#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/32/2203214.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_2203214 loop_ _publ_author_name 'Zhenfeng Zhang' 'Shuo Jin' 'Siqian Wang' 'Bo Liu' 'Jianping Guo' _publ_section_title ; 3-Methyl-3-pyrazolin-5-one ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o315 _journal_page_last o316 _journal_paper_doi 10.1107/S160053680302974X _journal_volume 60 _journal_year 2004 _chemical_formula_moiety 'C4 H6 N2 O' _chemical_formula_sum 'C4 H6 N2 O' _chemical_formula_weight 98.11 _chemical_melting_point 215 _chemical_name_common 3-Methyl-3-Pyrazolin-5-one _chemical_name_systematic ' 3-Methyl-3-Pyrazolin-5-one' _space_group_IT_number 43 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_space_group_name_H-M 'F d d 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 16 _cell_length_a 11.722(2) _cell_length_b 16.945(3) _cell_length_c 9.898(2) _cell_measurement_reflns_used 867 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 44.403 _cell_measurement_theta_min 5.899 _cell_volume 1966.0(6) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1999)' _computing_publication_material SHELXTL/PC _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1933 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.95 _diffrn_standards_decay_% 3.14 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1997)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 832 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.126 _refine_diff_density_min -0.163 _refine_ls_abs_structure_details 'see text' _refine_ls_extinction_coef 0.0020(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 66 _refine_ls_number_reflns 460 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.162 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0427 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0630P)^2^+1.0082P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1137 _refine_ls_wR_factor_ref 0.1152 _reflns_number_gt 439 _reflns_number_total 460 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ob6336.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1966.0(7) _cod_database_code 2203214 _cod_database_fobs_code 2203214 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' loop_ _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 _atom_site_type_symbol O1 0.9969(2) 0.38889(15) 0.3766(3) 0.0597(9) Uani d . 1 O N1 0.9383(3) 0.21227(16) 0.5257(3) 0.0489(9) Uani d . 1 N H1 0.8992 0.1829 0.5794 0.059 Uiso calc R 1 H N2 0.9171(3) 0.28983(16) 0.4984(3) 0.0464(9) Uani d . 1 N H2 0.8611 0.3168 0.5303 0.056 Uiso calc R 1 H C1 1.0662(5) 0.1058(2) 0.4573(6) 0.0750(15) Uani d . 1 C H1A 1.0528 0.0834 0.5450 0.113 Uiso calc R 1 H H1B 1.1461 0.1031 0.4366 0.113 Uiso calc R 1 H H1C 1.0240 0.0767 0.3907 0.113 Uiso calc R 1 H C2 1.0284(3) 0.1899(2) 0.4565(4) 0.0456(9) Uani d . 1 C C3 1.0689(3) 0.2535(2) 0.3862(4) 0.0481(10) Uani d . 1 C H3 1.1326 0.2545 0.3301 0.058 Uiso calc R 1 H C4 0.9962(3) 0.3171(2) 0.4151(4) 0.0435(9) Uani d . 1 C 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 0.0520(15) 0.0400(15) 0.087(2) 0.0018(12) 0.0107(14) 0.0231(14) N1 0.068(2) 0.0273(15) 0.0514(18) -0.0046(13) 0.0136(16) 0.0091(13) N2 0.0478(17) 0.0296(15) 0.062(2) 0.0035(12) 0.0154(14) 0.0064(13) C1 0.101(4) 0.043(2) 0.081(3) 0.025(2) 0.008(3) 0.003(2) C2 0.055(2) 0.040(2) 0.0419(17) 0.0078(16) -0.0005(16) -0.0021(16) C3 0.041(2) 0.053(2) 0.0502(19) 0.0032(16) 0.0044(16) 0.0086(17) C4 0.0385(17) 0.041(2) 0.051(2) 0.0032(14) 0.0016(16) 0.0068(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' 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 N2 108.7(3) yes C2 N1 H1 125.7 no N2 N1 H1 125.7 no C4 N2 N1 109.4(3) yes C4 N2 H2 125.3 no N1 N2 H2 125.3 no C2 C1 H1A 109.5 no C2 C1 H1B 109.5 no H1A C1 H1B 109.5 no C2 C1 H1C 109.5 no H1A C1 H1C 109.5 no H1B C1 H1C 109.5 no N1 C2 C3 108.5(3) yes N1 C2 C1 120.7(4) yes C3 C2 C1 130.7(4) yes C2 C3 C4 106.8(3) no C2 C3 H3 126.6 no C4 C3 H3 126.6 no O1 C4 N2 121.6(3) no O1 C4 C3 131.8(3) no N2 C4 C3 106.6(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C4 1.275(3) yes N1 C2 1.315(5) yes N1 N2 1.365(4) yes N1 H1 0.8600 no N2 C4 1.324(4) yes N2 H2 0.8600 no C1 C2 1.493(4) no C1 H1A 0.9600 no C1 H1B 0.9600 no C1 H1C 0.9600 no C2 C3 1.368(5) yes C3 C4 1.403(5) yes C3 H3 0.9300 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 N1 H1 O1 16_645 0.86 1.93 2.694(4) 147.9 N2 H2 O1 15_455 0.86 1.81 2.654(4) 168.6