Isotopomeric polymorphism in a “doubly-polymorphic” multi-component molecular crystal
Schmidtmann, Marc; Middlemiss, Derek S.; Wilson, Chick C.; CrystEngComm 17 (2015) 5273–; doi:10.1039/C5CE00123D

data_7219985
_publ_section_title
;
 Isotopomeric polymorphism in a &#x201C;doubly-polymorphic&#x201D;
 multi-component molecular crystal
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5273
_journal_paper_doi               10.1039/C5CE00123D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         '2[DC6H4D2N2O]+ [C2O4]2'
_chemical_formula_sum            'C14 H8 D6 N4 O6'
_chemical_formula_weight         340.33
_chemical_name_systematic        'bis(isonicotinamide)-d-oxalic acid Form I'
_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           SHELXL-97
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                98.262(4)
_cell_angle_beta                 90.019(4)
_cell_angle_gamma                91.709(5)
_cell_formula_units_Z            1
_cell_length_a                   3.7233(3)
_cell_length_b                   7.4294(5)
_cell_length_c                   12.3158(10)
_cell_measurement_reflns_used    5440
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.29
_cell_measurement_theta_min      2.77
_cell_volume                     336.99(4)
_computing_cell_refinement       'Bruker AXS SAINT V7.34A'
_computing_data_collection       'Bruker AXS X8 Apex2'
_computing_data_reduction        'Bruker AXS SAINT V7.34A'
_computing_molecular_graphics    'Bruker AXS XP'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10173
_diffrn_reflns_theta_full        33.99
_diffrn_reflns_theta_max         33.99
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             174
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: D2O'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                2505
_reflns_number_total             2744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00123d2.cif
_cod_data_source_block           doxaiso
_cod_depositor_comments
'Adding full bibliography for 7219985--7219986.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7219985