# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_ccdc764694 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H5 N O5 Sr' _chemical_formula_sum 'C7 H5 N O5 Sr' _chemical_formula_weight 270.74 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' 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 6.4411(4) _cell_length_b 6.8211(4) _cell_length_c 10.0120(6) _cell_angle_alpha 94.140(3) _cell_angle_beta 93.010(3) _cell_angle_gamma 117.310(3) _cell_volume 388.01(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 498 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.53 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 6.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2559 _exptl_absorpt_correction_T_max 0.4656 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5491 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_unetI/netI 0.0158 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1364 _reflns_number_gt 1337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, the command 'omit -3 50' was used to omit the reflections above 50 degree. ; _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^)+(0.0275P)^2^+0.2865P] 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 1364 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0491 _refine_ls_wR_factor_gt 0.0488 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _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 0.31470(3) 0.62625(3) 0.380908(18) 0.01426(10) Uani 1 1 d . . . O5 O -0.0433(3) 0.2629(3) 0.46505(16) 0.0214(4) Uani 1 1 d . . . O1 O 0.4418(3) 0.3218(3) 0.39945(16) 0.0207(4) Uani 1 1 d . . . O2 O 0.4512(3) 0.0132(3) 0.32280(17) 0.0230(4) Uani 1 1 d . . . N1 N 0.2870(3) 0.3688(3) 0.15259(19) 0.0153(4) Uani 1 1 d . . . O3 O 0.0393(3) 0.4078(3) -0.23246(17) 0.0257(4) Uani 1 1 d . . . O4 O 0.2068(3) 0.2124(3) -0.32285(16) 0.0252(4) Uani 1 1 d . . . C6 C 0.4128(4) 0.1739(4) 0.3079(2) 0.0143(4) Uani 1 1 d . . . C4 C 0.2143(4) 0.2580(4) -0.0866(2) 0.0151(4) Uani 1 1 d . . . C3 C 0.2564(4) 0.0799(4) -0.0680(2) 0.0165(5) Uani 1 1 d . . . H3 H 0.2492 -0.0157 -0.1413 0.020 Uiso 1 1 calc R . . C5 C 0.2253(4) 0.3933(4) 0.0280(2) 0.0158(5) Uani 1 1 d . . . H5 H 0.1873 0.5075 0.0168 0.019 Uiso 1 1 calc R . . C1 C 0.3310(4) 0.1963(4) 0.1681(2) 0.0135(4) Uani 1 1 d . . . C7 C 0.1479(4) 0.2974(4) -0.2247(2) 0.0174(5) Uani 1 1 d . . . C2 C 0.3094(4) 0.0463(4) 0.0611(2) 0.0158(5) Uani 1 1 d . . . H2 H 0.3304 -0.0767 0.0760 0.019 Uiso 1 1 calc R . . H5A H 0.0433 0.2574 0.5301 0.024 Uiso 1 1 d R . . H5B H -0.1185 0.1595 0.4014 0.024 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 0.01876(14) 0.01616(14) 0.01141(14) 0.00155(8) -0.00104(8) 0.01138(10) O5 0.0247(9) 0.0242(9) 0.0156(8) 0.0004(6) -0.0022(7) 0.0123(7) O1 0.0309(9) 0.0248(9) 0.0123(8) -0.0012(6) -0.0025(7) 0.0190(7) O2 0.0338(10) 0.0213(9) 0.0199(9) 0.0045(7) -0.0004(7) 0.0179(8) N1 0.0154(9) 0.0176(10) 0.0139(9) 0.0020(7) 0.0000(7) 0.0087(8) O3 0.0324(10) 0.0369(10) 0.0179(9) 0.0020(7) -0.0030(7) 0.0253(9) O4 0.0354(10) 0.0354(10) 0.0136(8) 0.0030(7) 0.0027(7) 0.0239(9) C6 0.0132(10) 0.0175(11) 0.0133(11) 0.0036(8) 0.0023(8) 0.0075(9) C4 0.0107(10) 0.0192(11) 0.0144(11) 0.0026(9) 0.0012(8) 0.0060(9) C3 0.0143(11) 0.0217(12) 0.0142(11) -0.0012(9) 0.0015(9) 0.0093(9) C5 0.0154(11) 0.0183(11) 0.0156(11) 0.0031(9) -0.0002(9) 0.0093(9) C1 0.0112(10) 0.0163(11) 0.0140(11) 0.0025(8) 0.0022(8) 0.0070(8) C7 0.0157(11) 0.0206(11) 0.0140(11) 0.0023(9) -0.0004(9) 0.0069(9) C2 0.0153(10) 0.0183(11) 0.0165(11) 0.0030(9) 0.0018(9) 0.0098(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O2 2.4948(16) 1_565 ? Sr1 O1 2.5371(16) 2_666 ? Sr1 O3 2.5635(17) 2_565 ? Sr1 O1 2.5722(16) . ? Sr1 O5 2.7077(17) 2_566 ? Sr1 O5 2.7259(17) . ? Sr1 N1 2.7260(19) . ? Sr1 O4 2.8662(19) 2_665 ? Sr1 Sr1 4.2566(4) 2_666 ? Sr1 Sr1 4.5044(5) 2_566 ? Sr1 H5A 2.8975 . ? O5 Sr1 2.7077(17) 2_566 ? O5 H5A 0.8493 . ? O5 H5B 0.8529 . ? O1 C6 1.252(3) . ? O1 Sr1 2.5371(16) 2_666 ? O2 C6 1.246(3) . ? O2 Sr1 2.4948(16) 1_545 ? N1 C5 1.334(3) . ? N1 C1 1.348(3) . ? O3 C7 1.244(3) . ? O3 Sr1 2.5635(17) 2_565 ? O4 C7 1.267(3) . ? O4 Sr1 2.8662(18) 2_665 ? C6 C1 1.513(3) . ? C4 C3 1.384(3) . ? C4 C5 1.397(3) . ? C4 C7 1.505(3) . ? C3 C2 1.382(3) . ? C3 H3 0.9300 . ? C5 H5 0.9300 . ? C1 C2 1.381(3) . ? C2 H2 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sr1 O1 103.39(5) 1_565 2_666 ? O2 Sr1 O3 77.59(6) 1_565 2_565 ? O1 Sr1 O3 155.73(6) 2_666 2_565 ? O2 Sr1 O1 143.06(6) 1_565 . ? O1 Sr1 O1 67.16(6) 2_666 . ? O3 Sr1 O1 126.04(6) 2_565 . ? O2 Sr1 O5 81.61(5) 1_565 2_566 ? O1 Sr1 O5 85.21(5) 2_666 2_566 ? O3 Sr1 O5 70.84(5) 2_565 2_566 ? O1 Sr1 O5 130.15(5) . 2_566 ? O2 Sr1 O5 146.03(5) 1_565 . ? O1 Sr1 O5 89.30(5) 2_666 . ? O3 Sr1 O5 78.33(6) 2_565 . ? O1 Sr1 O5 70.90(5) . . ? O5 Sr1 O5 68.01(6) 2_566 . ? O2 Sr1 N1 107.77(6) 1_565 . ? O1 Sr1 N1 126.25(5) 2_666 . ? O3 Sr1 N1 74.72(5) 2_565 . ? O1 Sr1 N1 61.49(5) . . ? O5 Sr1 N1 141.32(5) 2_566 . ? O5 Sr1 N1 88.42(5) . . ? O2 Sr1 O4 73.30(5) 1_565 2_665 ? O1 Sr1 O4 72.52(5) 2_666 2_665 ? O3 Sr1 O4 129.37(5) 2_565 2_665 ? O1 Sr1 O4 69.81(5) . 2_665 ? O5 Sr1 O4 140.99(5) 2_566 2_665 ? O5 Sr1 O4 140.56(5) . 2_665 ? N1 Sr1 O4 75.99(5) . 2_665 ? O2 Sr1 Sr1 128.39(4) 1_565 2_666 ? O1 Sr1 Sr1 33.84(4) 2_666 2_666 ? O3 Sr1 Sr1 154.01(4) 2_565 2_666 ? O1 Sr1 Sr1 33.32(4) . 2_666 ? O5 Sr1 Sr1 109.87(4) 2_566 2_666 ? O5 Sr1 Sr1 78.17(4) . 2_666 ? N1 Sr1 Sr1 93.67(4) . 2_666 ? O4 Sr1 Sr1 67.19(3) 2_665 2_666 ? O2 Sr1 Sr1 114.46(4) 1_565 2_566 ? O1 Sr1 Sr1 86.70(4) 2_666 2_566 ? O3 Sr1 Sr1 71.36(4) 2_565 2_566 ? O1 Sr1 Sr1 100.93(4) . 2_566 ? O5 Sr1 Sr1 34.13(4) 2_566 2_566 ? O5 Sr1 Sr1 33.88(4) . 2_566 ? N1 Sr1 Sr1 116.91(4) . 2_566 ? O4 Sr1 Sr1 159.15(3) 2_665 2_566 ? Sr1 Sr1 Sr1 94.606(8) 2_666 2_566 ? O2 Sr1 H5A 152.8 1_565 . ? O1 Sr1 H5A 72.7 2_666 . ? O3 Sr1 H5A 95.2 2_565 . ? O1 Sr1 H5A 61.5 . . ? O5 Sr1 H5A 71.2 2_566 . ? O5 Sr1 H5A 17.0 . . ? N1 Sr1 H5A 95.2 . . ? O4 Sr1 H5A 127.9 2_665 . ? Sr1 Sr1 H5A 62.2 2_666 . ? Sr1 Sr1 H5A 39.5 2_566 . ? Sr1 O5 Sr1 111.99(6) 2_566 . ? Sr1 O5 H5A 96.0 2_566 . ? Sr1 O5 H5A 93.0 . . ? Sr1 O5 H5B 114.9 2_566 . ? Sr1 O5 H5B 112.9 . . ? H5A O5 H5B 125.4 . . ? C6 O1 Sr1 120.84(14) . 2_666 ? C6 O1 Sr1 125.93(14) . . ? Sr1 O1 Sr1 112.84(6) 2_666 . ? C6 O2 Sr1 150.04(15) . 1_545 ? C5 N1 C1 117.29(19) . . ? C5 N1 Sr1 125.90(15) . . ? C1 N1 Sr1 116.76(14) . . ? C7 O3 Sr1 135.23(15) . 2_565 ? C7 O4 Sr1 122.58(15) . 2_665 ? O2 C6 O1 125.0(2) . . ? O2 C6 C1 117.8(2) . . ? O1 C6 C1 117.19(19) . . ? C3 C4 C5 117.5(2) . . ? C3 C4 C7 121.0(2) . . ? C5 C4 C7 121.4(2) . . ? C2 C3 C4 118.9(2) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? N1 C5 C4 124.1(2) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? N1 C1 C2 122.3(2) . . ? N1 C1 C6 117.64(19) . . ? C2 C1 C6 120.1(2) . . ? O3 C7 O4 126.0(2) . . ? O3 C7 C4 117.6(2) . . ? O4 C7 C4 116.4(2) . . ? C1 C2 C3 119.7(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? 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 O2 Sr1 O5 Sr1 -28.23(12) 1_565 . . 2_566 ? O1 Sr1 O5 Sr1 85.12(6) 2_666 . . 2_566 ? O3 Sr1 O5 Sr1 -73.86(6) 2_565 . . 2_566 ? O1 Sr1 O5 Sr1 151.13(7) . . . 2_566 ? O5 Sr1 O5 Sr1 0.0 2_566 . . 2_566 ? N1 Sr1 O5 Sr1 -148.58(7) . . . 2_566 ? O4 Sr1 O5 Sr1 145.92(6) 2_665 . . 2_566 ? Sr1 Sr1 O5 Sr1 117.33(5) 2_666 . . 2_566 ? O2 Sr1 O1 C6 -90.98(19) 1_565 . . . ? O1 Sr1 O1 C6 -172.8(2) 2_666 . . . ? O3 Sr1 O1 C6 30.7(2) 2_565 . . . ? O5 Sr1 O1 C6 125.47(17) 2_566 . . . ? O5 Sr1 O1 C6 89.62(18) . . . . ? N1 Sr1 O1 C6 -9.29(17) . . . . ? O4 Sr1 O1 C6 -93.91(18) 2_665 . . . ? Sr1 Sr1 O1 C6 -172.8(2) 2_666 . . . ? Sr1 Sr1 O1 C6 105.52(17) 2_566 . . . ? O2 Sr1 O1 Sr1 81.83(10) 1_565 . . 2_666 ? O1 Sr1 O1 Sr1 0.0 2_666 . . 2_666 ? O3 Sr1 O1 Sr1 -156.47(6) 2_565 . . 2_666 ? O5 Sr1 O1 Sr1 -61.72(9) 2_566 . . 2_666 ? O5 Sr1 O1 Sr1 -97.58(7) . . . 2_666 ? N1 Sr1 O1 Sr1 163.52(9) . . . 2_666 ? O4 Sr1 O1 Sr1 78.90(7) 2_665 . . 2_666 ? Sr1 Sr1 O1 Sr1 -81.67(6) 2_566 . . 2_666 ? O2 Sr1 N1 C5 -34.50(18) 1_565 . . . ? O1 Sr1 N1 C5 -156.94(16) 2_666 . . . ? O3 Sr1 N1 C5 36.75(17) 2_565 . . . ? O1 Sr1 N1 C5 -175.86(19) . . . . ? O5 Sr1 N1 C5 64.4(2) 2_566 . . . ? O5 Sr1 N1 C5 115.08(17) . . . . ? O4 Sr1 N1 C5 -101.48(17) 2_665 . . . ? Sr1 Sr1 N1 C5 -166.88(17) 2_666 . . . ? Sr1 Sr1 N1 C5 96.07(17) 2_566 . . . ? O2 Sr1 N1 C1 148.24(14) 1_565 . . . ? O1 Sr1 N1 C1 25.80(17) 2_666 . . . ? O3 Sr1 N1 C1 -140.51(16) 2_565 . . . ? O1 Sr1 N1 C1 6.88(14) . . . . ? O5 Sr1 N1 C1 -112.84(15) 2_566 . . . ? O5 Sr1 N1 C1 -62.18(15) . . . . ? O4 Sr1 N1 C1 81.26(15) 2_665 . . . ? Sr1 Sr1 N1 C1 15.86(14) 2_666 . . . ? Sr1 Sr1 N1 C1 -81.19(15) 2_566 . . . ? Sr1 O2 C6 O1 87.3(4) 1_545 . . . ? Sr1 O2 C6 C1 -94.4(3) 1_545 . . . ? Sr1 O1 C6 O2 16.3(3) 2_666 . . . ? Sr1 O1 C6 O2 -171.45(16) . . . . ? Sr1 O1 C6 C1 -162.07(14) 2_666 . . . ? Sr1 O1 C6 C1 10.2(3) . . . . ? C5 C4 C3 C2 -0.8(3) . . . . ? C7 C4 C3 C2 -177.9(2) . . . . ? C1 N1 C5 C4 -3.0(3) . . . . ? Sr1 N1 C5 C4 179.72(16) . . . . ? C3 C4 C5 N1 4.1(3) . . . . ? C7 C4 C5 N1 -178.8(2) . . . . ? C5 N1 C1 C2 -1.3(3) . . . . ? Sr1 N1 C1 C2 176.19(16) . . . . ? C5 N1 C1 C6 177.00(19) . . . . ? Sr1 N1 C1 C6 -5.5(2) . . . . ? O2 C6 C1 N1 179.24(19) . . . . ? O1 C6 C1 N1 -2.3(3) . . . . ? O2 C6 C1 C2 -2.4(3) . . . . ? O1 C6 C1 C2 176.1(2) . . . . ? Sr1 O3 C7 O4 43.0(4) 2_565 . . . ? Sr1 O3 C7 C4 -136.35(18) 2_565 . . . ? Sr1 O4 C7 O3 110.1(2) 2_665 . . . ? Sr1 O4 C7 C4 -70.6(2) 2_665 . . . ? C3 C4 C7 O3 156.7(2) . . . . ? C5 C4 C7 O3 -20.3(3) . . . . ? C3 C4 C7 O4 -22.7(3) . . . . ? C5 C4 C7 O4 160.2(2) . . . . ? N1 C1 C2 C3 4.5(3) . . . . ? C6 C1 C2 C3 -173.8(2) . . . . ? C4 C3 C2 C1 -3.2(3) . . . . ? 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 O5 H5A O4 0.85 1.89 2.735(2) 173.3 1_556 O5 H5A O3 0.85 2.53 3.057(2) 121.5 1_556 O5 H5B O4 0.85 2.39 3.113(2) 142.7 2 O5 H5B O2 0.85 2.53 3.099(2) 124.7 1_455 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.264 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 764694' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H14 Cu N2 O12 Sr' _chemical_formula_sum 'C14 H14 Cu N2 O12 Sr' _chemical_formula_weight 553.44 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' Cu Cu 0.3201 1.2651 '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' 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 7.4636(15) _cell_length_b 10.502(2) _cell_length_c 11.744(2) _cell_angle_alpha 98.50(3) _cell_angle_beta 94.57(3) _cell_angle_gamma 92.14(3) _cell_volume 906.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7736 _cell_measurement_theta_min 2.428 _cell_measurement_theta_max 28.246 _exptl_crystal_description platy _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 4.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4734 _exptl_absorpt_correction_T_max 0.6795 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17094 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_unetI/netI 0.0208 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.46 _reflns_number_total 4553 _reflns_number_gt 3990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0346P)^2^+0.2773P] 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 4553 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 O1 O -0.1159(2) 0.37753(12) 0.17417(12) 0.0315(3) Uani 1 1 d . . . N1 N 0.0724(2) 0.56339(14) 0.30704(13) 0.0212(3) Uani 1 1 d . . . C1 C 0.0814(2) 0.44649(16) 0.34047(15) 0.0212(3) Uani 1 1 d . . . Cu1 Cu -0.08851(3) 0.55972(2) 0.165581(18) 0.02398(7) Uani 1 1 d . . . Sr2 Sr 0.46613(2) 0.988069(15) 0.318393(14) 0.02275(6) Uani 1 1 d . . . O2 O -0.0396(2) 0.23232(13) 0.28629(14) 0.0380(4) Uani 1 1 d . . . C2 C 0.1861(3) 0.42717(17) 0.43793(16) 0.0249(4) Uani 1 1 d . . . H2 H 0.1902 0.3459 0.4602 0.030 Uiso 1 1 calc R . . N2 N 0.2212(2) 0.45142(14) -0.01139(13) 0.0213(3) Uani 1 1 d . . . O3 O 0.3979(2) 0.86705(12) 0.48396(11) 0.0302(3) Uani 1 1 d . . . C3 C 0.2852(3) 0.53158(17) 0.50196(15) 0.0239(4) Uani 1 1 d . . . H3 H 0.3553 0.5211 0.5687 0.029 Uiso 1 1 calc R . . O4 O 0.4689(2) 0.75739(13) 0.62641(12) 0.0352(3) Uani 1 1 d . . . C4 C 0.2799(2) 0.65187(16) 0.46637(15) 0.0211(3) Uani 1 1 d . . . C5 C 0.1691(2) 0.66379(16) 0.36802(15) 0.0223(4) Uani 1 1 d . . . H5 H 0.1622 0.7441 0.3439 0.027 Uiso 1 1 calc R . . O5 O 0.0359(2) 0.26251(13) -0.14480(12) 0.0326(3) Uani 1 1 d . . . C6 C -0.0322(3) 0.34176(17) 0.26221(16) 0.0243(4) Uani 1 1 d . . . O6 O 0.1325(2) 0.11627(13) -0.03961(13) 0.0411(4) Uani 1 1 d . . . C7 C 0.3912(2) 0.76675(16) 0.53092(15) 0.0220(4) Uani 1 1 d . . . O7 O 0.67322(19) 0.63748(13) 0.27412(12) 0.0309(3) Uani 1 1 d . . . O8 O 0.4625(2) 0.76210(13) 0.21244(13) 0.0362(3) Uani 1 1 d . . . C8 C 0.2407(3) 0.33289(16) 0.01791(15) 0.0227(4) Uani 1 1 d . . . O9 O 0.7896(2) 0.88832(15) 0.37482(13) 0.0388(4) Uani 1 1 d . . . H9A H 0.8857 0.9171 0.3517 0.058 Uiso 1 1 d R . . H9B H 0.7727 0.8119 0.3387 0.058 Uiso 1 1 d R . . C9 C 0.3551(3) 0.31224(18) 0.11057(16) 0.0281(4) Uani 1 1 d . . . H9 H 0.3677 0.2296 0.1287 0.034 Uiso 1 1 calc R . . O10 O 0.6658(2) 1.06912(16) 0.17554(15) 0.0505(5) Uani 1 1 d . . . H10A H 0.7330 1.0170 0.1385 0.076 Uiso 1 1 d R . . H10B H 0.7602 1.1172 0.1973 0.076 Uiso 1 1 d R . . C10 C 0.4509(3) 0.41687(18) 0.17622(16) 0.0259(4) Uani 1 1 d . . . H10 H 0.5311 0.4050 0.2381 0.031 Uiso 1 1 calc R . . O11 O 0.2389(2) 0.98189(18) 0.14249(14) 0.0522(5) Uani 1 1 d . . . H11A H 0.1527 0.9250 0.1349 0.078 Uiso 1 1 d R . . H11B H 0.2156 1.0369 0.0977 0.078 Uiso 1 1 d R . . C11 C 0.4265(2) 0.53945(16) 0.14907(14) 0.0213(3) Uani 1 1 d . . . O12 O 0.1465(2) 1.04353(15) 0.38393(13) 0.0394(4) Uani 1 1 d . . . H12A H 0.1584 1.0631 0.4571 0.059 Uiso 1 1 d R . . H12B H 0.0879 1.1041 0.3602 0.059 Uiso 1 1 d R . . C12 C 0.3088(2) 0.55320(16) 0.05417(15) 0.0211(3) Uani 1 1 d . . . H12 H 0.2907 0.6352 0.0359 0.025 Uiso 1 1 calc R . . C13 C 0.1296(3) 0.22719(18) -0.06020(16) 0.0268(4) Uani 1 1 d . . . C14 C 0.5284(3) 0.65663(17) 0.21783(15) 0.0229(4) 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 O1 0.0362(8) 0.0211(6) 0.0337(7) 0.0022(5) -0.0142(6) -0.0028(6) N1 0.0204(8) 0.0198(7) 0.0224(7) 0.0038(6) -0.0043(6) -0.0009(6) C1 0.0205(9) 0.0189(8) 0.0236(8) 0.0025(6) -0.0002(7) 0.0001(7) Cu1 0.02677(13) 0.01972(11) 0.02340(12) 0.00368(8) -0.00957(9) -0.00224(9) Sr2 0.02850(10) 0.01674(8) 0.02135(9) 0.00191(6) -0.00529(6) -0.00106(6) O2 0.0431(9) 0.0203(6) 0.0476(9) 0.0078(6) -0.0171(7) -0.0057(6) C2 0.0288(10) 0.0185(8) 0.0270(9) 0.0057(7) -0.0031(7) -0.0002(7) N2 0.0220(8) 0.0200(7) 0.0210(7) 0.0028(5) -0.0030(6) -0.0001(6) O3 0.0425(8) 0.0200(6) 0.0268(7) 0.0063(5) -0.0076(6) -0.0063(6) C3 0.0259(10) 0.0228(8) 0.0224(8) 0.0052(7) -0.0050(7) 0.0001(7) O4 0.0503(9) 0.0224(6) 0.0294(7) 0.0054(5) -0.0178(6) -0.0047(6) C4 0.0217(9) 0.0191(8) 0.0211(8) 0.0010(6) -0.0019(7) -0.0003(7) C5 0.0236(9) 0.0173(8) 0.0253(9) 0.0046(6) -0.0029(7) -0.0006(7) O5 0.0376(8) 0.0257(7) 0.0314(7) 0.0060(6) -0.0142(6) -0.0081(6) C6 0.0221(9) 0.0195(8) 0.0293(9) 0.0007(7) -0.0037(7) 0.0004(7) O6 0.0573(10) 0.0221(7) 0.0412(9) 0.0085(6) -0.0153(7) -0.0089(7) C7 0.0244(9) 0.0180(8) 0.0221(8) 0.0008(6) -0.0030(7) -0.0005(7) O7 0.0295(8) 0.0280(7) 0.0317(7) -0.0001(5) -0.0098(6) -0.0004(6) O8 0.0426(9) 0.0208(6) 0.0397(8) -0.0056(6) -0.0123(7) 0.0041(6) C8 0.0245(9) 0.0192(8) 0.0233(8) 0.0024(6) -0.0014(7) -0.0021(7) O9 0.0363(9) 0.0355(8) 0.0395(8) -0.0068(6) -0.0033(7) -0.0008(7) C9 0.0354(11) 0.0209(8) 0.0271(9) 0.0070(7) -0.0072(8) -0.0022(8) O10 0.0537(11) 0.0406(9) 0.0543(10) -0.0054(8) 0.0184(9) -0.0156(8) C10 0.0295(10) 0.0243(9) 0.0226(9) 0.0045(7) -0.0065(7) -0.0008(7) O11 0.0538(11) 0.0564(11) 0.0444(9) 0.0226(8) -0.0236(8) -0.0214(9) C11 0.0231(9) 0.0205(8) 0.0187(8) -0.0005(6) 0.0003(7) -0.0008(7) O12 0.0425(9) 0.0410(8) 0.0359(8) 0.0102(7) -0.0017(7) 0.0135(7) C12 0.0227(9) 0.0173(7) 0.0228(8) 0.0019(6) -0.0003(7) 0.0018(7) C13 0.0301(10) 0.0224(8) 0.0259(9) 0.0027(7) -0.0043(8) -0.0056(7) C14 0.0270(10) 0.0212(8) 0.0185(8) -0.0012(6) -0.0001(7) -0.0021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C6 1.277(2) . ? O1 Cu1 1.9350(14) . ? N1 C5 1.336(2) . ? N1 C1 1.346(2) . ? N1 Cu1 1.9654(16) . ? C1 C2 1.378(2) . ? C1 C6 1.510(2) . ? Cu1 O5 1.9479(14) 2_565 ? Cu1 N2 1.9791(16) 2_565 ? Cu1 O7 2.3698(17) 1_455 ? Sr2 O8 2.5095(15) . ? Sr2 O10 2.5469(18) . ? Sr2 O3 2.5485(14) . ? Sr2 O11 2.5579(17) . ? Sr2 O12 2.6244(18) . ? Sr2 O4 2.6725(15) 2_676 ? Sr2 O3 2.6828(16) 2_676 ? Sr2 O9 2.7394(18) . ? Sr2 C7 3.007(2) 2_676 ? Sr2 Sr2 4.2243(8) 2_676 ? O2 C6 1.224(2) . ? C2 C3 1.386(2) . ? C2 H2 0.9300 . ? N2 C12 1.337(2) . ? N2 C8 1.349(2) . ? N2 Cu1 1.9791(15) 2_565 ? O3 C7 1.260(2) . ? O3 Sr2 2.6828(16) 2_676 ? C3 C4 1.389(2) . ? C3 H3 0.9300 . ? O4 C7 1.240(2) . ? O4 Sr2 2.6725(15) 2_676 ? C4 C5 1.390(2) . ? C4 C7 1.508(2) . ? C5 H5 0.9300 . ? O5 C13 1.277(2) . ? O5 Cu1 1.9479(14) 2_565 ? O6 C13 1.225(2) . ? C7 Sr2 3.007(2) 2_676 ? O7 C14 1.260(2) . ? O7 Cu1 2.3698(17) 1_655 ? O8 C14 1.236(2) . ? C8 C9 1.377(3) . ? C8 C13 1.507(2) . ? O9 H9A 0.8478 . ? O9 H9B 0.8507 . ? C9 C10 1.384(3) . ? C9 H9 0.9300 . ? O10 H10A 0.8511 . ? O10 H10B 0.8500 . ? C10 C11 1.386(2) . ? C10 H10 0.9300 . ? O11 H11A 0.8515 . ? O11 H11B 0.8503 . ? C11 C12 1.391(2) . ? C11 C14 1.511(2) . ? O12 H12A 0.8500 . ? O12 H12B 0.8528 . ? C12 H12 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 O1 Cu1 115.08(11) . . ? C5 N1 C1 119.75(15) . . ? C5 N1 Cu1 128.17(12) . . ? C1 N1 Cu1 112.07(12) . . ? N1 C1 C2 121.77(16) . . ? N1 C1 C6 113.94(15) . . ? C2 C1 C6 124.29(15) . . ? O1 Cu1 O5 172.71(7) . 2_565 ? O1 Cu1 N1 83.64(6) . . ? O5 Cu1 N1 96.48(6) 2_565 . ? O1 Cu1 N2 95.39(7) . 2_565 ? O5 Cu1 N2 83.47(6) 2_565 2_565 ? N1 Cu1 N2 172.02(7) . 2_565 ? O1 Cu1 O7 100.15(6) . 1_455 ? O5 Cu1 O7 87.14(6) 2_565 1_455 ? N1 Cu1 O7 91.41(6) . 1_455 ? N2 Cu1 O7 96.55(6) 2_565 1_455 ? O8 Sr2 O10 91.14(6) . . ? O8 Sr2 O3 81.31(5) . . ? O10 Sr2 O3 154.83(6) . . ? O8 Sr2 O11 74.55(6) . . ? O10 Sr2 O11 79.37(6) . . ? O3 Sr2 O11 120.85(5) . . ? O8 Sr2 O12 110.85(6) . . ? O10 Sr2 O12 134.33(6) . . ? O3 Sr2 O12 70.38(5) . . ? O11 Sr2 O12 69.54(6) . . ? O8 Sr2 O4 161.21(5) . 2_676 ? O10 Sr2 O4 70.11(6) . 2_676 ? O3 Sr2 O4 116.18(5) . 2_676 ? O11 Sr2 O4 99.90(6) . 2_676 ? O12 Sr2 O4 82.96(6) . 2_676 ? O8 Sr2 O3 141.04(5) . 2_676 ? O10 Sr2 O3 100.62(5) . 2_676 ? O3 Sr2 O3 72.32(5) . 2_676 ? O11 Sr2 O3 143.95(6) . 2_676 ? O12 Sr2 O3 86.97(6) . 2_676 ? O4 Sr2 O3 48.72(4) 2_676 2_676 ? O8 Sr2 O9 72.30(5) . . ? O10 Sr2 O9 77.77(6) . . ? O3 Sr2 O9 77.05(5) . . ? O11 Sr2 O9 138.94(6) . . ? O12 Sr2 O9 146.08(5) . . ? O4 Sr2 O9 103.70(5) 2_676 . ? O3 Sr2 O9 74.16(5) 2_676 . ? O8 Sr2 C7 158.90(5) . 2_676 ? O10 Sr2 C7 82.65(6) . 2_676 ? O3 Sr2 C7 95.80(5) . 2_676 ? O11 Sr2 C7 123.50(6) . 2_676 ? O12 Sr2 C7 87.43(6) . 2_676 ? O4 Sr2 C7 24.31(4) 2_676 2_676 ? O3 Sr2 C7 24.76(4) 2_676 2_676 ? O9 Sr2 C7 86.66(5) . 2_676 ? O8 Sr2 Sr2 113.75(4) . 2_676 ? O10 Sr2 Sr2 131.53(5) . 2_676 ? O3 Sr2 Sr2 37.24(3) . 2_676 ? O11 Sr2 Sr2 145.37(5) . 2_676 ? O12 Sr2 Sr2 76.34(4) . 2_676 ? O4 Sr2 Sr2 81.21(4) 2_676 2_676 ? O3 Sr2 Sr2 35.09(3) 2_676 2_676 ? O9 Sr2 Sr2 72.03(4) . 2_676 ? C7 Sr2 Sr2 58.95(4) 2_676 2_676 ? C1 C2 C3 118.53(16) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C12 N2 C8 119.40(15) . . ? C12 N2 Cu1 129.14(12) . 2_565 ? C8 N2 Cu1 110.74(12) . 2_565 ? C7 O3 Sr2 152.56(13) . . ? C7 O3 Sr2 92.18(10) . 2_676 ? Sr2 O3 Sr2 107.68(5) . 2_676 ? C2 C3 C4 119.98(16) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C7 O4 Sr2 93.15(11) . 2_676 ? C3 C4 C5 117.98(16) . . ? C3 C4 C7 121.66(16) . . ? C5 C4 C7 120.37(15) . . ? N1 C5 C4 121.97(16) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C13 O5 Cu1 113.92(12) . 2_565 ? O2 C6 O1 125.06(17) . . ? O2 C6 C1 119.76(16) . . ? O1 C6 C1 115.18(15) . . ? O4 C7 O3 124.16(16) . . ? O4 C7 C4 118.49(15) . . ? O3 C7 C4 117.35(15) . . ? O4 C7 Sr2 62.54(10) . 2_676 ? O3 C7 Sr2 63.06(9) . 2_676 ? C4 C7 Sr2 166.97(13) . 2_676 ? C14 O7 Cu1 116.85(12) . 1_655 ? C14 O8 Sr2 142.04(12) . . ? N2 C8 C9 121.99(16) . . ? N2 C8 C13 114.23(15) . . ? C9 C8 C13 123.77(16) . . ? Sr2 O9 H9A 120.5 . . ? Sr2 O9 H9B 100.5 . . ? H9A O9 H9B 105.0 . . ? C8 C9 C10 118.71(17) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? Sr2 O10 H10A 119.3 . . ? Sr2 O10 H10B 122.3 . . ? H10A O10 H10B 87.0 . . ? C9 C10 C11 119.53(17) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? Sr2 O11 H11A 116.6 . . ? Sr2 O11 H11B 131.8 . . ? H11A O11 H11B 109.7 . . ? C10 C11 C12 118.66(16) . . ? C10 C11 C14 121.53(16) . . ? C12 C11 C14 119.78(16) . . ? Sr2 O12 H12A 106.8 . . ? Sr2 O12 H12B 122.1 . . ? H12A O12 H12B 104.9 . . ? N2 C12 C11 121.62(16) . . ? N2 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? O6 C13 O5 124.56(17) . . ? O6 C13 C8 119.81(17) . . ? O5 C13 C8 115.63(16) . . ? O8 C14 O7 126.32(17) . . ? O8 C14 C11 116.87(16) . . ? O7 C14 C11 116.80(16) . . ? 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 O9 H9A O12 0.85 2.29 3.056(2) 150.9 1_655 O9 H9B O7 0.85 1.97 2.799(2) 164.9 . O12 H12A O9 0.85 1.97 2.816(2) 174.6 2_676 O12 H12B O2 0.85 1.94 2.793(2) 172.7 1_565 O10 H10A O6 0.85 2.03 2.879(3) 173.5 2_665 O10 H10B O2 0.85 2.01 2.840(2) 166.2 1_665 O11 H11A O6 0.85 2.32 3.015(2) 139.1 2_565 O11 H11A O5 0.85 2.40 3.230(2) 164.9 2_565 O11 H11B O6 0.85 1.99 2.811(2) 162.2 1_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.458 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 762291' ####################################################################### # # 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 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C14 H18 Co N2 O14 Sr), H2 O' _chemical_formula_sum 'C28 H38 Co2 N4 O29 Sr2' _chemical_formula_weight 1187.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' 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 7.3083(5) _cell_length_b 12.0765(9) _cell_length_c 13.4566(9) _cell_angle_alpha 112.8180(10) _cell_angle_beta 95.8900(10) _cell_angle_gamma 103.9090(10) _cell_volume 1036.85(13) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3226 _cell_measurement_theta_min 2.941 _cell_measurement_theta_max 27.853 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 3.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3780 _exptl_absorpt_correction_T_max 0.4449 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6379 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_unetI/netI 0.0299 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.42 _reflns_number_total 4240 _reflns_number_gt 3566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, the command 'dfix' was used to restrain the bonds of Sr1 H9C, Sr1 H9D, Sr1 H10A, Sr1 H1OB, Sr1 H11C, Sr1 H11D, Sr1 h11a, Sr1 H11B, O9 H9A, O9 H9B, O9B H9C, O9 H9D, O10 H10A, O10 H10B, O11 H11A, O11 H11B, O11 H11B, O11B H11C and O11B H11D. 'Dang' was used to restain the distance and angle of h9a h9b, h9c h9d, h10a h10b, h11a h11b and h11c h11d. Thermal motion of O9 O9B, o11, o11b, o15 o15b are restrained by commond 'SIMU'. ; _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^)+(0.0270P)^2^+0.9000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4240 _refine_ls_number_parameters 375 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.017 _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 0.30698(4) 0.25902(2) 0.573984(19) 0.02879(8) Uani 1 1 d D . . Co1 Co 0.33170(5) 0.16819(3) 0.21187(3) 0.02127(9) Uani 1 1 d . . . O1 O 0.4068(3) 0.36389(17) 0.29223(14) 0.0317(4) Uani 1 1 d . A . O2 O 0.4554(3) 0.54027(17) 0.26765(16) 0.0426(6) Uani 1 1 d . . . O3 O 0.2668(4) 0.15728(19) -0.29801(16) 0.0449(6) Uani 1 1 d . . . O4 O 0.2050(3) -0.00921(17) -0.26027(14) 0.0307(4) Uani 1 1 d . A . O5 O 0.3160(3) 0.14904(17) 0.35761(14) 0.0300(4) Uani 1 1 d . A . O6 O 0.2805(4) 0.01776(19) 0.43611(16) 0.0435(6) Uani 1 1 d . A . O7 O 0.1502(4) -0.45502(18) -0.09992(16) 0.0464(6) Uani 1 1 d . A . O8 O 0.1184(3) -0.31445(18) -0.16304(15) 0.0369(5) Uani 1 1 d . A . O9 O 0.222(2) 0.3912(11) 0.4727(8) 0.050(2) Uani 0.470(16) 1 d PDU A 1 H9A H 0.206(14) 0.461(4) 0.490(5) 0.074 Uiso 0.470(16) 1 d PD A 1 H9B H 0.193(13) 0.345(6) 0.4062(18) 0.074 Uiso 0.470(16) 1 d PD A 1 O9B O 0.3267(18) 0.4272(7) 0.4998(6) 0.048(2) Uani 0.530(16) 1 d PDU A 2 H9C H 0.397(8) 0.4978(18) 0.544(2) 0.072 Uiso 0.530(16) 1 d PD A 2 H9D H 0.341(10) 0.405(3) 0.436(2) 0.072 Uiso 0.530(16) 1 d PD A 2 O10 O 0.0976(5) 0.3912(3) 0.6812(2) 0.0690(8) Uani 1 1 d D A . H10A H 0.135(5) 0.422(3) 0.7484(8) 0.083 Uiso 1 1 d D . . H10B H 0.081(6) 0.440(3) 0.655(2) 0.083 Uiso 1 1 d D . . O11 O 0.674(3) 0.2905(16) 0.5448(17) 0.069(4) Uani 0.470(16) 1 d PDU A 1 H11A H 0.674(5) 0.218(2) 0.510(7) 0.104 Uiso 0.470(16) 1 d PD A 1 H11B H 0.684(6) 0.334(8) 0.510(7) 0.104 Uiso 0.470(16) 1 d PD A 1 O11B O 0.650(2) 0.2669(17) 0.5645(14) 0.072(3) Uani 0.530(16) 1 d PDU A 2 H11C H 0.680(4) 0.202(3) 0.552(7) 0.109 Uiso 0.530(16) 1 d PD A 2 H11D H 0.737(3) 0.333(3) 0.601(7) 0.109 Uiso 0.530(16) 1 d PD A 2 O12 O -0.0606(4) 0.1394(2) 0.48626(16) 0.0452(6) Uani 1 1 d D A . H12A H -0.089(5) 0.103(3) 0.4186(8) 0.068 Uiso 1 1 d D . . H12B H -0.106(5) 0.096(3) 0.517(2) 0.068 Uiso 1 1 d D . . O13 O 0.0410(3) 0.1441(2) 0.17849(19) 0.0363(5) Uani 1 1 d D A . H13C H -0.024(4) 0.099(3) 0.203(3) 0.055 Uiso 1 1 d D . . H13D H -0.001(4) 0.200(2) 0.174(3) 0.055 Uiso 1 1 d D . . O14 O 0.6153(3) 0.1716(3) 0.2241(3) 0.0628(8) Uani 1 1 d D A . H14C H 0.655(5) 0.124(3) 0.243(4) 0.094 Uiso 1 1 d D . . H14D H 0.693(4) 0.224(3) 0.213(4) 0.094 Uiso 1 1 d D . . N1 N 0.3416(3) 0.22181(19) 0.07681(16) 0.0221(4) Uani 1 1 d . A . N2 N 0.2598(3) -0.03272(19) 0.15745(16) 0.0235(5) Uani 1 1 d . A . C1 C 0.3636(4) 0.3455(2) 0.1098(2) 0.0225(5) Uani 1 1 d . . . C2 C 0.3451(4) 0.3973(2) 0.0360(2) 0.0304(6) Uani 1 1 d . A . H2 H 0.3572 0.4827 0.0612 0.036 Uiso 1 1 calc R . . C3 C 0.3084(4) 0.3212(3) -0.0760(2) 0.0300(6) Uani 1 1 d . . . H3 H 0.2963 0.3549 -0.1270 0.036 Uiso 1 1 calc R A . C4 C 0.2898(4) 0.1943(2) -0.1112(2) 0.0226(5) Uani 1 1 d . A . C5 C 0.3053(4) 0.1493(2) -0.0313(2) 0.0242(5) Uani 1 1 d . . . H5 H 0.2895 0.0637 -0.0545 0.029 Uiso 1 1 calc R A . C6 C 0.4116(4) 0.4244(2) 0.2334(2) 0.0269(6) Uani 1 1 d . A . C7 C 0.2520(4) 0.1081(2) -0.2329(2) 0.0256(6) Uani 1 1 d . . . C8 C 0.2510(4) -0.0676(2) 0.2410(2) 0.0237(5) Uani 1 1 d . . . C9 C 0.2108(5) -0.1914(3) 0.2246(2) 0.0337(7) Uani 1 1 d . A . H9 H 0.2067 -0.2124 0.2841 0.040 Uiso 1 1 calc R . . C10 C 0.1765(4) -0.2843(3) 0.1184(2) 0.0329(7) Uani 1 1 d . . . H10 H 0.1495 -0.3686 0.1057 0.040 Uiso 1 1 calc R A . C11 C 0.1828(4) -0.2508(2) 0.0314(2) 0.0234(5) Uani 1 1 d . A . C12 C 0.2248(4) -0.1241(2) 0.0554(2) 0.0261(6) Uani 1 1 d . . . H12 H 0.2291 -0.1011 -0.0030 0.031 Uiso 1 1 calc R A . C13 C 0.2852(4) 0.0397(2) 0.3538(2) 0.0268(6) Uani 1 1 d . A . C14 C 0.1468(4) -0.3492(2) -0.0866(2) 0.0263(6) Uani 1 1 d . . . O15 O 0.111(2) 0.6022(11) 0.5863(9) 0.108(4) Uani 0.331(7) 1 d PU B 1 H15A H 0.0053 0.5524 0.5494 0.162 Uiso 0.331(7) 1 d PR B 1 H15B H 0.1971 0.6394 0.5656 0.162 Uiso 0.331(7) 1 d PR B 1 O15B O -0.030(3) 0.529(2) 0.6081(16) 0.085(5) Uani 0.169(7) 1 d PU B 2 H15C H -0.0793 0.5588 0.5710 0.128 Uiso 0.169(7) 1 d PR B 2 H15D H 0.0499 0.5945 0.6540 0.128 Uiso 0.169(7) 1 d PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.04878(18) 0.01864(13) 0.01414(12) 0.00584(10) 0.00546(11) 0.00458(11) Co1 0.0297(2) 0.01849(17) 0.01588(17) 0.00764(14) 0.00524(14) 0.00724(14) O1 0.0519(13) 0.0214(9) 0.0163(9) 0.0064(8) 0.0051(8) 0.0054(9) O2 0.0720(16) 0.0160(10) 0.0256(10) 0.0037(8) 0.0017(10) 0.0012(10) O3 0.0813(17) 0.0311(11) 0.0211(10) 0.0161(9) 0.0111(10) 0.0068(11) O4 0.0473(12) 0.0215(9) 0.0196(9) 0.0077(8) 0.0059(8) 0.0062(9) O5 0.0490(12) 0.0207(9) 0.0169(9) 0.0064(8) 0.0060(8) 0.0079(9) O6 0.0796(17) 0.0304(11) 0.0196(10) 0.0126(9) 0.0128(10) 0.0113(11) O7 0.0910(18) 0.0229(10) 0.0279(11) 0.0087(9) 0.0139(11) 0.0253(11) O8 0.0604(14) 0.0281(10) 0.0233(10) 0.0110(8) 0.0069(9) 0.0165(10) O9 0.082(6) 0.047(5) 0.036(4) 0.023(3) 0.023(4) 0.035(4) O9B 0.081(6) 0.030(3) 0.030(3) 0.013(2) 0.014(3) 0.012(3) O10 0.084(2) 0.0647(18) 0.0316(13) -0.0034(12) 0.0161(14) 0.0158(16) O11 0.061(5) 0.060(5) 0.070(8) 0.022(4) 0.008(4) 0.001(4) O11B 0.053(5) 0.105(8) 0.047(5) 0.012(5) 0.006(3) 0.040(6) O12 0.0631(15) 0.0365(12) 0.0207(10) 0.0077(9) 0.0049(10) -0.0019(11) O13 0.0318(11) 0.0400(12) 0.0534(13) 0.0330(11) 0.0138(10) 0.0148(10) O14 0.0373(13) 0.0761(19) 0.122(2) 0.0807(19) 0.0305(15) 0.0272(13) N1 0.0304(12) 0.0188(10) 0.0179(10) 0.0093(9) 0.0053(9) 0.0066(9) N2 0.0346(12) 0.0194(10) 0.0169(10) 0.0073(9) 0.0064(9) 0.0094(9) C1 0.0264(13) 0.0189(12) 0.0197(12) 0.0077(10) 0.0051(10) 0.0032(10) C2 0.0462(17) 0.0169(13) 0.0268(14) 0.0104(11) 0.0059(12) 0.0068(12) C3 0.0452(17) 0.0248(14) 0.0222(13) 0.0143(11) 0.0058(12) 0.0080(12) C4 0.0276(14) 0.0231(13) 0.0174(12) 0.0098(10) 0.0053(10) 0.0059(11) C5 0.0355(15) 0.0180(12) 0.0188(12) 0.0082(10) 0.0064(11) 0.0068(11) C6 0.0322(15) 0.0195(13) 0.0211(13) 0.0050(11) 0.0019(11) 0.0022(11) C7 0.0322(15) 0.0242(13) 0.0192(12) 0.0092(11) 0.0054(11) 0.0065(11) C8 0.0305(14) 0.0216(13) 0.0196(12) 0.0092(11) 0.0056(11) 0.0082(11) C9 0.0554(19) 0.0263(14) 0.0246(14) 0.0154(12) 0.0118(13) 0.0126(13) C10 0.0528(19) 0.0179(13) 0.0294(14) 0.0110(12) 0.0110(13) 0.0106(13) C11 0.0291(14) 0.0187(12) 0.0212(12) 0.0072(10) 0.0065(11) 0.0073(11) C12 0.0382(15) 0.0230(13) 0.0183(12) 0.0099(11) 0.0069(11) 0.0097(12) C13 0.0362(15) 0.0240(13) 0.0193(13) 0.0091(11) 0.0067(11) 0.0078(12) C14 0.0336(15) 0.0213(13) 0.0232(13) 0.0083(11) 0.0085(11) 0.0082(11) O15 0.125(7) 0.086(6) 0.108(6) 0.017(5) -0.003(5) 0.074(5) O15B 0.098(8) 0.081(7) 0.085(7) 0.023(6) -0.005(6) 0.071(6) _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 2.4768(18) 1_556 ? Sr1 O11B 2.508(15) . ? Sr1 O9B 2.571(7) . ? Sr1 O2 2.5775(19) 2_666 ? Sr1 O9 2.604(7) . ? Sr1 O10 2.610(3) . ? Sr1 O12 2.619(2) . ? Sr1 O11 2.706(19) . ? Sr1 O5 2.7071(17) . ? Sr1 O6 2.726(2) . ? Sr1 C13 3.072(3) . ? Sr1 H9B 2.96(6) . ? Co1 O13 2.051(2) . ? Co1 O14 2.051(2) . ? Co1 O5 2.0731(17) . ? Co1 O1 2.0806(18) . ? Co1 N2 2.151(2) . ? Co1 N1 2.155(2) . ? O1 C6 1.266(3) . ? O2 C6 1.236(3) . ? O2 Sr1 2.5775(19) 2_666 ? O3 C7 1.235(3) . ? O3 Sr1 2.4768(18) 1_554 ? O4 C7 1.263(3) . ? O5 C13 1.265(3) . ? O6 C13 1.236(3) . ? O7 C14 1.227(3) . ? O8 C14 1.268(3) . ? O9 H9A 0.822(10) . ? O9 H9B 0.821(10) . ? O9 H9D 1.05(5) . ? O9B H9A 1.07(7) . ? O9B H9B 1.36(5) . ? O9B H9C 0.822(10) . ? O9B H9D 0.823(10) . ? O10 H10A 0.819(10) . ? O10 H10B 0.816(10) . ? O11 H11A 0.821(10) . ? O11 H11B 0.824(10) . ? O11 H11C 1.12(5) . ? O11 H11D 0.76(8) . ? O11B H11A 0.81(5) . ? O11B H11B 1.29(3) . ? O11B H11C 0.821(10) . ? O11B H11D 0.821(10) . ? O12 H12A 0.820(10) . ? O12 H12B 0.823(10) . ? O13 H13C 0.821(10) . ? O13 H13D 0.823(10) . ? O14 H14C 0.812(10) . ? O14 H14D 0.813(10) . ? N1 C5 1.333(3) . ? N1 C1 1.346(3) . ? N2 C12 1.337(3) . ? N2 C8 1.347(3) . ? C1 C2 1.374(3) . ? C1 C6 1.513(3) . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C3 C4 1.384(4) . ? C3 H3 0.9300 . ? C4 C5 1.386(3) . ? C4 C7 1.513(3) . ? C5 H5 0.9300 . ? C8 C9 1.375(4) . ? C8 C13 1.512(3) . ? C9 C10 1.383(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 C12 1.382(3) . ? C11 C14 1.517(3) . ? C12 H12 0.9300 . ? O15 H15A 0.8200 . ? O15 H15B 0.8201 . ? O15 H15C 1.3268 . ? O15 H15D 1.0805 . ? O15B H15A 0.9745 . ? O15B H15C 0.8201 . ? O15B H15D 0.8201 . ? 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 O11B 98.3(4) 1_556 . ? O3 Sr1 O9B 159.44(16) 1_556 . ? O11B Sr1 O9B 91.3(4) . . ? O3 Sr1 O2 89.82(7) 1_556 2_666 ? O11B Sr1 O2 68.9(4) . 2_666 ? O9B Sr1 O2 76.7(2) . 2_666 ? O3 Sr1 O9 155.0(2) 1_556 . ? O11B Sr1 O9 105.1(4) . . ? O9B Sr1 O9 16.67(17) . . ? O2 Sr1 O9 90.6(3) 2_666 . ? O3 Sr1 O10 84.94(9) 1_556 . ? O11B Sr1 O10 142.1(4) . . ? O9B Sr1 O10 76.4(2) . . ? O2 Sr1 O10 73.47(8) 2_666 . ? O9 Sr1 O10 71.29(19) . . ? O3 Sr1 O12 85.78(7) 1_556 . ? O11B Sr1 O12 147.8(4) . . ? O9B Sr1 O12 95.7(3) . . ? O2 Sr1 O12 143.32(8) 2_666 . ? O9 Sr1 O12 79.0(3) . . ? O10 Sr1 O12 69.87(8) . . ? O3 Sr1 O11 107.7(4) 1_556 . ? O11B Sr1 O11 9.5(7) . . ? O9B Sr1 O11 82.0(4) . . ? O2 Sr1 O11 68.5(4) 2_666 . ? O9 Sr1 O11 95.6(4) . . ? O10 Sr1 O11 139.6(4) . . ? O12 Sr1 O11 146.9(4) . . ? O3 Sr1 O5 127.45(6) 1_556 . ? O11B Sr1 O5 72.8(4) . . ? O9B Sr1 O5 72.76(15) . . ? O2 Sr1 O5 129.67(6) 2_666 . ? O9 Sr1 O5 69.14(19) . . ? O10 Sr1 O5 133.44(8) . . ? O12 Sr1 O5 79.36(6) . . ? O11 Sr1 O5 68.4(4) . . ? O3 Sr1 O6 79.61(6) 1_556 . ? O11B Sr1 O6 76.2(4) . . ? O9B Sr1 O6 120.51(16) . . ? O2 Sr1 O6 141.49(8) 2_666 . ? O9 Sr1 O6 114.1(2) . . ? O10 Sr1 O6 140.79(8) . . ? O12 Sr1 O6 73.21(8) . . ? O11 Sr1 O6 79.6(4) . . ? O5 Sr1 O6 47.85(5) . . ? O3 Sr1 C13 103.21(7) 1_556 . ? O11B Sr1 C13 74.4(4) . . ? O9B Sr1 C13 96.85(16) . . ? O2 Sr1 C13 142.44(8) 2_666 . ? O9 Sr1 C13 91.5(2) . . ? O10 Sr1 C13 141.80(8) . . ? O12 Sr1 C13 73.56(7) . . ? O11 Sr1 C13 74.0(4) . . ? O5 Sr1 C13 24.26(6) . . ? O6 Sr1 C13 23.67(6) . . ? O3 Sr1 H9B 158.0(19) 1_556 . ? O11B Sr1 H9B 102.6(19) . . ? O9B Sr1 H9B 27.3(13) . . ? O2 Sr1 H9B 104.0(12) 2_666 . ? O9 Sr1 H9B 15.4(7) . . ? O10 Sr1 H9B 82.8(13) . . ? O12 Sr1 H9B 72.9(18) . . ? O11 Sr1 H9B 93.4(19) . . ? O5 Sr1 H9B 54.6(9) . . ? O6 Sr1 H9B 98.7(7) . . ? C13 Sr1 H9B 76.3(8) . . ? O13 Co1 O14 172.00(12) . . ? O13 Co1 O5 91.25(8) . . ? O14 Co1 O5 93.25(10) . . ? O13 Co1 O1 94.03(8) . . ? O14 Co1 O1 92.37(10) . . ? O5 Co1 O1 92.54(7) . . ? O13 Co1 N2 87.57(8) . . ? O14 Co1 N2 86.95(10) . . ? O5 Co1 N2 77.50(7) . . ? O1 Co1 N2 169.95(7) . . ? O13 Co1 N1 85.79(8) . . ? O14 Co1 N1 90.92(9) . . ? O5 Co1 N1 169.40(8) . . ? O1 Co1 N1 77.55(7) . . ? N2 Co1 N1 112.48(8) . . ? C6 O1 Co1 117.93(16) . . ? C6 O2 Sr1 139.35(19) . 2_666 ? C7 O3 Sr1 178.3(2) . 1_554 ? C13 O5 Co1 117.89(16) . . ? C13 O5 Sr1 94.23(15) . . ? Co1 O5 Sr1 147.67(8) . . ? C13 O6 Sr1 94.05(16) . . ? Sr1 O9 H9A 137(5) . . ? Sr1 O9 H9B 107(5) . . ? H9A O9 H9B 115(2) . . ? Sr1 O9 H9D 102(2) . . ? H9A O9 H9D 99(7) . . ? H9B O9 H9D 69(7) . . ? Sr1 O9B H9A 121(4) . . ? Sr1 O9B H9B 92(3) . . ? H9A O9B H9B 69(3) . . ? Sr1 O9B H9C 113.6(19) . . ? H9A O9B H9C 93(5) . . ? H9B O9B H9C 154(4) . . ? Sr1 O9B H9D 114.9(19) . . ? H9A O9B H9D 97(6) . . ? H9B O9B H9D 53(5) . . ? H9C O9B H9D 115(2) . . ? Sr1 O10 H10A 113.3(17) . . ? Sr1 O10 H10B 110.1(16) . . ? H10A O10 H10B 116.0(18) . . ? Sr1 O11 H11A 103(2) . . ? Sr1 O11 H11B 103(2) . . ? H11A O11 H11B 115(2) . . ? Sr1 O11 H11C 92.8(18) . . ? H11A O11 H11C 36(7) . . ? H11B O11 H11C 151(7) . . ? Sr1 O11 H11D 105(4) . . ? H11A O11 H11D 123(8) . . ? H11B O11 H11D 105(8) . . ? H11C O11 H11D 93(5) . . ? Sr1 O11B H11A 120(4) . . ? Sr1 O11B H11B 99.8(16) . . ? H11A O11B H11B 79(3) . . ? Sr1 O11B H11C 118(2) . . ? H11A O11B H11C 48(9) . . ? H11B O11B H11C 125(7) . . ? Sr1 O11B H11D 119(2) . . ? H11A O11B H11D 116(5) . . ? H11B O11B H11D 69(8) . . ? H11C O11B H11D 116(2) . . ? Sr1 O12 H12A 115(3) . . ? Sr1 O12 H12B 111(3) . . ? H12A O12 H12B 114.8(19) . . ? Co1 O13 H13C 115(2) . . ? Co1 O13 H13D 122(2) . . ? H13C O13 H13D 115.5(18) . . ? Co1 O14 H14C 122(3) . . ? Co1 O14 H14D 120(3) . . ? H14C O14 H14D 118(2) . . ? C5 N1 C1 117.9(2) . . ? C5 N1 Co1 129.44(17) . . ? C1 N1 Co1 112.07(16) . . ? C12 N2 C8 117.4(2) . . ? C12 N2 Co1 129.52(17) . . ? C8 N2 Co1 113.07(16) . . ? N1 C1 C2 122.2(2) . . ? N1 C1 C6 115.7(2) . . ? C2 C1 C6 122.0(2) . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 117.8(2) . . ? C3 C4 C7 120.8(2) . . ? C5 C4 C7 121.5(2) . . ? N1 C5 C4 123.7(2) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? O2 C6 O1 126.2(2) . . ? O2 C6 C1 117.9(2) . . ? O1 C6 C1 115.8(2) . . ? O3 C7 O4 124.9(2) . . ? O3 C7 C4 117.8(2) . . ? O4 C7 C4 117.3(2) . . ? N2 C8 C9 122.5(2) . . ? N2 C8 C13 114.8(2) . . ? C9 C8 C13 122.6(2) . . ? C8 C9 C10 119.1(2) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 119.3(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 117.7(2) . . ? C10 C11 C14 121.4(2) . . ? C12 C11 C14 120.9(2) . . ? N2 C12 C11 123.9(2) . . ? N2 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? O6 C13 O5 123.5(2) . . ? O6 C13 C8 120.0(2) . . ? O5 C13 C8 116.6(2) . . ? O6 C13 Sr1 62.29(14) . . ? O5 C13 Sr1 61.52(13) . . ? C8 C13 Sr1 173.19(19) . . ? O7 C14 O8 125.5(2) . . ? O7 C14 C11 117.3(2) . . ? O8 C14 C11 117.2(2) . . ? H15A O15 H15B 127.7 . . ? H15A O15 H15C 28.2 . . ? H15B O15 H15C 143.1 . . ? H15A O15 H15D 82.9 . . ? H15B O15 H15D 148.5 . . ? H15C O15 H15D 61.1 . . ? H15A O15B H15C 46.2 . . ? H15A O15B H15D 89.9 . . ? H15C O15B H15D 98.4 . . ? 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 O13 Co1 O1 C6 -80.0(2) . . . . ? O14 Co1 O1 C6 95.2(2) . . . . ? O5 Co1 O1 C6 -171.5(2) . . . . ? N2 Co1 O1 C6 -178.9(4) . . . . ? N1 Co1 O1 C6 4.7(2) . . . . ? O13 Co1 O5 C13 90.9(2) . . . . ? O14 Co1 O5 C13 -82.5(2) . . . . ? O1 Co1 O5 C13 -175.0(2) . . . . ? N2 Co1 O5 C13 3.7(2) . . . . ? N1 Co1 O5 C13 164.5(4) . . . . ? O13 Co1 O5 Sr1 -81.99(18) . . . . ? O14 Co1 O5 Sr1 104.62(19) . . . . ? O1 Co1 O5 Sr1 12.10(18) . . . . ? N2 Co1 O5 Sr1 -169.23(19) . . . . ? N1 Co1 O5 Sr1 -8.4(6) . . . . ? O3 Sr1 O5 C13 2.7(2) 1_556 . . . ? O11B Sr1 O5 C13 90.1(4) . . . . ? O9B Sr1 O5 C13 -173.0(3) . . . . ? O2 Sr1 O5 C13 131.76(16) 2_666 . . . ? O9 Sr1 O5 C13 -155.7(4) . . . . ? O10 Sr1 O5 C13 -122.20(18) . . . . ? O12 Sr1 O5 C13 -73.51(17) . . . . ? O11 Sr1 O5 C13 99.0(4) . . . . ? O6 Sr1 O5 C13 3.41(16) . . . . ? O3 Sr1 O5 Co1 176.41(16) 1_556 . . . ? O11B Sr1 O5 Co1 -96.2(5) . . . . ? O9B Sr1 O5 Co1 0.7(3) . . . . ? O2 Sr1 O5 Co1 -54.5(2) 2_666 . . . ? O9 Sr1 O5 Co1 18.0(4) . . . . ? O10 Sr1 O5 Co1 51.5(2) . . . . ? O12 Sr1 O5 Co1 100.20(18) . . . . ? O11 Sr1 O5 Co1 -87.3(4) . . . . ? O6 Sr1 O5 Co1 177.1(2) . . . . ? C13 Sr1 O5 Co1 173.7(3) . . . . ? O3 Sr1 O6 C13 175.94(19) 1_556 . . . ? O11B Sr1 O6 C13 -82.7(4) . . . . ? O9B Sr1 O6 C13 0.5(4) . . . . ? O2 Sr1 O6 C13 -107.69(19) 2_666 . . . ? O9 Sr1 O6 C13 17.9(4) . . . . ? O10 Sr1 O6 C13 107.5(2) . . . . ? O12 Sr1 O6 C13 87.25(18) . . . . ? O11 Sr1 O6 C13 -73.7(5) . . . . ? O5 Sr1 O6 C13 -3.49(16) . . . . ? O13 Co1 N1 C5 -83.7(2) . . . . ? O14 Co1 N1 C5 89.0(2) . . . . ? O5 Co1 N1 C5 -157.7(4) . . . . ? O1 Co1 N1 C5 -178.7(2) . . . . ? N2 Co1 N1 C5 2.0(3) . . . . ? O13 Co1 N1 C1 86.91(18) . . . . ? O14 Co1 N1 C1 -100.39(19) . . . . ? O5 Co1 N1 C1 12.9(5) . . . . ? O1 Co1 N1 C1 -8.16(17) . . . . ? N2 Co1 N1 C1 172.53(17) . . . . ? O13 Co1 N2 C12 85.5(2) . . . . ? O14 Co1 N2 C12 -88.7(2) . . . . ? O5 Co1 N2 C12 177.3(2) . . . . ? O1 Co1 N2 C12 -175.1(4) . . . . ? N1 Co1 N2 C12 1.0(3) . . . . ? O13 Co1 N2 C8 -94.89(18) . . . . ? O14 Co1 N2 C8 90.9(2) . . . . ? O5 Co1 N2 C8 -3.07(18) . . . . ? O1 Co1 N2 C8 4.5(6) . . . . ? N1 Co1 N2 C8 -179.31(17) . . . . ? C5 N1 C1 C2 1.6(4) . . . . ? Co1 N1 C1 C2 -170.2(2) . . . . ? C5 N1 C1 C6 -177.9(2) . . . . ? Co1 N1 C1 C6 10.4(3) . . . . ? N1 C1 C2 C3 -1.9(4) . . . . ? C6 C1 C2 C3 177.5(3) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C2 C3 C4 C7 -179.3(3) . . . . ? C1 N1 C5 C4 0.3(4) . . . . ? Co1 N1 C5 C4 170.38(19) . . . . ? C3 C4 C5 N1 -1.7(4) . . . . ? C7 C4 C5 N1 178.9(2) . . . . ? Sr1 O2 C6 O1 37.0(5) 2_666 . . . ? Sr1 O2 C6 C1 -141.3(2) 2_666 . . . ? Co1 O1 C6 O2 -179.1(2) . . . . ? Co1 O1 C6 C1 -0.7(3) . . . . ? N1 C1 C6 O2 171.7(3) . . . . ? C2 C1 C6 O2 -7.8(4) . . . . ? N1 C1 C6 O1 -6.9(4) . . . . ? C2 C1 C6 O1 173.7(3) . . . . ? Sr1 O3 C7 O4 -117(6) 1_554 . . . ? Sr1 O3 C7 C4 64(7) 1_554 . . . ? C3 C4 C7 O3 10.6(4) . . . . ? C5 C4 C7 O3 -170.1(3) . . . . ? C3 C4 C7 O4 -168.6(3) . . . . ? C5 C4 C7 O4 10.8(4) . . . . ? C12 N2 C8 C9 0.9(4) . . . . ? Co1 N2 C8 C9 -178.8(2) . . . . ? C12 N2 C8 C13 -178.0(2) . . . . ? Co1 N2 C8 C13 2.3(3) . . . . ? N2 C8 C9 C10 -0.5(5) . . . . ? C13 C8 C9 C10 178.4(3) . . . . ? C8 C9 C10 C11 -0.2(5) . . . . ? C9 C10 C11 C12 0.4(4) . . . . ? C9 C10 C11 C14 179.8(3) . . . . ? C8 N2 C12 C11 -0.7(4) . . . . ? Co1 N2 C12 C11 178.9(2) . . . . ? C10 C11 C12 N2 0.1(4) . . . . ? C14 C11 C12 N2 -179.4(2) . . . . ? Sr1 O6 C13 O5 6.7(3) . . . . ? Sr1 O6 C13 C8 -172.7(2) . . . . ? Co1 O5 C13 O6 177.1(2) . . . . ? Sr1 O5 C13 O6 -6.7(3) . . . . ? Co1 O5 C13 C8 -3.6(3) . . . . ? Sr1 O5 C13 C8 172.6(2) . . . . ? Co1 O5 C13 Sr1 -176.20(18) . . . . ? N2 C8 C13 O6 -179.9(3) . . . . ? C9 C8 C13 O6 1.1(4) . . . . ? N2 C8 C13 O5 0.7(4) . . . . ? C9 C8 C13 O5 -178.2(3) . . . . ? N2 C8 C13 Sr1 72.6(15) . . . . ? C9 C8 C13 Sr1 -106.3(14) . . . . ? O3 Sr1 C13 O6 -4.11(19) 1_556 . . . ? O11B Sr1 C13 O6 91.0(4) . . . . ? O9B Sr1 C13 O6 -179.5(3) . . . . ? O2 Sr1 C13 O6 103.35(19) 2_666 . . . ? O9 Sr1 C13 O6 -163.7(4) . . . . ? O10 Sr1 C13 O6 -102.8(2) . . . . ? O12 Sr1 C13 O6 -85.59(18) . . . . ? O11 Sr1 C13 O6 100.8(5) . . . . ? O5 Sr1 C13 O6 173.7(3) . . . . ? O3 Sr1 C13 O5 -177.80(16) 1_556 . . . ? O11B Sr1 C13 O5 -82.7(4) . . . . ? O9B Sr1 C13 O5 6.8(3) . . . . ? O2 Sr1 C13 O5 -70.3(2) 2_666 . . . ? O9 Sr1 C13 O5 22.6(3) . . . . ? O10 Sr1 C13 O5 83.5(2) . . . . ? O12 Sr1 C13 O5 100.72(17) . . . . ? O11 Sr1 C13 O5 -72.8(4) . . . . ? O6 Sr1 C13 O5 -173.7(3) . . . . ? O3 Sr1 C13 C8 106.9(15) 1_556 . . . ? O11B Sr1 C13 C8 -158.0(15) . . . . ? O9B Sr1 C13 C8 -68.5(15) . . . . ? O2 Sr1 C13 C8 -145.7(14) 2_666 . . . ? O9 Sr1 C13 C8 -52.7(15) . . . . ? O10 Sr1 C13 C8 8.2(15) . . . . ? O12 Sr1 C13 C8 25.4(15) . . . . ? O11 Sr1 C13 C8 -148.2(15) . . . . ? O5 Sr1 C13 C8 -75.3(15) . . . . ? O6 Sr1 C13 C8 111.0(15) . . . . ? C10 C11 C14 O7 -14.2(4) . . . . ? C12 C11 C14 O7 165.2(3) . . . . ? C10 C11 C14 O8 166.8(3) . . . . ? C12 C11 C14 O8 -13.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O15 0.822(10) 2.03(4) 2.779(12) 152(8) . O9 H9B O1 0.821(10) 2.33(8) 2.844(8) 121(8) . O9B H9C O1 0.822(10) 2.250(19) 3.006(10) 153(2) 2_666 O9B H9D O1 0.823(10) 1.942(16) 2.761(7) 173(7) . O10 H10A O7 0.819(10) 1.977(14) 2.730(3) 153(2) 1_566 O10 H10B O15 0.816(10) 2.45(2) 3.250(14) 167(4) . O10 H10B O15B 0.816(10) 1.75(2) 2.539(17) 161(4) . O11 H11A O12 0.821(10) 2.35(3) 2.94(2) 129(4) 1_655 O11 H11B O15 0.824(10) 2.27(3) 2.94(2) 139(3) 2_666 O11B H11C O12 0.821(10) 2.34(3) 2.949(16) 131(4) 1_655 O11B H11D O15B 0.821(10) 2.52(6) 3.25(3) 148(9) 1_655 O11B H11D O10 0.821(10) 2.55(3) 3.187(16) 135(3) 1_655 O12 H12A O4 0.820(10) 1.959(13) 2.769(3) 169(4) 2 O12 H12B O6 0.823(10) 1.971(15) 2.773(3) 164(4) 2_556 O13 H13C O4 0.821(10) 1.922(12) 2.736(3) 171(3) 2 O13 H13D O8 0.823(10) 1.838(11) 2.659(3) 175(3) 2 O14 H14C O4 0.812(10) 1.975(16) 2.767(3) 165(4) 2_655 O14 H14D O8 0.813(10) 1.893(15) 2.693(3) 167(5) 2_655 O15 H15A O15 0.82 1.95 2.64(2) 141.0 2_566 O15 H15A O9 0.82 1.98 2.514(17) 122.2 2_566 O15 H15B O11 0.82 2.17 2.94(2) 156.8 2_666 O15B H15C O9B 0.82 2.03 2.754(19) 147.0 2_566 O15B H15D O8 0.82 2.21 2.837(19) 132.9 1_566 C12 H12 O8 0.93 2.50 2.821(3) 100.2 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.649 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 943747' ####################################################################### # # 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_t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H14 N2 Ni O12 Sr, 3(H2 O)' _chemical_formula_sum 'C14 H20 N2 Ni O15 Sr' _chemical_formula_weight 602.65 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' Ni Ni 0.3393 1.1124 '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' Sr Sr -1.5307 3.2498 '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 18.324(3) _cell_length_b 13.794(3) _cell_length_c 8.7635(17) _cell_angle_alpha 90.00 _cell_angle_beta 107.405(3) _cell_angle_gamma 90.00 _cell_volume 2113.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3490 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 28.427 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 3.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4203 _exptl_absorpt_correction_T_max 0.4753 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7299 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.49 _reflns_number_total 2665 _reflns_number_gt 2321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0601P)^2^+1.2962P] 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 2665 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Sr1 Sr 0.5000 -0.03835(2) 0.2500 0.02208(11) Uani 1 2 d S . . Ni1 Ni 0.2500 0.2500 0.0000 0.02372(13) Uani 1 2 d S . . O1 O 0.32981(10) 0.14249(14) 0.0693(2) 0.0289(4) Uani 1 1 d . . . O2 O 0.36803(12) 0.02455(15) 0.2484(3) 0.0344(5) Uani 1 1 d . . . O3 O 0.08503(13) 0.20720(19) 0.5736(3) 0.0443(5) Uani 1 1 d . . . O4 O 0.07288(14) 0.32253(18) 0.3961(3) 0.0506(6) Uani 1 1 d . . . O5 O 0.46854(11) -0.09877(14) 0.5328(2) 0.0325(4) Uani 1 1 d . . . H5B H 0.4232 -0.1169 0.5243 0.049 Uiso 1 1 d R . . H5A H 0.4961 -0.1488 0.5361 0.049 Uiso 1 1 d R . . O6 O 0.33059(12) 0.35134(16) 0.1274(3) 0.0369(5) Uani 1 1 d . . . H6B H 0.3564 0.3354 0.2218 0.055 Uiso 1 1 d R . . H6A H 0.3655 0.3609 0.0833 0.055 Uiso 1 1 d R . . N1 N 0.22856(12) 0.20621(15) 0.2033(3) 0.0243(4) Uani 1 1 d . . . C1 C 0.26589(14) 0.12508(18) 0.2649(3) 0.0227(5) Uani 1 1 d . . . C2 C 0.25156(16) 0.0762(2) 0.3897(3) 0.0317(6) Uani 1 1 d . . . H2 H 0.2778 0.0195 0.4297 0.038 Uiso 1 1 calc R . . C3 C 0.19678(17) 0.1135(2) 0.4547(4) 0.0322(6) Uani 1 1 d . . . H3 H 0.1854 0.0813 0.5380 0.039 Uiso 1 1 calc R . . C4 C 0.15940(15) 0.19884(19) 0.3945(3) 0.0251(5) Uani 1 1 d . . . C5 C 0.17722(16) 0.24293(18) 0.2680(3) 0.0256(5) Uani 1 1 d . . . H5 H 0.1524 0.3003 0.2265 0.031 Uiso 1 1 calc R . . C6 C 0.32661(14) 0.09358(18) 0.1903(3) 0.0240(5) Uani 1 1 d . . . C7 C 0.10108(16) 0.2459(2) 0.4599(3) 0.0294(6) Uani 1 1 d . . . O7 O 0.0479(2) 0.1047(3) 0.9855(5) 0.1025(15) Uani 1 1 d . . . H7A H 0.0061 0.1359 0.9654 0.154 Uiso 1 1 d R . . H7B H 0.0627 0.0930 1.0853 0.154 Uiso 1 1 d R . . O8 O 0.0000 -0.0308(4) 0.7500 0.1002(19) Uani 1 2 d S . . H8 H 0.0263 0.0116 0.8178 0.150 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 0.02234(17) 0.02163(18) 0.02593(18) 0.000 0.01278(12) 0.000 Ni1 0.0286(3) 0.0250(2) 0.0242(2) 0.00642(16) 0.01815(19) 0.00768(16) O1 0.0326(9) 0.0307(9) 0.0308(10) 0.0079(7) 0.0209(8) 0.0108(7) O2 0.0328(10) 0.0367(11) 0.0402(11) 0.0115(8) 0.0207(9) 0.0153(8) O3 0.0441(12) 0.0674(15) 0.0319(11) 0.0086(10) 0.0274(9) 0.0074(11) O4 0.0593(15) 0.0518(14) 0.0538(14) 0.0148(11) 0.0367(12) 0.0311(12) O5 0.0294(9) 0.0308(10) 0.0440(11) -0.0070(9) 0.0213(8) -0.0027(8) O6 0.0381(11) 0.0407(12) 0.0363(11) 0.0043(9) 0.0180(9) 0.0004(9) N1 0.0295(10) 0.0245(10) 0.0251(10) 0.0042(8) 0.0177(8) 0.0057(8) C1 0.0243(11) 0.0231(12) 0.0239(12) 0.0021(9) 0.0119(9) 0.0054(9) C2 0.0403(15) 0.0261(13) 0.0369(15) 0.0122(11) 0.0239(12) 0.0115(11) C3 0.0395(15) 0.0327(14) 0.0336(14) 0.0126(11) 0.0250(12) 0.0094(11) C4 0.0288(12) 0.0279(13) 0.0248(12) 0.0019(10) 0.0174(10) 0.0042(9) C5 0.0315(13) 0.0258(12) 0.0265(13) 0.0052(9) 0.0194(10) 0.0087(10) C6 0.0241(11) 0.0249(12) 0.0270(12) -0.0007(10) 0.0137(9) 0.0038(9) C7 0.0270(13) 0.0386(15) 0.0276(14) -0.0006(10) 0.0161(11) 0.0057(10) O7 0.081(2) 0.127(3) 0.130(3) 0.058(3) 0.078(2) 0.035(2) O8 0.117(5) 0.109(5) 0.077(4) 0.000 0.034(3) 0.000 _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 O4 2.466(2) 4_545 ? Sr1 O4 2.466(2) 3_545 ? Sr1 O2 2.5652(19) 2_655 ? Sr1 O2 2.5652(19) . ? Sr1 O5 2.622(2) 5_656 ? Sr1 O5 2.622(2) 6 ? Sr1 O5 2.833(2) 2_655 ? Sr1 O5 2.833(2) . ? Ni1 N1 2.028(2) . ? Ni1 N1 2.028(2) 7 ? Ni1 O1 2.0434(18) . ? Ni1 O1 2.0434(18) 7 ? Ni1 O6 2.096(2) 7 ? Ni1 O6 2.096(2) . ? O1 C6 1.272(3) . ? O2 C6 1.229(3) . ? O3 C7 1.240(3) . ? O4 C7 1.234(3) . ? O4 Sr1 2.466(2) 3_455 ? O5 Sr1 2.622(2) 5_656 ? O5 H5B 0.8500 . ? O5 H5A 0.8503 . ? O6 H6B 0.8500 . ? O6 H6A 0.8499 . ? N1 C5 1.335(3) . ? N1 C1 1.338(3) . ? C1 C2 1.376(4) . ? C1 C6 1.513(3) . ? C2 C3 1.393(4) . ? C2 H2 0.9300 . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.387(3) . ? C4 C7 1.503(3) . ? C5 H5 0.9300 . ? O7 H7A 0.8501 . ? O7 H7B 0.8500 . ? O8 H8 0.8696 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Sr1 O4 77.82(14) 4_545 3_545 ? O4 Sr1 O2 129.00(7) 4_545 2_655 ? O4 Sr1 O2 84.10(8) 3_545 2_655 ? O4 Sr1 O2 84.10(8) 4_545 . ? O4 Sr1 O2 129.00(7) 3_545 . ? O2 Sr1 O2 140.46(10) 2_655 . ? O4 Sr1 O5 154.88(7) 4_545 5_656 ? O4 Sr1 O5 102.54(8) 3_545 5_656 ? O2 Sr1 O5 75.51(6) 2_655 5_656 ? O2 Sr1 O5 76.25(7) . 5_656 ? O4 Sr1 O5 102.54(8) 4_545 6 ? O4 Sr1 O5 154.88(7) 3_545 6 ? O2 Sr1 O5 76.25(7) 2_655 6 ? O2 Sr1 O5 75.51(6) . 6 ? O5 Sr1 O5 87.67(9) 5_656 6 ? O4 Sr1 O5 62.43(7) 4_545 2_655 ? O4 Sr1 O5 90.28(7) 3_545 2_655 ? O2 Sr1 O5 70.50(6) 2_655 2_655 ? O2 Sr1 O5 122.20(6) . 2_655 ? O5 Sr1 O5 142.10(6) 5_656 2_655 ? O5 Sr1 O5 68.61(7) 6 2_655 ? O4 Sr1 O5 90.28(7) 4_545 . ? O4 Sr1 O5 62.43(7) 3_545 . ? O2 Sr1 O5 122.20(6) 2_655 . ? O2 Sr1 O5 70.50(6) . . ? O5 Sr1 O5 68.61(7) 5_656 . ? O5 Sr1 O5 142.10(6) 6 . ? O5 Sr1 O5 145.78(8) 2_655 . ? N1 Ni1 N1 180.00(11) . 7 ? N1 Ni1 O1 80.33(8) . . ? N1 Ni1 O1 99.67(8) 7 . ? N1 Ni1 O1 99.67(8) . 7 ? N1 Ni1 O1 80.33(8) 7 7 ? O1 Ni1 O1 180.00(8) . 7 ? N1 Ni1 O6 88.77(9) . 7 ? N1 Ni1 O6 91.23(9) 7 7 ? O1 Ni1 O6 90.11(8) . 7 ? O1 Ni1 O6 89.89(8) 7 7 ? N1 Ni1 O6 91.23(9) . . ? N1 Ni1 O6 88.77(9) 7 . ? O1 Ni1 O6 89.89(8) . . ? O1 Ni1 O6 90.11(8) 7 . ? O6 Ni1 O6 180.00(9) 7 . ? C6 O1 Ni1 115.17(15) . . ? C6 O2 Sr1 136.77(17) . . ? C7 O4 Sr1 171.8(2) . 3_455 ? Sr1 O5 Sr1 111.39(7) 5_656 . ? Sr1 O5 H5B 105.9 5_656 . ? Sr1 O5 H5B 117.3 . . ? Sr1 O5 H5A 124.2 5_656 . ? Sr1 O5 H5A 89.7 . . ? H5B O5 H5A 108.6 . . ? Ni1 O6 H6B 116.3 . . ? Ni1 O6 H6A 111.5 . . ? H6B O6 H6A 102.0 . . ? C5 N1 C1 119.1(2) . . ? C5 N1 Ni1 127.31(17) . . ? C1 N1 Ni1 113.16(16) . . ? N1 C1 C2 122.3(2) . . ? N1 C1 C6 114.8(2) . . ? C2 C1 C6 122.9(2) . . ? C1 C2 C3 118.4(2) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.0(2) . . ? C3 C4 C7 123.3(2) . . ? C5 C4 C7 118.7(2) . . ? N1 C5 C4 122.5(2) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? O2 C6 O1 125.4(2) . . ? O2 C6 C1 119.1(2) . . ? O1 C6 C1 115.5(2) . . ? O4 C7 O3 124.4(3) . . ? O4 C7 C4 116.5(2) . . ? O3 C7 C4 119.1(2) . . ? H7A O7 H7B 107.5 . . ? 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 N1 Ni1 O1 C6 5.80(19) . . . . ? N1 Ni1 O1 C6 -174.20(19) 7 . . . ? O1 Ni1 O1 C6 105(100) 7 . . . ? O6 Ni1 O1 C6 -82.93(19) 7 . . . ? O6 Ni1 O1 C6 97.07(19) . . . . ? O4 Sr1 O2 C6 -115.3(3) 4_545 . . . ? O4 Sr1 O2 C6 175.6(3) 3_545 . . . ? O2 Sr1 O2 C6 35.0(3) 2_655 . . . ? O5 Sr1 O2 C6 80.4(3) 5_656 . . . ? O5 Sr1 O2 C6 -10.7(3) 6 . . . ? O5 Sr1 O2 C6 -63.3(3) 2_655 . . . ? O5 Sr1 O2 C6 152.3(3) . . . . ? Sr1 Sr1 O2 C6 117.4(3) 5_656 . . . ? Sr1 Sr1 O2 C6 -36.2(3) 5_655 . . . ? O4 Sr1 O5 Sr1 -166.04(9) 4_545 . . 5_656 ? O4 Sr1 O5 Sr1 117.88(11) 3_545 . . 5_656 ? O2 Sr1 O5 Sr1 55.64(10) 2_655 . . 5_656 ? O2 Sr1 O5 Sr1 -82.41(8) . . . 5_656 ? O5 Sr1 O5 Sr1 0.0 5_656 . . 5_656 ? O5 Sr1 O5 Sr1 -54.95(17) 6 . . 5_656 ? O5 Sr1 O5 Sr1 158.61(7) 2_655 . . 5_656 ? Sr1 Sr1 O5 Sr1 -127.12(17) 5_655 . . 5_656 ? N1 Ni1 N1 C5 42(100) 7 . . . ? O1 Ni1 N1 C5 178.4(2) . . . . ? O1 Ni1 N1 C5 -1.6(2) 7 . . . ? O6 Ni1 N1 C5 -91.3(2) 7 . . . ? O6 Ni1 N1 C5 88.7(2) . . . . ? N1 Ni1 N1 C1 -145(100) 7 . . . ? O1 Ni1 N1 C1 -9.13(18) . . . . ? O1 Ni1 N1 C1 170.87(18) 7 . . . ? O6 Ni1 N1 C1 81.19(19) 7 . . . ? O6 Ni1 N1 C1 -98.81(19) . . . . ? C5 N1 C1 C2 2.1(4) . . . . ? Ni1 N1 C1 C2 -171.1(2) . . . . ? C5 N1 C1 C6 -176.0(2) . . . . ? Ni1 N1 C1 C6 10.9(3) . . . . ? N1 C1 C2 C3 -0.7(4) . . . . ? C6 C1 C2 C3 177.2(3) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C2 C3 C4 C7 -178.3(3) . . . . ? C1 N1 C5 C4 -1.7(4) . . . . ? Ni1 N1 C5 C4 170.4(2) . . . . ? C3 C4 C5 N1 0.0(4) . . . . ? C7 C4 C5 N1 179.7(3) . . . . ? Sr1 O2 C6 O1 22.4(5) . . . . ? Sr1 O2 C6 C1 -157.84(19) . . . . ? Ni1 O1 C6 O2 178.1(2) . . . . ? Ni1 O1 C6 C1 -1.7(3) . . . . ? N1 C1 C6 O2 173.9(2) . . . . ? C2 C1 C6 O2 -4.1(4) . . . . ? N1 C1 C6 O1 -6.3(3) . . . . ? C2 C1 C6 O1 175.7(3) . . . . ? Sr1 O4 C7 O3 -75.8(15) 3_455 . . . ? Sr1 O4 C7 C4 105.0(14) 3_455 . . . ? C3 C4 C7 O4 179.2(3) . . . . ? C5 C4 C7 O4 -0.5(4) . . . . ? C3 C4 C7 O3 0.0(4) . . . . ? C5 C4 C7 O3 -179.7(3) . . . . ? 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 O5 H5B O1 0.85 1.90 2.723(3) 162.6 6_556 O5 H5A O4 0.85 2.16 2.764(3) 127.6 3_545 O5 H5A O3 0.85 2.53 3.375(3) 174.4 3_545 O6 H6B O3 0.85 1.89 2.736(3) 176.6 7_556 O6 H6A O7 0.85 1.92 2.761(4) 170.4 7_556 O7 H7A O3 0.85 1.88 2.728(4) 178.3 2_556 O7 H7B O8 0.85 2.27 2.898(4) 131.3 5_557 O8 H8 O7 0.87 1.90 2.727(6) 158.0 . C2 H2 O1 0.93 2.59 3.504(3) 168.4 6_556 C5 H5 O4 0.93 2.39 2.721(3) 100.6 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.977 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 943748' ####################################################################### # # 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_t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H10 N2 Ni O10, H12 O6 Sr, 3H2 O' _chemical_formula_sum 'C14 H28 N2 Ni O19 Sr' _chemical_formula_weight 674.71 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' Ni Ni 0.3393 1.1124 '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 n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.323(4) _cell_length_b 22.223(11) _cell_length_c 16.991(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2765(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4535 _cell_measurement_theta_min 2.992 _cell_measurement_theta_max 27.366 _exptl_crystal_description rod _exptl_crystal_colour light-blue _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 2.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5302 _exptl_absorpt_correction_T_max 0.5765 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13675 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2503 _reflns_number_gt 2185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, the command 'omit -3 50' was used to omit the reflections above 50 degree. Hydrogen atoms of the water molecule O12 were not observed nor calculated. ; _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^)+(0.0817P)^2^+2.8312P] 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 2503 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _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 Sr1 Sr -0.06009(7) 0.2500 0.18917(3) 0.0232(2) Uani 1 2 d S . . N1 N -0.0243(4) 0.52053(15) 0.11551(18) 0.0259(7) Uani 1 1 d . . . C1 C -0.0856(6) 0.57635(18) 0.1277(2) 0.0299(9) Uani 1 1 d . . . O1 O -0.0877(4) 0.58583(13) -0.00976(16) 0.0360(7) Uani 1 1 d . . . Ni2 Ni 0.0000 0.5000 0.0000 0.0264(2) Uani 1 2 d S . . C2 C -0.1082(7) 0.5992(2) 0.2019(2) 0.0368(10) Uani 1 1 d . . . H2 H -0.1500 0.6383 0.2092 0.044 Uiso 1 1 calc R . . O2 O -0.1911(6) 0.66130(15) 0.05939(19) 0.0638(11) Uani 1 1 d . . . O3 O -0.0014(5) 0.47844(18) 0.38626(17) 0.0494(9) Uani 1 1 d . . . C3 C -0.0679(6) 0.56328(19) 0.2654(2) 0.0335(10) Uani 1 1 d . . . H3 H -0.0838 0.5777 0.3163 0.040 Uiso 1 1 calc R . . O4 O 0.1297(5) 0.41808(14) 0.30196(16) 0.0402(8) Uani 1 1 d . . . C4 C -0.0041(5) 0.50598(17) 0.2532(2) 0.0253(8) Uani 1 1 d . . . O5 O 0.2658(4) 0.53274(14) 0.00863(16) 0.0377(7) Uani 1 1 d . . . H5A H 0.3388 0.5281 -0.0298 0.045 Uiso 1 1 d R . . H5B H 0.3240 0.5214 0.0493 0.045 Uiso 1 1 d R . . C5 C 0.0170(6) 0.48641(18) 0.1768(2) 0.0251(8) Uani 1 1 d . . . H5 H 0.0619 0.4478 0.1680 0.030 Uiso 1 1 calc R . . O6 O 0.2333(4) 0.31905(12) 0.21570(16) 0.0315(6) Uani 1 1 d . . . H6A H 0.2776 0.3291 0.1714 0.038 Uiso 1 1 d R . . H6B H 0.2028 0.3526 0.2357 0.038 Uiso 1 1 d R . . C6 C -0.1248(6) 0.61106(19) 0.0542(2) 0.0353(10) Uani 1 1 d . . . O7 O -0.1254(5) 0.34783(13) 0.11829(17) 0.0413(8) Uani 1 1 d . . . H7A H -0.0621 0.3666 0.0843 0.050 Uiso 1 1 d R . . H7B H -0.2037 0.3739 0.1323 0.050 Uiso 1 1 d R . . C7 C 0.0451(6) 0.4643(2) 0.3188(2) 0.0303(9) Uani 1 1 d . . . O8 O 0.1046(7) 0.2500 0.0548(2) 0.0414(11) Uani 1 2 d S . . H8A H 0.1234 0.2802 0.0252 0.050 Uiso 1 1 d R . . O9 O -0.4130(6) 0.2500 0.1550(2) 0.0349(10) Uani 1 2 d S . . H9A H -0.4509 0.2794 0.1274 0.042 Uiso 1 1 d R . . O10 O 0.4241(5) 0.34658(15) 0.08006(19) 0.0464(8) Uani 1 1 d . . . H10A H 0.4306 0.3837 0.0916 0.056 Uiso 1 1 d R . . H10B H 0.3652 0.3445 0.0370 0.056 Uiso 1 1 d R . . O12 O -0.706(4) 0.7500 0.0973(18) 0.264(18) Uani 0.50 2 d SP . . O11 O -0.335(5) 0.7500 0.1893(17) 0.227(14) Uiso 0.50 2 d SP . . H11A H -0.2675 0.7628 0.1521 0.341 Uiso 0.25 1 d PR . . H11B H -0.4406 0.7500 0.1688 0.341 Uiso 0.50 2 d SPR . . 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 0.0229(3) 0.0212(3) 0.0256(3) 0.000 0.0021(2) 0.000 N1 0.0276(17) 0.0294(18) 0.0206(16) 0.0033(14) 0.0029(13) 0.0030(14) C1 0.031(2) 0.028(2) 0.031(2) 0.0032(16) 0.0030(17) 0.0023(17) O1 0.0445(18) 0.0365(17) 0.0269(15) 0.0127(13) 0.0033(13) 0.0106(14) Ni2 0.0311(4) 0.0319(4) 0.0162(4) 0.0054(3) 0.0015(3) 0.0066(3) C2 0.050(3) 0.027(2) 0.034(2) -0.0016(17) 0.002(2) 0.007(2) O2 0.106(3) 0.043(2) 0.0427(19) 0.0120(15) 0.009(2) 0.031(2) O3 0.050(2) 0.081(3) 0.0172(15) 0.0012(16) 0.0010(13) 0.0254(19) C3 0.040(2) 0.037(2) 0.023(2) -0.0051(17) 0.0011(17) 0.0032(19) O4 0.055(2) 0.0374(17) 0.0279(15) 0.0049(12) -0.0035(14) 0.0139(16) C4 0.023(2) 0.033(2) 0.0205(19) 0.0014(16) -0.0015(15) -0.0009(16) O5 0.0303(16) 0.057(2) 0.0260(14) 0.0048(13) 0.0011(12) 0.0033(14) C5 0.031(2) 0.025(2) 0.0199(18) 0.0022(15) 0.0001(15) 0.0021(16) O6 0.0391(16) 0.0268(14) 0.0287(13) -0.0004(12) 0.0001(12) -0.0002(12) C6 0.043(3) 0.030(2) 0.033(2) 0.0073(18) 0.0043(19) 0.0068(19) O7 0.0474(19) 0.0307(16) 0.0457(18) 0.0087(13) 0.0163(15) 0.0090(14) C7 0.026(2) 0.044(3) 0.021(2) 0.0017(17) -0.0029(16) -0.0019(19) O8 0.063(3) 0.029(2) 0.032(2) 0.000 0.014(2) 0.000 O9 0.034(2) 0.031(2) 0.040(2) 0.000 -0.0099(19) 0.000 O10 0.055(2) 0.0389(18) 0.0454(18) 0.0078(14) -0.0153(16) -0.0078(15) O12 0.16(3) 0.42(5) 0.21(3) 0.000 -0.09(2) 0.000 _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 O7 2.531(3) 7_565 ? Sr1 O7 2.531(3) . ? Sr1 O8 2.582(4) . ? Sr1 O9 2.649(4) . ? Sr1 O6 2.678(3) . ? Sr1 O6 2.678(3) 7_565 ? Sr1 O6 2.694(3) 6_556 ? Sr1 O6 2.694(3) 4_455 ? Sr1 O9 2.858(5) 6_656 ? Sr1 Sr1 4.2047(18) 6_656 ? Sr1 Sr1 4.2047(18) 6_556 ? N1 C5 1.323(5) . ? N1 C1 1.335(5) . ? N1 Ni2 2.023(3) . ? C1 C2 1.370(6) . ? C1 C6 1.496(6) . ? O1 C6 1.252(5) . ? O1 Ni2 2.019(3) . ? Ni2 O1 2.019(3) 5_565 ? Ni2 O1 2.019(3) 5_565 ? Ni2 N1 2.023(3) 5_565 ? Ni2 O5 2.083(3) 5_565 ? Ni2 O5 2.083(3) . ? C2 C3 1.375(6) . ? C2 H2 0.9300 . ? O2 C6 1.221(5) . ? O3 C7 1.236(5) . ? C3 C4 1.372(6) . ? C3 H3 0.9300 . ? O4 C7 1.233(5) . ? C4 C5 1.378(5) . ? C4 C7 1.494(6) . ? O5 H5A 0.8499 . ? O5 H5B 0.8500 . ? C5 H5 0.9300 . ? O6 Sr1 2.694(3) 6_656 ? O6 H6A 0.8500 . ? O6 H6B 0.8499 . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? O8 H8A 0.8499 . ? O9 Sr1 2.858(5) 6_556 ? O9 H9A 0.8500 . ? O10 H10A 0.8500 . ? O10 H10B 0.8500 . ? O11 H11A 0.8500 . ? O11 H11B 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sr1 O7 118.41(15) 7_565 . ? O7 Sr1 O8 70.58(8) 7_565 . ? O7 Sr1 O8 70.58(8) . . ? O7 Sr1 O9 73.23(9) 7_565 . ? O7 Sr1 O9 73.23(9) . . ? O8 Sr1 O9 105.18(14) . . ? O7 Sr1 O6 136.37(10) 7_565 . ? O7 Sr1 O6 74.89(10) . . ? O8 Sr1 O6 76.94(11) . . ? O9 Sr1 O6 145.03(6) . . ? O7 Sr1 O6 74.89(10) 7_565 7_565 ? O7 Sr1 O6 136.37(10) . 7_565 ? O8 Sr1 O6 76.94(11) . 7_565 ? O9 Sr1 O6 145.03(6) . 7_565 ? O6 Sr1 O6 69.92(12) . 7_565 ? O7 Sr1 O6 131.97(10) 7_565 6_556 ? O7 Sr1 O6 71.95(9) . 6_556 ? O8 Sr1 O6 142.46(7) . 6_556 ? O9 Sr1 O6 65.38(10) . 6_556 ? O6 Sr1 O6 91.33(8) . 6_556 ? O6 Sr1 O6 132.53(5) 7_565 6_556 ? O7 Sr1 O6 71.95(9) 7_565 4_455 ? O7 Sr1 O6 131.97(10) . 4_455 ? O8 Sr1 O6 142.46(7) . 4_455 ? O9 Sr1 O6 65.38(10) . 4_455 ? O6 Sr1 O6 132.53(5) . 4_455 ? O6 Sr1 O6 91.33(8) 7_565 4_455 ? O6 Sr1 O6 69.45(12) 6_556 4_455 ? O7 Sr1 O9 120.79(8) 7_565 6_656 ? O7 Sr1 O9 120.79(8) . 6_656 ? O8 Sr1 O9 130.01(15) . 6_656 ? O9 Sr1 O9 124.81(12) . 6_656 ? O6 Sr1 O9 62.73(9) . 6_656 ? O6 Sr1 O9 62.73(9) 7_565 6_656 ? O6 Sr1 O9 69.88(9) 6_556 6_656 ? O6 Sr1 O9 69.88(9) 4_455 6_656 ? O7 Sr1 Sr1 113.48(8) 7_565 6_656 ? O7 Sr1 Sr1 113.48(8) . 6_656 ? O8 Sr1 Sr1 91.60(12) . 6_656 ? O9 Sr1 Sr1 163.22(9) . 6_656 ? O6 Sr1 Sr1 38.63(6) . 6_656 ? O6 Sr1 Sr1 38.63(6) 7_565 6_656 ? O6 Sr1 Sr1 101.20(7) 6_556 6_656 ? O6 Sr1 Sr1 101.20(7) 4_455 6_656 ? O9 Sr1 Sr1 38.41(8) 6_656 6_656 ? O7 Sr1 Sr1 93.98(7) 7_565 6_556 ? O7 Sr1 Sr1 93.98(7) . 6_556 ? O8 Sr1 Sr1 147.29(11) . 6_556 ? O9 Sr1 Sr1 42.11(10) . 6_556 ? O6 Sr1 Sr1 128.01(7) . 6_556 ? O6 Sr1 Sr1 128.01(7) 7_565 6_556 ? O6 Sr1 Sr1 38.36(6) 6_556 6_556 ? O6 Sr1 Sr1 38.36(6) 4_455 6_556 ? O9 Sr1 Sr1 82.70(9) 6_656 6_556 ? Sr1 Sr1 Sr1 121.11(4) 6_656 6_556 ? C5 N1 C1 119.2(3) . . ? C5 N1 Ni2 127.9(3) . . ? C1 N1 Ni2 112.9(3) . . ? N1 C1 C2 121.9(4) . . ? N1 C1 C6 114.5(4) . . ? C2 C1 C6 123.6(4) . . ? C6 O1 Ni2 114.9(2) . . ? O1 Ni2 O1 0.00(16) 5_565 5_565 ? O1 Ni2 O1 180.00(15) 5_565 . ? O1 Ni2 O1 180.00(15) 5_565 . ? O1 Ni2 N1 80.72(12) 5_565 5_565 ? O1 Ni2 N1 80.72(12) 5_565 5_565 ? O1 Ni2 N1 99.28(12) . 5_565 ? O1 Ni2 N1 99.28(12) 5_565 . ? O1 Ni2 N1 99.28(12) 5_565 . ? O1 Ni2 N1 80.72(12) . . ? N1 Ni2 N1 180.00(19) 5_565 . ? O1 Ni2 O5 88.45(13) 5_565 5_565 ? O1 Ni2 O5 88.45(13) 5_565 5_565 ? O1 Ni2 O5 91.55(13) . 5_565 ? N1 Ni2 O5 86.27(12) 5_565 5_565 ? N1 Ni2 O5 93.73(12) . 5_565 ? O1 Ni2 O5 91.55(13) 5_565 . ? O1 Ni2 O5 91.55(13) 5_565 . ? O1 Ni2 O5 88.45(13) . . ? N1 Ni2 O5 93.73(12) 5_565 . ? N1 Ni2 O5 86.27(12) . . ? O5 Ni2 O5 180.00(16) 5_565 . ? C1 C2 C3 118.8(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.3(4) . . ? C3 C4 C7 123.0(4) . . ? C5 C4 C7 118.7(4) . . ? Ni2 O5 H5A 119.4 . . ? Ni2 O5 H5B 114.9 . . ? H5A O5 H5B 105.8 . . ? N1 C5 C4 122.3(4) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? Sr1 O6 Sr1 103.01(10) . 6_656 ? Sr1 O6 H6A 107.9 . . ? Sr1 O6 H6A 117.8 6_656 . ? Sr1 O6 H6B 111.1 . . ? Sr1 O6 H6B 114.1 6_656 . ? H6A O6 H6B 103.0 . . ? O2 C6 O1 124.0(4) . . ? O2 C6 C1 119.2(4) . . ? O1 C6 C1 116.9(4) . . ? Sr1 O7 H7A 130.0 . . ? Sr1 O7 H7B 125.5 . . ? H7A O7 H7B 102.9 . . ? O4 C7 O3 124.5(4) . . ? O4 C7 C4 117.7(3) . . ? O3 C7 C4 117.8(4) . . ? Sr1 O8 H8A 126.8 . . ? Sr1 O9 Sr1 99.48(13) . 6_556 ? Sr1 O9 H9A 116.1 . . ? Sr1 O9 H9A 112.8 6_556 . ? H10A O10 H10B 106.2 . . ? H11A O11 H11B 103.0 . . ? 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 C5 N1 C1 C2 -0.5(6) . . . . ? Ni2 N1 C1 C2 -178.8(4) . . . . ? C5 N1 C1 C6 179.0(4) . . . . ? Ni2 N1 C1 C6 0.7(4) . . . . ? C6 O1 Ni2 O1 0(100) . . . 5_565 ? C6 O1 Ni2 O1 0(100) . . . 5_565 ? C6 O1 Ni2 N1 176.7(3) . . . 5_565 ? C6 O1 Ni2 N1 -3.3(3) . . . . ? C6 O1 Ni2 O5 90.2(3) . . . 5_565 ? C6 O1 Ni2 O5 -89.8(3) . . . . ? C5 N1 Ni2 O1 3.0(4) . . . 5_565 ? C1 N1 Ni2 O1 -178.8(3) . . . 5_565 ? C5 N1 Ni2 O1 3.0(4) . . . 5_565 ? C1 N1 Ni2 O1 -178.8(3) . . . 5_565 ? C5 N1 Ni2 O1 -177.0(4) . . . . ? C1 N1 Ni2 O1 1.2(3) . . . . ? C5 N1 Ni2 N1 -29.2(5) . . . 5_565 ? C1 N1 Ni2 N1 149.0(4) . . . 5_565 ? C5 N1 Ni2 O5 92.1(4) . . . 5_565 ? C1 N1 Ni2 O5 -89.7(3) . . . 5_565 ? C5 N1 Ni2 O5 -87.9(4) . . . . ? C1 N1 Ni2 O5 90.3(3) . . . . ? N1 C1 C2 C3 -0.6(7) . . . . ? C6 C1 C2 C3 180.0(4) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C2 C3 C4 C7 179.2(4) . . . . ? C1 N1 C5 C4 1.2(6) . . . . ? Ni2 N1 C5 C4 179.3(3) . . . . ? C3 C4 C5 N1 -0.9(6) . . . . ? C7 C4 C5 N1 179.7(4) . . . . ? O7 Sr1 O6 Sr1 -67.19(16) 7_565 . . 6_656 ? O7 Sr1 O6 Sr1 177.28(12) . . . 6_656 ? O8 Sr1 O6 Sr1 -109.64(11) . . . 6_656 ? O9 Sr1 O6 Sr1 152.45(17) . . . 6_656 ? O6 Sr1 O6 Sr1 -28.97(12) 7_565 . . 6_656 ? O6 Sr1 O6 Sr1 106.39(14) 6_556 . . 6_656 ? O6 Sr1 O6 Sr1 43.47(13) 4_455 . . 6_656 ? O9 Sr1 O6 Sr1 39.91(8) 6_656 . . 6_656 ? Sr1 Sr1 O6 Sr1 94.15(10) 6_556 . . 6_656 ? Ni2 O1 C6 O2 -174.9(4) . . . . ? Ni2 O1 C6 C1 4.6(5) . . . . ? N1 C1 C6 O2 175.9(4) . . . . ? C2 C1 C6 O2 -4.6(7) . . . . ? N1 C1 C6 O1 -3.6(6) . . . . ? C2 C1 C6 O1 175.9(4) . . . . ? C3 C4 C7 O4 -167.8(4) . . . . ? C5 C4 C7 O4 11.5(6) . . . . ? C3 C4 C7 O3 12.0(6) . . . . ? C5 C4 C7 O3 -168.7(4) . . . . ? O7 Sr1 O9 Sr1 116.21(8) 7_565 . . 6_556 ? O7 Sr1 O9 Sr1 -116.21(8) . . . 6_556 ? O8 Sr1 O9 Sr1 180.0 . . . 6_556 ? O6 Sr1 O9 Sr1 -91.17(17) . . . 6_556 ? O6 Sr1 O9 Sr1 91.17(17) 7_565 . . 6_556 ? O6 Sr1 O9 Sr1 -38.80(7) 6_556 . . 6_556 ? O6 Sr1 O9 Sr1 38.80(7) 4_455 . . 6_556 ? O9 Sr1 O9 Sr1 0.0 6_656 . . 6_556 ? Sr1 Sr1 O9 Sr1 0.0 6_656 . . 6_556 ? 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 O5 H5A O3 0.85 1.86 2.713(4) 177.4 2_564 O5 H5B O3 0.85 1.94 2.748(4) 159.7 6_656 O6 H6A O10 0.85 1.93 2.764(5) 168.4 . O6 H6B O4 0.85 1.92 2.751(4) 167.2 . O7 H7A O1 0.85 1.98 2.830(4) 176.6 5_565 O7 H7B O4 0.85 1.92 2.737(4) 159.9 6_556 O8 H8A O2 0.85 2.00 2.838(5) 168.2 5_565 O9 H9A O10 0.85 1.93 2.766(4) 168.5 1_455 O10 H10A O3 0.85 2.20 3.035(5) 169.6 6_656 O10 H10A O4 0.85 2.44 2.968(5) 120.5 6_656 O10 H10B O2 0.85 2.08 2.925(5) 172.6 5_565 O10 H10B O1 0.85 2.60 3.123(5) 121.2 5_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.803 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 943749' ####################################################################### # # 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 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H25 N3 Ni O20 Sr2, 2(H2 O)' _chemical_formula_sum 'C21 H29 N3 Ni O22 Sr2' _chemical_formula_weight 909.42 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' Ni Ni 0.3393 1.1124 '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 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 8.5324(13) _cell_length_b 22.302(3) _cell_length_c 16.570(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.783(3) _cell_angle_gamma 90.00 _cell_volume 3146.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5690 _cell_measurement_theta_min 2.203 _cell_measurement_theta_max 27.734 _exptl_crystal_description block _exptl_crystal_colour light-blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 4.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3221 _exptl_absorpt_correction_T_max 0.3470 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22085 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_unetI/netI 0.0378 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.38 _reflns_number_total 7838 _reflns_number_gt 5996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, DFIX and DANG restraints were used for reasonable bond distances between water O atoms and H atoms. Thermal motion of O20 O20B are restrained by commond 'DELU' and 'SIMU'. Free restrains were used to undo the bonds between Sr1 C21 and Sr2 C13. ; _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^)+(0.0300P)^2^+2.7000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7838 _refine_ls_number_parameters 500 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.009 _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 0.18308(3) 0.058616(11) 0.536328(17) 0.02854(7) Uani 1 1 d D . . Sr2 Sr 0.05412(3) 0.408877(11) 0.335231(16) 0.03013(7) Uani 1 1 d D . . Ni1 Ni 0.41236(4) 0.263114(14) 0.325787(19) 0.02012(8) Uani 1 1 d . . . O1 O 0.2824(2) 0.19778(8) 0.37782(11) 0.0259(4) Uani 1 1 d . A . O2 O 0.1994(2) 0.16662(9) 0.49542(13) 0.0356(5) Uani 1 1 d . . . O3 O 0.5631(3) 0.42984(11) 0.65401(14) 0.0503(6) Uani 1 1 d . A . O4 O 0.6695(3) 0.43649(11) 0.53674(15) 0.0618(8) Uani 1 1 d . A . O5 O 0.2264(2) 0.31807(8) 0.29354(11) 0.0260(4) Uani 1 1 d . A . O6 O 0.1158(2) 0.36516(9) 0.18740(11) 0.0315(4) Uani 1 1 d . A . O7 O 0.5020(3) 0.15428(10) -0.04285(13) 0.0498(6) Uani 1 1 d . . . O8 O 0.5766(3) 0.10724(11) 0.07234(15) 0.0543(7) Uani 1 1 d . A . O9 O 0.5693(2) 0.32665(8) 0.28858(12) 0.0288(4) Uani 1 1 d . A . O10 O 0.8244(2) 0.34080(9) 0.27161(13) 0.0370(5) Uani 1 1 d . . . O11 O 0.9400(2) 0.05187(9) 0.43478(14) 0.0370(5) Uani 1 1 d . . . O12 O 0.6815(2) 0.04571(8) 0.43496(12) 0.0327(5) Uani 1 1 d . . . O13 O 0.2943(3) 0.01867(13) 0.40524(15) 0.0611(8) Uani 1 1 d D . . H13A H 0.277(5) 0.0425(17) 0.3648(19) 0.092 Uiso 1 1 d D . . H13B H 0.387(3) 0.0043(19) 0.402(3) 0.092 Uiso 1 1 d D . . O14 O 0.4781(3) 0.08524(12) 0.54742(15) 0.0516(6) Uani 1 1 d D . . H14A H 0.5453 0.0765 0.5137 0.077 Uiso 1 1 d RD . . H14B H 0.5237 0.1010 0.5894 0.077 Uiso 1 1 d RD . . O15 O -0.0612(4) 0.08129(15) 0.6160(2) 0.0904(11) Uani 1 1 d D . . H15A H -0.1124 0.1089 0.6379 0.136 Uiso 1 1 d RD . . H15B H -0.1204 0.0506 0.6119 0.136 Uiso 1 1 d RD . . O16 O 0.2695(5) 0.05582(13) 0.68776(18) 0.0824(10) Uani 1 1 d D . . H16A H 0.246(6) 0.0870(10) 0.7131(13) 0.124 Uiso 1 1 d D . . H16B H 0.240(6) 0.0246(10) 0.7110(13) 0.124 Uiso 1 1 d D . . O17 O 0.2241(4) 0.44806(13) 0.45146(17) 0.0785(10) Uani 1 1 d D A . H17A H 0.253(5) 0.4847(8) 0.4504(16) 0.118 Uiso 1 1 d D . . H17B H 0.190(4) 0.4408(18) 0.4982(8) 0.118 Uiso 1 1 d D . . O18 O -0.2056(4) 0.44928(13) 0.38623(17) 0.0673(8) Uani 1 1 d D A . H18A H -0.216(3) 0.4409(18) 0.4350(11) 0.101 Uiso 1 1 d D . . H18B H -0.243(6) 0.4833(11) 0.374(2) 0.101 Uiso 1 1 d D . . O19 O 0.3568(4) 0.44685(14) 0.2915(2) 0.0693(8) Uani 1 1 d D A . H19A H 0.444(3) 0.4288(18) 0.289(3) 0.104 Uiso 1 1 d D . . H19B H 0.373(5) 0.4817(10) 0.311(3) 0.104 Uiso 1 1 d D . . O20 O 0.0465(6) 0.52424(18) 0.3116(4) 0.0565(17) Uani 0.688(12) 1 d PDU A 1 H20A H 0.098(7) 0.541(2) 0.276(3) 0.085 Uiso 0.688(12) 1 d PD A 1 H20B H 0.026(8) 0.549(2) 0.348(3) 0.085 Uiso 0.688(12) 1 d PD A 1 O20B O 0.0007(14) 0.5051(5) 0.2578(10) 0.068(5) Uani 0.312(12) 1 d PDU A 2 H20C H 0.080(3) 0.524(3) 0.243(7) 0.103 Uiso 0.312(12) 1 d PD A 2 H20D H -0.063(13) 0.529(3) 0.278(5) 0.103 Uiso 0.312(12) 1 d PD A 2 N1 N 0.4233(3) 0.29209(9) 0.44366(13) 0.0230(5) Uani 1 1 d . A . N2 N 0.3682(3) 0.23947(9) 0.20477(13) 0.0235(5) Uani 1 1 d . A . N3 N 0.6192(2) 0.21572(9) 0.34164(13) 0.0210(4) Uani 1 1 d . A . C1 C 0.3497(3) 0.25581(11) 0.49345(16) 0.0242(5) Uani 1 1 d . . . C2 C 0.3502(4) 0.26684(13) 0.57550(17) 0.0349(7) Uani 1 1 d . A . H2 H 0.3007 0.2407 0.6093 0.042 Uiso 1 1 calc R . . C3 C 0.4257(4) 0.31750(14) 0.60632(18) 0.0358(7) Uani 1 1 d . . . H3 H 0.4266 0.3259 0.6613 0.043 Uiso 1 1 calc R A . C4 C 0.4999(3) 0.35566(12) 0.55516(16) 0.0289(6) Uani 1 1 d . A . C5 C 0.4956(3) 0.34066(12) 0.47402(16) 0.0271(6) Uani 1 1 d . . . H5 H 0.5456 0.3658 0.4390 0.033 Uiso 1 1 calc R A . C6 C 0.2698(3) 0.20217(11) 0.45358(17) 0.0249(6) Uani 1 1 d . A . C7 C 0.5841(4) 0.41203(14) 0.58354(18) 0.0360(7) Uani 1 1 d . . . C8 C 0.2768(3) 0.27996(11) 0.16502(15) 0.0224(5) Uani 1 1 d . . . C9 C 0.2555(4) 0.28132(13) 0.08201(17) 0.0331(7) Uani 1 1 d . A . H9 H 0.1915 0.3101 0.0559 0.040 Uiso 1 1 calc R . . C10 C 0.3319(4) 0.23866(14) 0.03864(17) 0.0359(7) Uani 1 1 d . . . H10 H 0.3206 0.2388 -0.0176 0.043 Uiso 1 1 calc R A . C11 C 0.4249(3) 0.19587(12) 0.07817(17) 0.0291(6) Uani 1 1 d . A . C12 C 0.4398(3) 0.19781(12) 0.16158(17) 0.0273(6) Uani 1 1 d . . . H12 H 0.5018 0.1691 0.1890 0.033 Uiso 1 1 calc R A . C13 C 0.1998(3) 0.32472(11) 0.21762(15) 0.0221(5) Uani 1 1 d . A . C14 C 0.5085(4) 0.14837(14) 0.03163(19) 0.0354(7) Uani 1 1 d . . . C15 C 0.7453(3) 0.24669(11) 0.32028(15) 0.0219(5) Uani 1 1 d . . . C16 C 0.8951(3) 0.22326(12) 0.32692(17) 0.0279(6) Uani 1 1 d . A . H16 H 0.9800 0.2453 0.3106 0.033 Uiso 1 1 calc R . . C17 C 0.9163(3) 0.16599(12) 0.35849(17) 0.0276(6) Uani 1 1 d . . . H17 H 1.0160 0.1490 0.3635 0.033 Uiso 1 1 calc R A . C18 C 0.7878(3) 0.13435(11) 0.38237(15) 0.0215(5) Uani 1 1 d . A . C19 C 0.6410(3) 0.16064(11) 0.37163(15) 0.0226(5) Uani 1 1 d . . . H19 H 0.5539 0.1390 0.3859 0.027 Uiso 1 1 calc R A . C20 C 0.7110(3) 0.31026(12) 0.29109(16) 0.0257(6) Uani 1 1 d . A . C21 C 0.8050(3) 0.07281(11) 0.42031(16) 0.0249(6) Uani 1 1 d . . . O21 O 0.2675(3) 0.09583(11) 0.28066(16) 0.0531(6) Uani 1 1 d D . . H21A H 0.264(5) 0.1290(11) 0.306(2) 0.080 Uiso 1 1 d D . . H21B H 0.187(3) 0.0933(17) 0.247(2) 0.080 Uiso 1 1 d D . . O22 O 0.2761(5) 0.44499(19) 0.7093(3) 0.1254(17) Uani 1 1 d . . . H22A H 0.3739 0.4503 0.7050 0.188 Uiso 1 1 d R . . H22B H 0.2418 0.4178 0.6767 0.188 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 0.02689(14) 0.02000(12) 0.03925(16) 0.00358(11) 0.00607(11) 0.00004(10) Sr2 0.03952(16) 0.02234(13) 0.03010(14) -0.00199(11) 0.01415(11) -0.00293(11) Ni1 0.02130(17) 0.01884(15) 0.02012(16) 0.00117(13) 0.00062(12) 0.00086(13) O1 0.0260(10) 0.0235(9) 0.0282(10) -0.0010(8) 0.0022(8) -0.0043(8) O2 0.0434(12) 0.0264(10) 0.0376(12) 0.0076(9) 0.0065(10) -0.0102(9) O3 0.0673(17) 0.0487(14) 0.0352(13) -0.0169(11) 0.0068(11) -0.0180(12) O4 0.087(2) 0.0547(16) 0.0461(14) -0.0172(12) 0.0256(14) -0.0435(15) O5 0.0290(10) 0.0281(10) 0.0209(9) 0.0000(8) 0.0021(8) 0.0072(8) O6 0.0349(11) 0.0323(10) 0.0275(10) 0.0056(8) 0.0040(8) 0.0121(9) O7 0.0743(18) 0.0445(13) 0.0327(12) -0.0084(10) 0.0187(12) 0.0119(12) O8 0.0674(17) 0.0485(14) 0.0468(14) -0.0107(12) 0.0018(12) 0.0262(13) O9 0.0286(10) 0.0230(9) 0.0353(11) 0.0081(8) 0.0050(8) 0.0016(8) O10 0.0320(11) 0.0311(11) 0.0487(13) 0.0140(10) 0.0088(10) -0.0075(9) O11 0.0284(11) 0.0253(10) 0.0564(14) 0.0090(10) -0.0033(10) 0.0063(9) O12 0.0309(11) 0.0250(10) 0.0429(12) 0.0082(9) 0.0078(9) 0.0022(8) O13 0.0732(19) 0.0734(19) 0.0378(14) 0.0097(13) 0.0107(13) 0.0337(16) O14 0.0292(12) 0.0789(18) 0.0471(14) -0.0214(13) 0.0054(10) -0.0117(12) O15 0.090(2) 0.092(2) 0.097(3) 0.018(2) 0.058(2) 0.040(2) O16 0.138(3) 0.0612(19) 0.0509(17) -0.0268(15) 0.0254(18) -0.032(2) O17 0.120(3) 0.0682(19) 0.0479(16) -0.0001(14) 0.0117(17) -0.0563(19) O18 0.091(2) 0.0565(17) 0.0591(17) 0.0126(14) 0.0423(16) 0.0215(16) O19 0.077(2) 0.0594(18) 0.0702(19) -0.0079(16) -0.0018(17) -0.0174(15) O20 0.089(3) 0.034(2) 0.049(3) -0.0031(19) 0.023(3) -0.015(2) O20B 0.082(8) 0.044(6) 0.081(11) 0.018(6) 0.024(7) 0.006(5) N1 0.0270(12) 0.0199(10) 0.0220(11) 0.0023(9) 0.0011(9) -0.0016(9) N2 0.0248(11) 0.0226(11) 0.0230(11) -0.0010(9) 0.0015(9) 0.0033(9) N3 0.0215(11) 0.0201(10) 0.0213(10) 0.0030(9) -0.0001(8) -0.0008(9) C1 0.0258(14) 0.0212(12) 0.0257(13) 0.0028(10) 0.0018(11) -0.0014(11) C2 0.0477(19) 0.0325(15) 0.0255(14) 0.0034(12) 0.0097(13) -0.0092(14) C3 0.0485(19) 0.0365(16) 0.0230(14) -0.0027(12) 0.0066(13) -0.0080(14) C4 0.0352(16) 0.0258(14) 0.0255(14) -0.0018(11) 0.0014(12) -0.0048(12) C5 0.0331(15) 0.0232(13) 0.0252(14) 0.0030(11) 0.0032(11) -0.0076(11) C6 0.0230(13) 0.0192(12) 0.0322(15) 0.0018(11) 0.0010(11) 0.0013(10) C7 0.0443(18) 0.0345(16) 0.0292(15) -0.0084(13) 0.0034(13) -0.0120(14) C8 0.0229(13) 0.0230(13) 0.0215(13) 0.0011(10) 0.0034(10) 0.0003(10) C9 0.0434(18) 0.0329(15) 0.0228(14) 0.0026(12) 0.0009(12) 0.0114(13) C10 0.0499(19) 0.0381(16) 0.0199(13) -0.0022(12) 0.0044(13) 0.0075(15) C11 0.0328(15) 0.0265(14) 0.0288(14) -0.0070(11) 0.0060(12) -0.0001(12) C12 0.0287(14) 0.0254(13) 0.0279(14) -0.0019(11) 0.0023(11) 0.0044(11) C13 0.0208(13) 0.0222(12) 0.0235(13) 0.0004(10) 0.0041(10) 0.0006(10) C14 0.0388(17) 0.0333(16) 0.0350(17) -0.0108(13) 0.0091(14) -0.0003(14) C15 0.0258(13) 0.0225(12) 0.0175(12) 0.0021(10) 0.0027(10) -0.0018(10) C16 0.0223(14) 0.0293(14) 0.0327(15) 0.0049(12) 0.0066(11) -0.0021(11) C17 0.0224(13) 0.0283(14) 0.0320(15) 0.0009(12) 0.0013(11) 0.0046(11) C18 0.0228(13) 0.0199(12) 0.0218(13) -0.0013(10) 0.0007(10) 0.0015(10) C19 0.0243(13) 0.0193(12) 0.0239(13) 0.0031(10) -0.0001(10) -0.0033(10) C20 0.0309(15) 0.0236(13) 0.0228(13) 0.0039(11) 0.0037(11) -0.0008(11) C21 0.0307(15) 0.0205(12) 0.0233(13) -0.0013(10) -0.0002(11) 0.0020(11) O21 0.0725(19) 0.0418(14) 0.0451(15) -0.0065(11) 0.0034(13) 0.0022(13) O22 0.099(3) 0.134(4) 0.149(4) 0.041(3) 0.049(3) 0.065(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O2 2.5088(19) . ? Sr1 O16 2.569(3) . ? Sr1 O14 2.581(2) . ? Sr1 O13 2.586(3) . ? Sr1 O11 2.587(2) 1_455 ? Sr1 O15 2.589(3) . ? Sr1 O12 2.6271(19) 3_656 ? Sr1 O11 2.733(2) 3_656 ? Sr1 C21 3.018(3) 3_656 ? Sr1 Sr1 4.1893(7) 3_556 ? Sr1 H15B 2.9553 . ? Sr2 O17 2.492(3) . ? Sr2 O20B 2.526(9) . ? Sr2 O7 2.526(2) 4_566 ? Sr2 O18 2.586(3) . ? Sr2 O20 2.603(4) . ? Sr2 O5 2.6216(18) . ? Sr2 O10 2.643(2) 1_455 ? Sr2 O6 2.720(2) . ? Sr2 O19 2.856(3) . ? Sr2 H17B 2.956(18) . ? Ni1 O5 2.0479(18) . ? Ni1 N1 2.054(2) . ? Ni1 O1 2.0547(18) . ? Ni1 N3 2.059(2) . ? Ni1 O9 2.0714(19) . ? Ni1 N2 2.084(2) . ? O1 C6 1.271(3) . ? O2 C6 1.235(3) . ? O3 C7 1.257(4) . ? O4 C7 1.227(4) . ? O5 C13 1.272(3) . ? O6 C13 1.237(3) . ? O7 C14 1.239(4) . ? O7 Sr2 2.526(2) 4_665 ? O8 C14 1.258(4) . ? O9 C20 1.261(3) . ? O10 C20 1.243(3) . ? O10 Sr2 2.643(2) 1_655 ? O11 C21 1.251(3) . ? O11 Sr1 2.587(2) 1_655 ? O11 Sr1 2.733(2) 3_656 ? O12 C21 1.252(3) . ? O12 Sr1 2.6271(19) 3_656 ? O13 H13A 0.860(10) . ? O13 H13B 0.857(10) . ? O14 H14A 0.8500 . ? O14 H14B 0.8501 . ? O15 H15A 0.8499 . ? O15 H15B 0.8499 . ? O16 H16A 0.842(10) . ? O16 H16B 0.841(10) . ? O17 H17A 0.854(10) . ? O17 H17B 0.860(10) . ? O18 H18A 0.839(10) . ? O18 H18B 0.842(10) . ? O19 H19A 0.851(10) . ? O19 H19B 0.850(10) . ? O20 H20A 0.846(10) . ? O20 H20B 0.848(10) . ? O20 H20C 1.18(11) . ? O20 H20D 1.06(12) . ? O20B H20A 1.18(5) . ? O20B H20C 0.849(10) . ? O20B H20D 0.851(10) . ? N1 C5 1.329(3) . ? N1 C1 1.341(3) . ? N2 C8 1.337(3) . ? N2 C12 1.344(3) . ? N3 C19 1.333(3) . ? N3 C15 1.345(3) . ? C1 C2 1.381(4) . ? C1 C6 1.507(4) . ? C2 C3 1.382(4) . ? C2 H2 0.9300 . ? C3 C4 1.384(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 C7 1.508(4) . ? C5 H5 0.9300 . ? C8 C9 1.376(4) . ? C8 C13 1.505(4) . ? C9 C10 1.382(4) . ? C9 H9 0.9300 . ? C10 C11 1.379(4) . ? C10 H10 0.9300 . ? C11 C12 1.380(4) . ? C11 C14 1.516(4) . ? C12 H12 0.9300 . ? C15 C16 1.379(4) . ? C15 C20 1.520(4) . ? C16 C17 1.388(4) . ? C16 H16 0.9300 . ? C17 C18 1.383(4) . ? C17 H17 0.9300 . ? C18 C19 1.384(4) . ? C18 C21 1.513(4) . ? C19 H19 0.9300 . ? C21 Sr1 3.018(3) 3_656 ? O21 H21A 0.851(10) . ? O21 H21B 0.857(10) . ? O22 H22A 0.8501 . ? O22 H22B 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 O16 105.65(8) . . ? O2 Sr1 O14 74.16(8) . . ? O16 Sr1 O14 73.75(10) . . ? O2 Sr1 O13 94.23(8) . . ? O16 Sr1 O13 135.61(10) . . ? O14 Sr1 O13 74.26(9) . . ? O2 Sr1 O11 86.36(7) . 1_455 ? O16 Sr1 O11 143.12(10) . 1_455 ? O14 Sr1 O11 142.73(7) . 1_455 ? O13 Sr1 O11 75.91(8) . 1_455 ? O2 Sr1 O15 90.64(9) . . ? O16 Sr1 O15 72.28(12) . . ? O14 Sr1 O15 137.12(11) . . ? O13 Sr1 O15 148.00(11) . . ? O11 Sr1 O15 72.86(10) 1_455 . ? O2 Sr1 O12 150.20(7) . 3_656 ? O16 Sr1 O12 72.97(9) . 3_656 ? O14 Sr1 O12 77.04(7) . 3_656 ? O13 Sr1 O12 70.46(7) . 3_656 ? O11 Sr1 O12 112.97(6) 1_455 3_656 ? O15 Sr1 O12 116.08(8) . 3_656 ? O2 Sr1 O11 160.35(6) . 3_656 ? O16 Sr1 O11 84.03(8) . 3_656 ? O14 Sr1 O11 125.40(7) . 3_656 ? O13 Sr1 O11 90.18(9) . 3_656 ? O11 Sr1 O11 76.15(7) 1_455 3_656 ? O15 Sr1 O11 75.83(9) . 3_656 ? O12 Sr1 O11 48.65(6) 3_656 3_656 ? O2 Sr1 C21 174.42(7) . 3_656 ? O16 Sr1 C21 74.99(8) . 3_656 ? O14 Sr1 C21 100.91(8) . 3_656 ? O13 Sr1 C21 81.77(8) . 3_656 ? O11 Sr1 C21 96.39(7) 1_455 3_656 ? O15 Sr1 C21 94.81(9) . 3_656 ? O12 Sr1 C21 24.39(7) 3_656 3_656 ? O11 Sr1 C21 24.49(7) 3_656 3_656 ? O2 Sr1 Sr1 125.12(5) . 3_556 ? O16 Sr1 Sr1 115.22(7) . 3_556 ? O14 Sr1 Sr1 150.39(6) . 3_556 ? O13 Sr1 Sr1 81.47(8) . 3_556 ? O11 Sr1 Sr1 39.31(4) 1_455 3_556 ? O15 Sr1 Sr1 70.02(9) . 3_556 ? O12 Sr1 Sr1 79.04(5) 3_656 3_556 ? O11 Sr1 Sr1 36.84(4) 3_656 3_556 ? C21 Sr1 Sr1 58.33(5) 3_656 3_556 ? O2 Sr1 H15B 103.8 . . ? O16 Sr1 H15B 77.7 . . ? O14 Sr1 H15B 149.5 . . ? O13 Sr1 H15B 135.7 . . ? O11 Sr1 H15B 65.5 1_455 . ? O15 Sr1 H15B 15.9 . . ? O12 Sr1 H15B 104.9 3_656 . ? O11 Sr1 H15B 60.9 3_656 . ? C21 Sr1 H15B 81.8 3_656 . ? Sr1 Sr1 H15B 55.0 3_556 . ? O17 Sr2 O20B 99.8(4) . . ? O17 Sr2 O7 72.64(8) . 4_566 ? O20B Sr2 O7 147.6(3) . 4_566 ? O17 Sr2 O18 95.34(12) . . ? O20B Sr2 O18 74.9(3) . . ? O7 Sr2 O18 74.52(8) 4_566 . ? O17 Sr2 O20 77.12(17) . . ? O20B Sr2 O20 23.4(3) . . ? O7 Sr2 O20 131.88(13) 4_566 . ? O18 Sr2 O20 72.01(12) . . ? O17 Sr2 O5 99.59(10) . . ? O20B Sr2 O5 127.4(3) . . ? O7 Sr2 O5 84.92(7) 4_566 . ? O18 Sr2 O5 149.65(8) . . ? O20 Sr2 O5 137.13(11) . . ? O17 Sr2 O10 152.67(8) . 1_455 ? O20B Sr2 O10 100.4(4) . 1_455 ? O7 Sr2 O10 80.42(7) 4_566 1_455 ? O18 Sr2 O10 72.64(9) . 1_455 ? O20 Sr2 O10 119.83(15) . 1_455 ? O5 Sr2 O10 82.24(6) . 1_455 ? O17 Sr2 O6 133.19(9) . . ? O20B Sr2 O6 83.5(4) . . ? O7 Sr2 O6 125.10(7) 4_566 . ? O18 Sr2 O6 129.81(9) . . ? O20 Sr2 O6 102.90(13) . . ? O5 Sr2 O6 48.75(5) . . ? O10 Sr2 O6 67.49(6) 1_455 . ? O17 Sr2 O19 66.53(10) . . ? O20B Sr2 O19 75.8(3) . . ? O7 Sr2 O19 125.30(9) 4_566 . ? O18 Sr2 O19 142.03(10) . . ? O20 Sr2 O19 71.50(13) . . ? O5 Sr2 O19 68.30(8) . . ? O10 Sr2 O19 136.75(8) 1_455 . ? O6 Sr2 O19 69.28(8) . . ? O17 Sr2 H17B 15.3(4) . . ? O20B Sr2 H17B 107.8(9) . . ? O7 Sr2 H17B 58.9(5) 4_566 . ? O18 Sr2 H17B 84.9(8) . . ? O20 Sr2 H17B 84.5(8) . . ? O5 Sr2 H17B 103.5(9) . . ? O10 Sr2 H17B 137.7(4) 1_455 . ? O6 Sr2 H17B 145.2(8) . . ? O19 Sr2 H17B 81.5(4) . . ? O5 Ni1 N1 92.62(8) . . ? O5 Ni1 O1 95.95(8) . . ? N1 Ni1 O1 79.40(8) . . ? O5 Ni1 N3 169.54(8) . . ? N1 Ni1 N3 93.17(9) . . ? O1 Ni1 N3 93.68(8) . . ? O5 Ni1 O9 91.03(7) . . ? N1 Ni1 O9 94.47(8) . . ? O1 Ni1 O9 170.89(8) . . ? N3 Ni1 O9 79.83(8) . . ? O5 Ni1 N2 79.19(8) . . ? N1 Ni1 N2 171.49(9) . . ? O1 Ni1 N2 98.98(8) . . ? N3 Ni1 N2 95.27(8) . . ? O9 Ni1 N2 88.06(8) . . ? C6 O1 Ni1 116.30(16) . . ? C6 O2 Sr1 143.70(19) . . ? C13 O5 Ni1 114.35(16) . . ? C13 O5 Sr2 95.97(15) . . ? Ni1 O5 Sr2 146.29(9) . . ? C13 O6 Sr2 92.19(15) . . ? C14 O7 Sr2 137.6(2) . 4_665 ? C20 O9 Ni1 115.41(16) . . ? C20 O10 Sr2 141.31(19) . 1_655 ? C21 O11 Sr1 142.28(19) . 1_655 ? C21 O11 Sr1 90.60(16) . 3_656 ? Sr1 O11 Sr1 103.85(7) 1_655 3_656 ? C21 O12 Sr1 95.57(16) . 3_656 ? Sr1 O13 H13A 113(3) . . ? Sr1 O13 H13B 125(3) . . ? H13A O13 H13B 107.2(16) . . ? Sr1 O14 H14A 126.7 . . ? Sr1 O14 H14B 123.0 . . ? H14A O14 H14B 109.9 . . ? Sr1 O15 H15A 144.4 . . ? Sr1 O15 H15B 107.3 . . ? H15A O15 H15B 107.2 . . ? Sr1 O16 H16A 113.9(17) . . ? Sr1 O16 H16B 113.1(17) . . ? H16A O16 H16B 111.6(17) . . ? Sr2 O17 H17A 118.3(17) . . ? Sr2 O17 H17B 114.7(17) . . ? H17A O17 H17B 108.3(16) . . ? Sr2 O18 H18A 112.4(13) . . ? Sr2 O18 H18B 123(3) . . ? H18A O18 H18B 112.1(17) . . ? Sr2 O19 H19A 133(3) . . ? Sr2 O19 H19B 108(3) . . ? H19A O19 H19B 108.9(17) . . ? Sr2 O20 H20A 122(4) . . ? Sr2 O20 H20B 123(4) . . ? H20A O20 H20B 110.5(18) . . ? Sr2 O20 H20C 98(3) . . ? H20A O20 H20C 33(6) . . ? H20B O20 H20C 139(5) . . ? Sr2 O20 H20D 101(4) . . ? H20A O20 H20D 94(5) . . ? H20B O20 H20D 95(6) . . ? H20C O20 H20D 76(2) . . ? Sr2 O20B H20A 110(3) . . ? Sr2 O20B H20C 116(2) . . ? H20A O20B H20C 34(10) . . ? Sr2 O20B H20D 116(2) . . ? H20A O20B H20D 86(9) . . ? H20C O20B H20D 109.6(18) . . ? C5 N1 C1 118.9(2) . . ? C5 N1 Ni1 127.41(18) . . ? C1 N1 Ni1 113.66(17) . . ? C8 N2 C12 118.4(2) . . ? C8 N2 Ni1 111.44(17) . . ? C12 N2 Ni1 128.89(18) . . ? C19 N3 C15 118.5(2) . . ? C19 N3 Ni1 128.14(18) . . ? C15 N3 Ni1 113.34(16) . . ? N1 C1 C2 121.8(2) . . ? N1 C1 C6 115.2(2) . . ? C2 C1 C6 123.0(2) . . ? C1 C2 C3 118.7(3) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 117.5(3) . . ? C5 C4 C7 119.1(2) . . ? C3 C4 C7 123.3(3) . . ? N1 C5 C4 123.2(2) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? O2 C6 O1 125.5(2) . . ? O2 C6 C1 119.1(2) . . ? O1 C6 C1 115.4(2) . . ? O4 C7 O3 125.0(3) . . ? O4 C7 C4 117.7(3) . . ? O3 C7 C4 117.3(3) . . ? N2 C8 C9 122.8(2) . . ? N2 C8 C13 115.2(2) . . ? C9 C8 C13 122.0(2) . . ? C8 C9 C10 118.0(3) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 117.8(3) . . ? C10 C11 C14 121.2(3) . . ? C12 C11 C14 121.1(3) . . ? N2 C12 C11 122.7(3) . . ? N2 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? O6 C13 O5 123.1(2) . . ? O6 C13 C8 120.9(2) . . ? O5 C13 C8 116.1(2) . . ? O7 C14 O8 126.9(3) . . ? O7 C14 C11 116.1(3) . . ? O8 C14 C11 116.9(3) . . ? N3 C15 C16 122.5(2) . . ? N3 C15 C20 115.0(2) . . ? C16 C15 C20 122.5(2) . . ? C15 C16 C17 118.4(2) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 118.3(2) . . ? C17 C18 C21 121.6(2) . . ? C19 C18 C21 120.0(2) . . ? N3 C19 C18 122.8(2) . . ? N3 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? O10 C20 O9 126.4(2) . . ? O10 C20 C15 117.2(2) . . ? O9 C20 C15 116.4(2) . . ? O11 C21 O12 123.9(2) . . ? O11 C21 C18 118.8(2) . . ? O12 C21 C18 117.3(2) . . ? O11 C21 Sr1 64.91(14) . 3_656 ? O12 C21 Sr1 60.04(13) . 3_656 ? C18 C21 Sr1 168.79(17) . 3_656 ? H21A O21 H21B 108.9(17) . . ? H22A O22 H22B 110.2 . . ? 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 O5 Ni1 O1 C6 -93.27(18) . . . . ? N1 Ni1 O1 C6 -1.71(18) . . . . ? N3 Ni1 O1 C6 90.84(19) . . . . ? O9 Ni1 O1 C6 46.6(6) . . . . ? N2 Ni1 O1 C6 -173.23(18) . . . . ? O16 Sr1 O2 C6 113.5(3) . . . . ? O14 Sr1 O2 C6 46.0(3) . . . . ? O13 Sr1 O2 C6 -26.4(3) . . . . ? O11 Sr1 O2 C6 -101.9(3) 1_455 . . . ? O15 Sr1 O2 C6 -174.7(3) . . . . ? O12 Sr1 O2 C6 30.6(4) 3_656 . . . ? O11 Sr1 O2 C6 -128.9(3) 3_656 . . . ? C21 Sr1 O2 C6 17.8(9) 3_656 . . . ? Sr1 Sr1 O2 C6 -108.9(3) 3_556 . . . ? N1 Ni1 O5 C13 164.97(18) . . . . ? O1 Ni1 O5 C13 -115.42(18) . . . . ? N3 Ni1 O5 C13 41.4(5) . . . . ? O9 Ni1 O5 C13 70.44(18) . . . . ? N2 Ni1 O5 C13 -17.38(18) . . . . ? N1 Ni1 O5 Sr2 12.83(17) . . . . ? O1 Ni1 O5 Sr2 92.45(16) . . . . ? N3 Ni1 O5 Sr2 -110.7(4) . . . . ? O9 Ni1 O5 Sr2 -81.69(16) . . . . ? N2 Ni1 O5 Sr2 -169.51(17) . . . . ? O17 Sr2 O5 C13 -141.06(16) . . . . ? O20B Sr2 O5 C13 -30.7(5) . . . . ? O7 Sr2 O5 C13 147.53(16) 4_566 . . . ? O18 Sr2 O5 C13 100.6(2) . . . . ? O20 Sr2 O5 C13 -59.7(3) . . . . ? O10 Sr2 O5 C13 66.53(15) 1_455 . . . ? O6 Sr2 O5 C13 -0.25(14) . . . . ? O19 Sr2 O5 C13 -81.19(16) . . . . ? O17 Sr2 O5 Ni1 13.59(17) . . . . ? O20B Sr2 O5 Ni1 123.9(5) . . . . ? O7 Sr2 O5 Ni1 -57.82(17) 4_566 . . . ? O18 Sr2 O5 Ni1 -104.8(2) . . . . ? O20 Sr2 O5 Ni1 94.9(3) . . . . ? O10 Sr2 O5 Ni1 -138.82(17) 1_455 . . . ? O6 Sr2 O5 Ni1 154.4(2) . . . . ? O19 Sr2 O5 Ni1 73.46(17) . . . . ? O17 Sr2 O6 C13 59.0(2) . . . . ? O20B Sr2 O6 C13 156.3(3) . . . . ? O7 Sr2 O6 C13 -40.23(19) 4_566 . . . ? O18 Sr2 O6 C13 -139.49(16) . . . . ? O20 Sr2 O6 C13 143.3(2) . . . . ? O5 Sr2 O6 C13 0.26(14) . . . . ? O10 Sr2 O6 C13 -99.47(16) 1_455 . . . ? O19 Sr2 O6 C13 79.07(17) . . . . ? O5 Ni1 O9 C20 -174.56(19) . . . . ? N1 Ni1 O9 C20 92.74(19) . . . . ? O1 Ni1 O9 C20 45.3(6) . . . . ? N3 Ni1 O9 C20 0.31(19) . . . . ? N2 Ni1 O9 C20 -95.40(19) . . . . ? O5 Ni1 N1 C5 -83.9(2) . . . . ? O1 Ni1 N1 C5 -179.4(2) . . . . ? N3 Ni1 N1 C5 87.4(2) . . . . ? O9 Ni1 N1 C5 7.4(2) . . . . ? N2 Ni1 N1 C5 -99.7(6) . . . . ? O5 Ni1 N1 C1 97.34(19) . . . . ? O1 Ni1 N1 C1 1.77(18) . . . . ? N3 Ni1 N1 C1 -91.38(19) . . . . ? O9 Ni1 N1 C1 -171.42(18) . . . . ? N2 Ni1 N1 C1 81.6(6) . . . . ? O5 Ni1 N2 C8 15.65(18) . . . . ? N1 Ni1 N2 C8 31.7(7) . . . . ? O1 Ni1 N2 C8 110.05(18) . . . . ? N3 Ni1 N2 C8 -155.38(18) . . . . ? O9 Ni1 N2 C8 -75.78(18) . . . . ? O5 Ni1 N2 C12 -177.8(2) . . . . ? N1 Ni1 N2 C12 -161.8(5) . . . . ? O1 Ni1 N2 C12 -83.4(2) . . . . ? N3 Ni1 N2 C12 11.2(2) . . . . ? O9 Ni1 N2 C12 90.8(2) . . . . ? O5 Ni1 N3 C19 -153.5(4) . . . . ? N1 Ni1 N3 C19 83.0(2) . . . . ? O1 Ni1 N3 C19 3.5(2) . . . . ? O9 Ni1 N3 C19 177.0(2) . . . . ? N2 Ni1 N3 C19 -95.9(2) . . . . ? O5 Ni1 N3 C15 28.5(5) . . . . ? N1 Ni1 N3 C15 -94.98(18) . . . . ? O1 Ni1 N3 C15 -174.55(17) . . . . ? O9 Ni1 N3 C15 -1.00(17) . . . . ? N2 Ni1 N3 C15 86.07(18) . . . . ? C5 N1 C1 C2 -1.6(4) . . . . ? Ni1 N1 C1 C2 177.3(2) . . . . ? C5 N1 C1 C6 179.5(2) . . . . ? Ni1 N1 C1 C6 -1.6(3) . . . . ? N1 C1 C2 C3 1.6(5) . . . . ? C6 C1 C2 C3 -179.5(3) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C2 C3 C4 C7 179.6(3) . . . . ? C1 N1 C5 C4 0.5(4) . . . . ? Ni1 N1 C5 C4 -178.2(2) . . . . ? C3 C4 C5 N1 0.4(4) . . . . ? C7 C4 C5 N1 -179.6(3) . . . . ? Sr1 O2 C6 O1 56.5(5) . . . . ? Sr1 O2 C6 C1 -123.2(3) . . . . ? Ni1 O1 C6 O2 -178.4(2) . . . . ? Ni1 O1 C6 C1 1.3(3) . . . . ? N1 C1 C6 O2 180.0(2) . . . . ? C2 C1 C6 O2 1.0(4) . . . . ? N1 C1 C6 O1 0.2(3) . . . . ? C2 C1 C6 O1 -178.7(3) . . . . ? C5 C4 C7 O4 -13.1(5) . . . . ? C3 C4 C7 O4 166.9(3) . . . . ? C5 C4 C7 O3 168.0(3) . . . . ? C3 C4 C7 O3 -12.0(5) . . . . ? C12 N2 C8 C9 -1.2(4) . . . . ? Ni1 N2 C8 C9 166.9(2) . . . . ? C12 N2 C8 C13 179.5(2) . . . . ? Ni1 N2 C8 C13 -12.4(3) . . . . ? N2 C8 C9 C10 0.2(5) . . . . ? C13 C8 C9 C10 179.5(3) . . . . ? C8 C9 C10 C11 0.8(5) . . . . ? C9 C10 C11 C12 -0.8(5) . . . . ? C9 C10 C11 C14 179.5(3) . . . . ? C8 N2 C12 C11 1.2(4) . . . . ? Ni1 N2 C12 C11 -164.6(2) . . . . ? C10 C11 C12 N2 -0.2(4) . . . . ? C14 C11 C12 N2 179.6(3) . . . . ? Sr2 O6 C13 O5 -0.5(3) . . . . ? Sr2 O6 C13 C8 179.4(2) . . . . ? Ni1 O5 C13 O6 -164.4(2) . . . . ? Sr2 O5 C13 O6 0.5(3) . . . . ? Ni1 O5 C13 C8 15.8(3) . . . . ? Sr2 O5 C13 C8 -179.35(19) . . . . ? N2 C8 C13 O6 178.2(2) . . . . ? C9 C8 C13 O6 -1.1(4) . . . . ? N2 C8 C13 O5 -1.9(3) . . . . ? C9 C8 C13 O5 178.7(3) . . . . ? Sr2 O7 C14 O8 14.8(6) 4_665 . . . ? Sr2 O7 C14 C11 -165.0(2) 4_665 . . . ? C10 C11 C14 O7 7.5(4) . . . . ? C12 C11 C14 O7 -172.3(3) . . . . ? C10 C11 C14 O8 -172.4(3) . . . . ? C12 C11 C14 O8 7.9(4) . . . . ? C19 N3 C15 C16 1.2(4) . . . . ? Ni1 N3 C15 C16 179.4(2) . . . . ? C19 N3 C15 C20 -176.8(2) . . . . ? Ni1 N3 C15 C20 1.5(3) . . . . ? N3 C15 C16 C17 -1.4(4) . . . . ? C20 C15 C16 C17 176.4(2) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C16 C17 C18 C19 1.8(4) . . . . ? C16 C17 C18 C21 -177.5(2) . . . . ? C15 N3 C19 C18 0.6(4) . . . . ? Ni1 N3 C19 C18 -177.30(19) . . . . ? C17 C18 C19 N3 -2.1(4) . . . . ? C21 C18 C19 N3 177.2(2) . . . . ? Sr2 O10 C20 O9 97.7(3) 1_655 . . . ? Sr2 O10 C20 C15 -82.8(3) 1_655 . . . ? Ni1 O9 C20 O10 179.9(2) . . . . ? Ni1 O9 C20 C15 0.4(3) . . . . ? N3 C15 C20 O10 179.2(2) . . . . ? C16 C15 C20 O10 1.2(4) . . . . ? N3 C15 C20 O9 -1.3(3) . . . . ? C16 C15 C20 O9 -179.2(3) . . . . ? Sr1 O11 C21 O12 -102.4(3) 1_655 . . . ? Sr1 O11 C21 O12 11.5(3) 3_656 . . . ? Sr1 O11 C21 C18 78.0(4) 1_655 . . . ? Sr1 O11 C21 C18 -168.1(2) 3_656 . . . ? Sr1 O11 C21 Sr1 -113.9(3) 1_655 . . 3_656 ? Sr1 O12 C21 O11 -12.0(3) 3_656 . . . ? Sr1 O12 C21 C18 167.59(19) 3_656 . . . ? C17 C18 C21 O11 4.4(4) . . . . ? C19 C18 C21 O11 -174.8(3) . . . . ? C17 C18 C21 O12 -175.2(3) . . . . ? C19 C18 C21 O12 5.5(4) . . . . ? C17 C18 C21 Sr1 -101.9(9) . . . 3_656 ? C19 C18 C21 Sr1 78.8(10) . . . 3_656 ? 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 O13 H13A O21 0.860(10) 1.831(13) 2.686(4) 172(4) . O13 H13B O14 0.857(10) 2.43(3) 3.091(4) 135(3) 3_656 O14 H14A O12 0.85 1.93 2.773(3) 171.7 . O14 H14B O6 0.85 1.91 2.761(3) 176.5 4_666 O15 H15A O6 0.85 2.58 3.295(3) 142.9 4_566 O15 H15B O13 0.85 2.15 2.993(5) 172.2 3_556 O16 H16A O10 0.842(10) 1.97(3) 2.717(3) 147(5) 4_566 O16 H16B O22 0.841(10) 2.223(13) 3.043(5) 165(4) 2_546 O17 H17A O4 0.854(10) 1.884(10) 2.733(3) 172(2) 3_666 O17 H17B O8 0.860(10) 1.938(16) 2.730(4) 153(3) 4_566 O18 H18A O4 0.839(10) 2.007(10) 2.791(3) 155.0(19) 1_455 O18 H18B O22 0.842(10) 2.117(18) 2.881(5) 151(3) 3_566 O19 H19A O9 0.851(10) 2.52(3) 3.239(4) 143(4) . O19 H19B O3 0.850(10) 2.117(13) 2.960(4) 172(5) 3_666 O20 H20B O8 0.848(10) 2.083(19) 2.914(6) 167(6) 2 O20 H20A O21 0.846(10) 1.96(2) 2.779(5) 163(6) 2 O20 H20B O8 0.848(10) 2.083(19) 2.914(6) 167(6) 2 O20B H20C O21 0.849(10) 2.11(3) 2.929(11) 161(8) 2 O20B H20D O22 0.851(10) 1.93(7) 2.699(11) 149(13) 3_566 O21 H21A O1 0.851(10) 1.942(11) 2.784(3) 170(4) . O21 H21B O3 0.857(10) 1.884(16) 2.700(4) 159(4) 4_565 O22 H22A O3 0.85 1.93 2.692(4) 149.2 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.227 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 943750' ####################################################################### # # 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_t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H16 N2 O13 Sr Zn' _chemical_formula_sum 'C14 H16 N2 O13 Sr Zn' _chemical_formula_weight 573.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 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 7.917(4) _cell_length_b 10.835(5) _cell_length_c 20.769(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.825(10) _cell_angle_gamma 90.00 _cell_volume 1779.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4148 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.46 _exptl_crystal_description platy _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 4.427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3703 _exptl_absorpt_correction_T_max 0.4041 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9911 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_unetI/netI 0.0304 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3463 _reflns_number_gt 2891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, the command 'omit -2 52' was used to omit the reflections above 52 degree.Hydrogen atoms of the water molecule O12 were not observed nor calculated. ; _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^)+(0.0705P)^2^+1.3983P] 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 3463 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Zn1 Zn -0.12665(5) 0.33022(4) 0.031978(19) 0.02026(15) Uani 1 1 d . . . C1 C 0.0750(5) 0.1503(3) -0.02592(17) 0.0180(7) Uani 1 1 d . . . O1 O -0.1293(4) 0.2934(3) -0.06394(12) 0.0270(6) Uani 1 1 d . . . N1 N 0.0532(4) 0.1959(3) 0.03273(14) 0.0171(6) Uani 1 1 d . . . Sr1 Sr 0.48342(5) 0.24448(3) 0.249120(15) 0.02703(14) Uani 1 1 d . . . C2 C 0.1895(5) 0.0579(4) -0.03654(17) 0.0205(8) Uani 1 1 d . . . H2 H 0.2035 0.0279 -0.0779 0.025 Uiso 1 1 calc R . . N2 N -0.2223(4) 0.5081(3) 0.02026(14) 0.0179(6) Uani 1 1 d . . . O2 O -0.0132(4) 0.1715(3) -0.13494(12) 0.0302(7) Uani 1 1 d . . . C3 C 0.2829(5) 0.0109(4) 0.01563(17) 0.0209(8) Uani 1 1 d . . . H3 H 0.3602 -0.0523 0.0099 0.025 Uiso 1 1 calc R . . O3 O 0.4575(5) -0.0773(3) 0.12559(15) 0.0508(10) Uani 1 1 d . . . C4 C 0.2612(4) 0.0580(3) 0.07630(16) 0.0181(7) Uani 1 1 d . . . O4 O 0.3442(4) 0.0643(3) 0.18687(13) 0.0336(7) Uani 1 1 d . . . C5 C 0.1451(5) 0.1511(3) 0.08273(17) 0.0194(8) Uani 1 1 d . . . H5 H 0.1303 0.1839 0.1235 0.023 Uiso 1 1 calc R . . O5 O -0.0387(4) 0.4076(3) 0.11686(12) 0.0281(6) Uani 1 1 d . . . C6 C -0.0305(5) 0.2080(4) -0.08046(17) 0.0196(8) Uani 1 1 d . . . O6 O -0.0922(4) 0.5626(3) 0.18156(12) 0.0309(7) Uani 1 1 d . . . C7 C 0.3648(5) 0.0102(4) 0.13424(17) 0.0251(8) Uani 1 1 d . . . O7 O -0.6704(3) 0.7514(2) -0.06633(14) 0.0246(6) Uani 1 1 d . . . C8 C -0.2306(4) 0.5594(3) 0.07863(16) 0.0161(7) Uani 1 1 d . . . O8 O -0.4770(4) 0.6859(3) -0.13056(13) 0.0380(8) Uani 1 1 d . . . C9 C -0.3397(5) 0.6537(3) 0.09004(17) 0.0198(8) Uani 1 1 d . . . H9 H -0.3443 0.6875 0.1311 0.024 Uiso 1 1 calc R . . O9 O 0.2038(5) 0.1640(3) 0.31548(17) 0.0479(9) Uani 1 1 d . . . H9A H 0.0972 0.1568 0.3096 0.072 Uiso 1 1 d R . . H9B H 0.2298 0.1572 0.3555 0.072 Uiso 1 1 d R . . C10 C -0.4426(5) 0.6978(3) 0.03999(18) 0.0202(8) Uani 1 1 d . . . H10 H -0.5217 0.7591 0.0472 0.024 Uiso 1 1 calc R . . O10 O 0.7478(6) 0.1489(5) 0.1911(2) 0.0783(15) Uani 1 1 d . . . H10B H 0.7291 0.1659 0.1514 0.117 Uiso 1 1 d R . . H10A H 0.7874 0.0769 0.1980 0.117 Uiso 1 1 d R . . C11 C -0.4273(4) 0.6506(3) -0.02051(16) 0.0172(7) Uani 1 1 d . . . O11 O 0.8080(6) 0.3420(5) 0.2769(2) 0.0763(14) Uani 1 1 d . . . H11A H 0.8768 0.3582 0.3085 0.092 Uiso 1 1 d R . . H11B H 0.8100 0.4101 0.2566 0.092 Uiso 1 1 d R . . C12 C -0.3152(4) 0.5553(3) -0.02878(16) 0.0175(7) Uani 1 1 d . . . H12 H -0.3042 0.5231 -0.0699 0.021 Uiso 1 1 calc R . . O12 O 0.5110(6) 0.4888(4) 0.2467(2) 0.0854(17) Uani 1 1 d . . . C13 C -0.1114(5) 0.5071(3) 0.13104(17) 0.0210(8) Uani 1 1 d . . . O13 O 0.1857(5) 0.3599(4) 0.22745(17) 0.0524(10) Uani 1 1 d . . . H13A H 0.1304 0.3626 0.1914 0.063 Uiso 1 1 d R . . H13B H 0.1806 0.4282 0.2474 0.063 Uiso 1 1 d R . . C14 C -0.5321(5) 0.6990(3) -0.07785(17) 0.0180(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 Zn1 0.0217(2) 0.0202(3) 0.0187(2) -0.00275(17) -0.00061(16) 0.00508(18) C1 0.0168(18) 0.0158(18) 0.0217(18) 0.0007(14) 0.0037(14) -0.0020(14) O1 0.0337(16) 0.0291(15) 0.0181(13) -0.0015(11) -0.0009(11) 0.0121(13) N1 0.0182(15) 0.0158(15) 0.0173(14) -0.0005(12) 0.0004(11) 0.0012(13) Sr1 0.0456(3) 0.0222(2) 0.0130(2) 0.00123(13) -0.00070(16) 0.00272(17) C2 0.0225(19) 0.0201(19) 0.0193(17) -0.0017(14) 0.0042(14) 0.0013(16) N2 0.0187(15) 0.0161(16) 0.0190(14) -0.0013(12) 0.0009(11) 0.0018(12) O2 0.0432(18) 0.0312(16) 0.0163(13) 0.0008(11) 0.0026(12) 0.0098(14) C3 0.0226(19) 0.0163(19) 0.0239(18) -0.0030(15) 0.0027(14) 0.0046(15) O3 0.064(2) 0.054(2) 0.0326(17) -0.0092(16) -0.0148(15) 0.0436(19) C4 0.0191(18) 0.0153(18) 0.0199(17) 0.0012(14) 0.0020(14) 0.0003(15) O4 0.0469(18) 0.0320(16) 0.0211(13) -0.0064(12) -0.0068(12) 0.0074(15) C5 0.0206(19) 0.0194(19) 0.0180(17) -0.0056(14) -0.0013(14) 0.0008(15) O5 0.0341(16) 0.0245(15) 0.0243(14) -0.0078(11) -0.0124(11) 0.0124(13) C6 0.024(2) 0.0168(18) 0.0186(18) 0.0002(15) 0.0045(15) -0.0008(16) O6 0.0452(18) 0.0274(16) 0.0191(13) -0.0096(11) -0.0095(12) 0.0079(14) C7 0.026(2) 0.026(2) 0.0226(19) -0.0040(16) -0.0035(15) 0.0021(18) O7 0.0213(14) 0.0268(16) 0.0260(14) 0.0071(11) 0.0023(11) 0.0073(12) C8 0.0169(17) 0.0141(17) 0.0175(16) 0.0006(13) 0.0008(13) 0.0007(14) O8 0.0450(19) 0.052(2) 0.0179(14) 0.0095(13) 0.0063(13) 0.0223(16) C9 0.0249(19) 0.0178(19) 0.0170(17) -0.0054(14) 0.0024(14) -0.0016(16) O9 0.046(2) 0.056(2) 0.0406(19) -0.0026(16) -0.0054(15) -0.0107(18) C10 0.024(2) 0.0129(18) 0.0243(19) 0.0006(14) 0.0024(15) 0.0045(15) O10 0.071(3) 0.109(4) 0.055(2) 0.045(2) 0.013(2) 0.049(3) C11 0.0161(17) 0.0159(18) 0.0196(17) 0.0034(14) 0.0025(14) -0.0020(14) O11 0.071(3) 0.101(4) 0.057(3) 0.008(2) -0.002(2) -0.019(3) C12 0.0178(17) 0.0187(18) 0.0160(16) -0.0019(14) 0.0004(13) -0.0022(15) O12 0.104(4) 0.053(3) 0.094(4) 0.024(2) -0.048(3) -0.022(2) C13 0.0198(19) 0.020(2) 0.0226(18) -0.0033(15) -0.0025(14) 0.0000(16) O13 0.062(2) 0.054(2) 0.0412(19) -0.0077(16) -0.0050(17) 0.0227(19) C14 0.0194(19) 0.0151(18) 0.0195(18) 0.0005(14) 0.0012(14) -0.0001(15) _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 Zn1 O7 1.996(3) 3_465 ? Zn1 O1 2.031(3) . ? Zn1 N1 2.036(3) . ? Zn1 O5 2.043(3) . ? Zn1 N2 2.081(3) . ? C1 N1 1.333(5) . ? C1 C2 1.376(5) . ? C1 C6 1.509(5) . ? O1 C6 1.269(5) . ? N1 C5 1.330(5) . ? Sr1 O4 2.561(3) . ? Sr1 O6 2.564(3) 2_545 ? Sr1 O2 2.573(3) 4_666 ? Sr1 O8 2.573(3) 3_565 ? Sr1 O12 2.657(5) . ? Sr1 O10 2.675(4) . ? Sr1 O13 2.686(4) . ? Sr1 O9 2.804(4) . ? Sr1 O11 2.812(5) . ? C2 C3 1.379(5) . ? C2 H2 0.9300 . ? N2 C12 1.329(5) . ? N2 C8 1.338(4) . ? O2 C6 1.213(4) . ? O2 Sr1 2.573(3) 4_565 ? C3 C4 1.378(5) . ? C3 H3 0.9300 . ? O3 C7 1.218(5) . ? C4 C5 1.376(5) . ? C4 C7 1.514(5) . ? O4 C7 1.258(4) . ? C5 H5 0.9300 . ? O5 C13 1.264(4) . ? O6 C13 1.212(4) . ? O6 Sr1 2.564(3) 2 ? O7 C14 1.267(5) . ? O7 Zn1 1.996(3) 3_465 ? C8 C9 1.366(5) . ? C8 C13 1.516(5) . ? O8 C14 1.206(4) . ? O8 Sr1 2.573(3) 3_565 ? C9 C10 1.375(5) . ? C9 H9 0.9300 . ? O9 H9A 0.8500 . ? O9 H9B 0.8498 . ? C10 C11 1.368(5) . ? C10 H10 0.9300 . ? O10 H10B 0.8501 . ? O10 H10A 0.8501 . ? C11 C12 1.378(5) . ? C11 C14 1.511(5) . ? O11 H11A 0.8500 . ? O11 H11B 0.8501 . ? C12 H12 0.9300 . ? O13 H13A 0.8500 . ? O13 H13B 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O1 107.09(12) 3_465 . ? O7 Zn1 N1 104.79(12) 3_465 . ? O1 Zn1 N1 80.81(11) . . ? O7 Zn1 O5 96.86(12) 3_465 . ? O1 Zn1 O5 156.01(12) . . ? N1 Zn1 O5 94.47(11) . . ? O7 Zn1 N2 99.07(11) 3_465 . ? O1 Zn1 N2 94.66(12) . . ? N1 Zn1 N2 156.01(12) . . ? O5 Zn1 N2 80.08(11) . . ? N1 C1 C2 122.1(3) . . ? N1 C1 C6 116.2(3) . . ? C2 C1 C6 121.7(3) . . ? C6 O1 Zn1 115.6(2) . . ? C5 N1 C1 119.2(3) . . ? C5 N1 Zn1 128.5(2) . . ? C1 N1 Zn1 112.3(2) . . ? O4 Sr1 O6 79.74(10) . 2_545 ? O4 Sr1 O2 136.59(9) . 4_666 ? O6 Sr1 O2 76.04(10) 2_545 4_666 ? O4 Sr1 O8 75.69(11) . 3_565 ? O6 Sr1 O8 138.82(9) 2_545 3_565 ? O2 Sr1 O8 142.24(11) 4_666 3_565 ? O4 Sr1 O12 141.60(11) . . ? O6 Sr1 O12 138.66(11) 2_545 . ? O2 Sr1 O12 70.64(11) 4_666 . ? O8 Sr1 O12 71.78(12) 3_565 . ? O4 Sr1 O10 78.70(14) . . ? O6 Sr1 O10 72.96(11) 2_545 . ? O2 Sr1 O10 125.91(12) 4_666 . ? O8 Sr1 O10 70.19(11) 3_565 . ? O12 Sr1 O10 108.06(16) . . ? O4 Sr1 O13 85.30(11) . . ? O6 Sr1 O13 136.01(11) 2_545 . ? O2 Sr1 O13 87.74(10) 4_666 . ? O8 Sr1 O13 74.19(10) 3_565 . ? O12 Sr1 O13 66.75(14) . . ? O10 Sr1 O13 143.53(12) . . ? O4 Sr1 O9 71.37(10) . . ? O6 Sr1 O9 74.73(10) 2_545 . ? O2 Sr1 O9 67.79(10) 4_666 . ? O8 Sr1 O9 125.64(11) 3_565 . ? O12 Sr1 O9 112.77(13) . . ? O10 Sr1 O9 139.07(14) . . ? O13 Sr1 O9 61.29(12) . . ? O4 Sr1 O11 139.15(12) . . ? O6 Sr1 O11 83.99(12) 2_545 . ? O2 Sr1 O11 73.01(11) 4_666 . ? O8 Sr1 O11 93.49(12) 3_565 . ? O12 Sr1 O11 63.53(15) . . ? O10 Sr1 O11 60.70(16) . . ? O13 Sr1 O11 130.15(15) . . ? O9 Sr1 O11 138.74(11) . . ? C1 C2 C3 118.3(3) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C12 N2 C8 119.0(3) . . ? C12 N2 Zn1 129.1(3) . . ? C8 N2 Zn1 108.2(2) . . ? C6 O2 Sr1 139.6(3) . 4_565 ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 118.3(3) . . ? C5 C4 C7 120.8(3) . . ? C3 C4 C7 120.9(3) . . ? C7 O4 Sr1 136.3(3) . . ? N1 C5 C4 122.3(3) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C13 O5 Zn1 114.3(2) . . ? O2 C6 O1 126.1(4) . . ? O2 C6 C1 118.8(3) . . ? O1 C6 C1 115.1(3) . . ? C13 O6 Sr1 153.0(3) . 2 ? O3 C7 O4 126.6(4) . . ? O3 C7 C4 117.1(3) . . ? O4 C7 C4 116.3(3) . . ? C14 O7 Zn1 125.9(2) . 3_465 ? N2 C8 C9 121.9(3) . . ? N2 C8 C13 116.0(3) . . ? C9 C8 C13 122.1(3) . . ? C14 O8 Sr1 147.4(3) . 3_565 ? C8 C9 C10 119.0(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? Sr1 O9 H9A 139.5 . . ? Sr1 O9 H9B 110.4 . . ? H9A O9 H9B 108.9 . . ? C11 C10 C9 119.3(3) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? Sr1 O10 H10B 104.5 . . ? Sr1 O10 H10A 124.6 . . ? H10B O10 H10A 114.2 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 C14 121.6(3) . . ? C12 C11 C14 119.6(3) . . ? Sr1 O11 H11A 141.3 . . ? Sr1 O11 H11B 105.3 . . ? H11A O11 H11B 100.2 . . ? N2 C12 C11 121.9(3) . . ? N2 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? O6 C13 O5 125.9(4) . . ? O6 C13 C8 118.9(3) . . ? O5 C13 C8 115.3(3) . . ? Sr1 O13 H13A 125.0 . . ? Sr1 O13 H13B 112.8 . . ? H13A O13 H13B 111.3 . . ? O8 C14 O7 125.3(3) . . ? O8 C14 C11 117.7(3) . . ? O7 C14 C11 116.9(3) . . ? 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 O7 Zn1 O1 C6 -101.0(3) 3_465 . . . ? N1 Zn1 O1 C6 1.8(3) . . . . ? O5 Zn1 O1 C6 82.0(4) . . . . ? N2 Zn1 O1 C6 158.0(3) . . . . ? C2 C1 N1 C5 0.2(5) . . . . ? C6 C1 N1 C5 -178.5(3) . . . . ? C2 C1 N1 Zn1 -179.5(3) . . . . ? C6 C1 N1 Zn1 1.9(4) . . . . ? O7 Zn1 N1 C5 -76.2(3) 3_465 . . . ? O1 Zn1 N1 C5 178.5(3) . . . . ? O5 Zn1 N1 C5 22.1(3) . . . . ? N2 Zn1 N1 C5 97.7(4) . . . . ? O7 Zn1 N1 C1 103.5(3) 3_465 . . . ? O1 Zn1 N1 C1 -1.9(3) . . . . ? O5 Zn1 N1 C1 -158.2(3) . . . . ? N2 Zn1 N1 C1 -82.7(4) . . . . ? N1 C1 C2 C3 0.6(6) . . . . ? C6 C1 C2 C3 179.1(3) . . . . ? O7 Zn1 N2 C12 -84.0(3) 3_465 . . . ? O1 Zn1 N2 C12 24.1(3) . . . . ? N1 Zn1 N2 C12 102.0(4) . . . . ? O5 Zn1 N2 C12 -179.5(3) . . . . ? O7 Zn1 N2 C8 73.6(2) 3_465 . . . ? O1 Zn1 N2 C8 -178.3(2) . . . . ? N1 Zn1 N2 C8 -100.5(3) . . . . ? O5 Zn1 N2 C8 -21.9(2) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C2 C3 C4 C5 0.3(6) . . . . ? C2 C3 C4 C7 -178.6(4) . . . . ? O6 Sr1 O4 C7 -107.5(4) 2_545 . . . ? O2 Sr1 O4 C7 -164.3(3) 4_666 . . . ? O8 Sr1 O4 C7 39.2(4) 3_565 . . . ? O12 Sr1 O4 C7 71.9(4) . . . . ? O10 Sr1 O4 C7 -33.0(4) . . . . ? O13 Sr1 O4 C7 114.0(4) . . . . ? O9 Sr1 O4 C7 175.3(4) . . . . ? O11 Sr1 O4 C7 -39.3(4) . . . . ? C1 N1 C5 C4 -0.7(5) . . . . ? Zn1 N1 C5 C4 178.9(3) . . . . ? C3 C4 C5 N1 0.5(6) . . . . ? C7 C4 C5 N1 179.4(3) . . . . ? O7 Zn1 O5 C13 -81.2(3) 3_465 . . . ? O1 Zn1 O5 C13 95.9(4) . . . . ? N1 Zn1 O5 C13 173.3(3) . . . . ? N2 Zn1 O5 C13 16.8(3) . . . . ? Sr1 O2 C6 O1 34.6(7) 4_565 . . . ? Sr1 O2 C6 C1 -144.4(3) 4_565 . . . ? Zn1 O1 C6 O2 179.7(3) . . . . ? Zn1 O1 C6 C1 -1.3(4) . . . . ? N1 C1 C6 O2 178.7(3) . . . . ? C2 C1 C6 O2 0.0(5) . . . . ? N1 C1 C6 O1 -0.4(5) . . . . ? C2 C1 C6 O1 -179.1(4) . . . . ? Sr1 O4 C7 O3 89.0(6) . . . . ? Sr1 O4 C7 C4 -92.2(4) . . . . ? C5 C4 C7 O3 175.6(4) . . . . ? C3 C4 C7 O3 -5.6(6) . . . . ? C5 C4 C7 O4 -3.3(5) . . . . ? C3 C4 C7 O4 175.5(4) . . . . ? C12 N2 C8 C9 4.2(5) . . . . ? Zn1 N2 C8 C9 -156.0(3) . . . . ? C12 N2 C8 C13 -175.5(3) . . . . ? Zn1 N2 C8 C13 24.3(4) . . . . ? N2 C8 C9 C10 -0.6(5) . . . . ? C13 C8 C9 C10 179.0(3) . . . . ? C8 C9 C10 C11 -3.2(5) . . . . ? C9 C10 C11 C12 3.5(5) . . . . ? C9 C10 C11 C14 -177.6(3) . . . . ? C8 N2 C12 C11 -4.0(5) . . . . ? Zn1 N2 C12 C11 151.6(3) . . . . ? C10 C11 C12 N2 0.1(5) . . . . ? C14 C11 C12 N2 -178.8(3) . . . . ? Sr1 O6 C13 O5 109.0(6) 2 . . . ? Sr1 O6 C13 C8 -70.2(7) 2 . . . ? Zn1 O5 C13 O6 172.3(3) . . . . ? Zn1 O5 C13 C8 -8.4(4) . . . . ? N2 C8 C13 O6 167.6(3) . . . . ? C9 C8 C13 O6 -12.1(5) . . . . ? N2 C8 C13 O5 -11.7(5) . . . . ? C9 C8 C13 O5 168.6(3) . . . . ? Sr1 O8 C14 O7 19.2(8) 3_565 . . . ? Sr1 O8 C14 C11 -160.0(4) 3_565 . . . ? Zn1 O7 C14 O8 113.7(4) 3_465 . . . ? Zn1 O7 C14 C11 -67.1(4) 3_465 . . . ? C10 C11 C14 O8 155.5(4) . . . . ? C12 C11 C14 O8 -25.6(5) . . . . ? C10 C11 C14 O7 -23.7(5) . . . . ? C12 C11 C14 O7 155.3(3) . . . . ? 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 O9 H9A O12 0.85 2.31 2.819(6) 119.2 2_545 O9 H9B O1 0.85 2.04 2.812(5) 151.3 4_666 O10 H10B O7 0.85 2.01 2.845(5) 165.5 3_565 O10 H10B O8 0.85 2.58 3.019(5) 113.2 3_565 O10 H10A O12 0.85 2.14 2.843(6) 139.3 2_645 O11 H11A O3 0.85 1.98 2.818(6) 170.3 2_655 O11 H11B O6 0.85 2.42 3.227(6) 157.6 1_655 O13 H13A O5 0.85 2.05 2.880(5) 163.9 . O13 H13B O4 0.85 2.03 2.858(5) 166.0 2 C9 H9 O11 0.93 2.55 3.434(6) 159.8 2 C5 H5 O4 0.93 2.46 2.777(5) 99.9 . C10 H10 O3 0.93 2.42 3.140(5) 134.5 1_465 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.486 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 943751' ####################################################################### # # 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_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H29 N3 O22 Sr2 Zn, 2(H2 O)' _chemical_formula_sum 'C21 H33 N3 O24 Sr2 Zn' _chemical_formula_weight 952.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 b c a' _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' '-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 16.484(3) _cell_length_b 14.875(3) _cell_length_c 26.826(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6578(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 2.385 _cell_measurement_theta_max 28.258 _exptl_crystal_description platy _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3824 _exptl_absorpt_coefficient_mu 4.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2362 _exptl_absorpt_correction_T_max 0.4975 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26177 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0272 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5761 _reflns_number_gt 4812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, the command 'omit -3 50' was used to omit the reflections above 50 degree. Hydrogen aotms of disorder water molecular O13 and O13' were not obserbed nor calculated. The command 'EADP' were used to constrain the disorder atoms o13 and o13' have the same environment. SADI distance restraints were used for the Sr1 O13, Sr1 O13' Sr1 o15. Dang distance restraint was used for H15A and H15B. ; _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^)+(0.0275P)^2^+4.7966P] 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 5761 _refine_ls_number_parameters 463 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr -0.099854(17) 0.42837(2) 0.073307(10) 0.02109(8) Uani 1 1 d D . . N1 N 0.17333(14) 0.63541(18) 0.23020(9) 0.0219(6) Uani 1 1 d . . . O1 O 0.24116(14) 0.60763(16) 0.31891(8) 0.0312(5) Uani 1 1 d . . . C1 C 0.13999(18) 0.5731(2) 0.25988(11) 0.0235(7) Uani 1 1 d . . . Sr2 Sr 0.016205(17) 0.17986(2) 0.052988(10) 0.02203(8) Uani 1 1 d . . . N2 N 0.36374(15) 0.76130(19) 0.31578(9) 0.0245(6) Uani 1 1 d . . . O2 O 0.13915(15) 0.51907(19) 0.34269(9) 0.0431(7) Uani 1 1 d . . . C2 C 0.0788(2) 0.5170(2) 0.24388(12) 0.0351(8) Uani 1 1 d . . . H2 H 0.0563 0.4748 0.2654 0.042 Uiso 1 1 calc R . . N3 N 0.23567(15) 0.83819(18) 0.23043(9) 0.0229(6) Uani 1 1 d . . . Zn1 Zn 0.26176(2) 0.71578(3) 0.271454(12) 0.02280(10) Uani 1 1 d . . . O3 O 0.01128(15) 0.53774(17) 0.09368(9) 0.0405(6) Uani 1 1 d . A . C3 C 0.0512(2) 0.5244(2) 0.19520(12) 0.0338(8) Uani 1 1 d . . . H3 H 0.0098 0.4872 0.1838 0.041 Uiso 1 1 calc R . . O4 O 0.08988(16) 0.65707(18) 0.08472(8) 0.0419(7) Uani 1 1 d . A . C4 C 0.08585(18) 0.5875(2) 0.16375(11) 0.0235(7) Uani 1 1 d . A . O5 O 0.35941(13) 0.69610(16) 0.22309(8) 0.0294(5) Uani 1 1 d . . . C5 C 0.14607(18) 0.6425(2) 0.18327(11) 0.0235(7) Uani 1 1 d . . . H5 H 0.1686 0.6863 0.1628 0.028 Uiso 1 1 calc R . . O6 O 0.48151(14) 0.75292(19) 0.20626(8) 0.0420(7) Uani 1 1 d . . . C6 C 0.1757(2) 0.5651(2) 0.31172(12) 0.0276(7) Uani 1 1 d . . . C7 C 0.06004(19) 0.5946(2) 0.11016(11) 0.0259(7) Uani 1 1 d . . . O7 O 0.38378(13) 0.81134(18) 0.46840(8) 0.0353(6) Uani 1 1 d . . . C8 C 0.43057(18) 0.7712(2) 0.28763(11) 0.0223(7) Uani 1 1 d . . . O8 O 0.50885(13) 0.86149(16) 0.45888(8) 0.0284(5) Uani 1 1 d . . . O9 O 0.18212(13) 0.78678(16) 0.31911(8) 0.0284(5) Uani 1 1 d . . . C9 C 0.50144(19) 0.8057(2) 0.30616(12) 0.0285(8) Uani 1 1 d . . . H9 H 0.5462 0.8134 0.2855 0.034 Uiso 1 1 calc R . . C10 C 0.50576(19) 0.8289(2) 0.35576(12) 0.0304(8) Uani 1 1 d . . . H10 H 0.5532 0.8532 0.3688 0.036 Uiso 1 1 calc R . . O10 O 0.12335(14) 0.91919(16) 0.33287(8) 0.0336(6) Uani 1 1 d . . . O11 O 0.32602(15) 0.91064(19) 0.09294(9) 0.0440(7) Uani 1 1 d . . . C11 C 0.43862(18) 0.8155(2) 0.38616(11) 0.0231(7) Uani 1 1 d . . . O12 O 0.23963(14) 1.02421(17) 0.08565(8) 0.0347(6) Uani 1 1 d . . . C12 C 0.36817(19) 0.7833(2) 0.36398(11) 0.0266(7) Uani 1 1 d . . . H12 H 0.3220 0.7767 0.3836 0.032 Uiso 1 1 calc R . . C13 C 0.42315(19) 0.7380(2) 0.23432(11) 0.0254(7) Uani 1 1 d . . . O13 O -0.1788(6) 0.5671(6) 0.0942(7) 0.045(3) Uani 0.50 1 d PD A 1 O13' O -0.2050(6) 0.5447(6) 0.0929(7) 0.045(3) Uani 0.50 1 d PD A 2 O14 O -0.22488(16) 0.3972(2) 0.01385(10) 0.0578(8) Uani 1 1 d . A . H14A H -0.2738 0.3793 0.0144 0.087 Uiso 1 1 d R . . H14B H -0.2288 0.4119 -0.0167 0.087 Uiso 1 1 d R . . C14 C 0.44337(18) 0.8311(2) 0.44138(11) 0.0240(7) Uani 1 1 d . . . O15 O -0.09938(16) 0.5333(2) -0.00667(9) 0.0509(7) Uani 1 1 d D A . H15A H -0.1320 0.5486 -0.0349 0.076 Uiso 1 1 d RD . . H15B H -0.1301 0.5789 -0.0038 0.076 Uiso 1 1 d RD . . C15 C 0.18636(17) 0.8953(2) 0.25467(11) 0.0221(7) Uani 1 1 d . . . O16 O -0.13091(13) 0.25384(15) 0.08473(8) 0.0291(5) Uani 1 1 d . A . H16A H -0.1459 0.2550 0.1150 0.044 Uiso 1 1 d R . . H16B H -0.1703 0.2257 0.0715 0.044 Uiso 1 1 d R . . C16 C 0.16046(19) 0.9749(2) 0.23330(12) 0.0277(7) Uani 1 1 d . . . H16 H 0.1268 1.0137 0.2509 0.033 Uiso 1 1 calc R . . O17 O -0.01862(13) 0.33470(14) 0.00527(7) 0.0267(5) Uani 1 1 d . A . H17A H 0.0216 0.3704 0.0042 0.040 Uiso 1 1 d R . . H17B H -0.0407 0.3359 -0.0234 0.040 Uiso 1 1 d R . . C17 C 0.18523(19) 0.9962(2) 0.18545(12) 0.0278(7) Uani 1 1 d . . . H17 H 0.1671 1.0485 0.1701 0.033 Uiso 1 1 calc R . . O18 O 0.02636(12) 0.32891(15) 0.11070(8) 0.0270(5) Uani 1 1 d . A . H18A H 0.0703 0.3588 0.1119 0.040 Uiso 1 1 d R . . H18B H 0.0169 0.3198 0.1414 0.040 Uiso 1 1 d R . . C18 C 0.23764(18) 0.9381(2) 0.16050(11) 0.0236(7) Uani 1 1 d . . . C19 C 0.26127(18) 0.8604(2) 0.18459(11) 0.0251(7) Uani 1 1 d . . . H19 H 0.2966 0.8216 0.1683 0.030 Uiso 1 1 calc R . . O19 O 0.16615(16) 0.2022(2) 0.08463(11) 0.0552(8) Uani 1 1 d . . . H19A H 0.1942 0.1548 0.0885 0.083 Uiso 1 1 d R A . H19B H 0.1880 0.2532 0.0896 0.083 Uiso 1 1 d R . . O20 O 0.01231(16) 0.10877(18) 0.13963(9) 0.0450(7) Uani 1 1 d . . . H20A H 0.0176 0.1389 0.1663 0.067 Uiso 1 1 d R A . H20B H -0.0311 0.0811 0.1473 0.067 Uiso 1 1 d R . . C20 C 0.16152(17) 0.8654(2) 0.30657(11) 0.0231(7) Uani 1 1 d . . . O21 O 0.08943(13) 0.02520(15) 0.04182(8) 0.0312(5) Uani 1 1 d . . . H21A H 0.1351 0.0200 0.0563 0.047 Uiso 1 1 d R A . H21B H 0.0595 -0.0160 0.0538 0.047 Uiso 1 1 d R . . C21 C 0.27003(19) 0.9593(2) 0.10881(12) 0.0270(7) Uani 1 1 d . . . O22 O -0.09794(15) 0.05845(18) 0.05368(9) 0.0418(6) Uani 1 1 d . . . H22A H -0.1105 0.0236 0.0298 0.063 Uiso 1 1 d R A . H22B H -0.1299 0.0386 0.0760 0.063 Uiso 1 1 d R . . O23 O 0.17399(18) 0.8055(2) 0.06051(12) 0.0641(9) Uani 1 1 d . . . H23A H 0.1534 0.7592 0.0741 0.096 Uiso 1 1 d R . . H23B H 0.1300 0.8294 0.0507 0.096 Uiso 1 1 d R . . O24 O -0.26207(16) 0.18257(18) 0.02606(10) 0.0472(7) Uani 1 1 d . . . H24A H -0.2365 0.1869 -0.0013 0.071 Uiso 1 1 d R . . H24B H -0.2989 0.2216 0.0215 0.071 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 0.02453(15) 0.02080(16) 0.01792(15) -0.00021(11) 0.00126(11) 0.00024(12) N1 0.0245(13) 0.0227(15) 0.0186(13) -0.0006(11) -0.0013(10) -0.0002(11) O1 0.0361(13) 0.0332(14) 0.0242(12) 0.0063(10) -0.0091(10) -0.0043(11) C1 0.0275(16) 0.0246(18) 0.0185(16) 0.0010(13) 0.0016(13) -0.0008(14) Sr2 0.02614(15) 0.02222(16) 0.01774(15) -0.00097(12) 0.00054(12) 0.00045(12) N2 0.0227(13) 0.0328(17) 0.0181(14) -0.0010(12) -0.0008(11) -0.0003(12) O2 0.0507(15) 0.0534(19) 0.0252(13) 0.0122(12) -0.0003(11) -0.0125(13) C2 0.044(2) 0.038(2) 0.0237(18) 0.0060(16) -0.0002(15) -0.0159(17) N3 0.0244(13) 0.0268(16) 0.0176(13) -0.0008(11) 0.0015(11) -0.0011(11) Zn1 0.02470(19) 0.0263(2) 0.01740(18) -0.00033(15) -0.00145(14) -0.00137(15) O3 0.0502(15) 0.0428(16) 0.0286(13) 0.0012(11) -0.0128(11) -0.0190(13) C3 0.0355(19) 0.038(2) 0.0279(18) -0.0025(16) -0.0041(15) -0.0142(16) O4 0.0576(16) 0.0424(16) 0.0256(13) 0.0092(11) -0.0110(11) -0.0187(13) C4 0.0258(16) 0.0230(18) 0.0216(16) -0.0025(13) -0.0012(13) 0.0001(13) O5 0.0304(12) 0.0330(14) 0.0248(12) -0.0093(10) -0.0002(10) 0.0009(10) C5 0.0283(17) 0.0239(18) 0.0183(16) 0.0024(13) -0.0002(13) -0.0022(14) O6 0.0354(14) 0.068(2) 0.0231(13) -0.0043(12) 0.0078(11) -0.0048(13) C6 0.0348(18) 0.0264(19) 0.0215(17) 0.0020(14) -0.0008(14) 0.0013(15) C7 0.0289(17) 0.0255(19) 0.0234(17) -0.0005(14) -0.0024(14) -0.0013(14) O7 0.0291(12) 0.0523(17) 0.0244(12) -0.0059(11) 0.0027(10) -0.0063(11) C8 0.0221(15) 0.0233(18) 0.0214(16) 0.0053(13) 0.0009(13) 0.0030(13) O8 0.0302(12) 0.0311(13) 0.0239(12) -0.0016(10) -0.0062(10) -0.0058(10) O9 0.0335(12) 0.0315(14) 0.0203(11) 0.0042(10) 0.0069(9) 0.0035(11) C9 0.0243(16) 0.038(2) 0.0229(17) 0.0036(14) 0.0052(13) -0.0030(15) C10 0.0242(16) 0.040(2) 0.0267(18) 0.0013(15) -0.0033(14) -0.0051(15) O10 0.0408(13) 0.0371(15) 0.0230(12) -0.0031(11) 0.0079(10) 0.0042(11) O11 0.0371(14) 0.0642(19) 0.0308(14) 0.0162(13) 0.0120(11) 0.0186(13) C11 0.0241(16) 0.0234(18) 0.0220(16) 0.0004(13) -0.0020(13) 0.0017(13) O12 0.0357(13) 0.0379(15) 0.0306(13) 0.0127(11) 0.0017(10) 0.0048(11) C12 0.0243(16) 0.035(2) 0.0210(17) -0.0005(14) 0.0020(13) -0.0019(14) C13 0.0285(17) 0.0273(19) 0.0204(16) 0.0018(14) 0.0012(14) 0.0073(14) O13 0.053(6) 0.042(4) 0.0403(19) 0.008(4) 0.020(6) 0.019(4) O13' 0.053(6) 0.042(4) 0.0403(19) 0.008(4) 0.020(6) 0.019(4) O14 0.0482(16) 0.071(2) 0.0544(18) 0.0211(16) -0.0210(13) -0.0244(15) C14 0.0270(17) 0.0229(18) 0.0222(16) 0.0010(13) -0.0029(14) 0.0033(14) O15 0.0571(17) 0.061(2) 0.0344(14) 0.0203(13) -0.0175(12) -0.0210(15) C15 0.0212(15) 0.0263(18) 0.0187(15) -0.0056(13) 0.0005(12) -0.0025(13) O16 0.0308(12) 0.0301(13) 0.0263(12) -0.0037(10) 0.0039(10) -0.0061(10) C16 0.0292(17) 0.028(2) 0.0263(17) -0.0029(14) 0.0050(13) 0.0042(14) O17 0.0333(12) 0.0298(13) 0.0170(11) 0.0012(9) -0.0018(9) -0.0022(10) C17 0.0290(17) 0.0279(19) 0.0266(17) 0.0037(14) 0.0016(14) 0.0046(14) O18 0.0274(11) 0.0299(13) 0.0236(12) -0.0014(10) -0.0036(9) -0.0023(10) C18 0.0216(15) 0.0289(19) 0.0204(16) 0.0029(13) -0.0006(12) -0.0021(14) C19 0.0259(16) 0.0302(19) 0.0192(16) 0.0000(14) 0.0026(13) 0.0014(14) O19 0.0396(15) 0.0419(18) 0.084(2) -0.0208(16) -0.0098(14) -0.0004(13) O20 0.0608(17) 0.0502(17) 0.0238(13) 0.0008(12) -0.0034(12) -0.0109(14) C20 0.0208(15) 0.029(2) 0.0193(16) -0.0037(14) 0.0012(13) -0.0039(14) O21 0.0309(12) 0.0270(13) 0.0356(13) 0.0011(10) -0.0038(10) -0.0009(10) C21 0.0225(16) 0.038(2) 0.0209(16) 0.0051(15) 0.0012(13) -0.0026(15) O22 0.0470(15) 0.0439(17) 0.0346(14) -0.0099(12) 0.0081(11) -0.0140(12) O23 0.0544(18) 0.058(2) 0.079(2) 0.0022(17) 0.0149(16) -0.0117(15) O24 0.0487(16) 0.0469(18) 0.0460(16) 0.0104(13) 0.0043(13) 0.0052(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 Sr1 O13' 2.504(6) . ? Sr1 O13 2.503(7) . ? Sr1 O3 2.510(2) . ? Sr1 O10 2.550(2) 3_545 ? Sr1 O14 2.647(3) . ? Sr1 O15 2.653(2) . ? Sr1 O17 2.658(2) . ? Sr1 O16 2.664(2) . ? Sr1 O18 2.743(2) . ? Sr1 Sr2 4.1979(8) . ? Sr1 H16A 2.9125 . ? Sr1 H17A 2.8616 . ? N1 C1 1.340(4) . ? N1 C5 1.341(4) . ? N1 Zn1 2.186(2) . ? O1 C6 1.266(4) . ? O1 Zn1 2.079(2) . ? C1 C2 1.377(5) . ? C1 C6 1.515(4) . ? Sr2 O20 2.554(2) . ? Sr2 O22 2.608(2) . ? Sr2 O21 2.615(2) . ? Sr2 O8 2.631(2) 2_564 ? Sr2 O19 2.634(3) . ? Sr2 O17 2.697(2) . ? Sr2 O18 2.709(2) . ? Sr2 O16 2.796(2) . ? Sr2 O7 2.808(2) 2_564 ? Sr2 C14 3.072(3) 2_564 ? N2 C12 1.336(4) . ? N2 C8 1.344(4) . ? N2 Zn1 2.168(3) . ? O2 C6 1.234(4) . ? C2 C3 1.387(5) . ? C2 H2 0.9300 . ? N3 C19 1.341(4) . ? N3 C15 1.343(4) . ? N3 Zn1 2.171(3) . ? Zn1 O5 2.088(2) . ? Zn1 O9 2.115(2) . ? O3 C7 1.248(4) . ? C3 C4 1.385(5) . ? C3 H3 0.9300 . ? O4 C7 1.254(4) . ? C4 C5 1.389(4) . ? C4 C7 1.503(4) . ? O5 C13 1.258(4) . ? C5 H5 0.9300 . ? O6 C13 1.241(4) . ? O7 C14 1.255(4) . ? O7 Sr2 2.808(2) 2_565 ? C8 C9 1.370(4) . ? C8 C13 1.518(4) . ? O8 C14 1.261(4) . ? O8 Sr2 2.631(2) 2_565 ? O9 C20 1.264(4) . ? C9 C10 1.376(5) . ? C9 H9 0.9300 . ? C10 C11 1.389(4) . ? C10 H10 0.9300 . ? O10 C20 1.238(4) . ? O10 Sr1 2.550(2) 3 ? O11 C21 1.248(4) . ? C11 C12 1.390(4) . ? C11 C14 1.501(4) . ? O12 C21 1.253(4) . ? C12 H12 0.9300 . ? O14 H14A 0.8501 . ? O14 H14B 0.8500 . ? C14 Sr2 3.072(3) 2_565 ? O15 H15A 0.9570 . ? O15 H15B 0.8501 . ? C15 C16 1.383(5) . ? C15 C20 1.518(4) . ? O16 H16A 0.8501 . ? O16 H16B 0.8499 . ? C16 C17 1.383(4) . ? C16 H16 0.9300 . ? O17 H17A 0.8501 . ? O17 H17B 0.8500 . ? C17 C18 1.393(4) . ? C17 H17 0.9300 . ? O18 H18A 0.8501 . ? O18 H18B 0.8500 . ? C18 C19 1.380(5) . ? C18 C21 1.519(4) . ? C19 H19 0.9300 . ? O19 H19A 0.8500 . ? O19 H19B 0.8501 . ? O20 H20A 0.8500 . ? O20 H20B 0.8501 . ? O21 H21A 0.8500 . ? O21 H21B 0.8501 . ? O22 H22A 0.8500 . ? O22 H22B 0.8500 . ? O23 H23A 0.8499 . ? O23 H23B 0.8499 . ? O24 H24A 0.8499 . ? O24 H24B 0.8499 . ? 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 O13' Sr1 O13 12.5(4) . . ? O13' Sr1 O3 90.7(3) . . ? O13 Sr1 O3 78.2(3) . . ? O13' Sr1 O10 74.0(5) . 3_545 ? O13 Sr1 O10 75.2(5) . 3_545 ? O3 Sr1 O10 86.02(8) . 3_545 ? O13' Sr1 O14 73.0(4) . . ? O13 Sr1 O14 82.8(4) . . ? O3 Sr1 O14 144.37(8) . . ? O10 Sr1 O14 117.85(8) 3_545 . ? O13' Sr1 O15 76.4(4) . . ? O13 Sr1 O15 72.4(4) . . ? O3 Sr1 O15 78.04(8) . . ? O10 Sr1 O15 146.11(9) 3_545 . ? O14 Sr1 O15 67.53(8) . . ? O13' Sr1 O17 148.7(5) . . ? O13 Sr1 O17 147.9(4) . . ? O3 Sr1 O17 96.98(8) . . ? O10 Sr1 O17 136.56(7) 3_545 . ? O14 Sr1 O17 83.49(9) . . ? O15 Sr1 O17 75.61(8) . . ? O13' Sr1 O16 121.1(2) . . ? O13 Sr1 O16 132.7(2) . . ? O3 Sr1 O16 138.31(8) . . ? O10 Sr1 O16 78.76(7) 3_545 . ? O14 Sr1 O16 75.47(8) . . ? O15 Sr1 O16 131.82(8) . . ? O17 Sr1 O16 70.42(7) . . ? O13' Sr1 O18 145.2(5) . . ? O13 Sr1 O18 139.2(4) . . ? O3 Sr1 O18 73.53(8) . . ? O10 Sr1 O18 74.06(7) 3_545 . ? O14 Sr1 O18 135.77(8) . . ? O15 Sr1 O18 127.64(8) . . ? O17 Sr1 O18 65.56(6) . . ? O16 Sr1 O18 65.04(7) . . ? O13' Sr1 Sr2 162.0(2) . . ? O13 Sr1 Sr2 172.7(3) . . ? O3 Sr1 Sr2 105.45(6) . . ? O10 Sr1 Sr2 98.64(6) 3_545 . ? O14 Sr1 Sr2 97.03(7) . . ? O15 Sr1 Sr2 114.30(7) . . ? O17 Sr1 Sr2 38.71(5) . . ? O16 Sr1 Sr2 40.91(5) . . ? O18 Sr1 Sr2 39.36(4) . . ? O13' Sr1 H16A 110.5 . . ? O13 Sr1 H16A 120.6 . . ? O3 Sr1 H16A 132.9 . . ? O10 Sr1 H16A 62.2 3_545 . ? O14 Sr1 H16A 82.7 . . ? O15 Sr1 H16A 146.4 . . ? O17 Sr1 H16A 86.0 . . ? O16 Sr1 H16A 16.8 . . ? O18 Sr1 H16A 65.1 . . ? Sr2 Sr1 H16A 52.3 . . ? O13' Sr1 H17A 145.9 . . ? O13 Sr1 H17A 139.2 . . ? O3 Sr1 H17A 80.0 . . ? O10 Sr1 H17A 136.9 3_545 . ? O14 Sr1 H17A 95.8 . . ? O15 Sr1 H17A 69.6 . . ? O17 Sr1 H17A 17.2 . . ? O16 Sr1 H17A 85.2 . . ? O18 Sr1 H17A 62.9 . . ? Sr2 Sr1 H17A 48.1 . . ? H16A Sr1 H17A 99.5 . . ? C1 N1 C5 118.3(3) . . ? C1 N1 Zn1 110.56(19) . . ? C5 N1 Zn1 131.0(2) . . ? C6 O1 Zn1 115.6(2) . . ? N1 C1 C2 122.3(3) . . ? N1 C1 C6 116.1(3) . . ? C2 C1 C6 121.6(3) . . ? O20 Sr2 O22 71.86(8) . . ? O20 Sr2 O21 75.62(8) . . ? O22 Sr2 O21 74.02(8) . . ? O20 Sr2 O8 140.57(8) . 2_564 ? O22 Sr2 O8 74.44(7) . 2_564 ? O21 Sr2 O8 75.93(7) . 2_564 ? O20 Sr2 O19 77.45(9) . . ? O22 Sr2 O19 139.64(9) . . ? O21 Sr2 O19 73.44(8) . . ? O8 Sr2 O19 119.07(8) 2_564 . ? O20 Sr2 O17 141.27(8) . . ? O22 Sr2 O17 116.18(7) . . ? O21 Sr2 O17 142.67(7) . . ? O8 Sr2 O17 73.19(7) 2_564 . ? O19 Sr2 O17 104.17(8) . . ? O20 Sr2 O18 79.65(8) . . ? O22 Sr2 O18 127.38(7) . . ? O21 Sr2 O18 139.19(7) . . ? O8 Sr2 O18 138.53(7) 2_564 . ? O19 Sr2 O18 69.80(7) . . ? O17 Sr2 O18 65.51(7) . . ? O20 Sr2 O16 82.19(8) . . ? O22 Sr2 O16 69.18(7) . . ? O21 Sr2 O16 141.40(7) . . ? O8 Sr2 O16 104.36(7) 2_564 . ? O19 Sr2 O16 131.76(8) . . ? O17 Sr2 O16 67.90(6) . . ? O18 Sr2 O16 63.73(6) . . ? O20 Sr2 O7 140.30(8) . 2_564 ? O22 Sr2 O7 117.49(7) . 2_564 ? O21 Sr2 O7 71.18(7) . 2_564 ? O8 Sr2 O7 47.75(7) 2_564 2_564 ? O19 Sr2 O7 72.76(8) . 2_564 ? O17 Sr2 O7 72.63(7) . 2_564 ? O18 Sr2 O7 112.79(7) . 2_564 ? O16 Sr2 O7 137.48(7) . 2_564 ? O20 Sr2 C14 150.52(9) . 2_564 ? O22 Sr2 C14 97.29(8) . 2_564 ? O21 Sr2 C14 75.03(8) . 2_564 ? O8 Sr2 C14 23.99(7) 2_564 2_564 ? O19 Sr2 C14 96.73(9) . 2_564 ? O17 Sr2 C14 68.20(7) . 2_564 ? O18 Sr2 C14 125.93(8) . 2_564 ? O16 Sr2 C14 120.39(7) . 2_564 ? O7 Sr2 C14 24.13(7) 2_564 2_564 ? O20 Sr2 Sr1 103.59(6) . . ? O22 Sr2 Sr1 106.26(6) . . ? O21 Sr2 Sr1 179.06(5) . . ? O8 Sr2 Sr1 105.01(5) 2_564 . ? O19 Sr2 Sr1 105.94(6) . . ? O17 Sr2 Sr1 38.06(4) . . ? O18 Sr2 Sr1 39.94(4) . . ? O16 Sr2 Sr1 38.61(5) . . ? O7 Sr2 Sr1 109.36(5) 2_564 . ? C14 Sr2 Sr1 105.78(6) 2_564 . ? C12 N2 C8 118.2(3) . . ? C12 N2 Zn1 130.5(2) . . ? C8 N2 Zn1 111.21(19) . . ? C1 C2 C3 119.1(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C19 N3 C15 118.6(3) . . ? C19 N3 Zn1 127.5(2) . . ? C15 N3 Zn1 113.9(2) . . ? O1 Zn1 O5 113.44(10) . . ? O1 Zn1 O9 85.12(9) . . ? O5 Zn1 O9 157.53(9) . . ? O1 Zn1 N2 91.86(9) . . ? O5 Zn1 N2 77.69(9) . . ? O9 Zn1 N2 89.64(9) . . ? O1 Zn1 N3 157.98(9) . . ? O5 Zn1 N3 87.44(9) . . ? O9 Zn1 N3 76.38(9) . . ? N2 Zn1 N3 99.77(10) . . ? O1 Zn1 N1 77.17(9) . . ? O5 Zn1 N1 97.06(9) . . ? O9 Zn1 N1 99.51(9) . . ? N2 Zn1 N1 164.95(10) . . ? N3 Zn1 N1 94.01(10) . . ? C7 O3 Sr1 170.6(2) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 117.7(3) . . ? C3 C4 C7 120.9(3) . . ? C5 C4 C7 121.4(3) . . ? C13 O5 Zn1 115.18(19) . . ? N1 C5 C4 123.2(3) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? O2 C6 O1 126.2(3) . . ? O2 C6 C1 118.2(3) . . ? O1 C6 C1 115.6(3) . . ? O3 C7 O4 124.2(3) . . ? O3 C7 C4 118.3(3) . . ? O4 C7 C4 117.5(3) . . ? C14 O7 Sr2 89.79(18) . 2_565 ? N2 C8 C9 122.4(3) . . ? N2 C8 C13 115.3(3) . . ? C9 C8 C13 122.2(3) . . ? C14 O8 Sr2 97.99(18) . 2_565 ? C20 O9 Zn1 117.92(19) . . ? C8 C9 C10 119.3(3) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C9 C10 C11 119.4(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C20 O10 Sr1 132.4(2) . 3 ? C10 C11 C12 117.6(3) . . ? C10 C11 C14 121.1(3) . . ? C12 C11 C14 121.3(3) . . ? N2 C12 C11 123.0(3) . . ? N2 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? O6 C13 O5 126.2(3) . . ? O6 C13 C8 116.8(3) . . ? O5 C13 C8 117.0(3) . . ? Sr1 O14 H14A 141.6 . . ? Sr1 O14 H14B 126.5 . . ? H14A O14 H14B 91.4 . . ? O7 C14 O8 122.6(3) . . ? O7 C14 C11 119.5(3) . . ? O8 C14 C11 117.8(3) . . ? O7 C14 Sr2 66.08(16) . 2_565 ? O8 C14 Sr2 58.02(15) . 2_565 ? C11 C14 Sr2 164.8(2) . 2_565 ? Sr1 O15 H15A 141.2 . . ? Sr1 O15 H15B 113.2 . . ? H15A O15 H15B 63.1 . . ? N3 C15 C16 121.8(3) . . ? N3 C15 C20 115.0(3) . . ? C16 C15 C20 123.2(3) . . ? Sr1 O16 Sr2 100.48(7) . . ? Sr1 O16 H16A 98.4 . . ? Sr2 O16 H16A 123.5 . . ? Sr1 O16 H16B 125.4 . . ? Sr2 O16 H16B 110.0 . . ? H16A O16 H16B 100.7 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? Sr1 O17 Sr2 103.23(7) . . ? Sr1 O17 H17A 95.1 . . ? Sr2 O17 H17A 112.6 . . ? Sr1 O17 H17B 113.2 . . ? Sr2 O17 H17B 122.5 . . ? H17A O17 H17B 106.9 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? Sr2 O18 Sr1 100.70(7) . . ? Sr2 O18 H18A 120.1 . . ? Sr1 O18 H18A 112.2 . . ? Sr2 O18 H18B 114.4 . . ? Sr1 O18 H18B 107.5 . . ? H18A O18 H18B 101.7 . . ? C19 C18 C17 118.0(3) . . ? C19 C18 C21 120.1(3) . . ? C17 C18 C21 121.9(3) . . ? N3 C19 C18 123.1(3) . . ? N3 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? Sr2 O19 H19A 116.4 . . ? Sr2 O19 H19B 124.1 . . ? H19A O19 H19B 119.4 . . ? Sr2 O20 H20A 123.1 . . ? Sr2 O20 H20B 116.2 . . ? H20A O20 H20B 97.9 . . ? O10 C20 O9 125.6(3) . . ? O10 C20 C15 118.1(3) . . ? O9 C20 C15 116.3(3) . . ? Sr2 O21 H21A 115.9 . . ? Sr2 O21 H21B 108.9 . . ? H21A O21 H21B 106.1 . . ? O11 C21 O12 125.0(3) . . ? O11 C21 C18 116.8(3) . . ? O12 C21 C18 118.2(3) . . ? Sr2 O22 H22A 126.4 . . ? Sr2 O22 H22B 133.9 . . ? H22A O22 H22B 99.6 . . ? H23A O23 H23B 97.6 . . ? H24A O24 H24B 100.2 . . ? 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 C5 N1 C1 C2 -0.4(5) . . . . ? Zn1 N1 C1 C2 176.0(3) . . . . ? C5 N1 C1 C6 177.3(3) . . . . ? Zn1 N1 C1 C6 -6.3(3) . . . . ? O13' Sr1 Sr2 O20 -61.1(15) . . . . ? O13 Sr1 Sr2 O20 -28(3) . . . . ? O3 Sr1 Sr2 O20 91.58(8) . . . . ? O10 Sr1 Sr2 O20 3.35(8) 3_545 . . . ? O14 Sr1 Sr2 O20 -116.31(9) . . . . ? O15 Sr1 Sr2 O20 175.21(8) . . . . ? O17 Sr1 Sr2 O20 173.36(10) . . . . ? O16 Sr1 Sr2 O20 -58.20(9) . . . . ? O18 Sr1 Sr2 O20 54.80(9) . . . . ? O13' Sr1 Sr2 O22 13.7(15) . . . . ? O13 Sr1 Sr2 O22 46(3) . . . . ? O3 Sr1 Sr2 O22 166.33(8) . . . . ? O10 Sr1 Sr2 O22 78.10(8) 3_545 . . . ? O14 Sr1 Sr2 O22 -41.56(8) . . . . ? O15 Sr1 Sr2 O22 -110.04(8) . . . . ? O17 Sr1 Sr2 O22 -111.90(9) . . . . ? O16 Sr1 Sr2 O22 16.54(9) . . . . ? O18 Sr1 Sr2 O22 129.55(9) . . . . ? O13' Sr1 Sr2 O21 -94(3) . . . . ? O13 Sr1 Sr2 O21 -61(4) . . . . ? O3 Sr1 Sr2 O21 59(3) . . . . ? O10 Sr1 Sr2 O21 -29(3) 3_545 . . . ? O14 Sr1 Sr2 O21 -149(3) . . . . ? O15 Sr1 Sr2 O21 143(3) . . . . ? O17 Sr1 Sr2 O21 141(3) . . . . ? O16 Sr1 Sr2 O21 -91(3) . . . . ? O18 Sr1 Sr2 O21 22(3) . . . . ? O13' Sr1 Sr2 O8 91.5(15) . . . 2_564 ? O13 Sr1 Sr2 O8 124(3) . . . 2_564 ? O3 Sr1 Sr2 O8 -115.86(7) . . . 2_564 ? O10 Sr1 Sr2 O8 155.91(7) 3_545 . . 2_564 ? O14 Sr1 Sr2 O8 36.25(8) . . . 2_564 ? O15 Sr1 Sr2 O8 -32.23(8) . . . 2_564 ? O17 Sr1 Sr2 O8 -34.09(9) . . . 2_564 ? O16 Sr1 Sr2 O8 94.36(9) . . . 2_564 ? O18 Sr1 Sr2 O8 -152.64(9) . . . 2_564 ? O13' Sr1 Sr2 O19 -141.6(15) . . . . ? O13 Sr1 Sr2 O19 -109(3) . . . . ? O3 Sr1 Sr2 O19 10.99(9) . . . . ? O10 Sr1 Sr2 O19 -77.24(9) 3_545 . . . ? O14 Sr1 Sr2 O19 163.10(9) . . . . ? O15 Sr1 Sr2 O19 94.62(9) . . . . ? O17 Sr1 Sr2 O19 92.77(10) . . . . ? O16 Sr1 Sr2 O19 -138.79(10) . . . . ? O18 Sr1 Sr2 O19 -25.79(10) . . . . ? O13' Sr1 Sr2 O17 125.6(15) . . . . ? O13 Sr1 Sr2 O17 158(3) . . . . ? O3 Sr1 Sr2 O17 -81.77(9) . . . . ? O10 Sr1 Sr2 O17 -170.01(9) 3_545 . . . ? O14 Sr1 Sr2 O17 70.34(10) . . . . ? O15 Sr1 Sr2 O17 1.85(10) . . . . ? O16 Sr1 Sr2 O17 128.44(10) . . . . ? O18 Sr1 Sr2 O17 -118.55(10) . . . . ? O13' Sr1 Sr2 O18 -115.9(15) . . . . ? O13 Sr1 Sr2 O18 -83(3) . . . . ? O3 Sr1 Sr2 O18 36.78(9) . . . . ? O10 Sr1 Sr2 O18 -51.45(9) 3_545 . . . ? O14 Sr1 Sr2 O18 -171.11(9) . . . . ? O15 Sr1 Sr2 O18 120.41(9) . . . . ? O17 Sr1 Sr2 O18 118.55(10) . . . . ? O16 Sr1 Sr2 O18 -113.00(10) . . . . ? O13' Sr1 Sr2 O16 -2.9(15) . . . . ? O13 Sr1 Sr2 O16 30(3) . . . . ? O3 Sr1 Sr2 O16 149.79(9) . . . . ? O10 Sr1 Sr2 O16 61.55(9) 3_545 . . . ? O14 Sr1 Sr2 O16 -58.10(9) . . . . ? O15 Sr1 Sr2 O16 -126.59(9) . . . . ? O17 Sr1 Sr2 O16 -128.44(10) . . . . ? O18 Sr1 Sr2 O16 113.00(10) . . . . ? O13' Sr1 Sr2 O7 141.4(15) . . . 2_564 ? O13 Sr1 Sr2 O7 174(3) . . . 2_564 ? O3 Sr1 Sr2 O7 -65.92(7) . . . 2_564 ? O10 Sr1 Sr2 O7 -154.16(7) 3_545 . . 2_564 ? O14 Sr1 Sr2 O7 86.19(8) . . . 2_564 ? O15 Sr1 Sr2 O7 17.70(8) . . . 2_564 ? O17 Sr1 Sr2 O7 15.85(9) . . . 2_564 ? O16 Sr1 Sr2 O7 144.29(9) . . . 2_564 ? O18 Sr1 Sr2 O7 -102.71(9) . . . 2_564 ? O13' Sr1 Sr2 C14 116.4(15) . . . 2_564 ? O13 Sr1 Sr2 C14 149(3) . . . 2_564 ? O3 Sr1 Sr2 C14 -90.97(8) . . . 2_564 ? O10 Sr1 Sr2 C14 -179.21(8) 3_545 . . 2_564 ? O14 Sr1 Sr2 C14 61.14(9) . . . 2_564 ? O15 Sr1 Sr2 C14 -7.35(9) . . . 2_564 ? O17 Sr1 Sr2 C14 -9.20(10) . . . 2_564 ? O16 Sr1 Sr2 C14 119.24(9) . . . 2_564 ? O18 Sr1 Sr2 C14 -127.76(9) . . . 2_564 ? N1 C1 C2 C3 0.8(5) . . . . ? C6 C1 C2 C3 -176.8(3) . . . . ? C6 O1 Zn1 O5 -112.8(2) . . . . ? C6 O1 Zn1 O9 80.3(2) . . . . ? C6 O1 Zn1 N2 169.8(2) . . . . ? C6 O1 Zn1 N3 47.6(4) . . . . ? C6 O1 Zn1 N1 -20.6(2) . . . . ? C12 N2 Zn1 O1 -56.8(3) . . . . ? C8 N2 Zn1 O1 126.3(2) . . . . ? C12 N2 Zn1 O5 -170.4(3) . . . . ? C8 N2 Zn1 O5 12.7(2) . . . . ? C12 N2 Zn1 O9 28.3(3) . . . . ? C8 N2 Zn1 O9 -148.6(2) . . . . ? C12 N2 Zn1 N3 104.4(3) . . . . ? C8 N2 Zn1 N3 -72.5(2) . . . . ? C12 N2 Zn1 N1 -99.6(4) . . . . ? C8 N2 Zn1 N1 83.5(4) . . . . ? C19 N3 Zn1 O1 -143.3(3) . . . . ? C15 N3 Zn1 O1 34.9(4) . . . . ? C19 N3 Zn1 O5 18.7(3) . . . . ? C15 N3 Zn1 O5 -163.1(2) . . . . ? C19 N3 Zn1 O9 -177.0(3) . . . . ? C15 N3 Zn1 O9 1.2(2) . . . . ? C19 N3 Zn1 N2 95.8(3) . . . . ? C15 N3 Zn1 N2 -86.0(2) . . . . ? C19 N3 Zn1 N1 -78.2(3) . . . . ? C15 N3 Zn1 N1 100.0(2) . . . . ? C1 N1 Zn1 O1 13.4(2) . . . . ? C5 N1 Zn1 O1 -170.7(3) . . . . ? C1 N1 Zn1 O5 125.9(2) . . . . ? C5 N1 Zn1 O5 -58.2(3) . . . . ? C1 N1 Zn1 O9 -69.3(2) . . . . ? C5 N1 Zn1 O9 106.5(3) . . . . ? C1 N1 Zn1 N2 57.5(4) . . . . ? C5 N1 Zn1 N2 -126.7(4) . . . . ? C1 N1 Zn1 N3 -146.2(2) . . . . ? C5 N1 Zn1 N3 29.7(3) . . . . ? O13' Sr1 O3 C7 48.6(15) . . . . ? O13 Sr1 O3 C7 50.3(15) . . . . ? O10 Sr1 O3 C7 -25.4(14) 3_545 . . . ? O14 Sr1 O3 C7 109.6(14) . . . . ? O15 Sr1 O3 C7 124.6(14) . . . . ? O17 Sr1 O3 C7 -161.8(14) . . . . ? O16 Sr1 O3 C7 -93.5(15) . . . . ? O18 Sr1 O3 C7 -99.9(14) . . . . ? Sr2 Sr1 O3 C7 -123.2(14) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? C2 C3 C4 C5 -1.5(5) . . . . ? C2 C3 C4 C7 177.3(3) . . . . ? O1 Zn1 O5 C13 -104.2(2) . . . . ? O9 Zn1 O5 C13 39.4(4) . . . . ? N2 Zn1 O5 C13 -17.6(2) . . . . ? N3 Zn1 O5 C13 83.0(2) . . . . ? N1 Zn1 O5 C13 176.7(2) . . . . ? C1 N1 C5 C4 -1.0(5) . . . . ? Zn1 N1 C5 C4 -176.6(2) . . . . ? C3 C4 C5 N1 1.9(5) . . . . ? C7 C4 C5 N1 -176.8(3) . . . . ? Zn1 O1 C6 O2 -156.3(3) . . . . ? Zn1 O1 C6 C1 23.4(4) . . . . ? N1 C1 C6 O2 168.9(3) . . . . ? C2 C1 C6 O2 -13.4(5) . . . . ? N1 C1 C6 O1 -10.9(4) . . . . ? C2 C1 C6 O1 166.8(3) . . . . ? Sr1 O3 C7 O4 -133.8(13) . . . . ? Sr1 O3 C7 C4 47.0(16) . . . . ? C3 C4 C7 O3 -5.5(5) . . . . ? C5 C4 C7 O3 173.3(3) . . . . ? C3 C4 C7 O4 175.3(3) . . . . ? C5 C4 C7 O4 -6.0(5) . . . . ? C12 N2 C8 C9 -2.4(5) . . . . ? Zn1 N2 C8 C9 175.0(3) . . . . ? C12 N2 C8 C13 175.3(3) . . . . ? Zn1 N2 C8 C13 -7.3(3) . . . . ? O1 Zn1 O9 C20 -173.7(2) . . . . ? O5 Zn1 O9 C20 39.4(4) . . . . ? N2 Zn1 O9 C20 94.4(2) . . . . ? N3 Zn1 O9 C20 -5.7(2) . . . . ? N1 Zn1 O9 C20 -97.6(2) . . . . ? N2 C8 C9 C10 2.0(5) . . . . ? C13 C8 C9 C10 -175.6(3) . . . . ? C8 C9 C10 C11 1.0(5) . . . . ? C9 C10 C11 C12 -3.3(5) . . . . ? C9 C10 C11 C14 173.8(3) . . . . ? C8 N2 C12 C11 -0.2(5) . . . . ? Zn1 N2 C12 C11 -176.9(2) . . . . ? C10 C11 C12 N2 3.0(5) . . . . ? C14 C11 C12 N2 -174.1(3) . . . . ? Zn1 O5 C13 O6 -162.8(3) . . . . ? Zn1 O5 C13 C8 19.1(3) . . . . ? N2 C8 C13 O6 174.3(3) . . . . ? C9 C8 C13 O6 -8.0(5) . . . . ? N2 C8 C13 O5 -7.5(4) . . . . ? C9 C8 C13 O5 170.2(3) . . . . ? Sr2 O7 C14 O8 -13.8(3) 2_565 . . . ? Sr2 O7 C14 C11 164.2(3) 2_565 . . . ? Sr2 O8 C14 O7 14.9(3) 2_565 . . . ? Sr2 O8 C14 C11 -163.1(2) 2_565 . . . ? C10 C11 C14 O7 -174.1(3) . . . . ? C12 C11 C14 O7 2.8(5) . . . . ? C10 C11 C14 O8 4.0(5) . . . . ? C12 C11 C14 O8 -179.1(3) . . . . ? C10 C11 C14 Sr2 -66.2(9) . . . 2_565 ? C12 C11 C14 Sr2 110.7(8) . . . 2_565 ? C19 N3 C15 C16 1.2(4) . . . . ? Zn1 N3 C15 C16 -177.2(2) . . . . ? C19 N3 C15 C20 -179.1(3) . . . . ? Zn1 N3 C15 C20 2.5(3) . . . . ? O13' Sr1 O16 Sr2 179.0(5) . . . . ? O13 Sr1 O16 Sr2 -175.1(6) . . . . ? O3 Sr1 O16 Sr2 -46.83(13) . . . . ? O10 Sr1 O16 Sr2 -117.59(8) 3_545 . . . ? O14 Sr1 O16 Sr2 119.49(9) . . . . ? O15 Sr1 O16 Sr2 79.09(11) . . . . ? O17 Sr1 O16 Sr2 31.33(6) . . . . ? O18 Sr1 O16 Sr2 -40.08(6) . . . . ? O20 Sr2 O16 Sr1 123.50(8) . . . . ? O22 Sr2 O16 Sr1 -163.00(9) . . . . ? O21 Sr2 O16 Sr1 178.50(8) . . . . ? O8 Sr2 O16 Sr1 -96.18(8) 2_564 . . . ? O19 Sr2 O16 Sr1 58.12(13) . . . . ? O17 Sr2 O16 Sr1 -31.41(6) . . . . ? O18 Sr2 O16 Sr1 41.23(7) . . . . ? O7 Sr2 O16 Sr1 -54.57(12) 2_564 . . . ? C14 Sr2 O16 Sr1 -76.76(10) 2_564 . . . ? N3 C15 C16 C17 0.7(5) . . . . ? C20 C15 C16 C17 -179.1(3) . . . . ? O13' Sr1 O17 Sr2 -151.0(4) . . . . ? O13 Sr1 O17 Sr2 -175.0(5) . . . . ? O3 Sr1 O17 Sr2 106.04(8) . . . . ? O10 Sr1 O17 Sr2 14.45(13) 3_545 . . . ? O14 Sr1 O17 Sr2 -109.84(9) . . . . ? O15 Sr1 O17 Sr2 -178.26(9) . . . . ? O16 Sr1 O17 Sr2 -32.98(7) . . . . ? O18 Sr1 O17 Sr2 37.72(7) . . . . ? O20 Sr2 O17 Sr1 -10.36(15) . . . . ? O22 Sr2 O17 Sr1 83.00(9) . . . . ? O21 Sr2 O17 Sr1 -179.02(8) . . . . ? O8 Sr2 O17 Sr1 145.56(9) 2_564 . . . ? O19 Sr2 O17 Sr1 -97.87(9) . . . . ? O18 Sr2 O17 Sr1 -38.29(7) . . . . ? O16 Sr2 O17 Sr1 31.84(7) . . . . ? O7 Sr2 O17 Sr1 -164.34(9) 2_564 . . . ? C14 Sr2 O17 Sr1 170.46(10) 2_564 . . . ? C15 C16 C17 C18 -1.9(5) . . . . ? O20 Sr2 O18 Sr1 -126.16(9) . . . . ? O22 Sr2 O18 Sr1 -68.69(11) . . . . ? O21 Sr2 O18 Sr1 -179.46(8) . . . . ? O8 Sr2 O18 Sr1 42.09(12) 2_564 . . . ? O19 Sr2 O18 Sr1 153.53(10) . . . . ? O17 Sr2 O18 Sr1 36.51(6) . . . . ? O16 Sr2 O18 Sr1 -39.83(6) . . . . ? O7 Sr2 O18 Sr1 93.34(8) 2_564 . . . ? C14 Sr2 O18 Sr1 69.99(10) 2_564 . . . ? O13' Sr1 O18 Sr2 150.8(4) . . . . ? O13 Sr1 O18 Sr2 168.9(4) . . . . ? O3 Sr1 O18 Sr2 -143.00(9) . . . . ? O10 Sr1 O18 Sr2 126.48(9) 3_545 . . . ? O14 Sr1 O18 Sr2 12.70(14) . . . . ? O15 Sr1 O18 Sr2 -83.06(11) . . . . ? O17 Sr1 O18 Sr2 -37.11(7) . . . . ? O16 Sr1 O18 Sr2 41.68(7) . . . . ? C16 C17 C18 C19 1.3(5) . . . . ? C16 C17 C18 C21 -177.3(3) . . . . ? C15 N3 C19 C18 -1.8(5) . . . . ? Zn1 N3 C19 C18 176.3(2) . . . . ? C17 C18 C19 N3 0.6(5) . . . . ? C21 C18 C19 N3 179.2(3) . . . . ? Sr1 O10 C20 O9 19.7(5) 3 . . . ? Sr1 O10 C20 C15 -160.3(2) 3 . . . ? Zn1 O9 C20 O10 -171.1(2) . . . . ? Zn1 O9 C20 C15 8.8(3) . . . . ? N3 C15 C20 O10 172.4(3) . . . . ? C16 C15 C20 O10 -7.9(4) . . . . ? N3 C15 C20 O9 -7.5(4) . . . . ? C16 C15 C20 O9 172.2(3) . . . . ? C19 C18 C21 O11 -9.6(5) . . . . ? C17 C18 C21 O11 169.1(3) . . . . ? C19 C18 C21 O12 171.2(3) . . . . ? C17 C18 C21 O12 -10.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14A O7 0.85 2.13 2.953(4) 164.2 3_545 O14 H14B O12 0.85 2.14 2.972(3) 164.5 4_465 O15 H15A O11 0.96 1.81 2.750(3) 167.7 4_465 O15 H15B O24 0.85 2.49 3.305(4) 161.8 8_565 O16 H16A O9 0.85 1.92 2.758(3) 166.8 3_545 O16 H16B O24 0.85 2.05 2.877(3) 165.3 . O17 H17A O15 0.85 1.92 2.764(3) 169.8 5_565 O17 H17B O4 0.85 1.84 2.687(3) 177.7 5_565 O18 H18A O11 0.85 1.94 2.762(3) 161.3 8_655 O18 H18B O6 0.85 2.00 2.805(3) 156.7 8_655 O19 H19A O12 0.85 2.08 2.912(4) 164.9 1_545 O19 H19B O11 0.85 2.36 3.111(4) 148.3 8_655 O19 H19B O23 0.85 2.53 3.118(4) 127.5 8_655 O20 H20A O6 0.85 2.01 2.793(4) 153.8 8_655 O20 H20B O2 0.85 2.02 2.870(4) 173.1 3_545 O21 H21A O12 0.85 1.90 2.741(3) 172.4 1_545 O21 H21B O8 0.85 2.03 2.774(3) 145.3 6_546 O22 H22A O21 0.85 2.08 2.852(3) 150.1 5 O22 H22B O2 0.85 2.21 2.921(3) 141.6 3_545 O23 H23A O4 0.85 1.87 2.686(4) 161.5 . O23 H23B O8 0.85 2.07 2.894(4) 163.5 6_556 O24 H24A O23 0.85 1.90 2.745(4) 176.7 5_565 O24 H24B O7 0.85 1.95 2.778(4) 163.7 3_545 C19 H19 O11 0.93 2.46 2.783(4) 100.1 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.499 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 781987'