Polymorphism of a Hexa-host: Isolation of Four Different Single-Crystal Phases by Melt Crystallization
Dinabandhu Das; Leonard J. Barbour; Journal of the American Chemical Society 130 (2008) 14032–14033; doi:10.1021/ja804940v

data_4108551
_publ_contact_author_address
;
Department of Chemistry, 
University of Stellenbosch, 
Matieland, 7602, 
South Africa.
;
_publ_contact_author_email       ljb@sun.ac.za
_publ_contact_author_fax         '+27 21-808-384'
_publ_contact_author_name        'Prof. Loenard J. Barbour'
_publ_contact_author_phone       '+27 21-808-3335'
_publ_section_title
;
 Polymorphism of a Hexa-host: Isolation of Four Different Single-Crystal
 Phases by Melt Crystallization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14032
_journal_page_last               14033
_journal_paper_doi               10.1021/ja804940v
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C48 H24 N6 O6'
_chemical_formula_sum            'C48 H24 N6 O6'
_chemical_formula_weight         780.73
_chemical_name_common            Hexa-(4-Cyanophenyloxy)benzene
_chemical_name_systematic
; 
Hexa-(4-Cyanophenyloxy)benzene
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.650(3)
_cell_length_b                   11.8192(19)
_cell_length_c                   15.995(3)
_cell_measurement_reflns_used    2989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.36
_cell_volume                     3903.8(11)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22471
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9964
_exptl_absorpt_correction_T_min  0.9893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.062
_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     319
_refine_ls_number_reflns         4655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0654P)^2^+0.6626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                2981
_reflns_number_total             4655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804940v_si_002_4.cif
_cod_data_source_block           M3
_cod_database_code               4108551