Supramolecular Gels Derived from Simple Organic Salts of Flufenamic Acid: Design, Synthesis, Structures, and Plausible Biomedical Application
Parveen, Rumana; Jayamma, Bandi; Dastidar, Parthasarathi; ACS Biomaterials Science & Engineering 5 (2019) 2180–; doi:10.1021/acsbiomaterials.9b00153

data_4514605
_publ_section_title
;
 Supramolecular Gels Derived from Simple Organic Salts of Flufenamic Acid:
 Design, Synthesis, Structures, and Plausible Biomedical Application
;
_journal_issue                   5
_journal_name_full               'ACS Biomaterials Science &amp; Engineering'
_journal_page_first              2180
_journal_paper_doi               10.1021/acsbiomaterials.9b00153
_journal_volume                  5
_journal_year                    2019
_chemical_formula_moiety         'C17 H14 F3 N2 O3, C10 H13 N2'
_chemical_formula_sum            'C27 H27 F3 N4 O3'
_chemical_formula_weight         512.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.882(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   54.69(3)
_cell_length_b                   5.385(3)
_cell_length_c                   17.156(9)
_cell_measurement_reflns_used    927
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      16.81
_cell_measurement_theta_min      2.29
_cell_volume                     4925(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      120.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12140
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.557
_diffrn_reflns_theta_max         19.557
_diffrn_reflns_theta_min         1.528
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.6596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0692 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.8861.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.00058(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         2133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0509P)^2^+7.4467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1218
_reflns_number_total             2133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            S8.cif
_cod_data_source_block           S8
_cod_original_cell_volume        4925(4)
_cod_database_code               4514605
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F3)=Sof(F2)=Sof(F1)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C2(H2A,H2B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C26(H26), C21(H21), C6(H6), C12(H12), C16(H16), C9(H9),
 C8(H8), C7(H7), C23(H23), C14(H14), C25(H25), C24(H24), C15(H15)
3.c Idealised Me refined as rotating group:
 N3(H3C,H3D,H3E)
;
_shelx_res_checksum              46536
_shelx_hkl_checksum              82765
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'