data_chloro_methoxy_trifluoroethyl_pyrazinamine _vrf_PLAT027_chloro_methoxy_trifluoroethyl_pyrazinamine ; PROBLEM: _diffrn_reflns_theta_full (too) Low 60.00 RESPONSE: This experiment was done using Cu radiation: full set up to theta=60.00 with Cu radiation proved to be in great number of cases quite sufficient set of data for unambiguous determination of all structural details; in this case it was the simple question about regioisomerism, full set up to theta=60.00 is sufficient for this purpose. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H7 Cl F3 N3 O' _chemical_formula_weight 241.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 16.3661(6) _cell_length_b 6.7959(2) _cell_length_c 33.9544(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3776.5(2) _cell_formula_units_Z 16 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7832 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 68.14 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 3.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5927 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details SADASB _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 16261 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 68.33 _reflns_number_total 3394 _reflns_number_gt 2950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0379P)^2^+1.6004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00019(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3394 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Cl1 Cl 0.94588(2) 0.18874(6) 0.735726(12) 0.02097(12) Uani 1 1 d . . . F1 F 0.53993(6) 0.31149(17) 0.66775(3) 0.0253(2) Uani 1 1 d . . . F2 F 0.61570(7) 0.19637(16) 0.62118(3) 0.0225(2) Uani 1 1 d . . . F3 F 0.66150(7) 0.42312(16) 0.65959(3) 0.0250(2) Uani 1 1 d . . . O1 O 0.62626(7) 0.21301(19) 0.80352(3) 0.0195(3) Uani 1 1 d . . . N1 N 0.78639(9) 0.1778(2) 0.73283(4) 0.0152(3) Uani 1 1 d . . . N2 N 0.76623(9) 0.2275(2) 0.81401(4) 0.0184(3) Uani 1 1 d . . . N3 N 0.64492(8) 0.1611(2) 0.72623(4) 0.0170(3) Uani 1 1 d . . . H3N H 0.5968 0.1845 0.7368 0.020 Uiso 1 1 calc R . . C1 C 0.84953(10) 0.1961(2) 0.75770(5) 0.0165(3) Uani 1 1 d . . . C2 C 0.84211(10) 0.2204(3) 0.79739(5) 0.0185(3) Uani 1 1 d . . . H2 H 0.8895 0.2324 0.8134 0.022 Uiso 1 1 calc R . . C3 C 0.70392(10) 0.2092(2) 0.79052(5) 0.0152(3) Uani 1 1 d . . . C4 C 0.71272(10) 0.1829(2) 0.74883(5) 0.0146(3) Uani 1 1 d . . . C5 C 0.61532(12) 0.2295(3) 0.84559(5) 0.0292(4) Uani 1 1 d . . . H5A H 0.6424 0.1188 0.8587 0.044 Uiso 1 1 calc R . . H5B H 0.5569 0.2274 0.8518 0.044 Uiso 1 1 calc R . . H5C H 0.6392 0.3534 0.8548 0.044 Uiso 1 1 calc R . . C6 C 0.64875(10) 0.1013(3) 0.68560(5) 0.0181(3) Uani 1 1 d . . . H6A H 0.6162 -0.0201 0.6820 0.022 Uiso 1 1 calc R . . H6B H 0.7061 0.0712 0.6786 0.022 Uiso 1 1 calc R . . C7 C 0.61676(10) 0.2587(3) 0.65875(5) 0.0175(3) Uani 1 1 d . . . Cl1' Cl 0.94166(3) 0.26769(6) 0.915316(12) 0.02279(12) Uani 1 1 d . . . F1' F 0.80793(6) 0.20385(16) 1.10846(3) 0.0242(2) Uani 1 1 d . . . F2' F 0.93306(6) 0.30451(17) 1.10560(3) 0.0254(2) Uani 1 1 d . . . F3' F 0.88748(6) 0.09839(15) 1.06244(3) 0.0212(2) Uani 1 1 d . . . O1' O 0.63517(7) 0.30716(18) 0.99532(3) 0.0177(3) Uani 1 1 d . . . N1' N 0.84989(9) 0.3183(2) 0.97772(4) 0.0159(3) Uani 1 1 d . . . N2' N 0.70341(9) 0.2611(2) 0.93599(4) 0.0167(3) Uani 1 1 d . . . N3' N 0.77215(9) 0.3755(2) 1.03439(4) 0.0172(3) Uani 1 1 d . . . H3N' H 0.7238 0.3721 1.0457 0.021 Uiso 1 1 calc R . . C1' C 0.84742(11) 0.2798(2) 0.93892(5) 0.0167(3) Uani 1 1 d . . . C2' C 0.77737(11) 0.2531(2) 0.91766(5) 0.0174(3) Uani 1 1 d . . . H2' H 0.7803 0.2290 0.8901 0.021 Uiso 1 1 calc R . . C3' C 0.70410(10) 0.2971(2) 0.97365(5) 0.0146(3) Uani 1 1 d . . . C4' C 0.77773(10) 0.3306(2) 0.99533(5) 0.0149(3) Uani 1 1 d . . . C5' C 0.55902(10) 0.2825(3) 0.97437(5) 0.0204(4) Uani 1 1 d . . . H5A' H 0.5538 0.3858 0.9544 0.031 Uiso 1 1 calc R . . H5B' H 0.5134 0.2917 0.9930 0.031 Uiso 1 1 calc R . . H5C' H 0.5583 0.1533 0.9616 0.031 Uiso 1 1 calc R . . C7' C 0.84221(11) 0.4282(3) 1.05785(5) 0.0179(3) Uani 1 1 d . . . H7A' H 0.8287 0.5434 1.0745 0.021 Uiso 1 1 calc R . . H7B' H 0.8880 0.4653 1.0403 0.021 Uiso 1 1 calc R . . C8' C 0.86782(10) 0.2591(3) 1.08369(5) 0.0178(3) 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 Cl1 0.01031(19) 0.0305(2) 0.0221(2) -0.00069(15) 0.00022(14) 0.00131(15) F1 0.0139(5) 0.0410(6) 0.0210(5) 0.0005(4) -0.0016(4) 0.0070(4) F2 0.0258(5) 0.0309(6) 0.0109(4) -0.0006(4) -0.0031(4) 0.0003(4) F3 0.0281(6) 0.0253(5) 0.0217(5) 0.0007(4) -0.0021(4) -0.0085(4) O1 0.0135(6) 0.0323(7) 0.0128(6) 0.0001(5) 0.0010(4) -0.0012(5) N1 0.0130(7) 0.0183(7) 0.0144(6) -0.0004(5) -0.0003(5) 0.0013(5) N2 0.0168(7) 0.0237(8) 0.0146(6) 0.0003(6) -0.0019(5) -0.0010(6) N3 0.0108(6) 0.0272(8) 0.0130(6) -0.0008(6) -0.0007(5) 0.0009(5) C1 0.0115(8) 0.0176(8) 0.0203(8) 0.0006(6) -0.0005(6) -0.0002(6) C2 0.0141(8) 0.0233(9) 0.0183(8) 0.0002(7) -0.0041(6) -0.0008(7) C3 0.0149(8) 0.0167(8) 0.0140(8) 0.0005(6) 0.0000(6) -0.0009(6) C4 0.0145(8) 0.0153(7) 0.0139(7) 0.0022(6) -0.0013(6) 0.0000(6) C5 0.0228(9) 0.0521(13) 0.0126(8) -0.0011(8) 0.0044(7) -0.0024(9) C6 0.0163(8) 0.0237(9) 0.0143(8) -0.0016(7) -0.0031(6) 0.0003(7) C7 0.0132(8) 0.0255(9) 0.0138(8) -0.0026(7) -0.0007(6) -0.0016(7) Cl1' 0.0177(2) 0.0297(2) 0.0209(2) -0.00017(16) 0.00741(15) 0.00019(16) F1' 0.0201(5) 0.0354(6) 0.0171(5) 0.0057(4) 0.0044(4) 0.0008(4) F2' 0.0182(5) 0.0379(6) 0.0201(5) -0.0010(4) -0.0085(4) -0.0004(4) F3' 0.0194(5) 0.0241(5) 0.0202(5) -0.0016(4) -0.0002(4) 0.0029(4) O1' 0.0125(6) 0.0255(6) 0.0152(5) 0.0000(5) -0.0011(4) 0.0004(5) N1' 0.0151(7) 0.0159(7) 0.0167(7) 0.0024(5) 0.0004(5) -0.0001(5) N2' 0.0179(7) 0.0170(7) 0.0153(7) 0.0014(5) -0.0018(5) -0.0003(6) N3' 0.0137(7) 0.0245(8) 0.0135(6) -0.0010(6) -0.0009(5) 0.0008(6) C1' 0.0166(8) 0.0169(8) 0.0166(8) 0.0015(6) 0.0030(6) 0.0005(6) C2' 0.0216(9) 0.0174(8) 0.0132(7) -0.0007(6) 0.0009(6) 0.0008(7) C3' 0.0148(8) 0.0134(7) 0.0156(7) 0.0017(6) 0.0003(6) 0.0009(6) C4' 0.0170(8) 0.0136(7) 0.0142(7) 0.0021(6) -0.0009(6) 0.0010(6) C5' 0.0117(8) 0.0259(9) 0.0235(8) 0.0000(7) -0.0029(6) -0.0004(7) C7' 0.0178(8) 0.0213(8) 0.0145(7) -0.0015(6) -0.0037(6) -0.0014(7) C8' 0.0133(8) 0.0263(9) 0.0138(7) -0.0011(7) -0.0008(6) -0.0010(6) _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 Cl1 C1 1.7451(17) . ? F1 C7 1.343(2) . ? F2 C7 1.3442(19) . ? F3 C7 1.336(2) . ? O1 C3 1.346(2) . ? O1 C5 1.444(2) . ? N1 C4 1.323(2) . ? N1 C1 1.340(2) . ? N2 C3 1.301(2) . ? N2 C2 1.365(2) . ? N3 C4 1.357(2) . ? N3 C6 1.440(2) . ? N3 H3N 0.8800 . ? C1 C2 1.363(2) . ? C2 H2 0.9500 . ? C3 C4 1.434(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.500(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? Cl1' C1' 1.7401(17) . ? F1' C8' 1.345(2) . ? F2' C8' 1.338(2) . ? F3' C8' 1.348(2) . ? O1' C3' 1.348(2) . ? O1' C5' 1.445(2) . ? N1' C4' 1.326(2) . ? N1' C1' 1.344(2) . ? N2' C3' 1.302(2) . ? N2' C2' 1.362(2) . ? N3' C4' 1.364(2) . ? N3' C7' 1.442(2) . ? N3' H3N' 0.8800 . ? C1' C2' 1.367(3) . ? C2' H2' 0.9500 . ? C3' C4' 1.430(2) . ? C5' H5A' 0.9800 . ? C5' H5B' 0.9800 . ? C5' H5C' 0.9800 . ? C7' C8' 1.505(2) . ? C7' H7A' 0.9900 . ? C7' H7B' 0.9900 . ? 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 C3 O1 C5 116.30(13) . . ? C4 N1 C1 116.21(14) . . ? C3 N2 C2 117.16(15) . . ? C4 N3 C6 122.48(14) . . ? C4 N3 H3N 118.8 . . ? C6 N3 H3N 118.8 . . ? N1 C1 C2 124.43(15) . . ? N1 C1 Cl1 115.13(13) . . ? C2 C1 Cl1 120.44(13) . . ? C1 C2 N2 119.61(15) . . ? C1 C2 H2 120.2 . . ? N2 C2 H2 120.2 . . ? N2 C3 O1 122.51(15) . . ? N2 C3 C4 122.59(15) . . ? O1 C3 C4 114.90(14) . . ? N1 C4 N3 120.68(15) . . ? N1 C4 C3 120.01(15) . . ? N3 C4 C3 119.31(15) . . ? O1 C5 H5A 109.5 . . ? O1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 111.44(14) . . ? N3 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N3 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? F3 C7 F1 106.57(14) . . ? F3 C7 F2 106.93(13) . . ? F1 C7 F2 106.74(13) . . ? F3 C7 C6 113.08(14) . . ? F1 C7 C6 112.27(14) . . ? F2 C7 C6 110.87(14) . . ? C3' O1' C5' 116.56(13) . . ? C4' N1' C1' 115.30(15) . . ? C3' N2' C2' 116.64(15) . . ? C4' N3' C7' 122.66(14) . . ? C4' N3' H3N' 118.7 . . ? C7' N3' H3N' 118.7 . . ? N1' C1' C2' 124.66(16) . . ? N1' C1' Cl1' 115.72(13) . . ? C2' C1' Cl1' 119.61(13) . . ? N2' C2' C1' 119.93(15) . . ? N2' C2' H2' 120.0 . . ? C1' C2' H2' 120.0 . . ? N2' C3' O1' 122.55(15) . . ? N2' C3' C4' 122.86(15) . . ? O1' C3' C4' 114.59(14) . . ? N1' C4' N3' 120.81(15) . . ? N1' C4' C3' 120.55(15) . . ? N3' C4' C3' 118.65(15) . . ? O1' C5' H5A' 109.5 . . ? O1' C5' H5B' 109.5 . . ? H5A' C5' H5B' 109.5 . . ? O1' C5' H5C' 109.5 . . ? H5A' C5' H5C' 109.5 . . ? H5B' C5' H5C' 109.5 . . ? N3' C7' C8' 110.71(14) . . ? N3' C7' H7A' 109.5 . . ? C8' C7' H7A' 109.5 . . ? N3' C7' H7B' 109.5 . . ? C8' C7' H7B' 109.5 . . ? H7A' C7' H7B' 108.1 . . ? F2' C8' F1' 107.35(13) . . ? F2' C8' F3' 107.11(14) . . ? F1' C8' F3' 106.43(14) . . ? F2' C8' C7' 111.71(15) . . ? F1' C8' C7' 112.00(14) . . ? F3' C8' C7' 111.91(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N Cl1 0.88 2.64 3.5093(15) 169.5 8_557 N3' H3N' F3' 0.88 2.45 3.1665(17) 138.8 6_765 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.260 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.052 #===END data_chloro_trifluoroethylamino_pyrazinecarbonitrile _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H4 Cl F3 N4' _chemical_formula_weight 236.59 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 9.531(2) _cell_length_b 8.997(2) _cell_length_c 11.626(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.605(10) _cell_angle_gamma 90.00 _cell_volume 939.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3370 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 24.98 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 6677 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 25.07 _reflns_number_total 1644 _reflns_number_gt 1228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0600P)^2^+0.5700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1644 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Cl1 Cl 0.01022(7) 0.05613(7) 0.20894(7) 0.0243(2) Uani 1 1 d . . . F1 F -0.0710(2) -0.6506(2) 0.39581(17) 0.0435(5) Uani 1 1 d . . . F2 F -0.21863(19) -0.6021(2) 0.21340(17) 0.0405(5) Uani 1 1 d . . . F3 F -0.15059(19) -0.4276(2) 0.34954(18) 0.0442(5) Uani 1 1 d . . . N1 N 0.3014(3) 0.2644(3) 0.4523(2) 0.0263(6) Uani 1 1 d . . . N2 N 0.3336(2) -0.1126(3) 0.4911(2) 0.0207(5) Uani 1 1 d . . . N3 N 0.0888(2) -0.2104(2) 0.2943(2) 0.0182(5) Uani 1 1 d . . . N4 N 0.1501(2) -0.4530(2) 0.3595(2) 0.0212(5) Uani 1 1 d . . . H4A H 0.2120 -0.5140 0.4114 0.025 Uiso 1 1 calc R . . C1 C 0.2748(3) 0.1403(3) 0.4339(2) 0.0211(6) Uani 1 1 d . . . C2 C 0.2413(3) -0.0158(3) 0.4111(2) 0.0189(6) Uani 1 1 d . . . C3 C 0.3031(3) -0.2541(3) 0.4727(2) 0.0208(6) Uani 1 1 d . . . H3A H 0.3664 -0.3244 0.5265 0.025 Uiso 1 1 calc R . . C4 C 0.1229(3) -0.0677(3) 0.3145(2) 0.0186(6) Uani 1 1 d . . . C5 C 0.1779(3) -0.3063(3) 0.3747(2) 0.0179(6) Uani 1 1 d . . . C6 C 0.0259(3) -0.5172(3) 0.2643(2) 0.0201(6) Uani 1 1 d . . . H6A H 0.0583 -0.6110 0.2363 0.024 Uiso 1 1 calc R . . H6B H -0.0059 -0.4482 0.1940 0.024 Uiso 1 1 calc R . . C7 C -0.1040(3) -0.5485(3) 0.3057(3) 0.0288(7) 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 Cl1 0.0239(4) 0.0133(4) 0.0263(4) 0.0032(3) -0.0041(3) 0.0015(3) F1 0.0564(12) 0.0427(13) 0.0340(11) 0.0040(9) 0.0185(10) -0.0151(10) F2 0.0303(9) 0.0469(12) 0.0385(11) -0.0159(9) 0.0041(9) -0.0159(8) F3 0.0303(10) 0.0472(13) 0.0564(13) -0.0264(10) 0.0163(10) -0.0046(8) N1 0.0271(13) 0.0174(14) 0.0271(14) 0.0010(11) -0.0005(12) 0.0005(11) N2 0.0227(12) 0.0153(12) 0.0194(12) 0.0006(10) 0.0010(11) 0.0012(10) N3 0.0202(12) 0.0111(12) 0.0198(13) 0.0003(9) 0.0023(10) 0.0014(9) N4 0.0247(12) 0.0112(12) 0.0217(13) 0.0020(9) -0.0001(10) 0.0011(9) C1 0.0199(14) 0.0200(17) 0.0180(15) 0.0013(12) -0.0009(12) 0.0023(11) C2 0.0214(14) 0.0140(14) 0.0201(15) 0.0005(11) 0.0052(12) -0.0007(11) C3 0.0242(14) 0.0143(15) 0.0180(15) 0.0035(11) -0.0006(13) 0.0045(11) C4 0.0185(13) 0.0159(15) 0.0184(15) 0.0040(11) 0.0022(12) 0.0024(11) C5 0.0188(13) 0.0136(15) 0.0193(14) -0.0002(11) 0.0037(12) 0.0002(11) C6 0.0262(15) 0.0124(14) 0.0168(14) -0.0007(11) 0.0008(12) -0.0001(11) C7 0.0319(16) 0.0234(17) 0.0272(17) -0.0058(14) 0.0046(14) -0.0034(13) _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 Cl1 C4 1.737(3) . ? F1 C7 1.348(4) . ? F2 C7 1.338(3) . ? F3 C7 1.339(3) . ? N1 C1 1.149(3) . ? N2 C3 1.308(3) . ? N2 C2 1.359(4) . ? N3 C4 1.326(3) . ? N3 C5 1.344(3) . ? N4 C5 1.346(3) . ? N4 C6 1.443(3) . ? N4 H4A 0.8800 . ? C1 C2 1.445(4) . ? C2 C4 1.379(4) . ? C3 C5 1.425(4) . ? C3 H3A 0.9500 . ? C6 C7 1.498(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 C3 N2 C2 117.0(2) . . ? C4 N3 C5 116.0(2) . . ? C5 N4 C6 124.6(2) . . ? C5 N4 H4A 117.7 . . ? C6 N4 H4A 117.7 . . ? N1 C1 C2 179.8(3) . . ? N2 C2 C4 120.4(2) . . ? N2 C2 C1 116.4(2) . . ? C4 C2 C1 123.3(2) . . ? N2 C3 C5 122.2(2) . . ? N2 C3 H3A 118.9 . . ? C5 C3 H3A 118.9 . . ? N3 C4 C2 123.8(2) . . ? N3 C4 Cl1 116.0(2) . . ? C2 C4 Cl1 120.1(2) . . ? N3 C5 N4 119.2(2) . . ? N3 C5 C3 120.6(2) . . ? N4 C5 C3 120.2(2) . . ? N4 C6 C7 112.5(2) . . ? N4 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N4 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? F3 C7 F2 108.2(2) . . ? F3 C7 F1 106.2(2) . . ? F2 C7 F1 107.0(2) . . ? F3 C7 C6 112.6(2) . . ? F2 C7 C6 110.5(2) . . ? F1 C7 C6 112.0(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.414 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.070 #===END data_dichloropyrazine_carbonitrile _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H Cl2 N3' _chemical_formula_sum 'C5 H Cl2 N3' _chemical_formula_weight 173.99 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 10.9565(10) _cell_length_b 5.7167(6) _cell_length_c 16.5950(15) _cell_angle_alpha 90 _cell_angle_beta 108.605(3) _cell_angle_gamma 90 _cell_volume 985.11(16) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2219 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 26.32 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_F_000 516 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.897 _shelx_estimated_absorpt_T_min 0.877 _shelx_estimated_absorpt_T_max 0.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6398 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'micro-focus sealed tube' _diffrn_measurement_device_type 'Bruker Photon 100 CMOS CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '1024 x 1024' _diffrn_reflns_number 6211 _diffrn_reflns_av_unetI/netI 0.0401 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.590 _diffrn_reflns_theta_max 26.350 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 2007 _reflns_number_gt 1556 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.5977P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2007 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.99887(6) 0.33385(11) 1.24216(3) 0.02783(18) Uani 1 1 d . . . . . Cl2 Cl 0.64844(6) 0.15599(14) 0.95449(3) 0.0381(2) Uani 1 1 d . . . . . N1 N 0.82297(17) 0.2156(3) 1.10124(11) 0.0194(4) Uani 1 1 d . . . . . N2 N 0.76016(17) -0.2009(4) 1.16814(11) 0.0208(4) Uani 1 1 d . . . . . N3 N 0.96390(19) -0.1618(4) 1.37329(12) 0.0259(5) Uani 1 1 d . . . . . C1 C 0.8811(2) 0.1514(4) 1.18088(13) 0.0177(5) Uani 1 1 d . . . . . C2 C 0.8499(2) -0.0532(4) 1.21515(13) 0.0172(5) Uani 1 1 d . . . . . C3 C 0.9131(2) -0.1149(4) 1.30340(14) 0.0195(5) Uani 1 1 d . . . . . C4 C 0.7323(2) 0.0708(5) 1.05659(13) 0.0218(5) Uani 1 1 d . . . . . C5 C 0.7014(2) -0.1387(4) 1.08791(14) 0.0220(5) Uani 1 1 d . . . . . H5 H 0.6378 -0.2382 1.0517 0.026 Uiso 1 1 calc R U . . . Cl1' Cl 0.77840(12) 0.6763(2) 0.90367(7) 0.0262(3) Uani 0.5 1 d . . P A -1 Cl2' Cl 1.1560(2) 0.7851(4) 1.18509(18) 0.0259(5) Uani 0.5 1 d . . P A -1 N1' N 0.9746(7) 0.7042(10) 1.0425(4) 0.0185(11) Uani 0.5 1 d . . P A -1 N2' N 1.0829(5) 0.2852(11) 1.0122(4) 0.0251(11) Uani 0.5 1 d . . P A -1 N3' N 0.8693(10) 0.1346(14) 0.8195(7) 0.037(2) Uani 0.5 1 d . . P A -1 C1' C 0.9197(5) 0.5780(12) 0.9735(4) 0.0170(10) Uani 0.5 1 d . . P A -1 C2' C 0.9728(8) 0.3694(11) 0.9573(5) 0.0198(13) Uani 0.5 1 d . . P A -1 C3' C 0.9148(5) 0.2358(12) 0.8804(4) 0.0222(11) Uani 0.5 1 d . . P A -1 C4' C 1.0824(6) 0.6220(11) 1.0957(5) 0.0212(12) Uani 0.5 1 d . . P A -1 C5' C 1.1376(5) 0.4111(9) 1.0812(4) 0.0231(11) Uani 0.5 1 d . . P A -1 H5' H 1.2154 0.3580 1.1215 0.028 Uiso 0.5 1 calc R U P A -1 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 Cl1 0.0344(3) 0.0218(3) 0.0236(3) -0.0022(2) 0.0041(3) -0.0111(3) Cl2 0.0312(3) 0.0650(5) 0.0164(3) 0.0065(3) 0.0052(2) -0.0161(3) N1 0.0200(10) 0.0223(11) 0.0181(9) -0.0020(8) 0.0094(8) 0.0005(8) N2 0.0205(10) 0.0224(12) 0.0225(10) -0.0039(8) 0.0110(8) -0.0039(8) N3 0.0251(11) 0.0249(12) 0.0272(11) 0.0033(9) 0.0076(9) 0.0010(9) C1 0.0175(11) 0.0166(12) 0.0212(11) -0.0050(9) 0.0092(9) 0.0017(9) C2 0.0154(11) 0.0181(13) 0.0205(11) -0.0020(9) 0.0091(9) 0.0017(9) C3 0.0176(11) 0.0151(13) 0.0272(13) -0.0020(10) 0.0091(10) -0.0003(9) C4 0.0195(11) 0.0319(15) 0.0173(10) -0.0032(10) 0.0103(9) -0.0012(10) C5 0.0195(11) 0.0289(15) 0.0209(11) -0.0065(10) 0.0111(9) -0.0066(10) Cl1' 0.0272(7) 0.0227(7) 0.0265(6) 0.0014(5) 0.0054(5) 0.0074(6) Cl2' 0.0237(9) 0.0314(13) 0.0242(8) -0.0021(10) 0.0099(7) -0.0075(9) N1' 0.025(3) 0.018(3) 0.020(3) 0.003(2) 0.017(3) -0.002(2) N2' 0.029(3) 0.022(3) 0.030(3) 0.003(3) 0.017(3) 0.003(2) N3' 0.049(5) 0.029(5) 0.039(4) -0.005(4) 0.023(4) 0.004(3) C1' 0.018(3) 0.016(3) 0.019(3) 0.006(3) 0.010(3) 0.001(2) C2' 0.021(3) 0.017(3) 0.028(4) -0.001(3) 0.018(3) 0.001(3) C3' 0.026(3) 0.017(3) 0.029(3) 0.000(3) 0.017(3) 0.000(2) C4' 0.021(3) 0.029(4) 0.016(3) 0.002(3) 0.008(2) -0.008(2) C5' 0.016(3) 0.021(3) 0.032(3) 0.011(2) 0.007(2) 0.007(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 Cl1 C1 1.718(2) . ? Cl2 C4 1.720(2) . ? N1 C1 1.323(3) . ? N1 C4 1.323(3) . ? N2 C5 1.329(3) . ? N2 C2 1.341(3) . ? N3 C3 1.147(3) . ? C1 C2 1.390(3) . ? C2 C3 1.450(3) . ? C4 C5 1.390(3) . ? C5 H5 0.9500 . ? Cl1' C1' 1.705(6) . ? Cl2' C4' 1.720(9) . ? N1' C4' 1.315(8) . ? N1' C1' 1.325(9) . ? N2' C5' 1.322(8) . ? N2' C2' 1.347(10) . ? N3' C3' 1.132(11) . ? C1' C2' 1.390(8) . ? C2' C3' 1.450(9) . ? C4' C5' 1.404(8) . ? C5' H5' 0.9500 . ? 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 C1 N1 C4 115.0(2) . . ? C5 N2 C2 116.4(2) . . ? N1 C1 C2 122.6(2) . . ? N1 C1 Cl1 117.03(18) . . ? C2 C1 Cl1 120.33(16) . . ? N2 C2 C1 121.47(19) . . ? N2 C2 C3 117.4(2) . . ? C1 C2 C3 121.2(2) . . ? N3 C3 C2 179.3(3) . . ? N1 C4 C5 124.0(2) . . ? N1 C4 Cl2 116.37(19) . . ? C5 C4 Cl2 119.67(18) . . ? N2 C5 C4 120.5(2) . . ? N2 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C4' N1' C1' 116.7(7) . . ? C5' N2' C2' 116.8(6) . . ? N1' C1' C2' 122.1(6) . . ? N1' C1' Cl1' 118.1(6) . . ? C2' C1' Cl1' 119.8(7) . . ? N2' C2' C1' 121.1(6) . . ? N2' C2' C3' 117.0(7) . . ? C1' C2' C3' 121.9(9) . . ? N3' C3' C2' 178.9(8) . . ? N1' C4' C5' 122.4(8) . . ? N1' C4' Cl2' 117.3(5) . . ? C5' C4' Cl2' 120.3(6) . . ? N2' C5' C4' 121.0(7) . . ? N2' C5' H5' 119.5 . . ? C4' C5' H5' 119.5 . . ? _refine_diff_density_max 0.341 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.069 #===END