Thymine cocrystals based on DNA-inspired binding motifs
Koch, Elizabeth S.; McKenna, Kelly A.; Kim, Hyo Jung; Young, Victor G.; Swift, Jennifer A.; CrystEngComm  (2017) –; doi:10.1039/C7CE01347G

data_7229160
_publ_section_title
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 Thymine cocrystals based on DNA-inspired binding motifs
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01347G
_journal_year                    2017
_chemical_formula_moiety         'C5 H6 N2 O2, C4 H7 N5, O H2'
_chemical_formula_sum            'C9 H15 N7 O3'
_chemical_formula_weight         269.28
_chemical_name_common            Thymine:2,4,6-triaminopyrimidine
_chemical_name_systematic        T:246TAPM
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
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2016-09-12 deposited with the CCDC.
2017-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                104.7164(14)
_cell_angle_beta                 96.7763(13)
_cell_angle_gamma                90.5177(14)
_cell_formula_units_Z            4
_cell_length_a                   6.7793(2)
_cell_length_b                   12.3197(4)
_cell_length_c                   14.8694(4)
_cell_measurement_reflns_used    4566
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.754
_cell_measurement_theta_min      0.829
_cell_volume                     1191.76(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4424
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.715
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.753622
_exptl_absorpt_correction_T_min  0.308952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1546 before and 0.0514 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1674 before and 0.0755 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1074P)^2^+0.4075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4217
_reflns_number_total             4424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01347g2.cif
_cod_data_source_block           twin5c
_cod_database_code               7229160
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   40.0205
_shelx_estimated_absorpt_t_min   3.098
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.903(2) 0.097(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 N1A(H1AA), N2A(H2AA), C3A(H3AA), C8A(H8AA), N1B(H1BA), N2B(H2BA), C3B(H3BA),
 C8B(H8BA)
3.b Idealised Me refined as rotating group:
 C5A(H5AA,H5AB,H5AC), C5B(H5BA,H5BB,H5BC)
;
_olex2_submission_special_instructions 'No special instructions were received'