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_7113578
_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)2.(C8 H8 O3)2. 28H2O'
_chemical_formula_sum            'C100 H212 O104'
_chemical_formula_weight         3078.80
_chemical_melting_point          'dehydrates at 39C, decomposes from 251C'
_chemical_name_common
;
bis(Beta-cyclodextrin) bis(4-hydroxybenzoic acid methyl
ester) clathrate hydrate (triclinic form)
;
_chemical_name_systematic
;
bis(Beta-cyclodextrin) bis(4-hydroxybenzoic acid methyl ester) clathrate
hydrate (triclinic form)
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.464(1)
_cell_angle_beta                 113.122(1)
_cell_angle_gamma                99.254(1)
_cell_formula_units_Z            1
_cell_length_a                   18.0187(3)
_cell_length_b                   15.3431(4)
_cell_length_c                   15.4140(3)
_cell_measurement_reflns_used    18382
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      0.99
_cell_volume                     3656.65(14)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18382
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.128
_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             1644
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.7(16)
_refine_ls_extinction_coef       0.021(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     1210
_refine_ls_number_reflns         18382
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0937
_refine_ls_shift/su_max          0.265
_refine_ls_shift/su_mean         0.072
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1591P)^2^+10.4686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2582
_refine_ls_wR_factor_ref         0.2673
_reflns_number_gt                16651
_reflns_number_total             18382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305784b.txt
_cod_data_source_block           MPBCDP1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        3656.7(1)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7113578