Amino-diol borate complexation for controlling transport phenomena of penetrant molecules into polymeric matrices
Unthank, Matthew G.; Cameron, Colin; Wright, Anthony; Hughes, David; Alam, M. Ashraf; Probert, Michael R.; Polymer Chemistry 10 (2019) 4920–; doi:10.1039/C9PY00780F

data_1552237
_publ_section_title
;
 Amino-diol borate complexation for controlling transport phenomena of
 penetrant molecules into polymeric matrices
;
_journal_issue                   36
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4920
_journal_paper_doi               10.1039/C9PY00780F
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C26 H36 B N O5'
_chemical_formula_sum            'C26 H36 B N O5'
_chemical_formula_weight         453.37
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-19
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-28 deposited with the CCDC.    2019-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8609(4)
_cell_length_b                   20.1753(6)
_cell_length_c                   8.7717(3)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      68.26
_cell_measurement_theta_min      3.20
_cell_volume                     2443.86(13)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focussed source'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            44216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.257
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'Bruker TXS with Helios Optics'
_diffrn_source_type
;
'Incoatec microfocus 3.0 (Cu) X-ray Source'
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1192 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.8307.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0766P)^2^+0.9201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4345
_reflns_number_total             4478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9py00780f2.cif
_cod_data_source_block           19mrp002_sph_abs
_cod_depositor_comments          'Adding full bibliography for 1552237.cif.'
_cod_database_code               1552237
_shelx_shelxl_version_number     2016/6
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C12 \\sim O4-C12B
 with sigma of 0.02
 C12-C11 \\sim C12B-C11B
 with sigma of 0.02
 C11-C10 \\sim C11B-C10
 with sigma of 0.02
 O3B-C11B \\sim O3-C11
 with sigma of 0.02
 O3B-B1 \\sim O3-B1
 with sigma of 0.02
3. Others
 Sof(H10c)=Sof(H10d)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12c)=Sof(H12d)=Sof(O3)=1-
 FVAR(1)
 Sof(O3B)=Sof(H10a)=Sof(H10b)=Sof(C12B)=Sof(H12a)=Sof(H12b)=Sof(C11B)=
 Sof(H11B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C2(H2), C11B(H11B), C11(H11)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C3(H3a,H3b), C20(H20a,H20b), C10(H10a,H10b), C10(H10c,H10d),
 C24(H24a,H24b), C23(H23a,H23b), C22(H22a,H22b), C25(H25a,H25b), C21(H21a,H21b),
  C12B(H12a,H12b), C12(H12c,H12d)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C18(H18), C9(H9), C6(H6), C14(H14), C17(H17), C8(H8), C7(H7),
 C16(H16), C15(H15)
4.d Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c)
;
_olex2_exptl_crystal_mounting_method
'Crystal mounted on a kapton loop under oil'
_olex2_submission_special_instructions 'No special instructions were received'