#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/40/2104046.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_2104046
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_coeditor_code           BK5069
_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                103.39(3)
_cell_angle_beta                 136.81(2)
_cell_angle_gamma                85.19(3)
_cell_formula_units_Z            4
_cell_length_a                   10.663(4)
_cell_length_b                   5.142(2)
_cell_length_c                   11.234(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    50.0(10)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      29
_cell_volume                     406.8(3)
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_structure_refinement  'UPALS(Lundgren,82)&NOOT(Craven et al.,91)'
_diffrn_ambient_temperature      50.0(10)
_diffrn_measurement_device_type  'four-circle diffractometers H6S'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  'Ge 022'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'steady-state reactor'
_diffrn_radiation_type           Neutron
_diffrn_radiation_wavelength     1.1588
_diffrn_reflns_av_R_equivalents  0.019
_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            2653
_diffrn_reflns_theta_max         54.2
_diffrn_reflns_theta_min         1.8
_exptl_absorpt_coefficient_mu    0.018
_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    1.758
_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         0.27
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       0.102(2)
_refine_ls_extinction_method     'Becker & Coppens'
_refine_ls_goodness_of_fit_ref   1.53
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[s²(Fo²)+(0.02(Fo²)²+0.05]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.052
_reflns_number_total             2307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk5069.cif
_cod_data_source_block           50K
_cod_database_code               2104046
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C C0A 0.03930(9) 0.11744(12) 0.23688(8) 0.0148(2) Uani 1
C C1A 0.03043(8) 0.29771(12) 0.35716(8) 0.0111(2) Uani 1
C C2A 0.01821(8) 0.27417(12) 0.12644(8) 0.0122(2) Uani 1
O O11A 0.03285(10) 0.54168(14) 0.37702(9) 0.0169(2) Uani 1
O O12A 0.02100(10) 0.16141(14) 0.43609(10) 0.0218(2) Uani 1
O O21A 0.14782(10) 0.35536(17) 0.16073(11) 0.0318(2) Uani 1
O O22A -0.15367(10) 0.31321(16) -0.01041(10) 0.0236(2) Uani 1
H D12A 0.01040(13) 0.28907(17) 0.51169(12) 0.0334(2) Uani 1
H D21A -0.15710(12) 0.43044(18) -0.07171(12) 0.0336(2) Uani 1
H D01A 0.17288(13) 0.04118(19) 0.32179(12) 0.0487(2) Uani 1
H D02A -0.07034(13) -0.05104(17) 0.15137(12) 0.0314(2) Uani 1
C C0B 0.55989(9) 0.12874(12) 0.25322(8) 0.0142(2) Uani 1
C C1B 0.54465(8) 0.30473(12) 0.36932(8) 0.0119(2) Uani 1
C C2B 0.53347(8) 0.28585(12) 0.13977(8) 0.0113(2) Uani 1
O O11B 0.52689(10) 0.54377(14) 0.37533(9) 0.0192(2) Uani 1
O O12B 0.55247(11) 0.17081(14) 0.46038(10) 0.0239(2) Uani 1
O O21B 0.65638(10) 0.44400(15) 0.19758(10) 0.0213(2) Uani 1
O O22B 0.36557(10) 0.23937(15) -0.02523(10) 0.0186(2) Uani 1
H D12B 0.52762(12) 0.28434(17) 0.52534(12) 0.0408(2) Uani 1
H D21B 0.35396(12) 0.35973(18) -0.09028(12) 0.0331(2) Uani 1
H D01B 0.69712(13) 0.06327(18) 0.34140(12) 0.0488(2) Uani 1
H D02B 0.45644(17) -0.04789(17) 0.17098(12) 0.0248(2) 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'
