50000 -1.20000 AFIX 0 C7 1 0.670790 0.322838 0.667235 10.50000 0.04305 0.03108 = 0.03160 -0.00079 -0.01005 0.01089 AFIX 23 H7A 2 0.631802 0.323014 0.651449 10.50000 -1.20000 H7B 2 0.690926 0.363868 0.668951 10.50000 -1.20000 AFIX 0 C8 1 0.732390 0.280659 0.658105 10.50000 0.04461 0.04186 = 0.05540 -0.00844 -0.00928 0.01308 AFIX 33 H8A 2 0.753664 0.293692 0.638829 10.50000 -1.50000 H8B 2 0.712260 0.240196 0.655926 10.50000 -1.50000 H8C 2 0.771219 0.280717 0.673636 10.50000 -1.50000 AFIX 0 C9 1 0.476970 0.377451 0.742385 10.50000 0.04931 0.02573 = 0.02699 0.00668 -0.00344 0.00200 AFIX 23 H9A 2 0.443318 0.379121 0.724712 10.50000 -1.20000 H9B 2 0.501674 0.416851 0.744022 10.50000 -1.20000 AFIX 0 C10 1 0.429753 0.368066 0.770564 10.50000 0.05241 0.03200 = 0.02520 0.01046 -0.00016 -0.00062 AFIX 23 H10A 2 0.393969 0.335240 0.766883 10.50000 -1.20000 H10B 2 0.462354 0.356028 0.787520 10.50000 -1.20000 AFIX 0 C11 1 0.387410 0.424073 0.779265 10.50000 0.05253 0.04225 = 0.03258 0.00728 0.00042 0.00370 AFIX 23 H11A 2 0.423295 0.456658 0.783312 10.50000 -1.20000 H11B 2 0.355632 0.436552 0.762135 10.50000 -1.20000 AFIX 0 C12 1 0.339533 0.414836 0.806694 10.50000 0.05066 0.07290 = 0.04736 0.00666 0.01282 0.00957 AFIX 33 H12A 2 0.313830 0.452188 0.811642 10.50000 -1.50000 H12B 2 0.370786 0.402742 0.823761 10.50000 -1.50000 H12C 2 0.302768 0.383555 0.802561 10.50000 -1.50000 AFIX 0 C13 1 0.500199 0.269640 0.733058 10.50000 0.05306 0.02190 = 0.03917 0.00525 -0.00753 -0.00330 AFIX 23 H13A 2 0.540087 0.239177 0.732286 10.50000 -1.20000 H13B 2 0.470374 0.261835 0.751428 10.50000 -1.20000 AFIX 0 C14 1 0.450662 0.261217 0.705896 10.50000 0.05919 0.02945 = 0.04029 0.00645 -0.00970 -0.00886 AFIX 23 H14A 2 0.411223 0.292089 0.706090 10.50000 -1.20000 H14B 2 0.480449 0.266754 0.687306 10.50000 -1.20000 AFIX 0 C15 1 0.415273 0.200529 0.705318 10.50000 0.08140 0.03796 = 0.04513 -0.00312 0.00217 -0.02480 AFIX 23 H15A 2 0.454944 0.169848 0.705511 10.50000 -1.20000 H15B 2 0.385296 0.195357 0.723884 10.50000 -1.20000 AFIX 0 C16 1 0.366803 0.190277 0.678695 10.50000 0.11403 0.06193 = 0.05841 0.00432 -0.01894 -0.03940 AFIX 33 H16A 2 0.345987 0.149851 0.679630 10.50000 -1.50000 H16B 2 0.396156 0.194661 0.660183 10.50000 -1.50000 H16C 2 0.326258 0.219550 0.678692 10.50000 -1.50000 AFIX 0 PART -2 N2 6 0.144658 0.423503 0.583287 10.50000 0.03355 0.02288 = 0.03228 0.00317 0.00092 -0.00669 C17 1 0.124276 0.482603 0.598152 10.50000 0.05476 0.02203 = 0.03805 0.00543 0.00426 -0.00844 AFIX 23 H17A 2 0.170635 0.505313 0.601885 10.50000 -1.20000 H17B 2 0.093849 0.506068 0.583782 10.50000 -1.20000 AFIX 0 C18 1 0.081730 0.477625 0.627814 10.50000 0.05651 0.03386 = 0.03762 -0.00257 0.00498 -0.00455 AFIX 23 H18A 2 0.046757 0.443516 0.626785 10.50000 -1.20000 H18B 2 0.117069 0.470121 0.644532 10.50000 -1.20000 AFIX 0 C19 1 0.038775 0.534822 0.633947 10.50000 0.04670 0.04025 = 0.04407 -0.00876 0.00719 -0.00140 AFIX 23 H19A 2 0.073273 0.569163 0.632387 10.50000 -1.20000 H19B 2 0.000162 0.539707 0.618202 10.50000 -1.20000 AFIX 0 C20 1 0.002114 0.536044 0.664413 10.50000 0.07181 0.05799 = 0.04810 -0.00997 0.01250 -0.00058 AFIX 33 H20A 2 -0.025667 0.573437 0.666733 10.50000 -1.50000 H20B 2 0.040183 0.533361 0.680192 10.50000 -1.50000 H20C 2 -0.032093 0.502131 0.666190 10.50000 -1.50000 AFIX 0 C21 1 0.183985 0.382019 0.605616 10.50000 0.01729 0.01623 = 0.03569 0.00243 -0.00117 -0.01300 AFIX 23 H21A 2 0.148873 0.373093 0.622234 10.50000 -1.20000 H21B 2 0.194504 0.343872 0.595140 10.50000 -1.20000 AFIX 0 C22 1 0.256016 0.404139 0.619501 10.50000 0.03490 0.04123 = 0.03615 0.00255 -0.01337 -0.01364 AFIX 23 H22A 2 0.245133 0.435333 0.634719 10.50000 -1.20000 H22B 2 0.287855 0.421990 0.603651 10.50000 -1.20000 AFIX 0 C23 1 0.296730 0.352177 0.634418 10.50000 0.03694 0.04574 = 0.04255 0.00834 -0.01180 -0.01253 AFIX 23 H23A 2 0.335424 0.368372 0.648056 10.50000 -1.20000 H23B 2 0.260915 0.329444 0.646921 10.50000 -1.20000 AFIX 0 C24 1 0.332655 0.310333 0.612474 10.50000 0.04987 0.07155 = 0.06798 0.00174 -0.00802 0.01222 AFIX 33 H24A 2 0.357690 0.278173 0.623528 10.50000 -1.50000 H24B 2 0.369196 0.332198 0.600328 10.50000 -1.50000 H24C 2 0.294607 0.293224 0.599194 10.50000 -1.50000 AFIX 0 C25 1 0.073404 0.391628 0.572915 10.50000 0.02872 0.02410 = 0.04094 -0.00090 -0.00180 -0.00506 AFIX 23 H25A 2 0.087218 0.350983 0.566110 10.50000 -1.20000 H25B 2 0.040499 0.387023 0.590686 10.50000 -1.20000 AFIX 0 C26 1 0.028947 0.420821 0.548068 10.50000 0.03144 0.02406 = 0.04671 -0.00089 -0.00122 -0.00433 AFIX 23 H26A 2 0.062383 0.431171 0.531096 10.50000 -1.20000 H26B 2 0.006402 0.458238 0.555708 10.50000 -1.20000 AFIX 0 C27 1 -0.032287 0.379084 0.536852 10.50000 0.03139 0.02842 = 0.05255 -0.00523 -0.00805 -0.00122 AFIX 23 H27A 2 -0.058171 0.361869 0.554559 10.50000 -1.20000 H27B 2 -0.069099 0.402912 0.525389 10.50000 -1.20000 AFIX 0 C28 1 -0.005639 0.329001 0.517217 10.50000 0.03225 0.04375 = 0.03932 -0.00233 -0.00774 -0.00056 AFIX 33 H28A 2 -0.048072 0.304291 0.511128 10.50000 -1.50000 H28B 2 0.030048 0.304489 0.528458 10.50000 -1.50000 H28C 2 0.018548 0.345448 0.499215 10.50000 -1.50000 AFIX 0 C29 1 0.193941 0.437794 0.556399 10.50000 0.03557 0.03607 = 0.03328 0.00468 -0.00030 -0.00912 AFIX 23 H29A 2 0.167544 0.466888 0.543413 10.50000 -1.20000 H29B 2 0.239642 0.457514 0.563901 10.50000 -1.20000 AFIX 0 C30 1 0.216325 0.385499 0.537320 10.50000 0.04453 0.04636 = 0.03893 -0.00365 0.00538 -0.01067 AFIX 23 H30A 2 0.175270 0.356015 0.537203 10.50000 -1.20000 H30B 2 0.260254 0.366091 0.546570 10.50000 -1.20000 AFIX 0 C31 1 0.234796 0.402128 0.505158 10.50000 0.05208 0.05978 = 0.03650 -0.00430 0.00790 -0.01903 AFIX 23 H31A 2 0.193483 0.426027 0.496635 10.50000 -1.20000 H31B 2 0.280099 0.427281 0.504992 10.50000 -1.20000 AFIX 0 C32 1 0.247410 0.348362 0.485689 10.50000 0.06904 0.10106 = 0.06160 -0.03475 0.02084 -0.02154 AFIX 33 H32A 2 0.258242 0.361183 0.464997 10.50000 -1.50000 H32B 2 0.202678 0.323330 0.485758 10.50000 -1.50000 H32C 2 0.289563 0.325392 0.493574 10.50000 -1.50000 AFIX 0 PART -3 N3 6 0.677274 0.340712 0.544504 10.50000 0.02762 0.02801 = 0.02642 0.00015 -0.00011 0.00716 C33 1 0.670278 0.276823 0.556529 10.50000 0.03045 0.02822 = 0.02575 0.00246 0.00013 0.00661 AFIX 23 H33A 2 0.652730 0.250825 0.539909 10.50000 -1.20000 H33B 2 0.720359 0.262698 0.562492 10.50000 -1.20000 AFIX 0 C34 1 0.618403 0.269153 0.583140 10.50000 0.03626 0.03797 = 0.03308 0.00676 0.00629 0.00196 AFIX 23 H34A 2 0.641682 0.286836 0.601318 10.50000 -1.20000 H34B 2 0.571601 0.291081 0.579134 10.50000 -1.20000 AFIX 0 C35 1 0.600622 0.204589 0.589235 10.50000 0.04374 0.04316 = 0.03909 0.00864 0.00991 -0.00097 AFIX 23 H35A 2 0.572416 0.188327 0.571886 10.50000 -1.20000 H35B 2 0.647768 0.181930 0.590783 10.50000 -1.20000 AFIX 0 C36 1 0.556186 0.194849 0.617571 10.50000 0.03304 0.05621 = 0.04903 0.01088 0.01433 -0.00012 AFIX 33 H36A 2 0.546644 0.152051 0.620185 10.50000 -1.50000 H36B 2 0.508761 0.216233 0.616036 10.50000 -1.50000 H36C 2 0.584192 0.209914 0.634960 10.50000 -1.50000 AFIX 0 C37 1 0.602076 0.363755 0.534773 10.50000 0.02868 0.03255 = 0.02512 0.00804 0.00128 0.00941 AFIX 23 H37A 2 0.609805 0.402596 0.524550 10.50000 -1.20000 H37B 2 0.572607 0.371726 0.553219 10.50000 -1.20000 AFIX 0 C38 1 0.555366 0.324957 0.514127 10.50000 0.03285 0.06422 = 0.02241 0.00599 -0.00075 0.00473 AFIX 23 H38A 2 0.546173 0.285847 0.523878 10.50000 -1.20000 H38B 2 0.582515 0.317767 0.495023 10.50000 -1.20000 AFIX 0 C39 1 0.481468 0.355456 0.507414 10.50000 0.03924 0.08508 = 0.03909 0.01703 -0.01283 0.00297 AFIX 23 H39A 2 0.491695 0.396153 0.499705 10.50000 -1.20000 H39B 2 0.456024 0.333034 0.491149 10.50000 -1.20000 AFIX 0 C40 1 0.429421 0.360334 0.533958 10.50000 0.03272 0.09657 = 0.07063 -0.01720 -0.00333 0.00487 AFIX 33 H40A 2 0.383901 0.381050 0.527737 10.50000 -1.50000 H40B 2 0.453650 0.382893 0.550171 10.50000 -1.50000 H40C 2 0.416857 0.320233 0.541232 10.50000 -1.50000 AFIX 0 C41 1 0.730713 0.337579 0.517808 10.50000 0.02608 0.02620 = 0.03095 -0.00201 0.00123 0.00508 AFIX 23 H41A 2 0.775859 0.315884 0.524420 10.50000 -1.20000 H41B 2 0.706967 0.313341 0.501788 10.50000 -1.20000 AFIX 0 C42 1 0.754866 0.396044 0.504025 10.50000 0.03039 0.02946 = 0.02662 -0.00208 -0.00016 -0.00356 AFIX 23 H42A 2 0.783422 0.419309 0.519093 10.50000 -1.20000 H42B 2 0.710405 0.419608 0.498348 10.50000 -1.20000 AFIX 0 C43 1 0.802782 0.385668 0.476216 10.50000 0.02476 0.03713 = 0.03062 -0.00085 0.00453 0.00010 AFIX 23 H43A 2 0.843803 0.358240 0.481725 10.50000 -1.20000 H43B 2 0.772167 0.365387 0.460719 10.50000 -1.20000 AFIX 0 C44 1 0.835736 0.440892 0.462508 10.50000 0.03020 0.03726 = 0.04369 0.00387 0.00761 -0.00325 AFIX 33 H44A 2 0.866709 0.429826 0.445180 10.50000 -1.50000 H44B 2 0.866343 0.461467 0.477578 10.50000 -1.50000 H44C 2 0.795698 0.467484 0.455803 10.50000 -1.50000 AFIX 0 C45 1 0.705393 0.382248 0.569056 10.50000 0.02558 0.03623 = 0.03795 -0.01301 0.00474 -0.00218 AFIX 23 H45A 2 0.704123 0.423452 0.560945 10.50000 -1.20000 H45B 2 0.669454 0.380647 0.585972 10.50000 -1.20000 AFIX 0 C46 1 0.782063 0.371788 0.581977 10.50000 0.03535 0.08122 = 0.04323 -0.02308 0.00447 -0.00249 AFIX 23 H46A 2 0.820278 0.375284 0.565980 10.50000 -1.20000 H46B 2 0.785378 0.331422 0.591015 10.50000 -1.20000 AFIX 0 C47 1 0.793704 0.419589 0.606031 10.50000 0.06457 0.11488 = 0.05557 -0.04079 -0.00728 -0.00429 AFIX 23 H47A 2 0.760424 0.453533 0.601239 10.50000 -1.20000 H47B 2 0.777077 0.402903 0.625599 10.50000 -1.20000 AFIX 0 C48 1 0.867973 0.443078 0.610135 10.50000 0.10516 0.13372 = 0.09618 -0.06217 0.03474 -0.05309 AFIX 33 H48A 2 0.867313 0.473784 0.625905 10.50000 -1.50000 H48B 2 0.885394 0.460690 0.591153 10.50000 -1.50000 H48C 2 0.901539 0.410677 0.616127 10.50000 -1.50000 AFIX 0 PART -4 N4 6 0.439695 0.089196 0.548404 10.50000 0.11862 0.06098 = 0.10590 0.02764 0.03399 0.00841 C49 1 0.409856 0.127563 0.561286 10.50000 0.07890 0.05939 = 0.07458 0.03006 0.02136 -0.00212 C50 1 0.373621 0.175595 0.578094 10.50000 0.06226 0.08596 = 0.06592 0.01378 0.00883 0.00859 AFIX 33 H50A 2 0.326948 0.160837 0.586763 10.50000 -1.50000 H50B 2 0.363079 0.209003 0.564448 10.50000 -1.50000 H50C 2 0.406529 0.189165 0.594346 10.50000 -1.50000 PART 0 HKLF 4 REM rje411 in Cmca REM R1 = 0.0409 for 6224 Fo > 4sig(Fo) and 0.0607 for all 7887 data REM 794 parameters refined using 1005 restraints END ; #===END data_rje422_salt_of_2 _database_code_depnum_ccdc_archive 'CCDC 857417' #TrackingRef '- cc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C16 H36 N +,Mo12 V2 P O42 3-,C2 H3 N' _chemical_formula_sum 'C50 H111 Mo12 N4 O42 P V2' _chemical_formula_weight 2724.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0854 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.2702 0.4354 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -2.8890 0.5675 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 23.8622(17) _cell_length_b 14.4740(17) _cell_length_c 49.226(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.462(7) _cell_angle_gamma 90.00 _cell_volume 16925(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 979 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.0 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10720 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6393 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX2 CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37547 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.1252 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 65 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.27 _reflns_number_total 20469 _reflns_number_gt 11207 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20469 _refine_ls_number_parameters 1010 _refine_ls_number_restraints 980 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.69187(3) 0.07669(5) 0.442009(14) 0.02887(17) Uani 1 1 d . . . Mo2 Mo 0.74015(3) -0.07330(5) 0.388993(14) 0.02855(16) Uani 1 1 d . . . Mo3 Mo 0.77370(3) 0.11776(5) 0.354195(14) 0.02771(16) Uani 1 1 d . . . Mo4 Mo 0.68132(3) -0.05605(5) 0.322929(14) 0.02855(16) Uani 1 1 d . . . Mo5 Mo 0.56995(3) 0.13227(5) 0.302585(14) 0.02841(17) Uani 1 1 d . . . Mo6 Mo 0.53524(3) -0.07278(5) 0.341040(14) 0.02879(17) Uani 1 1 d . . . Mo7 Mo 0.48853(3) 0.06668(5) 0.389623(15) 0.03213(18) Uani 1 1 d . . . Mo8 Mo 0.66096(3) 0.30400(5) 0.336242(15) 0.03026(17) Uani 1 1 d . . . Mo9 Mo 0.58896(3) 0.25213(5) 0.423159(15) 0.03274(18) Uani 1 1 d . . . Mo10 Mo 0.59392(3) -0.10661(5) 0.406342(14) 0.02862(16) Uani 1 1 d . . . Mo11 Mo 0.72486(3) 0.26832(5) 0.406898(14) 0.02949(17) Uani 1 1 d . . . Mo12 Mo 0.52602(3) 0.27212(5) 0.351830(15) 0.03416(18) Uani 1 1 d . . . V1 V 0.56373(6) 0.05501(11) 0.44388(3) 0.0378(3) Uani 1 1 d . . . V2 V 0.69809(6) 0.14234(10) 0.30063(3) 0.0342(3) Uani 1 1 d . . . P1 P 0.63159(8) 0.09864(14) 0.37226(4) 0.0263(4) Uani 1 1 d . . . O1 O 0.4236(2) 0.0715(4) 0.39972(12) 0.0459(15) Uani 1 1 d . . . O2 O 0.5370(2) 0.0367(4) 0.47204(11) 0.0450(15) Uani 1 1 d . . . O3 O 0.7250(2) 0.1616(4) 0.27274(10) 0.0423(15) Uani 1 1 d . . . O4 O 0.6929(2) -0.1215(4) 0.29609(11) 0.0414(14) Uani 1 1 d . . . O5 O 0.5349(2) 0.0316(4) 0.31796(11) 0.0346(13) Uani 1 1 d . . . O6 O 0.7827(2) -0.1572(4) 0.40140(11) 0.0385(14) Uani 1 1 d . . . O7 O 0.4747(2) 0.3501(4) 0.34889(12) 0.0479(16) Uani 1 1 d . . . O8 O 0.7710(2) 0.3511(4) 0.41659(12) 0.0429(15) Uani 1 1 d . . . O9 O 0.5558(3) 0.3165(4) 0.44494(12) 0.0489(16) Uani 1 1 d . . . O10 O 0.5268(2) -0.0291(4) 0.41539(10) 0.0346(13) Uani 1 1 d . . . O11 O 0.5448(2) 0.1288(4) 0.26967(11) 0.0428(15) Uani 1 1 d . . . O12 O 0.6568(2) 0.3115(4) 0.42357(11) 0.0398(14) Uani 1 1 d . . . O13 O 0.5897(2) 0.3459(4) 0.33999(11) 0.0396(14) Uani 1 1 d . . . O14 O 0.6494(2) 0.1492(4) 0.39901(10) 0.0315(12) Uani 1 1 d . . . O15 O 0.4915(2) 0.1668(4) 0.36648(11) 0.0394(14) Uani 1 1 d . . . O16 O 0.5556(2) -0.1475(4) 0.37459(11) 0.0351(13) Uani 1 1 d . . . O17 O 0.5608(2) 0.2903(4) 0.38923(11) 0.0394(14) Uani 1 1 d . . . O18 O 0.6829(2) 0.0473(4) 0.36308(10) 0.0295(12) Uani 1 1 d . . . O19 O 0.7234(2) 0.2114(4) 0.33292(10) 0.0337(13) Uani 1 1 d . . . O20 O 0.4987(2) -0.1489(4) 0.32117(11) 0.0402(14) Uani 1 1 d . . . O21 O 0.5846(2) 0.0294(3) 0.37639(10) 0.0300(12) Uani 1 1 d . . . O22 O 0.5227(2) 0.2194(4) 0.31643(11) 0.0381(14) Uani 1 1 d . . . O23 O 0.6874(2) 0.3152(4) 0.37197(11) 0.0347(13) Uani 1 1 d . . . O24 O 0.7170(3) 0.0469(4) 0.47338(11) 0.0463(15) Uani 1 1 d . . . O25 O 0.6888(3) 0.3957(4) 0.32120(11) 0.0429(15) Uani 1 1 d . . . O26 O 0.7232(2) -0.1156(4) 0.35078(11) 0.0345(13) Uani 1 1 d . . . O27 O 0.6650(2) -0.1207(4) 0.39556(11) 0.0362(13) Uani 1 1 d . . . O28 O 0.5325(2) 0.1461(4) 0.41833(11) 0.0395(14) Uani 1 1 d . . . O29 O 0.7336(2) 0.1840(4) 0.43673(11) 0.0344(13) Uani 1 1 d . . . O30 O 0.7907(2) 0.0105(4) 0.37428(10) 0.0308(12) Uani 1 1 d . . . O31 O 0.8364(2) 0.1466(4) 0.34445(11) 0.0356(13) Uani 1 1 d . . . O32 O 0.6128(2) -0.0945(4) 0.33210(11) 0.0336(13) Uani 1 1 d . . . O33 O 0.6328(2) 0.2266(4) 0.30290(11) 0.0345(13) Uani 1 1 d . . . O34 O 0.6279(2) -0.0144(4) 0.43409(11) 0.0378(14) Uani 1 1 d . . . O35 O 0.6228(2) 0.1523(4) 0.44929(11) 0.0360(13) Uani 1 1 d . . . O36 O 0.7324(2) 0.0043(4) 0.41931(11) 0.0350(13) Uani 1 1 d . . . O37 O 0.5872(2) -0.1973(4) 0.42727(11) 0.0401(14) Uani 1 1 d . . . O38 O 0.4792(2) -0.0210(4) 0.36154(11) 0.0355(13) Uani 1 1 d . . . O39 O 0.7662(2) 0.1912(4) 0.38477(11) 0.0341(13) Uani 1 1 d . . . O40 O 0.6090(2) 0.1679(4) 0.35040(10) 0.0319(12) Uani 1 1 d . . . O41 O 0.7413(2) 0.0425(4) 0.32138(10) 0.0317(12) Uani 1 1 d . . . O42 O 0.6393(2) 0.0509(4) 0.30302(10) 0.0348(13) Uani 1 1 d . . . N1 N 0.3232(3) 1.0979(5) 0.11058(17) 0.069(2) Uani 1 1 d DU . . C1 C 0.3503(4) 1.1567(6) 0.1335(2) 0.066(3) Uani 1 1 d DU . . H1A H 0.3205 1.1940 0.1410 0.079 Uiso 1 1 calc R . . H1B H 0.3766 1.2002 0.1258 0.079 Uiso 1 1 calc R . . C2 C 0.3822(5) 1.1054(7) 0.1570(2) 0.076(3) Uani 1 1 d DU . . H2A H 0.3555 1.0680 0.1665 0.091 Uiso 1 1 calc R . . H2B H 0.4095 1.0626 0.1496 0.091 Uiso 1 1 calc R . . C3 C 0.4130(5) 1.1698(8) 0.1768(3) 0.095(4) Uani 1 1 d DU . . H3A H 0.4328 1.2160 0.1664 0.114 Uiso 1 1 calc R . . H3B H 0.3849 1.2034 0.1866 0.114 Uiso 1 1 calc R . . C4 C 0.4548(5) 1.1269(9) 0.1975(3) 0.100(5) Uani 1 1 d DU . . H4A H 0.4699 1.1742 0.2104 0.150 Uiso 1 1 calc R . . H4B H 0.4856 1.0999 0.1883 0.150 Uiso 1 1 calc R . . H4C H 0.4365 1.0784 0.2073 0.150 Uiso 1 1 calc R . . C5 C 0.3670(5) 1.0341(7) 0.0993(3) 0.112(5) Uani 1 1 d DU . . H5A H 0.3853 0.9966 0.1145 0.135 Uiso 1 1 calc R . . H5B H 0.3475 0.9912 0.0859 0.135 Uiso 1 1 calc R . . C6 C 0.4114(6) 1.0856(10) 0.0859(4) 0.144(6) Uani 1 1 d DU . . H6A H 0.4250 1.1358 0.0985 0.173 Uiso 1 1 calc R . . H6B H 0.3925 1.1155 0.0694 0.173 Uiso 1 1 calc R . . C7 C 0.4624(6) 1.0372(11) 0.0774(4) 0.156(7) Uani 1 1 d DU . . H7A H 0.4506 0.9874 0.0643 0.187 Uiso 1 1 calc R . . H7B H 0.4857 1.0816 0.0681 0.187 Uiso 1 1 calc R . . C8 C 0.4948(8) 0.9988(12) 0.1003(4) 0.183(10) Uani 1 1 d DU . . H8A H 0.5342 0.9935 0.0964 0.275 Uiso 1 1 calc R . . H8B H 0.4802 0.9375 0.1042 0.275 Uiso 1 1 calc R . . H8C H 0.4924 1.0390 0.1162 0.275 Uiso 1 1 calc R . . C9 C 0.2972(4) 1.1639(6) 0.08901(18) 0.059(2) Uani 1 1 d DU . . H9A H 0.2683 1.2009 0.0972 0.071 Uiso 1 1 calc R . . H9B H 0.3269 1.2071 0.0842 0.071 Uiso 1 1 calc R . . C10 C 0.2701(5) 1.1217(7) 0.0628(2) 0.081(3) Uani 1 1 d DU . . H10A H 0.2418 1.0753 0.0672 0.097 Uiso 1 1 calc R . . H10B H 0.2992 1.0898 0.0532 0.097 Uiso 1 1 calc R . . C11 C 0.2418(5) 1.1959(8) 0.0444(2) 0.077(3) Uani 1 1 d DU . . H11A H 0.2234 1.1658 0.0278 0.092 Uiso 1 1 calc R . . H11B H 0.2120 1.2256 0.0540 0.092 Uiso 1 1 calc R . . C12 C 0.2804(6) 1.2689(10) 0.0359(2) 0.114(6) Uani 1 1 d DU . . H12A H 0.2612 1.3050 0.0209 0.170 Uiso 1 1 calc R . . H12B H 0.3142 1.2401 0.0297 0.170 Uiso 1 1 calc R . . H12C H 0.2912 1.3097 0.0513 0.170 Uiso 1 1 calc R . . C13 C 0.2795(4) 1.0347(7) 0.1214(2) 0.077(3) Uani 1 1 d DU . . H13A H 0.2628 0.9965 0.1061 0.092 Uiso 1 1 calc R . . H13B H 0.2993 0.9923 0.1349 0.092 Uiso 1 1 calc R . . C14 C 0.2321(4) 1.0794(7) 0.1347(2) 0.072(3) Uani 1 1 d DU . . H14A H 0.2127 1.1252 0.1222 0.087 Uiso 1 1 calc R . . H14B H 0.2469 1.1115 0.1516 0.087 Uiso 1 1 calc R . . C15 C 0.1912(4) 1.0028(8) 0.1413(3) 0.079(3) Uani 1 1 d DU . . H15A H 0.1789 0.9686 0.1244 0.095 Uiso 1 1 calc R . . H15B H 0.2110 0.9588 0.1543 0.095 Uiso 1 1 calc R . . C16 C 0.1419(5) 1.0392(9) 0.1531(3) 0.094(4) Uani 1 1 d DU . . H16A H 0.1219 0.9884 0.1611 0.141 Uiso 1 1 calc R . . H16B H 0.1169 1.0690 0.1387 0.141 Uiso 1 1 calc R . . H16C H 0.1538 1.0845 0.1672 0.141 Uiso 1 1 calc R . . N2 N 0.6164(3) 0.4321(4) 0.23687(12) 0.0394(16) Uani 1 1 d DU . . C17 C 0.6260(4) 0.4698(6) 0.20889(16) 0.047(2) Uani 1 1 d DU . . H17A H 0.6643 0.4517 0.2048 0.056 Uiso 1 1 calc R . . H17B H 0.5990 0.4392 0.1952 0.056 Uiso 1 1 calc R . . C18 C 0.6203(4) 0.5730(6) 0.20491(18) 0.051(2) Uani 1 1 d DU . . H18A H 0.5813 0.5919 0.2076 0.061 Uiso 1 1 calc R . . H18B H 0.6460 0.6050 0.2188 0.061 Uiso 1 1 calc R . . C19 C 0.6338(5) 0.6016(7) 0.17695(18) 0.064(3) Uani 1 1 d DU . . H19A H 0.6694 0.5711 0.1733 0.077 Uiso 1 1 calc R . . H19B H 0.6039 0.5772 0.1635 0.077 Uiso 1 1 calc R . . C20 C 0.6397(4) 0.7005(7) 0.1718(2) 0.069(3) Uani 1 1 d DU . . H20A H 0.6477 0.7099 0.1528 0.104 Uiso 1 1 calc R . . H20B H 0.6706 0.7256 0.1841 0.104 Uiso 1 1 calc R . . H20C H 0.6046 0.7322 0.1749 0.104 Uiso 1 1 calc R . . C21 C 0.5540(3) 0.4366(6) 0.24087(17) 0.048(2) Uani 1 1 d DU . . H21A H 0.5430 0.5026 0.2411 0.057 Uiso 1 1 calc R . . H21B H 0.5329 0.4082 0.2247 0.057 Uiso 1 1 calc R . . C22 C 0.5347(4) 0.3918(7) 0.26577(18) 0.055(2) Uani 1 1 d DU . . H22A H 0.5561 0.4181 0.2822 0.066 Uiso 1 1 calc R . . H22B H 0.5431 0.3249 0.2653 0.066 Uiso 1 1 calc R . . C23 C 0.4722(4) 0.4047(8) 0.2681(2) 0.066(3) Uani 1 1 d DU . . H23A H 0.4642 0.3889 0.2870 0.079 Uiso 1 1 calc R . . H23B H 0.4626 0.4706 0.2651 0.079 Uiso 1 1 calc R . . C24 C 0.4360(6) 0.3486(12) 0.2489(3) 0.131(6) Uani 1 1 d DU . . H24A H 0.3974 0.3497 0.2542 0.197 Uiso 1 1 calc R . . H24B H 0.4499 0.2848 0.2493 0.197 Uiso 1 1 calc R . . H24C H 0.4365 0.3737 0.2305 0.197 Uiso 1 1 calc R . . C25 C 0.6359(4) 0.3305(5) 0.23808(18) 0.048(2) Uani 1 1 d DU . . H25A H 0.6757 0.3282 0.2340 0.058 Uiso 1 1 calc R . . H25B H 0.6344 0.3078 0.2570 0.058 Uiso 1 1 calc R . . C26 C 0.6022(4) 0.2650(6) 0.21888(18) 0.049(2) Uani 1 1 d DU . . H26A H 0.5996 0.2910 0.2002 0.059 Uiso 1 1 calc R . . H26B H 0.5636 0.2601 0.2244 0.059 Uiso 1 1 calc R . . C27 C 0.6280(4) 0.1684(6) 0.21845(18) 0.046(2) Uani 1 1 d DU . . H27A H 0.6373 0.1472 0.2375 0.055 Uiso 1 1 calc R . . H27B H 0.5997 0.1253 0.2095 0.055 Uiso 1 1 calc R . . C28 C 0.6798(4) 0.1647(6) 0.20381(19) 0.052(2) Uani 1 1 d DU . . H28A H 0.6897 0.1001 0.2008 0.077 Uiso 1 1 calc R . . H28B H 0.7108 0.1952 0.2148 0.077 Uiso 1 1 calc R . . H28C H 0.6729 0.1963 0.1862 0.077 Uiso 1 1 calc R . . C29 C 0.6494(3) 0.4867(6) 0.25918(16) 0.050(2) Uani 1 1 d DU . . H29A H 0.6320 0.5486 0.2599 0.059 Uiso 1 1 calc R . . H29B H 0.6448 0.4559 0.2768 0.059 Uiso 1 1 calc R . . C30 C 0.7107(4) 0.4994(7) 0.2570(2) 0.058(3) Uani 1 1 d DU A . H30A H 0.7166 0.5212 0.2385 0.069 Uiso 1 1 calc R . . H30B H 0.7302 0.4393 0.2600 0.069 Uiso 1 1 calc R . . C31 C 0.7362(4) 0.5696(7) 0.2782(2) 0.063(3) Uani 1 1 d DU . . H31A H 0.7118 0.6250 0.2777 0.075 Uiso 0.498(17) 1 calc PR A 1 H31B H 0.7369 0.5421 0.2966 0.075 Uiso 0.498(17) 1 calc PR A 1 H31C H 0.7216 0.5567 0.2959 0.075 Uiso 0.502(17) 1 calc PR A 2 H31D H 0.7776 0.5608 0.2805 0.075 Uiso 0.502(17) 1 calc PR A 2 C32 C 0.7933(7) 0.5979(14) 0.2734(4) 0.062(6) Uani 0.498(17) 1 d PDU A 1 H32A H 0.8101 0.6329 0.2892 0.093 Uiso 0.498(17) 1 calc PR A 1 H32B H 0.7920 0.6368 0.2571 0.093 Uiso 0.498(17) 1 calc PR A 1 H32C H 0.8162 0.5430 0.2708 0.093 Uiso 0.498(17) 1 calc PR A 1 C32A C 0.7243(10) 0.6654(10) 0.2709(6) 0.095(10) Uani 0.502(17) 1 d PDU A 2 H32D H 0.7495 0.7059 0.2824 0.143 Uiso 0.502(17) 1 calc PR A 2 H32E H 0.6851 0.6796 0.2737 0.143 Uiso 0.502(17) 1 calc PR A 2 H32F H 0.7303 0.6752 0.2517 0.143 Uiso 0.502(17) 1 calc PR A 2 N3 N 0.5829(3) 0.2975(4) 0.04032(12) 0.0401(16) Uani 1 1 d DU B 2 C33 C 0.5768(4) 0.4019(5) 0.04138(18) 0.048(2) Uani 1 1 d DU B 2 H33A H 0.5644 0.4244 0.0228 0.057 Uiso 1 1 calc R B 2 H33B H 0.5468 0.4171 0.0532 0.057 Uiso 1 1 calc R B 2 C34 C 0.6294(4) 0.4529(6) 0.0517(2) 0.073(3) Uani 1 1 d DU B 2 H34A H 0.6623 0.4239 0.0443 0.087 Uiso 1 1 calc R B 2 H34B H 0.6348 0.4487 0.0719 0.087 Uiso 1 1 calc R B 2 C35 C 0.6255(5) 0.5542(6) 0.0431(2) 0.070(3) Uani 1 1 d DU B 2 H35A H 0.5861 0.5753 0.0436 0.084 Uiso 1 1 calc R B 2 H35B H 0.6493 0.5914 0.0566 0.084 Uiso 1 1 calc R B 2 C36 C 0.6429(6) 0.5715(10) 0.0162(2) 0.105(5) Uani 1 1 d DU B 2 H36A H 0.6106 0.5934 0.0041 0.157 Uiso 1 1 calc R B 2 H36B H 0.6573 0.5142 0.0089 0.157 Uiso 1 1 calc R B 2 H36C H 0.6726 0.6185 0.0174 0.157 Uiso 1 1 calc R B 2 C37 C 0.6227(4) 0.2712(6) 0.01931(17) 0.048(2) Uani 1 1 d DU B 2 H37A H 0.6611 0.2907 0.0263 0.057 Uiso 1 1 calc R B 2 H37B H 0.6119 0.3067 0.0024 0.057 Uiso 1 1 calc R B 2 C38 C 0.6246(4) 0.1689(6) 0.01184(19) 0.051(2) Uani 1 1 d DU B 2 H38A H 0.6277 0.1311 0.0287 0.061 Uiso 1 1 calc R B 2 H38B H 0.5893 0.1515 0.0008 0.061 Uiso 1 1 calc R B 2 C39 C 0.6743(4) 0.1501(7) -0.0041(2) 0.058(3) Uani 1 1 d DU B 2 H39A H 0.6730 0.1940 -0.0196 0.069 Uiso 1 1 calc R B 2 H39B H 0.7092 0.1627 0.0078 0.069 Uiso 1 1 calc R B 2 C40 C 0.6771(5) 0.0549(8) -0.0150(2) 0.086(4) Uani 1 1 d DU B 2 H40A H 0.7108 0.0486 -0.0248 0.129 Uiso 1 1 calc R B 2 H40B H 0.6435 0.0425 -0.0274 0.129 Uiso 1 1 calc R B 2 H40C H 0.6791 0.0108 0.0002 0.129 Uiso 1 1 calc R B 2 C41 C 0.5247(3) 0.2550(7) 0.03316(17) 0.050(2) Uani 1 1 d DU B 2 H41A H 0.5283 0.1871 0.0350 0.059 Uiso 1 1 calc R B 2 H41B H 0.4998 0.2761 0.0469 0.059 Uiso 1 1 calc R B 2 C42 C 0.4959(4) 0.2759(7) 0.00522(17) 0.054(2) Uani 1 1 d DU B 2 H42A H 0.5224 0.2644 -0.0087 0.065 Uiso 1 1 calc R B 2 H42B H 0.4851 0.3419 0.0042 0.065 Uiso 1 1 calc R B 2 C43 C 0.4437(4) 0.2164(7) -0.0010(2) 0.071(3) Uani 1 1 d DU B 2 H43A H 0.4198 0.2219 0.0143 0.086 Uiso 1 1 calc R B 2 H43B H 0.4219 0.2404 -0.0176 0.086 Uiso 1 1 calc R B 2 C44 C 0.4563(6) 0.1168(8) -0.0052(3) 0.093(4) Uani 1 1 d DU B 2 H44A H 0.4209 0.0825 -0.0087 0.140 Uiso 1 1 calc R B 2 H44B H 0.4777 0.0922 0.0112 0.140 Uiso 1 1 calc R B 2 H44C H 0.4785 0.1103 -0.0208 0.140 Uiso 1 1 calc R B 2 C45 C 0.6072(4) 0.2588(7) 0.06761(15) 0.052(2) Uani 1 1 d DU B 2 H45A H 0.6447 0.2872 0.0721 0.063 Uiso 1 1 calc R B 2 H45B H 0.6133 0.1917 0.0652 0.063 Uiso 1 1 calc R B 2 C46 C 0.5735(4) 0.2714(7) 0.09217(16) 0.054(3) Uani 1 1 d DU B 2 H46A H 0.5769 0.3360 0.0987 0.065 Uiso 1 1 calc R B 2 H46B H 0.5332 0.2587 0.0868 0.065 Uiso 1 1 calc R B 2 C47 C 0.5952(4) 0.2060(7) 0.11483(16) 0.051(2) Uani 1 1 d DU B 2 H47A H 0.5926 0.1418 0.1079 0.061 Uiso 1 1 calc R B 2 H47B H 0.6353 0.2197 0.1202 0.061 Uiso 1 1 calc R B 2 C48 C 0.5633(4) 0.2133(7) 0.13931(17) 0.058(3) Uani 1 1 d DU B 2 H48A H 0.5775 0.1675 0.1529 0.087 Uiso 1 1 calc R B 2 H48B H 0.5232 0.2019 0.1340 0.087 Uiso 1 1 calc R B 2 H48C H 0.5680 0.2754 0.1471 0.087 Uiso 1 1 calc R B 2 N4 N 0.6300(6) 0.9471(11) 0.0681(3) 0.136(5) Uani 1 1 d U C 2 C49 C 0.6119(6) 0.8777(12) 0.0751(3) 0.100(5) Uani 1 1 d U C 2 C50 C 0.5907(6) 0.7886(10) 0.0851(3) 0.105(5) Uani 1 1 d U C 2 H50A H 0.5630 0.8008 0.0981 0.158 Uiso 1 1 calc R C 2 H50B H 0.6222 0.7532 0.0941 0.158 Uiso 1 1 calc R C 2 H50C H 0.5730 0.7532 0.0696 0.158 Uiso 1 1 calc R C 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 0.0292(4) 0.0326(4) 0.0240(3) -0.0008(3) -0.0016(3) 0.0026(3) Mo2 0.0255(4) 0.0278(4) 0.0322(4) 0.0027(3) 0.0021(3) 0.0034(3) Mo3 0.0235(4) 0.0305(4) 0.0292(4) 0.0004(3) 0.0030(3) -0.0012(3) Mo4 0.0262(4) 0.0302(4) 0.0291(4) -0.0052(3) 0.0025(3) -0.0006(3) Mo5 0.0254(4) 0.0340(4) 0.0252(3) 0.0029(3) -0.0005(3) -0.0008(3) Mo6 0.0257(4) 0.0327(4) 0.0275(4) -0.0005(3) 0.0000(3) -0.0039(3) Mo7 0.0233(4) 0.0433(5) 0.0300(4) 0.0011(3) 0.0036(3) 0.0022(3) Mo8 0.0326(4) 0.0273(4) 0.0303(4) 0.0030(3) -0.0003(3) 0.0004(3) Mo9 0.0337(4) 0.0356(4) 0.0290(4) -0.0056(3) 0.0036(3) 0.0069(3) Mo10 0.0261(4) 0.0314(4) 0.0284(4) 0.0040(3) 0.0028(3) -0.0010(3) Mo11 0.0312(4) 0.0281(4) 0.0285(4) -0.0034(3) -0.0010(3) 0.0001(3) Mo12 0.0313(4) 0.0365(4) 0.0343(4) 0.0035(3) 0.0013(3) 0.0101(3) V1 0.0343(8) 0.0497(10) 0.0301(7) 0.0006(7) 0.0069(6) 0.0031(7) V2 0.0322(8) 0.0419(9) 0.0290(7) 0.0021(6) 0.0043(6) -0.0032(7) P1 0.0260(10) 0.0268(10) 0.0259(10) 0.0004(8) 0.0019(8) 0.0008(8) O1 0.036(3) 0.055(4) 0.048(4) -0.001(3) 0.007(3) 0.002(3) O2 0.040(4) 0.057(4) 0.039(3) -0.001(3) 0.009(3) -0.002(3) O3 0.050(4) 0.053(4) 0.025(3) 0.010(3) 0.006(3) -0.001(3) O4 0.042(4) 0.044(4) 0.038(3) -0.010(3) 0.006(3) 0.003(3) O5 0.028(3) 0.042(3) 0.034(3) 0.003(3) 0.003(2) -0.003(3) O6 0.040(3) 0.029(3) 0.047(4) 0.010(3) 0.006(3) 0.008(3) O7 0.038(4) 0.053(4) 0.052(4) 0.005(3) -0.001(3) 0.020(3) O8 0.042(4) 0.035(3) 0.050(4) -0.004(3) -0.002(3) -0.001(3) O9 0.046(4) 0.057(4) 0.045(4) -0.008(3) 0.009(3) 0.009(3) O10 0.030(3) 0.046(4) 0.029(3) 0.001(3) 0.008(2) 0.000(3) O11 0.043(4) 0.049(4) 0.035(3) 0.001(3) -0.002(3) -0.004(3) O12 0.046(4) 0.036(3) 0.038(3) -0.003(3) 0.005(3) 0.007(3) O13 0.039(3) 0.033(3) 0.045(3) 0.004(3) -0.002(3) 0.010(3) O14 0.030(3) 0.030(3) 0.034(3) -0.002(2) 0.002(2) 0.005(2) O15 0.030(3) 0.047(4) 0.040(3) 0.003(3) -0.001(3) 0.002(3) O16 0.030(3) 0.037(3) 0.038(3) 0.006(3) 0.004(2) 0.001(3) O17 0.039(3) 0.041(4) 0.037(3) 0.002(3) 0.000(3) 0.006(3) O18 0.033(3) 0.031(3) 0.025(3) 0.000(2) 0.005(2) 0.004(2) O19 0.033(3) 0.037(3) 0.031(3) 0.002(3) 0.002(2) 0.000(3) O20 0.035(3) 0.043(4) 0.042(3) -0.001(3) -0.001(3) -0.008(3) O21 0.030(3) 0.030(3) 0.029(3) -0.002(2) 0.000(2) 0.001(2) O22 0.030(3) 0.047(4) 0.037(3) 0.003(3) 0.001(2) 0.005(3) O23 0.034(3) 0.033(3) 0.036(3) 0.006(3) -0.003(2) 0.001(3) O24 0.052(4) 0.054(4) 0.032(3) 0.005(3) -0.005(3) -0.005(3) O25 0.060(4) 0.031(3) 0.036(3) 0.009(3) -0.004(3) -0.006(3) O26 0.036(3) 0.033(3) 0.034(3) -0.002(3) 0.001(2) -0.002(3) O27 0.033(3) 0.034(3) 0.042(3) -0.003(3) 0.005(3) -0.003(3) O28 0.033(3) 0.050(4) 0.035(3) 0.005(3) 0.003(2) 0.003(3) O29 0.030(3) 0.037(3) 0.035(3) -0.004(3) -0.003(2) 0.000(3) O30 0.026(3) 0.033(3) 0.034(3) -0.003(2) 0.002(2) 0.002(2) O31 0.028(3) 0.041(3) 0.038(3) -0.003(3) 0.005(2) -0.004(3) O32 0.033(3) 0.026(3) 0.042(3) 0.002(3) 0.004(2) -0.001(2) O33 0.031(3) 0.038(3) 0.034(3) -0.001(3) 0.000(2) -0.002(3) O34 0.035(3) 0.043(4) 0.037(3) -0.003(3) 0.008(3) 0.000(3) O35 0.040(3) 0.038(3) 0.031(3) -0.001(3) 0.005(2) 0.004(3) O36 0.025(3) 0.044(4) 0.036(3) 0.006(3) 0.001(2) -0.001(3) O37 0.041(3) 0.044(4) 0.035(3) 0.013(3) 0.004(3) -0.005(3) O38 0.026(3) 0.042(3) 0.038(3) 0.005(3) -0.001(2) 0.001(3) O39 0.030(3) 0.036(3) 0.037(3) 0.000(3) 0.003(2) 0.000(2) O40 0.033(3) 0.035(3) 0.027(3) 0.004(2) -0.001(2) 0.002(2) O41 0.034(3) 0.033(3) 0.028(3) -0.001(2) 0.003(2) -0.004(2) O42 0.034(3) 0.042(3) 0.028(3) 0.001(3) 0.003(2) -0.005(3) N1 0.054(5) 0.039(5) 0.115(6) 0.004(4) 0.014(4) -0.009(4) C1 0.056(7) 0.038(5) 0.101(7) 0.023(5) -0.003(5) -0.006(4) C2 0.057(7) 0.053(7) 0.117(8) 0.027(6) 0.000(6) 0.006(5) C3 0.058(8) 0.070(8) 0.147(11) 0.040(7) -0.037(7) -0.026(6) C4 0.059(8) 0.106(11) 0.131(11) 0.060(9) -0.012(7) -0.020(7) C5 0.097(9) 0.041(7) 0.204(14) -0.010(7) 0.038(8) 0.014(6) C6 0.110(11) 0.117(13) 0.216(17) -0.011(12) 0.078(10) 0.002(8) C7 0.088(12) 0.073(11) 0.31(2) -0.009(13) 0.030(11) 0.019(8) C8 0.140(17) 0.102(15) 0.30(3) -0.051(15) -0.032(17) -0.009(11) C9 0.063(7) 0.042(5) 0.074(6) -0.014(4) 0.019(5) 0.001(4) C10 0.066(8) 0.064(7) 0.112(8) -0.038(6) 0.005(6) -0.008(6) C11 0.065(8) 0.094(9) 0.070(7) -0.037(6) -0.002(5) -0.023(6) C12 0.117(12) 0.169(13) 0.051(7) 0.001(8) -0.015(7) -0.074(10) C13 0.068(7) 0.057(7) 0.103(9) 0.002(6) 0.002(6) -0.021(5) C14 0.055(6) 0.085(8) 0.074(8) 0.019(6) -0.009(5) -0.011(5) C15 0.054(7) 0.085(9) 0.098(9) 0.022(7) -0.002(6) -0.001(5) C16 0.070(8) 0.083(10) 0.132(12) 0.011(9) 0.022(8) 0.007(7) N2 0.034(4) 0.046(4) 0.038(4) 0.001(3) 0.003(3) 0.010(3) C17 0.036(5) 0.058(5) 0.047(5) 0.003(4) 0.007(4) 0.006(4) C18 0.045(5) 0.049(5) 0.057(5) 0.006(4) -0.009(4) 0.012(4) C19 0.065(7) 0.070(6) 0.053(6) 0.019(5) -0.024(5) -0.027(6) C20 0.044(6) 0.065(7) 0.096(9) 0.027(6) -0.007(6) -0.011(5) C21 0.038(4) 0.055(6) 0.051(5) 0.005(4) 0.008(4) 0.015(4) C22 0.051(5) 0.062(7) 0.055(6) 0.003(5) 0.016(4) 0.012(5) C23 0.046(5) 0.081(8) 0.074(7) 0.014(6) 0.023(5) 0.014(5) C24 0.077(10) 0.192(17) 0.117(13) 0.009(11) -0.031(9) -0.022(10) C25 0.037(5) 0.058(5) 0.050(5) -0.001(4) 0.005(4) 0.010(4) C26 0.049(6) 0.052(5) 0.047(5) 0.005(4) 0.006(4) -0.007(4) C27 0.039(5) 0.054(5) 0.044(5) 0.005(4) 0.002(4) -0.004(4) C28 0.059(6) 0.045(6) 0.051(6) 0.000(5) 0.011(5) -0.001(5) C29 0.057(5) 0.053(6) 0.037(4) 0.002(4) -0.004(4) -0.005(5) C30 0.055(5) 0.061(6) 0.057(6) 0.004(5) -0.003(5) 0.001(5) C31 0.067(7) 0.064(7) 0.054(6) 0.004(5) -0.012(5) -0.018(5) C32 0.078(12) 0.055(14) 0.054(13) -0.001(10) 0.012(10) -0.011(10) C32A 0.075(18) 0.058(9) 0.15(3) -0.009(13) -0.013(17) 0.021(13) N3 0.037(4) 0.046(4) 0.038(4) 0.002(3) 0.011(3) 0.010(3) C33 0.047(5) 0.048(4) 0.047(5) -0.003(4) 0.002(4) 0.013(4) C34 0.062(7) 0.045(5) 0.110(9) -0.027(5) 0.005(6) 0.006(5) C35 0.061(7) 0.052(6) 0.098(8) -0.010(6) 0.017(6) 0.002(5) C36 0.084(10) 0.132(12) 0.102(10) 0.011(9) 0.030(8) 0.027(9) C37 0.046(5) 0.051(5) 0.048(5) 0.004(4) 0.016(4) 0.009(4) C38 0.045(5) 0.059(6) 0.048(5) -0.014(5) 0.008(4) 0.005(5) C39 0.049(6) 0.071(7) 0.054(6) -0.009(5) 0.013(5) 0.015(5) C40 0.081(9) 0.094(9) 0.084(9) -0.049(7) 0.009(7) 0.021(7) C41 0.040(4) 0.060(6) 0.050(5) 0.005(5) 0.007(4) -0.001(4) C42 0.048(5) 0.070(6) 0.043(5) -0.002(5) 0.004(4) 0.007(5) C43 0.051(6) 0.099(8) 0.061(7) 0.010(7) -0.009(5) -0.001(6) C44 0.102(11) 0.091(8) 0.086(9) -0.010(8) 0.007(8) -0.035(7) C45 0.053(6) 0.066(6) 0.036(4) 0.002(4) 0.003(4) 0.016(5) C46 0.068(7) 0.055(6) 0.039(4) -0.002(4) 0.007(4) 0.015(5) C47 0.057(6) 0.057(6) 0.037(5) -0.002(4) 0.001(4) -0.004(5) C48 0.064(7) 0.067(7) 0.045(5) 0.012(5) 0.015(5) 0.006(6) N4 0.118(12) 0.144(13) 0.146(13) 0.018(10) 0.013(10) -0.046(10) C49 0.083(10) 0.122(13) 0.098(11) 0.008(10) 0.021(8) -0.016(9) C50 0.093(11) 0.119(11) 0.104(11) -0.005(9) 0.004(9) -0.027(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O14 2.490(5) . ? Mo1 O24 1.660(6) . ? Mo1 O29 1.876(5) . ? Mo1 O34 2.026(6) . ? Mo1 O35 2.039(5) . ? Mo1 O36 1.867(5) . ? Mo2 O6 1.661(5) . ? Mo2 O18 2.491(5) . ? Mo2 O26 1.983(5) . ? Mo2 O27 1.975(5) . ? Mo2 O30 1.903(5) . ? Mo2 O36 1.891(6) . ? Mo3 O18 2.471(5) . ? Mo3 O19 2.033(5) . ? Mo3 O30 1.864(5) . ? Mo3 O31 1.667(5) . ? Mo3 O39 1.865(5) . ? Mo3 O41 2.038(5) . ? Mo4 O4 1.670(5) . ? Mo4 O18 2.476(5) . ? Mo4 O26 1.833(5) . ? Mo4 O32 1.824(5) . ? Mo4 O41 2.028(5) . ? Mo4 O42 2.043(5) . ? Mo5 O5 1.874(5) . ? Mo5 O11 1.674(5) . ? Mo5 O22 1.863(5) . ? Mo5 O33 2.028(5) . ? Mo5 O40 2.501(5) . ? Mo5 O42 2.030(6) . ? Mo6 O5 1.890(5) . ? Mo6 O16 1.995(5) . ? Mo6 O20 1.663(5) . ? Mo6 O21 2.493(5) . ? Mo6 O32 1.968(5) . ? Mo6 O38 1.903(5) . ? Mo7 O1 1.674(6) . ? Mo7 O10 2.036(5) . ? Mo7 O15 1.848(6) . ? Mo7 O21 2.501(5) . ? Mo7 O28 2.034(6) . ? Mo7 O38 1.874(6) . ? Mo8 O13 1.831(6) . ? Mo8 O19 2.023(5) . ? Mo8 O23 1.818(5) . ? Mo8 O25 1.687(6) . ? Mo8 O33 2.047(5) . ? Mo8 O40 2.464(5) . ? Mo9 O9 1.675(6) . ? Mo9 O12 1.831(6) . ? Mo9 O14 2.458(5) . ? Mo9 O17 1.825(5) . ? Mo9 O28 2.041(6) . ? Mo9 O35 2.048(5) . ? Mo10 O10 2.039(5) . ? Mo10 O16 1.832(5) . ? Mo10 O21 2.457(5) . ? Mo10 O27 1.836(5) . ? Mo10 O34 2.024(6) . ? Mo10 O37 1.686(5) . ? Mo11 O8 1.666(6) . ? Mo11 O12 1.989(6) . ? Mo11 O14 2.496(5) . ? Mo11 O23 1.981(5) . ? Mo11 O29 1.905(5) . ? Mo11 O39 1.900(5) . ? Mo12 O7 1.662(6) . ? Mo12 O13 1.990(6) . ? Mo12 O15 1.907(6) . ? Mo12 O17 1.964(5) . ? Mo12 O22 1.897(5) . ? Mo12 O40 2.495(5) . ? V1 O2 1.603(6) . ? V1 O10 1.998(6) . ? V1 O28 1.922(6) . ? V1 O34 1.930(6) . ? V1 O35 1.992(6) . ? V2 O3 1.594(5) . ? V2 O19 1.925(5) . ? V2 O33 1.989(5) . ? V2 O41 1.998(5) . ? V2 O42 1.940(5) . ? P1 O14 1.531(5) . ? P1 O18 1.537(5) . ? P1 O21 1.531(5) . ? P1 O40 1.531(5) . ? N1 C1 1.510(9) . ? N1 C5 1.536(10) . ? N1 C9 1.516(9) . ? N1 C13 1.522(9) . ? C1 C2 1.515(10) . ? C2 C3 1.492(11) . ? C3 C4 1.491(11) . ? C5 C6 1.499(12) . ? C6 C7 1.499(12) . ? C7 C8 1.420(13) . ? C9 C10 1.513(10) . ? C10 C11 1.523(11) . ? C11 C12 1.487(11) . ? C13 C14 1.503(11) . ? C14 C15 1.532(10) . ? C15 C16 1.458(11) . ? N2 C17 1.519(8) . ? N2 C21 1.523(8) . ? N2 C25 1.541(8) . ? N2 C29 1.511(8) . ? C17 C18 1.510(9) . ? C18 C19 1.502(10) . ? C19 C20 1.463(10) . ? C21 C22 1.497(9) . ? C22 C23 1.517(10) . ? C23 C24 1.464(11) . ? C25 C26 1.513(9) . ? C26 C27 1.528(9) . ? C27 C28 1.489(9) . ? C29 C30 1.489(10) . ? C30 C31 1.538(10) . ? C31 C32 1.462(12) . ? C31 C32A 1.453(13) . ? N3 C33 1.518(8) . ? N3 C37 1.518(8) . ? N3 C41 1.529(8) . ? N3 C45 1.519(8) . ? C33 C34 1.502(10) . ? C34 C35 1.526(10) . ? C35 C36 1.448(11) . ? C37 C38 1.526(9) . ? C38 C39 1.509(9) . ? C39 C40 1.482(10) . ? C41 C42 1.508(9) . ? C42 C43 1.521(10) . ? C43 C44 1.490(11) . ? C45 C46 1.526(9) . ? C46 C47 1.516(9) . ? C47 C48 1.489(9) . ? N4 C49 1.158(17) . ? C49 C50 1.486(19) . ? C1 H1A 0.990 . ? C1 H1B 0.990 . ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.990 . ? C5 H5B 0.990 . ? C6 H6A 0.990 . ? C6 H6B 0.990 . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 H28A 0.980 . ? C28 H28B 0.980 . ? C28 H28C 0.980 . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C31 H31C 0.990 . ? C31 H31D 0.990 . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C32A H32D 0.980 . ? C32A H32E 0.980 . ? C32A H32F 0.980 . ? C33 H33A 0.990 . ? C33 H33B 0.990 . ? C34 H34A 0.990 . ? C34 H34B 0.990 . ? C35 H35A 0.990 . ? C35 H35B 0.990 . ? C36 H36A 0.980 . ? C36 H36B 0.980 . ? C36 H36C 0.980 . ? C37 H37A 0.990 . ? C37 H37B 0.990 . ? C38 H38A 0.990 . ? C38 H38B 0.990 . ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? C41 H41A 0.990 . ? C41 H41B 0.990 . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C44 H44A 0.980 . ? C44 H44B 0.980 . ? C44 H44C 0.980 . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C46 H46A 0.990 . ? C46 H46B 0.990 . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C48 H48A 0.980 . ? C48 H48B 0.980 . ? C48 H48C 0.980 . ? C50 H50A 0.980 . ? C50 H50B 0.980 . ? C50 H50C 0.980 . ? 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 O14 Mo1 O24 169.2(2) . . ? O14 Mo1 O29 73.2(2) . . ? O14 Mo1 O34 82.7(2) . . ? O14 Mo1 O35 69.69(19) . . ? O14 Mo1 O36 85.4(2) . . ? O24 Mo1 O29 101.2(3) . . ? O24 Mo1 O34 102.0(3) . . ? O24 Mo1 O35 101.7(3) . . ? O24 Mo1 O36 104.4(3) . . ? O29 Mo1 O34 155.7(2) . . ? O29 Mo1 O35 91.6(2) . . ? O29 Mo1 O36 94.0(2) . . ? O34 Mo1 O35 77.1(2) . . ? O34 Mo1 O36 86.8(2) . . ? O35 Mo1 O36 151.6(2) . . ? O6 Mo2 O18 170.5(2) . . ? O6 Mo2 O26 100.7(3) . . ? O6 Mo2 O27 102.6(2) . . ? O6 Mo2 O30 102.6(2) . . ? O6 Mo2 O36 104.3(3) . . ? O18 Mo2 O26 71.24(19) . . ? O18 Mo2 O27 82.2(2) . . ? O18 Mo2 O30 72.25(19) . . ? O18 Mo2 O36 84.15(19) . . ? O26 Mo2 O27 86.6(2) . . ? O26 Mo2 O30 85.2(2) . . ? O26 Mo2 O36 154.9(2) . . ? O27 Mo2 O30 154.5(2) . . ? O27 Mo2 O36 85.3(2) . . ? O30 Mo2 O36 92.0(2) . . ? O18 Mo3 O19 83.20(19) . . ? O18 Mo3 O30 73.33(19) . . ? O18 Mo3 O31 168.6(2) . . ? O18 Mo3 O39 86.5(2) . . ? O18 Mo3 O41 69.33(18) . . ? O19 Mo3 O30 156.4(2) . . ? O19 Mo3 O31 100.7(2) . . ? O19 Mo3 O39 86.5(2) . . ? O19 Mo3 O41 77.7(2) . . ? O30 Mo3 O31 101.8(2) . . ? O30 Mo3 O39 94.5(2) . . ? O30 Mo3 O41 91.3(2) . . ? O31 Mo3 O39 104.3(2) . . ? O31 Mo3 O41 100.9(2) . . ? O39 Mo3 O41 152.3(2) . . ? O4 Mo4 O18 169.4(2) . . ? O4 Mo4 O26 101.8(3) . . ? O4 Mo4 O32 104.1(3) . . ? O4 Mo4 O41 101.4(2) . . ? O4 Mo4 O42 99.3(2) . . ? O18 Mo4 O26 73.8(2) . . ? O18 Mo4 O32 86.1(2) . . ? O18 Mo4 O41 69.38(19) . . ? O18 Mo4 O42 83.95(19) . . ? O26 Mo4 O32 96.2(2) . . ? O26 Mo4 O41 91.3(2) . . ? O26 Mo4 O42 157.3(2) . . ? O32 Mo4 O41 151.2(2) . . ? O32 Mo4 O42 86.5(2) . . ? O41 Mo4 O42 76.4(2) . . ? O5 Mo5 O11 103.6(3) . . ? O5 Mo5 O22 94.0(2) . . ? O5 Mo5 O33 151.4(2) . . ? O5 Mo5 O40 85.4(2) . . ? O5 Mo5 O42 86.5(2) . . ? O11 Mo5 O22 101.6(3) . . ? O11 Mo5 O33 103.0(2) . . ? O11 Mo5 O40 169.7(2) . . ? O11 Mo5 O42 102.1(3) . . ? O22 Mo5 O33 90.9(2) . . ? O22 Mo5 O40 72.6(2) . . ? O22 Mo5 O42 155.5(2) . . ? O33 Mo5 O40 69.20(19) . . ? O33 Mo5 O42 77.8(2) . . ? O40 Mo5 O42 83.08(19) . . ? O5 Mo6 O16 156.6(2) . . ? O5 Mo6 O20 101.8(3) . . ? O5 Mo6 O21 85.4(2) . . ? O5 Mo6 O32 86.7(2) . . ? O5 Mo6 O38 92.4(2) . . ? O16 Mo6 O20 101.6(3) . . ? O16 Mo6 O21 71.5(2) . . ? O16 Mo6 O32 86.4(2) . . ? O16 Mo6 O38 84.4(2) . . ? O20 Mo6 O21 171.8(2) . . ? O20 Mo6 O32 102.4(2) . . ? O20 Mo6 O38 102.6(3) . . ? O21 Mo6 O32 81.87(19) . . ? O21 Mo6 O38 72.9(2) . . ? O32 Mo6 O38 154.7(2) . . ? O1 Mo7 O10 102.5(3) . . ? O1 Mo7 O15 103.9(3) . . ? O1 Mo7 O21 169.8(2) . . ? O1 Mo7 O28 101.6(3) . . ? O1 Mo7 O38 101.5(3) . . ? O10 Mo7 O15 151.3(2) . . ? O10 Mo7 O21 69.37(18) . . ? O10 Mo7 O28 77.3(2) . . ? O10 Mo7 O38 90.7(2) . . ? O15 Mo7 O21 85.4(2) . . ? O15 Mo7 O28 86.4(2) . . ? O15 Mo7 O38 94.9(2) . . ? O21 Mo7 O28 82.96(19) . . ? O21 Mo7 O38 73.1(2) . . ? O28 Mo7 O38 155.8(2) . . ? O13 Mo8 O19 157.8(2) . . ? O13 Mo8 O23 96.5(2) . . ? O13 Mo8 O25 101.1(3) . . ? O13 Mo8 O33 91.5(2) . . ? O13 Mo8 O40 74.9(2) . . ? O19 Mo8 O23 87.0(2) . . ? O19 Mo8 O25 99.3(3) . . ? O19 Mo8 O33 76.1(2) . . ? O19 Mo8 O40 83.53(19) . . ? O23 Mo8 O25 103.9(3) . . ? O23 Mo8 O33 151.8(2) . . ? O23 Mo8 O40 86.3(2) . . ? O25 Mo8 O33 101.0(2) . . ? O25 Mo8 O40 169.5(2) . . ? O33 Mo8 O40 69.74(19) . . ? O9 Mo9 O12 101.7(3) . . ? O9 Mo9 O14 169.0(2) . . ? O9 Mo9 O17 105.2(3) . . ? O9 Mo9 O28 98.4(3) . . ? O9 Mo9 O35 99.9(3) . . ? O12 Mo9 O14 74.4(2) . . ? O12 Mo9 O17 96.7(3) . . ? O12 Mo9 O28 158.0(2) . . ? O12 Mo9 O35 91.7(2) . . ? O14 Mo9 O17 85.6(2) . . ? O14 Mo9 O28 84.2(2) . . ? O14 Mo9 O35 70.24(19) . . ? O17 Mo9 O28 86.5(2) . . ? O17 Mo9 O35 151.2(2) . . ? O28 Mo9 O35 76.0(2) . . ? O10 Mo10 O16 91.5(2) . . ? O10 Mo10 O21 70.27(19) . . ? O10 Mo10 O27 152.9(2) . . ? O10 Mo10 O34 76.3(2) . . ? O10 Mo10 O37 99.9(2) . . ? O16 Mo10 O21 74.8(2) . . ? O16 Mo10 O27 96.7(2) . . ? O16 Mo10 O34 157.6(2) . . ? O16 Mo10 O37 101.6(3) . . ? O21 Mo10 O27 87.0(2) . . ? O21 Mo10 O34 83.3(2) . . ? O21 Mo10 O37 169.2(2) . . ? O27 Mo10 O34 86.9(2) . . ? O27 Mo10 O37 103.6(3) . . ? O34 Mo10 O37 99.0(3) . . ? O8 Mo11 O12 101.5(3) . . ? O8 Mo11 O14 171.3(2) . . ? O8 Mo11 O23 103.5(3) . . ? O8 Mo11 O29 102.7(3) . . ? O8 Mo11 O39 102.8(3) . . ? O12 Mo11 O14 71.1(2) . . ? O12 Mo11 O23 86.1(2) . . ? O12 Mo11 O29 85.2(2) . . ? O12 Mo11 O39 155.5(2) . . ? O14 Mo11 O23 80.9(2) . . ? O14 Mo11 O29 72.6(2) . . ? O14 Mo11 O39 84.9(2) . . ? O23 Mo11 O29 153.6(2) . . ? O23 Mo11 O39 85.4(2) . . ? O29 Mo11 O39 92.4(2) . . ? O7 Mo12 O13 100.8(3) . . ? O7 Mo12 O15 103.5(3) . . ? O7 Mo12 O17 103.5(3) . . ? O7 Mo12 O22 103.1(3) . . ? O7 Mo12 O40 171.3(3) . . ? O13 Mo12 O15 155.5(2) . . ? O13 Mo12 O17 86.3(2) . . ? O13 Mo12 O22 85.0(2) . . ? O13 Mo12 O40 71.70(19) . . ? O15 Mo12 O17 85.0(2) . . ? O15 Mo12 O22 92.5(2) . . ? O15 Mo12 O40 84.3(2) . . ? O17 Mo12 O22 153.1(2) . . ? O17 Mo12 O40 80.9(2) . . ? O22 Mo12 O40 72.2(2) . . ? O2 V1 O10 108.7(3) . . ? O2 V1 O28 121.2(3) . . ? O2 V1 O34 121.4(3) . . ? O2 V1 O35 109.6(3) . . ? O10 V1 O28 80.9(2) . . ? O10 V1 O34 79.4(2) . . ? O10 V1 O35 141.6(2) . . ? O28 V1 O34 117.4(2) . . ? O28 V1 O35 80.1(2) . . ? O34 V1 O35 80.4(2) . . ? O3 V2 O19 120.0(3) . . ? O3 V2 O33 108.8(3) . . ? O3 V2 O41 109.6(3) . . ? O3 V2 O42 121.6(3) . . ? O19 V2 O33 79.7(2) . . ? O19 V2 O41 81.2(2) . . ? O19 V2 O42 118.4(2) . . ? O33 V2 O41 141.5(2) . . ? O33 V2 O42 80.8(2) . . ? O41 V2 O42 79.4(2) . . ? O14 P1 O18 108.6(3) . . ? O14 P1 O21 110.2(3) . . ? O14 P1 O40 110.0(3) . . ? O18 P1 O21 109.7(3) . . ? O18 P1 O40 110.3(3) . . ? O21 P1 O40 108.0(3) . . ? Mo5 O5 Mo6 152.6(3) . . ? Mo7 O10 Mo10 123.6(2) . . ? Mo7 O10 V1 99.4(2) . . ? Mo10 O10 V1 100.7(2) . . ? Mo9 O12 Mo11 127.1(3) . . ? Mo8 O13 Mo12 126.5(3) . . ? Mo1 O14 Mo9 93.11(17) . . ? Mo1 O14 Mo11 85.98(16) . . ? Mo1 O14 P1 126.0(3) . . ? Mo9 O14 Mo11 87.36(17) . . ? Mo9 O14 P1 125.3(3) . . ? Mo11 O14 P1 127.0(3) . . ? Mo7 O15 Mo12 154.5(3) . . ? Mo6 O16 Mo10 126.4(3) . . ? Mo9 O17 Mo12 154.6(3) . . ? Mo2 O18 Mo3 86.14(16) . . ? Mo2 O18 Mo4 87.22(16) . . ? Mo2 O18 P1 127.0(3) . . ? Mo3 O18 Mo4 93.16(16) . . ? Mo3 O18 P1 126.1(3) . . ? Mo4 O18 P1 125.1(3) . . ? Mo3 O19 Mo8 143.5(3) . . ? Mo3 O19 V2 101.7(2) . . ? Mo8 O19 V2 103.6(2) . . ? Mo6 O21 Mo7 85.74(16) . . ? Mo6 O21 Mo10 87.31(17) . . ? Mo6 O21 P1 126.8(3) . . ? Mo7 O21 Mo10 92.81(17) . . ? Mo7 O21 P1 126.5(3) . . ? Mo10 O21 P1 125.3(3) . . ? Mo5 O22 Mo12 129.4(3) . . ? Mo8 O23 Mo11 153.5(3) . . ? Mo2 O26 Mo4 127.7(3) . . ? Mo2 O27 Mo10 152.5(3) . . ? Mo7 O28 Mo9 142.9(3) . . ? Mo7 O28 V1 102.1(3) . . ? Mo9 O28 V1 103.3(3) . . ? Mo1 O29 Mo11 128.1(3) . . ? Mo2 O30 Mo3 128.2(3) . . ? Mo4 O32 Mo6 153.0(3) . . ? Mo5 O33 Mo8 124.1(3) . . ? Mo5 O33 V2 99.8(2) . . ? Mo8 O33 V2 100.5(2) . . ? Mo1 O34 Mo10 143.6(3) . . ? Mo1 O34 V1 102.4(3) . . ? Mo10 O34 V1 103.6(3) . . ? Mo1 O35 Mo9 123.0(3) . . ? Mo1 O35 V1 99.8(2) . . ? Mo9 O35 V1 100.6(2) . . ? Mo1 O36 Mo2 154.2(3) . . ? Mo6 O38 Mo7 128.2(3) . . ? Mo3 O39 Mo11 153.2(3) . . ? Mo5 O40 Mo8 92.93(17) . . ? Mo5 O40 Mo12 85.75(16) . . ? Mo5 O40 P1 127.0(3) . . ? Mo8 O40 Mo12 86.95(17) . . ? Mo8 O40 P1 124.7(3) . . ? Mo12 O40 P1 127.1(3) . . ? Mo3 O41 Mo4 124.2(2) . . ? Mo3 O41 V2 99.0(2) . . ? Mo4 O41 V2 101.3(2) . . ? Mo4 O42 Mo5 143.8(3) . . ? Mo4 O42 V2 102.8(2) . . ? Mo5 O42 V2 101.4(3) . . ? C1 N1 C5 110.5(8) . . ? C1 N1 C9 106.7(7) . . ? C1 N1 C13 109.6(8) . . ? C5 N1 C9 111.9(8) . . ? C5 N1 C13 106.1(7) . . ? C9 N1 C13 112.1(8) . . ? N1 C1 C2 116.2(8) . . ? C1 C2 C3 111.9(8) . . ? C2 C3 C4 116.3(10) . . ? N1 C5 C6 113.2(9) . . ? C5 C6 C7 121.3(12) . . ? C6 C7 C8 110.8(15) . . ? N1 C9 C10 117.1(8) . . ? C9 C10 C11 110.7(8) . . ? C10 C11 C12 114.7(10) . . ? N1 C13 C14 117.6(8) . . ? C13 C14 C15 107.5(9) . . ? C14 C15 C16 112.2(10) . . ? C17 N2 C21 109.6(6) . . ? C17 N2 C25 107.9(6) . . ? C17 N2 C29 111.0(6) . . ? C21 N2 C25 109.3(6) . . ? C21 N2 C29 109.4(6) . . ? C25 N2 C29 109.7(6) . . ? N2 C17 C18 117.0(7) . . ? C17 C18 C19 111.6(7) . . ? C18 C19 C20 117.6(9) . . ? N2 C21 C22 117.9(7) . . ? C21 C22 C23 113.0(8) . . ? C22 C23 C24 113.9(10) . . ? N2 C25 C26 115.7(7) . . ? C25 C26 C27 113.1(7) . . ? C26 C27 C28 113.2(7) . . ? N2 C29 C30 117.4(7) . . ? C29 C30 C31 111.3(8) . . ? C30 C31 C32 113.1(11) . . ? C30 C31 C32A 114.0(12) . . ? C33 N3 C37 110.0(6) . . ? C33 N3 C41 108.7(6) . . ? C33 N3 C45 111.5(6) . . ? C37 N3 C41 110.8(6) . . ? C37 N3 C45 107.4(6) . . ? C41 N3 C45 108.5(6) . . ? N3 C33 C34 114.9(7) . . ? C33 C34 C35 110.6(8) . . ? C34 C35 C36 113.8(10) . . ? N3 C37 C38 116.3(7) . . ? C37 C38 C39 110.1(7) . . ? C38 C39 C40 114.9(8) . . ? N3 C41 C42 117.0(7) . . ? C41 C42 C43 111.2(7) . . ? C42 C43 C44 113.8(9) . . ? N3 C45 C46 118.1(7) . . ? C45 C46 C47 109.8(7) . . ? C46 C47 C48 112.7(8) . . ? N4 C49 C50 177.4(19) . . ? N1 C1 H1A 108.2 . . ? N1 C1 H1B 108.2 . . ? H1A C1 H1B 107.4 . . ? H1A C1 C2 108.2 . . ? H1B C1 C2 108.2 . . ? C1 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? H2A C2 C3 109.2 . . ? H2B C2 C3 109.2 . . ? C2 C3 H3A 108.2 . . ? C2 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? H3A C3 C4 108.2 . . ? H3B C3 C4 108.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 108.9 . . ? N1 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? H5A C5 C6 108.9 . . ? H5B C5 C6 108.9 . . ? C5 C6 H6A 107.0 . . ? C5 C6 H6B 107.0 . . ? H6A C6 H6B 106.7 . . ? H6A C6 C7 107.0 . . ? H6B C6 C7 107.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? H7A C7 C8 109.5 . . ? H7B C7 C8 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 108.0 . . ? N1 C9 H9B 108.0 . . ? H9A C9 H9B 107.3 . . ? H9A C9 C10 108.0 . . ? H9B C9 C10 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? H10A C10 C11 109.5 . . ? H10B C10 C11 109.5 . . ? C10 C11 H11A 108.6 . . ? C10 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? H11A C11 C12 108.6 . . ? H11B C11 C12 108.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 H13A 107.9 . . ? N1 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? H13A C13 C14 107.9 . . ? H13B C13 C14 107.9 . . ? C13 C14 H14A 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? H14A C14 C15 110.2 . . ? H14B C14 C15 110.2 . . ? C14 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? H15A C15 C16 109.2 . . ? H15B C15 C16 109.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 108.1 . . ? N2 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? H17A C17 C18 108.1 . . ? H17B C17 C18 108.1 . . ? C17 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? H18A C18 C19 109.3 . . ? H18B C18 C19 109.3 . . ? C18 C19 H19A 107.9 . . ? C18 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? H19A C19 C20 107.9 . . ? H19B C19 C20 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 H21A 107.8 . . ? N2 C21 H21B 107.8 . . ? H21A C21 H21B 107.2 . . ? H21A C21 C22 107.8 . . ? H21B C21 C22 107.8 . . ? C21 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? H22A C22 C23 109.0 . . ? H22B C22 C23 109.0 . . ? C22 C23 H23A 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? H23A C23 C24 108.8 . . ? H23B C23 C24 108.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 H25A 108.4 . . ? N2 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? H25A C25 C26 108.4 . . ? H25B C25 C26 108.4 . . ? C25 C26 H26A 109.0 . . ? C25 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? H26A C26 C27 109.0 . . ? H26B C26 C27 109.0 . . ? C26 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.8 . . ? H27A C27 C28 108.9 . . ? H27B C27 C28 108.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 H29A 107.9 . . ? N2 C29 H29B 107.9 . . ? H29A C29 H29B 107.2 . . ? H29A C29 C30 107.9 . . ? H29B C29 C30 107.9 . . ? C29 C30 H30A 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? H30A C30 C31 109.4 . . ? H30B C30 C31 109.4 . . ? C30 C31 H31A 109.0 . . ? C30 C31 H31B 109.0 . . ? C30 C31 H31C 108.7 . . ? C30 C31 H31D 108.7 . . ? H31A C31 H31B 107.8 . . ? H31A C31 C32 109.0 . . ? H31B C31 C32 109.0 . . ? H31C C31 H31D 107.6 . . ? H31C C31 C32A 108.7 . . ? H31D C31 C32A 108.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C32A H32D 109.5 . . ? C31 C32A H32E 109.5 . . ? C31 C32A H32F 109.5 . . ? H32D C32A H32E 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? N3 C33 H33A 108.5 . . ? N3 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? H33A C33 C34 108.5 . . ? H33B C33 C34 108.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? H34A C34 C35 109.5 . . ? H34B C34 C35 109.5 . . ? C34 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? H35A C35 C36 108.8 . . ? H35B C35 C36 108.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 H37A 108.2 . . ? N3 C37 H37B 108.2 . . ? H37A C37 H37B 107.4 . . ? H37A C37 C38 108.2 . . ? H37B C37 C38 108.2 . . ? C37 C38 H38A 109.6 . . ? C37 C38 H38B 109.6 . . ? H38A C38 H38B 108.2 . . ? H38A C38 C39 109.6 . . ? H38B C38 C39 109.6 . . ? C38 C39 H39A 108.5 . . ? C38 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? H39A C39 C40 108.5 . . ? H39B C39 C40 108.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 H41A 108.0 . . ? N3 C41 H41B 108.0 . . ? H41A C41 H41B 107.3 . . ? H41A C41 C42 108.0 . . ? H41B C41 C42 108.0 . . ? C41 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? H42A C42 C43 109.4 . . ? H42B C42 C43 109.4 . . ? C42 C43 H43A 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? H43A C43 C44 108.8 . . ? H43B C43 C44 108.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 H45A 107.8 . . ? N3 C45 H45B 107.8 . . ? H45A C45 H45B 107.1 . . ? H45A C45 C46 107.8 . . ? H45B C45 C46 107.8 . . ? C45 C46 H46A 109.7 . . ? C45 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? H46A C46 C47 109.7 . . ? H46B C46 C47 109.7 . . ? C46 C47 H47A 109.0 . . ? C46 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? H47A C47 C48 109.0 . . ? H47B C47 C48 109.0 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.796 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.175 # Contents of RES file _computing_special_details ; TITL PM166 (RJE422) in I2/a CELL 0.6393 23.8622 14.4740 49.226 90.000 95.462 90.000 ZERR 8.00 0.0017 0.0017 0.004 0.000 0.007 0.000 LATT 2 SYMM 0.5-X, Y, -Z SFAC C H N O P V MO DISP P 0.08539 0.07631 274.94 DISP V 0.27018 0.43544 1568.86 DISP Mo -2.88896 0.56746 2044.55 UNIT 400 888 32 336 8 16 96 TEMP -153 SIZE 0.02 0.03 0.10 OMIT 16 1 13 OMIT -16 10 26 SIMU $N $C DELU $N $C L.S. 20 CONN $MO 6 CONN $V 5 ACTA BOND FMAP 2 PLAN 10 REM EXTI 0.000052 WGHT 0.042900 FVAR 0.01628 0.49751 MO1 7 0.691872 0.076687 0.442009 11.00000 0.02922 0.03260 = 0.02400 -0.00080 -0.00157 0.00257 MO2 7 0.740146 -0.073302 0.388993 11.00000 0.02551 0.02782 = 0.03220 0.00268 0.00208 0.00341 MO3 7 0.773698 0.117762 0.354195 11.00000 0.02347 0.03053 = 0.02920 0.00044 0.00296 -0.00120 MO4 7 0.681322 -0.056054 0.322929 11.00000 0.02624 0.03024 = 0.02914 -0.00520 0.00247 -0.00061 MO5 7 0.569945 0.132266 0.302585 11.00000 0.02541 0.03400 = 0.02525 0.00285 -0.00053 -0.00075 MO6 7 0.535240 -0.072780 0.341040 11.00000 0.02570 0.03266 = 0.02752 -0.00046 0.00004 -0.00390 MO7 7 0.488529 0.066679 0.389623 11.00000 0.02331 0.04329 = 0.02999 0.00108 0.00357 0.00221 MO8 7 0.660959 0.304000 0.336242 11.00000 0.03256 0.02729 = 0.03032 0.00304 -0.00033 0.00044 MO9 7 0.588957 0.252134 0.423159 11.00000 0.03372 0.03557 = 0.02905 -0.00556 0.00363 0.00695 MO10 7 0.593917 -0.106606 0.406342 11.00000 0.02609 0.03144 = 0.02836 0.00397 0.00280 -0.00100 MO11 7 0.724864 0.268317 0.406898 11.00000 0.03120 0.02808 = 0.02846 -0.00344 -0.00096 0.00013 MO12 7 0.526017 0.272117 0.351830 11.00000 0.03133 0.03649 = 0.03430 0.00354 0.00133 0.01013 V1 6 0.563729 0.055006 0.443877 11.00000 0.03434 0.04970 = 0.03009 0.00056 0.00691 0.00309 V2 6 0.698092 0.142337 0.300630 11.00000 0.03216 0.04186 = 0.02899 0.00206 0.00431 -0.00323 P1 5 0.631585 0.098640 0.372261 11.00000 0.02597 0.02684 = 0.02593 0.00040 0.00185 0.00084 O1 4 0.423571 0.071488 0.399724 11.00000 0.03557 0.05480 = 0.04813 -0.00072 0.00747 0.00157 O2 4 0.536974 0.036737 0.472044 11.00000 0.04018 0.05704 = 0.03878 -0.00106 0.00921 -0.00189 O3 4 0.724991 0.161599 0.272745 11.00000 0.04982 0.05289 = 0.02458 0.01001 0.00634 -0.00114 O4 4 0.692944 -0.121481 0.296087 11.00000 0.04232 0.04414 = 0.03823 -0.00976 0.00612 0.00261 O5 4 0.534938 0.031621 0.317963 11.00000 0.02778 0.04179 = 0.03432 0.00278 0.00337 -0.00327 O6 4 0.782658 -0.157164 0.401396 11.00000 0.03975 0.02851 = 0.04739 0.00999 0.00561 0.00770 O7 4 0.474686 0.350097 0.348894 11.00000 0.03841 0.05262 = 0.05179 0.00469 -0.00071 0.02008 O8 4 0.771006 0.351115 0.416589 11.00000 0.04185 0.03543 = 0.05009 -0.00363 -0.00208 -0.00087 O9 4 0.555805 0.316544 0.444945 11.00000 0.04568 0.05667 = 0.04538 -0.00811 0.00924 0.00936 O10 4 0.526781 -0.029120 0.415389 11.00000 0.02961 0.04597 = 0.02909 0.00076 0.00785 -0.00049 O11 4 0.544801 0.128815 0.269668 11.00000 0.04283 0.04919 = 0.03531 0.00136 -0.00169 -0.00445 O12 4 0.656783 0.311503 0.423569 11.00000 0.04622 0.03565 = 0.03781 -0.00286 0.00509 0.00715 O13 4 0.589712 0.345896 0.339987 11.00000 0.03886 0.03330 = 0.04544 0.00436 -0.00244 0.01025 O14 4 0.649439 0.149192 0.399006 11.00000 0.03039 0.03015 = 0.03386 -0.00187 0.00185 0.00464 O15 4 0.491456 0.166782 0.366483 11.00000 0.02998 0.04722 = 0.04021 0.00278 -0.00069 0.00217 O16 4 0.555632 -0.147500 0.374591 11.00000 0.03034 0.03709 = 0.03801 0.00620 0.00406 0.00126 O17 4 0.560825 0.290286 0.389226 11.00000 0.03949 0.04111 = 0.03708 0.00183 0.00022 0.00616 O18 4 0.682905 0.047283 0.363080 11.00000 0.03260 0.03090 = 0.02526 0.00024 0.00455 0.00404 O19 4 0.723404 0.211350 0.332924 11.00000 0.03267 0.03743 = 0.03081 0.00197 0.00199 -0.00006 O20 4 0.498737 -0.148854 0.321174 11.00000 0.03484 0.04313 = 0.04158 -0.00145 -0.00135 -0.00849 O21 4 0.584614 0.029419 0.376385 11.00000 0.03017 0.03037 = 0.02898 -0.00163 -0.00026 0.00081 O22 4 0.522677 0.219362 0.316429 11.00000 0.02991 0.04715 = 0.03693 0.00319 0.00113 0.00495 O23 4 0.687391 0.315239 0.371972 11.00000 0.03403 0.03259 = 0.03625 0.00581 -0.00297 0.00084 O24 4 0.716987 0.046871 0.473381 11.00000 0.05171 0.05362 = 0.03179 0.00491 -0.00505 -0.00512 O25 4 0.688817 0.395665 0.321195 11.00000 0.05968 0.03148 = 0.03606 0.00943 -0.00364 -0.00641 O26 4 0.723174 -0.115638 0.350778 11.00000 0.03621 0.03291 = 0.03389 -0.00187 0.00130 -0.00193 O27 4 0.664978 -0.120653 0.395563 11.00000 0.03309 0.03397 = 0.04188 -0.00290 0.00459 -0.00298 O28 4 0.532532 0.146096 0.418329 11.00000 0.03332 0.05004 = 0.03501 0.00518 0.00328 0.00258 O29 4 0.733557 0.184020 0.436727 11.00000 0.03000 0.03740 = 0.03472 -0.00352 -0.00254 0.00048 O30 4 0.790741 0.010549 0.374279 11.00000 0.02574 0.03295 = 0.03350 -0.00266 0.00223 0.00229 O31 4 0.836364 0.146648 0.344447 11.00000 0.02842 0.04125 = 0.03752 -0.00275 0.00487 -0.00383 O32 4 0.612824 -0.094476 0.332104 11.00000 0.03329 0.02557 = 0.04215 0.00165 0.00436 -0.00092 O33 4 0.632841 0.226584 0.302901 11.00000 0.03124 0.03800 = 0.03363 -0.00057 -0.00037 -0.00174 O34 4 0.627906 -0.014371 0.434091 11.00000 0.03473 0.04277 = 0.03673 -0.00340 0.00774 -0.00046 O35 4 0.622773 0.152338 0.449287 11.00000 0.03994 0.03787 = 0.03054 -0.00130 0.00533 0.00414 O36 4 0.732392 0.004290 0.419313 11.00000 0.02501 0.04356 = 0.03626 0.00581 0.00143 -0.00066 O37 4 0.587150 -0.197324 0.427273 11.00000 0.04124 0.04376 = 0.03514 0.01322 0.00354 -0.00537 O38 4 0.479230 -0.021028 0.361538 11.00000 0.02642 0.04174 = 0.03751 0.00482 -0.00123 0.00064 O39 4 0.766203 0.191198 0.384767 11.00000 0.02971 0.03602 = 0.03652 -0.00007 0.00302 -0.00028 O40 4 0.608977 0.167902 0.350399 11.00000 0.03298 0.03510 = 0.02690 0.00354 -0.00069 0.00154 O41 4 0.741310 0.042536 0.321379 11.00000 0.03423 0.03294 = 0.02788 -0.00091 0.00292 -0.00414 O42 4 0.639336 0.050918 0.303018 11.00000 0.03430 0.04239 = 0.02755 0.00106 0.00260 -0.00474 SAME N2 > C32 SAME N3 > C48 SAME N2 > C31 C32A SAME N1 C5 > C16 C1 > C4 SAME N1 C13 > C16 C9 > C12 C5 > C8 C1 > C4 N1 3 0.323189 1.097915 0.110580 11.00000 0.05418 0.03855 = 0.11469 0.00367 0.01420 -0.00866 C1 1 0.350296 1.156705 0.133533 11.00000 0.05605 0.03771 = 0.10146 0.02267 -0.00338 -0.00581 AFIX 23 H1A 2 0.320524 1.194034 0.140968 11.00000 -1.20000 H1B 2 0.376595 1.200191 0.125805 11.00000 -1.20000 AFIX 0 C2 1 0.382245 1.105372 0.156967 11.00000 0.05690 0.05259 = 0.11715 0.02706 0.00029 0.00608 AFIX 23 H2A 2 0.355474 1.067982 0.166536 11.00000 -1.20000 H2B 2 0.409502 1.062639 0.149646 11.00000 -1.20000 AFIX 0 C3 1 0.413003 1.169789 0.176816 11.00000 0.05810 0.07001 = 0.14675 0.04032 -0.03711 -0.02585 AFIX 23 H3A 2 0.432820 1.216015 0.166404 11.00000 -1.20000 H3B 2 0.384922 1.203435 0.186610 11.00000 -1.20000 AFIX 0 C4 1 0.454848 1.126899 0.197486 11.00000 0.05881 0.10590 = 0.13126 0.06003 -0.01177 -0.01956 AFIX 33 H4A 2 0.469926 1.174195 0.210429 11.00000 -1.50000 H4B 2 0.485642 1.099946 0.188290 11.00000 -1.50000 H4C 2 0.436470 1.078373 0.207320 11.00000 -1.50000 AFIX 0 C5 1 0.366968 1.034128 0.099334 11.00000 0.09719 0.04052 = 0.20362 -0.00982 0.03751 0.01394 AFIX 23 H5A 2 0.385284 0.996625 0.114489 11.00000 -1.20000 H5B 2 0.347455 0.991238 0.085913 11.00000 -1.20000 AFIX 0 C6 1 0.411375 1.085559 0.085911 11.00000 0.10969 0.11742 = 0.21640 -0.01119 0.07829 0.00164 AFIX 23 H6A 2 0.424962 1.135843 0.098491 11.00000 -1.20000 H6B 2 0.392471 1.115455 0.069419 11.00000 -1.20000 AFIX 0 C7 1 0.462402 1.037210 0.077356 11.00000 0.08798 0.07252 = 0.30911 -0.00906 0.02959 0.01885 AFIX 23 H7A 2 0.450561 0.987433 0.064255 11.00000 -1.20000 H7B 2 0.485717 1.081632 0.068073 11.00000 -1.20000 AFIX 0 C8 1 0.494814 0.998848 0.100298 11.00000 0.14043 0.10165 = 0.29793 -0.05147 -0.03199 -0.00946 AFIX 33 H8A 2 0.534181 0.993550 0.096365 11.00000 -1.50000 H8B 2 0.480203 0.937469 0.104197 11.00000 -1.50000 H8C 2 0.492431 1.039045 0.116166 11.00000 -1.50000 AFIX 0 C9 1 0.297179 1.163860 0.089015 11.00000 0.06298 0.04194 = 0.07414 -0.01427 0.01915 0.00068 AFIX 23 H9A 2 0.268289 1.200922 0.097240 11.00000 -1.20000 H9B 2 0.326872 1.207072 0.084242 11.00000 -1.20000 AFIX 0 C10 1 0.270129 1.121724 0.062838 11.00000 0.06565 0.06368 = 0.11227 -0.03768 0.00541 -0.00794 AFIX 23 H10A 2 0.241816 1.075350 0.067177 11.00000 -1.20000 H10B 2 0.299170 1.089837 0.053215 11.00000 -1.20000 AFIX 0 C11 1 0.241829 1.195922 0.044371 11.00000 0.06489 0.09355 = 0.06997 -0.03745 -0.00193 -0.02254 AFIX 23 H11A 2 0.223378 1.165842 0.027804 11.00000 -1.20000 H11B 2 0.212004 1.225633 0.053996 11.00000 -1.20000 AFIX 0 C12 1 0.280403 1.268897 0.035855 11.00000 0.11665 0.16896 = 0.05076 0.00129 -0.01513 -0.07426 AFIX 33 H12A 2 0.261248 1.304958 0.020883 11.00000 -1.50000 H12B 2 0.314160 1.240068 0.029723 11.00000 -1.50000 H12C 2 0.291218 1.309748 0.051348 11.00000 -1.50000 AFIX 0 C13 1 0.279473 1.034718 0.121442 11.00000 0.06830 0.05742 = 0.10319 0.00179 0.00225 -0.02092 AFIX 23 H13A 2 0.262761 0.996453 0.106081 11.00000 -1.20000 H13B 2 0.299317 0.992272 0.134888 11.00000 -1.20000 AFIX 0 C14 1 0.232146 1.079362 0.134707 11.00000 0.05543 0.08462 = 0.07444 0.01876 -0.00887 -0.01138 AFIX 23 H14A 2 0.212681 1.125191 0.122205 11.00000 -1.20000 H14B 2 0.246943 1.111510 0.151643 11.00000 -1.20000 AFIX 0 C15 1 0.191226 1.002794 0.141287 11.00000 0.05374 0.08487 = 0.09763 0.02233 -0.00172 -0.00080 AFIX 23 H15A 2 0.178889 0.968573 0.124354 11.00000 -1.20000 H15B 2 0.210983 0.958764 0.154280 11.00000 -1.20000 AFIX 0 C16 1 0.141905 1.039152 0.153053 11.00000 0.06966 0.08259 = 0.13182 0.01076 0.02177 0.00676 AFIX 33 H16A 2 0.121878 0.988435 0.161105 11.00000 -1.50000 H16B 2 0.116854 1.068979 0.138733 11.00000 -1.50000 H16C 2 0.153844 1.084470 0.167227 11.00000 -1.50000 AFIX 0 N2 3 0.616400 0.432077 0.236875 11.00000 0.03419 0.04640 = 0.03754 0.00134 0.00331 0.00950 PART 0 C17 1 0.626010 0.469814 0.208890 11.00000 0.03571 0.05760 = 0.04738 0.00313 0.00679 0.00626 AFIX 23 H17A 2 0.664329 0.451657 0.204823 11.00000 -1.20000 H17B 2 0.599042 0.439171 0.195239 11.00000 -1.20000 AFIX 0 C18 1 0.620292 0.572959 0.204909 11.00000 0.04482 0.04867 = 0.05690 0.00592 -0.00857 0.01154 AFIX 23 H18A 2 0.581312 0.591873 0.207551 11.00000 -1.20000 H18B 2 0.646024 0.604983 0.218810 11.00000 -1.20000 AFIX 0 C19 1 0.633832 0.601626 0.176945 11.00000 0.06509 0.06972 = 0.05259 0.01923 -0.02423 -0.02722 AFIX 23 H19A 2 0.669448 0.571063 0.173265 11.00000 -1.20000 H19B 2 0.603913 0.577198 0.163546 11.00000 -1.20000 AFIX 0 C20 1 0.639666 0.700492 0.171751 11.00000 0.04379 0.06521 = 0.09584 0.02682 -0.00749 -0.01080 AFIX 33 H20A 2 0.647734 0.709925 0.152797 11.00000 -1.50000 H20B 2 0.670605 0.725614 0.184082 11.00000 -1.50000 H20C 2 0.604568 0.732182 0.174892 11.00000 -1.50000 AFIX 0 C21 1 0.553950 0.436635 0.240872 11.00000 0.03839 0.05489 = 0.05106 0.00532 0.00758 0.01527 AFIX 23 H21A 2 0.542977 0.502573 0.241098 11.00000 -1.20000 H21B 2 0.532880 0.408208 0.224693 11.00000 -1.20000 AFIX 0 C22 1 0.534673 0.391811 0.265769 11.00000 0.05072 0.06187 = 0.05529 0.00286 0.01568 0.01159 AFIX 23 H22A 2 0.556132 0.418117 0.282168 11.00000 -1.20000 H22B 2 0.543099 0.324890 0.265287 11.00000 -1.20000 AFIX 0 C23 1 0.472224 0.404707 0.268145 11.00000 0.04642 0.08137 = 0.07361 0.01439 0.02308 0.01437 AFIX 23 H23A 2 0.464235 0.388949 0.286963 11.00000 -1.20000 H23B 2 0.462607 0.470649 0.265057 11.00000 -1.20000 AFIX 0 C24 1 0.436014 0.348589 0.248947 11.00000 0.07716 0.19183 = 0.11700 0.00866 -0.03138 -0.02242 AFIX 33 H24A 2 0.397410 0.349650 0.254181 11.00000 -1.50000 H24B 2 0.449853 0.284811 0.249320 11.00000 -1.50000 H24C 2 0.436545 0.373747 0.230490 11.00000 -1.50000 AFIX 0 C25 1 0.635852 0.330481 0.238078 11.00000 0.03735 0.05752 = 0.04968 -0.00130 0.00527 0.01029 AFIX 23 H25A 2 0.675670 0.328227 0.234013 11.00000 -1.20000 H25B 2 0.634376 0.307799 0.256970 11.00000 -1.20000 AFIX 0 C26 1 0.602243 0.265028 0.218880 11.00000 0.04877 0.05235 = 0.04740 0.00542 0.00592 -0.00712 AFIX 23 H26A 2 0.599605 0.291039 0.200202 11.00000 -1.20000 H26B 2 0.563555 0.260134 0.224435 11.00000 -1.20000 AFIX 0 C27 1 0.627987 0.168425 0.218446 11.00000 0.03893 0.05448 = 0.04435 0.00457 0.00223 -0.00401 AFIX 23 H27A 2 0.637271 0.147204 0.237461 11.00000 -1.20000 H27B 2 0.599712 0.125334 0.209540 11.00000 -1.20000 AFIX 0 C28 1 0.679776 0.164675 0.203811 11.00000 0.05930 0.04513 = 0.05127 -0.00050 0.01088 -0.00091 AFIX 33 H28A 2 0.689730 0.100063 0.200758 11.00000 -1.50000 H28B 2 0.710789 0.195162 0.214835 11.00000 -1.50000 H28C 2 0.672882 0.196332 0.186212 11.00000 -1.50000 AFIX 0 C29 1 0.649364 0.486650 0.259178 11.00000 0.05735 0.05275 = 0.03682 0.00172 -0.00386 -0.00479 AFIX 23 H29A 2 0.631983 0.548605 0.259882 11.00000 -1.20000 H29B 2 0.644818 0.455854 0.276791 11.00000 -1.20000 AFIX 0 C30 1 0.710713 0.499412 0.257043 11.00000 0.05461 0.06081 = 0.05677 0.00436 -0.00252 0.00080 AFIX 23 H30A 2 0.716603 0.521236 0.238468 11.00000 -1.20000 H30B 2 0.730186 0.439335 0.259975 11.00000 -1.20000 AFIX 0 C31 1 0.736242 0.569621 0.278163 11.00000 0.06701 0.06368 = 0.05416 0.00398 -0.01249 -0.01793 PART 1 AFIX 23 H31A 2 0.711817 0.624997 0.277698 21.00000 -1.20000 H31B 2 0.736921 0.542105 0.296604 21.00000 -1.20000 AFIX 23 PART 2 H31C 2 0.721575 0.556669 0.295922 -21.00000 -1.20000 H31D 2 0.777564 0.560850 0.280543 -21.00000 -1.20000 AFIX 0 PART 1 C32 1 0.793330 0.597907 0.273416 21.00000 0.07818 0.05544 = 0.05437 -0.00077 0.01161 -0.01116 AFIX 33 H32A 2 0.810060 0.632892 0.289199 21.00000 -1.50000 H32B 2 0.791964 0.636801 0.257070 21.00000 -1.50000 H32C 2 0.816223 0.542985 0.270797 21.00000 -1.50000 AFIX 0 PART 2 C32A 1 0.724298 0.665355 0.270869 -21.00000 0.07542 0.05768 = 0.14756 -0.00882 -0.01271 0.02053 AFIX 33 H32D 2 0.749451 0.705895 0.282371 -21.00000 -1.50000 H32E 2 0.685105 0.679593 0.273657 -21.00000 -1.50000 H32F 2 0.730281 0.675155 0.251659 -21.00000 -1.50000 AFIX 0 N3 3 0.582872 0.297535 0.040321 11.00000 0.03727 0.04647 = 0.03790 0.00212 0.01070 0.01035 C33 1 0.576814 0.401852 0.041378 11.00000 0.04691 0.04800 = 0.04720 -0.00267 0.00164 0.01291 AFIX 23 H33A 2 0.564372 0.424436 0.022795 11.00000 -1.20000 H33B 2 0.546837 0.417064 0.053231 11.00000 -1.20000 AFIX 0 C34 1 0.629363 0.452878 0.051710 11.00000 0.06211 0.04503 = 0.11038 -0.02678 0.00495 0.00562 AFIX 23 H34A 2 0.662306 0.423932 0.044323 11.00000 -1.20000 H34B 2 0.634752 0.448716 0.071863 11.00000 -1.20000 AFIX 0 C35 1 0.625513 0.554195 0.043140 11.00000 0.06120 0.05161 = 0.09825 -0.00986 0.01665 0.00158 AFIX 23 H35A 2 0.586137 0.575256 0.043576 11.00000 -1.20000 H35B 2 0.649329 0.591404 0.056596 11.00000 -1.20000 AFIX 0 C36 1 0.642912 0.571474 0.016218 11.00000 0.08422 0.13213 = 0.10212 0.01054 0.02957 0.02653 AFIX 33 H36A 2 0.610614 0.593393 0.004149 11.00000 -1.50000 H36B 2 0.657326 0.514195 0.008863 11.00000 -1.50000 H36C 2 0.672574 0.618531 0.017417 11.00000 -1.50000 AFIX 0 C37 1 0.622671 0.271164 0.019314 11.00000 0.04637 0.05066 = 0.04805 0.00369 0.01603 0.00876 AFIX 23 H37A 2 0.661143 0.290739 0.026256 11.00000 -1.20000 H37B 2 0.611939 0.306693 0.002432 11.00000 -1.20000 AFIX 0 C38 1 0.624581 0.168928 0.011844 11.00000 0.04548 0.05890 = 0.04823 -0.01381 0.00814 0.00535 AFIX 23 H38A 2 0.627725 0.131097 0.028675 11.00000 -1.20000 H38B 2 0.589329 0.151492 0.000793 11.00000 -1.20000 AFIX 0 C39 1 0.674269 0.150144 -0.004145 11.00000 0.04949 0.07124 = 0.05382 -0.00870 0.01291 0.01546 AFIX 23 H39A 2 0.672989 0.193971 -0.019632 11.00000 -1.20000 H39B 2 0.709246 0.162664 0.007767 11.00000 -1.20000 AFIX 0 C40 1 0.677146 0.054918 -0.014975 11.00000 0.08064 0.09409 = 0.08376 -0.04903 0.00937 0.02052 AFIX 33 H40A 2 0.710752 0.048564 -0.024820 11.00000 -1.50000 H40B 2 0.643491 0.042452 -0.027444 11.00000 -1.50000 H40C 2 0.679097 0.010757 0.000177 11.00000 -1.50000 AFIX 0 C41 1 0.524676 0.254993 0.033155 11.00000 0.03983 0.05978 = 0.04954 0.00536 0.00691 -0.00113 AFIX 23 H41A 2 0.528280 0.187083 0.034976 11.00000 -1.20000 H41B 2 0.499753 0.276074 0.046885 11.00000 -1.20000 AFIX 0 C42 1 0.495894 0.275887 0.005215 11.00000 0.04827 0.07009 = 0.04333 -0.00164 0.00413 0.00702 AFIX 23 H42A 2 0.522420 0.264450 -0.008704 11.00000 -1.20000 H42B 2 0.485058 0.341914 0.004240 11.00000 -1.20000 AFIX 0 C43 1 0.443692 0.216351 -0.000973 11.00000 0.05085 0.09932 = 0.06138 0.00960 -0.00929 -0.00095 AFIX 23 H43A 2 0.419769 0.221891 0.014311 11.00000 -1.20000 H43B 2 0.421881 0.240399 -0.017590 11.00000 -1.20000 AFIX 0 C44 1 0.456287 0.116804 -0.005176 11.00000 0.10210 0.09092 = 0.08574 -0.00990 0.00706 -0.03454 AFIX 33 H44A 2 0.420945 0.082464 -0.008691 11.00000 -1.50000 H44B 2 0.477693 0.092192 0.011215 11.00000 -1.50000 H44C 2 0.478505 0.110295 -0.020816 11.00000 -1.50000 AFIX 0 C45 1 0.607196 0.258763 0.067607 11.00000 0.05328 0.06644 = 0.03643 0.00181 0.00300 0.01582 AFIX 23 H45A 2 0.644652 0.287221 0.072121 11.00000 -1.20000 H45B 2 0.613296 0.191709 0.065226 11.00000 -1.20000 AFIX 0 C46 1 0.573453 0.271364 0.092167 11.00000 0.06776 0.05548 = 0.03851 -0.00224 0.00703 0.01494 AFIX 23 H46A 2 0.576928 0.335960 0.098724 11.00000 -1.20000 H46B 2 0.533165 0.258656 0.086764 11.00000 -1.20000 AFIX 0 C47 1 0.595170 0.206028 0.114833 11.00000 0.05677 0.05697 = 0.03726 -0.00207 0.00149 -0.00438 AFIX 23 H47A 2 0.592629 0.141817 0.107896 11.00000 -1.20000 H47B 2 0.635348 0.219713 0.120206 11.00000 -1.20000 AFIX 0 C48 1 0.563265 0.213316 0.139308 11.00000 0.06385 0.06651 = 0.04509 0.01202 0.01484 0.00648 AFIX 33 H48A 2 0.577517 0.167452 0.152896 11.00000 -1.50000 H48B 2 0.523234 0.201887 0.134013 11.00000 -1.50000 H48C 2 0.568046 0.275407 0.147126 11.00000 -1.50000 AFIX 0 N4 3 0.630022 0.947091 0.068131 11.00000 0.11796 0.14425 = 0.14629 0.01807 0.01256 -0.04633 C49 1 0.611938 0.877703 0.075107 11.00000 0.08302 0.12165 = 0.09757 0.00802 0.02128 -0.01596 C50 1 0.590718 0.788642 0.085098 11.00000 0.09271 0.11850 = 0.10415 -0.00512 0.00430 -0.02707 AFIX 33 H50A 2 0.562990 0.800799 0.098120 11.00000 -1.50000 H50B 2 0.622184 0.753224 0.094121 11.00000 -1.50000 H50C 2 0.572982 0.753157 0.069643 11.00000 -1.50000 HKLF 4 REM PM166 (RJE422) in I2/a REM R1 = 0.0588 for 11207 Fo > 4sig(Fo) and 0.1175 for all 20469 data REM 1010 parameters refined using 980 restraints END ; #===END data_rje419_salt_of_3 _database_code_depnum_ccdc_archive 'CCDC 857418' #TrackingRef '- cc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C16 H36 N +,Mo12 O40 P Sb2 3-' _chemical_formula_sum 'C48 H108 Mo12 N3 O40 P Sb2' _chemical_formula_weight 2793.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 26.922(10) _cell_length_b 14.066(4) _cell_length_c 11.8345(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.447(16) _cell_angle_gamma 90.00 _cell_volume 4453(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27116 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2716 _exptl_absorpt_coefficient_mu 2.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.457 _exptl_absorpt_correction_T_max 0.543 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27110 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9548 _reflns_number_gt 8182 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+58.2558P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(5) _refine_ls_number_reflns 9548 _refine_ls_number_parameters 461 _refine_ls_number_restraints 326 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.46501(2) 0.55874(17) 0.19499(5) 0.0490(3) Uani 1 1 d . . . Mo2 Mo 0.41903(4) 0.38044(8) 0.35898(11) 0.0368(3) Uani 1 1 d . . . Mo3 Mo 0.54784(4) 0.37665(8) 0.33850(11) 0.0383(3) Uani 1 1 d . . . Mo4 Mo 0.632197(15) 0.56783(11) 0.48229(4) 0.02280(12) Uani 1 1 d . . . Mo5 Mo 0.55025(4) 0.75404(8) 0.34119(13) 0.0433(4) Uani 1 1 d . . . Mo6 Mo 0.58198(4) 0.75011(8) 0.63794(13) 0.0427(4) Uani 1 1 d . . . Sb Sb 0.587416(14) 0.56278(11) 0.21179(3) 0.03759(14) Uani 1 1 d . . . P P 0.5000 0.5675(4) 0.5000 0.0140(3) Uani 1 2 d S . . O1 O 0.45271(18) 0.5573(15) 0.0540(4) 0.073(3) Uani 1 1 d . . . O2 O 0.4246(4) 0.4591(11) 0.2294(12) 0.089(5) Uani 1 1 d . . . O3 O 0.3802(4) 0.2994(9) 0.3009(12) 0.077(4) Uani 1 1 d . . . O4 O 0.4827(2) 0.3217(6) 0.3147(7) 0.052(2) Uani 1 1 d . . . O5 O 0.5740(5) 0.2904(10) 0.2686(14) 0.087(5) Uani 1 1 d . . . O6 O 0.5606(2) 0.3470(5) 0.4817(7) 0.0427(18) Uani 1 1 d . . . O7 O 0.5271(4) 0.4689(9) 0.2168(12) 0.069(4) Uani 1 1 d . . . O8 O 0.5265(3) 0.6449(9) 0.2157(10) 0.060(3) Uani 1 1 d . . . O9 O 0.6088(4) 0.6561(7) 0.3430(8) 0.044(2) Uani 1 1 d . . . O10 O 0.5996(4) 0.4820(7) 0.3579(7) 0.040(2) Uani 1 1 d . . . O11 O 0.4866(2) 0.7788(6) 0.3600(7) 0.0462(18) Uani 1 1 d . . . O12 O 0.5748(4) 0.8311(8) 0.2571(12) 0.066(4) Uani 1 1 d . . . O13 O 0.6257(5) 0.4751(9) 0.5856(9) 0.062(3) Uani 1 1 d . . . O14 O 0.69307(15) 0.5620(10) 0.4626(4) 0.0405(14) Uani 1 1 d . . . O15 O 0.5789(3) 0.8055(5) 0.4856(7) 0.0447(19) Uani 1 1 d . . . O16 O 0.6311(5) 0.6681(8) 0.5830(8) 0.057(3) Uani 1 1 d . . . O17 O 0.5720(4) 0.6505(11) 0.7511(12) 0.076(4) Uani 1 1 d . . . O18 O 0.6169(4) 0.8359(10) 0.7033(15) 0.099(6) Uani 1 1 d . . . O19 O 0.54636(17) 0.6253(4) 0.4887(4) 0.0234(11) Uani 1 1 d . . . O20 O 0.48946(17) 0.4977(4) 0.3932(4) 0.0226(10) Uani 1 1 d . . . N1 N 0.7345(3) 0.8491(6) 0.3416(7) 0.0625(14) Uani 1 1 d DU . . C1 C 0.6842(3) 0.8921(7) 0.3521(10) 0.0630(18) Uani 1 1 d DU A . H1A H 0.6651 0.8476 0.3954 0.076 Uiso 1 1 calc R . . H1B H 0.6661 0.8982 0.2750 0.076 Uiso 1 1 calc R . . C2 C 0.6849(3) 0.9884(8) 0.4094(12) 0.069(2) Uani 1 1 d DU . . H2A H 0.7079 1.0314 0.3741 0.082 Uiso 0.69(2) 1 calc PR A -1 H2B H 0.6974 0.9816 0.4909 0.082 Uiso 0.69(2) 1 calc PR A -1 H2C H 0.7034 1.0343 0.3663 0.082 Uiso 0.31(2) 1 calc PR A -2 H2D H 0.7025 0.9835 0.4873 0.082 Uiso 0.31(2) 1 calc PR A -2 C3 C 0.6318(4) 1.0320(11) 0.398(2) 0.071(2) Uani 0.69(2) 1 d PDU A -1 H3A H 0.6200 1.0410 0.3161 0.085 Uiso 0.69(2) 1 calc PR A -1 H3B H 0.6087 0.9871 0.4295 0.085 Uiso 0.69(2) 1 calc PR A -1 C4 C 0.6301(6) 1.1248(12) 0.4573(18) 0.074(3) Uani 0.69(2) 1 d PDU A -1 H4A H 0.5960 1.1502 0.4459 0.110 Uiso 0.69(2) 1 calc PR A -1 H4B H 0.6530 1.1695 0.4265 0.110 Uiso 0.69(2) 1 calc PR A -1 H4C H 0.6402 1.1157 0.5387 0.110 Uiso 0.69(2) 1 calc PR A -1 C5 C 0.7665(5) 0.9100(10) 0.2740(10) 0.073(2) Uani 1 1 d DU B . H5A H 0.7986 0.8767 0.2693 0.088 Uiso 1 1 calc R . . H5B H 0.7741 0.9701 0.3159 0.088 Uiso 1 1 calc R . . C6 C 0.7439(5) 0.9341(11) 0.1544(10) 0.091(2) Uani 1 1 d DU . . H6A H 0.7184 0.9846 0.1564 0.109 Uiso 0.683(16) 1 calc PR B -1 H6B H 0.7276 0.8773 0.1173 0.109 Uiso 0.683(16) 1 calc PR B -1 H6C H 0.7082 0.9508 0.1552 0.109 Uiso 0.317(16) 1 calc PR B -2 H6D H 0.7458 0.8779 0.1047 0.109 Uiso 0.317(16) 1 calc PR B -2 C7 C 0.7872(7) 0.9690(16) 0.0872(14) 0.096(3) Uani 0.683(16) 1 d PDU B -1 H7A H 0.8154 0.9238 0.1002 0.115 Uiso 0.683(16) 1 calc PR B -1 H7B H 0.7754 0.9684 0.0049 0.115 Uiso 0.683(16) 1 calc PR B -1 C8 C 0.8055(7) 1.0659(17) 0.1195(17) 0.108(4) Uani 0.683(16) 1 d PDU B -1 H8A H 0.8334 1.0822 0.0768 0.162 Uiso 0.683(16) 1 calc PR B -1 H8B H 0.8167 1.0676 0.2012 0.162 Uiso 0.683(16) 1 calc PR B -1 H8C H 0.7783 1.1119 0.1020 0.162 Uiso 0.683(16) 1 calc PR B -1 C9 C 0.7239(4) 0.7540(8) 0.2873(12) 0.0627(19) Uani 1 1 d DU . . H9A H 0.7042 0.7641 0.2124 0.075 Uiso 1 1 calc R . . H9B H 0.7026 0.7176 0.3348 0.075 Uiso 1 1 calc R . . C10 C 0.7692(3) 0.6934(7) 0.2696(11) 0.065(2) Uani 1 1 d DU B . H10A H 0.7901 0.6852 0.3433 0.078 Uiso 1 1 calc R . . H10B H 0.7896 0.7269 0.2173 0.078 Uiso 1 1 calc R . . C11 C 0.7543(4) 0.5948(7) 0.2200(11) 0.072(2) Uani 1 1 d DU . . H11A H 0.7399 0.5568 0.2788 0.087 Uiso 0.683(16) 1 calc PR B -1 H11B H 0.7279 0.6030 0.1553 0.087 Uiso 0.683(16) 1 calc PR B -1 H11C H 0.7282 0.5677 0.2632 0.087 Uiso 0.317(16) 1 calc PR B -2 H11D H 0.7393 0.6029 0.1402 0.087 Uiso 0.317(16) 1 calc PR B -2 C12 C 0.7966(6) 0.5411(13) 0.1803(17) 0.082(4) Uani 0.683(16) 1 d PDU B -1 H12A H 0.7842 0.4816 0.1445 0.123 Uiso 0.683(16) 1 calc PR B -1 H12B H 0.8213 0.5268 0.2453 0.123 Uiso 0.683(16) 1 calc PR B -1 H12C H 0.8122 0.5795 0.1250 0.123 Uiso 0.683(16) 1 calc PR B -1 C13 C 0.7650(5) 0.8401(11) 0.4554(10) 0.0579(17) Uani 1 1 d DU . . H13A H 0.7722 0.9045 0.4868 0.069 Uiso 1 1 calc R . . H13B H 0.7974 0.8099 0.4447 0.069 Uiso 1 1 calc R . . C14 C 0.7397(5) 0.7823(11) 0.5406(10) 0.0580(18) Uani 1 1 d DU C . H14A H 0.7377 0.7149 0.5164 0.070 Uiso 1 1 calc R . . H14B H 0.7052 0.8060 0.5435 0.070 Uiso 1 1 calc R . . C15 C 0.7693(5) 0.7897(9) 0.6597(10) 0.062(2) Uani 1 1 d DU . . H15A H 0.8031 0.7626 0.6570 0.074 Uiso 0.60(2) 1 calc PR C -1 H15B H 0.7733 0.8576 0.6809 0.074 Uiso 0.60(2) 1 calc PR C -1 H15C H 0.7541 0.7457 0.7112 0.074 Uiso 0.40(2) 1 calc PR C -2 H15D H 0.8039 0.7674 0.6543 0.074 Uiso 0.40(2) 1 calc PR C -2 C16 C 0.7444(8) 0.7390(15) 0.7486(14) 0.063(4) Uani 0.60(2) 1 d PDU C -1 H16A H 0.7647 0.7453 0.8222 0.094 Uiso 0.60(2) 1 calc PR C -1 H16B H 0.7407 0.6716 0.7285 0.094 Uiso 0.60(2) 1 calc PR C -1 H16C H 0.7113 0.7668 0.7533 0.094 Uiso 0.60(2) 1 calc PR C -1 C3A C 0.6310(6) 1.025(2) 0.415(3) 0.071(3) Uani 0.31(2) 1 d PDU A -2 H3C H 0.6125 0.9775 0.4558 0.085 Uiso 0.31(2) 1 calc PR A -2 H3D H 0.6324 1.0847 0.4592 0.085 Uiso 0.31(2) 1 calc PR A -2 C4A C 0.6034(10) 1.042(3) 0.301(3) 0.078(4) Uani 0.31(2) 1 d PDU A -2 H4D H 0.5687 1.0589 0.3095 0.117 Uiso 0.31(2) 1 calc PR A -2 H4E H 0.6040 0.9844 0.2548 0.117 Uiso 0.31(2) 1 calc PR A -2 H4F H 0.6192 1.0944 0.2638 0.117 Uiso 0.31(2) 1 calc PR A -2 C7A C 0.7718(11) 1.018(2) 0.106(3) 0.095(3) Uani 0.317(16) 1 d PDU B -2 H7C H 0.7916 1.0516 0.1699 0.114 Uiso 0.317(16) 1 calc PR B -2 H7D H 0.7955 0.9932 0.0553 0.114 Uiso 0.317(16) 1 calc PR B -2 C8A C 0.7383(16) 1.088(2) 0.042(4) 0.103(6) Uani 0.317(16) 1 d PDU B -2 H8D H 0.7584 1.1376 0.0101 0.155 Uiso 0.317(16) 1 calc PR B -2 H8E H 0.7166 1.1178 0.0930 0.155 Uiso 0.317(16) 1 calc PR B -2 H8F H 0.7177 1.0559 -0.0201 0.155 Uiso 0.317(16) 1 calc PR B -2 C12A C 0.7961(9) 0.5259(18) 0.222(4) 0.079(4) Uani 0.317(16) 1 d PDU B -2 H12D H 0.7838 0.4657 0.1881 0.118 Uiso 0.317(16) 1 calc PR B -2 H12E H 0.8102 0.5147 0.3013 0.118 Uiso 0.317(16) 1 calc PR B -2 H12F H 0.8221 0.5516 0.1793 0.118 Uiso 0.317(16) 1 calc PR B -2 C16A C 0.7721(11) 0.8849(16) 0.712(2) 0.062(5) Uani 0.40(2) 1 d PDU C -2 H16D H 0.7916 0.8815 0.7870 0.093 Uiso 0.40(2) 1 calc PR C -2 H16E H 0.7382 0.9074 0.7206 0.093 Uiso 0.40(2) 1 calc PR C -2 H16F H 0.7882 0.9291 0.6635 0.093 Uiso 0.40(2) 1 calc PR C -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 0.0160(2) 0.1130(8) 0.0182(2) -0.0014(8) 0.00227(17) -0.0039(7) Mo2 0.0221(5) 0.0414(7) 0.0482(8) -0.0231(6) 0.0096(5) -0.0147(4) Mo3 0.0301(6) 0.0374(7) 0.0509(8) -0.0148(5) 0.0197(5) 0.0031(5) Mo4 0.01212(18) 0.0323(3) 0.0243(2) 0.0039(5) 0.00361(15) -0.0031(5) Mo5 0.0300(6) 0.0318(6) 0.0702(10) 0.0253(6) 0.0148(6) -0.0058(5) Mo6 0.0211(5) 0.0426(7) 0.0634(10) -0.0245(6) 0.0006(5) -0.0087(5) Sb 0.01734(17) 0.0745(4) 0.02211(18) 0.0021(5) 0.00741(13) -0.0024(5) P 0.0096(7) 0.0157(9) 0.0168(8) 0.000 0.0012(6) 0.000 O1 0.027(2) 0.169(9) 0.023(2) -0.010(7) 0.0007(19) -0.025(7) O2 0.018(4) 0.151(13) 0.103(9) 0.056(8) 0.019(5) 0.005(5) O3 0.048(6) 0.073(9) 0.106(10) -0.059(7) -0.009(6) 0.003(5) O4 0.027(3) 0.068(6) 0.063(5) -0.037(4) 0.016(3) -0.006(3) O5 0.070(8) 0.075(9) 0.123(12) -0.058(8) 0.046(8) -0.030(6) O6 0.035(4) 0.017(4) 0.077(5) 0.010(3) 0.007(3) 0.009(3) O7 0.021(4) 0.083(8) 0.105(10) 0.036(6) 0.012(5) 0.010(4) O8 0.019(4) 0.089(8) 0.071(7) -0.028(6) 0.001(4) 0.008(4) O9 0.059(5) 0.042(5) 0.029(4) 0.011(3) 0.002(3) 0.014(4) O10 0.055(4) 0.038(5) 0.025(4) 0.000(3) -0.003(3) -0.013(3) O11 0.029(3) 0.050(5) 0.060(5) 0.020(4) 0.008(3) 0.002(3) O12 0.065(7) 0.042(6) 0.098(9) 0.040(6) 0.042(6) -0.004(5) O13 0.086(8) 0.058(7) 0.039(6) 0.009(5) -0.002(5) -0.017(6) O14 0.0179(18) 0.071(4) 0.034(2) 0.021(6) 0.0069(16) 0.007(5) O15 0.039(4) 0.017(4) 0.077(5) 0.001(3) -0.002(4) -0.006(3) O16 0.101(8) 0.044(6) 0.025(5) -0.007(4) 0.005(5) 0.040(5) O17 0.023(4) 0.113(9) 0.094(8) 0.037(7) 0.015(5) 0.015(5) O18 0.034(5) 0.083(10) 0.180(15) -0.082(10) 0.006(7) -0.028(6) O19 0.015(2) 0.025(3) 0.031(3) -0.001(2) 0.0060(18) -0.0033(19) O20 0.018(2) 0.033(3) 0.018(2) -0.006(2) 0.0058(17) -0.0043(19) N1 0.045(3) 0.069(3) 0.074(3) -0.002(3) 0.006(3) -0.011(3) C1 0.041(3) 0.065(4) 0.083(4) -0.004(4) 0.006(3) -0.008(3) C2 0.043(3) 0.067(4) 0.096(5) -0.005(4) 0.006(4) -0.004(3) C3 0.046(4) 0.066(5) 0.099(6) -0.005(5) 0.007(4) 0.000(4) C4 0.050(6) 0.064(6) 0.105(8) -0.006(6) 0.001(6) 0.000(5) C5 0.057(4) 0.082(5) 0.083(4) 0.012(4) 0.010(3) -0.012(4) C6 0.079(5) 0.104(6) 0.088(4) 0.020(5) 0.005(4) -0.008(5) C7 0.085(6) 0.111(7) 0.090(5) 0.025(5) 0.008(5) -0.009(6) C8 0.088(7) 0.128(8) 0.105(8) 0.021(8) -0.001(7) -0.023(7) C9 0.045(3) 0.073(4) 0.071(4) -0.011(3) 0.010(3) -0.010(3) C10 0.045(4) 0.078(4) 0.075(4) -0.009(4) 0.017(4) -0.010(3) C11 0.061(4) 0.081(5) 0.078(5) -0.013(4) 0.021(4) -0.004(4) C12 0.075(6) 0.093(8) 0.082(8) -0.015(7) 0.029(6) 0.004(6) C13 0.047(3) 0.061(4) 0.065(3) -0.005(3) 0.004(3) -0.017(3) C14 0.053(4) 0.060(4) 0.059(3) -0.012(3) -0.001(3) -0.028(3) C15 0.061(5) 0.065(5) 0.058(3) -0.009(4) 0.003(4) -0.027(4) C16 0.067(8) 0.057(9) 0.065(6) 0.005(7) 0.011(7) -0.004(7) C3A 0.046(4) 0.066(5) 0.100(6) -0.005(5) 0.006(4) -0.001(4) C4A 0.057(7) 0.069(8) 0.106(8) -0.003(8) 0.000(6) 0.008(7) C7A 0.085(6) 0.108(7) 0.091(5) 0.024(5) 0.005(5) -0.010(6) C8A 0.098(11) 0.109(10) 0.100(11) 0.025(9) -0.004(10) -0.009(9) C12A 0.071(7) 0.087(7) 0.080(9) -0.012(8) 0.024(8) 0.003(6) C16A 0.060(9) 0.063(8) 0.061(8) -0.011(7) 0.003(8) -0.047(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.664(5) . ? Mo1 O2 1.847(13) . ? Mo1 O7 2.089(11) . ? Mo1 O8 2.044(11) . ? Mo1 O17 1.790(13) 2_656 ? Mo1 O20 2.515(5) . ? Mo2 O2 1.910(13) . ? Mo2 O3 1.645(11) . ? Mo2 O4 2.024(7) . ? Mo2 O6 1.961(9) 2_656 ? Mo2 O13 1.957(12) 2_656 ? Mo2 O20 2.512(5) . ? Mo3 O4 1.910(7) . ? Mo3 O5 1.668(12) . ? Mo3 O6 1.741(8) . ? Mo3 O7 1.972(12) . ? Mo3 O10 2.031(9) . ? Mo3 O20 2.453(5) . ? Mo4 O9 2.103(9) . ? Mo4 O10 2.025(9) . ? Mo4 O13 1.810(11) . ? Mo4 O14 1.683(4) . ? Mo4 O16 1.849(9) . ? Mo4 O19 2.458(5) . ? Mo5 O8 2.181(11) . ? Mo5 O9 2.091(10) . ? Mo5 O11 1.787(7) . ? Mo5 O12 1.659(9) . ? Mo5 O15 1.935(8) . ? Mo6 O11 1.893(7) 2_656 ? Mo6 O15 1.957(8) . ? Mo6 O16 1.923(10) . ? Mo6 O17 1.978(13) . ? Mo6 O18 1.666(10) . ? Sb O7 2.098(11) . ? Sb O8 2.012(10) . ? Sb O9 2.065(10) . ? Sb O10 2.064(9) . ? P O19 1.508(6) . ? P O19 1.508(6) 2_656 ? P O20 1.600(6) . ? P O20 1.600(6) 2_656 ? O6 Mo2 1.961(9) 2_656 ? O11 Mo6 1.893(7) 2_656 ? O13 Mo2 1.957(12) 2_656 ? O17 Mo1 1.790(13) 2_656 ? N1 C1 1.499(8) . ? N1 C5 1.508(9) . ? N1 C9 1.498(9) . ? N1 C13 1.502(9) . ? C1 C2 1.514(10) . ? C2 C3 1.549(11) . ? C2 C3A 1.548(11) . ? C3 C4 1.486(12) . ? C5 C6 1.515(10) . ? C6 C7 1.563(11) . ? C6 C7A 1.548(11) . ? C7 C8 1.485(13) . ? C9 C10 1.522(10) . ? C10 C11 1.543(10) . ? C11 C12 1.487(12) . ? C11 C12A 1.485(12) . ? C13 C14 1.516(9) . ? C14 C15 1.543(10) . ? C15 C16 1.492(12) . ? C15 C16A 1.474(12) . ? C3A C4A 1.485(13) . ? C7A C8A 1.486(13) . ? C1 H1A 0.990 . ? C1 H1B 0.990 . ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C2 H2C 0.990 . ? C2 H2D 0.990 . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.990 . ? C5 H5B 0.990 . ? C6 H6A 0.990 . ? C6 H6B 0.990 . ? C6 H6C 0.990 . ? C6 H6D 0.990 . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 H11C 0.990 . ? C11 H11D 0.990 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 H15C 0.990 . ? C15 H15D 0.990 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C3A H3C 0.990 . ? C3A H3D 0.990 . ? C4A H4D 0.980 . ? C4A H4E 0.980 . ? C4A H4F 0.980 . ? C7A H7C 0.990 . ? C7A H7D 0.990 . ? C8A H8D 0.980 . ? C8A H8E 0.980 . ? C8A H8F 0.980 . ? C12A H12D 0.980 . ? C12A H12E 0.980 . ? C12A H12F 0.980 . ? C16A H16D 0.980 . ? C16A H16E 0.980 . ? C16A H16F 0.980 . ? 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 99.0(7) . . ? O1 Mo1 O7 100.5(7) . . ? O1 Mo1 O8 101.2(6) . . ? O1 Mo1 O17 108.0(7) . 2_656 ? O1 Mo1 O20 158.9(8) . . ? O2 Mo1 O7 89.8(5) . . ? O2 Mo1 O8 155.8(5) . . ? O2 Mo1 O17 96.0(4) . 2_656 ? O2 Mo1 O20 68.6(4) . . ? O7 Mo1 O8 73.6(3) . . ? O7 Mo1 O17 149.5(6) . 2_656 ? O7 Mo1 O20 63.7(4) . . ? O8 Mo1 O17 90.3(5) . 2_656 ? O8 Mo1 O20 88.1(4) . . ? O17 Mo1 O20 90.7(5) 2_656 . ? O2 Mo2 O3 99.8(7) . . ? O2 Mo2 O4 83.3(4) . . ? O2 Mo2 O6 150.7(5) . 2_656 ? O2 Mo2 O13 89.0(6) . 2_656 ? O2 Mo2 O20 67.9(4) . . ? O3 Mo2 O4 97.2(5) . . ? O3 Mo2 O6 109.4(6) . 2_656 ? O3 Mo2 O13 103.0(6) . 2_656 ? O3 Mo2 O20 162.9(5) . . ? O4 Mo2 O6 89.9(3) . 2_656 ? O4 Mo2 O13 159.3(5) . 2_656 ? O4 Mo2 O20 70.4(2) . . ? O6 Mo2 O13 87.5(4) 2_656 2_656 ? O6 Mo2 O20 83.0(2) 2_656 . ? O13 Mo2 O20 88.9(4) 2_656 . ? O4 Mo3 O5 93.7(5) . . ? O4 Mo3 O6 97.1(4) . . ? O4 Mo3 O7 88.8(4) . . ? O4 Mo3 O10 157.0(4) . . ? O4 Mo3 O20 73.4(3) . . ? O5 Mo3 O6 105.1(7) . . ? O5 Mo3 O7 102.5(7) . . ? O5 Mo3 O10 105.3(5) . . ? O5 Mo3 O20 162.7(6) . . ? O6 Mo3 O7 151.3(5) . . ? O6 Mo3 O10 90.4(4) . . ? O6 Mo3 O20 88.4(3) . . ? O7 Mo3 O10 74.7(4) . . ? O7 Mo3 O20 66.4(4) . . ? O10 Mo3 O20 85.2(3) . . ? O9 Mo4 O10 73.4(2) . . ? O9 Mo4 O13 155.7(5) . . ? O9 Mo4 O14 97.5(4) . . ? O9 Mo4 O16 91.7(4) . . ? O9 Mo4 O19 68.3(3) . . ? O10 Mo4 O13 89.7(5) . . ? O10 Mo4 O14 102.7(5) . . ? O10 Mo4 O16 152.4(5) . . ? O10 Mo4 O19 83.5(3) . . ? O13 Mo4 O14 103.2(6) . . ? O13 Mo4 O16 96.0(3) . . ? O13 Mo4 O19 93.0(5) . . ? O14 Mo4 O16 102.2(6) . . ? O14 Mo4 O19 162.5(4) . . ? O16 Mo4 O19 69.3(4) . . ? O8 Mo5 O9 72.9(4) . . ? O8 Mo5 O11 90.6(4) . . ? O8 Mo5 O12 99.1(6) . . ? O8 Mo5 O15 157.2(4) . . ? O9 Mo5 O11 149.2(4) . . ? O9 Mo5 O12 94.9(5) . . ? O9 Mo5 O15 90.7(4) . . ? O11 Mo5 O12 113.6(5) . . ? O11 Mo5 O15 96.3(4) . . ? O12 Mo5 O15 98.0(6) . . ? O11 Mo6 O15 89.2(3) 2_656 . ? O11 Mo6 O16 147.3(4) 2_656 . ? O11 Mo6 O17 86.3(4) 2_656 . ? O11 Mo6 O18 109.9(5) 2_656 . ? O15 Mo6 O16 83.5(4) . . ? O15 Mo6 O17 155.6(5) . . ? O15 Mo6 O18 95.9(7) . . ? O16 Mo6 O17 87.4(5) . . ? O16 Mo6 O18 102.6(6) . . ? O17 Mo6 O18 108.2(8) . . ? O7 Sb O8 74.1(3) . . ? O7 Sb O9 122.0(5) . . ? O7 Sb O10 71.4(4) . . ? O8 Sb O9 77.1(4) . . ? O8 Sb O10 110.5(5) . . ? O9 Sb O10 73.5(2) . . ? O19 P O19 114.8(6) . 2_656 ? O19 P O20 109.6(3) . . ? O19 P O20 109.0(3) . 2_656 ? O19 P O20 109.6(3) 2_656 2_656 ? O19 P O20 109.0(3) 2_656 . ? O20 P O20 104.3(5) . 2_656 ? Mo1 O2 Mo2 135.9(8) . . ? Mo2 O4 Mo3 125.9(4) . . ? Mo2 O6 Mo3 151.9(4) 2_656 . ? Mo1 O7 Mo3 130.2(6) . . ? Mo1 O7 Sb 103.1(6) . . ? Mo3 O7 Sb 106.2(5) . . ? Mo1 O8 Mo5 132.2(5) . . ? Mo1 O8 Sb 107.9(6) . . ? Mo5 O8 Sb 104.0(4) . . ? Mo4 O9 Mo5 123.8(4) . . ? Mo4 O9 Sb 104.3(4) . . ? Mo5 O9 Sb 105.4(4) . . ? Mo3 O10 Mo4 138.8(5) . . ? Mo3 O10 Sb 105.3(4) . . ? Mo4 O10 Sb 107.2(4) . . ? Mo5 O11 Mo6 155.6(5) . 2_656 ? Mo2 O13 Mo4 145.8(7) 2_656 . ? Mo5 O15 Mo6 129.5(4) . . ? Mo4 O16 Mo6 137.4(8) . . ? Mo1 O17 Mo6 151.1(7) 2_656 . ? Mo4 O19 P 128.0(4) . . ? Mo1 O20 Mo2 87.70(15) . . ? Mo1 O20 Mo3 95.68(16) . . ? Mo1 O20 P 122.1(3) . . ? Mo2 O20 Mo3 89.76(18) . . ? Mo2 O20 P 126.5(2) . . ? Mo3 O20 P 124.9(3) . . ? C1 N1 C5 112.9(7) . . ? C1 N1 C9 105.4(7) . . ? C1 N1 C13 111.6(7) . . ? C5 N1 C9 111.8(8) . . ? C5 N1 C13 103.6(7) . . ? C9 N1 C13 111.6(7) . . ? N1 C1 C2 115.6(7) . . ? C1 C2 C3 110.5(8) . . ? C1 C2 C3A 110.5(11) . . ? C2 C3 C4 112.5(10) . . ? N1 C5 C6 115.4(8) . . ? C5 C6 C7 107.5(9) . . ? C5 C6 C7A 110.8(11) . . ? C6 C7 C8 113.7(11) . . ? N1 C9 C10 116.2(8) . . ? C9 C10 C11 112.1(7) . . ? C10 C11 C12 113.6(9) . . ? C10 C11 C12A 114.5(12) . . ? N1 C13 C14 113.5(7) . . ? C13 C14 C15 110.2(7) . . ? C14 C15 C16 112.6(9) . . ? C14 C15 C16A 116.3(11) . . ? C2 C3A C4A 113.0(12) . . ? C6 C7A C8A 113.8(13) . . ? N1 C1 H1A 108.4 . . ? N1 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? H1A C1 C2 108.4 . . ? H1B C1 C2 108.4 . . ? C1 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C1 C2 H2C 109.5 . . ? C1 C2 H2D 109.5 . . ? H2A C2 H2B 108.1 . . ? H2A C2 C3 109.6 . . ? H2B C2 C3 109.6 . . ? H2C C2 H2D 108.1 . . ? H2C C2 C3A 109.5 . . ? H2D C2 C3A 109.5 . . ? C2 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? H3A C3 C4 109.1 . . ? H3B C3 C4 109.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 108.4 . . ? N1 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? H5A C5 C6 108.4 . . ? H5B C5 C6 108.4 . . ? C5 C6 H6A 110.2 . . ? C5 C6 H6B 110.2 . . ? C5 C6 H6C 109.5 . . ? C5 C6 H6D 109.5 . . ? H6A C6 H6B 108.5 . . ? H6A C6 C7 110.2 . . ? H6B C6 C7 110.2 . . ? H6C C6 H6D 108.1 . . ? H6C C6 C7A 109.5 . . ? H6D C6 C7A 109.5 . . ? C6 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? H7A C7 C8 108.9 . . ? H7B C7 C8 108.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 108.2 . . ? N1 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? H9A C9 C10 108.2 . . ? H9B C9 C10 108.2 . . ? C9 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? H10A C10 C11 109.2 . . ? H10B C10 C11 109.2 . . ? C10 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? C10 C11 H11C 108.6 . . ? C10 C11 H11D 108.6 . . ? H11A C11 H11B 107.7 . . ? H11A C11 C12 108.8 . . ? H11B C11 C12 108.9 . . ? H11C C11 H11D 107.6 . . ? H11C C11 C12A 108.6 . . ? H11D C11 C12A 108.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 H13A 108.9 . . ? N1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? H13A C13 C14 108.9 . . ? H13B C13 C14 108.9 . . ? C13 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? H14A C14 C15 109.6 . . ? H14B C14 C15 109.6 . . ? C14 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C14 C15 H15C 108.2 . . ? C14 C15 H15D 108.2 . . ? H15A C15 H15B 107.8 . . ? H15A C15 C16 109.1 . . ? H15B C15 H15C 119.1 . . ? H15B C15 C16 109.1 . . ? H15C C15 H15D 107.4 . . ? H15C C15 C16A 108.2 . . ? H15D C15 C16A 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C3A H3C 109.0 . . ? C2 C3A H3D 109.0 . . ? H3C C3A H3D 107.8 . . ? H3C C3A C4A 109.0 . . ? H3D C3A C4A 109.0 . . ? C3A C4A H4D 109.5 . . ? C3A C4A H4E 109.5 . . ? C3A C4A H4F 109.5 . . ? H4D C4A H4E 109.5 . . ? H4D C4A H4F 109.5 . . ? H4E C4A H4F 109.5 . . ? C6 C7A H7C 108.8 . . ? C6 C7A H7D 108.8 . . ? H7C C7A H7D 107.7 . . ? H7C C7A C8A 108.8 . . ? H7D C7A C8A 108.8 . . ? C7A C8A H8D 109.5 . . ? C7A C8A H8E 109.5 . . ? C7A C8A H8F 109.5 . . ? H8D C8A H8E 109.5 . . ? H8D C8A H8F 109.5 . . ? H8E C8A H8F 109.5 . . ? C11 C12A H12D 109.5 . . ? C11 C12A H12E 109.5 . . ? C11 C12A H12F 109.5 . . ? H12D C12A H12E 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C15 C16A H16D 109.5 . . ? C15 C16A H16E 109.5 . . ? C15 C16A H16F 109.5 . . ? H16D C16A H16E 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.022 _refine_diff_density_min -1.387 _refine_diff_density_rms 0.148 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.546 -0.008 585 89 ' ' 2 0.500 1.046 0.029 585 89 ' ' _platon_squeeze_details ; ; # Contents of RES file _computing_special_details ; TITL rje419 in C2 CELL 0.71073 26.922 14.066 11.8345 90.000 96.447 90.000 ZERR 2.00 0.010 0.004 0.0011 0.000 0.016 0.000 LATT -7 SYMM -X, Y, -Z SFAC C H N O P MO SB UNIT 96 216 6 80 2 24 4 TEMP -123 SIZE 0.4 0.35 0.3 OMIT -4 0 4 L.S. 8 ACTA 50 BOND FMAP 2 PLAN 10 FREE MO3 SB REM DELU $MO SB $O DELU 0.005 $C $N SIMU 0.005 $C $N TWIN WGHT 0.035300 58.255802 EXTI 0.000145 BASF 0.46571 FVAR 0.40627 0.59608 0.68258 0.68993 MO1 6 0.465005 0.558738 0.194994 11.00000 0.01598 0.11298 = 0.01825 -0.00144 0.00227 -0.00390 MO2 6 0.419028 0.380444 0.358975 11.00000 0.02210 0.04137 = 0.04819 -0.02311 0.00961 -0.01475 MO3 6 0.547842 0.376650 0.338501 11.00000 0.03007 0.03741 = 0.05095 -0.01477 0.01965 0.00311 MO4 6 0.632197 0.567833 0.482286 11.00000 0.01212 0.03231 = 0.02434 0.00391 0.00361 -0.00311 MO5 6 0.550246 0.754041 0.341189 11.00000 0.02995 0.03179 = 0.07019 0.02534 0.01482 -0.00577 MO6 6 0.581975 0.750115 0.637937 11.00000 0.02112 0.04259 = 0.06340 -0.02448 0.00062 -0.00874 SB 7 0.587416 0.562780 0.211793 11.00000 0.01734 0.07449 = 0.02211 0.00207 0.00741 -0.00236 P 5 0.500000 0.567545 0.500000 10.50000 0.00955 0.01567 = 0.01685 0.00000 0.00124 0.00000 O1 4 0.452706 0.557295 0.054025 11.00000 0.02668 0.16864 = 0.02282 -0.00981 0.00068 -0.02450 O2 4 0.424634 0.459066 0.229389 11.00000 0.01791 0.15072 = 0.10258 0.05610 0.01931 0.00528 O3 4 0.380170 0.299400 0.300926 11.00000 0.04791 0.07256 = 0.10621 -0.05917 -0.00862 0.00293 O4 4 0.482651 0.321656 0.314653 11.00000 0.02749 0.06823 = 0.06253 -0.03670 0.01625 -0.00553 O5 4 0.574029 0.290410 0.268621 11.00000 0.06969 0.07548 = 0.12290 -0.05764 0.04566 -0.02951 O6 4 0.560594 0.347038 0.481674 11.00000 0.03511 0.01655 = 0.07654 0.00980 0.00709 0.00883 O7 4 0.527128 0.468888 0.216764 11.00000 0.02120 0.08318 = 0.10508 0.03624 0.01206 0.01002 O8 4 0.526470 0.644939 0.215745 11.00000 0.01878 0.08924 = 0.07055 -0.02804 0.00099 0.00806 O9 4 0.608775 0.656117 0.342993 11.00000 0.05868 0.04226 = 0.02915 0.01148 0.00246 0.01379 O10 4 0.599645 0.482040 0.357881 11.00000 0.05496 0.03843 = 0.02475 0.00048 -0.00292 -0.01306 O11 4 0.486605 0.778753 0.360039 11.00000 0.02907 0.04984 = 0.06025 0.01977 0.00807 0.00166 O12 4 0.574839 0.831093 0.257095 11.00000 0.06511 0.04230 = 0.09831 0.04016 0.04180 -0.00389 O13 4 0.625664 0.475106 0.585597 11.00000 0.08554 0.05770 = 0.03938 0.00861 -0.00205 -0.01729 O14 4 0.693065 0.562041 0.462633 11.00000 0.01788 0.07104 = 0.03360 0.02114 0.00694 0.00748 O15 4 0.578897 0.805508 0.485589 11.00000 0.03906 0.01662 = 0.07666 0.00128 -0.00174 -0.00580 O16 4 0.631123 0.668112 0.583040 11.00000 0.10130 0.04421 = 0.02495 -0.00744 0.00481 0.03998 O17 4 0.571986 0.650467 0.751127 11.00000 0.02293 0.11311 = 0.09371 0.03658 0.01463 0.01532 O18 4 0.616885 0.835949 0.703306 11.00000 0.03357 0.08292 = 0.18048 -0.08188 0.00634 -0.02841 O19 4 0.546363 0.625333 0.488728 11.00000 0.01496 0.02461 = 0.03133 -0.00110 0.00605 -0.00330 O20 4 0.489457 0.497732 0.393226 11.00000 0.01815 0.03311 = 0.01754 -0.00616 0.00578 -0.00426 SAME 0.01 N1 C5 > C16 C1 > C4 SAME 0.01 N1 C13 > C16 C9 > C12 C5 > C8 C1 > C4 SAME 0.01 N1 > C2 C3A C4A C5 C6 C7A C8A C9 > C11 C12A C13 > C15 C16A N1 3 0.734471 0.849105 0.341638 11.00000 0.04478 0.06888 = 0.07378 -0.00199 0.00600 -0.01082 C1 1 0.684249 0.892094 0.352125 11.00000 0.04133 0.06476 = 0.08277 -0.00418 0.00599 -0.00835 AFIX 23 H1A 2 0.665077 0.847585 0.395406 11.00000 -1.20000 H1B 2 0.666086 0.898187 0.274961 11.00000 -1.20000 AFIX 0 C2 1 0.684934 0.988429 0.409382 11.00000 0.04325 0.06685 = 0.09553 -0.00521 0.00582 -0.00382 PART -1 AFIX 23 H2A 2 0.707878 1.031436 0.374070 41.00000 -1.20000 H2B 2 0.697435 0.981586 0.490890 41.00000 -1.20000 AFIX 23 PART -2 H2C 2 0.703412 1.034295 0.366337 -41.00000 -1.20000 H2D 2 0.702462 0.983481 0.487300 -41.00000 -1.20000 AFIX 0 PART -1 C3 1 0.631763 1.032019 0.397744 41.00000 0.04634 0.06600 = 0.09897 -0.00454 0.00676 -0.00036 AFIX 23 H3A 2 0.620046 1.041005 0.316123 41.00000 -1.20000 H3B 2 0.608653 0.987070 0.429455 41.00000 -1.20000 AFIX 0 C4 1 0.630100 1.124758 0.457274 41.00000 0.05029 0.06400 = 0.10465 -0.00557 0.00076 -0.00039 AFIX 33 H4A 2 0.596022 1.150222 0.445891 41.00000 -1.50000 H4B 2 0.653029 1.169480 0.426451 41.00000 -1.50000 H4C 2 0.640152 1.115749 0.538748 41.00000 -1.50000 AFIX 0 PART 0 C5 1 0.766511 0.909991 0.273962 11.00000 0.05654 0.08151 = 0.08258 0.01215 0.01021 -0.01208 AFIX 23 H5A 2 0.798618 0.876708 0.269302 11.00000 -1.20000 H5B 2 0.774068 0.970093 0.315932 11.00000 -1.20000 AFIX 0 C6 1 0.743865 0.934080 0.154403 11.00000 0.07930 0.10394 = 0.08766 0.01990 0.00533 -0.00773 PART -1 AFIX 23 H6A 2 0.718377 0.984603 0.156413 31.00000 -1.20000 H6B 2 0.727614 0.877260 0.117272 31.00000 -1.20000 AFIX 23 PART -2 H6C 2 0.708185 0.950803 0.155186 -31.00000 -1.20000 H6D 2 0.745759 0.877855 0.104749 -31.00000 -1.20000 AFIX 0 PART -1 C7 1 0.787172 0.968986 0.087175 31.00000 0.08547 0.11146 = 0.09032 0.02510 0.00820 -0.00876 AFIX 23 H7A 2 0.815416 0.923774 0.100228 31.00000 -1.20000 H7B 2 0.775368 0.968354 0.004879 31.00000 -1.20000 AFIX 0 C8 1 0.805470 1.065883 0.119549 31.00000 0.08753 0.12791 = 0.10506 0.02102 -0.00084 -0.02316 AFIX 33 H8A 2 0.833415 1.082196 0.076777 31.00000 -1.50000 H8B 2 0.816728 1.067553 0.201201 31.00000 -1.50000 H8C 2 0.778344 1.111854 0.102036 31.00000 -1.50000 AFIX 0 PART 0 C9 1 0.723859 0.753987 0.287290 11.00000 0.04516 0.07261 = 0.07125 -0.01067 0.01043 -0.01030 AFIX 23 H9A 2 0.704235 0.764103 0.212381 11.00000 -1.20000 H9B 2 0.702573 0.717552 0.334835 11.00000 -1.20000 AFIX 0 C10 1 0.769221 0.693437 0.269607 11.00000 0.04537 0.07752 = 0.07491 -0.00924 0.01704 -0.00962 AFIX 23 H10A 2 0.790086 0.685222 0.343333 11.00000 -1.20000 H10B 2 0.789566 0.726880 0.217331 11.00000 -1.20000 AFIX 0 C11 1 0.754252 0.594771 0.219968 11.00000 0.06073 0.08095 = 0.07817 -0.01253 0.02094 -0.00351 PART -1 AFIX 23 H11A 2 0.739858 0.556849 0.278803 31.00000 -1.20000 H11B 2 0.727921 0.602999 0.155279 31.00000 -1.20000 AFIX 23 PART -2 H11C 2 0.728180 0.567679 0.263186 -31.00000 -1.20000 H11D 2 0.739346 0.602912 0.140207 -31.00000 -1.20000 AFIX 0 PART -1 C12 1 0.796598 0.541086 0.180293 31.00000 0.07516 0.09330 = 0.08240 -0.01482 0.02937 0.00399 AFIX 33 H12A 2 0.784154 0.481597 0.144455 31.00000 -1.50000 H12B 2 0.821308 0.526769 0.245322 31.00000 -1.50000 H12C 2 0.812244 0.579506 0.124951 31.00000 -1.50000 AFIX 0 PART 0 C13 1 0.765044 0.840089 0.455383 11.00000 0.04696 0.06103 = 0.06506 -0.00495 0.00359 -0.01744 AFIX 23 H13A 2 0.772169 0.904495 0.486846 11.00000 -1.20000 H13B 2 0.797410 0.809915 0.444701 11.00000 -1.20000 AFIX 0 C14 1 0.739698 0.782275 0.540604 11.00000 0.05341 0.05969 = 0.05939 -0.01175 -0.00087 -0.02810 AFIX 23 H14A 2 0.737653 0.714885 0.516395 11.00000 -1.20000 H14B 2 0.705249 0.806021 0.543524 11.00000 -1.20000 AFIX 0 C15 1 0.769338 0.789731 0.659678 11.00000 0.06111 0.06473 = 0.05850 -0.00924 0.00312 -0.02734 PART -1 AFIX 23 H15A 2 0.803125 0.762649 0.656953 21.00000 -1.20000 H15B 2 0.773297 0.857616 0.680879 21.00000 -1.20000 AFIX 23 PART -2 H15C 2 0.754093 0.745732 0.711241 -21.00000 -1.20000 H15D 2 0.803865 0.767392 0.654301 -21.00000 -1.20000 AFIX 0 PART -1 C16 1 0.744391 0.738993 0.748555 21.00000 0.06678 0.05685 = 0.06478 0.00543 0.01107 -0.00444 AFIX 33 H16A 2 0.764727 0.745273 0.822221 21.00000 -1.50000 H16B 2 0.740739 0.671557 0.728519 21.00000 -1.50000 H16C 2 0.711318 0.766817 0.753312 21.00000 -1.50000 AFIX 0 PART -2 C3A 1 0.631001 1.024832 0.415004 -41.00000 0.04628 0.06617 = 0.09957 -0.00478 0.00578 -0.00054 AFIX 23 H3C 2 0.612467 0.977497 0.455850 -41.00000 -1.20000 H3D 2 0.632353 1.084728 0.459174 -41.00000 -1.20000 AFIX 0 C4A 1 0.603393 1.042113 0.301092 -41.00000 0.05656 0.06898 = 0.10594 -0.00300 0.00009 0.00832 AFIX 33 H4D 2 0.568673 1.058922 0.309497 -41.00000 -1.50000 H4E 2 0.604036 0.984435 0.254828 -41.00000 -1.50000 H4F 2 0.619244 1.094389 0.263755 -41.00000 -1.50000 AFIX 0 C7A 1 0.771805 1.018422 0.106124 -31.00000 0.08484 0.10847 = 0.09064 0.02439 0.00524 -0.01016 AFIX 23 H7C 2 0.791591 1.051589 0.169861 -31.00000 -1.20000 H7D 2 0.795490 0.993182 0.055326 -31.00000 -1.20000 AFIX 0 C8A 1 0.738277 1.088373 0.041822 -31.00000 0.09758 0.10917 = 0.09952 0.02537 -0.00450 -0.00899 AFIX 33 H8D 2 0.758432 1.137583 0.010086 -31.00000 -1.50000 H8E 2 0.716552 1.117797 0.093039 -31.00000 -1.50000 H8F 2 0.717732 1.055874 -0.020071 -31.00000 -1.50000 AFIX 0 C12A 1 0.796129 0.525855 0.222393 -31.00000 0.07150 0.08728 = 0.08019 -0.01188 0.02354 0.00332 AFIX 33 H12D 2 0.783755 0.465732 0.188113 -31.00000 -1.50000 H12E 2 0.810158 0.514719 0.301318 -31.00000 -1.50000 H12F 2 0.822116 0.551624 0.179347 -31.00000 -1.50000 AFIX 0 C16A 1 0.772056 0.884885 0.712099 -21.00000 0.06029 0.06345 = 0.06062 -0.01135 0.00336 -0.04676 AFIX 33 H16D 2 0.791594 0.881525 0.787023 -21.00000 -1.50000 H16E 2 0.738220 0.907352 0.720601 -21.00000 -1.50000 H16F 2 0.788162 0.929061 0.663534 -21.00000 -1.50000 PART 0 HKLF 4 REM rje419 in C2 REM R1 = 0.0468 for 8182 Fo > 4sig(Fo) and 0.0585 for all 9548 data REM 461 parameters refined using 326 restraints END ; #===END