#------------------------------------------------------------------------------
#$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: svn://www.crystallography.net/cod/cif/2/2104048.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_2104048
loop_
_publ_author_name
'McMullan, R. K.'
'Klooster, W. T.'
'Weber, H.-P.'
_publ_section_title
;
 Deuterated \g-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_volume                  64
_journal_year                    2008
_chemical_formula_sum            'C3 D4 O4'
_chemical_formula_weight         108.03
_chemical_name_common            'Malonic Acid'
_chemical_name_systematic
;
 ?
;
_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                103.33(3)
_cell_angle_beta                 136.40(2)
_cell_angle_gamma                84.76(3)
_cell_formula_units_Z            2
_cell_length_a                   5.333(2)
_cell_length_b                   5.158(2)
_cell_length_c                   11.250(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    153.0(10)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      29
_cell_volume                     206.34(15)
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_structure_refinement  'UPALS(Lundgren,'82)& NOOT(Craven et al.,91)'
_diffrn_ambient_temperature      153.0(10)
_diffrn_measurement_device_type  'four-circle diffractometers H6S'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  'Ge 022'
_diffrn_radiation_source         'steady-state reactor'
_diffrn_radiation_type           Neutron
_diffrn_radiation_wavelength     1.1588
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_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            1345
_diffrn_reflns_theta_max         54.2
_diffrn_reflns_theta_min         1.8
_exptl_absorpt_coefficient_mu    0.0177
_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    1.733
_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         0.53
_refine_diff_density_min         -0.60
_refine_ls_extinction_coef       0.125(3)
_refine_ls_extinction_method     'Becker & Coppens'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.020 (Fo^2^))^2^+514]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.040
_reflns_number_total             1169
_reflns_threshold_expression     >0*sigma(I)
_[local]_cod_data_source_file    bk5069.cif
_[local]_cod_data_source_block   153K
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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'
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
C0 0.60455(14) 0.12563(10) 0.24685(7) 0.0309(5) Uani 1
C1 0.57591(13) 0.30175(10) 0.36341(6) 0.0247(4) Uani 1
C2 0.55587(14) 0.28324(10) 0.13513(7) 0.0255(4) Uani 1
O11 0.55832(17) 0.54299(12) 0.37553(8) 0.0362(6) Uani 1
O12 0.5723(5) 0.1654(4) 0.4458(3) 0.0531(8) Uani 1
O21 0.8066(5) 0.4133(4) 0.1845(3) 0.0436(7) Uani 1
O22 0.2170(5) 0.2676(5) -0.0190(3) 0.0343(6) Uani 1
D12 0.5371(2) 0.28112(18) 0.51686(12) 0.0552(8) Uani 1
D21 0.1988(2) 0.3852(2) -0.08380(13) 0.0451(7) Uani 1
D01 0.8758(2) 0.05620(15) 0.33327(10) 0.0742(10) Uani 1
D02 0.3974(2) -0.04627(14) 0.16512(10) 0.0431(7) Uani 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C0 0.0195(2) 0.0123(2) 0.0155(2) 0.0034(2) 0.0145(2) 0.0043(2)
C1 0.0136(2) 0.0114(2) 0.0126(2) 0.0025(2) 0.0106(2) 0.0043(2)
C2 0.0152(2) 0.0136(2) 0.0126(2) 0.0017(2) 0.0112(2) 0.0035(2)
O11 0.0207(3) 0.0115(2) 0.0184(3) 0.0035(2) 0.0167(3) 0.0047(2)
O12 0.0285(3) 0.0131(3) 0.0215(3) 0.0055(2) 0.0220(3) 0.0070(2)
O21 0.0145(3) 0.0379(4) 0.0210(3) 0.0019(3) 0.0110(2) 0.0171(3)
O22 0.0172(3) 0.0313(3) 0.0154(3) -0.0051(3) 0.0082(3) 0.0094(3)
D12 0.0337(5) 0.0204(4) 0.0268(4) 0.0055(3) 0.0258(4) 0.0076(3)
D21 0.0239(4) 0.0374(5) 0.0211(4) -0.0013(3) 0.0135(3) 0.0123(3)
D01 0.0318(5) 0.0314(4) 0.0325(4) 0.0177(3) 0.0266(4) 0.0188(3)
D02 0.0410(5) 0.0197(4) 0.0285(4) -0.0066(3) 0.0269(4) -0.0006(3)
_cod_database_code 2104048