Tuning a modular system - synthesis and characterisation of a boron-rich s-triazine-based carboxylic acid and amine bearing a galactopyranosyl moiety.
Kellert, Martin; Hoppenz, Paul; Lönnecke, Peter; Worm, Dennis J.; Riedl, Bernd; Koebberling, Johannes; Beck-Sickinger, Annette G; Hey-Hawkins, Evamarie; Dalton transactions (Cambridge, England : 2003) 49 (2020) 57–69; doi:10.1039/c9dt04031e

data_7702272
_publ_section_title
;
 Tuning a modular system - synthesis and characterisation of a boron-rich
 s-triazine-based carboxylic acid and amine bearing a galactopyranosyl
 moiety.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              57
_journal_page_last               69
_journal_paper_doi               10.1039/c9dt04031e
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C23 H41 B10 Cl N4 O7 S'
_chemical_formula_sum            'C23 H41 B10 Cl N4 O7 S'
_chemical_formula_weight         661.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-08 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.622(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9441(2)
_cell_length_b                   11.0847(2)
_cell_length_c                   13.6080(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      31.9890
_cell_measurement_theta_min      2.3860
_cell_volume                     1750.98(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
 or
 DIAMOND Version 3.2k
 K. Brandenburg, Crystal Impact GbR, Bonn, Germany
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT-2014-5
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.3560
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        30.510
_diffrn_reflns_theta_max         32.596
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 4033 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.056(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         11515
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0370P)^2^+0.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                10040
_reflns_number_total             11515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04031e2.cif
_cod_data_source_block           SP1_x2952fin
_cod_depositor_comments
'Adding full bibliography for 7702266--7702273.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7702272
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              1585