# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H10 Mg N O8 P' _chemical_formula_sum 'C5 H10 Mg N O8 P' _chemical_formula_weight 267.42 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 5.1548(3) _cell_length_b 12.4592(8) _cell_length_c 14.0203(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.608(2) _cell_angle_gamma 90.00 _cell_volume 899.52(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5519 _cell_measurement_theta_min 2.188 _cell_measurement_theta_max 28.322 _exptl_crystal_description tabular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8703 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 8796 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2225 _reflns_number_gt 2019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2009)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2010)' _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^)+(0.0573P)^2^+0.4407P] 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 2225 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 P1 P 0.08694(7) 0.23897(3) 0.31902(3) 0.01239(12) Uani 1 1 d . . . Mg1 Mg 0.21348(10) 0.48006(4) 0.22455(4) 0.01294(14) Uani 1 1 d . . . O1 O 0.1015(2) 0.32470(8) 0.24534(8) 0.0178(2) Uani 1 1 d . . . O2 O -0.2062(2) 0.21438(10) 0.33971(9) 0.0243(3) Uani 1 1 d . . . H2C H -0.2270 0.1493 0.3438 0.036 Uiso 1 1 calc R . . O3 O 0.2267(2) 0.13657(9) 0.30257(8) 0.0204(3) Uani 1 1 d . . . O4 O 0.0119(2) 0.53022(9) 0.34176(8) 0.0194(2) Uani 1 1 d . . . O5 O 0.2605(2) 0.62199(12) 0.44767(10) 0.0321(3) Uani 1 1 d . . . O6 O -0.1498(2) 0.50302(9) 0.14189(8) 0.0184(2) Uani 1 1 d . . . O7 O 0.5177(2) 0.46515(11) 0.32494(9) 0.0269(3) Uani 1 1 d . . . H7A H 0.6590 0.4829 0.3003 0.040 Uiso 1 1 d R . . H7B H 0.4905 0.5056 0.3723 0.040 Uiso 1 1 d R . . O8 O 0.4501(2) 0.43405(9) 0.11254(8) 0.0191(2) Uani 1 1 d . . . N1 N -0.1330(3) 0.76348(9) 0.48214(9) 0.0128(3) Uani 1 1 d . . . H1A H 0.0333 0.7871 0.4912 0.015 Uiso 1 1 calc R . . C1 C 0.0621(3) 0.60879(12) 0.39702(11) 0.0172(3) Uani 1 1 d . . . C2 C -0.1471(3) 0.69435(12) 0.39496(11) 0.0178(3) Uani 1 1 d . . . H2A H -0.1296 0.7391 0.3390 0.021 Uiso 1 1 calc R . . H2B H -0.3161 0.6601 0.3896 0.021 Uiso 1 1 calc R . . C3 C -0.3051(3) 0.85907(12) 0.46653(11) 0.0160(3) Uani 1 1 d . . . H3A H -0.3284 0.8946 0.5271 0.019 Uiso 1 1 calc R . . H3B H -0.4743 0.8357 0.4415 0.019 Uiso 1 1 calc R . . C4 C 0.2018(3) 0.29950(11) 0.43097(10) 0.0145(3) Uani 1 1 d . . . H4A H 0.3891 0.3068 0.4308 0.017 Uiso 1 1 calc R . . H4B H 0.1286 0.3710 0.4352 0.017 Uiso 1 1 calc R . . C5 C -0.3095(3) 0.43795(11) 0.10277(10) 0.0143(3) 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 P1 0.0153(2) 0.00926(19) 0.0125(2) 0.00039(12) -0.00010(14) -0.00019(12) Mg1 0.0134(3) 0.0103(3) 0.0152(3) -0.00005(17) 0.00138(19) -0.00053(17) O1 0.0270(6) 0.0119(5) 0.0142(5) 0.0021(4) -0.0024(4) -0.0040(4) O2 0.0172(6) 0.0198(6) 0.0360(7) -0.0006(5) 0.0024(5) -0.0044(4) O3 0.0257(6) 0.0118(5) 0.0238(6) -0.0019(4) 0.0029(5) 0.0032(4) O4 0.0187(5) 0.0182(5) 0.0217(6) -0.0065(4) 0.0048(4) -0.0013(4) O5 0.0191(6) 0.0439(8) 0.0327(7) -0.0156(6) -0.0048(5) 0.0044(5) O6 0.0179(6) 0.0144(5) 0.0224(6) -0.0043(4) -0.0034(4) -0.0006(4) O7 0.0187(6) 0.0347(7) 0.0271(6) 0.0044(5) -0.0022(5) -0.0055(5) O8 0.0153(5) 0.0200(6) 0.0222(5) -0.0042(4) 0.0040(4) 0.0000(4) N1 0.0143(6) 0.0108(6) 0.0132(6) 0.0005(4) 0.0011(4) 0.0001(4) C1 0.0172(7) 0.0185(7) 0.0164(7) -0.0016(5) 0.0052(5) -0.0001(6) C2 0.0239(8) 0.0160(7) 0.0133(7) -0.0033(5) -0.0020(6) 0.0019(6) C3 0.0163(7) 0.0134(7) 0.0185(7) 0.0031(5) 0.0038(5) 0.0032(5) C4 0.0199(7) 0.0111(7) 0.0125(7) 0.0021(5) 0.0004(5) -0.0022(5) C5 0.0163(7) 0.0126(7) 0.0139(6) -0.0005(5) 0.0012(5) 0.0005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O3 1.4883(11) . ? P1 O1 1.4903(11) . ? P1 O2 1.5817(12) . ? P1 C4 1.8161(15) . ? Mg1 O3 2.0131(12) 2 ? Mg1 O1 2.0446(11) . ? Mg1 O7 2.0672(13) . ? Mg1 O4 2.0799(12) . ? Mg1 O8 2.1111(12) . ? Mg1 O6 2.1757(12) . ? O2 H2C 0.8200 . ? O3 Mg1 2.0131(12) 2_545 ? O4 C1 1.2677(19) . ? O5 C1 1.229(2) . ? O6 C5 1.2628(18) . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? O8 C5 1.2541(18) 1_655 ? N1 C3 1.4951(18) . ? N1 C2 1.4944(18) . ? N1 C4 1.5048(18) 3_566 ? N1 H1A 0.9100 . ? C1 C2 1.516(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C5 1.520(2) 2_455 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N1 1.5048(18) 3_566 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O8 1.2541(18) 1_455 ? C5 C3 1.520(2) 2_445 ? 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 O3 P1 O1 117.85(7) . . ? O3 P1 O2 109.61(7) . . ? O1 P1 O2 110.15(7) . . ? O3 P1 C4 110.42(7) . . ? O1 P1 C4 106.07(6) . . ? O2 P1 C4 101.45(7) . . ? O3 Mg1 O1 172.14(6) 2 . ? O3 Mg1 O7 95.60(5) 2 . ? O1 Mg1 O7 91.62(5) . . ? O3 Mg1 O4 86.82(5) 2 . ? O1 Mg1 O4 91.00(5) . . ? O7 Mg1 O4 83.09(5) . . ? O3 Mg1 O8 91.37(5) 2 . ? O1 Mg1 O8 91.46(5) . . ? O7 Mg1 O8 92.07(5) . . ? O4 Mg1 O8 174.64(5) . . ? O3 Mg1 O6 84.70(5) 2 . ? O1 Mg1 O6 87.63(5) . . ? O7 Mg1 O6 169.19(5) . . ? O4 Mg1 O6 86.14(5) . . ? O8 Mg1 O6 98.73(5) . . ? P1 O1 Mg1 143.21(7) . . ? P1 O2 H2C 109.5 . . ? P1 O3 Mg1 159.89(8) . 2_545 ? C1 O4 Mg1 128.28(10) . . ? C5 O6 Mg1 132.47(10) . . ? Mg1 O7 H7A 109.7 . . ? Mg1 O7 H7B 109.4 . . ? H7A O7 H7B 109.8 . . ? C5 O8 Mg1 132.68(10) 1_655 . ? C3 N1 C2 109.45(12) . . ? C3 N1 C4 111.95(12) . 3_566 ? C2 N1 C4 110.92(11) . 3_566 ? C3 N1 H1A 108.1 . . ? C2 N1 H1A 108.1 . . ? C4 N1 H1A 108.1 3_566 . ? O5 C1 O4 126.70(15) . . ? O5 C1 C2 119.30(14) . . ? O4 C1 C2 113.97(14) . . ? N1 C2 C1 112.44(13) . . ? N1 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N1 C3 C5 111.31(12) . 2_455 ? N1 C3 H3A 109.4 . . ? C5 C3 H3A 109.4 2_455 . ? N1 C3 H3B 109.4 . . ? C5 C3 H3B 109.4 2_455 . ? H3A C3 H3B 108.0 . . ? N1 C4 P1 113.81(10) 3_566 . ? N1 C4 H4A 108.8 3_566 . ? P1 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 3_566 . ? P1 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? O8 C5 O6 127.26(14) 1_455 . ? O8 C5 C3 117.34(13) 1_455 2_445 ? O6 C5 C3 115.35(13) . 2_445 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Mg1 -121.11(12) . . . . ? O2 P1 O1 Mg1 112.15(13) . . . . ? C4 P1 O1 Mg1 3.14(15) . . . . ? O3 Mg1 O1 P1 -123.2(4) 2 . . . ? O7 Mg1 O1 P1 33.62(13) . . . . ? O4 Mg1 O1 P1 -49.50(13) . . . . ? O8 Mg1 O1 P1 125.73(13) . . . . ? O6 Mg1 O1 P1 -135.59(13) . . . . ? O1 P1 O3 Mg1 -111.6(2) . . . 2_545 ? O2 P1 O3 Mg1 15.4(2) . . . 2_545 ? C4 P1 O3 Mg1 126.4(2) . . . 2_545 ? O3 Mg1 O4 C1 -36.88(14) 2 . . . ? O1 Mg1 O4 C1 150.67(14) . . . . ? O7 Mg1 O4 C1 59.16(14) . . . . ? O8 Mg1 O4 C1 33.5(6) . . . . ? O6 Mg1 O4 C1 -121.77(14) . . . . ? O3 Mg1 O6 C5 163.62(14) 2 . . . ? O1 Mg1 O6 C5 -18.06(14) . . . . ? O7 Mg1 O6 C5 -104.3(3) . . . . ? O4 Mg1 O6 C5 -109.22(14) . . . . ? O8 Mg1 O6 C5 73.05(14) . . . . ? O3 Mg1 O8 C5 71.35(14) 2 . . 1_655 ? O1 Mg1 O8 C5 -115.99(14) . . . 1_655 ? O7 Mg1 O8 C5 -24.31(14) . . . 1_655 ? O4 Mg1 O8 C5 1.2(6) . . . 1_655 ? O6 Mg1 O8 C5 156.19(13) . . . 1_655 ? Mg1 O4 C1 O5 -60.9(2) . . . . ? Mg1 O4 C1 C2 116.96(13) . . . . ? C3 N1 C2 C1 168.08(12) . . . . ? C4 N1 C2 C1 -67.89(16) 3_566 . . . ? O5 C1 C2 N1 -22.5(2) . . . . ? O4 C1 C2 N1 159.45(13) . . . . ? C2 N1 C3 C5 -72.42(15) . . . 2_455 ? C4 N1 C3 C5 164.17(12) 3_566 . . 2_455 ? O3 P1 C4 N1 -67.44(12) . . . 3_566 ? O1 P1 C4 N1 163.81(10) . . . 3_566 ? O2 P1 C4 N1 48.71(12) . . . 3_566 ? Mg1 O6 C5 O8 127.67(15) . . . 1_455 ? Mg1 O6 C5 C3 -54.88(19) . . . 2_445 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.530 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 930267' ####################################################################### # # 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_3 #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H10 N O8 P Sr' _chemical_formula_sum 'C5 H10 N O8 P Sr' _chemical_formula_weight 330.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall ' P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.3705(2) _cell_length_b 8.0800(3) _cell_length_c 16.6038(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 988.82(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6795 _cell_measurement_theta_min 2.8036 _cell_measurement_theta_max 28.2346 _exptl_crystal_description columnar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 5.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3981 _exptl_absorpt_correction_T_max 0.4298 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 9252 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2440 _reflns_number_gt 2212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2009)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2010)' _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.120(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 2440 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0395 _refine_ls_wR_factor_gt 0.0385 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.002 _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 Sr1 Sr 0.92736(3) 0.33007(3) 0.568286(12) 0.01700(6) Uani 1 1 d . . . P1 P 0.91214(8) 0.19162(7) 0.37196(3) 0.01534(13) Uani 1 1 d . . . O1 O 0.7747(2) 0.20830(17) 0.43776(10) 0.0200(4) Uani 1 1 d . . . O2 O 0.6062(2) 0.3063(2) 0.60379(10) 0.0280(4) Uani 1 1 d . . . O3 O 0.8805(2) 0.3261(2) 0.30495(9) 0.0236(4) Uani 1 1 d . . . H3C H 0.7745 0.3228 0.2900 0.035 Uiso 1 1 calc R . . O4 O 1.0434(2) 0.2298(2) 0.72172(9) 0.0301(4) Uani 1 1 d . . . O5 O 0.9552(2) 0.5884(2) 0.66243(10) 0.0299(4) Uani 1 1 d . . . O6 O 1.0858(2) 0.5664(2) 0.48385(9) 0.0297(4) Uani 1 1 d . . . O7 O 0.7868(2) 0.6014(2) 0.47577(10) 0.0299(4) Uani 1 1 d . . . N1 N 0.8141(2) -0.1489(2) 0.36194(10) 0.0172(4) Uani 1 1 d . . . H1A H 0.7420 -0.1207 0.4035 0.021 Uiso 1 1 d R . . C1 C 0.8578(3) 0.0060(2) 0.31526(13) 0.0184(6) Uani 1 1 d . . . H1B H 0.7549 0.0308 0.2809 0.022 Uiso 1 1 calc R . . H1C H 0.9597 -0.0182 0.2802 0.022 Uiso 1 1 calc R . . C2 C 0.7088(3) -0.2606(3) 0.30684(14) 0.0214(6) Uani 1 1 d . . . H2A H 0.6938 -0.3680 0.3321 0.026 Uiso 1 1 calc R . . H2B H 0.7755 -0.2761 0.2571 0.026 Uiso 1 1 calc R . . C3 C 0.9818(3) -0.2283(3) 0.39500(14) 0.0210(6) Uani 1 1 d . . . H3A H 1.0562 -0.1437 0.4200 0.025 Uiso 1 1 calc R . . H3B H 1.0507 -0.2751 0.3507 0.025 Uiso 1 1 calc R . . C4 C 0.5223(3) -0.1866(3) 0.28827(13) 0.0181(5) Uani 1 1 d . . . C5 C 0.9448(4) -0.3636(3) 0.45631(13) 0.0214(5) Uani 1 1 d . . . O1W O 0.9249(3) 0.0093(2) 0.58210(11) 0.0429(5) Uani 1 1 d . . . H1WB H 1.0131 -0.0312 0.5557 0.064 Uiso 1 1 d R . . H1WA H 0.8254 -0.0284 0.5639 0.064 Uiso 1 1 d 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 Sr1 0.01078(10) 0.02171(11) 0.01852(10) 0.00040(11) -0.00050(10) -0.00163(11) P1 0.0123(3) 0.0171(3) 0.0167(3) 0.0003(2) -0.0008(2) -0.0010(3) O1 0.0194(8) 0.0237(9) 0.0169(8) -0.0008(8) 0.0041(7) -0.0022(7) O2 0.0152(9) 0.0316(10) 0.0371(9) 0.0004(8) 0.0089(7) 0.0010(8) O3 0.0186(9) 0.0264(9) 0.0258(8) 0.0090(9) 0.0000(7) -0.0020(9) O4 0.0217(10) 0.0418(11) 0.0267(9) 0.0111(8) 0.0073(8) -0.0001(8) O5 0.0200(10) 0.0384(11) 0.0313(9) -0.0090(8) 0.0009(8) -0.0012(9) O6 0.0277(10) 0.0295(9) 0.0320(9) 0.0107(8) 0.0007(9) 0.0087(9) O7 0.0244(10) 0.0343(10) 0.0310(10) 0.0069(8) 0.0045(8) -0.0027(8) N1 0.0177(10) 0.0160(10) 0.0180(10) -0.0015(9) -0.0009(8) 0.0018(9) C1 0.0208(13) 0.0167(13) 0.0176(12) 0.0033(11) -0.0011(10) 0.0032(10) C2 0.0235(13) 0.0198(12) 0.0210(13) -0.0036(10) -0.0037(11) -0.0033(11) C3 0.0181(13) 0.0208(13) 0.0241(13) 0.0017(11) -0.0038(10) 0.0012(10) C4 0.0204(12) 0.0155(12) 0.0185(12) -0.0024(11) -0.0034(9) -0.0014(11) C5 0.0288(14) 0.0157(12) 0.0198(11) -0.0014(9) -0.0001(11) 0.0014(12) O1W 0.0414(12) 0.0359(10) 0.0513(12) 0.0008(9) -0.0155(12) 0.0027(10) _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 Sr1 O2 2.4468(15) . ? Sr1 O1 2.5808(15) 4_556 ? Sr1 O1W 2.6017(16) . ? Sr1 O5 2.6156(17) . ? Sr1 O1 2.6326(16) . ? Sr1 O6 2.6412(16) . ? Sr1 O4 2.8067(16) . ? Sr1 O7 2.8702(17) . ? Sr1 C5 3.098(2) 1_565 ? Sr1 P1 3.4482(6) . ? Sr1 P1 3.7124(6) 4_556 ? Sr1 Sr1 4.5163(3) 4_456 ? P1 O2 1.4861(15) 4_556 ? P1 O1 1.4959(16) . ? P1 O3 1.5726(16) . ? P1 C1 1.815(2) . ? P1 Sr1 3.7124(6) 4_456 ? O1 Sr1 2.5808(15) 4_456 ? O2 P1 1.4861(15) 4_456 ? O3 H3C 0.8200 . ? O4 C4 1.256(2) 2_655 ? O5 C4 1.242(3) 4_556 ? O6 C5 1.268(3) 1_565 ? O7 C5 1.241(3) 1_565 ? N1 C3 1.497(3) . ? N1 C2 1.502(3) . ? N1 C1 1.507(3) . ? N1 H1A 0.9000 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C4 1.531(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C5 1.518(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O5 1.242(3) 4_456 ? C4 O4 1.256(2) 2_654 ? C5 O7 1.241(3) 1_545 ? C5 O6 1.268(3) 1_545 ? C5 Sr1 3.098(2) 1_545 ? O1W H1WB 0.8501 . ? O1W H1WA 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sr1 O1 163.65(5) . 4_556 ? O2 Sr1 O1W 83.90(6) . . ? O1 Sr1 O1W 83.73(6) 4_556 . ? O2 Sr1 O5 89.69(5) . . ? O1 Sr1 O5 92.36(5) 4_556 . ? O1W Sr1 O5 137.96(5) . . ? O2 Sr1 O1 75.86(5) . . ? O1 Sr1 O1 110.31(3) 4_556 . ? O1W Sr1 O1 72.38(5) . . ? O5 Sr1 O1 145.46(5) . . ? O2 Sr1 O6 127.75(5) . . ? O1 Sr1 O6 68.14(5) 4_556 . ? O1W Sr1 O6 140.37(6) . . ? O5 Sr1 O6 72.87(5) . . ? O1 Sr1 O6 91.27(5) . . ? O2 Sr1 O4 93.06(5) . . ? O1 Sr1 O4 72.45(5) 4_556 . ? O1W Sr1 O4 68.57(5) . . ? O5 Sr1 O4 70.37(5) . . ? O1 Sr1 O4 140.31(5) . . ? O6 Sr1 O4 123.77(5) . . ? O2 Sr1 O7 80.77(5) . . ? O1 Sr1 O7 115.40(5) 4_556 . ? O1W Sr1 O7 143.65(5) . . ? O5 Sr1 O7 74.86(5) . . ? O1 Sr1 O7 71.98(5) . . ? O6 Sr1 O7 47.41(5) . . ? O4 Sr1 O7 144.71(5) . . ? O2 Sr1 C5 104.31(6) . 1_565 ? O1 Sr1 C5 91.81(6) 4_556 1_565 ? O1W Sr1 C5 148.10(6) . 1_565 ? O5 Sr1 C5 73.62(5) . 1_565 ? O1 Sr1 C5 79.76(5) . 1_565 ? O6 Sr1 C5 23.87(5) . 1_565 ? O4 Sr1 C5 139.70(5) . 1_565 ? O7 Sr1 C5 23.60(5) . 1_565 ? O2 Sr1 P1 99.84(4) . . ? O1 Sr1 P1 87.51(4) 4_556 . ? O1W Sr1 P1 76.11(4) . . ? O5 Sr1 P1 145.73(4) . . ? O1 Sr1 P1 24.02(3) . . ? O6 Sr1 P1 75.36(4) . . ? O4 Sr1 P1 140.74(4) . . ? O7 Sr1 P1 74.34(4) . . ? C5 Sr1 P1 72.13(4) 1_565 . ? O2 Sr1 P1 149.65(4) . 4_556 ? O1 Sr1 P1 18.19(4) 4_556 4_556 ? O1W Sr1 P1 86.34(5) . 4_556 ? O5 Sr1 P1 78.60(4) . 4_556 ? O1 Sr1 P1 127.86(3) . 4_556 ? O6 Sr1 P1 75.56(4) . 4_556 ? O4 Sr1 P1 56.67(4) . 4_556 ? O7 Sr1 P1 121.77(4) . 4_556 ? C5 Sr1 P1 99.11(5) 1_565 4_556 ? P1 Sr1 P1 105.584(15) . 4_556 ? O2 Sr1 Sr1 46.30(4) . 4_456 ? O1 Sr1 Sr1 139.07(4) 4_556 4_456 ? O1W Sr1 Sr1 75.71(4) . 4_456 ? O5 Sr1 Sr1 126.35(4) . 4_456 ? O1 Sr1 Sr1 29.64(3) . 4_456 ? O6 Sr1 Sr1 107.54(4) . 4_456 ? O4 Sr1 Sr1 128.43(3) . 4_456 ? O7 Sr1 Sr1 69.85(4) . 4_456 ? C5 Sr1 Sr1 87.78(5) 1_565 4_456 ? P1 Sr1 Sr1 53.550(11) . 4_456 ? P1 Sr1 Sr1 154.962(12) 4_556 4_456 ? O2 P1 O1 116.92(10) 4_556 . ? O2 P1 O3 109.07(9) 4_556 . ? O1 P1 O3 110.73(8) . . ? O2 P1 C1 111.23(10) 4_556 . ? O1 P1 C1 107.69(10) . . ? O3 P1 C1 99.86(9) . . ? O2 P1 Sr1 73.08(7) 4_556 . ? O1 P1 Sr1 45.76(6) . . ? O3 P1 Sr1 116.71(6) . . ? C1 P1 Sr1 139.94(7) . . ? O2 P1 Sr1 148.70(7) 4_556 4_456 ? O1 P1 Sr1 32.58(6) . 4_456 ? O3 P1 Sr1 94.53(6) . 4_456 ? C1 P1 Sr1 83.53(8) . 4_456 ? Sr1 P1 Sr1 78.109(12) . 4_456 ? P1 O1 Sr1 129.23(9) . 4_456 ? P1 O1 Sr1 110.22(8) . . ? Sr1 O1 Sr1 120.05(6) 4_456 . ? P1 O2 Sr1 174.58(10) 4_456 . ? P1 O3 H3C 109.5 . . ? C4 O4 Sr1 139.60(14) 2_655 . ? C4 O5 Sr1 159.15(15) 4_556 . ? C5 O6 Sr1 98.71(14) 1_565 . ? C5 O7 Sr1 88.57(13) 1_565 . ? C3 N1 C2 113.10(18) . . ? C3 N1 C1 111.62(17) . . ? C2 N1 C1 107.25(16) . . ? C3 N1 H1A 108.4 . . ? C2 N1 H1A 108.2 . . ? C1 N1 H1A 108.1 . . ? N1 C1 P1 117.81(14) . . ? N1 C1 H1B 107.9 . . ? P1 C1 H1B 107.9 . . ? N1 C1 H1C 107.9 . . ? P1 C1 H1C 107.9 . . ? H1B C1 H1C 107.2 . . ? N1 C2 C4 110.61(18) . . ? N1 C2 H2A 109.5 . . ? C4 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N1 C3 C5 113.97(18) . . ? N1 C3 H3A 108.8 . . ? C5 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C5 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? O5 C4 O4 127.2(2) 4_456 2_654 ? O5 C4 C2 118.30(19) 4_456 . ? O4 C4 C2 114.5(2) 2_654 . ? O7 C5 O6 125.0(2) 1_545 1_545 ? O7 C5 C3 120.5(2) 1_545 . ? O6 C5 C3 114.5(2) 1_545 . ? O7 C5 Sr1 67.83(12) 1_545 1_545 ? O6 C5 Sr1 57.42(11) 1_545 1_545 ? C3 C5 Sr1 170.01(16) . 1_545 ? Sr1 O1W H1WB 109.4 . . ? Sr1 O1W H1WA 109.4 . . ? H1WB O1W H1WA 109.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3C O4 0.82 1.77 2.564(2) 163.7 4_456 N1 H1A O6 0.90 2.24 3.136(2) 173.2 4_456 O1W H1WB O7 0.85 2.16 2.973(3) 160.2 4_556 O1W H1WA O6 0.85 1.96 2.797(3) 167.9 4_456 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.353 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.069 _database_code_depnum_ccdc_archive 'CCDC 930269' ####################################################################### # # 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_4 #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H8 N O8 P Sr2' _chemical_formula_sum 'C5 H8 N O8 P Sr2' _chemical_formula_weight 416.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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 6.8609(5) _cell_length_b 7.2044(6) _cell_length_c 11.5167(9) _cell_angle_alpha 96.1220(10) _cell_angle_beta 103.5390(10) _cell_angle_gamma 95.2600(10) _cell_volume 546.26(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3369 _cell_measurement_theta_min 2.865 _cell_measurement_theta_max 28.249 _exptl_crystal_description lamellar _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 9.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1092 _exptl_absorpt_correction_T_max 0.2411 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6430 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2690 _reflns_number_gt 2365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2008)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2008)' _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^)+(0.0474P)^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 2690 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Sr1 Sr 0.46001(4) 0.85179(3) 0.14334(2) 0.01384(9) Uani 1 1 d . . . Sr2 Sr 0.80426(4) 0.66386(3) -0.07866(2) 0.01433(9) Uani 1 1 d . . . P1 P 0.31177(10) 0.63132(10) -0.12866(7) 0.01301(16) Uani 1 1 d . . . O1 O 0.5489(3) 1.1822(3) 0.09556(19) 0.0163(4) Uani 1 1 d . . . O2 O 1.1798(3) 0.6177(3) -0.03858(19) 0.0173(4) Uani 1 1 d . . . O3 O 0.5599(3) 0.5277(3) 0.1359(2) 0.0213(5) Uani 1 1 d . . . O4 O 0.2551(3) 0.6255(3) 0.2517(2) 0.0240(5) Uani 1 1 d . . . O5 O 0.6529(4) 0.2804(3) -0.4497(2) 0.0400(7) Uani 1 1 d . . . O6 O 0.8647(3) 0.9981(3) -0.1272(2) 0.0223(5) Uani 1 1 d . . . O7 O 0.8381(3) 0.8581(3) 0.1346(2) 0.0232(5) Uani 1 1 d . . . O1W O 0.5522(4) 0.9866(4) 0.3624(2) 0.0439(7) Uani 1 1 d . . . H1WA H 0.6033 1.0690 0.4175 0.053 Uiso 1 1 d R . . H1WB H 0.4876 0.8940 0.4059 0.053 Uiso 1 1 d R . . N1 N 0.9534(3) 0.7009(3) -0.2856(2) 0.0162(5) Uani 1 1 d . . . C1 C 1.1403(4) 0.6094(4) -0.2759(3) 0.0182(6) Uani 1 1 d . . . H1A H 1.2135 0.6607 -0.3302 0.022 Uiso 1 1 calc R . . H1B H 1.1016 0.4765 -0.3046 0.022 Uiso 1 1 calc R . . C2 C 0.9889(5) 0.9044(4) -0.2978(3) 0.0203(6) Uani 1 1 d . . . H2A H 0.8769 0.9375 -0.3574 0.024 Uiso 1 1 calc R . . H2B H 1.1108 0.9282 -0.3255 0.024 Uiso 1 1 calc R . . C3 C 0.7958(5) 0.5979(4) -0.3865(3) 0.0214(6) Uani 1 1 d . . . H3A H 0.8470 0.5860 -0.4583 0.026 Uiso 1 1 calc R . . H3B H 0.6808 0.6686 -0.4021 0.026 Uiso 1 1 calc R . . C4 C 1.0102(4) 1.0261(4) -0.1775(3) 0.0167(6) Uani 1 1 d . . . C5 C 0.7270(5) 0.4016(4) -0.3603(3) 0.0213(6) 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 Sr1 0.01252(14) 0.01188(14) 0.01798(16) 0.00131(10) 0.00594(11) 0.00102(10) Sr2 0.01101(14) 0.01391(15) 0.01886(17) 0.00266(11) 0.00512(11) 0.00129(10) P1 0.0099(3) 0.0130(3) 0.0161(4) 0.0017(3) 0.0035(3) 0.0008(2) O1 0.0156(9) 0.0114(9) 0.0211(11) 0.0015(8) 0.0045(8) -0.0023(7) O2 0.0116(9) 0.0232(11) 0.0187(11) 0.0054(9) 0.0055(8) 0.0027(8) O3 0.0162(10) 0.0151(10) 0.0323(13) 0.0022(9) 0.0049(9) 0.0042(8) O4 0.0282(11) 0.0217(11) 0.0219(12) 0.0020(9) 0.0092(10) -0.0046(9) O5 0.0597(18) 0.0295(14) 0.0225(14) -0.0059(11) 0.0070(13) -0.0181(13) O6 0.0194(11) 0.0207(11) 0.0313(13) 0.0062(9) 0.0136(10) 0.0036(8) O7 0.0175(10) 0.0217(11) 0.0283(13) -0.0037(9) 0.0076(9) -0.0050(8) O1W 0.0584(17) 0.0440(16) 0.0245(14) -0.0118(12) 0.0206(13) -0.0260(13) N1 0.0128(11) 0.0165(12) 0.0171(13) -0.0005(10) 0.0015(9) -0.0010(9) C1 0.0137(13) 0.0219(15) 0.0174(15) -0.0010(12) 0.0020(11) 0.0025(11) C2 0.0228(15) 0.0170(14) 0.0210(16) 0.0044(12) 0.0057(13) -0.0013(12) C3 0.0197(14) 0.0215(16) 0.0191(17) 0.0021(13) -0.0013(12) -0.0010(12) C4 0.0130(12) 0.0157(14) 0.0225(16) 0.0044(12) 0.0051(11) 0.0037(10) C5 0.0205(14) 0.0205(15) 0.0198(16) -0.0005(12) 0.0026(12) -0.0050(12) _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 Sr1 O3 2.491(2) . ? Sr1 O1W 2.515(3) . ? Sr1 O6 2.541(2) 2_675 ? Sr1 O1 2.5516(19) . ? Sr1 O7 2.616(2) . ? Sr1 O4 2.650(2) . ? Sr1 O1 2.722(2) 2_675 ? Sr1 O2 2.774(2) 1_455 ? Sr1 P1 3.2436(8) . ? Sr1 Sr2 3.8968(4) 2_665 ? Sr1 Sr2 4.0773(4) . ? Sr1 Sr2 4.1353(4) 2_675 ? Sr1 H1WB 2.9659 . ? Sr2 O6 2.549(2) . ? Sr2 O2 2.550(2) 2_765 ? Sr2 O2 2.5685(19) . ? Sr2 O3 2.643(2) 2_665 ? Sr2 O7 2.643(2) . ? Sr2 O4 2.657(2) 2_665 ? Sr2 O1 2.731(2) 2_675 ? Sr2 N1 2.833(2) . ? Sr2 P1 3.2739(8) . ? Sr2 C4 3.288(3) . ? Sr2 C4 3.410(3) 2_775 ? Sr2 P1 3.5383(8) 2_665 ? P1 O3 1.515(2) 2_665 ? P1 O2 1.533(2) 1_455 ? P1 O1 1.533(2) 2_675 ? P1 C1 1.806(3) 1_455 ? P1 Sr2 3.5383(8) 2_665 ? P1 Sr2 3.6838(8) 1_455 ? O1 P1 1.533(2) 2_675 ? O1 Sr1 2.722(2) 2_675 ? O1 Sr2 2.731(2) 2_675 ? O2 P1 1.533(2) 1_655 ? O2 Sr2 2.550(2) 2_765 ? O2 Sr1 2.774(2) 1_655 ? O3 P1 1.515(2) 2_665 ? O3 Sr2 2.643(2) 2_665 ? O4 C5 1.266(4) 2_665 ? O4 Sr2 2.657(2) 2_665 ? O5 C5 1.250(4) . ? O6 C4 1.277(3) . ? O6 Sr1 2.541(2) 2_675 ? O7 C4 1.239(4) 2_775 ? O1W H1WA 0.8090 . ? O1W H1WB 1.0064 . ? N1 C3 1.467(4) . ? N1 C1 1.482(3) . ? N1 C2 1.490(4) . ? C1 P1 1.806(3) 1_655 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.528(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C5 1.532(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O7 1.239(3) 2_775 ? C4 Sr2 3.410(3) 2_775 ? C5 O4 1.266(4) 2_665 ? 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 O3 Sr1 O1W 106.04(9) . . ? O3 Sr1 O6 137.02(7) . 2_675 ? O1W Sr1 O6 86.60(9) . 2_675 ? O3 Sr1 O1 143.74(7) . . ? O1W Sr1 O1 87.72(8) . . ? O6 Sr1 O1 75.77(7) 2_675 . ? O3 Sr1 O7 69.55(7) . . ? O1W Sr1 O7 92.81(8) . . ? O6 Sr1 O7 152.31(7) 2_675 . ? O1 Sr1 O7 76.55(7) . . ? O3 Sr1 O4 66.77(7) . . ? O1W Sr1 O4 73.89(7) . . ? O6 Sr1 O4 78.38(7) 2_675 . ? O1 Sr1 O4 149.01(7) . . ? O7 Sr1 O4 127.98(7) . . ? O3 Sr1 O1 85.59(7) . 2_675 ? O1W Sr1 O1 159.30(7) . 2_675 ? O6 Sr1 O1 96.53(7) 2_675 2_675 ? O1 Sr1 O1 73.35(7) . 2_675 ? O7 Sr1 O1 74.97(7) . 2_675 ? O4 Sr1 O1 126.80(6) . 2_675 ? O3 Sr1 O2 70.95(6) . 1_455 ? O1W Sr1 O2 145.56(7) . 1_455 ? O6 Sr1 O2 75.82(7) 2_675 1_455 ? O1 Sr1 O2 115.40(7) . 1_455 ? O7 Sr1 O2 116.37(6) . 1_455 ? O4 Sr1 O2 73.69(6) . 1_455 ? O1 Sr1 O2 54.13(6) 2_675 1_455 ? O3 Sr1 P1 69.35(6) . . ? O1W Sr1 P1 172.59(6) . . ? O6 Sr1 P1 93.06(6) 2_675 . ? O1 Sr1 P1 99.38(5) . . ? O7 Sr1 P1 90.92(5) . . ? O4 Sr1 P1 98.78(5) . . ? O1 Sr1 P1 28.07(4) 2_675 . ? O2 Sr1 P1 28.16(4) 1_455 . ? O3 Sr1 Sr2 42.10(5) . 2_665 ? O1W Sr1 Sr2 114.08(6) . 2_665 ? O6 Sr1 Sr2 95.06(5) 2_675 2_665 ? O1 Sr1 Sr2 156.11(5) . 2_665 ? O7 Sr1 Sr2 110.28(5) . 2_665 ? O4 Sr1 Sr2 42.83(5) . 2_665 ? O1 Sr1 Sr2 86.11(4) 2_675 2_665 ? O2 Sr1 Sr2 40.76(4) 1_455 2_665 ? P1 Sr1 Sr2 58.557(14) . 2_665 ? O3 Sr1 Sr2 57.89(5) . . ? O1W Sr1 Sr2 131.47(6) . . ? O6 Sr1 Sr2 138.19(5) 2_675 . ? O1 Sr1 Sr2 87.67(5) . . ? O7 Sr1 Sr2 39.41(5) . . ? O4 Sr1 Sr2 123.22(5) . . ? O1 Sr1 Sr2 41.68(4) 2_675 . ? O2 Sr1 Sr2 77.37(4) 1_455 . ? P1 Sr1 Sr2 51.609(13) . . ? Sr2 Sr1 Sr2 84.809(8) 2_665 . ? O3 Sr1 Sr2 166.18(5) . 2_675 ? O1W Sr1 Sr2 86.46(7) . 2_675 ? O6 Sr1 Sr2 35.73(5) 2_675 2_675 ? O1 Sr1 Sr2 40.04(4) . 2_675 ? O7 Sr1 Sr2 116.59(5) . 2_675 ? O4 Sr1 Sr2 112.53(5) . 2_675 ? O1 Sr1 Sr2 84.34(4) 2_675 2_675 ? O2 Sr1 Sr2 95.42(4) 1_455 2_675 ? P1 Sr1 Sr2 97.588(15) . 2_675 ? Sr2 Sr1 Sr2 127.494(10) 2_665 2_675 ? Sr2 Sr1 Sr2 117.988(8) . 2_675 ? O3 Sr1 H1WB 94.2 . . ? O1W Sr1 H1WB 19.0 . . ? O6 Sr1 H1WB 85.2 2_675 . ? O1 Sr1 H1WB 105.6 . . ? O7 Sr1 H1WB 102.8 . . ? O4 Sr1 H1WB 55.1 . . ? O1 Sr1 H1WB 177.7 2_675 . ? O2 Sr1 H1WB 128.0 1_455 . ? P1 Sr1 H1WB 153.6 . . ? Sr2 Sr1 H1WB 95.3 2_665 . ? Sr2 Sr1 H1WB 136.5 . . ? Sr2 Sr1 H1WB 96.2 2_675 . ? O6 Sr2 O2 160.43(8) . 2_765 ? O6 Sr2 O2 93.44(6) . . ? O2 Sr2 O2 77.81(7) 2_765 . ? O6 Sr2 O3 121.94(6) . 2_665 ? O2 Sr2 O3 72.30(6) 2_765 2_665 ? O2 Sr2 O3 141.62(6) . 2_665 ? O6 Sr2 O7 79.45(7) . . ? O2 Sr2 O7 83.81(7) 2_765 . ? O2 Sr2 O7 94.62(7) . . ? O3 Sr2 O7 105.34(7) 2_665 . ? O6 Sr2 O4 119.94(7) . 2_665 ? O2 Sr2 O4 77.32(7) 2_765 2_665 ? O2 Sr2 O4 85.95(7) . 2_665 ? O3 Sr2 O4 64.60(6) 2_665 2_665 ? O7 Sr2 O4 160.57(7) . 2_665 ? O6 Sr2 O1 72.56(6) . 2_675 ? O2 Sr2 O1 112.54(6) 2_765 2_675 ? O2 Sr2 O1 163.38(7) . 2_675 ? O3 Sr2 O1 54.80(6) 2_665 2_675 ? O7 Sr2 O1 74.39(6) . 2_675 ? O4 Sr2 O1 108.61(6) 2_665 2_675 ? O6 Sr2 N1 64.08(7) . . ? O2 Sr2 N1 126.30(7) 2_765 . ? O2 Sr2 N1 68.68(7) . . ? O3 Sr2 N1 111.40(7) 2_665 . ? O7 Sr2 N1 137.87(7) . . ? O4 Sr2 N1 60.06(6) 2_665 . ? O1 Sr2 N1 111.08(6) 2_675 . ? O6 Sr2 P1 97.86(5) . . ? O2 Sr2 P1 92.09(4) 2_765 . ? O2 Sr2 P1 168.45(5) . . ? O3 Sr2 P1 27.07(4) 2_665 . ? O7 Sr2 P1 89.78(5) . . ? O4 Sr2 P1 86.38(5) 2_665 . ? O1 Sr2 P1 27.73(4) 2_675 . ? N1 Sr2 P1 114.42(5) . . ? O6 Sr2 C4 20.72(6) . . ? O2 Sr2 C4 153.09(6) 2_765 . ? O2 Sr2 C4 76.03(6) . . ? O3 Sr2 C4 134.01(7) 2_665 . ? O7 Sr2 C4 92.09(7) . . ? O4 Sr2 C4 106.83(7) 2_665 . ? O1 Sr2 C4 91.68(6) 2_675 . ? N1 Sr2 C4 47.18(7) . . ? P1 Sr2 C4 114.54(5) . . ? O6 Sr2 C4 68.75(7) . 2_775 ? O2 Sr2 C4 92.34(7) 2_765 2_775 ? O2 Sr2 C4 80.23(7) . 2_775 ? O3 Sr2 C4 123.87(7) 2_665 2_775 ? O7 Sr2 C4 18.67(6) . 2_775 ? O4 Sr2 C4 164.26(7) 2_665 2_775 ? O1 Sr2 C4 86.21(6) 2_675 2_775 ? N1 Sr2 C4 120.37(7) . 2_775 ? P1 Sr2 C4 106.06(5) . 2_775 ? C4 Sr2 C4 77.16(8) . 2_775 ? O6 Sr2 P1 147.49(5) . 2_665 ? O2 Sr2 P1 22.50(4) 2_765 2_665 ? O2 Sr2 P1 95.86(5) . 2_665 ? O3 Sr2 P1 63.05(5) 2_665 2_665 ? O7 Sr2 P1 68.81(5) . 2_665 ? O4 Sr2 P1 91.80(5) 2_665 2_665 ? O1 Sr2 P1 91.75(4) 2_675 2_665 ? N1 Sr2 P1 147.76(5) . 2_665 ? P1 Sr2 P1 75.77(2) . 2_665 ? C4 Sr2 P1 158.84(6) . 2_665 ? C4 Sr2 P1 82.24(5) 2_775 2_665 ? O3 P1 O2 114.51(12) 2_665 1_455 ? O3 P1 O1 108.56(12) 2_665 2_675 ? O2 P1 O1 109.34(12) 1_455 2_675 ? O3 P1 C1 104.96(13) 2_665 1_455 ? O2 P1 C1 106.31(12) 1_455 1_455 ? O1 P1 C1 113.21(13) 2_675 1_455 ? O3 P1 Sr1 107.00(9) 2_665 . ? O2 P1 Sr1 58.64(8) 1_455 . ? O1 P1 Sr1 56.68(8) 2_675 . ? C1 P1 Sr1 148.02(10) 1_455 . ? O3 P1 Sr2 52.57(8) 2_665 . ? O2 P1 Sr2 128.91(8) 1_455 . ? O1 P1 Sr2 56.00(8) 2_675 . ? C1 P1 Sr2 124.65(9) 1_455 . ? Sr1 P1 Sr2 77.448(17) . . ? O3 P1 Sr2 74.97(9) 2_665 2_665 ? O2 P1 Sr2 39.55(8) 1_455 2_665 ? O1 P1 Sr2 125.41(9) 2_675 2_665 ? C1 P1 Sr2 118.23(10) 1_455 2_665 ? Sr1 P1 Sr2 69.988(17) . 2_665 ? Sr2 P1 Sr2 104.23(2) . 2_665 ? O3 P1 Sr2 134.07(8) 2_665 1_455 ? O2 P1 Sr2 34.36(8) 1_455 1_455 ? O1 P1 Sr2 114.00(8) 2_675 1_455 ? C1 P1 Sr2 73.54(9) 1_455 1_455 ? Sr1 P1 Sr2 83.462(17) . 1_455 ? Sr2 P1 Sr2 160.83(3) . 1_455 ? Sr2 P1 Sr2 66.914(14) 2_665 1_455 ? P1 O1 Sr1 148.61(13) 2_675 . ? P1 O1 Sr1 95.25(9) 2_675 2_675 ? Sr1 O1 Sr1 106.65(7) . 2_675 ? P1 O1 Sr2 96.27(9) 2_675 2_675 ? Sr1 O1 Sr2 103.00(7) . 2_675 ? Sr1 O1 Sr2 96.80(7) 2_675 2_675 ? P1 O2 Sr2 117.95(11) 1_655 2_765 ? P1 O2 Sr2 125.95(11) 1_655 . ? Sr2 O2 Sr2 102.19(7) 2_765 . ? P1 O2 Sr1 93.20(9) 1_655 1_655 ? Sr2 O2 Sr1 93.99(7) 2_765 1_655 ? Sr2 O2 Sr1 119.78(8) . 1_655 ? P1 O3 Sr1 160.02(12) 2_665 . ? P1 O3 Sr2 100.36(10) 2_665 2_665 ? Sr1 O3 Sr2 98.71(6) . 2_665 ? C5 O4 Sr1 133.74(19) 2_665 . ? C5 O4 Sr2 120.45(19) 2_665 2_665 ? Sr1 O4 Sr2 94.49(7) . 2_665 ? C4 O6 Sr1 131.35(19) . 2_675 ? C4 O6 Sr2 114.35(17) . . ? Sr1 O6 Sr2 108.67(7) 2_675 . ? C4 O7 Sr1 133.15(19) 2_775 . ? C4 O7 Sr2 118.29(19) 2_775 . ? Sr1 O7 Sr2 101.67(7) . . ? Sr1 O1W H1WA 152.6 . . ? Sr1 O1W H1WB 106.7 . . ? H1WA O1W H1WB 100.6 . . ? C3 N1 C1 108.8(2) . . ? C3 N1 C2 112.2(2) . . ? C1 N1 C2 111.8(2) . . ? C3 N1 Sr2 105.05(17) . . ? C1 N1 Sr2 109.76(17) . . ? C2 N1 Sr2 109.03(17) . . ? N1 C1 P1 117.2(2) . 1_655 ? N1 C1 H1A 108.0 . . ? P1 C1 H1A 108.0 1_655 . ? N1 C1 H1B 108.0 . . ? P1 C1 H1B 108.0 1_655 . ? H1A C1 H1B 107.2 . . ? N1 C2 C4 110.8(2) . . ? N1 C2 H2A 109.5 . . ? C4 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N1 C3 C5 111.8(2) . . ? N1 C3 H3A 109.3 . . ? C5 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C5 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? O7 C4 O6 124.3(3) 2_775 . ? O7 C4 C2 120.1(3) 2_775 . ? O6 C4 C2 115.6(3) . . ? O7 C4 Sr2 133.6(2) 2_775 . ? O6 C4 Sr2 44.93(14) . . ? C2 C4 Sr2 89.19(16) . . ? O7 C4 Sr2 43.04(15) 2_775 2_775 ? O6 C4 Sr2 81.31(18) . 2_775 ? C2 C4 Sr2 162.99(19) . 2_775 ? Sr2 C4 Sr2 102.84(8) . 2_775 ? O5 C5 O4 124.9(3) . 2_665 ? O5 C5 C3 116.5(3) . . ? O4 C5 C3 118.6(3) 2_665 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.359 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.147 _database_code_depnum_ccdc_archive 'CCDC 930270' ####################################################################### # # 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_5 #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 N2 O22 P4 Sr4' _chemical_formula_weight 992.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall ' P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.2567(4) _cell_length_b 8.7839(6) _cell_length_c 26.5490(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1225.88(15) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 120 _cell_measurement_theta_min 2.7578 _cell_measurement_theta_max 25.9094 _exptl_crystal_description columnar _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 9.025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1727 _exptl_absorpt_correction_T_max 0.2112 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 6837 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.38 _reflns_number_total 2881 _reflns_number_gt 2698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 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^)+(0.0212P)^2^+0.7427P] 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 0.582(7) _chemical_absolute_configuration ad _refine_ls_number_reflns 2881 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0542 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 N1 N -0.0460(7) -0.0111(3) 0.06315(10) 0.0151(6) Uani 1 1 d . . . H1A H -0.2111 -0.0069 0.0734 0.018 Uiso 1 1 calc R . . Sr1 Sr 0.02609(7) 0.19969(4) 0.242724(12) 0.01485(9) Uani 1 1 d . . . Sr2 Sr 0.44577(8) 0.54917(4) 0.151676(12) 0.01455(8) Uani 1 1 d . . . P1 P 0.5205(2) 0.42046(10) 0.26525(3) 0.0135(2) Uani 1 1 d . . . O1 O 0.2564(5) 0.4665(3) 0.24731(10) 0.0187(6) Uani 1 1 d . . . O2 O 0.5182(7) 0.2604(3) 0.28509(10) 0.0289(7) Uani 1 1 d . . . O3 O 0.7205(5) 0.4399(3) 0.22473(10) 0.0192(6) Uani 1 1 d . . . O4 O 0.6160(6) 0.5375(3) 0.30702(10) 0.0236(7) Uani 1 1 d . . . H4A H 0.4928 0.5773 0.3206 0.035 Uiso 1 1 calc R . . O5 O 0.1807(6) 0.3090(3) 0.14721(11) 0.0250(7) Uani 1 1 d . . . O6 O -0.2195(6) 0.1546(3) 0.14906(11) 0.0292(7) Uani 1 1 d . . . O7 O -0.2055(6) 0.3955(3) 0.09785(10) 0.0225(7) Uani 1 1 d . . . H7A H -0.1072 0.4571 0.0852 0.034 Uiso 1 1 calc R . . O8 O 0.6974(6) 0.7570(4) 0.10221(11) 0.0276(7) Uani 1 1 d . . . O9 O 0.0005(6) 0.1891(3) 0.34303(9) 0.0243(7) Uani 1 1 d . . . O10 O 0.0444(7) 0.4666(4) -0.00956(10) 0.0370(8) Uani 1 1 d . . . O11 O 0.2030(6) 0.5498(3) 0.06269(10) 0.0264(7) Uani 1 1 d . . . P2 P -0.0494(2) 0.25547(10) 0.11927(3) 0.0171(2) Uani 1 1 d . . . C2 C -0.0491(9) -0.0776(4) 0.01118(13) 0.0201(8) Uani 1 1 d . . . H2A H -0.0474 -0.1879 0.0131 0.024 Uiso 1 1 calc R . . H2B H 0.1006 -0.0450 -0.0072 0.024 Uiso 1 1 calc R . . C3 C 0.2122(8) 0.5243(5) 0.01589(14) 0.0192(9) Uani 1 1 d . . . C4 C 0.0482(10) 0.1499(4) 0.06263(13) 0.0196(8) Uani 1 1 d . . . H4B H -0.0174 0.2013 0.0330 0.023 Uiso 1 1 calc R . . H4C H 0.2324 0.1497 0.0604 0.023 Uiso 1 1 calc R . . C6 C 0.0890(9) -0.1088(4) 0.10044(14) 0.0190(9) Uani 1 1 d . . . H6A H 0.1515 -0.0462 0.1279 0.023 Uiso 1 1 calc R . . H6B H 0.2341 -0.1569 0.0844 0.023 Uiso 1 1 calc R . . C7 C 0.9118(9) 0.7691(4) 0.12124(14) 0.0175(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 N1 0.0182(17) 0.0110(13) 0.0162(14) 0.0013(11) 0.0008(15) 0.0004(15) Sr1 0.01665(19) 0.01133(15) 0.01657(15) 0.00017(12) 0.00037(15) -0.00108(15) Sr2 0.01820(18) 0.01211(15) 0.01332(15) -0.00078(13) -0.00087(15) 0.00004(17) P1 0.0157(5) 0.0092(4) 0.0156(4) -0.0004(3) -0.0006(4) 0.0002(4) O1 0.0169(15) 0.0151(14) 0.0241(16) -0.0050(12) -0.0043(11) -0.0003(12) O2 0.047(2) 0.0146(12) 0.0252(13) 0.0046(11) 0.0002(16) -0.0008(16) O3 0.0181(16) 0.0192(14) 0.0204(15) -0.0019(12) -0.0001(11) 0.0022(14) O4 0.0242(18) 0.0237(15) 0.0229(14) -0.0080(12) -0.0024(12) 0.0045(14) O5 0.0325(18) 0.0179(14) 0.0246(15) 0.0008(13) -0.0066(14) 0.0007(15) O6 0.036(2) 0.0218(15) 0.0295(16) 0.0018(14) 0.0137(15) -0.0044(15) O7 0.0246(17) 0.0178(14) 0.0250(15) 0.0011(12) 0.0047(13) 0.0041(13) O8 0.0227(17) 0.0285(17) 0.0317(17) 0.0102(14) -0.0025(14) -0.0043(15) O9 0.0334(19) 0.0225(14) 0.0171(12) -0.0075(11) 0.0044(13) -0.0099(15) O10 0.0271(18) 0.059(2) 0.0250(14) -0.0005(15) 0.0004(15) -0.013(2) O11 0.0384(19) 0.0275(16) 0.0133(14) 0.0001(13) 0.0058(13) -0.0023(17) P2 0.0237(6) 0.0125(4) 0.0151(4) -0.0006(3) 0.0034(5) -0.0007(5) C2 0.027(2) 0.0179(19) 0.0154(17) -0.0044(14) 0.0004(18) 0.003(2) C3 0.022(2) 0.020(2) 0.016(2) 0.0029(16) -0.0008(17) -0.0032(19) C4 0.028(2) 0.0116(17) 0.0193(18) -0.0014(14) 0.006(2) -0.0035(19) C6 0.021(2) 0.0133(17) 0.0228(19) -0.0015(15) -0.0055(17) -0.0004(18) C7 0.022(2) 0.0132(18) 0.0173(18) -0.0003(14) 0.0060(16) 0.0025(17) _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 N1 C6 1.490(5) . ? N1 C4 1.498(5) . ? N1 C2 1.498(4) . ? N1 H1A 0.9100 . ? Sr1 O1 2.544(3) 3_545 ? Sr1 O1 2.641(3) . ? Sr1 O9 2.668(2) . ? Sr1 O3 2.695(3) 1_455 ? Sr1 O4 2.705(3) 3_645 ? Sr1 O3 2.780(3) 3_645 ? Sr1 O6 2.830(3) . ? Sr1 O5 2.831(3) . ? Sr1 O2 2.871(3) . ? Sr1 O2 2.946(3) 1_455 ? Sr1 P1 3.2974(11) . ? Sr1 P2 3.3376(10) . ? Sr2 O2 2.509(2) 3_655 ? Sr2 O5 2.531(3) . ? Sr2 O3 2.602(3) . ? Sr2 O8 2.609(3) . ? Sr2 O9 2.652(3) 3 ? Sr2 O11 2.685(3) . ? Sr2 O7 2.688(3) 1_655 ? Sr2 O1 2.822(3) . ? Sr2 O9 3.163(3) 3_655 ? Sr2 C7 3.223(4) . ? Sr2 P1 3.2440(9) . ? Sr2 Sr1 3.9700(5) 3 ? P1 O2 1.502(3) . ? P1 O3 1.514(3) . ? P1 O1 1.522(3) . ? P1 O4 1.593(3) . ? P1 Sr1 3.3440(11) 1_655 ? P1 Sr1 3.4265(10) 3_655 ? O1 Sr1 2.544(3) 3 ? O2 Sr2 2.509(2) 3_645 ? O2 Sr1 2.946(3) 1_655 ? O3 Sr1 2.695(3) 1_655 ? O3 Sr1 2.780(3) 3_655 ? O4 Sr1 2.705(3) 3_655 ? O4 H4A 0.8200 . ? O5 P2 1.495(3) . ? O6 P2 1.486(3) . ? O7 P2 1.584(3) . ? O7 Sr2 2.688(3) 1_455 ? O7 H7A 0.8200 . ? O8 C7 1.240(5) . ? O9 C7 1.267(4) 3_645 ? O9 Sr2 2.652(3) 3_545 ? O9 Sr2 3.163(3) 3_645 ? O10 C3 1.222(5) . ? O11 C3 1.263(5) . ? P2 C4 1.840(4) . ? C2 C3 1.519(6) 4_455 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C2 1.519(6) 4 ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C6 C7 1.524(6) 1_445 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O9 1.267(4) 3_655 ? C7 C6 1.524(6) 1_665 ? 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 C6 N1 C4 113.1(3) . . ? C6 N1 C2 113.1(3) . . ? C4 N1 C2 111.3(3) . . ? C6 N1 H1A 106.2 . . ? C4 N1 H1A 106.2 . . ? C2 N1 H1A 106.2 . . ? O1 Sr1 O1 167.82(5) 3_545 . ? O1 Sr1 O9 80.72(8) 3_545 . ? O1 Sr1 O9 90.46(8) . . ? O1 Sr1 O3 107.51(9) 3_545 1_455 ? O1 Sr1 O3 65.58(8) . 1_455 ? O9 Sr1 O3 100.03(9) . 1_455 ? O1 Sr1 O4 91.88(9) 3_545 3_645 ? O1 Sr1 O4 99.85(9) . 3_645 ? O9 Sr1 O4 120.27(8) . 3_645 ? O3 Sr1 O4 137.80(8) 1_455 3_645 ? O1 Sr1 O3 65.58(8) 3_545 3_645 ? O1 Sr1 O3 119.63(9) . 3_645 ? O9 Sr1 O3 71.66(8) . 3_645 ? O3 Sr1 O3 169.59(3) 1_455 3_645 ? O4 Sr1 O3 52.11(8) 3_645 3_645 ? O1 Sr1 O6 73.29(9) 3_545 . ? O1 Sr1 O6 111.95(8) . . ? O9 Sr1 O6 148.13(9) . . ? O3 Sr1 O6 71.44(8) 1_455 . ? O4 Sr1 O6 79.32(9) 3_645 . ? O3 Sr1 O6 112.15(8) 3_645 . ? O1 Sr1 O5 122.27(9) 3_545 . ? O1 Sr1 O5 66.96(8) . . ? O9 Sr1 O5 156.99(8) . . ? O3 Sr1 O5 75.33(9) 1_455 . ? O4 Sr1 O5 62.72(8) 3_645 . ? O3 Sr1 O5 114.79(9) 3_645 . ? O6 Sr1 O5 52.49(9) . . ? O1 Sr1 O2 129.41(8) 3_545 . ? O1 Sr1 O2 53.42(8) . . ? O9 Sr1 O2 70.17(9) . . ? O3 Sr1 O2 117.47(8) 1_455 . ? O4 Sr1 O2 70.26(8) 3_645 . ? O3 Sr1 O2 66.35(8) 3_645 . ? O6 Sr1 O2 141.39(9) . . ? O5 Sr1 O2 91.68(8) . . ? O1 Sr1 O2 64.96(8) 3_545 1_455 ? O1 Sr1 O2 103.73(8) . 1_455 ? O9 Sr1 O2 65.13(9) . 1_455 ? O3 Sr1 O2 52.10(8) 1_455 1_455 ? O4 Sr1 O2 155.83(8) 3_645 1_455 ? O3 Sr1 O2 117.65(8) 3_645 1_455 ? O6 Sr1 O2 86.99(8) . 1_455 ? O5 Sr1 O2 122.75(8) . 1_455 ? O2 Sr1 O2 129.31(9) . 1_455 ? O1 Sr1 P1 156.18(6) 3_545 . ? O1 Sr1 P1 26.91(6) . . ? O9 Sr1 P1 83.07(6) . . ? O3 Sr1 P1 92.38(6) 1_455 . ? O4 Sr1 P1 81.38(6) 3_645 . ? O3 Sr1 P1 92.79(6) 3_645 . ? O6 Sr1 P1 126.95(6) . . ? O5 Sr1 P1 74.73(6) . . ? O2 Sr1 P1 27.07(5) . . ? O2 Sr1 P1 122.60(6) 1_455 . ? O1 Sr1 P2 98.68(6) 3_545 . ? O1 Sr1 P2 88.25(6) . . ? O9 Sr1 P2 168.31(7) . . ? O3 Sr1 P2 68.91(6) 1_455 . ? O4 Sr1 P2 71.37(6) 3_645 . ? O3 Sr1 P2 118.86(6) 3_645 . ? O6 Sr1 P2 26.27(6) . . ? O5 Sr1 P2 26.45(7) . . ? O2 Sr1 P2 117.69(6) . . ? O2 Sr1 P2 103.92(6) 1_455 . ? P1 Sr1 P2 100.69(3) . . ? O2 Sr2 O5 133.56(10) 3_655 . ? O2 Sr2 O3 74.46(9) 3_655 . ? O5 Sr2 O3 91.89(9) . . ? O2 Sr2 O8 77.37(10) 3_655 . ? O5 Sr2 O8 147.00(9) . . ? O3 Sr2 O8 110.61(9) . . ? O2 Sr2 O9 71.86(10) 3_655 3 ? O5 Sr2 O9 84.37(9) . 3 ? O3 Sr2 O9 128.50(8) . 3 ? O8 Sr2 O9 98.68(9) . 3 ? O2 Sr2 O11 128.55(9) 3_655 . ? O5 Sr2 O11 72.47(9) . . ? O3 Sr2 O11 156.99(9) . . ? O8 Sr2 O11 78.27(9) . . ? O9 Sr2 O11 68.00(8) 3 . ? O2 Sr2 O7 132.49(11) 3_655 1_655 ? O5 Sr2 O7 86.10(10) . 1_655 ? O3 Sr2 O7 80.36(9) . 1_655 ? O8 Sr2 O7 74.81(10) . 1_655 ? O9 Sr2 O7 149.79(8) 3 1_655 ? O11 Sr2 O7 81.80(9) . 1_655 ? O2 Sr2 O1 67.35(8) 3_655 . ? O5 Sr2 O1 68.50(8) . . ? O3 Sr2 O1 55.26(8) . . ? O8 Sr2 O1 144.27(9) . . ? O9 Sr2 O1 76.09(7) 3 . ? O11 Sr2 O1 128.65(8) . . ? O7 Sr2 O1 126.13(8) 1_655 . ? O2 Sr2 O9 67.26(9) 3_655 3_655 ? O5 Sr2 O9 146.37(9) . 3_655 ? O3 Sr2 O9 66.39(8) . 3_655 ? O8 Sr2 O9 44.26(8) . 3_655 ? O9 Sr2 O9 129.17(10) 3 3_655 ? O11 Sr2 O9 118.40(8) . 3_655 ? O7 Sr2 O9 65.86(8) 1_655 3_655 ? O1 Sr2 O9 112.62(7) . 3_655 ? O2 Sr2 C7 70.55(10) 3_655 . ? O5 Sr2 C7 155.01(9) . . ? O3 Sr2 C7 89.21(9) . . ? O8 Sr2 C7 21.40(9) . . ? O9 Sr2 C7 114.06(9) 3 . ? O11 Sr2 C7 98.02(10) . . ? O7 Sr2 C7 69.48(9) 1_655 . ? O1 Sr2 C7 130.38(9) . . ? O9 Sr2 C7 22.87(8) 3_655 . ? O2 Sr2 P1 68.08(6) 3_655 . ? O5 Sr2 P1 79.61(7) . . ? O3 Sr2 P1 27.29(6) . . ? O8 Sr2 P1 130.57(7) . . ? O9 Sr2 P1 102.67(5) 3 . ? O11 Sr2 P1 151.17(7) . . ? O7 Sr2 P1 103.68(6) 1_655 . ? O1 Sr2 P1 27.97(6) . . ? O9 Sr2 P1 89.01(5) 3_655 . ? C7 Sr2 P1 110.48(7) . . ? O2 Sr2 Sr1 47.82(8) 3_655 3 ? O5 Sr2 Sr1 88.09(7) . 3 ? O3 Sr2 Sr1 86.74(6) . 3 ? O8 Sr2 Sr1 116.06(7) . 3 ? O9 Sr2 Sr1 41.89(5) 3 3 ? O11 Sr2 Sr1 108.89(7) . 3 ? O7 Sr2 Sr1 165.65(6) 1_655 3 ? O1 Sr2 Sr1 39.64(6) . 3 ? O9 Sr2 Sr1 114.47(5) 3_655 3 ? C7 Sr2 Sr1 116.89(7) . 3 ? P1 Sr2 Sr1 62.312(19) . 3 ? O2 P1 O3 111.14(17) . . ? O2 P1 O1 110.56(18) . . ? O3 P1 O1 112.40(16) . . ? O2 P1 O4 111.25(15) . . ? O3 P1 O4 101.72(16) . . ? O1 P1 O4 109.48(16) . . ? O2 P1 Sr2 130.65(11) . . ? O3 P1 Sr2 52.00(11) . . ? O1 P1 Sr2 60.41(11) . . ? O4 P1 Sr2 117.41(11) . . ? O2 P1 Sr1 60.43(13) . . ? O3 P1 Sr1 119.01(11) . . ? O1 P1 Sr1 51.74(11) . . ? O4 P1 Sr1 138.93(12) . . ? Sr2 P1 Sr1 86.62(2) . . ? O2 P1 Sr1 61.72(14) . 1_655 ? O3 P1 Sr1 52.15(11) . 1_655 ? O1 P1 Sr1 145.38(11) . 1_655 ? O4 P1 Sr1 104.37(12) . 1_655 ? Sr2 P1 Sr1 97.59(3) . 1_655 ? Sr1 P1 Sr1 104.65(3) . 1_655 ? O2 P1 Sr1 134.23(14) . 3_655 ? O3 P1 Sr1 52.57(11) . 3_655 ? O1 P1 Sr1 115.14(11) . 3_655 ? O4 P1 Sr1 50.36(11) . 3_655 ? Sr2 P1 Sr1 77.14(2) . 3_655 ? Sr1 P1 Sr1 163.34(3) . 3_655 ? Sr1 P1 Sr1 81.44(2) 1_655 3_655 ? P1 O1 Sr1 135.55(15) . 3 ? P1 O1 Sr1 101.34(13) . . ? Sr1 O1 Sr1 116.85(10) 3 . ? P1 O1 Sr2 91.61(12) . . ? Sr1 O1 Sr2 95.30(9) 3 . ? Sr1 O1 Sr2 110.40(9) . . ? P1 O2 Sr2 157.88(16) . 3_645 ? P1 O2 Sr1 92.50(15) . . ? Sr2 O2 Sr1 101.13(10) 3_645 . ? P1 O2 Sr1 91.61(15) . 1_655 ? Sr2 O2 Sr1 93.06(10) 3_645 1_655 ? Sr1 O2 Sr1 129.31(9) . 1_655 ? P1 O3 Sr2 100.71(14) . . ? P1 O3 Sr1 101.52(14) . 1_655 ? Sr2 O3 Sr1 138.76(11) . 1_655 ? P1 O3 Sr1 101.81(13) . 3_655 ? Sr2 O3 Sr1 101.24(9) . 3_655 ? Sr1 O3 Sr1 107.58(9) 1_655 3_655 ? P1 O4 Sr1 102.66(13) . 3_655 ? P1 O4 H4A 109.5 . . ? Sr1 O4 H4A 122.7 3_655 . ? P2 O5 Sr2 136.97(17) . . ? P2 O5 Sr1 96.05(14) . . ? Sr2 O5 Sr1 113.51(10) . . ? P2 O6 Sr1 96.31(16) . . ? P2 O7 Sr2 123.53(15) . 1_455 ? P2 O7 H7A 109.5 . . ? Sr2 O7 H7A 108.4 1_455 . ? C7 O8 Sr2 108.4(2) . . ? C7 O9 Sr2 122.6(2) 3_645 3_545 ? C7 O9 Sr1 135.2(2) 3_645 . ? Sr2 O9 Sr1 96.53(8) 3_545 . ? C7 O9 Sr2 81.2(2) 3_645 3_645 ? Sr2 O9 Sr2 129.17(10) 3_545 3_645 ? Sr1 O9 Sr2 90.66(8) . 3_645 ? C3 O11 Sr2 147.9(3) . . ? O6 P2 O5 114.22(18) . . ? O6 P2 O7 110.01(19) . . ? O5 P2 O7 110.67(17) . . ? O6 P2 C4 107.60(18) . . ? O5 P2 C4 109.8(2) . . ? O7 P2 C4 104.03(16) . . ? O6 P2 Sr1 57.42(13) . . ? O5 P2 Sr1 57.50(12) . . ? O7 P2 Sr1 121.88(11) . . ? C4 P2 Sr1 134.06(13) . . ? N1 C2 C3 108.9(3) . 4_455 ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 4_455 . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 4_455 . ? H2A C2 H2B 108.3 . . ? O10 C3 O11 126.1(4) . . ? O10 C3 C2 117.5(3) . 4 ? O11 C3 C2 116.3(4) . 4 ? N1 C4 P2 112.1(3) . . ? N1 C4 H4B 109.2 . . ? P2 C4 H4B 109.2 . . ? N1 C4 H4C 109.2 . . ? P2 C4 H4C 109.2 . . ? H4B C4 H4C 107.9 . . ? N1 C6 C7 110.8(3) . 1_445 ? N1 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 1_445 . ? N1 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 1_445 . ? H6A C6 H6B 108.1 . . ? O8 C7 O9 126.0(4) . 3_655 ? O8 C7 C6 118.0(3) . 1_665 ? O9 C7 C6 116.0(4) 3_655 1_665 ? O8 C7 Sr2 50.2(2) . . ? O9 C7 Sr2 75.9(2) 3_655 . ? C6 C7 Sr2 167.8(3) 1_665 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.510 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 930271' ####################################################################### # # 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_6 #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Ba2 N O11 P2' _chemical_formula_weight 595.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.4357(4) _cell_length_b 9.0996(6) _cell_length_c 27.1031(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1340.59(16) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7973 _cell_measurement_theta_min 2.361 _cell_measurement_theta_max 28.296 _exptl_crystal_description columnar _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 6.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1928 _exptl_absorpt_correction_T_max 0.2227 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 9902 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3324 _reflns_number_gt 3286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2009)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0187P)^2^+0.5442P] 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 ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.683(14) _chemical_absolute_configuration ad _refine_ls_number_reflns 3324 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0169 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0396 _refine_ls_wR_factor_gt 0.0394 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 N1 N -0.0473(6) -0.0060(3) 0.06350(9) 0.0175(5) Uani 1 1 d . . . H1A H -0.2065 0.0008 0.0736 0.021 Uiso 1 1 calc R . . Ba1 Ba 0.02433(3) 0.207143(19) 0.241976(6) 0.01418(5) Uani 1 1 d . . . Ba2 Ba 0.45107(4) 0.55014(2) 0.149084(7) 0.01524(5) Uani 1 1 d . . . P1 P 0.52304(15) 0.42727(8) 0.26710(3) 0.01299(15) Uani 1 1 d . . . O1 O 0.2704(4) 0.4700(2) 0.24773(9) 0.0165(5) Uani 1 1 d . . . O2 O 0.5260(5) 0.2703(2) 0.28548(8) 0.0227(5) Uani 1 1 d . . . O3 O 0.7235(4) 0.4517(3) 0.22865(8) 0.0164(5) Uani 1 1 d . . . O4 O 0.6039(5) 0.5381(3) 0.31001(9) 0.0246(5) Uani 1 1 d . . . H4A H 0.4811 0.5748 0.3225 0.037 Uiso 1 1 calc R . . O5 O 0.1662(5) 0.3058(3) 0.14483(9) 0.0248(5) Uani 1 1 d . . . O6 O -0.2337(5) 0.1663(3) 0.14402(10) 0.0307(6) Uani 1 1 d . . . O7 O -0.1887(5) 0.3936(3) 0.09216(9) 0.0246(6) Uani 1 1 d . . . H7A H -0.0866 0.4499 0.0804 0.037 Uiso 1 1 calc R . . O8 O 0.6993(5) 0.7688(3) 0.09849(10) 0.0322(6) Uani 1 1 d . . . O9 O 0.0142(5) 0.1945(3) 0.34772(8) 0.0244(5) Uani 1 1 d . . . O10 O 0.0493(6) 0.4607(4) -0.01286(10) 0.0428(8) Uani 1 1 d . . . O11 O 0.1910(5) 0.5491(3) 0.05826(9) 0.0287(6) Uani 1 1 d . . . P2 P -0.05202(18) 0.25609(9) 0.11593(3) 0.01839(17) Uani 1 1 d . . . C2 C -0.0552(7) -0.0714(4) 0.01263(12) 0.0211(7) Uani 1 1 d . . . H2A H -0.0515 -0.1778 0.0146 0.025 Uiso 1 1 calc R . . H2B H 0.0861 -0.0390 -0.0063 0.025 Uiso 1 1 calc R . . C3 C 0.2076(7) 0.5208(4) 0.01226(13) 0.0234(8) Uani 1 1 d . . . C4 C 0.0503(8) 0.1487(4) 0.06264(12) 0.0239(7) Uani 1 1 d . . . H4B H -0.0042 0.1968 0.0326 0.029 Uiso 1 1 calc R . . H4C H 0.2286 0.1458 0.0622 0.029 Uiso 1 1 calc R . . C6 C 0.0787(7) -0.1025(4) 0.10023(12) 0.0210(7) Uani 1 1 d . . . H6A H 0.1321 -0.0438 0.1281 0.025 Uiso 1 1 calc R . . H6B H 0.2232 -0.1462 0.0852 0.025 Uiso 1 1 calc R . . C7 C 0.9061(6) 0.7760(4) 0.11822(12) 0.0191(7) 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 N1 0.0209(14) 0.0139(12) 0.0176(13) -0.0011(10) 0.0033(12) -0.0006(11) Ba1 0.01311(9) 0.01164(8) 0.01780(9) 0.00094(7) -0.00011(7) -0.00049(7) Ba2 0.01534(9) 0.01560(9) 0.01479(8) -0.00079(7) -0.00002(7) -0.00083(8) P1 0.0109(3) 0.0112(3) 0.0169(3) 0.0003(3) -0.0007(3) 0.0001(3) O1 0.0117(10) 0.0120(11) 0.0257(14) -0.0022(10) -0.0024(9) 0.0009(8) O2 0.0266(13) 0.0136(10) 0.0281(12) 0.0059(9) 0.0017(11) 0.0026(10) O3 0.0125(10) 0.0163(11) 0.0204(12) 0.0007(10) 0.0006(9) -0.0005(9) O4 0.0198(13) 0.0262(13) 0.0279(13) -0.0085(11) -0.0008(10) 0.0015(11) O5 0.0291(13) 0.0228(13) 0.0226(12) 0.0005(11) -0.0028(11) -0.0053(11) O6 0.0365(16) 0.0301(14) 0.0255(13) -0.0020(12) 0.0110(12) -0.0109(11) O7 0.0237(13) 0.0198(12) 0.0302(14) 0.0015(11) 0.0056(11) 0.0046(11) O8 0.0224(13) 0.0375(16) 0.0365(15) 0.0144(13) -0.0051(12) -0.0099(12) O9 0.0305(13) 0.0235(11) 0.0193(10) -0.0055(10) 0.0023(11) -0.0057(11) O10 0.0287(15) 0.072(2) 0.0282(14) -0.0059(14) 0.0003(13) -0.0190(18) O11 0.0331(14) 0.0366(15) 0.0165(12) -0.0020(12) 0.0059(11) -0.0017(13) P2 0.0195(4) 0.0175(4) 0.0181(4) -0.0009(3) 0.0030(4) -0.0020(3) C2 0.0238(17) 0.0228(16) 0.0167(15) -0.0035(13) -0.0025(14) 0.0024(15) C3 0.0220(18) 0.027(2) 0.0210(17) 0.0046(15) 0.0005(14) -0.0014(15) C4 0.0289(19) 0.0189(16) 0.0240(17) -0.0031(13) 0.0093(17) -0.0030(15) C6 0.0208(19) 0.0204(16) 0.0218(16) 0.0008(13) -0.0043(14) -0.0032(14) C7 0.0213(17) 0.0179(16) 0.0181(15) 0.0009(13) 0.0019(12) -0.0001(13) _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 N1 C6 1.493(4) . ? N1 C2 1.502(4) . ? N1 C4 1.504(4) . ? N1 H1A 0.9100 . ? Ba1 O1 2.702(2) 3_545 ? Ba1 O1 2.745(2) . ? Ba1 O3 2.785(2) 1_455 ? Ba1 O3 2.813(2) 3_645 ? Ba1 O9 2.869(2) . ? Ba1 O5 2.887(3) . ? Ba1 O4 2.904(3) 3_645 ? Ba1 O2 3.010(3) 1_455 ? Ba1 O6 3.025(3) . ? Ba1 O2 3.026(3) . ? Ba1 P1 3.4387(8) . ? Ba1 P1 3.4497(8) 1_455 ? Ba2 O2 2.679(2) 3_655 ? Ba2 O5 2.712(3) . ? Ba2 O8 2.768(3) . ? Ba2 O3 2.765(2) . ? Ba2 O11 2.839(3) . ? Ba2 O9 2.851(2) 3 ? Ba2 O7 2.871(3) 1_655 ? Ba2 O1 2.940(2) . ? Ba2 O9 3.191(3) 3_655 ? Ba2 C7 3.323(3) . ? Ba2 P1 3.4110(8) . ? Ba2 Ba1 4.1757(3) 3 ? P1 O2 1.512(2) . ? P1 O1 1.521(2) . ? P1 O3 1.524(2) . ? P1 O4 1.601(2) . ? P1 Ba1 3.4498(8) 1_655 ? P1 Ba1 3.5497(8) 3_655 ? O1 Ba1 2.702(2) 3 ? O2 Ba2 2.679(2) 3_645 ? O2 Ba1 3.009(3) 1_655 ? O3 Ba1 2.785(2) 1_655 ? O3 Ba1 2.814(2) 3_655 ? O4 Ba1 2.904(3) 3_655 ? O4 H4A 0.8200 . ? O5 P2 1.492(3) . ? O6 P2 1.491(3) . ? O7 P2 1.591(3) . ? O7 Ba2 2.871(3) 1_455 ? O7 H7A 0.8200 . ? O8 C7 1.247(4) . ? O9 C7 1.261(4) 3_645 ? O9 Ba2 2.851(2) 3_545 ? O9 Ba2 3.191(3) 3_645 ? O10 C3 1.226(5) . ? O11 C3 1.276(4) . ? P2 C4 1.831(3) . ? C2 C3 1.526(5) 4_455 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C2 1.526(5) 4 ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C6 C7 1.530(5) 1_445 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O9 1.261(4) 3_655 ? C7 C6 1.530(5) 1_665 ? 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 C6 N1 C2 113.1(3) . . ? C6 N1 C4 113.5(3) . . ? C2 N1 C4 111.5(2) . . ? C6 N1 H1A 106.0 . . ? C2 N1 H1A 106.0 . . ? C4 N1 H1A 106.0 . . ? O1 Ba1 O1 168.23(3) 3_545 . ? O1 Ba1 O3 107.66(7) 3_545 1_455 ? O1 Ba1 O3 66.25(7) . 1_455 ? O1 Ba1 O3 66.41(7) 3_545 3_645 ? O1 Ba1 O3 117.80(7) . 3_645 ? O3 Ba1 O3 169.387(17) 1_455 3_645 ? O1 Ba1 O9 81.57(7) 3_545 . ? O1 Ba1 O9 89.29(7) . . ? O3 Ba1 O9 98.65(7) 1_455 . ? O3 Ba1 O9 72.15(7) 3_645 . ? O1 Ba1 O5 120.06(7) 3_545 . ? O1 Ba1 O5 69.55(7) . . ? O3 Ba1 O5 77.88(7) 1_455 . ? O3 Ba1 O5 112.63(7) 3_645 . ? O9 Ba1 O5 158.25(7) . . ? O1 Ba1 O4 92.27(7) 3_545 3_645 ? O1 Ba1 O4 98.63(7) . 3_645 ? O3 Ba1 O4 140.25(6) 1_455 3_645 ? O3 Ba1 O4 50.26(6) 3_645 3_645 ? O9 Ba1 O4 118.46(7) . 3_645 ? O5 Ba1 O4 62.38(7) . 3_645 ? O1 Ba1 O2 65.07(6) 3_545 1_455 ? O1 Ba1 O2 104.47(6) . 1_455 ? O3 Ba1 O2 50.93(6) 1_455 1_455 ? O3 Ba1 O2 119.04(6) 3_645 1_455 ? O9 Ba1 O2 66.36(7) . 1_455 ? O5 Ba1 O2 122.58(7) . 1_455 ? O4 Ba1 O2 156.56(7) 3_645 1_455 ? O1 Ba1 O6 73.60(7) 3_545 . ? O1 Ba1 O6 112.51(7) . . ? O3 Ba1 O6 73.27(7) 1_455 . ? O3 Ba1 O6 111.88(7) 3_645 . ? O9 Ba1 O6 149.64(7) . . ? O5 Ba1 O6 50.33(7) . . ? O4 Ba1 O6 80.32(7) 3_645 . ? O2 Ba1 O6 87.14(7) 1_455 . ? O1 Ba1 O2 130.23(6) 3_545 . ? O1 Ba1 O2 51.18(6) . . ? O3 Ba1 O2 115.33(6) 1_455 . ? O3 Ba1 O2 66.90(6) 3_645 . ? O9 Ba1 O2 68.63(7) . . ? O5 Ba1 O2 93.18(7) . . ? O4 Ba1 O2 70.28(7) 3_645 . ? O2 Ba1 O2 128.47(8) 1_455 . ? O6 Ba1 O2 141.53(7) . . ? O1 Ba1 P1 155.81(5) 3_545 . ? O1 Ba1 P1 25.44(5) . . ? O3 Ba1 P1 91.32(5) 1_455 . ? O3 Ba1 P1 92.36(5) 3_645 . ? O9 Ba1 P1 80.83(5) . . ? O5 Ba1 P1 77.81(5) . . ? O4 Ba1 P1 81.73(5) 3_645 . ? O2 Ba1 P1 121.37(5) 1_455 . ? O6 Ba1 P1 127.64(5) . . ? O2 Ba1 P1 26.07(4) . . ? O1 Ba1 P1 88.57(5) 3_545 1_455 ? O1 Ba1 P1 82.40(5) . 1_455 ? O3 Ba1 P1 25.57(5) 1_455 1_455 ? O3 Ba1 P1 143.96(5) 3_645 1_455 ? O9 Ba1 P1 79.11(5) . 1_455 ? O5 Ba1 P1 102.16(6) . 1_455 ? O4 Ba1 P1 162.35(5) 3_645 1_455 ? O2 Ba1 P1 25.95(4) 1_455 1_455 ? O6 Ba1 P1 83.02(6) . 1_455 ? O2 Ba1 P1 121.64(5) . 1_455 ? P1 Ba1 P1 104.20(2) . 1_455 ? O2 Ba2 O5 131.91(8) 3_655 . ? O2 Ba2 O8 76.56(8) 3_655 . ? O5 Ba2 O8 147.86(8) . . ? O2 Ba2 O3 72.61(7) 3_655 . ? O5 Ba2 O3 94.20(7) . . ? O8 Ba2 O3 110.99(7) . . ? O2 Ba2 O11 126.85(8) 3_655 . ? O5 Ba2 O11 71.10(8) . . ? O8 Ba2 O11 79.37(8) . . ? O3 Ba2 O11 160.38(8) . . ? O2 Ba2 O9 71.13(8) 3_655 3 ? O5 Ba2 O9 82.67(8) . 3 ? O8 Ba2 O9 96.68(8) . 3 ? O3 Ba2 O9 126.91(6) . 3 ? O11 Ba2 O9 65.55(7) . 3 ? O2 Ba2 O7 134.05(8) 3_655 1_655 ? O5 Ba2 O7 87.69(8) . 1_655 ? O8 Ba2 O7 76.01(8) . 1_655 ? O3 Ba2 O7 83.86(7) . 1_655 ? O11 Ba2 O7 82.65(8) . 1_655 ? O9 Ba2 O7 148.20(7) 3 1_655 ? O2 Ba2 O1 66.36(7) 3_655 . ? O5 Ba2 O1 69.18(7) . . ? O8 Ba2 O1 142.34(8) . . ? O3 Ba2 O1 52.36(6) . . ? O11 Ba2 O1 128.42(7) . . ? O9 Ba2 O1 77.90(6) 3 . ? O7 Ba2 O1 126.39(7) 1_655 . ? O2 Ba2 O9 68.40(7) 3_655 3_655 ? O5 Ba2 O9 149.17(7) . 3_655 ? O8 Ba2 O9 43.41(7) . 3_655 ? O3 Ba2 O9 67.93(6) . 3_655 ? O11 Ba2 O9 118.60(7) . 3_655 ? O9 Ba2 O9 128.15(8) 3 3_655 ? O7 Ba2 O9 66.27(7) 1_655 3_655 ? O1 Ba2 O9 112.43(6) . 3_655 ? O2 Ba2 C7 70.70(8) 3_655 . ? O5 Ba2 C7 157.12(8) . . ? O8 Ba2 C7 21.21(8) . . ? O3 Ba2 C7 89.89(7) . . ? O11 Ba2 C7 98.89(8) . . ? O9 Ba2 C7 112.53(8) 3 . ? O7 Ba2 C7 70.36(8) 1_655 . ? O1 Ba2 C7 129.12(7) . . ? O9 Ba2 C7 22.21(7) 3_655 . ? O2 Ba2 P1 67.60(5) 3_655 . ? O5 Ba2 P1 80.60(6) . . ? O8 Ba2 P1 130.12(6) . . ? O3 Ba2 P1 25.98(5) . . ? O11 Ba2 P1 150.37(6) . . ? O9 Ba2 P1 102.96(5) 3 . ? O7 Ba2 P1 105.25(5) 1_655 . ? O1 Ba2 P1 26.39(4) . . ? O9 Ba2 P1 90.28(4) 3_655 . ? C7 Ba2 P1 110.70(6) . . ? O2 Ba2 Ba1 45.95(5) 3_655 3 ? O5 Ba2 Ba1 87.55(6) . 3 ? O8 Ba2 Ba1 113.95(7) . 3 ? O3 Ba2 Ba1 83.73(5) . 3 ? O11 Ba2 Ba1 107.83(5) . 3 ? O9 Ba2 Ba1 43.28(5) 3 3 ? O7 Ba2 Ba1 166.34(5) 1_655 3 ? O1 Ba2 Ba1 40.11(4) . 3 ? O9 Ba2 Ba1 113.81(4) 3_655 3 ? C7 Ba2 Ba1 115.29(6) . 3 ? P1 Ba2 Ba1 61.317(14) . 3 ? O2 P1 O1 111.39(14) . . ? O2 P1 O3 110.80(14) . . ? O1 P1 O3 111.85(13) . . ? O2 P1 O4 110.65(14) . . ? O1 P1 O4 109.75(13) . . ? O3 P1 O4 102.04(14) . . ? O2 P1 Ba2 128.28(10) . . ? O1 P1 Ba2 59.26(9) . . ? O3 P1 Ba2 52.62(9) . . ? O4 P1 Ba2 120.42(10) . . ? O2 P1 Ba1 61.56(10) . . ? O1 P1 Ba1 50.85(9) . . ? O3 P1 Ba1 120.87(9) . . ? O4 P1 Ba1 136.66(10) . . ? Ba2 P1 Ba1 85.113(18) . . ? O2 P1 Ba1 60.55(10) . 1_655 ? O1 P1 Ba1 142.51(10) . 1_655 ? O3 P1 Ba1 52.05(9) . 1_655 ? O4 P1 Ba1 106.99(10) . 1_655 ? Ba2 P1 Ba1 95.50(2) . 1_655 ? Ba1 P1 Ba1 104.20(2) . 1_655 ? O2 P1 Ba1 133.85(11) . 3_655 ? O1 P1 Ba1 114.75(9) . 3_655 ? O3 P1 Ba1 49.64(9) . 3_655 ? O4 P1 Ba1 53.70(10) . 3_655 ? Ba2 P1 Ba1 77.251(16) . 3_655 ? Ba1 P1 Ba1 161.92(2) . 3_655 ? Ba1 P1 Ba1 81.687(18) 1_655 3_655 ? P1 O1 Ba1 134.74(13) . 3 ? P1 O1 Ba1 103.71(11) . . ? Ba1 O1 Ba1 114.38(7) 3 . ? P1 O1 Ba2 94.35(10) . . ? Ba1 O1 Ba2 95.38(7) 3 . ? Ba1 O1 Ba2 109.10(7) . . ? P1 O2 Ba2 157.63(14) . 3_645 ? P1 O2 Ba1 93.50(11) . 1_655 ? Ba2 O2 Ba1 94.28(7) 3_645 1_655 ? P1 O2 Ba1 92.37(11) . . ? Ba2 O2 Ba1 99.07(7) 3_645 . ? Ba1 O2 Ba1 128.47(8) 1_655 . ? P1 O3 Ba2 101.40(11) . . ? P1 O3 Ba1 102.39(12) . 1_655 ? Ba2 O3 Ba1 132.41(9) . 1_655 ? P1 O3 Ba1 105.98(12) . 3_655 ? Ba2 O3 Ba1 102.36(8) . 3_655 ? Ba1 O3 Ba1 109.72(7) 1_655 3_655 ? P1 O4 Ba1 99.93(11) . 3_655 ? P1 O4 H4A 109.5 . . ? Ba1 O4 H4A 123.5 3_655 . ? P2 O5 Ba2 136.47(15) . . ? P2 O5 Ba1 99.91(12) . . ? Ba2 O5 Ba1 111.64(9) . . ? P2 O6 Ba1 94.23(13) . . ? P2 O7 Ba2 119.40(13) . 1_455 ? P2 O7 H7A 109.5 . . ? Ba2 O7 H7A 111.1 1_455 . ? C7 O8 Ba2 105.3(2) . . ? C7 O9 Ba2 123.6(2) 3_645 3_545 ? C7 O9 Ba1 134.5(2) 3_645 . ? Ba2 O9 Ba1 93.78(7) 3_545 . ? C7 O9 Ba2 84.8(2) 3_645 3_645 ? Ba2 O9 Ba2 128.15(8) 3_545 3_645 ? Ba1 O9 Ba2 91.51(7) . 3_645 ? C3 O11 Ba2 144.4(2) . . ? O6 P2 O5 115.15(16) . . ? O6 P2 O7 109.17(17) . . ? O5 P2 O7 110.22(15) . . ? O6 P2 C4 108.14(16) . . ? O5 P2 C4 109.55(18) . . ? O7 P2 C4 104.01(15) . . ? O6 P2 Ba1 60.40(11) . . ? O5 P2 Ba1 55.04(10) . . ? O7 P2 Ba1 123.74(10) . . ? C4 P2 Ba1 132.21(12) . . ? N1 C2 C3 108.1(3) . 4_455 ? N1 C2 H2A 110.1 . . ? C3 C2 H2A 110.1 4_455 . ? N1 C2 H2B 110.1 . . ? C3 C2 H2B 110.1 4_455 . ? H2A C2 H2B 108.4 . . ? O10 C3 O11 125.6(4) . . ? O10 C3 C2 118.8(3) . 4 ? O11 C3 C2 115.5(3) . 4 ? N1 C4 P2 112.4(2) . . ? N1 C4 H4B 109.1 . . ? P2 C4 H4B 109.1 . . ? N1 C4 H4C 109.1 . . ? P2 C4 H4C 109.1 . . ? H4B C4 H4C 107.9 . . ? N1 C6 C7 110.9(3) . 1_445 ? N1 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 1_445 . ? N1 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 1_445 . ? H6A C6 H6B 108.1 . . ? O8 C7 O9 126.4(3) . 3_655 ? O8 C7 C6 117.0(3) . 1_665 ? O9 C7 C6 116.6(3) 3_655 1_665 ? O8 C7 Ba2 53.45(18) . . ? O9 C7 Ba2 72.99(19) 3_655 . ? C6 C7 Ba2 169.6(2) 1_665 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.624 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 930272' ####################################################################### # # 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_7 #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H9 Ba N O7.50 P' _chemical_formula_weight 371.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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' _symmetry_space_group_name_Hall '-C 2yc' 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 21.4194(14) _cell_length_b 5.1337(3) _cell_length_c 18.4721(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.377(2) _cell_angle_gamma 90.00 _cell_volume 1991.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7599 _cell_measurement_theta_min 2.4267 _cell_measurement_theta_max 28.4668 _exptl_crystal_description lamellar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 4.173 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3879 _exptl_absorpt_correction_T_max 0.6804 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8986 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.67 _reflns_number_total 2455 _reflns_number_gt 2325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2009)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0196P)^2^+2.6608P] 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 2455 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0466 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.002 _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 Ba1 Ba 0.950308(6) 0.85993(2) 0.388375(7) 0.01547(6) Uani 1 1 d . . . P1 P 0.91345(3) 0.59314(12) 0.55030(3) 0.01564(12) Uani 1 1 d . . . O1 O 0.95609(8) 0.8208(3) 0.54508(10) 0.0224(4) Uani 1 1 d . . . O2 O 1.06468(9) 0.6087(3) 0.39173(11) 0.0258(4) Uani 1 1 d . . . O3 O 0.89924(9) 0.4791(3) 0.46986(9) 0.0246(4) Uani 1 1 d . . . H1 H 0.8714 0.3516 0.4551 0.029 Uiso 1 1 d R . . O4 O 0.83903(8) 1.0747(4) 0.42009(11) 0.0274(4) Uani 1 1 d . . . O5 O 0.75282(9) 0.2100(4) 0.58895(13) 0.0348(5) Uani 1 1 d . . . O6 O 0.92400(10) 1.3291(3) 0.32012(10) 0.0298(4) Uani 1 1 d . . . O7 O 0.86008(10) 0.6413(3) 0.26412(11) 0.0325(5) Uani 1 1 d . . . O8 O 1.0000 0.7975(6) 0.2500 0.0335(6) Uani 1 2 d S . . H2 H 0.9669 0.6782 0.2198 0.050 Uiso 1 1 d R . . N1 N 0.82383(9) 0.6196(4) 0.63897(10) 0.0147(4) Uani 1 1 d . . . H3 H 0.8357 0.4420 0.6466 0.018 Uiso 1 1 d R . . C1 C 0.83513(11) 0.7027(5) 0.56456(12) 0.0177(4) Uani 1 1 d . . . H1A H 0.8327 0.8910 0.5608 0.021 Uiso 1 1 calc R . . H1B H 0.8021 0.6301 0.5263 0.021 Uiso 1 1 calc R . . C2 C 0.75471(11) 0.6295(4) 0.64258(14) 0.0190(5) Uani 1 1 d . . . H2A H 0.7362 0.7913 0.6212 0.023 Uiso 1 1 calc R . . H2B H 0.7498 0.6227 0.6936 0.023 Uiso 1 1 calc R . . C3 C 0.72063(12) 0.3995(5) 0.60024(14) 0.0193(5) Uani 1 1 d . . . C4 C 0.86479(11) 0.7630(5) 0.70126(12) 0.0188(5) Uani 1 1 d . . . H4A H 0.8417 0.9118 0.7149 0.023 Uiso 1 1 calc R . . H4B H 0.9027 0.8265 0.6857 0.023 Uiso 1 1 calc R . . C5 C 0.88377(12) 0.5825(5) 0.76779(13) 0.0199(5) 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 Ba1 0.01402(8) 0.01660(9) 0.01522(8) -0.00023(5) 0.00148(6) -0.00002(5) P1 0.0139(3) 0.0155(3) 0.0177(3) -0.0008(2) 0.0035(2) -0.0001(2) O1 0.0174(9) 0.0243(9) 0.0246(9) -0.0025(7) 0.0019(7) -0.0066(7) O2 0.0233(10) 0.0261(9) 0.0292(10) 0.0072(8) 0.0079(8) 0.0088(7) O3 0.0292(10) 0.0238(9) 0.0231(9) -0.0093(7) 0.0108(8) -0.0107(7) O4 0.0155(9) 0.0251(9) 0.0409(11) -0.0088(8) 0.0036(8) -0.0029(7) O5 0.0234(10) 0.0210(10) 0.0588(14) -0.0088(9) 0.0053(9) 0.0026(8) O6 0.0393(12) 0.0261(10) 0.0187(9) 0.0036(7) -0.0068(8) 0.0027(8) O7 0.0438(13) 0.0211(10) 0.0270(10) -0.0061(7) -0.0069(9) 0.0056(8) O8 0.0337(16) 0.0419(17) 0.0262(14) 0.000 0.0093(12) 0.000 N1 0.0145(10) 0.0142(9) 0.0147(9) -0.0002(7) 0.0013(8) 0.0002(7) C1 0.0162(11) 0.0228(11) 0.0139(10) 0.0040(9) 0.0023(9) 0.0042(9) C2 0.0148(12) 0.0206(12) 0.0222(12) -0.0026(9) 0.0050(10) -0.0008(8) C3 0.0195(12) 0.0161(11) 0.0229(12) -0.0002(9) 0.0059(10) -0.0020(9) C4 0.0223(12) 0.0182(11) 0.0144(10) -0.0009(9) -0.0005(9) -0.0033(9) C5 0.0228(12) 0.0202(11) 0.0159(11) 0.0002(9) 0.0016(9) 0.0037(10) _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 Ba1 O1 2.6914(17) 5_776 ? Ba1 O6 2.7255(18) . ? Ba1 O2 2.7585(18) . ? Ba1 O4 2.7911(18) . ? Ba1 O3 2.8167(17) . ? Ba1 O1 2.8799(18) . ? Ba1 O7 2.918(2) . ? Ba1 O8 2.9736(4) . ? Ba1 O6 3.0088(18) 1_545 ? Ba1 C5 3.301(2) 6_565 ? Ba1 P1 3.5181(6) . ? Ba1 P1 3.7290(6) 5_766 ? P1 O2 1.4973(18) 5_766 ? P1 O1 1.4983(17) . ? P1 O3 1.5700(17) . ? P1 C1 1.837(2) . ? P1 Ba1 3.7289(6) 5_766 ? O1 Ba1 2.6914(17) 5_776 ? O2 P1 1.4973(18) 5_766 ? O4 C3 1.266(3) 7_666 ? O5 C3 1.233(3) . ? O6 C5 1.247(3) 6_575 ? O6 Ba1 3.0088(18) 1_565 ? O7 C5 1.252(3) 6_565 ? O8 Ba1 2.9736(4) 2_755 ? N1 C4 1.496(3) . ? N1 C2 1.496(3) . ? N1 C1 1.504(3) . ? C2 C3 1.521(3) . ? C3 O4 1.266(3) 7_666 ? C4 C5 1.529(3) . ? C5 O6 1.247(3) 6_576 ? C5 O7 1.252(3) 6_566 ? C5 Ba1 3.301(2) 6_566 ? 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 Ba1 O6 74.96(6) 5_776 . ? O1 Ba1 O2 72.31(6) 5_776 . ? O6 Ba1 O2 121.68(6) . . ? O1 Ba1 O4 104.69(5) 5_776 . ? O6 Ba1 O4 68.95(6) . . ? O2 Ba1 O4 166.25(6) . . ? O1 Ba1 O3 120.76(5) 5_776 . ? O6 Ba1 O3 142.56(6) . . ? O2 Ba1 O3 95.75(5) . . ? O4 Ba1 O3 74.00(5) . . ? O1 Ba1 O1 72.72(6) 5_776 . ? O6 Ba1 O1 119.38(5) . . ? O2 Ba1 O1 94.76(5) . . ? O4 Ba1 O1 71.68(5) . . ? O3 Ba1 O1 50.12(5) . . ? O1 Ba1 O7 155.73(6) 5_776 . ? O6 Ba1 O7 86.08(5) . . ? O2 Ba1 O7 106.58(6) . . ? O4 Ba1 O7 81.75(6) . . ? O3 Ba1 O7 83.49(5) . . ? O1 Ba1 O7 130.88(5) . . ? O1 Ba1 O8 95.60(5) 5_776 . ? O6 Ba1 O8 76.94(7) . . ? O2 Ba1 O8 60.13(5) . . ? O4 Ba1 O8 133.49(5) . . ? O3 Ba1 O8 128.84(7) . . ? O1 Ba1 O8 154.79(4) . . ? O7 Ba1 O8 64.92(5) . . ? O1 Ba1 O6 143.51(6) 5_776 1_545 ? O6 Ba1 O6 127.01(7) . 1_545 ? O2 Ba1 O6 71.22(6) . 1_545 ? O4 Ba1 O6 110.40(6) . 1_545 ? O3 Ba1 O6 62.28(5) . 1_545 ? O1 Ba1 O6 108.99(5) . 1_545 ? O7 Ba1 O6 44.09(5) . 1_545 ? O8 Ba1 O6 67.13(7) . 1_545 ? O1 Ba1 C5 155.59(6) 5_776 6_565 ? O6 Ba1 C5 105.87(6) . 6_565 ? O2 Ba1 C5 87.53(6) . 6_565 ? O4 Ba1 C5 98.07(6) . 6_565 ? O3 Ba1 C5 73.83(5) . 6_565 ? O1 Ba1 C5 123.89(5) . 6_565 ? O7 Ba1 C5 22.14(5) . 6_565 ? O8 Ba1 C5 61.70(6) . 6_565 ? O6 Ba1 C5 22.17(5) 1_545 6_565 ? O1 Ba1 P1 96.93(4) 5_776 . ? O6 Ba1 P1 132.59(4) . . ? O2 Ba1 P1 98.40(4) . . ? O4 Ba1 P1 68.36(4) . . ? O3 Ba1 P1 25.78(3) . . ? O1 Ba1 P1 24.59(3) . . ? O7 Ba1 P1 107.11(4) . . ? O8 Ba1 P1 150.14(6) . . ? O6 Ba1 P1 87.07(4) 1_545 . ? C5 Ba1 P1 99.58(4) 6_565 . ? O1 Ba1 P1 76.89(4) 5_776 5_766 ? O6 Ba1 P1 140.33(5) . 5_766 ? O2 Ba1 P1 20.48(4) . 5_766 ? O4 Ba1 P1 146.32(4) . 5_766 ? O3 Ba1 P1 76.58(4) . 5_766 ? O1 Ba1 P1 77.01(4) . 5_766 ? O7 Ba1 P1 110.88(4) . 5_766 ? O8 Ba1 P1 78.61(4) . 5_766 ? O6 Ba1 P1 68.47(4) 1_545 5_766 ? C5 Ba1 P1 89.07(5) 6_565 5_766 ? P1 Ba1 P1 78.014(15) . 5_766 ? O2 P1 O1 118.50(11) 5_766 . ? O2 P1 O3 113.19(11) 5_766 . ? O1 P1 O3 103.71(10) . . ? O2 P1 C1 105.96(10) 5_766 . ? O1 P1 C1 110.85(11) . . ? O3 P1 C1 103.76(10) . . ? O2 P1 Ba1 141.85(7) 5_766 . ? O1 P1 Ba1 53.11(7) . . ? O3 P1 Ba1 51.29(6) . . ? C1 P1 Ba1 111.55(7) . . ? O2 P1 Ba1 40.13(7) 5_766 5_766 ? O1 P1 Ba1 93.19(7) . 5_766 ? O3 P1 Ba1 92.80(7) . 5_766 ? C1 P1 Ba1 146.04(8) . 5_766 ? Ba1 P1 Ba1 101.987(15) . 5_766 ? P1 O1 Ba1 148.69(10) . 5_776 ? P1 O1 Ba1 102.30(8) . . ? Ba1 O1 Ba1 107.28(6) 5_776 . ? P1 O2 Ba1 119.40(10) 5_766 . ? P1 O3 Ba1 102.93(8) . . ? C3 O4 Ba1 146.42(16) 7_666 . ? C5 O6 Ba1 136.77(16) 6_575 . ? C5 O6 Ba1 92.22(14) 6_575 1_565 ? Ba1 O6 Ba1 127.02(7) . 1_565 ? C5 O7 Ba1 96.43(15) 6_565 . ? Ba1 O8 Ba1 167.62(12) 2_755 . ? C4 N1 C2 112.61(18) . . ? C4 N1 C1 112.83(18) . . ? C2 N1 C1 111.74(18) . . ? N1 C1 P1 111.14(15) . . ? N1 C2 C3 109.23(18) . . ? O5 C3 O4 126.7(2) . 7_666 ? O5 C3 C2 118.1(2) . . ? O4 C3 C2 115.2(2) 7_666 . ? N1 C4 C5 110.05(19) . . ? O6 C5 O7 125.9(2) 6_576 6_566 ? O6 C5 C4 115.9(2) 6_576 . ? O7 C5 C4 118.2(2) 6_566 . ? O6 C5 Ba1 65.60(13) 6_576 6_566 ? O7 C5 Ba1 61.43(13) 6_566 6_566 ? C4 C5 Ba1 166.01(16) . 6_566 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.67 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.441 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.107 _database_code_depnum_ccdc_archive 'CCDC 930273' ####################################################################### # # 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_5_Eu #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H8.95 Eu0.05 N O11 P2 Sr1.95' _chemical_formula_sum 'C5 H8.95 Eu0.05 N O11 P2 Sr1.95' _chemical_formula_weight 499.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.2590(2) _cell_length_b 8.7686(3) _cell_length_c 26.5295(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1223.38(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 9267 _cell_measurement_theta_min 2.7846 _cell_measurement_theta_max 28.2872 _exptl_crystal_description columnar _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 967 _exptl_absorpt_coefficient_mu 9.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2636 _exptl_absorpt_correction_T_max 0.4083 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 14071 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2995 _reflns_number_gt 2794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 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^)+(0.0072P)^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 0.011(6) _chemical_absolute_configuration ad _refine_ls_number_reflns 2995 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0433 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _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 N1 N -0.0462(6) -0.0116(2) 0.06317(8) 0.0164(6) Uani 1 1 d . . . H1A H -0.2116 -0.0083 0.0732 0.020 Uiso 0.95 1 calc PR . . Sr1 Sr 0.02665(6) 0.19852(3) 0.242634(9) 0.01450(9) Uani 0.981(2) 1 d P . . Eu1 Eu 0.02665(6) 0.19852(3) 0.242634(9) 0.01450(9) Uani 0.019(2) 1 d P . . Sr2 Sr 0.44604(6) 0.54800(3) 0.151651(9) 0.01423(9) Uani 0.966(2) 1 d P . . Eu2 Eu 0.44604(6) 0.54800(3) 0.151651(9) 0.01423(9) Uani 0.034(2) 1 d P . . P1 P 0.51963(16) 0.41969(8) 0.26532(3) 0.01309(18) Uani 1 1 d . . . O1 O 0.2567(4) 0.4653(2) 0.24713(8) 0.0181(5) Uani 1 1 d . . . O2 O 0.5179(5) 0.2591(2) 0.28530(8) 0.0281(6) Uani 1 1 d . . . O3 O 0.7193(4) 0.4392(3) 0.22447(8) 0.0188(5) Uani 1 1 d . . . O4 O 0.6154(5) 0.5365(2) 0.30718(7) 0.0226(6) Uani 1 1 d . . . H4A H 0.4924 0.5764 0.3209 0.034 Uiso 1 1 calc R . . O5 O 0.1797(5) 0.3086(3) 0.14740(8) 0.0250(5) Uani 1 1 d . . . O6 O -0.2180(5) 0.1529(3) 0.14937(9) 0.0309(6) Uani 1 1 d . . . O7 O -0.2082(5) 0.3949(3) 0.09818(8) 0.0252(6) Uani 1 1 d . . . H7A H -0.1108 0.4569 0.0855 0.038 Uiso 1 1 calc R . . O8 O 0.6973(5) 0.7564(3) 0.10260(9) 0.0278(6) Uani 1 1 d . . . O9 O -0.0009(5) 0.1883(2) 0.34291(7) 0.0255(6) Uani 1 1 d . . . O10 O 0.0451(6) 0.4668(3) -0.00934(8) 0.0397(7) Uani 1 1 d . . . O11 O 0.2064(5) 0.5488(3) 0.06302(8) 0.0266(6) Uani 1 1 d . . . P2 P -0.0505(2) 0.25505(8) 0.11949(3) 0.0183(2) Uani 1 1 d . . . C2 C -0.0464(7) -0.0777(3) 0.01114(10) 0.0191(7) Uani 1 1 d . . . H2A H -0.0439 -0.1881 0.0129 0.023 Uiso 1 1 calc R . . H2B H 0.1038 -0.0443 -0.0070 0.023 Uiso 1 1 calc R . . C3 C 0.2156(7) 0.5244(4) 0.01617(12) 0.0215(8) Uani 1 1 d . . . C4 C 0.0469(8) 0.1501(3) 0.06305(11) 0.0220(7) Uani 1 1 d . . . H4B H -0.0188 0.2018 0.0335 0.026 Uiso 1 1 calc R . . H4C H 0.2310 0.1503 0.0609 0.026 Uiso 1 1 calc R . . C6 C 0.0902(7) -0.1098(3) 0.10060(11) 0.0189(7) Uani 1 1 d . . . H6A H 0.1532 -0.0472 0.1280 0.023 Uiso 1 1 calc R . . H6B H 0.2347 -0.1583 0.0845 0.023 Uiso 1 1 calc R . . C7 C 0.9115(7) 0.7683(3) 0.12144(10) 0.0173(7) 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 N1 0.0172(16) 0.0146(11) 0.0174(11) 0.0003(9) 0.0026(12) 0.0004(11) Sr1 0.01388(18) 0.01305(13) 0.01656(13) 0.00015(10) 0.00024(12) -0.00123(11) Eu1 0.01388(18) 0.01305(13) 0.01656(13) 0.00015(10) 0.00024(12) -0.00123(11) Sr2 0.01549(17) 0.01391(13) 0.01328(13) -0.00069(10) -0.00023(12) -0.00017(12) Eu2 0.01549(17) 0.01391(13) 0.01328(13) -0.00069(10) -0.00023(12) -0.00017(12) P1 0.0131(5) 0.0110(3) 0.0151(3) -0.0002(3) -0.0007(3) 0.0007(3) O1 0.0112(13) 0.0158(11) 0.0275(13) -0.0041(10) -0.0042(9) -0.0009(9) O2 0.0440(19) 0.0143(10) 0.0262(11) 0.0058(8) -0.0014(12) 0.0021(11) O3 0.0129(14) 0.0224(12) 0.0210(11) 0.0004(10) 0.0020(9) 0.0016(10) O4 0.0207(16) 0.0246(12) 0.0226(11) -0.0074(10) -0.0026(10) 0.0031(11) O5 0.0289(15) 0.0219(12) 0.0243(12) -0.0010(10) -0.0075(11) -0.0011(11) O6 0.0364(18) 0.0275(13) 0.0287(13) 0.0014(11) 0.0150(12) -0.0045(11) O7 0.0250(16) 0.0222(12) 0.0282(13) 0.0018(10) 0.0026(11) 0.0044(10) O8 0.0229(16) 0.0296(14) 0.0309(13) 0.0099(11) -0.0039(11) -0.0067(11) O9 0.0325(17) 0.0243(11) 0.0196(10) -0.0064(9) 0.0028(11) -0.0105(11) O10 0.0237(16) 0.0668(18) 0.0286(12) -0.0013(12) 0.0009(12) -0.0133(16) O11 0.0324(16) 0.0329(13) 0.0146(11) 0.0000(10) 0.0071(10) -0.0016(12) P2 0.0232(5) 0.0152(3) 0.0166(3) 0.0000(3) 0.0029(4) -0.0016(4) C2 0.022(2) 0.0199(15) 0.0158(13) -0.0055(11) -0.0005(14) 0.0034(14) C3 0.023(2) 0.0230(18) 0.0185(16) 0.0027(13) 0.0028(14) -0.0012(15) C4 0.027(2) 0.0163(15) 0.0222(14) 0.0000(11) 0.0075(16) -0.0040(15) C6 0.018(2) 0.0192(15) 0.0198(15) -0.0013(12) -0.0058(14) 0.0000(14) C7 0.020(2) 0.0162(14) 0.0153(13) 0.0009(11) 0.0040(13) 0.0012(13) _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 N1 C2 1.497(3) . ? N1 C6 1.498(4) . ? N1 C4 1.500(4) . ? N1 H1A 0.9100 . ? Sr1 O1 2.545(2) 3_545 ? Sr1 O1 2.636(2) . ? Sr1 O9 2.6657(19) . ? Sr1 O3 2.701(2) 1_455 ? Sr1 O4 2.703(2) 3_645 ? Sr1 O3 2.778(2) 3_645 ? Sr1 O6 2.817(3) . ? Sr1 O5 2.822(2) . ? Sr1 O2 2.870(3) . ? Sr1 O2 2.953(3) 1_455 ? Sr1 P1 3.2932(9) . ? Sr1 P2 3.3293(8) . ? Sr2 O2 2.5023(19) 3_655 ? Sr2 O5 2.526(2) . ? Sr2 O3 2.590(2) . ? Sr2 O8 2.604(2) . ? Sr2 O9 2.649(2) 3 ? Sr2 O11 2.668(2) . ? Sr2 O7 2.669(2) 1_655 ? Sr2 O1 2.817(2) . ? Sr2 O9 3.170(3) 3_655 ? Sr2 C7 3.220(3) . ? Sr2 P1 3.2417(7) . ? Sr2 Sr1 3.9733(4) 3 ? P1 O2 1.504(2) . ? P1 O3 1.519(2) . ? P1 O1 1.518(2) . ? P1 O4 1.593(2) . ? P1 Eu1 3.3516(8) 1_655 ? P1 Sr1 3.3516(8) 1_655 ? P1 Eu1 3.4228(8) 3_655 ? P1 Sr1 3.4228(8) 3_655 ? O1 Eu1 2.545(2) 3 ? O1 Sr1 2.545(2) 3 ? O2 Eu2 2.5023(19) 3_645 ? O2 Sr2 2.5023(19) 3_645 ? O2 Sr1 2.953(3) 1_655 ? O2 Eu1 2.953(3) 1_655 ? O3 Eu1 2.701(2) 1_655 ? O3 Sr1 2.701(2) 1_655 ? O3 Eu1 2.778(2) 3_655 ? O3 Sr1 2.778(2) 3_655 ? O4 Eu1 2.703(2) 3_655 ? O4 Sr1 2.703(2) 3_655 ? O4 H4A 0.8200 . ? O5 P2 1.495(3) . ? O6 P2 1.485(2) . ? O7 P2 1.584(2) . ? O7 Eu2 2.669(2) 1_455 ? O7 Sr2 2.669(2) 1_455 ? O7 H7A 0.8200 . ? O8 C7 1.237(4) . ? O9 C7 1.268(3) 3_645 ? O9 Eu2 2.649(2) 3_545 ? O9 Sr2 2.649(2) 3_545 ? O9 Sr2 3.170(2) 3_645 ? O10 C3 1.232(4) . ? O11 C3 1.262(4) . ? P2 C4 1.830(3) . ? C2 C3 1.520(5) 4_455 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C2 1.520(5) 4 ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C6 C7 1.526(4) 1_445 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O9 1.268(3) 3_655 ? C7 C6 1.526(4) 1_665 ? 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 C2 N1 C6 112.9(2) . . ? C2 N1 C4 111.3(2) . . ? C6 N1 C4 112.9(3) . . ? C2 N1 H1A 106.4 . . ? C6 N1 H1A 106.4 . . ? C4 N1 H1A 106.4 . . ? O1 Sr1 O1 167.67(4) 3_545 . ? O1 Sr1 O9 80.49(6) 3_545 . ? O1 Sr1 O9 90.55(6) . . ? O1 Sr1 O3 107.24(7) 3_545 1_455 ? O1 Sr1 O3 65.76(7) . 1_455 ? O9 Sr1 O3 99.89(7) . 1_455 ? O1 Sr1 O4 92.15(7) 3_545 3_645 ? O1 Sr1 O4 99.73(7) . 3_645 ? O9 Sr1 O4 120.53(7) . 3_645 ? O3 Sr1 O4 137.72(6) 1_455 3_645 ? O1 Sr1 O3 65.81(7) 3_545 3_645 ? O1 Sr1 O3 119.44(7) . 3_645 ? O9 Sr1 O3 71.65(7) . 3_645 ? O3 Sr1 O3 169.48(2) 1_455 3_645 ? O4 Sr1 O3 52.31(6) 3_645 3_645 ? O1 Sr1 O6 73.27(7) 3_545 . ? O1 Sr1 O6 112.04(7) . . ? O9 Sr1 O6 147.87(7) . . ? O3 Sr1 O6 71.39(7) 1_455 . ? O4 Sr1 O6 79.29(7) 3_645 . ? O3 Sr1 O6 112.29(7) 3_645 . ? O1 Sr1 O5 122.50(7) 3_545 . ? O1 Sr1 O5 66.81(7) . . ? O9 Sr1 O5 157.00(7) . . ? O3 Sr1 O5 75.16(7) 1_455 . ? O4 Sr1 O5 62.83(7) 3_645 . ? O3 Sr1 O5 115.08(7) 3_645 . ? O6 Sr1 O5 52.59(7) . . ? O1 Sr1 O2 129.33(6) 3_545 . ? O1 Sr1 O2 53.47(6) . . ? O9 Sr1 O2 70.22(7) . . ? O3 Sr1 O2 117.66(6) 1_455 . ? O4 Sr1 O2 70.33(6) 3_645 . ? O3 Sr1 O2 66.10(6) 3_645 . ? O6 Sr1 O2 141.60(7) . . ? O5 Sr1 O2 91.89(6) . . ? O1 Sr1 O2 64.74(6) 3_545 1_455 ? O1 Sr1 O2 103.80(6) . 1_455 ? O9 Sr1 O2 64.81(7) . 1_455 ? O3 Sr1 O2 52.10(6) 1_455 1_455 ? O4 Sr1 O2 155.89(6) 3_645 1_455 ? O3 Sr1 O2 117.56(6) 3_645 1_455 ? O6 Sr1 O2 87.04(7) . 1_455 ? O5 Sr1 O2 122.69(7) . 1_455 ? O2 Sr1 O2 129.12(7) . 1_455 ? O1 Sr1 P1 156.17(5) 3_545 . ? O1 Sr1 P1 26.86(5) . . ? O9 Sr1 P1 83.12(5) . . ? O3 Sr1 P1 92.50(5) 1_455 . ? O4 Sr1 P1 81.41(5) 3_645 . ? O3 Sr1 P1 92.64(5) 3_645 . ? O6 Sr1 P1 127.13(5) . . ? O5 Sr1 P1 74.79(5) . . ? O2 Sr1 P1 27.16(4) . . ? O2 Sr1 P1 122.49(4) 1_455 . ? O1 Sr1 P2 98.80(5) 3_545 . ? O1 Sr1 P2 88.18(5) . . ? O9 Sr1 P2 167.87(6) . . ? O3 Sr1 P2 68.64(5) 1_455 . ? O4 Sr1 P2 71.54(5) 3_645 . ? O3 Sr1 P2 119.26(5) 3_645 . ? O6 Sr1 P2 26.32(5) . . ? O5 Sr1 P2 26.52(5) . . ? O2 Sr1 P2 117.98(5) . . ? O2 Sr1 P2 103.82(4) 1_455 . ? P1 Sr1 P2 100.81(2) . . ? O2 Sr2 O5 133.38(8) 3_655 . ? O2 Sr2 O3 74.45(7) 3_655 . ? O5 Sr2 O3 91.99(7) . . ? O2 Sr2 O8 77.07(8) 3_655 . ? O5 Sr2 O8 147.38(7) . . ? O3 Sr2 O8 110.48(7) . . ? O2 Sr2 O9 71.75(8) 3_655 3 ? O5 Sr2 O9 84.17(7) . 3 ? O3 Sr2 O9 128.39(6) . 3 ? O8 Sr2 O9 98.61(7) . 3 ? O2 Sr2 O11 128.53(7) 3_655 . ? O5 Sr2 O11 72.60(7) . . ? O3 Sr2 O11 157.01(7) . . ? O8 Sr2 O11 78.30(7) . . ? O9 Sr2 O11 68.24(6) 3 . ? O2 Sr2 O7 132.53(8) 3_655 1_655 ? O5 Sr2 O7 86.32(8) . 1_655 ? O3 Sr2 O7 80.39(7) . 1_655 ? O8 Sr2 O7 75.03(8) . 1_655 ? O9 Sr2 O7 149.87(7) 3 1_655 ? O11 Sr2 O7 81.64(7) . 1_655 ? O2 Sr2 O1 67.43(7) 3_655 . ? O5 Sr2 O1 68.30(7) . . ? O3 Sr2 O1 55.29(7) . . ? O8 Sr2 O1 144.06(7) . . ? O9 Sr2 O1 76.00(6) 3 . ? O11 Sr2 O1 128.78(7) . . ? O7 Sr2 O1 126.12(7) 1_655 . ? O2 Sr2 O9 67.21(7) 3_655 3_655 ? O5 Sr2 O9 146.60(7) . 3_655 ? O3 Sr2 O9 66.31(6) . 3_655 ? O8 Sr2 O9 44.21(7) . 3_655 ? O9 Sr2 O9 129.11(8) 3 3_655 ? O11 Sr2 O9 118.29(6) . 3_655 ? O7 Sr2 O9 65.94(7) 1_655 3_655 ? O1 Sr2 O9 112.61(5) . 3_655 ? O2 Sr2 C7 70.42(8) 3_655 . ? O5 Sr2 C7 155.37(7) . . ? O3 Sr2 C7 89.14(7) . . ? O8 Sr2 C7 21.35(7) . . ? O9 Sr2 C7 114.00(8) 3 . ? O11 Sr2 C7 97.94(7) . . ? O7 Sr2 C7 69.61(7) 1_655 . ? O1 Sr2 C7 130.33(7) . . ? O9 Sr2 C7 22.88(6) 3_655 . ? O2 Sr2 P1 68.04(5) 3_655 . ? O5 Sr2 P1 79.59(5) . . ? O3 Sr2 P1 27.38(5) . . ? O8 Sr2 P1 130.39(6) . . ? O9 Sr2 P1 102.48(4) 3 . ? O11 Sr2 P1 151.31(5) . . ? O7 Sr2 P1 103.80(5) 1_655 . ? O1 Sr2 P1 27.91(4) . . ? O9 Sr2 P1 89.00(4) 3_655 . ? C7 Sr2 P1 110.43(6) . . ? O2 Sr2 Sr1 47.92(6) 3_655 3 ? O5 Sr2 Sr1 87.75(6) . 3 ? O3 Sr2 Sr1 86.73(5) . 3 ? O8 Sr2 Sr1 115.92(6) . 3 ? O9 Sr2 Sr1 41.78(4) 3 3 ? O11 Sr2 Sr1 109.01(5) . 3 ? O7 Sr2 Sr1 165.61(5) 1_655 3 ? O1 Sr2 Sr1 39.60(4) . 3 ? O9 Sr2 Sr1 114.51(4) 3_655 3 ? C7 Sr2 Sr1 116.88(5) . 3 ? P1 Sr2 Sr1 62.185(15) . 3 ? O2 P1 O3 111.16(13) . . ? O2 P1 O1 110.67(14) . . ? O3 P1 O1 111.93(12) . . ? O2 P1 O4 110.98(12) . . ? O3 P1 O4 101.93(13) . . ? O1 P1 O4 109.88(12) . . ? O2 P1 Sr2 130.69(9) . . ? O3 P1 Sr2 51.66(9) . . ? O1 P1 Sr2 60.28(8) . . ? O4 P1 Sr2 117.60(8) . . ? O2 P1 Sr1 60.56(10) . . ? O3 P1 Sr1 118.70(9) . . ? O1 P1 Sr1 51.69(8) . . ? O4 P1 Sr1 139.04(9) . . ? Sr2 P1 Sr1 86.585(19) . . ? O2 P1 Eu1 61.75(10) . 1_655 ? O3 P1 Eu1 52.18(9) . 1_655 ? O1 P1 Eu1 145.09(9) . 1_655 ? O4 P1 Eu1 104.23(9) . 1_655 ? Sr2 P1 Eu1 97.40(2) . 1_655 ? Sr1 P1 Eu1 104.64(2) . 1_655 ? O2 P1 Sr1 61.75(10) . 1_655 ? O3 P1 Sr1 52.18(9) . 1_655 ? O1 P1 Sr1 145.09(9) . 1_655 ? O4 P1 Sr1 104.23(9) . 1_655 ? Sr2 P1 Sr1 97.40(2) . 1_655 ? Sr1 P1 Sr1 104.64(2) . 1_655 ? Eu1 P1 Sr1 0.000(11) 1_655 1_655 ? O2 P1 Eu1 133.98(11) . 3_655 ? O3 P1 Eu1 52.67(9) . 3_655 ? O1 P1 Eu1 115.29(9) . 3_655 ? O4 P1 Eu1 50.44(8) . 3_655 ? Sr2 P1 Eu1 77.174(17) . 3_655 ? Sr1 P1 Eu1 163.38(2) . 3_655 ? Eu1 P1 Eu1 81.238(19) 1_655 3_655 ? Sr1 P1 Eu1 81.238(19) 1_655 3_655 ? O2 P1 Sr1 133.98(11) . 3_655 ? O3 P1 Sr1 52.67(9) . 3_655 ? O1 P1 Sr1 115.29(9) . 3_655 ? O4 P1 Sr1 50.44(8) . 3_655 ? Sr2 P1 Sr1 77.174(17) . 3_655 ? Sr1 P1 Sr1 163.38(2) . 3_655 ? Eu1 P1 Sr1 81.238(19) 1_655 3_655 ? Sr1 P1 Sr1 81.238(19) 1_655 3_655 ? Eu1 P1 Sr1 0.000(10) 3_655 3_655 ? P1 O1 Eu1 135.33(12) . 3 ? P1 O1 Sr1 135.33(12) . 3 ? Eu1 O1 Sr1 0.000(15) 3 3 ? P1 O1 Sr1 101.45(10) . . ? Eu1 O1 Sr1 116.70(8) 3 . ? Sr1 O1 Sr1 116.70(8) 3 . ? P1 O1 Sr2 91.80(10) . . ? Eu1 O1 Sr2 95.52(7) 3 . ? Sr1 O1 Sr2 95.52(7) 3 . ? Sr1 O1 Sr2 110.48(7) . . ? P1 O2 Eu2 158.06(13) . 3_645 ? P1 O2 Sr2 158.06(13) . 3_645 ? Eu2 O2 Sr2 0.000(18) 3_645 3_645 ? P1 O2 Sr1 92.28(11) . . ? Eu2 O2 Sr1 101.23(8) 3_645 . ? Sr2 O2 Sr1 101.23(8) 3_645 . ? P1 O2 Sr1 91.59(11) . 1_655 ? Eu2 O2 Sr1 93.11(7) 3_645 1_655 ? Sr2 O2 Sr1 93.11(7) 3_645 1_655 ? Sr1 O2 Sr1 129.12(7) . 1_655 ? P1 O2 Eu1 91.59(11) . 1_655 ? Eu2 O2 Eu1 93.11(7) 3_645 1_655 ? Sr2 O2 Eu1 93.11(7) 3_645 1_655 ? Sr1 O2 Eu1 129.12(7) . 1_655 ? Sr1 O2 Eu1 0.000(14) 1_655 1_655 ? P1 O3 Sr2 100.96(11) . . ? P1 O3 Eu1 101.45(11) . 1_655 ? Sr2 O3 Eu1 138.84(9) . 1_655 ? P1 O3 Sr1 101.45(11) . 1_655 ? Sr2 O3 Sr1 138.84(9) . 1_655 ? Eu1 O3 Sr1 0.000(16) 1_655 1_655 ? P1 O3 Eu1 101.57(10) . 3_655 ? Sr2 O3 Eu1 101.51(7) . 3_655 ? Eu1 O3 Eu1 107.20(7) 1_655 3_655 ? Sr1 O3 Eu1 107.20(7) 1_655 3_655 ? P1 O3 Sr1 101.57(10) . 3_655 ? Sr2 O3 Sr1 101.51(7) . 3_655 ? Eu1 O3 Sr1 107.20(7) 1_655 3_655 ? Sr1 O3 Sr1 107.20(7) 1_655 3_655 ? Eu1 O3 Sr1 0.000(11) 3_655 3_655 ? P1 O4 Eu1 102.54(10) . 3_655 ? P1 O4 Sr1 102.54(10) . 3_655 ? Eu1 O4 Sr1 0.000(13) 3_655 3_655 ? P1 O4 H4A 109.5 . . ? Eu1 O4 H4A 122.8 3_655 . ? Sr1 O4 H4A 122.8 3_655 . ? P2 O5 Sr2 137.06(13) . . ? P2 O5 Sr1 96.04(11) . . ? Sr2 O5 Sr1 113.72(8) . . ? P2 O6 Sr1 96.45(13) . . ? P2 O7 Eu2 123.80(12) . 1_455 ? P2 O7 Sr2 123.80(12) . 1_455 ? Eu2 O7 Sr2 0.000(13) 1_455 1_455 ? P2 O7 H7A 109.5 . . ? Eu2 O7 H7A 108.1 1_455 . ? Sr2 O7 H7A 108.1 1_455 . ? C7 O8 Sr2 108.64(19) . . ? C7 O9 Eu2 123.0(2) 3_645 3_545 ? C7 O9 Sr2 123.0(2) 3_645 3_545 ? Eu2 O9 Sr2 0.000(10) 3_545 3_545 ? C7 O9 Sr1 134.88(19) 3_645 . ? Eu2 O9 Sr1 96.78(7) 3_545 . ? Sr2 O9 Sr1 96.78(7) 3_545 . ? C7 O9 Sr2 80.8(2) 3_645 3_645 ? Eu2 O9 Sr2 129.11(8) 3_545 3_645 ? Sr2 O9 Sr2 129.11(8) 3_545 3_645 ? Sr1 O9 Sr2 90.48(6) . 3_645 ? C3 O11 Sr2 148.2(2) . . ? O6 P2 O5 113.90(14) . . ? O6 P2 O7 110.27(16) . . ? O5 P2 O7 110.97(13) . . ? O6 P2 C4 107.43(14) . . ? O5 P2 C4 109.66(17) . . ? O7 P2 C4 104.10(13) . . ? O6 P2 Sr1 57.23(10) . . ? O5 P2 Sr1 57.44(9) . . ? O7 P2 Sr1 121.94(9) . . ? C4 P2 Sr1 133.93(11) . . ? N1 C2 C3 108.7(3) . 4_455 ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 4_455 . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 4_455 . ? H2A C2 H2B 108.3 . . ? O10 C3 O11 125.6(3) . . ? O10 C3 C2 117.6(3) . 4 ? O11 C3 C2 116.7(3) . 4 ? N1 C4 P2 112.5(2) . . ? N1 C4 H4B 109.1 . . ? P2 C4 H4B 109.1 . . ? N1 C4 H4C 109.1 . . ? P2 C4 H4C 109.1 . . ? H4B C4 H4C 107.8 . . ? N1 C6 C7 110.3(3) . 1_445 ? N1 C6 H6A 109.6 . . ? C7 C6 H6A 109.6 1_445 . ? N1 C6 H6B 109.6 . . ? C7 C6 H6B 109.6 1_445 . ? H6A C6 H6B 108.1 . . ? O8 C7 O9 126.3(3) . 3_655 ? O8 C7 C6 118.3(3) . 1_665 ? O9 C7 C6 115.4(3) 3_655 1_665 ? O8 C7 Sr2 50.01(16) . . ? O9 C7 Sr2 76.36(18) 3_655 . ? C6 C7 Sr2 168.0(2) 1_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.422 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 930274' ####################################################################### # # 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_5_Tb #TrackingRef 'All.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H8.93 N O11 P2 Sr1.93 Tb0.07' _chemical_formula_weight 501.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.2543(2) _cell_length_b 8.7559(3) _cell_length_c 26.5187(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1220.02(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6902 _cell_measurement_theta_min 2.7878 _cell_measurement_theta_max 28.3281 _exptl_crystal_description columnar _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 9.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2614 _exptl_absorpt_correction_T_max 0.4058 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 12463 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3015 _reflns_number_gt 2723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 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^)+(0.0052P)^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 0.014(6) _chemical_absolute_configuration ad _refine_ls_number_reflns 3015 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0457 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Sr1 Sr 0.02734(7) 0.19818(4) 0.242626(11) 0.01497(11) Uani 0.972(2) 1 d P . . Tb1 Tb 0.02734(7) 0.19818(4) 0.242626(11) 0.01497(11) Uani 0.028(2) 1 d P . . Sr2 Sr 0.44515(7) 0.54814(4) 0.151523(11) 0.01450(10) Uani 0.956(2) 1 d P . . Tb2 Tb 0.44515(7) 0.54814(4) 0.151523(11) 0.01450(10) Uani 0.044(2) 1 d P . . N1 N -0.0464(6) -0.0113(3) 0.06318(9) 0.0160(6) Uani 1 1 d . . . H1A H -0.2118 -0.0078 0.0733 0.019 Uiso 0.93 1 calc PR . . P1 P 0.51999(19) 0.41973(9) 0.26526(3) 0.0129(2) Uani 1 1 d . . . O1 O 0.2564(4) 0.4654(3) 0.24738(9) 0.0186(6) Uani 1 1 d . . . O2 O 0.5187(6) 0.2595(3) 0.28548(9) 0.0281(7) Uani 1 1 d . . . O3 O 0.7187(5) 0.4389(3) 0.22442(9) 0.0186(6) Uani 1 1 d . . . O4 O 0.6151(5) 0.5372(3) 0.30709(8) 0.0205(6) Uani 1 1 d . . . H4A H 0.4917 0.5770 0.3207 0.031 Uiso 1 1 calc R . . O5 O 0.1782(5) 0.3093(3) 0.14753(10) 0.0249(6) Uani 1 1 d . . . O6 O -0.2195(6) 0.1521(3) 0.14925(11) 0.0314(8) Uani 1 1 d . . . O7 O -0.2102(5) 0.3944(3) 0.09826(10) 0.0262(7) Uani 1 1 d . . . H7A H -0.1130 0.4567 0.0855 0.039 Uiso 1 1 calc R . . O8 O 0.6975(6) 0.7571(3) 0.10297(10) 0.0285(7) Uani 1 1 d . . . O9 O -0.0017(5) 0.1890(3) 0.34287(8) 0.0254(7) Uani 1 1 d . . . O10 O 0.0453(6) 0.4666(4) -0.00922(10) 0.0389(8) Uani 1 1 d . . . O11 O 0.2079(5) 0.5490(4) 0.06290(9) 0.0278(7) Uani 1 1 d . . . P2 P -0.0524(2) 0.25548(11) 0.11953(3) 0.0193(2) Uani 1 1 d . . . C2 C -0.0477(8) -0.0775(4) 0.01110(12) 0.0197(8) Uani 1 1 d . . . H2A H -0.0450 -0.1881 0.0130 0.024 Uiso 1 1 calc R . . H2B H 0.1026 -0.0442 -0.0071 0.024 Uiso 1 1 calc R . . C3 C 0.2154(7) 0.5250(5) 0.01631(14) 0.0199(9) Uani 1 1 d . . . C4 C 0.0462(9) 0.1512(4) 0.06287(12) 0.0230(9) Uani 1 1 d . . . H4B H -0.0203 0.2028 0.0333 0.028 Uiso 1 1 calc R . . H4C H 0.2304 0.1518 0.0606 0.028 Uiso 1 1 calc R . . C6 C 0.0891(8) -0.1094(4) 0.10055(13) 0.0198(9) Uani 1 1 d . . . H6A H 0.1525 -0.0465 0.1279 0.024 Uiso 1 1 calc R . . H6B H 0.2337 -0.1579 0.0844 0.024 Uiso 1 1 calc R . . C7 C 0.9127(8) 0.7689(4) 0.12159(12) 0.0176(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 Sr1 0.0143(2) 0.01459(16) 0.01599(15) -0.00051(12) 0.00024(14) -0.00155(14) Tb1 0.0143(2) 0.01459(16) 0.01599(15) -0.00051(12) 0.00024(14) -0.00155(14) Sr2 0.01593(19) 0.01424(16) 0.01333(15) -0.00074(12) 0.00005(15) 0.00015(15) Tb2 0.01593(19) 0.01424(16) 0.01333(15) -0.00074(12) 0.00005(15) 0.00015(15) N1 0.0155(17) 0.0158(15) 0.0165(13) -0.0001(11) 0.0003(14) 0.0004(13) P1 0.0131(6) 0.0118(4) 0.0137(4) -0.0007(3) -0.0005(4) 0.0005(4) O1 0.0104(14) 0.0180(15) 0.0274(15) -0.0040(12) -0.0065(11) 0.0013(11) O2 0.046(2) 0.0137(12) 0.0243(12) 0.0034(10) 0.0003(15) 0.0045(14) O3 0.0118(15) 0.0243(15) 0.0196(13) -0.0039(12) 0.0031(10) 0.0023(12) O4 0.0199(17) 0.0221(15) 0.0195(13) -0.0050(11) -0.0015(11) 0.0015(12) O5 0.0275(17) 0.0228(15) 0.0244(14) 0.0008(13) -0.0080(13) -0.0006(13) O6 0.034(2) 0.0273(17) 0.0328(16) 0.0005(14) 0.0157(15) -0.0053(13) O7 0.0275(19) 0.0215(16) 0.0297(16) 0.0010(12) 0.0019(13) 0.0050(13) O8 0.0228(18) 0.0314(18) 0.0314(16) 0.0105(13) -0.0042(13) -0.0058(14) O9 0.0316(19) 0.0265(14) 0.0180(11) -0.0071(10) 0.0024(13) -0.0118(13) O10 0.0222(17) 0.065(2) 0.0299(14) 0.0015(15) 0.0019(15) -0.0145(19) O11 0.0336(19) 0.0327(17) 0.0171(14) -0.0003(13) 0.0070(12) 0.0020(15) P2 0.0260(6) 0.0160(4) 0.0159(4) 0.0000(3) 0.0025(5) -0.0014(5) C2 0.023(2) 0.021(2) 0.0150(15) -0.0055(14) 0.0011(17) 0.0030(18) C3 0.022(2) 0.020(2) 0.0182(19) 0.0005(16) 0.0011(17) 0.0025(17) C4 0.031(2) 0.0176(19) 0.0205(17) 0.0009(14) 0.008(2) -0.0071(19) C6 0.021(3) 0.0179(19) 0.0202(18) -0.0014(14) -0.0038(17) -0.0026(17) C7 0.023(3) 0.0155(18) 0.0142(16) 0.0014(14) 0.0044(16) 0.0008(16) _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 Sr1 O1 2.539(3) 3_545 ? Sr1 O1 2.634(3) . ? Sr1 O9 2.664(2) . ? Sr1 O3 2.703(3) 1_455 ? Sr1 O4 2.693(3) 3_645 ? Sr1 O3 2.774(3) 3_645 ? Sr1 O6 2.824(3) . ? Sr1 O5 2.817(3) . ? Sr1 O2 2.871(3) . ? Sr1 O2 2.953(3) 1_455 ? Sr1 P1 3.2899(10) . ? Sr1 P2 3.3291(9) . ? Sr2 O2 2.500(2) 3_655 ? Sr2 O5 2.520(3) . ? Sr2 O3 2.592(3) . ? Sr2 O8 2.601(3) . ? Sr2 O9 2.640(3) 3 ? Sr2 O7 2.662(3) 1_655 ? Sr2 O11 2.660(3) . ? Sr2 O1 2.823(3) . ? Sr2 O9 3.177(3) 3_655 ? Sr2 C7 3.225(4) . ? Sr2 P1 3.2429(9) . ? Sr2 Sr1 3.9710(5) 3 ? N1 C2 1.498(4) . ? N1 C6 1.492(4) . ? N1 C4 1.503(4) . ? N1 H1A 0.9100 . ? P1 O2 1.502(2) . ? P1 O1 1.518(2) . ? P1 O3 1.514(3) . ? P1 O4 1.593(3) . ? P1 Tb1 3.3511(10) 1_655 ? P1 Sr1 3.3511(10) 1_655 ? P1 Sr1 3.4125(10) 3_655 ? O1 Tb1 2.539(3) 3 ? O1 Sr1 2.539(3) 3 ? O2 Tb2 2.500(2) 3_645 ? O2 Sr2 2.500(2) 3_645 ? O2 Sr1 2.953(3) 1_655 ? O3 Tb1 2.703(3) 1_655 ? O3 Sr1 2.703(3) 1_655 ? O3 Tb1 2.774(3) 3_655 ? O3 Sr1 2.774(3) 3_655 ? O4 Tb1 2.693(3) 3_655 ? O4 Sr1 2.693(3) 3_655 ? O4 H4A 0.8200 . ? O5 P2 1.497(3) . ? O6 P2 1.487(3) . ? O7 P2 1.577(3) . ? O7 Tb2 2.662(3) 1_455 ? O7 Sr2 2.662(3) 1_455 ? O7 H7A 0.8200 . ? O8 C7 1.238(5) . ? O9 C7 1.264(4) 3_645 ? O9 Tb2 2.640(3) 3_545 ? O9 Sr2 2.640(3) 3_545 ? O9 Sr2 3.177(3) 3_645 ? O10 C3 1.232(5) . ? O11 C3 1.254(4) . ? P2 C4 1.833(4) . ? C2 C3 1.513(5) 4_455 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C2 1.513(5) 4 ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C6 C7 1.518(5) 1_445 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O9 1.264(4) 3_655 ? C7 C6 1.518(5) 1_665 ? 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 Sr1 O1 167.49(5) 3_545 . ? O1 Sr1 O9 80.66(8) 3_545 . ? O1 Sr1 O9 90.31(7) . . ? O1 Sr1 O3 107.01(8) 3_545 1_455 ? O1 Sr1 O3 65.79(8) . 1_455 ? O9 Sr1 O3 99.64(8) . 1_455 ? O1 Sr1 O4 92.33(8) 3_545 3_645 ? O1 Sr1 O4 99.76(8) . 3_645 ? O9 Sr1 O4 120.83(8) . 3_645 ? O3 Sr1 O4 137.66(7) 1_455 3_645 ? O1 Sr1 O3 65.96(8) 3_545 3_645 ? O1 Sr1 O3 119.47(8) . 3_645 ? O9 Sr1 O3 71.85(8) . 3_645 ? O3 Sr1 O3 169.38(3) 1_455 3_645 ? O4 Sr1 O3 52.45(7) 3_645 3_645 ? O1 Sr1 O6 72.97(8) 3_545 . ? O1 Sr1 O6 112.25(8) . . ? O9 Sr1 O6 147.59(8) . . ? O3 Sr1 O6 71.30(8) 1_455 . ? O4 Sr1 O6 79.42(8) 3_645 . ? O3 Sr1 O6 112.33(8) 3_645 . ? O1 Sr1 O5 122.41(8) 3_545 . ? O1 Sr1 O5 66.89(8) . . ? O9 Sr1 O5 156.93(8) . . ? O3 Sr1 O5 74.90(8) 1_455 . ? O4 Sr1 O5 63.02(8) 3_645 . ? O3 Sr1 O5 115.42(8) 3_645 . ? O6 Sr1 O5 52.68(8) . . ? O1 Sr1 O2 129.54(7) 3_545 . ? O1 Sr1 O2 53.44(7) . . ? O9 Sr1 O2 70.26(8) . . ? O3 Sr1 O2 117.67(7) 1_455 . ? O4 Sr1 O2 70.38(7) 3_645 . ? O3 Sr1 O2 66.16(7) 3_645 . ? O6 Sr1 O2 141.87(8) . . ? O5 Sr1 O2 92.11(7) . . ? O1 Sr1 O2 64.81(8) 3_545 1_455 ? O1 Sr1 O2 103.51(7) . 1_455 ? O9 Sr1 O2 64.51(8) . 1_455 ? O3 Sr1 O2 51.99(7) 1_455 1_455 ? O4 Sr1 O2 156.16(8) 3_645 1_455 ? O3 Sr1 O2 117.56(7) 3_645 1_455 ? O6 Sr1 O2 87.01(8) . 1_455 ? O5 Sr1 O2 122.44(8) . 1_455 ? O2 Sr1 O2 128.86(8) . 1_455 ? O1 Sr1 P1 156.38(5) 3_545 . ? O1 Sr1 P1 26.88(5) . . ? O9 Sr1 P1 83.16(6) . . ? O3 Sr1 P1 92.56(6) 1_455 . ? O4 Sr1 P1 81.31(6) 3_645 . ? O3 Sr1 P1 92.67(6) 3_645 . ? O6 Sr1 P1 127.27(6) . . ? O5 Sr1 P1 74.83(6) . . ? O2 Sr1 P1 27.15(5) . . ? O2 Sr1 P1 122.32(5) 1_455 . ? O1 Sr1 P2 98.59(6) 3_545 . ? O1 Sr1 P2 88.31(6) . . ? O9 Sr1 P2 167.37(6) . . ? O3 Sr1 P2 68.40(6) 1_455 . ? O4 Sr1 P2 71.75(5) 3_645 . ? O3 Sr1 P2 119.52(6) 3_645 . ? O6 Sr1 P2 26.37(6) . . ? O5 Sr1 P2 26.56(6) . . ? O2 Sr1 P2 118.24(5) . . ? O2 Sr1 P2 103.65(5) 1_455 . ? P1 Sr1 P2 100.90(3) . . ? O2 Sr2 O5 133.19(9) 3_655 . ? O2 Sr2 O3 74.48(8) 3_655 . ? O5 Sr2 O3 91.94(9) . . ? O2 Sr2 O8 76.78(9) 3_655 . ? O5 Sr2 O8 147.86(8) . . ? O3 Sr2 O8 110.25(9) . . ? O2 Sr2 O9 71.57(9) 3_655 3 ? O5 Sr2 O9 84.19(9) . 3 ? O3 Sr2 O9 128.30(7) . 3 ? O8 Sr2 O9 98.57(9) . 3 ? O2 Sr2 O7 132.61(10) 3_655 1_655 ? O5 Sr2 O7 86.38(9) . 1_655 ? O3 Sr2 O7 80.32(8) . 1_655 ? O8 Sr2 O7 75.30(9) . 1_655 ? O9 Sr2 O7 150.04(8) 3 1_655 ? O2 Sr2 O11 128.59(9) 3_655 . ? O5 Sr2 O11 72.82(9) . . ? O3 Sr2 O11 156.91(9) . . ? O8 Sr2 O11 78.43(9) . . ? O9 Sr2 O11 68.58(7) 3 . ? O7 Sr2 O11 81.46(8) 1_655 . ? O2 Sr2 O1 67.35(8) 3_655 . ? O5 Sr2 O1 68.24(8) . . ? O3 Sr2 O1 55.15(7) . . ? O8 Sr2 O1 143.65(8) . . ? O9 Sr2 O1 76.06(7) 3 . ? O7 Sr2 O1 125.94(8) 1_655 . ? O11 Sr2 O1 129.17(8) . . ? O2 Sr2 O9 67.15(8) 3_655 3_655 ? O5 Sr2 O9 146.75(8) . 3_655 ? O3 Sr2 O9 66.28(7) . 3_655 ? O8 Sr2 O9 44.02(7) . 3_655 ? O9 Sr2 O9 128.93(9) 3 3_655 ? O7 Sr2 O9 66.10(8) 1_655 3_655 ? O11 Sr2 O9 118.12(7) . 3_655 ? O1 Sr2 O9 112.39(6) . 3_655 ? O2 Sr2 C7 70.31(9) 3_655 . ? O5 Sr2 C7 155.63(9) . . ? O3 Sr2 C7 88.98(9) . . ? O8 Sr2 C7 21.28(8) . . ? O9 Sr2 C7 113.96(9) 3 . ? O7 Sr2 C7 69.77(9) 1_655 . ? O11 Sr2 C7 97.91(9) . . ? O1 Sr2 C7 130.02(8) . . ? O9 Sr2 C7 22.75(7) 3_655 . ? O2 Sr2 P1 68.03(6) 3_655 . ? O5 Sr2 P1 79.56(6) . . ? O3 Sr2 P1 27.27(6) . . ? O8 Sr2 P1 129.98(7) . . ? O9 Sr2 P1 102.51(5) 3 . ? O7 Sr2 P1 103.63(6) 1_655 . ? O11 Sr2 P1 151.59(7) . . ? O1 Sr2 P1 27.89(5) . . ? O9 Sr2 P1 88.82(4) 3_655 . ? C7 Sr2 P1 110.14(7) . . ? O2 Sr2 Sr1 47.96(7) 3_655 3 ? O5 Sr2 Sr1 87.49(6) . 3 ? O3 Sr2 Sr1 86.65(5) . 3 ? O8 Sr2 Sr1 115.84(7) . 3 ? O9 Sr2 Sr1 41.76(5) 3 3 ? O7 Sr2 Sr1 165.39(6) 1_655 3 ? O11 Sr2 Sr1 109.31(6) . 3 ? O1 Sr2 Sr1 39.54(5) . 3 ? O9 Sr2 Sr1 114.46(4) 3_655 3 ? C7 Sr2 Sr1 116.87(6) . 3 ? P1 Sr2 Sr1 62.162(18) . 3 ? C2 N1 C6 113.0(3) . . ? C2 N1 C4 111.3(3) . . ? C6 N1 C4 113.2(3) . . ? C2 N1 H1A 106.2 . . ? C6 N1 H1A 106.2 . . ? C4 N1 H1A 106.2 . . ? O2 P1 O1 110.70(16) . . ? O2 P1 O3 111.24(16) . . ? O1 P1 O3 112.13(14) . . ? O2 P1 O4 110.87(14) . . ? O1 P1 O4 109.49(15) . . ? O3 P1 O4 102.12(14) . . ? O2 P1 Sr2 130.94(10) . . ? O1 P1 Sr2 60.48(10) . . ? O3 P1 Sr2 51.66(10) . . ? O4 P1 Sr2 117.49(10) . . ? O2 P1 Sr1 60.71(12) . . ? O1 P1 Sr1 51.70(10) . . ? O3 P1 Sr1 118.54(10) . . ? O4 P1 Sr1 138.98(10) . . ? Sr2 P1 Sr1 86.52(2) . . ? O2 P1 Tb1 61.76(12) . 1_655 ? O1 P1 Tb1 145.34(10) . 1_655 ? O3 P1 Tb1 52.22(11) . 1_655 ? O4 P1 Tb1 104.43(10) . 1_655 ? Sr2 P1 Tb1 97.50(2) . 1_655 ? Sr1 P1 Tb1 104.59(2) . 1_655 ? O2 P1 Sr1 61.76(12) . 1_655 ? O1 P1 Sr1 145.34(10) . 1_655 ? O3 P1 Sr1 52.22(11) . 1_655 ? O4 P1 Sr1 104.43(10) . 1_655 ? Sr2 P1 Sr1 97.50(2) . 1_655 ? Sr1 P1 Sr1 104.59(2) . 1_655 ? Tb1 P1 Sr1 0.000(15) 1_655 1_655 ? O2 P1 Sr1 133.82(13) . 3_655 ? O1 P1 Sr1 115.39(11) . 3_655 ? O3 P1 Sr1 52.84(10) . 3_655 ? O4 P1 Sr1 50.41(9) . 3_655 ? Sr2 P1 Sr1 77.28(2) . 3_655 ? Sr1 P1 Sr1 163.43(3) . 3_655 ? Tb1 P1 Sr1 81.27(2) 1_655 3_655 ? Sr1 P1 Sr1 81.27(2) 1_655 3_655 ? P1 O1 Tb1 135.62(14) . 3 ? P1 O1 Sr1 135.62(14) . 3 ? Tb1 O1 Sr1 0.000(18) 3 3 ? P1 O1 Sr1 101.41(13) . . ? Tb1 O1 Sr1 116.73(9) 3 . ? Sr1 O1 Sr1 116.73(9) 3 . ? P1 O1 Sr2 91.62(11) . . ? Tb1 O1 Sr2 95.41(8) 3 . ? Sr1 O1 Sr2 95.41(8) 3 . ? Sr1 O1 Sr2 110.21(9) . . ? P1 O2 Tb2 158.35(15) . 3_645 ? P1 O2 Sr2 158.35(15) . 3_645 ? Tb2 O2 Sr2 0.00(2) 3_645 3_645 ? P1 O2 Sr1 92.14(13) . . ? Tb2 O2 Sr1 101.21(9) 3_645 . ? Sr2 O2 Sr1 101.21(9) 3_645 . ? P1 O2 Sr1 91.62(13) . 1_655 ? Tb2 O2 Sr1 93.09(8) 3_645 1_655 ? Sr2 O2 Sr1 93.09(8) 3_645 1_655 ? Sr1 O2 Sr1 128.86(8) . 1_655 ? P1 O3 Sr2 101.07(12) . . ? P1 O3 Tb1 101.50(13) . 1_655 ? Sr2 O3 Tb1 138.90(10) . 1_655 ? P1 O3 Sr1 101.50(13) . 1_655 ? Sr2 O3 Sr1 138.90(10) . 1_655 ? Tb1 O3 Sr1 0.000(15) 1_655 1_655 ? P1 O3 Tb1 101.38(12) . 3_655 ? Sr2 O3 Tb1 101.53(10) . 3_655 ? Tb1 O3 Tb1 107.06(8) 1_655 3_655 ? Sr1 O3 Tb1 107.06(8) 1_655 3_655 ? P1 O3 Sr1 101.38(12) . 3_655 ? Sr2 O3 Sr1 101.53(10) . 3_655 ? Tb1 O3 Sr1 107.06(8) 1_655 3_655 ? Sr1 O3 Sr1 107.06(8) 1_655 3_655 ? Tb1 O3 Sr1 0.000(14) 3_655 3_655 ? P1 O4 Tb1 102.47(11) . 3_655 ? P1 O4 Sr1 102.47(11) . 3_655 ? Tb1 O4 Sr1 0.000(16) 3_655 3_655 ? P1 O4 H4A 109.5 . . ? Tb1 O4 H4A 123.0 3_655 . ? Sr1 O4 H4A 123.0 3_655 . ? P2 O5 Sr2 137.09(16) . . ? P2 O5 Sr1 96.17(13) . . ? Sr2 O5 Sr1 113.93(9) . . ? P2 O6 Sr1 96.12(14) . . ? P2 O7 Tb2 123.93(14) . 1_455 ? P2 O7 Sr2 123.93(14) . 1_455 ? Tb2 O7 Sr2 0.000(15) 1_455 1_455 ? P2 O7 H7A 109.5 . . ? Tb2 O7 H7A 107.8 1_455 . ? Sr2 O7 H7A 107.8 1_455 . ? C7 O8 Sr2 109.1(2) . . ? C7 O9 Tb2 122.9(2) 3_645 3_545 ? C7 O9 Sr2 122.9(2) 3_645 3_545 ? Tb2 O9 Sr2 0.000(17) 3_545 3_545 ? C7 O9 Sr1 134.9(2) 3_645 . ? Tb2 O9 Sr1 96.95(8) 3_545 . ? Sr2 O9 Sr1 96.95(8) 3_545 . ? C7 O9 Sr2 80.8(2) 3_645 3_645 ? Tb2 O9 Sr2 128.93(9) 3_545 3_645 ? Sr2 O9 Sr2 128.93(9) 3_545 3_645 ? Sr1 O9 Sr2 90.32(7) . 3_645 ? C3 O11 Sr2 148.8(3) . . ? O6 P2 O5 113.99(17) . . ? O6 P2 O7 110.43(18) . . ? O5 P2 O7 111.10(16) . . ? O6 P2 C4 107.33(17) . . ? O5 P2 C4 109.55(19) . . ? O7 P2 C4 103.88(16) . . ? O6 P2 Sr1 57.51(12) . . ? O5 P2 Sr1 57.27(11) . . ? O7 P2 Sr1 122.22(11) . . ? C4 P2 Sr1 133.87(13) . . ? N1 C2 C3 109.2(3) . 4_455 ? N1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 4_455 . ? N1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 4_455 . ? H2A C2 H2B 108.3 . . ? O10 C3 O11 126.0(4) . . ? O10 C3 C2 117.3(3) . 4 ? O11 C3 C2 116.6(3) . 4 ? N1 C4 P2 112.1(2) . . ? N1 C4 H4B 109.2 . . ? P2 C4 H4B 109.2 . . ? N1 C4 H4C 109.2 . . ? P2 C4 H4C 109.2 . . ? H4B C4 H4C 107.9 . . ? N1 C6 C7 110.9(3) . 1_445 ? N1 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 1_445 . ? N1 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 1_445 . ? H6A C6 H6B 108.0 . . ? O8 C7 O9 126.1(4) . 3_655 ? O8 C7 C6 118.0(3) . 1_665 ? O9 C7 C6 115.9(4) 3_655 1_665 ? O8 C7 Sr2 49.65(19) . . ? O9 C7 Sr2 76.5(2) 3_655 . ? C6 C7 Sr2 167.4(3) 1_665 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.588 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 930275'