Glucose selective bis-boronic acid click-fluor.
Zhai, Wenlei; Male, Louise; Fossey, John S.; Chemical communications (Cambridge, England) 53 (2017) 2218–2221; doi:10.1039/c6cc08534b

data_7119670
_publ_section_title
;
 Glucose selective bis-boronic acid click-fluor.
;
_journal_issue                   14
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2218
_journal_page_last               2221
_journal_paper_doi               10.1039/c6cc08534b
_journal_volume                  53
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H42 B2 N6 O4'
_chemical_formula_sum            'C36 H42 B2 N6 O4'
_chemical_formula_weight         644.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-10-20 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0090(3)
_cell_length_b                   6.56488(9)
_cell_length_c                   20.4434(3)
_cell_measurement_reflns_used    7353
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3790
_cell_measurement_theta_min      3.3770
_cell_volume                     3490.63(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3537
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -80.00   36.00   1.0000    9.6300
omega____ theta____ kappa____ phi______ frames
    -      -42.8107   19.0000  -90.0000 116

  2 omega  -44.00   23.00   1.0000    9.6300
omega____ theta____ kappa____ phi______ frames
    -      -42.8107   38.0000  150.0000 67

  3 omega   61.00   88.00   1.0000    9.6300
omega____ theta____ kappa____ phi______ frames
    -       42.8107 -125.0000 -180.0000 27

  4 omega   41.00   98.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257  -45.0000  120.0000 57

  5 omega   94.00  154.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257  125.0000    0.0000 60

  6 omega   36.00   68.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257  -30.0000  -90.0000 32

  7 omega   49.00  107.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257 -125.0000  150.0000 58

  8 omega   55.00   99.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257  -94.0000 -180.0000 44

  9 omega   61.00   91.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257  -30.0000  -30.0000 30

 10 omega   68.00  165.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257   15.0000 -150.0000 97

 11 omega  107.00  178.00   1.0000   38.5150
omega____ theta____ kappa____ phi______ frames
    -      106.6257  125.0000  150.0000 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0233398000
_diffrn_orient_matrix_UB_12      0.0581107000
_diffrn_orient_matrix_UB_13      -0.0666924000
_diffrn_orient_matrix_UB_21      -0.0192182000
_diffrn_orient_matrix_UB_22      0.2027798000
_diffrn_orient_matrix_UB_23      0.0290659000
_diffrn_orient_matrix_UB_31      0.0509153000
_diffrn_orient_matrix_UB_32      0.1027918000
_diffrn_orient_matrix_UB_33      -0.0197457000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13862
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.775
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.588
_diffrn_reflns_theta_min         3.399
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.2202
_exptl_crystal_size_mid          0.1067
_exptl_crystal_size_min          0.0635
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1801 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5551
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0542P)^2^+1.2194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.540
_reflns_Friedel_fraction_full    0.608
_reflns_Friedel_fraction_max     0.560
_reflns_number_gt                5344
_reflns_number_total             5551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08534b2.cif
_cod_data_source_block           7b
_cod_original_cell_volume        3490.62(8)
_cod_database_code               7119670
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C36 H42 B2 N6 O4'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C17(H17), C19(H19), C20(H20),
 C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              95820
_shelx_hkl_checksum              17771
_olex2_submission_special_instructions 'No special instructions were received'