Inclusion Compounds of Tetrakis(4-nitrophenyl)methane: C-H...O Networks, Pseudopolymorphism, and Structural Transformations
Ram Thaimattam; Feng Xue; Jagarlapudi A. R. P. Sarma; Thomas C. W. Mak; Gautam R. Desiraju; Journal of the American Chemical Society 123 (2001) 4432–4445; doi:10.1021/ja0031826

data_4115532
_publ_section_title
;
 Inclusion Compounds of Tetrakis(4-nitrophenyl)methane: C-H...O Networks,
 Pseudopolymorphism, and Structural Transformations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4432
_journal_page_last               4445
_journal_paper_doi               10.1021/ja0031826
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C26 H18.33 N4.33 O8.33'
_chemical_formula_weight         524.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.73(1)
_cell_angle_beta                 91.73(1)
_cell_angle_gamma                91.73(1)
_cell_formula_units_Z            6
_cell_length_a                   15.427(2)
_cell_length_b                   15.427(2)
_cell_length_c                   15.427(2)
_cell_measurement_reflns_used    'Take 4 still photos'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3666.4(8)
_computing_cell_refinement       'BioteX ver. 1.0 (MSC, 1995)'
_computing_data_collection       'BioteX ver. 1.0 (MSC, 1995)'
_computing_data_reduction        'BioteX ver. 1.0 (MSC, 1995)'
_computing_molecular_graphics    'SHELXTL-PC (Siemens, 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
The data was collected to 0.82\%A and is 86% complete, by taking 28 
oscillation photos in the range of 0 - 168\%, \D\f = 6\%, 8 min. per 
frame.  Crystal to detector distance 78.064mm, background level -60.   
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;
Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8632
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  1.105
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   ABSCOR
_exptl_absorpt_process_details
;
"ABSCOR: An empirical Absorption Correction Based on Fourier Coefficient 
Fitting", T. Higashi, Rigaku Corp., Tokyo, (c) 1995.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       prism
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0125(16)
_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   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         3474
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0898P)^2^+0.5334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1835
_reflns_number_gt                2980
_reflns_number_total             3474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0031826_11.cif
_cod_data_source_block           11
_cod_original_cell_volume        3666.4(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4115532