# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_GUANX _database_code_depnum_ccdc_archive 'CCDC 888680' #TrackingRef 'Guan_X_pub.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Guanidinium Carbamoyldicyanomethanide ; _chemical_name_common 'Guanidinium Carbamoyldicyanomethanide' _chemical_melting_point ? _chemical_formula_moiety 'C4 H2 N3 O, C H6 N3' _chemical_formula_sum 'C5 H8 N6 O' _chemical_formula_weight 168.17 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.8489(7) _cell_length_b 4.9807(4) _cell_length_c 18.7046(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.158(2) _cell_angle_gamma 90.00 _cell_volume 811.46(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 4388 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9692 _exptl_absorpt_correction_T_max 0.9917 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4388 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1832 _reflns_number_gt 1692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 1832 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 O1 O 0.06445(9) 0.74208(17) 0.07465(5) 0.0231(2) Uani 1 1 d . . . N1 N 0.20580(12) 0.4468(2) 0.02283(6) 0.0208(2) Uani 1 1 d . . . N2 N 0.59249(12) 0.5538(2) 0.09846(6) 0.0237(2) Uani 1 1 d . . . N3 N 0.31441(13) 1.1549(2) 0.19608(6) 0.0263(3) Uani 1 1 d . . . N4 N -0.13307(13) 1.1508(2) 0.11576(6) 0.0228(2) Uani 1 1 d . . . N5 N -0.08734(12) 0.8040(2) 0.19776(6) 0.0207(2) Uani 1 1 d . . . N6 N -0.28261(12) 1.1040(2) 0.20395(6) 0.0208(2) Uani 1 1 d . . . C1 C 0.33367(13) 0.7675(2) 0.10803(6) 0.0172(2) Uani 1 1 d . . . C2 C 0.47741(13) 0.6553(2) 0.10392(6) 0.0178(2) Uani 1 1 d . . . C3 C 0.32319(13) 0.9815(2) 0.15597(6) 0.0182(2) Uani 1 1 d . . . C4 C 0.19437(13) 0.6525(2) 0.06777(6) 0.0168(2) Uani 1 1 d . . . C5 C -0.16997(12) 1.0185(2) 0.17165(6) 0.0170(2) Uani 1 1 d . . . H1A H 0.1225(18) 0.382(3) -0.0031(8) 0.030(4) Uiso 1 1 d . . . H1B H 0.2955(19) 0.389(3) 0.0155(8) 0.031(4) Uiso 1 1 d . . . H4A H -0.0584(19) 1.087(3) 0.0948(9) 0.032(4) Uiso 1 1 d . . . H4B H -0.192(2) 1.285(3) 0.0964(9) 0.037(4) Uiso 1 1 d . . . H5A H -0.1272(19) 0.702(3) 0.2292(9) 0.034(4) Uiso 1 1 d . . . H5B H -0.0258(19) 0.739(3) 0.1707(9) 0.034(4) Uiso 1 1 d . . . H6A H -0.3389(19) 1.246(3) 0.1855(9) 0.038(4) Uiso 1 1 d . . . H6B H -0.3117(19) 1.003(4) 0.2386(10) 0.040(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0160(4) 0.0269(4) 0.0273(5) -0.0059(4) 0.0060(3) 0.0034(3) N1 0.0159(5) 0.0239(5) 0.0223(5) -0.0060(4) 0.0026(4) 0.0032(4) N2 0.0195(5) 0.0255(5) 0.0260(5) -0.0030(4) 0.0038(4) 0.0038(4) N3 0.0317(6) 0.0221(5) 0.0269(6) -0.0033(4) 0.0104(4) 0.0006(4) N4 0.0243(6) 0.0218(5) 0.0249(5) 0.0053(4) 0.0115(4) 0.0063(4) N5 0.0203(5) 0.0196(5) 0.0230(5) 0.0034(4) 0.0061(4) 0.0041(4) N6 0.0211(5) 0.0194(5) 0.0237(5) 0.0012(4) 0.0087(4) 0.0035(4) C1 0.0166(5) 0.0167(5) 0.0190(5) -0.0010(4) 0.0048(4) 0.0027(4) C2 0.0196(6) 0.0171(5) 0.0164(5) -0.0012(4) 0.0023(4) -0.0015(4) C3 0.0174(6) 0.0177(5) 0.0202(5) 0.0038(4) 0.0051(4) 0.0007(4) C4 0.0172(5) 0.0170(5) 0.0168(5) 0.0030(4) 0.0050(4) 0.0025(4) C5 0.0168(6) 0.0162(5) 0.0175(5) -0.0029(4) 0.0015(4) -0.0016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C4 1.2608(14) . ? N1 C4 1.3400(15) . ? N1 H1A 0.870(16) . ? N1 H1B 0.878(16) . ? N2 C2 1.1573(16) . ? N3 C3 1.1553(15) . ? N4 C5 1.3244(15) . ? N4 H4A 0.886(17) . ? N4 H4B 0.887(17) . ? N5 C5 1.3375(15) . ? N5 H5A 0.896(17) . ? N5 H5B 0.869(18) . ? N6 C5 1.3238(15) . ? N6 H6A 0.899(17) . ? N6 H6B 0.894(19) . ? C1 C2 1.4037(16) . ? C1 C3 1.4067(16) . ? C1 C4 1.4447(15) . ? 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 C4 N1 H1A 118.9(10) . . ? C4 N1 H1B 121.4(10) . . ? H1A N1 H1B 119.3(14) . . ? C5 N4 H4A 118.5(10) . . ? C5 N4 H4B 119.3(11) . . ? H4A N4 H4B 121.5(15) . . ? C5 N5 H5A 116.2(10) . . ? C5 N5 H5B 116.3(11) . . ? H5A N5 H5B 122.0(15) . . ? C5 N6 H6A 119.2(11) . . ? C5 N6 H6B 119.2(11) . . ? H6A N6 H6B 120.7(15) . . ? C2 C1 C3 119.92(10) . . ? C2 C1 C4 120.77(10) . . ? C3 C1 C4 119.12(10) . . ? N2 C2 C1 176.87(12) . . ? N3 C3 C1 179.07(13) . . ? O1 C4 N1 120.38(10) . . ? O1 C4 C1 121.06(10) . . ? N1 C4 C1 118.56(10) . . ? N6 C5 N4 120.70(11) . . ? N6 C5 N5 119.83(11) . . ? N4 C5 N5 119.39(11) . . ? 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 N1 H1A O1 0.870(16) 2.032(16) 2.8967(13) 172.6(14) 3_565 N1 H1B N2 0.878(16) 2.520(16) 3.1243(15) 126.6(13) 3_665 N4 H4A O1 0.886(17) 2.101(17) 2.8750(14) 145.5(14) . N4 H4B N2 0.887(17) 2.334(18) 3.1231(15) 148.2(15) 1_465 N5 H5A N3 0.896(17) 2.360(17) 3.1526(16) 147.5(14) 2_545 N5 H5B O1 0.869(18) 2.090(18) 2.8798(15) 150.7(14) . N6 H6A N2 0.899(17) 2.240(17) 3.0603(15) 151.5(15) 1_465 N6 H6B N3 0.894(19) 2.124(19) 2.9607(15) 155.6(15) 2_545 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.268 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.041 data_guanN _database_code_depnum_ccdc_archive 'CCDC 888681' #TrackingRef 'guan_N_pub.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 'Guanidinium Carbamoyldicyanomethanide' _chemical_melting_point ? _chemical_formula_moiety 'C H6 N3, C4 H2 N3 O' _chemical_formula_sum 'C5 H8 N6 O' _chemical_formula_weight 168.16 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source H 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 -3.7409 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' C 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 6.6484 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' N 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 9.3600 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' O 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 5.8050 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.8489(7) _cell_length_b 4.9807(4) _cell_length_c 18.7046(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.158(2) _cell_angle_gamma 90.00 _cell_volume 811.46(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid 1.00 _exptl_crystal_size_min 1.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 261 _exptl_absorpt_coefficient_mu none _exptl_absorpt_correction_type none _exptl_special_details 'Laue neutron diffraction study' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.8-1.6 _diffrn_radiation_type neutron _diffrn_radiation_source 'OPAL nuclear reactor' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'KOALA Laue ' _diffrn_measurement_method Laue _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12844 _diffrn_reflns_av_R_equivalents 0.1143 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.63 _diffrn_reflns_theta_max 26.43 _reflns_number_total 1361 _reflns_number_gt 1130 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MAATEL software for control of the instrument KOALA ; _computing_cell_refinement 'not applicable' _computing_data_reduction ; LAUE1234 (Piltz R.O. 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0338P)^2^+0.1958P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1361 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 O1 O 0.06461(18) 0.7413(3) 0.07432(8) 0.0279(3) Uani 1 1 d . . . N1 N 0.20599(13) 0.44670(18) 0.02226(5) 0.0256(2) Uani 1 1 d . . . N2 N 0.59109(11) 0.55064(19) 0.09894(5) 0.0300(2) Uani 1 1 d . . . N3 N 0.31322(13) 1.15171(19) 0.19581(5) 0.0331(2) Uani 1 1 d . . . N4 N -0.13393(12) 1.14888(19) 0.11551(5) 0.0286(2) Uani 1 1 d . . . N5 N -0.08766(11) 0.80257(18) 0.19738(5) 0.0252(2) Uani 1 1 d . . . N6 N -0.28338(11) 1.10115(18) 0.20388(5) 0.0256(2) Uani 1 1 d . . . C1 C 0.33264(15) 0.7656(2) 0.10786(6) 0.0201(3) Uani 1 1 d . . . C2 C 0.47568(14) 0.6533(2) 0.10407(6) 0.0219(3) Uani 1 1 d . . . C3 C 0.32225(16) 0.9783(2) 0.15552(6) 0.0221(3) Uani 1 1 d . . . C4 C 0.19395(13) 0.6519(2) 0.06758(5) 0.0196(2) Uani 1 1 d . . . C5 C -0.17033(14) 1.0164(2) 0.17150(6) 0.0189(3) Uani 1 1 d . . . H1 H 0.1089(3) 0.3696(5) -0.00763(13) 0.0354(6) Uani 1 1 d . . . H2 H -0.1267(4) 0.6869(6) 0.23421(16) 0.0445(7) Uani 1 1 d . . . H3 H -0.3460(4) 1.2598(5) 0.18371(16) 0.0423(7) Uani 1 1 d . . . H4 H -0.0500(4) 1.0737(6) 0.09108(15) 0.0433(6) Uani 1 1 d . . . H5 H -0.0153(4) 0.7255(5) 0.16655(15) 0.0396(6) Uani 1 1 d . . . H6 H -0.3131(4) 0.9883(5) 0.24377(15) 0.0422(6) Uani 1 1 d . . . H7 H -0.1999(4) 1.3024(6) 0.09431(15) 0.0450(7) Uani 1 1 d . . . H8 H 0.3071(4) 0.3837(6) 0.01315(16) 0.0460(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 O1 0.0150(9) 0.0340(8) 0.0355(7) -0.0100(5) 0.0066(6) 0.0039(5) N1 0.0214(7) 0.0289(4) 0.0263(4) -0.0078(3) 0.0037(4) 0.0046(4) N2 0.0193(6) 0.0340(5) 0.0368(5) -0.0033(4) 0.0052(4) 0.0087(4) N3 0.0442(6) 0.0252(5) 0.0328(4) -0.0076(4) 0.0145(4) 0.0002(4) N4 0.0313(6) 0.0272(5) 0.0307(4) 0.0063(4) 0.0150(4) 0.0071(4) N5 0.0235(5) 0.0235(4) 0.0292(4) 0.0039(4) 0.0062(4) 0.0066(4) N6 0.0245(5) 0.0244(5) 0.0305(4) -0.0001(4) 0.0119(4) 0.0046(4) C1 0.0163(7) 0.0217(6) 0.0229(5) -0.0022(4) 0.0049(5) 0.0027(4) C2 0.0165(7) 0.0249(6) 0.0246(5) -0.0010(4) 0.0046(4) 0.0038(5) C3 0.0249(7) 0.0201(6) 0.0228(5) -0.0015(4) 0.0085(5) 0.0025(4) C4 0.0166(6) 0.0215(6) 0.0217(5) -0.0010(4) 0.0057(4) 0.0034(4) C5 0.0186(7) 0.0176(5) 0.0211(5) 0.0004(4) 0.0049(4) 0.0022(4) H1 0.0270(15) 0.0395(14) 0.0400(12) -0.0110(10) 0.0063(11) -0.0015(11) H2 0.0509(19) 0.0355(13) 0.0493(14) 0.0144(12) 0.0144(13) 0.0041(13) H3 0.0381(18) 0.0357(15) 0.0557(16) 0.0023(11) 0.0158(13) 0.0128(12) H4 0.0411(18) 0.0472(15) 0.0477(14) 0.0038(12) 0.0242(13) 0.0074(13) H5 0.0339(17) 0.0389(14) 0.0481(14) -0.0001(10) 0.0135(13) 0.0124(11) H6 0.0408(19) 0.0452(15) 0.0456(14) 0.0049(12) 0.0216(12) 0.0031(12) H7 0.052(2) 0.0382(14) 0.0458(14) 0.0134(12) 0.0115(13) 0.0141(15) H8 0.0274(18) 0.0520(17) 0.0584(16) -0.0222(13) 0.0076(13) 0.0092(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 O1 C4 1.2548(19) . ? N1 C4 1.3441(14) . ? N1 H1 1.014(3) . ? N1 H8 0.991(4) . ? N2 C2 1.1611(15) . ? N3 C3 1.1583(14) . ? N4 C5 1.3246(14) . ? N4 H4 1.010(3) . ? N4 H7 1.001(3) . ? N5 C5 1.3338(14) . ? N5 H2 1.005(3) . ? N5 H5 1.010(3) . ? N6 C5 1.3265(15) . ? N6 H3 1.000(3) . ? N6 H6 1.006(3) . ? C1 C2 1.3970(17) . ? C1 C3 1.3981(16) . ? C1 C4 1.4380(17) . ? 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 C4 N1 H1 118.82(18) . . ? C4 N1 H8 121.58(19) . . ? H1 N1 H8 119.2(2) . . ? C5 N4 H4 118.28(18) . . ? C5 N4 H7 119.2(2) . . ? H4 N4 H7 121.9(2) . . ? C5 N5 H2 118.29(19) . . ? C5 N5 H5 117.31(17) . . ? H2 N5 H5 120.2(2) . . ? C5 N6 H3 119.42(19) . . ? C5 N6 H6 118.57(19) . . ? H3 N6 H6 121.4(3) . . ? C2 C1 C3 119.85(11) . . ? C2 C1 C4 120.86(10) . . ? C3 C1 C4 119.10(11) . . ? N2 C2 C1 176.86(12) . . ? N3 C3 C1 178.96(13) . . ? O1 C4 N1 120.54(12) . . ? O1 C4 C1 121.14(11) . . ? N1 C4 C1 118.32(10) . . ? N6 C5 N4 120.71(10) . . ? N6 C5 N5 119.86(10) . . ? N4 C5 N5 119.37(11) . . ? _diffrn_measured_fraction_theta_max 0.814 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.814 _refine_diff_density_max 0.388 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.095 # start Validation Reply Form _vrf_TYPE031_I ; PROBLEM: _diffrn_radiation_wavelength is not of type numb. RESPONSE: Wavelength is a range - Laue data ; _vrf_CELL004_I ; PROBLEM: _cell_measurement_theta_min is missing RESPONSE: cell dimensions not defined by Laue data ; _vrf_CELL005_I ; PROBLEM: _cell_measurement_theta_max is missing RESPONSE: cell dimensions not defined by Laue data ; _vrf_DIFF019_I ; PROBLEM: _diffrn_standards_number is missing RESPONSE: Internal comparisons of Laue data applied ; _vrf_DIFF020_I ; PROBLEM: _diffrn_standards_interval_count and RESPONSE: not required in Laue data collection ; _vrf_DIFF022_I ; PROBLEM: _diffrn_standards_decay_% is missing RESPONSE: Laue data ; _vrf_ABSTY01_I ; PROBLEM: The absorption correction should be one of the following RESPONSE: ... ; _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.814 RESPONSE: This is an acceptable velue for Laue neutron data ; _vrf_PLAT091_I ; PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed RESPONSE: multiple wavelength Laue data ; _vrf_PLAT050_I ; PROBLEM: Absorption Coefficient mu Missing RESPONSE: Absorption varies with wavelength for neutrons no single value is reportable ; # end Validation Reply Form