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

data_7243486
_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
;
(C54 H96 O30), (C8 H16 O2), 1.2 (H2 O)
;
_chemical_formula_sum            'C62 H114.4 O33.2'
_chemical_formula_weight         1391.13
_chemical_melting_point          'decomp. onset 368 K'
_chemical_name_common
;             
permethylated alpha-cyclodextrin valproic acid hydrate
;
_chemical_name_systematic
'hexakis-(2,3,6-tri-O-methyl)-cyclomaltohexaose 2-propylpentanoic acid clathrate hydrate'
_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     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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.337(3)
_cell_length_b                   20.728(4)
_cell_length_c                   23.104(5)
_cell_measurement_reflns_used    4866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.29
_cell_measurement_theta_min      2.37
_cell_volume                     7345(3)
_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    'SHELXS (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.1078
_diffrn_reflns_av_unetI/netI     0.1073
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.243
_diffrn_reflns_theta_min         1.320
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS-2012/1, Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3008
_exptl_crystal_recrystallization_method
'Co-precipitation and slow evaporation'
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 3088 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         16290
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0802P)^2^+0.8167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                9581
_reflns_number_total             16290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01024g2.cif
_cod_data_source_block           TMAVAL2
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__diffrn_source' was replaced with '_diffrn_source'.

Automatic conversion script
Id: cif_correct_tags 7550 2019-12-06 10:49:48Z antanas 

The following automatic conversions were performed:

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_formula_sum        'C62 H114.40 O33.20'
_cod_database_code               7243486
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              31153
_shelx_hkl_checksum              35542