Shape memory and self-healing in a molecular crystal with inverse temperature symmetry breaking.
Meng, Jiantao; Su, Yuan; Zhu, Hang; Cai, Ting; Chemical science 15 (2024) 5738–5745; doi:10.1039/d3sc06800e

data_1571211
_publ_section_title
;
 Shape memory and self-healing in a molecular crystal with inverse
 temperature symmetry breaking.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              5738
_journal_page_last               5745
_journal_paper_doi               10.1039/d3sc06800e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C10 H15 N5 O3'
_chemical_formula_sum            'C10 H15 N5 O3'
_chemical_formula_weight         253.27
_chemical_name_common
2-amino-9-[4-hydroxy-3-(hydroxymethyl)butyl]-1H-purin-6-one
_chemical_name_systematic        penciclovir
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-12 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                87.335(12)
_cell_angle_beta                 80.598(13)
_cell_angle_gamma                86.279(15)
_cell_formula_units_Z            4
_cell_length_a                   9.093(4)
_cell_length_b                   10.918(4)
_cell_length_c                   11.805(4)
_cell_measurement_reflns_used    3119
_cell_measurement_temperature    400
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      3.12
_cell_volume                     1153.0(8)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      400
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13021
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.451
_diffrn_reflns_theta_min         1.870
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1526 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.8721. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_recrystallization_method 'Cooperative phase transition'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4689
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0759P)^2^+0.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2826
_reflns_number_total             4689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06800e15.cif
_cod_data_source_block           mo_2022710_0m
_cod_depositor_comments
'Adding full bibliography for 1571210--1571211.cif.'
_cod_original_cell_volume        1153.1(8)
_cod_database_code               1571211
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 C19, C18
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C19 \\sim C18: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
4.a Ternary CH refined with riding coordinates:
 C18(H18), C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C7(H7a,H7b), C6(H6a,H6b), C16(H16a,H16b), C10(H10a,H10b),
 C19(H19a,H19b), C9(H9a,H9b), C20(H20a,H20b)
4.c Aromatic/amide H refined with riding coordinates:
 N007(H007), N008(H008), C5(H5), C15(H15)
4.d X=CH2 refined with riding coordinates:
 N00A(H00a,H00b), N00B(H00c,H00d)
4.e Idealised tetrahedral OH refined as rotating group:
 O5(H5a), O6(H6), O2(H2), O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'