Crystal structure of 14-O-acetyldelcosine, C26H41NO8
Liu, Huan-Ni; Hao, Yi-Kun; Chen, Neng-Hua; Li, Lai-Ming; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 75–77; doi:10.1515/ncrs-2022-0501

data_8107357
_publ_section_title
;
 Crystal structure of 14-O-acetyldelcosine, C26H41NO8
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              75
_journal_page_last               77
_journal_paper_doi               10.1515/ncrs-2022-0501
_journal_volume                  238
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H41 N O8'
_chemical_formula_sum            'C26 H41 N O8'
_chemical_formula_weight         495.60
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.24370(10)
_cell_length_b                   13.1867(2)
_cell_length_c                   22.8490(4)
_cell_measurement_reflns_used    8866
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      73.6280
_cell_measurement_theta_min      3.8370
_cell_volume                     2483.85(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.971
_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    --  -40.73  77.00 -30.00  108
  2  \w     23.00  97.00   1.00    1.00    --   40.73-125.00-120.00   74
  3  \w     23.00  97.00   1.00    1.00    --   40.73-125.00   0.00   74
  4  \w     16.00 115.00   1.00    1.00    --   40.73  38.00   0.00   99
  5  \w     35.00 133.00   1.00    1.00    --  107.58 -45.00   0.00   98
  6  \w     97.00 178.00   1.00    1.00    --  107.58 119.00  -0.00   81
  7  \w     78.00 178.00   1.00    1.00    --  107.58  61.00 150.00  100
  8  \w     94.00 178.00   1.00    1.00    --  107.58 125.00  60.00   84
  9  \w     94.00 176.00   1.00    1.00    --  107.58 125.00-180.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0974734000
_diffrn_orient_matrix_UB_12      -0.0842482000
_diffrn_orient_matrix_UB_13      -0.0307313000
_diffrn_orient_matrix_UB_21      0.0754640000
_diffrn_orient_matrix_UB_22      0.0794760000
_diffrn_orient_matrix_UB_23      -0.0412560000
_diffrn_orient_matrix_UB_31      0.1405008000
_diffrn_orient_matrix_UB_32      0.0157633000
_diffrn_orient_matrix_UB_33      0.0435107000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11294
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.658
_diffrn_reflns_theta_min         3.869
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light colourless'
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 1815 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0592P)^2^+0.2346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.892
_reflns_number_gt                4616
_reflns_number_total             4713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0501_suppl.cif
_cod_data_source_block           fy-2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'AD' was changed
to 'ad' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_database_code               8107357
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C17(H17), C9(H9), C10(H10), C6(H6), C5(H5), C13(H13), C14(H14), C16(H16),
 C1(H1a)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b), C20(H20a,H20b), C12(H12a,H12b), C19(H19a,H19b), C18(H18a,
 H18b), C3(H3a,H3b), C2(H2a,H2b)
2.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C24(H24a,H24b,
 H24c), C26(H26a,H26b,H26c)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O1(H1)
;
_shelx_res_checksum              56868
_shelx_hkl_checksum              8044
_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 2.078
_oxdiff_exptl_absorpt_empirical_full_min 0.440