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

data_7243487
_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
;
3(C48 H80 O40), 4(C8 H16 O2), 49(H2 O)
;
_chemical_formula_sum            'C176 H402 O177'
_chemical_formula_weight         5350.95
_chemical_name_common
;
tris(gamma-cyclodextrin) tetrakis(valproic acid) clathrate hydrate
;
_chemical_name_systematic
;
tris(cyclooctylamylose) tetrakis(2-propylpentanoic acid) clathrate hydrate
;
_chemical_temperature_decomposition 538.5
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_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            2
_cell_length_a                   23.745(4)
_cell_length_b                   23.745(4)
_cell_length_c                   23.100(5)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.645
_cell_measurement_theta_min      2.426
_cell_volume                     13024(4)
_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      293(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II Duo diffractometer'
_diffrn_measurement_method       'phi- and omega-scans of 0.80 deg.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            149732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.558
_diffrn_reflns_theta_min         1.230
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS-2012/1, Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             5748
_exptl_crystal_recrystallization_method
'Co-precipitation and slow evaporation'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 3375 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.730
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         12162
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.730
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.1431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_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          0.4024
_refine_ls_wR_factor_ref         0.4101
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                10116
_reflns_number_total             12162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01024g2.cif
_cod_data_source_block           NUGAM2
_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.538.5 K'. The value 'decomp.538.5 K' was changed to '538.5'.

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        13025(5)
_cod_database_code               7243487
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              36786
_shelx_hkl_checksum              54057