Hydrogen bonding-induced conformational change in a crystalline sugar derivative
Pal, Kumar Bhaskar; Sarkar, Vikramjit; Mukhopadhyay, Balaram; CrystEngComm 18 (2016) 1156–; doi:10.1039/C5CE01893E

data_7223799
_publ_section_title
;
 Hydrogen bonding-induced conformational change in a crystalline sugar
 derivative
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1156
_journal_paper_doi               10.1039/C5CE01893E
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H26 O6 S'
_chemical_formula_sum            'C23 H26 O6 S'
_chemical_formula_weight         430.50
_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_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-07 deposited with the CCDC.
2016-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8253(7)
_cell_length_b                   8.3302(5)
_cell_length_c                   42.609(2)
_cell_measurement_reflns_used    1715
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.5120
_cell_measurement_theta_min      2.4860
_cell_volume                     2067.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   59.00  120.50   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3512  178.0000   90.0000 82

  2 omega   39.00   84.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3512   57.0000 -180.0000 60

  3 omega  -45.00   15.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3512  -77.0000  120.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0018008000
_diffrn_orient_matrix_UB_12      -0.0000043000
_diffrn_orient_matrix_UB_13      0.0166499000
_diffrn_orient_matrix_UB_21      0.1024046000
_diffrn_orient_matrix_UB_22      -0.0459963000
_diffrn_orient_matrix_UB_23      -0.0002319000
_diffrn_orient_matrix_UB_31      0.0657836000
_diffrn_orient_matrix_UB_32      0.0716428000
_diffrn_orient_matrix_UB_33      -0.0001231000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            5054
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.91
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
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    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+3.0903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                3210
_reflns_number_total             3465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01893e2.cif
_cod_data_source_block           galiso1obzstol
_cod_depositor_comments
'Adding full bibliography for 7223799--7223801.cif.'
_cod_database_code               7223799
_chemical_oxdiff_formula         'C H O S'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C7) = Uanis(C6)
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23)
Uanis(C12) = Uanis(C17)
3.a Ternary CH refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_date_sample_data_collection 2015-01-15
_olex2_submission_special_instructions 'No special instructions were received'