############################################################################## ### FullProf-generated CIF output file (version: February 2008) ### ### Template of CIF submission form for structure report ### ############################################################################## # This file has been generated using FullProf.2k taking one example of # structure report provided by Acta Cryst. It is given as a 'template' with # filled structural items. Many other items are left unfilled and it is the # responsibility of the user to properly fill or suppress them. In principle # all question marks '?' should be replaced by the appropriate text or # numerical value depending on the kind of CIF item. # See the document: cif_core.dic (URL: http://www.iucr.org) for details. # Please notify any error or suggestion to: # Juan Rodriguez-Carvajal (jrc@ill.eu) # Improvements will be progressively added as needed. #============================================================================= data_global #============================================================================= # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name ? # Name of author for correspondence _publ_contact_author_address # Address of author for correspondence ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_contact_letter ; ? ; _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_requested_category ? # Acta C: one of CI/CM/CO/FI/FM/FO # Definition of non standard CIF items (Reliability indices used in FULLPROF) loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_info _publ_manuscript_incl_extra_defn # Name Explanation Standard? # ------ ----------- --------- '_pd_proc_ls_prof_cR_factor' 'Prof. R-factor CORRECTED for background' no '_pd_proc_ls_prof_cwR_factor' 'wProf.R-factor CORRECTED for background' no '_pd_proc_ls_prof_cwR_expected' 'wProf.Expected CORRECTED for background' no '_pd_proc_ls_prof_chi2' 'Chi-square for all considered points' no '_pd_proc_ls_prof_echi2' 'Chi-2 for points with Bragg contribution' no #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ' Fox/ObjCryst exported file:sq13_se_pb_xray' ; _publ_section_title_footnote ; ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address ? #<--'Last name, first name' ; ? ; ; ? ; #============================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= #============================================================================= # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_sq13_se_pb #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C22 H32 N4 O6' _chemical_formula_structural 'C22 H32 N4 O6' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H32 N4 O6' _chemical_formula_weight 448 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _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_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' 'x,y,z' '-x,y+1/2,-z+1/2' '-x,-y,-z' 'x,-y+1/2,z+1/2' _cell_length_a 12.9142(5) _cell_length_b 13.4373(2) _cell_length_c 6.82870(13) _cell_angle_alpha 90.00000 _cell_angle_beta 96.9271(17) _cell_angle_gamma 90.00000 _cell_volume 1176.35(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour 'colourless' # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source 'rotating-anode X-ray tube' _diffrn_radiation_type 'Cu K\a' _diffrn_source_target ? _diffrn_radiation_wavelength 1.54175 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 4999 _pd_meas_2theta_range_min 5.00800 _pd_meas_2theta_range_max 69.98200 _pd_meas_2theta_range_inc 0.013003 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 4.0535 _pd_proc_ls_prof_wR_factor 5.7888 _pd_proc_ls_prof_wR_expected 0.8686 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 11.9729 _pd_proc_ls_prof_cwR_factor 12.7844 _pd_proc_ls_prof_cwR_expected 1.9182 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 44.4188 _pd_proc_ls_prof_echi2 44.8518 # Items related to LS refinement _refine_ls_R_I_factor 3.3887 _refine_ls_number_reflns 1385 _refine_ls_number_parameters 112 _refine_ls_number_restraints 87 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 5.0038 _pd_proc_2theta_range_max 69.9778 _pd_proc_2theta_range_inc 0.013003 _pd_proc_wavelength 1.541840 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol C1 0.4450(7) 0.9288(8) 0.8872(13) 0.064(5) 1.00000 Uiso C C2 0.5052(7) 0.9632(10) 1.2141(12) 0.064(5) 1.00000 Uiso C N3 0.4120(7) 0.9535(7) 1.0865(11) 0.003(5) 1.00000 Uiso N C4 0.3637(6) 0.8656(5) 1.1542(12) 0.064(5) 1.00000 Uiso C H5 0.34986 0.87757 1.30441 0.12(2) 1.00000 Uiso H H6 0.40436 0.79645 1.14802 0.12(2) 1.00000 Uiso H C7 0.2519(6) 0.8488(5) 1.0528(12) 0.064(5) 1.00000 Uiso C H8 0.26020 0.81871 0.89664 0.12(2) 1.00000 Uiso H H9 0.21419 0.78316 1.11786 0.12(2) 1.00000 Uiso H C10 0.1771(6) 0.9357(6) 1.0289(12) 0.064(5) 1.00000 Uiso C H11 0.20730 0.99155 0.93255 0.12(2) 1.00000 Uiso H H12 0.18071 0.96537 1.17869 0.12(2) 1.00000 Uiso H N13 0.0782(6) 0.8977(6) 0.9550(10) 0.003(5) 1.00000 Uiso N H14 0.03884 0.87530 1.06841 0.12(2) 1.00000 Uiso H C15 0.0456(7) 0.8837(13) 0.7732(10) 0.064(5) 1.00000 Uiso C C16 0.0985(6) 0.8938(15) 0.5907(12) 0.064(5) 1.00000 Uiso C C17 -0.0456(6) 0.8618(15) 0.6673(12) 0.064(5) 1.00000 Uiso C C18 -0.0055(8) 0.8770(16) 0.4710(10) 0.064(5) 1.00000 Uiso C O19 0.1810(6) 0.9246(6) 0.5422(15) 0.040(4) 1.00000 Uiso O O20 -0.0420(7) 0.8788(5) 0.2921(10) 0.040(4) 1.00000 Uiso O O21 -0.1364(5) 0.8467(6) 0.7083(12) 0.040(4) 1.00000 Uiso O C22 -0.2142(6) 0.8363(6) 0.5462(12) 0.064(5) 1.00000 Uiso C H23 -0.20052 0.89755 0.45299 0.12(2) 1.00000 Uiso H C24 -0.3182(6) 0.8429(5) 0.6140(11) 0.064(5) 1.00000 Uiso C H25 -0.36648 0.88464 0.50919 0.12(2) 1.00000 Uiso H H26 -0.34489 0.76806 0.64416 0.12(2) 1.00000 Uiso H H27 -0.30390 0.88556 0.75884 0.12(2) 1.00000 Uiso H H28 -0.19841 0.76579 0.47056 0.12(2) 1.00000 Uiso H H29 0.56525 0.91799 1.19551 0.12(2) 1.00000 Uiso H H30 0.48658 0.98018 1.35782 0.12(2) 1.00000 Uiso H H31 0.37641 0.90414 0.77409 0.12(2) 1.00000 Uiso H H32 0.50273 0.86737 0.88678 0.12(2) 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag ? ? ? ? ? ? C1 N3 ? ? 1.51(1) ? C1 H31 ? ? 1.150 ? C1 H32 ? ? 1.110 ? C2 N3 ? ? 1.40(1) ? C2 H29 ? ? 1.010 ? C2 H30 ? ? 1.060 ? N3 C4 ? ? 1.44(1) ? C4 H5 ? ? 1.070 ? C4 H6 ? ? 1.070 ? C4 C7 ? ? 1.54(1) ? C7 H8 ? ? 1.16 ? C7 H9 ? ? 1.120 ? C7 C10 ? ? 1.51(1) ? C10 H11 ? ? 1.100 ? C10 H12 ? ? 1.090 ? C10 N13 ? ? 1.41(1) ? N13 H14 ? ? 1.020 ? N13 C15 ? ? 1.28(1) ? C15 C16 ? ? 1.50(1) ? C15 C17 ? ? 1.34(1) ? C16 C18 ? ? 1.50(1) ? C16 O19 ? ? 1.23(1) ? C17 C18 ? ? 1.51(1) ? C17 O21 ? ? 1.25(1) ? C18 O20 ? ? 1.26(1) ? O21 C22 ? ? 1.41(1) ? C22 H23 ? ? 1.07 ? C22 C24 ? ? 1.48(1) ? C22 H28 ? ? 1.110 ? C24 H25 ? ? 1.050 ? C24 H26 ? ? 1.090 ? C24 H27 ? ? 1.140 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag ? ? ? ? ? ? ? ? N3 C1 H31 ? ? ? 113.0 ? N3 C1 H32 ? ? ? 115.0 ? H31 C1 H32 ? ? ? 104.0 ? N3 C2 H29 ? ? ? 119.0 ? N3 C2 H30 ? ? ? 109.0 ? H29 C2 H30 ? ? ? 121 ? C1 N3 C2 ? ? ? 105.4(8) ? C1 N3 C4 ? ? ? 106.8(7) ? C2 N3 C4 ? ? ? 104.4(8) ? N3 C4 H5 ? ? ? 108.0 ? N3 C4 H6 ? ? ? 118.0 ? N3 C4 C7 ? ? ? 113.3(7) ? H5 C4 H6 ? ? ? 108.0 ? H5 C4 C7 ? ? ? 101.0 ? H6 C4 C7 ? ? ? 107.0 ? C4 C7 H8 ? ? ? 106.0 ? C4 C7 H9 ? ? ? 111.0 ? C4 C7 C10 ? ? ? 119.2(6) ? H8 C7 H9 ? ? ? 101.0 ? H8 C7 C10 ? ? ? 107.0 ? H9 C7 C10 ? ? ? 110.0 ? C7 C10 H11 ? ? ? 109.0 ? C7 C10 H12 ? ? ? 103.0 ? C7 C10 N13 ? ? ? 107.3(7) ? H11 C10 H12 ? ? ? 109.0 ? H11 C10 N13 ? ? ? 114.0 ? H12 C10 N13 ? ? ? 114.0 ? C10 N13 H14 ? ? ? 110.0 ? C10 N13 C15 ? ? ? 125.4(8) ? H14 N13 C15 ? ? ? 124.0 ? N13 C15 C16 ? ? ? 132(1) ? N13 C15 C17 ? ? ? 136(1) ? C16 C15 C17 ? ? ? 91.7(9) ? C15 C16 C18 ? ? ? 88.4(9) ? C15 C16 O19 ? ? ? 139(1) ? C18 C16 O19 ? ? ? 131(1) ? C15 C17 C18 ? ? ? 94(1) ? C15 C17 O21 ? ? ? 134(1) ? C18 C17 O21 ? ? ? 131(1) ? C16 C18 C17 ? ? ? 85.2(9) ? C16 C18 O20 ? ? ? 137(1) ? C17 C18 O20 ? ? ? 138(1) ? C17 O21 C22 ? ? ? 116.0(8) ? O21 C22 H23 ? ? ? 104.0 ? O21 C22 C24 ? ? ? 109.7(7) ? O21 C22 H28 ? ? ? 107.0 ? H23 C22 C24 ? ? ? 111.0 ? H23 C22 H28 ? ? ? 109.0 ? C24 C22 H28 ? ? ? 115.0 ? C22 C24 H25 ? ? ? 108.0 ? C22 C24 H26 ? ? ? 109.0 ? C22 C24 H27 ? ? ? 104.0 ? H25 C24 H26 ? ? ? 116.0 ? H25 C24 H27 ? ? ? 110.0 ? H26 C24 H27 ? ? ? 109.0 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _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 ? ? ? ? ? ? ? ? ? ? ? #============================================================================= #============================================================================= # Additional structures (last six sections and associated data_? identifiers) # may be added at this point. #============================================================================= # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./