Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Srinivasan Natarajan' 'A. Thirumurugan' _publ_contact_author_name 'Prof Srinivasan Natarajan' _publ_contact_author_address ; Framework Solids Laboratory, Chemistry and Physics of Materials Unit JNCASR Jakkur P.O. Bangalore Karnataka 560 064 INDIA ; _publ_contact_author_email RAJ@JNCASR.AC.IN _publ_section_title ; Synthesis and Structure of a New Three-dimensional Indium Phosphate with 16-membered One-dimensional Channels ; data_sad _database_code_CSD 204105 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2.50 H2.50 F2 In1.75 N2.50 O9 P2' _chemical_formula_weight 512.45 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' 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 C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.569(5) _cell_length_b 9.7034(18) _cell_length_c 14.927(6) _cell_angle_alpha 90.00 _cell_angle_beta 119.091(14) _cell_angle_gamma 90.00 _cell_volume 2476.9(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle-like _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 2.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1926 _exptl_absorpt_coefficient_mu 3.600 _exptl_absorpt_correction_type 'emprical SADABS' _exptl_absorpt_correction_T_min 0.775438 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5154 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 23.27 _reflns_number_total 1897 _reflns_number_gt 1672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0350P)^2^+11.2457P] 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 1897 _refine_ls_number_parameters 210 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.166 _refine_ls_shift/su_mean 0.004 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 0.78207(3) -0.5000 0.01392(4) 0.01423(18) Uani 1 2 d S . . In2 In 0.51224(3) -0.5000 -0.23927(4) 0.01528(18) Uani 1 2 d S . . In3 In 0.5000 -0.5000 0.0000 0.0106(2) Uani 1 4 d S . . In4 In 0.5000 -0.5000 -0.5000 0.0187(2) Uani 1 4 d S . . In5 In 0.5000 0.0000 -0.5000 0.0201(4) Uani 0.790(4) 4 d SP . . P1 P 0.57746(12) -0.26007(18) -0.57434(13) 0.0360(5) Uani 1 1 d . . . P2 P 0.62653(8) -0.29954(15) -0.03635(11) 0.0146(3) Uani 1 1 d . . . F1 F 0.7344(3) -0.5000 -0.1433(3) 0.0262(11) Uani 1 2 d S . . O2 O 0.7098(2) -0.3521(4) 0.0277(3) 0.0296(10) Uani 1 1 d . . . O3 O 0.8717(2) -0.3591(4) 0.0337(3) 0.0213(9) Uani 1 1 d . . . F4 F 0.8368(3) -0.5000 0.1796(3) 0.0260(11) Uani 1 2 d S . . O5 O 0.5897(3) -0.3461(5) -0.1474(3) 0.0364(12) Uani 1 1 d . . . F6 F 0.4467(2) -0.5000 -0.1619(3) 0.0196(10) Uani 1 2 d S . . F7 F 0.5619(3) -0.5000 -0.3380(3) 0.0215(11) Uani 1 2 d S . . O8 O 0.5630(2) -0.3389(5) -0.6682(3) 0.0350(11) Uani 1 1 d . . . O9 O 0.5786(2) -0.3448(4) 0.0143(3) 0.0309(11) Uani 1 1 d . . . O10 O 0.5822(2) -0.3502(4) -0.4894(3) 0.0289(10) Uani 1 1 d . . . O11 O 0.3849(4) 0.0000 -0.5980(6) 0.076(3) Uani 1 2 d S . . H30 H 0.3622 0.0423 -0.5727 0.114 Uiso 0.50 1 calc PR . . O12 O 0.5180(5) -0.1467(6) -0.5979(4) 0.093(3) Uani 1 1 d . . . O13 O 0.6593(5) -0.1949(10) -0.5310(5) 0.131(4) Uani 1 1 d . . . H20 H 0.6662 -0.1698 -0.5785 0.196 Uiso 1 1 calc R . . O100 O 0.7489(6) -0.5000 -0.4337(8) 0.097(3) Uani 1 2 d S . . N1 N 0.6795(3) -0.2624(5) -0.2591(4) 0.0342(14) Uani 1 1 d . . . H1 H 0.6738 -0.3427 -0.2347 0.051 Uiso 1 1 calc R . . H2 H 0.6438 -0.2551 -0.3249 0.051 Uiso 1 1 calc R . . H3 H 0.6735 -0.1939 -0.2239 0.051 Uiso 1 1 calc R . . C1 C 0.7586(4) -0.2550(7) -0.2486(5) 0.0346(17) Uani 1 1 d . . . H4 H 0.7969 -0.2662 -0.1768 0.041 Uiso 1 1 calc R . . H5 H 0.7649 -0.3318 -0.2857 0.041 Uiso 1 1 calc R . . C2 C 0.7761(4) -0.1265(7) -0.2860(5) 0.0356(17) Uani 1 1 d . . . H6 H 0.7368 -0.1139 -0.3572 0.043 Uiso 1 1 calc R . . H7 H 0.8262 -0.1369 -0.2839 0.043 Uiso 1 1 calc R . . N2 N 0.7788(4) 0.0000 -0.2284(5) 0.0248(17) Uani 1 2 d S . . H8 H 0.7380 0.0000 -0.2163 0.030 Uiso 1 2 calc SR . . H9 H 0.8230 0.0000 -0.1675 0.030 Uiso 1 2 calc SR . . N3 N 1.0082(4) -0.5000 -0.2136(6) 0.036(2) Uani 1 2 d S . . H10 H 0.9917 -0.5000 -0.2807 0.054 Uiso 1 2 calc SR . . H11 H 1.0369 -0.5749 -0.1854 0.054 Uiso 0.50 1 calc PR . . H12 H 1.0369 -0.4251 -0.1854 0.054 Uiso 0.50 1 calc PR . . C3 C 0.9418(6) -0.5000 -0.1966(7) 0.084(5) Uani 1 2 d SD . . H13 H 0.9106 -0.4198 -0.2316 0.101 Uiso 0.50 1 calc PR . . H14 H 0.9106 -0.5802 -0.2316 0.101 Uiso 0.50 1 calc PR . . C4 C 0.9511(6) -0.5000 -0.0961(6) 0.083(5) Uani 1 2 d SD . . N4 N 1.0000 -0.4441(14) 0.0000 0.037(4) Uani 0.50 2 d SPD . . 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 0.0116(3) 0.0148(3) 0.0164(3) 0.000 0.0069(3) 0.000 In2 0.0178(3) 0.0167(3) 0.0124(3) 0.000 0.0082(3) 0.000 In3 0.0104(4) 0.0091(4) 0.0130(4) 0.000 0.0063(3) 0.000 In4 0.0266(5) 0.0168(5) 0.0134(4) 0.000 0.0103(4) 0.000 In5 0.0311(7) 0.0128(7) 0.0168(7) 0.000 0.0120(5) 0.000 P1 0.0651(13) 0.0228(10) 0.0253(10) -0.0086(8) 0.0259(10) -0.0202(9) P2 0.0166(8) 0.0088(7) 0.0206(8) -0.0021(6) 0.0108(7) -0.0034(6) F1 0.033(3) 0.029(3) 0.016(3) 0.000 0.011(2) 0.000 O2 0.026(2) 0.019(2) 0.041(3) 0.001(2) 0.014(2) 0.0105(19) O3 0.016(2) 0.012(2) 0.037(2) 0.0015(18) 0.0141(19) 0.0002(17) F4 0.020(3) 0.037(3) 0.019(3) 0.000 0.008(2) 0.000 O5 0.045(3) 0.042(3) 0.027(2) -0.017(2) 0.022(2) -0.023(2) F6 0.013(2) 0.033(3) 0.013(2) 0.000 0.007(2) 0.000 F7 0.022(3) 0.029(3) 0.015(2) 0.000 0.010(2) 0.000 O8 0.042(3) 0.040(3) 0.029(2) -0.019(2) 0.022(2) -0.021(2) O9 0.042(3) 0.030(3) 0.032(3) -0.011(2) 0.027(2) -0.023(2) O10 0.037(3) 0.028(3) 0.022(2) 0.0028(19) 0.015(2) -0.006(2) O11 0.041(5) 0.149(10) 0.037(5) 0.000 0.018(4) 0.000 O12 0.194(8) 0.036(4) 0.051(4) 0.019(3) 0.061(4) 0.058(4) O13 0.168(7) 0.196(9) 0.063(4) -0.082(5) 0.084(5) -0.162(7) O100 0.082(7) 0.148(10) 0.072(7) 0.000 0.047(6) 0.000 N1 0.045(4) 0.020(3) 0.037(3) -0.002(3) 0.020(3) -0.008(3) C1 0.032(4) 0.036(4) 0.034(4) -0.009(3) 0.014(3) -0.002(3) C2 0.039(4) 0.039(4) 0.037(4) -0.015(3) 0.024(3) -0.010(3) N2 0.021(4) 0.027(4) 0.025(4) 0.000 0.010(3) 0.000 N3 0.024(4) 0.067(6) 0.019(4) 0.000 0.011(4) 0.000 C3 0.020(6) 0.196(18) 0.031(7) 0.000 0.009(5) 0.000 C4 0.030(7) 0.199(18) 0.020(7) 0.000 0.012(6) 0.000 N4 0.034(9) 0.033(10) 0.037(10) 0.000 0.013(8) 0.000 _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 F1 2.061(4) . ? In1 O2 2.094(4) 6_545 ? In1 O2 2.094(4) . ? In1 O3 2.129(4) . ? In1 O3 2.129(4) 6_545 ? In1 F4 2.165(5) . ? In2 O5 2.094(4) 6_545 ? In2 O5 2.094(4) . ? In2 F6 2.102(4) . ? In2 F7 2.124(4) . ? In2 O8 2.131(4) 5_644 ? In2 O8 2.131(4) 2_654 ? In3 O9 2.088(4) . ? In3 O9 2.088(4) 5_645 ? In3 O9 2.088(4) 2_655 ? In3 O9 2.088(4) 6_545 ? In3 F6 2.116(4) 5_645 ? In3 F6 2.116(4) . ? In4 F7 2.113(4) 5_644 ? In4 F7 2.113(4) . ? In4 O10 2.116(4) . ? In4 O10 2.116(4) 5_644 ? In4 O10 2.116(4) 2_654 ? In4 O10 2.116(4) 6_545 ? In5 O11 2.002(7) . ? In5 O11 2.002(7) 5_654 ? In5 O12 2.188(5) 6 ? In5 O12 2.188(5) . ? In5 O12 2.188(5) 5_654 ? In5 O12 2.188(5) 2_654 ? P1 O8 1.498(4) . ? P1 O10 1.506(4) . ? P1 O12 1.513(6) . ? P1 O13 1.541(6) . ? P2 O5 1.519(4) . ? P2 O2 1.522(4) . ? P2 O9 1.528(4) . ? P2 O3 1.540(4) 7_645 ? O3 P2 1.540(4) 7_645 ? O8 In2 2.131(4) 5_644 ? O11 H30 0.8200 . ? O13 H20 0.8201 . ? N1 C1 1.480(7) . ? N1 H1 0.8900 . ? N1 H2 0.8900 . ? N1 H3 0.8900 . ? C1 C2 1.473(9) . ? C1 H4 0.9700 . ? C1 H5 0.9700 . ? C2 N2 1.486(7) . ? C2 H6 0.9700 . ? C2 H7 0.9700 . ? N2 C2 1.485(7) 6 ? N2 H8 0.9000 . ? N2 H9 0.9000 . ? N3 C3 1.439(12) . ? N3 H10 0.8900 . ? N3 H11 0.8900 . ? N3 H12 0.8900 . ? C3 C4 1.422(9) . ? C3 H13 0.9700 . ? C3 H14 0.9700 . ? C4 N4 1.390(8) . ? C4 N4 1.390(8) 5_745 ? N4 N4 1.08(3) 5_745 ? N4 C4 1.390(8) 5_745 ? 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 F1 In1 O2 99.13(15) . 6_545 ? F1 In1 O2 99.13(15) . . ? O2 In1 O2 86.5(2) 6_545 . ? F1 In1 O3 92.52(15) . . ? O2 In1 O3 167.70(16) 6_545 . ? O2 In1 O3 95.57(16) . . ? F1 In1 O3 92.52(15) . 6_545 ? O2 In1 O3 95.57(16) 6_545 6_545 ? O2 In1 O3 167.70(16) . 6_545 ? O3 In1 O3 79.9(2) . 6_545 ? F1 In1 F4 177.70(17) . . ? O2 In1 F4 82.53(14) 6_545 . ? O2 In1 F4 82.53(14) . . ? O3 In1 F4 85.72(14) . . ? O3 In1 F4 85.72(14) 6_545 . ? O5 In2 O5 90.9(3) 6_545 . ? O5 In2 F6 94.62(14) 6_545 . ? O5 In2 F6 94.62(14) . . ? O5 In2 F7 91.44(14) 6_545 . ? O5 In2 F7 91.44(14) . . ? F6 In2 F7 171.35(16) . . ? O5 In2 O8 87.33(19) 6_545 5_644 ? O5 In2 O8 177.92(18) . 5_644 ? F6 In2 O8 86.68(13) . 5_644 ? F7 In2 O8 87.44(14) . 5_644 ? O5 In2 O8 177.92(18) 6_545 2_654 ? O5 In2 O8 87.33(19) . 2_654 ? F6 In2 O8 86.68(13) . 2_654 ? F7 In2 O8 87.44(14) . 2_654 ? O8 In2 O8 94.4(3) 5_644 2_654 ? O9 In3 O9 180.0 . 5_645 ? O9 In3 O9 87.7(3) . 2_655 ? O9 In3 O9 92.3(3) 5_645 2_655 ? O9 In3 O9 92.3(3) . 6_545 ? O9 In3 O9 87.7(3) 5_645 6_545 ? O9 In3 O9 180.00(19) 2_655 6_545 ? O9 In3 F6 87.36(14) . 5_645 ? O9 In3 F6 92.64(14) 5_645 5_645 ? O9 In3 F6 92.64(14) 2_655 5_645 ? O9 In3 F6 87.36(14) 6_545 5_645 ? O9 In3 F6 92.64(14) . . ? O9 In3 F6 87.36(14) 5_645 . ? O9 In3 F6 87.36(14) 2_655 . ? O9 In3 F6 92.64(14) 6_545 . ? F6 In3 F6 180.0 5_645 . ? F7 In4 F7 179.998(1) 5_644 . ? F7 In4 O10 94.46(14) 5_644 . ? F7 In4 O10 85.54(14) . . ? F7 In4 O10 85.54(14) 5_644 5_644 ? F7 In4 O10 94.46(14) . 5_644 ? O10 In4 O10 180.0 . 5_644 ? F7 In4 O10 85.54(13) 5_644 2_654 ? F7 In4 O10 94.46(13) . 2_654 ? O10 In4 O10 93.2(2) . 2_654 ? O10 In4 O10 86.8(2) 5_644 2_654 ? F7 In4 O10 94.46(13) 5_644 6_545 ? F7 In4 O10 85.54(13) . 6_545 ? O10 In4 O10 86.8(2) . 6_545 ? O10 In4 O10 93.2(2) 5_644 6_545 ? O10 In4 O10 179.998(2) 2_654 6_545 ? O11 In5 O11 179.998(1) . 5_654 ? O11 In5 O12 90.1(3) . 6 ? O11 In5 O12 89.9(3) 5_654 6 ? O11 In5 O12 90.1(3) . . ? O11 In5 O12 89.9(3) 5_654 . ? O12 In5 O12 81.2(3) 6 . ? O11 In5 O12 89.9(3) . 5_654 ? O11 In5 O12 90.1(3) 5_654 5_654 ? O12 In5 O12 98.8(3) 6 5_654 ? O12 In5 O12 179.999(1) . 5_654 ? O11 In5 O12 89.9(3) . 2_654 ? O11 In5 O12 90.1(3) 5_654 2_654 ? O12 In5 O12 180.0 6 2_654 ? O12 In5 O12 98.8(3) . 2_654 ? O12 In5 O12 81.2(3) 5_654 2_654 ? O8 P1 O10 113.4(3) . . ? O8 P1 O12 112.3(3) . . ? O10 P1 O12 110.1(3) . . ? O8 P1 O13 106.7(3) . . ? O10 P1 O13 105.0(4) . . ? O12 P1 O13 108.9(5) . . ? O5 P2 O2 112.4(2) . . ? O5 P2 O9 111.9(2) . . ? O2 P2 O9 108.7(3) . . ? O5 P2 O3 108.6(3) . 7_645 ? O2 P2 O3 108.4(2) . 7_645 ? O9 P2 O3 106.6(2) . 7_645 ? P2 O2 In1 137.4(3) . . ? P2 O3 In1 130.7(2) 7_645 . ? P2 O5 In2 137.3(3) . . ? In2 F6 In3 122.27(19) . . ? In4 F7 In2 126.4(2) . . ? P1 O8 In2 137.5(3) . 5_644 ? P2 O9 In3 139.1(3) . . ? P1 O10 In4 127.0(2) . . ? In5 O11 H30 109.5 . . ? P1 O12 In5 132.3(4) . . ? P1 O13 H20 109.5 . . ? C1 N1 H1 109.5 . . ? C1 N1 H2 109.5 . . ? H1 N1 H2 109.5 . . ? C1 N1 H3 109.5 . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? C2 C1 N1 115.1(6) . . ? C2 C1 H4 108.5 . . ? N1 C1 H4 108.5 . . ? C2 C1 H5 108.5 . . ? N1 C1 H5 108.5 . . ? H4 C1 H5 107.5 . . ? C1 C2 N2 115.4(5) . . ? C1 C2 H6 108.4 . . ? N2 C2 H6 108.4 . . ? C1 C2 H7 108.4 . . ? N2 C2 H7 108.4 . . ? H6 C2 H7 107.5 . . ? C2 N2 C2 111.5(7) 6 . ? C2 N2 H8 109.3 6 . ? C2 N2 H8 109.3 . . ? C2 N2 H9 109.3 6 . ? C2 N2 H9 109.3 . . ? H8 N2 H9 108.0 . . ? C3 N3 H10 109.5 . . ? C3 N3 H11 109.5 . . ? H10 N3 H11 109.5 . . ? C3 N3 H12 109.5 . . ? H10 N3 H12 109.5 . . ? H11 N3 H12 109.5 . . ? C4 C3 N3 121.6(9) . . ? C4 C3 H13 106.9 . . ? N3 C3 H13 106.9 . . ? C4 C3 H14 106.9 . . ? N3 C3 H14 106.9 . . ? H13 C3 H14 106.7 . . ? N4 C4 N4 45.9(12) . 5_745 ? N4 C4 C3 139.4(8) . . ? N4 C4 C3 139.4(8) 5_745 . ? N4 N4 C4 67.0(6) 5_745 5_745 ? N4 N4 C4 67.0(6) 5_745 . ? C4 N4 C4 134.1(12) 5_745 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.631 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.126