Supramolecular Hydrogel Derived from A C3-symmetric Boronic acid Derivative for Stimuli Responsive Release of Insulin and Doxorubicin.
Sarkar, Koushik; Dastidar, Parthasarathi; Langmuir : the ACS journal of surfaces and colloids  (2017) –; doi:10.1021/acs.langmuir.7b03326

data_4514323
_publ_section_title
;
 Supramolecular Hydrogel Derived from A C3-symmetric Boronic acid
 Derivative for Stimuli Responsive Release of Insulin and Doxorubicin.
;
_journal_name_full
'Langmuir : the ACS journal of surfaces and colloids'
_journal_paper_doi               10.1021/acs.langmuir.7b03326
_journal_year                    2017
_chemical_formula_moiety         'C21 H18 N6, 2(C2 O)'
_chemical_formula_sum            'C25 H18 N6 O2'
_chemical_formula_weight         434.45
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.332(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.795(7)
_cell_length_b                   5.3123(19)
_cell_length_c                   22.606(8)
_cell_measurement_reflns_used    907
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.976
_cell_measurement_theta_min      2.410
_cell_volume                     2281.3(14)
_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      120.01
_diffrn_measured_fraction_theta_full 0.447
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1121
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_Laue_measured_fraction_full 0.447
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10335
_diffrn_reflns_point_group_measured_fraction_full 0.447
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         19.097
_diffrn_reflns_theta_min         1.072
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.6045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0775 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.8122.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.047(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         1847
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1266P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                886
_reflns_number_total             1847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            la7b03326_si_003.cif
_cod_data_source_block           NG1
_cod_database_code               4514323
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Others
 1*[Sof(C26)+Sof(C27)+Sof(O4)+Sof(C28)+Sof(C29)+Sof(O3)]+1*[Sof(O5)+Sof(C31)+
 Sof(C30)+Sof(C32)+Sof(C33)+Sof(O6)]+1*[Sof(O2)+Sof(C23)+Sof(C22)+Sof(O1)+
 Sof(C25)+Sof(C24)]=1 with esd of 0.0001
 Sof(C26)=Sof(C27)=Sof(O4)=Sof(C28)=Sof(C29)=Sof(O3)=FVAR(1)
 Sof(O5)=Sof(C31)=Sof(C30)=Sof(C32)=Sof(C33)=Sof(O6)=FVAR(2)
 Sof(O2)=Sof(C23)=Sof(C22)=Sof(O1)=Sof(C25)=Sof(C24)=FVAR(3)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C2(H2), C5(H5), C12(H12), C20(H20), C17(H17), C21(H21),
 C15(H15), C18(H18), C6(H6), C14(H14)
3.b X=CH2 refined with riding coordinates:
 N6(H6A,H6B), N4(H4A,H4B), N5(H5A,H5B)
;
_shelx_res_checksum              54539
_shelx_hkl_checksum              73827
_olex2_submission_special_instructions 'No special instructions were received'