Enclathration of bases by a fluorenyl host: structure, stability and selectivity
Bourne, Susan A.; Corin, Kirsten; Cruickshank, Dyanne L.; Davson, Jessica; Nassimbeni, Luigi R.; Su, Hong; Weber, Edwin; New Journal of Chemistry 35 (2011) 1556–; doi:10.1039/c1nj20241c

data_7052692
_publ_section_title
;
 Enclathration of bases by a fluorenyl host: structure, stability and
 selectivity
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1556
_journal_paper_doi               10.1039/c1nj20241c
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         'C32 H22 O2, 2(C6 H7 N)'
_chemical_formula_sum            'C44 H36 N2 O2'
_chemical_formula_weight         624.75
_chemical_melting_point          264.5(5)
_chemical_name_common
;
1,4-bis(9-hydroxyfluoren-9-yl)benzene. 3-picoline clathrate
;
_chemical_name_systematic
;
1,4-bis(9-hydroxyfluoren-9-yl)benzene. 3-picoline clathrate
;
_space_group_IT_number           2
_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                82.2870(10)
_cell_angle_beta                 81.0670(10)
_cell_angle_gamma                72.2300(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4854(2)
_cell_length_b                   13.3617(3)
_cell_length_c                   14.0639(4)
_cell_measurement_reflns_used    3704
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.1
_cell_volume                     1669.69(7)
_computing_cell_refinement       'Collect (Nonius, 2000)'
_computing_data_collection       'Collect (Nonius, 2000)'
_computing_data_reduction        'Collect (Nonius, 2000)'
_computing_molecular_graphics    'XSEED, graphical interface to SHELX (1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Combination of phi and omega'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11272
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'clear blocks'
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                3704
_reflns_number_total             6022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20241c.txt
_cod_data_source_block           h3pic
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '264-265' was changed to '264.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7052692