#------------------------------------------------------------------------------
#$Date: 2018-09-03 19:38:49 +0300 (Mon, 03 Sep 2018) $
#$Revision: 210357 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/08/7050890.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_7050890
loop_
_publ_author_name
'Evans, David J.'
'Junk, Peter C.'
'Smith, Matthew K.'
_publ_section_title
;
 Intramolecular C???H????? interactions influence the conformation of
 N,N???-dibenzyl-4,13-diaza-18-crown-6 molecules
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1043
_journal_paper_doi               10.1039/b203646k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C26 H42 N6 O22 U2'
_chemical_formula_weight         1266.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.865(2)
_cell_angle_beta                 102.057(2)
_cell_angle_gamma                91.201(2)
_cell_formula_units_Z            1
_cell_length_a                   8.1390(7)
_cell_length_b                   10.6432(10)
_cell_length_c                   12.1312(11)
_cell_measurement_temperature    296(2)
_cell_volume                     999.37(16)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4565
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    8.181
_exptl_absorpt_correction_T_max  0.3733
_exptl_absorpt_correction_T_min  0.2662
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2807
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0333
_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/[σ²(Fo²)+(0.0577P)²+1.8651P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                2554
_reflns_number_total             2807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203646k.txt
_cod_data_source_block           compound3
_cod_depositor_comments
;

2018-09-03
Formula fixed to put correct number of uranium atoms
                 miguel
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26 H42 N6 O22 U1'
_cod_database_code               7050890
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U -0.13461(4) 0.12298(3) -0.06690(2) 0.03431(15) Uani 1 1 d . . .
O5 O -0.1633(9) 0.3330(6) -0.1318(6) 0.0519(16) Uani 1 1 d . . .
N2 N -0.5114(10) 0.0920(8) -0.1356(7) 0.055(2) Uani 1 1 d . . .
O4 O 0.0906(8) 0.2957(6) -0.0627(6) 0.0536(16) Uani 1 1 d . . .
O6 O 0.0426(10) 0.4667(6) -0.1281(7) 0.0641(19) Uani 1 1 d . . .
N3 N 0.6071(11) 0.4460(7) 0.2744(6) 0.0459(18) Uani 1 1 d . . .
C2 C 0.8034(11) 0.3185(9) 0.3831(7) 0.044(2) Uani 1 1 d . . .
C3 C 0.7963(13) 0.3655(10) 0.4983(8) 0.058(3) Uani 1 1 d . . .
H3 H 0.7837 0.4528 0.5256 0.070 Uiso 1 1 calc R . .
C1 C 0.7855(13) 0.4075(10) 0.3026(8) 0.054(2) Uani 1 1 d . . .
H1A H 0.8176 0.3651 0.2315 0.065 Uiso 1 1 calc R . .
H1B H 0.8607 0.4843 0.3380 0.065 Uiso 1 1 calc R . .
C13 C 0.4036(14) 0.4299(10) 0.7675(9) 0.056(3) Uani 1 1 d . . .
H13A H 0.5210 0.4139 0.7923 0.068 Uiso 1 1 calc R . .
H13B H 0.3519 0.4390 0.8338 0.068 Uiso 1 1 calc R . .
O2C O 0.3715(9) 0.3259(6) 0.5716(6) 0.0575(17) Uani 1 1 d . . .
C6 C 0.8335(14) 0.1065(10) 0.4210(9) 0.063(3) Uani 1 1 d . . .
H6 H 0.8481 0.0192 0.3953 0.076 Uiso 1 1 calc R . .
C7 C 0.8223(12) 0.1877(9) 0.3442(8) 0.048(2) Uani 1 1 d . . .
H7 H 0.8273 0.1544 0.2674 0.058 Uiso 1 1 calc R . .
C4 C 0.8078(14) 0.2846(12) 0.5713(9) 0.065(3) Uani 1 1 d . . .
H4 H 0.8049 0.3181 0.6484 0.078 Uiso 1 1 calc R . .
C12 C 0.3165(15) 0.3167(9) 0.6737(9) 0.061(3) Uani 1 1 d . . .
H12A H 0.3467 0.2361 0.6946 0.073 Uiso 1 1 calc R . .
H12B H 0.1952 0.3203 0.6616 0.073 Uiso 1 1 calc R . .
C11 C 0.2809(15) 0.2322(10) 0.4743(10) 0.067(3) Uani 1 1 d . . .
H11A H 0.1628 0.2498 0.4591 0.081 Uiso 1 1 calc R . .
H11B H 0.2893 0.1469 0.4902 0.081 Uiso 1 1 calc R . .
C5 C 0.8235(14) 0.1540(12) 0.5342(9) 0.068(3) Uani 1 1 d . . .
H5 H 0.8272 0.0993 0.5846 0.082 Uiso 1 1 calc R . .
O9 O -0.6636(8) 0.0846(8) -0.1580(7) 0.070(2) Uani 1 1 d . . .
O7 O -0.4263(9) 0.1923(7) -0.1388(8) 0.077(2) Uani 1 1 d . . .
O1C O 0.3225(9) 0.3561(6) 0.3396(6) 0.0621(18) Uani 1 1 d . . .
O3 O -0.1331(7) -0.0713(6) -0.0075(6) 0.0441(15) Uani 1 1 d D . .
O8 O -0.4250(9) 0.0013(7) -0.1103(6) 0.0584(17) Uani 1 1 d . . .
C9 C 0.3186(16) 0.3483(11) 0.2210(9) 0.074(4) Uani 1 1 d . . .
H9A H 0.2685 0.4237 0.1995 0.089 Uiso 1 1 calc R . .
H9B H 0.2478 0.2726 0.1746 0.089 Uiso 1 1 calc R . .
N1 N -0.0079(11) 0.3686(7) -0.1083(7) 0.0489(19) Uani 1 1 d . . .
C10 C 0.3518(15) 0.2362(10) 0.3708(10) 0.070(3) Uani 1 1 d . . .
H10A H 0.4719 0.2257 0.3883 0.084 Uiso 1 1 calc R . .
H10B H 0.2990 0.1658 0.3064 0.084 Uiso 1 1 calc R . .
C8 C 0.4914(14) 0.3403(10) 0.1938(8) 0.059(3) Uani 1 1 d . . .
H8A H 0.5341 0.2575 0.2013 0.071 Uiso 1 1 calc R . .
H8B H 0.4844 0.3473 0.1146 0.071 Uiso 1 1 calc R . .
O1 O -0.1569(9) 0.2056(6) 0.0718(5) 0.0520(16) Uani 1 1 d . . .
O2 O -0.1190(8) 0.0445(6) -0.2089(5) 0.0496(15) Uiso 1 1 d . . .
H3S H -0.223(6) -0.089(7) 0.033(5) 0.022(18) Uiso 1 1 d D . .
H2 H 0.572(8) 0.458(6) 0.338(6) 0.010(16) Uiso 1 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'
U U -9.6767 9.6646 '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
_geom_angle_publ_flag
O1 U1 O2 177.4(3) . . ?
O1 U1 O3 91.5(3) . 2 ?
O2 U1 O3 90.9(3) . 2 ?
O1 U1 O3 89.4(3) . . ?
O2 U1 O3 92.5(3) . . ?
O3 U1 O3 67.3(2) 2 . ?
O1 U1 O5 89.2(3) . . ?
O2 U1 O5 88.7(3) . . ?
O3 U1 O5 117.5(2) 2 . ?
O3 U1 O5 175.0(2) . . ?
O1 U1 O7 85.5(3) . . ?
O2 U1 O7 92.2(3) . . ?
O3 U1 O7 176.5(2) 2 . ?
O3 U1 O7 114.4(2) . . ?
O5 U1 O7 60.8(2) . . ?
O1 U1 O4 90.0(3) . . ?
O2 U1 O4 89.9(3) . . ?
O3 U1 O4 67.7(2) 2 . ?
O3 U1 O4 134.9(2) . . ?
O5 U1 O4 49.9(2) . . ?
O7 U1 O4 110.5(2) . . ?
O1 U1 O8 92.0(3) . . ?
O2 U1 O8 87.2(3) . . ?
O3 U1 O8 132.5(2) 2 . ?
O3 U1 O8 65.5(2) . . ?
O5 U1 O8 109.8(2) . . ?
O7 U1 O8 49.5(2) . . ?
O4 U1 O8 159.6(2) . . ?
O1 U1 U1 90.5(2) . 2 ?
O2 U1 U1 92.0(2) . 2 ?
O3 U1 U1 33.88(14) 2 2 ?
O3 U1 U1 33.38(14) . 2 ?
O5 U1 U1 151.41(15) . 2 ?
O7 U1 U1 147.66(17) . 2 ?
O4 U1 U1 101.55(14) . 2 ?
O8 U1 U1 98.75(15) . 2 ?
N1 O5 U1 97.5(5) . . ?
O9 N2 O8 123.3(9) . . ?
O9 N2 O7 121.7(9) . . ?
O8 N2 O7 115.0(8) . . ?
N1 O4 U1 96.6(5) . . ?
C8 N3 C1 112.5(7) . . ?
C8 N3 C13 112.0(8) . 2_666 ?
C1 N3 C13 112.3(8) . 2_666 ?
C3 C2 C7 118.8(8) . . ?
C3 C2 C1 120.0(8) . . ?
C7 C2 C1 121.2(8) . . ?
C4 C3 C2 120.3(10) . . ?
C2 C1 N3 111.3(8) . . ?
C12 C13 N3 111.3(8) . 2_666 ?
C11 O2C C12 110.7(8) . . ?
C5 C6 C7 120.8(10) . . ?
C2 C7 C6 119.7(9) . . ?
C3 C4 C5 121.9(10) . . ?
O2C C12 C13 106.3(8) . . ?
O2C C11 C10 109.5(8) . . ?
C6 C5 C4 118.5(10) . . ?
N2 O7 U1 98.2(5) . . ?
C9 O1C C10 112.6(8) . . ?
U1 O3 U1 112.7(2) 2 . ?
N2 O8 U1 97.0(5) . . ?
O1C C9 C8 112.7(9) . . ?
O6 N1 O4 121.9(9) . . ?
O6 N1 O5 122.0(8) . . ?
O4 N1 O5 116.0(7) . . ?
O1C C10 C11 109.8(9) . . ?
N3 C8 C9 109.7(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.765(6) . ?
U1 O2 1.771(6) . ?
U1 O3 2.305(6) 2 ?
U1 O3 2.336(6) . ?
U1 O5 2.529(6) . ?
U1 O7 2.537(7) . ?
U1 O4 2.554(6) . ?
U1 O8 2.567(7) . ?
U1 U1 3.8646(6) 2 ?
O5 N1 1.268(10) . ?
N2 O9 1.208(10) . ?
N2 O8 1.262(10) . ?
N2 O7 1.272(11) . ?
O4 N1 1.258(10) . ?
O6 N1 1.204(10) . ?
N3 C8 1.480(12) . ?
N3 C1 1.507(12) . ?
N3 C13 1.516(12) 2_666 ?
C2 C3 1.389(13) . ?
C2 C7 1.390(13) . ?
C2 C1 1.494(13) . ?
C3 C4 1.357(15) . ?
C13 C12 1.505(15) . ?
C13 N3 1.516(12) 2_666 ?
O2C C11 1.419(12) . ?
O2C C12 1.424(12) . ?
C6 C5 1.373(15) . ?
C6 C7 1.396(13) . ?
C4 C5 1.380(16) . ?
C11 C10 1.496(16) . ?
O1C C9 1.417(14) . ?
O1C C10 1.421(13) . ?
O3 U1 2.305(6) 2 ?
C9 C8 1.510(17) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3S O9 1.002(10) 1.92(3) 2.880(10) 159(6) 2_455
N3 H2 O1C 0.86(7) 2.29(7) 2.813(12) 119(5) .
