Synthesis of N,N′-bis(9-phenylxanthen-9-yl)ethylenediamine and an investigation of its host–guest inclusion potential
Barton, Benita; Caira, Mino R.; McCleland, Cedric W.; Taljaard, Benjamin; Journal of the Chemical Society, Perkin Transactions 2  (2000) 865–; doi:10.1039/a907232b

data_7213188
_publ_contact_author
;
     Prof. Cedric W McCleland
     Department of Chemistry,
     University of Port Elizabeth
     PO Box 1600
     Port Elizabeth 6000
     South Africa
;
_publ_section_title
;
 Synthesis of N,N&#x2032;-bis(9-phenylxanthen-9-yl)ethylenediamine and an
 investigation of its host--guest inclusion potential
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              865
_journal_paper_doi               10.1039/a907232b
_journal_year                    2000
_chemical_formula_moiety         'C40 H32 N2 O2.C4 H8 O1'
_chemical_formula_sum            'C44 H40 N2 O3'
_chemical_formula_weight         644.81
_chemical_melting_point          'desolvates 74C; host mp 207C'
_chemical_name_common            none
_chemical_name_systematic
; N,N'-bis(9-phenyl-9-xanthenyl)-ethylenediamine.tetrahydrofuran 
inclusion complex

;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.525(2)
_cell_length_b                   14.705(3)
_cell_length_c                   24.448(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    243(1)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      16
_cell_volume                     3424.3(12)
_computing_cell_refinement       'Enraf-Nonius Structure Determination Package'
_computing_data_collection       'Enraf-Nonius Structure Determination Package'
_computing_data_reduction        'Enraf-Nonius Structure Determination Package'
_computing_molecular_graphics    'PLUTO (Motherwell, 1979)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      243(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega-2-theta scan mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1729
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3398
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        +3.2
_diffrn_standards_interval_time  3600s
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_meas      'unstable, not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.47mm
_exptl_crystal_size_mid          0.31mm
_exptl_crystal_size_min          0.31mm
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                1755
_reflns_number_total             3398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907232bsup1.cif
_cod_data_source_block           art2c1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7213188