Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Christopher L. Cahill' _publ_contact_author_address ; Department of Chemistry George Washington University 725 21st Street, NW Washington, DC 20052 ; _publ_contact_author_email cahill@gwu.edu _publ_contact_author_phone 202-994-6959 _publ_contact_author_fax 202-994-5873 _publ_section_title ; Homo- and heterometallic coordination polymers from the f elements ; loop_ _publ_author_name _publ_author_address C.L.Cahill ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 AND Carnegie Insitution of Washington Geophysical Laboratory 5251 Broad Branch Road, NW Washington, DC 20015 ; 'D.T.de Lill' ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 ; M.Frisch ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 ; data_DB2_71 _database_code_depnum_ccdc_archive 'CCDC 625116' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Nd2 O14, C13 H14 N2' _chemical_formula_sum 'C31 H38 N2 Nd2 O14' _chemical_formula_weight 951.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.768(3) _cell_length_b 14.344(6) _cell_length_c 16.125(7) _cell_angle_alpha 92.980(7) _cell_angle_beta 95.605(7) _cell_angle_gamma 99.593(7) _cell_volume 1758.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 29.34 _exptl_crystal_description needle _exptl_crystal_colour 'light purple' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 2.988 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker Apex CCD' _diffrn_measurement_method 'omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29371 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7145 _reflns_number_gt 4730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0030P)^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 7145 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.858 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O14 O -0.4019(5) 0.1962(3) 0.0810(2) 0.0307(10) Uani 1 1 d . . . O13 O -0.4466(5) 0.4000(3) 0.1307(2) 0.0278(10) Uani 1 1 d . . . O12 O 0.3711(5) 0.3359(3) 0.4121(2) 0.0344(11) Uani 1 1 d . . . O11 O -0.0711(5) 0.3502(3) 0.1139(2) 0.0296(10) Uani 1 1 d . . . O8 O 0.4136(5) 0.1488(3) 0.3432(2) 0.0304(10) Uani 1 1 d . . . O9 O 0.0375(5) 0.1723(3) 0.3782(2) 0.0294(10) Uani 1 1 d . . . O10 O 0.2085(5) 0.3416(3) 0.1551(2) 0.0345(11) Uani 1 1 d . . . O7 O 0.0900(5) 0.0785(3) 0.2149(2) 0.0285(10) Uani 1 1 d . . . C15 C -0.5471(7) 0.1754(4) 0.1062(4) 0.0239(14) Uani 1 1 d . . . C13 C 0.5080(8) 0.3638(4) 0.3816(4) 0.0269(15) Uani 1 1 d . . . C10 C 0.0873(8) 0.3636(4) 0.1032(4) 0.0256(14) Uani 1 1 d . . . C16 C -0.4287(8) 0.1464(4) 0.3602(4) 0.0284(15) Uani 1 1 d . . . C9 C -0.3052(8) -0.1105(5) -0.0560(4) 0.0387(17) Uani 1 1 d . . . H9A H -0.2800 -0.0530 -0.0851 0.046 Uiso 1 1 calc R . . H9B H -0.2019 -0.1404 -0.0545 0.046 Uiso 1 1 calc R . . C14 C 0.6715(8) 0.4093(4) 0.4360(4) 0.0364(16) Uani 1 1 d . . . H14A H 0.7045 0.4734 0.4195 0.044 Uiso 1 1 calc R . . H14B H 0.7649 0.3751 0.4241 0.044 Uiso 1 1 calc R . . C11 C 0.1434(8) 0.4039(4) 0.0246(4) 0.0347(16) Uani 1 1 d . . . H11A H 0.1677 0.3529 -0.0119 0.042 Uiso 1 1 calc R . . H11B H 0.2525 0.4483 0.0385 0.042 Uiso 1 1 calc R . . C12 C 0.0130(8) 0.4544(4) -0.0235(3) 0.0340(16) Uani 1 1 d . . . H12A H -0.0992 0.4121 -0.0344 0.041 Uiso 1 1 calc R . . H12B H 0.0541 0.4696 -0.0769 0.041 Uiso 1 1 calc R . . C55 C 1.0165(9) 0.8830(5) 0.3253(4) 0.0480(19) Uani 1 1 d . . . H55 H 1.0549 0.9348 0.2954 0.058 Uiso 1 1 calc R . . C59 C 1.4137(9) 0.7165(5) 0.1079(5) 0.0438(18) Uani 1 1 d . . . H59 H 1.3672 0.7463 0.0632 0.053 Uiso 1 1 calc R . . C17 C -0.3810(8) 0.0798(5) 0.4245(4) 0.060(2) Uani 1 1 d . . . H17A H -0.3285 0.0313 0.3972 0.072 Uiso 1 1 calc R . . H17B H -0.2919 0.1151 0.4660 0.072 Uiso 1 1 calc R . . C18 C -0.5261(8) 0.0322(5) 0.4684(4) 0.057(2) Uani 1 1 d . . . H18A H -0.6150 -0.0040 0.4273 0.068 Uiso 1 1 calc R . . H18B H -0.5793 0.0803 0.4958 0.068 Uiso 1 1 calc R . . C58 C 1.4152(9) 0.7536(5) 0.1879(5) 0.0459(19) Uani 1 1 d . . . C56 C 0.9797(10) 0.8968(6) 0.4064(4) 0.053(2) Uani 1 1 d . . . H56 H 0.9946 0.9587 0.4298 0.063 Uiso 1 1 calc R . . C57 C 1.3460(12) 0.8444(6) 0.2068(6) 0.081(3) Uani 1 1 d . . . H57A H 1.3464 0.8546 0.2668 0.097 Uiso 1 1 calc R . . H57B H 1.4243 0.8972 0.1881 0.097 Uiso 1 1 calc R . . N2 N 1.5455(8) 0.5876(4) 0.1528(5) 0.0574(18) Uani 1 1 d . . . C60 C 1.4804(9) 0.6360(5) 0.0938(5) 0.0453(18) Uani 1 1 d . . . H60 H 1.4801 0.6135 0.0386 0.054 Uiso 1 1 calc R . . C62 C 1.4810(11) 0.7041(6) 0.2503(5) 0.068(3) Uani 1 1 d . . . H62 H 1.4830 0.7252 0.3059 0.081 Uiso 1 1 calc R . . C61 C 1.5450(10) 0.6216(6) 0.2295(6) 0.066(3) Uani 1 1 d . . . H61 H 1.5899 0.5891 0.2727 0.080 Uiso 1 1 calc R . . Nd1 Nd 0.22432(4) 0.24325(2) 0.275948(18) 0.01727(9) Uani 1 1 d . . . Nd2 Nd -0.27176(4) 0.30122(2) 0.212399(18) 0.01712(9) Uani 1 1 d . . . O1 O -0.3029(5) 0.1943(3) 0.3289(2) 0.0334(11) Uani 1 1 d . . . O6 O -0.0816(5) 0.1829(3) 0.2029(2) 0.0237(9) Uani 1 1 d . . . O5 O 0.4251(5) 0.2069(3) 0.1777(2) 0.0229(9) Uani 1 1 d . . . O4 O 0.5180(5) 0.3545(3) 0.3036(2) 0.0239(9) Uani 1 1 d . . . O3 O 0.0190(5) 0.3537(3) 0.3030(2) 0.0226(9) Uani 1 1 d . . . O2 O -0.1208(5) 0.4676(3) 0.2651(3) 0.0329(11) Uani 1 1 d . . . C5 C -0.0580(8) 0.0975(4) 0.1960(3) 0.0227(14) Uani 1 1 d . . . C2 C 0.1725(7) 0.5120(4) 0.3321(3) 0.0249(14) Uani 1 1 d . . . H2A H 0.1699 0.5724 0.3081 0.030 Uiso 1 1 calc R . . H2B H 0.2783 0.4898 0.3183 0.030 Uiso 1 1 calc R . . C1 C 0.0148(8) 0.4421(4) 0.2962(3) 0.0233(14) Uani 1 1 d . . . C6 C -0.2087(7) 0.0223(4) 0.1619(3) 0.0287(15) Uani 1 1 d . . . H6A H -0.3184 0.0452 0.1661 0.034 Uiso 1 1 calc R . . H6B H -0.2098 -0.0331 0.1940 0.034 Uiso 1 1 calc R . . C3 C 0.1750(7) 0.5244(4) 0.4265(3) 0.0279(14) Uani 1 1 d . . . H3A H 0.0734 0.5515 0.4390 0.033 Uiso 1 1 calc R . . H3B H 0.1634 0.4623 0.4486 0.033 Uiso 1 1 calc R . . C4 C 0.6640(7) 0.4144(4) 0.5291(3) 0.0320(15) Uani 1 1 d . . . H4A H 0.5609 0.4400 0.5418 0.038 Uiso 1 1 calc R . . H4B H 0.6537 0.3511 0.5486 0.038 Uiso 1 1 calc R . . C7 C -0.1913(8) -0.0038(4) 0.0726(3) 0.0306(15) Uani 1 1 d . . . H7A H -0.0777 -0.0226 0.0692 0.037 Uiso 1 1 calc R . . H7B H -0.1938 0.0519 0.0412 0.037 Uiso 1 1 calc R . . C8 C -0.3320(8) -0.0829(4) 0.0317(3) 0.0320(15) Uani 1 1 d . . . H8A H -0.3339 -0.1378 0.0644 0.038 Uiso 1 1 calc R . . H8B H -0.4454 -0.0630 0.0320 0.038 Uiso 1 1 calc R . . C52 C 0.9968(9) 0.7930(6) 0.2888(4) 0.0440(18) Uani 1 1 d . . . C53 C 1.0269(11) 0.7728(7) 0.1988(4) 0.075(3) Uani 1 1 d . . . H53A H 1.0592 0.7105 0.1932 0.090 Uiso 1 1 calc R . . H53B H 0.9170 0.7707 0.1640 0.090 Uiso 1 1 calc R . . C50 C 0.9040(11) 0.7420(7) 0.4179(5) 0.069(3) Uani 1 1 d . . . H50 H 0.8633 0.6921 0.4495 0.083 Uiso 1 1 calc R . . N1 N 0.9249(9) 0.8279(5) 0.4523(4) 0.0588(18) Uani 1 1 d . . . C51 C 0.9389(10) 0.7202(6) 0.3363(5) 0.063(2) Uani 1 1 d . . . H51 H 0.9232 0.6576 0.3148 0.076 Uiso 1 1 calc R . . C54 C 1.1649(14) 0.8427(6) 0.1660(5) 0.085(3) Uani 1 1 d . . . H54A H 1.1633 0.8279 0.1065 0.102 Uiso 1 1 calc R . . H54B H 1.1355 0.9055 0.1735 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O14 0.018(2) 0.046(3) 0.026(2) -0.008(2) 0.0024(19) 0.002(2) O13 0.019(2) 0.039(3) 0.026(2) 0.0127(19) -0.0046(18) 0.0081(19) O12 0.017(2) 0.059(3) 0.025(2) -0.005(2) 0.0012(19) 0.000(2) O11 0.020(2) 0.043(3) 0.028(2) 0.017(2) 0.0029(19) 0.007(2) O8 0.018(2) 0.040(3) 0.038(3) 0.022(2) 0.0023(19) 0.011(2) O9 0.019(2) 0.045(3) 0.026(2) 0.012(2) 0.0054(18) 0.0040(19) O10 0.024(3) 0.054(3) 0.029(2) 0.019(2) 0.0010(19) 0.012(2) O7 0.016(2) 0.026(2) 0.043(3) -0.004(2) -0.0020(19) 0.0055(18) C15 0.015(3) 0.027(4) 0.028(4) -0.001(3) -0.002(3) 0.002(3) C13 0.027(4) 0.024(4) 0.028(4) -0.004(3) 0.002(3) 0.003(3) C10 0.024(4) 0.022(3) 0.031(4) 0.004(3) 0.005(3) 0.006(3) C16 0.022(4) 0.037(4) 0.030(4) 0.012(3) 0.003(3) 0.012(3) C9 0.029(4) 0.049(5) 0.031(4) -0.011(3) 0.003(3) -0.010(3) C14 0.026(4) 0.041(4) 0.036(4) -0.013(3) -0.003(3) -0.004(3) C11 0.029(4) 0.047(4) 0.036(4) 0.023(3) 0.012(3) 0.017(3) C12 0.027(4) 0.049(4) 0.027(4) 0.018(3) 0.000(3) 0.006(3) C55 0.048(5) 0.059(5) 0.040(4) 0.015(4) 0.001(4) 0.014(4) C59 0.040(5) 0.038(4) 0.058(5) 0.014(4) 0.018(4) 0.010(3) C17 0.026(4) 0.089(6) 0.075(6) 0.064(5) 0.011(4) 0.021(4) C18 0.031(4) 0.081(6) 0.068(5) 0.063(5) 0.012(4) 0.015(4) C58 0.042(5) 0.042(5) 0.055(5) 0.005(4) 0.022(4) -0.001(4) C56 0.064(6) 0.057(5) 0.036(4) 0.001(4) 0.001(4) 0.013(4) C57 0.087(8) 0.050(6) 0.116(8) 0.005(5) 0.060(6) 0.012(5) N2 0.044(4) 0.051(4) 0.078(5) 0.013(4) -0.001(4) 0.010(3) C60 0.035(4) 0.042(5) 0.058(5) -0.001(4) 0.011(4) 0.001(3) C62 0.073(7) 0.072(7) 0.053(5) -0.002(5) 0.020(5) -0.008(5) C61 0.056(6) 0.065(6) 0.074(7) 0.028(5) -0.005(5) -0.001(5) Nd1 0.01084(18) 0.0224(2) 0.01778(19) 0.00217(15) -0.00170(14) 0.00214(14) Nd2 0.01082(18) 0.02141(19) 0.01820(19) 0.00238(15) -0.00153(14) 0.00156(14) O1 0.019(2) 0.044(3) 0.041(3) 0.025(2) 0.011(2) 0.005(2) O6 0.020(2) 0.024(2) 0.027(2) -0.0037(19) -0.0022(18) 0.0085(18) O5 0.018(2) 0.030(2) 0.018(2) -0.0063(18) -0.0011(17) 0.0011(18) O4 0.019(2) 0.030(2) 0.021(2) -0.0026(18) 0.0001(17) -0.0012(18) O3 0.019(2) 0.022(2) 0.024(2) -0.0044(18) -0.0065(17) 0.0014(17) O2 0.020(2) 0.026(2) 0.051(3) 0.000(2) -0.009(2) 0.0049(19) C5 0.022(4) 0.026(4) 0.018(3) -0.001(3) 0.004(3) -0.004(3) C2 0.022(3) 0.025(3) 0.023(3) 0.001(3) -0.005(3) -0.004(3) C1 0.023(4) 0.025(4) 0.019(3) -0.008(3) 0.005(3) -0.002(3) C6 0.022(4) 0.026(4) 0.036(4) 0.001(3) 0.008(3) -0.006(3) C3 0.022(4) 0.032(4) 0.026(3) -0.003(3) -0.002(3) -0.001(3) C4 0.023(4) 0.038(4) 0.031(4) -0.004(3) -0.003(3) -0.001(3) C7 0.024(4) 0.039(4) 0.024(3) -0.002(3) -0.003(3) -0.004(3) C8 0.024(4) 0.038(4) 0.029(4) -0.004(3) -0.003(3) -0.001(3) C52 0.035(4) 0.058(5) 0.040(4) -0.001(4) -0.001(3) 0.017(4) C53 0.063(6) 0.130(9) 0.042(5) -0.015(5) -0.006(4) 0.058(6) C50 0.074(7) 0.075(7) 0.058(6) 0.032(5) 0.002(5) 0.007(5) N1 0.066(5) 0.074(5) 0.038(4) 0.011(4) 0.002(3) 0.016(4) C51 0.064(6) 0.047(5) 0.076(6) 0.003(5) -0.015(5) 0.017(4) C54 0.135(10) 0.088(7) 0.066(6) 0.037(6) 0.054(6) 0.081(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O14 C15 1.232(6) . ? O14 Nd2 2.554(4) . ? O13 Nd2 2.464(3) . ? O12 C13 1.231(7) . ? O12 Nd1 2.567(4) . ? O11 C10 1.244(6) . ? O11 Nd2 2.383(4) . ? O8 C16 1.235(6) 1_655 ? O8 Nd1 2.383(4) . ? O9 Nd1 2.451(4) . ? O10 C10 1.288(6) . ? O10 Nd1 2.470(4) . ? O7 C5 1.239(6) . ? O7 Nd1 2.525(4) . ? C15 O5 1.268(6) 1_455 ? C15 C9 1.491(7) 2_455 ? C15 Nd2 2.906(6) . ? C13 O4 1.269(6) . ? C13 C14 1.501(7) . ? C13 Nd1 2.905(6) . ? C10 C11 1.493(7) . ? C16 O8 1.235(6) 1_455 ? C16 O1 1.261(6) . ? C16 C17 1.508(7) . ? C9 C15 1.491(7) 2_455 ? C9 C8 1.493(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C14 C4 1.506(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C11 C12 1.517(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C12 1.530(11) 2_565 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C55 C52 1.369(9) . ? C55 C56 1.377(9) . ? C55 H55 0.9300 . ? C59 C60 1.361(8) . ? C59 C58 1.369(9) . ? C59 H59 0.9300 . ? C17 C18 1.479(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C18 1.481(10) 2_456 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C58 C62 1.367(10) . ? C58 C57 1.517(10) . ? C56 N1 1.304(8) . ? C56 H56 0.9300 . ? C57 C54 1.490(11) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? N2 C61 1.306(10) . ? N2 C60 1.317(8) . ? C60 H60 0.9300 . ? C62 C61 1.395(10) . ? C62 H62 0.9300 . ? C61 H61 0.9300 . ? Nd1 O5 2.425(4) . ? Nd1 O3 2.480(4) . ? Nd1 O6 2.539(4) . ? Nd1 O4 2.543(4) . ? Nd1 C5 2.912(6) . ? Nd1 Nd2 4.1050(16) 1_655 ? Nd2 O6 2.437(4) . ? Nd2 O4 2.487(4) 1_455 ? Nd2 O1 2.491(4) . ? Nd2 O5 2.508(4) 1_455 ? Nd2 O2 2.540(4) . ? Nd2 O3 2.545(4) . ? Nd2 C1 2.914(6) . ? Nd2 Nd1 4.1050(16) 1_455 ? O6 C5 1.269(6) . ? O5 C15 1.268(6) 1_655 ? O5 Nd2 2.508(4) 1_655 ? O4 Nd2 2.487(4) 1_655 ? O3 C1 1.285(6) . ? O2 C1 1.240(6) . ? C5 C6 1.494(7) . ? C2 C1 1.494(7) . ? C2 C3 1.521(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C6 C7 1.494(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C3 C4 1.497(7) 2_666 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C3 1.497(7) 2_666 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C7 C8 1.511(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C52 C51 1.368(9) . ? C52 C53 1.514(9) . ? C53 C54 1.497(11) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C50 N1 1.303(10) . ? C50 C51 1.398(10) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 O14 Nd2 93.7(3) . . ? C13 O12 Nd1 93.1(3) . . ? C10 O11 Nd2 143.2(4) . . ? C16 O8 Nd1 140.8(4) 1_655 . ? C10 O10 Nd1 136.9(4) . . ? C5 O7 Nd1 95.2(3) . . ? O14 C15 O5 120.6(5) . 1_455 ? O14 C15 C9 122.1(5) . 2_455 ? O5 C15 C9 117.3(5) 1_455 2_455 ? O14 C15 Nd2 61.3(3) . . ? O5 C15 Nd2 59.3(3) 1_455 . ? C9 C15 Nd2 176.6(4) 2_455 . ? O12 C13 O4 121.8(6) . . ? O12 C13 C14 120.9(5) . . ? O4 C13 C14 117.3(5) . . ? O12 C13 Nd1 61.9(3) . . ? O4 C13 Nd1 60.9(3) . . ? C14 C13 Nd1 168.8(4) . . ? O11 C10 O10 123.8(5) . . ? O11 C10 C11 119.4(5) . . ? O10 C10 C11 116.8(5) . . ? O8 C16 O1 126.4(5) 1_455 . ? O8 C16 C17 117.1(5) 1_455 . ? O1 C16 C17 116.5(5) . . ? C15 C9 C8 116.8(5) 2_455 . ? C15 C9 H9A 108.1 2_455 . ? C8 C9 H9A 108.1 . . ? C15 C9 H9B 108.1 2_455 . ? C8 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C13 C14 C4 117.5(5) . . ? C13 C14 H14A 107.9 . . ? C4 C14 H14A 107.9 . . ? C13 C14 H14B 107.9 . . ? C4 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C10 C11 C12 115.7(5) . . ? C10 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? C10 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C11 C12 C12 112.6(6) . 2_565 ? C11 C12 H12A 109.1 . . ? C12 C12 H12A 109.1 2_565 . ? C11 C12 H12B 109.1 . . ? C12 C12 H12B 109.1 2_565 . ? H12A C12 H12B 107.8 . . ? C52 C55 C56 120.0(7) . . ? C52 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C60 C59 C58 119.9(7) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C18 C17 C16 116.4(5) . . ? C18 C17 H17A 108.2 . . ? C16 C17 H17A 108.2 . . ? C18 C17 H17B 108.2 . . ? C16 C17 H17B 108.2 . . ? H17A C17 H17B 107.3 . . ? C17 C18 C18 114.8(7) . 2_456 ? C17 C18 H18A 108.6 . . ? C18 C18 H18A 108.6 2_456 . ? C17 C18 H18B 108.6 . . ? C18 C18 H18B 108.6 2_456 . ? H18A C18 H18B 107.5 . . ? C62 C58 C59 116.5(7) . . ? C62 C58 C57 121.6(8) . . ? C59 C58 C57 121.9(7) . . ? N1 C56 C55 123.6(7) . . ? N1 C56 H56 118.2 . . ? C55 C56 H56 118.2 . . ? C54 C57 C58 112.9(7) . . ? C54 C57 H57A 109.0 . . ? C58 C57 H57A 109.0 . . ? C54 C57 H57B 109.0 . . ? C58 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? C61 N2 C60 116.0(7) . . ? N2 C60 C59 124.5(7) . . ? N2 C60 H60 117.7 . . ? C59 C60 H60 117.7 . . ? C58 C62 C61 119.3(8) . . ? C58 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? N2 C61 C62 123.6(8) . . ? N2 C61 H61 118.2 . . ? C62 C61 H61 118.2 . . ? O8 Nd1 O5 72.47(13) . . ? O8 Nd1 O9 79.69(13) . . ? O5 Nd1 O9 142.58(13) . . ? O8 Nd1 O10 139.90(13) . . ? O5 Nd1 O10 69.21(13) . . ? O9 Nd1 O10 139.90(13) . . ? O8 Nd1 O3 143.00(13) . . ? O5 Nd1 O3 141.78(12) . . ? O9 Nd1 O3 73.37(13) . . ? O10 Nd1 O3 72.74(13) . . ? O8 Nd1 O7 77.91(13) . . ? O5 Nd1 O7 76.26(12) . . ? O9 Nd1 O7 73.81(13) . . ? O10 Nd1 O7 103.60(14) . . ? O3 Nd1 O7 116.92(12) . . ? O8 Nd1 O6 125.77(13) . . ? O5 Nd1 O6 105.65(12) . . ? O9 Nd1 O6 71.25(12) . . ? O10 Nd1 O6 76.71(13) . . ? O3 Nd1 O6 68.21(12) . . ? O7 Nd1 O6 50.71(12) . . ? O8 Nd1 O4 76.31(13) . . ? O5 Nd1 O4 68.79(12) . . ? O9 Nd1 O4 128.07(12) . . ? O10 Nd1 O4 79.30(13) . . ? O3 Nd1 O4 100.92(12) . . ? O7 Nd1 O4 141.34(12) . . ? O6 Nd1 O4 155.69(12) . . ? O8 Nd1 O12 72.58(14) . . ? O5 Nd1 O12 114.97(12) . . ? O9 Nd1 O12 78.47(13) . . ? O10 Nd1 O12 113.91(14) . . ? O3 Nd1 O12 77.49(13) . . ? O7 Nd1 O12 142.46(13) . . ? O6 Nd1 O12 139.22(12) . . ? O4 Nd1 O12 50.61(12) . . ? O8 Nd1 C13 70.05(15) . . ? O5 Nd1 C13 91.23(15) . . ? O9 Nd1 C13 102.39(15) . . ? O10 Nd1 C13 99.18(15) . . ? O3 Nd1 C13 91.30(15) . . ? O7 Nd1 C13 147.84(14) . . ? O6 Nd1 C13 159.46(15) . . ? O4 Nd1 C13 25.85(13) . . ? O12 Nd1 C13 25.03(13) . . ? O8 Nd1 C5 101.03(15) . . ? O5 Nd1 C5 92.32(14) . . ? O9 Nd1 C5 68.76(14) . . ? O10 Nd1 C5 91.93(15) . . ? O3 Nd1 C5 92.42(15) . . ? O7 Nd1 C5 25.06(13) . . ? O6 Nd1 C5 25.77(13) . . ? O4 Nd1 C5 160.94(14) . . ? O12 Nd1 C5 147.22(14) . . ? C13 Nd1 C5 168.88(16) . . ? O8 Nd1 Nd2 67.08(9) . 1_655 ? O5 Nd1 Nd2 34.32(8) . 1_655 ? O9 Nd1 Nd2 145.09(9) . 1_655 ? O10 Nd1 Nd2 74.68(9) . 1_655 ? O3 Nd1 Nd2 129.29(9) . 1_655 ? O7 Nd1 Nd2 107.77(9) . 1_655 ? O6 Nd1 Nd2 137.64(9) . 1_655 ? O4 Nd1 Nd2 34.85(9) . 1_655 ? O12 Nd1 Nd2 81.58(9) . 1_655 ? C13 Nd1 Nd2 57.13(12) . 1_655 ? C5 Nd1 Nd2 126.53(12) . 1_655 ? O11 Nd2 O6 72.56(13) . . ? O11 Nd2 O13 81.00(13) . . ? O6 Nd2 O13 144.27(13) . . ? O11 Nd2 O4 144.41(13) . 1_455 ? O6 Nd2 O4 140.67(12) . 1_455 ? O13 Nd2 O4 72.43(12) . 1_455 ? O11 Nd2 O1 139.75(13) . . ? O6 Nd2 O1 69.32(13) . . ? O13 Nd2 O1 139.04(13) . . ? O4 Nd2 O1 71.40(13) 1_455 . ? O11 Nd2 O5 125.56(13) . 1_455 ? O6 Nd2 O5 103.68(13) . 1_455 ? O13 Nd2 O5 72.68(12) . 1_455 ? O4 Nd2 O5 68.41(12) 1_455 1_455 ? O1 Nd2 O5 76.64(12) . 1_455 ? O11 Nd2 O2 74.51(14) . . ? O6 Nd2 O2 116.02(13) . . ? O13 Nd2 O2 78.03(13) . . ? O4 Nd2 O2 77.10(12) 1_455 . ? O1 Nd2 O2 111.45(14) . . ? O5 Nd2 O2 139.92(12) 1_455 . ? O11 Nd2 O3 76.60(13) . . ? O6 Nd2 O3 68.76(12) . . ? O13 Nd2 O3 127.99(12) . . ? O4 Nd2 O3 101.44(12) 1_455 . ? O1 Nd2 O3 78.04(12) . . ? O5 Nd2 O3 154.60(12) 1_455 . ? O2 Nd2 O3 50.99(12) . . ? O11 Nd2 O14 77.08(13) . . ? O6 Nd2 O14 75.44(12) . . ? O13 Nd2 O14 75.54(13) . . ? O4 Nd2 O14 117.09(12) 1_455 . ? O1 Nd2 O14 104.87(14) . . ? O5 Nd2 O14 50.80(12) 1_455 . ? O2 Nd2 O14 143.66(13) . . ? O3 Nd2 O14 140.42(12) . . ? O11 Nd2 C15 100.98(15) . . ? O6 Nd2 C15 89.55(15) . . ? O13 Nd2 C15 72.09(14) . . ? O4 Nd2 C15 93.06(15) 1_455 . ? O1 Nd2 C15 91.26(15) . . ? O5 Nd2 C15 25.78(13) 1_455 . ? O2 Nd2 C15 150.12(14) . . ? O3 Nd2 C15 158.01(14) . . ? O14 Nd2 C15 25.02(13) . . ? O11 Nd2 C1 71.40(14) . . ? O6 Nd2 C1 91.97(15) . . ? O13 Nd2 C1 102.07(15) . . ? O4 Nd2 C1 91.17(14) 1_455 . ? O1 Nd2 C1 97.27(15) . . ? O5 Nd2 C1 159.58(14) 1_455 . ? O2 Nd2 C1 25.11(13) . . ? O3 Nd2 C1 26.12(13) . . ? O14 Nd2 C1 148.32(14) . . ? C15 Nd2 C1 171.33(16) . . ? O11 Nd2 Nd1 150.41(9) . 1_455 ? O6 Nd2 Nd1 123.73(9) . 1_455 ? O13 Nd2 Nd1 72.62(9) . 1_455 ? O4 Nd2 Nd1 35.75(8) 1_455 1_455 ? O1 Nd2 Nd1 66.85(9) . 1_455 ? O5 Nd2 Nd1 33.04(8) 1_455 1_455 ? O2 Nd2 Nd1 111.77(9) . 1_455 ? O3 Nd2 Nd1 130.69(9) . 1_455 ? O14 Nd2 Nd1 83.46(9) . 1_455 ? C15 Nd2 Nd1 58.54(12) . 1_455 ? C1 Nd2 Nd1 126.63(11) . 1_455 ? C16 O1 Nd2 136.0(4) . . ? C5 O6 Nd2 151.5(4) . . ? C5 O6 Nd1 93.8(3) . . ? Nd2 O6 Nd1 111.78(14) . . ? C15 O5 Nd1 150.5(4) 1_655 . ? C15 O5 Nd2 94.9(3) 1_655 1_655 ? Nd1 O5 Nd2 112.63(14) . 1_655 ? C13 O4 Nd2 136.2(4) . 1_655 ? C13 O4 Nd1 93.3(3) . . ? Nd2 O4 Nd1 109.40(14) 1_655 . ? C1 O3 Nd1 136.9(4) . . ? C1 O3 Nd2 93.2(3) . . ? Nd1 O3 Nd2 110.18(14) . . ? C1 O2 Nd2 94.6(3) . . ? O7 C5 O6 119.7(5) . . ? O7 C5 C6 121.3(5) . . ? O6 C5 C6 119.0(5) . . ? O7 C5 Nd1 59.7(3) . . ? O6 C5 Nd1 60.5(3) . . ? C6 C5 Nd1 175.2(4) . . ? C1 C2 C3 110.0(4) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O2 C1 O3 120.1(5) . . ? O2 C1 C2 121.9(5) . . ? O3 C1 C2 117.8(5) . . ? O2 C1 Nd2 60.3(3) . . ? O3 C1 Nd2 60.7(3) . . ? C2 C1 Nd2 174.1(4) . . ? C5 C6 C7 109.4(5) . . ? C5 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C4 C3 C2 115.2(5) 2_666 . ? C4 C3 H3A 108.5 2_666 . ? C2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 2_666 . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 C14 111.0(5) 2_666 . ? C3 C4 H4A 109.4 2_666 . ? C14 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 2_666 . ? C14 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C7 C8 114.6(5) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 113.1(5) . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C51 C52 C55 116.9(7) . . ? C51 C52 C53 120.3(8) . . ? C55 C52 C53 122.7(7) . . ? C54 C53 C52 115.5(7) . . ? C54 C53 H53A 108.4 . . ? C52 C53 H53A 108.4 . . ? C54 C53 H53B 108.4 . . ? C52 C53 H53B 108.4 . . ? H53A C53 H53B 107.5 . . ? N1 C50 C51 124.0(8) . . ? N1 C50 H50 118.0 . . ? C51 C50 H50 118.0 . . ? C50 N1 C56 117.0(7) . . ? C52 C51 C50 118.6(8) . . ? C52 C51 H51 120.7 . . ? C50 C51 H51 120.7 . . ? C57 C54 C53 114.2(7) . . ? C57 C54 H54A 108.7 . . ? C53 C54 H54A 108.7 . . ? C57 C54 H54B 108.7 . . ? C53 C54 H54B 108.7 . . ? H54A C54 H54B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.167 _refine_diff_density_min -1.249 _refine_diff_density_rms 0.139 #===END data_DC1_45b _database_code_depnum_ccdc_archive 'CCDC 625117' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 O7 Pr, C5 H4 N' _chemical_formula_sum 'C17 H24 N O7 Pr' _chemical_formula_weight 495.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7447(12) _cell_length_b 10.1935(16) _cell_length_c 12.1464(19) _cell_angle_alpha 80.751(3) _cell_angle_beta 80.287(3) _cell_angle_gamma 82.818(3) _cell_volume 928.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3539 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 29.98 _exptl_crystal_description ' needle-like ' _exptl_crystal_colour ' light green ' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 2.663 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker Apex CCD' _diffrn_measurement_method 'omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11270 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.1234 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3757 _reflns_number_gt 2728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0433P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3757 _refine_ls_number_parameters 243 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.26092(5) 0.99001(4) 0.44102(4) 0.01746(13) Uani 1 1 d . . . O6 O 0.4951(8) 0.9802(6) 0.2730(5) 0.0325(13) Uani 1 1 d D . . O3 O 0.1885(6) 1.0624(5) 0.6366(4) 0.0266(12) Uani 1 1 d . . . O1 O 0.3872(6) 0.7397(5) 0.4548(4) 0.0291(12) Uani 1 1 d . . . C11 C 0.4932(9) 0.7501(7) 0.5181(6) 0.0196(16) Uani 1 1 d . . . C6 C 0.0493(10) 1.1115(7) 0.6929(6) 0.0222(17) Uani 1 1 d . . . N1 N 0.4908(10) 0.7997(8) 0.1198(7) 0.049(2) Uani 1 1 d . . . C4 C 0.4485(14) 0.5692(9) 0.1374(8) 0.059(3) Uani 1 1 d . . . H4 H 0.4141 0.4931 0.1852 0.071 Uiso 1 1 calc R . . C14 C 0.9088(9) 0.5012(7) 0.5375(7) 0.0258(17) Uani 1 1 d . . . H14A H 0.8644 0.4149 0.5447 0.031 Uiso 1 1 calc R . . H14B H 0.9209 0.5172 0.6123 0.031 Uiso 1 1 calc R . . C7 C 0.0685(10) 1.2070(7) 0.7716(6) 0.0263(18) Uani 1 1 d . . . H7A H 0.1913 1.2234 0.7614 0.032 Uiso 1 1 calc R . . H7B H 0.0013 1.2913 0.7501 0.032 Uiso 1 1 calc R . . C10 C -0.0481(11) 1.2256(8) 1.0925(7) 0.034(2) Uani 1 1 d . . . H10A H 0.0437 1.1582 1.1160 0.041 Uiso 1 1 calc R . . H10B H -0.1571 1.1840 1.1060 0.041 Uiso 1 1 calc R . . C9 C -0.0026(11) 1.2722(8) 0.9674(6) 0.033(2) Uani 1 1 d . . . H9A H 0.1092 1.3101 0.9535 0.039 Uiso 1 1 calc R . . H9B H -0.0914 1.3424 0.9445 0.039 Uiso 1 1 calc R . . C5 C 0.4491(14) 0.6850(11) 0.1817(8) 0.058(3) Uani 1 1 d . . . H5 H 0.4187 0.6829 0.2593 0.069 Uiso 1 1 calc R . . C8 C 0.0099(11) 1.1609(8) 0.8947(6) 0.034(2) Uani 1 1 d . . . H8A H 0.0924 1.0877 0.9210 0.041 Uiso 1 1 calc R . . H8B H -0.1044 1.1277 0.9038 0.041 Uiso 1 1 calc R . . C12 C 0.6029(9) 0.6296(7) 0.5671(6) 0.0251(17) Uani 1 1 d . . . H12A H 0.5396 0.5512 0.5763 0.030 Uiso 1 1 calc R . . H12B H 0.6252 0.6420 0.6407 0.030 Uiso 1 1 calc R . . C13 C 0.7784(9) 0.6087(7) 0.4884(6) 0.0254(17) Uani 1 1 d . . . H13A H 0.7548 0.5855 0.4184 0.030 Uiso 1 1 calc R . . H13B H 0.8314 0.6924 0.4706 0.030 Uiso 1 1 calc R . . C3 C 0.4975(10) 0.5635(8) 0.0244(7) 0.035(2) Uani 1 1 d . . . C1 C 0.5359(12) 0.7941(10) 0.0111(9) 0.053(3) Uani 1 1 d . . . H1 H 0.5673 0.8723 -0.0348 0.063 Uiso 1 1 calc R . . C2 C 0.5405(12) 0.6819(9) -0.0409(8) 0.048(3) Uani 1 1 d . . . H2 H 0.5721 0.6864 -0.1186 0.058 Uiso 1 1 calc R . . O4 O 0.5120(6) 0.8649(4) 0.5420(4) 0.0210(11) Uani 1 1 d . . . C17 C -0.0685(10) 1.3373(7) 1.1645(6) 0.0276(18) Uani 1 1 d . . . H17A H -0.1556 1.4070 1.1383 0.033 Uiso 1 1 calc R . . H17B H 0.0426 1.3756 1.1543 0.033 Uiso 1 1 calc R . . C16 C -0.1238(9) 1.2917(7) 1.2892(6) 0.0237(17) Uani 1 1 d . . . H16A H -0.1613 1.3700 1.3265 0.028 Uiso 1 1 calc R . . H16B H -0.2247 1.2413 1.2979 0.028 Uiso 1 1 calc R . . C15 C 0.0175(9) 1.2064(7) 1.3484(6) 0.0192(16) Uani 1 1 d . . . O5 O 0.1763(6) 1.2013(5) 1.3044(4) 0.0280(12) Uani 1 1 d . . . O7 O -0.1031(6) 1.0864(5) 0.6879(4) 0.0264(12) Uani 1 1 d . . . O2 O -0.0291(6) 1.1407(4) 0.4456(4) 0.0202(11) Uani 1 1 d . . . HW1 H 0.495(9) 0.925(5) 0.234(5) 0.02(2) Uiso 1 1 d D . . HW2 H 0.595(6) 0.967(11) 0.287(9) 0.08(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0134(2) 0.0175(2) 0.0226(2) -0.00640(15) -0.00567(15) 0.00248(14) O6 0.024(3) 0.044(4) 0.034(3) -0.027(3) -0.001(3) 0.002(3) O3 0.020(3) 0.031(3) 0.034(3) -0.014(2) -0.008(2) -0.002(2) O1 0.026(3) 0.028(3) 0.036(3) -0.012(2) -0.012(3) 0.006(2) C11 0.014(4) 0.022(4) 0.022(4) -0.006(3) 0.000(3) 0.002(3) C6 0.026(4) 0.019(4) 0.023(4) -0.003(3) -0.005(4) -0.006(3) N1 0.044(5) 0.055(5) 0.054(6) -0.026(4) -0.013(4) 0.002(4) C4 0.105(9) 0.041(6) 0.030(5) -0.008(4) -0.006(5) -0.003(6) C14 0.023(4) 0.015(4) 0.041(5) -0.006(3) -0.010(4) 0.003(3) C7 0.026(4) 0.032(4) 0.025(4) -0.014(4) -0.007(4) -0.001(3) C10 0.044(5) 0.028(5) 0.031(5) -0.006(4) -0.003(4) -0.004(4) C9 0.042(5) 0.036(5) 0.024(5) -0.009(4) -0.009(4) -0.005(4) C5 0.078(8) 0.068(8) 0.032(6) -0.024(5) -0.011(5) -0.001(6) C8 0.048(5) 0.032(5) 0.027(5) -0.003(4) -0.016(4) -0.007(4) C12 0.028(4) 0.019(4) 0.030(4) -0.003(3) -0.007(4) -0.001(3) C13 0.024(4) 0.022(4) 0.029(4) -0.003(3) -0.007(4) 0.006(3) C3 0.033(5) 0.044(5) 0.031(5) -0.015(4) -0.009(4) 0.002(4) C1 0.062(7) 0.046(6) 0.054(7) -0.020(5) -0.003(5) -0.012(5) C2 0.056(6) 0.050(6) 0.043(6) -0.021(5) -0.011(5) -0.002(5) O4 0.020(3) 0.015(2) 0.030(3) -0.006(2) -0.010(2) 0.000(2) C17 0.032(5) 0.026(4) 0.027(4) -0.006(4) -0.010(4) 0.002(3) C16 0.022(4) 0.025(4) 0.027(4) -0.008(3) -0.008(3) 0.001(3) C15 0.022(4) 0.016(4) 0.023(4) -0.006(3) -0.010(3) -0.003(3) O5 0.021(3) 0.035(3) 0.025(3) 0.000(2) -0.001(2) -0.003(2) O7 0.017(3) 0.036(3) 0.030(3) -0.011(2) -0.007(2) -0.001(2) O2 0.023(3) 0.020(3) 0.016(3) -0.004(2) 0.000(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O7 2.415(5) 2_576 ? Pr1 O2 2.464(5) 2_576 ? Pr1 O4 2.489(4) 2_676 ? Pr1 O6 2.497(5) . ? Pr1 O3 2.552(5) . ? Pr1 O2 2.556(4) . ? Pr1 O4 2.568(4) . ? Pr1 O5 2.586(5) 1_554 ? Pr1 O1 2.605(5) . ? Pr1 C15 2.926(7) 1_554 ? Pr1 C11 2.970(7) . ? Pr1 Pr1 4.0451(10) 2_576 ? O6 HW1 0.79(2) . ? O6 HW2 0.81(2) . ? O3 C6 1.267(8) . ? O1 C11 1.240(8) . ? C11 O4 1.280(8) . ? C11 C12 1.503(9) . ? C6 O7 1.251(8) . ? C6 C7 1.506(9) . ? N1 C1 1.316(11) . ? N1 C5 1.329(12) . ? C4 C3 1.369(11) . ? C4 C5 1.374(13) . ? C4 H4 0.9300 . ? C14 C13 1.514(9) . ? C14 C14 1.545(14) 2_766 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C7 C8 1.503(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C10 C9 1.513(10) . ? C10 C17 1.522(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 C8 1.530(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C5 H5 0.9300 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C12 C13 1.536(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C3 C2 1.379(12) . ? C3 C3 1.502(15) 2_665 ? C1 C2 1.387(12) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? O4 Pr1 2.489(4) 2_676 ? C17 C16 1.515(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C16 C15 1.516(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C15 O5 1.254(8) . ? C15 O2 1.278(8) 1_556 ? C15 Pr1 2.926(7) 1_556 ? O5 Pr1 2.586(5) 1_556 ? O7 Pr1 2.415(5) 2_576 ? O2 C15 1.278(8) 1_554 ? O2 Pr1 2.464(5) 2_576 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Pr1 O2 72.32(16) 2_576 2_576 ? O7 Pr1 O4 145.09(16) 2_576 2_676 ? O2 Pr1 O4 142.12(15) 2_576 2_676 ? O7 Pr1 O6 79.32(18) 2_576 . ? O2 Pr1 O6 140.67(17) 2_576 . ? O4 Pr1 O6 72.17(17) 2_676 . ? O7 Pr1 O3 136.81(15) 2_576 . ? O2 Pr1 O3 71.18(15) 2_576 . ? O4 Pr1 O3 72.32(15) 2_676 . ? O6 Pr1 O3 143.53(17) . . ? O7 Pr1 O2 74.63(15) 2_576 . ? O2 Pr1 O2 72.63(17) 2_576 . ? O4 Pr1 O2 105.89(14) 2_676 . ? O6 Pr1 O2 125.20(17) . . ? O3 Pr1 O2 73.10(15) . . ? O7 Pr1 O4 128.95(15) 2_576 . ? O2 Pr1 O4 95.48(15) 2_576 . ? O4 Pr1 O4 66.52(17) 2_676 . ? O6 Pr1 O4 81.55(18) . . ? O3 Pr1 O4 77.01(15) . . ? O2 Pr1 O4 150.00(15) . . ? O7 Pr1 O5 74.79(16) 2_576 1_554 ? O2 Pr1 O5 119.86(15) 2_576 1_554 ? O4 Pr1 O5 79.20(15) 2_676 1_554 ? O6 Pr1 O5 76.41(18) . 1_554 ? O3 Pr1 O5 104.73(16) . 1_554 ? O2 Pr1 O5 50.65(15) . 1_554 ? O4 Pr1 O5 143.58(15) . 1_554 ? O7 Pr1 O1 79.44(16) 2_576 . ? O2 Pr1 O1 73.14(15) 2_576 . ? O4 Pr1 O1 111.36(15) 2_676 . ? O6 Pr1 O1 75.35(18) . . ? O3 Pr1 O1 110.62(16) . . ? O2 Pr1 O1 141.88(15) . . ? O4 Pr1 O1 49.95(15) . . ? O5 Pr1 O1 144.65(16) 1_554 . ? O7 Pr1 C15 69.19(17) 2_576 1_554 ? O2 Pr1 C15 95.21(18) 2_576 1_554 ? O4 Pr1 C15 95.84(16) 2_676 1_554 ? O6 Pr1 C15 99.6(2) . 1_554 ? O3 Pr1 C15 91.97(18) . 1_554 ? O2 Pr1 C15 25.84(17) . 1_554 ? O4 Pr1 C15 161.25(16) . 1_554 ? O5 Pr1 C15 25.35(17) 1_554 1_554 ? O1 Pr1 C15 148.60(17) . 1_554 ? O7 Pr1 C11 103.97(18) 2_576 . ? O2 Pr1 C11 82.45(17) 2_576 . ? O4 Pr1 C11 89.88(18) 2_676 . ? O6 Pr1 C11 78.54(19) . . ? O3 Pr1 C11 93.33(17) . . ? O2 Pr1 C11 154.33(17) . . ? O4 Pr1 C11 25.43(16) . . ? O5 Pr1 C11 154.70(18) 1_554 . ? O1 Pr1 C11 24.59(16) . . ? C15 Pr1 C11 173.17(18) 1_554 . ? O7 Pr1 Pr1 69.36(11) 2_576 2_576 ? O2 Pr1 Pr1 37.09(10) 2_576 2_576 ? O4 Pr1 Pr1 130.82(10) 2_676 2_576 ? O6 Pr1 Pr1 146.65(14) . 2_576 ? O3 Pr1 Pr1 67.65(10) . 2_576 ? O2 Pr1 Pr1 35.54(10) . 2_576 ? O4 Pr1 Pr1 127.25(11) . 2_576 ? O5 Pr1 Pr1 84.41(11) 1_554 2_576 ? O1 Pr1 Pr1 108.69(11) . 2_576 ? C15 Pr1 Pr1 59.11(15) 1_554 2_576 ? C11 Pr1 Pr1 119.31(14) . 2_576 ? Pr1 O6 HW1 119(5) . . ? Pr1 O6 HW2 115(8) . . ? HW1 O6 HW2 102(9) . . ? C6 O3 Pr1 133.8(5) . . ? C11 O1 Pr1 94.4(4) . . ? O1 C11 O4 120.2(6) . . ? O1 C11 C12 121.0(6) . . ? O4 C11 C12 118.8(6) . . ? O1 C11 Pr1 61.0(4) . . ? O4 C11 Pr1 59.4(3) . . ? C12 C11 Pr1 175.2(5) . . ? O7 C6 O3 124.8(7) . . ? O7 C6 C7 117.5(6) . . ? O3 C6 C7 117.6(6) . . ? C1 N1 C5 114.7(8) . . ? C3 C4 C5 121.5(9) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C13 C14 C14 111.6(7) . 2_766 ? C13 C14 H14A 109.3 . . ? C14 C14 H14A 109.3 2_766 . ? C13 C14 H14B 109.3 . . ? C14 C14 H14B 109.3 2_766 . ? H14A C14 H14B 108.0 . . ? C8 C7 C6 115.3(6) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C10 C17 113.6(6) . . ? C9 C10 H10A 108.8 . . ? C17 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C17 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C9 C8 113.6(7) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N1 C5 C4 123.7(9) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C7 C8 C9 112.7(6) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C11 C12 C13 109.8(6) . . ? C11 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C14 C13 C12 114.0(6) . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C4 C3 C2 115.5(8) . . ? C4 C3 C3 121.9(10) . 2_665 ? C2 C3 C3 122.6(9) . 2_665 ? N1 C1 C2 125.7(10) . . ? N1 C1 H1 117.2 . . ? C2 C1 H1 117.2 . . ? C1 C2 C3 119.0(9) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C11 O4 Pr1 142.6(4) . 2_676 ? C11 O4 Pr1 95.1(4) . . ? Pr1 O4 Pr1 113.48(17) 2_676 . ? C10 C17 C16 113.5(6) . . ? C10 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? C10 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C15 C16 C17 115.0(6) . . ? C15 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? O5 C15 O2 120.6(6) . 1_556 ? O5 C15 C16 121.2(6) . . ? O2 C15 C16 118.2(6) 1_556 . ? O5 C15 Pr1 62.0(4) . 1_556 ? O2 C15 Pr1 60.7(3) 1_556 1_556 ? C16 C15 Pr1 166.2(5) . 1_556 ? C15 O5 Pr1 92.7(4) . 1_556 ? C6 O7 Pr1 139.2(5) . 2_576 ? C15 O2 Pr1 143.6(4) 1_554 2_576 ? C15 O2 Pr1 93.5(4) 1_554 . ? Pr1 O2 Pr1 107.37(17) 2_576 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 HW1 N1 0.79(2) 2.04(2) 2.826(9) 174(7) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.414 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.195 #===End data_MF7_82_c2onc_new _database_code_depnum_ccdc_archive 'CCDC 625118' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H2 N2 O6 U' _chemical_formula_sum 'C5 H2 N2 O6 U' _chemical_formula_weight 424.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.433(15) _cell_length_b 6.762(5) _cell_length_c 13.529(12) _cell_angle_alpha 90.00 _cell_angle_beta 122.77(2) _cell_angle_gamma 90.00 _cell_volume 1572(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5470 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.55 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 20.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 0.662 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD' _diffrn_measurement_method 'omega and psi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12609 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.55 _reflns_number_total 1641 _reflns_number_gt 1379 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0169P)^2^+2.1610P] 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 1641 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0429 _refine_ls_wR_factor_gt 0.0397 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.371217(13) 0.59334(3) 0.510194(19) 0.01545(7) Uani 1 1 d . . . O1 O 0.2706(2) 0.6116(7) 0.4248(4) 0.0329(11) Uani 1 1 d . . . O2 O 0.4719(2) 0.5750(7) 0.5955(4) 0.0322(11) Uani 1 1 d . . . N1 N 0.3851(3) 0.8128(7) 0.3739(4) 0.0266(13) Uani 1 1 d . . . C1 C 0.3953(5) 1.0043(9) 0.3710(6) 0.0351(18) Uani 1 1 d . . . H1 H 0.4019 1.0944 0.4276 0.042 Uiso 1 1 calc R . . N2 N 0.3948(3) 1.0499(7) 0.2749(5) 0.0284(14) Uani 1 1 d . . . H2 H 0.4005 1.1669 0.2557 0.034 Uiso 1 1 calc R . . C2 C 0.3840(4) 0.8823(8) 0.2119(5) 0.0178(13) Uani 1 1 d . . . C5 C 0.3774(4) 0.9002(9) 0.0991(5) 0.0193(13) Uani 1 1 d . . . O6 O 0.3664(3) 0.7481(6) 0.0401(4) 0.0327(11) Uani 1 1 d . . . O5 O 0.3823(3) 1.0721(6) 0.0696(4) 0.0280(11) Uani 1 1 d . . . C3 C 0.3795(3) 0.7335(8) 0.2773(5) 0.0185(13) Uani 1 1 d . . . C4 C 0.3680(4) 0.5200(8) 0.2632(5) 0.0157(13) Uani 1 1 d . . . O4 O 0.3667(3) 0.4300(6) 0.1816(4) 0.0224(10) Uani 1 1 d . . . O3 O 0.3629(2) 0.4377(5) 0.3424(4) 0.0222(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.03145(14) 0.00917(11) 0.01333(12) 0.00100(11) 0.01709(10) 0.00128(11) O1 0.038(3) 0.039(3) 0.026(3) -0.001(2) 0.020(2) 0.005(2) O2 0.033(3) 0.039(3) 0.026(3) 0.002(2) 0.017(2) 0.004(2) N1 0.064(4) 0.011(3) 0.022(3) -0.002(2) 0.034(3) 0.003(3) C1 0.084(6) 0.011(3) 0.035(4) 0.001(3) 0.049(4) 0.004(4) N2 0.071(4) 0.009(3) 0.024(3) 0.000(2) 0.038(3) -0.005(2) C2 0.043(4) 0.005(3) 0.015(3) -0.003(2) 0.022(3) 0.000(3) C5 0.040(4) 0.008(3) 0.022(3) 0.005(3) 0.025(3) 0.008(3) O6 0.077(4) 0.012(2) 0.024(3) -0.0008(19) 0.037(3) 0.003(2) O5 0.063(3) 0.015(2) 0.025(2) 0.0053(19) 0.036(2) 0.005(2) C3 0.036(4) 0.014(3) 0.017(3) 0.002(3) 0.022(3) 0.003(3) C4 0.028(3) 0.012(3) 0.013(3) 0.005(2) 0.015(3) 0.003(2) O4 0.050(3) 0.010(2) 0.021(2) -0.0027(18) 0.028(2) 0.0005(19) O3 0.048(3) 0.011(2) 0.021(2) -0.0011(17) 0.027(2) -0.0027(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. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.733(5) . ? U1 O2 1.735(5) . ? U1 O6 2.355(4) 6_566 ? U1 O5 2.370(4) 6_576 ? U1 O4 2.376(4) 6_566 ? U1 O3 2.423(4) . ? U1 N1 2.500(5) . ? N1 C1 1.316(7) . ? N1 C3 1.358(7) . ? C1 N2 1.330(7) . ? C1 H1 0.9300 . ? N2 C2 1.362(7) . ? N2 H2 0.8600 . ? C2 C3 1.376(8) . ? C2 C5 1.462(7) . ? C5 O6 1.246(7) . ? C5 O5 1.252(7) . ? O6 U1 2.355(4) 6_565 ? O5 U1 2.370(4) 6_575 ? C3 C4 1.459(8) . ? C4 O4 1.248(7) . ? C4 O3 1.261(6) . ? O4 U1 2.376(4) 6_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 179.9(2) . . ? O1 U1 O6 92.26(19) . 6_566 ? O2 U1 O6 87.74(19) . 6_566 ? O1 U1 O5 91.10(19) . 6_576 ? O2 U1 O5 88.94(19) . 6_576 ? O6 U1 O5 151.96(14) 6_566 6_576 ? O1 U1 O4 89.82(19) . 6_566 ? O2 U1 O4 90.28(18) . 6_566 ? O6 U1 O4 74.91(13) 6_566 6_566 ? O5 U1 O4 77.27(13) 6_576 6_566 ? O1 U1 O3 87.14(18) . . ? O2 U1 O3 92.77(18) . . ? O6 U1 O3 75.36(13) 6_566 . ? O5 U1 O3 132.64(13) 6_576 . ? O4 U1 O3 149.95(13) 6_566 . ? O1 U1 N1 91.9(2) . . ? O2 U1 N1 88.1(2) . . ? O6 U1 N1 137.82(14) 6_566 . ? O5 U1 N1 69.81(15) 6_576 . ? O4 U1 N1 147.07(15) 6_566 . ? O3 U1 N1 62.96(15) . . ? C1 N1 C3 107.0(5) . . ? C1 N1 U1 133.6(4) . . ? C3 N1 U1 119.4(4) . . ? N1 C1 N2 109.9(5) . . ? N1 C1 H1 125.1 . . ? N2 C1 H1 125.1 . . ? C1 N2 C2 109.3(5) . . ? C1 N2 H2 125.3 . . ? C2 N2 H2 125.3 . . ? N2 C2 C3 104.5(5) . . ? N2 C2 C5 118.5(5) . . ? C3 C2 C5 137.0(5) . . ? O6 C5 O5 125.4(5) . . ? O6 C5 C2 118.9(5) . . ? O5 C5 C2 115.6(5) . . ? C5 O6 U1 155.5(4) . 6_565 ? C5 O5 U1 170.3(4) . 6_575 ? N1 C3 C2 109.2(5) . . ? N1 C3 C4 116.1(5) . . ? C2 C3 C4 134.6(5) . . ? O4 C4 O3 124.4(5) . . ? O4 C4 C3 121.6(5) . . ? O3 C4 C3 114.0(5) . . ? C4 O4 U1 154.5(4) . 6_565 ? C4 O3 U1 127.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.773 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.199 #===End data_MF7_84b_p21onn_new _database_code_depnum_ccdc_archive 'CCDC 625119' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H6 Cu3 N8 O24 U2' _chemical_formula_sum 'C20 H6 Cu3 N8 O24 U2' _chemical_formula_weight 1409.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.3964(3) _cell_length_b 13.7766(7) _cell_length_c 20.9426(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.2160(10) _cell_angle_gamma 90.00 _cell_volume 1552.74(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7043 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 26.53 _exptl_crystal_description plates _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 12.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.606 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD' _diffrn_measurement_method 'omega and psi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16924 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.53 _reflns_number_total 3204 _reflns_number_gt 2562 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms on the unbound water molecule, O12, were not found. PLAT780 Alert "Coordinates do not Form a Properly Connected Set" - this is a common error when dealing with coordination polymers and results from Platon. ; _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^)+(0.0231P)^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 0.00028(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3204 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.96990(4) 0.122089(15) 0.112153(11) 0.00652(8) Uani 1 1 d . . . Cu2 Cu 0.25878(13) 0.36320(5) 0.26205(3) 0.00906(17) Uani 1 1 d . . . Cu3 Cu 0.5000 0.5000 0.0000 0.0065(2) Uani 1 2 d S . . C1 C 0.6554(11) 0.2704(4) 0.2120(3) 0.0074(13) Uani 1 1 d . . . C2 C 0.5640(11) 0.3415(4) 0.1635(3) 0.0078(13) Uani 1 1 d . . . C3 C 0.8329(11) 0.3447(4) 0.0649(3) 0.0081(13) Uani 1 1 d . . . C4 C 0.6267(11) 0.3715(4) 0.1043(3) 0.0060(12) Uani 1 1 d . . . C5 C -0.1515(11) 0.4567(4) 0.3056(3) 0.0071(9) Uani 1 1 d . . . C6 C 0.1801(11) 0.2750(4) 0.3951(3) 0.0091(13) Uani 1 1 d . . . H6 H 0.3037 0.2279 0.3993 0.011 Uiso 1 1 calc R . . C7 C -0.0606(11) 0.3912(4) 0.3580(3) 0.0087(13) Uani 1 1 d . . . C8 C 0.3190(11) 0.4586(4) 0.1317(3) 0.0094(13) Uani 1 1 d . . . H8 H 0.1931 0.5048 0.1303 0.011 Uiso 1 1 calc R . . C9 C -0.1360(11) 0.3686(4) 0.4174(3) 0.0088(13) Uani 1 1 d . . . C10 C -0.3416(11) 0.4016(4) 0.4567(3) 0.0071(9) Uani 1 1 d . . . N1 N 0.3693(9) 0.3976(3) 0.1806(2) 0.0067(8) Uani 1 1 d . . . N2 N 0.4712(9) 0.4452(3) 0.0851(2) 0.0067(8) Uani 1 1 d . . . N3 N 0.0194(9) 0.2946(3) 0.4391(2) 0.0084(11) Uani 1 1 d . . . H3 H 0.0141 0.2655 0.4753 0.010 Uiso 1 1 calc R . . N4 N 0.1372(9) 0.3327(3) 0.3447(2) 0.0081(11) Uani 1 1 d . . . O1 O 0.8293(8) 0.2120(3) 0.20361(19) 0.0097(9) Uani 1 1 d . . . O2 O 0.5456(8) 0.2731(3) 0.26473(18) 0.0093(9) Uani 1 1 d . . . O3 O -0.3510(8) 0.3612(3) 0.50948(19) 0.0119(9) Uani 1 1 d . . . O5 O 0.9982(7) 0.2852(3) 0.08737(19) 0.0093(9) Uani 1 1 d . . . O6 O 1.2684(7) 0.1163(3) 0.15299(19) 0.0090(9) Uani 1 1 d . . . O7 O -0.3383(8) 0.5100(3) 0.30928(18) 0.0096(9) Uani 1 1 d . . . O8 O -0.4937(7) 0.4647(3) 0.43224(19) 0.0085(9) Uani 1 1 d . . . O9 O -0.0311(7) 0.4511(3) 0.25535(19) 0.0093(9) Uani 1 1 d . . . O10 O 0.8369(8) 0.3851(3) 0.01076(19) 0.0107(9) Uani 1 1 d . . . O11 O 0.7174(7) 0.6080(3) 0.03815(19) 0.0086(9) Uani 1 1 d . . . O12 O 0.6478(8) 0.1051(3) 0.33670(19) 0.0147(10) Uani 1 1 d . . . O4 O 0.6692(7) 0.1273(3) 0.07308(18) 0.0105(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.00621(12) 0.00755(12) 0.00599(12) 0.00008(10) 0.00170(8) 0.00004(10) Cu2 0.0096(4) 0.0114(4) 0.0065(4) 0.0012(3) 0.0030(3) 0.0026(3) Cu3 0.0078(6) 0.0074(5) 0.0044(5) 0.0008(4) 0.0017(4) -0.0004(4) C1 0.006(3) 0.007(3) 0.009(3) 0.001(2) 0.001(3) -0.004(2) C2 0.007(3) 0.010(3) 0.006(3) -0.002(2) 0.000(3) 0.000(2) C3 0.008(3) 0.008(3) 0.008(3) -0.002(2) 0.003(3) -0.004(2) C4 0.010(3) 0.005(3) 0.003(3) 0.000(2) 0.001(2) -0.002(2) C5 0.010(2) 0.005(2) 0.006(2) -0.0013(17) -0.0003(18) -0.0050(16) C6 0.007(3) 0.009(3) 0.012(3) -0.001(3) 0.002(3) 0.002(2) C7 0.006(3) 0.008(3) 0.012(3) 0.002(3) 0.001(3) -0.002(2) C8 0.007(3) 0.006(3) 0.014(3) 0.003(3) -0.004(3) 0.000(2) C9 0.011(3) 0.009(3) 0.007(3) 0.000(3) -0.001(2) -0.001(2) C10 0.010(2) 0.005(2) 0.006(2) -0.0013(17) -0.0003(18) -0.0050(16) N1 0.0089(19) 0.0080(18) 0.0031(18) 0.0016(14) 0.0002(15) -0.0011(14) N2 0.0089(19) 0.0080(18) 0.0031(18) 0.0016(14) 0.0002(15) -0.0011(14) N3 0.008(3) 0.008(3) 0.009(3) 0.002(2) 0.003(2) 0.000(2) N4 0.009(3) 0.008(2) 0.008(3) 0.000(2) 0.000(2) 0.002(2) O1 0.013(2) 0.009(2) 0.007(2) -0.0027(17) 0.0018(19) 0.0028(17) O2 0.015(2) 0.010(2) 0.004(2) -0.0017(17) 0.0043(18) -0.0003(17) O3 0.013(2) 0.012(2) 0.011(2) 0.0027(18) 0.0040(19) 0.0025(18) O5 0.010(2) 0.008(2) 0.010(2) -0.0006(18) 0.0018(18) 0.0004(17) O6 0.005(2) 0.012(2) 0.011(2) 0.0021(18) 0.0035(17) -0.0013(17) O7 0.015(2) 0.009(2) 0.005(2) 0.0001(17) 0.0049(19) 0.0049(17) O8 0.009(2) 0.008(2) 0.008(2) 0.0060(17) 0.0009(18) -0.0004(16) O9 0.009(2) 0.012(2) 0.007(2) 0.0002(18) 0.0042(18) 0.0052(17) O10 0.015(2) 0.012(2) 0.006(2) 0.0005(19) 0.0045(18) 0.0002(18) O11 0.009(2) 0.005(2) 0.012(2) -0.0025(17) 0.0018(18) -0.0007(16) O12 0.024(3) 0.014(2) 0.006(2) 0.0030(18) 0.0007(19) -0.0033(19) O4 0.010(2) 0.012(2) 0.010(2) -0.0003(19) 0.0023(18) -0.0022(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O4 1.764(4) . ? U1 O6 1.769(4) . ? U1 O5 2.314(4) . ? U1 O8 2.366(4) 2_545 ? U1 O7 2.402(4) 2_545 ? U1 O3 2.432(4) 4_765 ? U1 O1 2.448(4) . ? Cu2 N1 1.908(5) . ? Cu2 N4 1.941(5) . ? Cu2 O9 1.975(4) . ? Cu2 O2 1.982(4) . ? Cu3 N2 1.953(5) . ? Cu3 N2 1.953(5) 3_665 ? Cu3 O11 2.023(4) . ? Cu3 O11 2.023(4) 3_665 ? Cu3 O10 2.409(4) . ? Cu3 O10 2.409(4) 3_665 ? C1 O1 1.258(7) . ? C1 O2 1.292(7) . ? C1 C2 1.470(8) . ? C2 N1 1.372(7) . ? C2 C4 1.374(8) . ? C3 O10 1.265(7) . ? C3 O5 1.275(7) . ? C3 C4 1.480(8) . ? C4 N2 1.358(7) . ? C5 O7 1.254(7) . ? C5 O9 1.279(7) . ? C5 C7 1.476(8) . ? C6 N4 1.329(7) . ? C6 N3 1.338(7) . ? C6 H6 0.9300 . ? C7 C9 1.373(8) . ? C7 N4 1.382(7) . ? C8 N2 1.333(7) . ? C8 N1 1.337(7) . ? C8 H8 0.9300 . ? C9 N3 1.376(7) . ? C9 C10 1.499(8) . ? C10 O3 1.243(7) . ? C10 O8 1.277(7) . ? N3 H3 0.8600 . ? O3 U1 2.432(4) 4_466 ? O7 U1 2.402(4) 2 ? O8 U1 2.366(4) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 U1 O6 178.70(18) . . ? O4 U1 O5 85.98(16) . . ? O6 U1 O5 94.57(16) . . ? O4 U1 O8 85.97(16) . 2_545 ? O6 U1 O8 94.29(16) . 2_545 ? O5 U1 O8 142.68(14) . 2_545 ? O4 U1 O7 92.05(16) . 2_545 ? O6 U1 O7 86.81(16) . 2_545 ? O5 U1 O7 143.70(13) . 2_545 ? O8 U1 O7 72.99(13) 2_545 2_545 ? O4 U1 O3 89.88(16) . 4_765 ? O6 U1 O3 91.42(16) . 4_765 ? O5 U1 O3 70.89(13) . 4_765 ? O8 U1 O3 72.71(13) 2_545 4_765 ? O7 U1 O3 145.41(13) 2_545 4_765 ? O4 U1 O1 90.85(16) . . ? O6 U1 O1 88.18(16) . . ? O5 U1 O1 73.35(13) . . ? O8 U1 O1 143.13(13) 2_545 . ? O7 U1 O1 70.43(13) 2_545 . ? O3 U1 O1 144.09(13) 4_765 . ? N1 Cu2 N4 177.7(2) . . ? N1 Cu2 O9 94.73(18) . . ? N4 Cu2 O9 83.00(18) . . ? N1 Cu2 O2 83.44(18) . . ? N4 Cu2 O2 98.84(18) . . ? O9 Cu2 O2 177.40(17) . . ? N2 Cu3 N2 180.0(3) . 3_665 ? N2 Cu3 O11 90.38(18) . . ? N2 Cu3 O11 89.62(18) 3_665 . ? N2 Cu3 O11 89.62(18) . 3_665 ? N2 Cu3 O11 90.38(18) 3_665 3_665 ? O11 Cu3 O11 180.0(2) . 3_665 ? N2 Cu3 O10 76.74(17) . . ? N2 Cu3 O10 103.26(17) 3_665 . ? O11 Cu3 O10 91.99(14) . . ? O11 Cu3 O10 88.01(14) 3_665 . ? N2 Cu3 O10 103.26(17) . 3_665 ? N2 Cu3 O10 76.74(17) 3_665 3_665 ? O11 Cu3 O10 88.01(14) . 3_665 ? O11 Cu3 O10 91.99(14) 3_665 3_665 ? O10 Cu3 O10 180.0 . 3_665 ? O1 C1 O2 122.1(5) . . ? O1 C1 C2 123.1(5) . . ? O2 C1 C2 114.8(5) . . ? N1 C2 C4 108.0(5) . . ? N1 C2 C1 114.8(5) . . ? C4 C2 C1 137.1(6) . . ? O10 C3 O5 123.8(5) . . ? O10 C3 C4 116.9(5) . . ? O5 C3 C4 119.3(5) . . ? N2 C4 C2 107.7(5) . . ? N2 C4 C3 119.8(5) . . ? C2 C4 C3 132.3(6) . . ? O7 C5 O9 123.1(5) . . ? O7 C5 C7 122.5(5) . . ? O9 C5 C7 114.4(5) . . ? N4 C6 N3 110.0(5) . . ? N4 C6 H6 125.0 . . ? N3 C6 H6 125.0 . . ? C9 C7 N4 109.6(5) . . ? C9 C7 C5 135.0(5) . . ? N4 C7 C5 115.3(5) . . ? N2 C8 N1 111.8(5) . . ? N2 C8 H8 124.1 . . ? N1 C8 H8 124.1 . . ? C7 C9 N3 104.7(5) . . ? C7 C9 C10 135.1(6) . . ? N3 C9 C10 120.1(5) . . ? O3 C10 O8 126.5(5) . . ? O3 C10 C9 115.7(5) . . ? O8 C10 C9 117.8(5) . . ? C8 N1 C2 105.7(5) . . ? C8 N1 Cu2 141.4(4) . . ? C2 N1 Cu2 112.9(4) . . ? C8 N2 C4 106.8(5) . . ? C8 N2 Cu3 135.1(4) . . ? C4 N2 Cu3 118.0(4) . . ? C6 N3 C9 109.4(5) . . ? C6 N3 H3 125.3 . . ? C9 N3 H3 125.3 . . ? C6 N4 C7 106.3(5) . . ? C6 N4 Cu2 142.0(4) . . ? C7 N4 Cu2 111.7(4) . . ? C1 O1 U1 135.2(4) . . ? C1 O2 Cu2 113.6(4) . . ? C10 O3 U1 142.1(4) . 4_466 ? C3 O5 U1 130.6(4) . . ? C5 O7 U1 134.3(4) . 2 ? C10 O8 U1 136.9(4) . 2 ? C5 O9 Cu2 115.2(4) . . ? C3 O10 Cu3 108.1(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.485 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.210 #===End data_MF7_84g_c2onc_new _database_code_depnum_ccdc_archive 'CCDC 625120' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H4 Cu N4 O16 U2' _chemical_formula_sum ' C10 H4 Cu N4 O16 U2' _chemical_formula_weight 975.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.529(3) _cell_length_b 9.4144(15) _cell_length_c 14.660(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.848(3) _cell_angle_gamma 90.00 _cell_volume 1912.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6535 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.39 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 18.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.424 _exptl_absorpt_correction_T_max 0.485 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD' _diffrn_measurement_method 'omega and psi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14788 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 26.39 _reflns_number_total 1965 _reflns_number_gt 1661 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms on the unbound water molecule, O8, were not found. PLAT780 Alert "Coordinates do not Form a Properly Connected Set" - this is a common error when dealing with coordination polymers and results from Platon. ; _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^)+(0.0279P)^2^+84.2683P] 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 1965 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.25060(3) 0.55119(4) 0.03778(3) 0.01686(13) Uani 1 1 d . . . O1 O 0.1272(5) 0.5620(8) 0.0059(6) 0.0290(18) Uani 1 1 d . . . O2 O 0.3754(6) 0.5348(8) 0.0705(6) 0.0300(18) Uani 1 1 d . . . O4 O 0.1983(6) 0.4105(7) -0.1166(6) 0.0273(18) Uani 1 1 d . . . O6 O 0.2516(6) 0.1864(7) -0.0921(5) 0.0248(18) Uani 1 1 d . . . C1 C 0.2000(8) 0.2824(11) -0.1441(7) 0.019(2) Uani 1 1 d . . . C2 C 0.1303(8) 0.2524(11) -0.2531(7) 0.019(2) Uani 1 1 d . . . N1 N 0.0697(7) 0.3570(9) -0.3172(6) 0.020(2) Uani 1 1 d . . . H1 H 0.0679 0.4441 -0.3003 0.025 Uiso 1 1 calc R . . C3 C 0.0154(8) 0.3011(12) -0.4084(8) 0.025(2) Uani 1 1 d . . . H3 H -0.0310 0.3504 -0.4637 0.030 Uiso 1 1 calc R . . N2 N 0.0364(6) 0.1659(9) -0.4095(6) 0.0192(19) Uani 1 1 d . . . C4 C 0.1078(7) 0.1321(10) -0.3136(7) 0.014(2) Uani 1 1 d . . . C5 C 0.1408(8) -0.0178(11) -0.2979(8) 0.019(2) Uani 1 1 d . . . O3 O 0.2077(6) -0.0612(7) -0.2155(5) 0.0243(17) Uani 1 1 d . . . O7 O 0.0975(5) -0.0958(7) -0.3753(5) 0.0222(17) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 -0.5000 0.0195(4) Uani 1 2 d S . . O8 O -0.0728(8) 0.6499(9) -0.2185(7) 0.054(3) Uani 1 1 d . . . O5 O 0.2312(6) 0.7085(7) -0.0923(5) 0.0259(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0224(2) 0.00912(18) 0.01735(19) -0.00127(17) 0.00742(15) -0.00017(17) O1 0.025(4) 0.022(4) 0.035(4) -0.006(4) 0.009(4) -0.003(3) O2 0.026(4) 0.026(4) 0.039(5) -0.003(4) 0.016(4) 0.000(3) O4 0.046(5) 0.012(4) 0.021(4) -0.003(3) 0.013(4) -0.001(3) O6 0.043(5) 0.011(4) 0.014(4) 0.001(3) 0.007(3) -0.004(3) C1 0.035(6) 0.016(5) 0.013(5) 0.000(4) 0.016(5) -0.005(5) C2 0.026(6) 0.013(5) 0.020(5) -0.002(4) 0.012(5) -0.002(4) N1 0.036(6) 0.002(4) 0.025(5) -0.001(3) 0.016(4) 0.004(4) C3 0.031(6) 0.019(5) 0.022(6) 0.005(4) 0.010(5) 0.000(5) N2 0.027(5) 0.009(4) 0.020(4) -0.002(3) 0.009(4) 0.002(4) C4 0.020(5) 0.008(5) 0.012(4) -0.003(4) 0.006(4) -0.004(4) C5 0.023(6) 0.019(6) 0.019(5) 0.000(4) 0.012(5) 0.003(4) O3 0.038(5) 0.013(4) 0.016(4) 0.003(3) 0.007(3) 0.005(3) O7 0.030(4) 0.011(3) 0.012(3) -0.004(3) -0.002(3) 0.002(3) Cu1 0.0271(10) 0.0077(7) 0.0173(9) -0.0031(7) 0.0043(8) -0.0004(7) O8 0.071(7) 0.014(4) 0.054(6) -0.003(4) 0.007(5) 0.007(5) O5 0.049(5) 0.008(3) 0.022(4) 0.000(3) 0.017(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. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.759(8) . ? U1 O2 1.780(8) . ? U1 O5 2.324(7) . ? U1 O5 2.373(7) 7_565 ? U1 O6 2.379(7) 7 ? U1 O3 2.386(7) 7 ? U1 O4 2.424(7) . ? U1 U1 3.9014(9) 7_565 ? O4 C1 1.276(12) . ? O6 C1 1.220(13) . ? O6 U1 2.379(7) 7 ? C1 C2 1.498(14) . ? C2 C4 1.382(13) . ? C2 N1 1.393(13) . ? N1 C3 1.326(14) . ? N1 H1 0.8600 . ? C3 N2 1.316(14) . ? C3 H3 0.9300 . ? N2 C4 1.378(12) . ? N2 Cu1 1.960(8) . ? C4 C5 1.484(13) . ? C5 O3 1.253(12) . ? C5 O7 1.261(12) . ? O3 U1 2.386(7) 7 ? O7 Cu1 1.987(7) . ? Cu1 N2 1.960(8) 5_554 ? Cu1 O7 1.987(7) 5_554 ? O5 U1 2.373(7) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 178.3(4) . . ? O1 U1 O5 91.3(3) . . ? O2 U1 O5 89.9(3) . . ? O1 U1 O5 89.1(3) . 7_565 ? O2 U1 O5 92.4(3) . 7_565 ? O5 U1 O5 67.7(3) . 7_565 ? O1 U1 O6 88.0(3) . 7 ? O2 U1 O6 90.4(3) . 7 ? O5 U1 O6 149.0(2) . 7 ? O5 U1 O6 143.2(2) 7_565 7 ? O1 U1 O3 90.8(3) . 7 ? O2 U1 O3 89.1(3) . 7 ? O5 U1 O3 137.9(2) . 7 ? O5 U1 O3 70.3(2) 7_565 7 ? O6 U1 O3 73.1(2) 7 7 ? O1 U1 O4 85.3(3) . . ? O2 U1 O4 94.0(3) . . ? O5 U1 O4 73.6(2) . . ? O5 U1 O4 140.7(2) 7_565 . ? O6 U1 O4 75.5(2) 7 . ? O3 U1 O4 148.5(2) 7 . ? O1 U1 U1 90.2(3) . 7_565 ? O2 U1 U1 91.4(3) . 7_565 ? O5 U1 U1 34.25(17) . 7_565 ? O5 U1 U1 33.45(17) 7_565 7_565 ? O6 U1 U1 176.28(18) 7 7_565 ? O3 U1 U1 103.68(17) 7 7_565 ? O4 U1 U1 107.62(17) . 7_565 ? C1 O4 U1 140.0(7) . . ? C1 O6 U1 143.2(7) . 7 ? O6 C1 O4 127.2(10) . . ? O6 C1 C2 118.8(9) . . ? O4 C1 C2 114.0(9) . . ? C4 C2 N1 104.4(8) . . ? C4 C2 C1 133.7(9) . . ? N1 C2 C1 122.0(9) . . ? C3 N1 C2 109.1(8) . . ? C3 N1 H1 125.4 . . ? C2 N1 H1 125.4 . . ? N2 C3 N1 110.4(10) . . ? N2 C3 H3 124.8 . . ? N1 C3 H3 124.8 . . ? C3 N2 C4 107.5(9) . . ? C3 N2 Cu1 141.4(8) . . ? C4 N2 Cu1 111.1(6) . . ? N2 C4 C2 108.6(8) . . ? N2 C4 C5 116.1(8) . . ? C2 C4 C5 135.2(9) . . ? O3 C5 O7 123.4(9) . . ? O3 C5 C4 122.5(9) . . ? O7 C5 C4 114.1(9) . . ? C5 O3 U1 137.5(7) . 7 ? C5 O7 Cu1 116.0(6) . . ? N2 Cu1 N2 180.0(5) . 5_554 ? N2 Cu1 O7 82.7(3) . . ? N2 Cu1 O7 97.3(3) 5_554 . ? N2 Cu1 O7 97.3(3) . 5_554 ? N2 Cu1 O7 82.7(3) 5_554 5_554 ? O7 Cu1 O7 180.0(3) . 5_554 ? U1 O5 U1 112.3(3) . 7_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.586 _refine_diff_density_min -1.366 _refine_diff_density_rms 0.269