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_4115522
_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            'C29 H24 N4 O9'
_chemical_formula_weight         572.52
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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            16
_cell_length_a                   24.365(3)
_cell_length_b                   28.629(4)
_cell_length_c                   15.257(1)
_cell_measurement_reflns_used    '83 from 4 still photos'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     10642(2)
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
Data was collected to 0.82\%A with 81% completeness by taking 
50 oscillation photos in the range of 0 - 180\%, \D\f = 3.6\%, 
exposure time 8 min. per frame.  Crystal to detector distance 
is 78.303 mm, background level -40.
;
_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  0.0932
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6201
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  1.136
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00055(12)
_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   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2187
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0913P)^2^+7.3898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1969
_reflns_number_gt                1843
_reflns_number_total             2187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0031826_01.cif
_cod_data_source_block           1
_cod_original_cell_volume        10642.5(9)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4115522