Optically active derivatives of terephthalic acid: four crystal structures from two powder patterns
Veselovsky, Vladimir V.; Lozanova, Antonina V.; Isaeva, Vera I.; Lobova, Anna A.; Fitch, Andrew N.; Chernyshev, Vladimir V.; Acta Crystallographica Section C Structural Chemistry 74 (2018) –; doi:10.1107/S2053229618001705

data_2021006
_publ_section_title
;
 Optically active derivatives of terephthalic acid: four crystal
 structures from two powder patterns
;
_journal_issue                   3
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229618001705
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C18 H22 N2 O7, 2.08H2 O'
_chemical_formula_moiety         'C18 H22 N2 O7, 2.08(H2 O)'
_chemical_formula_sum            'C18 H26.16 N2 O9.08'
_chemical_formula_weight         415.89
_chemical_name_systematic
;
1-{[1-(1-<i>tert</i>-Butoxycarbonyl)-<i>L</i>-prolyl]amino}terephthalic acid
2.08-hydrate
;
_space_group_IT_number           17
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c 2'
_symmetry_space_group_name_H-M   'P 2 2 21'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.4332(13)
_cell_length_b                   12.3817(12)
_cell_length_c                   21.3581(17)
_cell_measurement_reflns_used    1089
_cell_measurement_temperature    295.0(10)
_cell_measurement_theta_max      8.495
_cell_measurement_theta_min      0.697
_cell_volume                     4345.8(6)
_computing_cell_refinement
;
MRIA (Zlokazov & Chernyshev, 1992)
;
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
MRIA (Zlokazov & Chernyshev, 1992)
;
_computing_structure_solution
;
MRIA (Zlokazov & Chernyshev, 1992)
;
_diffrn_ambient_temperature      295.0(10)
_diffrn_measurement_device_type  'ESRF powder diffractometer'
_diffrn_radiation_monochromator  'Si 111 double crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.399962(3)
_exptl_absorpt_coefficient_mu    0.023
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1767
_pd_block_diffractogram_id       V03_pattern
_pd_char_colour                  colorless
_pd_char_particle_morphology     'no specific habit'
_pd_instr_location
;
ID31 beam line, ESRF, Grenoble, France
;
_pd_meas_2theta_range_inc        0.0015
_pd_meas_2theta_range_max        16.9995
_pd_meas_2theta_range_min        1.2000
_pd_meas_number_of_points        10534
_pd_meas_scan_method             cont
_pd_prep_pressure                101
_pd_prep_temperature             295.0(10)
_pd_proc_2theta_range_inc        0.0015
_pd_proc_2theta_range_max        16.9995
_pd_proc_2theta_range_min        1.2000
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function
;
split-type pseudo-Voigt (Toraya, 1986)
[Toraya, H. (1986). <i>J. Appl. Cryst.</i> <b>19</b>, 440--447]
;
_pd_proc_ls_prof_R_factor        0.0308
_pd_proc_ls_prof_wR_expected     0.0279
_pd_proc_ls_prof_wR_factor       0.0395
_pd_proc_wavelength              0.399962(3)
_pd_spec_mounting
;
Specimen was sealed in a 1.0 mm diameter borosilicate glass capillary
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              15
_pd_spec_size_equat              1.0
_pd_spec_size_thick              1.0
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.4151
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    86
_refine_ls_number_parameters     334
_refine_ls_number_restraints     210
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            yo3046sup1.cif
_cod_data_source_block           1b
_cod_database_code               2021006
_cod_database_fobs_code          2021006