1. Cif files for all compounds data_(en)(HDTMP) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H20 N2 O8 P2' _chemical_formula_weight 310.18 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' _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 6.1950(11) _cell_length_b 7.4889(13) _cell_length_c 15.955(3) _cell_angle_alpha 84.472(3) _cell_angle_beta 85.319(3) _cell_angle_gamma 67.881(3) _cell_volume 681.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max .22 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 0.352 _exptl_absorpt_correction_type none _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4795 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3056 _reflns_number_gt 2398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+0.6434P] 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 3056 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.002 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 0.8040(5) 0.1947(4) 0.1934(2) 0.0249(6) Uani 1 1 d . . . H1 H 0.6919 0.1548 0.2282 0.030 Uiso 1 1 calc R . . H2 H 0.8188 0.1440 0.1386 0.030 Uiso 1 1 calc R . . C2 C 1.0886(6) -0.0927(4) 0.2704(2) 0.0306(7) Uani 1 1 d . . . H3 H 1.2383 -0.1368 0.2960 0.037 Uiso 1 1 calc R . . H4 H 1.1034 -0.1756 0.2254 0.037 Uiso 1 1 calc R . . C3 C 1.2334(5) 0.1263(4) 0.17426(19) 0.0261(6) Uani 1 1 d . . . H7 H 1.2109 0.2618 0.1639 0.031 Uiso 1 1 calc R . . H6 H 1.3781 0.0624 0.2028 0.031 Uiso 1 1 calc R . . C4 C 1.2585(6) 0.0407(5) 0.0904(2) 0.0304(7) Uani 1 1 d . . . H9 H 1.1269 0.1173 0.0568 0.036 Uiso 1 1 calc R . . H8 H 1.2598 -0.0897 0.0994 0.036 Uiso 1 1 calc R . . C5 C 1.4849(6) 0.0370(5) 0.0436(2) 0.0304(7) Uani 1 1 d . . . H11 H 1.4866 0.1666 0.0384 0.037 Uiso 1 1 calc R . . H10 H 1.6157 -0.0448 0.0765 0.037 Uiso 1 1 calc R . . C6 C 0.4360(6) 0.4603(5) 0.5342(2) 0.0322(7) Uani 1 1 d . . . H18 H 0.4219 0.3447 0.5169 0.039 Uiso 1 1 calc R . . H17 H 0.5225 0.4260 0.5852 0.039 Uiso 1 1 calc R . . N1 N 1.0339(4) 0.1105(3) 0.23273(16) 0.0225(5) Uani 1 1 d . . . N2 N 0.2002(5) 0.6082(4) 0.55117(17) 0.0314(6) Uani 1 1 d . . . H15 H 0.2137 0.7080 0.5732 0.047 Uiso 1 1 calc R . . H16 H 0.1185 0.5569 0.5873 0.047 Uiso 1 1 calc R . . H14 H 0.1270 0.6483 0.5032 0.047 Uiso 1 1 calc R . . O1 O 0.4237(4) 0.5098(3) 0.18713(16) 0.0369(6) Uani 1 1 d . . . H12 H 0.3727 0.5365 0.1398 0.055 Uiso 1 1 calc R . . O2 O 0.7685(5) 0.5139(3) 0.25762(16) 0.0415(6) Uani 1 1 d . . . O3 O 0.7696(4) 0.5256(4) 0.09649(16) 0.0400(6) Uani 1 1 d . . . O4 O 0.7574(5) 0.0653(4) 0.39080(17) 0.0434(7) Uani 1 1 d . . . O5 O 0.6784(4) -0.1465(3) 0.29920(16) 0.0333(5) Uani 1 1 d . . . H13 H 0.7200 -0.2596 0.2881 0.050 Uiso 1 1 calc R . . O6 O 0.9983(4) -0.3042(4) 0.40061(15) 0.0380(6) Uani 1 1 d . . . O7 O 0.1627(6) 0.6073(5) 0.0616(2) 0.0476(7) Uani 1 1 d . . . O8 O 0.2544(6) 0.2655(5) 0.3505(2) 0.0712(10) Uani 1 1 d . . . P1 P 0.69371(14) 0.45808(11) 0.18044(5) 0.0254(2) Uani 1 1 d . . . P2 P 0.87098(14) -0.12077(12) 0.34982(5) 0.0261(2) Uani 1 1 d . . . H5 H 1.027(6) 0.184(5) 0.275(2) 0.028(9) Uiso 1 1 d . . . H20 H 0.026(11) 0.594(8) 0.074(4) 0.080(17) Uiso 1 1 d . . . H19 H 0.214(13) 0.555(11) 0.020(5) 0.11(3) Uiso 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 C1 0.0226(14) 0.0203(14) 0.0324(16) -0.0022(12) -0.0005(11) -0.0086(11) C2 0.0284(15) 0.0238(15) 0.0355(17) 0.0037(13) 0.0030(13) -0.0074(12) C3 0.0238(14) 0.0264(15) 0.0304(16) -0.0018(12) 0.0044(12) -0.0131(12) C4 0.0314(16) 0.0350(17) 0.0277(16) -0.0041(13) 0.0032(12) -0.0163(14) C5 0.0296(16) 0.0320(17) 0.0308(17) -0.0044(13) 0.0054(12) -0.0136(13) C6 0.0325(16) 0.0296(16) 0.0323(17) -0.0002(13) 0.0023(13) -0.0104(13) N1 0.0240(12) 0.0198(12) 0.0242(13) -0.0027(10) 0.0029(10) -0.0094(10) N2 0.0322(14) 0.0369(15) 0.0270(14) -0.0029(11) 0.0014(11) -0.0154(12) O1 0.0268(12) 0.0364(13) 0.0409(14) -0.0028(10) -0.0008(10) -0.0045(10) O2 0.0547(16) 0.0277(13) 0.0421(14) -0.0077(11) -0.0154(12) -0.0114(11) O3 0.0440(14) 0.0418(14) 0.0381(14) 0.0084(11) -0.0020(11) -0.0231(12) O4 0.0523(16) 0.0453(15) 0.0440(15) -0.0207(12) 0.0147(12) -0.0302(13) O5 0.0329(12) 0.0225(11) 0.0470(14) -0.0015(10) -0.0120(10) -0.0115(9) O6 0.0432(14) 0.0444(14) 0.0334(13) 0.0132(11) -0.0131(10) -0.0258(12) O7 0.0436(16) 0.0584(19) 0.0502(18) 0.0027(15) -0.0091(13) -0.0298(14) O8 0.056(2) 0.079(2) 0.078(2) -0.032(2) 0.0038(17) -0.0206(17) P1 0.0274(4) 0.0198(4) 0.0287(4) -0.0020(3) -0.0026(3) -0.0082(3) P2 0.0303(4) 0.0282(4) 0.0246(4) -0.0012(3) -0.0003(3) -0.0168(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 C1 N1 1.488(4) . ? C1 P1 1.825(3) . ? C1 H1 0.9700 . ? C1 H2 0.9700 . ? C2 N1 1.504(4) . ? C2 P2 1.830(3) . ? C2 H3 0.9700 . ? C2 H4 0.9700 . ? C3 C4 1.510(4) . ? C3 N1 1.521(4) . ? C3 H7 0.9700 . ? C3 H6 0.9700 . ? C4 C5 1.526(4) . ? C4 H9 0.9700 . ? C4 H8 0.9700 . ? C5 C5 1.519(6) 2_855 ? C5 H11 0.9700 . ? C5 H10 0.9700 . ? C6 N2 1.486(4) . ? C6 C6 1.505(6) 2_666 ? C6 H18 0.9700 . ? C6 H17 0.9700 . ? N1 H5 0.91(4) . ? N2 H15 0.8900 . ? N2 H16 0.8900 . ? N2 H14 0.8900 . ? O1 P1 1.565(2) . ? O1 H12 0.8200 . ? O2 P1 1.498(2) . ? O3 P1 1.489(3) . ? O4 P2 1.492(3) . ? O5 P2 1.572(2) . ? O5 H13 0.8200 . ? O6 P2 1.497(2) . ? O7 H20 0.89(7) . ? O7 H19 0.79(8) . ? 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 N1 C1 P1 112.84(19) . . ? N1 C1 H1 109.0 . . ? P1 C1 H1 109.0 . . ? N1 C1 H2 109.0 . . ? P1 C1 H2 109.0 . . ? H1 C1 H2 107.8 . . ? N1 C2 P2 114.5(2) . . ? N1 C2 H3 108.6 . . ? P2 C2 H3 108.6 . . ? N1 C2 H4 108.6 . . ? P2 C2 H4 108.6 . . ? H3 C2 H4 107.6 . . ? C4 C3 N1 114.9(2) . . ? C4 C3 H7 108.5 . . ? N1 C3 H7 108.5 . . ? C4 C3 H6 108.5 . . ? N1 C3 H6 108.5 . . ? H7 C3 H6 107.5 . . ? C3 C4 C5 109.8(2) . . ? C3 C4 H9 109.7 . . ? C5 C4 H9 109.7 . . ? C3 C4 H8 109.7 . . ? C5 C4 H8 109.7 . . ? H9 C4 H8 108.2 . . ? C5 C5 C4 112.7(3) 2_855 . ? C5 C5 H11 109.0 2_855 . ? C4 C5 H11 109.0 . . ? C5 C5 H10 109.0 2_855 . ? C4 C5 H10 109.0 . . ? H11 C5 H10 107.8 . . ? N2 C6 C6 109.4(3) . 2_666 ? N2 C6 H18 109.8 . . ? C6 C6 H18 109.8 2_666 . ? N2 C6 H17 109.8 . . ? C6 C6 H17 109.8 2_666 . ? H18 C6 H17 108.2 . . ? C1 N1 C2 113.2(2) . . ? C1 N1 C3 113.1(2) . . ? C2 N1 C3 111.5(2) . . ? C1 N1 H5 107(2) . . ? C2 N1 H5 107(2) . . ? C3 N1 H5 104(2) . . ? C6 N2 H15 109.5 . . ? C6 N2 H16 109.5 . . ? H15 N2 H16 109.5 . . ? C6 N2 H14 109.5 . . ? H15 N2 H14 109.5 . . ? H16 N2 H14 109.5 . . ? P1 O1 H12 109.5 . . ? P2 O5 H13 109.5 . . ? H20 O7 H19 106(6) . . ? O3 P1 O2 118.24(15) . . ? O3 P1 O1 111.15(14) . . ? O2 P1 O1 109.71(15) . . ? O3 P1 C1 111.02(15) . . ? O2 P1 C1 103.54(14) . . ? O1 P1 C1 101.68(13) . . ? O4 P2 O6 120.82(16) . . ? O4 P2 O5 106.58(14) . . ? O6 P2 O5 110.12(13) . . ? O4 P2 C2 108.03(14) . . ? O6 P2 C2 104.70(14) . . ? O5 P2 C2 105.65(15) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 1.870 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.090 data_Sr-HDTMP _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H42 N2 O20 P4 Sr' _chemical_formula_weight 721.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Sr' 'Sr' -1.5307 3.2498 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.999(4) _cell_length_b 5.9939(13) _cell_length_c 33.447(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.52(2) _cell_angle_gamma 90.00 _cell_volume 2750.1(14) _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 block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 2.279 _exptl_absorpt_correction_type none _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6177 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 23.29 _reflns_number_total 1992 _reflns_number_gt 1936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+9.2986P] 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 1992 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 1.0000 0.12171(9) 0.7500 0.0252(2) Uani 1 2 d S . . P1 P 1.02756(7) 0.29361(16) 0.58901(3) 0.0221(3) Uani 1 1 d . . . P2 P 0.78278(7) 0.32759(17) 0.67274(3) 0.0229(3) Uani 1 1 d . . . C1 C 0.8644(3) -0.0986(6) 0.58680(11) 0.0229(8) Uani 1 1 d . . . H1A H 0.8418 -0.2296 0.5992 0.028 Uiso 1 1 calc R . . H1B H 0.9286 -0.1322 0.5816 0.028 Uiso 1 1 calc R . . C2 C 0.7962(3) -0.0551(7) 0.54641(11) 0.0280(9) Uani 1 1 d . . . H2A H 0.8231 0.0607 0.5317 0.034 Uiso 1 1 calc R . . H2B H 0.7337 -0.0040 0.5512 0.034 Uiso 1 1 calc R . . C3 C 0.7822(3) -0.2676(7) 0.52106(12) 0.0300(9) Uani 1 1 d . . . H3A H 0.7529 -0.3806 0.5355 0.051(15) Uiso 1 1 calc R . . H3B H 0.8454 -0.3223 0.5178 0.064(17) Uiso 1 1 calc R . . C4 C 0.9062(3) 0.3061(6) 0.60075(11) 0.0228(8) Uani 1 1 d . . . H4A H 0.9052 0.4230 0.6207 0.027 Uiso 1 1 calc R . . H4B H 0.8600 0.3467 0.5762 0.027 Uiso 1 1 calc R . . C5 C 0.7826(3) 0.1148(7) 0.63411(12) 0.0275(9) Uani 1 1 d . . . H5A H 0.7698 -0.0279 0.6457 0.033 Uiso 1 1 calc R . . H5B H 0.7287 0.1451 0.6116 0.033 Uiso 1 1 calc R . . N1 N 0.8736(2) 0.0920(5) 0.61699(10) 0.0196(7) Uani 1 1 d . . . O1 O 1.0264(2) 0.1988(5) 0.54772(9) 0.0358(7) Uani 1 1 d . . . O2 O 1.08686(19) 0.1728(5) 0.62500(9) 0.0345(7) Uani 1 1 d . . . O3 O 1.0554(2) 0.5457(5) 0.59099(10) 0.0314(7) Uani 1 1 d . . . O4 O 0.6994(2) 0.2667(5) 0.69232(9) 0.0345(7) Uani 1 1 d . . . O5 O 0.7633(2) 0.5541(5) 0.64894(10) 0.0344(7) Uani 1 1 d . . . O6 O 0.8834(2) 0.3457(5) 0.69813(8) 0.0356(7) Uani 1 1 d . . . O7 O 0.9980(2) -0.1552(5) 0.68190(9) 0.0380(7) Uani 1 1 d . . . O8 O 0.8536(3) -0.1641(6) 0.73537(10) 0.0540(9) Uani 1 1 d . . . O9 O 1.1074(2) 0.3195(6) 0.70550(10) 0.0487(9) Uani 1 1 d . . . O10 O 0.0772(2) 0.7809(5) 0.53046(9) 0.0416(7) Uani 1 1 d . . . H1 H 0.915(3) 0.059(7) 0.6333(13) 0.020(12) Uiso 1 1 d . . . H2 H 1.058(4) 0.599(9) 0.5714(16) 0.044(17) Uiso 1 1 d . . . H3 H 0.708(5) 0.576(12) 0.636(2) 0.08(2) Uiso 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 0.0233(3) 0.0315(3) 0.0192(3) 0.000 0.0004(2) 0.000 P1 0.0193(5) 0.0249(5) 0.0222(5) 0.0010(4) 0.0048(4) 0.0015(4) P2 0.0221(5) 0.0262(5) 0.0205(5) -0.0014(4) 0.0046(4) 0.0041(4) C1 0.0259(19) 0.0210(19) 0.0215(19) -0.0056(15) 0.0037(15) 0.0003(15) C2 0.031(2) 0.029(2) 0.0217(19) -0.0033(17) -0.0001(16) 0.0013(17) C3 0.032(2) 0.032(2) 0.024(2) -0.0034(17) -0.0012(17) 0.0003(18) C4 0.0234(19) 0.0204(19) 0.0246(19) 0.0009(15) 0.0050(15) 0.0006(15) C5 0.026(2) 0.030(2) 0.028(2) -0.0089(17) 0.0107(17) -0.0059(16) N1 0.0175(16) 0.0228(17) 0.0171(16) -0.0022(13) 0.0001(14) 0.0013(13) O1 0.0440(17) 0.0358(16) 0.0306(15) -0.0036(13) 0.0148(13) 0.0027(13) O2 0.0252(14) 0.0452(17) 0.0322(15) 0.0102(13) 0.0033(12) 0.0067(13) O3 0.0331(16) 0.0285(15) 0.0337(17) -0.0009(14) 0.0089(13) -0.0090(13) O4 0.0329(15) 0.0411(17) 0.0334(15) 0.0008(13) 0.0163(12) 0.0036(13) O5 0.0270(15) 0.0301(16) 0.0465(18) 0.0091(14) 0.0081(13) 0.0055(13) O6 0.0280(15) 0.0484(18) 0.0272(15) -0.0017(13) -0.0020(12) 0.0022(13) O7 0.0341(16) 0.0462(18) 0.0323(16) 0.0043(14) 0.0037(13) 0.0082(14) O8 0.056(2) 0.069(2) 0.0367(18) -0.0018(17) 0.0083(16) -0.0275(18) O9 0.0484(19) 0.061(2) 0.0385(18) -0.0048(16) 0.0138(15) -0.0156(17) O10 0.0541(19) 0.0326(16) 0.0400(17) 0.0080(14) 0.0143(15) 0.0070(14) _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 O6 2.519(3) 2_756 ? Sr1 O6 2.519(3) . ? Sr1 O9 2.603(3) 2_756 ? Sr1 O9 2.603(3) . ? Sr1 O8 2.641(3) . ? Sr1 O8 2.641(3) 2_756 ? Sr1 O7 2.814(3) . ? Sr1 O7 2.814(3) 2_756 ? P1 O1 1.490(3) . ? P1 O2 1.505(3) . ? P1 O3 1.558(3) . ? P1 C4 1.820(4) . ? P2 O4 1.494(3) . ? P2 O6 1.497(3) . ? P2 O5 1.570(3) . ? P2 C5 1.815(4) . ? C1 N1 1.513(5) . ? C1 C2 1.513(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.521(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C3 1.528(7) 7_646 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N1 1.500(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.503(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N1 H1 0.74(4) . ? O3 H2 0.73(5) . ? O5 H3 0.81(7) . ? 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 O6 Sr1 O6 115.59(14) 2_756 . ? O6 Sr1 O9 74.47(11) 2_756 2_756 ? O6 Sr1 O9 77.42(10) . 2_756 ? O6 Sr1 O9 77.42(10) 2_756 . ? O6 Sr1 O9 74.47(11) . . ? O9 Sr1 O9 125.81(17) 2_756 . ? O6 Sr1 O8 147.72(10) 2_756 . ? O6 Sr1 O8 81.14(11) . . ? O9 Sr1 O8 83.44(12) 2_756 . ? O9 Sr1 O8 134.84(10) . . ? O6 Sr1 O8 81.14(11) 2_756 2_756 ? O6 Sr1 O8 147.72(10) . 2_756 ? O9 Sr1 O8 134.84(10) 2_756 2_756 ? O9 Sr1 O8 83.44(12) . 2_756 ? O8 Sr1 O8 99.11(18) . 2_756 ? O6 Sr1 O7 140.56(9) 2_756 . ? O6 Sr1 O7 81.75(9) . . ? O9 Sr1 O7 144.88(10) 2_756 . ? O9 Sr1 O7 73.70(10) . . ? O8 Sr1 O7 65.51(10) . . ? O8 Sr1 O7 69.47(10) 2_756 . ? O6 Sr1 O7 81.75(9) 2_756 2_756 ? O6 Sr1 O7 140.56(9) . 2_756 ? O9 Sr1 O7 73.70(10) 2_756 2_756 ? O9 Sr1 O7 144.88(10) . 2_756 ? O8 Sr1 O7 69.47(10) . 2_756 ? O8 Sr1 O7 65.51(10) 2_756 2_756 ? O7 Sr1 O7 107.71(13) . 2_756 ? O1 P1 O2 117.39(18) . . ? O1 P1 O3 111.43(18) . . ? O2 P1 O3 109.84(18) . . ? O1 P1 C4 112.19(17) . . ? O2 P1 C4 103.70(16) . . ? O3 P1 C4 100.77(16) . . ? O4 P2 O6 119.92(17) . . ? O4 P2 O5 111.20(17) . . ? O6 P2 O5 105.88(18) . . ? O4 P2 C5 104.49(18) . . ? O6 P2 C5 108.79(18) . . ? O5 P2 C5 105.74(18) . . ? N1 C1 C2 114.9(3) . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? C1 C2 C3 110.0(3) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C3 112.7(4) . 7_646 ? C2 C3 H3A 109.1 . . ? C3 C3 H3A 109.1 7_646 . ? C2 C3 H3B 109.1 . . ? C3 C3 H3B 109.1 7_646 . ? H3A C3 H3B 107.8 . . ? N1 C4 P1 114.1(2) . . ? N1 C4 H4A 108.7 . . ? P1 C4 H4A 108.7 . . ? N1 C4 H4B 108.7 . . ? P1 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N1 C5 P2 117.0(3) . . ? N1 C5 H5A 108.0 . . ? P2 C5 H5A 108.0 . . ? N1 C5 H5B 108.0 . . ? P2 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? C4 N1 C5 113.7(3) . . ? C4 N1 C1 113.3(3) . . ? C5 N1 C1 111.0(3) . . ? C4 N1 H1 104(3) . . ? C5 N1 H1 110(3) . . ? C1 N1 H1 104(3) . . ? P1 O3 H2 116(4) . . ? P2 O5 H3 117(5) . . ? P2 O6 Sr1 139.39(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.592 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.098 data_Ba-HDTMP _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H42 Ba N2 O20 P4' _chemical_formula_weight 771.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ba' 'Ba' -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.084(4) _cell_length_b 6.0158(15) _cell_length_c 33.793(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.717(4) _cell_angle_gamma 90.00 _cell_volume 2813.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.723 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8568 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.01 _reflns_number_total 3086 _reflns_number_gt 2982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+7.5933P] 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 3086 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.281 _refine_ls_restrained_S_all 1.281 _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 Ba1 Ba 0.5000 0.13076(5) 0.2500 0.02374(10) Uani 1 2 d S . . C1 C 0.6375(2) -0.0981(5) 0.41463(9) 0.0215(6) Uani 1 1 d . . . H1A H 0.5738 -0.1331 0.4200 0.026 Uiso 1 1 calc R . . H1B H 0.6606 -0.2279 0.4023 0.026 Uiso 1 1 calc R . . C2 C 0.7045(2) -0.0542(6) 0.45442(10) 0.0271(7) Uani 1 1 d . . . H2A H 0.6774 0.0609 0.4691 0.033 Uiso 1 1 calc R . . H2B H 0.7666 -0.0028 0.4495 0.033 Uiso 1 1 calc R . . C3 C 0.7181(3) -0.2675(6) 0.47946(10) 0.0287(7) Uani 1 1 d . . . H3B H 0.6554 -0.3215 0.4831 0.045(13) Uiso 1 1 calc R . . H3A H 0.7470 -0.3803 0.4649 0.062(17) Uiso 1 1 calc R . . C4 C 0.7185(2) 0.1120(6) 0.36712(11) 0.0277(7) Uani 1 1 d . . . H4A H 0.7282 -0.0282 0.3543 0.033 Uiso 1 1 calc R . . H4B H 0.7727 0.1323 0.3891 0.033 Uiso 1 1 calc R . . C5 C 0.5965(2) 0.3060(5) 0.40119(10) 0.0208(6) Uani 1 1 d . . . H5A H 0.5987 0.4234 0.3817 0.025 Uiso 1 1 calc R . . H5B H 0.6418 0.3442 0.4255 0.025 Uiso 1 1 calc R . . H1C H 0.579(3) 0.055(7) 0.3659(12) 0.025(10) Uiso 1 1 d . . . N1 N 0.62800(19) 0.0925(4) 0.38477(8) 0.0186(5) Uani 1 1 d . . . O1 O 0.80510(18) 0.2724(5) 0.31084(8) 0.0328(6) Uani 1 1 d . . . O2 O 0.74357(17) 0.5519(4) 0.35617(8) 0.0321(6) Uani 1 1 d . . . H2C H 0.8021 0.5667 0.3633 0.053(15) Uiso 1 1 calc R . . O3 O 0.62353(19) 0.3627(5) 0.30540(8) 0.0364(6) Uani 1 1 d . . . O4 O 0.41832(18) 0.1700(5) 0.37727(8) 0.0339(6) Uani 1 1 d . . . O5 O 0.44642(18) 0.5455(4) 0.41012(8) 0.0307(5) Uani 1 1 d . . . H5D H 0.4423 0.5909 0.4326 0.046 Uiso 1 1 calc R . . O6 O 0.4751(2) 0.2013(5) 0.45366(8) 0.0345(6) Uani 1 1 d . . . O7 O 0.6507(3) -0.1788(6) 0.26387(10) 0.0561(9) Uani 1 1 d . . . O8 O 0.5071(2) -0.1596(5) 0.32123(8) 0.0370(6) Uani 1 1 d . . . O9 O 0.3908(3) 0.3407(6) 0.29888(10) 0.0520(8) Uani 1 1 d . . . O10 O 0.4231(2) 0.7819(5) 0.46962(9) 0.0408(6) Uani 1 1 d . . . P1 P 0.72214(6) 0.33349(14) 0.33066(2) 0.02114(17) Uani 1 1 d . . . P2 P 0.47521(6) 0.29378(14) 0.41267(2) 0.02069(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.02395(15) 0.02740(16) 0.01786(14) 0.000 -0.00132(10) 0.000 C1 0.0249(14) 0.0179(14) 0.0214(14) 0.0042(11) 0.0032(12) -0.0017(11) C2 0.0291(16) 0.0273(16) 0.0220(15) 0.0046(13) -0.0029(13) -0.0015(13) C3 0.0319(17) 0.0307(17) 0.0213(16) 0.0074(13) -0.0007(14) 0.0004(14) C4 0.0245(15) 0.0276(17) 0.0341(17) 0.0102(14) 0.0138(13) 0.0065(13) C5 0.0204(14) 0.0186(14) 0.0234(14) -0.0010(11) 0.0041(12) -0.0011(11) N1 0.0182(11) 0.0180(12) 0.0192(12) 0.0017(9) 0.0023(10) 0.0003(10) O1 0.0338(13) 0.0376(14) 0.0306(13) -0.0035(11) 0.0157(11) -0.0042(11) O2 0.0229(11) 0.0290(13) 0.0454(15) -0.0096(11) 0.0089(11) -0.0066(10) O3 0.0297(13) 0.0474(16) 0.0279(13) 0.0004(11) -0.0058(10) -0.0031(11) O4 0.0247(12) 0.0408(15) 0.0344(14) -0.0126(11) 0.0008(10) -0.0071(10) O5 0.0316(12) 0.0247(12) 0.0368(13) 0.0011(10) 0.0088(10) 0.0089(10) O6 0.0429(14) 0.0351(14) 0.0282(13) 0.0037(11) 0.0135(11) -0.0016(12) O7 0.066(2) 0.066(2) 0.0361(16) 0.0035(15) 0.0105(15) 0.0328(18) O8 0.0361(14) 0.0436(16) 0.0304(13) -0.0019(11) 0.0036(11) -0.0110(12) O9 0.0581(19) 0.059(2) 0.0423(17) 0.0056(15) 0.0180(15) 0.0214(16) O10 0.0535(17) 0.0332(14) 0.0367(15) -0.0070(11) 0.0110(13) -0.0056(13) P1 0.0212(4) 0.0220(4) 0.0203(4) 0.0002(3) 0.0040(3) -0.0035(3) P2 0.0177(4) 0.0234(4) 0.0210(4) -0.0011(3) 0.0039(3) -0.0017(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 Ba1 O3 2.696(3) . ? Ba1 O3 2.696(3) 2_655 ? Ba1 O9 2.763(3) 2_655 ? Ba1 O9 2.763(3) . ? Ba1 O7 2.797(3) 2_655 ? Ba1 O7 2.797(3) . ? Ba1 O8 2.961(3) 2_655 ? Ba1 O8 2.961(3) . ? C1 C2 1.515(4) . ? C1 N1 1.517(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.529(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C3 1.521(6) 7_646 ? C3 H3B 0.9700 . ? C3 H3A 0.9700 . ? C4 N1 1.509(4) . ? C4 P1 1.822(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.499(4) . ? C5 P2 1.822(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N1 H1C 0.88(4) . ? O1 P1 1.497(3) . ? O2 P1 1.570(3) . ? O2 H2C 0.8200 . ? O3 P1 1.499(3) . ? O4 P2 1.507(3) . ? O5 P2 1.566(3) . ? O5 H5D 0.8200 . ? O6 P2 1.493(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 O3 Ba1 O3 117.66(12) . 2_655 ? O3 Ba1 O9 79.59(9) . 2_655 ? O3 Ba1 O9 72.99(10) 2_655 2_655 ? O3 Ba1 O9 72.99(10) . . ? O3 Ba1 O9 79.59(9) 2_655 . ? O9 Ba1 O9 125.60(15) 2_655 . ? O3 Ba1 O7 146.37(9) . 2_655 ? O3 Ba1 O7 81.76(10) 2_655 2_655 ? O9 Ba1 O7 133.92(9) 2_655 2_655 ? O9 Ba1 O7 85.13(12) . 2_655 ? O3 Ba1 O7 81.76(10) . . ? O3 Ba1 O7 146.37(9) 2_655 . ? O9 Ba1 O7 85.13(12) 2_655 . ? O9 Ba1 O7 133.92(9) . . ? O7 Ba1 O7 96.50(18) 2_655 . ? O3 Ba1 O8 142.16(8) . 2_655 ? O3 Ba1 O8 79.69(8) 2_655 2_655 ? O9 Ba1 O8 73.86(9) 2_655 2_655 ? O9 Ba1 O8 144.82(10) . 2_655 ? O7 Ba1 O8 63.97(9) 2_655 2_655 ? O7 Ba1 O8 69.71(9) . 2_655 ? O3 Ba1 O8 79.69(8) . . ? O3 Ba1 O8 142.16(8) 2_655 . ? O9 Ba1 O8 144.82(10) 2_655 . ? O9 Ba1 O8 73.86(9) . . ? O7 Ba1 O8 69.71(9) 2_655 . ? O7 Ba1 O8 63.97(9) . . ? O8 Ba1 O8 107.69(11) 2_655 . ? C2 C1 N1 115.0(3) . . ? C2 C1 H1A 108.5 . . ? N1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? N1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C1 C2 C3 109.8(3) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C3 C3 C2 112.4(4) 7_646 . ? C3 C3 H3B 109.1 7_646 . ? C2 C3 H3B 109.1 . . ? C3 C3 H3A 109.1 7_646 . ? C2 C3 H3A 109.1 . . ? H3B C3 H3A 107.9 . . ? N1 C4 P1 117.2(2) . . ? N1 C4 H4A 108.0 . . ? P1 C4 H4A 108.0 . . ? N1 C4 H4B 108.0 . . ? P1 C4 H4B 108.0 . . ? H4A C4 H4B 107.2 . . ? N1 C5 P2 113.5(2) . . ? N1 C5 H5A 108.9 . . ? P2 C5 H5A 108.9 . . ? N1 C5 H5B 108.9 . . ? P2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 N1 C4 114.2(2) . . ? C5 N1 C1 113.4(2) . . ? C4 N1 C1 110.2(2) . . ? C5 N1 H1C 104(3) . . ? C4 N1 H1C 110(3) . . ? C1 N1 H1C 104(3) . . ? P1 O2 H2C 109.5 . . ? P1 O3 Ba1 138.13(17) . . ? P2 O5 H5D 109.5 . . ? O1 P1 O3 119.45(16) . . ? O1 P1 O2 111.40(15) . . ? O3 P1 O2 106.13(16) . . ? O1 P1 C4 104.23(16) . . ? O3 P1 C4 109.32(16) . . ? O2 P1 C4 105.52(17) . . ? O6 P2 O4 117.40(17) . . ? O6 P2 O5 111.52(15) . . ? O4 P2 O5 109.88(16) . . ? O6 P2 C5 112.03(16) . . ? O4 P2 C5 103.41(15) . . ? O5 P2 C5 101.11(14) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.603 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.146 data_Cu-HDTMP _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H46 Cu N2 O22 P4' _chemical_formula_weight 733.91 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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 6.267(2) _cell_length_b 7.6810(12) _cell_length_c 16.879(7) _cell_angle_alpha 86.36(3) _cell_angle_beta 83.74(2) _cell_angle_gamma 66.44(2) _cell_volume 740.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour 'PALE BLUE' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 385 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type none _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4540 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2857 _reflns_number_gt 2457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.2989P] 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 2857 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.002 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 Cu1 Cu 0.5000 0.0000 0.5000 0.02571(13) Uani 1 2 d S . . C1 C 0.3461(5) -0.0968(3) 0.25422(16) 0.0285(5) Uani 1 1 d . . . C2 C 0.4047(4) 0.1876(3) 0.19382(14) 0.0239(5) Uani 1 1 d . . . H2A H 0.4891 0.1210 0.1458 0.029 Uiso 1 1 calc R . . H2B H 0.5173 0.1648 0.2325 0.029 Uiso 1 1 calc R . . C3 C 0.0513(4) 0.1264(3) 0.16959(13) 0.0254(5) Uani 1 1 d . . . H3A H -0.0417 0.2606 0.1612 0.031 Uiso 1 1 calc R . . H3B H -0.0526 0.0694 0.1948 0.031 Uiso 1 1 calc R . . C4 C 0.1509(4) 0.0369(4) 0.08889(14) 0.0318(5) Uani 1 1 d . . . H4A H 0.2600 -0.0934 0.0964 0.038 Uiso 1 1 calc R . . H4B H 0.2353 0.1059 0.0595 0.038 Uiso 1 1 calc R . . C5 C -0.0443(4) 0.0406(4) 0.04135(14) 0.0332(6) Uani 1 1 d . . . H5A H -0.1249 -0.0318 0.0704 0.040 Uiso 1 1 calc R . . H5B H -0.1564 0.1707 0.0363 0.040 Uiso 1 1 calc R . . N1 N 0.2327(3) 0.1059(3) 0.22622(11) 0.0210(4) Uani 1 1 d . . . O1 O 0.5967(3) -0.3474(2) 0.35844(9) 0.0291(4) Uani 1 1 d . . . O2 O 0.7907(3) -0.1552(2) 0.27594(11) 0.0367(4) Uani 1 1 d . . . H2C H 0.8810 -0.2653 0.2671 0.055 Uiso 1 1 calc R . . O3 O 0.4795(3) 0.0046(2) 0.38386(9) 0.0330(4) Uani 1 1 d . . . O4 O 0.1009(3) 0.5251(2) 0.24028(11) 0.0369(4) Uani 1 1 d . . . O5 O 0.1854(3) 0.4837(3) 0.08996(10) 0.0362(4) Uani 1 1 d . . . O6 O 0.4931(3) 0.4911(3) 0.17466(11) 0.0363(4) Uani 1 1 d . . . H6A H 0.5293 0.5283 0.1307 0.054 Uiso 1 1 calc R . . O7 O 0.5022(4) 0.2556(3) 0.48647(13) 0.0344(4) Uani 1 1 d . . . O8 O 0.2356(4) 0.5361(3) 0.39169(13) 0.0435(5) Uani 1 1 d . . . O9 O 0.7137(4) 0.6150(4) 0.06581(14) 0.0463(5) Uani 1 1 d . . . O10 O 0.8978(7) 0.2649(4) 0.35123(16) 0.0647(8) Uani 1 1 d . . . P1 P 0.56482(10) -0.15352(8) 0.32511(3) 0.02308(15) Uani 1 1 d . . . P2 P 0.27579(10) 0.44208(8) 0.17028(3) 0.02377(15) Uani 1 1 d . . . H1A H 0.410(5) -0.172(4) 0.2116(17) 0.033(7) Uiso 1 1 d . . . H1C H 0.160(5) 0.163(4) 0.2644(17) 0.026(7) Uiso 1 1 d . . . H1B H 0.228(5) -0.122(4) 0.2799(18) 0.040(8) Uiso 1 1 d . . . H9A H 0.856(9) 0.572(6) 0.083(3) 0.093(15) Uiso 1 1 d . . . H9B H 0.718(6) 0.586(5) 0.025(2) 0.040(10) Uiso 1 1 d . . . H8A H 0.191(7) 0.506(6) 0.362(3) 0.070(14) Uiso 1 1 d . . . H10B H 0.991(5) 0.299(5) 0.3543(19) 0.022(10) Uiso 1 1 d . . . O11 O 0.9249(4) -0.1524(4) 0.49059(17) 0.0563(6) Uani 1 1 d . . . H7A H 0.471(6) 0.302(4) 0.526(2) 0.042(9) Uiso 1 1 d . . . H7B H 0.420(6) 0.320(5) 0.455(2) 0.054(11) Uiso 1 1 d . . . H11A H 1.005(8) -0.248(7) 0.455(3) 0.085(14) Uiso 1 1 d . . . H10A H 0.825(12) 0.368(10) 0.350(4) 0.16(3) Uiso 1 1 d . . . H11B H 0.913(6) -0.087(5) 0.455(2) 0.039(11) Uiso 1 1 d . . . H8B H 0.391(15) 0.582(12) 0.368(5) 0.23(4) Uiso 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 Cu1 0.0339(2) 0.0227(2) 0.0213(2) -0.00043(15) -0.00450(16) -0.01149(17) C1 0.0346(14) 0.0219(12) 0.0310(12) 0.0037(10) -0.0115(11) -0.0117(10) C2 0.0205(11) 0.0203(11) 0.0287(11) 0.0008(9) -0.0035(9) -0.0057(9) C3 0.0222(11) 0.0276(12) 0.0267(11) 0.0012(9) -0.0079(9) -0.0088(9) C4 0.0302(13) 0.0377(14) 0.0276(12) -0.0046(10) -0.0080(10) -0.0117(11) C5 0.0303(13) 0.0412(14) 0.0290(13) -0.0058(11) -0.0087(10) -0.0129(11) N1 0.0208(9) 0.0203(9) 0.0208(9) -0.0028(8) -0.0035(8) -0.0061(8) O1 0.0331(9) 0.0218(8) 0.0289(8) 0.0021(7) -0.0051(7) -0.0070(7) O2 0.0254(9) 0.0238(9) 0.0527(11) 0.0028(8) 0.0040(8) -0.0036(7) O3 0.0452(10) 0.0253(9) 0.0229(8) -0.0022(7) -0.0080(7) -0.0068(8) O4 0.0346(10) 0.0301(9) 0.0354(9) -0.0053(8) 0.0036(8) -0.0027(8) O5 0.0367(10) 0.0407(10) 0.0310(9) 0.0075(8) -0.0121(8) -0.0139(8) O6 0.0399(10) 0.0379(10) 0.0402(10) 0.0058(8) -0.0110(8) -0.0241(8) O7 0.0504(12) 0.0298(10) 0.0256(9) 0.0014(8) -0.0080(9) -0.0178(9) O8 0.0495(13) 0.0446(12) 0.0389(11) 0.0012(9) -0.0134(10) -0.0191(10) O9 0.0365(12) 0.0668(15) 0.0362(12) 0.0015(11) -0.0020(9) -0.0219(11) O10 0.0658(19) 0.0461(15) 0.0533(15) 0.0012(11) 0.0142(13) 0.0028(15) P1 0.0243(3) 0.0197(3) 0.0223(3) -0.0003(2) -0.0049(2) -0.0049(2) P2 0.0235(3) 0.0205(3) 0.0253(3) -0.0002(2) -0.0042(2) -0.0062(2) O11 0.0396(13) 0.0592(16) 0.0630(16) -0.0130(15) -0.0003(12) -0.0115(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O7 1.9672(19) . ? Cu1 O7 1.9672(19) 2_656 ? Cu1 O3 1.9757(17) . ? Cu1 O3 1.9757(17) 2_656 ? Cu1 O11 2.434(3) . ? Cu1 O11 2.434(3) 2_656 ? C1 N1 1.500(3) . ? C1 P1 1.821(2) . ? C1 H1A 0.90(3) . ? C1 H1B 0.90(3) . ? C2 N1 1.492(3) . ? C2 P2 1.827(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.518(3) . ? C3 C4 1.519(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.525(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C5 1.520(5) 2 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N1 H1C 0.79(3) . ? O1 P1 1.5015(17) . ? O2 P1 1.5566(19) . ? O2 H2C 0.8200 . ? O3 P1 1.5042(18) . ? O4 P2 1.5028(19) . ? O5 P2 1.4931(18) . ? O6 P2 1.5612(18) . ? O6 H6A 0.8200 . ? O7 H7A 0.75(3) . ? O7 H7B 0.78(4) . ? O8 H8A 0.69(4) . ? O8 H8B 1.18(9) . ? O9 H9A 0.89(5) . ? O9 H9B 0.72(3) . ? O10 H10B 0.74(3) . ? O10 H10A 0.74(7) . ? O11 H11A 0.92(5) . ? O11 H11B 0.74(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 O7 Cu1 O7 180.0 . 2_656 ? O7 Cu1 O3 87.49(8) . . ? O7 Cu1 O3 92.51(8) 2_656 . ? O7 Cu1 O3 92.51(8) . 2_656 ? O7 Cu1 O3 87.49(8) 2_656 2_656 ? O3 Cu1 O3 180.0 . 2_656 ? O7 Cu1 O11 92.52(10) . . ? O7 Cu1 O11 87.48(10) 2_656 . ? O3 Cu1 O11 94.73(9) . . ? O3 Cu1 O11 85.27(9) 2_656 . ? O7 Cu1 O11 87.48(10) . 2_656 ? O7 Cu1 O11 92.52(10) 2_656 2_656 ? O3 Cu1 O11 85.27(9) . 2_656 ? O3 Cu1 O11 94.73(9) 2_656 2_656 ? O11 Cu1 O11 180.0 . 2_656 ? N1 C1 P1 117.80(16) . . ? N1 C1 H1A 109.5(17) . . ? P1 C1 H1A 108.5(17) . . ? N1 C1 H1B 104.1(19) . . ? P1 C1 H1B 106.0(19) . . ? H1A C1 H1B 111(3) . . ? N1 C2 P2 114.49(15) . . ? N1 C2 H2A 108.6 . . ? P2 C2 H2A 108.6 . . ? N1 C2 H2B 108.6 . . ? P2 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N1 C3 C4 114.82(19) . . ? N1 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? C3 C4 C5 110.6(2) . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C5 C5 C4 112.9(3) 2 . ? C5 C5 H5A 109.0 2 . ? C4 C5 H5A 109.0 . . ? C5 C5 H5B 109.0 2 . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C2 N1 C1 113.05(18) . . ? C2 N1 C3 113.67(17) . . ? C1 N1 C3 110.21(17) . . ? C2 N1 H1C 108.8(19) . . ? C1 N1 H1C 105.4(19) . . ? C3 N1 H1C 105.1(19) . . ? P1 O2 H2C 109.5 . . ? P1 O3 Cu1 131.02(10) . . ? P2 O6 H6A 109.5 . . ? Cu1 O7 H7A 109(2) . . ? Cu1 O7 H7B 114(3) . . ? H7A O7 H7B 111(4) . . ? H8A O8 H8B 114(5) . . ? H9A O9 H9B 112(4) . . ? H10B O10 H10A 82(6) . . ? O1 P1 O3 116.40(10) . . ? O1 P1 O2 111.62(10) . . ? O3 P1 O2 109.18(11) . . ? O1 P1 C1 105.41(11) . . ? O3 P1 C1 107.56(11) . . ? O2 P1 C1 106.01(12) . . ? O5 P2 O4 116.56(11) . . ? O5 P2 O6 112.70(10) . . ? O4 P2 O6 109.55(11) . . ? O5 P2 C2 112.47(11) . . ? O4 P2 C2 104.22(11) . . ? O6 P2 C2 99.74(10) . . ? Cu1 O11 H11A 121(3) . . ? Cu1 O11 H11B 82(3) . . ? H11A O11 H11B 85(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.316 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.065