#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2015278.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2015278 loop_ _publ_author_name 'Portilla, Jaime' 'Quiroga, Jairo' 'Cobo, Justo' 'Low, John N.' 'Glidewell, Christopher' _publ_section_title ; 7-Amino-2,5-dimethylpyrazolo[1,5-a]pyrimidine hemihydrate redetermined at 120K: a three-dimensional hydrogen-bonded framework ; _journal_coeditor_code SK3006 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o186 _journal_page_last o189 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac 'C8 H10 N4, 0.5H2 O' _chemical_formula_moiety 'C8 H10 N4, 0.5H2 O' _chemical_formula_sum 'C8 H11 N4 O0.5' _chemical_formula_weight 171.21 _chemical_name_systematic ; 7-Amino-2,5-dimethylpyrazolo[1,5-a]pyrimidine hemihydrate ; _space_group_IT_number 5 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 117.309(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.0851(5) _cell_length_b 7.9458(3) _cell_length_c 8.0003(3) _cell_measurement_reflns_used 1116 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 4.54 _cell_volume 908.55(6) _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) and COLLECT' _computing_data_collection 'COLLECT (Hooft, 1999)' _computing_data_reduction 'DENZO and COLLECT' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXL97 and PRPKAPPA (Ferguson, 1999)' _computing_structure_refinement 'OSCAIL and SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 9.091 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Bruker-Nonius FR91 rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 6163 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 4.54 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 364 _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.171 _refine_diff_density_min -0.197 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 116 _refine_ls_number_reflns 1116 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0335 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.2034P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.0897 _reflns_number_gt 1032 _reflns_number_total 1116 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk3006.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2' _cod_database_code 2015278 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy O O1 0.5000 0.4489(2) 0.5000 0.0264(4) Uani d S 1 N N1 0.88429(10) 0.2722(2) 0.9820(2) 0.0269(3) Uani d . 1 N N4 0.65962(10) 0.26477(18) 0.5803(2) 0.0283(3) Uani d . 1 N N7 0.93536(10) 0.1362(2) 0.7256(2) 0.0321(4) Uani d . 1 N N7A 0.82186(10) 0.24015(17) 0.7987(2) 0.0232(3) Uani d . 1 C C2 0.83100(13) 0.3410(2) 1.0528(3) 0.0286(4) Uani d . 1 C C3 0.73665(13) 0.3543(2) 0.9203(3) 0.0309(4) Uani d . 1 C C3A 0.73131(11) 0.2868(2) 0.7552(2) 0.0256(4) Uani d . 1 C C5 0.68064(12) 0.1943(2) 0.4533(3) 0.0286(4) Uani d . 1 C C6 0.77084(12) 0.1459(3) 0.4915(3) 0.0281(4) Uani d . 1 C C7 0.84535(11) 0.1708(2) 0.6691(2) 0.0250(4) Uani d . 1 C C21 0.87585(15) 0.3949(3) 1.2553(3) 0.0391(5) Uani d . 1 C C51 0.60139(13) 0.1680(3) 0.2592(3) 0.0406(5) Uani d . 1 H H1 0.5531 0.3776 0.5331 0.040 Uiso d R 1 H H3 0.6870 0.3996 0.9392 0.037 Uiso calc R 1 H H6 0.7815 0.0955 0.3954 0.034 Uiso calc R 1 H H7A 0.9770 0.1579 0.8421 0.038 Uiso calc R 1 H H7B 0.9531 0.0917 0.6464 0.038 Uiso calc R 1 H H21A 0.9232 0.3122 1.3318 0.059 Uiso calc R 1 H H21B 0.8280 0.4028 1.2986 0.059 Uiso calc R 1 H H21C 0.9055 0.5051 1.2675 0.059 Uiso calc R 1 H H51A 0.5704 0.0608 0.2550 0.061 Uiso calc R 1 H H51B 0.6259 0.1659 0.1675 0.061 Uiso calc R 1 H H51C 0.5562 0.2601 0.2288 0.061 Uiso calc R 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0218(7) 0.0284(9) 0.0316(9) 0.000 0.0144(7) 0.000 N1 0.0279(7) 0.0281(7) 0.0247(7) 0.0020(6) 0.0122(6) -0.0009(6) N4 0.0231(7) 0.0270(8) 0.0341(8) 0.0002(6) 0.0126(6) 0.0016(7) N7 0.0249(7) 0.0404(9) 0.0323(8) 0.0015(7) 0.0143(6) -0.0112(7) N7A 0.0227(6) 0.0230(7) 0.0249(7) 0.0018(5) 0.0118(5) -0.0012(6) C2 0.0357(9) 0.0281(9) 0.0272(9) 0.0042(7) 0.0189(7) 0.0018(7) C3 0.0324(9) 0.0317(10) 0.0359(9) 0.0067(8) 0.0218(8) 0.0029(8) C3A 0.0241(8) 0.0235(8) 0.0323(9) 0.0031(7) 0.0156(7) 0.0032(7) C5 0.0275(8) 0.0241(9) 0.0318(9) -0.0016(7) 0.0115(7) -0.0004(7) C6 0.0288(8) 0.0277(8) 0.0277(8) -0.0024(7) 0.0128(7) -0.0065(7) C7 0.0245(8) 0.0235(9) 0.0295(9) 0.0014(7) 0.0145(7) -0.0016(7) C21 0.0442(11) 0.0452(11) 0.0312(10) 0.0071(9) 0.0200(9) -0.0035(9) C51 0.0303(9) 0.0429(12) 0.0386(11) -0.0014(9) 0.0071(8) -0.0063(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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2 N1 N7A 103.37(14) no N1 C2 C3 113.07(16) no N1 C2 C21 119.20(16) no C3 C2 C21 127.73(16) no C2 C21 H21A 109.5 no C2 C21 H21B 109.5 no H21A C21 H21B 109.5 no C2 C21 H21C 109.5 no H21A C21 H21C 109.5 no H21B C21 H21C 109.5 no C3A C3 C2 105.24(15) no C3A C3 H3 127.4 no C2 C3 H3 127.4 no N4 C3A N7A 121.62(15) no N4 C3A C3 133.03(16) no N7A C3A C3 105.35(15) no C5 N4 C3A 116.61(14) no N4 C5 C6 123.51(16) no N4 C5 C51 117.00(16) no C6 C5 C51 119.48(17) no C5 C51 H51A 109.5 no C5 C51 H51B 109.5 no H51A C51 H51B 109.5 no C5 C51 H51C 109.5 no H51A C51 H51C 109.5 no H51B C51 H51C 109.5 no C7 C6 C5 120.49(16) no C7 C6 H6 119.8 no C5 C6 H6 119.8 no N7 C7 N7A 117.38(15) y N7 C7 C6 127.60(16) y N7A C7 C6 115.02(15) no C7 N7 H7A 120.0 no C7 N7 H7B 120.0 no H7A N7 H7B 120.0 no N1 N7A C7 124.31(14) no N1 N7A C3A 112.97(13) no C7 N7A C3A 122.72(15) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 1.342(2) y C2 C3 1.401(3) y C3 C3A 1.392(3) y C3A N4 1.355(2) y N4 C5 1.332(2) y C5 C6 1.393(3) y C6 C7 1.390(2) y C7 N7A 1.371(2) y N7A N1 1.368(2) y C3A N7A 1.384(2) y C7 N7 1.333(2) y C2 C21 1.502(3) no C21 H21A 0.98 no C21 H21B 0.98 no C21 H21C 0.98 no C3 H3 0.95 no C5 C51 1.504(2) no C51 H51A 0.98 no C51 H51B 0.98 no C51 H51C 0.98 no C6 H6 0.95 no N7 H7A 0.88 no N7 H7B 0.88 no O1 H1 0.96 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 N4 . 0.96 1.81 2.763(2) 172 y N7 H7A N1 2_757 0.88 2.21 2.971(2) 144 y N7 H7B O1 3_545 0.88 2.01 2.877(2) 168 y 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_publ_flag N7A N1 C2 C3 -0.2(2) no N7A N1 C2 C21 -179.70(17) no N1 C2 C3 C3A 0.6(2) no C21 C2 C3 C3A -179.95(19) no C2 C3 C3A N4 -179.99(19) no C2 C3 C3A N7A -0.7(2) no N7A C3A N4 C5 0.7(2) no C3 C3A N4 C5 179.9(2) no C3A N4 C5 C6 -0.8(3) no C3A N4 C5 C51 179.48(17) no N4 C5 C6 C7 -0.4(3) no C51 C5 C6 C7 179.24(19) no C5 C6 C7 N7 -177.84(18) no C5 C6 C7 N7A 1.7(3) no C2 N1 N7A C7 179.03(15) no C2 N1 N7A C3A -0.32(19) no N7 C7 N7A N1 -1.5(2) no C6 C7 N7A N1 178.83(16) no N7 C7 N7A C3A 177.76(17) no C6 C7 N7A C3A -1.9(2) no N4 C3A N7A N1 -179.95(15) no C3 C3A N7A N1 0.7(2) no N4 C3A N7A C7 0.7(3) no C3 C3A N7A C7 -178.70(16) no