Crystal forms and phase transformation of 1,5-pentanediamine-terephthalate: a bio-based nylon 5T monomer
Li, Zihan; Yang, Pengpeng; Liu, Haodong; Liu, Jun; Zhu, Sha; Li, Xiaojie; Zhuang, Wei; Wu, Jinglan; Ying, Hanjie; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620006265

data_2108619
_publ_section_title
;
 Crystal forms and phase transformation of
 1,5-pentanediamine-terephthalate: a bio-based nylon 5T monomer
;
_journal_coeditor_code           UM5041SUP1
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620006265
_journal_volume                  76
_journal_year                    2020
_chemical_formula_sum            'C13 H22 N2 O5'
_chemical_formula_weight         286.32
_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-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 96.728(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8441(8)
_cell_length_b                   10.8561(9)
_cell_length_c                   13.5205(12)
_cell_measurement_reflns_used    2154
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.048
_cell_measurement_theta_min      2.413
_cell_volume                     1435.0(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6997
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         2.413
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9829
_exptl_absorpt_correction_T_min  0.9528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0646P)^2^+0.0978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1801
_reflns_number_total             2515
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {b6ef982a-b86a-4f90-9861-ccf2d7492dd8}
_cod_data_source_file            um5041sup1.cif
_cod_data_source_block           monohydrate
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2108619
_cod_database_fobs_code          2108619
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              60352
_shelx_hkl_checksum              89337