#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/40/2104047.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_2104047
loop_
_publ_author_name
'McMullan, R. K.'
'Klooster, W. T.'
'Weber, H.-P.'
_publ_section_title
;
 Deuterated γ-malonic acid: its neutron crystal structure in
 relationship to other polymorphs of aliphatic dicarboxylic acids
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              230
_journal_page_last               239
_journal_paper_doi               10.1107/S0108768108000268
_journal_volume                  64
_journal_year                    2008
_chemical_formula_sum            'C3 D4 O4'
_chemical_formula_weight         108.03
_chemical_name_common            'Malonic Acid'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           NOOT-91
_cell_angle_alpha                103.350(10)
_cell_angle_beta                 136.680(10)
_cell_angle_gamma                85.070(10)
_cell_formula_units_Z            4
_cell_length_a                   10.6750(10)
_cell_length_b                   5.1520(10)
_cell_length_c                   11.2380(10)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    56.0(10)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      29
_cell_volume                     409.45(13)
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_structure_refinement  'UPALS (Lundgren,82)& NOOT(Craven et al.,91)'
_diffrn_ambient_temperature      56.0(10)
_diffrn_measurement_device_type  'four-circle diffractometers H6M'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  'Be 002'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'steady-state reactor'
_diffrn_radiation_type           Neutron
_diffrn_radiation_wavelength     1.0411
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4641
_diffrn_reflns_theta_max         55.3
_diffrn_reflns_theta_min         1.8
_exptl_absorpt_coefficient_mu    0.017
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Templeton & Templeton, 1973'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          3.0
_exptl_crystal_size_mid          2.4
_exptl_crystal_size_min          2.0
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.50
_refine_ls_extinction_coef       0.103(3)
_refine_ls_extinction_method     'Becker & Coppens'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[s²(Fo²)+(0.02(Fo²))²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.049
_reflns_number_total             3203
_reflns_threshold_expression     >0*sigma(I)
_cod_data_source_file            bk5069.cif
_cod_data_source_block           56K
_cod_database_code               2104047
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
C0A 0.04205(7) 0.11896(9) 0.23879(6) 0.0194(3) Uani 1
C1A 0.03183(6) 0.29815(9) 0.35818(6) 0.0138(2) Uani 1
C2A 0.02027(6) 0.27620(9) 0.12820(6) 0.0165(2) Uani 1
O11A 0.03222(8) 0.54172(11) 0.37671(7) 0.0188(3) Uani 1
O12A 0.02349(8) 0.16217(11) 0.43784(8) 0.0233(4) Uani 1
O21A 0.15011(8) 0.36856(15) 0.16683(9) 0.0406(7) Uani 1
O22A -0.15193(8) 0.30361(14) -0.01291(8) 0.0231(4) Uani 1
D12A 0.01138(10) 0.28128(14) 0.51244(9) 0.0360(5) Uani 1
D21A -0.15632(10) 0.42136(16) -0.07479(10) 0.0391(6) Uani 1
D01A 0.17582(11) 0.04376(16) 0.32382(10) 0.0533(8) Uani 1
D02A -0.06682(11) -0.05039(14) 0.15360(10) 0.0295(6) Uani 1
C0B 0.55955(7) 0.12864(9) 0.25266(6) 0.0168(2) Uani 1
C1B 0.54391(6) 0.30411(9) 0.36861(6) 0.0154(2) Uani 1
C2B 0.53307(6) 0.28594(9) 0.13935(6) 0.0135(2) Uani 1
O11B 0.52746(8) 0.54355(11) 0.37560(7) 0.0228(3) Uani 1
O12B 0.54962(8) 0.16994(11) 0.45802(8) 0.0284(4) Uani 1
O21B 0.65628(8) 0.43881(12) 0.19565(8) 0.0169(3) Uani 1
O22B 0.36412(8) 0.24381(12) -0.02455(7) 0.0148(2) Uani 1
D12B 0.52587(10) 0.28417(14) 0.52391(10) 0.0413(7) Uani 1
D21B 0.35296(10) 0.36400(10) -0.08948(9) 0.0308(5) Uani 1
D01B 0.69645(10) 0.06306(15) 0.34061(10) 0.0454(7) Uani 1
D02B 0.45652(11) -0.04779(14) 0.17057(10) 0.0272(4) Uani 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
O O 'International Tables Vol C Tables 4.4.4.1'
D D 'International Tables Vol C Tables 4.4.4.4'
C C 'International Tables Vol C Tables 4.4.4.4'
