β-Cyclodextrin dimethylformamide 12.5 hydrate: a deeper insight into β-cyclodextrin crystal packing
Granero-García, Rubén; Fabbiani, Francesca P. A.; Acta Crystallographica Section B 70 (2014) 586–594; doi:10.1107/S2052520614002285

data_2105864
_publ_section_title
;
 \b-Cyclodextrin dimethylformamide 12.5 hydrate: a deeper insight into
 \b-cyclodextrin crystal packing
;
_journal_coeditor_code           PS5033
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              586
_journal_page_last               594
_journal_paper_doi               10.1107/S2052520614002285
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C42 H70 O35, C3 H7 N1 O1, 12.5(H2 O)'
_chemical_formula_sum            'C45 H102 N O48.5'
_chemical_formula_weight         1433.27
_chemical_name_common            '\b-cyclodextrin DMF 12.5 hydrate'
_chemical_name_systematic
'cycloheptaamylose dimethylformamide 12.5-hydrate'
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.138(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.500(3)
_cell_length_b                   9.794(2)
_cell_length_c                   21.689(5)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.28
_cell_volume                     3292.5(12)
_computing_cell_refinement       'APEX2 v2012.4-0'
_computing_data_collection       'APEX2 v2012.4-0'
_computing_data_reduction        'SAINT (Bruker-AXS, 2011)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012)
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
Platon(Speck, 2009)
XPac(Gelbrich & Hursthouse, 2005)
CLP(Gavezzotti, 2011)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008b)'
_computing_structure_solution    'PATSEE (Egert & Sheldrick, 1985)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38760
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.408
_diffrn_reflns_theta_min         1.613
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6877
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1534
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.342
_refine_ls_abs_structure_details
;
 Flack x determined using 4424 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.5(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         13449
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0343P)^2^+4.2154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                11103
_reflns_number_total             13449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ps5033sup1.cif
_cod_data_source_block           I
_cod_database_code               2105864
_shelx_hkl_checksum              83611
_shelx_res_checksum              23825
_shelxl_version_number           2.013