X-ray wavefunction refinement and comprehensive structural studies on bromo-substituted analogues of 2-deoxy-d-glucose in solid state and solution
Ziemniak, Marcin; Pawlędzio, Sylwia; Zawadzka-Kaźmierczuk, Anna; Dominiak, Paulina M.; Trzybiński, Damian; Koźmiński, Wiktor; Zieliński, Rafał; Fokt, Izabela; Priebe, Waldemar; Woźniak, Krzysztof; Pająk, Beata; RSC Advances 12 (2022) 8345–8360; doi:10.1039/D1RA08312K

data_7244614
_publ_section_title
;
 X-ray wavefunction refinement and comprehensive structural studies on
 bromo-substituted analogues of 2-deoxy-d-glucose in solid state and
 solution
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              8345
_journal_page_last               8360
_journal_paper_doi               10.1039/D1RA08312K
_journal_volume                  12
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C12 H22 O11'
_chemical_formula_sum            'C12 H22 O11'
_chemical_formula_weight         342.302
_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'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.983(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7727(9)
_cell_length_b                   8.7216(11)
_cell_length_c                   10.8637(11)
_cell_measurement_reflns_used    4334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8820
_cell_measurement_theta_min      2.0180
_cell_volume                     717.63(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9588
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -74.00 109.00   1.00    3.27    --   20.00  54.00   6.06  183
  2  \w     65.00 110.00   1.00    3.27    --   20.00  54.00-180.00   45
  3  \w    -74.00 109.00   1.00    3.27    --   20.00  54.00 -60.00  183
  4  \w    -74.00 109.00   1.00    3.27    --   20.00  54.00-150.00  183
  5  \w    -74.00 109.00   1.00    3.27    --   20.00  54.00-150.00  183
  6  \w    -74.00 109.00   1.00    3.27    --   20.00  54.00-180.00  183
  7  \w    -74.00 109.00   1.00    3.27    --   20.00  54.00-180.00  183
  8  \w    -74.00  69.00   1.00    3.27    --   20.00  54.00-120.00  143
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0067778000
_diffrn_orient_matrix_UB_12      0.0437926000
_diffrn_orient_matrix_UB_13      -0.0557807000
_diffrn_orient_matrix_UB_21      -0.0263053000
_diffrn_orient_matrix_UB_22      -0.0666037000
_diffrn_orient_matrix_UB_23      -0.0370776000
_diffrn_orient_matrix_UB_31      -0.0895987000
_diffrn_orient_matrix_UB_32      0.0162712000
_diffrn_orient_matrix_UB_33      -0.0005508000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.9971
_diffrn_reflns_Laue_measured_fraction_max 0.9588
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13618
_diffrn_reflns_point_group_measured_fraction_full 0.9228
_diffrn_reflns_point_group_measured_fraction_max 0.8545
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.12b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       prism
_exptl_crystal_F_000             364.302
_refine_diff_density_max         0.1220
_refine_diff_density_min         -0.1424
_refine_diff_density_rms         0.0311
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.1(8)
_refine_ls_d_res_high            0.7283
_refine_ls_d_res_low             7.5740
_refine_ls_goodness_of_fit_ref   1.0926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     400
_refine_ls_number_reflns         3318
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0926
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0410
_reflns_Friedel_coverage         0.736
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              9
_reflns_limit_k_min              -11
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                3002
_reflns_number_total             3318
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ra08312k2.cif
_cod_data_source_block           sucrose
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7244614
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.075
_oxdiff_exptl_absorpt_empirical_full_min 0.948