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_4514607
_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         '4(C14 H9 F3 N O2), 4(C10 H16 N O2), O'
_chemical_formula_sum            'C96 H100 F12 N8 O17'
_chemical_formula_weight         1865.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.770(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.469(4)
_cell_length_b                   6.0807(8)
_cell_length_c                   28.774(3)
_cell_measurement_reflns_used    3680
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      18.445
_cell_measurement_theta_min      2.268
_cell_volume                     4630.8(10)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0931
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28253
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        19.489
_diffrn_reflns_theta_max         19.489
_diffrn_reflns_theta_min         1.052
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.6054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1344 before and 0.0706 after correction. The Ratio of minimum to maximum transmission is 0.8134. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         3783
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+18.9912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2691
_reflns_number_total             3783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            S5.cif
_cod_data_source_block           S5
_cod_original_cell_volume        4630.9(10)
_cod_database_code               4514607
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.960
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C10, C14, C36, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(F5A)=Sof(F6A)=Sof(F1A)=Sof(F4A)=Sof(F3A)=Sof(F2A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F1)=Sof(F6)=Sof(F5)=Sof(F4)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C39(H39A,H39B), C16(H16A,H16B), C15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3A), C37(H37), C46(H46), C42(H42), C43(H43), C22(H22), C9(H9),
 C27(H27), C6(H6), C33(H33), C30(H30), C3(H3), C13(H13), C12(H12), C11(H11),
 C19(H19), C18(H18), C34(H34), C5(H5), C35(H35), C29(H29), C28(H28), C4(H4)
4.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N4(H4A,H4B,H4C), C48(H48A,H48B,H48C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              7210
_shelx_hkl_checksum              37488
_olex2_submission_special_instructions 'No special instructions were received'