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_7052694
_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, C6 H7 N, C4 H9 N O'
_chemical_formula_sum            'C42 H38 N2 O3'
_chemical_formula_weight         618.74
_chemical_melting_point          ?
_chemical_name_systematic
;
1,4-bis(9-hydroxyfluoren-9-yl)benzene. 4-picoline and morpholine clathrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 90.1030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.8977(2)
_cell_length_b                   13.9004(2)
_cell_length_c                   28.3312(4)
_cell_measurement_reflns_used    21801
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      3.44
_cell_volume                     6654.56(16)
_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 0.994
_diffrn_measured_fraction_theta_max 0.885
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21801
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0047(3)
_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   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6135
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0686P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                4111
_reflns_number_total             6135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20241c.txt
_cod_data_source_block           hmix
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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 

2018-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      c2/c
_cod_original_formula_moiety     '2(C32 H22 O2), 2(C6 H7 N), 2(C4 H9 N O)'
_cod_original_formula_sum        'C84 H76 N4 O6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1237.49
_cod_database_code               7052694