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_4115531
_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            'C25.33333 H16.33333 Br N4 O8'
_chemical_formula_weight         584.67
_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                93.02(1)
_cell_angle_beta                 93.02(1)
_cell_angle_gamma                93.02(1)
_cell_formula_units_Z            6
_cell_length_a                   15.437(2)
_cell_length_b                   15.437(2)
_cell_length_c                   15.437(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                     3662.8(8)
_computing_cell_refinement       'MSC bioteX 1.0 (MSC, 1995)'
_computing_data_collection       'MSC bioteX 1.0 (MSC, 1995)'
_computing_data_reduction        'MSC bioteX 1.0 (MSC, 1995)'
_computing_molecular_graphics    'Siemens 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 0.887
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
Take 36 oscillation photos in the range of 0 - 180\%,
\D\f = 5\%, background -40.  Crystal to detector distance 
78.057 mm.
;
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9570
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  1.057
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.8222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                3261
_reflns_number_total             4063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0031826_10.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.8222P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.8222P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2020-12-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3662.8(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C76 H49 Br3 N12 O24'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1754.00
_cod_database_code               4115531