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_4115526
_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            'C28.5 H20 N4 O8.5'
_chemical_formula_weight         554.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   18.236(2)
_cell_length_b                   15.685(1)
_cell_length_c                   18.191(1)
_cell_measurement_reflns_used    '118 from 4 still frames'
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     5203.2(7)
_computing_cell_refinement       'BioteX 1.0 (MSC, 1995)'
_computing_data_collection       'BioteX 1.0 (MSC, 1995)'
_computing_data_reduction        'BioteX 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      294(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
Data was collected at 0.82\%A and 82% completeness by taking
33 oscillation frames in the range of 0 - 162\%, \D\f = 6\%
with \f = 0 - 60\%, 78 - 106\% and 126 - 162\%, \D\f = 3\%
with \f = 60 - 78\% and 108 - 126\%, 10 min. per frame.  Crystal
to detector distance is 78.061mm, background level -45. 
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;
Rigaku RU-200 rotating-anode generator powered at 50kV / 40mA
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11669
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  1.649
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       prism
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0060(5)
_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   1.218
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4089
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0792
_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^)+(0.0653P)^2^+1.4715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1884
_reflns_number_gt                3341
_reflns_number_total             4089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0031826_05.cif
_cod_data_source_block           5
_cod_original_cell_volume        5203.2(5)
_cod_original_formula_sum        'C28.50 H20 N4 O8.50'
_cod_database_code               4115526