Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global #============================================================================== # 2. TITLE AND AUTHOR LIST _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 #============================================================================== #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Richard M Ibberson' _publ_contact_author_address ; ISIS Facility CCLRC - Rutherford Appleton Laboratory Chilton, Didcot Oxfordshire UK OX11 0QX ; _publ_contact_author_email r.m.ibberson@rl.ac.uk _publ_contact_author_fax '+44 (0)1235 445383' _publ_contact_author_phone '+44 (0)1235 445871' _publ_contact_letter ; This cif file contains details of the low-temperature crystal structure of alloxan, C4N2O4D2, at 2 K for deposition. Details of the research paper (to be submitted) relating to the structure are given below. ; _publ_section_title ; Alloxan - the phase II structure ; # 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_address R.M.Ibberson ; ISIS Facility STFC - Rutherford Appleton Laboratory Harwell Science and Innovation Campus Didcot Oxfordshire, OX11 0QX UK ; W.G.Marshall ; ISIS Facility STFC - Rutherford Appleton Laboratory Harwell Science and Innovation Campus Didcot Oxfordshire, OX11 0QX UK ; L.E.Budd ; School of Chemistry University of Edinburgh Joseph Black Building West Mains Road Edinburgh, EH9 3JJ UK ; S.Parsons ; School of Chemistry University of Edinburgh Joseph Black Building West Mains Road Edinburgh, EH9 3JJ UK ; C.R.Pulham ; School of Chemistry University of Edinburgh Joseph Black Building West Mains Road Edinburgh, EH9 3JJ UK ; ; C.K.Spanswick ; ; School of Chemistry University of Edinburgh Joseph Black Building West Mains Road Edinburgh, EH9 3JJ UK ; data_ALLOXAN_2K _database_code_depnum_ccdc_archive 'CCDC 664982' _chemical_name_systematic ; perdeuteroalloxan ; _chemical_name_common perdeuteroalloxan _chemical_formula_moiety 'C4 D2 N2 O4 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_length_neutron _atom_type_scat_source C 16.0 0.6646 International_Tables_Vol_C N 8.0 0.9360 International_Tables_Vol_C O 16.0 0.5803 International_Tables_Vol_C D 8.0 0.6671 International_Tables_Vol_C _diffrn_radiation_probe neutron #============================================================================== # 4. POWDER SPECIMEN AND CRYSTAL DATA _pd_phase_name Alloxan-d2 _cell_length_a 5.82141(4) _cell_length_b 5.85450(4) _cell_length_c 13.85255(9) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 472.115(4) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _cell_measurement_temperature 2 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C4 D2 N2 O4' _chemical_formula_weight 144.08 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.0270 _cell_special_details ; ? ; _geom_special_details ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity C C1 0.2019(5) -0.0436(4) 0.1306(2) 1.0 Uiso 0.00931(19) 4 N N1 0.38944(3) -0.0712(3) 0.07071(15) 1.0 Uiso 0.00931(19) 4 C C3 0.5679(4) 0.0784(5) 0.0601(2) 1.0 Uiso 0.00931(19) 4 C C2 0.5569(5) 0.2919(4) 0.1212(2) 1.0 Uiso 0.00931(19) 4 C C3A 0.3486(4) 0.3259(4) 0.1870(2) 1.0 Uiso 0.00931(19) 4 N N1A 0.1908(3) 0.1541(3) 0.18521(14) 1.0 Uiso 0.00931(19) 4 O O1 0.0570(5) -0.1948(5) 0.1367(2) 1.0 Uiso 0.0116(4) 4 D D1 0.3875(5) -0.2143(5) 0.0279(2) 1.0 Uiso 0.0234(5) 4 O O3 0.7305(5) 0.0430(5) 0.0069(2) 1.0 Uiso 0.0116(4) 4 O O2 0.7053(6) 0.4325(5) 0.1179(3) 1.0 Uiso 0.0116(4) 4 O O3A 0.3354(5) 0.4913(5) 0.2397(2) 1.0 Uiso 0.0116(4) 4 D D1A 0.0583(5) 0.1648(5) 0.2353(2) 1.0 Uiso 0.0234(5) 4 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.381(3) . 1_555 N C1 N1A 1.384(3) . 1_555 N C1 O1 1.226(3) . 1_555 N N1 C1 1.381(3) . 1_555 N N1 C3 1.367(3) . 1_555 N N1 D1 1.027(3) . 1_555 N C3 N1 1.367(3) . 1_555 N C3 C2 1.511(4) . 1_555 N C3 O3 1.217(4) . 1_555 N C2 C3 1.511(4) . 1_555 N C2 C3A 1.530(4) . 1_555 N C2 O2 1.194(3) . 1_555 N C3A C2 1.530(4) . 1_555 N C3A N1A 1.363(3) . 1_555 N C3A O3A 1.215(4) . 1_555 N N1A D1A 1.039(3) . 1_555 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N1A 117.59(21) 1_555 . 1_555 N N1 C1 O1 120.02(24) 1_555 . 1_555 N N1A C1 O1 122.34(26) 1_555 . 1_555 N C1 N1 C3 126.21(19) 1_555 . 1_555 N C1 N1 D1 115.76(25) 1_555 . 1_555 N C3 N1 D1 117.94(25) 1_555 . 1_555 N N1 C3 C2 115.95(20) 1_555 . 1_555 N N1 C3 O3 123.21(28) 1_555 . 1_555 N C2 C3 O3 120.82(26) 1_555 . 1_555 N C3 C2 C3A 118.36(19) 1_555 . 1_555 N C3 C2 O2 121.24(25) 1_555 . 1_555 N C3A C2 O2 120.39(26) 1_555 . 1_555 N C2 C3A N1A 115.30(21) 1_555 . 1_555 N C2 C3A O3A 120.80(26) 1_555 . 1_555 N N1A C3A O3A 123.81(26) 1_555 . 1_555 N C1 N1A C3A 126.58(21) 1_555 . 1_555 N C1 N1A D1A 116.71(27) 1_555 . 1_555 N C3A N1A D1A 116.35(25) 1_555 . 1_555 N loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 D1 O1 1.027(3) 2.541(4) 3.329(3) 133.2(2) . . 3_545 N N1 D1 O3 1.027(3) 2.184(4) 3.105(3) 148.3(2) . . 3_445 N N1A D1A O1 1.039(3) 2.066(4) 2.992(3) 146.9(3) . . 4_555 N N1A D1A O3A 1.039(3) 2.531(4) 3.373(3) 137.7(2) . . 4_545 N #============================================================================== # 5. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; None ; # 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 ; ISIS Facility, Rutherford Appleton Laboratory, UK. ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; HRPD is calibrated using the Si standard reference material 640C suppplied by N.I.S.T.. ; _diffrn_ambient_temperature ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type 'time-of-flight neutron' _diffrn_measurement_device_type HRPD _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _diffrn_radiation_wavelength 1.24-5.36 _pd_meas_scan_method 'tof 30-130 ms' # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # 6. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 20 # perpendicular to # equatorial plane _pd_spec_size_equat 15 # parallel to # scattering vector # in transmission _pd_spec_size_thick 2 # 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. ; standard cylindrical vanadium sample holder ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology 'irregular powder' _pd_char_colour yellow # use ICDD colour descriptions _pd_proc_ls_prof_R_factor 0.0468 _pd_proc_ls_prof_wR_factor 0.0524 _pd_proc_ls_prof_wR_expected 0.0315 _refine_ls_R_Fsqd_factor 0.04559 _refine_diff_density_max 0.068 _refine_diff_density_min -0.064 _pd_proc_ls_profile_function ; TOPAS TOF Profile function ; _pd_proc_ls_background_function ; Shifted Chebyshev function (10 terms) ; _pd_proc_ls_pref_orient_corr ; None ; _pd_calc_method 'Rietveld Refinement' _pd_instr_dist_src/spec 95000. _pd_instr_dist_spec/detc 890. _pd_meas_2theta_fixed 168.33 #============================================================================== # 7. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; Uiso values were constrained to be equal for similar atomic species. Checkcif output TYPE031_ALERT_1_A _diffrn_radiation_wavelength is not of type numb. Time-of-flight neutron diffraction utilises a polychromatic beam at fixed scattering angle. Accordingly minimum and maximum values for the radiation wavelength have been quoted. PLAT432_ALERT_2_A Short Inter X...Y Contact O3A .. C2 .. 2.68 Ang. No action taken PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O3A .. 2.84 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O3 .. C2 .. 2.77 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O3 .. C3A .. 2.88 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O3A .. C3A .. 2.87 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O3A .. C3 .. 2.88 Ang. No action taken CELLK01_ALERT_1_C Check that the cell measurement temperature is in Kelvin. Value of measurement temperature given = 2.000 No action taken PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ? Sample is deuterated. PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 4 Ang. PLAT142_ALERT_4_C su on b - Axis Small or Missing (x 100000) ..... 4 Ang. PLAT143_ALERT_4_C su on c - Axis Small or Missing (x 100000) ..... 9 Ang. This level of precision on lattice parameters determined by high-resolution powder diffraction is not unusual. RADNT01_ALERT_1_G Extra text has been found in the _diffrn_radiation_type field. Radiation given as time-of-flight neutron Radiation identified as neutron No action taken ; _pd_proc_ls_special_details ; ? ; _refine_ls_shift/su_max 0.02 _refine_ls_shift/su_mean 0.00 _computing_structure_refinement TOPAS _refine_ls_number_parameters 55 _refine_ls_goodness_of_fit_all 1.67 _refine_ls_number_restraints 0 _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints 0 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution 'TOPAS-Academic (Coehlo)' _computing_data_collection 'ISIS instrument control program (ICP)' _computing_cell_refinement 'TOPAS-Academic (Coehlo)' _computing_data_reduction 'Standard HRPD normalisation routines' #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#