Deuterated γ-malonic acid: its neutron crystal structure in relationship to other polymorphs of aliphatic dicarboxylic acids
McMullan, R. K.; Klooster, W. T.; Weber, H.-P.; Acta Crystallographica Section B 64 (2008) 230–239; doi:10.1107/S0108768108000268

data_2104047
_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_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/[s^2^(Fo^2^)+(0.02(Fo^2^))^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