Crystal Engineering of Nutraceutical Phytosterols: New Cocrystal Solid-Solutions
Prohens, Rafel; Barbas, Rafael; Bofill, Lidia; de Sande, Dafne; Font-Bardia, Merce; CrystEngComm  (2020) –; doi:10.1039/D0CE00704H

data_7240609
_publ_section_title
;
 Crystal Engineering of Nutraceutical Phytosterols: New Cocrystal
 Solid-Solutions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00704H
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C29 H50 O, 0.25(C3 H6 O2), 0.25(H2 O)'
_chemical_formula_sum            'C29.75 H52 O1.75'
_chemical_formula_weight         437.71
_chemical_name_systematic
'Sitosterol Propionic acid hydrate cocrystal form II'
_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
_audit_update_record
;
2020-05-01 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.569(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.373(3)
_cell_length_b                   7.4971(7)
_cell_length_c                   27.183(3)
_cell_measurement_reflns_used    3805
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      2.71
_cell_volume                     5369.2(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.5074
_diffrn_reflns_av_unetI/netI     0.4780
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            84425
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         2.202
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       needle
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 1748 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1166
_refine_ls_number_reflns         21902
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.3448
_refine_ls_R_factor_gt           0.1012
_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^)+(0.0730P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.2356
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                6859
_reflns_number_total             21902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00704h2.cif
_cod_data_source_block           mo_023WB72_0m_a
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_moiety     '4(C29 H50 O), C3 H6 O2, H2 O'
_cod_original_formula_sum        'C119 H208 O7'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1750.84
_cod_database_code               7240609
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              94361