# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address N.Stavgianoudaki ;Crystal Engineering, Growth and Design Laboratory Department of Chemistry University of Crete, Voutes Campus Crete, GR-71003 Greece ; K.E.Papathanasiou ;Crystal Engineering, Growth and Design Laboratory Department of Chemistry University of Crete, Voutes Campus Crete, GR-71003 Greece ; R.M.P.Colodrero ;Departamento de Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 Malaga Spain ; A.Cabeza ;Departamento de Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 Malaga Spain ; ; D.Choquesillo-Lazarte ; ;Laboratorio de Estudios Cristalogr\'aficos, IACT-CSIC, Granada Spain ; M.A.G.Aranda ;Departamento de Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 M\'alaga Spain ; K.D.Demadis ;Crystal Engineering, Growth and Design Laboratory Department of Chemistry University of Crete, Voutes Campus Crete, GR-71003 Greece ; _publ_contact_author_address ;Crystal Engineering, Growth and Design Laboratory Department of Chemistry University of Crete, Voutes Campus Crete, GR-71003 Greece ; _publ_contact_author_email aurelio@uma.es _publ_contact_author_name 'K.D. Demadis' #===END data_ca2000 _database_code_depnum_ccdc_archive 'CCDC 870775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H12 Ca N O10 P3, 3.5(H2O)' _chemical_formula_sum 'C3 H19 Ca N O13.5 P3' _chemical_formula_weight 417.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.236(5) _cell_length_b 8.459(3) _cell_length_c 15.532(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.586(1) _cell_angle_gamma 90.00 _cell_volume 1476.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4357 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 31.7 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.798 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18987 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 31.85 _reflns_number_total 5162 _reflns_number_gt 4090 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+2.1550P] 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 5162 _refine_ls_number_parameters 229 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.100 _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 0.96208(4) 0.34388(6) 0.16256(3) 0.01223(12) Uani 1 1 d . . . P1 P 1.19706(6) 0.01364(8) -0.24284(4) 0.01286(15) Uani 1 1 d . . . P2 P 0.92064(6) 0.27897(8) -0.06635(4) 0.01220(15) Uani 1 1 d . . . P3 P 1.23711(6) 0.20091(9) 0.07381(4) 0.01437(15) Uani 1 1 d . . . O1 O 1.30410(17) -0.0050(2) -0.29923(12) 0.0159(4) Uani 1 1 d . . . O2 O 1.13271(18) -0.1352(2) -0.22098(13) 0.0189(4) Uani 1 1 d . . . O3 O 1.10756(18) 0.1379(3) -0.28143(13) 0.0199(4) Uani 1 1 d . . . O4 O 0.81590(17) 0.2055(3) -0.12128(12) 0.0171(4) Uani 1 1 d . . . O5 O 0.88663(17) 0.2781(3) 0.02706(12) 0.0170(4) Uani 1 1 d . . . O6 O 0.95396(18) 0.4329(3) -0.10607(13) 0.0189(4) Uani 1 1 d . . . O7 O 1.12656(17) 0.1970(2) 0.12633(12) 0.0167(4) Uani 1 1 d . . . O8 O 1.28866(19) 0.0410(3) 0.05490(14) 0.0203(4) Uani 1 1 d . . . O9 O 1.33471(19) 0.3083(3) 0.11689(14) 0.0243(5) Uani 1 1 d . . . N1 N 1.15887(19) 0.2207(3) -0.10365(14) 0.0136(4) Uani 1 1 d . . . H1 H 1.1421 0.2944 -0.1447 0.016 Uiso 1 1 calc R . . C1 C 1.2474(2) 0.1087(3) -0.14270(16) 0.0156(5) Uani 1 1 d . . . H1A H 1.2661 0.0270 -0.1009 0.019 Uiso 1 1 calc R . . H1B H 1.3202 0.1663 -0.1541 0.019 Uiso 1 1 calc R . . C2 C 1.0440(2) 0.1415(3) -0.08351(17) 0.0145(5) Uani 1 1 d . . . H2A H 1.0548 0.0776 -0.0322 0.017 Uiso 1 1 calc R . . H2B H 1.0231 0.0710 -0.1305 0.017 Uiso 1 1 calc R . . C3 C 1.2116(2) 0.3095(3) -0.02786(16) 0.0160(5) Uani 1 1 d . . . H3A H 1.1596 0.3980 -0.0156 0.019 Uiso 1 1 calc R . . H3B H 1.2873 0.3531 -0.0457 0.019 Uiso 1 1 calc R . . O10 O 1.1424(2) 0.2283(4) -0.43748(16) 0.0380(7) Uani 1 1 d D . . H10A H 1.124(4) 0.180(5) -0.392(2) 0.046 Uiso 1 1 d D . . H10B H 1.214(2) 0.242(6) -0.450(3) 0.046 Uiso 1 1 d D . . O11 O 1.2738(3) 0.5367(3) 0.22616(17) 0.0360(6) Uani 1 1 d D . . H11A H 1.340(3) 0.548(6) 0.199(3) 0.043 Uiso 1 1 d D . . H11B H 1.261(4) 0.629(3) 0.201(3) 0.043 Uiso 1 1 d D . . O12 O 1.0522(2) 0.3861(4) 0.29886(17) 0.0368(6) Uani 1 1 d D . . H12A H 1.036(4) 0.437(5) 0.343(2) 0.044 Uiso 1 1 d D . . H12B H 1.118(3) 0.432(5) 0.294(3) 0.044 Uiso 1 1 d D . . O13 O 1.4897(3) 0.6258(4) 0.0807(2) 0.0445(7) Uani 1 1 d D . . H13A H 1.514(5) 0.625(6) 0.0291(16) 0.053 Uiso 1 1 d D . . H13B H 1.499(4) 0.550(5) 0.118(3) 0.053 Uiso 1 1 d D . . O14 O 1.0185(4) 0.4833(7) -0.4555(3) 0.0276(10) Uani 0.50 1 d PD . . H14A H 0.947(3) 0.501(10) -0.471(5) 0.033 Uiso 0.50 1 d PD . . H14B H 1.065(6) 0.532(9) -0.489(5) 0.033 Uiso 0.50 1 d PD . . 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 0.0126(2) 0.0117(3) 0.0125(2) 0.00075(17) 0.00457(17) 0.00003(17) P1 0.0140(3) 0.0122(3) 0.0125(3) -0.0006(2) 0.0049(2) -0.0013(2) P2 0.0124(3) 0.0118(3) 0.0124(3) 0.0002(2) 0.0031(2) -0.0007(2) P3 0.0122(3) 0.0163(4) 0.0147(3) 0.0004(2) 0.0031(2) 0.0013(2) O1 0.0160(8) 0.0159(10) 0.0158(8) -0.0021(7) 0.0073(7) -0.0014(7) O2 0.0226(9) 0.0138(10) 0.0206(9) 0.0001(8) 0.0085(8) -0.0038(8) O3 0.0190(9) 0.0215(11) 0.0192(9) 0.0025(8) 0.0040(7) 0.0023(8) O4 0.0166(9) 0.0189(10) 0.0159(8) 0.0015(7) -0.0023(7) -0.0028(8) O5 0.0159(8) 0.0223(11) 0.0127(8) -0.0006(7) 0.0027(7) 0.0002(8) O6 0.0186(9) 0.0156(10) 0.0227(9) 0.0033(8) 0.0046(7) -0.0015(8) O7 0.0141(8) 0.0191(10) 0.0170(8) 0.0013(7) 0.0043(7) 0.0034(7) O8 0.0216(10) 0.0162(10) 0.0234(10) 0.0019(8) 0.0089(8) 0.0043(8) O9 0.0177(9) 0.0324(13) 0.0228(10) -0.0011(9) -0.0010(8) -0.0061(9) N1 0.0134(9) 0.0132(11) 0.0144(9) -0.0007(8) 0.0034(7) 0.0011(8) C1 0.0134(10) 0.0179(13) 0.0155(11) -0.0025(9) 0.0049(9) 0.0029(9) C2 0.0136(10) 0.0113(12) 0.0187(11) -0.0011(9) 0.0049(9) -0.0013(9) C3 0.0193(11) 0.0163(13) 0.0126(10) -0.0011(9) 0.0022(9) -0.0022(10) O10 0.0216(11) 0.068(2) 0.0242(11) 0.0189(12) 0.0071(9) 0.0086(12) O11 0.0483(16) 0.0291(14) 0.0304(13) -0.0006(11) -0.0122(11) 0.0032(13) O12 0.0302(13) 0.0555(19) 0.0246(11) -0.0135(12) -0.0054(10) -0.0011(13) O13 0.0466(17) 0.0418(18) 0.0453(17) 0.0056(14) 0.0128(14) -0.0007(14) O14 0.0154(18) 0.042(3) 0.026(2) 0.002(2) 0.0037(16) -0.0016(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O2 2.257(2) 3_755 ? Ca1 O6 2.289(2) 3_765 ? Ca1 O7 2.302(2) . ? Ca1 O1 2.3199(19) 4_566 ? Ca1 O5 2.328(2) . ? Ca1 O12 2.365(3) . ? Ca1 H12B 2.79(4) . ? P1 O2 1.493(2) . ? P1 O1 1.5033(19) . ? P1 O3 1.569(2) . ? P1 C1 1.835(3) . ? P1 Ca1 3.5451(8) 4_665 ? P2 O6 1.490(2) . ? P2 O5 1.5042(19) . ? P2 O4 1.574(2) . ? P2 C2 1.831(3) . ? P3 O7 1.4934(19) . ? P3 O8 1.502(2) . ? P3 O9 1.568(2) . ? P3 C3 1.846(3) . ? O1 Ca1 2.3199(19) 4_665 ? O2 Ca1 2.257(2) 3_755 ? O6 Ca1 2.289(2) 3_765 ? N1 C2 1.490(3) . ? N1 C1 1.506(3) . ? N1 C3 1.512(4) . ? N1 H1 0.9100 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? O10 H10A 0.845(19) . ? O10 H10B 0.841(19) . ? O11 H11A 0.859(19) . ? O11 H11B 0.881(19) . ? O12 H12A 0.834(19) . ? O12 H12B 0.844(19) . ? O13 H13A 0.851(19) . ? O13 H13B 0.870(19) . ? O14 O14 1.468(10) 3_764 ? O14 H14A 0.85(2) . ? O14 H14B 0.85(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ca1 O6 175.65(8) 3_755 3_765 ? O2 Ca1 O7 93.40(7) 3_755 . ? O6 Ca1 O7 90.95(7) 3_765 . ? O2 Ca1 O1 89.49(7) 3_755 4_566 ? O6 Ca1 O1 86.16(7) 3_765 4_566 ? O7 Ca1 O1 176.47(8) . 4_566 ? O2 Ca1 O5 90.42(8) 3_755 . ? O6 Ca1 O5 89.91(8) 3_765 . ? O7 Ca1 O5 86.31(7) . . ? O1 Ca1 O5 95.70(7) 4_566 . ? O2 Ca1 O12 87.57(10) 3_755 . ? O6 Ca1 O12 92.54(10) 3_765 . ? O7 Ca1 O12 87.86(9) . . ? O1 Ca1 O12 90.24(9) 4_566 . ? O5 Ca1 O12 173.72(9) . . ? O2 Ca1 H12B 102.2(8) 3_755 . ? O6 Ca1 H12B 78.5(8) 3_765 . ? O7 Ca1 H12B 79.8(10) . . ? O1 Ca1 H12B 97.6(10) 4_566 . ? O5 Ca1 H12B 161.7(7) . . ? O12 Ca1 H12B 16.4(7) . . ? O2 P1 O1 115.87(12) . . ? O2 P1 O3 109.99(12) . . ? O1 P1 O3 111.17(11) . . ? O2 P1 C1 108.81(12) . . ? O1 P1 C1 107.37(11) . . ? O3 P1 C1 102.76(12) . . ? O2 P1 Ca1 142.36(8) . 4_665 ? O1 P1 Ca1 27.60(8) . 4_665 ? O3 P1 Ca1 98.72(8) . 4_665 ? C1 P1 Ca1 87.12(8) . 4_665 ? O6 P2 O5 118.11(12) . . ? O6 P2 O4 108.07(12) . . ? O5 P2 O4 108.95(11) . . ? O6 P2 C2 107.52(12) . . ? O5 P2 C2 109.72(12) . . ? O4 P2 C2 103.48(12) . . ? O7 P3 O8 114.28(12) . . ? O7 P3 O9 111.21(12) . . ? O8 P3 O9 109.61(13) . . ? O7 P3 C3 110.84(12) . . ? O8 P3 C3 109.72(12) . . ? O9 P3 C3 100.29(13) . . ? P1 O1 Ca1 134.93(12) . 4_665 ? P1 O2 Ca1 169.37(13) . 3_755 ? P2 O5 Ca1 140.98(12) . . ? P2 O6 Ca1 170.21(13) . 3_765 ? P3 O7 Ca1 142.74(13) . . ? C2 N1 C1 112.2(2) . . ? C2 N1 C3 113.2(2) . . ? C1 N1 C3 111.8(2) . . ? C2 N1 H1 106.4 . . ? C1 N1 H1 106.4 . . ? C3 N1 H1 106.4 . . ? N1 C1 P1 114.74(18) . . ? N1 C1 H1A 108.6 . . ? P1 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? N1 C2 P2 113.79(19) . . ? N1 C2 H2A 108.8 . . ? P2 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? P2 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N1 C3 P3 118.36(19) . . ? N1 C3 H3A 107.7 . . ? P3 C3 H3A 107.7 . . ? N1 C3 H3B 107.7 . . ? P3 C3 H3B 107.7 . . ? H3A C3 H3B 107.1 . . ? H10A O10 H10B 121(5) . . ? H11A O11 H11B 80(4) . . ? Ca1 O12 H12A 136(3) . . ? Ca1 O12 H12B 111(3) . . ? H12A O12 H12B 92(4) . . ? H13A O13 H13B 126(5) . . ? O14 O14 H14A 56(6) 3_764 . ? O14 O14 H14B 60(6) 3_764 . ? H14A O14 H14B 109(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10A O3 0.845(19) 1.76(3) 2.575(3) 160(5) . O11 H11A O13 0.859(19) 2.59(3) 3.416(4) 160(4) . O12 H12B O11 0.844(19) 2.23(3) 3.026(4) 157(5) . N1 H1 O1 0.91 2.00 2.801(3) 145.5 2_754 O13 H13A O10 0.851(19) 2.42(5) 2.800(5) 108(4) 2_754 O14 H14B O8 0.85(2) 1.94(5) 2.718(5) 150(8) 2_754 O10 H10B O5 0.841(19) 1.98(2) 2.805(3) 167(5) 4_665 O11 H11B O4 0.881(19) 2.06(3) 2.897(3) 159(4) 3_765 O12 H12A O14 0.834(19) 1.97(2) 2.794(5) 168(5) 3_765 O13 H13B O3 0.870(19) 2.53(3) 3.355(4) 158(5) 4_666 O14 H14A O8 0.85(2) 1.86(5) 2.597(5) 143(8) 4_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.85 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.909 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.149 #===END data_cahedp _database_code_depnum_ccdc_archive 'CCDC 870776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Ca O7 P2, 2(H2 O)' _chemical_formula_sum 'C2 H10 Ca O9 P2' _chemical_formula_weight 280.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.943(5) _cell_length_b 7.581(6) _cell_length_c 9.662(6) _cell_angle_alpha 92.734(5) _cell_angle_beta 106.176(10) _cell_angle_gamma 112.524(14) _cell_volume 444.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 1867 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 26.3 _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Rigaku Saturn724 (2x2 bin mode) ; _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3382 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1550 _reflns_number_gt 1415 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms of the water ligands could not be detected in Fourier maps. ; _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' _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 1550 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.2858 _refine_ls_wR_factor_gt 0.2432 _refine_ls_goodness_of_fit_ref 1.287 _refine_ls_restrained_S_all 1.287 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.003 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 0.09207(16) -0.20575(14) 0.51489(12) 0.0098(6) Uani 1 1 d . . . P1 P 0.4830(2) 0.2575(2) 0.62450(16) 0.0091(6) Uani 1 1 d . . . P2 P 0.8594(2) 0.2024(2) 0.84394(16) 0.0122(6) Uani 1 1 d . . . C1 C 0.5678(9) 0.1531(8) 0.7869(6) 0.0127(13) Uani 1 1 d . . . C2 C 0.4959(9) 0.2138(8) 0.9069(6) 0.0139(13) Uani 1 1 d . . . H2A H 0.5739 0.3515 0.9392 0.021 Uiso 1 1 calc R . . H2B H 0.5274 0.1486 0.9874 0.021 Uiso 1 1 calc R . . H2C H 0.3405 0.1801 0.8708 0.021 Uiso 1 1 calc R . . O1 O 0.6076(6) 0.2497(5) 0.5225(4) 0.0122(10) Uani 1 1 d . . . O2 O 0.5322(6) 0.4753(6) 0.6834(5) 0.0147(10) Uani 1 1 d . . . H2 H 0.6264 0.5500 0.6532 0.022 Uiso 1 1 calc R . . O3 O 0.2350(6) 0.1468(5) 0.5648(4) 0.0095(9) Uani 1 1 d . . . O4 O 0.9842(6) 0.4246(6) 0.8771(4) 0.0152(10) Uani 1 1 d . . . H4 H 1.0060 0.4640 0.8029 0.023 Uiso 1 1 calc R . . O5 O 0.9126(6) 0.1191(5) 0.9838(4) 0.0131(10) Uani 1 1 d . . . O6 O 0.9036(6) 0.1119(5) 0.7197(5) 0.0150(10) Uani 1 1 d . . . O7 O 0.4459(6) -0.0567(5) 0.7379(5) 0.0140(10) Uani 1 1 d . . . H7 H 0.5067 -0.1174 0.7924 0.021 Uiso 1 1 d R . . O8 O -0.1432(6) -0.5223(6) 0.3514(4) 0.0125(9) Uani 1 1 d . . . O9 O -0.0755(6) -0.2308(5) 0.7143(5) 0.0130(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0097(8) 0.0060(8) 0.0125(8) 0.0015(5) 0.0020(6) 0.0030(6) P1 0.0094(9) 0.0065(9) 0.0108(10) 0.0019(6) 0.0017(7) 0.0038(6) P2 0.0100(9) 0.0123(10) 0.0145(10) 0.0026(7) 0.0027(7) 0.0055(7) C1 0.016(3) 0.012(3) 0.010(3) 0.002(2) 0.001(2) 0.007(2) C2 0.013(3) 0.015(3) 0.013(3) 0.000(2) -0.001(2) 0.009(2) O1 0.0102(19) 0.010(2) 0.015(2) 0.0006(16) 0.0020(16) 0.0036(15) O2 0.017(2) 0.010(2) 0.020(2) 0.0038(17) 0.0072(17) 0.0070(16) O3 0.0117(19) 0.009(2) 0.008(2) 0.0014(15) 0.0025(15) 0.0052(15) O4 0.016(2) 0.015(2) 0.013(2) 0.0033(17) 0.0057(17) 0.0027(17) O5 0.0097(18) 0.015(2) 0.015(2) 0.0068(18) 0.0007(15) 0.0071(16) O6 0.015(2) 0.010(2) 0.018(2) 0.0014(17) -0.0004(17) 0.0077(16) O7 0.0082(19) 0.010(2) 0.024(2) 0.0070(17) 0.0060(16) 0.0029(15) O8 0.0121(19) 0.012(2) 0.013(2) 0.0046(16) 0.0057(15) 0.0028(15) O9 0.0092(19) 0.011(2) 0.022(2) 0.0047(17) 0.0077(16) 0.0043(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 Ca1 O1 2.352(4) 2_656 ? Ca1 O3 2.405(4) 2_556 ? Ca1 O6 2.412(5) 2_656 ? Ca1 O3 2.437(4) . ? Ca1 O8 2.474(4) . ? Ca1 O9 2.493(4) . ? Ca1 O8 2.570(4) 2_546 ? Ca1 O7 2.578(4) . ? Ca1 P1 3.400(3) . ? P1 O1 1.494(4) . ? P1 O3 1.515(4) . ? P1 O2 1.593(4) . ? P1 C1 1.843(6) . ? P2 O6 1.515(4) . ? P2 O5 1.531(4) . ? P2 O4 1.538(4) . ? P2 C1 1.822(6) . ? C1 O7 1.463(7) . ? C1 C2 1.501(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? O1 Ca1 2.352(4) 2_656 ? O2 H2 0.8200 . ? O3 Ca1 2.405(4) 2_556 ? O4 H4 0.8200 . ? O6 Ca1 2.412(5) 2_656 ? O7 H7 0.8455 . ? O8 Ca1 2.570(4) 2_546 ? 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 Ca1 O3 152.97(14) 2_656 2_556 ? O1 Ca1 O6 75.97(14) 2_656 2_656 ? O3 Ca1 O6 77.50(13) 2_556 2_656 ? O1 Ca1 O3 101.37(14) 2_656 . ? O3 Ca1 O3 76.89(14) 2_556 . ? O6 Ca1 O3 75.91(13) 2_656 . ? O1 Ca1 O8 86.46(13) 2_656 . ? O3 Ca1 O8 83.81(13) 2_556 . ? O6 Ca1 O8 79.65(14) 2_656 . ? O3 Ca1 O8 151.53(14) . . ? O1 Ca1 O9 136.66(14) 2_656 . ? O3 Ca1 O9 70.23(13) 2_556 . ? O6 Ca1 O9 147.17(13) 2_656 . ? O3 Ca1 O9 90.82(13) . . ? O8 Ca1 O9 102.21(13) . . ? O1 Ca1 O8 71.45(13) 2_656 2_546 ? O3 Ca1 O8 127.77(13) 2_556 2_546 ? O6 Ca1 O8 136.68(14) 2_656 2_546 ? O3 Ca1 O8 137.76(14) . 2_546 ? O8 Ca1 O8 70.70(16) . 2_546 ? O9 Ca1 O8 71.78(13) . 2_546 ? O1 Ca1 O7 66.40(14) 2_656 . ? O3 Ca1 O7 133.70(14) 2_556 . ? O6 Ca1 O7 119.97(14) 2_656 . ? O3 Ca1 O7 68.26(13) . . ? O8 Ca1 O7 138.40(13) . . ? O9 Ca1 O7 80.54(14) . . ? O8 Ca1 O7 71.00(13) 2_546 . ? O1 Ca1 P1 80.03(11) 2_656 . ? O3 Ca1 P1 100.30(11) 2_556 . ? O6 Ca1 P1 79.83(10) 2_656 . ? O3 Ca1 P1 23.43(9) . . ? O8 Ca1 P1 157.64(10) . . ? O9 Ca1 P1 99.84(10) . . ? O8 Ca1 P1 120.51(11) 2_546 . ? O7 Ca1 P1 49.73(9) . . ? O1 Ca1 Ca1 133.76(11) 2_656 2_556 ? O3 Ca1 Ca1 38.74(9) 2_556 2_556 ? O6 Ca1 Ca1 72.92(10) 2_656 2_556 ? O3 Ca1 Ca1 38.15(9) . 2_556 ? O8 Ca1 Ca1 119.77(11) . 2_556 ? O9 Ca1 Ca1 78.15(10) . 2_556 ? O8 Ca1 Ca1 149.79(11) 2_546 2_556 ? O7 Ca1 Ca1 101.55(10) . 2_556 ? P1 Ca1 Ca1 61.56(7) . 2_556 ? O1 Ca1 Ca1 76.35(10) 2_656 2_546 ? O3 Ca1 Ca1 108.53(10) 2_556 2_546 ? O6 Ca1 Ca1 110.26(10) 2_656 2_546 ? O3 Ca1 Ca1 172.33(11) . 2_546 ? O8 Ca1 Ca1 36.12(10) . 2_546 ? O9 Ca1 Ca1 86.09(9) . 2_546 ? O8 Ca1 Ca1 34.58(9) 2_546 2_546 ? O7 Ca1 Ca1 104.26(10) . 2_546 ? P1 Ca1 Ca1 150.84(6) . 2_546 ? Ca1 Ca1 Ca1 146.97(6) 2_556 2_546 ? O1 P1 O3 116.4(2) . . ? O1 P1 O2 111.4(2) . . ? O3 P1 O2 107.0(2) . . ? O1 P1 C1 110.5(3) . . ? O3 P1 C1 104.5(2) . . ? O2 P1 C1 106.4(3) . . ? O1 P1 Ca1 97.38(15) . . ? O3 P1 Ca1 39.77(15) . . ? O2 P1 Ca1 145.09(16) . . ? C1 P1 Ca1 80.14(18) . . ? O6 P2 O5 112.5(2) . . ? O6 P2 O4 112.1(2) . . ? O5 P2 O4 109.8(2) . . ? O6 P2 C1 108.2(3) . . ? O5 P2 C1 108.1(2) . . ? O4 P2 C1 105.9(2) . . ? O7 C1 C2 108.8(4) . . ? O7 C1 P2 106.7(3) . . ? C2 C1 P2 113.6(4) . . ? O7 C1 P1 104.4(3) . . ? C2 C1 P1 109.9(4) . . ? P2 C1 P1 112.9(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 O1 Ca1 148.0(2) . 2_656 ? P1 O2 H2 109.5 . . ? P1 O3 Ca1 140.0(2) . 2_556 ? P1 O3 Ca1 116.8(2) . . ? Ca1 O3 Ca1 103.11(14) 2_556 . ? P2 O4 H4 109.5 . . ? P2 O6 Ca1 129.8(2) . 2_656 ? C1 O7 Ca1 122.2(3) . . ? C1 O7 H7 111.0 . . ? Ca1 O7 H7 126.8 . . ? Ca1 O8 Ca1 109.30(16) . 2_546 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.241 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.332 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 870777' #TrackingRef '- ALL cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H10 Ca N O8 P' _chemical_formula_weight 283.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.3340(2) _cell_length_b 14.2250(3) _cell_length_c 13.0920(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.1210(14) _cell_angle_gamma 90.00 _cell_volume 992.69(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4417 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0286 _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 -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.45 _reflns_number_total 2258 _reflns_number_gt 1908 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2258 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.85412(8) 0.23299(3) 0.52271(3) 0.01392(18) Uani 1 1 d . . . P2 P 0.54601(12) 0.17863(4) 0.26977(4) 0.0159(2) Uani 1 1 d . . . C3 C 0.6742(4) 0.07483(14) 0.20935(17) 0.0164(5) Uani 1 1 d . . . H3A H 0.5943 0.0717 0.1412 0.020 Uiso 1 1 d R . . H3B H 0.8446 0.0768 0.2020 0.020 Uiso 1 1 d R . . N4 N 0.6078(4) -0.01465(12) 0.26270(14) 0.0151(4) Uani 1 1 d . . . H4 H 0.4459 -0.0093 0.2812 0.018 Uiso 1 1 d R . . O5 O 0.8037(3) -0.13001(11) 0.49894(11) 0.0192(4) Uani 1 1 d . . . O6 O 0.3778(3) -0.14965(11) 0.04363(12) 0.0197(4) Uani 1 1 d . . . O7 O 0.4233(3) -0.11076(12) 0.42196(13) 0.0228(4) Uani 1 1 d . . . O8 O 0.7049(3) 0.20275(11) 0.36230(12) 0.0185(4) Uani 1 1 d . . . O9 O 0.5167(3) 0.25029(11) 0.18680(12) 0.0198(4) Uani 1 1 d . . . C10 C 0.6517(4) -0.09727(15) 0.43085(17) 0.0152(5) Uani 1 1 d . . . O11 O 0.5885(3) 0.35891(12) 0.54737(13) 0.0252(4) Uani 1 1 d . . . H11A H 0.4426 0.3591 0.5190 0.030 Uiso 1 1 d R . . H11B H 0.6186 0.4194 0.5689 0.030 Uiso 1 1 d R . . O12 O 0.2812(3) 0.14172(12) 0.30347(12) 0.0223(4) Uani 1 1 d . . . H12 H 0.2653 0.1445 0.3746 0.027 Uiso 1 1 d R . . O13 O 0.2080(3) -0.03528(12) 0.13653(13) 0.0229(4) Uani 1 1 d . . . C14 C 0.3761(4) -0.09232(14) 0.11700(17) 0.0146(5) Uani 1 1 d . . . C15 C 0.7741(4) -0.03154(16) 0.35510(17) 0.0166(5) Uani 1 1 d . . . H15A H 0.9294 -0.0567 0.3293 0.020 Uiso 1 1 d R . . H15B H 0.8113 0.0253 0.3886 0.020 Uiso 1 1 d R . . C16 C 0.6045(4) -0.09715(15) 0.19119(17) 0.0176(5) Uani 1 1 d . . . H16A H 0.7563 -0.1009 0.1588 0.021 Uiso 1 1 d R . . H16B H 0.5845 -0.1543 0.2349 0.021 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 Ca1 0.0150(3) 0.0150(3) 0.0116(3) -0.00041(15) -0.00146(19) -0.00040(16) P2 0.0197(4) 0.0155(3) 0.0123(3) 0.0004(2) -0.0021(2) -0.0008(2) C3 0.0191(12) 0.0167(10) 0.0134(10) 0.0015(8) 0.0011(9) -0.0001(9) N4 0.0157(10) 0.0147(9) 0.0148(9) -0.0005(7) -0.0001(7) 0.0004(7) O5 0.0216(9) 0.0225(8) 0.0135(8) 0.0021(6) 0.0014(7) 0.0065(6) O6 0.0182(9) 0.0233(9) 0.0175(8) -0.0066(7) -0.0021(7) 0.0019(6) O7 0.0218(10) 0.0235(9) 0.0231(9) 0.0060(7) 0.0001(7) -0.0021(7) O8 0.0247(10) 0.0169(8) 0.0134(8) 0.0005(6) -0.0046(7) -0.0015(7) O9 0.0271(10) 0.0174(7) 0.0144(8) 0.0017(6) -0.0052(7) -0.0008(7) C10 0.0181(12) 0.0148(10) 0.0126(10) -0.0004(8) 0.0003(8) 0.0003(8) O11 0.0196(10) 0.0271(9) 0.0284(10) -0.0073(7) -0.0072(7) 0.0053(7) O12 0.0196(10) 0.0301(9) 0.0173(8) -0.0035(7) 0.0013(7) -0.0019(7) O13 0.0191(10) 0.0222(8) 0.0271(9) -0.0056(7) -0.0038(7) 0.0053(7) C14 0.0138(11) 0.0130(10) 0.0168(11) -0.0010(8) -0.0014(9) -0.0008(8) C15 0.0187(13) 0.0180(11) 0.0127(10) 0.0006(8) -0.0045(9) -0.0019(9) C16 0.0195(13) 0.0160(10) 0.0172(11) -0.0051(9) -0.0016(9) 0.0039(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 Ca1 O8 2.2595(16) . ? Ca1 O9 2.2991(16) 4_666 ? Ca1 O11 2.3138(17) . ? Ca1 O5 2.3654(16) 3_756 ? Ca1 O6 2.3829(16) 2_655 ? Ca1 O7 2.4119(17) 3_656 ? P2 O8 1.4924(17) . ? P2 O9 1.4936(16) . ? P2 O12 1.5850(17) . ? P2 C3 1.820(2) . ? C3 N4 1.501(3) . ? C3 H3A 0.9758 . ? C3 H3B 0.9180 . ? N4 C15 1.493(3) . ? N4 C16 1.501(3) . ? N4 H4 0.9089 . ? O5 C10 1.271(3) . ? O5 Ca1 2.3654(16) 3_756 ? O6 C14 1.260(3) . ? O6 Ca1 2.3829(16) 2_645 ? O7 C10 1.234(3) . ? O7 Ca1 2.4119(17) 3_656 ? O9 Ca1 2.2990(16) 4_565 ? C10 C15 1.527(3) . ? O11 H11A 0.8499 . ? O11 H11B 0.9180 . ? O12 H12 0.9397 . ? O13 C14 1.243(3) . ? C14 C16 1.531(3) . ? C15 H15A 0.9743 . ? C15 H15B 0.9374 . ? C16 H16A 0.9292 . ? C16 H16B 1.0026 . ? 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 O8 Ca1 O9 174.81(6) . 4_666 ? O8 Ca1 O11 94.62(6) . . ? O9 Ca1 O11 90.07(6) 4_666 . ? O8 Ca1 O5 91.01(6) . 3_756 ? O9 Ca1 O5 84.84(6) 4_666 3_756 ? O11 Ca1 O5 167.23(7) . 3_756 ? O8 Ca1 O6 89.44(6) . 2_655 ? O9 Ca1 O6 93.29(6) 4_666 2_655 ? O11 Ca1 O6 83.53(6) . 2_655 ? O5 Ca1 O6 85.07(6) 3_756 2_655 ? O8 Ca1 O7 86.73(6) . 3_656 ? O9 Ca1 O7 90.47(6) 4_666 3_656 ? O11 Ca1 O7 97.50(7) . 3_656 ? O5 Ca1 O7 94.26(6) 3_756 3_656 ? O6 Ca1 O7 176.10(6) 2_655 3_656 ? O8 P2 O9 118.33(10) . . ? O8 P2 O12 109.60(9) . . ? O9 P2 O12 110.98(10) . . ? O8 P2 C3 109.15(10) . . ? O9 P2 C3 105.58(9) . . ? O12 P2 C3 101.84(10) . . ? N4 C3 P2 112.76(15) . . ? N4 C3 H3A 106.6 . . ? P2 C3 H3A 106.0 . . ? N4 C3 H3B 109.1 . . ? P2 C3 H3B 114.2 . . ? H3A C3 H3B 107.8 . . ? C15 N4 C3 111.74(17) . . ? C15 N4 C16 111.87(17) . . ? C3 N4 C16 111.74(17) . . ? C15 N4 H4 109.9 . . ? C3 N4 H4 107.2 . . ? C16 N4 H4 104.0 . . ? C10 O5 Ca1 128.17(13) . 3_756 ? C14 O6 Ca1 138.78(15) . 2_645 ? C10 O7 Ca1 134.27(15) . 3_656 ? P2 O8 Ca1 165.49(11) . . ? P2 O9 Ca1 140.89(9) . 4_565 ? O7 C10 O5 127.7(2) . . ? O7 C10 C15 118.6(2) . . ? O5 C10 C15 113.8(2) . . ? Ca1 O11 H11A 119.8 . . ? Ca1 O11 H11B 131.9 . . ? H11A O11 H11B 106.1 . . ? P2 O12 H12 112.1 . . ? O13 C14 O6 127.2(2) . . ? O13 C14 C16 117.51(19) . . ? O6 C14 C16 115.25(18) . . ? N4 C15 C10 111.68(19) . . ? N4 C15 H15A 105.4 . . ? C10 C15 H15A 112.9 . . ? N4 C15 H15B 110.5 . . ? C10 C15 H15B 108.2 . . ? H15A C15 H15B 108.1 . . ? N4 C16 C14 110.56(17) . . ? N4 C16 H16A 109.9 . . ? C14 C16 H16A 113.5 . . ? N4 C16 H16B 106.1 . . ? C14 C16 H16B 107.4 . . ? H16A C16 H16B 109.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.394 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.078 #===END data_mgpmida _database_code_depnum_ccdc_archive 'CCDC 877820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H26 Mg N2 O18 P2, 2(H2 O)' _chemical_formula_sum 'C10 H30 Mg N2 O20 P2' _chemical_formula_weight 584.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 7.098(2) _cell_length_b 26.678(8) _cell_length_c 12.591(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.191(15) _cell_angle_gamma 90.00 _cell_volume 2383.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2988 _cell_measurement_theta_min 3.313 _cell_measurement_theta_max 61.453 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.805 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7297 _exptl_absorpt_correction_T_max 0.8498 _exptl_absorpt_process_details 'Bruker SADABS, 2010' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'graded multilayer optics' _diffrn_measurement_device_type 'Bruker X8 Proteum' _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 23821 _diffrn_reflns_av_R_equivalents 0.2516 _diffrn_reflns_av_sigmaI/netI 0.1967 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 61.89 _reflns_number_total 3595 _reflns_number_gt 1859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the fact of the poor crystallinity of the single crystal used for the analysis, the R factors reported in this work are high and the completeness and bond precision are relatively low. Hydrogen atoms of the water ligands could not be detected in Fourier maps. Nevertheless, this was the maximum which we could do. ; _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^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3595 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1624 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2160 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 P3 P 0.0921(3) 0.39488(7) 0.19406(15) 0.0304(6) Uani 1 1 d . . . P23 P 0.3771(3) 0.60373(7) 0.56829(15) 0.0311(6) Uani 1 1 d . . . Mg1 Mg 0.1722(3) 0.51576(9) 0.22957(19) 0.0342(7) Uani 1 1 d . . . O4 O 0.1896(6) 0.44367(16) 0.1821(4) 0.0364(13) Uani 1 1 d . . . O25 O 0.5856(6) 0.59226(17) 0.5725(4) 0.0363(13) Uani 1 1 d . . . O30 O 0.1395(7) 0.64806(19) 0.1379(4) 0.0463(15) Uani 1 1 d . . . O33 O 0.0334(7) 0.76088(19) 0.6020(4) 0.0426(14) Uani 1 1 d . . . H33 H 0.0715 0.7898 0.6065 0.064 Uiso 1 1 calc R . . O42 O 0.4236(7) 0.52207(19) 0.1444(4) 0.0484(15) Uani 1 1 d . . . O26 O 0.2438(7) 0.56116(17) 0.5527(4) 0.0394(14) Uani 1 1 d . . . O24 O 0.3281(7) 0.63707(18) 0.6654(4) 0.0385(14) Uani 1 1 d . . . H24 H 0.2544 0.6220 0.7033 0.058 Uiso 1 1 calc R . . N21 N 0.1434(7) 0.65586(19) 0.4264(4) 0.0237(14) Uani 1 1 d . . . H21 H 0.0849 0.6255 0.4248 0.028 Uiso 1 1 calc R . . O29 O 0.1706(7) 0.59111(18) 0.2675(4) 0.0400(14) Uani 1 1 d . . . O41 O 0.3149(8) 0.50521(19) 0.3728(4) 0.0534(16) Uani 1 1 d . . . O44 O -0.0866(8) 0.50874(19) 0.3024(4) 0.0526(16) Uani 1 1 d . . . O43 O 0.0237(8) 0.5368(2) 0.0857(4) 0.0536(16) Uani 1 1 d . . . C27 C 0.1219(10) 0.6763(3) 0.3154(5) 0.0274(18) Uani 1 1 d . . . H27A H 0.2155 0.7022 0.3043 0.033 Uiso 1 1 calc R . . H27B H -0.0018 0.6913 0.3061 0.033 Uiso 1 1 calc R . . O34 O 0.2356(8) 0.75676(19) 0.4681(5) 0.0528(16) Uani 1 1 d . . . C32 C 0.1156(11) 0.7383(3) 0.5231(6) 0.0322(18) Uani 1 1 d . . . C7 C 0.3872(10) 0.3259(2) -0.0482(5) 0.0290(18) Uani 1 1 d . . . H7A H 0.3062 0.2969 -0.0574 0.035 Uiso 1 1 calc R . . H7B H 0.5167 0.3145 -0.0521 0.035 Uiso 1 1 calc R . . C22 C 0.3473(9) 0.6448(3) 0.4563(6) 0.0313(19) Uani 1 1 d . . . H22A H 0.4109 0.6762 0.4719 0.038 Uiso 1 1 calc R . . H22B H 0.4079 0.6299 0.3956 0.038 Uiso 1 1 calc R . . C28 C 0.1465(10) 0.6344(3) 0.2334(6) 0.0314(19) Uani 1 1 d . . . C31 C 0.0407(10) 0.6861(2) 0.5065(6) 0.0301(19) Uani 1 1 d . . . H31A H 0.0462 0.6685 0.5739 0.036 Uiso 1 1 calc R . . H31B H -0.0908 0.6883 0.4844 0.036 Uiso 1 1 calc R . . O10 O 0.3649(7) 0.34471(18) -0.2321(4) 0.0423(15) Uani 1 1 d . . . O9 O 0.3049(7) 0.40643(18) -0.1170(4) 0.0380(13) Uani 1 1 d . . . C8 C 0.3475(10) 0.3626(3) -0.1384(6) 0.0312(19) Uani 1 1 d . . . C2 C 0.1501(10) 0.3543(3) 0.0835(6) 0.0321(18) Uani 1 1 d . . . H2A H 0.0978 0.3214 0.0972 0.038 Uiso 1 1 calc R . . H2B H 0.0869 0.3673 0.0202 0.038 Uiso 1 1 calc R . . N1 N 0.3566(8) 0.3479(2) 0.0594(4) 0.0269(15) Uani 1 1 d . . . H1 H 0.4072 0.3792 0.0584 0.032 Uiso 1 1 calc R . . C11 C 0.4618(10) 0.3196(3) 0.1438(6) 0.0325(19) Uani 1 1 d . . . H11A H 0.5939 0.3186 0.1258 0.039 Uiso 1 1 calc R . . H11B H 0.4518 0.3376 0.2103 0.039 Uiso 1 1 calc R . . O13 O 0.4787(8) 0.24605(19) 0.2418(4) 0.0477(16) Uani 1 1 d . . . H13 H 0.4291 0.2188 0.2528 0.072 Uiso 1 1 calc R . . O14 O 0.2778(8) 0.24631(19) 0.1047(5) 0.0543(17) Uani 1 1 d . . . C12 C 0.3952(11) 0.2677(3) 0.1594(6) 0.0342(19) Uani 1 1 d . . . O5 O 0.1636(7) 0.36638(18) 0.2957(4) 0.0374(13) Uani 1 1 d . . . H5 H 0.2475 0.3827 0.3253 0.056 Uiso 1 1 calc R . . O6 O -0.1185(6) 0.39454(18) 0.1912(4) 0.0361(13) Uani 1 1 d . . . O2 O 0.8083(7) 0.59769(19) 0.3947(4) 0.0422(14) Uani 1 1 d G . . H2C H 0.7480 0.5987 0.4522 0.063 Uiso 1 1 d G . . H2D H 0.7624 0.6173 0.3476 0.063 Uiso 1 1 d G . . O1 O -0.3999(8) 0.43260(19) 0.0703(4) 0.0424(14) Uani 1 1 d G . . H1A H -0.3968 0.4345 0.0029 0.064 Uiso 1 1 d G . . H1B H -0.4592 0.4577 0.0946 0.064 Uiso 1 1 d G . . 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 P3 0.0347(13) 0.0348(12) 0.0218(13) 0.0006(9) 0.0049(9) 0.0032(9) P23 0.0352(13) 0.0390(12) 0.0191(12) 0.0018(9) 0.0020(9) 0.0032(9) Mg1 0.0402(17) 0.0349(15) 0.0276(16) -0.0016(11) 0.0047(12) 0.0036(11) O4 0.038(3) 0.027(3) 0.045(4) -0.005(2) 0.009(2) -0.005(2) O25 0.027(3) 0.051(3) 0.031(3) 0.002(2) 0.001(2) 0.010(2) O30 0.064(4) 0.050(3) 0.025(4) 0.002(3) 0.001(3) -0.004(3) O33 0.050(4) 0.048(3) 0.030(3) -0.013(3) 0.013(3) -0.004(3) O42 0.047(4) 0.049(4) 0.049(4) -0.003(3) 0.012(3) -0.005(3) O26 0.050(3) 0.037(3) 0.031(3) -0.004(2) 0.005(2) -0.009(3) O24 0.047(4) 0.053(3) 0.015(3) -0.010(2) 0.006(2) -0.007(3) N21 0.034(4) 0.020(3) 0.018(3) -0.002(2) 0.005(3) 0.001(3) O29 0.056(4) 0.029(3) 0.035(4) -0.001(2) 0.000(3) -0.001(3) O41 0.078(4) 0.048(3) 0.033(4) -0.003(3) -0.011(3) 0.012(3) O44 0.056(4) 0.047(3) 0.055(4) 0.002(3) 0.021(3) -0.002(3) O43 0.071(4) 0.065(4) 0.025(3) -0.004(3) -0.002(3) 0.014(3) C27 0.033(5) 0.036(4) 0.013(4) 0.008(3) 0.006(3) 0.003(3) O34 0.064(4) 0.047(4) 0.049(4) -0.008(3) 0.026(3) -0.012(3) C32 0.034(5) 0.043(5) 0.020(5) 0.004(4) 0.009(4) 0.007(4) C7 0.035(5) 0.031(4) 0.022(5) -0.010(3) 0.000(3) 0.007(3) C22 0.019(4) 0.047(5) 0.028(5) 0.002(3) -0.001(3) 0.006(3) C28 0.033(5) 0.042(5) 0.019(5) 0.000(4) 0.001(4) -0.008(3) C31 0.028(5) 0.034(5) 0.028(5) 0.004(3) 0.006(3) 0.004(3) O10 0.075(4) 0.038(3) 0.013(3) -0.006(2) 0.001(3) 0.006(3) O9 0.048(3) 0.033(3) 0.033(3) 0.001(2) 0.004(2) 0.003(2) C8 0.033(5) 0.030(5) 0.031(5) 0.010(4) 0.002(4) 0.000(3) C2 0.040(5) 0.039(4) 0.018(4) -0.003(3) 0.006(3) 0.002(4) N1 0.034(4) 0.029(3) 0.018(4) -0.006(3) -0.001(3) 0.002(3) C11 0.027(5) 0.037(4) 0.033(5) -0.004(4) -0.004(4) 0.003(3) O13 0.062(4) 0.042(4) 0.039(4) 0.013(3) -0.009(3) -0.006(3) O14 0.071(4) 0.043(3) 0.049(4) 0.006(3) -0.017(3) -0.017(3) C12 0.042(5) 0.035(5) 0.025(5) 0.005(4) -0.005(4) -0.001(4) O5 0.041(4) 0.049(3) 0.022(3) 0.008(2) 0.001(2) 0.001(2) O6 0.017(3) 0.062(4) 0.030(3) 0.000(2) 0.007(2) 0.005(2) O2 0.051(4) 0.043(3) 0.033(4) 0.002(3) 0.008(3) -0.001(3) O1 0.048(4) 0.050(4) 0.029(3) -0.003(3) 0.008(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P3 O4 1.483(5) . ? P3 O6 1.495(5) . ? P3 O5 1.564(5) . ? P3 C2 1.817(7) . ? P23 O26 1.488(5) . ? P23 O25 1.511(5) . ? P23 O24 1.558(5) . ? P23 C22 1.796(7) . ? Mg1 O4 2.019(5) . ? Mg1 O29 2.066(5) . ? Mg1 O41 2.069(5) . ? Mg1 O44 2.079(6) . ? Mg1 O42 2.108(6) . ? Mg1 O43 2.151(5) . ? O30 C28 1.255(8) . ? O33 C32 1.310(9) . ? O33 H33 0.8200 . ? O24 H24 0.8200 . ? N21 C31 1.494(8) . ? N21 C27 1.505(8) . ? N21 C22 1.517(8) . ? N21 H21 0.9100 . ? O29 C28 1.244(8) . ? C27 C28 1.534(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? O34 C32 1.213(9) . ? C32 C31 1.504(10) . ? C7 N1 1.497(8) . ? C7 C8 1.521(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? O10 C8 1.281(8) . ? O9 C8 1.240(8) . ? C2 N1 1.513(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N1 C11 1.491(8) . ? N1 H1 0.9100 . ? C11 C12 1.476(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? O13 C12 1.319(8) . ? O13 H13 0.8200 . ? O14 C12 1.213(8) . ? O5 H5 0.8200 . ? O2 H2C 0.8497 . ? O2 H2D 0.8503 . ? O1 H1A 0.8501 . ? O1 H1B 0.8503 . ? 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 P3 O6 118.1(3) . . ? O4 P3 O5 111.5(3) . . ? O6 P3 O5 108.9(3) . . ? O4 P3 C2 109.3(3) . . ? O6 P3 C2 102.7(3) . . ? O5 P3 C2 105.2(3) . . ? O26 P23 O25 118.0(3) . . ? O26 P23 O24 112.8(3) . . ? O25 P23 O24 108.8(3) . . ? O26 P23 C22 107.4(3) . . ? O25 P23 C22 104.5(3) . . ? O24 P23 C22 104.1(3) . . ? O4 Mg1 O29 174.9(2) . . ? O4 Mg1 O41 95.5(2) . . ? O29 Mg1 O41 86.3(2) . . ? O4 Mg1 O44 96.0(2) . . ? O29 Mg1 O44 88.7(2) . . ? O41 Mg1 O44 91.4(3) . . ? O4 Mg1 O42 82.4(2) . . ? O29 Mg1 O42 92.8(2) . . ? O41 Mg1 O42 92.8(2) . . ? O44 Mg1 O42 175.6(2) . . ? O4 Mg1 O43 91.8(2) . . ? O29 Mg1 O43 86.3(2) . . ? O41 Mg1 O43 172.6(2) . . ? O44 Mg1 O43 88.5(2) . . ? O42 Mg1 O43 87.5(2) . . ? P3 O4 Mg1 140.7(3) . . ? C32 O33 H33 109.5 . . ? P23 O24 H24 109.5 . . ? C31 N21 C27 113.0(5) . . ? C31 N21 C22 114.4(5) . . ? C27 N21 C22 112.2(5) . . ? C31 N21 H21 105.4 . . ? C27 N21 H21 105.4 . . ? C22 N21 H21 105.4 . . ? C28 O29 Mg1 145.7(5) . . ? N21 C27 C28 110.5(5) . . ? N21 C27 H27A 109.5 . . ? C28 C27 H27A 109.6 . . ? N21 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? O34 C32 O33 125.2(7) . . ? O34 C32 C31 123.2(7) . . ? O33 C32 C31 111.7(7) . . ? N1 C7 C8 113.3(6) . . ? N1 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N21 C22 P23 114.2(5) . . ? N21 C22 H22A 108.7 . . ? P23 C22 H22A 108.7 . . ? N21 C22 H22B 108.7 . . ? P23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? O29 C28 O30 127.0(7) . . ? O29 C28 C27 117.5(6) . . ? O30 C28 C27 115.5(6) . . ? N21 C31 C32 114.7(6) . . ? N21 C31 H31A 108.6 . . ? C32 C31 H31A 108.6 . . ? N21 C31 H31B 108.6 . . ? C32 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? O9 C8 O10 125.4(7) . . ? O9 C8 C7 119.2(7) . . ? O10 C8 C7 115.4(6) . . ? N1 C2 P3 117.2(5) . . ? N1 C2 H2A 108.0 . . ? P3 C2 H2A 108.0 . . ? N1 C2 H2B 108.0 . . ? P3 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C11 N1 C7 111.5(5) . . ? C11 N1 C2 112.8(5) . . ? C7 N1 C2 112.7(5) . . ? C11 N1 H1 106.5 . . ? C7 N1 H1 106.5 . . ? C2 N1 H1 106.5 . . ? C12 C11 N1 114.4(6) . . ? C12 C11 H11A 108.7 . . ? N1 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? N1 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C12 O13 H13 109.5 . . ? O14 C12 O13 122.2(7) . . ? O14 C12 C11 125.8(7) . . ? O13 C12 C11 112.1(6) . . ? P3 O5 H5 109.5 . . ? H2C O2 H2D 112.6 . . ? H1A O1 H1B 109.5 . . ? 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 N21 H21 O2 0.91 2.13 2.861(8) 137.2 1_455 N1 H1 O1 0.91 1.98 2.846(8) 158.9 1_655 O33 H33 O30 0.82 1.77 2.581(7) 170.4 4_576 O24 H24 O6 0.82 1.72 2.509(7) 162.2 3_566 O13 H13 O10 0.82 1.77 2.576(7) 168.6 4_566 O5 H5 O25 0.82 1.86 2.649(7) 162.3 3_666 O2 H2C O25 0.85 1.93 2.772(7) 170.5 . O2 H2D O10 0.85 1.98 2.821(7) 172.5 3_665 O1 H1B O42 0.85 2.01 2.861(7) 173.3 1_455 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 61.89 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.502 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.110 #===END