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_7245170
_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             2022-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                71.2540(10)
_cell_angle_beta                 76.887(2)
_cell_angle_gamma                76.887(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2019(8)
_cell_length_b                   9.8663(9)
_cell_length_c                   9.8663(8)
_cell_measurement_reflns_used    1014
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.907
_cell_measurement_theta_min      2.668
_cell_volume                     637.49(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 0.966
_diffrn_measured_fraction_theta_max 0.957
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3466
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9669
_exptl_absorpt_correction_T_min  0.9562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2485
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0866P)^2^+0.5134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1582
_reflns_number_total             2485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00388k2.cif
_cod_data_source_block           201114g
_cod_database_code               7245170
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Restrained distances
 O6-H6B
 0.85 with sigma of 0.01
 H6B-H6A
 1.45 with sigma of 0.01
3.a Riding coordinates:
 O6(H6A)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
3.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              52048
_olex2_submission_special_instructions 'No special instructions were received'