# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 888169' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 La Mo2 N2 O20' _chemical_formula_weight 866.09 _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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5065(12) _cell_length_b 20.537(3) _cell_length_c 15.485(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.114(3) _cell_angle_gamma 90.00 _cell_volume 2373.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1823 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.64 _exptl_crystal_description bar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 2.909 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3967 _exptl_absorpt_correction_T_max 0.7216 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11947 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4180 _reflns_number_gt 3831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0310P)^2^+3.2256P] 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 4180 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _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 La1 La 0.42936(3) 1.038975(10) 0.276286(13) 0.01584(8) Uani 1 1 d . . . Mo1 Mo 0.40188(4) 0.841402(14) 0.336102(19) 0.01255(9) Uani 1 1 d . . . Mo2 Mo -0.10276(4) 0.835536(15) 0.334862(19) 0.01430(9) Uani 1 1 d . . . O1 O 0.4411(3) 0.78839(13) 0.25605(16) 0.0237(6) Uani 1 1 d . . . O2 O 0.1718(3) 0.82455(14) 0.34687(17) 0.0237(6) Uani 1 1 d . . . O3 O 0.3944(4) 0.91903(13) 0.29066(17) 0.0247(6) Uani 1 1 d . . . O4 O -0.0814(4) 0.89803(14) 0.26182(18) 0.0287(7) Uani 1 1 d . . . O5 O -0.1452(4) 0.76732(13) 0.27285(17) 0.0247(6) Uani 1 1 d . . . O6 O -0.3191(3) 0.85247(13) 0.37080(17) 0.0222(6) Uani 1 1 d . . . O7 O 0.4143(3) 0.88532(12) 0.46860(16) 0.0203(6) Uani 1 1 d . . . O8 O 0.4886(4) 0.87385(14) 0.61079(17) 0.0319(7) Uani 1 1 d . . . O9 O 0.6967(5) 0.54997(14) 0.51002(19) 0.0404(8) Uani 1 1 d . . . O10 O 0.6114(4) 0.57644(13) 0.37362(16) 0.0277(7) Uani 1 1 d . . . O11 O -0.0215(3) 0.89230(13) 0.45699(17) 0.0222(6) Uani 1 1 d . . . O12 O 0.0382(4) 0.89481(14) 0.60041(18) 0.0325(7) Uani 1 1 d . . . O13 O 0.2099(5) 0.56010(16) 0.54555(19) 0.0451(9) Uani 1 1 d . . . O14 O 0.1077(5) 0.57487(15) 0.40768(19) 0.0392(8) Uani 1 1 d . . . N2 N -0.0252(4) 0.76451(15) 0.45104(19) 0.0169(6) Uani 1 1 d . . . N1 N 0.4794(4) 0.76221(14) 0.43761(18) 0.0137(6) Uani 1 1 d . . . C1 C 0.5158(5) 0.70057(17) 0.4182(2) 0.0160(7) Uani 1 1 d . . . H1A H 0.4909 0.6865 0.3611 0.019 Uiso 1 1 calc R . . C2 C 0.5894(5) 0.65681(17) 0.4800(2) 0.0162(8) Uani 1 1 d . . . C3 C 0.6257(5) 0.67793(19) 0.5657(2) 0.0224(8) Uani 1 1 d . . . H3A H 0.6751 0.6496 0.6086 0.027 Uiso 1 1 calc R . . C4 C 0.5869(5) 0.74174(18) 0.5859(2) 0.0206(8) Uani 1 1 d . . . H4A H 0.6094 0.7569 0.6426 0.025 Uiso 1 1 calc R . . C5 C 0.5147(5) 0.78235(17) 0.5206(2) 0.0147(7) Uani 1 1 d . . . C6 C 0.4704(5) 0.85293(18) 0.5354(2) 0.0167(8) Uani 1 1 d . . . C7 C 0.6363(5) 0.58917(18) 0.4526(2) 0.0190(8) Uani 1 1 d . . . C8 C 0.0041(5) 0.70137(18) 0.4401(2) 0.0206(8) Uani 1 1 d . . . H8A H -0.0333 0.6826 0.3866 0.025 Uiso 1 1 calc R . . C9 C 0.0885(5) 0.66221(18) 0.5055(2) 0.0207(8) Uani 1 1 d . . . C10 C 0.1345(6) 0.6894(2) 0.5865(3) 0.0266(9) Uani 1 1 d . . . H10A H 0.1853 0.6639 0.6323 0.032 Uiso 1 1 calc R . . C11 C 0.1039(6) 0.7553(2) 0.5986(3) 0.0262(9) Uani 1 1 d . . . H11A H 0.1337 0.7746 0.6525 0.031 Uiso 1 1 calc R . . C12 C 0.0282(5) 0.79152(18) 0.5290(2) 0.0180(8) Uani 1 1 d . . . C13 C 0.0130(5) 0.86518(19) 0.5297(2) 0.0208(8) Uani 1 1 d . . . C14 C 0.1344(5) 0.59419(19) 0.4822(2) 0.0231(8) Uani 1 1 d . . . O1W O 0.2575(5) 1.01250(16) 0.4103(2) 0.0433(8) Uani 1 1 d . . . O2W O 0.6846(4) 0.99548(15) 0.3843(2) 0.0374(8) Uani 1 1 d . . . O3W O 0.1137(4) 1.00472(15) 0.2201(2) 0.0354(7) Uani 1 1 d . . . O4W O 0.1902(4) 1.13448(14) 0.2678(2) 0.0348(7) Uani 1 1 d . . . O5W O 0.6434(4) 0.97688(14) 0.18574(18) 0.0306(7) Uani 1 1 d . . . O6W O 0.7102(4) 1.10997(15) 0.24830(18) 0.0321(7) Uani 1 1 d . . . _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 La1 0.02225(13) 0.01219(12) 0.01291(12) 0.00089(8) 0.00107(8) 0.00156(8) Mo1 0.01246(16) 0.01157(16) 0.01356(16) 0.00111(12) 0.00109(12) 0.00181(11) Mo2 0.01228(16) 0.01282(16) 0.01753(17) 0.00274(12) 0.00025(12) 0.00091(12) O1 0.0266(15) 0.0251(15) 0.0191(13) -0.0035(12) 0.0013(11) 0.0035(12) O2 0.0140(13) 0.0277(15) 0.0296(15) 0.0056(12) 0.0033(11) 0.0018(11) O3 0.0277(15) 0.0168(14) 0.0289(15) 0.0052(12) -0.0001(11) 0.0018(11) O4 0.0241(15) 0.0258(15) 0.0363(16) 0.0119(13) 0.0037(12) -0.0013(12) O5 0.0261(15) 0.0213(14) 0.0252(14) -0.0052(12) -0.0047(11) 0.0020(12) O6 0.0149(13) 0.0235(14) 0.0283(14) 0.0007(12) 0.0030(11) 0.0011(11) O7 0.0272(14) 0.0143(13) 0.0190(13) 0.0002(11) 0.0001(11) 0.0059(11) O8 0.054(2) 0.0203(15) 0.0201(15) -0.0072(12) -0.0005(13) 0.0062(14) O9 0.077(2) 0.0203(15) 0.0223(15) 0.0015(13) 0.0000(15) 0.0220(16) O10 0.0444(18) 0.0218(15) 0.0156(14) -0.0052(11) -0.0027(12) 0.0096(13) O11 0.0237(14) 0.0168(13) 0.0254(14) -0.0008(12) -0.0011(11) 0.0005(11) O12 0.0430(18) 0.0266(16) 0.0270(16) -0.0083(13) -0.0003(13) 0.0050(14) O13 0.079(3) 0.0281(17) 0.0257(16) 0.0022(14) -0.0058(16) 0.0268(17) O14 0.063(2) 0.0237(16) 0.0279(16) -0.0046(14) -0.0073(15) 0.0079(15) N2 0.0174(15) 0.0142(15) 0.0192(15) 0.0015(13) 0.0021(12) 0.0013(13) N1 0.0161(15) 0.0108(15) 0.0140(14) 0.0000(12) 0.0008(11) 0.0006(12) C1 0.0185(18) 0.0140(18) 0.0154(17) -0.0033(15) 0.0004(14) 0.0006(15) C2 0.0176(18) 0.0127(18) 0.0185(18) -0.0013(15) 0.0030(14) 0.0011(14) C3 0.034(2) 0.0180(19) 0.0152(18) 0.0043(16) 0.0007(16) 0.0048(17) C4 0.030(2) 0.0160(19) 0.0159(18) -0.0031(15) 0.0029(15) 0.0010(16) C5 0.0159(17) 0.0148(18) 0.0140(17) -0.0020(14) 0.0041(13) 0.0000(15) C6 0.0178(19) 0.0158(18) 0.0169(18) -0.0031(15) 0.0049(14) -0.0024(15) C7 0.0214(19) 0.0159(19) 0.0195(19) 0.0007(16) 0.0014(15) 0.0008(15) C8 0.024(2) 0.0170(19) 0.0210(19) -0.0004(16) 0.0008(15) -0.0020(16) C9 0.022(2) 0.019(2) 0.022(2) 0.0050(16) 0.0039(16) 0.0007(16) C10 0.034(2) 0.025(2) 0.0196(19) 0.0049(17) -0.0018(17) 0.0043(18) C11 0.034(2) 0.024(2) 0.0197(19) -0.0029(17) 0.0004(17) 0.0040(18) C12 0.0152(18) 0.0200(19) 0.0189(18) -0.0018(16) 0.0029(14) 0.0014(15) C13 0.0162(19) 0.021(2) 0.025(2) -0.0046(17) 0.0008(15) -0.0002(16) C14 0.031(2) 0.0159(19) 0.022(2) 0.0020(16) 0.0007(16) -0.0036(17) O1W 0.070(2) 0.0325(18) 0.0317(17) 0.0046(15) 0.0234(16) 0.0110(17) O2W 0.0455(19) 0.0247(16) 0.0384(17) -0.0009(14) -0.0120(14) 0.0074(14) O3W 0.0288(16) 0.0305(17) 0.0448(19) 0.0128(15) -0.0065(13) -0.0088(13) O4W 0.0400(18) 0.0219(15) 0.0415(17) -0.0005(14) 0.0004(14) 0.0094(14) O5W 0.0411(17) 0.0279(15) 0.0242(15) 0.0022(13) 0.0100(13) 0.0118(14) O6W 0.0357(17) 0.0308(16) 0.0296(16) -0.0036(13) 0.0031(13) -0.0075(14) _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. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O10 2.434(2) 2_655 ? La1 O3 2.490(3) . ? La1 O8 2.532(3) 3_676 ? La1 O3W 2.535(3) . ? La1 O2W 2.565(3) . ? La1 O5W 2.580(3) . ? La1 O1W 2.615(3) . ? La1 O6W 2.637(3) . ? La1 O4W 2.653(3) . ? Mo1 O1 1.699(3) . ? Mo1 O3 1.741(3) . ? Mo1 O2 1.786(3) . ? Mo1 O6 2.119(3) 1_655 ? Mo1 O7 2.234(2) . ? Mo1 N1 2.293(3) . ? Mo2 O5 1.709(3) . ? Mo2 O4 1.729(3) . ? Mo2 O6 1.805(3) . ? Mo2 O2 2.062(3) . ? Mo2 O11 2.250(3) . ? Mo2 N2 2.341(3) . ? O6 Mo1 2.119(3) 1_455 ? O7 C6 1.263(4) . ? O8 C6 1.238(4) . ? O8 La1 2.532(3) 3_676 ? O9 C7 1.249(5) . ? O10 C7 1.244(4) . ? O10 La1 2.434(2) 2_645 ? O11 C13 1.259(5) . ? O12 C13 1.249(5) . ? O13 C14 1.286(5) . ? O14 C14 1.217(5) . ? N2 C8 1.329(5) . ? N2 C12 1.350(5) . ? N1 C1 1.336(5) . ? N1 C5 1.350(4) . ? C1 C2 1.384(5) . ? C1 H1A 0.9300 . ? C2 C3 1.395(5) . ? C2 C7 1.506(5) . ? C3 C4 1.385(5) . ? C3 H3A 0.9300 . ? C4 C5 1.376(5) . ? C4 H4A 0.9300 . ? C5 C6 1.510(5) . ? C8 C9 1.391(5) . ? C8 H8A 0.9300 . ? C9 C10 1.383(6) . ? C9 C14 1.492(5) . ? C10 C11 1.389(6) . ? C10 H10A 0.9300 . ? C11 C12 1.381(5) . ? C11 H11A 0.9300 . ? C12 C13 1.517(5) . ? _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 O10 La1 O3 113.22(9) 2_655 . ? O10 La1 O8 115.58(9) 2_655 3_676 ? O3 La1 O8 131.14(9) . 3_676 ? O10 La1 O3W 75.09(10) 2_655 . ? O3 La1 O3W 69.66(9) . . ? O8 La1 O3W 125.64(11) 3_676 . ? O10 La1 O2W 137.81(11) 2_655 . ? O3 La1 O2W 71.08(9) . . ? O8 La1 O2W 71.72(10) 3_676 . ? O3W La1 O2W 137.12(10) . . ? O10 La1 O5W 70.13(10) 2_655 . ? O3 La1 O5W 68.73(9) . . ? O8 La1 O5W 127.24(10) 3_676 . ? O3W La1 O5W 106.86(10) . . ? O2W La1 O5W 73.56(10) . . ? O10 La1 O1W 143.16(11) 2_655 . ? O3 La1 O1W 69.98(10) . . ? O8 La1 O1W 72.73(10) 3_676 . ? O3W La1 O1W 72.08(11) . . ? O2W La1 O1W 78.91(11) . . ? O5W La1 O1W 135.82(10) . . ? O10 La1 O6W 71.93(9) 2_655 . ? O3 La1 O6W 130.96(9) . . ? O8 La1 O6W 65.34(9) 3_676 . ? O3W La1 O6W 146.26(9) . . ? O2W La1 O6W 75.22(10) . . ? O5W La1 O6W 68.21(10) . . ? O1W La1 O6W 135.74(10) . . ? O10 La1 O4W 72.76(10) 2_655 . ? O3 La1 O4W 131.20(9) . . ? O8 La1 O4W 67.97(10) 3_676 . ? O3W La1 O4W 65.50(10) . . ? O2W La1 O4W 138.08(10) . . ? O5W La1 O4W 142.77(9) . . ? O1W La1 O4W 78.72(10) . . ? O6W La1 O4W 97.57(10) . . ? O1 Mo1 O3 107.01(13) . . ? O1 Mo1 O2 100.84(13) . . ? O3 Mo1 O2 103.01(13) . . ? O1 Mo1 O6 90.60(11) . 1_655 ? O3 Mo1 O6 89.59(12) . 1_655 ? O2 Mo1 O6 159.49(12) . 1_655 ? O1 Mo1 O7 159.28(11) . . ? O3 Mo1 O7 89.88(11) . . ? O2 Mo1 O7 86.49(11) . . ? O6 Mo1 O7 77.31(10) 1_655 . ? O1 Mo1 N1 89.69(11) . . ? O3 Mo1 N1 157.11(11) . . ? O2 Mo1 N1 88.61(11) . . ? O6 Mo1 N1 74.36(10) 1_655 . ? O7 Mo1 N1 70.98(10) . . ? O5 Mo2 O4 105.40(14) . . ? O5 Mo2 O6 102.19(13) . . ? O4 Mo2 O6 101.98(12) . . ? O5 Mo2 O2 94.91(12) . . ? O4 Mo2 O2 88.79(12) . . ? O6 Mo2 O2 156.41(12) . . ? O5 Mo2 O11 156.15(11) . . ? O4 Mo2 O11 97.44(12) . . ? O6 Mo2 O11 79.25(11) . . ? O2 Mo2 O11 78.57(10) . . ? O5 Mo2 N2 86.40(12) . . ? O4 Mo2 N2 158.79(12) . . ? O6 Mo2 N2 92.37(11) . . ? O2 Mo2 N2 72.43(10) . . ? O11 Mo2 N2 69.75(10) . . ? Mo1 O2 Mo2 159.60(16) . . ? Mo1 O3 La1 160.54(15) . . ? Mo2 O6 Mo1 142.99(15) . 1_455 ? C6 O7 Mo1 121.1(2) . . ? C6 O8 La1 153.0(3) . 3_676 ? C7 O10 La1 173.6(3) . 2_645 ? C13 O11 Mo2 122.3(2) . . ? C8 N2 C12 118.5(3) . . ? C8 N2 Mo2 122.8(2) . . ? C12 N2 Mo2 117.2(2) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Mo1 124.1(2) . . ? C5 N1 Mo1 116.4(2) . . ? N1 C1 C2 122.4(3) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 118.6(3) . . ? C1 C2 C7 119.4(3) . . ? C3 C2 C7 121.9(3) . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 C6 114.5(3) . . ? C4 C5 C6 123.2(3) . . ? O8 C6 O7 125.6(3) . . ? O8 C6 C5 118.1(3) . . ? O7 C6 C5 116.2(3) . . ? O10 C7 O9 124.7(4) . . ? O10 C7 C2 117.1(3) . . ? O9 C7 C2 118.1(3) . . ? N2 C8 C9 122.7(3) . . ? N2 C8 H8A 118.7 . . ? C9 C8 H8A 118.7 . . ? C10 C9 C8 118.5(4) . . ? C10 C9 C14 123.7(4) . . ? C8 C9 C14 117.7(3) . . ? C9 C10 C11 119.1(4) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? N2 C12 C11 122.3(3) . . ? N2 C12 C13 113.6(3) . . ? C11 C12 C13 123.8(3) . . ? O12 C13 O11 124.5(4) . . ? O12 C13 C12 119.2(3) . . ? O11 C13 C12 116.3(3) . . ? O14 C14 O13 124.1(4) . . ? O14 C14 C9 121.0(4) . . ? O13 C14 C9 114.8(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.815 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.118 data_2 _database_code_depnum_ccdc_archive 'CCDC 888170' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 Ce Mo2 N2 O20' _chemical_formula_weight 867.30 _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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.495(3) _cell_length_b 20.471(7) _cell_length_c 15.448(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.162(7) _cell_angle_gamma 90.00 _cell_volume 2356.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1278 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 22.96 _exptl_crystal_description bar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 3.049 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4066 _exptl_absorpt_correction_T_max 0.7502 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11668 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4124 _reflns_number_gt 3578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0149P)^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 4124 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _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 Ce1 Ce 0.43047(4) 1.039501(13) 0.27630(2) 0.01736(12) Uani 1 1 d . . . Mo1 Mo 0.40314(6) 0.84248(2) 0.33600(3) 0.01414(14) Uani 1 1 d . . . Mo2 Mo -0.10185(6) 0.83644(2) 0.33448(3) 0.01617(14) Uani 1 1 d . . . O1 O 0.4416(5) 0.78964(18) 0.2555(2) 0.0245(9) Uani 1 1 d . . . O2 O 0.1733(5) 0.82565(19) 0.3466(3) 0.0250(9) Uani 1 1 d . . . O3 O 0.3956(5) 0.92036(17) 0.2912(3) 0.0257(9) Uani 1 1 d . . . O4 O -0.0816(5) 0.8987(2) 0.2620(3) 0.0309(10) Uani 1 1 d . . . O5 O -0.1446(5) 0.76784(18) 0.2723(3) 0.0266(9) Uani 1 1 d . . . O6 O -0.3175(5) 0.85312(18) 0.3700(3) 0.0226(9) Uani 1 1 d . . . O7 O 0.4159(5) 0.88577(16) 0.4690(2) 0.0206(8) Uani 1 1 d . . . O8 O 0.4874(6) 0.87396(18) 0.6123(3) 0.0318(10) Uani 1 1 d . . . O9 O 0.6971(8) 0.55006(19) 0.5087(3) 0.0437(13) Uani 1 1 d . . . O10 O 0.6116(6) 0.57716(18) 0.3725(3) 0.0295(10) Uani 1 1 d . . . O11 O -0.0202(5) 0.89346(17) 0.4569(3) 0.0234(9) Uani 1 1 d . . . O12 O 0.0397(6) 0.89608(19) 0.6010(3) 0.0323(10) Uani 1 1 d . . . O13 O 0.2095(8) 0.5605(2) 0.5461(3) 0.0488(14) Uani 1 1 d . . . O14 O 0.1068(7) 0.5751(2) 0.4075(3) 0.0422(12) Uani 1 1 d . . . N2 N -0.0245(6) 0.7654(2) 0.4509(3) 0.0172(10) Uani 1 1 d . . . N1 N 0.4806(6) 0.76281(19) 0.4378(3) 0.0155(10) Uani 1 1 d . . . C1 C 0.5165(7) 0.7015(2) 0.4174(4) 0.0192(12) Uani 1 1 d . . . H1A H 0.4922 0.6878 0.3600 0.023 Uiso 1 1 calc R . . C2 C 0.5899(8) 0.6571(2) 0.4800(4) 0.0203(12) Uani 1 1 d . . . C3 C 0.6239(8) 0.6779(2) 0.5652(4) 0.0227(13) Uani 1 1 d . . . H3A H 0.6719 0.6493 0.6083 0.027 Uiso 1 1 calc R . . C4 C 0.5855(8) 0.7418(2) 0.5855(4) 0.0219(12) Uani 1 1 d . . . H4A H 0.6076 0.7569 0.6424 0.026 Uiso 1 1 calc R . . C5 C 0.5138(7) 0.7826(2) 0.5196(4) 0.0157(11) Uani 1 1 d . . . C6 C 0.4713(7) 0.8532(2) 0.5355(4) 0.0196(12) Uani 1 1 d . . . C7 C 0.6354(7) 0.5890(2) 0.4510(4) 0.0203(12) Uani 1 1 d . . . C8 C 0.0045(8) 0.7024(2) 0.4404(4) 0.0211(12) Uani 1 1 d . . . H8A H -0.0328 0.6835 0.3867 0.025 Uiso 1 1 calc R . . C9 C 0.0888(8) 0.6626(2) 0.5064(4) 0.0230(13) Uani 1 1 d . . . C10 C 0.1334(9) 0.6903(3) 0.5877(4) 0.0276(14) Uani 1 1 d . . . H10A H 0.1830 0.6649 0.6341 0.033 Uiso 1 1 calc R . . C11 C 0.1032(8) 0.7556(3) 0.5987(4) 0.0260(13) Uani 1 1 d . . . H11A H 0.1324 0.7751 0.6528 0.031 Uiso 1 1 calc R . . C12 C 0.0286(7) 0.7925(3) 0.5283(4) 0.0210(12) Uani 1 1 d . . . C13 C 0.0153(7) 0.8661(3) 0.5296(4) 0.0227(13) Uani 1 1 d . . . C14 C 0.1351(8) 0.5944(3) 0.4831(4) 0.0262(14) Uani 1 1 d . . . O1W O 0.2626(7) 1.0139(2) 0.4096(3) 0.0414(12) Uani 1 1 d . . . O2W O 0.6851(6) 0.99658(19) 0.3832(3) 0.0360(11) Uani 1 1 d . . . O3W O 0.1168(6) 1.0056(2) 0.2204(3) 0.0369(11) Uani 1 1 d . . . O4W O 0.1918(6) 1.13444(19) 0.2683(3) 0.0368(11) Uani 1 1 d . . . O5W O 0.6416(6) 0.9771(2) 0.1851(3) 0.0328(10) Uani 1 1 d . . . O6W O 0.7088(5) 1.10987(19) 0.2479(3) 0.0321(10) Uani 1 1 d . . . _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 Ce1 0.0215(2) 0.01327(18) 0.0166(2) 0.00119(11) -0.00089(14) 0.00123(12) Mo1 0.0119(3) 0.0125(2) 0.0175(3) 0.00123(16) -0.0007(2) 0.00170(17) Mo2 0.0119(3) 0.0140(2) 0.0219(3) 0.00279(17) -0.0016(2) 0.00054(17) O1 0.025(2) 0.027(2) 0.021(2) -0.0038(16) -0.0001(18) 0.0033(16) O2 0.015(2) 0.030(2) 0.029(2) 0.0040(17) 0.0007(18) 0.0011(17) O3 0.025(2) 0.018(2) 0.033(2) 0.0083(16) 0.0015(19) 0.0008(16) O4 0.023(2) 0.030(2) 0.039(3) 0.0158(19) -0.001(2) 0.0011(17) O5 0.025(2) 0.024(2) 0.030(2) -0.0036(17) -0.0035(18) 0.0002(17) O6 0.014(2) 0.0243(19) 0.029(2) 0.0036(17) -0.0010(17) -0.0013(16) O7 0.025(2) 0.0154(18) 0.020(2) -0.0008(15) -0.0032(17) 0.0057(16) O8 0.050(3) 0.022(2) 0.023(2) -0.0066(17) 0.000(2) 0.0038(19) O9 0.085(4) 0.022(2) 0.021(3) 0.0009(17) -0.005(2) 0.022(2) O10 0.042(3) 0.024(2) 0.021(2) -0.0068(16) -0.002(2) 0.0109(18) O11 0.023(2) 0.0181(19) 0.027(2) 0.0017(16) -0.0031(18) -0.0001(16) O12 0.038(3) 0.029(2) 0.029(3) -0.0119(18) -0.004(2) 0.0044(19) O13 0.085(4) 0.029(2) 0.029(3) 0.002(2) -0.012(3) 0.026(2) O14 0.065(3) 0.025(2) 0.033(3) -0.0078(19) -0.010(2) 0.010(2) N2 0.015(2) 0.016(2) 0.022(3) 0.0020(18) 0.004(2) 0.0020(18) N1 0.013(2) 0.012(2) 0.021(3) -0.0003(17) -0.0028(19) 0.0018(17) C1 0.021(3) 0.017(3) 0.019(3) -0.004(2) 0.002(2) 0.000(2) C2 0.020(3) 0.015(3) 0.026(3) -0.002(2) 0.002(3) -0.001(2) C3 0.033(4) 0.017(3) 0.017(3) 0.000(2) -0.003(3) 0.002(2) C4 0.030(3) 0.017(3) 0.018(3) -0.003(2) 0.001(3) -0.003(2) C5 0.012(3) 0.016(3) 0.019(3) -0.005(2) 0.003(2) 0.000(2) C6 0.016(3) 0.015(3) 0.029(4) -0.005(2) 0.006(3) 0.000(2) C7 0.023(3) 0.016(3) 0.021(3) -0.003(2) 0.000(3) -0.002(2) C8 0.025(3) 0.016(3) 0.022(3) -0.002(2) -0.002(3) 0.002(2) C9 0.023(3) 0.018(3) 0.027(4) 0.001(2) -0.002(3) 0.001(2) C10 0.037(4) 0.023(3) 0.021(3) 0.002(2) -0.005(3) 0.006(3) C11 0.034(4) 0.024(3) 0.020(3) -0.003(2) 0.000(3) 0.005(3) C12 0.016(3) 0.022(3) 0.025(3) 0.001(2) 0.004(2) 0.002(2) C13 0.012(3) 0.022(3) 0.034(4) -0.004(3) 0.004(3) -0.001(2) C14 0.031(3) 0.019(3) 0.028(4) 0.003(2) -0.003(3) 0.001(2) O1W 0.057(3) 0.035(2) 0.036(3) 0.006(2) 0.023(2) 0.011(2) O2W 0.041(3) 0.022(2) 0.040(3) -0.0005(18) -0.015(2) 0.0080(19) O3W 0.029(2) 0.029(2) 0.050(3) 0.013(2) -0.009(2) -0.0087(19) O4W 0.037(3) 0.025(2) 0.047(3) 0.0010(19) -0.002(2) 0.0075(19) O5W 0.036(3) 0.034(2) 0.029(3) 0.0009(18) 0.007(2) 0.009(2) O6W 0.029(2) 0.033(2) 0.033(3) -0.0011(18) 0.000(2) -0.0073(19) _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. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O10 2.413(4) 2_655 ? Ce1 O3 2.466(4) . ? Ce1 O8 2.500(4) 3_676 ? Ce1 O3W 2.513(4) . ? Ce1 O2W 2.542(4) . ? Ce1 O5W 2.569(4) . ? Ce1 O1W 2.579(4) . ? Ce1 O6W 2.611(4) . ? Ce1 O4W 2.635(4) . ? Mo1 O1 1.697(4) . ? Mo1 O3 1.736(4) . ? Mo1 O2 1.781(4) . ? Mo1 O6 2.114(4) 1_655 ? Mo1 O7 2.230(4) . ? Mo1 N1 2.297(4) . ? Mo2 O5 1.712(4) . ? Mo2 O4 1.714(4) . ? Mo2 O6 1.795(4) . ? Mo2 O2 2.063(4) . ? Mo2 O11 2.251(4) . ? Mo2 N2 2.337(4) . ? O6 Mo1 2.114(4) 1_455 ? O7 C6 1.257(7) . ? O8 C6 1.255(7) . ? O8 Ce1 2.500(4) 3_676 ? O9 C7 1.246(7) . ? O10 C7 1.231(7) . ? O10 Ce1 2.413(4) 2_645 ? O11 C13 1.257(7) . ? O12 C13 1.258(7) . ? O13 C14 1.274(7) . ? O14 C14 1.230(7) . ? N2 C8 1.321(6) . ? N2 C12 1.340(7) . ? N1 C5 1.325(7) . ? N1 C1 1.329(6) . ? C1 C2 1.396(8) . ? C1 H1A 0.9300 . ? C2 C3 1.381(8) . ? C2 C7 1.514(7) . ? C3 C4 1.382(7) . ? C3 H3A 0.9300 . ? C4 C5 1.381(7) . ? C4 H4A 0.9300 . ? C5 C6 1.504(7) . ? C8 C9 1.401(8) . ? C8 H8A 0.9300 . ? C9 C10 1.386(8) . ? C9 C14 1.493(8) . ? C10 C11 1.370(8) . ? C10 H10A 0.9300 . ? C11 C12 1.392(8) . ? C11 H11A 0.9300 . ? C12 C13 1.511(7) . ? _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 O10 Ce1 O3 113.61(13) 2_655 . ? O10 Ce1 O8 115.26(13) 2_655 3_676 ? O3 Ce1 O8 131.08(13) . 3_676 ? O10 Ce1 O3W 74.87(14) 2_655 . ? O3 Ce1 O3W 69.81(13) . . ? O8 Ce1 O3W 125.74(16) 3_676 . ? O10 Ce1 O2W 137.85(16) 2_655 . ? O3 Ce1 O2W 71.17(13) . . ? O8 Ce1 O2W 71.67(13) 3_676 . ? O3W Ce1 O2W 137.48(14) . . ? O10 Ce1 O5W 70.21(14) 2_655 . ? O3 Ce1 O5W 68.73(14) . . ? O8 Ce1 O5W 127.52(15) 3_676 . ? O3W Ce1 O5W 106.44(15) . . ? O2W Ce1 O5W 73.79(14) . . ? O10 Ce1 O1W 143.16(15) 2_655 . ? O3 Ce1 O1W 70.08(14) . . ? O8 Ce1 O1W 72.51(15) 3_676 . ? O3W Ce1 O1W 72.55(16) . . ? O2W Ce1 O1W 78.92(16) . . ? O5W Ce1 O1W 135.97(13) . . ? O10 Ce1 O6W 71.84(13) 2_655 . ? O3 Ce1 O6W 130.99(13) . . ? O8 Ce1 O6W 65.34(14) 3_676 . ? O3W Ce1 O6W 146.00(13) . . ? O2W Ce1 O6W 75.08(14) . . ? O5W Ce1 O6W 68.38(14) . . ? O1W Ce1 O6W 135.51(15) . . ? O10 Ce1 O4W 72.59(15) 2_655 . ? O3 Ce1 O4W 130.96(14) . . ? O8 Ce1 O4W 68.02(14) 3_676 . ? O3W Ce1 O4W 65.29(14) . . ? O2W Ce1 O4W 138.06(14) . . ? O5W Ce1 O4W 142.73(14) . . ? O1W Ce1 O4W 78.49(15) . . ? O6W Ce1 O4W 97.80(13) . . ? O1 Mo1 O3 107.09(19) . . ? O1 Mo1 O2 100.72(19) . . ? O3 Mo1 O2 102.93(18) . . ? O1 Mo1 O6 90.37(17) . 1_655 ? O3 Mo1 O6 89.62(16) . 1_655 ? O2 Mo1 O6 159.81(18) . 1_655 ? O1 Mo1 O7 159.24(16) . . ? O3 Mo1 O7 89.93(16) . . ? O2 Mo1 O7 86.47(16) . . ? O6 Mo1 O7 77.68(15) 1_655 . ? O1 Mo1 N1 89.94(17) . . ? O3 Mo1 N1 156.91(17) . . ? O2 Mo1 N1 88.61(17) . . ? O6 Mo1 N1 74.46(14) 1_655 . ? O7 Mo1 N1 70.64(14) . . ? O5 Mo2 O4 105.6(2) . . ? O5 Mo2 O6 101.96(19) . . ? O4 Mo2 O6 101.77(18) . . ? O5 Mo2 O2 95.06(18) . . ? O4 Mo2 O2 88.92(17) . . ? O6 Mo2 O2 156.52(17) . . ? O5 Mo2 O11 156.12(16) . . ? O4 Mo2 O11 97.35(18) . . ? O6 Mo2 O11 79.45(16) . . ? O2 Mo2 O11 78.48(15) . . ? O5 Mo2 N2 86.38(17) . . ? O4 Mo2 N2 158.98(17) . . ? O6 Mo2 N2 92.31(16) . . ? O2 Mo2 N2 72.57(15) . . ? O11 Mo2 N2 69.74(14) . . ? Mo1 O2 Mo2 159.8(2) . . ? Mo1 O3 Ce1 161.1(2) . . ? Mo2 O6 Mo1 143.6(2) . 1_455 ? C6 O7 Mo1 121.3(3) . . ? C6 O8 Ce1 152.0(4) . 3_676 ? C7 O10 Ce1 172.7(4) . 2_645 ? C13 O11 Mo2 122.2(3) . . ? C8 N2 C12 118.5(5) . . ? C8 N2 Mo2 122.9(4) . . ? C12 N2 Mo2 117.0(3) . . ? C5 N1 C1 119.6(4) . . ? C5 N1 Mo1 116.3(3) . . ? C1 N1 Mo1 123.4(4) . . ? N1 C1 C2 121.7(5) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 118.5(5) . . ? C3 C2 C7 122.8(5) . . ? C1 C2 C7 118.7(5) . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 118.7(5) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 122.4(5) . . ? N1 C5 C6 115.3(4) . . ? C4 C5 C6 122.3(5) . . ? O8 C6 O7 125.6(5) . . ? O8 C6 C5 118.6(5) . . ? O7 C6 C5 115.7(5) . . ? O10 C7 O9 125.6(5) . . ? O10 C7 C2 117.3(5) . . ? O9 C7 C2 117.1(5) . . ? N2 C8 C9 123.0(5) . . ? N2 C8 H8A 118.5 . . ? C9 C8 H8A 118.5 . . ? C10 C9 C8 118.0(5) . . ? C10 C9 C14 124.2(5) . . ? C8 C9 C14 117.7(5) . . ? C11 C10 C9 119.0(5) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 119.3(5) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? N2 C12 C11 122.0(5) . . ? N2 C12 C13 114.4(5) . . ? C11 C12 C13 123.5(5) . . ? O11 C13 O12 124.3(5) . . ? O11 C13 C12 116.1(5) . . ? O12 C13 C12 119.7(5) . . ? O14 C14 O13 124.5(5) . . ? O14 C14 C9 120.6(5) . . ? O13 C14 C9 114.8(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.308 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.167 data_3 _database_code_depnum_ccdc_archive 'CCDC 888171' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 Mo2 N2 O20 Pr' _chemical_formula_weight 868.09 _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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.540(7) _cell_length_b 20.599(18) _cell_length_c 15.512(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.219(19) _cell_angle_gamma 90.00 _cell_volume 2395(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 409 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 16.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 3.133 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5591 _exptl_absorpt_correction_T_max 0.8343 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11921 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4205 _reflns_number_gt 3336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0365P)^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 4205 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 Pr1 Pr 0.43112(4) 1.039766(14) 0.27633(2) 0.02013(10) Uani 1 1 d . . . Mo1 Mo 0.40356(6) 0.84317(2) 0.33589(3) 0.01682(13) Uani 1 1 d . . . Mo2 Mo -0.10146(6) 0.83704(2) 0.33420(3) 0.01865(13) Uani 1 1 d . . . O1 O 0.4429(5) 0.79052(18) 0.2553(2) 0.0280(9) Uani 1 1 d . . . O2 O 0.1734(5) 0.82627(18) 0.3464(3) 0.0280(9) Uani 1 1 d . . . O3 O 0.3964(5) 0.92120(18) 0.2912(3) 0.0280(9) Uani 1 1 d . . . O4 O -0.0819(5) 0.89948(19) 0.2609(3) 0.0326(10) Uani 1 1 d . . . O5 O -0.1452(5) 0.76814(18) 0.2722(3) 0.0287(9) Uani 1 1 d . . . O6 O -0.3171(5) 0.85420(17) 0.3709(3) 0.0271(9) Uani 1 1 d . . . O7 O 0.4164(5) 0.88657(17) 0.4690(2) 0.0224(9) Uani 1 1 d . . . O8 O 0.4865(6) 0.87380(18) 0.6124(3) 0.0324(10) Uani 1 1 d . . . O9 O 0.6957(7) 0.54949(19) 0.5079(3) 0.0462(13) Uani 1 1 d . . . O10 O 0.6126(5) 0.57718(19) 0.3711(3) 0.0319(10) Uani 1 1 d . . . O11 O -0.0194(5) 0.89436(17) 0.4568(3) 0.0245(9) Uani 1 1 d . . . O12 O 0.0400(5) 0.89642(19) 0.6014(3) 0.0341(10) Uani 1 1 d . . . O13 O 0.2077(7) 0.5601(2) 0.5461(3) 0.0500(13) Uani 1 1 d . . . O14 O 0.1081(6) 0.5751(2) 0.4078(3) 0.0423(12) Uani 1 1 d . . . N2 N -0.0235(6) 0.7661(2) 0.4511(3) 0.0202(10) Uani 1 1 d . . . N1 N 0.4809(5) 0.7635(2) 0.4373(3) 0.0186(10) Uani 1 1 d . . . C1 C 0.5177(7) 0.7017(2) 0.4170(4) 0.0216(12) Uani 1 1 d . . . H1A H 0.4928 0.6879 0.3599 0.026 Uiso 1 1 calc R . . C2 C 0.5919(7) 0.6577(2) 0.4790(4) 0.0208(12) Uani 1 1 d . . . C3 C 0.6245(8) 0.6775(3) 0.5650(4) 0.0260(13) Uani 1 1 d . . . H3A H 0.6715 0.6488 0.6077 0.031 Uiso 1 1 calc R . . C4 C 0.5848(8) 0.7418(3) 0.5859(4) 0.0269(13) Uani 1 1 d . . . H4A H 0.6055 0.7566 0.6428 0.032 Uiso 1 1 calc R . . C5 C 0.5147(7) 0.7826(2) 0.5205(4) 0.0192(12) Uani 1 1 d . . . C6 C 0.4691(7) 0.8536(3) 0.5363(4) 0.0204(12) Uani 1 1 d . . . C7 C 0.6362(7) 0.5888(3) 0.4507(4) 0.0245(13) Uani 1 1 d . . . C8 C 0.0050(7) 0.7028(3) 0.4402(4) 0.0252(13) Uani 1 1 d . . . H8A H -0.0329 0.6841 0.3868 0.030 Uiso 1 1 calc R . . C9 C 0.0889(7) 0.6639(3) 0.5054(4) 0.0234(13) Uani 1 1 d . . . C10 C 0.1325(8) 0.6897(3) 0.5870(4) 0.0289(14) Uani 1 1 d . . . H10A H 0.1806 0.6639 0.6329 0.035 Uiso 1 1 calc R . . C11 C 0.1019(8) 0.7567(3) 0.5988(4) 0.0306(14) Uani 1 1 d . . . H11A H 0.1302 0.7759 0.6528 0.037 Uiso 1 1 calc R . . C12 C 0.0295(7) 0.7932(3) 0.5292(4) 0.0233(13) Uani 1 1 d . . . C13 C 0.0154(7) 0.8669(3) 0.5297(4) 0.0261(14) Uani 1 1 d . . . C14 C 0.1339(8) 0.5940(3) 0.4824(4) 0.0253(13) Uani 1 1 d . . . O1W O 0.2673(6) 1.0149(2) 0.4097(3) 0.0408(11) Uani 1 1 d . . . O2W O 0.6841(6) 0.99690(19) 0.3821(3) 0.0370(11) Uani 1 1 d . . . O3W O 0.1190(5) 1.0063(2) 0.2216(3) 0.0394(11) Uani 1 1 d . . . O4W O 0.1935(5) 1.13410(19) 0.2687(3) 0.0372(11) Uani 1 1 d . . . O5W O 0.6394(5) 0.97734(19) 0.1852(3) 0.0349(11) Uani 1 1 d . . . O6W O 0.7069(5) 1.10980(19) 0.2476(3) 0.0344(10) Uani 1 1 d . . . _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 Pr1 0.02227(17) 0.01733(17) 0.02095(18) 0.00128(14) 0.00302(13) 0.00137(13) Mo1 0.0126(2) 0.0164(2) 0.0216(3) 0.0012(2) 0.00246(19) 0.00151(18) Mo2 0.0125(2) 0.0180(3) 0.0254(3) 0.0023(2) 0.0018(2) 0.00075(18) O1 0.028(2) 0.029(2) 0.028(2) -0.0032(19) 0.0060(19) 0.0036(17) O2 0.016(2) 0.033(2) 0.035(2) 0.004(2) 0.0031(18) -0.0013(16) O3 0.031(2) 0.022(2) 0.031(2) 0.0062(19) 0.0043(19) 0.0006(17) O4 0.025(2) 0.034(2) 0.039(3) 0.017(2) 0.003(2) 0.0012(18) O5 0.026(2) 0.027(2) 0.032(2) -0.0037(19) 0.0006(19) 0.0024(17) O6 0.017(2) 0.027(2) 0.038(3) 0.002(2) 0.0049(18) -0.0003(16) O7 0.023(2) 0.0191(19) 0.025(2) 0.0008(18) 0.0017(17) 0.0059(16) O8 0.050(3) 0.021(2) 0.025(2) -0.0023(19) 0.002(2) 0.0025(19) O9 0.085(4) 0.024(2) 0.029(3) 0.002(2) 0.002(2) 0.023(2) O10 0.041(3) 0.028(2) 0.026(2) -0.008(2) -0.001(2) 0.0071(19) O11 0.025(2) 0.020(2) 0.028(2) -0.0020(19) 0.0001(18) 0.0027(16) O12 0.036(2) 0.036(2) 0.030(3) -0.010(2) -0.001(2) 0.0031(19) O13 0.081(4) 0.032(3) 0.034(3) 0.004(2) -0.011(3) 0.022(2) O14 0.062(3) 0.025(2) 0.036(3) -0.008(2) -0.008(2) 0.006(2) N2 0.018(2) 0.021(3) 0.022(3) 0.003(2) 0.002(2) 0.0007(19) N1 0.016(2) 0.020(2) 0.021(3) 0.001(2) 0.0045(19) 0.0036(18) C1 0.022(3) 0.017(3) 0.025(3) 0.000(3) 0.004(2) 0.000(2) C2 0.021(3) 0.017(3) 0.025(3) 0.000(2) 0.004(2) 0.003(2) C3 0.035(3) 0.016(3) 0.027(3) 0.005(3) -0.001(3) 0.003(2) C4 0.033(3) 0.024(3) 0.024(3) -0.002(3) 0.003(3) 0.005(3) C5 0.016(3) 0.020(3) 0.022(3) -0.002(2) 0.004(2) 0.002(2) C6 0.020(3) 0.020(3) 0.022(3) -0.005(3) 0.003(2) -0.005(2) C7 0.023(3) 0.022(3) 0.028(3) 0.000(3) -0.001(3) -0.001(2) C8 0.023(3) 0.025(3) 0.028(3) -0.002(3) 0.002(3) 0.000(2) C9 0.021(3) 0.021(3) 0.028(3) 0.002(3) 0.003(3) -0.004(2) C10 0.029(3) 0.026(3) 0.032(4) 0.007(3) 0.000(3) 0.007(3) C11 0.038(4) 0.026(3) 0.028(4) -0.005(3) 0.004(3) 0.001(3) C12 0.013(3) 0.027(3) 0.030(3) 0.001(3) 0.005(2) 0.002(2) C13 0.012(3) 0.030(3) 0.036(4) -0.001(3) 0.004(3) 0.004(2) C14 0.029(3) 0.022(3) 0.025(3) 0.002(3) 0.003(3) -0.002(2) O1W 0.052(3) 0.037(3) 0.037(3) 0.003(2) 0.020(2) 0.005(2) O2W 0.041(3) 0.030(2) 0.038(3) 0.002(2) -0.005(2) 0.007(2) O3W 0.028(2) 0.034(2) 0.053(3) 0.012(2) -0.006(2) -0.0106(19) O4W 0.036(3) 0.030(2) 0.044(3) 0.001(2) 0.001(2) 0.0114(19) O5W 0.040(3) 0.032(2) 0.035(3) -0.002(2) 0.013(2) 0.0093(19) O6W 0.037(2) 0.030(2) 0.036(3) -0.003(2) 0.003(2) -0.0093(19) _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. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O10 2.402(4) 2_655 ? Pr1 O3 2.470(4) . ? Pr1 O8 2.511(4) 3_676 ? Pr1 O3W 2.510(4) . ? Pr1 O2W 2.536(4) . ? Pr1 O5W 2.569(4) . ? Pr1 O1W 2.573(4) . ? Pr1 O6W 2.609(4) . ? Pr1 O4W 2.637(4) . ? Mo1 O1 1.705(4) . ? Mo1 O3 1.749(4) . ? Mo1 O2 1.795(4) . ? Mo1 O6 2.129(4) 1_655 ? Mo1 O7 2.243(4) . ? Mo1 N1 2.304(5) . ? Mo2 O5 1.726(4) . ? Mo2 O4 1.733(4) . ? Mo2 O6 1.815(4) . ? Mo2 O2 2.073(4) . ? Mo2 O11 2.267(4) . ? Mo2 N2 2.354(5) . ? O6 Mo1 2.129(4) 1_455 ? O7 C6 1.272(6) . ? O8 C6 1.246(7) . ? O8 Pr1 2.511(4) 3_676 ? O9 C7 1.248(7) . ? O10 C7 1.251(7) . ? O10 Pr1 2.402(4) 2_645 ? O11 C13 1.267(7) . ? O12 C13 1.262(7) . ? O13 C14 1.286(7) . ? O14 C14 1.218(7) . ? N2 C8 1.335(7) . ? N2 C12 1.353(7) . ? N1 C1 1.347(6) . ? N1 C5 1.348(7) . ? C1 C2 1.393(7) . ? C1 H1A 0.9300 . ? C2 C3 1.391(8) . ? C2 C7 1.535(7) . ? C3 C4 1.404(7) . ? C3 H3A 0.9300 . ? C4 C5 1.378(8) . ? C4 H4A 0.9300 . ? C5 C6 1.527(7) . ? C8 C9 1.389(8) . ? C8 H8A 0.9300 . ? C9 C10 1.380(8) . ? C9 C14 1.529(8) . ? C10 C11 1.414(8) . ? C10 H10A 0.9300 . ? C11 C12 1.379(8) . ? C11 H11A 0.9300 . ? C12 C13 1.523(8) . ? _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 O10 Pr1 O3 113.66(13) 2_655 . ? O10 Pr1 O8 115.17(14) 2_655 3_676 ? O3 Pr1 O8 131.13(14) . 3_676 ? O10 Pr1 O3W 74.90(14) 2_655 . ? O3 Pr1 O3W 69.80(13) . . ? O8 Pr1 O3W 125.49(15) 3_676 . ? O10 Pr1 O2W 138.05(15) 2_655 . ? O3 Pr1 O2W 71.04(13) . . ? O8 Pr1 O2W 71.90(14) 3_676 . ? O3W Pr1 O2W 137.29(14) . . ? O10 Pr1 O5W 70.47(15) 2_655 . ? O3 Pr1 O5W 68.52(13) . . ? O8 Pr1 O5W 127.79(14) 3_676 . ? O3W Pr1 O5W 106.44(15) . . ? O2W Pr1 O5W 73.73(15) . . ? O10 Pr1 O1W 143.23(15) 2_655 . ? O3 Pr1 O1W 70.30(13) . . ? O8 Pr1 O1W 72.12(15) 3_676 . ? O3W Pr1 O1W 72.72(16) . . ? O2W Pr1 O1W 78.66(16) . . ? O5W Pr1 O1W 135.89(13) . . ? O10 Pr1 O6W 71.92(13) 2_655 . ? O3 Pr1 O6W 131.10(13) . . ? O8 Pr1 O6W 65.34(14) 3_676 . ? O3W Pr1 O6W 146.08(14) . . ? O2W Pr1 O6W 75.25(15) . . ? O5W Pr1 O6W 68.69(14) . . ? O1W Pr1 O6W 135.10(14) . . ? O10 Pr1 O4W 72.46(14) 2_655 . ? O3 Pr1 O4W 130.87(13) . . ? O8 Pr1 O4W 67.95(14) 3_676 . ? O3W Pr1 O4W 65.16(14) . . ? O2W Pr1 O4W 138.18(14) . . ? O5W Pr1 O4W 142.86(14) . . ? O1W Pr1 O4W 78.44(14) . . ? O6W Pr1 O4W 97.78(15) . . ? O1 Mo1 O3 107.13(19) . . ? O1 Mo1 O2 100.95(18) . . ? O3 Mo1 O2 103.04(17) . . ? O1 Mo1 O6 90.51(17) . 1_655 ? O3 Mo1 O6 89.45(16) . 1_655 ? O2 Mo1 O6 159.55(18) . 1_655 ? O1 Mo1 O7 159.23(16) . . ? O3 Mo1 O7 89.71(17) . . ? O2 Mo1 O7 86.52(16) . . ? O6 Mo1 O7 77.29(14) 1_655 . ? O1 Mo1 N1 89.76(18) . . ? O3 Mo1 N1 156.92(17) . . ? O2 Mo1 N1 88.60(16) . . ? O6 Mo1 N1 74.44(15) 1_655 . ? O7 Mo1 N1 70.92(15) . . ? O5 Mo2 O4 105.6(2) . . ? O5 Mo2 O6 102.18(18) . . ? O4 Mo2 O6 101.78(18) . . ? O5 Mo2 O2 95.27(17) . . ? O4 Mo2 O2 89.08(16) . . ? O6 Mo2 O2 155.97(18) . . ? O5 Mo2 O11 156.08(16) . . ? O4 Mo2 O11 97.40(18) . . ? O6 Mo2 O11 78.93(16) . . ? O2 Mo2 O11 78.45(15) . . ? O5 Mo2 N2 86.32(18) . . ? O4 Mo2 N2 159.09(17) . . ? O6 Mo2 N2 92.10(17) . . ? O2 Mo2 N2 72.50(15) . . ? O11 Mo2 N2 69.77(16) . . ? Mo1 O2 Mo2 159.7(2) . . ? Mo1 O3 Pr1 161.2(2) . . ? Mo2 O6 Mo1 142.6(2) . 1_455 ? C6 O7 Mo1 121.4(3) . . ? C6 O8 Pr1 151.9(4) . 3_676 ? C7 O10 Pr1 172.3(4) . 2_645 ? C13 O11 Mo2 121.9(4) . . ? C8 N2 C12 118.7(5) . . ? C8 N2 Mo2 122.6(4) . . ? C12 N2 Mo2 117.2(4) . . ? C1 N1 C5 118.5(5) . . ? C1 N1 Mo1 123.9(4) . . ? C5 N1 Mo1 116.9(3) . . ? N1 C1 C2 122.0(5) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C1 C2 C3 119.2(5) . . ? C1 C2 C7 119.2(5) . . ? C3 C2 C7 121.6(5) . . ? C2 C3 C4 118.6(5) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 123.0(5) . . ? N1 C5 C6 114.2(5) . . ? C4 C5 C6 122.7(5) . . ? O8 C6 O7 126.1(5) . . ? O8 C6 C5 118.0(5) . . ? O7 C6 C5 115.9(5) . . ? O9 C7 O10 125.4(5) . . ? O9 C7 C2 118.0(5) . . ? O10 C7 C2 116.6(5) . . ? N2 C8 C9 122.6(5) . . ? N2 C8 H8A 118.7 . . ? C9 C8 H8A 118.7 . . ? C10 C9 C8 119.3(5) . . ? C10 C9 C14 122.7(5) . . ? C8 C9 C14 118.0(5) . . ? C9 C10 C11 118.0(6) . . ? C9 C10 H10A 121.0 . . ? C11 C10 H10A 121.0 . . ? C12 C11 C10 119.2(6) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? N2 C12 C11 121.9(5) . . ? N2 C12 C13 113.8(5) . . ? C11 C12 C13 124.1(5) . . ? O12 C13 O11 124.7(5) . . ? O12 C13 C12 118.8(5) . . ? O11 C13 C12 116.6(5) . . ? O14 C14 O13 124.6(5) . . ? O14 C14 C9 120.4(5) . . ? O13 C14 C9 114.9(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.977 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.144 data_4 _database_code_depnum_ccdc_archive 'CCDC 888172' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 Mo2 N2 Nd O20' _chemical_formula_weight 871.42 _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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.458(4) _cell_length_b 20.353(10) _cell_length_c 15.350(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.200(12) _cell_angle_gamma 90.00 _cell_volume 2317(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 305 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 16.20 _exptl_crystal_description bar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 3.378 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2940 _exptl_absorpt_correction_T_max 0.8230 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11509 _diffrn_reflns_av_R_equivalents 0.0836 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4065 _reflns_number_gt 2715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0245P)^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 SHELXL _refine_ls_extinction_coef 0.00450(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4065 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 Nd1 Nd 0.43146(7) 1.03984(3) 0.27643(4) 0.0295(2) Uani 1 1 d . . . Mo1 Mo 0.40390(11) 0.84366(4) 0.33589(6) 0.0269(2) Uani 1 1 d . . . Mo2 Mo -0.10134(11) 0.83737(4) 0.33400(6) 0.0287(2) Uani 1 1 d . . . O1 O 0.4424(8) 0.7909(3) 0.2554(4) 0.0322(17) Uani 1 1 d . . . O2 O 0.1734(8) 0.8263(3) 0.3450(4) 0.0341(17) Uani 1 1 d . . . O3 O 0.3986(8) 0.9228(3) 0.2916(4) 0.0349(17) Uani 1 1 d . . . O4 O -0.0825(8) 0.8991(3) 0.2610(4) 0.0393(19) Uani 1 1 d . . . O5 O -0.1436(9) 0.7697(3) 0.2731(4) 0.0359(18) Uani 1 1 d . . . O6 O -0.3179(8) 0.8551(3) 0.3701(4) 0.0338(17) Uani 1 1 d . . . O7 O 0.4176(8) 0.8874(3) 0.4692(4) 0.0301(16) Uani 1 1 d . . . O8 O 0.4855(9) 0.8741(3) 0.6135(5) 0.0422(19) Uani 1 1 d . . . O9 O 0.6936(11) 0.5489(4) 0.5075(5) 0.051(2) Uani 1 1 d . . . O10 O 0.6139(10) 0.5774(3) 0.3705(4) 0.0420(19) Uani 1 1 d . . . O11 O -0.0199(9) 0.8944(3) 0.4561(5) 0.0342(17) Uani 1 1 d . . . O12 O 0.0421(9) 0.8976(4) 0.6016(5) 0.043(2) Uani 1 1 d . . . O13 O 0.2082(12) 0.5597(4) 0.5450(5) 0.059(2) Uani 1 1 d . . . O14 O 0.1103(11) 0.5752(4) 0.4082(5) 0.053(2) Uani 1 1 d . . . N2 N -0.0259(10) 0.7669(4) 0.4503(5) 0.031(2) Uani 1 1 d . . . N1 N 0.4800(10) 0.7642(4) 0.4364(5) 0.029(2) Uani 1 1 d . . . C1 C 0.5171(13) 0.7009(5) 0.4172(6) 0.032(2) Uani 1 1 d . . . H1A H 0.4917 0.6867 0.3596 0.038 Uiso 1 1 calc R . . C2 C 0.5893(12) 0.6572(5) 0.4780(7) 0.028(2) Uani 1 1 d . . . C3 C 0.6257(14) 0.6784(5) 0.5638(7) 0.037(3) Uani 1 1 d . . . H3A H 0.6781 0.6497 0.6064 0.045 Uiso 1 1 calc R . . C4 C 0.5848(13) 0.7416(5) 0.5862(7) 0.032(2) Uani 1 1 d . . . H4A H 0.6044 0.7559 0.6440 0.038 Uiso 1 1 calc R . . C5 C 0.5131(12) 0.7834(5) 0.5198(6) 0.024(2) Uani 1 1 d . . . C6 C 0.4699(13) 0.8538(5) 0.5370(7) 0.032(3) Uani 1 1 d . . . C7 C 0.6334(13) 0.5887(5) 0.4497(8) 0.035(3) Uani 1 1 d . . . C8 C 0.0034(13) 0.7032(6) 0.4388(7) 0.037(3) Uani 1 1 d . . . H8A H -0.0339 0.6844 0.3847 0.045 Uiso 1 1 calc R . . C9 C 0.0886(14) 0.6634(5) 0.5054(7) 0.034(3) Uani 1 1 d . . . C10 C 0.1345(15) 0.6907(6) 0.5877(7) 0.043(3) Uani 1 1 d . . . H10A H 0.1855 0.6648 0.6338 0.052 Uiso 1 1 calc R . . C11 C 0.1030(14) 0.7570(5) 0.6000(7) 0.037(3) Uani 1 1 d . . . H11A H 0.1305 0.7766 0.6545 0.045 Uiso 1 1 calc R . . C12 C 0.0296(12) 0.7928(5) 0.5287(7) 0.029(2) Uani 1 1 d . . . C13 C 0.0158(13) 0.8664(5) 0.5301(8) 0.035(3) Uani 1 1 d . . . C14 C 0.1341(14) 0.5936(5) 0.4822(8) 0.037(3) Uani 1 1 d . . . O1W O 0.2695(10) 1.0157(3) 0.4088(4) 0.044(2) Uani 1 1 d . . . O2W O 0.6828(9) 0.9966(3) 0.3814(4) 0.0417(19) Uani 1 1 d . . . O3W O 0.1196(9) 1.0062(4) 0.2209(5) 0.046(2) Uani 1 1 d . . . O4W O 0.1939(9) 1.1333(3) 0.2693(4) 0.0421(19) Uani 1 1 d . . . O5W O 0.6397(9) 0.9775(3) 0.1849(4) 0.0418(19) Uani 1 1 d . . . O6W O 0.7058(9) 1.1091(3) 0.2480(4) 0.0412(19) Uani 1 1 d . . . _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 Nd1 0.0239(3) 0.0289(4) 0.0365(4) 0.0018(3) 0.0067(2) 0.0010(3) Mo1 0.0150(4) 0.0290(6) 0.0372(6) 0.0014(4) 0.0055(4) 0.0015(4) Mo2 0.0146(5) 0.0308(6) 0.0410(6) 0.0026(4) 0.0047(4) 0.0014(4) O1 0.023(4) 0.033(4) 0.041(4) -0.007(3) 0.007(3) -0.003(3) O2 0.017(4) 0.042(5) 0.043(4) 0.001(3) 0.000(3) 0.003(3) O3 0.032(4) 0.024(4) 0.048(4) 0.014(3) 0.003(3) 0.000(3) O4 0.018(4) 0.047(5) 0.055(5) 0.014(4) 0.013(3) 0.005(3) O5 0.036(4) 0.030(4) 0.041(4) -0.004(3) 0.003(3) 0.009(3) O6 0.013(3) 0.041(5) 0.048(4) 0.007(3) 0.004(3) 0.006(3) O7 0.022(4) 0.029(4) 0.039(4) 0.002(3) 0.002(3) 0.003(3) O8 0.049(5) 0.035(5) 0.042(5) 0.000(4) 0.002(4) 0.008(4) O9 0.072(6) 0.036(5) 0.045(5) -0.002(4) 0.004(4) 0.015(5) O10 0.056(5) 0.037(5) 0.033(4) -0.011(3) 0.002(4) 0.007(4) O11 0.029(4) 0.029(4) 0.045(5) -0.001(4) 0.006(3) 0.003(3) O12 0.038(5) 0.041(5) 0.050(5) -0.007(4) 0.005(4) 0.000(4) O13 0.082(7) 0.050(6) 0.044(5) 0.005(4) -0.001(4) 0.023(5) O14 0.079(6) 0.033(5) 0.046(5) -0.010(4) -0.004(4) 0.007(4) N2 0.023(5) 0.026(5) 0.044(6) -0.006(4) 0.008(4) 0.000(4) N1 0.021(5) 0.028(5) 0.040(5) 0.003(4) 0.011(4) -0.002(4) C1 0.029(6) 0.035(7) 0.031(6) -0.006(5) 0.006(5) -0.001(5) C2 0.016(5) 0.031(7) 0.039(6) 0.001(5) 0.011(4) -0.003(5) C3 0.046(7) 0.028(7) 0.038(7) 0.006(5) 0.004(5) 0.007(5) C4 0.035(6) 0.027(7) 0.034(6) -0.007(5) 0.010(5) -0.006(5) C5 0.019(5) 0.024(6) 0.031(6) -0.003(5) 0.011(4) 0.003(4) C6 0.028(6) 0.027(7) 0.043(7) -0.001(5) 0.016(5) -0.004(5) C7 0.017(6) 0.032(7) 0.053(8) -0.016(6) 0.000(5) -0.006(5) C8 0.025(6) 0.054(8) 0.034(6) -0.005(6) 0.009(5) 0.006(6) C9 0.032(6) 0.027(7) 0.042(7) 0.007(5) 0.011(5) 0.003(5) C10 0.049(8) 0.048(8) 0.032(7) 0.010(6) 0.003(5) -0.006(6) C11 0.043(7) 0.020(7) 0.050(7) -0.003(5) 0.011(6) 0.000(5) C12 0.018(5) 0.024(6) 0.046(7) -0.001(5) 0.015(5) 0.000(5) C13 0.015(5) 0.038(7) 0.054(8) -0.004(6) 0.010(5) -0.007(5) C14 0.031(6) 0.034(7) 0.049(8) -0.006(6) 0.014(6) 0.002(5) O1W 0.054(5) 0.041(5) 0.041(4) 0.006(3) 0.016(4) 0.004(4) O2W 0.045(5) 0.032(5) 0.048(5) 0.004(4) 0.005(4) 0.005(4) O3W 0.033(4) 0.043(5) 0.060(5) 0.007(4) -0.005(4) -0.009(4) O4W 0.031(4) 0.039(5) 0.057(5) 0.000(4) 0.007(4) 0.007(4) O5W 0.045(5) 0.041(5) 0.042(5) -0.002(3) 0.015(4) 0.007(4) O6W 0.045(5) 0.035(5) 0.045(5) -0.005(3) 0.011(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O10 2.371(7) 2_655 ? Nd1 O3 2.409(6) . ? Nd1 O8 2.465(7) 3_676 ? Nd1 O3W 2.485(7) . ? Nd1 O2W 2.497(7) . ? Nd1 O1W 2.523(7) . ? Nd1 O5W 2.543(6) . ? Nd1 O6W 2.560(7) . ? Nd1 O4W 2.594(7) . ? Mo1 O1 1.685(6) . ? Mo1 O3 1.746(6) . ? Mo1 O2 1.775(6) . ? Mo1 O6 2.097(6) 1_655 ? Mo1 O7 2.224(6) . ? Mo1 N1 2.264(8) . ? Mo2 O5 1.675(6) . ? Mo2 O4 1.699(6) . ? Mo2 O6 1.800(6) . ? Mo2 O2 2.050(6) . ? Mo2 O11 2.231(7) . ? Mo2 N2 2.312(8) . ? O6 Mo1 2.097(6) 1_455 ? O7 C6 1.271(11) . ? O8 C6 1.239(11) . ? O8 Nd1 2.465(7) 3_676 ? O9 C7 1.248(12) . ? O10 C7 1.231(11) . ? O10 Nd1 2.371(7) 2_645 ? O11 C13 1.274(12) . ? O12 C13 1.264(11) . ? O13 C14 1.264(12) . ? O14 C14 1.190(11) . ? N2 C8 1.328(12) . ? N2 C12 1.339(12) . ? N1 C5 1.335(11) . ? N1 C1 1.358(12) . ? C1 C2 1.358(13) . ? C1 H1A 0.9300 . ? C2 C3 1.385(13) . ? C2 C7 1.507(13) . ? C3 C4 1.374(13) . ? C3 H3A 0.9300 . ? C4 C5 1.390(12) . ? C4 H4A 0.9300 . ? C5 C6 1.498(13) . ? C8 C9 1.401(13) . ? C8 H8A 0.9300 . ? C9 C10 1.388(14) . ? C9 C14 1.512(13) . ? C10 C11 1.386(13) . ? C10 H10A 0.9300 . ? C11 C12 1.378(13) . ? C11 H11A 0.9300 . ? C12 C13 1.501(14) . ? _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 O10 Nd1 O3 113.9(2) 2_655 . ? O10 Nd1 O8 115.0(2) 2_655 3_676 ? O3 Nd1 O8 131.1(2) . 3_676 ? O10 Nd1 O3W 74.4(2) 2_655 . ? O3 Nd1 O3W 70.1(2) . . ? O8 Nd1 O3W 126.0(2) 3_676 . ? O10 Nd1 O2W 138.4(2) 2_655 . ? O3 Nd1 O2W 70.5(2) . . ? O8 Nd1 O2W 72.1(2) 3_676 . ? O3W Nd1 O2W 137.2(2) . . ? O10 Nd1 O1W 142.9(2) 2_655 . ? O3 Nd1 O1W 70.5(2) . . ? O8 Nd1 O1W 72.1(2) 3_676 . ? O3W Nd1 O1W 73.2(2) . . ? O2W Nd1 O1W 78.6(2) . . ? O10 Nd1 O5W 70.6(2) 2_655 . ? O3 Nd1 O5W 68.6(2) . . ? O8 Nd1 O5W 127.6(2) 3_676 . ? O3W Nd1 O5W 106.2(2) . . ? O2W Nd1 O5W 73.7(2) . . ? O1W Nd1 O5W 136.2(2) . . ? O10 Nd1 O6W 72.2(2) 2_655 . ? O3 Nd1 O6W 130.7(2) . . ? O8 Nd1 O6W 65.1(2) 3_676 . ? O3W Nd1 O6W 146.0(2) . . ? O2W Nd1 O6W 75.3(2) . . ? O1W Nd1 O6W 134.9(2) . . ? O5W Nd1 O6W 68.5(2) . . ? O10 Nd1 O4W 72.3(2) 2_655 . ? O3 Nd1 O4W 130.8(2) . . ? O8 Nd1 O4W 68.2(2) 3_676 . ? O3W Nd1 O4W 65.0(2) . . ? O2W Nd1 O4W 138.4(2) . . ? O1W Nd1 O4W 78.0(2) . . ? O5W Nd1 O4W 142.9(2) . . ? O6W Nd1 O4W 98.3(2) . . ? O1 Mo1 O3 107.5(3) . . ? O1 Mo1 O2 100.0(3) . . ? O3 Mo1 O2 103.5(3) . . ? O1 Mo1 O6 90.7(3) . 1_655 ? O3 Mo1 O6 88.6(3) . 1_655 ? O2 Mo1 O6 160.4(3) . 1_655 ? O1 Mo1 O7 159.3(3) . . ? O3 Mo1 O7 89.2(3) . . ? O2 Mo1 O7 87.4(3) . . ? O6 Mo1 O7 77.2(2) 1_655 . ? O1 Mo1 N1 89.7(3) . . ? O3 Mo1 N1 156.5(3) . . ? O2 Mo1 N1 88.7(3) . . ? O6 Mo1 N1 74.9(3) 1_655 . ? O7 Mo1 N1 71.0(3) . . ? O5 Mo2 O4 105.3(3) . . ? O5 Mo2 O6 102.5(3) . . ? O4 Mo2 O6 101.3(3) . . ? O5 Mo2 O2 94.7(3) . . ? O4 Mo2 O2 89.0(3) . . ? O6 Mo2 O2 156.7(3) . . ? O5 Mo2 O11 156.0(3) . . ? O4 Mo2 O11 97.8(3) . . ? O6 Mo2 O11 79.0(3) . . ? O2 Mo2 O11 79.0(2) . . ? O5 Mo2 N2 86.4(3) . . ? O4 Mo2 N2 159.6(3) . . ? O6 Mo2 N2 92.2(3) . . ? O2 Mo2 N2 73.2(3) . . ? O11 Mo2 N2 69.7(3) . . ? Mo1 O2 Mo2 159.9(4) . . ? Mo1 O3 Nd1 162.0(4) . . ? Mo2 O6 Mo1 142.8(4) . 1_455 ? C6 O7 Mo1 121.2(6) . . ? C6 O8 Nd1 151.4(7) . 3_676 ? C7 O10 Nd1 171.8(7) . 2_645 ? C13 O11 Mo2 121.9(7) . . ? C8 N2 C12 117.7(9) . . ? C8 N2 Mo2 122.2(7) . . ? C12 N2 Mo2 118.4(7) . . ? C5 N1 C1 117.7(8) . . ? C5 N1 Mo1 116.9(6) . . ? C1 N1 Mo1 124.9(7) . . ? N1 C1 C2 123.2(9) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C1 C2 C3 118.2(9) . . ? C1 C2 C7 119.4(10) . . ? C3 C2 C7 122.4(10) . . ? C4 C3 C2 120.2(10) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 117.9(9) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? N1 C5 C4 122.8(9) . . ? N1 C5 C6 115.3(9) . . ? C4 C5 C6 122.0(9) . . ? O8 C6 O7 125.8(10) . . ? O8 C6 C5 119.1(10) . . ? O7 C6 C5 115.0(9) . . ? O10 C7 O9 125.2(10) . . ? O10 C7 C2 116.8(10) . . ? O9 C7 C2 117.9(10) . . ? N2 C8 C9 122.4(10) . . ? N2 C8 H8A 118.8 . . ? C9 C8 H8A 118.8 . . ? C10 C9 C8 118.6(10) . . ? C10 C9 C14 123.4(10) . . ? C8 C9 C14 117.9(10) . . ? C9 C10 C11 119.0(10) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 117.7(10) . . ? C12 C11 H11A 121.2 . . ? C10 C11 H11A 121.2 . . ? N2 C12 C11 124.3(9) . . ? N2 C12 C13 113.0(9) . . ? C11 C12 C13 122.6(10) . . ? O12 C13 O11 123.2(10) . . ? O12 C13 C12 120.6(10) . . ? O11 C13 C12 116.2(10) . . ? O14 C14 O13 124.3(11) . . ? O14 C14 C9 120.4(11) . . ? O13 C14 C9 115.1(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.702 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.202 data_5 _database_code_depnum_ccdc_archive 'CCDC 888173' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 Eu2 Mo4 N4 O41' _chemical_formula_weight 1776.3 _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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5163(7) _cell_length_b 20.764(2) _cell_length_c 15.2434(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.337(2) _cell_angle_gamma 90.00 _cell_volume 2364.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 723 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 19.84 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 3.769 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3140 _exptl_absorpt_correction_T_max 0.6400 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11879 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4147 _reflns_number_gt 3594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0376P)^2^+2.7501P] 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 4147 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _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 Eu1 Eu 0.42698(3) 1.035980(11) 0.273950(15) 0.01698(9) Uani 1 1 d . . . Mo1 Mo 0.42951(5) 0.845879(19) 0.34567(3) 0.01296(11) Uani 1 1 d . . . Mo2 Mo -0.07092(5) 0.84399(2) 0.34430(3) 0.01695(12) Uani 1 1 d . . . O1 O 0.4355(6) 0.79329(18) 0.2609(2) 0.0355(10) Uani 1 1 d . . . O2 O 0.2042(5) 0.8393(2) 0.3693(3) 0.0372(10) Uani 1 1 d . . . O3 O 0.4310(5) 0.92254(17) 0.2999(2) 0.0274(8) Uani 1 1 d . . . O4 O -0.0496(5) 0.91496(18) 0.2854(3) 0.0337(10) Uani 1 1 d . . . O5 O -0.0826(6) 0.7838(2) 0.2686(2) 0.0404(10) Uani 1 1 d . . . O6 O -0.2949(5) 0.84912(19) 0.3710(3) 0.0328(9) Uani 1 1 d . . . O7 O 0.4715(5) 0.88739(16) 0.4829(2) 0.0270(8) Uani 1 1 d . . . O8 O 0.5759(5) 0.87381(17) 0.6240(2) 0.0284(9) Uani 1 1 d . . . O9 O 0.7238(6) 0.55425(18) 0.5153(3) 0.0432(11) Uani 1 1 d . . . O10 O 0.5782(5) 0.57062(16) 0.3828(2) 0.0248(8) Uani 1 1 d . . . O11 O -0.0205(5) 0.89100(17) 0.4767(2) 0.0299(9) Uani 1 1 d . . . O12 O 0.0297(5) 0.88200(19) 0.6221(2) 0.0336(9) Uani 1 1 d . . . O13 O 0.2308(6) 0.55886(18) 0.5264(2) 0.0355(10) Uani 1 1 d . . . O14 O 0.1333(5) 0.58103(17) 0.3876(2) 0.0327(9) Uani 1 1 d . . . N2 N -0.0013(5) 0.76610(18) 0.4518(3) 0.0174(9) Uani 1 1 d . . . N1 N 0.5091(5) 0.76374(18) 0.4458(3) 0.0153(8) Uani 1 1 d . . . C1 C 0.5328(6) 0.7027(2) 0.4248(3) 0.0160(10) Uani 1 1 d . . . H1A H 0.4999 0.6896 0.3670 0.019 Uiso 1 1 calc R . . C2 C 0.6049(6) 0.6575(2) 0.4859(3) 0.0166(10) Uani 1 1 d . . . C3 C 0.6524(7) 0.6767(2) 0.5722(3) 0.0230(11) Uani 1 1 d . . . H3A H 0.6999 0.6472 0.6143 0.028 Uiso 1 1 calc R . . C4 C 0.6282(7) 0.7406(2) 0.5950(3) 0.0216(11) Uani 1 1 d . . . H4A H 0.6586 0.7546 0.6527 0.026 Uiso 1 1 calc R . . C5 C 0.5589(6) 0.7826(2) 0.5309(3) 0.0154(10) Uani 1 1 d . . . C6 C 0.5351(6) 0.8534(2) 0.5479(3) 0.0179(10) Uani 1 1 d . . . C7 C 0.6344(7) 0.5891(2) 0.4565(3) 0.0197(11) Uani 1 1 d . . . C8 C 0.0317(6) 0.7047(2) 0.4336(3) 0.0186(10) Uani 1 1 d . . . H8A H -0.0026 0.6896 0.3768 0.022 Uiso 1 1 calc R . . C9 C 0.1140(6) 0.6628(2) 0.4948(3) 0.0174(10) Uani 1 1 d . . . C10 C 0.1607(7) 0.6844(3) 0.5799(3) 0.0252(12) Uani 1 1 d . . . H10A H 0.2144 0.6567 0.6230 0.030 Uiso 1 1 calc R . . C11 C 0.1256(7) 0.7489(2) 0.6004(3) 0.0244(11) Uani 1 1 d . . . H11A H 0.1547 0.7646 0.6573 0.029 Uiso 1 1 calc R . . C12 C 0.0479(6) 0.7877(2) 0.5349(3) 0.0176(10) Uani 1 1 d . . . C13 C 0.0174(7) 0.8592(2) 0.5460(4) 0.0226(11) Uani 1 1 d . . . C14 C 0.1589(6) 0.5959(2) 0.4663(3) 0.0192(11) Uani 1 1 d . . . O1W O 0.2069(5) 1.01130(18) 0.3813(2) 0.0309(9) Uani 1 1 d . . . O2W O 0.6453(5) 1.01145(18) 0.4036(2) 0.0348(9) Uani 1 1 d . . . O3W O 0.1703(5) 0.98369(17) 0.1890(2) 0.0264(8) Uani 1 1 d . . . O4W O 0.1794(5) 1.11421(17) 0.2336(2) 0.0288(9) Uani 1 1 d . . . O5W O 0.6660(5) 0.98322(19) 0.2030(3) 0.0372(10) Uani 1 1 d . . . O6W O 0.6705(5) 1.11603(19) 0.2556(2) 0.0333(9) Uani 1 1 d . . . O7W O 0.0743(9) 0.9655(3) 0.7276(5) 0.0300(18) Uani 0.50 1 d P . . _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 Eu1 0.01987(15) 0.01495(14) 0.01589(14) 0.00041(10) 0.00088(10) 0.00093(10) Mo1 0.0100(2) 0.0133(2) 0.0154(2) 0.00164(15) 0.00046(16) 0.00158(15) Mo2 0.0106(2) 0.0198(2) 0.0203(2) 0.00632(17) 0.00094(17) 0.00114(16) O1 0.060(3) 0.025(2) 0.020(2) -0.0037(16) -0.0032(19) 0.0107(19) O2 0.0128(19) 0.053(3) 0.046(3) 0.019(2) 0.0045(17) 0.0037(17) O3 0.035(2) 0.0194(19) 0.028(2) 0.0052(15) 0.0007(17) 0.0015(16) O4 0.026(2) 0.030(2) 0.046(2) 0.0231(18) 0.0043(18) 0.0010(16) O5 0.055(3) 0.038(3) 0.025(2) -0.0038(18) -0.008(2) 0.004(2) O6 0.0127(19) 0.044(3) 0.042(2) 0.0182(18) 0.0058(17) -0.0003(16) O7 0.045(2) 0.0153(19) 0.0199(19) 0.0005(15) -0.0010(16) 0.0103(16) O8 0.042(2) 0.023(2) 0.0190(19) -0.0061(16) -0.0035(16) 0.0022(17) O9 0.076(3) 0.025(2) 0.025(2) -0.0008(17) -0.010(2) 0.025(2) O10 0.034(2) 0.0183(19) 0.022(2) -0.0046(15) 0.0011(16) 0.0030(15) O11 0.038(2) 0.0174(19) 0.033(2) -0.0005(17) -0.0029(17) 0.0075(16) O12 0.037(2) 0.036(2) 0.027(2) -0.0136(18) -0.0016(17) 0.0043(18) O13 0.063(3) 0.022(2) 0.021(2) 0.0034(16) 0.0022(19) 0.0158(19) O14 0.049(3) 0.024(2) 0.024(2) -0.0034(16) -0.0011(18) 0.0101(18) N2 0.017(2) 0.017(2) 0.018(2) 0.0026(17) 0.0021(17) 0.0018(16) N1 0.016(2) 0.012(2) 0.018(2) -0.0024(16) 0.0013(16) -0.0031(16) C1 0.019(3) 0.016(3) 0.013(2) -0.0038(19) 0.0003(19) -0.0021(19) C2 0.015(2) 0.014(3) 0.021(3) -0.0005(19) 0.005(2) 0.0011(18) C3 0.030(3) 0.017(3) 0.021(3) 0.004(2) -0.001(2) 0.004(2) C4 0.027(3) 0.022(3) 0.016(3) 0.001(2) -0.001(2) 0.000(2) C5 0.013(2) 0.012(2) 0.023(3) -0.0016(19) 0.007(2) 0.0004(18) C6 0.016(3) 0.017(3) 0.021(3) -0.006(2) 0.006(2) -0.0030(19) C7 0.023(3) 0.018(3) 0.018(3) -0.001(2) 0.003(2) 0.003(2) C8 0.019(3) 0.018(3) 0.018(3) -0.001(2) 0.002(2) 0.004(2) C9 0.016(2) 0.015(2) 0.022(3) -0.001(2) 0.005(2) 0.0000(19) C10 0.030(3) 0.026(3) 0.019(3) 0.002(2) -0.002(2) 0.002(2) C11 0.027(3) 0.024(3) 0.021(3) 0.000(2) -0.003(2) 0.002(2) C12 0.014(2) 0.018(3) 0.021(3) -0.003(2) 0.004(2) 0.0022(19) C13 0.017(3) 0.021(3) 0.030(3) -0.008(2) 0.001(2) 0.002(2) C14 0.019(3) 0.020(3) 0.019(3) 0.003(2) 0.005(2) 0.001(2) O1W 0.037(2) 0.025(2) 0.032(2) -0.0043(17) 0.0120(18) -0.0020(17) O2W 0.043(2) 0.028(2) 0.030(2) 0.0017(17) -0.0078(18) -0.0012(18) O3W 0.025(2) 0.028(2) 0.025(2) 0.0006(16) -0.0011(16) -0.0059(16) O4W 0.031(2) 0.026(2) 0.028(2) -0.0002(16) -0.0036(16) 0.0052(17) O5W 0.040(2) 0.040(2) 0.034(2) 0.0097(18) 0.0161(19) 0.0173(19) O6W 0.032(2) 0.034(2) 0.033(2) 0.0006(18) 0.0011(17) -0.0113(18) O7W 0.027(4) 0.022(4) 0.040(5) -0.001(3) -0.001(4) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.388(3) . ? Eu1 O8 2.437(3) 3_676 ? Eu1 O5W 2.455(4) . ? Eu1 O3W 2.455(3) . ? Eu1 O2W 2.479(4) . ? Eu1 O10 2.492(3) 2_655 ? Eu1 O4W 2.496(4) . ? Eu1 O1W 2.505(4) . ? Eu1 O6W 2.511(4) . ? Mo1 O1 1.696(4) . ? Mo1 O3 1.739(3) . ? Mo1 O2 1.775(4) . ? Mo1 O6 2.066(4) 1_655 ? Mo1 O7 2.252(3) . ? Mo1 N1 2.323(4) . ? Mo2 O5 1.697(4) . ? Mo2 O4 1.742(3) . ? Mo2 O6 1.778(3) . ? Mo2 O2 2.063(4) . ? Mo2 O11 2.236(4) . ? Mo2 N2 2.321(4) . ? O6 Mo1 2.066(3) 1_455 ? O7 C6 1.267(6) . ? O8 C6 1.241(6) . ? O8 Eu1 2.437(3) 3_676 ? O9 C7 1.283(6) . ? O10 C7 1.218(6) . ? O10 Eu1 2.492(3) 2_645 ? O11 C13 1.253(6) . ? O12 C13 1.246(6) . ? O13 C14 1.271(6) . ? O14 C14 1.234(6) . ? N2 C8 1.334(6) . ? N2 C12 1.357(6) . ? N1 C1 1.324(6) . ? N1 C5 1.367(6) . ? C1 C2 1.389(6) . ? C1 H1A 0.9300 . ? C2 C3 1.383(7) . ? C2 C7 1.512(6) . ? C3 C4 1.390(7) . ? C3 H3A 0.9300 . ? C4 C5 1.368(7) . ? C4 H4A 0.9300 . ? C5 C6 1.507(6) . ? C8 C9 1.371(7) . ? C8 H8A 0.9300 . ? C9 C10 1.381(7) . ? C9 C14 1.505(7) . ? C10 C11 1.407(7) . ? C10 H10A 0.9300 . ? C11 C12 1.364(7) . ? C11 H11A 0.9300 . ? C12 C13 1.513(7) . ? _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 O3 Eu1 O8 130.79(12) . 3_676 ? O3 Eu1 O5W 68.67(13) . . ? O8 Eu1 O5W 133.07(14) 3_676 . ? O3 Eu1 O3W 69.28(12) . . ? O8 Eu1 O3W 127.96(12) 3_676 . ? O5W Eu1 O3W 98.10(14) . . ? O3 Eu1 O2W 70.72(12) . . ? O8 Eu1 O2W 72.58(12) 3_676 . ? O5W Eu1 O2W 78.88(14) . . ? O3W Eu1 O2W 137.95(12) . . ? O3 Eu1 O10 116.25(12) . 2_655 ? O8 Eu1 O10 112.96(11) 3_676 2_655 ? O5W Eu1 O10 68.97(12) . 2_655 ? O3W Eu1 O10 72.14(12) . 2_655 ? O2W Eu1 O10 139.73(13) . 2_655 ? O3 Eu1 O4W 132.72(12) . . ? O8 Eu1 O4W 66.30(12) 3_676 . ? O5W Eu1 O4W 138.08(12) . . ? O3W Eu1 O4W 68.69(12) . . ? O2W Eu1 O4W 137.76(12) . . ? O10 Eu1 O4W 69.12(12) 2_655 . ? O3 Eu1 O1W 71.78(12) . . ? O8 Eu1 O1W 71.76(12) 3_676 . ? O5W Eu1 O1W 139.88(13) . . ? O3W Eu1 O1W 73.57(12) . . ? O2W Eu1 O1W 82.18(13) . . ? O10 Eu1 O1W 138.07(12) 2_655 . ? O4W Eu1 O1W 76.45(12) . . ? O3 Eu1 O6W 132.48(13) . . ? O8 Eu1 O6W 67.68(13) 3_676 . ? O5W Eu1 O6W 70.63(14) . . ? O3W Eu1 O6W 140.70(12) . . ? O2W Eu1 O6W 78.37(13) . . ? O10 Eu1 O6W 68.67(12) 2_655 . ? O4W Eu1 O6W 94.27(13) . . ? O1W Eu1 O6W 138.62(12) . . ? O1 Mo1 O3 106.39(17) . . ? O1 Mo1 O2 102.2(2) . . ? O3 Mo1 O2 101.59(18) . . ? O1 Mo1 O6 93.05(18) . 1_655 ? O3 Mo1 O6 89.67(16) . 1_655 ? O2 Mo1 O6 157.50(19) . 1_655 ? O1 Mo1 O7 160.24(15) . . ? O3 Mo1 O7 90.90(15) . . ? O2 Mo1 O7 83.13(17) . . ? O6 Mo1 O7 77.22(15) 1_655 . ? O1 Mo1 N1 90.08(16) . . ? O3 Mo1 N1 157.42(15) . . ? O2 Mo1 N1 89.55(16) . . ? O6 Mo1 N1 73.79(14) 1_655 . ? O7 Mo1 N1 70.80(12) . . ? O5 Mo2 O4 105.8(2) . . ? O5 Mo2 O6 102.8(2) . . ? O4 Mo2 O6 102.14(17) . . ? O5 Mo2 O2 93.80(19) . . ? O4 Mo2 O2 89.32(16) . . ? O6 Mo2 O2 156.25(19) . . ? O5 Mo2 O11 157.88(16) . . ? O4 Mo2 O11 94.57(17) . . ? O6 Mo2 O11 80.64(17) . . ? O2 Mo2 O11 77.74(16) . . ? O5 Mo2 N2 87.59(17) . . ? O4 Mo2 N2 157.97(16) . . ? O6 Mo2 N2 91.46(15) . . ? O2 Mo2 N2 72.13(14) . . ? O11 Mo2 N2 70.40(13) . . ? Mo1 O2 Mo2 156.6(2) . . ? Mo1 O3 Eu1 165.7(2) . . ? Mo2 O6 Mo1 155.5(2) . 1_455 ? C6 O7 Mo1 121.0(3) . . ? C6 O8 Eu1 147.2(3) . 3_676 ? C7 O10 Eu1 160.5(3) . 2_645 ? C13 O11 Mo2 122.1(3) . . ? C8 N2 C12 118.2(4) . . ? C8 N2 Mo2 123.5(3) . . ? C12 N2 Mo2 116.5(3) . . ? C1 N1 C5 118.2(4) . . ? C1 N1 Mo1 125.2(3) . . ? C5 N1 Mo1 115.9(3) . . ? N1 C1 C2 122.6(4) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 C7 121.4(4) . . ? C1 C2 C7 119.7(4) . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 122.6(4) . . ? N1 C5 C6 114.6(4) . . ? C4 C5 C6 122.8(4) . . ? O8 C6 O7 125.0(4) . . ? O8 C6 C5 118.2(4) . . ? O7 C6 C5 116.8(4) . . ? O10 C7 O9 124.7(5) . . ? O10 C7 C2 121.4(4) . . ? O9 C7 C2 113.9(4) . . ? N2 C8 C9 123.0(5) . . ? N2 C8 H8A 118.5 . . ? C9 C8 H8A 118.5 . . ? C8 C9 C10 118.9(5) . . ? C8 C9 C14 119.2(4) . . ? C10 C9 C14 121.9(4) . . ? C9 C10 C11 118.8(5) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C12 C11 C10 118.5(5) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N2 C12 C11 122.6(5) . . ? N2 C12 C13 113.6(4) . . ? C11 C12 C13 123.8(5) . . ? O12 C13 O11 124.8(5) . . ? O12 C13 C12 118.7(5) . . ? O11 C13 C12 116.5(4) . . ? O14 C14 O13 123.9(5) . . ? O14 C14 C9 119.7(4) . . ? O13 C14 C9 116.3(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.845 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.131 data_6 _database_code_depnum_ccdc_archive 'CCDC 888174' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H7 Mo2 N2 O20 Sm' _chemical_formula_weight 865.44 _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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 3.7485(9) _cell_length_b 20.733(5) _cell_length_c 15.234(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.310(5) _cell_angle_gamma 90.00 _cell_volume 1176.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 510 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 19.85 _exptl_crystal_description bar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 3.612 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3190 _exptl_absorpt_correction_T_max 0.7369 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5922 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.1182 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2079 _reflns_number_gt 1472 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^+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 2079 _refine_ls_number_parameters 181 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.735 _refine_ls_restrained_S_all 0.738 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -1.14556(15) 1.34430(3) -0.15491(4) 0.01612(18) Uani 1 1 d . . . Sm1 Sm -0.85259(19) 1.03546(3) -0.27358(4) 0.01523(19) Uani 0.50 1 d P . . N1 N -0.9977(14) 1.2644(3) -0.0514(3) 0.0163(13) Uani 1 1 d . . . O1 O -1.1507(14) 1.2883(2) -0.2344(3) 0.0426(15) Uani 1 1 d . . . O2 O -1.1211(13) 1.4178(2) -0.2059(3) 0.0421(15) Uani 1 1 d . . . O3 O -1.5999(11) 1.3435(3) -0.1321(3) 0.0371(14) Uani 1 1 d U . . O4 O -1.0525(13) 1.3879(2) -0.0206(3) 0.0309(13) Uani 1 1 d . . . O5 O -0.8979(15) 1.3768(2) 0.1228(3) 0.0438(16) Uani 1 1 d . . . O6 O -0.5509(15) 1.0556(2) 0.0211(3) 0.0451(16) Uani 1 1 d . . . O7 O -0.7968(16) 1.0748(2) -0.1145(3) 0.0456(16) Uani 1 1 d . . . O8 O -1.3490(13) 1.1144(2) -0.2444(4) 0.0427(15) Uani 1 1 d . . . O9 O -1.3349(13) 0.9822(2) -0.1959(3) 0.0354(14) Uani 1 1 d . . . O10 O -0.3480(17) 1.0105(3) -0.3932(4) 0.066(2) Uani 1 1 d . . . C1 C -0.8977(17) 1.2844(3) 0.0321(4) 0.0157(15) Uani 1 1 d . . . C2 C -0.7510(18) 1.2439(3) 0.0973(5) 0.0252(18) Uani 1 1 d . . . H2A H -0.6911 1.2588 0.1546 0.030 Uiso 1 1 calc R . . C3 C -0.6938(18) 1.1798(3) 0.0755(5) 0.0266(18) Uani 1 1 d . . . H3A H -0.5941 1.1511 0.1183 0.032 Uiso 1 1 calc R . . C4 C -0.7863(17) 1.1592(3) -0.0102(4) 0.0182(16) Uani 1 1 d . . . C5 C -0.9397(17) 1.2034(3) -0.0715(5) 0.0198(16) Uani 1 1 d . . . H5A H -1.0047 1.1896 -0.1291 0.024 Uiso 1 1 calc R . . C6 C -0.7091(19) 1.0923(3) -0.0375(5) 0.0258(18) Uani 1 1 d . . . C7 C -0.9509(18) 1.3548(3) 0.0469(5) 0.0224(17) Uani 1 1 d . . . _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 0.0101(3) 0.0212(3) 0.0174(3) 0.0045(3) 0.0033(2) 0.0019(3) Sm1 0.0173(4) 0.0167(4) 0.0121(4) -0.0007(3) 0.0033(3) -0.0012(3) N1 0.011(3) 0.021(3) 0.018(3) 0.000(3) 0.005(2) -0.002(3) O1 0.051(4) 0.043(3) 0.030(3) -0.008(3) -0.012(3) 0.014(3) O2 0.033(3) 0.041(3) 0.049(4) 0.018(3) -0.008(3) -0.005(3) O3 0.006(2) 0.067(4) 0.038(3) 0.020(3) 0.000(2) 0.002(3) O4 0.043(3) 0.021(3) 0.029(3) -0.006(3) 0.004(3) 0.007(3) O5 0.074(4) 0.039(3) 0.018(3) -0.013(3) 0.001(3) -0.007(3) O6 0.077(5) 0.036(3) 0.021(3) 0.004(3) 0.001(3) 0.028(3) O7 0.079(5) 0.038(3) 0.020(3) -0.002(3) 0.006(3) 0.025(3) O8 0.036(3) 0.040(3) 0.049(4) -0.003(3) -0.008(3) 0.002(3) O9 0.030(3) 0.032(3) 0.046(4) -0.006(3) 0.012(3) -0.007(3) O10 0.103(6) 0.035(4) 0.050(4) -0.005(3) -0.037(4) 0.006(4) C1 0.010(3) 0.019(4) 0.019(4) 0.001(3) 0.008(3) 0.000(3) C2 0.027(4) 0.032(5) 0.016(4) -0.003(4) 0.000(3) 0.000(4) C3 0.029(4) 0.027(4) 0.023(4) 0.016(4) -0.001(3) 0.010(4) C4 0.019(4) 0.019(4) 0.018(4) 0.004(3) 0.006(3) 0.003(3) C5 0.019(4) 0.017(4) 0.024(4) -0.004(3) 0.006(3) -0.006(3) C6 0.022(4) 0.028(5) 0.030(5) 0.004(4) 0.011(4) 0.002(4) C7 0.021(4) 0.025(4) 0.022(4) 0.001(4) 0.005(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _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 1.676(5) . ? Mo1 O2 1.717(5) . ? Mo1 O3 1.775(4) . ? Mo1 O3 2.037(4) 1_655 ? Mo1 O4 2.229(5) . ? Mo1 N1 2.313(5) . ? Sm1 O5 2.402(5) 4_585 ? Sm1 O9 2.425(5) 1_655 ? Sm1 O2 2.461(5) 2_344 ? Sm1 O8 2.501(5) 1_655 ? Sm1 O10 2.509(6) 1_455 ? Sm1 O9 2.521(5) . ? Sm1 O7 2.544(5) . ? Sm1 O8 2.554(5) . ? Sm1 O10 2.815(7) . ? Sm1 Sm1 3.7485(9) 1_655 ? Sm1 Sm1 3.7485(9) 1_455 ? N1 C5 1.325(8) . ? N1 C1 1.352(8) . ? O2 Sm1 2.461(5) 2_354 ? O3 Mo1 2.037(4) 1_455 ? O4 C7 1.259(8) . ? O5 C7 1.239(8) . ? O5 Sm1 2.402(5) 4_586 ? O6 C6 1.269(8) . ? O7 C6 1.238(8) . ? O8 Sm1 2.501(5) 1_455 ? O9 Sm1 2.425(5) 1_455 ? O10 Sm1 2.509(6) 1_655 ? C1 C2 1.369(8) . ? C1 C7 1.495(9) . ? C2 C3 1.392(9) . ? C2 H2A 0.9300 . ? C3 C4 1.381(9) . ? C3 H3A 0.9300 . ? C4 C5 1.387(8) . ? C4 C6 1.484(9) . ? C5 H5A 0.9300 . ? _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 106.6(3) . . ? O1 Mo1 O3 101.5(3) . . ? O2 Mo1 O3 101.4(2) . . ? O1 Mo1 O3 92.8(2) . 1_655 ? O2 Mo1 O3 89.0(2) . 1_655 ? O3 Mo1 O3 159.0(3) . 1_655 ? O1 Mo1 O4 158.8(2) . . ? O2 Mo1 O4 92.6(2) . . ? O3 Mo1 O4 83.1(2) . . ? O3 Mo1 O4 78.08(19) 1_655 . ? O1 Mo1 N1 88.8(2) . . ? O2 Mo1 N1 157.5(2) . . ? O3 Mo1 N1 91.3(2) . . ? O3 Mo1 N1 73.54(19) 1_655 . ? O4 Mo1 N1 70.32(18) . . ? O5 Sm1 O9 131.32(18) 4_585 1_655 ? O5 Sm1 O2 131.96(17) 4_585 2_344 ? O9 Sm1 O2 68.25(16) 1_655 2_344 ? O5 Sm1 O8 67.59(18) 4_585 1_655 ? O9 Sm1 O8 70.30(16) 1_655 1_655 ? O2 Sm1 O8 133.66(17) 2_344 1_655 ? O5 Sm1 O10 71.69(19) 4_585 1_455 ? O9 Sm1 O10 138.54(17) 1_655 1_455 ? O2 Sm1 O10 71.75(16) 2_344 1_455 ? O8 Sm1 O10 138.44(19) 1_655 1_455 ? O5 Sm1 O9 129.59(18) 4_585 . ? O9 Sm1 O9 98.55(18) 1_655 . ? O2 Sm1 O9 66.72(17) 2_344 . ? O8 Sm1 O9 140.27(17) 1_655 . ? O10 Sm1 O9 74.9(2) 1_455 . ? O5 Sm1 O7 112.04(17) 4_585 . ? O9 Sm1 O7 72.76(17) 1_655 . ? O2 Sm1 O7 115.93(17) 2_344 . ? O8 Sm1 O7 68.84(19) 1_655 . ? O10 Sm1 O7 137.3(2) 1_455 . ? O9 Sm1 O7 71.43(18) . . ? O5 Sm1 O8 68.22(18) 4_585 . ? O9 Sm1 O8 140.01(17) 1_655 . ? O2 Sm1 O8 129.63(17) 2_344 . ? O8 Sm1 O8 95.73(17) 1_655 . ? O10 Sm1 O8 76.32(18) 1_455 . ? O9 Sm1 O8 67.97(16) . . ? O7 Sm1 O8 67.26(17) . . ? O5 Sm1 O10 73.62(17) 4_585 . ? O9 Sm1 O10 70.94(17) 1_655 . ? O2 Sm1 O10 75.86(17) 2_344 . ? O8 Sm1 O10 71.81(17) 1_655 . ? O10 Sm1 O10 89.32(18) 1_455 . ? O9 Sm1 O10 142.25(16) . . ? O7 Sm1 O10 133.24(18) . . ? O8 Sm1 O10 141.72(17) . . ? O5 Sm1 Sm1 89.91(14) 4_585 1_655 ? O9 Sm1 Sm1 41.69(12) 1_655 1_655 ? O2 Sm1 Sm1 91.50(12) 2_344 1_655 ? O8 Sm1 Sm1 42.67(12) 1_655 1_655 ? O10 Sm1 Sm1 131.33(16) 1_455 1_655 ? O9 Sm1 Sm1 140.23(12) . 1_655 ? O7 Sm1 Sm1 91.29(14) . 1_655 ? O8 Sm1 Sm1 138.41(11) . 1_655 ? O10 Sm1 Sm1 42.01(11) . 1_655 ? O5 Sm1 Sm1 90.09(14) 4_585 1_455 ? O9 Sm1 Sm1 138.31(12) 1_655 1_455 ? O2 Sm1 Sm1 88.50(12) 2_344 1_455 ? O8 Sm1 Sm1 137.33(12) 1_655 1_455 ? O10 Sm1 Sm1 48.67(16) 1_455 1_455 ? O9 Sm1 Sm1 39.77(12) . 1_455 ? O7 Sm1 Sm1 88.71(14) . 1_455 ? O8 Sm1 Sm1 41.59(11) . 1_455 ? O10 Sm1 Sm1 137.99(11) . 1_455 ? Sm1 Sm1 Sm1 180.00(2) 1_655 1_455 ? C5 N1 C1 118.3(6) . . ? C5 N1 Mo1 124.0(5) . . ? C1 N1 Mo1 116.3(4) . . ? Mo1 O2 Sm1 159.0(3) . 2_354 ? Mo1 O3 Mo1 159.0(3) . 1_455 ? C7 O4 Mo1 122.1(4) . . ? C7 O5 Sm1 152.2(5) . 4_586 ? C6 O7 Sm1 169.3(5) . . ? Sm1 O8 Sm1 95.73(17) 1_455 . ? Sm1 O9 Sm1 98.55(18) 1_455 . ? Sm1 O10 Sm1 89.32(18) 1_655 . ? N1 C1 C2 122.9(6) . . ? N1 C1 C7 114.4(6) . . ? C2 C1 C7 122.7(6) . . ? C1 C2 C3 118.2(6) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C4 C3 C2 119.5(6) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 118.3(6) . . ? C3 C4 C6 121.1(6) . . ? C5 C4 C6 120.5(6) . . ? N1 C5 C4 122.8(6) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O7 C6 O6 123.1(7) . . ? O7 C6 C4 119.9(7) . . ? O6 C6 C4 117.0(7) . . ? O5 C7 O4 124.5(7) . . ? O5 C7 C1 119.3(7) . . ? O4 C7 C1 116.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.775 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.131 data_7 _database_code_depnum_ccdc_archive 'CCDC 888175' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H45 Er2 Mo4 N4 Na O44' _chemical_formula_weight 1882.94 _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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 12.494(2) _cell_length_b 7.5743(14) _cell_length_c 16.854(2) _cell_angle_alpha 90.00 _cell_angle_beta 125.951(10) _cell_angle_gamma 90.00 _cell_volume 1291.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 510 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 20.67 _exptl_crystal_description bar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 907 _exptl_absorpt_coefficient_mu 4.289 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4521 _exptl_absorpt_correction_T_max 0.6271 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6214 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3407 _reflns_number_gt 2958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 3407 _refine_ls_number_parameters 380 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 Er1 Er 0.83534(10) 0.89034(8) 0.21650(9) 0.01712(19) Uani 1 1 d . . . Mo1 Mo 0.42507(12) 0.58112(15) 0.48705(11) 0.0123(3) Uani 1 1 d . . . Mo2 Mo 0.43382(11) 0.08139(14) 0.49213(10) 0.0111(3) Uani 1 1 d . . . Na1 Na 0.834(2) 1.3911(14) 0.2252(16) 0.014(4) Uani 0.50 1 d PU . . O1 O 0.4243(11) 0.3522(13) 0.4695(8) 0.020(2) Uani 1 1 d . . . O2 O 0.5849(10) 0.6092(13) 0.5903(8) 0.019(2) Uani 1 1 d U . . O3 O 0.3284(11) 0.5989(14) 0.5294(9) 0.021(2) Uani 1 1 d U . . O4 O 0.4272(11) 0.8562(13) 0.4692(9) 0.024(3) Uani 1 1 d . . . O5 O 0.2518(10) 0.6218(13) 0.3383(7) 0.014(2) Uani 1 1 d . . . O6 O 0.1661(13) 0.734(2) 0.1894(11) 0.044(4) Uani 1 1 d . . . O7 O 0.8647(12) 0.5424(19) 0.4381(10) 0.041(3) Uani 1 1 d . . . O8 O 0.7993(11) 0.6992(17) 0.3049(9) 0.034(3) Uani 1 1 d . . . O9 O 0.3382(10) 0.0957(13) 0.5352(8) 0.018(2) Uani 1 1 d U . . O10 O 0.5957(9) 0.8953(13) 0.0965(8) 0.017(2) Uani 1 1 d U . . O11 O 0.2568(10) 1.1187(13) 0.3402(8) 0.016(2) Uani 1 1 d . . . O12 O 0.1730(12) 1.2361(17) 0.1923(9) 0.028(3) Uani 1 1 d . . . O13 O 0.8731(11) 1.0347(19) 0.4571(9) 0.040(3) Uani 1 1 d . . . O14 O 0.7963(12) 1.0719(16) 0.3031(10) 0.034(3) Uani 1 1 d . . . N1 N 0.4917(13) 0.6104(16) 0.3807(10) 0.016(3) Uani 1 1 d . . . N2 N 0.4946(13) 1.1126(17) 0.3848(10) 0.016(3) Uani 1 1 d U . . C1 C 0.3932(15) 0.663(2) 0.2882(12) 0.020(3) Uani 1 1 d . . . C2 C 0.4127(16) 0.703(2) 0.2182(13) 0.026(4) Uani 1 1 d . . . H2A H 0.3424 0.7388 0.1558 0.031 Uiso 1 1 calc R . . C3 C 0.5371(18) 0.690(3) 0.2418(14) 0.020(4) Uani 1 1 d U . . H3A H 0.5531 0.7162 0.1958 0.023 Uiso 1 1 calc R . . C4 C 0.6413(14) 0.6353(18) 0.3374(11) 0.014(3) Uani 1 1 d . . . C5 C 0.6124(14) 0.5956(17) 0.3999(11) 0.013(3) Uani 1 1 d . . . H5A H 0.6809 0.5545 0.4615 0.016 Uiso 1 1 calc R . . C6 C 0.2582(15) 0.672(2) 0.2666(12) 0.019(3) Uani 1 1 d U . . C7 C 0.7811(17) 0.623(2) 0.3628(13) 0.022(4) Uani 1 1 d . . . C8 C 0.4050(14) 1.174(2) 0.2974(12) 0.018(3) Uani 1 1 d . . . C9 C 0.4277(17) 1.220(2) 0.2290(13) 0.021(4) Uani 1 1 d . . . H9A H 0.3613 1.2691 0.1690 0.025 Uiso 1 1 calc R . . C10 C 0.5537(16) 1.190(2) 0.2534(13) 0.018(4) Uani 1 1 d U . . H10A H 0.5736 1.2140 0.2093 0.022 Uiso 1 1 calc R . . C11 C 0.6497(14) 1.1218(18) 0.3469(12) 0.014(3) Uani 1 1 d U . . C12 C 0.6206(15) 1.0886(19) 0.4096(12) 0.017(3) Uani 1 1 d . . . H12A H 0.6869 1.0480 0.4721 0.021 Uiso 1 1 calc R . . C13 C 0.2662(14) 1.178(2) 0.2717(11) 0.016(3) Uani 1 1 d U . . C14 C 0.7861(15) 1.077(2) 0.3733(14) 0.027(4) Uani 1 1 d . . . O1W O 0.7704(10) 1.1443(13) 0.1186(9) 0.027(3) Uani 1 1 d . . . O2W O 1.0212(11) 1.0813(18) 0.3147(9) 0.038(3) Uani 1 1 d . . . O3W O 1.0291(10) 0.7088(15) 0.3197(9) 0.029(3) Uani 1 1 d . . . O4W O 0.7726(11) 0.6290(14) 0.1248(10) 0.032(3) Uani 1 1 d . . . O5W O 0.9426(10) 0.8842(14) 0.1381(9) 0.022(3) Uani 1 1 d . . . O6W O 0.1142(17) 0.903(2) 0.5103(12) 0.051(4) Uani 1 1 d . . . O7W O 1.0545(15) 1.3903(17) 0.4217(12) 0.051(4) Uani 1 1 d . . . O8W O 0.9345(11) 1.3853(15) 0.1228(10) 0.031(3) Uani 1 1 d . . . _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 Er1 0.0138(3) 0.0199(3) 0.0187(4) 0.0004(5) 0.0101(3) 0.0011(4) Mo1 0.0133(6) 0.0082(6) 0.0178(7) 0.0002(5) 0.0105(6) -0.0002(5) Mo2 0.0115(6) 0.0087(6) 0.0127(7) 0.0003(5) 0.0070(6) 0.0000(5) Na1 0.018(4) 0.020(4) 0.006(5) -0.002(3) 0.009(3) 0.000(3) O1 0.028(6) 0.017(6) 0.023(7) -0.001(4) 0.019(6) -0.010(5) O2 0.022(4) 0.022(4) 0.016(4) -0.001(3) 0.014(3) -0.001(3) O3 0.025(4) 0.027(4) 0.020(4) -0.003(3) 0.018(3) -0.002(3) O4 0.034(7) 0.017(6) 0.031(7) 0.002(5) 0.025(6) -0.005(5) O5 0.011(5) 0.028(6) 0.003(5) 0.002(4) 0.004(5) -0.001(4) O6 0.023(7) 0.067(11) 0.043(9) 0.018(8) 0.019(8) 0.020(8) O7 0.030(7) 0.063(9) 0.036(8) 0.024(7) 0.023(7) 0.027(6) O8 0.035(7) 0.043(8) 0.037(8) 0.018(6) 0.028(6) 0.013(6) O9 0.020(4) 0.022(4) 0.017(4) -0.001(3) 0.014(3) -0.002(3) O10 0.018(5) 0.026(5) 0.010(5) 0.003(4) 0.009(4) -0.002(4) O11 0.016(5) 0.028(6) 0.006(5) 0.004(4) 0.007(5) -0.001(4) O12 0.017(6) 0.038(8) 0.026(7) 0.005(6) 0.011(6) 0.010(6) O13 0.015(6) 0.073(10) 0.024(8) -0.002(7) 0.007(6) 0.012(6) O14 0.036(7) 0.050(9) 0.037(8) -0.009(6) 0.033(7) -0.004(6) N1 0.024(7) 0.014(6) 0.019(8) 0.005(5) 0.018(7) 0.004(5) N2 0.015(4) 0.018(4) 0.014(4) 0.001(3) 0.009(3) 0.001(3) C1 0.016(8) 0.016(8) 0.028(10) 0.008(7) 0.013(8) 0.007(6) C2 0.020(9) 0.039(11) 0.021(10) 0.009(8) 0.013(9) 0.011(8) C3 0.025(8) 0.029(8) 0.013(7) 0.005(6) 0.016(6) -0.001(6) C4 0.016(7) 0.017(8) 0.013(8) 0.006(6) 0.010(7) 0.005(6) C5 0.011(7) 0.013(7) 0.013(8) 0.000(6) 0.005(7) 0.001(6) C6 0.020(7) 0.023(7) 0.021(7) 0.001(6) 0.015(6) 0.005(6) C7 0.030(9) 0.027(9) 0.021(10) 0.005(7) 0.022(9) 0.002(7) C8 0.007(7) 0.018(8) 0.021(9) 0.003(7) 0.004(7) 0.003(6) C9 0.021(8) 0.024(10) 0.022(9) 0.007(7) 0.016(8) 0.005(7) C10 0.022(5) 0.024(5) 0.015(5) 0.001(3) 0.014(4) 0.000(4) C11 0.015(4) 0.016(4) 0.013(4) -0.002(3) 0.010(3) 0.001(3) C12 0.011(7) 0.027(9) 0.017(9) -0.006(7) 0.010(7) 0.000(6) C13 0.015(4) 0.018(5) 0.016(5) -0.004(3) 0.011(4) 0.000(3) C14 0.010(8) 0.046(12) 0.029(11) -0.003(8) 0.014(9) 0.003(7) O1W 0.015(5) 0.020(6) 0.032(8) 0.001(5) 0.007(6) 0.000(5) O2W 0.021(6) 0.070(10) 0.029(8) -0.013(6) 0.017(6) -0.006(6) O3W 0.020(6) 0.029(7) 0.044(8) 0.017(6) 0.021(6) 0.009(5) O4W 0.021(6) 0.019(6) 0.049(9) -0.012(5) 0.017(6) -0.001(5) O5W 0.016(6) 0.028(6) 0.023(7) 0.007(5) 0.013(6) 0.009(5) O6W 0.043(9) 0.081(12) 0.022(9) 0.002(7) 0.016(8) 0.004(8) O7W 0.061(10) 0.043(8) 0.066(12) -0.005(7) 0.047(10) -0.001(7) O8W 0.017(6) 0.034(7) 0.041(8) 0.007(6) 0.017(6) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O14 2.257(11) . ? Er1 O8 2.303(11) . ? Er1 O4W 2.345(11) . ? Er1 O1W 2.347(11) . ? Er1 O5W 2.371(11) . ? Er1 O2W 2.390(12) . ? Er1 O3W 2.415(10) . ? Er1 O10 2.439(10) . ? Er1 Na1 3.785(11) 1_545 ? Er1 Na1 3.796(11) . ? Mo1 O2 1.727(11) . ? Mo1 O3 1.732(11) . ? Mo1 O1 1.758(10) . ? Mo1 O4 2.108(10) . ? Mo1 O5 2.167(10) . ? Mo1 N1 2.390(13) . ? Mo2 O9 1.727(11) . ? Mo2 O4 1.740(10) 1_545 ? Mo2 O10 1.743(10) 2_565 ? Mo2 O1 2.077(10) . ? Mo2 O11 2.209(10) 1_545 ? Mo2 N2 2.348(14) 1_545 ? Na1 O4W 2.27(2) 1_565 ? Na1 O1W 2.382(19) . ? Na1 O2 2.56(3) 2_574 ? Na1 O8W 2.66(3) . ? Na1 O7W 2.80(3) . ? Na1 O8 2.85(2) 1_565 ? Na1 O14 2.92(2) . ? Na1 O2W 3.02(2) . ? Na1 Er1 3.785(11) 1_565 ? O2 Na1 2.56(3) 2_575 ? O4 Mo2 1.740(10) 1_565 ? O5 C6 1.313(19) . ? O6 C6 1.22(2) . ? O7 C7 1.23(2) . ? O8 C7 1.264(19) . ? O8 Na1 2.85(2) 1_545 ? O10 Mo2 1.743(10) 2_564 ? O11 C13 1.305(19) . ? O11 Mo2 2.209(10) 1_565 ? O12 C13 1.229(19) . ? O13 C14 1.22(2) . ? O14 C14 1.26(2) . ? N1 C5 1.349(19) . ? N1 C1 1.36(2) . ? N2 C8 1.31(2) . ? N2 C12 1.384(19) . ? N2 Mo2 2.348(14) 1_565 ? C1 C2 1.37(2) . ? C1 C6 1.50(2) . ? C2 C3 1.36(2) . ? C2 H2A 0.9300 . ? C3 C4 1.41(2) . ? C3 H3A 0.9300 . ? C4 C5 1.33(2) . ? C4 C7 1.54(2) . ? C5 H5A 0.9300 . ? C8 C9 1.38(2) . ? C8 C13 1.521(19) . ? C9 C10 1.39(2) . ? C9 H9A 0.9300 . ? C10 C11 1.40(2) . ? C10 H10A 0.9300 . ? C11 C12 1.33(2) . ? C11 C14 1.53(2) . ? C12 H12A 0.9300 . ? O4W Na1 2.27(2) 1_545 ? _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 Er1 O8 76.5(5) . . ? O14 Er1 O4W 145.6(4) . . ? O8 Er1 O4W 77.2(5) . . ? O14 Er1 O1W 80.7(5) . . ? O8 Er1 O1W 148.4(4) . . ? O4W Er1 O1W 112.6(5) . . ? O14 Er1 O5W 141.2(4) . . ? O8 Er1 O5W 137.5(4) . . ? O4W Er1 O5W 72.3(4) . . ? O1W Er1 O5W 72.5(4) . . ? O14 Er1 O2W 71.0(4) . . ? O8 Er1 O2W 114.3(4) . . ? O4W Er1 O2W 141.3(4) . . ? O1W Er1 O2W 77.6(4) . . ? O5W Er1 O2W 76.1(4) . . ? O14 Er1 O3W 112.8(4) . . ? O8 Er1 O3W 70.8(4) . . ? O4W Er1 O3W 78.5(4) . . ? O1W Er1 O3W 139.4(4) . . ? O5W Er1 O3W 74.6(4) . . ? O2W Er1 O3W 72.0(5) . . ? O14 Er1 O10 84.3(4) . . ? O8 Er1 O10 86.3(4) . . ? O4W Er1 O10 72.2(4) . . ? O1W Er1 O10 69.8(3) . . ? O5W Er1 O10 111.0(4) . . ? O2W Er1 O10 141.8(4) . . ? O3W Er1 O10 146.1(4) . . ? O14 Er1 Na1 125.2(5) . 1_545 ? O8 Er1 Na1 48.7(5) . 1_545 ? O4W Er1 Na1 34.4(5) . 1_545 ? O1W Er1 Na1 147.0(5) . 1_545 ? O5W Er1 Na1 91.1(4) . 1_545 ? O2W Er1 Na1 127.0(5) . 1_545 ? O3W Er1 Na1 55.1(5) . 1_545 ? O10 Er1 Na1 90.9(5) . 1_545 ? O14 Er1 Na1 50.1(5) . . ? O8 Er1 Na1 126.6(5) . . ? O4W Er1 Na1 149.5(5) . . ? O1W Er1 Na1 36.9(4) . . ? O5W Er1 Na1 93.3(4) . . ? O2W Er1 Na1 52.6(5) . . ? O3W Er1 Na1 124.5(5) . . ? O10 Er1 Na1 89.2(5) . . ? Na1 Er1 Na1 175.3(7) 1_545 . ? O2 Mo1 O3 104.4(5) . . ? O2 Mo1 O1 100.4(5) . . ? O3 Mo1 O1 102.1(5) . . ? O2 Mo1 O4 85.3(5) . . ? O3 Mo1 O4 93.0(5) . . ? O1 Mo1 O4 161.8(5) . . ? O2 Mo1 O5 158.1(4) . . ? O3 Mo1 O5 90.1(5) . . ? O1 Mo1 O5 92.4(5) . . ? O4 Mo1 O5 77.4(4) . . ? O2 Mo1 N1 92.2(5) . . ? O3 Mo1 N1 159.5(5) . . ? O1 Mo1 N1 86.3(5) . . ? O4 Mo1 N1 76.2(4) . . ? O5 Mo1 N1 70.7(4) . . ? O9 Mo2 O4 101.6(5) . 1_545 ? O9 Mo2 O10 104.4(5) . 2_565 ? O4 Mo2 O10 101.5(5) 1_545 2_565 ? O9 Mo2 O1 92.1(4) . . ? O4 Mo2 O1 159.6(6) 1_545 . ? O10 Mo2 O1 89.6(5) 2_565 . ? O9 Mo2 O11 90.6(5) . 1_545 ? O4 Mo2 O11 89.0(5) 1_545 1_545 ? O10 Mo2 O11 159.3(4) 2_565 1_545 ? O1 Mo2 O11 75.5(4) . 1_545 ? O9 Mo2 N2 158.9(5) . 1_545 ? O4 Mo2 N2 85.5(5) 1_545 1_545 ? O10 Mo2 N2 93.4(5) 2_565 1_545 ? O1 Mo2 N2 76.6(4) . 1_545 ? O11 Mo2 N2 69.5(4) 1_545 1_545 ? O4W Na1 O1W 104.1(9) 1_565 . ? O4W Na1 O2 68.7(7) 1_565 2_574 ? O1W Na1 O2 68.7(7) . 2_574 ? O4W Na1 O8W 67.2(6) 1_565 . ? O1W Na1 O8W 64.8(6) . . ? O2 Na1 O8W 102.4(8) 2_574 . ? O4W Na1 O7W 123.3(8) 1_565 . ? O1W Na1 O7W 123.5(7) . . ? O2 Na1 O7W 152.7(10) 2_574 . ? O8W Na1 O7W 104.8(9) . . ? O4W Na1 O8 67.9(5) 1_565 1_565 ? O1W Na1 O8 157.2(11) . 1_565 ? O2 Na1 O8 88.7(7) 2_574 1_565 ? O8W Na1 O8 125.4(6) . 1_565 ? O7W Na1 O8 76.1(6) . 1_565 ? O4W Na1 O14 156.6(11) 1_565 . ? O1W Na1 O14 67.6(5) . . ? O2 Na1 O14 88.0(7) 2_574 . ? O8W Na1 O14 122.7(6) . . ? O7W Na1 O14 76.9(6) . . ? O8 Na1 O14 110.9(8) 1_565 . ? O4W Na1 O2W 144.3(10) 1_565 . ? O1W Na1 O2W 65.4(5) . . ? O2 Na1 O2W 128.7(6) 2_574 . ? O8W Na1 O2W 77.9(6) . . ? O7W Na1 O2W 58.1(6) . . ? O8 Na1 O2W 133.5(9) 1_565 . ? O14 Na1 O2W 54.1(4) . . ? O4W Na1 Er1 35.6(4) 1_565 1_565 ? O1W Na1 Er1 139.6(8) . 1_565 ? O2 Na1 Er1 89.8(5) 2_574 1_565 ? O8W Na1 Er1 88.7(5) . 1_565 ? O7W Na1 Er1 91.4(5) . 1_565 ? O8 Na1 Er1 37.4(3) 1_565 1_565 ? O14 Na1 Er1 148.3(7) . 1_565 ? O2W Na1 Er1 141.0(8) . 1_565 ? O4W Na1 Er1 140.4(8) 1_565 . ? O1W Na1 Er1 36.3(3) . . ? O2 Na1 Er1 89.7(5) 2_574 . ? O8W Na1 Er1 86.8(5) . . ? O7W Na1 Er1 91.2(5) . . ? O8 Na1 Er1 147.3(7) 1_565 . ? O14 Na1 Er1 36.4(3) . . ? O2W Na1 Er1 39.0(3) . . ? Er1 Na1 Er1 175.3(7) 1_565 . ? Mo1 O1 Mo2 161.6(7) . . ? Mo1 O2 Na1 168.2(7) . 2_575 ? Mo2 O4 Mo1 160.1(7) 1_565 . ? C6 O5 Mo1 123.1(9) . . ? C7 O8 Er1 168.0(12) . . ? C7 O8 Na1 97.9(10) . 1_545 ? Er1 O8 Na1 93.9(6) . 1_545 ? Mo2 O10 Er1 166.1(6) 2_564 . ? C13 O11 Mo2 121.4(9) . 1_565 ? C14 O14 Er1 143.5(12) . . ? C14 O14 Na1 121.9(11) . . ? Er1 O14 Na1 93.5(6) . . ? C5 N1 C1 115.6(13) . . ? C5 N1 Mo1 130.2(11) . . ? C1 N1 Mo1 114.0(9) . . ? C8 N2 C12 117.2(14) . . ? C8 N2 Mo2 117.1(10) . 1_565 ? C12 N2 Mo2 125.4(11) . 1_565 ? N1 C1 C2 123.5(14) . . ? N1 C1 C6 115.1(14) . . ? C2 C1 C6 121.4(15) . . ? C3 C2 C1 118.7(16) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.0(16) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 118.1(14) . . ? C5 C4 C7 123.8(14) . . ? C3 C4 C7 118.1(14) . . ? C4 C5 N1 125.1(15) . . ? C4 C5 H5A 117.4 . . ? N1 C5 H5A 117.4 . . ? O6 C6 O5 124.5(14) . . ? O6 C6 C1 120.0(15) . . ? O5 C6 C1 115.4(14) . . ? O7 C7 O8 126.4(15) . . ? O7 C7 C4 117.0(14) . . ? O8 C7 C4 116.5(14) . . ? N2 C8 C9 124.8(14) . . ? N2 C8 C13 114.0(14) . . ? C9 C8 C13 121.0(14) . . ? C8 C9 C10 117.5(16) . . ? C8 C9 H9A 121.2 . . ? C10 C9 H9A 121.2 . . ? C9 C10 C11 117.7(15) . . ? C9 C10 H10A 121.2 . . ? C11 C10 H10A 121.2 . . ? C12 C11 C10 120.7(14) . . ? C12 C11 C14 120.4(14) . . ? C10 C11 C14 118.8(14) . . ? C11 C12 N2 122.0(15) . . ? C11 C12 H12A 119.0 . . ? N2 C12 H12A 119.0 . . ? O12 C13 O11 124.5(13) . . ? O12 C13 C8 120.6(14) . . ? O11 C13 C8 114.9(13) . . ? O13 C14 O14 124.5(14) . . ? O13 C14 C11 118.8(15) . . ? O14 C14 C11 116.3(16) . . ? Er1 O1W Na1 106.8(6) . . ? Er1 O2W Na1 88.4(5) . . ? Na1 O4W Er1 110.0(7) 1_545 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.171 _refine_diff_density_min -2.150 _refine_diff_density_rms 0.216 #===END