#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/07/2100708.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_2100708 loop_ _publ_author_name 'P. A. Wood' 'R. S. Forgan' 'D. Henderson' 'S. Parsons' 'E. Pidcock' 'P. A. Tasker' 'J. E. Warren' _publ_contact_author_email P.A.Wood@sms.ed.ac.uk _publ_contact_author_name 'Peter A. Wood' _publ_section_title ; Effect of pressure on the crystal structure of salicylaldoxime-I, and the structure of salicylaldoxime-II at 5.93GPa ; _journal_coeditor_code SO5004 _journal_date_accepted 2006-08-11 _journal_date_recd_electronic 2006-06-03 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 1099 _journal_page_last 1111 _journal_paper_category FA _journal_volume 62 _journal_year 2006 _chemical_formula_moiety 'C7 H7 N1 O2' _chemical_formula_sum 'C7 H7 N O2' _chemical_formula_weight 137.14 _chemical_melting_point 60.0(10) _chemical_name_common salicylaldoxime _chemical_name_systematic '2-hydroxybenzaldehyde oxime' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method CRYSTALS_ver_12.80 _cell_angle_alpha 90 _cell_angle_beta 111.938(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.1833(16) _cell_length_b 4.9766(3) _cell_length_c 13.0109(15) _cell_measurement_reflns_used 363 _cell_measurement_temperature 293 _cell_measurement_theta_max 25 _cell_measurement_theta_min 3 _cell_volume 611.62(13) _computing_cell_refinement SAINT _computing_data_collection 'APEX-II (Bruker-Nonius, 2000)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.411 _diffrn_measured_fraction_theta_max 0.396 _diffrn_measurement_device_type 'Bruker-Nonius Apex II CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.6889 _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2288 _diffrn_reflns_theta_full 25.147 _diffrn_reflns_theta_max 26.752 _diffrn_reflns_theta_min 3.197 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS version 2004/1' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.489 _exptl_crystal_description block _exptl_crystal_F_000 288 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.11 _refine_diff_density_min -0.11 _refine_ls_extinction_coef 261.538 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _refine_ls_goodness_of_fit_ref 0.7929 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 97 _refine_ls_number_reflns 514 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0485 _refine_ls_shift/su_max 0.000129 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 625. 966. 587. 219. 45.4 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1359 _refine_ls_wR_factor_gt 0.1095 _refine_ls_wR_factor_ref 0.1359 _reflns_number_gt 335 _reflns_number_total 547 _reflns_threshold_expression I>2.00u(I) _[local]_cod_data_source_file so5004.cif _[local]_cod_data_source_block 0_75GPa _[local]_cod_cif_authors_sg_H-M 'P 1 21/n 1 ' _[local]_cod_chemical_formula_sum_orig 'C7 H7 N1 O2' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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: '_chemical_melting_point' value '59-61' was changed to '60.0(10)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value '59-61' was changed to '60.0(10)' - the average value was taken and precision was estimated. '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_database_code 2100708 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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_occupancy O O1 0.7422(5) 1.0304(5) 0.6845(2) 0.0410 Uani 1.0000 N N2 0.6891(6) 0.8738(5) 0.5881(2) 0.0315 Uani 1.0000 C C3 0.7755(7) 0.7001(6) 0.5847(3) 0.0304 Uani 1.0000 C C4 0.7451(7) 0.5146(6) 0.4903(3) 0.0275 Uani 1.0000 C C5 0.6093(7) 0.5109(6) 0.4046(3) 0.0276 Uani 1.0000 O O5 0.5073(5) 0.6860(5) 0.4024(2) 0.0362 Uani 1.0000 C C6 0.5818(7) 0.3273(6) 0.3186(3) 0.0330 Uani 1.0000 C C7 0.6832(8) 0.1496(6) 0.3176(3) 0.0365 Uani 1.0000 C C8 0.8188(8) 0.1508(7) 0.4009(3) 0.0383 Uani 1.0000 C C9 0.8444(8) 0.3316(6) 0.4872(3) 0.0318 Uani 1.0000 H H3 0.8692 0.6940 0.6468 0.0420 Uiso 1.0000 H H6 0.4876 0.3197 0.2603 0.0416 Uiso 1.0000 H H7 0.6602 0.0151 0.2592 0.0614 Uiso 1.0000 H H8 0.8909 0.0241 0.4001 0.0479 Uiso 1.0000 H H9 0.9385 0.3315 0.5476 0.0535 Uiso 1.0000 H H1 0.683(4) 1.152(7) 0.666(4) 0.0586 Uiso 1.0000 H H5 0.535(8) 0.794(6) 0.454(2) 0.0644 Uiso 1.0000 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 0.030(5) 0.0507(14) 0.0382(14) 0.0030(15) 0.009(2) -0.0073(10) N2 0.024(5) 0.0360(14) 0.0360(15) -0.0021(15) 0.013(2) -0.0012(10) C3 0.023(6) 0.0425(17) 0.0336(16) -0.001(2) 0.019(2) 0.0053(12) C4 0.021(4) 0.0355(14) 0.0342(17) 0.0023(18) 0.020(2) 0.0088(11) C5 0.020(4) 0.0318(14) 0.0394(18) 0.0038(17) 0.021(2) 0.0051(11) O5 0.020(4) 0.0459(13) 0.0457(14) 0.0068(14) 0.016(2) -0.0071(10) C6 0.026(5) 0.0421(17) 0.0394(18) -0.0019(19) 0.022(3) 0.0000(12) C7 0.044(5) 0.0407(16) 0.0418(19) 0.002(2) 0.036(3) -0.0018(13) C8 0.034(6) 0.0433(17) 0.057(2) 0.0133(19) 0.039(3) 0.0093(13) C9 0.016(5) 0.0432(16) 0.0463(19) 0.0026(19) 0.023(3) 0.0105(12) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 'International Tables Vol C 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 N2 O1 H1 99(3) no O1 N2 C3 112.1(4) yes N2 C3 C4 122.2(4) yes N2 C3 H3 117.9 no C4 C3 H3 119.8 no C3 C4 C5 120.2(6) yes C3 C4 C9 120.9(4) yes C5 C4 C9 118.8(4) yes C4 C5 O5 121.8(4) yes C4 C5 C6 119.1(5) yes O5 C5 C6 119.1(4) yes C5 O5 H5 112(5) no C5 C6 C7 120.6(4) yes C5 C6 H6 119.7 no C7 C6 H6 119.7 no C6 C7 C8 121.4(4) yes C6 C7 H7 119.4 no C8 C7 H7 119.2 no C7 C8 C9 117.5(6) yes C7 C8 H8 121.3 no C9 C8 H8 121.1 no C8 C9 C4 122.5(4) yes C8 C9 H9 118.6 no C4 C9 H9 118.9 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 N2 1.402(4) yes O1 H1 0.8200(9) no N2 C3 1.246(8) yes C3 C4 1.473(5) yes C3 H3 0.994 no C4 C5 1.416(6) yes C4 C9 1.372(9) yes C5 O5 1.348(7) yes C5 C6 1.390(5) yes O5 H5 0.8200(9) no C6 C7 1.363(9) yes C6 H6 0.977 no C7 C8 1.401(8) yes C7 H7 0.974 no C8 C9 1.385(6) yes C8 H8 0.971 no C9 H9 0.987 no _cod_database_fobs_code 2100708