Crystallization of two forms of a cyclodextrin inclusion complex containing a common organic guest
Caira, Mino R.; de Vries, Elise J. C.; Nassimbeni, Luigi R.; Chemical Communications  (2003) 2058–; doi:10.1039/b305784b

data_7113579
_publ_section_title
;
 Crystallization of two forms of a cyclodextrin inclusion complex
 containing a common organic guest
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              2058
_journal_paper_doi               10.1039/b305784b
_journal_year                    2003
_chemical_formula_moiety         'C42 H70 O35.C8 H8 O3. 7.2 H2O'
_chemical_formula_sum            'C50 H92.4 O45.2'
_chemical_formula_weight         1416.80
_chemical_melting_point          'dehydration onset 20C, decomp. from 194C'
_chemical_name_common
;
bis(beta-cyclodextrin) bis(4-hydroxybenzoic acid methyl
ester) clathrate hydrate (monoclinic form)
;
_chemical_name_systematic
;
bis(beta-cyclodextrin) bis(4-hydroxybenzoic acid methyl ester) clathrate
hydrate (monoclinic form)
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.668(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8632(4)
_cell_length_b                   24.4542(5)
_cell_length_c                   15.5942(5)
_cell_measurement_reflns_used    21970
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.0
_cell_volume                     6730.4(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT 2000'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'WebLab Viewer Pro 3.7 (MSI Inc.)'
_computing_publication_material  'Parst (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       'phi- and omega-scans of 1.0 deg.'
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21970
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.218
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(14)
_refine_ls_extinction_coef       0.022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         14557
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.346
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.1002
_refine_ls_shift/su_max          0.513
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1959P)^2^+2.1929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2532
_refine_ls_wR_factor_ref         0.2854
_reflns_number_gt                10463
_reflns_number_total             14557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305784b.txt
_cod_data_source_block           MPBCD
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      C2
_cod_original_formula_sum        'C50 H92.40 O45.20'
_cod_database_code               7113579