#------------------------------------------------------------------------------
#$Date: 2022-04-07 01:54:17 +0300 (Thu, 07 Apr 2022) $
#$Revision: 274408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/99/7709935.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_7709935
loop_
_publ_author_name
'Takeyama, Tomoyuki'
'Iwatsuki, Satoshi'
'Tsushima, Satoru'
'Takao, Koichiro'
_publ_section_title
;
 Synthesis and characterization of uranyl(VI) complex with
 2,6-pyridine-bis(methylaminophenolato) and its ligand-centred aerobic
 oxidation mechanism to diimino derivative
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00325B
_journal_year                    2022
_chemical_formula_moiety         'C35 H49 N3 O4 U, C H2 Cl2'
_chemical_formula_sum            'C36 H51 Cl2 N3 O4 U'
_chemical_formula_weight         898.72
_chemical_properties_physical    Air-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-04-05 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.234(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9394(7)
_cell_length_b                   13.7474(11)
_cell_length_c                   21.7612(11)
_cell_measurement_reflns_used    3838
_cell_measurement_temperature    123
_cell_measurement_theta_max      74.4720
_cell_measurement_theta_min      3.7790
_cell_volume                     4169.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  23.00   0.50   40.00    --    0.00  77.00 -90.00  100
  2  ω     18.00  86.00   0.50   40.00    --    0.00  82.00 -60.00  136
  3  ω    -22.00   6.00   0.50   40.00    --    0.00 -37.00-120.00   56
  4  ω     45.00  78.00   0.50   40.00    --    0.00  77.00 -90.00   66
  5  ω    -72.00 -47.00   0.50   40.00    --    0.00 -37.00-120.00   50
  6  ω    -29.00   4.00   0.50   40.00    --    0.00  82.00 -60.00   66
  7  ω     93.00 118.00   0.50  120.00    --   96.10 -82.00 -60.00   50
  8  ω      8.00 107.00   0.50  120.00    --   96.10 -30.00 150.00  198
  9  ω      8.00  33.00   0.50  120.00    --   96.10   0.00-180.00   50
 10  ω     10.00 119.00   0.50  120.00    --   96.10 -15.00-150.00  218
 11  ω     27.00 111.00   0.50  120.00    --   96.10 -30.00  60.00  168
 12  ω     16.00 118.00   0.50  120.00    --   96.10 -61.00-180.00  204
 13  ω     83.00 108.00   0.50  120.00    --   96.10 -82.00 -30.00   50
 14  ω     77.00 104.00   0.50  120.00    --   96.10 -82.00   0.00   54
 15  ω     73.00 119.00   0.50  120.00    --   96.10 -82.00 -90.00   92
 16  ω    134.00 159.00   0.50  120.00    --   96.10   0.00-180.00   50
 17  ω     82.00 126.00   0.50  120.00    --   96.10 -82.00  52.39   88
 18  ω     49.00 114.00   0.50  120.00    --   96.10 -82.00  22.85  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0627822000
_diffrn_orient_matrix_UB_12      -0.0029918000
_diffrn_orient_matrix_UB_13      -0.0591262000
_diffrn_orient_matrix_UB_21      0.0910069000
_diffrn_orient_matrix_UB_22      -0.0017810000
_diffrn_orient_matrix_UB_23      -0.0388745000
_diffrn_orient_matrix_UB_31      0.0002089000
_diffrn_orient_matrix_UB_32      -0.1120126000
_diffrn_orient_matrix_UB_33      0.0022736000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1993
_diffrn_reflns_av_unetI/netI     0.1915
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25037
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.013
_diffrn_reflns_theta_min         3.803
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.013
_refine_diff_density_max         3.182
_refine_diff_density_min         -6.316
_refine_diff_density_rms         0.301
_refine_ls_extinction_coef       0.00029(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         8183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1934
_refine_ls_R_factor_gt           0.1061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1876P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2765
_refine_ls_wR_factor_ref         0.3447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3745
_reflns_number_total             8183
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00325b2.cif
_cod_data_source_block           UO2tBupdaop
_cod_database_code               7709935
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C35H49N3O4U1Cl2
_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.
;
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) = Uanis(C1) = Uanis(C2)
Uanis(C19) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18)
Uanis(O3) = Uanis(O4) = Uanis(N3) = Uanis(N2) = Uanis(N1)
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) =
Uanis(C13)
Uanis(C23) = Uanis(C21) = Uanis(C20) = Uanis(C22)
Uanis(C25) = Uanis(C26) = Uanis(C24) = Uanis(C27)
Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35)
Uanis(C30) = Uanis(C29) = Uanis(C31) = Uanis(C28)
Uanis(O1) = Uanis(O2)
Uanis(O3) = Uanis(N1) = Uanis(N2) = Uanis(O1) = Uanis(O2) = Uanis(O4) =
Uanis(N3)
Uanis(C36) = Uanis(Cl2) = Uanis(Cl1)
3.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C17(H17), C11(H11), C5(H5), C3(H3A), C10(H10), C15(H15)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C), C22(H22A,H22B,
 H22C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,
 H34B,H34C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C),
 C27(H27A,H27B,H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id 210317UO2-tBupdaop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.827
_oxdiff_exptl_absorpt_empirical_full_min 0.340
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_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.62291(4) 0.41065(7) 0.71521(3) 0.0573(4) Uani 1 1 d . . . . .
Cl1 Cl 0.3923(4) 0.1232(6) 0.6653(3) 0.0832(15) Uani 1 1 d . . . . .
Cl2 Cl 0.2218(4) 0.2347(6) 0.6973(3) 0.0832(15) Uani 1 1 d . . . . .
O3 O 0.5473(10) 0.4029(12) 0.8024(7) 0.0639(18) Uani 1 1 d . . . . .
O4 O 0.5801(10) 0.5601(13) 0.6876(6) 0.0639(18) Uani 1 1 d . . . . .
N1 N 0.6354(12) 0.2439(16) 0.7672(8) 0.0639(18) Uani 1 1 d . . . . .
H1 H 0.692188 0.245858 0.796003 0.077 Uiso 1 1 calc R U . . .
O1 O 0.7299(9) 0.4507(14) 0.7528(6) 0.0639(18) Uani 1 1 d . . . . .
N2 N 0.7298(12) 0.2880(17) 0.6612(8) 0.0639(18) Uani 1 1 d . . . . .
C14 C 0.7007(13) 0.5794(19) 0.6165(9) 0.057(3) Uani 1 1 d . . . . .
C9 C 0.7778(13) 0.130(2) 0.6453(9) 0.063(3) Uani 1 1 d . . . . .
H9 H 0.771921 0.063375 0.655623 0.075 Uiso 1 1 calc R U . . .
C32 C 0.7995(14) 0.795(2) 0.5288(9) 0.067(4) Uani 1 1 d . . . . .
C17 C 0.6735(12) 0.774(2) 0.6105(8) 0.057(3) Uani 1 1 d . . . . .
H17 H 0.664325 0.842567 0.609286 0.069 Uiso 1 1 calc R U . . .
C8 C 0.7228(13) 0.197(2) 0.6762(9) 0.063(3) Uani 1 1 d . . . . .
C16 C 0.7450(13) 0.734(2) 0.5755(8) 0.057(3) Uani 1 1 d . . . . .
C6 C 0.5499(12) 0.229(2) 0.8044(8) 0.060(3) Uani 1 1 d . . . . .
C23 C 0.2806(13) 0.3898(19) 0.9088(10) 0.061(3) Uani 1 1 d . . . . .
H23A H 0.233980 0.351525 0.884625 0.092 Uiso 1 1 calc R U . . .
H23B H 0.250389 0.450284 0.922340 0.092 Uiso 1 1 calc R U . . .
H23C H 0.302021 0.352170 0.944803 0.092 Uiso 1 1 calc R U . . .
C11 C 0.8467(13) 0.253(2) 0.5867(9) 0.063(3) Uani 1 1 d . . . . .
H11 H 0.889796 0.274372 0.556332 0.075 Uiso 1 1 calc R U . . .
C28 C 0.5343(13) 0.769(2) 0.6854(9) 0.074(4) Uani 1 1 d . . . . .
C20 C 0.3676(14) 0.4140(19) 0.8689(10) 0.061(3) Uani 1 1 d . . . . .
O2 O 0.5275(9) 0.3613(14) 0.6729(6) 0.0639(18) Uani 1 1 d . . . . .
C2 C 0.4209(12) 0.313(2) 0.8550(8) 0.060(3) Uani 1 1 d . . . . .
N3 N 0.7027(12) 0.4691(17) 0.6149(8) 0.0639(18) Uani 1 1 d . . . . .
H3 H 0.663072 0.446253 0.578846 0.077 Uiso 1 1 calc R U . . .
C4 C 0.4274(12) 0.137(2) 0.8547(8) 0.060(3) Uani 1 1 d . . . . .
C18 C 0.6127(13) 0.717(2) 0.6484(8) 0.057(3) Uani 1 1 d . . . . .
C5 C 0.5134(12) 0.142(2) 0.8216(8) 0.060(3) Uani 1 1 d . . . . .
H5 H 0.546083 0.083830 0.811289 0.072 Uiso 1 1 calc R U . . .
C7 C 0.6501(14) 0.159(2) 0.7230(9) 0.063(3) Uani 1 1 d . . . . .
H7A H 0.588909 0.140527 0.702182 0.075 Uiso 1 1 calc R U . . .
H7B H 0.676158 0.101438 0.745195 0.075 Uiso 1 1 calc R U . . .
C3 C 0.3837(12) 0.225(2) 0.8705(8) 0.060(3) Uani 1 1 d . . . . .
H3A H 0.325986 0.223395 0.892915 0.072 Uiso 1 1 calc R U . . .
C10 C 0.8392(13) 0.155(2) 0.6013(9) 0.063(3) Uani 1 1 d . . . . .
H10 H 0.876305 0.107788 0.580878 0.075 Uiso 1 1 calc R U . . .
C35 C 0.7413(14) 0.800(2) 0.4700(9) 0.067(4) Uani 1 1 d . . . . .
H35A H 0.728401 0.734500 0.454643 0.101 Uiso 1 1 calc R U . . .
H35B H 0.777067 0.836857 0.439328 0.101 Uiso 1 1 calc R U . . .
H35C H 0.680401 0.833404 0.477631 0.101 Uiso 1 1 calc R U . . .
C19 C 0.6305(13) 0.621(2) 0.6529(9) 0.057(3) Uani 1 1 d . . . . .
C31 C 0.5258(13) 0.881(2) 0.6721(10) 0.074(4) Uani 1 1 d . . . . .
H31A H 0.573617 0.916407 0.697232 0.111 Uiso 1 1 calc R U . . .
H31B H 0.461376 0.903786 0.682345 0.111 Uiso 1 1 calc R U . . .
H31C H 0.537143 0.893546 0.628508 0.111 Uiso 1 1 calc R U . . .
C1 C 0.5051(12) 0.319(2) 0.8193(8) 0.060(3) Uani 1 1 d . . . . .
C22 C 0.3287(13) 0.455(2) 0.8085(9) 0.061(3) Uani 1 1 d . . . . .
H22A H 0.276254 0.413737 0.792981 0.092 Uiso 1 1 calc R U . . .
H22B H 0.380087 0.456555 0.778448 0.092 Uiso 1 1 calc R U . . .
H22C H 0.304806 0.521121 0.815096 0.092 Uiso 1 1 calc R U . . .
C33 C 0.8999(13) 0.755(2) 0.5169(9) 0.067(4) Uani 1 1 d . . . . .
H33A H 0.938688 0.757983 0.554951 0.101 Uiso 1 1 calc R U . . .
H33B H 0.930286 0.794904 0.485299 0.101 Uiso 1 1 calc R U . . .
H33C H 0.895248 0.687733 0.502730 0.101 Uiso 1 1 calc R U . . .
C24 C 0.3789(18) 0.041(3) 0.8742(13) 0.086(4) Uani 1 1 d . . . . .
C29 C 0.5439(13) 0.750(2) 0.7542(9) 0.074(4) Uani 1 1 d . . . . .
H29A H 0.573072 0.686312 0.761397 0.111 Uiso 1 1 calc R U . . .
H29B H 0.480225 0.751991 0.772409 0.111 Uiso 1 1 calc R U . . .
H29C H 0.584514 0.800703 0.773059 0.111 Uiso 1 1 calc R U . . .
C12 C 0.7874(13) 0.322(2) 0.6187(9) 0.063(3) Uani 1 1 d . . . . .
C15 C 0.7580(13) 0.632(2) 0.5787(8) 0.057(3) Uani 1 1 d . . . . .
H15 H 0.805644 0.601224 0.555155 0.069 Uiso 1 1 calc R U . . .
C30 C 0.4360(12) 0.722(2) 0.6642(9) 0.074(4) Uani 1 1 d . . . . .
H30A H 0.436473 0.710264 0.619813 0.111 Uiso 1 1 calc R U . . .
H30B H 0.383568 0.766701 0.673756 0.111 Uiso 1 1 calc R U . . .
H30C H 0.426779 0.660390 0.685839 0.111 Uiso 1 1 calc R U . . .
C13 C 0.7934(13) 0.429(2) 0.6114(9) 0.063(3) Uani 1 1 d . . . . .
H13A H 0.835610 0.456682 0.644076 0.075 Uiso 1 1 calc R U . . .
H13B H 0.821235 0.444869 0.571128 0.075 Uiso 1 1 calc R U . . .
C34 C 0.8125(15) 0.8984(19) 0.5536(10) 0.067(4) Uani 1 1 d . . . . .
H34A H 0.749472 0.928756 0.558278 0.101 Uiso 1 1 calc R U . . .
H34B H 0.850267 0.936516 0.524777 0.101 Uiso 1 1 calc R U . . .
H34C H 0.846044 0.896074 0.593626 0.101 Uiso 1 1 calc R U . . .
C21 C 0.4351(13) 0.4825(19) 0.9048(10) 0.061(3) Uani 1 1 d . . . . .
H21A H 0.411853 0.549521 0.900750 0.092 Uiso 1 1 calc R U . . .
H21B H 0.499817 0.477828 0.888418 0.092 Uiso 1 1 calc R U . . .
H21C H 0.436636 0.463902 0.948322 0.092 Uiso 1 1 calc R U . . .
C36 C 0.3472(15) 0.230(2) 0.7022(12) 0.0832(15) Uani 1 1 d . . . . .
H36A H 0.368061 0.229548 0.745968 0.100 Uiso 1 1 calc R U . . .
H36B H 0.374262 0.288286 0.682615 0.100 Uiso 1 1 calc R U . . .
C26 C 0.3632(17) 0.044(2) 0.9413(12) 0.086(4) Uani 1 1 d . . . . .
H26A H 0.337718 -0.018913 0.954836 0.129 Uiso 1 1 calc R U . . .
H26B H 0.317280 0.095464 0.950560 0.129 Uiso 1 1 calc R U . . .
H26C H 0.424249 0.056823 0.962968 0.129 Uiso 1 1 calc R U . . .
C25 C 0.4396(18) -0.045(2) 0.8577(13) 0.086(4) Uani 1 1 d . . . . .
H25A H 0.500034 -0.042340 0.881466 0.129 Uiso 1 1 calc R U . . .
H25B H 0.453131 -0.042403 0.813692 0.129 Uiso 1 1 calc R U . . .
H25C H 0.405330 -0.104815 0.867037 0.129 Uiso 1 1 calc R U . . .
C27 C 0.2793(17) 0.036(2) 0.8412(12) 0.086(4) Uani 1 1 d . . . . .
H27A H 0.244554 -0.021474 0.855095 0.129 Uiso 1 1 calc R U . . .
H27B H 0.287749 0.032458 0.796681 0.129 Uiso 1 1 calc R U . . .
H27C H 0.242489 0.094740 0.851010 0.129 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -9 0 0.1749
0 9 0 0.0811
-2 0 -14 0.0054
2 0 14 0.0072
9 0 -2 0.0072
-9 0 2 0.0144
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
O3 U1 O4 98.5(6) . . ?
O3 U1 N1 66.6(6) . . ?
O3 U1 N2 131.5(6) . . ?
O3 U1 N3 164.7(7) . . ?
O4 U1 N1 164.6(5) . . ?
O4 U1 N2 130.0(6) . . ?
O4 U1 N3 66.6(6) . . ?
N1 U1 N3 128.4(6) . . ?
O1 U1 O3 91.8(6) . . ?
O1 U1 O4 93.2(7) . . ?
O1 U1 N1 91.5(7) . . ?
O1 U1 N2 85.6(7) . . ?
O1 U1 N3 85.4(6) . . ?
N2 U1 N1 65.0(6) . . ?
N2 U1 N3 63.4(7) . . ?
O2 U1 O3 93.6(6) . . ?
O2 U1 O4 91.1(7) . . ?
O2 U1 N1 85.9(7) . . ?
O2 U1 O1 172.5(7) . . ?
O2 U1 N2 86.9(7) . . ?
O2 U1 N3 90.7(6) . . ?
C1 O3 U1 119.8(13) . . ?
C19 O4 U1 126.4(13) . . ?
U1 N1 H1 107.4 . . ?
C6 N1 U1 108.7(14) . . ?
C6 N1 H1 107.4 . . ?
C6 N1 C7 111.2(18) . . ?
C7 N1 U1 114.6(12) . . ?
C7 N1 H1 107.4 . . ?
C8 N2 U1 118.2(13) . . ?
C8 N2 C12 124(2) . . ?
C12 N2 U1 117.4(18) . . ?
C19 C14 N3 116(2) . . ?
C15 C14 N3 120.4(19) . . ?
C15 C14 C19 123(2) . . ?
C8 C9 H9 118.6 . . ?
C10 C9 H9 118.6 . . ?
C10 C9 C8 123(3) . . ?
C16 C32 C34 109.4(18) . . ?
C35 C32 C16 109.1(17) . . ?
C35 C32 C33 110.7(18) . . ?
C35 C32 C34 108(2) . . ?
C33 C32 C16 113(2) . . ?
C33 C32 C34 106.7(19) . . ?
C16 C17 H17 118.8 . . ?
C16 C17 C18 122(2) . . ?
C18 C17 H17 118.8 . . ?
N2 C8 C9 118(2) . . ?
N2 C8 C7 123(2) . . ?
C9 C8 C7 118(2) . . ?
C17 C16 C32 121(2) . . ?
C17 C16 C15 118(2) . . ?
C15 C16 C32 120.8(19) . . ?
C5 C6 N1 126(2) . . ?
C5 C6 C1 122.1(17) . . ?
C1 C6 N1 112(2) . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
C10 C11 H11 120.8 . . ?
C10 C11 C12 118(2) . . ?
C12 C11 H11 120.8 . . ?
C18 C28 C31 114.1(19) . . ?
C18 C28 C30 106(2) . . ?
C29 C28 C18 112.9(17) . . ?
C29 C28 C31 110(2) . . ?
C29 C28 C30 106.2(18) . . ?
C30 C28 C31 106.4(17) . . ?
C23 C20 C2 106.9(19) . . ?
C22 C20 C23 107.3(16) . . ?
C22 C20 C2 108.4(17) . . ?
C22 C20 C21 115(2) . . ?
C21 C20 C23 109.0(17) . . ?
C21 C20 C2 110.2(16) . . ?
C3 C2 C20 122.7(16) . . ?
C3 C2 C1 121(2) . . ?
C1 C2 C20 116(2) . . ?
U1 N3 H3 108.8 . . ?
C14 N3 U1 106.3(12) . . ?
C14 N3 H3 108.8 . . ?
C13 N3 U1 109.3(14) . . ?
C13 N3 C14 114.7(18) . . ?
C13 N3 H3 108.8 . . ?
C5 C4 C24 124(3) . . ?
C3 C4 C5 117(2) . . ?
C3 C4 C24 118.5(18) . . ?
C17 C18 C28 119(2) . . ?
C19 C18 C17 118.2(19) . . ?
C19 C18 C28 123(2) . . ?
C6 C5 C4 121(2) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
N1 C7 C8 105(2) . . ?
N1 C7 H7A 110.8 . . ?
N1 C7 H7B 110.8 . . ?
C8 C7 H7A 110.8 . . ?
C8 C7 H7B 110.8 . . ?
H7A C7 H7B 108.9 . . ?
C2 C3 C4 122.5(17) . . ?
C2 C3 H3A 118.8 . . ?
C4 C3 H3A 118.8 . . ?
C9 C10 C11 118(2) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O4 C19 C14 116(2) . . ?
C18 C19 O4 124.0(19) . . ?
C18 C19 C14 120(2) . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O3 C1 C6 118.9(16) . . ?
O3 C1 C2 124(2) . . ?
C6 C1 C2 117(2) . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C4 C24 C27 107(2) . . ?
C26 C24 C4 109(2) . . ?
C26 C24 C25 111(3) . . ?
C26 C24 C27 108(2) . . ?
C25 C24 C4 111(2) . . ?
C25 C24 C27 111(3) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N2 C12 C11 118(2) . . ?
N2 C12 C13 117(2) . . ?
C11 C12 C13 124.2(19) . . ?
C14 C15 C16 119(2) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C13 C12 109.7(18) . . ?
N3 C13 H13A 109.7 . . ?
N3 C13 H13B 109.7 . . ?
C12 C13 H13A 109.7 . . ?
C12 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Cl1 C36 H36A 109.3 . . ?
Cl1 C36 H36B 109.3 . . ?
Cl2 C36 Cl1 111.4(15) . . ?
Cl2 C36 H36A 109.3 . . ?
Cl2 C36 H36B 109.3 . . ?
H36A C36 H36B 108.0 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
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 O3 2.193(14) . ?
U1 O4 2.220(18) . ?
U1 N1 2.56(2) . ?
U1 O1 1.773(14) . ?
U1 N2 2.554(19) . ?
U1 O2 1.738(14) . ?
U1 N3 2.599(17) . ?
Cl1 C36 1.79(3) . ?
Cl2 C36 1.75(2) . ?
O3 C1 1.35(3) . ?
O4 C19 1.34(3) . ?
N1 H1 1.0000 . ?
N1 C6 1.47(2) . ?
N1 C7 1.53(3) . ?
N2 C8 1.29(3) . ?
N2 C12 1.32(2) . ?
C14 N3 1.52(3) . ?
C14 C19 1.40(3) . ?
C14 C15 1.37(3) . ?
C9 H9 0.9500 . ?
C9 C8 1.38(3) . ?
C9 C10 1.34(3) . ?
C32 C16 1.53(3) . ?
C32 C35 1.50(3) . ?
C32 C33 1.53(3) . ?
C32 C34 1.53(3) . ?
C17 H17 0.9500 . ?
C17 C16 1.39(2) . ?
C17 C18 1.43(3) . ?
C8 C7 1.55(3) . ?
C16 C15 1.40(3) . ?
C6 C5 1.36(3) . ?
C6 C1 1.42(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C20 1.54(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.38(3) . ?
C11 C12 1.44(3) . ?
C28 C18 1.55(3) . ?
C28 C31 1.58(4) . ?
C28 C29 1.52(3) . ?
C28 C30 1.57(3) . ?
C20 C2 1.61(3) . ?
C20 C22 1.52(3) . ?
C20 C21 1.53(3) . ?
C2 C3 1.36(3) . ?
C2 C1 1.42(2) . ?
N3 H3 1.0000 . ?
N3 C13 1.38(3) . ?
C4 C5 1.41(2) . ?
C4 C3 1.40(3) . ?
C4 C24 1.55(4) . ?
C18 C19 1.33(3) . ?
C5 H5 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C3 H3A 0.9500 . ?
C10 H10 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C24 C26 1.48(4) . ?
C24 C25 1.49(4) . ?
C24 C27 1.55(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C12 C13 1.49(3) . ?
C15 H15 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O3 C1 C6 36(2) . . . . ?
U1 O3 C1 C2 -148.6(14) . . . . ?
U1 O4 C19 C14 20(2) . . . . ?
U1 O4 C19 C18 -164.9(15) . . . . ?
U1 N1 C6 C5 156.3(15) . . . . ?
U1 N1 C6 C1 -21.4(17) . . . . ?
U1 N1 C7 C8 41.2(17) . . . . ?
U1 N2 C8 C9 177.5(13) . . . . ?
U1 N2 C8 C7 3(3) . . . . ?
U1 N2 C12 C11 -178.6(13) . . . . ?
U1 N2 C12 C13 7(2) . . . . ?
U1 N3 C13 C12 53.0(19) . . . . ?
N1 C6 C5 C4 -176.5(16) . . . . ?
N1 C6 C1 O3 -4(2) . . . . ?
N1 C6 C1 C2 179.6(15) . . . . ?
N2 C8 C7 N1 -29(3) . . . . ?
N2 C12 C13 N3 -42(3) . . . . ?
C14 N3 C13 C12 172.3(16) . . . . ?
C9 C8 C7 N1 156.0(18) . . . . ?
C32 C16 C15 C14 -173.2(17) . . . . ?
C17 C16 C15 C14 -1(3) . . . . ?
C17 C18 C19 O4 178.9(17) . . . . ?
C17 C18 C19 C14 -6(3) . . . . ?
C8 N2 C12 C11 0(3) . . . . ?
C8 N2 C12 C13 -174.3(19) . . . . ?
C8 C9 C10 C11 0(3) . . . . ?
C16 C17 C18 C28 -179.6(17) . . . . ?
C16 C17 C18 C19 5(3) . . . . ?
C6 N1 C7 C8 164.8(16) . . . . ?
C23 C20 C2 C3 8(2) . . . . ?
C23 C20 C2 C1 -179.0(16) . . . . ?
C11 C12 C13 N3 144.2(19) . . . . ?
C28 C18 C19 O4 3(3) . . . . ?
C28 C18 C19 C14 178.1(18) . . . . ?
C20 C2 C3 C4 175.7(17) . . . . ?
C20 C2 C1 O3 7(3) . . . . ?
C20 C2 C1 C6 -177.0(15) . . . . ?
N3 C14 C19 O4 7(3) . . . . ?
N3 C14 C19 C18 -168.1(18) . . . . ?
N3 C14 C15 C16 171.6(17) . . . . ?
C18 C17 C16 C32 171.5(18) . . . . ?
C18 C17 C16 C15 -1(3) . . . . ?
C5 C6 C1 O3 177.8(17) . . . . ?
C5 C6 C1 C2 2(2) . . . . ?
C5 C4 C3 C2 0(3) . . . . ?
C5 C4 C24 C26 126(2) . . . . ?
C5 C4 C24 C25 5(3) . . . . ?
C5 C4 C24 C27 -117(2) . . . . ?
C7 N1 C6 C5 29(3) . . . . ?
C7 N1 C6 C1 -148.4(16) . . . . ?
C3 C2 C1 O3 -179.3(16) . . . . ?
C3 C2 C1 C6 -3(2) . . . . ?
C3 C4 C5 C6 -2(3) . . . . ?
C3 C4 C24 C26 -54(3) . . . . ?
C3 C4 C24 C25 -176(2) . . . . ?
C3 C4 C24 C27 63(3) . . . . ?
C10 C9 C8 N2 1(3) . . . . ?
C10 C9 C8 C7 176.2(18) . . . . ?
C10 C11 C12 N2 1(3) . . . . ?
C10 C11 C12 C13 174.9(19) . . . . ?
C35 C32 C16 C17 -83(3) . . . . ?
C35 C32 C16 C15 90(2) . . . . ?
C19 C14 N3 U1 -23.5(19) . . . . ?
C19 C14 N3 C13 -144.5(17) . . . . ?
C19 C14 C15 C16 -1(3) . . . . ?
C31 C28 C18 C17 5(3) . . . . ?
C31 C28 C18 C19 -179.6(19) . . . . ?
C1 C6 C5 C4 1(3) . . . . ?
C1 C2 C3 C4 3(3) . . . . ?
C22 C20 C2 C3 -108(2) . . . . ?
C22 C20 C2 C1 66(2) . . . . ?
C33 C32 C16 C17 153.9(19) . . . . ?
C33 C32 C16 C15 -34(3) . . . . ?
C24 C4 C5 C6 177.8(18) . . . . ?
C24 C4 C3 C2 -179.6(18) . . . . ?
C29 C28 C18 C17 -122(2) . . . . ?
C29 C28 C18 C19 53(3) . . . . ?
C12 N2 C8 C9 -1(3) . . . . ?
C12 N2 C8 C7 -175.8(18) . . . . ?
C12 C11 C10 C9 -1(3) . . . . ?
C15 C14 N3 U1 163.3(14) . . . . ?
C15 C14 N3 C13 42(3) . . . . ?
C15 C14 C19 O4 -180.0(18) . . . . ?
C15 C14 C19 C18 5(3) . . . . ?
C30 C28 C18 C17 122(2) . . . . ?
C30 C28 C18 C19 -63(3) . . . . ?
C34 C32 C16 C17 35(2) . . . . ?
C34 C32 C16 C15 -152.5(19) . . . . ?
C21 C20 C2 C3 126(2) . . . . ?
C21 C20 C2 C1 -61(2) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.5443 -8.9064 0.1619 -0.0171 0.0591 0.9981
0.0671 8.9224 0.1743 -0.0412 -0.0166 -0.9990
-1.9987 0.0013 -13.9973 0.9531 0.3622 -0.0324
1.9987 -0.0013 13.9973 -0.9531 -0.3622 0.0324
9.0007 0.0037 -1.9992 -0.4469 0.8968 -0.0031
-9.0007 -0.0037 1.9992 0.4469 -0.8968 0.0031
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.588 0.000 342.1 125.9 ?
2 0.042 0.208 0.625 7.2 0.2 ?
3 -0.042 0.792 0.375 7.2 0.0 ?
4 0.500 0.403 0.500 342.1 125.9 ?
5 0.458 0.708 0.875 7.2 0.0 ?
6 0.542 0.292 0.125 7.2 0.2 ?
