Studies on polymorph conversion in a new cyclodextrin inclusion compound
Fernandes, José A.; Ramos, Ana I.; Ribeiro-Claro, Paulo; Almeida Paz, Filipe A.; Braga, Susana S.; CrystEngComm 17 (2015) 937–; doi:10.1039/C4CE02041C

data_7218911
_publ_section_title
;
 Studies on polymorph conversion in a new cyclodextrin inclusion compound
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              937
_journal_paper_doi               10.1039/C4CE02041C
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C42 H70 O35, C11 H9 N O, 11(H2O)'
_chemical_formula_sum            'C106 H202 N2 O94'
_chemical_formula_weight         3008.68
_chemical_name_systematic
'4-Phenyl-Pyridine-N-oxide b-cyclodextrin hendecahydrate'
_chemical_properties_physical    'degrades when dry'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2014-10-03 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                99.573(9)
_cell_angle_beta                 113.073(9)
_cell_angle_gamma                102.518(10)
_cell_formula_units_Z            1
_cell_length_a                   15.281(3)
_cell_length_b                   15.431(3)
_cell_length_c                   17.911(4)
_cell_measurement_reflns_used    7471
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.89
_cell_measurement_theta_min      3.17
_cell_volume                     3641.8(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31719
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.709
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.528
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1604
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.292
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Flack x determined using 3477 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.9(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.405
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1559
_refine_ls_number_reflns         18955
_refine_ls_number_restraints     627
_refine_ls_restrained_S_all      1.394
_refine_ls_R_factor_all          0.1808
_refine_ls_R_factor_gt           0.1384
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3494
_refine_ls_wR_factor_ref         0.3831
_reflns_Friedel_coverage         0.461
_reflns_Friedel_fraction_full    0.453
_reflns_Friedel_fraction_max     0.448
_reflns_number_gt                12782
_reflns_number_total             18955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02041c2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7218911--7218912.cif.'
_cod_original_cell_volume        3641.9(13)
_cod_database_code               7218911
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              22523