Cyclodextrin complexes of the anticonvulsant agent valproic acid
Vicatos, A. I.; Caira, M. R.; CrystEngComm 23 (2021) 6582–6590; doi:10.1039/D1CE01024G

data_7243485
_publ_section_title
;
 Cyclodextrin complexes of the anticonvulsant agent valproic acid
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              6582
_journal_page_last               6590
_journal_paper_doi               10.1039/D1CE01024G
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety
;
(C56 H98 O35), (C57 H100 O35), 2(C8 H16 O2), 3.9(H2 O)'
;
_chemical_formula_sum            'C129 H237.8 O77.88'
_chemical_formula_weight         3035.06
_chemical_name_common            'DIMEB valproic acid clathrate hydrate'
_chemical_name_systematic
'heptakis(2,6-di-O-methyl)-beta-cyclodextrin 2-propylpentanoic acidhydrate (2:2:3.9)'
_chemical_temperature_decomposition 567.55
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-12 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                83.247(4)
_cell_angle_beta                 81.556(4)
_cell_angle_gamma                89.475(4)
_cell_formula_units_Z            1
_cell_length_a                   10.396(2)
_cell_length_b                   15.111(3)
_cell_length_c                   25.494(5)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.615
_cell_measurement_theta_min      2.2485
_cell_volume                     3933.9(13)
_computing_cell_refinement       'Program SAINT, v8.34A, Bruker AXS'
_computing_data_collection       'Bruker 2013, APEX2, v2013.10-0.'
_computing_data_reduction        'Program SAINT, v8.34A, Bruker AXS'
_computing_molecular_graphics
'POV-Ray in interface X-Seed (LJ Barbour, 1999)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Program SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II Duo diffractometer'
_diffrn_measurement_method       'phi- and omega-scans of 0.50 deg.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44688
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.041
_diffrn_reflns_theta_max         25.041
_diffrn_reflns_theta_min         1.357
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS-2012/1, Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1635
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 5967 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1664
_refine_ls_number_reflns         26358
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.1055
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2904
_refine_ls_wR_factor_ref         0.3294
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.900
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                16661
_reflns_number_total             26358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01024g2.cif
_cod_data_source_block           dimebval
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_temperature_decomposition' since the value had been
'decomp. 567.55 K'. The value 'decomp. 567.55 K' was changed to
'567.55'.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7243484--7243487.cif.
;
_cod_original_cell_volume        3934.0(14)
_cod_original_formula_sum        'C129 H237.80 O77.88'
_cod_database_code               7243485
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              19178
_shelx_hkl_checksum              45635