Crystal-to-crystal polymorphic phase transition in a cocrystal accompanied by expansion and surface wettability change
Saikia, Plabon; Gupta, Poonam; Nath, Tridib R.; Nath, Naba K.; CrystEngComm 26 (2024) 4259–4263; doi:10.1039/D4CE00407H

data_7249052
_publ_section_title
;
 Crystal-to-crystal polymorphic phase transition in a cocrystal
 accompanied by expansion and surface wettability change
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4259
_journal_page_last               4263
_journal_paper_doi               10.1039/D4CE00407H
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C10 H12 O3, C6 H5 N2'
_chemical_formula_sum            'C16 H17 N2 O3'
_chemical_formula_weight         285.325
_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_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-04-01
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-03 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.09(3)
_cell_angle_beta                 84.05(3)
_cell_angle_gamma                69.20(3)
_cell_formula_units_Z            2
_cell_length_a                   7.048(8)
_cell_length_b                   7.351(8)
_cell_length_c                   15.499(16)
_cell_measurement_reflns_used    2658
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.69
_cell_volume                     734.1(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-beta (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9521
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.9947
_diffrn_reflns_Laue_measured_fraction_max 0.9521
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23890
_diffrn_reflns_point_group_measured_fraction_full 0.9947
_diffrn_reflns_point_group_measured_fraction_max 0.9521
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.04
_diffrn_reflns_theta_min         3.02
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3714
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1468 before and 0.0892 after correction.
The Ratio of minimum to maximum transmission is 0.4981.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             302.206
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.3308
_refine_diff_density_min         -0.2977
_refine_diff_density_rms         0.0740
_refine_ls_d_res_high            0.7321
_refine_ls_d_res_low             6.7562
_refine_ls_extinction_coef       0.123(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0435
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0435
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.1060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              9
_reflns_limit_k_min              -9
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2170
_reflns_number_total             3717
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00407h3.cif
_cod_data_source_block           BPA-PP
_cod_depositor_comments          'Adding full bibliography for 7249052.cif.'
_cod_database_code               7249052
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2a), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c)
;
_olex2_submission_special_instructions 'No special instructions were received'