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_7214713
_publ_section_title
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 A novel hydrate of \a-cyclodextrin crystallised under high-pressure
 conditions
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_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(H2 O)'
_chemical_formula_sum            'C36 H72 O36'
_chemical_formula_weight         1080.94
_chemical_name_common            '\a-cyclodextrin hexahydrate'
_chemical_name_systematic
;
cyclohexaamylose hexahydrate, cyclomaltohexaose hexahydrate
;
_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                   14.8815(4)
_cell_length_b                   33.7011(10)
_cell_length_c                   9.4872(2)
_cell_measurement_reflns_used    6135
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.07
_cell_measurement_theta_min      2.27
_cell_volume                     4758.0(2)
_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    'known coordinates'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w and \j scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0988
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            67820
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         7533
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                5711
_reflns_number_total             7540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26362a.txt
_cod_data_source_block           alpha_CDX_form_I_150K
_cod_depositor_comments
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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 
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_cod_database_code               7214713