data_compoundI _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Indiumphosphiteoxalate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H23 In N3 O13 P S0' _chemical_formula_weight 539.10 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' 'S' 'S' 0.1246 0.1234 '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' _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 9.7495(16) _cell_length_b 10.0012(16) _cell_length_c 10.3398(17) _cell_angle_alpha 93.078(3) _cell_angle_beta 104.573(2) _cell_angle_gamma 96.886(2) _cell_volume 965.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4471 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 28.04 _exptl_crystal_description plate-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type ‘Multi-scan’ _exptl_absorpt_correction_T_min 0.8096 _exptl_absorpt_correction_T_max 0.8745 _exptl_absorpt_process_details ‘(SADABS;Sheldrick,1996)’ _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 ‘BrukerSMARTCCDareadetector’ _diffrn_measurement_method ‘\fand\wscans’ _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11279 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.04 _reflns_number_total 4471 _reflns_number_gt 4180 _reflns_threshold_expression >2sigma(I) _computing_data_collection ‘SMART(Bruker,2000)’ _computing_cell_refinement ‘SMART’ _computing_data_reduction ‘SAINT(Bruker,2000)’ _computing_structure_solution ‘SIR92(Altomareetal.,1993)’ _computing_structure_refinement 'SHELXL-97(Sheldrick,1997)' _computing_molecular_graphics ‘Ortep-3forWindows(Farrugia,1997)andCAMERON _computing_publication_material ‘PLATON(Spek,1990)’ _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^)+(0.0447P)^2^+1.8513P] 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 4471 _refine_ls_number_parameters 269 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.004 _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 In1 In 0.14889(2) 0.12991(2) 0.69877(2) 0.02068(8) Uani 1 1 d . . . P1 P 0.11493(9) -0.18655(8) 0.56040(8) 0.02313(17) Uani 1 1 d . . . H1 H 0.0936 -0.2067 0.6456 0.028 Uiso 1 1 calc R . . O1 O 0.0235(3) 0.2280(2) 0.5484(3) 0.0354(6) Uani 1 1 d . . . O2 O 0.1665(3) -0.0357(2) 0.5727(3) 0.0308(5) Uani 1 1 d . . . O3 O 0.3498(3) 0.2272(2) 0.6810(3) 0.0305(5) Uani 1 1 d . . . O4 O -0.0294(2) 0.0385(3) 0.7655(2) 0.0283(5) Uani 1 1 d . . . O5 O 0.2507(2) 0.0272(3) 0.8712(2) 0.0286(5) Uani 1 1 d . . . O6 O 0.1858(3) 0.3167(2) 0.8302(3) 0.0331(6) Uani 1 1 d . . . O7 O 0.2299(3) -0.2696(3) 0.5450(3) 0.0345(6) Uani 1 1 d . . . O8 O 0.1992(3) -0.1374(2) 0.9942(3) 0.0304(5) Uani 1 1 d . . . O9 O -0.0876(2) -0.1212(2) 0.8908(2) 0.0271(5) Uani 1 1 d . . . O10 O 0.4957(3) 0.4211(3) 0.7288(3) 0.0437(7) Uani 1 1 d . . . O11 O 0.3126(4) 0.5213(3) 0.8604(4) 0.0540(9) Uani 1 1 d . . . C1 C 0.1637(3) -0.0543(3) 0.9118(3) 0.0215(6) Uani 1 1 d . . . C2 C 0.0015(3) -0.0463(3) 0.8526(3) 0.0217(6) Uani 1 1 d . . . C3 C 0.2886(4) 0.4040(4) 0.8170(4) 0.0307(7) Uani 1 1 d . . . C4 C 0.3875(4) 0.3479(4) 0.7353(4) 0.0295(7) Uani 1 1 d . . . C14 C 0.4790(3) 0.7017(3) 0.7269(3) 0.0257(6) Uani 1 1 d . . . H14A H 0.3894 0.7133 0.6644 0.031 Uiso 1 1 calc R . . H14B H 0.4698 0.6103 0.7537 0.031 Uiso 1 1 calc R . . C10 C 0.9813(3) 0.3556(3) 0.9747(3) 0.0214(6) Uani 1 1 d . . . H10A H 1.0636 0.3423 0.9414 0.026 Uiso 1 1 calc R . . H10B H 0.9276 0.2676 0.9754 0.026 Uiso 1 1 calc R . . C12 C 0.6495(3) 0.9588(3) 0.7464(3) 0.0206(6) Uani 1 1 d . . . H12A H 0.7363 0.9431 0.8104 0.025 Uiso 1 1 calc R . . H12B H 0.6633 1.0510 0.7224 0.025 Uiso 1 1 calc R . . N2 N 0.5290(4) 0.9417(4) 0.8091(4) 0.0460(9) Uani 1 1 d . . . H2A H 0.4492 0.9605 0.7515 0.055 Uiso 1 1 calc R . . H2B H 0.5481 0.9999 0.8829 0.055 Uiso 1 1 calc R . . C11 C 1.0305(5) 0.4225(4) 1.1134(4) 0.0377(8) Uani 1 1 d . . . H11A H 1.0932 0.3684 1.1700 0.045 Uiso 1 1 calc R . . H11B H 0.9487 0.4289 1.1496 0.045 Uiso 1 1 calc R . . N3 N 0.5959(4) 0.7201(4) 0.6584(5) 0.0601(11) Uani 1 1 d . . . H3A H 0.5723 0.6644 0.5825 0.072 Uiso 1 1 calc R . . H3B H 0.6765 0.6977 0.7119 0.072 Uiso 1 1 calc R . . C13 C 0.6230(5) 0.8640(4) 0.6247(4) 0.0400(9) Uani 1 1 d . . . H13A H 0.7054 0.8750 0.5877 0.048 Uiso 1 1 calc R . . H13B H 0.5408 0.8845 0.5576 0.048 Uiso 1 1 calc R . . N1 N 0.8907(4) 0.4380(4) 0.8856(4) 0.0541(10) Uani 1 1 d . . . H1A H 0.8108 0.4446 0.9126 0.065 Uiso 1 1 calc R . . H1B H 0.8648 0.3976 0.8015 0.065 Uiso 1 1 calc R . . C15 C 0.5050(4) 0.7989(4) 0.8469(4) 0.0385(9) Uani 1 1 d . . . H15A H 0.5884 0.7809 0.9142 0.046 Uiso 1 1 calc R . . H15B H 0.4234 0.7879 0.8848 0.046 Uiso 1 1 calc R . . O100 O 0.3389(4) 0.7888(3) 0.3338(3) 0.0465(7) Uani 1 1 d D . . O200 O 0.1796(6) 0.4504(4) 0.4438(5) 0.0766(13) Uani 1 1 d D . . H101 H 0.282(4) 0.761(5) 0.380(4) 0.043(13) Uiso 1 1 d D . . H102 H 0.405(4) 0.746(5) 0.322(6) 0.067(18) Uiso 1 1 d D . . H201 H 0.204(6) 0.453(6) 0.5287(13) 0.056(17) Uiso 1 1 d D . . H202 H 0.166(14) 0.532(4) 0.457(13) 0.22(6) Uiso 1 1 d 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 0.02005(12) 0.01856(12) 0.02449(13) 0.00226(8) 0.00816(8) 0.00165(8) P1 0.0250(4) 0.0201(4) 0.0250(4) 0.0030(3) 0.0070(3) 0.0042(3) O1 0.0311(13) 0.0245(12) 0.0444(15) 0.0098(11) -0.0019(11) 0.0016(10) O2 0.0378(13) 0.0216(11) 0.0347(13) -0.0022(10) 0.0147(11) 0.0009(10) O3 0.0277(12) 0.0248(12) 0.0431(14) -0.0014(10) 0.0187(11) 0.0008(10) O4 0.0189(11) 0.0350(13) 0.0339(12) 0.0131(10) 0.0094(9) 0.0059(9) O5 0.0192(11) 0.0357(13) 0.0316(12) 0.0107(10) 0.0071(9) 0.0018(9) O6 0.0362(13) 0.0252(12) 0.0430(14) -0.0053(10) 0.0242(12) -0.0018(10) O7 0.0315(13) 0.0281(12) 0.0448(15) 0.0024(11) 0.0087(11) 0.0108(10) O8 0.0257(12) 0.0293(12) 0.0351(13) 0.0111(10) 0.0045(10) 0.0025(10) O9 0.0221(11) 0.0266(11) 0.0344(12) 0.0057(10) 0.0117(10) 0.0000(9) O10 0.0324(14) 0.0282(13) 0.075(2) -0.0019(13) 0.0285(14) -0.0067(11) O11 0.061(2) 0.0276(14) 0.080(2) -0.0164(15) 0.0426(18) -0.0100(13) C1 0.0203(14) 0.0219(14) 0.0214(14) -0.0005(11) 0.0049(11) 0.0015(11) C2 0.0214(14) 0.0220(14) 0.0227(14) -0.0004(11) 0.0081(12) 0.0029(12) C3 0.0303(17) 0.0277(17) 0.0354(18) -0.0031(14) 0.0142(14) -0.0005(14) C4 0.0257(16) 0.0267(16) 0.0383(18) 0.0024(14) 0.0129(14) 0.0032(13) C14 0.0192(14) 0.0179(14) 0.0365(17) 0.0045(13) 0.0017(13) -0.0003(11) C10 0.0267(15) 0.0115(12) 0.0292(15) 0.0010(11) 0.0142(12) 0.0003(11) C12 0.0133(12) 0.0229(14) 0.0236(14) 0.0000(11) 0.0036(11) -0.0020(11) N2 0.0329(17) 0.046(2) 0.058(2) -0.0091(17) 0.0165(16) -0.0001(15) C11 0.052(2) 0.0302(18) 0.0318(18) 0.0075(15) 0.0107(17) 0.0090(17) N3 0.046(2) 0.053(2) 0.079(3) -0.017(2) 0.016(2) 0.0063(19) C13 0.040(2) 0.046(2) 0.0329(19) -0.0058(17) 0.0129(16) -0.0047(17) N1 0.052(2) 0.046(2) 0.054(2) -0.0029(18) -0.0001(18) -0.0020(18) C15 0.0351(19) 0.044(2) 0.0349(19) 0.0044(16) 0.0107(16) -0.0064(17) O100 0.0490(18) 0.0410(16) 0.062(2) 0.0105(14) 0.0317(16) 0.0141(14) O200 0.107(4) 0.046(2) 0.090(3) -0.004(2) 0.055(3) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 O1 2.091(2) . ? In1 O2 2.103(2) . ? In1 O3 2.136(2) . ? In1 O4 2.151(2) . ? In1 O5 2.184(2) . ? In1 O6 2.188(2) . ? P1 O7 1.507(3) . ? P1 O1 1.520(3) 2_556 ? P1 O2 1.520(2) . ? O1 P1 1.520(3) 2_556 ? O3 C4 1.274(4) . ? O4 C2 1.276(4) . ? O5 C1 1.269(4) . ? O6 C3 1.287(4) . ? O8 C1 1.238(4) . ? O9 C2 1.233(4) . ? O10 C4 1.229(4) . ? O11 C3 1.207(4) . ? C1 C2 1.558(4) . ? C3 C4 1.564(5) . ? C14 C15 1.484(5) . ? C14 N3 1.485(5) . ? C10 N1 1.468(5) . ? C10 C11 1.486(5) . ? C12 N2 1.475(4) . ? C12 C13 1.482(5) . ? N2 C15 1.508(5) . ? C11 N1 1.508(5) 2_767 ? N3 C13 1.507(6) . ? N1 C11 1.508(5) 2_767 ? 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 In1 O2 96.19(11) . . ? O1 In1 O3 95.68(10) . . ? O2 In1 O3 89.56(9) . . ? O1 In1 O4 94.52(10) . . ? O2 In1 O4 97.80(10) . . ? O3 In1 O4 166.71(10) . . ? O1 In1 O5 170.57(10) . . ? O2 In1 O5 88.75(10) . . ? O3 In1 O5 92.37(9) . . ? O4 In1 O5 76.82(9) . . ? O1 In1 O6 88.06(11) . . ? O2 In1 O6 165.82(10) . . ? O3 In1 O6 76.53(9) . . ? O4 In1 O6 95.34(9) . . ? O5 In1 O6 89.05(10) . . ? O7 P1 O1 112.02(16) . 2_556 ? O7 P1 O2 112.03(15) . . ? O1 P1 O2 112.88(14) 2_556 . ? P1 O1 In1 134.87(15) 2_556 . ? P1 O2 In1 134.33(15) . . ? C4 O3 In1 115.9(2) . . ? C2 O4 In1 114.66(19) . . ? C1 O5 In1 113.7(2) . . ? C3 O6 In1 114.4(2) . . ? O8 C1 O5 124.6(3) . . ? O8 C1 C2 119.0(3) . . ? O5 C1 C2 116.4(3) . . ? O9 C2 O4 124.4(3) . . ? O9 C2 C1 119.1(3) . . ? O4 C2 C1 116.5(3) . . ? O11 C3 O6 126.0(3) . . ? O11 C3 C4 119.3(3) . . ? O6 C3 C4 114.6(3) . . ? O10 C4 O3 124.6(3) . . ? O10 C4 C3 118.6(3) . . ? O3 C4 C3 116.8(3) . . ? C15 C14 N3 112.2(3) . . ? N1 C10 C11 110.7(3) . . ? N2 C12 C13 111.4(3) . . ? C12 N2 C15 110.3(3) . . ? C10 C11 N1 110.6(3) . 2_767 ? C14 N3 C13 111.3(3) . . ? C12 C13 N3 110.4(3) . . ? C10 N1 C11 110.7(3) . 2_767 ? C14 C15 N2 110.1(3) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.829 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.117 ####EOF##### data_compoundII _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Indiumoxalatephosphite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 F0 In N O5 P S0' _chemical_formula_weight 317.91 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' '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' 'F' 'F' 0.0171 0.0103 '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' 'S' 'S' 0.1246 0.1234 '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' _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 8.9931(18) _cell_length_b 9.2163(18) _cell_length_c 11.988(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.907(3) _cell_angle_gamma 90.00 _cell_volume 986.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2291 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.98 _exptl_crystal_description hexagon _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 2.553 _exptl_absorpt_correction_type ‘Multi-scan’ _exptl_absorpt_correction_T_min 0.6855 _exptl_absorpt_correction_T_max 0.8218 _exptl_absorpt_process_details ‘(SADABS;Sheldrick,1996)’ _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 ‘BrukerSMARTCCDareadetector’ _diffrn_measurement_method ‘\fand\wscans’ _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8253 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.98 _reflns_number_total 2291 _reflns_number_gt 1946 _reflns_threshold_expression >2sigma(I) _computing_data_collection ‘SMART(Bruker,2000)’ _computing_cell_refinement ‘SMART’ _computing_data_reduction ‘SAINT(Bruker,2000)’ _computing_structure_solution ‘SIR92(Altomareetal.,1993)’ _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^)+(0.0398P)^2^+4.5394P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2291 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 In1 In 0.09874(4) 0.23415(4) 0.60503(3) 0.02812(13) Uani 1 1 d . . . P1 P -0.03078(15) -0.09327(14) 0.65279(11) 0.0279(3) Uani 1 1 d . . . H10 H 0.0670 -0.1404 0.6538 0.034 Uiso 1 1 calc R . . O1 O 0.1079(7) 0.3473(7) 0.7534(5) 0.086(2) Uani 1 1 d . . . O2 O -0.0075(6) 0.0650(5) 0.6770(5) 0.0740(17) Uani 1 1 d . . . O3 O 0.1194(5) 0.1185(7) 0.4583(4) 0.0701(16) Uani 1 1 d . . . O4 O -0.1053(4) 0.3519(4) 0.5390(4) 0.0441(10) Uani 1 1 d . . . O5 O 0.1837(4) 0.4329(5) 0.5302(4) 0.0496(11) Uani 1 1 d . . . N1 N 0.3353(5) 0.1712(6) 0.6628(4) 0.0396(11) Uani 1 1 d . . . C10 C -0.0840(6) 0.4772(6) 0.5027(5) 0.0394(13) Uani 1 1 d . . . C5 C 0.4392(8) 0.1765(10) 0.5938(7) 0.067(2) Uani 1 1 d . . . H5 H 0.4103 0.1978 0.5185 0.080 Uiso 1 1 calc R . . C1 C 0.3769(9) 0.1355(10) 0.7696(6) 0.072(2) Uani 1 1 d . . . H1 H 0.3047 0.1306 0.8189 0.086 Uiso 1 1 calc R . . C2 C 0.5240(11) 0.1056(13) 0.8091(8) 0.098(4) Uani 1 1 d . . . H2 H 0.5499 0.0785 0.8836 0.118 Uiso 1 1 calc R . . C3 C 0.6313(10) 0.1159(11) 0.7384(9) 0.088(3) Uani 1 1 d . . . H3 H 0.7314 0.0989 0.7645 0.105 Uiso 1 1 calc R . . C4 C 0.5895(9) 0.1516(13) 0.6292(9) 0.092(3) Uani 1 1 d . . . H4 H 0.6604 0.1592 0.5791 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0362(2) 0.0259(2) 0.0232(2) -0.00655(13) 0.00773(14) -0.00568(14) P1 0.0336(7) 0.0265(6) 0.0234(6) 0.0032(5) 0.0022(5) -0.0031(5) O1 0.093(4) 0.108(5) 0.060(3) -0.055(3) 0.025(3) -0.007(4) O2 0.076(3) 0.038(3) 0.119(5) -0.007(3) 0.055(3) -0.018(2) O3 0.048(3) 0.123(5) 0.040(3) -0.041(3) 0.008(2) -0.003(3) O4 0.033(2) 0.036(2) 0.063(3) 0.0105(19) 0.0037(18) -0.0114(17) O5 0.029(2) 0.048(3) 0.070(3) 0.024(2) -0.0022(19) -0.0090(18) N1 0.039(3) 0.044(3) 0.036(3) 0.002(2) 0.004(2) 0.004(2) C10 0.033(3) 0.039(3) 0.046(3) 0.008(3) 0.001(2) -0.011(2) C5 0.052(4) 0.097(6) 0.053(4) 0.020(4) 0.014(3) 0.014(4) C1 0.060(5) 0.113(7) 0.040(4) 0.012(4) 0.001(3) 0.025(5) C2 0.081(6) 0.147(10) 0.061(5) 0.006(6) -0.016(5) 0.050(7) C3 0.056(5) 0.111(8) 0.092(7) -0.010(6) -0.010(5) 0.035(5) C4 0.049(5) 0.132(9) 0.099(7) 0.027(7) 0.026(5) 0.027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 O1 2.055(5) . ? In1 O2 2.071(4) . ? In1 O3 2.084(4) . ? In1 O4 2.196(4) . ? In1 O5 2.215(4) . ? In1 N1 2.233(5) . ? P1 O3 1.486(5) 3_556 ? P1 O1 1.494(5) 2_546 ? P1 O2 1.497(5) . ? O1 P1 1.494(5) 2_556 ? O3 P1 1.486(5) 3_556 ? O4 C10 1.257(7) . ? O5 C10 1.249(7) 3_566 ? N1 C5 1.321(8) . ? N1 C1 1.332(8) . ? C10 O5 1.249(7) 3_566 ? C10 C10 1.577(10) 3_566 ? C5 C4 1.386(10) . ? C1 C2 1.379(11) . ? C2 C3 1.362(13) . ? C3 C4 1.359(13) . ? 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 In1 O2 89.6(2) . . ? O1 In1 O3 172.6(2) . . ? O2 In1 O3 93.4(2) . . ? O1 In1 O4 90.3(2) . . ? O2 In1 O4 96.57(19) . . ? O3 In1 O4 95.98(19) . . ? O1 In1 O5 87.2(2) . . ? O2 In1 O5 171.97(18) . . ? O3 In1 O5 90.6(2) . . ? O4 In1 O5 76.09(14) . . ? O1 In1 N1 85.8(2) . . ? O2 In1 N1 98.4(2) . . ? O3 In1 N1 87.15(18) . . ? O4 In1 N1 164.54(16) . . ? O5 In1 N1 88.76(17) . . ? O3 P1 O1 111.7(3) 3_556 2_546 ? O3 P1 O2 112.0(4) 3_556 . ? O1 P1 O2 106.1(4) 2_546 . ? P1 O1 In1 149.7(4) 2_556 . ? P1 O2 In1 135.5(3) . . ? P1 O3 In1 138.1(3) 3_556 . ? C10 O4 In1 115.0(3) . . ? C10 O5 In1 114.0(3) 3_566 . ? C5 N1 C1 118.3(6) . . ? C5 N1 In1 121.0(4) . . ? C1 N1 In1 120.6(4) . . ? O5 C10 O4 125.8(5) 3_566 . ? O5 C10 C10 117.7(6) 3_566 3_566 ? O4 C10 C10 116.5(6) . 3_566 ? N1 C5 C4 122.6(7) . . ? N1 C1 C2 121.8(8) . . ? C3 C2 C1 119.7(8) . . ? C4 C3 C2 118.8(8) . . ? C3 C4 C5 118.8(8) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.704 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.142 #####EOF##### data_compoundIII _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Indiumphosphiteoxalate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 F0 In N O5 P S0' _chemical_formula_weight 317.91 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' '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' 'F' 'F' 0.0171 0.0103 '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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.7198(18) _cell_length_b 6.5947(11) _cell_length_c 13.771(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.104(3) _cell_angle_gamma 90.00 _cell_volume 939.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2210 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.99 _exptl_crystal_description plate-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 2.679 _exptl_absorpt_correction_type ‘Multi-scan’ _exptl_absorpt_correction_T_min 0.5657 _exptl_absorpt_correction_T_max 0.8142 _exptl_absorpt_process_details SADABS;Sheldrick1996 _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 ‘BrukerSMARTCCDareadetector’ _diffrn_measurement_method ‘\fand\wscans’ _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7835 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.99 _reflns_number_total 2210 _reflns_number_gt 1771 _reflns_threshold_expression >2sigma(I) _computing_data_collection ‘SMART(Bruker,2000)’ _computing_cell_refinement ‘SMART’ _computing_data_reduction ‘SAINT(Bruker,2000)’ _computing_structure_solution ‘SIR92(Altomareetal,1993)’ _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^)+(0.0262P)^2^+0.0491P] 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 2210 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.57659(2) 0.04968(4) 0.21367(2) 0.02271(10) Uani 1 1 d . . . P1 P 0.60698(9) 0.55810(15) 0.17066(8) 0.0250(2) Uani 1 1 d . . . H10 H 0.5638 0.5756 0.0991 0.030 Uiso 1 1 calc R . . O1 O 0.7511(3) 0.0592(5) 0.3224(2) 0.0390(7) Uani 1 1 d . . . O2 O 0.5562(3) 0.3638(5) 0.2007(3) 0.0503(9) Uani 1 1 d . . . O3 O 0.5627(3) -0.2672(4) 0.2233(2) 0.0413(8) Uani 1 1 d . . . O4 O 0.6551(2) 0.0289(4) 0.0813(2) 0.0303(6) Uani 1 1 d . . . O5 O 0.4028(2) 0.0271(4) 0.0838(2) 0.0311(7) Uani 1 1 d . . . N1 N 0.4493(3) 0.0710(5) 0.3182(3) 0.0310(8) Uani 1 1 d . . . C1 C 0.3675(5) -0.0769(9) 0.3250(4) 0.0534(14) Uani 1 1 d . . . H1 H 0.360(4) -0.184(7) 0.279(3) 0.056(16) Uiso 1 1 d . . . C2 C 0.4540(6) 0.2329(8) 0.3768(4) 0.0555(14) Uani 1 1 d . . . H2 H 0.524(5) 0.342(9) 0.376(4) 0.10(2) Uiso 1 1 d . . . C3 C 0.2900(6) -0.0644(11) 0.3904(5) 0.072(2) Uani 1 1 d . . . H3 H 0.230(6) -0.165(10) 0.387(5) 0.11(2) Uiso 1 1 d . . . C4 C 0.2966(6) 0.1000(10) 0.4519(5) 0.0654(18) Uani 1 1 d . . . H4 H 0.244(5) 0.108(8) 0.499(4) 0.081(19) Uiso 1 1 d . . . C5 C 0.3791(7) 0.2511(10) 0.4439(4) 0.0700(18) Uani 1 1 d . . . H5 H 0.401(7) 0.370(11) 0.490(5) 0.13(3) Uiso 1 1 d . . . C10 C 0.5733(4) 0.0014(5) -0.0006(3) 0.0248(9) 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 In1 0.02609(15) 0.01199(15) 0.03380(17) -0.00062(13) 0.01451(11) -0.00035(12) P1 0.0267(5) 0.0146(5) 0.0331(6) -0.0004(5) 0.0071(4) -0.0008(4) O1 0.0268(14) 0.052(2) 0.0402(17) -0.0031(15) 0.0128(13) -0.0011(14) O2 0.056(2) 0.0134(15) 0.092(3) 0.0015(17) 0.0382(19) -0.0006(14) O3 0.0553(19) 0.0118(14) 0.068(2) -0.0015(14) 0.0364(17) 0.0010(13) O4 0.0251(14) 0.0346(17) 0.0341(16) 0.0018(13) 0.0129(12) -0.0024(12) O5 0.0248(14) 0.0386(18) 0.0341(16) -0.0011(13) 0.0153(12) 0.0010(12) N1 0.0290(17) 0.030(2) 0.039(2) -0.0018(16) 0.0176(15) 0.0008(15) C1 0.056(3) 0.049(4) 0.064(4) -0.011(3) 0.032(3) -0.019(3) C2 0.073(4) 0.047(3) 0.061(3) -0.017(3) 0.043(3) -0.009(3) C3 0.064(4) 0.075(5) 0.099(5) 0.003(4) 0.057(4) -0.019(3) C4 0.063(4) 0.081(5) 0.067(4) 0.009(3) 0.043(3) 0.023(3) C5 0.092(5) 0.073(4) 0.060(4) -0.024(3) 0.047(3) -0.002(4) C10 0.029(2) 0.014(2) 0.035(2) 0.0042(15) 0.0139(18) 0.0007(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 In1 O1 2.070(3) . ? In1 O2 2.086(3) . ? In1 O3 2.102(3) . ? In1 O4 2.202(3) . ? In1 O5 2.226(3) . ? In1 N1 2.231(3) . ? P1 O2 1.493(3) . ? P1 O1 1.500(3) 2_655 ? P1 O3 1.502(3) 1_565 ? O1 P1 1.500(3) 2_645 ? O3 P1 1.502(3) 1_545 ? O4 C10 1.249(5) . ? O5 C10 1.251(5) 3_655 ? N1 C1 1.331(6) . ? N1 C2 1.332(6) . ? C1 C3 1.379(7) . ? C2 C5 1.378(7) . ? C3 C4 1.365(9) . ? C4 C5 1.356(8) . ? C10 O5 1.251(5) 3_655 ? C10 C10 1.576(7) 3_655 ? 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 In1 O2 94.97(12) . . ? O1 In1 O3 92.87(12) . . ? O2 In1 O3 170.17(11) . . ? O1 In1 O4 97.63(11) . . ? O2 In1 O4 92.60(11) . . ? O3 In1 O4 92.22(10) . . ? O1 In1 O5 172.99(10) . . ? O2 In1 O5 87.16(12) . . ? O3 In1 O5 85.76(11) . . ? O4 In1 O5 75.58(10) . . ? O1 In1 N1 96.91(12) . . ? O2 In1 N1 85.66(12) . . ? O3 In1 N1 87.53(11) . . ? O4 In1 N1 165.46(11) . . ? O5 In1 N1 89.90(11) . . ? O2 P1 O1 115.11(18) . 2_655 ? O2 P1 O3 109.92(18) . 1_565 ? O1 P1 O3 114.10(18) 2_655 1_565 ? P1 O1 In1 139.12(18) 2_645 . ? P1 O2 In1 146.98(19) . . ? P1 O3 In1 134.10(17) 1_545 . ? C10 O4 In1 115.3(2) . . ? C10 O5 In1 114.7(2) 3_655 . ? C1 N1 C2 117.8(4) . . ? C1 N1 In1 121.6(3) . . ? C2 N1 In1 120.6(3) . . ? N1 C1 C3 121.5(6) . . ? N1 C2 C5 122.7(5) . . ? C4 C3 C1 120.7(6) . . ? C5 C4 C3 117.6(6) . . ? C4 C5 C2 119.7(6) . . ? O4 C10 O5 125.9(4) . 3_655 ? O4 C10 C10 117.3(4) . 3_655 ? O5 C10 C10 116.8(4) 3_655 3_655 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.724 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.129 #####EOF##### data_compoundIV _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Indiumphosphiteoxalate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31 In2 N4 O20 P3' _chemical_formula_weight 873.96 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' 'In' 'In' -0.7276 1.3100 '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 9.195(3) _cell_length_b 12.390(4) _cell_length_c 13.126(4) _cell_angle_alpha 76.559(5) _cell_angle_beta 78.326(5) _cell_angle_gamma 76.967(5) _cell_volume 1399.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6423 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 28.06 _exptl_crystal_description platelike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.912 _exptl_absorpt_correction_type ‘Multi-scan’ _exptl_absorpt_correction_T_min 0.7010 _exptl_absorpt_correction_T_max 0.8621 _exptl_absorpt_process_details ‘(SADABS;Sheldrick,1996)’ _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 'BrukerSMARTCCDareadetector' _diffrn_measurement_method '\fand\wscans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15648 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.06 _reflns_number_total 6423 _reflns_number_gt 5736 _reflns_threshold_expression >2sigma(I) _computing_data_collection ‘SMART(Bruker,2000)’ _computing_cell_refinement ‘SMART’ _computing_data_reduction ‘SAINT(Bruker,2000)’ _computing_structure_solution ‘SIR92(Altomareetal.,1993)’ _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ‘Ortep3forWindows(Farrugia,1997)andCAMERON _computing_publication_material ‘PLATON(Spek,1990)’ _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^)+(0.0377P)^2^+9.4140P] 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 6423 _refine_ls_number_parameters 386 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 H201 H 0.333(19) 0.532(13) 0.208(5) 0.18(8) Uiso 1 1 d D . . H202 H 0.258(10) 0.534(9) 0.112(8) 0.09(4) Uiso 1 1 d D . . H301 H 0.193(11) 0.382(6) 0.387(7) 0.10(4) Uiso 1 1 d D . . H302 H 0.238(11) 0.477(7) 0.390(6) 0.08(3) Uiso 1 1 d D . . In1 In 0.20143(3) 0.10271(3) -0.00185(2) 0.01451(9) Uani 1 1 d . . . In2 In 0.18364(3) -0.09731(3) 0.35809(2) 0.01522(9) Uani 1 1 d . . . P1 P 0.45569(12) -0.06789(10) 0.14521(9) 0.0156(2) Uani 1 1 d . . . H1 H 0.4441 -0.1220 0.1050 0.019 Uiso 1 1 calc R . . P2 P -0.08700(12) 0.13149(10) -0.13271(9) 0.0150(2) Uani 1 1 d . . . H2 H -0.1565 0.2042 -0.1448 0.018 Uiso 1 1 calc R . . P3 P 0.11055(14) 0.14479(11) 0.44575(10) 0.0193(2) Uani 1 1 d . . . H3 H 0.0308 0.1946 0.4083 0.023 Uiso 1 1 calc R . . O1 O 0.1531(4) -0.0619(3) 0.0289(2) 0.0193(7) Uani 1 1 d . . . O2 O 0.3688(4) 0.0461(3) 0.1005(3) 0.0223(7) Uani 1 1 d . . . O3 O 0.3743(4) 0.0677(3) -0.1329(3) 0.0211(7) Uani 1 1 d . . . O4 O 0.0182(4) 0.1734(3) 0.1075(3) 0.0261(8) Uani 1 1 d . . . O5 O 0.0666(4) 0.1563(3) -0.1270(3) 0.0229(7) Uani 1 1 d . . . O6 O 0.2411(4) 0.2706(3) -0.0159(3) 0.0268(8) Uani 1 1 d . . . O7 O 0.1995(4) 0.0633(3) 0.3745(3) 0.0285(8) Uani 1 1 d . . . O8 O 0.0744(4) -0.0772(3) 0.2275(3) 0.0237(7) Uani 1 1 d . . . O9 O -0.0341(4) -0.0869(3) 0.4488(3) 0.0285(8) Uani 1 1 d . . . O10 O 0.3990(4) -0.1108(3) 0.2616(3) 0.0255(8) Uani 1 1 d . . . O11 O 0.3054(4) -0.1743(3) 0.4920(3) 0.0235(7) Uani 1 1 d . . . O12 O 0.1942(5) -0.2818(3) 0.3802(3) 0.0292(8) Uani 1 1 d . . . O13 O 0.2116(4) 0.2186(4) 0.4621(3) 0.0354(10) Uani 1 1 d . . . O14 O 0.1746(6) 0.4160(4) 0.0662(5) 0.0580(14) Uani 1 1 d . . . O15 O -0.0607(6) 0.3174(4) 0.1911(4) 0.0528(13) Uani 1 1 d . . . O16 O 0.3721(5) -0.3362(3) 0.6025(3) 0.0321(9) Uani 1 1 d . . . O17 O 0.2395(6) -0.4418(4) 0.4978(4) 0.0475(12) Uani 1 1 d . . . C1 C 0.2424(6) -0.3412(4) 0.4632(4) 0.0231(10) Uani 1 1 d . . . C2 C 0.3122(5) -0.2793(4) 0.5260(4) 0.0219(10) Uani 1 1 d . . . C3 C 0.1580(6) 0.3253(5) 0.0540(5) 0.0298(11) Uani 1 1 d . . . C4 C 0.0268(6) 0.2696(5) 0.1254(4) 0.0286(11) Uani 1 1 d . . . C10 C 0.4860(5) 0.1942(4) 0.3306(4) 0.0199(9) Uani 1 1 d . . . H10A H 0.3851 0.1952 0.3711 0.024 Uiso 1 1 calc R . . H10B H 0.5312 0.2474 0.3519 0.024 Uiso 1 1 calc R . . C11 C 0.4759(6) 0.2293(5) 0.2164(5) 0.0334(12) Uani 1 1 d . . . H11A H 0.4164 0.3050 0.2025 0.040 Uiso 1 1 calc R . . H11B H 0.4260 0.1786 0.1956 0.040 Uiso 1 1 calc R . . C12 C 0.7328(5) 0.1147(4) 0.1789(4) 0.0180(9) Uani 1 1 d . . . H12A H 0.6970 0.0587 0.1545 0.022 Uiso 1 1 calc R . . H12B H 0.8347 0.1185 0.1419 0.022 Uiso 1 1 calc R . . C13 C 0.7361(6) 0.0786(5) 0.2945(4) 0.0295(11) Uani 1 1 d . . . H13A H 0.7827 0.1295 0.3179 0.035 Uiso 1 1 calc R . . H13B H 0.7961 0.0033 0.3090 0.035 Uiso 1 1 calc R . . C14 C 0.6278(7) 0.6416(5) 0.2843(5) 0.0360(13) Uani 1 1 d . . . H14A H 0.5280 0.6225 0.3058 0.043 Uiso 1 1 calc R . . H14B H 0.6302 0.6911 0.2151 0.043 Uiso 1 1 calc R . . C15 C 0.7413(6) 0.5378(4) 0.2767(4) 0.0234(10) Uani 1 1 d . . . H15A H 0.7222 0.5022 0.2235 0.028 Uiso 1 1 calc R . . H15B H 0.7327 0.4854 0.3442 0.028 Uiso 1 1 calc R . . C16 C 0.8135(5) 0.7264(4) 0.3365(4) 0.0180(9) Uani 1 1 d . . . H16A H 0.8230 0.7803 0.2699 0.022 Uiso 1 1 calc R . . H16B H 0.8322 0.7602 0.3912 0.022 Uiso 1 1 calc R . . C17 C 0.9285(6) 0.6221(5) 0.3271(4) 0.0290(11) Uani 1 1 d . . . H17A H 0.9276 0.5717 0.3959 0.035 Uiso 1 1 calc R . . H17B H 1.0282 0.6415 0.3047 0.035 Uiso 1 1 calc R . . N1 N 0.6569(6) 0.7027(5) 0.3633(5) 0.0477(14) Uani 1 1 d . . . H1A H 0.5900 0.7681 0.3629 0.057 Uiso 1 1 calc R . . H1B H 0.6440 0.6601 0.4289 0.057 Uiso 1 1 calc R . . N2 N 0.8970(6) 0.5627(5) 0.2480(5) 0.0443(13) Uani 1 1 d . . . H2A H 0.9075 0.6065 0.1829 0.053 Uiso 1 1 calc R . . H2B H 0.9645 0.4977 0.2464 0.053 Uiso 1 1 calc R . . N3 N 0.6330(7) 0.2272(5) 0.1521(5) 0.0504(15) Uani 1 1 d . . . H3A H 0.6265 0.2426 0.0826 0.060 Uiso 1 1 calc R . . H3B H 0.6741 0.2810 0.1652 0.060 Uiso 1 1 calc R . . N4 N 0.5780(6) 0.0792(5) 0.3544(4) 0.0419(13) Uani 1 1 d . . . H4A H 0.5362 0.0294 0.3353 0.050 Uiso 1 1 calc R . . H4B H 0.5807 0.0585 0.4245 0.050 Uiso 1 1 calc R . . O100 O 0.6252(6) 0.4949(5) 0.1142(4) 0.0564(13) Uani 1 1 d . . . O200 O 0.3107(9) 0.5572(6) 0.1459(7) 0.0752(18) Uani 1 1 d D . . O300 O 0.2307(9) 0.4369(5) 0.3477(5) 0.0676(17) Uani 1 1 d 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 0.01296(15) 0.01777(17) 0.01246(15) -0.00239(11) -0.00083(11) -0.00384(11) In2 0.01557(16) 0.01963(18) 0.01066(15) -0.00272(12) 0.00035(11) -0.00616(12) P1 0.0123(5) 0.0218(6) 0.0132(5) -0.0040(4) 0.0001(4) -0.0053(4) P2 0.0134(5) 0.0175(6) 0.0134(5) -0.0001(4) -0.0030(4) -0.0040(4) P3 0.0178(6) 0.0221(6) 0.0179(6) -0.0057(5) 0.0019(4) -0.0059(5) O1 0.0212(16) 0.0247(18) 0.0133(15) -0.0038(13) 0.0010(12) -0.0106(13) O2 0.0226(17) 0.0274(19) 0.0184(16) -0.0029(14) -0.0081(13) -0.0049(14) O3 0.0129(15) 0.033(2) 0.0180(16) -0.0074(14) 0.0008(12) -0.0063(13) O4 0.0222(17) 0.028(2) 0.0270(18) -0.0111(15) 0.0073(14) -0.0064(15) O5 0.0201(16) 0.034(2) 0.0167(16) 0.0032(14) -0.0051(13) -0.0148(15) O6 0.0294(19) 0.0226(19) 0.0285(19) -0.0031(15) -0.0002(15) -0.0109(15) O7 0.033(2) 0.032(2) 0.0236(18) -0.0143(16) 0.0129(15) -0.0176(16) O8 0.0266(18) 0.031(2) 0.0148(16) -0.0047(14) -0.0061(13) -0.0050(15) O9 0.0207(18) 0.041(2) 0.0204(18) -0.0056(16) 0.0069(14) -0.0077(16) O10 0.0162(16) 0.034(2) 0.0173(17) 0.0027(15) 0.0035(13) 0.0002(14) O11 0.0314(19) 0.0225(19) 0.0195(17) -0.0006(14) -0.0088(14) -0.0103(15) O12 0.042(2) 0.025(2) 0.0257(19) -0.0049(15) -0.0127(16) -0.0115(17) O13 0.033(2) 0.039(2) 0.041(2) -0.0235(19) 0.0110(17) -0.0195(18) O14 0.070(3) 0.039(3) 0.076(4) -0.031(3) 0.006(3) -0.027(3) O15 0.054(3) 0.050(3) 0.056(3) -0.035(3) 0.017(2) -0.010(2) O16 0.044(2) 0.026(2) 0.027(2) 0.0038(16) -0.0174(17) -0.0084(17) O17 0.088(4) 0.023(2) 0.040(2) 0.0050(18) -0.029(2) -0.021(2) C1 0.033(3) 0.019(2) 0.019(2) -0.0028(19) -0.0046(19) -0.007(2) C2 0.020(2) 0.029(3) 0.016(2) -0.0045(19) 0.0002(17) -0.0079(19) C3 0.031(3) 0.029(3) 0.032(3) -0.008(2) -0.008(2) -0.008(2) C4 0.032(3) 0.025(3) 0.030(3) -0.010(2) -0.004(2) -0.004(2) C10 0.012(2) 0.028(3) 0.023(2) -0.016(2) 0.0054(17) -0.0066(18) C11 0.029(3) 0.034(3) 0.038(3) -0.012(3) -0.011(2) 0.001(2) C12 0.017(2) 0.020(2) 0.017(2) -0.0106(18) 0.0063(16) -0.0050(17) C13 0.024(3) 0.037(3) 0.029(3) -0.012(2) -0.004(2) -0.005(2) C14 0.028(3) 0.043(4) 0.035(3) 0.001(3) -0.008(2) -0.009(2) C15 0.030(3) 0.020(2) 0.024(2) -0.0004(19) -0.008(2) -0.013(2) C16 0.028(2) 0.010(2) 0.016(2) -0.0028(16) -0.0010(17) -0.0042(17) C17 0.025(3) 0.032(3) 0.030(3) -0.005(2) -0.004(2) -0.007(2) N1 0.044(3) 0.051(4) 0.038(3) -0.004(3) -0.002(2) 0.002(3) N2 0.045(3) 0.041(3) 0.049(3) -0.016(3) -0.005(3) -0.006(2) N3 0.063(4) 0.051(4) 0.036(3) -0.008(3) -0.001(3) -0.015(3) N4 0.045(3) 0.049(3) 0.037(3) -0.013(2) 0.001(2) -0.019(3) O100 0.071(4) 0.053(3) 0.056(3) -0.010(3) -0.019(3) -0.024(3) O200 0.081(5) 0.076(5) 0.083(5) -0.038(4) -0.021(4) -0.014(4) O300 0.109(5) 0.044(3) 0.058(4) -0.013(3) -0.024(4) -0.018(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 In1 O1 2.115(3) . ? In1 O2 2.139(3) . ? In1 O3 2.145(3) . ? In1 O4 2.146(3) . ? In1 O5 2.150(3) . ? In1 O6 2.152(4) . ? In2 O7 2.091(4) . ? In2 O8 2.097(3) . ? In2 O9 2.105(3) . ? In2 O10 2.118(3) . ? In2 O11 2.188(3) . ? In2 O12 2.219(4) . ? P1 O2 1.508(4) . ? P1 O10 1.521(3) . ? P1 O3 1.539(3) 2_655 ? P2 O8 1.519(3) 2 ? P2 O1 1.524(3) 2 ? P2 O5 1.531(3) . ? P3 O9 1.516(4) 2_556 ? P3 O13 1.517(4) . ? P3 O7 1.523(4) . ? O1 P2 1.524(3) 2 ? O3 P1 1.539(3) 2_655 ? O4 C4 1.290(6) . ? O6 C3 1.287(7) . ? O8 P2 1.519(3) 2 ? O9 P3 1.516(4) 2_556 ? O11 C2 1.265(6) . ? O12 C1 1.265(6) . ? O14 C3 1.218(7) . ? O15 C4 1.217(7) . ? O16 C2 1.236(6) . ? O17 C1 1.228(6) . ? C1 C2 1.553(7) . ? C3 C4 1.558(8) . ? C10 C11 1.477(7) . ? C10 N4 1.484(8) . ? C11 N3 1.516(8) . ? C12 C13 1.483(7) . ? C12 N3 1.494(8) . ? C13 N4 1.505(7) . ? C14 C15 1.471(8) . ? C14 N1 1.513(8) . ? C15 N2 1.488(7) . ? C16 C17 1.486(7) . ? C16 N1 1.490(7) . ? C17 N2 1.510(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 O1 In1 O2 90.58(13) . . ? O1 In1 O3 91.84(13) . . ? O2 In1 O3 89.00(13) . . ? O1 In1 O4 98.03(13) . . ? O2 In1 O4 98.53(14) . . ? O3 In1 O4 167.48(14) . . ? O1 In1 O5 90.95(13) . . ? O2 In1 O5 169.84(13) . . ? O3 In1 O5 80.91(13) . . ? O4 In1 O5 91.21(14) . . ? O1 In1 O6 173.96(13) . . ? O2 In1 O6 87.00(14) . . ? O3 In1 O6 93.65(13) . . ? O4 In1 O6 76.88(14) . . ? O5 In1 O6 92.41(14) . . ? O7 In2 O8 107.76(15) . . ? O7 In2 O9 92.20(14) . . ? O8 In2 O9 85.70(14) . . ? O7 In2 O10 89.72(14) . . ? O8 In2 O10 91.88(14) . . ? O9 In2 O10 177.28(15) . . ? O7 In2 O11 90.24(15) . . ? O8 In2 O11 161.90(14) . . ? O9 In2 O11 95.75(14) . . ? O10 In2 O11 86.16(14) . . ? O7 In2 O12 164.58(15) . . ? O8 In2 O12 87.63(14) . . ? O9 In2 O12 87.87(15) . . ? O10 In2 O12 90.79(15) . . ? O11 In2 O12 74.42(13) . . ? O2 P1 O10 113.4(2) . . ? O2 P1 O3 111.9(2) . 2_655 ? O10 P1 O3 108.2(2) . 2_655 ? O8 P2 O1 112.7(2) 2 2 ? O8 P2 O5 110.0(2) 2 . ? O1 P2 O5 112.05(19) 2 . ? O9 P3 O13 110.9(2) 2_556 . ? O9 P3 O7 113.6(2) 2_556 . ? O13 P3 O7 110.1(2) . . ? P2 O1 In1 129.38(19) 2 . ? P1 O2 In1 134.4(2) . . ? P1 O3 In1 127.94(19) 2_655 . ? C4 O4 In1 115.6(3) . . ? P2 O5 In1 130.51(19) . . ? C3 O6 In1 115.0(3) . . ? P3 O7 In2 134.5(2) . . ? P2 O8 In2 139.3(2) 2 . ? P3 O9 In2 138.2(2) 2_556 . ? P1 O10 In2 134.4(2) . . ? C2 O11 In2 116.8(3) . . ? C1 O12 In2 115.7(3) . . ? O17 C1 O12 126.4(5) . . ? O17 C1 C2 117.8(5) . . ? O12 C1 C2 115.8(4) . . ? O16 C2 O11 125.8(5) . . ? O16 C2 C1 117.9(5) . . ? O11 C2 C1 116.2(4) . . ? O14 C3 O6 124.6(5) . . ? O14 C3 C4 119.3(5) . . ? O6 C3 C4 116.1(4) . . ? O15 C4 O4 124.3(5) . . ? O15 C4 C3 120.5(5) . . ? O4 C4 C3 115.2(4) . . ? C11 C10 N4 111.1(4) . . ? C10 C11 N3 109.9(5) . . ? C13 C12 N3 112.2(4) . . ? C12 C13 N4 110.2(4) . . ? C15 C14 N1 111.4(5) . . ? C14 C15 N2 111.2(4) . . ? C17 C16 N1 111.8(4) . . ? C16 C17 N2 110.9(4) . . ? C16 N1 C14 110.8(5) . . ? C15 N2 C17 110.8(5) . . ? C12 N3 C11 111.3(5) . . ? C10 N4 C13 109.4(4) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.073 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.173 #####EOF#######