A novel hydrate of α-cyclodextrin crystallised under high-pressure conditions
Granero-García, Rubén; Lahoz, Fernando J.; Paulmann, Carsten; Saouane, Sofiane; Fabbiani, Francesca P. A.; CrystEngComm 14 (2012) 8664–; doi:10.1039/c2ce26362a

data_7214714
_publ_section_title
;
 A novel hydrate of \a-cyclodextrin crystallised under high-pressure
 conditions
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              8664
_journal_paper_doi               10.1039/c2ce26362a
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C36 H60 O30, 6.8(H2 O)'
_chemical_formula_sum            'C36 H73.6 O36.8'
_chemical_formula_weight         1095.35
_chemical_name_common            '\a-cyclodextrin 6.8-hydrate'
_chemical_name_systematic
;
cyclohexaamylose 6.8-hydrate, cyclomaltohexaose 6.8-hydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     notdet
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.657(5)
_cell_length_b                   34.253(14)
_cell_length_c                   9.217(4)
_cell_measurement_reflns_used    2515
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.07
_cell_measurement_theta_min      1.70
_cell_volume                     4627(3)
_computing_cell_refinement       'APEX2 v2012.4-0'
_computing_data_collection       'APEX2 v2012.4-0'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
ORTEP3 for Windows (Burnett & Johnson, 1996)
and Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            'MarCCD detector'
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Huber 4-circle diffractometer'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'HASYLAB/DESY F1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.50000
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_sigmaI/netI    0.0936
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11053
_diffrn_reflns_theta_full        11.38
_diffrn_reflns_theta_max         11.38
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.4618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SHADE (Parsons, 2004)
SADABS (Sheldrick, 2008<i>a</i>)
;
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   6(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         1301
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+31.1673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1799
_reflns_number_gt                1048
_reflns_number_total             1301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26362a.txt
_cod_data_source_block           alpha_CDX_form_Ib_HP
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4628(3)
_cod_database_code               7214714