#------------------------------------------------------------------------------
#$Date: 2016-11-16 04:08:19 +0200 (Wed, 16 Nov 2016) $
#$Revision: 188490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/19/2241945.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241945
loop_
_publ_author_name
'Im, Hansu'
'Moon, Suk-Hee'
'Kim, Tae Ho'
'Park, Ki-Min'
_publ_section_title
;
Crystal structure of N,N'-dibenzylpyromellitic diimide
;
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1809
_journal_page_last 1811
_journal_paper_doi 10.1107/S2056989016017710
_journal_volume 72
_journal_year 2016
_chemical_formula_iupac 'C24 H16 N2 O4'
_chemical_formula_moiety 'C24 H16 N2 O4'
_chemical_formula_sum 'C24 H16 N2 O4'
_chemical_formula_weight 396.39
_chemical_name_common
;
N,N'-Dibenzylpyromellitic diimide
;
_chemical_name_systematic
;
2,6-Dibenzylpyrrolo[3,4-f]isoindole-1,3,5,7(2H,6H)-\
tetraone
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 90.461(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 6.1500(5)
_cell_length_b 4.7475(3)
_cell_length_c 31.002(2)
_cell_measurement_reflns_used 874
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 24.82
_cell_measurement_theta_min 2.63
_cell_volume 905.14(11)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2010)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2008)
;
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0343
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -2
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 4593
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.495
_diffrn_reflns_theta_min 1.314
_exptl_absorpt_coefficient_mu 0.101
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6611
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker 2013)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.454
_exptl_crystal_description needle
_exptl_crystal_F_000 412
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.060
_exptl_crystal_size_min 0.020
_refine_diff_density_max 0.254
_refine_diff_density_min -0.215
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 136
_refine_ls_number_reflns 2016
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.042
_refine_ls_R_factor_all 0.0692
_refine_ls_R_factor_gt 0.0478
_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^)+(0.0529P)^2^+0.0890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1087
_refine_ls_wR_factor_ref 0.1194
_reflns_number_gt 1444
_reflns_number_total 2016
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file sj5513sup1.cif
_cod_data_source_block I
_cod_database_code 2241945
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.951
_shelx_estimated_absorpt_t_max 0.998
_shelx_hkl_file
;
0 0 -1 -1.30 0.40
0 0 1 -0.50 0.50
0 0 1 -0.20 0.40
0 0 -2 -0.50 1.00
0 0 2 -2.30 0.80
0 0 -3 0.00 1.40
0 0 3 0.50 1.30
0 0 4 280.47 10.80
0 0 -4 286.57 11.50
0 0 -5 -1.80 1.60
0 0 5 -2.20 1.30
0 0 6 -1.40 1.60
0 0 -6 1.60 2.30
0 0 -7 2.70 2.60
0 0 7 0.70 1.90
0 0 8 91.59 9.20
0 0 -8 97.99 10.10
0 0 -9 0.40 2.60
0 0 9 0.40 2.40
0 0 10 -3.90 2.00
0 0 11 -0.20 2.60
0 0 12 103.09 13.00
0 0 13 1.90 3.90
0 -1 0 -0.40 0.50
0 -1 0 -0.60 0.40
0 -1 -1 0.30 1.00
0 -1 -1 0.00 0.80
0 1 2 852.01 22.00
0 -1 -2 836.02 23.00
0 -1 2 871.41 20.70
0 -1 2 860.71 21.10
0 1 3 0.00 1.30
0 -1 -3 -0.40 1.50
0 -1 3 -0.90 1.00
0 -1 3 2.00 1.10
0 1 4 44.70 4.70
0 -1 4 50.69 4.80
0 -1 4 46.60 4.20
0 -1 -4 47.40 5.60
0 1 5 0.20 1.50
0 -1 5 0.50 0.80
0 -1 5 -0.90 1.20
0 -1 -5 0.00 1.90
0 1 6 30.30 5.10
0 -1 6 31.90 1.30
0 -1 -6 36.80 6.00
0 -1 6 29.90 4.80
0 -1 6 30.00 4.60
0 1 -7 -0.90 1.90
0 1 7 0.30 2.00
0 -1 7 -0.40 0.50
0 -1 7 -0.80 1.40
0 -1 -7 -1.30 2.10
0 1 8 25.00 5.30
0 -1 8 29.10 2.20
0 -1 -8 25.20 5.80
0 -1 8 22.00 4.80
0 1 9 -1.60 2.30
0 -1 -9 2.10 3.20
0 -1 9 -1.10 0.60
0 -1 9 2.50 2.80
0 1 10 2.60 3.10
0 -1 -10 4.10 3.80
0 -1 10 7.00 3.30
0 -1 11 1.10 2.80
0 -1 12 88.29 11.60
0 -1 13 3.30 4.00
0 -1 14 48.60 10.20
0 -1 15 2.30 4.40
0 -2 0 178.58 5.90
0 -2 0 171.88 5.50
0 -2 -1 0.00 0.90
0 -2 -1 -0.30 1.10
0 -2 -2 152.48 6.80
0 -2 2 144.59 4.70
0 -2 -2 149.79 7.40
0 -2 2 154.78 4.60
0 -2 3 -0.60 0.80
0 -2 -3 -1.40 1.10
0 -2 -3 0.80 1.80
0 -2 3 -0.70 0.80
0 -2 4 3.20 1.60
0 -2 -4 4.00 2.00
0 -2 4 6.20 1.70
0 -2 -4 6.10 2.60
0 2 5 -1.90 1.20
0 -2 5 0.30 1.20
0 -2 -5 -3.30 1.60
0 -2 5 0.00 1.30
0 2 6 29.80 4.90
0 -2 -6 30.60 6.00
0 -2 6 22.00 3.70
0 -2 6 24.20 4.20
0 -2 -7 2.20 2.80
0 -2 7 0.60 1.80
0 -2 7 0.50 1.70
0 -2 8 32.70 5.50
0 -2 -8 47.80 8.40
0 -2 9 -1.10 2.10
0 -2 -9 0.30 2.90
0 -2 -10 34.20 8.10
0 -2 10 30.40 6.10
0 -2 11 -1.90 2.10
0 -2 -11 -1.90 3.50
0 -2 12 40.40 8.10
0 -2 13 0.90 3.50
0 -2 14 28.60 8.00
0 -2 15 -2.20 4.40
0 -3 0 0.90 1.10
0 -3 0 -0.40 0.90
0 -3 1 0.40 0.80
0 -3 1 0.30 0.60
0 -3 -1 0.70 1.40
0 -3 -1 2.00 1.20
0 -3 -2 94.59 6.50
0 -3 2 88.09 3.50
0 -3 -2 87.09 5.50
0 -3 2 82.89 3.40
0 -3 3 0.30 0.80
0 -3 3 0.40 0.80
0 -3 -3 -2.50 1.50
0 -3 -3 -1.00 1.30
0 -3 -4 3.30 1.90
0 -3 4 2.10 1.30
0 -3 4 1.90 1.30
0 -3 -4 3.80 2.90
0 -3 5 0.80 1.30
0 -3 5 -0.70 1.10
0 -3 -5 3.00 2.70
0 -3 -6 59.09 8.70
0 -3 6 62.09 6.30
0 -3 6 56.99 5.50
0 -3 -7 0.80 2.90
0 -3 7 1.00 1.80
0 -3 -8 77.89 11.20
0 -3 8 82.69 8.00
0 -3 9 0.90 2.20
0 -3 -9 1.90 3.60
0 -3 -10 72.19 11.70
0 -3 10 65.09 8.50
0 -3 -11 2.10 4.50
0 -3 11 -1.50 2.60
0 -3 12 -2.20 2.70
0 -3 -12 8.40 6.10
0 -3 13 1.60 4.20
0 -4 0 0.00 1.30
0 -4 0 -0.50 1.10
0 -4 -1 0.40 1.40
0 -4 1 0.70 1.10
0 -4 1 -1.40 1.00
0 -4 -1 -1.60 1.40
0 -4 -2 193.18 10.50
0 -4 2 197.08 6.80
0 -4 2 195.38 6.60
0 -4 3 -0.50 0.90
0 -4 3 -0.40 0.70
0 -4 -3 3.40 2.50
0 -4 4 152.48 6.30
0 -4 -4 135.49 10.20
0 -4 4 143.89 6.10
0 -4 5 0.00 1.20
0 -4 -5 -3.30 1.90
0 -4 5 0.40 1.30
0 -4 6 34.00 4.30
0 -4 -6 55.79 9.00
0 -4 -7 1.10 3.20
0 -4 7 1.40 1.90
0 -4 -8 0.60 3.80
0 -4 8 1.90 2.00
0 -4 -9 2.30 4.30
0 -4 9 0.50 2.30
0 -4 -10 1.10 4.50
0 -4 10 0.50 2.40
0 -4 11 1.30 2.80
0 -4 -11 8.10 5.90
0 -4 12 13.80 5.00
0 -4 -12 13.80 7.50
0 -5 0 2.90 1.90
0 -5 -1 -0.30 1.70
0 -5 1 0.80 1.40
0 -5 -2 2.50 2.40
0 -5 2 3.40 1.30
0 -5 2 3.50 1.30
0 -5 3 0.40 0.90
0 -5 -3 -2.00 2.10
0 -5 3 -0.60 0.80
0 -5 4 1.10 0.90
0 -5 4 -0.50 1.00
0 -5 -4 -1.10 2.60
0 -5 -5 -3.20 2.30
0 -5 5 0.90 1.20
0 -5 6 76.19 5.00
0 -5 -6 78.79 11.30
0 -5 7 0.30 1.70
0 -5 -7 -0.40 3.90
0 -5 -8 32.60 8.30
0 -5 8 23.90 4.20
0 -5 9 0.80 2.20
0 -5 -9 -0.70 4.40
0 -6 0 82.49 6.10
0 -6 1 -1.00 1.50
0 -6 -1 0.90 2.10
0 -6 -2 16.10 4.30
0 -6 -3 3.10 3.00
-1 0 13 1.00 3.90
-1 0 12 -1.60 3.20
-1 0 11 -0.40 2.70
-1 0 10 89.39 10.70
1 0 -9 0.60 2.70
-1 0 9 2.20 2.90
-1 0 8 2.10 2.80
1 0 -8 -1.80 2.10
-1 0 7 -1.00 1.60
1 0 -7 -0.90 2.00
-1 0 6 1518.25 41.70
1 0 -6 1536.25 43.00
1 0 -5 -0.50 1.70
-1 0 5 -2.00 1.10
-1 0 4 -1.00 1.30
1 0 -4 1.10 2.00
1 0 -3 2.50 1.60
-1 0 3 1.00 1.30
1 0 -2 775.02 20.10
-1 0 2 759.82 19.60
-1 0 1 1.00 0.50
-1 0 1 -0.20 0.50
1 0 -1 0.00 0.60
1 0 0 -2.70 0.10
1 0 0 -2.60 0.10
-1 0 0 -2.70 0.10
-1 0 0 -2.80 0.10
1 0 1 -0.10 0.40
-1 0 -1 0.10 0.60
1 0 1 -0.50 0.50
-1 0 -2 110.49 5.00
1 0 2 106.59 4.60
-1 0 -3 0.40 1.50
1 0 3 -0.80 1.10
-1 0 -4 0.60 1.80
1 0 4 -0.30 1.40
1 0 5 0.20 1.60
-1 0 -5 1.00 2.00
1 0 6 -2.10 1.70
-1 0 -6 1.40 2.40
1 0 7 -0.30 1.70
-1 0 -7 1.20 2.20
1 0 8 -1.90 1.70
-1 0 -8 3.60 3.00
1 0 9 2.20 2.70
-1 0 -9 1.30 2.90
1 0 10 801.82 30.10
1 0 11 -0.40 2.50
1 0 12 -1.00 2.90
1 0 13 2.50 3.90
-1 -1 15 -2.00 4.30
-1 -1 14 13.50 6.10
-1 -1 13 0.30 3.60
-1 -1 12 17.00 5.60
-1 -1 11 4.20 3.40
-1 1 10 68.39 9.50
-1 -1 10 54.39 7.80
1 -1 -10 86.89 11.60
-1 1 9 0.80 2.80
1 -1 -9 0.70 2.90
-1 -1 9 -1.60 2.10
-1 -1 9 0.10 0.60
-1 1 8 -0.50 1.90
-1 -1 8 -0.90 1.90
-1 -1 8 -0.10 0.60
1 -1 -8 -4.00 1.70
-1 1 7 -0.10 2.10
-1 -1 7 -0.60 1.50
1 -1 -7 -0.10 2.50
-1 -1 7 0.20 0.50
1 -1 -6 23.40 5.10
-1 -1 6 22.70 3.90
-1 -1 6 21.60 3.90
-1 1 5 0.10 1.60
1 -1 -5 -1.60 1.80
-1 -1 5 0.10 1.40
-1 -1 5 -0.10 0.70
-1 1 4 304.27 11.50
-1 -1 4 279.77 10.80
-1 -1 4 275.57 10.20
1 -1 -4 298.77 12.60
-1 1 3 -0.30 1.10
1 -1 -3 0.10 1.70
-1 -1 3 0.50 1.10
-1 -1 3 1.40 1.10
-1 1 2 1229.78 30.00
1 -1 -2 1070.79 29.90
-1 -1 2 1230.88 28.70
-1 -1 2 1240.28 28.30
1 -1 -2 1237.78 31.10
1 -1 -1 -0.30 1.00
1 -1 -1 0.10 0.80
1 -1 0 1896.01 43.20
1 -1 0 1888.61 42.90
1 -1 1 -0.10 0.50
-1 -1 -1 -0.30 0.90
-1 -1 -1 -0.60 0.70
1 -1 1 0.30 0.50
1 1 2 208.68 7.30
-1 -1 -2 197.98 8.00
1 -1 2 199.88 6.30
1 -1 2 203.08 6.70
1 1 3 -1.50 1.10
-1 -1 -3 -1.20 1.30
1 -1 3 0.20 1.20
1 -1 3 0.30 1.10
1 1 4 764.92 22.40
1 -1 4 777.72 22.30
1 -1 4 759.82 21.30
-1 -1 -4 742.63 23.70
1 1 5 0.80 1.60
1 -1 5 0.60 1.40
-1 -1 -5 -3.60 1.40
1 -1 5 0.40 0.90
1 1 6 242.88 11.60
-1 -1 -6 222.58 12.40
1 -1 6 240.98 11.70
1 -1 6 245.08 11.00
1 -1 6 233.18 6.20
-1 1 -7 1.60 2.10
1 1 7 0.70 1.80
1 -1 7 0.10 0.60
1 -1 7 -0.90 1.50
-1 -1 -7 -1.60 2.00
1 1 8 7.50 3.30
1 -1 8 11.60 1.50
1 -1 8 12.00 3.60
-1 -1 -8 11.20 4.30
1 1 9 -0.30 2.30
1 -1 9 -1.10 1.80
-1 -1 -9 -0.60 2.70
1 1 10 271.97 16.10
1 -1 10 270.77 15.30
-1 -1 -10 278.47 17.50
1 -1 11 -1.30 2.40
1 -1 12 338.57 19.30
1 -1 13 2.20 4.00
1 -1 14 57.09 10.70
1 -1 15 7.90 5.60
-1 -2 15 -4.90 3.80
-1 -2 14 15.10 6.20
-1 -2 13 -3.90 2.60
-1 -2 12 13.60 5.60
-1 -2 11 -0.20 2.60
1 -2 -11 -2.60 2.80
1 -2 -10 10.80 5.20
-1 -2 10 19.10 5.20
-1 -2 9 -0.70 2.00
1 -2 -9 1.40 3.60
-1 -2 8 230.68 12.20
1 -2 -8 248.98 15.60
-1 -2 7 -0.80 1.70
-1 -2 7 -1.20 1.60
1 -2 -7 -2.60 2.00
-1 2 6 426.76 17.10
-1 -2 6 441.16 16.50
1 -2 -6 422.46 19.20
-1 -2 6 472.95 16.00
-1 2 5 3.10 1.90
-1 -2 5 0.20 1.20
1 -2 -5 2.90 2.40
-1 -2 5 -0.40 1.10
1 -2 -4 39.40 5.00
1 -2 -4 31.30 5.10
-1 -2 4 31.40 3.50
-1 -2 4 31.50 3.20
1 -2 -3 0.60 1.70
-1 -2 3 -0.10 0.70
-1 -2 3 -0.50 0.80
1 -2 -3 1.20 1.40
1 -2 -2 68.49 4.50
1 -2 -2 62.79 4.90
1 -2 -1 -1.00 0.80
1 -2 -1 0.20 1.20
1 -2 0 39.50 2.40
1 -2 0 45.70 2.90
-1 -2 0 47.00 2.50
-1 -2 0 40.40 2.10
-1 -2 0 39.80 2.10
1 -2 1 -0.20 0.60
-1 -2 -1 -1.10 0.90
-1 -2 -1 0.20 0.90
1 -2 1 -0.40 0.60
1 -2 2 143.79 5.00
-1 -2 -2 136.59 6.40
1 -2 2 155.38 5.00
-1 -2 -2 136.89 7.00
-1 -2 -3 -0.40 1.00
1 -2 3 0.00 0.80
1 -2 3 2.10 1.10
-1 -2 -3 1.70 1.80
-1 -2 -4 70.89 6.70
1 -2 4 75.49 4.50
-1 -2 -4 68.29 7.10
1 -2 4 88.59 5.30
1 2 5 0.00 1.40
1 -2 5 -1.10 1.10
1 -2 5 -0.10 1.40
-1 -2 -5 1.10 2.30
1 2 6 63.19 6.80
1 -2 6 56.09 5.60
1 -2 6 74.69 7.30
-1 -2 -6 75.59 8.70
-1 -2 -7 -1.80 2.20
1 -2 7 1.50 2.00
1 -2 7 0.00 1.60
1 -2 8 30.80 5.20
-1 -2 -8 47.60 8.30
-1 -2 -9 5.80 4.00
1 -2 9 -0.10 2.10
1 -2 10 55.99 8.20
-1 -2 -10 41.20 8.70
1 -2 11 2.50 3.30
-1 -2 -11 -3.90 3.70
1 -2 12 -2.40 2.70
1 -2 13 0.20 3.20
1 -2 14 68.99 11.30
1 -2 15 -3.10 4.00
-1 -3 13 -2.10 3.50
1 -3 -12 -1.40 4.10
-1 -3 12 0.90 3.20
1 -3 -11 -3.50 3.40
-1 -3 11 -2.90 2.40
-1 -3 10 1.00 2.50
1 -3 -10 1.80 3.60
-1 -3 9 0.60 2.20
1 -3 -9 0.30 3.40
-1 -3 8 17.20 4.00
1 -3 -8 19.30 5.80
-1 -3 7 -0.30 1.60
1 -3 -7 -0.50 2.70
-1 -3 6 52.79 5.30
1 -3 -6 55.19 8.50
-1 -3 6 53.29 5.80
-1 -3 5 0.30 1.20
1 -3 -5 -1.60 1.90
-1 -3 5 -0.50 1.10
-1 -3 4 3.90 1.50
1 -3 -4 4.50 2.30
-1 -3 4 5.20 1.50
1 -3 -4 0.80 2.50
-1 -3 3 -0.10 0.70
-1 -3 3 -0.10 0.70
1 -3 -3 -0.60 1.70
1 -3 -3 -1.20 1.20
1 -3 -2 9.30 2.50
1 -3 -2 11.30 2.90
1 -3 -1 0.30 1.10
1 -3 -1 -0.50 1.20
-1 -3 1 1.30 0.90
-1 -3 1 0.90 0.60
-1 -3 0 345.37 11.00
1 -3 0 344.37 10.80
1 -3 0 350.36 10.80
-1 -3 0 348.57 10.40
1 -3 0 346.97 11.40
1 -3 1 -1.20 0.70
-1 -3 -1 0.90 1.40
1 -3 1 0.10 0.80
-1 -3 -1 -1.30 0.80
1 -3 2 81.59 3.70
-1 -3 -2 72.89 6.60
1 -3 2 82.19 3.60
-1 -3 -2 83.09 5.30
1 -3 3 -0.70 0.80
-1 -3 -3 0.10 1.30
-1 -3 -3 -1.40 1.60
1 -3 3 1.10 0.90
-1 -3 -4 82.89 8.60
1 -3 4 92.59 5.20
1 -3 4 97.39 5.00
-1 -3 -4 99.49 7.00
-1 -3 -5 -1.90 2.00
1 -3 5 -0.10 1.30
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37 0 4 3.60 2.90
37 0 5 0.80 2.70
37 0 6 0.50 2.60
-37 -1 5 3.20 5.70
-37 -1 4 30.10 8.60
-37 -1 3 -0.50 4.60
37 -1 -3 -0.40 2.50
37 -1 -2 23.10 5.10
-37 -1 2 20.90 7.80
-37 -1 1 -2.10 4.50
37 -1 -1 -2.50 2.10
-37 -1 0 3.40 5.70
37 -1 0 0.30 2.50
37 1 1 2.60 2.80
37 -1 1 0.40 2.40
37 1 2 117.19 9.80
37 -1 2 116.39 10.00
37 1 3 1.10 2.80
37 -1 3 -4.50 1.90
37 1 4 2.40 2.90
37 -1 4 1.80 2.50
37 1 5 -2.70 2.60
37 -1 5 -0.90 2.20
-37 -2 3 -4.30 4.30
-37 -2 2 20.90 7.60
-37 -2 1 -4.40 3.90
-37 -2 0 120.89 16.70
-37 -2 -1 1.20 4.70
-37 -2 -2 3.40 5.10
-37 -2 -3 -5.30 4.00
38 0 -5 -0.20 3.30
38 0 -4 19.40 4.70
38 0 -3 0.10 2.70
38 0 -2 3.70 2.90
38 0 -1 3.20 2.90
38 0 0 57.49 7.40
38 0 1 -2.30 2.20
38 0 2 4.10 2.90
38 0 3 -5.00 1.90
38 0 4 67.19 7.50
38 0 5 -2.30 2.00
-38 -1 4 49.20 11.90
-38 -1 3 -3.60 3.60
38 -1 -3 -3.70 2.20
38 -1 -2 5.00 3.30
-38 -1 2 -2.00 4.90
38 -1 -1 -3.00 2.30
38 -1 0 31.20 5.70
38 -1 1 -4.40 1.90
38 1 2 10.00 3.60
38 -1 2 2.30 2.70
38 1 3 1.40 2.70
38 -1 3 0.30 2.20
38 1 4 1.20 2.90
38 -1 4 2.80 2.90
-38 -2 1 -1.30 4.30
-38 -2 0 -2.30 4.30
39 0 -4 -2.70 2.90
39 0 -3 -3.50 2.50
39 0 -2 15.40 4.70
39 0 -1 -0.10 2.90
39 0 0 0.90 2.90
39 0 1 3.90 2.90
39 0 2 30.00 5.80
39 0 3 -4.20 2.20
39 -1 -3 -0.50 2.90
39 -1 -2 5.40 3.70
39 -1 -1 -1.60 2.90
39 -1 0 24.50 5.20
39 -1 1 0.80 2.60
39 1 2 2.70 3.20
39 -1 2 9.60 3.60
40 0 -1 -1.10 2.60
40 0 0 21.30 5.00
40 0 1 -1.30 2.50
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 28530
_shelx_res_file
;
PMDI.res created by SHELXL-2014/7
TITL PMDI.res in P21/n
CELL 0.71073 6.1500 4.7475 31.0020 90.000 90.461 90.000
ZERR 2 0.0005 0.0003 0.0020 0.000 0.003 0.000
LATT 1
SYMM 0.50000 - X , 0.50000 + Y , 0.50000 - Z
SFAC C H N O
UNIT 48 32 4 8
SIZE 0.020 0.060 0.500
TEMP -100
L.S. 5
ACTA
BOND $H
FMAP 2
PLAN 10
CONF
WGHT 0.052900 0.089000
FVAR 0.79828
O1 4 0.914484 0.961741 0.097589 11.00000 0.03441 0.03054 =
0.02929 -0.00983 0.00228 -0.00604
O2 4 0.473705 0.251351 0.049209 11.00000 0.02469 0.02849 =
0.03161 -0.00145 0.00297 -0.00557
N1 3 0.658932 0.617626 0.082166 11.00000 0.02302 0.02193 =
0.02043 -0.00079 0.00335 0.00007
C1 1 0.278342 0.327931 0.154452 11.00000 0.02638 0.02998 =
0.03456 -0.00406 0.00363 0.00024
AFIX 43
H1 2 0.161662 0.365866 0.135042 11.00000 -1.20000
AFIX 0
C2 1 0.250457 0.131143 0.187114 11.00000 0.04025 0.02866 =
0.04013 -0.00148 0.01694 -0.00232
AFIX 43
H2 2 0.115739 0.035447 0.190077 11.00000 -1.20000
AFIX 0
C3 1 0.420569 0.075989 0.215244 11.00000 0.05800 0.03072 =
0.03130 0.00347 0.01507 0.00422
AFIX 43
H3 2 0.402126 -0.056829 0.237841 11.00000 -1.20000
AFIX 0
C4 1 0.617546 0.212962 0.210706 11.00000 0.04598 0.03414 =
0.02672 0.00393 -0.00451 0.00385
AFIX 43
H4 2 0.734594 0.172400 0.229902 11.00000 -1.20000
AFIX 0
C5 1 0.643862 0.409392 0.178124 11.00000 0.03008 0.03151 =
0.02788 -0.00034 -0.00092 -0.00275
AFIX 43
H5 2 0.779188 0.503608 0.175141 11.00000 -1.20000
AFIX 0
C6 1 0.473902 0.469924 0.149733 11.00000 0.02585 0.02282 =
0.02143 -0.00456 0.00493 0.00093
C7 1 0.499373 0.689505 0.115233 11.00000 0.02476 0.02691 =
0.02397 -0.00093 0.00429 0.00255
AFIX 23
H7A 2 0.356503 0.720079 0.101054 11.00000 -1.20000
H7B 2 0.543210 0.869142 0.128992 11.00000 -1.20000
AFIX 0
C8 1 0.849936 0.768659 0.075478 11.00000 0.02272 0.01981 =
0.02140 0.00159 -0.00102 0.00109
C9 1 0.950668 0.645540 0.036182 11.00000 0.02115 0.01839 =
0.02016 0.00103 -0.00251 0.00106
C10 1 0.816836 0.428300 0.021687 11.00000 0.01870 0.01811 =
0.01901 0.00243 0.00007 0.00054
C11 1 0.627901 0.409294 0.051176 11.00000 0.02393 0.01944 =
0.01991 0.00275 -0.00207 0.00115
C12 1 1.138897 0.724860 0.015200 11.00000 0.02291 0.01815 =
0.01954 0.00050 -0.00192 -0.00140
AFIX 43
H12 2 1.230286 0.872494 0.025307 11.00000 -1.20000
AFIX 0
HKLF 4 1 0.0000 0.0000 0.5000 0.0000 -1.0000
0.0000 1.0000 0.0000 0.0000
REM PMDI.res in P21/n
REM R1 = 0.0478 for 1444 Fo > 4sig(Fo) and 0.0692 for all 2016 data
REM 136 parameters refined using 0 restraints
END
WGHT 0.0529 0.0890
REM Highest difference peak 0.254, deepest hole -0.215, 1-sigma level 0.051
Q1 1 0.9038 0.5219 0.0289 11.00000 0.05 0.25
Q2 1 0.2761 0.2185 0.1735 11.00000 0.05 0.22
Q3 1 0.4560 -0.0800 0.2484 11.00000 0.05 0.19
Q4 1 0.8673 0.3178 0.0137 11.00000 0.05 0.19
Q5 1 0.2855 0.1951 0.2092 11.00000 0.05 0.19
Q6 1 0.9160 0.6910 0.0536 11.00000 0.05 0.19
Q7 1 0.4842 0.5974 0.1369 11.00000 0.05 0.18
Q8 1 -0.0409 0.0836 0.1796 11.00000 0.05 0.18
Q9 1 0.7277 0.4195 0.0290 11.00000 0.05 0.17
Q10 1 0.5920 1.1512 0.1329 11.00000 0.05 0.17
;
_shelx_res_checksum 71708
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
O O1 0.9145(2) 0.9617(3) 0.09759(4) 0.0314(4) Uani d 1
O O2 0.4737(2) 0.2514(3) 0.04921(4) 0.0282(3) Uani d 1
N N1 0.6589(2) 0.6176(3) 0.08217(5) 0.0218(4) Uani d 1
C C1 0.2783(3) 0.3279(4) 0.15445(6) 0.0303(5) Uani d 1
H H1 0.1617 0.3659 0.1350 0.036 Uiso calc 1
C C2 0.2505(4) 0.1311(4) 0.18711(7) 0.0363(5) Uani d 1
H H2 0.1157 0.0354 0.1901 0.044 Uiso calc 1
C C3 0.4206(4) 0.0760(4) 0.21524(7) 0.0399(6) Uani d 1
H H3 0.4021 -0.0568 0.2378 0.048 Uiso calc 1
C C4 0.6175(4) 0.2130(4) 0.21071(6) 0.0356(5) Uani d 1
H H4 0.7346 0.1724 0.2299 0.043 Uiso calc 1
C C5 0.6439(3) 0.4094(4) 0.17812(6) 0.0298(5) Uani d 1
H H5 0.7792 0.5036 0.1751 0.036 Uiso calc 1
C C6 0.4739(3) 0.4699(4) 0.14973(6) 0.0233(4) Uani d 1
C C7 0.4994(3) 0.6895(4) 0.11523(6) 0.0252(4) Uani d 1
H H7A 0.3565 0.7201 0.1011 0.030 Uiso calc 1
H H7B 0.5432 0.8691 0.1290 0.030 Uiso calc 1
C C8 0.8499(3) 0.7687(3) 0.07548(6) 0.0213(4) Uani d 1
C C9 0.9507(3) 0.6455(3) 0.03618(5) 0.0199(4) Uani d 1
C C10 0.8168(3) 0.4283(3) 0.02169(5) 0.0186(4) Uani d 1
C C11 0.6279(3) 0.4093(3) 0.05118(5) 0.0211(4) Uani d 1
C C12 1.1389(3) 0.7249(3) 0.01520(5) 0.0202(4) Uani d 1
H H12 1.2303 0.8725 0.0253 0.024 Uiso calc 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0344(9) 0.0305(7) 0.0293(7) -0.0060(6) 0.0023(6) -0.0098(6)
O2 0.0247(8) 0.0285(7) 0.0316(7) -0.0056(6) 0.0030(6) -0.0014(6)
N1 0.0230(9) 0.0219(7) 0.0204(8) 0.0001(6) 0.0034(6) -0.0008(6)
C1 0.0264(11) 0.0300(9) 0.0346(11) 0.0002(8) 0.0036(9) -0.0041(9)
C2 0.0402(14) 0.0287(10) 0.0401(12) -0.0023(10) 0.0169(10) -0.0015(10)
C3 0.0580(17) 0.0307(10) 0.0313(12) 0.0042(11) 0.0151(11) 0.0035(9)
C4 0.0460(14) 0.0341(10) 0.0267(10) 0.0039(10) -0.0045(9) 0.0039(9)
C5 0.0301(12) 0.0315(9) 0.0279(10) -0.0028(9) -0.0009(9) -0.0003(9)
C6 0.0258(11) 0.0228(8) 0.0214(9) 0.0009(8) 0.0049(8) -0.0046(7)
C7 0.0248(11) 0.0269(9) 0.0240(9) 0.0025(8) 0.0043(8) -0.0009(8)
C8 0.0227(10) 0.0198(8) 0.0214(9) 0.0011(7) -0.0010(8) 0.0016(7)
C9 0.0211(10) 0.0184(8) 0.0202(9) 0.0011(7) -0.0025(7) 0.0010(7)
C10 0.0187(9) 0.0181(7) 0.0190(8) 0.0005(7) 0.0001(7) 0.0024(7)
C11 0.0239(10) 0.0194(8) 0.0199(9) 0.0012(8) -0.0021(7) 0.0027(7)
C12 0.0229(11) 0.0182(7) 0.0195(9) -0.0014(7) -0.0019(7) 0.0005(7)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle
C11 N1 C8 . 111.98(15)
C11 N1 C7 . 124.05(15)
C8 N1 C7 . 123.68(14)
C6 C1 C2 . 121.05(19)
C6 C1 H1 . 119.5
C2 C1 H1 . 119.5
C3 C2 C1 . 119.4(2)
C3 C2 H2 . 120.3
C1 C2 H2 . 120.3
C2 C3 C4 . 120.40(19)
C2 C3 H3 . 119.8
C4 C3 H3 . 119.8
C3 C4 C5 . 119.9(2)
C3 C4 H4 . 120.1
C5 C4 H4 . 120.1
C4 C5 C6 . 120.59(19)
C4 C5 H5 . 119.7
C6 C5 H5 . 119.7
C1 C6 C5 . 118.72(17)
C1 C6 C7 . 120.50(17)
C5 C6 C7 . 120.77(17)
N1 C7 C6 . 114.25(14)
N1 C7 H7A . 108.7
C6 C7 H7A . 108.7
N1 C7 H7B . 108.7
C6 C7 H7B . 108.7
H7A C7 H7B . 107.6
O1 C8 N1 . 125.37(17)
O1 C8 C9 . 128.58(17)
N1 C8 C9 . 106.04(14)
C12 C9 C10 . 122.98(16)
C12 C9 C8 . 129.19(15)
C10 C9 C8 . 107.81(16)
C12 C10 C9 3_765 122.44(16)
C12 C10 C11 3_765 129.49(16)
C9 C10 C11 . 108.03(15)
O2 C11 N1 . 125.35(18)
O2 C11 C10 . 128.50(16)
N1 C11 C10 . 106.14(15)
C10 C12 C9 3_765 114.59(15)
C10 C12 H12 3_765 122.7
C9 C12 H12 . 122.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O1 C8 . 1.210(2)
O2 C11 . 1.210(2)
N1 C11 . 1.391(2)
N1 C8 . 1.393(2)
N1 C7 . 1.465(2)
C1 C6 . 1.387(3)
C1 C2 . 1.389(3)
C1 H1 . 0.9500
C2 C3 . 1.382(3)
C2 H2 . 0.9500
C3 C4 . 1.383(3)
C3 H3 . 0.9500
C4 C5 . 1.385(3)
C4 H4 . 0.9500
C5 C6 . 1.391(2)
C5 H5 . 0.9500
C6 C7 . 1.503(2)
C7 H7A . 0.9900
C7 H7B . 0.9900
C8 C9 . 1.491(2)
C9 C12 . 1.385(2)
C9 C10 . 1.392(2)
C10 C12 3_765 1.384(2)
C10 C11 . 1.487(3)
C12 C10 3_765 1.384(2)
C12 H12 . 0.9500
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C7 H7B O1 . 0.99 2.53 2.917(2) 103.2 y
C12 H12 O2 1_665 0.95 2.45 3.401(2) 178.1 y
C7 H7B Cg1 1_565 0.99 2.60 3.478(2) 148 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C6 C1 C2 C3 . . -0.1(3)
C1 C2 C3 C4 . . -0.7(3)
C2 C3 C4 C5 . . 0.8(3)
C3 C4 C5 C6 . . -0.2(3)
C2 C1 C6 C5 . . 0.7(3)
C2 C1 C6 C7 . . -177.86(17)
C4 C5 C6 C1 . . -0.6(3)
C4 C5 C6 C7 . . 178.03(17)
C11 N1 C7 C6 . . 71.0(2)
C8 N1 C7 C6 . . -115.62(18)
C1 C6 C7 N1 . . -115.50(19)
C5 C6 C7 N1 . . 65.9(2)
C11 N1 C8 O1 . . 179.57(16)
C7 N1 C8 O1 . . 5.5(3)
C11 N1 C8 C9 . . 0.27(18)
C7 N1 C8 C9 . . -173.83(14)
O1 C8 C9 C12 . . -1.3(3)
N1 C8 C9 C12 . . 178.00(17)
O1 C8 C9 C10 . . -179.63(17)
N1 C8 C9 C10 . . -0.36(18)
C12 C9 C10 C12 . 3_765 -0.4(3)
C8 C9 C10 C12 . 3_765 178.05(15)
C12 C9 C10 C11 . . -178.18(15)
C8 C9 C10 C11 . . 0.31(18)
C8 N1 C11 O2 . . -178.89(16)
C7 N1 C11 O2 . . -4.8(3)
C8 N1 C11 C10 . . -0.08(18)
C7 N1 C11 C10 . . 173.99(14)
C12 C10 C11 O2 3_765 . 1.1(3)
C9 C10 C11 O2 . . 178.61(17)
C12 C10 C11 N1 3_765 . -177.67(16)
C9 C10 C11 N1 . . -0.15(18)
C10 C9 C12 C10 . 3_765 0.4(3)
C8 C9 C12 C10 . 3_765 -177.73(16)
_cod_database_fobs_code 2241945