#------------------------------------------------------------------------------
#$Date: 2020-12-04 08:04:18 +0200 (Fri, 04 Dec 2020) $
#$Revision: 259535 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/55/4115530.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4115530
loop_
_publ_author_name
'Ram Thaimattam'
'Feng Xue'
'Jagarlapudi A. R. P. Sarma'
'Thomas C. W. Mak'
'Gautam R. Desiraju'
_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 Cl N4 O8'
_chemical_formula_weight         540.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   22.276(1)
_cell_length_b                   22.276(1)
_cell_length_c                   25.348(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     10893.0(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'MSC/AFC Diffractometer Control'
_computing_molecular_graphics    'Siemens SHELXTL-PC'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       'ω scan'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0762
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5055
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        -0.0346
_diffrn_standards_interval_count 190
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       Block
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.284
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4754
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.224
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_obs          0.0483
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0721P)²+0.7477P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1616
_refine_ls_wR_factor_obs         0.1331
_reflns_number_observed          2277
_reflns_number_total             4754
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0031826_09.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.7477P] 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^)+(0.0721P)^2^+0.7477P] 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_formula_sum            'C76 H49 Cl3 N12 O24'
_cod_original_formula_weight         1620.62
_cod_original_formula_units_Z            6
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4115530
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.14330(12) 0.78479(13) 0.02625(9) 0.0472(6) Uani 1 d D
C2 C 0.10303(12) 0.81907(12) 0.04803(9) 0.0456(6) Uani 1 d D
C3 C 0.06223(13) 0.83334(13) 0.01463(10) 0.0502(7) Uani 1 d D
H3 H 0.06278(13) 0.82597(13) -0.02144(10) 0.060 Uiso 1 calc R
C4 C 0.02103(12) 0.85819(12) 0.03392(10) 0.0473(6) Uani 1 d D
H4 H -0.00615(12) 0.86736(12) 0.01115(10) 0.057 Uiso 1 calc R
C5 C 0.02051(12) 0.86924(12) 0.08690(10) 0.0474(6) Uani 1 d D
C6 C 0.05960(14) 0.85554(14) 0.12171(10) 0.0554(7) Uani 1 d D
H6 H 0.05883(14) 0.86342(14) 0.15767(10) 0.066 Uiso 1 calc R
C7 C 0.10003(14) 0.82975(14) 0.10182(10) 0.0549(7) Uani 1 d D
H7 H 0.12588(14) 0.81928(14) 0.12499(10) 0.066 Uiso 1 calc R
N1 N -0.02419(12) 0.89489(12) 0.10761(10) 0.0587(6) Uani 1 d D
O1 O -0.02427(11) 0.90393(11) 0.15522(9) 0.0770(6) Uani 1 d D
O2 O -0.05910(11) 0.90570(12) 0.07626(9) 0.0856(7) Uani 1 d D
C8 C 0.20987(13) 0.80288(13) 0.05716(9) 0.0477(6) Uani 1 d D
C9 C 0.24941(13) 0.86608(14) 0.08195(10) 0.0521(7) Uani 1 d D
H9 H 0.23371(13) 0.89769(14) 0.08271(10) 0.062 Uiso 1 calc R
C10 C 0.31163(13) 0.88305(15) 0.10553(10) 0.0564(7) Uani 1 d D
H10 H 0.33748(13) 0.92510(15) 0.12298(10) 0.068 Uiso 1 calc R
C11 C 0.33459(13) 0.83581(15) 0.10254(10) 0.0539(7) Uani 1 d D
C12 C 0.29775(14) 0.7734(2) 0.07813(11) 0.0629(8) Uani 1 d D
H12 H 0.31436(14) 0.7425(2) 0.07680(11) 0.075 Uiso 1 calc R
C13 C 0.23530(14) 0.75703(15) 0.05545(11) 0.0578(7) Uani 1 d D
H13 H 0.20950(14) 0.71451(15) 0.03862(11) 0.069 Uiso 1 calc R
N2 N 0.40132(13) 0.8537(2) 0.12614(9) 0.0692(7) Uani 1 d D
O3 O 0.42294(11) 0.81324(14) 0.12164(10) 0.0944(7) Uani 1 d D
O4 O 0.43293(11) 0.90932(14) 0.14921(9) 0.0899(7) Uani 1 d D
C14 C 0.08919(13) 0.70680(13) 0.02998(10) 0.0501(6) Uani 1 d D
C15 C 0.08022(14) 0.67266(14) 0.07778(11) 0.0579(7) Uani 1 d D
H15 H 0.10957(14) 0.69643(14) 0.10577(11) 0.069 Uiso 1 calc R
C16 C 0.02946(14) 0.60508(15) 0.08485(11) 0.0619(8) Uani 1 d D
H16 H 0.02376(14) 0.58322(15) 0.11722(11) 0.074 Uiso 1 calc R
C17 C -0.01234(14) 0.57081(14) 0.04343(12) 0.0617(8) Uani 1 d D
C18 C -0.0068(2) 0.6022(2) -0.00410(13) 0.0731(9) Uani 1 d D
H18 H -0.0365(2) 0.5778(2) -0.03174(13) 0.088 Uiso 1 calc R
C19 C 0.0439(2) 0.67099(15) -0.01037(11) 0.0648(8) Uani 1 d D
H19 H 0.0474(2) 0.69325(15) -0.04221(11) 0.078 Uiso 1 calc R
N3 N -0.06548(15) 0.4970(2) 0.04910(14) 0.0870(9) Uani 1 d D
O5 O -0.09861(14) 0.46549(13) 0.00997(12) 0.1034(8) Uani 1 d D
O6 O -0.0725(2) 0.4702(2) 0.09199(12) 0.1370(13) Uani 1 d D
C20 C 0.17322(13) 0.81074(14) -0.02964(9) 0.0498(6) Uani 1 d D
C21 C 0.19975(13) 0.88005(14) -0.04271(10) 0.0557(7) Uani 1 d D
H21 H 0.19444(13) 0.90902(14) -0.01910(10) 0.067 Uiso 1 calc R
C22 C 0.23378(14) 0.9071(2) -0.08981(11) 0.0617(8) Uani 1 d D
H22 H 0.25071(14) 0.9535(2) -0.09825(11) 0.074 Uiso 1 calc R
C23 C 0.24197(15) 0.8639(2) -0.12375(11) 0.0651(8) Uani 1 d D
C24 C 0.2181(2) 0.7957(2) -0.11218(12) 0.0765(9) Uani 1 d D
H24 H 0.2246(2) 0.7674(2) -0.13572(12) 0.092 Uiso 1 calc R
C25 C 0.1839(2) 0.7693(2) -0.06468(11) 0.0695(8) Uani 1 d D
H25 H 0.1678(2) 0.7231(2) -0.05628(11) 0.083 Uiso 1 calc R
N4 N 0.27777(15) 0.8918(2) -0.17456(11) 0.0886(9) Uani 1 d D
O7 O 0.29989(15) 0.9531(2) -0.18341(10) 0.1149(10) Uani 1 d D
O8 O 0.2815(2) 0.8524(2) -0.20560(11) 0.1331(11) Uani 1 d D
C26 C -0.3333 0.3333 0.0745(2) 0.072(2) Uani 1 d S
H26 H -0.3333 0.3333 0.1132(2) 0.109 Uiso 1 calc SR
Cl1 Cl -0.24782(5) 0.37802(6) 0.05297(5) 0.1167(4) Uani 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C8 C1 C2 114.2(2) . .
C8 C1 C14 111.7(2) . .
C2 C1 C14 102.4(2) . .
C8 C1 C20 100.9(2) . .
C2 C1 C20 113.0(2) . .
C14 C1 C20 115.1(2) . .
C3 C2 C7 117.7(2) . .
C3 C2 C1 120.3(2) . .
C7 C2 C1 121.7(2) . .
C4 C3 C2 121.3(2) . .
C5 C4 C3 119.3(2) . .
C4 C5 C6 121.8(2) . .
C4 C5 N1 119.3(2) . .
C6 C5 N1 118.9(2) . .
C5 C6 C7 118.3(2) . .
C6 C7 C2 121.7(2) . .
O2 N1 O1 123.9(2) . .
O2 N1 C5 117.9(2) . .
O1 N1 C5 118.2(2) . .
C9 C8 C13 118.3(2) . .
C9 C8 C1 122.5(2) . .
C13 C8 C1 118.9(2) . .
C10 C9 C8 121.2(3) . .
C9 C10 C11 118.1(3) . .
C12 C11 C10 122.6(3) . .
C12 C11 N2 118.4(3) . .
C10 C11 N2 118.9(3) . .
C11 C12 C13 118.3(3) . .
C12 C13 C8 121.4(3) . .
O3 N2 O4 123.5(3) . .
O3 N2 C11 119.0(3) . .
O4 N2 C11 117.5(3) . .
C19 C14 C15 117.8(2) . .
C19 C14 C1 122.7(2) . .
C15 C14 C1 119.1(2) . .
C16 C15 C14 121.9(3) . .
C17 C16 C15 118.3(3) . .
C16 C17 C18 122.2(3) . .
C16 C17 N3 119.6(3) . .
C18 C17 N3 118.2(3) . .
C17 C18 C19 118.9(3) . .
C14 C19 C18 120.8(3) . .
O6 N3 O5 123.5(3) . .
O6 N3 C17 118.0(3) . .
O5 N3 C17 118.5(3) . .
C25 C20 C21 117.9(2) . .
C25 C20 C1 121.5(2) . .
C21 C20 C1 119.8(2) . .
C22 C21 C20 121.8(3) . .
C23 C22 C21 118.3(3) . .
C24 C23 C22 122.1(3) . .
C24 C23 N4 118.8(3) . .
C22 C23 N4 119.1(3) . .
C23 C24 C25 118.8(3) . .
C20 C25 C24 121.0(3) . .
O8 N4 O7 123.8(3) . .
O8 N4 C23 118.7(3) . .
O7 N4 C23 117.5(3) . .
Cl1 C26 Cl1 110.6(2) 3_455 .
Cl1 C26 Cl1 110.6(2) 3_455 2_565
Cl1 C26 Cl1 110.6(2) . 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C8 1.542(3) .
C1 C2 1.542(3) .
C1 C14 1.545(3) .
C1 C20 1.549(3) .
C2 C3 1.390(3) .
C2 C7 1.391(3) .
C3 C4 1.377(3) .
C4 C5 1.366(3) .
C5 C6 1.377(4) .
C5 N1 1.471(3) .
C6 C7 1.383(4) .
N1 O2 1.217(3) .
N1 O1 1.224(3) .
C8 C9 1.383(3) .
C8 C13 1.394(4) .
C9 C10 1.377(4) .
C10 C11 1.383(4) .
C11 C12 1.360(4) .
C11 N2 1.461(4) .
C12 C13 1.375(4) .
N2 O3 1.220(3) .
N2 O4 1.226(3) .
C14 C19 1.377(4) .
C14 C15 1.391(4) .
C15 C16 1.369(4) .
C16 C17 1.357(4) .
C17 C18 1.367(4) .
C17 N3 1.476(4) .
C18 C19 1.385(4) .
N3 O6 1.212(4) .
N3 O5 1.226(4) .
C20 C25 1.384(4) .
C20 C21 1.389(4) .
C21 C22 1.381(4) .
C22 C23 1.369(4) .
C23 C24 1.368(4) .
C23 N4 1.478(4) .
C24 C25 1.388(4) .
N4 O8 1.212(4) .
N4 O7 1.219(4) .
C26 Cl1 1.738(2) 3_455
C26 Cl1 1.738(2) .
C26 Cl1 1.739(2) 2_565
