# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Fmd _database_code_depnum_ccdc_archive 'CCDC 850689' #TrackingRef 'Fmd_ccdc_deposit.cif' _audit_creation_date 2011-01-07T16:07:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C4 H8 Mg1 N2 O6' _chemical_formula_sum 'C4 H8 Mg N2 O6' _chemical_formula_weight 204.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.709(4) _cell_length_b 11.587(5) _cell_length_c 8.280(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 835.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2080 _cell_measurement_theta_min 4.6716 _cell_measurement_theta_max 28.8909 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a' _symmetry_space_group_name_Hall '-P 2a 2bc' _symmetry_Int_Tables_number 52 _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.92191 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 -0.0036131 _diffrn_orient_matrix_ub_12 -0.0511748 _diffrn_orient_matrix_ub_13 0.0469087 _diffrn_orient_matrix_ub_21 0.0285488 _diffrn_orient_matrix_ub_22 0.0306322 _diffrn_orient_matrix_ub_23 0.0678504 _diffrn_orient_matrix_ub_31 -0.0761423 _diffrn_orient_matrix_ub_32 0.0139159 _diffrn_orient_matrix_ub_33 0.023155 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_number 3247 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.68 _diffrn_reflns_theta_max 28.95 _diffrn_reflns_theta_full 28.95 _diffrn_measured_fraction_theta_full 0.888 _diffrn_measured_fraction_theta_max 0.888 _reflns_number_total 991 _reflns_number_gt 891 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0446P)^2^+0.1639P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 991 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.19 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.062 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C 0.25 0.5 0.18840(19) 0.0140(3) Uani 1 2 d S . . H1 H 0.25 0.5 0.3031 0.017 Uiso 1 2 calc SR . . C2 C -0.02971(13) 0.21972(9) 0.02571(13) 0.0151(2) Uani 1 1 d . . . H2 H -0.082 0.2804 0.08 0.018 Uiso 1 1 calc R . . C3 C 0.75 0 0.2059(2) 0.0193(4) Uani 1 2 d S . . H3 H 0.75 0 0.088(3) 0.023 Uiso 1 2 d S . . N1 N 0.65035(13) 0.06509(9) 0.27941(13) 0.0214(3) Uani 1 1 d . . . H4 H 0.6577(18) 0.0712(13) 0.385(2) 0.026 Uiso 1 1 d . . . H5 H 0.5843(19) 0.1018(14) 0.2257(17) 0.026 Uiso 1 1 d . . . O1 O 0.24059(8) 0.40404(7) 0.11873(9) 0.0138(2) Uani 1 1 d . . . O2 O 0.08746(9) 0.17983(7) 0.09078(9) 0.0174(2) Uani 1 1 d . . . O3 O 0.41591(9) 0.18578(7) 0.10638(9) 0.0156(2) Uani 1 1 d . . . Mg1 Mg 0.24103(5) 0.25 0.25 0.01005(17) Uani 1 2 d S . . 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 C1 0.0174(8) 0.0142(8) 0.0105(7) 0 0 0.0002(5) C2 0.0159(5) 0.0151(5) 0.0142(5) -0.0006(4) -0.0015(4) 0.0012(4) C3 0.0252(9) 0.0206(9) 0.0122(7) 0 0 -0.0017(6) N1 0.0234(6) 0.0249(6) 0.0160(5) 0.0017(4) -0.0039(4) 0.0074(4) O1 0.0183(4) 0.0111(4) 0.0120(4) 0.0000(3) -0.0003(3) 0.0003(3) O2 0.0176(4) 0.0158(4) 0.0187(4) -0.0006(3) -0.0077(3) 0.0006(3) O3 0.0154(4) 0.0180(4) 0.0135(4) 0.0028(3) 0.0042(3) 0.0030(3) Mg1 0.0100(3) 0.0107(3) 0.0094(3) -0.00015(18) 0 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 O1 1.2553(12) . ? C1 O1 1.2553(12) 2_565 ? C1 H1 0.95 . ? C2 O2 1.2431(14) . ? C2 O3 1.2550(14) 6 ? C2 H2 0.95 . ? C3 N1 1.3009(14) . ? C3 N1 1.3009(14) 2_655 ? C3 H3 0.97(2) . ? N1 H4 0.878(16) . ? N1 H5 0.842(16) . ? O1 Mg1 2.0897(11) . ? O2 Mg1 2.0464(11) . ? O3 C2 1.2550(14) 6_655 ? O3 Mg1 2.0706(11) . ? Mg1 O2 2.0464(11) 3 ? Mg1 O3 2.0706(11) 3 ? Mg1 O1 2.0897(11) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O1 125.29(15) . 2_565 ? O1 C1 H1 117.4 . . ? O1 C1 H1 117.4 2_565 . ? O2 C2 O3 124.82(11) . 6 ? O2 C2 H2 117.6 . . ? O3 C2 H2 117.6 6 . ? N1 C3 N1 124.22(17) . 2_655 ? N1 C3 H3 117.89(9) . . ? N1 C3 H3 117.89(9) 2_655 . ? C3 N1 H4 117.6(10) . . ? C3 N1 H5 120.1(10) . . ? H4 N1 H5 122.2(14) . . ? C1 O1 Mg1 121.16(9) . . ? C2 O2 Mg1 131.91(8) . . ? C2 O3 Mg1 131.72(7) 6_655 . ? O2 Mg1 O2 98.38(7) . 3 ? O2 Mg1 O3 173.45(3) . 3 ? O2 Mg1 O3 88.16(5) 3 3 ? O2 Mg1 O3 88.16(5) . . ? O2 Mg1 O3 173.45(4) 3 . ? O3 Mg1 O3 85.29(6) 3 . ? O2 Mg1 O1 89.69(4) . 3 ? O2 Mg1 O1 90.18(4) 3 3 ? O3 Mg1 O1 90.55(4) 3 3 ? O3 Mg1 O1 89.61(4) . 3 ? O2 Mg1 O1 90.18(4) . . ? O2 Mg1 O1 89.69(4) 3 . ? O3 Mg1 O1 89.61(4) 3 . ? O3 Mg1 O1 90.55(4) . . ? O1 Mg1 O1 179.79(5) 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 N1 H4 O1 0.878(16) 2.086(17) 2.939(2) 163.5(14) 8_666 N1 H5 O3 0.842(16) 2.019(17) 2.8596(17) 176.4(15) . data_Gua _database_code_depnum_ccdc_archive 'CCDC 850690' #TrackingRef 'Gua_ccdc_deposit.cif' _audit_creation_date 2011-10-21T16:49:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C4 H9 Mg1 N3 O6' _chemical_formula_sum 'C4 H9 Mg N3 O6' _chemical_formula_weight 219.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.391(2) _cell_length_b 11.831(2) _cell_length_c 8.842(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 877.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2681 _cell_measurement_theta_min 4.1355 _cell_measurement_theta_max 26.9465 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _symmetry_space_group_name_H-M 'P n n a' _symmetry_space_group_name_Hall '-P 2a 2bc' _symmetry_Int_Tables_number 52 _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.7969 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 -0.0216768 _diffrn_orient_matrix_ub_12 0.0336373 _diffrn_orient_matrix_ub_13 0.0630886 _diffrn_orient_matrix_ub_21 0.0485381 _diffrn_orient_matrix_ub_22 0.0447283 _diffrn_orient_matrix_ub_23 -0.027485 _diffrn_orient_matrix_ub_31 -0.0656109 _diffrn_orient_matrix_ub_32 0.021587 _diffrn_orient_matrix_ub_33 -0.0412791 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.2563 _diffrn_reflns_av_unetI/netI 0.0915 _diffrn_reflns_number 9952 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 27 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.901 _diffrn_measured_fraction_theta_max 0.901 _reflns_number_total 873 _reflns_number_gt 558 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 873 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.3236 _refine_ls_wR_factor_gt 0.2709 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.169 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.181 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C 0.75 0 0.8000(6) 0.0420(19) Uani 1 2 d S . . H1 H 0.75 0 0.6948 0.05 Uiso 1 2 calc SR . . C2 C 0.5181(5) 0.2770(4) 1.0190(4) 0.0374(13) Uani 1 1 d . . . H2 H 0.5808 0.2237 1.0683 0.045 Uiso 1 1 calc R . . C3 C 0.75 0.5 0.2436(6) 0.0345(18) Uani 1 2 d S . . N1 N 0.8372(5) 0.4255(3) 0.3166(4) 0.0559(15) Uani 1 1 d . . . H4 H 0.823(6) 0.426(4) 0.411(6) 0.067 Uiso 1 1 d . . . H5 H 0.916(6) 0.376(4) 0.263(6) 0.067 Uiso 1 1 d . . . N2 N 0.75 0.5 0.0941(5) 0.0474(18) Uani 1 2 d S . . H3 H 0.801(7) 0.458(5) 0.053(7) 0.057 Uiso 1 1 d . . . O1 O 0.7516(3) 0.0943(3) 0.8602(3) 0.0351(11) Uani 1 1 d . . . O2 O 0.5608(4) 0.3048(2) 0.8894(3) 0.0366(10) Uani 1 1 d . . . O3 O 0.9024(4) 0.3124(2) 0.9117(3) 0.0405(11) Uani 1 1 d . . . Mg1 Mg 0.74743(18) 0.25 0.75 0.0282(9) Uani 1 2 d S . . 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 C1 0.088(6) 0.024(3) 0.014(3) 0 0 -0.002(2) C2 0.052(3) 0.038(3) 0.023(2) 0.0045(16) 0.0054(17) 0.0037(17) C3 0.055(5) 0.028(4) 0.020(3) 0 0 0.000(2) N1 0.083(4) 0.059(3) 0.025(2) 0.0051(16) 0.0049(18) 0.021(2) N2 0.084(5) 0.041(4) 0.017(3) 0 0 0.016(3) O1 0.060(3) 0.029(2) 0.0165(16) 0.0012(11) 0.0004(10) 0.0030(10) O2 0.049(2) 0.0427(19) 0.0177(15) -0.0009(11) 0.0067(10) 0.0042(12) O3 0.055(2) 0.0406(19) 0.0255(16) -0.0015(11) -0.0159(13) -0.0004(14) Mg1 0.0470(18) 0.0260(15) 0.0117(12) 0.0004(6) 0 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 O1 1.236(4) 2_655 ? C1 O1 1.236(4) . ? C1 H1 0.93 . ? C2 O3 1.222(5) 6_557 ? C2 O2 1.245(4) . ? C2 H2 0.93 . ? C3 N1 1.315(4) . ? C3 N1 1.315(4) 2_665 ? C3 N2 1.322(7) . ? N1 H4 0.84(6) . ? N1 H5 1.00(5) . ? N2 H3 0.75(5) . ? O1 Mg1 2.084(3) . ? O2 Mg1 2.095(3) . ? O3 C2 1.222(5) 6_657 ? O3 Mg1 2.069(3) . ? Mg1 O3 2.069(3) 3_556 ? Mg1 O1 2.084(3) 3_556 ? Mg1 O2 2.095(3) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O1 129.0(5) 2_655 . ? O1 C1 H1 115.5 2_655 . ? O1 C1 H1 115.5 . . ? O3 C2 O2 126.9(4) 6_557 . ? O3 C2 H2 116.6 6_557 . ? O2 C2 H2 116.6 . . ? N1 C3 N1 121.2(5) . 2_665 ? N1 C3 N2 119.4(2) . . ? N1 C3 N2 119.4(2) 2_665 . ? C3 N1 H4 114(4) . . ? C3 N1 H5 122(3) . . ? H4 N1 H5 124(5) . . ? C3 N2 H3 119(5) . . ? C1 O1 Mg1 126.6(3) . . ? C2 O2 Mg1 132.5(3) . . ? C2 O3 Mg1 136.3(3) 6_657 . ? O3 Mg1 O3 102.12(19) . 3_556 ? O3 Mg1 O1 89.83(11) . 3_556 ? O3 Mg1 O1 88.96(11) 3_556 3_556 ? O3 Mg1 O1 88.96(11) . . ? O3 Mg1 O1 89.83(10) 3_556 . ? O1 Mg1 O1 178.08(15) 3_556 . ? O3 Mg1 O2 170.58(13) . 3_556 ? O3 Mg1 O2 87.30(12) 3_556 3_556 ? O1 Mg1 O2 90.63(10) 3_556 3_556 ? O1 Mg1 O2 90.80(11) . 3_556 ? O3 Mg1 O2 87.30(12) . . ? O3 Mg1 O2 170.58(13) 3_556 . ? O1 Mg1 O2 90.80(11) 3_556 . ? O1 Mg1 O2 90.63(10) . . ? O2 Mg1 O2 83.29(17) 3_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 N1 H4 O1 0.84(6) 2.12(6) 2.956(5) 170(5) 3_556 N1 H5 O2 1.00(5) 2.00(6) 2.980(5) 165(4) 6_656 N2 H3 O3 0.75(5) 2.29(6) 3.027(4) 167(6) 1_554 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF