# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1228 data_1 # (C4H12N2)[In2(C2O4)(HPO4)3].H2O _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H17 In2 N2 O17 P3' _chemical_formula_weight 711.77 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'In' 'In' -0.7276 1.3100 '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' 'H' 'H' 0.0000 0.0000 '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, y+1/2, -z' _cell_length_a 6.5052(2) _cell_length_b 17.5005(2) _cell_length_c 8.1811(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.6560(10) _cell_angle_gamma 90.00 _cell_volume 887.50(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3255 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description bladed _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12mm _exptl_crystal_size_mid 0.05mm _exptl_crystal_size_min 0.01mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.663 _exptl_crystal_density_method ? _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 2.966 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.956 _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 'Seimens Smart CCD' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5228 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.85 _reflns_number_total 3644 _reflns_number_observed 3151 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0504P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(4) _refine_ls_number_reflns 3644 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_obs 0.0435 _refine_ls_wR_factor_all 0.1012 _refine_ls_wR_factor_obs 0.0944 _refine_ls_goodness_of_fit_all 0.999 _refine_ls_goodness_of_fit_obs 1.008 _refine_ls_restrained_S_all 0.999 _refine_ls_restrained_S_obs 1.008 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group In1 In 0.25563(11) 0.0025 0.77951(8) 0.0102(2) Uani 1 d . . In2 In -0.11908(10) 0.14147(5) 0.12599(8) 0.0104(2) Uani 1 d . . P1 P -0.2639(4) 0.0474(2) 0.7570(3) 0.0094(6) Uani 1 d . . P2 P -0.6060(4) 0.0913(2) 0.1582(4) 0.0117(6) Uani 1 d . . P3 P 0.0705(4) -0.16326(14) 0.8707(3) 0.0122(5) Uani 1 d . . O1 O -0.4482(11) -0.0117(4) 0.7273(9) 0.013(2) Uani 1 d . . O2 O -0.0468(10) 0.0066(6) 0.8324(8) 0.0156(15) Uani 1 d . . O3 O -0.2919(11) 0.1127(4) 0.8717(8) 0.0129(15) Uani 1 d . . O4 O -0.2707(12) 0.0824(4) 0.5814(9) 0.016(2) Uani 1 d . . O5 O -0.5934(11) 0.0282(4) 0.0322(9) 0.014(2) Uani 1 d . . O6 O -0.5809(11) 0.0526(4) 0.3331(8) 0.015(2) Uani 1 d . . O7 O -0.8132(10) 0.1367(5) 0.0928(8) 0.0150(15) Uani 1 d . . O8 O -0.4222(11) 0.1493(5) 0.1763(8) 0.015(2) Uani 1 d . . O9 O 0.2383(11) -0.1191(4) 0.8151(9) 0.016(2) Uani 1 d . . O10 O -0.1386(12) -0.1703(4) 0.7225(9) 0.022(2) Uani 1 d . . O11 O 0.0172(15) -0.1193(5) 1.0212(10) 0.022(2) Uani 1 d . . O12 O 0.1618(12) -0.2402(4) 0.9470(9) 0.015(2) Uani 1 d . . O13 O 0.2115(11) 0.1145(4) 0.6509(9) 0.0121(15) Uani 1 d . . O14 O 0.0451(12) 0.1702(4) 0.4014(9) 0.016(2) Uani 1 d . . O15 O 0.0818(12) -0.0245(4) 0.5083(9) 0.015(2) Uani 1 d . . O16 O -0.0731(12) 0.0307(4) 0.2562(8) 0.016(2) Uani 1 d . . C1 C 0.1028(16) 0.1133(6) 0.4952(13) 0.011(2) Uani 1 d . . C2 C 0.0322(16) 0.0334(6) 0.4121(14) 0.014(2) Uani 1 d . . N1 N -0.4315(20) -0.0998(6) 0.3943(14) 0.040(3) Uani 1 d . . N2 N -0.4678(17) -0.2531(5) 0.2523(12) 0.027(2) Uani 1 d . . C3 C -0.6175(21) -0.1517(8) 0.3977(17) 0.038(3) Uani 1 d . . C4 C -0.5506(21) -0.2349(6) 0.4000(15) 0.026(3) Uani 1 d . . C5 C -0.2769(21) -0.2040(7) 0.2605(16) 0.033(3) Uani 1 d . . C6 C -0.3457(24) -0.1190(8) 0.2491(17) 0.039(3) Uani 1 d . . OW1 O -0.4366(14) -0.2103(5) 0.8276(13) 0.042(2) Uani 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 In1 0.0097(3) 0.0097(3) 0.0107(3) 0.0010(3) 0.0023(3) 0.0000(3) In2 0.0097(3) 0.0106(3) 0.0102(3) 0.0005(3) 0.0018(3) 0.0003(3) P1 0.0082(13) 0.0106(14) 0.0087(12) 0.0003(10) 0.0013(10) 0.0022(10) P2 0.0114(13) 0.0130(13) 0.0109(13) -0.0008(11) 0.0038(10) -0.0024(10) P3 0.0132(13) 0.0089(12) 0.0146(12) 0.0037(10) 0.0044(10) 0.0028(10) O1 0.011(3) 0.009(5) 0.020(4) -0.007(3) 0.006(3) -0.005(3) O2 0.009(3) 0.020(4) 0.016(3) 0.005(4) 0.001(3) 0.000(4) O3 0.013(4) 0.013(3) 0.010(3) -0.006(3) -0.001(3) -0.001(3) O4 0.016(4) 0.018(4) 0.013(4) 0.005(3) 0.003(3) -0.001(3) O5 0.011(4) 0.016(4) 0.013(4) -0.003(3) 0.001(3) 0.002(3) O6 0.021(4) 0.018(4) 0.005(3) 0.002(3) 0.002(3) -0.007(3) O7 0.015(3) 0.015(4) 0.015(3) 0.005(4) 0.004(3) 0.003(4) O8 0.015(3) 0.014(4) 0.017(4) 0.004(4) 0.007(3) 0.000(4) O9 0.017(4) 0.008(3) 0.022(4) 0.000(3) 0.006(3) 0.000(3) O10 0.025(4) 0.018(4) 0.020(4) 0.000(3) 0.005(3) 0.005(3) O11 0.036(5) 0.018(4) 0.017(4) 0.004(3) 0.014(4) 0.007(4) O12 0.017(4) 0.010(4) 0.016(4) 0.008(3) 0.000(3) 0.004(3) O13 0.011(3) 0.010(3) 0.013(4) 0.004(3) 0.001(3) 0.000(3) O14 0.017(4) 0.013(4) 0.013(4) -0.007(3) -0.005(3) -0.006(3) O15 0.022(4) 0.008(3) 0.015(4) 0.003(3) 0.004(3) -0.002(3) O16 0.021(4) 0.016(4) 0.008(3) 0.002(3) -0.001(3) -0.002(3) C1 0.011(5) 0.015(5) 0.009(5) 0.000(4) 0.006(4) 0.001(4) C2 0.009(5) 0.017(5) 0.015(5) -0.007(5) 0.001(4) 0.002(4) N1 0.058(8) 0.015(5) 0.038(7) -0.007(5) 0.002(6) 0.007(5) N2 0.036(6) 0.020(5) 0.024(5) -0.003(4) 0.005(4) 0.002(5) C3 0.038(8) 0.038(8) 0.035(7) -0.006(6) 0.008(6) 0.005(6) C4 0.039(7) 0.009(5) 0.028(6) -0.005(5) 0.010(5) -0.001(5) C5 0.034(7) 0.027(7) 0.033(7) 0.004(5) 0.004(6) -0.006(6) C6 0.055(9) 0.029(7) 0.027(7) 0.004(6) 0.006(6) -0.014(7) OW1 0.031(5) 0.026(5) 0.083(7) 0.008(5) 0.036(5) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 O5 2.052(7) 1_656 ? In1 O1 2.111(7) 1_655 ? In1 O2 2.140(6) . ? In1 O9 2.155(7) . ? In1 O13 2.201(7) . ? In1 O15 2.214(7) . ? In2 O7 2.089(6) 1_655 ? In2 O3 2.104(6) 1_554 ? In2 O8 2.137(7) . ? In2 O12 2.150(7) 2_556 ? In2 O16 2.188(7) . ? In2 O14 2.239(7) . ? P1 O3 1.524(7) . ? P1 O2 1.535(8) . ? P1 O1 1.546(7) . ? P1 O4 1.550(7) . ? P2 O7 1.517(8) . ? P2 O5 1.529(7) . ? P2 O8 1.541(8) . ? P2 O6 1.546(7) . ? P3 O9 1.516(7) . ? P3 O12 1.527(7) . ? P3 O10 1.528(7) . ? P3 O11 1.577(8) . ? O1 In1 2.111(7) 1_455 ? O3 In2 2.104(6) 1_556 ? O5 In1 2.052(7) 1_454 ? O7 In2 2.089(6) 1_455 ? O12 In2 2.150(7) 2_546 ? O13 C1 1.255(12) . ? O14 C1 1.243(11) . ? O15 C2 1.264(12) . ? O16 C2 1.252(12) . ? C1 C2 1.561(12) . ? N1 C6 1.50(2) . ? N1 C3 1.52(2) . ? N2 C5 1.50(2) . ? N2 C4 1.498(15) . ? C3 C4 1.52(2) . ? C5 C6 1.55(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 O5 In1 O1 92.4(3) 1_656 1_655 ? O5 In1 O2 88.7(3) 1_656 . ? O1 In1 O2 175.1(4) 1_655 . ? O5 In1 O9 96.2(3) 1_656 . ? O1 In1 O9 90.0(3) 1_655 . ? O2 In1 O9 85.2(3) . . ? O5 In1 O13 103.9(3) 1_656 . ? O1 In1 O13 90.2(3) 1_655 . ? O2 In1 O13 94.2(3) . . ? O9 In1 O13 159.8(3) . . ? O5 In1 O15 178.0(3) 1_656 . ? O1 In1 O15 89.5(3) 1_655 . ? O2 In1 O15 89.3(3) . . ? O9 In1 O15 83.8(3) . . ? O13 In1 O15 76.0(2) . . ? O7 In2 O3 96.1(3) 1_655 1_554 ? O7 In2 O8 176.2(3) 1_655 . ? O3 In2 O8 87.6(3) 1_554 . ? O7 In2 O12 92.9(3) 1_655 2_556 ? O3 In2 O12 88.3(3) 1_554 2_556 ? O8 In2 O12 86.7(3) . 2_556 ? O7 In2 O16 91.9(3) 1_655 . ? O3 In2 O16 102.8(3) 1_554 . ? O8 In2 O16 87.8(3) . . ? O12 In2 O16 167.3(3) 2_556 . ? O7 In2 O14 87.5(3) 1_655 . ? O3 In2 O14 176.2(3) 1_554 . ? O8 In2 O14 88.7(3) . . ? O12 In2 O14 92.6(3) 2_556 . ? O16 In2 O14 75.9(3) . . ? O3 P1 O2 111.6(4) . . ? O3 P1 O1 111.5(4) . . ? O2 P1 O1 109.1(5) . . ? O3 P1 O4 107.4(4) . . ? O2 P1 O4 108.7(4) . . ? O1 P1 O4 108.4(4) . . ? O7 P2 O5 111.4(4) . . ? O7 P2 O8 105.6(5) . . ? O5 P2 O8 110.0(4) . . ? O7 P2 O6 112.9(4) . . ? O5 P2 O6 107.2(4) . . ? O8 P2 O6 109.8(4) . . ? O9 P3 O12 110.2(4) . . ? O9 P3 O10 110.6(4) . . ? O12 P3 O10 113.3(4) . . ? O9 P3 O11 109.5(4) . . ? O12 P3 O11 105.2(4) . . ? O10 P3 O11 107.8(4) . . ? P1 O1 In1 127.0(4) . 1_455 ? P1 O2 In1 136.4(5) . . ? P1 O3 In2 131.4(4) . 1_556 ? P2 O5 In1 136.9(4) . 1_454 ? P2 O7 In2 139.0(5) . 1_455 ? P2 O8 In2 132.3(5) . . ? P3 O9 In1 128.0(4) . . ? P3 O12 In2 137.3(4) . 2_546 ? C1 O13 In1 115.0(6) . . ? C1 O14 In2 113.8(6) . . ? C2 O15 In1 114.1(6) . . ? C2 O16 In2 114.4(7) . . ? O14 C1 O13 125.8(9) . . ? O14 C1 C2 117.0(8) . . ? O13 C1 C2 117.2(8) . . ? O16 C2 O15 124.1(9) . . ? O16 C2 C1 118.4(8) . . ? O15 C2 C1 117.5(8) . . ? C6 N1 C3 111.8(10) . . ? C5 N2 C4 109.8(9) . . ? C4 C3 N1 110.3(10) . . ? N2 C4 C3 111.4(10) . . ? N2 C5 C6 109.2(11) . . ? N1 C6 C5 109.8(10) . . ? _refine_diff_density_max 0.904 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.189