# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_twin4_a
_database_code_depnum_ccdc_archive 'CCDC 1479739'
_audit_update_record             
;
2016-05-20 deposited with the CCDC.
2016-07-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_twin4_a             
;
PROBLEM: D-H Without Acceptor       O5     --  H5A    ...     Please Check 
RESPONSE: Hydrogen is likely oriented towards an unmodeled CH3OH molecule for
 which Q-peaks could not be located. See response to PLAT601.
;
# end Validation Reply Form
# start Validation Reply Form
_vrf_PLAT601_twin4_a             
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        164 Ang3  
RESPONSE: Elemental analysis supports the presence of 0.5 CH3OH (the
 crystallization solvent) per uranium complex (4 CH3OH per unit cell). Using
 Squeeze to measure the electron density reveals 75 unmodeled electrons per
 unit cell: 4 CH3OH would have 72 electrons, supporting this conclusion
 (Squeeze was not applied to the final data). Therefore this void is likely to
 contain disordered methanol peaks. However, appropriate Q-peaks could not be
 located within this void.
# end Validation Reply Form
;
# start Validation Reply Form
_vrf_CHEMW03_twin4_a             
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: The 0.5 CH3OH found via EA and SQUEEZE has been added into the 
 formula, causing this discrepancy. 
;
_vrf_PLAT041_twin4_a             
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The 0.5 CH3OH found via EA and SQUEEZE has been added into the 
 formula, causing this discrepancy. 
;
_vrf_PLAT043_twin4_a             
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The 0.5 CH3OH found via EA and SQUEEZE has been added into the
  formula, causing this discrepancy. 
;
# end Validation Reply Form
_audit_creation_date             2016-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-3
_chemical_name_common            UO2(Salophen)tBu
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H48 N2 O5 U, 0.5(C1 H4 O)'
_chemical_formula_sum            'C36.50 H50 N2 O5.50 U'
_chemical_formula_weight         842.81
_chemical_melting_point          ?
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'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   12.9744(6)
_cell_length_b                   17.1766(7)
_cell_length_c                   34.6304(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7717.6(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    296.15
#No means of determining temeprature present in xrd room. 
#temperature was probably between 15-19 C
_cell_measurement_theta_max      70.08
_cell_measurement_theta_min      3.83
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.163
_exptl_absorpt_correction_T_max  0.753396
_exptl_absorpt_correction_T_min  0.256267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 2:
 wR2(int) was 0.1787 before and 0.1339 after correction.
 The Ratio of minimum to maximum transmission is 0.34.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 196361 reflections, Rint = 0.1060
 (79939 with I > 3sig(I), Rint = 0.0898)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3352
_exptl_crystal_recrystallization_method 
'Crystallized via slow evaporation from methanol'
_exptl_crystal_size_max          0.738
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.164
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7065
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.236
_diffrn_reflns_theta_min         2.552
_diffrn_ambient_temperature      296.15

# No means of determining temeprature present in xrd room. 
#Temperature was probably between 15-19 C

_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II DUO CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   
'Microfocus sealed X-ray tub fitted with HELIOS multilayer optics'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5124
_reflns_number_total             7065

_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    
'Olex2 (Dolomanov et al., 2009), ShelXle (Hübschle et al., 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         4.815
_refine_diff_density_min         -2.866
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       0.000052(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7065
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0681
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1373P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.1937
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1 0
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Rigid body (RIGU) restrains
 C24, C35, C34, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C18(H18),
 C20(H20)
4.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

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 0.56937(2) 0.09315(2) 0.26689(2) 0.03457(18) Uani 1 1 d . . . . .
N1 N 0.6600(6) 0.0348(4) 0.32479(19) 0.0374(17) Uani 1 1 d . . . . .
O1 O 0.6757(6) 0.1570(4) 0.2583(2) 0.0508(18) Uani 1 1 d . . . . .
C1 C 0.7068(7) -0.0708(5) 0.2823(2) 0.0340(19) Uani 1 1 d . . . . .
O2 O 0.4738(6) 0.0219(5) 0.27536(19) 0.0568(19) Uani 1 1 d . . . . .
C2 C 0.6883(7) -0.0439(5) 0.3200(2) 0.0336(19) Uani 1 1 d . . . . .
N2 N 0.6911(6) -0.0149(4) 0.2519(2) 0.0355(17) Uani 1 1 d . . . . .
C3 C 0.6936(9) -0.0961(5) 0.3505(3) 0.046(2) Uani 1 1 d . . . . .
H3 H 0.6792 -0.0793 0.3754 0.055 Uiso 1 1 calc R U . . .
O3 O 0.5715(4) 0.0750(4) 0.20357(18) 0.0352(14) Uani 1 1 d . . . . .
C4 C 0.7203(9) -0.1731(5) 0.3439(3) 0.050(3) Uani 1 1 d . . . . .
H4 H 0.7265 -0.2072 0.3647 0.060 Uiso 1 1 calc R U . . .
O4 O 0.5333(6) 0.1641(4) 0.31978(18) 0.0497(17) Uani 1 1 d . . . . .
O5 O 0.4144(7) 0.1757(5) 0.2449(3) 0.067(2) Uani 1 1 d . . . . .
H5A H 0.4054 0.2262 0.2585 0.100 Uiso 1 1 d R U . . .
H5B H 0.3468 0.1504 0.2481 0.100 Uiso 1 1 d R U . . .
C5 C 0.7376(9) -0.1993(5) 0.3072(3) 0.051(3) Uani 1 1 d . . . . .
H5 H 0.7546 -0.2512 0.3029 0.061 Uiso 1 1 calc R U . . .
C6 C 0.7297(9) -0.1482(5) 0.2765(3) 0.051(3) Uani 1 1 d . . . . .
H6 H 0.7400 -0.1664 0.2515 0.061 Uiso 1 1 calc R U . . .
C7 C 0.7433(8) -0.0252(5) 0.2206(3) 0.041(2) Uani 1 1 d . . . . .
H7 H 0.7941 -0.0634 0.2212 0.049 Uiso 1 1 calc R U . . .
C8 C 0.6808(8) 0.0689(5) 0.3570(2) 0.037(2) Uani 1 1 d . . . . .
H8 H 0.7249 0.0417 0.3733 0.044 Uiso 1 1 calc R U . . .
C9 C 0.7303(8) 0.0172(5) 0.1844(2) 0.039(2) Uani 1 1 d . . . . .
C10 C 0.8008(8) 0.0019(6) 0.1551(3) 0.045(2) Uani 1 1 d . . . . .
H10 H 0.8573 -0.0298 0.1603 0.054 Uiso 1 1 calc R U . . .
C11 C 0.7889(9) 0.0329(6) 0.1184(3) 0.050(2) Uani 1 1 d . . . . .
C12 C 0.7053(9) 0.0814(7) 0.1131(3) 0.056(3) Uani 1 1 d . . . . .
H12 H 0.6975 0.1034 0.0887 0.067 Uiso 1 1 calc R U . . .
C13 C 0.6317(9) 0.1007(6) 0.1407(3) 0.052(3) Uani 1 1 d . . . . .
C14 C 0.6443(7) 0.0651(6) 0.1771(2) 0.040(2) Uani 1 1 d . . . . .
C15 C 0.6462(8) 0.1426(5) 0.3715(2) 0.039(2) Uani 1 1 d . . . . .
C16 C 0.5698(7) 0.1869(5) 0.3527(3) 0.038(2) Uani 1 1 d . . . . .
C17 C 0.5339(9) 0.2559(5) 0.3711(3) 0.044(2) Uani 1 1 d . . . . .
C18 C 0.5760(8) 0.2749(6) 0.4066(3) 0.052(3) Uani 1 1 d . . . . .
H18 H 0.5518 0.3196 0.4187 0.062 Uiso 1 1 calc R U . . .
C19 C 0.6522(9) 0.2317(5) 0.4257(2) 0.048(2) Uani 1 1 d . . . . .
C20 C 0.6854(8) 0.1658(5) 0.4079(2) 0.041(2) Uani 1 1 d . . . . .
H20 H 0.7351 0.1351 0.4199 0.050 Uiso 1 1 calc R U . . .
C21 C 0.8628(10) 0.0141(7) 0.0848(3) 0.066(3) Uani 1 1 d . U . . .
C22 C 0.5417(10) 0.1580(9) 0.1332(3) 0.070(4) Uani 1 1 d . . . . .
C23 C 0.4518(9) 0.3082(7) 0.3525(3) 0.059(3) Uani 1 1 d . . . . .
C24 C 0.6939(15) 0.2590(8) 0.4650(3) 0.093(4) Uani 1 1 d . U . . .
C25 C 0.9538(12) -0.0330(10) 0.0979(4) 0.097(4) Uani 1 1 d . U . . .
H25A H 1.0050 -0.0339 0.0779 0.145 Uiso 1 1 calc R U . . .
H25B H 0.9321 -0.0853 0.1034 0.145 Uiso 1 1 calc R U . . .
H25C H 0.9825 -0.0101 0.1208 0.145 Uiso 1 1 calc R U . . .
C26 C 0.9042(12) 0.0914(8) 0.0675(4) 0.080(4) Uani 1 1 d . U . . .
H26A H 0.9455 0.0804 0.0452 0.120 Uiso 1 1 calc R U . . .
H26B H 0.9455 0.1178 0.0865 0.120 Uiso 1 1 calc R U . . .
H26C H 0.8473 0.1240 0.0603 0.120 Uiso 1 1 calc R U . . .
C27 C 0.8017(13) -0.0258(10) 0.0530(4) 0.102(5) Uani 1 1 d . U . . .
H27A H 0.8418 -0.0268 0.0297 0.153 Uiso 1 1 calc R U . . .
H27B H 0.7388 0.0023 0.0485 0.153 Uiso 1 1 calc R U . . .
H27C H 0.7858 -0.0782 0.0606 0.153 Uiso 1 1 calc R U . . .
C28 C 0.5473(13) 0.1925(12) 0.0918(4) 0.119(7) Uani 1 1 d . . . . .
H28A H 0.5456 0.1510 0.0732 0.178 Uiso 1 1 calc R U . . .
H28B H 0.6102 0.2214 0.0889 0.178 Uiso 1 1 calc R U . . .
H28C H 0.4896 0.2265 0.0876 0.178 Uiso 1 1 calc R U . . .
C29 C 0.4408(10) 0.1150(10) 0.1376(4) 0.080(4) Uani 1 1 d . . . . .
H29A H 0.3848 0.1490 0.1309 0.121 Uiso 1 1 calc R U . . .
H29B H 0.4330 0.0982 0.1639 0.121 Uiso 1 1 calc R U . . .
H29C H 0.4403 0.0705 0.1208 0.121 Uiso 1 1 calc R U . . .
C30 C 0.5531(11) 0.2280(8) 0.1607(4) 0.077(4) Uani 1 1 d . . . . .
H30A H 0.6184 0.2528 0.1564 0.115 Uiso 1 1 calc R U . . .
H30B H 0.5494 0.2103 0.1870 0.115 Uiso 1 1 calc R U . . .
H30C H 0.4986 0.2646 0.1560 0.115 Uiso 1 1 calc R U . . .
C31 C 0.4885(12) 0.3390(7) 0.3138(3) 0.077(4) Uani 1 1 d . . . . .
H31A H 0.5256 0.2988 0.3004 0.116 Uiso 1 1 calc R U . . .
H31B H 0.5331 0.3828 0.3178 0.116 Uiso 1 1 calc R U . . .
H31C H 0.4302 0.3547 0.2986 0.116 Uiso 1 1 calc R U . . .
C32 C 0.4229(14) 0.3769(9) 0.3782(5) 0.106(6) Uani 1 1 d . . . . .
H32A H 0.4824 0.4092 0.3822 0.159 Uiso 1 1 calc R U . . .
H32B H 0.3986 0.3579 0.4026 0.159 Uiso 1 1 calc R U . . .
H32C H 0.3696 0.4067 0.3659 0.159 Uiso 1 1 calc R U . . .
C33 C 0.3519(11) 0.2595(8) 0.3461(4) 0.084(4) Uani 1 1 d . . . . .
H33A H 0.2970 0.2934 0.3381 0.126 Uiso 1 1 calc R U . . .
H33B H 0.3331 0.2341 0.3697 0.126 Uiso 1 1 calc R U . . .
H33C H 0.3640 0.2212 0.3264 0.126 Uiso 1 1 calc R U . . .
C34 C 0.7740(16) 0.2045(10) 0.4822(4) 0.117(5) Uani 1 1 d . U . . .
H34A H 0.8366 0.2079 0.4675 0.175 Uiso 1 1 calc R U . . .
H34B H 0.7486 0.1521 0.4815 0.175 Uiso 1 1 calc R U . . .
H34C H 0.7875 0.2193 0.5084 0.175 Uiso 1 1 calc R U . . .
C35 C 0.7443(19) 0.3352(11) 0.4604(6) 0.155(7) Uani 1 1 d . U . . .
H35A H 0.7094 0.3731 0.4761 0.232 Uiso 1 1 calc R U . . .
H35B H 0.7414 0.3508 0.4338 0.232 Uiso 1 1 calc R U . . .
H35C H 0.8150 0.3315 0.4684 0.232 Uiso 1 1 calc R U . . .
C36 C 0.609(2) 0.2612(14) 0.4931(5) 0.167(7) Uani 1 1 d . U . . .
H36A H 0.5441 0.2573 0.4797 0.251 Uiso 1 1 calc R U . . .
H36B H 0.6111 0.3093 0.5072 0.251 Uiso 1 1 calc R U . . .
H36C H 0.6153 0.2183 0.5107 0.251 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O2 1.767(8) . ?
U1 O1 1.787(7) . ?
U1 O3 2.215(6) . ?
U1 O4 2.249(6) . ?
U1 N2 2.491(7) . ?
U1 N1 2.531(7) . ?
U1 O5 2.575(7) . ?
N1 C8 1.287(11) . ?
N1 C2 1.411(10) . ?
C1 C6 1.377(12) . ?
C1 C2 1.405(12) . ?
C1 N2 1.441(11) . ?
C2 C3 1.387(12) . ?
N2 C7 1.289(12) . ?
C3 C4 1.385(12) . ?
C3 H3 0.9300 . ?
O3 C14 1.328(10) . ?
C4 C5 1.369(13) . ?
C4 H4 0.9300 . ?
O4 C16 1.296(11) . ?
O5 H5A 0.9942 . ?
O5 H5B 0.9862 . ?
C5 C6 1.382(13) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C9 1.459(12) . ?
C7 H7 0.9300 . ?
C8 C15 1.434(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.391(13) . ?
C9 C14 1.411(14) . ?
C10 C11 1.386(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(15) . ?
C11 C21 1.543(14) . ?
C12 C13 1.390(15) . ?
C12 H12 0.9300 . ?
C13 C14 1.409(14) . ?
C13 C22 1.550(17) . ?
C15 C16 1.408(13) . ?
C15 C20 1.417(12) . ?
C16 C17 1.424(13) . ?
C17 C18 1.386(14) . ?
C17 C23 1.534(15) . ?
C18 C19 1.403(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.360(13) . ?
C19 C24 1.535(14) . ?
C20 H20 0.9300 . ?
C21 C25 1.502(19) . ?
C21 C27 1.521(17) . ?
C21 C26 1.553(17) . ?
C22 C29 1.511(19) . ?
C22 C30 1.541(19) . ?
C22 C28 1.554(16) . ?
C23 C31 1.519(16) . ?
C23 C32 1.524(16) . ?
C23 C33 1.558(18) . ?
C24 C35 1.47(2) . ?
C24 C36 1.47(3) . ?
C24 C34 1.52(2) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

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
O2 U1 O1 173.9(4) . . ?
O2 U1 O3 94.3(3) . . ?
O1 U1 O3 85.0(3) . . ?
O2 U1 O4 95.4(3) . . ?
O1 U1 O4 87.9(3) . . ?
O3 U1 O4 152.3(2) . . ?
O2 U1 N2 87.9(3) . . ?
O1 U1 N2 86.1(3) . . ?
O3 U1 N2 71.4(2) . . ?
O4 U1 N2 134.9(2) . . ?
O2 U1 N1 85.5(3) . . ?
O1 U1 N1 90.9(3) . . ?
O3 U1 N1 136.3(2) . . ?
O4 U1 N1 70.5(2) . . ?
N2 U1 N1 64.9(2) . . ?
O2 U1 O5 83.2(3) . . ?
O1 U1 O5 102.5(3) . . ?
O3 U1 O5 78.2(3) . . ?
O4 U1 O5 77.3(3) . . ?
N2 U1 O5 147.5(3) . . ?
N1 U1 O5 144.6(3) . . ?
C8 N1 C2 118.9(7) . . ?
C8 N1 U1 127.1(6) . . ?
C2 N1 U1 114.0(5) . . ?
C6 C1 C2 119.3(8) . . ?
C6 C1 N2 124.6(8) . . ?
C2 C1 N2 115.8(7) . . ?
C3 C2 C1 119.1(7) . . ?
C3 C2 N1 122.9(8) . . ?
C1 C2 N1 118.0(7) . . ?
C7 N2 C1 116.6(8) . . ?
C7 N2 U1 127.7(6) . . ?
C1 N2 U1 115.7(5) . . ?
C4 C3 C2 120.4(9) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C14 O3 U1 135.3(5) . . ?
C5 C4 C3 120.5(8) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C16 O4 U1 143.5(6) . . ?
U1 O5 H5A 115.6 . . ?
U1 O5 H5B 114.7 . . ?
H5A O5 H5B 103.1 . . ?
C4 C5 C6 119.6(8) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 121.2(9) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
N2 C7 C9 126.3(9) . . ?
N2 C7 H7 116.9 . . ?
C9 C7 H7 116.9 . . ?
N1 C8 C15 129.7(8) . . ?
N1 C8 H8 115.1 . . ?
C15 C8 H8 115.1 . . ?
C10 C9 C14 119.9(8) . . ?
C10 C9 C7 117.2(9) . . ?
C14 C9 C7 122.5(8) . . ?
C11 C10 C9 121.6(10) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C12 C11 C10 116.2(9) . . ?
C12 C11 C21 120.9(9) . . ?
C10 C11 C21 122.9(10) . . ?
C11 C12 C13 126.3(10) . . ?
C11 C12 H12 116.9 . . ?
C13 C12 H12 116.9 . . ?
C12 C13 C14 115.6(10) . . ?
C12 C13 C22 123.7(9) . . ?
C14 C13 C22 120.8(9) . . ?
O3 C14 C13 118.7(9) . . ?
O3 C14 C9 120.8(8) . . ?
C13 C14 C9 120.4(9) . . ?
C16 C15 C20 120.8(8) . . ?
C16 C15 C8 122.4(8) . . ?
C20 C15 C8 116.6(8) . . ?
O4 C16 C15 120.0(8) . . ?
O4 C16 C17 121.6(9) . . ?
C15 C16 C17 118.3(9) . . ?
C18 C17 C16 117.5(9) . . ?
C18 C17 C23 120.6(9) . . ?
C16 C17 C23 121.9(9) . . ?
C17 C18 C19 125.0(9) . . ?
C17 C18 H18 117.5 . . ?
C19 C18 H18 117.5 . . ?
C20 C19 C18 116.7(9) . . ?
C20 C19 C24 123.0(10) . . ?
C18 C19 C24 120.3(9) . . ?
C19 C20 C15 121.6(9) . . ?
C19 C20 H20 119.2 . . ?
C15 C20 H20 119.2 . . ?
C25 C21 C27 112.7(13) . . ?
C25 C21 C11 111.9(10) . . ?
C27 C21 C11 108.5(11) . . ?
C25 C21 C26 107.8(12) . . ?
C27 C21 C26 106.7(11) . . ?
C11 C21 C26 109.0(10) . . ?
C29 C22 C30 113.7(11) . . ?
C29 C22 C13 109.0(11) . . ?
C30 C22 C13 108.7(10) . . ?
C29 C22 C28 108.7(12) . . ?
C30 C22 C28 105.6(13) . . ?
C13 C22 C28 111.2(10) . . ?
C31 C23 C32 108.9(11) . . ?
C31 C23 C17 110.8(10) . . ?
C32 C23 C17 112.3(10) . . ?
C31 C23 C33 108.7(11) . . ?
C32 C23 C33 107.1(11) . . ?
C17 C23 C33 108.9(10) . . ?
C35 C24 C36 112.4(16) . . ?
C35 C24 C34 106.6(17) . . ?
C36 C24 C34 105.6(14) . . ?
C35 C24 C19 109.5(12) . . ?
C36 C24 C19 109.1(15) . . ?
C34 C24 C19 113.5(10) . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C21 C27 H27A 109.5 . . ?
C21 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C21 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 C29 H29A 109.5 . . ?
C22 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C22 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C23 C31 H31A 109.5 . . ?
C23 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C23 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C23 C32 H32A 109.5 . . ?
C23 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C23 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C23 C33 H33A 109.5 . . ?
C23 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C23 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C24 C34 H34A 109.5 . . ?
C24 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C24 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C24 C35 H35A 109.5 . . ?
C24 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C24 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C24 C36 H36A 109.5 . . ?
C24 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C24 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

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
C6 C1 C2 C3 0.0(14) . . . . ?
N2 C1 C2 C3 174.8(9) . . . . ?
C6 C1 C2 N1 -176.9(9) . . . . ?
N2 C1 C2 N1 -2.2(12) . . . . ?
C8 N1 C2 C3 29.8(14) . . . . ?
U1 N1 C2 C3 -149.5(8) . . . . ?
C8 N1 C2 C1 -153.4(9) . . . . ?
U1 N1 C2 C1 27.3(10) . . . . ?
C6 C1 N2 C7 -32.1(13) . . . . ?
C2 C1 N2 C7 153.4(8) . . . . ?
C6 C1 N2 U1 149.6(9) . . . . ?
C2 C1 N2 U1 -24.8(10) . . . . ?
C1 C2 C3 C4 2.2(15) . . . . ?
N1 C2 C3 C4 179.0(10) . . . . ?
C2 C3 C4 C5 -2.7(17) . . . . ?
C3 C4 C5 C6 0.9(17) . . . . ?
C2 C1 C6 C5 -1.8(16) . . . . ?
N2 C1 C6 C5 -176.1(10) . . . . ?
C4 C5 C6 C1 1.4(17) . . . . ?
C1 N2 C7 C9 171.3(8) . . . . ?
U1 N2 C7 C9 -10.7(12) . . . . ?
C2 N1 C8 C15 -168.5(9) . . . . ?
U1 N1 C8 C15 10.8(15) . . . . ?
N2 C7 C9 C10 174.3(9) . . . . ?
N2 C7 C9 C14 -12.8(14) . . . . ?
C14 C9 C10 C11 0.1(14) . . . . ?
C7 C9 C10 C11 173.1(9) . . . . ?
C9 C10 C11 C12 2.0(15) . . . . ?
C9 C10 C11 C21 -177.0(10) . . . . ?
C10 C11 C12 C13 -1.3(17) . . . . ?
C21 C11 C12 C13 177.7(11) . . . . ?
C11 C12 C13 C14 -1.4(17) . . . . ?
C11 C12 C13 C22 177.7(12) . . . . ?
U1 O3 C14 C13 -141.2(8) . . . . ?
U1 O3 C14 C9 41.6(13) . . . . ?
C12 C13 C14 O3 -173.7(9) . . . . ?
C22 C13 C14 O3 7.2(15) . . . . ?
C12 C13 C14 C9 3.5(14) . . . . ?
C22 C13 C14 C9 -175.6(10) . . . . ?
C10 C9 C14 O3 174.2(8) . . . . ?
C7 C9 C14 O3 1.5(13) . . . . ?
C10 C9 C14 C13 -3.0(14) . . . . ?
C7 C9 C14 C13 -175.7(9) . . . . ?
N1 C8 C15 C16 7.8(17) . . . . ?
N1 C8 C15 C20 -178.1(10) . . . . ?
U1 O4 C16 C15 -25.1(15) . . . . ?
U1 O4 C16 C17 155.6(8) . . . . ?
C20 C15 C16 O4 -178.6(8) . . . . ?
C8 C15 C16 O4 -4.8(14) . . . . ?
C20 C15 C16 C17 0.7(14) . . . . ?
C8 C15 C16 C17 174.5(9) . . . . ?
O4 C16 C17 C18 178.7(9) . . . . ?
C15 C16 C17 C18 -0.6(14) . . . . ?
O4 C16 C17 C23 -1.5(15) . . . . ?
C15 C16 C17 C23 179.3(9) . . . . ?
C16 C17 C18 C19 0.8(16) . . . . ?
C23 C17 C18 C19 -179.1(10) . . . . ?
C17 C18 C19 C20 -1.0(16) . . . . ?
C17 C18 C19 C24 179.3(12) . . . . ?
C18 C19 C20 C15 1.1(15) . . . . ?
C24 C19 C20 C15 -179.3(11) . . . . ?
C16 C15 C20 C19 -1.0(14) . . . . ?
C8 C15 C20 C19 -175.1(9) . . . . ?
C12 C11 C21 C25 174.2(12) . . . . ?
C10 C11 C21 C25 -6.8(16) . . . . ?
C12 C11 C21 C27 -60.7(15) . . . . ?
C10 C11 C21 C27 118.3(13) . . . . ?
C12 C11 C21 C26 55.1(15) . . . . ?
C10 C11 C21 C26 -125.9(12) . . . . ?
C12 C13 C22 C29 117.9(12) . . . . ?
C14 C13 C22 C29 -63.0(15) . . . . ?
C12 C13 C22 C30 -117.7(12) . . . . ?
C14 C13 C22 C30 61.4(14) . . . . ?
C12 C13 C22 C28 -1.9(19) . . . . ?
C14 C13 C22 C28 177.2(12) . . . . ?
C18 C17 C23 C31 119.7(11) . . . . ?
C16 C17 C23 C31 -60.1(14) . . . . ?
C18 C17 C23 C32 -2.3(16) . . . . ?
C16 C17 C23 C32 177.9(12) . . . . ?
C18 C17 C23 C33 -120.8(11) . . . . ?
C16 C17 C23 C33 59.4(13) . . . . ?
C20 C19 C24 C35 117.9(15) . . . . ?
C18 C19 C24 C35 -62.5(19) . . . . ?
C20 C19 C24 C36 -118.7(15) . . . . ?
C18 C19 C24 C36 61.0(17) . . . . ?
C20 C19 C24 C34 -1(2) . . . . ?
C18 C19 C24 C34 178.5(14) . . . . ?




_olex2_exptl_crystal_mounting_method 
'MiTeGen dual-thickness MicroMounts using parabar oil'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1
2 0
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kh140_a
_database_code_depnum_ccdc_archive 'CCDC 1479740'
_audit_update_record             
;
2016-05-20 deposited with the CCDC.
2016-07-13 downloaded from the CCDC.
;
_audit_creation_date             2016-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-3
_chemical_name_common            UO2(Salophen)OMe
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C30 H36 N2 O7 U), C H Cl3'
_chemical_formula_sum            'C61 H73 Cl3 N4 O14 U2'
_chemical_formula_weight         1668.64
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0190 0.0100 '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 0.3660 0.7110 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0330 0.0190 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0520 0.0340 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.2470 13.6570 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   9.4679(4)
_cell_length_b                   10.7796(5)
_cell_length_c                   30.4674(14)
_cell_angle_alpha                90
_cell_angle_beta                 91.856(3)
_cell_angle_gamma                90
_cell_volume                     3107.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4599
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.454
_cell_measurement_theta_min      2.903
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.208
_exptl_absorpt_correction_T_max  0.467166
_exptl_absorpt_correction_T_min  0.210861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1239 before and 0.0517 after correction.
 The Ratio of minimum to maximum transmission is 0.45.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1283 before and 0.0599 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 38731 reflections, Rint = 0.0803
 (19723 with I > 3sig(I), Rint = 0.0669)
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1628
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystallized from CDCl3 in an NMR tube via slow evaporation.'
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.029
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9028
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.499
_diffrn_reflns_theta_min         2.902
_diffrn_ambient_temperature      149.97
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II DUO CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   
'Microfocus sealed X-ray tub fitted with HELIOS multilayer optics'
_diffrn_source_target            Cu
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8111
_reflns_number_total             9028
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    
'Olex2 (Dolomanov et al., 2009), ShelXle (Hübschle et al., 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.128
_refine_diff_density_min         -4.506
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.000066(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         9028
_refine_ls_number_restraints     411
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0559
_refine_ls_restrained_S_all      1.168
_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/[σ²(Fo²)+(0.0063P)²+64.1379P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1285
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5812(12) 0.4188(12)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H31 of C31, All O(H,H) groups
 At 1.2 times of:
  H3 of C3, H14 of C14, H16 of C16, H15 of C15, H21 of C21, H23 of C23, H5 of
  C5, H17 of C17, H19 of C19, H12 of C12
3. Restrained distances
 H5A-H5B
 1.518 with sigma of 0.02
 O5-H5A
 0.96 with sigma of 0.02
 O5-H5B
 0.96 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C31(0.5) H31(0.5) Cl4(0.5) Cl5(0.5) Cl6(0.5)
7.a Free rotating group:
 C31(H31,Cl4,Cl5,Cl6)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C12(H12), C14(H14), C16(H16), C15(H15),
 C21(H21), C23(H23)
7.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.43654(4) 0.77466(4) 0.24646(2) 0.01642(13) Uani 1 1 d . U . . .
O1 O 0.5709(9) 0.8860(9) 0.2453(3) 0.021(2) Uani 1 1 d . U . . .
N1 N 0.5713(13) 0.6108(11) 0.2924(3) 0.020(2) Uani 1 1 d . U . . .
O3 O 0.4054(10) 0.8055(8) 0.1745(3) 0.020(2) Uani 1 1 d . U . . .
C3 C 0.5288(16) 0.8807(13) 0.4295(4) 0.024(3) Uani 1 1 d . U . . .
H3 H 0.5110 0.9389 0.4520 0.029 Uiso 1 1 calc R . . . .
C2 C 0.4577(16) 0.8952(13) 0.3897(4) 0.021(3) Uani 1 1 d . U . . .
O2 O 0.2931(11) 0.6612(8) 0.2455(3) 0.026(2) Uani 1 1 d . U . . .
N2 N 0.5849(11) 0.6246(11) 0.2038(3) 0.018(2) Uani 1 1 d . U . . .
C4 C 0.6240(15) 0.7873(15) 0.4385(4) 0.029(3) Uani 1 1 d . U . . .
O4 O 0.4205(10) 0.8103(9) 0.3174(3) 0.023(2) Uani 1 1 d . U . . .
C7 C 0.3549(15) 1.0011(14) 0.3798(5) 0.023(3) Uani 1 1 d . U . . .
O7 O 0.6793(13) 0.7860(11) 0.4809(3) 0.043(3) Uani 1 1 d . U . . .
C6 C 0.5897(14) 0.7126(14) 0.3648(4) 0.022(3) Uani 1 1 d . U . . .
O6 O 0.7540(11) 0.8843(11) 0.0357(3) 0.034(3) Uani 1 1 d . U . . .
C5 C 0.6559(16) 0.7017(14) 0.4067(5) 0.029(3) Uani 1 1 d . U . . .
H5 H 0.7211 0.6366 0.4130 0.034 Uiso 1 1 calc R . . . .
O5 O 0.2355(10) 0.9177(9) 0.2459(4) 0.028(2) Uani 1 1 d D U . . .
H5A H 0.201(13) 0.998(5) 0.254(6) 0.042 Uiso 1 1 d DR . . . .
H5B H 0.158(9) 0.863(9) 0.249(6) 0.042 Uiso 1 1 d DR . . . .
C9 C 0.2077(16) 0.9523(15) 0.3659(5) 0.027(3) Uani 1 1 d . U . . .
H9A H 0.1433 1.0224 0.3608 0.041 Uiso 1 1 calc GR . . . .
H9B H 0.1716 0.8996 0.3892 0.041 Uiso 1 1 calc GR . . . .
H9C H 0.2141 0.9037 0.3388 0.041 Uiso 1 1 calc GR . . . .
C8 C 0.4122(16) 1.0852(15) 0.3446(5) 0.028(3) Uani 1 1 d . U . . .
H8A H 0.5011 1.1226 0.3553 0.043 Uiso 1 1 calc GR . . . .
H8B H 0.3434 1.1508 0.3376 0.043 Uiso 1 1 calc GR . . . .
H8C H 0.4290 1.0365 0.3181 0.043 Uiso 1 1 calc GR . . . .
C17 C 0.6114(16) 0.3958(13) 0.1987(4) 0.022(3) Uani 1 1 d . U . . .
H17 H 0.6169 0.3996 0.1677 0.026 Uiso 1 1 calc R . . . .
C19 C 0.6409(14) 0.6459(12) 0.1662(4) 0.018(3) Uani 1 1 d . U . . .
H19 H 0.7068 0.5864 0.1563 0.021 Uiso 1 1 calc R . . . .
C10 C 0.3339(17) 1.0817(14) 0.4211(5) 0.029(3) Uani 1 1 d . U . . .
H10A H 0.4251 1.1161 0.4312 0.044 Uiso 1 1 calc GR . . . .
H10B H 0.2950 1.0305 0.4444 0.044 Uiso 1 1 calc GR . . . .
H10C H 0.2684 1.1496 0.4139 0.044 Uiso 1 1 calc GR . . . .
C11 C 0.776(2) 0.6904(16) 0.4921(5) 0.041(4) Uani 1 1 d . U . . .
H11A H 0.8571 0.6949 0.4730 0.061 Uiso 1 1 calc GR . . . .
H11B H 0.7295 0.6097 0.4884 0.061 Uiso 1 1 calc GR . . . .
H11C H 0.8086 0.7002 0.5228 0.061 Uiso 1 1 calc GR . . . .
C116 C 0.6146(14) 0.2820(15) 0.2197(5) 0.026(3) Uani 1 1 d . U . . .
H116 H 0.6224 0.2083 0.2028 0.031 Uiso 1 1 calc R . . . .
C114 C 0.5941(13) 0.3831(13) 0.2895(4) 0.020(3) Uani 1 1 d . U . . .
H114 H 0.5856 0.3781 0.3204 0.024 Uiso 1 1 calc R . . . .
C12 C 0.6180(15) 0.6172(13) 0.3329(4) 0.020(3) Uani 1 1 d . U . . .
H12 H 0.6778 0.5514 0.3427 0.024 Uiso 1 1 calc R . . . .
C13 C 0.5939(14) 0.4988(13) 0.2691(4) 0.020(3) Uani 1 1 d . U . . .
C14 C 0.4932(16) 0.8260(13) 0.1422(4) 0.020(2) Uani 1 1 d . U . . .
C16 C 0.4884(15) 0.8069(13) 0.3558(4) 0.023(3) Uani 1 1 d . U . . .
C15 C 0.6068(13) 0.2739(15) 0.2649(4) 0.025(3) Uani 1 1 d . U . . .
H15 H 0.6099 0.1954 0.2791 0.029 Uiso 1 1 calc R . . . .
C18 C 0.6000(13) 0.5051(13) 0.2229(4) 0.016(2) Uani 1 1 d . U . . .
C20 C 0.6128(14) 0.7507(12) 0.1378(4) 0.020(3) Uani 1 1 d . U . . .
C21 C 0.7050(14) 0.7671(15) 0.1023(4) 0.026(3) Uani 1 1 d . U . . .
H21 H 0.7860 0.7160 0.0995 0.031 Uiso 1 1 calc R . . . .
C22 C 0.6740(16) 0.8582(14) 0.0725(5) 0.025(3) Uani 1 1 d . U . . .
C23 C 0.5547(15) 0.9323(13) 0.0761(4) 0.022(3) Uani 1 1 d . U . . .
H23 H 0.5351 0.9930 0.0542 0.027 Uiso 1 1 calc R . . . .
C24 C 0.4641(15) 0.9214(13) 0.1103(4) 0.020(3) Uani 1 1 d . U . . .
C26 C 0.8815(17) 0.8146(19) 0.0311(6) 0.047(5) Uani 1 1 d . U . . .
H26A H 0.9307 0.8442 0.0052 0.071 Uiso 1 1 calc GR . . . .
H26B H 0.8584 0.7266 0.0274 0.071 Uiso 1 1 calc GR . . . .
H26C H 0.9426 0.8256 0.0573 0.071 Uiso 1 1 calc GR . . . .
C27 C 0.3363(16) 1.0093(14) 0.1143(4) 0.023(3) Uani 1 1 d . U . . .
C28 C 0.1977(15) 0.9382(14) 0.1177(5) 0.026(3) Uani 1 1 d . U . . .
H28A H 0.1970 0.8941 0.1458 0.039 Uiso 1 1 calc GR . . . .
H28B H 0.1888 0.8783 0.0935 0.039 Uiso 1 1 calc GR . . . .
H28C H 0.1183 0.9966 0.1158 0.039 Uiso 1 1 calc GR . . . .
C29 C 0.3222(18) 1.0983(15) 0.0752(5) 0.031(3) Uani 1 1 d . U . . .
H29A H 0.2392 1.1514 0.0787 0.046 Uiso 1 1 calc GR . . . .
H29B H 0.3112 1.0506 0.0480 0.046 Uiso 1 1 calc GR . . . .
H29C H 0.4071 1.1500 0.0741 0.046 Uiso 1 1 calc GR . . . .
C30 C 0.3614(19) 1.0895(14) 0.1553(5) 0.032(3) Uani 1 1 d . U . . .
H30A H 0.3714 1.0359 0.1812 0.047 Uiso 1 1 calc GR . . . .
H30B H 0.2810 1.1455 0.1587 0.047 Uiso 1 1 calc GR . . . .
H30C H 0.4479 1.1383 0.1523 0.047 Uiso 1 1 calc GR . . . .
C31 C 0.0027(9) 0.0333(7) 0.4851(3) 0.086(10) Uani 0.5 1 d . U P A -1
H31 H 0.0940 0.0829 0.4730 0.130 Uiso 0.5 1 d G . P A -1
Cl4 Cl -0.0885(15) -0.0341(9) 0.4392(3) 0.085(4) Uani 0.5 1 d G U P A -1
Cl5 Cl -0.1051(12) 0.1428(8) 0.5119(3) 0.062(3) Uani 0.5 1 d G U P A -1
Cl6 Cl 0.0663(14) -0.0822(10) 0.5223(4) 0.104(5) Uani 0.5 1 d G U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.750(9) . ?
U1 N1 2.567(11) . ?
U1 O3 2.229(8) . ?
U1 O2 1.828(9) . ?
U1 N2 2.529(11) . ?
U1 O4 2.206(9) . ?
U1 O5 2.449(10) . ?
N1 C12 1.298(17) . ?
N1 C13 1.421(17) . ?
O3 C14 1.327(16) . ?
C3 H3 0.9500 . ?
C3 C2 1.375(19) . ?
C3 C4 1.37(2) . ?
C2 C7 1.52(2) . ?
C2 C16 1.441(18) . ?
N2 C19 1.300(17) . ?
N2 C18 1.418(17) . ?
C4 O7 1.378(16) . ?
C4 C5 1.38(2) . ?
O4 C16 1.317(16) . ?
C7 C9 1.54(2) . ?
C7 C8 1.52(2) . ?
C7 C10 1.548(19) . ?
O7 C11 1.414(19) . ?
C6 C5 1.410(19) . ?
C6 C12 1.446(19) . ?
C6 C16 1.418(19) . ?
O6 C22 1.400(17) . ?
O6 C26 1.432(18) . ?
C5 H5 0.9500 . ?
O5 H5A 0.96(3) . ?
O5 H5B 0.95(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C17 H17 0.9500 . ?
C17 C116 1.38(2) . ?
C17 C18 1.395(19) . ?
C19 H19 0.9500 . ?
C19 C20 1.442(18) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C116 H116 0.9500 . ?
C116 C15 1.385(19) . ?
C114 H114 0.9500 . ?
C114 C13 1.393(19) . ?
C114 C15 1.40(2) . ?
C12 H12 0.9500 . ?
C13 C18 1.412(17) . ?
C14 C20 1.403(19) . ?
C14 C24 1.435(18) . ?
C15 H15 0.9500 . ?
C20 C21 1.423(18) . ?
C21 H21 0.9500 . ?
C21 C22 1.36(2) . ?
C22 C23 1.39(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(19) . ?
C24 C27 1.55(2) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.53(2) . ?
C27 C29 1.530(19) . ?
C27 C30 1.53(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 1.0904 . ?
C31 Cl4 1.7764 . ?
C31 Cl5 1.7762 . ?
C31 Cl6 1.7760 . ?

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 N1 97.7(4) . . ?
O1 U1 O3 87.2(4) . . ?
O1 U1 O2 177.6(4) . . ?
O1 U1 N2 90.7(4) . . ?
O1 U1 O4 88.5(4) . . ?
O1 U1 O5 97.7(4) . . ?
O3 U1 N1 133.4(3) . . ?
O3 U1 N2 69.4(3) . . ?
O3 U1 O5 79.7(4) . . ?
O2 U1 N1 84.5(4) . . ?
O2 U1 O3 90.5(4) . . ?
O2 U1 N2 89.3(4) . . ?
O2 U1 O4 93.3(4) . . ?
O2 U1 O5 81.0(4) . . ?
N2 U1 N1 64.2(3) . . ?
O4 U1 N1 68.5(3) . . ?
O4 U1 O3 158.0(3) . . ?
O4 U1 N2 132.2(3) . . ?
O4 U1 O5 79.6(4) . . ?
O5 U1 N1 144.0(4) . . ?
O5 U1 N2 147.5(4) . . ?
C12 N1 U1 129.0(9) . . ?
C12 N1 C13 117.9(12) . . ?
C13 N1 U1 113.1(8) . . ?
C14 O3 U1 133.5(8) . . ?
C2 C3 H3 118.0 . . ?
C4 C3 H3 118.0 . . ?
C4 C3 C2 124.0(13) . . ?
C3 C2 C7 123.5(12) . . ?
C3 C2 C16 116.9(13) . . ?
C16 C2 C7 119.6(12) . . ?
C19 N2 U1 126.1(9) . . ?
C19 N2 C18 118.9(11) . . ?
C18 N2 U1 114.9(8) . . ?
C3 C4 O7 115.0(13) . . ?
C3 C4 C5 120.5(13) . . ?
O7 C4 C5 124.5(14) . . ?
C16 O4 U1 145.0(9) . . ?
C2 C7 C9 111.5(12) . . ?
C2 C7 C10 110.9(12) . . ?
C9 C7 C10 106.1(12) . . ?
C8 C7 C2 110.3(12) . . ?
C8 C7 C9 110.6(12) . . ?
C8 C7 C10 107.3(13) . . ?
C4 O7 C11 117.3(12) . . ?
C5 C6 C12 117.7(13) . . ?
C5 C6 C16 120.8(13) . . ?
C16 C6 C12 121.2(12) . . ?
C22 O6 C26 116.9(11) . . ?
C4 C5 C6 118.7(14) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
U1 O5 H5A 147(9) . . ?
U1 O5 H5B 102(8) . . ?
H5A O5 H5B 106(4) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C116 C17 H17 119.8 . . ?
C116 C17 C18 120.4(13) . . ?
C18 C17 H17 119.8 . . ?
N2 C19 H19 116.8 . . ?
N2 C19 C20 126.5(13) . . ?
C20 C19 H19 116.8 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C11 H11A 109.5 . . ?
O7 C11 H11B 109.5 . . ?
O7 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C17 C116 H116 119.5 . . ?
C17 C116 C15 120.9(15) . . ?
C15 C116 H116 119.5 . . ?
C13 C114 H114 119.6 . . ?
C13 C114 C15 120.8(13) . . ?
C15 C114 H114 119.6 . . ?
N1 C12 C6 127.7(13) . . ?
N1 C12 H12 116.1 . . ?
C6 C12 H12 116.1 . . ?
C114 C13 N1 122.4(12) . . ?
C114 C13 C18 119.2(13) . . ?
C18 C13 N1 117.9(12) . . ?
O3 C14 C20 120.0(12) . . ?
O3 C14 C24 120.7(13) . . ?
C20 C14 C24 119.2(12) . . ?
O4 C16 C2 121.0(12) . . ?
O4 C16 C6 119.9(12) . . ?
C6 C16 C2 119.1(12) . . ?
C116 C15 C114 119.1(15) . . ?
C116 C15 H15 120.4 . . ?
C114 C15 H15 120.4 . . ?
C17 C18 N2 124.0(11) . . ?
C17 C18 C13 119.4(13) . . ?
C13 C18 N2 116.4(12) . . ?
C14 C20 C19 122.1(12) . . ?
C14 C20 C21 121.1(12) . . ?
C21 C20 C19 116.5(12) . . ?
C20 C21 H21 120.9 . . ?
C22 C21 C20 118.2(14) . . ?
C22 C21 H21 120.9 . . ?
C21 C22 O6 124.6(13) . . ?
C21 C22 C23 121.2(13) . . ?
C23 C22 O6 114.2(12) . . ?
C22 C23 H23 118.7 . . ?
C24 C23 C22 122.7(13) . . ?
C24 C23 H23 118.7 . . ?
C14 C24 C27 121.3(12) . . ?
C23 C24 C14 117.6(13) . . ?
C23 C24 C27 121.1(12) . . ?
O6 C26 H26A 109.5 . . ?
O6 C26 H26B 109.5 . . ?
O6 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C24 112.0(12) . . ?
C28 C27 C29 108.3(12) . . ?
C28 C27 C30 109.8(13) . . ?
C29 C27 C24 111.9(12) . . ?
C29 C27 C30 106.7(13) . . ?
C30 C27 C24 108.0(12) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Cl4 C31 H31 107.7 . . ?
Cl5 C31 H31 107.7 . . ?
Cl5 C31 Cl4 111.2 . . ?
Cl6 C31 H31 107.7 . . ?
Cl6 C31 Cl4 111.2 . . ?
Cl6 C31 Cl5 111.2 . . ?

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
O5 H5A O2 0.96(3) 1.76(6) 2.653(13) 154(12) 2
C11 H11B O6 0.98 2.55 3.42(2) 148.1 2_645

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 N1 C12 C6 9(2) . . . . ?
U1 N1 C13 C114 -145.8(11) . . . . ?
U1 N1 C13 C18 26.8(15) . . . . ?
U1 O3 C14 C20 48.0(18) . . . . ?
U1 O3 C14 C24 -134.7(11) . . . . ?
U1 N2 C19 C20 -10.2(19) . . . . ?
U1 N2 C18 C17 146.8(11) . . . . ?
U1 N2 C18 C13 -29.1(14) . . . . ?
U1 O4 C16 C2 148.2(12) . . . . ?
U1 O4 C16 C6 -34(2) . . . . ?
N1 C13 C18 N2 0.9(18) . . . . ?
N1 C13 C18 C17 -175.2(12) . . . . ?
O3 C14 C20 C19 3.5(19) . . . . ?
O3 C14 C20 C21 177.1(12) . . . . ?
O3 C14 C24 C23 -176.0(12) . . . . ?
O3 C14 C24 C27 4(2) . . . . ?
C3 C2 C7 C9 -122.4(15) . . . . ?
C3 C2 C7 C8 114.3(16) . . . . ?
C3 C2 C7 C10 -4(2) . . . . ?
C3 C2 C16 O4 176.9(13) . . . . ?
C3 C2 C16 C6 -1(2) . . . . ?
C3 C4 O7 C11 178.9(14) . . . . ?
C3 C4 C5 C6 1(2) . . . . ?
C2 C3 C4 O7 -177.3(14) . . . . ?
C2 C3 C4 C5 1(2) . . . . ?
N2 C19 C20 C14 -18(2) . . . . ?
N2 C19 C20 C21 168.6(13) . . . . ?
C4 C3 C2 C7 -178.5(14) . . . . ?
C4 C3 C2 C16 -1(2) . . . . ?
C7 C2 C16 O4 -6(2) . . . . ?
C7 C2 C16 C6 176.7(13) . . . . ?
O7 C4 C5 C6 178.9(14) . . . . ?
O6 C22 C23 C24 -179.3(13) . . . . ?
C5 C4 O7 C11 0(2) . . . . ?
C5 C6 C12 N1 -178.2(14) . . . . ?
C5 C6 C16 C2 2(2) . . . . ?
C5 C6 C16 O4 -175.3(13) . . . . ?
C17 C116 C15 C114 1(2) . . . . ?
C19 N2 C18 C17 -30.2(19) . . . . ?
C19 N2 C18 C13 153.9(12) . . . . ?
C19 C20 C21 C22 173.9(13) . . . . ?
C116 C17 C18 N2 -174.9(13) . . . . ?
C116 C17 C18 C13 1(2) . . . . ?
C114 C13 C18 N2 173.8(11) . . . . ?
C114 C13 C18 C17 -2(2) . . . . ?
C12 N1 C13 C114 33.5(19) . . . . ?
C12 N1 C13 C18 -153.9(13) . . . . ?
C12 C6 C5 C4 -176.2(14) . . . . ?
C12 C6 C16 C2 176.1(13) . . . . ?
C12 C6 C16 O4 -2(2) . . . . ?
C13 N1 C12 C6 -170.0(13) . . . . ?
C13 C114 C15 C116 -2.0(19) . . . . ?
C14 C20 C21 C22 0(2) . . . . ?
C14 C24 C27 C28 -55.0(17) . . . . ?
C14 C24 C27 C29 -176.8(13) . . . . ?
C14 C24 C27 C30 66.0(17) . . . . ?
C16 C2 C7 C9 60.2(17) . . . . ?
C16 C2 C7 C8 -63.1(17) . . . . ?
C16 C2 C7 C10 178.2(13) . . . . ?
C16 C6 C5 C4 -2(2) . . . . ?
C16 C6 C12 N1 8(2) . . . . ?
C15 C114 C13 N1 175.4(12) . . . . ?
C15 C114 C13 C18 3(2) . . . . ?
C18 N2 C19 C20 166.4(12) . . . . ?
C18 C17 C116 C15 0(2) . . . . ?
C20 C14 C24 C23 1(2) . . . . ?
C20 C14 C24 C27 -178.1(12) . . . . ?
C20 C21 C22 O6 -179.4(13) . . . . ?
C20 C21 C22 C23 -1(2) . . . . ?
C21 C22 C23 C24 2(2) . . . . ?
C22 C23 C24 C14 -2(2) . . . . ?
C22 C23 C24 C27 177.3(13) . . . . ?
C23 C24 C27 C28 125.4(14) . . . . ?
C23 C24 C27 C29 3.6(19) . . . . ?
C23 C24 C27 C30 -113.6(15) . . . . ?
C24 C14 C20 C19 -173.9(12) . . . . ?
C24 C14 C20 C21 0(2) . . . . ?
C26 O6 C22 C21 -4(2) . . . . ?
C26 O6 C22 C23 177.4(14) . . . . ?

_olex2_date_sample_completion    2015-02-18
_olex2_date_sample_data_collection 2015-02-18
_olex2_date_sample_submission    2015-02-18
_olex2_exptl_crystal_mounting_method 
'MiTeGen dual-thickness MicroMounts using parabar oil'
_olex2_submission_original_sample_id KH_1_40
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5812(12)
2 0.4188(12)

# start Validation Reply Form
_vrf_ABSMU01_kh140_a             
;
PROBLEM: The ratio of given/expected absorption coefficient lies
RESPONSE: This is the value as determined by shelxl.
;
_vrf_PLAT051_kh140_a             
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       5.31 %     
RESPONSE: this is the value as determined by shelxl.
;
_vrf_PLAT420_kh140_a             
;
PROBLEM: D-H Without Acceptor       O5     --  H5B    ...     Please Check 
RESPONSE: The other hydrogen (H5A) on the bound water is pointing at an 
acceptor. Due to the size of the ligand and packing of the structure, 
there is simply nothing else nearby for the other hydrogen to H-bond with.
;
# end Validation Reply Form

