Insights Into the Properties of Amygdalin Solvatomorphs: X-ray Structures, Intermolecular Interactions, and Transformations.
Zhang, Tingting; Yang, Shiying; Zhang, Baoxi; Yang, Dezhi; Lu, Yang; Du, Guanhua; ACS omega 7 (2022) 8906–8918; doi:10.1021/acsomega.1c07314

data_4519401
_publ_section_title
;
 Insights Into the Properties of Amygdalin Solvatomorphs: X-ray
 Structures, Intermolecular Interactions, and Transformations.
;
_journal_issue                   10
_journal_name_full               'ACS omega'
_journal_page_first              8906
_journal_page_last               8918
_journal_paper_doi               10.1021/acsomega.1c07314
_journal_volume                  7
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H27 N O11, C5 H12 O, 2(H2 O)'
_chemical_formula_sum            'C25 H43 N O14'
_chemical_formula_weight         581.60
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-10-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5366(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.41201(5)
_cell_length_b                   7.94140(5)
_cell_length_c                   19.98256(11)
_cell_measurement_reflns_used    24719
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.1450
_cell_measurement_theta_min      4.4540
_cell_volume                     1480.684(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MicroMax 002+'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29319
_diffrn_reflns_theta_full        72.24
_diffrn_reflns_theta_max         72.24
_diffrn_reflns_theta_min         4.46
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.906
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(10)
_refine_ls_extinction_coef       0.0050(5)
_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   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0634P)^2^+0.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                5022
_reflns_number_total             5063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao1c07314_si_003.cif
_cod_data_source_block           6347-20210913
_cod_database_code               4519401
_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, All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Ternary CH refined with riding coordinates:
 C1(H1), C9(H9A), C10(H10), C11(H11A), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19)
2.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C20(H20A,H20B), C1P(H1PA,H1PB), C2P(H2PA,H2PB), C3P(H3PA,
 H3PB), C4P(H4PA,H4PB)
2.d Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C6(H6), C7(H7A), C8(H8A)
2.e Idealised Me refined as rotating group:
 C5P(H5PA,H5PB,H5PC)
2.f Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3), O4(H4), O7(H7), O8(H8), O9(H9), O11(H11), O1P(H1P)
;
_olex2_submission_special_instructions 'No special instructions were received'