1,2-<i>O</i>-Isopropylidene-β-<small>D</small>-<i>lyxo</i>-furanose
Doboszewski, Bogdan; Nazarenko, Alexander Y.; IUCrData 5 (2020) x201630–; doi:10.1107/S2414314620016302

data_1559848
_publ_section_title
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 1,2-<i>O</i>-Isopropylidene-\b-<small>D</small>-<i>lyxo</i>-furanose
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_journal_issue                   12
_journal_name_full               IUCrData
_journal_page_first              x201630
_journal_paper_doi               10.1107/S2414314620016302
_journal_volume                  5
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H14 O5'
_chemical_formula_sum            'C8 H14 O5'
_chemical_formula_weight         190.19
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-05
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9216(3)
_cell_length_b                   7.3539(4)
_cell_length_c                   21.1087(12)
_cell_measurement_reflns_used    4274
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      75.44
_cell_measurement_theta_min      4.19
_cell_volume                     919.22(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       APEX2
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.8
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker PHOTON-100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5619
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.605
_diffrn_reflns_theta_min         4.189
_diffrn_source                   sealedtube
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.7793
_exptl_absorpt_correction_T_min  0.6933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0578 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8896.
The \l/2 correction factor is 0.00150.
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.462
_exptl_crystal_size_min          0.398
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 559 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.09(13)
_refine_ls_extinction_coef       0.0124(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0450P)^2^+0.2390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                1553
_reflns_number_total             1811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq4044sup4.txt
_cod_data_source_block           cu_an528_0m
_cod_database_code               1559848
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.641
_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 Ternary CH refined with riding coordinates:
 C10(H10), C5(H5), C6(H6), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              47440
_shelx_hkl_checksum              17458
_olex2_submission_special_instructions 'No special instructions were received'