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--#


