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_7218912
_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, 9(H2O)'
_chemical_formula_sum            'C53 H97 N O45'
_chemical_formula_weight         1468.31
_chemical_name_systematic
'4-Phenylpyridine-N-oxide beta-cyclodextrin nonahydrate'
_chemical_properties_physical    'degrades when dry'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                90
_cell_angle_beta                 109.642(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7766(6)
_cell_length_b                   24.6489(8)
_cell_length_c                   15.3471(5)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.09
_cell_measurement_theta_min      2.73
_cell_volume                     6689.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0502
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52904
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.126
_diffrn_reflns_theta_min         3.554
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       Block
_exptl_crystal_F_000             3128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 3440 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         17578
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1439
_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
'w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+5.7869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                9912
_reflns_number_total             17578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02041c2.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 7218911--7218912.cif.'
_cod_database_code               7218912
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              49982