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_7244612
_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 ad
_chemical_formula_moiety         'C6 H11 Br O5'
_chemical_formula_sum            'C6 H11 Br O5'
_chemical_formula_weight         243.055
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_audit_creation_date             2021-04-16
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8069(3)
_cell_length_b                   6.8839(3)
_cell_length_c                   17.1166(10)
_cell_measurement_reflns_used    1408
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.4260
_cell_measurement_theta_min      5.1510
_cell_volume                     802.05(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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    -73.00  35.00   1.00    1.00    --  -41.53  77.00 -60.00  108
  2  \w     77.00 104.00   1.00    1.00    --   41.53  57.00 -60.00   27
  3  \w     22.00  63.00   1.00    1.00    --   41.53  57.00 -60.00   41
  4  \w    113.00 140.00   1.00    4.00    --  103.66 178.00   0.00   27
  5  \w     53.00 106.00   1.00    4.00    --  103.66 -94.00-180.00   53
  6  \w     64.00  89.00   1.00    4.00    --  103.66 178.00  60.00   25
  7  \w    114.00 167.00   1.00    4.00    --  103.66  77.00  90.00   53
  8  \w    117.00 143.00   1.00    4.00    --  103.66 178.00  60.00   26
  9  \w    103.00 168.00   1.00    4.00    --  103.66  77.00-120.00   65
 10  \w     84.00 129.00   1.00    4.00    --  103.66 -45.00 120.00   45
 11  \w     33.00 116.00   1.00    4.00    --  103.66 -30.00  90.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2663
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9993
_diffrn_reflns_theta_full        67.0794
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         5.17
_exptl_absorpt_coefficient_mu    6.915
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    2.013
_exptl_crystal_description       prism
_exptl_crystal_F_000             486.856
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.5337
_refine_diff_density_min         -0.5112
_refine_diff_density_rms         0.1272
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.06(4)
_refine_ls_d_res_high            0.8370
_refine_ls_d_res_low             8.5583
_refine_ls_goodness_of_fit_ref   0.9480
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1437
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.9469
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.998
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              8
_reflns_limit_k_min              -8
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                1310
_reflns_number_total             1437
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ra08312k2.cif
_cod_data_source_block           2020_12_04_DT-2BG-3_N
_cod_original_cell_volume        802.06(7)
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7244612
_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,H) groups
2. Restrained distances
 O2-H2A
 0.97 with sigma of 0.01
 H3A-O3
 0.97 with sigma of 0.01
 C5-H5
 1.09 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C2(H2)
;
_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
;