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_4519400
_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_sum            'C23 H39 N O14'
_chemical_formula_weight         553.55
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 91.4070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.50870(10)
_cell_length_b                   7.87930(10)
_cell_length_c                   18.5965(2)
_cell_measurement_reflns_used    11062
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.1620
_cell_measurement_theta_min      4.6430
_cell_volume                     1392.87(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Cu K\a'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13386
_diffrn_reflns_point_group_measured_fraction_full 0.857
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.098
_diffrn_reflns_theta_min         4.652
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.44611
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1473 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(13)
_refine_ls_extinction_coef       0.0037(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4598
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0837P)^2^+0.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.708
_reflns_Friedel_fraction_max     0.680
_reflns_number_gt                4357
_reflns_number_total             4598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c07314_si_002.cif
_cod_data_source_block           6245
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4519400
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.912
_shelx_res_checksum              37855
_shelx_hkl_checksum              9544