# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email shangao67@yahoo.com _publ_contact_author_name 'Shan Gao ' loop_ _publ_author_name 'Zhao-Peng Deng' 'Wei Kang' 'Zhi-Biao Zhu' 'Li-Hua Huo' 'Hui Zhao' 'Shan Gao ' data_k _database_code_depnum_ccdc_archive 'CCDC 853184' #TrackingRef 'complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H14 Mg N4 O8' _chemical_formula_sum 'C8 H14 Mg N4 O8' _chemical_formula_weight 318.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.1545(10) _cell_length_b 13.940(3) _cell_length_c 9.1871(18) _cell_angle_alpha 90.00 _cell_angle_beta 98.45(3) _cell_angle_gamma 90.00 _cell_volume 652.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5071 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 332 _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9214 _exptl_absorpt_correction_T_max 0.9692 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6244 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1494 _reflns_number_gt 1266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0465P)^2^+0.2804P] 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 1494 _refine_ls_number_parameters 112 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.036 _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 Mg1 Mg 0.0000 0.5000 0.5000 0.02407(19) Uani 1 2 d S . . O1 O 0.2312(2) 0.38617(7) 0.43656(13) 0.0301(3) Uani 1 1 d . . . O1W O 0.1131(3) 0.58748(8) 0.34213(14) 0.0390(3) Uani 1 1 d D . . H1W1 H 0.076(4) 0.6455(9) 0.362(2) 0.058 Uiso 1 1 d D . . H1W2 H 0.214(4) 0.5887(15) 0.2758(19) 0.058 Uiso 1 1 d D . . O2 O 0.5860(2) 0.07854(7) 0.37398(13) 0.0345(3) Uani 1 1 d . . . O2W O 0.3171(2) 0.54519(8) 0.65301(13) 0.0332(3) Uani 1 1 d D . . H2W1 H 0.453(3) 0.5654(14) 0.620(2) 0.050 Uiso 1 1 d D . . H2W2 H 0.363(4) 0.5042(12) 0.7200(18) 0.050 Uiso 1 1 d D . . N1 N 0.0867(2) 0.25497(9) 0.54962(14) 0.0287(3) Uani 1 1 d . . . N2 N 0.2748(3) 0.10528(8) 0.51959(14) 0.0281(3) Uani 1 1 d D . . H2N H 0.293(4) 0.0461(8) 0.545(2) 0.042 Uiso 1 1 d D . . C1 C 0.1092(3) 0.16339(10) 0.57658(17) 0.0289(3) Uani 1 1 d . . . H1 H 0.0032 0.1366 0.6396 0.035 Uiso 1 1 calc R . . C2 C 0.4396(3) 0.13951(10) 0.42535(16) 0.0255(3) Uani 1 1 d . . . C3 C 0.4261(3) 0.23718(10) 0.39716(17) 0.0282(3) Uani 1 1 d . . . H3 H 0.5352 0.2643 0.3362 0.034 Uiso 1 1 calc R . . C4 C 0.2504(3) 0.29563(10) 0.45918(16) 0.0242(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0240(3) 0.0186(3) 0.0319(4) 0.0020(2) 0.0116(3) 0.0031(3) O1 0.0300(5) 0.0182(5) 0.0450(7) 0.0029(4) 0.0158(5) 0.0050(4) O1W 0.0538(8) 0.0228(5) 0.0482(7) 0.0063(5) 0.0338(6) 0.0087(5) O2 0.0452(7) 0.0216(5) 0.0420(7) 0.0018(4) 0.0236(5) 0.0092(5) O2W 0.0290(6) 0.0298(6) 0.0414(7) 0.0054(5) 0.0072(5) -0.0027(4) N1 0.0296(6) 0.0234(6) 0.0359(7) 0.0005(5) 0.0137(5) 0.0035(5) N2 0.0365(7) 0.0179(6) 0.0322(7) 0.0039(5) 0.0129(5) 0.0039(5) C1 0.0318(7) 0.0252(7) 0.0323(8) 0.0020(6) 0.0136(6) 0.0016(6) C2 0.0284(7) 0.0226(7) 0.0269(7) -0.0001(5) 0.0086(5) 0.0033(6) C3 0.0298(7) 0.0222(7) 0.0356(8) 0.0026(6) 0.0148(6) 0.0018(6) C4 0.0243(7) 0.0202(6) 0.0285(7) 0.0004(5) 0.0054(5) 0.0017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1W 2.0442(11) 3_566 ? Mg1 O1W 2.0442(11) . ? Mg1 O2W 2.0901(13) . ? Mg1 O2W 2.0901(13) 3_566 ? Mg1 O1 2.1169(10) 3_566 ? Mg1 O1 2.1169(10) . ? O1 C4 1.281(2) . ? O1W H1W1 0.86(2) . ? O1W H1W2 0.86(2) . ? O2 C2 1.273(2) . ? O2W H2W1 0.85(2) . ? O2W H2W2 0.85(2) . ? N1 C1 1.302(2) . ? N1 C4 1.389(2) . ? N2 C1 1.338(2) . ? N2 C2 1.384(2) . ? N2 H2N 0.860(9) . ? C1 H1 0.9300 . ? C2 C3 1.386(2) . ? C3 C4 1.400(2) . ? C3 H3 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 O1W Mg1 O1W 180.00(5) 3_566 . ? O1W Mg1 O2W 88.79(5) 3_566 . ? O1W Mg1 O2W 91.21(5) . . ? O1W Mg1 O2W 91.21(5) 3_566 3_566 ? O1W Mg1 O2W 88.79(5) . 3_566 ? O2W Mg1 O2W 180.0 . 3_566 ? O1W Mg1 O1 91.21(5) 3_566 3_566 ? O1W Mg1 O1 88.79(5) . 3_566 ? O2W Mg1 O1 90.29(4) . 3_566 ? O2W Mg1 O1 89.71(4) 3_566 3_566 ? O1W Mg1 O1 88.79(5) 3_566 . ? O1W Mg1 O1 91.21(5) . . ? O2W Mg1 O1 89.71(5) . . ? O2W Mg1 O1 90.29(4) 3_566 . ? O1 Mg1 O1 180.00(6) 3_566 . ? C4 O1 Mg1 136.67(9) . . ? Mg1 O1W H1W1 108.3(14) . . ? Mg1 O1W H1W2 141.5(14) . . ? H1W1 O1W H1W2 108.2(14) . . ? Mg1 O2W H2W1 117.4(14) . . ? Mg1 O2W H2W2 113.1(14) . . ? H2W1 O2W H2W2 109.1(13) . . ? C1 N1 C4 117.95(12) . . ? C1 N2 C2 121.45(12) . . ? C1 N2 H2N 121.6(13) . . ? C2 N2 H2N 116.7(13) . . ? N1 C1 N2 124.27(13) . . ? N1 C1 H1 117.9 . . ? N2 C1 H1 117.9 . . ? O2 C2 N2 116.99(12) . . ? O2 C2 C3 127.09(13) . . ? N2 C2 C3 115.92(12) . . ? C2 C3 C4 120.90(13) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? O1 C4 N1 117.37(12) . . ? O1 C4 C3 123.16(13) . . ? N1 C4 C3 119.47(12) . . ? 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 O1W Mg1 O1 C4 14.45(15) 3_566 . . . ? O1W Mg1 O1 C4 -165.55(15) . . . . ? O2W Mg1 O1 C4 103.25(15) . . . . ? O2W Mg1 O1 C4 -76.75(15) 3_566 . . . ? C4 N1 C1 N2 -1.9(2) . . . . ? C2 N2 C1 N1 0.2(2) . . . . ? C1 N2 C2 O2 -178.45(14) . . . . ? C1 N2 C2 C3 1.5(2) . . . . ? O2 C2 C3 C4 178.56(15) . . . . ? N2 C2 C3 C4 -1.3(2) . . . . ? Mg1 O1 C4 N1 -1.1(2) . . . . ? Mg1 O1 C4 C3 178.67(11) . . . . ? C1 N1 C4 O1 -178.24(14) . . . . ? C1 N1 C4 C3 2.0(2) . . . . ? C2 C3 C4 O1 179.89(14) . . . . ? C2 C3 C4 N1 -0.3(2) . . . . ? 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 O1W H1W1 N1 0.86(2) 1.87(2) 2.678(2) 157(2) 3_566 O1W H1W2 O2 0.86(2) 1.84(2) 2.696(2) 174(2) 2_655 O2W H2W1 O1 0.85(2) 1.90(2) 2.753(2) 175(2) 3_666 O2W H2W2 O2 0.85(2) 2.04(2) 2.862(2) 162.2(17) 4_566 N2 H2N O2 0.860(9) 1.95(2) 2.798(2) 166.8(19) 3_656 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.332 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.068 # Attachment 'complex 2.cif' data_w _database_code_depnum_ccdc_archive 'CCDC 853185' #TrackingRef 'complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H12 Ca N4 O7, H2 O' _chemical_formula_sum 'C8 H14 Ca N4 O8' _chemical_formula_weight 334.31 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' Ca Ca 0.2262 0.3064 '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 c c a' _symmetry_space_group_name_Hall '-P 2a 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 14.347(3) _cell_length_b 14.902(3) _cell_length_c 12.099(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2586.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 17751 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8779 _exptl_absorpt_correction_T_max 0.9241 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23744 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.44 _reflns_number_total 2953 _reflns_number_gt 2513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0678P)^2^+0.8192P] 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 2953 _refine_ls_number_parameters 220 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.048 _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 Ca1 Ca 0.64411(2) 0.75946(2) 0.77894(3) 0.01757(12) Uani 1 1 d . . . O1 O 0.62817(10) 0.60077(9) 0.72616(10) 0.0299(3) Uani 1 1 d . . . O1W O 0.80927(10) 0.75692(9) 0.80607(12) 0.0318(3) Uani 1 1 d D . . H1W1 H 0.8427(16) 0.7525(15) 0.7482(12) 0.048 Uiso 1 1 d D . . H1W2 H 0.8377(16) 0.7352(16) 0.8604(13) 0.048 Uiso 1 1 d D . . O2W O 0.72230(9) 0.74230(9) 0.59694(11) 0.0255(3) Uani 1 1 d D . . H2W1 H 0.7534(14) 0.7785(13) 0.5560(16) 0.038 Uiso 1 1 d D . . H2W2 H 0.6857(13) 0.7132(14) 0.5549(15) 0.038 Uiso 1 1 d D . . O2 O 0.59049(9) 0.34798(8) 0.95958(10) 0.0288(3) Uani 1 1 d . . . O3W O 0.48836(9) 0.75143(7) 0.86565(10) 0.0201(3) Uani 1 1 d D . . H3W1 H 0.4771(15) 0.7045(7) 0.9022(15) 0.030 Uiso 1 1 d D . . H3W2 H 0.4706(15) 0.7969(8) 0.9028(15) 0.030 Uiso 1 1 d D . . O3 O 0.62576(10) 0.90935(8) 0.70893(10) 0.0275(3) Uani 1 1 d . . . O4W O 0.55946(11) 0.75262(11) 1.13450(13) 0.0398(4) Uani 1 1 d D . . H4W1 H 0.5840(17) 0.7718(18) 1.0746(14) 0.060 Uiso 1 1 d D . . H4W2 H 0.5104(12) 0.7242(17) 1.121(2) 0.060 Uiso 1 1 d D . . O4 O 0.66183(9) 1.15223(8) 0.45747(10) 0.0268(3) Uani 1 1 d . . . N1 N 0.64645(11) 0.61375(10) 0.91091(13) 0.0260(3) Uani 1 1 d . . . N2 N 0.62696(11) 0.48715(10) 1.02390(12) 0.0250(3) Uani 1 1 d D . . H2N H 0.6267(16) 0.4621(15) 1.0891(11) 0.038 Uiso 1 1 d D . . N3 N 0.58746(10) 0.89460(10) 0.52785(12) 0.0247(3) Uani 1 1 d . . . N4 N 0.61742(11) 1.01215(10) 0.40498(11) 0.0244(3) Uani 1 1 d D . . H4N H 0.6189(15) 1.0364(15) 0.3394(11) 0.037 Uiso 1 1 d D . . C1 C 0.62679(12) 0.56033(11) 0.81919(14) 0.0234(4) Uani 1 1 d . . . C2 C 0.60744(13) 0.46867(11) 0.83223(14) 0.0264(4) Uani 1 1 d . . . H2 H 0.5952 0.4335 0.7704 0.032 Uiso 1 1 calc R . . C3 C 0.60644(11) 0.43009(11) 0.93669(14) 0.0206(3) Uani 1 1 d . . . C4 C 0.64561(12) 0.57428(11) 1.00633(14) 0.0245(4) Uani 1 1 d . . . H4 H 0.6591 0.6093 1.0679 0.029 Uiso 1 1 calc R . . C5 C 0.62021(12) 0.94787(11) 0.61356(13) 0.0205(3) Uani 1 1 d . . . C6 C 0.64415(12) 1.03746(12) 0.59419(14) 0.0230(4) Uani 1 1 d . . . H6 H 0.6610 1.0741 0.6531 0.028 Uiso 1 1 calc R . . C7 C 0.64289(11) 1.07217(10) 0.48742(14) 0.0190(3) Uani 1 1 d . . . C8 C 0.58927(12) 0.92880(11) 0.42909(14) 0.0228(3) Uani 1 1 d . . . H8 H 0.5696 0.8927 0.3709 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0214(2) 0.01791(19) 0.01344(19) 0.00047(11) 0.00025(11) 0.00012(12) O1 0.0527(8) 0.0193(6) 0.0177(6) 0.0051(5) 0.0005(5) -0.0018(6) O1W 0.0263(7) 0.0484(8) 0.0206(7) 0.0024(6) -0.0008(6) 0.0046(6) O2W 0.0267(7) 0.0320(7) 0.0179(6) -0.0003(5) 0.0021(5) -0.0034(5) O2 0.0435(7) 0.0199(6) 0.0230(6) 0.0044(5) 0.0011(5) -0.0045(5) O3W 0.0253(6) 0.0193(6) 0.0156(5) 0.0001(4) 0.0041(5) 0.0007(5) O3 0.0484(8) 0.0200(6) 0.0142(6) -0.0005(5) -0.0001(5) 0.0001(6) O4W 0.0343(8) 0.0542(10) 0.0307(8) 0.0033(6) -0.0056(7) -0.0088(6) O4 0.0375(7) 0.0204(6) 0.0225(6) 0.0053(5) -0.0024(5) -0.0040(5) N1 0.0356(8) 0.0211(7) 0.0212(8) 0.0011(6) 0.0008(6) 0.0004(6) N2 0.0365(8) 0.0230(7) 0.0155(7) 0.0020(6) -0.0003(6) -0.0007(6) N3 0.0357(8) 0.0203(7) 0.0181(7) 0.0012(5) -0.0010(6) -0.0020(6) N4 0.0369(8) 0.0226(7) 0.0138(7) 0.0025(5) -0.0012(6) -0.0005(6) C1 0.0296(8) 0.0213(8) 0.0193(8) 0.0018(6) 0.0007(7) 0.0011(7) C2 0.0405(10) 0.0210(8) 0.0178(8) -0.0011(6) -0.0032(7) -0.0026(7) C3 0.0255(8) 0.0185(8) 0.0178(8) 0.0017(6) 0.0014(6) 0.0000(6) C4 0.0337(9) 0.0207(8) 0.0192(8) -0.0016(6) -0.0009(7) 0.0003(7) C5 0.0252(8) 0.0205(8) 0.0158(8) 0.0010(6) 0.0011(6) 0.0028(7) C6 0.0315(9) 0.0217(8) 0.0159(8) -0.0009(6) -0.0032(6) -0.0003(7) C7 0.0199(8) 0.0169(7) 0.0201(8) 0.0010(6) -0.0004(6) 0.0009(6) C8 0.0345(9) 0.0182(8) 0.0159(7) -0.0011(6) -0.0018(7) -0.0002(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 Ca1 O1W 2.3925(16) . ? Ca1 O3 2.4034(13) . ? Ca1 O1 2.4602(14) . ? Ca1 O3W 2.4715(13) . ? Ca1 O2W 2.4846(14) . ? Ca1 O4 2.5421(13) 7_576 ? Ca1 O3W 2.5860(13) 3_656 ? Ca1 N1 2.6954(16) . ? Ca1 C1 3.0173(18) . ? O1 C1 1.277(2) . ? O1W H1W1 0.85(9) . ? O1W H1W2 0.84(9) . ? O2W H2W1 0.86(9) . ? O2W H2W2 0.85(9) . ? O2 C3 1.275(2) . ? O3W Ca1 2.5860(13) 3_656 ? O3W H3W1 0.84(9) . ? O3W H3W2 0.85(9) . ? O3 C5 1.291(2) . ? O4W H4W1 0.86(9) . ? O4W H4W2 0.84(9) . ? O4 C7 1.276(2) . ? O4 Ca1 2.5421(13) 7_575 ? N1 C4 1.296(2) . ? N1 C1 1.395(2) . ? N2 C4 1.343(2) . ? N2 C3 1.387(2) . ? N2 H2N 0.87(9) . ? N3 C8 1.299(2) . ? N3 C5 1.388(2) . ? N4 C8 1.338(2) . ? N4 C7 1.389(2) . ? N4 H4N 0.87(9) . ? C1 C2 1.403(2) . ? C2 C3 1.389(2) . ? C2 H2 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.398(2) . ? C6 C7 1.392(2) . ? C6 H6 0.9300 . ? C8 H8 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 O1W Ca1 O3 99.88(5) . . ? O1W Ca1 O1 96.46(5) . . ? O3 Ca1 O1 142.34(5) . . ? O1W Ca1 O3W 146.77(5) . . ? O3 Ca1 O3W 95.48(4) . . ? O1 Ca1 O3W 88.83(4) . . ? O1W Ca1 O2W 70.90(5) . . ? O3 Ca1 O2W 80.37(4) . . ? O1 Ca1 O2W 73.32(4) . . ? O3W Ca1 O2W 141.21(4) . . ? O1W Ca1 O4 78.03(5) . 7_576 ? O3 Ca1 O4 80.17(4) . 7_576 ? O1 Ca1 O4 136.67(4) . 7_576 ? O3W Ca1 O4 75.80(4) . 7_576 ? O2W Ca1 O4 139.57(5) . 7_576 ? O1W Ca1 O3W 145.09(5) . 3_656 ? O3 Ca1 O3W 73.98(4) . 3_656 ? O1 Ca1 O3W 73.24(4) . 3_656 ? O3W Ca1 O3W 67.69(5) . 3_656 ? O2W Ca1 O3W 74.19(4) . 3_656 ? O4 Ca1 O3W 132.24(4) 7_576 3_656 ? O1W Ca1 N1 83.90(5) . . ? O3 Ca1 N1 163.50(5) . . ? O1 Ca1 N1 51.73(4) . . ? O3W Ca1 N1 73.79(4) . . ? O2W Ca1 N1 115.88(5) . . ? O4 Ca1 N1 84.97(4) 7_576 . ? O3W Ca1 N1 111.88(4) 3_656 . ? O1W Ca1 C1 92.52(5) . . ? O3 Ca1 C1 164.13(5) . . ? O1 Ca1 C1 24.34(4) . . ? O3W Ca1 C1 79.01(4) . . ? O2W Ca1 C1 94.53(5) . . ? O4 Ca1 C1 112.35(5) 7_576 . ? O3W Ca1 C1 90.18(4) 3_656 . ? N1 Ca1 C1 27.53(5) . . ? O1W Ca1 Ca1 178.05(4) . 3_656 ? O3 Ca1 Ca1 80.39(4) . 3_656 ? O1 Ca1 Ca1 82.24(4) . 3_656 ? O3W Ca1 Ca1 34.86(3) . 3_656 ? O2W Ca1 Ca1 107.29(3) . 3_656 ? O4 Ca1 Ca1 103.91(3) 7_576 3_656 ? O3W Ca1 Ca1 33.11(3) 3_656 3_656 ? N1 Ca1 Ca1 96.38(3) . 3_656 ? C1 Ca1 Ca1 86.89(3) . 3_656 ? C1 O1 Ca1 103.08(11) . . ? Ca1 O1W H1W1 116.5(18) . . ? Ca1 O1W H1W2 126.5(17) . . ? H1W1 O1W H1W2 109.9(15) . . ? Ca1 O2W H2W1 133.0(15) . . ? Ca1 O2W H2W2 107.7(14) . . ? H2W1 O2W H2W2 107.3(14) . . ? Ca1 O3W Ca1 112.03(5) . 3_656 ? Ca1 O3W H3W1 115.9(14) . . ? Ca1 O3W H3W1 104.6(15) 3_656 . ? Ca1 O3W H3W2 117.2(14) . . ? Ca1 O3W H3W2 95.7(15) 3_656 . ? H3W1 O3W H3W2 109.0(14) . . ? C5 O3 Ca1 137.30(11) . . ? H4W1 O4W H4W2 110.3(16) . . ? C7 O4 Ca1 134.74(11) . 7_575 ? C4 N1 C1 116.61(15) . . ? C4 N1 Ca1 153.30(12) . . ? C1 N1 Ca1 89.19(10) . . ? C4 N2 C3 120.99(15) . . ? C4 N2 H2N 123.9(16) . . ? C3 N2 H2N 115.1(16) . . ? C8 N3 C5 117.13(15) . . ? C8 N4 C7 121.38(14) . . ? C8 N4 H4N 126.2(16) . . ? C7 N4 H4N 112.3(16) . . ? O1 C1 N1 115.40(15) . . ? O1 C1 C2 124.17(16) . . ? N1 C1 C2 120.42(15) . . ? O1 C1 Ca1 52.58(9) . . ? N1 C1 Ca1 63.28(9) . . ? C2 C1 Ca1 172.79(13) . . ? C3 C2 C1 120.50(16) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? O2 C3 C2 126.64(16) . . ? O2 C3 N2 117.47(15) . . ? C2 C3 N2 115.88(15) . . ? N1 C4 N2 125.59(16) . . ? N1 C4 H4 117.2 . . ? N2 C4 H4 117.2 . . ? O3 C5 N3 115.74(14) . . ? O3 C5 C6 123.99(15) . . ? N3 C5 C6 120.27(15) . . ? C7 C6 C5 120.48(15) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O4 C7 C6 127.46(15) . . ? O4 C7 N4 117.02(15) . . ? C6 C7 N4 115.52(14) . . ? N3 C8 N4 124.78(16) . . ? N3 C8 H8 117.6 . . ? N4 C8 H8 117.6 . . ? 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 O1W Ca1 O1 C1 81.78(12) . . . . ? O3 Ca1 O1 C1 -162.80(10) . . . . ? O3W Ca1 O1 C1 -65.33(11) . . . . ? O2W Ca1 O1 C1 149.59(12) . . . . ? O4 Ca1 O1 C1 2.39(15) 7_576 . . . ? O3W Ca1 O1 C1 -132.35(12) 3_656 . . . ? N1 Ca1 O1 C1 4.82(10) . . . . ? Ca1 Ca1 O1 C1 -99.69(11) 3_656 . . . ? O1W Ca1 O3W Ca1 -178.09(6) . . . 3_656 ? O3 Ca1 O3W Ca1 64.46(5) . . . 3_656 ? O1 Ca1 O3W Ca1 -78.05(5) . . . 3_656 ? O2W Ca1 O3W Ca1 -16.97(9) . . . 3_656 ? O4 Ca1 O3W Ca1 142.86(5) 7_576 . . 3_656 ? O3W Ca1 O3W Ca1 -5.72(5) 3_656 . . 3_656 ? N1 Ca1 O3W Ca1 -128.32(5) . . . 3_656 ? C1 Ca1 O3W Ca1 -100.49(5) . . . 3_656 ? O1W Ca1 O3 C5 95.55(18) . . . . ? O1 Ca1 O3 C5 -18.8(2) . . . . ? O3W Ca1 O3 C5 -114.03(17) . . . . ? O2W Ca1 O3 C5 27.05(17) . . . . ? O4 Ca1 O3 C5 171.43(18) 7_576 . . . ? O3W Ca1 O3 C5 -49.14(17) 3_656 . . . ? N1 Ca1 O3 C5 -162.45(17) . . . . ? C1 Ca1 O3 C5 -45.3(3) . . . . ? Ca1 Ca1 O3 C5 -82.49(17) 3_656 . . . ? O1W Ca1 N1 C4 86.8(3) . . . . ? O3 Ca1 N1 C4 -17.5(4) . . . . ? O1 Ca1 N1 C4 -170.0(3) . . . . ? O3W Ca1 N1 C4 -68.3(3) . . . . ? O2W Ca1 N1 C4 152.1(3) . . . . ? O4 Ca1 N1 C4 8.3(3) 7_576 . . . ? O3W Ca1 N1 C4 -125.5(3) 3_656 . . . ? C1 Ca1 N1 C4 -165.7(3) . . . . ? Ca1 Ca1 N1 C4 -95.2(3) 3_656 . . . ? O1W Ca1 N1 C1 -107.50(10) . . . . ? O3 Ca1 N1 C1 148.22(17) . . . . ? O1 Ca1 N1 C1 -4.30(9) . . . . ? O3W Ca1 N1 C1 97.38(10) . . . . ? O2W Ca1 N1 C1 -42.19(11) . . . . ? O4 Ca1 N1 C1 174.03(10) 7_576 . . . ? O3W Ca1 N1 C1 40.25(11) 3_656 . . . ? Ca1 Ca1 N1 C1 70.56(10) 3_656 . . . ? Ca1 O1 C1 N1 -8.11(17) . . . . ? Ca1 O1 C1 C2 172.05(15) . . . . ? C4 N1 C1 O1 -179.91(16) . . . . ? Ca1 N1 C1 O1 7.21(15) . . . . ? C4 N1 C1 C2 -0.1(2) . . . . ? Ca1 N1 C1 C2 -172.95(15) . . . . ? C4 N1 C1 Ca1 172.88(17) . . . . ? O1W Ca1 C1 O1 -100.14(12) . . . . ? O3 Ca1 C1 O1 41.3(2) . . . . ? O3W Ca1 C1 O1 112.26(12) . . . . ? O2W Ca1 C1 O1 -29.11(12) . . . . ? O4 Ca1 C1 O1 -178.23(11) 7_576 . . . ? O3W Ca1 C1 O1 45.04(12) 3_656 . . . ? N1 Ca1 C1 O1 -171.80(17) . . . . ? Ca1 Ca1 C1 O1 78.00(11) 3_656 . . . ? O1W Ca1 C1 N1 71.66(10) . . . . ? O3 Ca1 C1 N1 -146.86(16) . . . . ? O1 Ca1 C1 N1 171.80(17) . . . . ? O3W Ca1 C1 N1 -75.95(10) . . . . ? O2W Ca1 C1 N1 142.69(10) . . . . ? O4 Ca1 C1 N1 -6.43(11) 7_576 . . . ? O3W Ca1 C1 N1 -143.16(10) 3_656 . . . ? Ca1 Ca1 C1 N1 -110.20(10) 3_656 . . . ? O1 C1 C2 C3 -179.35(17) . . . . ? N1 C1 C2 C3 0.8(3) . . . . ? C1 C2 C3 O2 -179.55(17) . . . . ? C1 C2 C3 N2 -1.0(3) . . . . ? C4 N2 C3 O2 179.22(16) . . . . ? C4 N2 C3 C2 0.6(2) . . . . ? C1 N1 C4 N2 -0.4(3) . . . . ? Ca1 N1 C4 N2 163.55(19) . . . . ? C3 N2 C4 N1 0.2(3) . . . . ? Ca1 O3 C5 N3 25.7(3) . . . . ? Ca1 O3 C5 C6 -154.76(14) . . . . ? C8 N3 C5 O3 -173.75(16) . . . . ? C8 N3 C5 C6 6.7(2) . . . . ? O3 C5 C6 C7 175.14(16) . . . . ? N3 C5 C6 C7 -5.4(3) . . . . ? Ca1 O4 C7 C6 -169.48(13) 7_575 . . . ? Ca1 O4 C7 N4 10.1(2) 7_575 . . . ? C5 C6 C7 O4 179.13(16) . . . . ? C5 C6 C7 N4 -0.4(2) . . . . ? C8 N4 C7 O4 -174.70(16) . . . . ? C8 N4 C7 C6 4.9(2) . . . . ? C5 N3 C8 N4 -2.3(3) . . . . ? C7 N4 C8 N3 -3.7(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 O1W H1W1 O4W 0.85(9) 1.96(9) 2.804(2) 168(3) 8_755 O1W H1W2 O2 0.84(9) 2.01(9) 2.822(9) 163(2) 2_665 O2W H2W1 O4 0.86(9) 1.99(9) 2.843(9) 172(2) 2_675 O2W H2W2 O2 0.85(9) 2.01(9) 2.855(9) 175(2) 7_565 O3W H3W1 O2 0.84(9) 2.09(9) 2.819(9) 145.2(16) 5_667 O3W H3W2 N3 0.85(9) 1.88(9) 2.720(9) 170(2) 3_656 O3W H3W2 O3 0.85(9) 2.56(9) 3.006(9) 113.8(16) 3_656 O4W H4W1 O4 0.86(9) 2.13(9) 2.959(2) 163(2) 7_576 O4W H4W2 O2 0.84(9) 2.05(9) 2.859(2) 162(2) 5_667 N2 H2N O1 0.87(9) 1.91(9) 2.776(2) 176(2) 7_566 N4 H4N O3 0.87(9) 1.78(9) 2.648(9) 177(2) 7_575 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.681 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.118 # Attachment 'complex 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 853186' #TrackingRef 'complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H12 N4 O7 Sr, H2 O' _chemical_formula_sum 'C8 H14 N4 O8 Sr' _chemical_formula_weight 381.85 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 orthorhombic _symmetry_space_group_name_H-M 'P bca' _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 12.169(2) _cell_length_b 14.549(3) _cell_length_c 15.315(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2711.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 16547 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.40 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 4.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5311 _exptl_absorpt_correction_T_max 0.6438 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18149 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3072 _reflns_number_gt 2047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0197P)^2^+9.8788P] 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 3072 _refine_ls_number_parameters 220 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.096 _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 0.53196(3) 0.35187(2) 0.49928(5) 0.02551(13) Uani 1 1 d . . . O1 O 0.4686(3) 0.3709(3) 0.6577(2) 0.0404(10) Uani 1 1 d . . . O1W O 0.5608(3) 0.1795(2) 0.4952(4) 0.0398(8) Uani 1 1 d D . . H1W1 H 0.507(3) 0.142(3) 0.494(6) 0.060 Uiso 1 1 d D . . H1W2 H 0.614(3) 0.158(4) 0.466(4) 0.060 Uiso 1 1 d D . . O2W O 0.3404(2) 0.2740(2) 0.5013(5) 0.0404(8) Uani 1 1 d D . . H2W1 H 0.287(3) 0.284(5) 0.467(3) 0.061 Uiso 1 1 d D . . H2W2 H 0.323(5) 0.232(3) 0.537(3) 0.061 Uiso 1 1 d D . . O2 O 0.7071(3) 0.4230(3) 0.8987(2) 0.0401(9) Uani 1 1 d . . . O3W O 0.6228(2) 0.5146(2) 0.4984(3) 0.0271(6) Uani 1 1 d D . . H3W1 H 0.672(3) 0.519(5) 0.459(3) 0.041 Uiso 1 1 d D . . H3W2 H 0.647(4) 0.537(4) 0.546(2) 0.041 Uiso 1 1 d D . . O3 O 0.4655(5) 0.3727(4) 0.3403(4) 0.0544(14) Uani 1 1 d . . . O4 O 0.2087(3) 0.3365(3) 0.1029(2) 0.0357(9) Uani 1 1 d . . . O4W O 0.3851(3) 0.0586(3) 0.5016(6) 0.0586(10) Uani 1 1 d D . . H4W1 H 0.321(2) 0.076(5) 0.486(5) 0.088 Uiso 1 1 d D . . H4W2 H 0.381(5) 0.014(4) 0.537(4) 0.088 Uiso 1 1 d D . . N1 N 0.6606(3) 0.3535(3) 0.6438(3) 0.0294(9) Uani 1 1 d . . . N2 N 0.7732(3) 0.3788(3) 0.7659(3) 0.0308(9) Uani 1 1 d D . . H2N H 0.8414(18) 0.370(5) 0.778(5) 0.046 Uiso 1 1 d D . . N3 N 0.2766(3) 0.4070(3) 0.3536(3) 0.0326(10) Uani 1 1 d . . . N4 N 0.1563(3) 0.3814(3) 0.2377(3) 0.0300(9) Uani 1 1 d D . . H4N H 0.0865(14) 0.378(5) 0.229(5) 0.045 Uiso 1 1 d D . . C1 C 0.7501(4) 0.3552(3) 0.6781(3) 0.058(2) Uani 1 1 d . . . H1A H 0.8098 0.3394 0.6433 0.055 Uiso 1 1 calc R . . C2 C 0.5702(4) 0.3729(4) 0.6944(3) 0.0259(10) Uani 1 1 d . . . C3 C 0.5827(4) 0.3957(4) 0.7820(4) 0.0340(12) Uani 1 1 d . . . H3A H 0.5205 0.4068 0.8156 0.041 Uiso 1 1 calc R . . C4 C 0.6862(4) 0.4025(3) 0.8206(4) 0.0226(11) Uani 1 1 d . . . C5 C 0.1781(5) 0.4045(5) 0.3189(4) 0.0383(16) Uani 1 1 d . . . H5A H 0.1191 0.4204 0.3544 0.046 Uiso 1 1 calc R . . C6 C 0.3621(4) 0.3778(4) 0.3016(3) 0.0251(10) Uani 1 1 d . . . C7 C 0.3441(4) 0.3528(4) 0.2142(3) 0.0298(11) Uani 1 1 d . . . H7A H 0.4012 0.3344 0.1778 0.036 Uiso 1 1 calc R . . C8 C 0.2432(7) 0.3569(6) 0.1870(5) 0.053(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.01821(18) 0.0265(2) 0.0318(2) -0.0071(3) 0.0088(3) -0.00083(14) O1 0.036(2) 0.059(3) 0.025(2) -0.0130(19) -0.0027(17) -0.005(2) O1W 0.0370(17) 0.0334(17) 0.049(2) -0.004(3) 0.020(2) -0.0007(14) O2W 0.0269(15) 0.0381(19) 0.056(2) 0.017(3) -0.010(2) -0.0055(13) O2 0.0319(18) 0.062(3) 0.0267(19) -0.0126(18) -0.0026(16) -0.0079(18) O3W 0.0226(13) 0.0322(16) 0.0267(14) 0.023(2) -0.0055(18) -0.0053(11) O3 0.058(3) 0.059(3) 0.047(3) -0.005(3) -0.003(3) -0.010(3) O4 0.0296(18) 0.051(2) 0.0263(18) -0.0116(16) -0.0092(15) 0.0040(17) O4W 0.0376(18) 0.042(2) 0.096(3) -0.004(4) -0.006(4) -0.0024(16) N1 0.0248(19) 0.047(3) 0.0162(18) -0.0041(18) 0.0044(16) 0.0042(19) N2 0.027(2) 0.038(2) 0.027(2) -0.0012(18) -0.0058(17) 0.0014(18) N3 0.0210(19) 0.053(3) 0.024(2) -0.0052(19) -0.0031(16) 0.0044(19) N4 0.0186(18) 0.046(2) 0.025(2) -0.0034(19) 0.0018(16) 0.0029(18) C1 0.057(4) 0.075(6) 0.048(5) 0.005(4) 0.001(4) 0.003(4) C2 0.018(2) 0.042(3) 0.019(2) -0.001(2) -0.0005(17) 0.0011(19) C3 0.022(2) 0.051(3) 0.029(3) -0.008(2) 0.003(2) 0.003(2) C4 0.019(2) 0.023(3) 0.026(3) -0.006(2) 0.009(2) -0.0026(19) C5 0.024(3) 0.072(5) 0.019(3) -0.001(3) -0.012(2) 0.001(3) C6 0.019(2) 0.033(2) 0.023(2) 0.002(2) -0.0051(17) -0.0022(18) C7 0.022(2) 0.047(3) 0.021(2) -0.007(2) 0.0047(18) 0.006(2) C8 0.050(4) 0.066(5) 0.043(4) 0.001(4) 0.006(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1W 2.533(3) . ? Sr1 O1 2.560(4) . ? Sr1 O3 2.583(6) . ? Sr1 O2W 2.591(3) . ? Sr1 O3W 2.612(3) . ? Sr1 O4 2.670(3) 6_656 ? Sr1 O3W 2.706(3) 5_666 ? Sr1 N1 2.711(4) . ? Sr1 C2 3.040(5) . ? O1 C2 1.358(6) . ? O1W H1W1 0.849(10) . ? O1W H1W2 0.848(10) . ? O2W H2W1 0.851(10) . ? O2W H2W2 0.850(10) . ? O2 C4 1.259(6) . ? O3W Sr1 2.706(3) 5_666 ? O3W H3W1 0.851(10) . ? O3W H3W2 0.849(10) . ? O3 C6 1.393(7) . ? O4 C8 1.386(9) . ? O4 Sr1 2.670(3) 6_556 ? O4W H4W1 0.849(10) . ? O4W H4W2 0.847(10) . ? N1 C1 1.209(7) . ? N1 C2 1.376(6) . ? N2 C4 1.393(6) . ? N2 C1 1.417(6) . ? N2 H2N 0.861(10) . ? N3 C5 1.311(7) . ? N3 C6 1.377(6) . ? N4 C5 1.315(8) . ? N4 C8 1.360(9) . ? N4 H4N 0.861(10) . ? C1 H1A 0.9300 . ? C2 C3 1.390(7) . ? C3 C4 1.395(7) . ? C3 H3A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.405(7) . ? C7 C8 1.297(10) . ? C7 H7A 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 O1W Sr1 O1 99.90(17) . . ? O1W Sr1 O3 97.83(18) . . ? O1 Sr1 O3 141.83(11) . . ? O1W Sr1 O2W 72.08(11) . . ? O1 Sr1 O2W 76.43(18) . . ? O3 Sr1 O2W 77.3(2) . . ? O1W Sr1 O3W 146.97(10) . . ? O1 Sr1 O3W 91.97(16) . . ? O3 Sr1 O3W 91.22(16) . . ? O2W Sr1 O3W 140.94(10) . . ? O1W Sr1 O4 77.94(13) . 6_656 ? O1 Sr1 O4 143.81(12) . 6_656 ? O3 Sr1 O4 73.11(16) . 6_656 ? O2W Sr1 O4 134.03(17) . 6_656 ? O3W Sr1 O4 74.46(13) . 6_656 ? O1W Sr1 O3W 143.87(9) . 5_666 ? O1 Sr1 O3W 72.57(15) . 5_666 ? O3 Sr1 O3W 73.18(18) . 5_666 ? O2W Sr1 O3W 71.81(9) . 5_666 ? O3W Sr1 O3W 69.13(9) . 5_666 ? O4 Sr1 O3W 128.95(12) 6_656 5_666 ? O1W Sr1 N1 87.04(16) . . ? O1 Sr1 N1 53.09(12) . . ? O3 Sr1 N1 161.65(16) . . ? O2W Sr1 N1 120.90(17) . . ? O3W Sr1 N1 75.66(13) . . ? O4 Sr1 N1 90.80(13) 6_656 . ? O3W Sr1 N1 112.64(14) 5_666 . ? O1W Sr1 C2 95.87(18) . . ? O1 Sr1 C2 26.32(12) . . ? O3 Sr1 C2 164.30(17) . . ? O2W Sr1 C2 99.78(18) . . ? O3W Sr1 C2 81.34(15) . . ? O4 Sr1 C2 117.49(12) 6_656 . ? O3W Sr1 C2 91.21(14) 5_666 . ? N1 Sr1 C2 26.91(12) . . ? O1W Sr1 Sr1 177.47(10) . 5_666 ? O1 Sr1 Sr1 80.52(11) . 5_666 ? O3 Sr1 Sr1 80.45(12) . 5_666 ? O2W Sr1 Sr1 105.67(8) . 5_666 ? O3W Sr1 Sr1 35.26(6) . 5_666 ? O4 Sr1 Sr1 103.21(9) 6_656 5_666 ? O3W Sr1 Sr1 33.87(5) 5_666 5_666 ? N1 Sr1 Sr1 95.17(10) . 5_666 ? C2 Sr1 Sr1 85.60(10) . 5_666 ? C2 O1 Sr1 97.0(3) . . ? Sr1 O1W H1W1 122(4) . . ? Sr1 O1W H1W2 119(4) . . ? H1W1 O1W H1W2 110(6) . . ? Sr1 O2W H2W1 127(4) . . ? Sr1 O2W H2W2 123(4) . . ? H2W1 O2W H2W2 109(6) . . ? Sr1 O3W Sr1 110.87(9) . 5_666 ? Sr1 O3W H3W1 111(4) . . ? Sr1 O3W H3W1 116(4) 5_666 . ? Sr1 O3W H3W2 120(5) . . ? Sr1 O3W H3W2 87(4) 5_666 . ? H3W1 O3W H3W2 110(5) . . ? C6 O3 Sr1 133.6(4) . . ? C8 O4 Sr1 140.4(4) . 6_556 ? H4W1 O4W H4W2 111(6) . . ? C1 N1 C2 118.1(4) . . ? C1 N1 Sr1 151.1(3) . . ? C2 N1 Sr1 90.0(3) . . ? C4 N2 C1 118.6(4) . . ? C4 N2 H2N 130(5) . . ? C1 N2 H2N 111(5) . . ? C5 N3 C6 116.6(5) . . ? C5 N4 C8 116.7(5) . . ? C5 N4 H4N 111(5) . . ? C8 N4 H4N 132(5) . . ? N1 C1 N2 126.7(4) . . ? N1 C1 H1A 116.7 . . ? N2 C1 H1A 116.7 . . ? O1 C2 N1 119.3(4) . . ? O1 C2 C3 120.3(4) . . ? N1 C2 C3 120.4(4) . . ? O1 C2 Sr1 56.7(2) . . ? N1 C2 Sr1 63.1(2) . . ? C3 C2 Sr1 171.6(4) . . ? C2 C3 C4 121.7(5) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? O2 C4 N2 118.4(4) . . ? O2 C4 C3 127.0(5) . . ? N2 C4 C3 114.5(5) . . ? N3 C5 N4 125.1(6) . . ? N3 C5 H5A 117.4 . . ? N4 C5 H5A 117.4 . . ? N3 C6 O3 117.0(4) . . ? N3 C6 C7 120.9(4) . . ? O3 C6 C7 122.1(5) . . ? C8 C7 C6 116.2(5) . . ? C8 C7 H7A 121.9 . . ? C6 C7 H7A 121.9 . . ? C7 C8 N4 124.4(7) . . ? C7 C8 O4 125.1(7) . . ? N4 C8 O4 110.5(7) . . ? 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 O1W Sr1 O1 C2 83.2(3) . . . . ? O3 Sr1 O1 C2 -160.3(3) . . . . ? O2W Sr1 O1 C2 151.9(4) . . . . ? O3W Sr1 O1 C2 -65.8(3) . . . . ? O4 Sr1 O1 C2 0.1(5) 6_656 . . . ? O3W Sr1 O1 C2 -133.2(3) 5_666 . . . ? N1 Sr1 O1 C2 4.5(3) . . . . ? Sr1 Sr1 O1 C2 -99.3(3) 5_666 . . . ? O1W Sr1 O3W Sr1 177.9(3) . . . 5_666 ? O1 Sr1 O3W Sr1 -70.49(19) . . . 5_666 ? O3 Sr1 O3W Sr1 71.5(2) . . . 5_666 ? O2W Sr1 O3W Sr1 0.2(4) . . . 5_666 ? O4 Sr1 O3W Sr1 143.6(2) 6_656 . . 5_666 ? O3W Sr1 O3W Sr1 0.0 5_666 . . 5_666 ? N1 Sr1 O3W Sr1 -121.5(2) . . . 5_666 ? C2 Sr1 O3W Sr1 -94.65(19) . . . 5_666 ? O1W Sr1 O3 C6 95.9(5) . . . . ? O1 Sr1 O3 C6 -21.2(6) . . . . ? O2W Sr1 O3 C6 26.4(5) . . . . ? O3W Sr1 O3 C6 -115.9(5) . . . . ? O4 Sr1 O3 C6 170.7(6) 6_656 . . . ? O3W Sr1 O3 C6 -48.2(5) 5_666 . . . ? N1 Sr1 O3 C6 -159.6(5) . . . . ? C2 Sr1 O3 C6 -54.6(9) . . . . ? Sr1 Sr1 O3 C6 -82.2(5) 5_666 . . . ? O1W Sr1 N1 C1 84.3(8) . . . . ? O1 Sr1 N1 C1 -171.0(8) . . . . ? O3 Sr1 N1 C1 -21.8(11) . . . . ? O2W Sr1 N1 C1 151.3(7) . . . . ? O3W Sr1 N1 C1 -67.3(8) . . . . ? O4 Sr1 N1 C1 6.4(8) 6_656 . . . ? O3W Sr1 N1 C1 -127.0(7) 5_666 . . . ? C2 Sr1 N1 C1 -166.6(9) . . . . ? Sr1 Sr1 N1 C1 -96.9(8) 5_666 . . . ? O1W Sr1 N1 C2 -109.2(3) . . . . ? O1 Sr1 N1 C2 -4.4(3) . . . . ? O3 Sr1 N1 C2 144.7(5) . . . . ? O2W Sr1 N1 C2 -42.1(3) . . . . ? O3W Sr1 N1 C2 99.2(3) . . . . ? O4 Sr1 N1 C2 173.0(3) 6_656 . . . ? O3W Sr1 N1 C2 39.6(3) 5_666 . . . ? Sr1 Sr1 N1 C2 69.6(3) 5_666 . . . ? C2 N1 C1 N2 -2.6(8) . . . . ? Sr1 N1 C1 N2 162.2(5) . . . . ? C4 N2 C1 N1 0.3(8) . . . . ? Sr1 O1 C2 N1 -8.2(5) . . . . ? Sr1 O1 C2 C3 170.7(5) . . . . ? C1 N1 C2 O1 -179.6(5) . . . . ? Sr1 N1 C2 O1 7.7(5) . . . . ? C1 N1 C2 C3 1.4(8) . . . . ? Sr1 N1 C2 C3 -171.3(5) . . . . ? C1 N1 C2 Sr1 172.7(5) . . . . ? O1W Sr1 C2 O1 -100.5(3) . . . . ? O3 Sr1 C2 O1 50.2(8) . . . . ? O2W Sr1 C2 O1 -27.7(3) . . . . ? O3W Sr1 C2 O1 112.7(3) . . . . ? O4 Sr1 C2 O1 -179.9(3) 6_656 . . . ? O3W Sr1 C2 O1 44.0(3) 5_666 . . . ? N1 Sr1 C2 O1 -172.0(5) . . . . ? Sr1 Sr1 C2 O1 77.5(3) 5_666 . . . ? O1W Sr1 C2 N1 71.5(3) . . . . ? O1 Sr1 C2 N1 172.0(5) . . . . ? O3 Sr1 C2 N1 -137.8(6) . . . . ? O2W Sr1 C2 N1 144.3(3) . . . . ? O3W Sr1 C2 N1 -75.3(3) . . . . ? O4 Sr1 C2 N1 -7.9(3) 6_656 . . . ? O3W Sr1 C2 N1 -144.0(3) 5_666 . . . ? Sr1 Sr1 C2 N1 -110.6(3) 5_666 . . . ? O1 C2 C3 C4 -177.0(5) . . . . ? N1 C2 C3 C4 2.0(9) . . . . ? C1 N2 C4 O2 179.6(5) . . . . ? C1 N2 C4 C3 3.0(7) . . . . ? C2 C3 C4 O2 179.7(5) . . . . ? C2 C3 C4 N2 -4.0(8) . . . . ? C6 N3 C5 N4 -4.0(10) . . . . ? C8 N4 C5 N3 1.2(10) . . . . ? C5 N3 C6 O3 -174.6(6) . . . . ? C5 N3 C6 C7 4.2(8) . . . . ? Sr1 O3 C6 N3 25.0(8) . . . . ? Sr1 O3 C6 C7 -153.8(4) . . . . ? N3 C6 C7 C8 -1.6(8) . . . . ? O3 C6 C7 C8 177.1(7) . . . . ? C6 C7 C8 N4 -1.4(11) . . . . ? C6 C7 C8 O4 178.9(6) . . . . ? C5 N4 C8 C7 1.8(11) . . . . ? C5 N4 C8 O4 -178.5(6) . . . . ? Sr1 O4 C8 C7 -168.6(5) 6_556 . . . ? Sr1 O4 C8 N4 11.7(10) 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 N2 H2N O1 0.861(10) 1.83(3) 2.653(6) 159(7) 6_657 N4 H4N O3 0.861(10) 1.82(3) 2.613(7) 153(7) 6_556 O3W H3W1 O2 0.851(10) 1.93(3) 2.728(5) 155(6) 2_664 O3W H3W2 N3 0.849(10) 1.975(16) 2.818(6) 172(5) 5_666 O1W H1W1 O4W 0.849(10) 1.923(13) 2.770(5) 176(9) . O4W H4W1 O4 0.849(10) 2.59(8) 3.057(7) 116(7) 7_566 O4W H4W2 O2 0.847(10) 1.97(4) 2.735(7) 151(6) 3_646 O2W H2W1 N3 0.851(10) 2.50(5) 3.076(7) 126(5) . O2W H2W2 O4 0.850(10) 1.98(3) 2.752(6) 150(6) 7_566 O1W H1W2 O2 0.848(10) 1.93(2) 2.753(6) 163(6) 7_565 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.534 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.081 # Attachment 'complex 4.cif' data_d _database_code_depnum_ccdc_archive 'CCDC 853187' #TrackingRef 'complex 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 Ba N4 O6, H2 O ' _chemical_formula_sum 'C8 H12 Ba N4 O7' _chemical_formula_weight 413.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C m' _symmetry_space_group_name_Hall 'C -2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 9.5261(6) _cell_length_b 15.7700(9) _cell_length_c 4.3128(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.767(2) _cell_angle_gamma 90.00 _cell_volume 641.95(6) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3123 _cell_measurement_theta_min 4.32 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 3.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6025 _exptl_absorpt_correction_T_max 0.7244 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3127 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 4.32 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1489 _reflns_number_gt 1327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0319P)^2^+1.3500P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 1489 _refine_ls_number_parameters 113 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.087 _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 Ba1 Ba 0.5000 0.5000 0.5000 0.02082(10) Uani 1 2 d S . . O1 O 0.4074(4) 0.6000(2) 0.9671(9) 0.0299(7) Uani 1 1 d . . . O2 O 0.1605(4) 0.8447(2) 0.5485(10) 0.0361(9) Uani 1 1 d . . . O1W O 0.2074(7) 0.5000 0.3373(18) 0.073(3) Uani 1 2 d SD . . H1W1 H 0.140(10) 0.5000 0.45(3) 0.109 Uiso 1 2 d SD . . H1W2 H 0.174(14) 0.5000 0.144(8) 0.109 Uiso 1 2 d SD . . O2W O 0.6945(5) 0.5000 1.0703(13) 0.0280(10) Uani 1 2 d SD . . H2W H 0.746(3) 0.5440(3) 1.062(17) 0.042 Uiso 1 1 d D . . O3W O -0.0009(8) 0.5000 0.705(2) 0.061(2) Uani 1 2 d SD . . H3W1 H -0.05(3) 0.544(12) 0.70(6) 0.092 Uiso 0.50 1 d PD . . H3W2 H -0.04(3) 0.458(12) 0.77(6) 0.092 Uiso 0.50 1 d PD . . N1 N 0.4722(5) 0.7337(3) 1.1171(11) 0.0279(8) Uani 1 1 d D . . H1N H 0.536(6) 0.715(5) 1.261(12) 0.042 Uiso 1 1 d D . . N2 N 0.3558(5) 0.8556(3) 0.9086(12) 0.0346(10) Uani 1 1 d . . . C1 C 0.3828(5) 0.6788(3) 0.9346(11) 0.0236(9) Uani 1 1 d . . . C2 C 0.2740(5) 0.7173(3) 0.7354(13) 0.0292(10) Uani 1 1 d . . . H2 H 0.2099 0.6835 0.6089 0.035 Uiso 1 1 calc R . . C3 C 0.2585(5) 0.8058(3) 0.7207(12) 0.0263(10) Uani 1 1 d . . . C4 C 0.4547(6) 0.8175(3) 1.0945(15) 0.0361(12) Uani 1 1 d . . . H3 H 0.5183 0.8514 1.2221 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.02454(15) 0.01796(14) 0.01898(15) 0.000 -0.00058(10) 0.000 O1 0.0399(19) 0.0169(15) 0.0305(18) -0.0020(14) -0.0040(15) 0.0068(14) O2 0.036(2) 0.0232(17) 0.042(2) 0.0014(17) -0.0181(17) 0.0071(15) O1W 0.030(3) 0.148(9) 0.041(4) 0.000 0.005(3) 0.000 O2W 0.024(2) 0.020(2) 0.040(3) 0.000 0.004(2) 0.000 O3W 0.056(4) 0.041(4) 0.096(6) 0.000 0.040(4) 0.000 N1 0.028(2) 0.0206(19) 0.031(2) 0.0001(18) -0.0092(16) 0.0037(16) N2 0.037(2) 0.0188(19) 0.043(3) 0.000(2) -0.013(2) 0.0021(18) C1 0.024(2) 0.022(2) 0.025(2) -0.0002(19) 0.0026(18) 0.0017(17) C2 0.029(2) 0.022(2) 0.033(3) 0.001(2) -0.009(2) 0.0011(18) C3 0.025(2) 0.023(2) 0.029(2) 0.004(2) -0.0024(18) 0.0023(18) C4 0.039(3) 0.022(2) 0.042(3) -0.005(2) -0.014(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O1W 2.781(7) . ? Ba1 O2W 2.792(5) 1_554 ? Ba1 O1 2.793(4) . ? Ba1 O1 2.793(4) 2_565 ? Ba1 O1 2.828(4) 2_564 ? Ba1 O1 2.828(4) 1_554 ? Ba1 O2W 2.872(6) . ? Ba1 O2 2.880(4) 4_565 ? Ba1 O2 2.880(4) 3_545 ? O1 C1 1.270(6) . ? O1 Ba1 2.828(4) 1_556 ? O2 C3 1.269(6) . ? O2 Ba1 2.880(4) 3_455 ? O1W H1W1 0.85(6) . ? O1W H1W2 0.85(6) . ? O2W Ba1 2.792(5) 1_556 ? O2W H2W 0.85(6) . ? O3W H3W1 0.85(6) . ? O3W H3W2 0.85(6) . ? N1 C4 1.334(7) . ? N1 C1 1.383(7) . ? N1 H1N 0.86(3) . ? N2 C4 1.299(7) . ? N2 C3 1.389(7) . ? C1 C2 1.393(7) . ? C2 C3 1.404(7) . ? C2 H2 0.9300 . ? C4 H3 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 O1W Ba1 O2W 124.4(2) . 1_554 ? O1W Ba1 O1 77.20(15) . . ? O2W Ba1 O1 141.37(9) 1_554 . ? O1W Ba1 O1 77.20(15) . 2_565 ? O2W Ba1 O1 141.37(9) 1_554 2_565 ? O1 Ba1 O1 68.74(15) . 2_565 ? O1W Ba1 O1 66.61(15) . 2_564 ? O2W Ba1 O1 67.83(12) 1_554 2_564 ? O1 Ba1 O1 143.76(16) . 2_564 ? O1 Ba1 O1 100.20(11) 2_565 2_564 ? O1W Ba1 O1 66.61(15) . 1_554 ? O2W Ba1 O1 67.83(12) 1_554 1_554 ? O1 Ba1 O1 100.20(11) . 1_554 ? O1 Ba1 O1 143.76(16) 2_565 1_554 ? O1 Ba1 O1 67.77(14) 2_564 1_554 ? O1W Ba1 O2W 136.44(19) . . ? O2W Ba1 O2W 99.16(15) 1_554 . ? O1 Ba1 O2W 67.21(11) . . ? O1 Ba1 O2W 67.21(11) 2_565 . ? O1 Ba1 O2W 142.19(9) 2_564 . ? O1 Ba1 O2W 142.19(9) 1_554 . ? O1W Ba1 O2 121.50(8) . 4_565 ? O2W Ba1 O2 69.81(10) 1_554 4_565 ? O1 Ba1 O2 71.57(12) . 4_565 ? O1 Ba1 O2 130.09(12) 2_565 4_565 ? O1 Ba1 O2 129.60(12) 2_564 4_565 ? O1 Ba1 O2 71.89(11) 1_554 4_565 ? O2W Ba1 O2 70.31(9) . 4_565 ? O1W Ba1 O2 121.50(8) . 3_545 ? O2W Ba1 O2 69.81(10) 1_554 3_545 ? O1 Ba1 O2 130.09(12) . 3_545 ? O1 Ba1 O2 71.57(12) 2_565 3_545 ? O1 Ba1 O2 71.89(11) 2_564 3_545 ? O1 Ba1 O2 129.60(12) 1_554 3_545 ? O2W Ba1 O2 70.31(9) . 3_545 ? O2 Ba1 O2 116.52(16) 4_565 3_545 ? O1W Ba1 Ba1 83.29(16) . 1_554 ? O2W Ba1 Ba1 41.11(11) 1_554 1_554 ? O1 Ba1 Ba1 139.80(8) . 1_554 ? O1 Ba1 Ba1 139.80(8) 2_565 1_554 ? O1 Ba1 Ba1 39.60(7) 2_564 1_554 ? O1 Ba1 Ba1 39.60(7) 1_554 1_554 ? O2W Ba1 Ba1 140.27(10) . 1_554 ? O2 Ba1 Ba1 90.05(9) 4_565 1_554 ? O2 Ba1 Ba1 90.05(9) 3_545 1_554 ? O1W Ba1 Ba1 96.71(16) . 1_556 ? O2W Ba1 Ba1 138.89(11) 1_554 1_556 ? O1 Ba1 Ba1 40.20(8) . 1_556 ? O1 Ba1 Ba1 40.20(8) 2_565 1_556 ? O1 Ba1 Ba1 140.40(7) 2_564 1_556 ? O1 Ba1 Ba1 140.40(7) 1_554 1_556 ? O2W Ba1 Ba1 39.73(10) . 1_556 ? O2 Ba1 Ba1 89.95(9) 4_565 1_556 ? O2 Ba1 Ba1 89.95(9) 3_545 1_556 ? Ba1 Ba1 Ba1 180.0 1_554 1_556 ? C1 O1 Ba1 123.0(3) . . ? C1 O1 Ba1 131.9(3) . 1_556 ? Ba1 O1 Ba1 100.20(11) . 1_556 ? C3 O2 Ba1 142.6(3) . 3_455 ? Ba1 O1W H1W1 132(10) . . ? Ba1 O1W H1W2 118(10) . . ? H1W1 O1W H1W2 110(12) . . ? Ba1 O2W Ba1 99.16(15) 1_556 . ? Ba1 O2W H2W 118(4) 1_556 . ? Ba1 O2W H2W 106(5) . . ? H3W1 O3W H3W2 113.00 . . ? C4 N1 C1 121.1(5) . . ? C4 N1 H1N 118(5) . . ? C1 N1 H1N 121(5) . . ? C4 N2 C3 118.1(4) . . ? O1 C1 N1 117.4(4) . . ? O1 C1 C2 127.3(5) . . ? N1 C1 C2 115.4(4) . . ? C1 C2 C3 121.7(5) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? O2 C3 N2 116.7(4) . . ? O2 C3 C2 124.8(5) . . ? N2 C3 C2 118.5(5) . . ? N2 C4 N1 125.2(5) . . ? N2 C4 H3 117.4 . . ? N1 C4 H3 117.4 . . ? 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 O1W Ba1 O1 C1 -85.0(4) . . . . ? O2W Ba1 O1 C1 45.1(5) 1_554 . . . ? O1 Ba1 O1 C1 -166.1(3) 2_565 . . . ? O1 Ba1 O1 C1 -88.2(4) 2_564 . . . ? O1 Ba1 O1 C1 -22.1(4) 1_554 . . . ? O2W Ba1 O1 C1 120.6(4) . . . . ? O2 Ba1 O1 C1 44.8(4) 4_565 . . . ? O2 Ba1 O1 C1 154.4(3) 3_545 . . . ? Ba1 Ba1 O1 C1 -22.1(4) 1_554 . . . ? Ba1 Ba1 O1 C1 157.9(4) 1_556 . . . ? O1W Ba1 O1 Ba1 117.03(14) . . . 1_556 ? O2W Ba1 O1 Ba1 -112.89(19) 1_554 . . 1_556 ? O1 Ba1 O1 Ba1 35.97(14) 2_565 . . 1_556 ? O1 Ba1 O1 Ba1 113.88(17) 2_564 . . 1_556 ? O1 Ba1 O1 Ba1 180.0 1_554 . . 1_556 ? O2W Ba1 O1 Ba1 -37.33(10) . . . 1_556 ? O2 Ba1 O1 Ba1 -113.14(14) 4_565 . . 1_556 ? O2 Ba1 O1 Ba1 -3.58(19) 3_545 . . 1_556 ? Ba1 Ba1 O1 Ba1 180.000(1) 1_554 . . 1_556 ? O1W Ba1 O2W Ba1 0.0 . . . 1_556 ? O2W Ba1 O2W Ba1 180.0 1_554 . . 1_556 ? O1 Ba1 O2W Ba1 37.76(9) . . . 1_556 ? O1 Ba1 O2W Ba1 -37.76(9) 2_565 . . 1_556 ? O1 Ba1 O2W Ba1 -114.57(17) 2_564 . . 1_556 ? O1 Ba1 O2W Ba1 114.57(17) 1_554 . . 1_556 ? O2 Ba1 O2W Ba1 115.41(10) 4_565 . . 1_556 ? O2 Ba1 O2W Ba1 -115.41(10) 3_545 . . 1_556 ? Ba1 Ba1 O2W Ba1 180.0 1_554 . . 1_556 ? Ba1 O1 C1 N1 -112.3(4) . . . . ? Ba1 O1 C1 N1 37.9(6) 1_556 . . . ? Ba1 O1 C1 C2 68.2(6) . . . . ? Ba1 O1 C1 C2 -141.6(4) 1_556 . . . ? C4 N1 C1 O1 179.2(5) . . . . ? C4 N1 C1 C2 -1.3(7) . . . . ? O1 C1 C2 C3 -179.8(5) . . . . ? N1 C1 C2 C3 0.8(7) . . . . ? Ba1 O2 C3 N2 -25.9(8) 3_455 . . . ? Ba1 O2 C3 C2 153.6(4) 3_455 . . . ? C4 N2 C3 O2 177.9(5) . . . . ? C4 N2 C3 C2 -1.6(8) . . . . ? C1 C2 C3 O2 -178.8(5) . . . . ? C1 C2 C3 N2 0.7(8) . . . . ? C3 N2 C4 N1 1.1(10) . . . . ? C1 N1 C4 N2 0.4(10) . . . . ? 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 N1 H1N O2 0.86(6) 1.85(6) 2.703(6) 170(7) 4_566 O1W H1W1 O3W 0.85(6) 1.85(6) 2.702(6) 177(14) . O1W H1W2 O3W 0.85(6) 2.35(6) 3.149(6) 157(13) 1_554 O2W H2W N2 0.85(6) 2.06(2) 2.885(5) 164(7) 4_565 O3W H3W1 N2 0.85(6) 2.07(6) 2.854(6) 153(25) 4_465 O3W H3W2 N2 0.85(6) 2.00(2) 2.854(6) 177(27) 3_445 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.750 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.110