Polymorphic transition due to grinding: the case of 3-[1-(<i>tert</i>-butoxycarbonyl)azetidin-3-yl]-1,2-oxazole-4-carboxylic acid
Konovalova, Irina S.; Shaposhnyk, Anna M.; Baumer, Vyacheslav N.; Chalyk, Bohdan A.; Shishkina, Svitlana V.; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S2052520622003900

data_2108997
_publ_section_title
;
 Polymorphic transition due to grinding: the case of
 3-[1-(<i>tert</i>-butoxycarbonyl)azetidin-3-yl]-1,2-oxazole-4-carboxylic
 acid
;
_journal_issue                   '3 Part 2'
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520622003900
_journal_volume                  78
_journal_year                    2022
_chemical_formula_moiety         'C12 H16 N2 O5'
_chemical_formula_sum            'C12 H16 N2 O5'
_chemical_formula_weight         268.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 112.480(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3254(10)
_cell_length_b                   8.7613(7)
_cell_length_c                   11.4085(8)
_cell_measurement_reflns_used    1931
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.876
_cell_measurement_theta_min      3.694
_cell_volume                     1323.07(18)
_computing_molecular_graphics    'Mercury 3.1 (Macrae et al., 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8684
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.023
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       stick
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0893P)^2^+0.1233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1858
_reflns_number_total             2319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5096sup1.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2108997
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              13319
_shelx_hkl_checksum              19996
_cod_database_fobs_code 2108997