Discovery and characterization of new crystal forms of bio-based nylon 4F salt
Wang, Yingying; Yang, Pengpeng; Li, Zihan; Shi, Yuzhong; Fu, Jinqiu; Zhang, Yajie; Zhang, Keke; Zhuang, Wei; Ying, Hanjie; CrystEngComm  (2022) –; doi:10.1039/D2CE00388K

data_7245171
_publ_section_title
;
 Discovery and characterization of new crystal forms of bio-based nylon 4F
 salt
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00388K
_journal_year                    2022
_chemical_formula_moiety         '2(C2 H7 N), C6 H2 O5, H2 O'
_chemical_formula_sum            'C10 H18 N2 O6'
_chemical_formula_weight         262.26
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-07-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                83.234(3)
_cell_angle_beta                 74.443(2)
_cell_angle_gamma                84.182(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9385(6)
_cell_length_b                   9.2887(8)
_cell_length_c                   10.7058(9)
_cell_measurement_reflns_used    1187
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.069
_cell_measurement_theta_min      2.256
_cell_volume                     658.32(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.961
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3620
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.214
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.9627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.050(10)
_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   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2591
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0781P)^2^+0.2879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1735
_reflns_number_total             2591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00388k2.cif
_cod_data_source_block           210519d
_cod_database_code               7245171
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Restrained distances
 C9-C10' = C9-C10
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C10 \\sim C10': within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C10) \\sim Ueq, Uanis(C10') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H9BC)=Sof(H9BD)=Sof(C10')=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
5.a Riding coordinates:
 O6(H6A,H6B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9AA,H9AB), C10(H10A,H10B), C10'(H10C,H10D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
5.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              39900
_olex2_submission_special_instructions 'No special instructions were received'