# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_email KATRAN@AMU.EDU.PL _publ_section_title ; Density, Freezing and Molecular Aggregation in Pyridazine, Pyridine and Benzene ; loop_ _publ_author_name 'Andrzej Katrusiak' 'Katarzyna Jakobek' 'Marcin Podsiadlo' # Attachment 'all.txt' data_1pir_0.27GPa _database_code_depnum_ccdc_archive 'CCDC 759555' #TrackingRef 'all.txt' # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; pyridazine ; _chemical_name_common pyridazine _chemical_melting_point 265 _chemical_formula_moiety 'C4 H4 N2' _chemical_formula_sum 'C4 H4 N2' _chemical_formula_weight 80.09 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' # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 3.8432(8) _cell_length_b 10.964(2) _cell_length_c 9.778(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.13(3) _cell_angle_gamma 90.00 _cell_volume 411.95(15) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2829 _cell_measurement_theta_min 4.17 _cell_measurement_theta_max 24.99 _exptl_crystal_description cylinder _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 168 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.26 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details ; Correction for absorption of the diamond-anvil cell and the sample were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam Mickiewicz University Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr. 219, 461-467). ; # EXPERIMENTAL DATA _exptl_special_details ; Data were collected at room temperature and pressure of 0.27(5) GPa (270000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 295(2) _diffrn_ambient_environment 'diamond-anvil cell' _diffrn_ambient_pressure 270000 _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 'KM-4 CCD' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2829 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 24.99 _reflns_number_total 301 _reflns_number_gt 234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)' _computing_structure_solution 'SHELXS--97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL--97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXL--97 (Sheldrick, 1997)' # REFINEMENT DATA _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. The DAC imposes severe restrictions on which reflections can be collected, resulting in a low data:parameter ratio. ; _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^)+(0.0830P)^2^+0.1292P] 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 0.81(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 301 _refine_ls_number_parameters 56 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1686 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 N1 N -0.0416(11) 0.8574(11) 0.3820(4) 0.079(4) Uani 1 1 d U . . N2 N -0.1200(10) 0.7472(10) 0.3047(4) 0.072(4) Uani 1 1 d U . . C3 C -0.0448(12) 0.7605(10) 0.1738(5) 0.059(4) Uani 1 1 d U . . H3 H -0.1061 0.6951 0.1176 0.070 Uiso 1 1 calc R . . C4 C 0.1073(11) 0.8548(11) 0.1103(4) 0.052(3) Uani 1 1 d U . . H4 H 0.1562 0.8525 0.0176 0.062 Uiso 1 1 calc R . . C5 C 0.1854(11) 0.9533(11) 0.1885(5) 0.074(4) Uani 1 1 d U . . H5 H 0.2964 1.0202 0.1505 0.089 Uiso 1 1 calc R . . C6 C 0.0988(12) 0.9538(12) 0.3256(5) 0.071(4) Uani 1 1 d U . . H6 H 0.1408 1.0232 0.3782 0.085 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 N1 0.078(3) 0.100(11) 0.059(2) 0.006(4) 0.0105(19) -0.003(4) N2 0.074(3) 0.078(11) 0.065(2) -0.008(4) 0.0018(17) -0.005(4) C3 0.070(3) 0.052(11) 0.053(2) -0.015(4) -0.0045(19) 0.015(4) C4 0.062(2) 0.056(11) 0.039(2) -0.004(4) 0.0033(17) 0.012(4) C5 0.066(3) 0.099(11) 0.058(3) 0.021(4) 0.0092(19) 0.006(4) C6 0.071(3) 0.084(12) 0.058(3) -0.016(4) -0.0028(19) 0.009(4) # MOLECULAR GEOMETRY _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 N1 C6 1.313(15) . ? N1 N2 1.454(13) . ? N2 C3 1.327(7) . ? C3 C4 1.346(13) . ? C3 H3 0.9300 . ? C4 C5 1.353(15) . ? C4 H4 0.9300 . ? C5 C6 1.388(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? 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 C6 N1 N2 122.3(5) . . ? C3 N2 N1 111.3(8) . . ? N2 C3 C4 129.4(9) . . ? N2 C3 H3 115.3 . . ? C4 C3 H3 115.3 . . ? C3 C4 C5 116.6(6) . . ? C3 C4 H4 121.7 . . ? C5 C4 H4 121.7 . . ? C4 C5 C6 119.6(9) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? N1 C6 C5 120.7(9) . . ? N1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 N2 C3 -2.5(8) . . . . ? N1 N2 C3 C4 4.8(9) . . . . ? N2 C3 C4 C5 -2.8(9) . . . . ? C3 C4 C5 C6 -1.7(9) . . . . ? N2 N1 C6 C5 -1.3(10) . . . . ? C4 C5 C6 N1 3.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.414 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.414 _refine_diff_density_max 0.109 _refine_diff_density_min -0.132 _refine_diff_density_rms 0.026 data_2pir_0.61GPa _database_code_depnum_ccdc_archive 'CCDC 759556' #TrackingRef 'all.txt' # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; pyridazine ; _chemical_name_common pyridazine _chemical_melting_point 265 _chemical_formula_moiety 'C4 H4 N2' _chemical_formula_sum 'C4 H4 N2' _chemical_formula_weight 80.09 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' # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 3.7189(7) _cell_length_b 10.748(2) _cell_length_c 9.6823(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.50(3) _cell_angle_gamma 90.00 _cell_volume 386.86(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2663 _cell_measurement_theta_min 4.21 _cell_measurement_theta_max 24.92 _exptl_crystal_description cylinder _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 168 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ; Correction for absorption of the diamond-anvil cell and the sample were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam Mickiewicz University Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr. 219, 461-467). ; # EXPERIMENTAL DATA _exptl_special_details ; Data were collected at room temperature and pressure of 0.61(5) GPa (610000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 295(2) _diffrn_ambient_environment 'diamond-anvil cell' _diffrn_ambient_pressure 610000 _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 'KM-4 CCD' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2663 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 24.92 _reflns_number_total 321 _reflns_number_gt 250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)' _computing_structure_solution 'SHELXS--97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL--97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXL--97 (Sheldrick, 1997)' # REFINEMENT DATA _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. The DAC imposes severe restrictions on which reflections can be collected, resulting in a low data:parameter ratio. ; _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^)+(0.1544P)^2^+0.0551P] 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 0.01(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 321 _refine_ls_number_parameters 56 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.2146 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.246 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 N1 N -0.0452(11) 0.8585(10) 0.3817(4) 0.074(3) Uani 1 1 d U . . N2 N -0.1266(10) 0.7483(9) 0.3041(4) 0.065(3) Uani 1 1 d U . . C3 C -0.0548(13) 0.7588(10) 0.1701(4) 0.050(3) Uani 1 1 d U . . H3 H -0.1211 0.6923 0.1135 0.060 Uiso 1 1 calc R . . C4 C 0.1058(12) 0.8570(11) 0.1086(4) 0.058(3) Uani 1 1 d U . . H4 H 0.1586 0.8549 0.0153 0.069 Uiso 1 1 calc R . . C5 C 0.1874(13) 0.9587(11) 0.1873(5) 0.066(3) Uani 1 1 d U . . H5 H 0.2977 1.0279 0.1491 0.079 Uiso 1 1 calc R . . C6 C 0.1015(14) 0.9565(12) 0.3263(5) 0.083(4) Uani 1 1 d U . . H6 H 0.1494 1.0261 0.3808 0.099 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 N1 0.061(2) 0.110(10) 0.051(2) -0.001(3) 0.0078(18) -0.017(4) N2 0.059(2) 0.075(10) 0.060(3) -0.005(3) 0.0067(16) 0.003(3) C3 0.066(3) 0.033(11) 0.051(2) -0.015(3) -0.0035(19) 0.003(4) C4 0.059(2) 0.077(10) 0.037(2) -0.006(3) 0.0020(17) -0.005(4) C5 0.056(3) 0.090(10) 0.052(3) 0.012(4) 0.0055(19) 0.016(4) C6 0.063(3) 0.131(11) 0.053(3) -0.007(4) -0.002(2) -0.002(4) # MOLECULAR GEOMETRY _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 N1 C6 1.308(15) . ? N1 N2 1.431(12) . ? N2 C3 1.336(6) . ? C3 C4 1.358(14) . ? C3 H3 0.9300 . ? C4 C5 1.362(15) . ? C4 H4 0.9300 . ? C5 C6 1.392(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? 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 C6 N1 N2 122.4(5) . . ? C3 N2 N1 113.3(7) . . ? N2 C3 C4 126.3(8) . . ? N2 C3 H3 116.8 . . ? C4 C3 H3 116.8 . . ? C3 C4 C5 118.2(5) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 118.3(9) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? N1 C6 C5 121.3(9) . . ? N1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 N2 C3 -3.2(8) . . . . ? N1 N2 C3 C4 5.1(9) . . . . ? N2 C3 C4 C5 -3.7(10) . . . . ? C3 C4 C5 C6 -0.1(9) . . . . ? N2 N1 C6 C5 -0.1(10) . . . . ? C4 C5 C6 N1 1.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.469 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.469 _refine_diff_density_max 0.176 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.045 data_pir_1.23GPa _database_code_depnum_ccdc_archive 'CCDC 759557' #TrackingRef 'all.txt' # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; pyridine ; _chemical_name_common pyridine _chemical_melting_point 231 _chemical_formula_moiety 'C5 H5 N' _chemical_formula_sum 'C5 H5 N' _chemical_formula_weight 79.10 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' # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.267(4) _cell_length_b 8.7640(18) _cell_length_c 11.006(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1665.5(6) _cell_formula_units_Z 16 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12352 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.98 _exptl_crystal_description cylinder _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details ; Correction for absorption of the diamond-anvil cell and the sample were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam Mickiewicz University Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr. 219, 461-467). ; # EXPERIMENTAL DATA _exptl_special_details ; Data were collected at room temperature and pressure of 1.23(5) GPa (1230000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. ; _diffrn_ambient_temperature 295(2) _diffrn_ambient_environment 'diamond-anvil cell' _diffrn_ambient_pressure 1230000 _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 'KM-4 CCD' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12352 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.0764 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2143 _reflns_number_gt 1266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)' _computing_structure_solution 'SHELXS--97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL--97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXL--97 (Sheldrick, 1997)' # REFINEMENT DATA _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. The DAC imposes severe restrictions on which reflections can be collected, resulting in a low data:parameter ratio. ; _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^)+(0.0914P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(10) _refine_ls_number_reflns 2143 _refine_ls_number_parameters 217 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.1611 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2302 _refine_ls_wR_factor_gt 0.1960 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 N1 N 0.1235(4) 0.2834(8) 0.2400(7) 0.0563(17) Uani 1 1 d U . . C11 C 0.0779(4) 0.2106(11) 0.1651(7) 0.049(2) Uani 1 1 d U . . H11 H 0.0480 0.2690 0.1124 0.059 Uiso 1 1 calc R . . C12 C 0.0708(4) 0.0575(12) 0.1579(8) 0.067(2) Uani 1 1 d U . . H12 H 0.0382 0.0108 0.1018 0.081 Uiso 1 1 calc R . . C13 C 0.1142(4) -0.0238(10) 0.2376(9) 0.074(2) Uani 1 1 d U . . H13 H 0.1114 -0.1297 0.2353 0.089 Uiso 1 1 calc R . . C14 C 0.1601(4) 0.0410(12) 0.3185(9) 0.077(3) Uani 1 1 d U . . H14 H 0.1899 -0.0176 0.3712 0.093 Uiso 1 1 calc R . . C15 C 0.1627(4) 0.2000(11) 0.3225(8) 0.061(2) Uani 1 1 d U . . H15 H 0.1916 0.2487 0.3824 0.073 Uiso 1 1 calc R . . N2 N 0.0834(3) 0.6934(11) 0.4997(7) 0.0661(19) Uani 1 1 d U . . C21 C 0.1254(4) 0.7745(13) 0.5803(9) 0.073(3) Uani 1 1 d U . . H21 H 0.1005 0.8357 0.6373 0.088 Uiso 1 1 calc R . . C22 C 0.2082(4) 0.7666(13) 0.5785(10) 0.082(3) Uani 1 1 d U . . H22 H 0.2373 0.8232 0.6334 0.098 Uiso 1 1 calc R . . C23 C 0.2429(4) 0.6771(12) 0.4972(9) 0.065(2) Uani 1 1 d U . . H23 H 0.2965 0.6663 0.4980 0.077 Uiso 1 1 calc R . . C24 C 0.1985(4) 0.5992(11) 0.4103(8) 0.070(3) Uani 1 1 d U . . H24 H 0.2213 0.5427 0.3484 0.084 Uiso 1 1 calc R . . C25 C 0.1180(3) 0.6109(12) 0.4217(8) 0.062(3) Uani 1 1 d U . . H25 H 0.0877 0.5543 0.3684 0.074 Uiso 1 1 calc R . . N3 N 0.1121(3) 0.1103(8) 0.7356(7) 0.0540(18) Uani 1 1 d U . . C31 C 0.0719(4) 0.1929(13) 0.8215(9) 0.071(3) Uani 1 1 d U . . H31 H 0.0348 0.1474 0.8709 0.085 Uiso 1 1 calc R . . C32 C 0.0895(4) 0.3483(14) 0.8311(9) 0.081(3) Uani 1 1 d U . . H32 H 0.0656 0.4063 0.8911 0.097 Uiso 1 1 calc R . . C33 C 0.1441(4) 0.4209(11) 0.7497(9) 0.068(2) Uani 1 1 d U . . H33 H 0.1522 0.5258 0.7471 0.081 Uiso 1 1 calc R . . C34 C 0.1821(4) 0.3214(12) 0.6781(7) 0.059(2) Uani 1 1 d U . . H34 H 0.2239 0.3557 0.6325 0.071 Uiso 1 1 calc R . . C35 C 0.1612(3) 0.1733(11) 0.6704(6) 0.043(2) Uani 1 1 d U . . H35 H 0.1856 0.1139 0.6117 0.052 Uiso 1 1 calc R . . N4 N 0.1695(3) 0.7001(10) 0.9942(7) 0.0582(19) Uani 1 1 d U . . C41 C 0.1283(4) 0.6072(10) 1.0767(7) 0.055(2) Uani 1 1 d U . . H41 H 0.1555 0.5450 1.1303 0.066 Uiso 1 1 calc R . . C42 C 0.0490(4) 0.6070(11) 1.0793(8) 0.062(2) Uani 1 1 d U . . H42 H 0.0236 0.5423 1.1333 0.075 Uiso 1 1 calc R . . C43 C 0.0067(4) 0.6972(12) 1.0064(9) 0.065(2) Uani 1 1 d U . . H43 H -0.0470 0.7013 1.0125 0.078 Uiso 1 1 calc R . . C44 C 0.0464(4) 0.7833(10) 0.9224(7) 0.051(2) Uani 1 1 d U . . H44 H 0.0199 0.8449 0.8677 0.061 Uiso 1 1 calc R . . C45 C 0.1242(4) 0.7766(11) 0.9207(7) 0.053(2) Uani 1 1 d U . . H45 H 0.1487 0.8330 0.8604 0.063 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 N1 0.057(3) 0.057(5) 0.055(4) 0.012(4) -0.013(3) 0.002(3) C11 0.049(3) 0.038(6) 0.061(5) -0.002(4) 0.002(3) 0.005(3) C12 0.077(4) 0.054(6) 0.071(5) 0.007(4) 0.001(4) -0.004(4) C13 0.085(4) 0.064(6) 0.073(5) 0.005(5) 0.012(4) 0.006(5) C14 0.077(4) 0.067(7) 0.088(5) 0.039(4) -0.002(4) 0.019(5) C15 0.055(4) 0.065(6) 0.063(5) -0.012(4) 0.003(4) -0.027(4) N2 0.078(4) 0.061(5) 0.060(4) -0.003(3) 0.002(4) 0.005(4) C21 0.082(5) 0.064(7) 0.074(6) 0.003(4) -0.018(4) -0.002(4) C22 0.079(5) 0.078(7) 0.087(6) 0.015(5) -0.029(5) -0.007(4) C23 0.054(3) 0.068(6) 0.072(5) 0.016(4) 0.000(4) -0.005(4) C24 0.067(4) 0.066(7) 0.077(5) 0.012(4) 0.018(4) 0.004(4) C25 0.052(3) 0.057(7) 0.076(5) -0.006(4) -0.002(4) -0.016(3) N3 0.054(3) 0.039(5) 0.069(4) 0.015(3) 0.016(3) -0.017(3) C31 0.075(4) 0.072(7) 0.065(5) -0.003(4) -0.015(4) 0.015(4) C32 0.096(4) 0.083(7) 0.064(5) -0.011(4) -0.012(4) 0.002(5) C33 0.085(4) 0.043(6) 0.075(5) 0.004(4) 0.005(4) -0.003(4) C34 0.056(3) 0.065(6) 0.056(5) -0.013(4) -0.003(3) -0.024(4) C35 0.048(3) 0.038(6) 0.043(5) -0.020(3) -0.006(3) 0.015(4) N4 0.055(3) 0.063(5) 0.056(4) -0.005(3) 0.001(3) 0.001(3) C41 0.071(4) 0.041(6) 0.054(5) 0.002(4) 0.000(4) 0.024(4) C42 0.070(4) 0.047(6) 0.070(5) 0.003(4) 0.009(4) 0.001(4) C43 0.059(3) 0.057(6) 0.078(5) -0.008(4) 0.015(4) -0.002(4) C44 0.062(4) 0.039(6) 0.053(5) -0.017(4) -0.018(3) 0.007(4) C45 0.063(4) 0.050(6) 0.045(5) 0.018(3) 0.003(4) -0.018(3) # MOLECULAR GEOMETRY _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 N1 C11 1.306(10) . ? N1 C15 1.348(11) . ? C11 C12 1.350(11) . ? C11 H11 0.9300 . ? C12 C13 1.356(12) . ? C12 H12 0.9300 . ? C13 C14 1.321(12) . ? C13 H13 0.9300 . ? C14 C15 1.395(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? N2 C25 1.272(11) . ? N2 C21 1.349(11) . ? C21 C22 1.430(9) . ? C21 H21 0.9300 . ? C22 C23 1.333(12) . ? C22 H22 0.9300 . ? C23 C24 1.403(12) . ? C23 H23 0.9300 . ? C24 C25 1.399(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? N3 C35 1.241(9) . ? N3 C31 1.379(13) . ? C31 C32 1.400(14) . ? C31 H31 0.9300 . ? C32 C33 1.448(13) . ? C32 H32 0.9300 . ? C33 C34 1.345(12) . ? C33 H33 0.9300 . ? C34 C35 1.349(13) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? N4 C45 1.310(9) . ? N4 C41 1.413(11) . ? C41 C42 1.370(8) . ? C41 H41 0.9300 . ? C42 C43 1.342(11) . ? C42 H42 0.9300 . ? C43 C44 1.376(12) . ? C43 H43 0.9300 . ? C44 C45 1.345(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? 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 C11 N1 C15 117.6(7) . . ? N1 C11 C12 125.3(8) . . ? N1 C11 H11 117.4 . . ? C12 C11 H11 117.4 . . ? C11 C12 C13 115.7(9) . . ? C11 C12 H12 122.1 . . ? C13 C12 H12 122.1 . . ? C14 C13 C12 122.8(9) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C15 118.1(8) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? N1 C15 C14 120.3(8) . . ? N1 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C25 N2 C21 119.3(6) . . ? N2 C21 C22 120.2(9) . . ? N2 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.2(9) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 116.5(8) . . ? C25 C24 H24 121.8 . . ? C23 C24 H24 121.8 . . ? N2 C25 C24 124.7(7) . . ? N2 C25 H25 117.6 . . ? C24 C25 H25 117.6 . . ? C35 N3 C31 120.5(8) . . ? N3 C31 C32 116.9(9) . . ? N3 C31 H31 121.5 . . ? C32 C31 H31 121.5 . . ? C31 C32 C33 121.5(9) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C34 C33 C32 113.2(10) . . ? C34 C33 H33 123.4 . . ? C32 C33 H33 123.4 . . ? C33 C34 C35 122.0(8) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? N3 C35 C34 125.1(7) . . ? N3 C35 H35 117.5 . . ? C34 C35 H35 117.5 . . ? C45 N4 C41 113.0(5) . . ? C42 C41 N4 121.2(7) . . ? C42 C41 H41 119.4 . . ? N4 C41 H41 119.4 . . ? C43 C42 C41 122.0(8) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C42 C43 C44 117.0(6) . . ? C42 C43 H43 121.5 . . ? C44 C43 H43 121.5 . . ? C45 C44 C43 118.9(8) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? N4 C45 C44 127.6(7) . . ? N4 C45 H45 116.2 . . ? C44 C45 H45 116.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N1 C11 C12 -4.8(12) . . . . ? N1 C11 C12 C13 1.3(12) . . . . ? C11 C12 C13 C14 0.6(13) . . . . ? C12 C13 C14 C15 1.1(14) . . . . ? C11 N1 C15 C14 6.4(13) . . . . ? C13 C14 C15 N1 -4.7(13) . . . . ? C25 N2 C21 C22 -0.5(16) . . . . ? N2 C21 C22 C23 -0.7(15) . . . . ? C21 C22 C23 C24 3.7(17) . . . . ? C22 C23 C24 C25 -5.4(16) . . . . ? C21 N2 C25 C24 -1.5(18) . . . . ? C23 C24 C25 N2 4.4(15) . . . . ? C35 N3 C31 C32 -0.2(12) . . . . ? N3 C31 C32 C33 3.5(12) . . . . ? C31 C32 C33 C34 -8.3(12) . . . . ? C32 C33 C34 C35 10.2(12) . . . . ? C31 N3 C35 C34 2.2(12) . . . . ? C33 C34 C35 N3 -8.0(12) . . . . ? C45 N4 C41 C42 -2.8(13) . . . . ? N4 C41 C42 C43 -1.8(14) . . . . ? C41 C42 C43 C44 4.3(15) . . . . ? C42 C43 C44 C45 -2.3(15) . . . . ? C41 N4 C45 C44 5.1(15) . . . . ? C43 C44 C45 N4 -2.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.734 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.734 _refine_diff_density_max 0.156 _refine_diff_density_min -0.158 _refine_diff_density_rms 0.043 data_pirmet_1.80GPa _database_code_depnum_ccdc_archive 'CCDC 759558' #TrackingRef 'all.txt' # CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; pyridine:methanol 3:1 cocrystal ; _chemical_name_common 'pyridine:methanol 3:1 cocrystal' _chemical_melting_point ? _chemical_formula_moiety '3(C5 H5 N), C H4 O' _chemical_formula_sum 'C16 H19 N3 O' _chemical_formula_weight 269.34 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' # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 6.7710(14) _cell_length_b 5.5910(11) _cell_length_c 18.100(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.40(3) _cell_angle_gamma 90.00 _cell_volume 685.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4755 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 24.96 _exptl_crystal_description cylinder _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ; Correction for absorption of the diamond-anvil cell and the sample were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam Mickiewicz University Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr. 219, 461-467). ; # EXPERIMENTAL DATA _exptl_special_details ; Data were collected at room temperature and pressure of 1.80(5) GPa (1800000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line. The quality of the crystal in the DAC was poor, and the diffraction data and linal structural parameters are of a very low accuracy. This is a very rough model where the atomic positions and even the atomic type assignments can be wrong. ; _diffrn_ambient_temperature 295(2) _diffrn_ambient_environment 'diamond-anvil cell' _diffrn_ambient_pressure 1800000 _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 'KM-4 CCD' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4755 _diffrn_reflns_av_R_equivalents 0.2065 _diffrn_reflns_av_sigmaI/netI 0.1638 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.96 _reflns_number_total 907 _reflns_number_gt 585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2004)' _computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2004)' _computing_data_reduction 'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)' _computing_structure_solution 'SHELXS--97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL--97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXL--97 (Sheldrick, 1997)' # REFINEMENT DATA _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. The DAC imposes severe restrictions on which reflections can be collected, resulting in a low data:parameter ratio. ; _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^)+(0.0300P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 907 _refine_ls_number_parameters 27 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.3587 _refine_ls_R_factor_gt 0.3001 _refine_ls_wR_factor_ref 0.3070 _refine_ls_wR_factor_gt 0.2850 _refine_ls_goodness_of_fit_ref 2.301 _refine_ls_restrained_S_all 2.299 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 N1 N -0.3160(17) 1.011(3) 1.6577(19) 0.0485(16) Uiso 1 1 d G . . C2 C -0.3802(16) 1.200(2) 1.6199(19) 0.0485(16) Uiso 1 1 d G . . H2 H -0.4286 1.3319 1.6453 0.058 Uiso 1 1 calc R . . C3 C -0.377(2) 1.205(2) 1.541(2) 0.0485(16) Uiso 1 1 d G . . H3 H -0.4229 1.3410 1.5171 0.058 Uiso 1 1 calc R . . C4 C -0.309(2) 1.022(3) 1.501(2) 0.0485(16) Uiso 1 1 d G . . H4 H -0.3070 1.0264 1.4494 0.058 Uiso 1 1 calc R . . C5 C -0.245(2) 0.833(2) 1.539(2) 0.0485(16) Uiso 1 1 d G . . H5 H -0.1963 0.7011 1.5131 0.058 Uiso 1 1 calc R . . C6 C -0.2483(18) 0.828(2) 1.617(2) 0.0485(16) Uiso 1 1 d G . . H6 H -0.2019 0.6921 1.6414 0.058 Uiso 1 1 calc R . . N11 N -0.8582(14) 0.418(3) 1.6460(14) 0.0485(16) Uiso 1 1 d G . . C12 C -0.753(2) 0.697(2) 1.5564(15) 0.0485(16) Uiso 1 1 d G . . H12 H -0.6977 0.8464 1.5472 0.058 Uiso 1 1 calc R . . C13 C -0.7807(18) 0.627(2) 1.6305(14) 0.0485(16) Uiso 1 1 d G . . H13 H -0.7437 0.7300 1.6686 0.058 Uiso 1 1 calc R . . C14 C -0.803(2) 0.558(3) 1.4978(15) 0.0485(16) Uiso 1 1 d G . . H14 H -0.7834 0.6079 1.4494 0.058 Uiso 1 1 calc R . . C15 C -0.9082(14) 0.279(2) 1.5874(15) 0.0485(16) Uiso 1 1 d G . . H15 H -0.9635 0.1300 1.5965 0.058 Uiso 1 1 calc R . . C16 C -0.881(2) 0.349(2) 1.5133(15) 0.0485(16) Uiso 1 1 d G . . H16 H -0.9176 0.2464 1.4752 0.058 Uiso 1 1 calc R . . N21 N -0.215(2) 1.692(2) 1.367(2) 0.0485(16) Uiso 1 1 d G . . C22 C -0.206(3) 1.3346(19) 1.308(3) 0.0485(16) Uiso 1 1 d G . . H22 H -0.1340 1.2124 1.2856 0.058 Uiso 1 1 calc R . . C23 C -0.398(3) 1.3222(15) 1.310(2) 0.0485(16) Uiso 1 1 d G . . H23 H -0.4639 1.1912 1.2903 0.058 Uiso 1 1 calc R . . C24 C -0.499(2) 1.4948(13) 1.342(3) 0.0485(16) Uiso 1 1 d G . . H24 H -0.6362 1.4858 1.3436 0.058 Uiso 1 1 calc R . . C25 C -0.407(2) 1.6797(17) 1.370(3) 0.0485(16) Uiso 1 1 d G . . H25 H -0.4790 1.8019 1.3923 0.058 Uiso 1 1 calc R . . C26 C -0.114(2) 1.519(2) 1.336(3) 0.0485(16) Uiso 1 1 d G . . H26 H 0.0232 1.5284 1.3342 0.058 Uiso 1 1 calc R . . O31 O -0.790(3) 1.009(2) 1.345(3) 0.049(4) Uiso 1 1 d G . . H31 H -0.8530 0.9000 1.3635 0.058 Uiso 1 1 calc R . . C32 C -0.796(4) 0.984(4) 1.260(4) 0.049(4) Uiso 1 1 d . . . H321 H -0.8605 0.8365 1.2472 0.063 Uiso 1 1 calc R . . H322 H -0.6637 0.9827 1.2415 0.063 Uiso 1 1 calc R . . H323 H -0.8675 1.1156 1.2393 0.063 Uiso 1 1 calc R . . # MOLECULAR GEOMETRY _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 N1 C2 1.330(8) . ? N1 C6 1.345(8) . ? C2 C3 1.422(8) . ? C3 C4 1.345(8) . ? C4 C5 1.330(8) . ? C5 C6 1.422(8) . ? N11 C13 1.312(8) . ? N11 C15 1.356(8) . ? C12 C14 1.356(8) . ? C12 C13 1.411(8) . ? C14 C16 1.312(8) . ? C15 C16 1.410(8) . ? N21 C25 1.308(5) . ? N21 C26 1.312(5) . ? C22 C23 1.308(5) . ? C22 C26 1.310(5) . ? C23 C24 1.312(5) . ? C24 C25 1.310(5) . ? O31 C32 1.53(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 C2 N1 C6 115.8 . . ? N1 C2 C3 121.6 . . ? C4 C3 C2 122.6 . . ? C5 C4 C3 115.8 . . ? C4 C5 C6 121.6 . . ? N1 C6 C5 122.6 . . ? C13 N11 C15 116.2 . . ? C14 C12 C13 123.4 . . ? N11 C13 C12 120.4 . . ? C16 C14 C12 116.2 . . ? N11 C15 C16 123.4 . . ? C14 C16 C15 120.4 . . ? C25 N21 C26 120.0 . . ? C23 C22 C26 119.8 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.2 . . ? N21 C25 C24 119.8 . . ? C22 C26 N21 120.2 . . ? _diffrn_measured_fraction_theta_max 0.395 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.395 _refine_diff_density_max 0.397 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.091 # # h,k,l, Fc-squared, Fo-squared, sigma(Fo-squared) and status flag # loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 5 1 -7 59.86 18.18 24.50 o 0 5 -7 7.93 36.53 61.82 o 1 5 -7 52.55 174.65 60.59 o 4 5 -7 7.02 63.75 43.46 o 0 6 -7 16.67 74.11 48.82 o 2 6 -7 7.09 64.01 60.50 o 5 0 -6 1.40 0.00 35.65 o 6 0 -6 28.33 40.22 24.94 o 7 0 -6 0.19 53.47 47.94 o 4 1 -6 24.78 20.37 30.03 o 5 1 -6 11.67 106.21 35.07 o 6 1 -6 4.20 13.52 23.36 o 7 1 -6 13.92 43.73 52.42 o 5 2 -6 64.03 32.86 15.59 o 6 2 -6 27.80 28.67 25.11 o 7 2 -6 0.77 46.36 49.52 o 5 3 -6 3.50 37.72 24.24 o 6 3 -6 0.70 16.04 20.57 o -2 4 -6 21.28 16.92 16.95 o -1 4 -6 74.66 49.59 24.37 o 0 4 -6 36.50 54.97 46.27 o 1 4 -6 34.38 27.22 23.88 o 6 4 -6 17.09 22.92 51.45 o -3 5 -6 13.75 41.17 25.82 o -2 5 -6 54.82 278.70 105.37 o -1 5 -6 18.81 29.68 75.34 o 0 5 -6 32.13 241.20 68.05 o 1 5 -6 12.96 118.71 47.06 o 4 5 -6 2.22 59.80 47.94 o -2 6 -6 0.96 61.24 42.59 o -1 6 -6 14.08 87.19 69.54 o 0 6 -6 21.35 41.73 36.17 o 1 6 -6 14.17 0.00 65.94 o 2 6 -6 1.85 86.58 69.63 o 4 1 -5 57.41 39.50 18.43 o 5 1 -5 54.89 22.54 16.01 o 6 1 -5 16.45 14.70 27.51 o 7 1 -5 2.46 57.52 27.98 o 3 2 -5 24.93 18.81 16.82 o 4 2 -5 24.34 52.08 41.35 o 5 2 -5 34.28 47.55 20.49 o 6 2 -5 17.53 68.32 29.38 o 7 2 -5 2.12 44.34 30.60 o -5 3 -5 45.16 45.54 29.11 o -4 3 -5 52.98 48.18 22.59 o -3 3 -5 50.48 0.00 23.90 o -2 3 -5 28.53 27.17 27.88 o -1 3 -5 12.61 34.86 38.99 o 2 3 -5 51.29 19.67 14.34 o 3 3 -5 16.46 43.26 20.40 o 4 3 -5 30.53 65.20 23.99 o 5 3 -5 6.80 47.17 18.41 o 6 3 -5 1.49 31.38 21.71 o -6 4 -5 0.50 60.46 40.24 o -5 4 -5 37.11 60.37 43.50 o -4 4 -5 6.36 21.69 43.35 o -3 4 -5 52.55 33.53 24.17 o -2 4 -5 55.84 29.28 25.27 o -1 4 -5 39.55 22.52 18.74 o 0 4 -5 120.15 28.98 36.26 o 1 4 -5 74.59 31.35 25.73 o 2 4 -5 18.31 50.93 45.40 o 3 4 -5 0.80 19.41 20.92 o 4 4 -5 22.75 76.86 21.87 o 5 4 -5 7.54 45.84 23.17 o 6 4 -5 5.40 57.35 26.00 o -4 5 -5 0.17 60.82 29.28 o -3 5 -5 16.45 69.69 42.81 o -2 5 -5 12.14 33.10 38.81 o -1 5 -5 15.50 136.98 70.42 o 0 5 -5 53.29 111.78 56.11 o 1 5 -5 6.01 78.32 48.56 o 2 5 -5 9.01 77.09 62.25 o 3 5 -5 11.31 68.13 23.41 o 4 5 -5 11.98 34.97 19.99 o -2 6 -5 4.07 44.52 37.73 o -1 6 -5 7.46 50.61 39.14 o 0 6 -5 21.68 47.71 30.03 o 1 6 -5 13.11 43.91 38.77 o 2 6 -5 15.75 22.98 41.30 o -6 0 -4 52.01 29.33 29.94 o -5 0 -4 77.99 35.91 27.66 o 3 0 -4 232.77 277.28 87.98 o 4 0 -4 122.35 70.83 15.21 o 5 0 -4 40.21 30.15 13.47 o 6 0 -4 81.11 52.54 27.69 o 7 0 -4 31.54 55.59 31.98 o -7 1 -4 1.07 82.01 65.59 o -6 1 -4 0.83 0.00 56.90 o -5 1 -4 27.55 86.55 31.24 o -4 1 -4 24.30 90.09 54.70 o 3 1 -4 54.70 30.38 42.34 o 4 1 -4 22.24 56.75 19.33 o 5 1 -4 91.94 93.19 13.04 o 6 1 -4 1.92 69.23 26.76 o 7 1 -4 3.86 63.56 27.13 o -7 2 -4 7.55 66.38 55.05 o -6 2 -4 63.28 54.88 39.69 o -5 2 -4 41.27 60.62 33.57 o -4 2 -4 78.51 41.56 24.17 o -3 2 -4 139.18 154.28 57.16 o 2 2 -4 478.16 320.75 122.90 o 3 2 -4 120.29 80.88 12.83 o 4 2 -4 10.02 79.10 18.72 o 5 2 -4 29.24 42.60 11.91 o 6 2 -4 19.49 58.02 22.86 o 7 2 -4 3.30 38.82 29.57 o -7 3 -4 9.37 68.84 40.18 o -6 3 -4 17.23 63.66 40.02 o -5 3 -4 80.86 76.60 44.11 o -4 3 -4 29.07 79.75 54.82 o -3 3 -4 21.07 25.37 15.74 o -2 3 -4 51.27 120.25 22.13 o -1 3 -4 171.95 237.56 34.66 o 0 3 -4 3.17 7.56 29.68 o 1 3 -4 188.12 198.61 41.06 o 2 3 -4 114.98 86.72 27.11 o 3 3 -4 78.59 49.06 20.07 o 4 3 -4 4.22 69.95 19.89 o 5 3 -4 82.08 65.79 20.82 o 6 3 -4 4.47 53.47 17.85 o 7 3 -4 0.61 70.71 28.56 o -6 4 -4 3.59 54.44 54.84 o -5 4 -4 2.18 49.54 34.22 o -4 4 -4 14.05 188.60 45.64 o -3 4 -4 71.93 31.60 32.25 o -2 4 -4 26.25 50.19 28.74 o -1 4 -4 68.28 15.26 18.99 o 0 4 -4 27.31 29.91 21.07 o 1 4 -4 47.97 61.55 23.53 o 2 4 -4 12.05 47.63 15.59 o 3 4 -4 18.28 56.82 18.81 o 4 4 -4 2.51 57.26 17.73 o 5 4 -4 20.72 58.51 25.60 o 6 4 -4 4.44 53.90 24.61 o -5 5 -4 4.36 47.88 46.31 o -4 5 -4 7.38 49.17 29.51 o -3 5 -4 4.29 150.02 40.78 o -2 5 -4 10.56 93.05 41.67 o -1 5 -4 15.25 34.99 33.78 o 0 5 -4 31.95 27.81 23.81 o 1 5 -4 8.54 42.73 13.72 o 2 5 -4 3.92 35.45 12.55 o 3 5 -4 1.64 51.19 16.11 o 4 5 -4 3.60 73.84 21.69 o 5 5 -4 7.95 37.20 23.43 o -3 6 -4 1.75 57.47 37.21 o -2 6 -4 0.54 58.48 39.70 o -1 6 -4 14.54 56.59 45.37 o 0 6 -4 40.28 74.30 23.64 o 1 6 -4 9.87 29.98 20.29 o 2 6 -4 8.41 55.63 21.18 o 3 6 -4 24.27 50.19 19.94 o -7 1 -3 2.55 24.22 38.07 o -6 1 -3 24.28 35.29 24.75 o -5 1 -3 12.08 44.50 12.37 o -4 1 -3 311.10 404.38 33.17 o -3 1 -3 18.85 23.75 20.68 o 2 1 -3 737.34 814.15 62.78 o 3 1 -3 11.23 19.68 8.72 o 4 1 -3 337.93 319.52 11.51 o 5 1 -3 10.42 39.01 9.89 o 6 1 -3 47.42 74.41 21.25 o 7 1 -3 0.30 64.52 23.97 o -7 2 -3 3.61 107.14 50.78 o -6 2 -3 1.49 96.34 55.89 o -5 2 -3 28.81 200.21 40.23 o -4 2 -3 16.18 30.32 12.60 o -3 2 -3 112.75 164.52 31.13 o -2 2 -3 81.54 73.72 26.93 o -1 2 -3 172.02 81.84 25.55 o 1 2 -3 142.24 42.35 13.14 o 2 2 -3 11.66 57.93 21.34 o 3 2 -3 180.98 177.65 8.53 o 4 2 -3 31.05 31.13 10.92 o 5 2 -3 64.17 79.53 15.44 o 6 2 -3 28.04 21.67 15.87 o 7 2 -3 2.15 75.32 24.62 o -7 3 -3 1.95 43.38 39.02 o -6 3 -3 10.66 103.18 46.25 o -5 3 -3 1.39 47.46 19.28 o -4 3 -3 14.36 37.38 19.09 o -3 3 -3 19.04 64.90 29.16 o -2 3 -3 74.36 32.97 12.45 o -1 3 -3 26.19 0.00 16.91 o 0 3 -3 82.36 79.74 62.49 o 1 3 -3 43.18 0.00 8.39 o 2 3 -3 14.75 32.12 11.05 o 3 3 -3 29.58 3.03 14.98 o 4 3 -3 2.55 30.93 10.54 o 5 3 -3 33.04 64.95 19.01 o 6 3 -3 1.31 52.30 16.31 o 7 3 -3 8.03 55.29 23.64 o -6 4 -3 10.79 39.12 29.35 o -5 4 -3 27.22 100.70 31.15 o -4 4 -3 23.35 80.74 20.34 o -3 4 -3 127.02 90.51 27.83 o -2 4 -3 17.08 38.51 14.86 o -1 4 -3 116.85 34.16 14.40 o 0 4 -3 33.64 57.12 15.86 o 1 4 -3 33.05 60.28 14.71 o 2 4 -3 46.14 21.95 11.49 o 3 4 -3 36.20 64.64 14.14 o 4 4 -3 19.98 58.46 18.87 o 5 4 -3 21.38 95.20 24.94 o 6 4 -3 1.95 68.56 25.03 o -5 5 -3 0.20 55.70 33.36 o -4 5 -3 9.71 31.76 18.27 o -3 5 -3 0.82 70.13 18.73 o -2 5 -3 32.84 38.99 15.48 o -1 5 -3 31.91 48.18 16.26 o 0 5 -3 8.20 44.45 13.06 o 1 5 -3 65.16 45.19 13.44 o 2 5 -3 9.68 53.32 16.91 o 3 5 -3 24.59 143.00 34.00 o 4 5 -3 0.86 53.86 21.44 o 5 5 -3 5.79 49.00 25.99 o -3 6 -3 3.27 9.44 28.82 o -2 6 -3 9.63 55.08 23.59 o -1 6 -3 1.51 47.41 18.37 o 0 6 -3 3.64 41.45 16.14 o 1 6 -3 24.58 63.58 25.69 o 2 6 -3 4.91 49.63 25.10 o 3 6 -3 7.67 52.63 26.08 o -8 0 -2 6.10 42.18 47.62 o -7 0 -2 15.39 55.71 50.26 o -6 0 -2 14.85 75.46 34.61 o -5 0 -2 89.91 88.76 13.76 o -4 0 -2 91.82 32.01 9.61 o -3 0 -2 884.71 1041.98 56.90 o -2 0 -2 1722.57 1873.08 55.49 o 2 0 -2 1842.01 2143.12 71.44 o 3 0 -2 727.00 881.32 19.11 o 4 0 -2 66.88 28.07 10.50 o 5 0 -2 80.57 79.27 19.57 o 6 0 -2 30.12 84.43 20.76 o 7 0 -2 17.98 106.23 28.10 o 8 0 -2 8.60 55.96 47.80 o -7 1 -2 0.27 121.40 71.92 o -6 1 -2 10.36 46.79 21.90 o -5 1 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