# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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 
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data_1_Ce
_database_code_depnum_ccdc_archive 'CCDC 2238465'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_audit_creation_date             2021-06-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H53.61 Ce Cl N2 O, C4 H10 O'
_chemical_formula_sum            'C50 H63.61 Ce Cl N2 O2'
_chemical_formula_weight         900.21
_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 0.0033 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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5933(2)
_cell_length_b                   13.7861(4)
_cell_length_c                   16.9187(4)
_cell_angle_alpha                78.8260(10)
_cell_angle_beta                 73.7280(10)
_cell_angle_gamma                69.7330(10)
_cell_volume                     2212.12(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.29
_cell_measurement_theta_min      2.81
_shelx_estimated_absorpt_T_max   0.806
_shelx_estimated_absorpt_T_min   0.465
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1145 before and 0.0478 after correction. The Ratio of minimum to maximum transmission is 0.9383. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             937
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            69199
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_min         2.107
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_target            Mo
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17233
_reflns_number_total             20123
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.872
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         20123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.040
_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)+(0.0269P)²+1.8476P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0783
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H014)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C00R(H00R), C011(H011), C012(H012), C014(H014)
3.b Secondary CH2 refined with riding coordinates:
 C00V(H00A,H00B), C013(H01A,H01B), C01C(H01P,H01Q), C01D(H01W,H01X), C01F(H01U,
 H01V), C01G(H01Y,H)
3.c Aromatic/amide H refined with riding coordinates:
 C008(H008), C00C(H00C), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I),
 C00L(H00L), C00N(H00N), C00P(H00P), C00Q(H00Q), C00T(H00T), C00U(H00U),
 C00W(H00W), C00X(H00X), C010(H010), C015(H015), C018(H018), C01B(H01O)
3.d Idealised Me refined as rotating group:
 C00Z(H00D,H00E,H00J), C016(H01C,H01D,H01E), C017(H01F,H01G,H01H), C019(H01I,
 H01J,H01K), C01A(H01L,H01M,H01N), C01E(H01R,H01S,H01T), C01H(H01Z,HA,HB),
 C01I(H01,HC,HD), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,
 H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Ce1 Ce 0.25404(2) 0.83424(2) 0.22431(2) 0.01434(2) Uani 1 1 d . . . . .
Cl1 Cl -0.00400(4) 0.90171(4) 0.30926(3) 0.02676(8) Uani 1 1 d . . . . .
O1 O 0.31906(14) 0.74936(10) 0.35711(8) 0.0255(3) Uani 1 1 d . . . . .
N2 N 0.24162(13) 0.67185(10) 0.19027(8) 0.0160(2) Uani 1 1 d . . . . .
N1 N 0.36080(13) 0.97256(10) 0.21757(8) 0.0166(2) Uani 1 1 d . . . . .
C18 C 0.18433(15) 0.65427(12) 0.13200(9) 0.0157(2) Uani 1 1 d . . . . .
C12 C 0.35360(15) 1.06650(12) 0.16907(10) 0.0174(3) Uani 1 1 d . . . . .
C2 C 0.35530(15) 0.91489(12) 0.04921(9) 0.0170(3) Uani 1 1 d . . . . .
H008 H 0.449485 0.912932 0.032139 0.020 Uiso 1 1 calc R . . . .
C13 C 0.14526(16) 0.73567(12) 0.06946(9) 0.0167(3) Uani 1 1 d . . . . .
C31 C 0.29056(17) 0.58115(12) 0.24498(10) 0.0184(3) Uani 1 1 d . . . . .
C19 C 0.42091(16) 0.95557(13) 0.28712(10) 0.0186(3) Uani 1 1 d . . . . .
C5 C 0.07926(16) 0.92110(12) 0.09576(10) 0.0176(3) Uani 1 1 d . . . . .
H00C H -0.015395 0.924392 0.110412 0.021 Uiso 1 1 calc R . . . .
C1 C 0.25363(15) 1.00402(11) 0.08187(9) 0.0156(2) Uani 1 1 d . . . . .
C7 C 0.29443(15) 1.08853(12) 0.09942(10) 0.0166(3) Uani 1 1 d . . . . .
C6 C 0.11564(15) 1.00661(12) 0.10337(10) 0.0169(3) Uani 1 1 d . . . . .
H00F H 0.045476 1.067141 0.123409 0.020 Uiso 1 1 calc R . . . .
C3 C 0.31930(16) 0.83019(12) 0.04178(9) 0.0174(3) Uani 1 1 d . . . . .
H00G H 0.388997 0.770805 0.019477 0.021 Uiso 1 1 calc R . . . .
C17 C 0.15816(17) 0.56085(12) 0.13095(10) 0.0199(3) Uani 1 1 d . . . . .
H00H H 0.188220 0.502588 0.169215 0.024 Uiso 1 1 calc R . . . .
C11 C 0.39886(17) 1.14494(14) 0.18401(11) 0.0231(3) Uani 1 1 d . . . . .
H00I H 0.444948 1.131679 0.227573 0.028 Uiso 1 1 calc R . . . .
C4 C 0.18009(15) 0.83116(12) 0.06698(9) 0.0158(3) Uani 1 1 d . . . . .
O2 O 0.79234(18) 0.23737(14) 0.28626(14) 0.0527(5) Uani 1 1 d . . . . .
C8 C 0.27417(17) 1.18513(13) 0.05250(11) 0.0212(3) Uani 1 1 d . . . . .
H00L H 0.232199 1.198558 0.007052 0.025 Uiso 1 1 calc R . . . .
C24 C 0.55605(17) 0.88484(13) 0.28380(11) 0.0208(3) Uani 1 1 d . . . . .
C23 C 0.6074(2) 0.85855(15) 0.35502(13) 0.0293(4) Uani 1 1 d . . . . .
H00N H 0.697559 0.810847 0.353557 0.035 Uiso 1 1 calc R . . . .
C20 C 0.34635(18) 1.00552(15) 0.35944(11) 0.0240(3) Uani 1 1 d . . . . .
C14 C 0.07649(19) 0.72598(14) 0.01408(11) 0.0236(3) Uani 1 1 d . . . . .
H00P H 0.049638 0.782478 -0.026251 0.028 Uiso 1 1 calc R . . . .
C33 C 0.4800(2) 0.43281(14) 0.27849(13) 0.0291(4) Uani 1 1 d . . . . .
H00Q H 0.573615 0.390264 0.264430 0.035 Uiso 1 1 calc R . . . .
C37 C 0.04791(19) 0.61180(15) 0.34189(11) 0.0260(3) Uani 1 1 d . . . . .
H00R H 0.026725 0.672665 0.299271 0.031 Uiso 1 1 calc R . . . .
C32 C 0.42910(18) 0.51727(13) 0.22287(11) 0.0225(3) Uani 1 1 d . . . . .
C16 C 0.08925(18) 0.55265(14) 0.07494(11) 0.0234(3) Uani 1 1 d . . . . .
H00T H 0.071207 0.489326 0.076595 0.028 Uiso 1 1 calc R . . . .
C9 C 0.31450(18) 1.26232(13) 0.07120(12) 0.0260(3) Uani 1 1 d . . . . .
H00U H 0.298971 1.328563 0.039637 0.031 Uiso 1 1 calc R . . . .
C46 C 0.4473(2) 0.66484(16) 0.36314(14) 0.0337(4) Uani 1 1 d . . . . .
H00A H 0.528282 0.683431 0.326398 0.040 Uiso 1 1 calc R . . . .
H00B H 0.445132 0.600090 0.347247 0.040 Uiso 1 1 calc R . . . .
C10 C 0.37775(19) 1.24059(14) 0.13680(13) 0.0265(3) Uani 1 1 d . . . . .
H00W H 0.407149 1.292265 0.149589 0.032 Uiso 1 1 calc R . . . .
C34 C 0.3958(2) 0.41054(15) 0.35369(13) 0.0316(4) Uani 1 1 d . . . . .
H00X H 0.432108 0.354047 0.391577 0.038 Uiso 1 1 calc R . . . .
C36 C 0.20245(19) 0.55543(13) 0.31984(11) 0.0228(3) Uani 1 1 d . . . . .
C30 C 0.7008(2) 0.93165(16) 0.14745(13) 0.0308(4) Uani 1 1 d . . . . .
H00D H 0.622571 0.989901 0.133759 0.046 Uiso 1 1 calc GR . . . .
H00E H 0.764123 0.904868 0.096360 0.046 Uiso 1 1 calc GR . . . .
H00J H 0.749929 0.955536 0.177152 0.046 Uiso 1 1 calc GR . . . .
C21 C 0.4018(2) 0.97518(17) 0.42918(12) 0.0320(4) Uani 1 1 d . . . . .
H010 H 0.350919 1.006243 0.478721 0.038 Uiso 1 1 calc R . . . .
C25 C 0.2101(2) 1.09407(16) 0.36304(12) 0.0292(4) Uani 1 1 d . . . . .
H011 H 0.189921 1.109561 0.306804 0.035 Uiso 1 1 calc R . . . .
C28 C 0.64766(17) 0.84525(14) 0.20222(12) 0.0241(3) Uani 1 1 d . . . . .
H012 H 0.589581 0.827471 0.173198 0.029 Uiso 1 1 calc R . . . .
C43 C 0.2456(3) 0.78020(18) 0.44016(12) 0.0350(4) Uani 1 1 d . . . . .
H01A H 0.144653 0.795631 0.448271 0.042 Uiso 1 1 calc R . . . .
H01B H 0.264072 0.842302 0.449387 0.042 Uiso 1 1 calc R . . . .
C40 C 0.52337(19) 0.53823(14) 0.13980(12) 0.0275(4) Uani 1 1 d . . . . .
H014 H 0.468869 0.605755 0.114131 0.033 Uiso 0.61(3) 1 calc R . P A 1
C22 C 0.5295(2) 0.90071(17) 0.42775(13) 0.0343(4) Uani 1 1 d . . . . .
H015 H 0.563540 0.878595 0.476712 0.041 Uiso 1 1 calc R . . . .
C39 C -0.0338(2) 0.53967(19) 0.33982(14) 0.0361(4) Uani 1 1 d . . . . .
H01C H -0.012167 0.521125 0.283412 0.054 Uiso 1 1 calc GR . . . .
H01D H -0.133087 0.575530 0.357144 0.054 Uiso 1 1 calc GR . . . .
H01E H -0.008064 0.476404 0.377605 0.054 Uiso 1 1 calc GR . . . .
C38 C -0.0016(2) 0.65203(18) 0.42663(13) 0.0351(4) Uani 1 1 d . . . . .
H01F H 0.017231 0.593399 0.469458 0.053 Uiso 1 1 calc GR . . . .
H01G H -0.101228 0.688443 0.437012 0.053 Uiso 1 1 calc GR . . . .
H01H H 0.047466 0.700128 0.427914 0.053 Uiso 1 1 calc GR . . . .
C35 C 0.2593(2) 0.47038(15) 0.37354(12) 0.0293(4) Uani 1 1 d . . . . .
H018 H 0.201995 0.453638 0.424987 0.035 Uiso 1 1 calc R . . . .
C27 C 0.2210(2) 1.19389(18) 0.38556(16) 0.0397(5) Uani 1 1 d . . . . .
H01I H 0.238228 1.181095 0.441194 0.060 Uiso 1 1 calc GR . . . .
H01J H 0.134229 1.250423 0.384325 0.060 Uiso 1 1 calc GR . . . .
H01K H 0.297336 1.213428 0.345423 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.7716(2) 0.74897(16) 0.21109(15) 0.0357(5) Uani 1 1 d . . . . .
H01L H 0.837618 0.767499 0.231137 0.054 Uiso 1 1 calc GR . . . .
H01M H 0.816557 0.722283 0.157139 0.054 Uiso 1 1 calc GR . . . .
H01N H 0.740022 0.695348 0.250668 0.054 Uiso 1 1 calc GR . . . .
C15 C 0.04625(19) 0.63466(14) 0.01676(12) 0.0262(3) Uani 1 1 d . . . . .
H01O H -0.002674 0.628751 -0.020410 0.031 Uiso 1 1 calc R . . . .
C45 C 0.4546(3) 0.65076(19) 0.45315(15) 0.0458(6) Uani 1 1 d . . . . .
H01P H 0.499526 0.577069 0.471439 0.055 Uiso 1 1 calc R . . . .
H01Q H 0.505575 0.694173 0.462250 0.055 Uiso 1 1 calc R . . . .
C48 C 0.9143(3) 0.2443(2) 0.23216(19) 0.0542(7) Uani 1 1 d . . . . .
H01W H 0.903573 0.255571 0.174499 0.065 Uiso 1 1 calc R . . . .
H01X H 0.989217 0.178229 0.238584 0.065 Uiso 1 1 calc R . . . .
C26 C 0.0893(2) 1.0656(2) 0.42443(15) 0.0409(5) Uani 1 1 d . . . . .
H01R H 0.081378 1.002745 0.410001 0.061 Uiso 1 1 calc GR . . . .
H01S H 0.003663 1.122960 0.422394 0.061 Uiso 1 1 calc GR . . . .
H01T H 0.105168 1.052594 0.480426 0.061 Uiso 1 1 calc GR . . . .
C44 C 0.3034(3) 0.6867(2) 0.49783(15) 0.0521(7) Uani 1 1 d . . . . .
H01U H 0.258912 0.632444 0.503716 0.063 Uiso 1 1 calc R . . . .
H01V H 0.291974 0.706398 0.553252 0.063 Uiso 1 1 calc R . . . .
C49 C 0.7522(3) 0.1564(2) 0.26267(19) 0.0502(6) Uani 1 1 d . . . . .
H01Y H 0.716044 0.182690 0.211993 0.060 Uiso 1 1 calc R . . . .
H H 0.833761 0.094100 0.251019 0.060 Uiso 1 1 calc R . . . .
C50 C 0.6496(3) 0.1303(2) 0.3282(2) 0.0638(9) Uani 1 1 d . . . . .
H01Z H 0.632033 0.069787 0.316751 0.096 Uiso 1 1 calc GR . . . .
HA H 0.564234 0.189276 0.333806 0.096 Uiso 1 1 calc GR . . . .
HB H 0.681278 0.113743 0.379856 0.096 Uiso 1 1 calc GR . . . .
C47 C 0.9521(3) 0.3307(3) 0.2483(2) 0.0654(9) Uani 1 1 d . . . . .
H01 H 1.041615 0.331714 0.211674 0.098 Uiso 1 1 calc GR . . . .
HC H 0.958422 0.321180 0.306130 0.098 Uiso 1 1 calc GR . . . .
HD H 0.881272 0.396647 0.237800 0.098 Uiso 1 1 calc GR . . . .
C41 C 0.6057(14) 0.5982(10) 0.1555(7) 0.038(2) Uani 0.39(3) 1 d . . P A 2
H1A H 0.658509 0.557264 0.196481 0.057 Uiso 0.39(3) 1 calc GR . P A 2
H1B H 0.543064 0.663780 0.176522 0.057 Uiso 0.39(3) 1 calc GR . P A 2
H1C H 0.669484 0.613054 0.103696 0.057 Uiso 0.39(3) 1 calc GR . P A 2
C42 C 0.5979(9) 0.4391(3) 0.0986(5) 0.053(2) Uani 0.63(2) 1 d . . P A 2
H2A H 0.655337 0.454460 0.044293 0.080 Uiso 0.63(2) 1 calc GR . P A 2
H2B H 0.529918 0.409956 0.091638 0.080 Uiso 0.63(2) 1 calc GR . P A 2
H2C H 0.656633 0.388736 0.133258 0.080 Uiso 0.63(2) 1 calc GR . P A 2
C41b C 0.6560(16) 0.5571(13) 0.1457(4) 0.060(3) Uani 0.61(3) 1 d . . P A 1
H3A H 0.709723 0.571610 0.089839 0.090 Uiso 0.61(3) 1 calc GR . P A 1
H3B H 0.711831 0.495107 0.174031 0.090 Uiso 0.61(3) 1 calc GR . P A 1
H3C H 0.630558 0.616678 0.176914 0.090 Uiso 0.61(3) 1 calc GR . P A 1
C42b C 0.5578(13) 0.4622(17) 0.0791(7) 0.064(4) Uani 0.37(2) 1 d . . P A 1
H5A H 0.621434 0.480646 0.028541 0.096 Uiso 0.37(2) 1 calc GR . P A 1
H5B H 0.472900 0.464086 0.065491 0.096 Uiso 0.37(2) 1 calc GR . P A 1
H5C H 0.601775 0.392133 0.103258 0.096 Uiso 0.37(2) 1 calc GR . 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
Ce1 Cl1 2.6377(4) . ?
Ce1 O1 2.4863(12) . ?
Ce1 N2 2.4713(13) . ?
Ce1 N1 2.5032(13) . ?
Ce1 C2 2.9886(15) . ?
Ce1 C5 3.0501(15) . ?
Ce1 C1 3.0164(14) . ?
Ce1 C6 3.0604(15) . ?
Ce1 C3 2.9769(15) . ?
Ce1 C4 2.9893(15) . ?
O1 C46 1.466(2) . ?
O1 C43 1.466(2) . ?
N2 C18 1.389(2) . ?
N2 C31 1.4354(19) . ?
N1 C12 1.382(2) . ?
N1 C19 1.433(2) . ?
C18 C13 1.419(2) . ?
C18 C17 1.412(2) . ?
C12 C7 1.420(2) . ?
C12 C11 1.413(2) . ?
C2 C1 1.410(2) . ?
C2 C3 1.385(2) . ?
C13 C4 1.476(2) . ?
C13 C14 1.387(2) . ?
C31 C32 1.412(2) . ?
C31 C36 1.412(2) . ?
C19 C24 1.419(2) . ?
C19 C20 1.415(2) . ?
C5 C6 1.399(2) . ?
C5 C4 1.393(2) . ?
C1 C7 1.479(2) . ?
C1 C6 1.393(2) . ?
C7 C8 1.392(2) . ?
C3 C4 1.412(2) . ?
C17 C16 1.389(2) . ?
C11 C10 1.384(3) . ?
O2 C48 1.381(3) . ?
O2 C49 1.477(3) . ?
C8 C9 1.391(3) . ?
C24 C23 1.393(2) . ?
C24 C28 1.523(3) . ?
C23 C22 1.382(3) . ?
C20 C21 1.392(3) . ?
C20 C25 1.529(3) . ?
C14 C15 1.392(3) . ?
C33 C32 1.399(2) . ?
C33 C34 1.382(3) . ?
C37 C36 1.520(3) . ?
C37 C39 1.538(3) . ?
C37 C38 1.524(3) . ?
C32 C40 1.521(3) . ?
C16 C15 1.385(3) . ?
C9 C10 1.385(3) . ?
C46 C45 1.518(3) . ?
C34 C35 1.376(3) . ?
C36 C35 1.403(2) . ?
C30 C28 1.530(3) . ?
C21 C22 1.383(3) . ?
C25 C27 1.546(3) . ?
C25 C26 1.521(3) . ?
C28 C29 1.528(2) . ?
C43 C44 1.513(3) . ?
C40 C41 1.493(11) . ?
C40 C42 1.513(5) . ?
C40 C41b 1.548(9) . ?
C40 C42b 1.493(14) . ?
C45 C44 1.516(4) . ?
C48 C47 1.473(4) . ?
C49 C50 1.407(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
Cl1 Ce1 C2 123.81(3) . . ?
Cl1 Ce1 C5 74.28(3) . . ?
Cl1 Ce1 C1 100.36(3) . . ?
Cl1 Ce1 C6 76.94(3) . . ?
Cl1 Ce1 C3 120.90(3) . . ?
Cl1 Ce1 C4 95.13(3) . . ?
O1 Ce1 Cl1 88.05(3) . . ?
O1 Ce1 N1 91.53(4) . . ?
O1 Ce1 C2 145.56(4) . . ?
O1 Ce1 C5 159.38(4) . . ?
O1 Ce1 C1 150.06(4) . . ?
O1 Ce1 C6 157.82(4) . . ?
O1 Ce1 C3 146.55(4) . . ?
O1 Ce1 C4 152.37(4) . . ?
N2 Ce1 Cl1 97.16(3) . . ?
N2 Ce1 O1 92.64(4) . . ?
N2 Ce1 N1 156.15(4) . . ?
N2 Ce1 C2 95.51(4) . . ?
N2 Ce1 C5 79.41(4) . . ?
N2 Ce1 C1 114.41(4) . . ?
N2 Ce1 C6 105.22(4) . . ?
N2 Ce1 C3 69.07(4) . . ?
N2 Ce1 C4 59.72(4) . . ?
N1 Ce1 Cl1 106.45(3) . . ?
N1 Ce1 C2 68.65(4) . . ?
N1 Ce1 C5 103.45(4) . . ?
N1 Ce1 C1 58.53(4) . . ?
N1 Ce1 C6 77.49(4) . . ?
N1 Ce1 C3 95.22(4) . . ?
N1 Ce1 C4 113.62(4) . . ?
C2 Ce1 C5 54.86(4) . . ?
C2 Ce1 C1 27.15(4) . . ?
C2 Ce1 C6 46.93(4) . . ?
C2 Ce1 C4 47.97(4) . . ?
C5 Ce1 C6 26.46(4) . . ?
C1 Ce1 C5 47.16(4) . . ?
C1 Ce1 C6 26.50(4) . . ?
C3 Ce1 C2 26.84(4) . . ?
C3 Ce1 C5 47.11(4) . . ?
C3 Ce1 C1 47.80(4) . . ?
C3 Ce1 C6 54.87(4) . . ?
C3 Ce1 C4 27.37(4) . . ?
C4 Ce1 C5 26.65(4) . . ?
C4 Ce1 C1 56.11(4) . . ?
C4 Ce1 C6 47.30(4) . . ?
C46 O1 Ce1 124.12(11) . . ?
C46 O1 C43 108.75(15) . . ?
C43 O1 Ce1 126.89(12) . . ?
C18 N2 Ce1 131.20(10) . . ?
C18 N2 C31 113.98(13) . . ?
C31 N2 Ce1 114.54(9) . . ?
C12 N1 Ce1 132.65(10) . . ?
C12 N1 C19 115.87(13) . . ?
C19 N1 Ce1 110.57(9) . . ?
N2 C18 C13 118.85(14) . . ?
N2 C18 C17 124.76(14) . . ?
C17 C18 C13 116.37(14) . . ?
N1 C12 C7 118.74(14) . . ?
N1 C12 C11 124.95(15) . . ?
C11 C12 C7 116.30(15) . . ?
C1 C2 Ce1 77.52(8) . . ?
C3 C2 Ce1 76.11(9) . . ?
C3 C2 C1 120.69(14) . . ?
C18 C13 C4 116.67(13) . . ?
C14 C13 C18 121.45(15) . . ?
C14 C13 C4 121.87(14) . . ?
C32 C31 N2 118.94(14) . . ?
C36 C31 N2 120.99(14) . . ?
C36 C31 C32 120.07(15) . . ?
C24 C19 N1 118.97(14) . . ?
C20 C19 N1 121.19(14) . . ?
C20 C19 C24 119.81(15) . . ?
C6 C5 Ce1 77.18(9) . . ?
C4 C5 Ce1 74.24(8) . . ?
C4 C5 C6 120.83(14) . . ?
C2 C1 Ce1 75.33(8) . . ?
C2 C1 C7 120.30(13) . . ?
C7 C1 Ce1 111.80(9) . . ?
C6 C1 Ce1 78.52(9) . . ?
C6 C1 C2 118.53(14) . . ?
C6 C1 C7 120.96(13) . . ?
C12 C7 C1 115.91(13) . . ?
C8 C7 C12 121.14(15) . . ?
C8 C7 C1 122.94(14) . . ?
C5 C6 Ce1 76.35(9) . . ?
C1 C6 Ce1 74.99(8) . . ?
C1 C6 C5 120.74(14) . . ?
C2 C3 Ce1 77.05(9) . . ?
C2 C3 C4 120.68(14) . . ?
C4 C3 Ce1 76.80(8) . . ?
C16 C17 C18 121.17(15) . . ?
C10 C11 C12 121.66(17) . . ?
C13 C4 Ce1 110.45(9) . . ?
C5 C4 Ce1 79.11(9) . . ?
C5 C4 C13 121.25(14) . . ?
C5 C4 C3 118.42(14) . . ?
C3 C4 Ce1 75.83(9) . . ?
C3 C4 C13 120.11(13) . . ?
C48 O2 C49 108.6(2) . . ?
C9 C8 C7 120.95(16) . . ?
C19 C24 C28 120.56(14) . . ?
C23 C24 C19 118.81(17) . . ?
C23 C24 C28 120.45(16) . . ?
C22 C23 C24 121.08(18) . . ?
C19 C20 C25 122.62(16) . . ?
C21 C20 C19 118.65(17) . . ?
C21 C20 C25 118.70(17) . . ?
C13 C14 C15 120.96(16) . . ?
C34 C33 C32 120.79(18) . . ?
C36 C37 C39 110.27(17) . . ?
C36 C37 C38 113.17(16) . . ?
C38 C37 C39 108.82(16) . . ?
C31 C32 C40 121.30(14) . . ?
C33 C32 C31 119.17(17) . . ?
C33 C32 C40 119.53(16) . . ?
C15 C16 C17 121.51(16) . . ?
C10 C9 C8 118.65(16) . . ?
O1 C46 C45 105.60(19) . . ?
C11 C10 C9 121.15(17) . . ?
C35 C34 C33 119.86(17) . . ?
C31 C36 C37 122.75(14) . . ?
C35 C36 C31 118.18(17) . . ?
C35 C36 C37 118.96(16) . . ?
C22 C21 C20 121.31(19) . . ?
C20 C25 C27 111.12(17) . . ?
C26 C25 C20 112.36(18) . . ?
C26 C25 C27 109.20(17) . . ?
C24 C28 C30 109.54(15) . . ?
C24 C28 C29 114.62(16) . . ?
C29 C28 C30 108.52(16) . . ?
O1 C43 C44 104.15(19) . . ?
C32 C40 C41b 114.6(3) . . ?
C41 C40 C32 106.1(5) . . ?
C41 C40 C42 119.3(7) . . ?
C42 C40 C32 110.5(2) . . ?
C42b C40 C32 115.5(6) . . ?
C42b C40 C41b 110.4(7) . . ?
C23 C22 C21 119.91(17) . . ?
C34 C35 C36 121.77(18) . . ?
C16 C15 C14 118.37(16) . . ?
C44 C45 C46 102.62(18) . . ?
O2 C48 C47 110.6(2) . . ?
C43 C44 C45 101.67(19) . . ?
C50 C49 O2 108.8(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_1_Np
_database_code_depnum_ccdc_archive 'CCDC 2238466'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_audit_creation_date             2021-02-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H54 Cl N2 Np O'
_chemical_formula_sum            'C46 H54 Cl N2 Np O'
_chemical_formula_weight         923.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Np Cl2 K C40 N2 O '
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'
Cl Cl 0.1484 0.1585 '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'
Np Np -11.4937 4.1493 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8086(18)
_cell_length_b                   13.8161(17)
_cell_length_c                   17.097(3)
_cell_angle_alpha                78.952(12)
_cell_angle_beta                 73.607(15)
_cell_angle_gamma                69.594(13)
_cell_volume                     2283.2(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4970
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.9050
_cell_measurement_theta_min      1.9300
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.798
_exptl_absorpt_coefficient_mu    2.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_preparation       'By JM.'
_exptl_crystal_recrystallization_method 'From Et2O at -35C.'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1897
_diffrn_reflns_av_unetI/netI     0.1705
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30922
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.068
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.40 135.60   1.00   50.00    --  -11.10  73.75 118.26  165
  2  ω    -29.40 135.60   1.00   50.00    --  -11.10  73.75 -25.74  165
  3  ω    -29.40 135.60   1.00   50.00    --  -11.10  73.75-169.74  165
  4  ω    -29.40 135.60   1.00   50.00    --  -11.10  73.75  46.26  165
  5  ω    -29.40 135.60   1.00   50.00    --  -11.10  73.75 -97.74  165
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0494140000
_diffrn_orient_matrix_UB_12      -0.0190660000
_diffrn_orient_matrix_UB_13      0.0293981000
_diffrn_orient_matrix_UB_21      0.0409936000
_diffrn_orient_matrix_UB_22      -0.0135733000
_diffrn_orient_matrix_UB_23      0.0287676000
_diffrn_orient_matrix_UB_31      -0.0326291000
_diffrn_orient_matrix_UB_32      0.0498527000
_diffrn_orient_matrix_UB_33      0.0140953000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4961
_reflns_number_total             8223
_reflns_odcompleteness_completeness 97.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8223
_refine_ls_number_restraints     318
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0722
_refine_ls_restrained_S_all      0.988
_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)+(0.0601P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1782
_refine_special_details          
;A disorded Et2O molecule (the solvent of crystallization) was identified in a 
lattice void. The Squeeze command was used through PLATON to generate a solvent 
masked hkl file, and the model was refined against this. Electron density 
correlating to 2x44 electrons over two voids was removed from the P1 unit cell, 
which agrees excellently with a single Et2O (42 electrons) per P-1 unit cell. 

Similarity restraints (SIMU) were applied globally.,SQUEEZE
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 2A
3.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C37(H37), C40(H40)
3.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C23(H23), C22(H22), C21(H21), C34(H34), C35(H35),
  C33(H33)
3.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C18(C13,C14,C15,C16,C17), C23(C22,C21,C20,C19,C24),
 C34(C35,C36,C31,C32,C33)
3.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Np1 Np 0.75568(5) 0.83360(4) 0.72079(3) 0.04782(18) Uani 1 1 d . . . . .
Cl1 Cl 0.5119(3) 0.9063(3) 0.8080(2) 0.0784(10) Uani 1 1 d . . . . .
O1 O 0.8298(10) 0.7449(7) 0.8476(5) 0.080(2) Uani 1 1 d . U . . .
N2 N 0.7355(9) 0.6740(7) 0.6883(6) 0.056(2) Uani 1 1 d . U . . .
N1 N 0.8654(9) 0.9657(7) 0.7201(6) 0.053(2) Uani 1 1 d . U . . .
C14 C 0.6832(7) 0.6546(5) 0.6285(4) 0.049(2) Uani 1 1 d G U . . .
C15 C 0.6575(7) 0.5626(5) 0.6290(4) 0.060(3) Uani 1 1 d G U . . .
H2 H 0.682567 0.505992 0.668874 0.072 Uiso 1 1 calc R U . . .
C16 C 0.5951(8) 0.5536(5) 0.5712(5) 0.066(3) Uani 1 1 d G U . . .
H3 H 0.577497 0.490717 0.571488 0.079 Uiso 1 1 calc R U . . .
C17 C 0.5584(8) 0.6364(6) 0.5128(4) 0.067(3) Uani 1 1 d G U . . .
H4 H 0.515726 0.630233 0.473276 0.080 Uiso 1 1 calc R U . . .
C18 C 0.5841(8) 0.7284(5) 0.5123(4) 0.063(3) Uani 1 1 d G U . . .
H5 H 0.559025 0.785025 0.472449 0.075 Uiso 1 1 calc R U . . .
C13 C 0.6465(7) 0.7375(4) 0.5702(4) 0.049(2) Uani 1 1 d G U . . .
C4 C 0.6835(11) 0.8303(8) 0.5672(6) 0.048(2) Uani 1 1 d . U . . .
C5 C 0.5852(11) 0.9195(8) 0.5971(7) 0.052(2) Uani 1 1 d . U . . .
H8 H 0.492114 0.923675 0.610939 0.062 Uiso 1 1 calc R U . . .
C6 C 0.6217(11) 1.0032(9) 0.6071(7) 0.054(3) Uani 1 1 d . U . . .
H9 H 0.553223 1.063037 0.628575 0.064 Uiso 1 1 calc R U . . .
C1 C 0.7572(11) 0.9997(9) 0.5860(7) 0.052(2) Uani 1 1 d . U . . .
C2 C 0.8558(11) 0.9123(9) 0.5521(6) 0.050(3) Uani 1 1 d . U . . .
H11 H 0.948289 0.910048 0.535062 0.060 Uiso 1 1 calc R U . . .
C3 C 0.8196(11) 0.8290(9) 0.5430(6) 0.053(3) Uani 1 1 d . U . . .
H12 H 0.887854 0.769980 0.520138 0.063 Uiso 1 1 calc R U . . .
C8 C 0.8575(7) 1.0621(4) 0.6695(4) 0.051(2) Uani 1 1 d G U . . .
C7 C 0.7957(7) 1.0832(5) 0.6044(5) 0.052(2) Uani 1 1 d G U . . .
C12 C 0.7770(7) 1.1791(6) 0.5577(4) 0.063(3) Uani 1 1 d G U . . .
H14 H 0.734755 1.193467 0.513202 0.076 Uiso 1 1 calc R U . . .
C11 C 0.8203(8) 1.2539(4) 0.5762(5) 0.072(3) Uani 1 1 d G U . . .
H15 H 0.807577 1.319416 0.544285 0.087 Uiso 1 1 calc R U . . .
C10 C 0.8822(8) 1.2328(5) 0.6413(5) 0.071(3) Uani 1 1 d G U . . .
H16 H 0.911730 1.283923 0.653927 0.085 Uiso 1 1 calc R U . . .
C9 C 0.9008(7) 1.1369(6) 0.6880(4) 0.064(3) Uani 1 1 d G U . . .
H17 H 0.943062 1.122482 0.732489 0.077 Uiso 1 1 calc R U . . .
C35 C 0.7514(8) 0.4706(6) 0.8716(4) 0.070(3) Uani 1 1 d G U . . .
H23 H 0.694105 0.454439 0.922237 0.083 Uiso 1 1 calc R U . . .
C34 C 0.8861(9) 0.4088(5) 0.8505(5) 0.079(3) Uani 1 1 d G U . . .
H22 H 0.920758 0.350414 0.886695 0.094 Uiso 1 1 calc R U . . .
C33 C 0.9700(6) 0.4324(6) 0.7764(5) 0.072(3) Uani 1 1 d G U . . .
H21 H 1.061995 0.390129 0.761993 0.086 Uiso 1 1 calc R U . . .
C32 C 0.9192(7) 0.5177(6) 0.7235(4) 0.066(3) Uani 1 1 d G U . . .
C31 C 0.7846(8) 0.5795(5) 0.7446(4) 0.054(2) Uani 1 1 d G U . . .
C36 C 0.7007(6) 0.5559(6) 0.8186(5) 0.064(3) Uani 1 1 d G U . . .
C40 C 0.5496(14) 0.6121(11) 0.8395(9) 0.082(3) Uani 1 1 d . U . . .
H25 H 0.531236 0.672920 0.797284 0.098 Uiso 1 1 calc R U . . .
C41 C 0.4992(15) 0.6540(11) 0.9227(9) 0.094(4) Uani 1 1 d . U . . .
H26A H 0.500221 0.596195 0.966103 0.141 Uiso 1 1 calc R U . . .
H26B H 0.406330 0.701622 0.927712 0.141 Uiso 1 1 calc R U . . .
H26C H 0.558515 0.691137 0.927747 0.141 Uiso 1 1 calc R U . . .
C42 C 0.4667(15) 0.5452(12) 0.8360(10) 0.098(4) Uani 1 1 d . U . . .
H27A H 0.467298 0.492870 0.883686 0.148 Uiso 1 1 calc R U . . .
H27B H 0.506034 0.510510 0.785677 0.148 Uiso 1 1 calc R U . . .
H27C H 0.373045 0.588839 0.836417 0.148 Uiso 1 1 calc R U . . .
C37 C 1.0107(14) 0.5332(11) 0.6389(9) 0.081(3) Uani 1 1 d . U . . .
H28 H 0.952772 0.587680 0.605148 0.098 Uiso 1 1 calc R U . . .
C38 C 1.1149(17) 0.5725(13) 0.6449(11) 0.117(5) Uani 1 1 d . U . . .
H29A H 1.073241 0.643471 0.660563 0.176 Uiso 1 1 calc R U . . .
H29B H 1.180062 0.572624 0.591771 0.176 Uiso 1 1 calc R U . . .
H29C H 1.162047 0.528085 0.686458 0.176 Uiso 1 1 calc R U . . .
C39 C 1.0778(15) 0.4408(11) 0.5923(9) 0.098(4) Uani 1 1 d . U . . .
H30A H 1.146492 0.389848 0.619166 0.147 Uiso 1 1 calc R U . . .
H30B H 1.121439 0.461807 0.536228 0.147 Uiso 1 1 calc R U . . .
H30C H 1.009804 0.409640 0.590922 0.147 Uiso 1 1 calc R U . . .
C22 C 1.0530(10) 0.8999(7) 0.9170(5) 0.088(3) Uani 1 1 d G U . . .
H34 H 1.095003 0.882738 0.961877 0.105 Uiso 1 1 calc R U . . .
C23 C 1.1241(7) 0.8586(6) 0.8432(6) 0.084(3) Uani 1 1 d G U . . .
H35 H 1.214647 0.813183 0.837596 0.101 Uiso 1 1 calc R U . . .
C24 C 1.0627(8) 0.8838(6) 0.7775(4) 0.069(3) Uani 1 1 d G U . . .
C19 C 0.9303(8) 0.9502(7) 0.7856(5) 0.059(3) Uani 1 1 d G U . . .
C20 C 0.8592(7) 0.9916(6) 0.8595(6) 0.073(3) Uani 1 1 d G U . . .
C21 C 0.9206(9) 0.9664(7) 0.9251(4) 0.082(3) Uani 1 1 d G U . . .
H33 H 0.872014 0.994637 0.975591 0.098 Uiso 1 1 calc R U . . .
C28 C 1.1514(13) 0.8487(11) 0.6953(9) 0.075(3) Uani 1 1 d . U . . .
H37 H 1.092835 0.835241 0.665367 0.091 Uiso 1 1 calc R U . . .
C29 C 1.2700(14) 0.7480(11) 0.7024(10) 0.099(4) Uani 1 1 d . U . . .
H38A H 1.338747 0.762499 0.721339 0.149 Uiso 1 1 calc R U . . .
H38B H 1.310496 0.721437 0.648724 0.149 Uiso 1 1 calc R U . . .
H38C H 1.236190 0.696069 0.741796 0.149 Uiso 1 1 calc R U . . .
C30 C 1.2069(14) 0.9274(11) 0.6455(9) 0.088(4) Uani 1 1 d . U . . .
H39A H 1.260121 0.945589 0.674933 0.132 Uiso 1 1 calc R U . . .
H39B H 1.132664 0.989242 0.633801 0.132 Uiso 1 1 calc R U . . .
H39C H 1.265488 0.900857 0.593928 0.132 Uiso 1 1 calc R U . . .
C25 C 0.7237(15) 1.0778(12) 0.8659(10) 0.091(3) Uani 1 1 d . U . . .
H40 H 0.695733 1.089178 0.813013 0.110 Uiso 1 1 calc R U . . .
C26 C 0.6134(16) 1.0517(13) 0.9345(9) 0.108(5) Uani 1 1 d . U . . .
H41A H 0.592022 0.994182 0.921332 0.162 Uiso 1 1 calc R U . . .
H41B H 0.531869 1.112574 0.941245 0.162 Uiso 1 1 calc R U . . .
H41C H 0.644546 1.031228 0.985584 0.162 Uiso 1 1 calc R U . . .
C27 C 0.7289(16) 1.1824(12) 0.8837(10) 0.105(4) Uani 1 1 d . U . . .
H42A H 0.652598 1.239409 0.868277 0.157 Uiso 1 1 calc R U . . .
H42B H 0.814537 1.193656 0.851827 0.157 Uiso 1 1 calc R U . . .
H42C H 0.722922 1.180134 0.942285 0.157 Uiso 1 1 calc R U . . .
C46 C 0.7622(18) 0.7652(12) 0.9311(9) 0.100(4) Uani 1 1 d . U . . .
H43A H 0.663746 0.776471 0.940473 0.120 Uiso 1 1 calc R U . . .
H43B H 0.774772 0.827761 0.943462 0.120 Uiso 1 1 calc R U . . .
C45 C 0.8238(19) 0.6735(13) 0.9829(10) 0.116(4) Uani 1 1 d . U . . .
H44A H 0.781111 0.618763 0.989473 0.139 Uiso 1 1 calc R U . . .
H44B H 0.816752 0.691540 1.037677 0.139 Uiso 1 1 calc R U . . .
C44 C 0.9665(19) 0.6407(13) 0.9359(10) 0.113(4) Uani 1 1 d . U . . .
H45A H 1.019131 0.678968 0.948966 0.136 Uiso 1 1 calc R U . . .
H45B H 1.009850 0.565329 0.948129 0.136 Uiso 1 1 calc R U . . .
C43 C 0.9585(17) 0.6659(12) 0.8501(9) 0.093(4) Uani 1 1 d . U . . .
H46A H 1.034184 0.691920 0.817381 0.112 Uiso 1 1 calc R U . . .
H46B H 0.964556 0.603379 0.827207 0.112 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
Np1 Cl1 2.586(3) . ?
Np1 O1 2.474(9) . ?
Np1 N2 2.468(10) . ?
Np1 N1 2.496(9) . ?
Np1 C4 2.955(11) . ?
Np1 C5 2.997(11) . ?
Np1 C6 2.973(10) . ?
Np1 C1 2.925(10) . ?
Np1 C2 2.921(10) . ?
Np1 C3 2.928(11) . ?
O1 C46 1.439(16) . ?
O1 C43 1.444(16) . ?
N2 C14 1.405(11) . ?
N2 C31 1.494(10) . ?
N1 C8 1.432(10) . ?
N1 C19 1.428(11) . ?
C14 C15 1.3900 . ?
C14 C13 1.3900 . ?
C15 H2 0.9500 . ?
C15 C16 1.3900 . ?
C16 H3 0.9500 . ?
C16 C17 1.3900 . ?
C17 H4 0.9500 . ?
C17 C18 1.3900 . ?
C18 H5 0.9500 . ?
C18 C13 1.3900 . ?
C13 C4 1.459(12) . ?
C4 C5 1.390(15) . ?
C4 C3 1.406(14) . ?
C5 H8 0.9500 . ?
C5 C6 1.397(15) . ?
C6 H9 0.9500 . ?
C6 C1 1.392(15) . ?
C1 C2 1.397(15) . ?
C1 C7 1.466(13) . ?
C2 H11 0.9500 . ?
C2 C3 1.385(15) . ?
C3 H12 0.9500 . ?
C8 C7 1.3900 . ?
C8 C9 1.3900 . ?
C7 C12 1.3900 . ?
C12 H14 0.9500 . ?
C12 C11 1.3900 . ?
C11 H15 0.9500 . ?
C11 C10 1.3900 . ?
C10 H16 0.9500 . ?
C10 C9 1.3900 . ?
C9 H17 0.9500 . ?
C35 H23 0.9500 . ?
C35 C34 1.3900 . ?
C35 C36 1.3900 . ?
C34 H22 0.9500 . ?
C34 C33 1.3900 . ?
C33 H21 0.9500 . ?
C33 C32 1.3900 . ?
C32 C31 1.3900 . ?
C32 C37 1.528(15) . ?
C31 C36 1.3900 . ?
C36 C40 1.513(15) . ?
C40 H25 1.0000 . ?
C40 C41 1.520(18) . ?
C40 C42 1.514(19) . ?
C41 H26A 0.9800 . ?
C41 H26B 0.9800 . ?
C41 H26C 0.9800 . ?
C42 H27A 0.9800 . ?
C42 H27B 0.9800 . ?
C42 H27C 0.9800 . ?
C37 H28 1.0000 . ?
C37 C38 1.44(2) . ?
C37 C39 1.486(18) . ?
C38 H29A 0.9800 . ?
C38 H29B 0.9800 . ?
C38 H29C 0.9800 . ?
C39 H30A 0.9800 . ?
C39 H30B 0.9800 . ?
C39 H30C 0.9800 . ?
C22 H34 0.9500 . ?
C22 C23 1.3900 . ?
C22 C21 1.3900 . ?
C23 H35 0.9500 . ?
C23 C24 1.3900 . ?
C24 C19 1.3900 . ?
C24 C28 1.517(15) . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C20 C25 1.523(16) . ?
C21 H33 0.9500 . ?
C28 H37 1.0000 . ?
C28 C29 1.541(18) . ?
C28 C30 1.441(17) . ?
C29 H38A 0.9800 . ?
C29 H38B 0.9800 . ?
C29 H38C 0.9800 . ?
C30 H39A 0.9800 . ?
C30 H39B 0.9800 . ?
C30 H39C 0.9800 . ?
C25 H40 1.0000 . ?
C25 C26 1.510(18) . ?
C25 C27 1.556(19) . ?
C26 H41A 0.9800 . ?
C26 H41B 0.9800 . ?
C26 H41C 0.9800 . ?
C27 H42A 0.9800 . ?
C27 H42B 0.9800 . ?
C27 H42C 0.9800 . ?
C46 H43A 0.9900 . ?
C46 H43B 0.9900 . ?
C46 C45 1.465(19) . ?
C45 H44A 0.9900 . ?
C45 H44B 0.9900 . ?
C45 C44 1.48(2) . ?
C44 H45A 0.9900 . ?
C44 H45B 0.9900 . ?
C44 C43 1.461(18) . ?
C43 H46A 0.9900 . ?
C43 H46B 0.9900 . ?

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
Cl1 Np1 C4 97.8(2) . . ?
Cl1 Np1 C5 75.9(2) . . ?
Cl1 Np1 C6 76.9(2) . . ?
Cl1 Np1 C1 100.2(2) . . ?
Cl1 Np1 C2 124.9(2) . . ?
Cl1 Np1 C3 123.4(2) . . ?
O1 Np1 Cl1 89.2(2) . . ?
O1 Np1 N1 88.4(3) . . ?
O1 Np1 C4 151.3(3) . . ?
O1 Np1 C5 161.0(3) . . ?
O1 Np1 C6 159.0(3) . . ?
O1 Np1 C1 148.6(3) . . ?
O1 Np1 C2 142.6(3) . . ?
O1 Np1 C3 143.8(3) . . ?
N2 Np1 Cl1 98.4(2) . . ?
N2 Np1 O1 92.3(3) . . ?
N2 Np1 N1 157.7(3) . . ?
N2 Np1 C4 59.2(3) . . ?
N2 Np1 C5 78.5(3) . . ?
N2 Np1 C6 105.1(3) . . ?
N2 Np1 C1 115.5(3) . . ?
N2 Np1 C2 96.7(3) . . ?
N2 Np1 C3 69.6(3) . . ?
N1 Np1 Cl1 103.8(2) . . ?
N1 Np1 C4 116.5(3) . . ?
N1 Np1 C5 106.5(3) . . ?
N1 Np1 C6 79.9(3) . . ?
N1 Np1 C1 60.4(3) . . ?
N1 Np1 C2 70.3(3) . . ?
N1 Np1 C3 97.3(3) . . ?
C4 Np1 C5 27.0(3) . . ?
C4 Np1 C6 48.2(3) . . ?
C6 Np1 C5 27.1(3) . . ?
C1 Np1 C4 57.3(3) . . ?
C1 Np1 C5 48.3(3) . . ?
C1 Np1 C6 27.3(3) . . ?
C1 Np1 C3 48.7(3) . . ?
C2 Np1 C4 48.9(3) . . ?
C2 Np1 C5 55.9(3) . . ?
C2 Np1 C6 48.0(3) . . ?
C2 Np1 C1 27.7(3) . . ?
C2 Np1 C3 27.4(3) . . ?
C3 Np1 C4 27.6(3) . . ?
C3 Np1 C5 47.7(3) . . ?
C3 Np1 C6 55.9(3) . . ?
C46 O1 Np1 128.4(9) . . ?
C46 O1 C43 106.5(11) . . ?
C43 O1 Np1 124.9(8) . . ?
C14 N2 Np1 132.6(6) . . ?
C14 N2 C31 113.2(8) . . ?
C31 N2 Np1 114.2(6) . . ?
C8 N1 Np1 128.8(6) . . ?
C19 N1 Np1 115.8(6) . . ?
C19 N1 C8 114.8(8) . . ?
C15 C14 N2 124.0(6) . . ?
C15 C14 C13 120.0 . . ?
C13 C14 N2 115.8(6) . . ?
C14 C15 H2 120.0 . . ?
C14 C15 C16 120.0 . . ?
C16 C15 H2 120.0 . . ?
C15 C16 H3 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 H3 120.0 . . ?
C16 C17 H4 120.0 . . ?
C16 C17 C18 120.0 . . ?
C18 C17 H4 120.0 . . ?
C17 C18 H5 120.0 . . ?
C13 C18 C17 120.0 . . ?
C13 C18 H5 120.0 . . ?
C14 C13 C4 118.9(6) . . ?
C18 C13 C14 120.0 . . ?
C18 C13 C4 121.0(6) . . ?
C13 C4 Np1 110.7(6) . . ?
C5 C4 Np1 78.2(7) . . ?
C5 C4 C13 120.0(10) . . ?
C5 C4 C3 118.1(11) . . ?
C3 C4 Np1 75.1(6) . . ?
C3 C4 C13 121.5(10) . . ?
Np1 C5 H8 121.3 . . ?
C4 C5 Np1 74.8(6) . . ?
C4 C5 H8 119.6 . . ?
C4 C5 C6 120.8(11) . . ?
C6 C5 Np1 75.5(6) . . ?
C6 C5 H8 119.6 . . ?
Np1 C6 H9 119.4 . . ?
C5 C6 Np1 77.4(6) . . ?
C5 C6 H9 119.6 . . ?
C1 C6 Np1 74.4(6) . . ?
C1 C6 C5 120.7(11) . . ?
C1 C6 H9 119.6 . . ?
C6 C1 Np1 78.3(6) . . ?
C6 C1 C2 118.7(11) . . ?
C6 C1 C7 120.2(10) . . ?
C2 C1 Np1 76.0(6) . . ?
C2 C1 C7 120.9(10) . . ?
C7 C1 Np1 112.3(6) . . ?
Np1 C2 H11 118.1 . . ?
C1 C2 Np1 76.3(6) . . ?
C1 C2 H11 119.8 . . ?
C3 C2 Np1 76.6(6) . . ?
C3 C2 C1 120.4(10) . . ?
C3 C2 H11 119.8 . . ?
Np1 C3 H12 118.1 . . ?
C4 C3 Np1 77.2(6) . . ?
C4 C3 H12 119.4 . . ?
C2 C3 Np1 76.0(6) . . ?
C2 C3 C4 121.1(11) . . ?
C2 C3 H12 119.4 . . ?
C7 C8 N1 118.4(6) . . ?
C7 C8 C9 120.0 . . ?
C9 C8 N1 121.4(6) . . ?
C8 C7 C1 117.4(6) . . ?
C8 C7 C12 120.0 . . ?
C12 C7 C1 122.6(6) . . ?
C7 C12 H14 120.0 . . ?
C7 C12 C11 120.0 . . ?
C11 C12 H14 120.0 . . ?
C12 C11 H15 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H15 120.0 . . ?
C11 C10 H16 120.0 . . ?
C11 C10 C9 120.0 . . ?
C9 C10 H16 120.0 . . ?
C8 C9 H17 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H17 120.0 . . ?
C34 C35 H23 120.0 . . ?
C34 C35 C36 120.0 . . ?
C36 C35 H23 120.0 . . ?
C35 C34 H22 120.0 . . ?
C35 C34 C33 120.0 . . ?
C33 C34 H22 120.0 . . ?
C34 C33 H21 120.0 . . ?
C34 C33 C32 120.0 . . ?
C32 C33 H21 120.0 . . ?
C33 C32 C37 117.8(8) . . ?
C31 C32 C33 120.0 . . ?
C31 C32 C37 121.8(8) . . ?
C32 C31 N2 118.6(6) . . ?
C32 C31 C36 120.0 . . ?
C36 C31 N2 121.4(6) . . ?
C35 C36 C40 117.6(8) . . ?
C31 C36 C35 120.0 . . ?
C31 C36 C40 121.9(8) . . ?
C36 C40 H25 107.3 . . ?
C36 C40 C41 113.3(12) . . ?
C36 C40 C42 112.5(12) . . ?
C41 C40 H25 107.3 . . ?
C42 C40 H25 107.3 . . ?
C42 C40 C41 108.9(12) . . ?
C40 C41 H26A 109.5 . . ?
C40 C41 H26B 109.5 . . ?
C40 C41 H26C 109.5 . . ?
H26A C41 H26B 109.5 . . ?
H26A C41 H26C 109.5 . . ?
H26B C41 H26C 109.5 . . ?
C40 C42 H27A 109.5 . . ?
C40 C42 H27B 109.5 . . ?
C40 C42 H27C 109.5 . . ?
H27A C42 H27B 109.5 . . ?
H27A C42 H27C 109.5 . . ?
H27B C42 H27C 109.5 . . ?
C32 C37 H28 107.2 . . ?
C38 C37 C32 110.5(13) . . ?
C38 C37 H28 107.2 . . ?
C38 C37 C39 108.0(13) . . ?
C39 C37 C32 116.4(11) . . ?
C39 C37 H28 107.2 . . ?
C37 C38 H29A 109.5 . . ?
C37 C38 H29B 109.5 . . ?
C37 C38 H29C 109.5 . . ?
H29A C38 H29B 109.5 . . ?
H29A C38 H29C 109.5 . . ?
H29B C38 H29C 109.5 . . ?
C37 C39 H30A 109.5 . . ?
C37 C39 H30B 109.5 . . ?
C37 C39 H30C 109.5 . . ?
H30A C39 H30B 109.5 . . ?
H30A C39 H30C 109.5 . . ?
H30B C39 H30C 109.5 . . ?
C23 C22 H34 120.0 . . ?
C23 C22 C21 120.0 . . ?
C21 C22 H34 120.0 . . ?
C22 C23 H35 120.0 . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H35 120.0 . . ?
C23 C24 C28 117.4(8) . . ?
C19 C24 C23 120.0 . . ?
C19 C24 C28 122.0(8) . . ?
C24 C19 N1 118.5(7) . . ?
C24 C19 C20 120.0 . . ?
C20 C19 N1 121.2(7) . . ?
C19 C20 C25 120.9(8) . . ?
C21 C20 C19 120.0 . . ?
C21 C20 C25 118.3(8) . . ?
C22 C21 H33 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H33 120.0 . . ?
C24 C28 H37 107.6 . . ?
C24 C28 C29 113.7(12) . . ?
C29 C28 H37 107.6 . . ?
C30 C28 C24 112.2(12) . . ?
C30 C28 H37 107.6 . . ?
C30 C28 C29 108.0(12) . . ?
C28 C29 H38A 109.5 . . ?
C28 C29 H38B 109.5 . . ?
C28 C29 H38C 109.5 . . ?
H38A C29 H38B 109.5 . . ?
H38A C29 H38C 109.5 . . ?
H38B C29 H38C 109.5 . . ?
C28 C30 H39A 109.5 . . ?
C28 C30 H39B 109.5 . . ?
C28 C30 H39C 109.5 . . ?
H39A C30 H39B 109.5 . . ?
H39A C30 H39C 109.5 . . ?
H39B C30 H39C 109.5 . . ?
C20 C25 H40 108.6 . . ?
C20 C25 C27 113.2(12) . . ?
C26 C25 C20 112.3(13) . . ?
C26 C25 H40 108.6 . . ?
C26 C25 C27 105.3(12) . . ?
C27 C25 H40 108.6 . . ?
C25 C26 H41A 109.5 . . ?
C25 C26 H41B 109.5 . . ?
C25 C26 H41C 109.5 . . ?
H41A C26 H41B 109.5 . . ?
H41A C26 H41C 109.5 . . ?
H41B C26 H41C 109.5 . . ?
C25 C27 H42A 109.5 . . ?
C25 C27 H42B 109.5 . . ?
C25 C27 H42C 109.5 . . ?
H42A C27 H42B 109.5 . . ?
H42A C27 H42C 109.5 . . ?
H42B C27 H42C 109.5 . . ?
O1 C46 H43A 110.4 . . ?
O1 C46 H43B 110.4 . . ?
O1 C46 C45 106.5(13) . . ?
H43A C46 H43B 108.6 . . ?
C45 C46 H43A 110.4 . . ?
C45 C46 H43B 110.4 . . ?
C46 C45 H44A 111.3 . . ?
C46 C45 H44B 111.3 . . ?
C46 C45 C44 102.1(14) . . ?
H44A C45 H44B 109.2 . . ?
C44 C45 H44A 111.3 . . ?
C44 C45 H44B 111.3 . . ?
C45 C44 H45A 110.8 . . ?
C45 C44 H45B 110.8 . . ?
H45A C44 H45B 108.9 . . ?
C43 C44 C45 104.6(14) . . ?
C43 C44 H45A 110.8 . . ?
C43 C44 H45B 110.8 . . ?
O1 C43 C44 107.3(13) . . ?
O1 C43 H46A 110.3 . . ?
O1 C43 H46B 110.3 . . ?
C44 C43 H46A 110.3 . . ?
C44 C43 H46B 110.3 . . ?
H46A C43 H46B 108.5 . . ?

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
Np1 O1 C46 C45 162.9(10) . . . . ?
Np1 O1 C43 C44 175.3(10) . . . . ?
Np1 N2 C14 C15 -167.5(5) . . . . ?
Np1 N2 C14 C13 7.3(10) . . . . ?
Np1 N2 C31 C32 -91.6(6) . . . . ?
Np1 N2 C31 C36 85.0(7) . . . . ?
Np1 N1 C8 C7 -8.9(9) . . . . ?
Np1 N1 C8 C9 166.2(4) . . . . ?
Np1 N1 C19 C24 84.5(7) . . . . ?
Np1 N1 C19 C20 -88.8(7) . . . . ?
Np1 C4 C5 C6 62.3(10) . . . . ?
Np1 C4 C3 C2 -64.8(10) . . . . ?
Np1 C5 C6 C1 63.1(10) . . . . ?
Np1 C6 C1 C2 66.7(9) . . . . ?
Np1 C6 C1 C7 -109.1(9) . . . . ?
Np1 C1 C2 C3 65.2(10) . . . . ?
Np1 C1 C7 C8 15.9(8) . . . . ?
Np1 C1 C7 C12 -166.5(4) . . . . ?
Np1 C2 C3 C4 65.4(9) . . . . ?
O1 C46 C45 C44 34.5(19) . . . . ?
N2 C14 C15 C16 174.6(8) . . . . ?
N2 C14 C13 C18 -175.0(7) . . . . ?
N2 C14 C13 C4 9.4(8) . . . . ?
N2 C31 C36 C35 -176.6(8) . . . . ?
N2 C31 C36 C40 11.4(10) . . . . ?
N1 C8 C7 C1 -7.2(8) . . . . ?
N1 C8 C7 C12 175.2(7) . . . . ?
N1 C8 C9 C10 -175.1(8) . . . . ?
N1 C19 C20 C21 173.2(9) . . . . ?
N1 C19 C20 C25 -17.0(11) . . . . ?
C14 N2 C31 C32 90.1(8) . . . . ?
C14 N2 C31 C36 -93.3(8) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C14 C13 C4 Np1 -17.0(8) . . . . ?
C14 C13 C4 C5 -105.0(10) . . . . ?
C14 C13 C4 C3 67.8(11) . . . . ?
C15 C14 C13 C18 0.0 . . . . ?
C15 C14 C13 C4 -175.6(8) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C16 C17 C18 C13 0.0 . . . . ?
C17 C18 C13 C14 0.0 . . . . ?
C17 C18 C13 C4 175.5(8) . . . . ?
C18 C13 C4 Np1 167.5(4) . . . . ?
C18 C13 C4 C5 79.4(11) . . . . ?
C18 C13 C4 C3 -107.7(10) . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C13 C4 C5 Np1 107.2(9) . . . . ?
C13 C4 C5 C6 169.6(9) . . . . ?
C13 C4 C3 Np1 -105.4(9) . . . . ?
C13 C4 C3 C2 -170.2(9) . . . . ?
C4 C5 C6 Np1 -62.0(10) . . . . ?
C4 C5 C6 C1 1.1(17) . . . . ?
C5 C4 C3 Np1 67.6(9) . . . . ?
C5 C4 C3 C2 2.8(16) . . . . ?
C5 C6 C1 Np1 -64.7(10) . . . . ?
C5 C6 C1 C2 2.1(16) . . . . ?
C5 C6 C1 C7 -173.8(10) . . . . ?
C6 C1 C2 Np1 -68.0(9) . . . . ?
C6 C1 C2 C3 -2.8(16) . . . . ?
C6 C1 C7 C8 105.0(10) . . . . ?
C6 C1 C7 C12 -77.4(11) . . . . ?
C1 C2 C3 Np1 -65.1(10) . . . . ?
C1 C2 C3 C4 0.3(17) . . . . ?
C1 C7 C12 C11 -177.5(8) . . . . ?
C2 C1 C7 C8 -70.7(11) . . . . ?
C2 C1 C7 C12 106.8(10) . . . . ?
C3 C4 C5 Np1 -65.9(9) . . . . ?
C3 C4 C5 C6 -3.5(16) . . . . ?
C8 N1 C19 C24 -103.3(8) . . . . ?
C8 N1 C19 C20 83.4(9) . . . . ?
C8 C7 C12 C11 0.0 . . . . ?
C7 C1 C2 Np1 107.9(9) . . . . ?
C7 C1 C2 C3 173.1(9) . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C7 C12 C11 C10 0.0 . . . . ?
C12 C11 C10 C9 0.0 . . . . ?
C11 C10 C9 C8 0.0 . . . . ?
C9 C8 C7 C1 177.6(8) . . . . ?
C9 C8 C7 C12 0.0 . . . . ?
C35 C34 C33 C32 0.0 . . . . ?
C35 C36 C40 C41 58.9(13) . . . . ?
C35 C36 C40 C42 -65.2(13) . . . . ?
C34 C35 C36 C31 0.0 . . . . ?
C34 C35 C36 C40 172.3(9) . . . . ?
C34 C33 C32 C31 0.0 . . . . ?
C34 C33 C32 C37 -173.3(9) . . . . ?
C33 C32 C31 N2 176.7(8) . . . . ?
C33 C32 C31 C36 0.0 . . . . ?
C33 C32 C37 C38 -75.6(13) . . . . ?
C33 C32 C37 C39 48.1(16) . . . . ?
C32 C31 C36 C35 0.0 . . . . ?
C32 C31 C36 C40 -172.0(9) . . . . ?
C31 N2 C14 C15 10.4(10) . . . . ?
C31 N2 C14 C13 -174.8(6) . . . . ?
C31 C32 C37 C38 111.3(12) . . . . ?
C31 C32 C37 C39 -125.0(12) . . . . ?
C31 C36 C40 C41 -129.0(10) . . . . ?
C31 C36 C40 C42 107.0(11) . . . . ?
C36 C35 C34 C33 0.0 . . . . ?
C37 C32 C31 N2 -10.3(10) . . . . ?
C37 C32 C31 C36 173.0(10) . . . . ?
C22 C23 C24 C19 0.0 . . . . ?
C22 C23 C24 C28 171.6(9) . . . . ?
C23 C22 C21 C20 0.0 . . . . ?
C23 C24 C19 N1 -173.4(8) . . . . ?
C23 C24 C19 C20 0.0 . . . . ?
C23 C24 C28 C29 29.8(14) . . . . ?
C23 C24 C28 C30 -93.1(12) . . . . ?
C24 C19 C20 C21 0.0 . . . . ?
C24 C19 C20 C25 169.8(10) . . . . ?
C19 N1 C8 C7 -179.9(6) . . . . ?
C19 N1 C8 C9 -4.8(10) . . . . ?
C19 C24 C28 C29 -158.8(9) . . . . ?
C19 C24 C28 C30 78.3(13) . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C19 C20 C25 C26 127.0(11) . . . . ?
C19 C20 C25 C27 -113.8(12) . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C21 C20 C25 C26 -63.0(14) . . . . ?
C21 C20 C25 C27 56.1(14) . . . . ?
C28 C24 C19 N1 15.4(10) . . . . ?
C28 C24 C19 C20 -171.2(10) . . . . ?
C25 C20 C21 C22 -170.1(10) . . . . ?
C46 O1 C43 C44 -0.6(17) . . . . ?
C46 C45 C44 C43 -34.2(19) . . . . ?
C45 C44 C43 O1 22.0(18) . . . . ?
C43 O1 C46 C45 -21.5(17) . . . . ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  ?
# end Validation Reply Form
# SQUEEZE RESULTS (Version = 211220)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.309 0.238 0.774 202 44 ' '
2 0.691 0.762 0.226 202 44 ' '

_platon_squeeze_void_probe_radius 1.20
_LANL_internal_archive_date      ?
_LANL_internal_coll_client       JM/LMS/AJG
_LANL_internal_coll_date         12/17/20
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_frame_time   50s
_LANL_internal_coll_frame_width  1.0
_LANL_internal_coll_name         ms0495
_LANL_internal_coll_type         custom
_LANL_internal_coll_user         CAPG
_LANL_internal_LA-UR             ?
_LANL_internal_process_date      12/18/20
_LANL_internal_process_user      CAPG
_LANL_internal_refinement_date   2/24/21
_LANL_internal_refinement_user   CAPG
_LANL_internal_solution_date     12/18/20
_LANL_internal_solution_user     CAPG
_LANL_internal_validation_date   ?
_LANL_internal_validation_user   ?
_olex2_exptl_crystal_mounting_method 
'From NVH oil, mounted into a quartz capillary that was sealed at both ends with capillary wax. The outside was then coated with Tough As Nails clear nail varnish to provide shatter resistance.'
_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 3.473
_oxdiff_exptl_absorpt_empirical_full_min 0.366
_vrf_PLAT020_1_Np                
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.190 Report
RESPONSE: 
The diffraction was extremely weak and marred by absorption issues due to local
rules which dictate the containment method for crystals. There is no significant
diffraction beyond 1.5A. Numerous attempts were made to mount the crystals in 
different oils (Paratone, NVH, Krytox), and the was the only crystal which
survived the mounting and sealing process. The bulk characterisation data 
however supports the structure depicted here.
;
_vrf_PLAT973_1_Np                
;
PROBLEM: Check Calcd Positive Resid. Density on       Np1       1.63 eA-3  
RESPONSE: 
The diffraction was extremely weak and marred by absorption issues due to local
rules which dictate the containment method for crystals. There is no significant
diffraction beyond 1.5A. 

The location of the residual density does not correspond to any chemically 
sensible species, and there is no significant non-merohedral twinning apparent
in the raw data. This artefact is therefore attributed to the issues outlined
above - very weak data and absorption correction issues which could not be 
satisfactorally dealt with.
;
# start Validation Reply Form
_vrf_RINTA01_1_Np                
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: 
The diffraction was extremely weak and marred by absorption issues due to local
rules which dictate the containment method for crystals. There is no significant
diffraction beyond 1.5A. Numerous attempts were made to mount the crystals in 
different oils (Paratone, NVH, Krytox), and the was the only crystal which
survived the mounting and sealing process. The bulk characterisation data 
however supports the structure depicted here.
;
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_3_Np
_database_code_depnum_ccdc_archive 'CCDC 2238471'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
# end Validation Reply Form
_audit_creation_date             2022-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H54 I N2 Np O, C5 H12'
_chemical_formula_sum            'C51 H66 I N2 Np O'
_chemical_formula_weight         1086.95
_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 0.0033 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'
I I -0.4742 1.8119 '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'
Np Np -11.4937 4.1493 '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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.8802(7)
_cell_length_b                   15.5249(8)
_cell_length_c                   22.0162(12)
_cell_angle_alpha                90
_cell_angle_beta                 107.630(3)
_cell_angle_gamma                90
_cell_volume                     4521.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   0.464
_shelx_estimated_absorpt_T_min   0.196
_exptl_absorpt_coefficient_mu    3.019
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1768 before and 0.0663 after correction. The Ratio of minimum to maximum transmission is 0.6020. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear brownish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_unetI/netI     0.1039
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27035
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.032
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5501
_reflns_number_total             7780
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.715
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.00060(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   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7780
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0612
_refine_ls_restrained_S_all      1.028
_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)+(0.0385P)²+30.2516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1245
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C00D) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
3.a Ternary CH refined with riding coordinates:
 C00P(H00P), C00T(H00T), C00X(H00X), C018(H018)
3.b Secondary CH2 refined with riding coordinates:
 C00E(H00B,H00D), C00J(H00E,H00F), C00K(H00I,H00J), C016(H01J,H01K), C01I(H0AA,
 HD), C01J(H1AA,HE), C01K(H2AA,HF)
3.c Aromatic/amide H refined with riding coordinates:
 C006(H006), C008(H008), C009(H009), C00A(H00A), C00C(H00C), C00G(H00G),
 C00H(H00H), C00M(H00M), C00Q(H00Q), C00U(H00U), C00W(H00W), C010(H010),
 C012(H012), C013(H013), C017(H017), C019(H019), C01B(H01O), C01C(H01P)
3.d Idealised Me refined as rotating group:
 C00S(H00K,H00L,H00N), C011(H01A,H01B,H01C), C014(H01D,H01E,H01F), C015(H01G,
 H01H,H01I), C01A(H01L,H01M,H01N), C01D(H01Z,H,HA), C01E(H01Q,H01R,H01S),
 C01F(H01T,H01U,H01V), C01G(H01,HB,HC), C01H(H01W,H01X,H01Y)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Np1 Np 0.35586(3) 0.29542(2) 0.60822(2) 0.01615(13) Uani 1 1 d . . . . .
I1 I 0.31942(5) 0.33070(4) 0.73478(3) 0.02558(19) Uani 1 1 d . . . . .
O1 O 0.4210(5) 0.1499(4) 0.6456(3) 0.0205(15) Uani 1 1 d . . . . .
N2 N 0.1974(5) 0.2278(5) 0.5446(4) 0.0172(18) Uani 1 1 d . . . . .
C1 C 0.3915(7) 0.4712(5) 0.5795(4) 0.014(2) Uani 1 1 d . . . . .
C5 C 0.2213(7) 0.4479(6) 0.5836(5) 0.022(2) Uani 1 1 d . . . . .
H006 H 0.171516 0.455719 0.604681 0.026 Uiso 1 1 calc R . . . .
N1 N 0.5334(6) 0.3444(5) 0.6275(4) 0.0181(18) Uani 1 1 d . . . . .
C3 C 0.2695(7) 0.3966(6) 0.4940(5) 0.019(2) Uani 1 1 d . . . . .
H008 H 0.252635 0.368187 0.453931 0.023 Uiso 1 1 calc R . . . .
C6 C 0.3192(7) 0.4818(6) 0.6100(5) 0.021(2) Uani 1 1 d . . . . .
H009 H 0.335417 0.512260 0.649187 0.025 Uiso 1 1 calc R . . . .
C9 C 0.6717(7) 0.4524(6) 0.6485(5) 0.020(2) Uani 1 1 d . . . . .
H00A H 0.722447 0.409076 0.658037 0.025 Uiso 1 1 calc R . . . .
C4 C 0.1980(7) 0.4029(6) 0.5264(5) 0.021(2) Uani 1 1 d . . . . .
C12 C 0.5289(7) 0.5816(6) 0.6160(4) 0.019(2) Uani 1 1 d . . . . .
H00C H 0.479225 0.625700 0.604680 0.023 Uiso 1 1 calc R . . . .
C8 C 0.5685(7) 0.4280(6) 0.6282(4) 0.016(2) Uani 1 1 d . U . . .
C46 C 0.3966(7) 0.1024(6) 0.6961(5) 0.026(2) Uani 1 1 d . . . . .
H00B H 0.328936 0.075499 0.680195 0.031 Uiso 1 1 calc R . . . .
H00D H 0.398278 0.140578 0.732400 0.031 Uiso 1 1 calc R . . . .
C7 C 0.4996(7) 0.4972(6) 0.6088(5) 0.020(2) Uani 1 1 d . . . . .
C2 C 0.3650(7) 0.4313(6) 0.5195(4) 0.018(2) Uani 1 1 d . . . . .
H00G H 0.412643 0.428211 0.496449 0.021 Uiso 1 1 calc R . . . .
C11 C 0.6300(8) 0.6034(6) 0.6397(5) 0.024(2) Uani 1 1 d . . . . .
H00H H 0.650469 0.661988 0.645568 0.029 Uiso 1 1 calc R . . . .
C14 C 0.1065(7) 0.2653(6) 0.5093(5) 0.022(2) Uani 1 1 d . . . . .
C45 C 0.4783(8) 0.0348(6) 0.7154(5) 0.026(2) Uani 1 1 d . . . . .
H00E H 0.457054 -0.014468 0.736914 0.031 Uiso 1 1 calc R . . . .
H00F H 0.542017 0.059001 0.743766 0.031 Uiso 1 1 calc R . . . .
C43 C 0.4778(7) 0.0944(6) 0.6161(5) 0.021(2) Uani 1 1 d . . . . .
H00I H 0.544945 0.119674 0.620197 0.026 Uiso 1 1 calc R . . . .
H00J H 0.441211 0.086570 0.570306 0.026 Uiso 1 1 calc R . . . .
C19 C 0.6115(7) 0.2804(6) 0.6449(5) 0.017(2) Uani 1 1 d . . . . .
C15 C 0.0179(7) 0.2186(6) 0.4786(5) 0.023(2) Uani 1 1 d . . . . .
H00M H 0.018896 0.157542 0.481385 0.028 Uiso 1 1 calc R . . . .
C24 C 0.6547(7) 0.2494(6) 0.5995(5) 0.020(2) Uani 1 1 d . . . . .
C31 C 0.1971(7) 0.1356(6) 0.5450(5) 0.020(2) Uani 1 1 d . . . . .
C28 C 0.6243(7) 0.2822(6) 0.5312(4) 0.020(2) Uani 1 1 d . . . . .
H00P H 0.581462 0.334446 0.529642 0.025 Uiso 1 1 calc R . . . .
C22 C 0.7539(7) 0.1489(6) 0.6768(5) 0.024(2) Uani 1 1 d . . . . .
H00Q H 0.799369 0.101605 0.686942 0.028 Uiso 1 1 calc R . . . .
C32 C 0.2394(7) 0.0899(6) 0.5046(5) 0.025(2) Uani 1 1 d . . . . .
C39 C 0.1982(9) 0.1710(8) 0.3995(6) 0.043(3) Uani 1 1 d . . . . .
H00K H 0.155138 0.123196 0.378017 0.064 Uiso 1 1 calc GR . . . .
H00L H 0.229428 0.198139 0.369876 0.064 Uiso 1 1 calc GR . . . .
H00N H 0.157052 0.213614 0.413271 0.064 Uiso 1 1 calc GR . . . .
C37 C 0.2810(8) 0.1368(7) 0.4577(5) 0.032(3) Uani 1 1 d . . . . .
H00T H 0.320427 0.187462 0.480318 0.038 Uiso 1 1 calc R . . . .
C23 C 0.7254(7) 0.1821(6) 0.6166(5) 0.022(2) Uani 1 1 d . . . . .
H00U H 0.753875 0.159374 0.585783 0.026 Uiso 1 1 calc R . . . .
C36 C 0.1498(7) 0.0910(6) 0.5852(5) 0.028(3) Uani 1 1 d . . . . .
C10 C 0.6999(7) 0.5382(6) 0.6546(5) 0.027(3) Uani 1 1 d . . . . .
H00W H 0.769692 0.552417 0.669531 0.032 Uiso 1 1 calc R . . . .
C40 C 0.0964(8) 0.1356(8) 0.6264(5) 0.035(3) Uani 1 1 d . . . . .
H00X H 0.099901 0.199194 0.620188 0.042 Uiso 1 1 calc R . . . .
C13 C 0.0997(7) 0.3553(6) 0.5003(5) 0.022(2) Uani 1 1 d . . . . .
C20 C 0.6482(7) 0.2507(7) 0.7091(5) 0.024(2) Uani 1 1 d . . . . .
C35 C 0.1522(8) 0.0009(7) 0.5834(6) 0.036(3) Uani 1 1 d . . . . .
H010 H 0.120845 -0.030791 0.609169 0.044 Uiso 1 1 calc R . . . .
C29 C 0.5599(9) 0.2177(7) 0.4858(5) 0.040(3) Uani 1 1 d . . . . .
H01A H 0.594006 0.161692 0.492057 0.060 Uiso 1 1 calc GR . . . .
H01B H 0.549244 0.237105 0.441888 0.060 Uiso 1 1 calc GR . . . .
H01C H 0.494503 0.212358 0.493864 0.060 Uiso 1 1 calc GR . . . .
C33 C 0.2409(9) 0.0014(7) 0.5073(5) 0.035(3) Uani 1 1 d . . . . .
H012 H 0.272784 -0.029567 0.481418 0.042 Uiso 1 1 calc R . . . .
C21 C 0.7173(7) 0.1832(6) 0.7224(5) 0.024(2) Uani 1 1 d . . . . .
H013 H 0.739639 0.160349 0.764357 0.029 Uiso 1 1 calc R . . . .
C41 C 0.1411(8) 0.1156(8) 0.6978(5) 0.041(3) Uani 1 1 d . . . . .
H01D H 0.144131 0.053112 0.704143 0.061 Uiso 1 1 calc GR . . . .
H01E H 0.098193 0.141231 0.721076 0.061 Uiso 1 1 calc GR . . . .
H01F H 0.209315 0.139845 0.713573 0.061 Uiso 1 1 calc GR . . . .
C38 C 0.3516(8) 0.0830(7) 0.4310(6) 0.041(3) Uani 1 1 d . . . . .
H01G H 0.406431 0.059291 0.466305 0.062 Uiso 1 1 calc GR . . . .
H01H H 0.380085 0.119481 0.404426 0.062 Uiso 1 1 calc GR . . . .
H01I H 0.313312 0.035691 0.405207 0.062 Uiso 1 1 calc GR . . . .
C44 C 0.4895(9) 0.0082(6) 0.6509(6) 0.035(3) Uani 1 1 d . . . . .
H01J H 0.556620 -0.017713 0.655831 0.042 Uiso 1 1 calc R . . . .
H01K H 0.436088 -0.032908 0.628473 0.042 Uiso 1 1 calc R . . . .
C18 C 0.0118(8) 0.3954(7) 0.4655(5) 0.035(3) Uani 1 1 d . . . . .
H017 H 0.010277 0.456228 0.460662 0.042 Uiso 1 1 calc R . . . .
C25 C 0.6204(7) 0.2946(7) 0.7625(5) 0.028(2) Uani 1 1 d . . . . .
H018 H 0.557929 0.329253 0.743099 0.034 Uiso 1 1 calc R . . . .
C16 C -0.0700(8) 0.2593(7) 0.4446(5) 0.031(3) Uani 1 1 d . . . . .
H019 H -0.128630 0.225708 0.425746 0.037 Uiso 1 1 calc R . . . .
C26 C 0.5990(9) 0.2342(7) 0.8110(5) 0.036(3) Uani 1 1 d . . . . .
H01L H 0.660822 0.202823 0.833433 0.055 Uiso 1 1 calc GR . . . .
H01M H 0.546237 0.193167 0.789253 0.055 Uiso 1 1 calc GR . . . .
H01N H 0.576181 0.267714 0.841839 0.055 Uiso 1 1 calc GR . . . .
C17 C -0.0751(8) 0.3472(7) 0.4373(6) 0.036(3) Uani 1 1 d . . . . .
H01O H -0.136214 0.374404 0.413600 0.044 Uiso 1 1 calc R . . . .
C34 C 0.1981(9) -0.0434(7) 0.5459(6) 0.043(3) Uani 1 1 d . . . . .
H01P H 0.200130 -0.104516 0.546756 0.051 Uiso 1 1 calc R . . . .
C47 C 0.0399(13) 0.0006(12) 0.1960(9) 0.095(6) Uani 1 1 d . . . . .
H01Z H 0.034359 -0.051612 0.170085 0.143 Uiso 1 1 calc GR . . . .
H H 0.016421 -0.011662 0.232795 0.143 Uiso 1 1 calc GR . . . .
HA H 0.110595 0.019360 0.210735 0.143 Uiso 1 1 calc GR . . . .
C27 C 0.7060(8) 0.3580(7) 0.7979(5) 0.033(3) Uani 1 1 d . . . . .
H01Q H 0.688988 0.384185 0.833861 0.049 Uiso 1 1 calc GR . . . .
H01R H 0.712810 0.403196 0.768416 0.049 Uiso 1 1 calc GR . . . .
H01S H 0.769883 0.326507 0.813712 0.049 Uiso 1 1 calc GR . . . .
C30 C 0.7148(8) 0.3107(8) 0.5123(6) 0.039(3) Uani 1 1 d . . . . .
H01T H 0.752310 0.354411 0.542410 0.059 Uiso 1 1 calc GR . . . .
H01U H 0.692362 0.335266 0.469287 0.059 Uiso 1 1 calc GR . . . .
H01V H 0.758800 0.261148 0.512934 0.059 Uiso 1 1 calc GR . . . .
C51 C -0.0166(15) 0.2461(14) 0.2834(9) 0.106(7) Uani 1 1 d . . . . .
H01 H -0.050797 0.292462 0.254724 0.160 Uiso 1 1 calc GR . . . .
HB H 0.056619 0.255913 0.296543 0.160 Uiso 1 1 calc GR . . . .
HC H -0.040102 0.245343 0.321097 0.160 Uiso 1 1 calc GR . . . .
C42 C -0.0166(9) 0.1085(11) 0.6080(6) 0.064(4) Uani 1 1 d . . . . .
H01W H -0.047198 0.113910 0.561800 0.095 Uiso 1 1 calc GR . . . .
H01X H -0.052423 0.145850 0.629843 0.095 Uiso 1 1 calc GR . . . .
H01Y H -0.021399 0.048522 0.620739 0.095 Uiso 1 1 calc GR . . . .
C48 C -0.0226(15) 0.0691(12) 0.1573(9) 0.102(7) Uani 1 1 d . . . . .
H0AA H -0.094134 0.050287 0.143752 0.123 Uiso 1 1 calc R . . . .
HD H -0.002034 0.077704 0.118451 0.123 Uiso 1 1 calc R . . . .
C50 C -0.0430(17) 0.151(2) 0.2453(13) 0.161(13) Uani 1 1 d . . . . .
H1AA H -0.006098 0.103975 0.273105 0.193 Uiso 1 1 calc R . . . .
HE H -0.116325 0.138937 0.233830 0.193 Uiso 1 1 calc R . . . .
C49 C -0.0143(18) 0.1561(13) 0.1931(12) 0.121(9) Uani 1 1 d . . . . .
H2AA H 0.056658 0.176314 0.204923 0.145 Uiso 1 1 calc R . . . .
HF H -0.056712 0.199421 0.163961 0.145 Uiso 1 1 calc R . . . .


_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
Np1 I1 3.0288(8) . ?
Np1 O1 2.480(6) . ?
Np1 N2 2.457(7) . ?
Np1 C1 2.877(9) . ?
Np1 C5 2.962(9) . ?
Np1 N1 2.490(8) . ?
Np1 C3 2.899(9) . ?
Np1 C6 2.940(9) . ?
Np1 C4 2.906(9) . ?
Np1 C2 2.903(9) . ?
O1 C46 1.456(11) . ?
O1 C43 1.448(11) . ?
N2 C14 1.392(11) . ?
N2 C31 1.432(11) . ?
C1 C6 1.376(13) . ?
C1 C7 1.498(13) . ?
C1 C2 1.403(12) . ?
C5 H006 0.9500 . ?
C5 C6 1.408(13) . ?
C5 C4 1.389(13) . ?
N1 C8 1.385(11) . ?
N1 C19 1.435(11) . ?
C3 H008 0.9500 . ?
C3 C4 1.391(13) . ?
C3 C2 1.382(12) . ?
C6 H009 0.9500 . ?
C9 H00A 0.9500 . ?
C9 C8 1.417(12) . ?
C9 C10 1.384(13) . ?
C4 C13 1.504(13) . ?
C12 H00C 0.9500 . ?
C12 C7 1.367(13) . ?
C12 C11 1.383(13) . ?
C8 C7 1.414(13) . ?
C46 H00B 0.9900 . ?
C46 H00D 0.9900 . ?
C46 C45 1.508(13) . ?
C2 H00G 0.9500 . ?
C11 H00H 0.9500 . ?
C11 C10 1.371(14) . ?
C14 C15 1.412(13) . ?
C14 C13 1.412(13) . ?
C45 H00E 0.9900 . ?
C45 H00F 0.9900 . ?
C45 C44 1.531(15) . ?
C43 H00I 0.9900 . ?
C43 H00J 0.9900 . ?
C43 C44 1.525(13) . ?
C19 C24 1.398(13) . ?
C19 C20 1.426(14) . ?
C15 H00M 0.9500 . ?
C15 C16 1.376(13) . ?
C24 C28 1.520(13) . ?
C24 C23 1.405(13) . ?
C31 C32 1.398(14) . ?
C31 C36 1.429(14) . ?
C28 H00P 1.0000 . ?
C28 C29 1.503(13) . ?
C28 C30 1.505(14) . ?
C22 H00Q 0.9500 . ?
C22 C23 1.364(14) . ?
C22 C21 1.363(14) . ?
C32 C37 1.515(15) . ?
C32 C33 1.375(14) . ?
C39 H00K 0.9800 . ?
C39 H00L 0.9800 . ?
C39 H00N 0.9800 . ?
C39 C37 1.535(15) . ?
C37 H00T 1.0000 . ?
C37 C38 1.534(15) . ?
C23 H00U 0.9500 . ?
C36 C40 1.503(15) . ?
C36 C35 1.401(14) . ?
C10 H00W 0.9500 . ?
C40 H00X 1.0000 . ?
C40 C41 1.535(15) . ?
C40 C42 1.555(15) . ?
C13 C18 1.377(13) . ?
C20 C21 1.391(14) . ?
C20 C25 1.507(14) . ?
C35 H010 0.9500 . ?
C35 C34 1.370(16) . ?
C29 H01A 0.9800 . ?
C29 H01B 0.9800 . ?
C29 H01C 0.9800 . ?
C33 H012 0.9500 . ?
C33 C34 1.366(16) . ?
C21 H013 0.9500 . ?
C41 H01D 0.9800 . ?
C41 H01E 0.9800 . ?
C41 H01F 0.9800 . ?
C38 H01G 0.9800 . ?
C38 H01H 0.9800 . ?
C38 H01I 0.9800 . ?
C44 H01J 0.9900 . ?
C44 H01K 0.9900 . ?
C18 H017 0.9500 . ?
C18 C17 1.395(14) . ?
C25 H018 1.0000 . ?
C25 C26 1.517(14) . ?
C25 C27 1.558(14) . ?
C16 H019 0.9500 . ?
C16 C17 1.373(14) . ?
C26 H01L 0.9800 . ?
C26 H01M 0.9800 . ?
C26 H01N 0.9800 . ?
C17 H01O 0.9500 . ?
C34 H01P 0.9500 . ?
C47 H01Z 0.9800 . ?
C47 H 0.9800 . ?
C47 HA 0.9800 . ?
C47 C48 1.47(2) . ?
C27 H01Q 0.9800 . ?
C27 H01R 0.9800 . ?
C27 H01S 0.9800 . ?
C30 H01T 0.9800 . ?
C30 H01U 0.9800 . ?
C30 H01V 0.9800 . ?
C51 H01 0.9800 . ?
C51 HB 0.9800 . ?
C51 HC 0.9800 . ?
C51 C50 1.68(3) . ?
C42 H01W 0.9800 . ?
C42 H01X 0.9800 . ?
C42 H01Y 0.9800 . ?
C48 H0AA 0.9900 . ?
C48 HD 0.9900 . ?
C48 C49 1.55(3) . ?
C50 H1AA 0.9900 . ?
C50 HE 0.9900 . ?
C50 C49 1.33(3) . ?
C49 H2AA 0.9900 . ?
C49 HF 0.9900 . ?

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 Np1 I1 90.27(16) . . ?
O1 Np1 C1 150.1(2) . . ?
O1 Np1 C5 159.3(2) . . ?
O1 Np1 N1 88.8(2) . . ?
O1 Np1 C3 142.7(3) . . ?
O1 Np1 C6 160.0(2) . . ?
O1 Np1 C4 149.3(2) . . ?
O1 Np1 C2 143.1(2) . . ?
N2 Np1 I1 103.39(19) . . ?
N2 Np1 O1 88.5(2) . . ?
N2 Np1 C1 117.6(2) . . ?
N2 Np1 C5 80.3(3) . . ?
N2 Np1 N1 153.7(3) . . ?
N2 Np1 C3 70.9(2) . . ?
N2 Np1 C6 107.4(2) . . ?
N2 Np1 C4 61.0(3) . . ?
N2 Np1 C2 98.1(3) . . ?
C1 Np1 I1 96.79(18) . . ?
C1 Np1 C5 48.9(3) . . ?
C1 Np1 C3 49.4(3) . . ?
C1 Np1 C6 27.3(3) . . ?
C1 Np1 C4 57.8(3) . . ?
C1 Np1 C2 28.1(2) . . ?
C5 Np1 I1 75.7(2) . . ?
N1 Np1 I1 102.74(18) . . ?
N1 Np1 C1 61.3(2) . . ?
N1 Np1 C5 108.9(3) . . ?
N1 Np1 C3 96.3(2) . . ?
N1 Np1 C6 82.1(3) . . ?
N1 Np1 C4 116.9(3) . . ?
N1 Np1 C2 69.5(2) . . ?
C3 Np1 I1 124.04(19) . . ?
C3 Np1 C5 48.4(3) . . ?
C3 Np1 C6 56.7(3) . . ?
C3 Np1 C4 27.7(3) . . ?
C3 Np1 C2 27.6(2) . . ?
C6 Np1 I1 74.5(2) . . ?
C6 Np1 C5 27.6(3) . . ?
C4 Np1 I1 99.3(2) . . ?
C4 Np1 C5 27.4(3) . . ?
C4 Np1 C6 48.8(3) . . ?
C2 Np1 I1 122.73(19) . . ?
C2 Np1 C5 56.6(3) . . ?
C2 Np1 C6 48.4(3) . . ?
C2 Np1 C4 49.0(3) . . ?
C46 O1 Np1 124.7(5) . . ?
C43 O1 Np1 125.9(5) . . ?
C43 O1 C46 108.9(7) . . ?
C14 N2 Np1 130.0(6) . . ?
C14 N2 C31 114.7(7) . . ?
C31 N2 Np1 115.3(5) . . ?
C6 C1 Np1 78.9(5) . . ?
C6 C1 C7 122.8(9) . . ?
C6 C1 C2 119.3(9) . . ?
C7 C1 Np1 112.2(6) . . ?
C2 C1 Np1 77.0(5) . . ?
C2 C1 C7 117.9(8) . . ?
Np1 C5 H006 121.6 . . ?
C6 C5 Np1 75.3(5) . . ?
C6 C5 H006 120.2 . . ?
C4 C5 Np1 74.1(5) . . ?
C4 C5 H006 120.2 . . ?
C4 C5 C6 119.5(9) . . ?
C8 N1 Np1 128.0(6) . . ?
C8 N1 C19 114.3(7) . . ?
C19 N1 Np1 117.5(5) . . ?
Np1 C3 H008 118.3 . . ?
C4 C3 Np1 76.4(5) . . ?
C4 C3 H008 119.7 . . ?
C2 C3 Np1 76.4(6) . . ?
C2 C3 H008 119.7 . . ?
C2 C3 C4 120.6(9) . . ?
Np1 C6 H009 120.5 . . ?
C1 C6 Np1 73.8(5) . . ?
C1 C6 C5 120.7(9) . . ?
C1 C6 H009 119.7 . . ?
C5 C6 Np1 77.1(5) . . ?
C5 C6 H009 119.7 . . ?
C8 C9 H00A 119.4 . . ?
C10 C9 H00A 119.4 . . ?
C10 C9 C8 121.1(9) . . ?
C5 C4 Np1 78.6(5) . . ?
C5 C4 C3 119.6(9) . . ?
C5 C4 C13 121.9(9) . . ?
C3 C4 Np1 75.9(5) . . ?
C3 C4 C13 118.3(9) . . ?
C13 C4 Np1 112.4(6) . . ?
C7 C12 H00C 119.7 . . ?
C7 C12 C11 120.7(9) . . ?
C11 C12 H00C 119.7 . . ?
N1 C8 C9 124.9(8) . . ?
N1 C8 C7 120.3(8) . . ?
C7 C8 C9 114.8(8) . . ?
O1 C46 H00B 111.0 . . ?
O1 C46 H00D 111.0 . . ?
O1 C46 C45 103.8(8) . . ?
H00B C46 H00D 109.0 . . ?
C45 C46 H00B 111.0 . . ?
C45 C46 H00D 111.0 . . ?
C12 C7 C1 122.1(8) . . ?
C12 C7 C8 122.9(9) . . ?
C8 C7 C1 115.0(8) . . ?
Np1 C2 H00G 120.1 . . ?
C1 C2 Np1 74.9(5) . . ?
C1 C2 H00G 120.0 . . ?
C3 C2 Np1 76.0(5) . . ?
C3 C2 C1 120.1(9) . . ?
C3 C2 H00G 120.0 . . ?
C12 C11 H00H 120.9 . . ?
C10 C11 C12 118.2(9) . . ?
C10 C11 H00H 120.9 . . ?
N2 C14 C15 124.4(8) . . ?
N2 C14 C13 120.2(8) . . ?
C13 C14 C15 115.4(9) . . ?
C46 C45 H00E 111.4 . . ?
C46 C45 H00F 111.4 . . ?
C46 C45 C44 101.9(8) . . ?
H00E C45 H00F 109.3 . . ?
C44 C45 H00E 111.4 . . ?
C44 C45 H00F 111.4 . . ?
O1 C43 H00I 110.4 . . ?
O1 C43 H00J 110.4 . . ?
O1 C43 C44 106.6(8) . . ?
H00I C43 H00J 108.6 . . ?
C44 C43 H00I 110.4 . . ?
C44 C43 H00J 110.4 . . ?
C24 C19 N1 120.1(9) . . ?
C24 C19 C20 119.7(9) . . ?
C20 C19 N1 120.2(8) . . ?
C14 C15 H00M 119.1 . . ?
C16 C15 C14 121.7(9) . . ?
C16 C15 H00M 119.1 . . ?
C19 C24 C28 122.7(9) . . ?
C19 C24 C23 118.7(9) . . ?
C23 C24 C28 118.5(9) . . ?
C32 C31 N2 120.0(9) . . ?
C32 C31 C36 120.5(9) . . ?
C36 C31 N2 119.4(9) . . ?
C24 C28 H00P 106.8 . . ?
C29 C28 C24 111.4(8) . . ?
C29 C28 H00P 106.8 . . ?
C29 C28 C30 113.0(9) . . ?
C30 C28 C24 111.5(8) . . ?
C30 C28 H00P 106.8 . . ?
C23 C22 H00Q 119.8 . . ?
C21 C22 H00Q 119.8 . . ?
C21 C22 C23 120.4(9) . . ?
C31 C32 C37 120.7(9) . . ?
C33 C32 C31 119.0(10) . . ?
C33 C32 C37 120.3(10) . . ?
H00K C39 H00L 109.5 . . ?
H00K C39 H00N 109.5 . . ?
H00L C39 H00N 109.5 . . ?
C37 C39 H00K 109.5 . . ?
C37 C39 H00L 109.5 . . ?
C37 C39 H00N 109.5 . . ?
C32 C37 C39 113.1(9) . . ?
C32 C37 H00T 107.6 . . ?
C32 C37 C38 114.8(9) . . ?
C39 C37 H00T 107.6 . . ?
C38 C37 C39 105.8(9) . . ?
C38 C37 H00T 107.6 . . ?
C24 C23 H00U 119.5 . . ?
C22 C23 C24 121.0(9) . . ?
C22 C23 H00U 119.5 . . ?
C31 C36 C40 123.6(9) . . ?
C35 C36 C31 116.6(11) . . ?
C35 C36 C40 119.8(11) . . ?
C9 C10 H00W 119.0 . . ?
C11 C10 C9 121.9(9) . . ?
C11 C10 H00W 119.0 . . ?
C36 C40 H00X 108.6 . . ?
C36 C40 C41 113.9(9) . . ?
C36 C40 C42 111.2(10) . . ?
C41 C40 H00X 108.6 . . ?
C41 C40 C42 106.0(9) . . ?
C42 C40 H00X 108.6 . . ?
C14 C13 C4 114.7(8) . . ?
C18 C13 C4 122.6(9) . . ?
C18 C13 C14 122.4(9) . . ?
C19 C20 C25 121.9(9) . . ?
C21 C20 C19 118.0(10) . . ?
C21 C20 C25 120.0(9) . . ?
C36 C35 H010 118.8 . . ?
C34 C35 C36 122.5(11) . . ?
C34 C35 H010 118.8 . . ?
C28 C29 H01A 109.5 . . ?
C28 C29 H01B 109.5 . . ?
C28 C29 H01C 109.5 . . ?
H01A C29 H01B 109.5 . . ?
H01A C29 H01C 109.5 . . ?
H01B C29 H01C 109.5 . . ?
C32 C33 H012 119.0 . . ?
C34 C33 C32 122.0(12) . . ?
C34 C33 H012 119.0 . . ?
C22 C21 C20 121.7(10) . . ?
C22 C21 H013 119.1 . . ?
C20 C21 H013 119.1 . . ?
C40 C41 H01D 109.5 . . ?
C40 C41 H01E 109.5 . . ?
C40 C41 H01F 109.5 . . ?
H01D C41 H01E 109.5 . . ?
H01D C41 H01F 109.5 . . ?
H01E C41 H01F 109.5 . . ?
C37 C38 H01G 109.5 . . ?
C37 C38 H01H 109.5 . . ?
C37 C38 H01I 109.5 . . ?
H01G C38 H01H 109.5 . . ?
H01G C38 H01I 109.5 . . ?
H01H C38 H01I 109.5 . . ?
C45 C44 H01J 111.4 . . ?
C45 C44 H01K 111.4 . . ?
C43 C44 C45 101.8(8) . . ?
C43 C44 H01J 111.4 . . ?
C43 C44 H01K 111.4 . . ?
H01J C44 H01K 109.3 . . ?
C13 C18 H017 119.8 . . ?
C13 C18 C17 120.4(10) . . ?
C17 C18 H017 119.8 . . ?
C20 C25 H018 107.7 . . ?
C20 C25 C26 115.0(9) . . ?
C20 C25 C27 109.9(8) . . ?
C26 C25 H018 107.7 . . ?
C26 C25 C27 108.6(9) . . ?
C27 C25 H018 107.7 . . ?
C15 C16 H019 119.1 . . ?
C17 C16 C15 121.7(10) . . ?
C17 C16 H019 119.1 . . ?
C25 C26 H01L 109.5 . . ?
C25 C26 H01M 109.5 . . ?
C25 C26 H01N 109.5 . . ?
H01L C26 H01M 109.5 . . ?
H01L C26 H01N 109.5 . . ?
H01M C26 H01N 109.5 . . ?
C18 C17 H01O 120.9 . . ?
C16 C17 C18 118.3(10) . . ?
C16 C17 H01O 120.9 . . ?
C35 C34 H01P 120.3 . . ?
C33 C34 C35 119.3(11) . . ?
C33 C34 H01P 120.3 . . ?
H01Z C47 H 109.5 . . ?
H01Z C47 HA 109.5 . . ?
H C47 HA 109.5 . . ?
C48 C47 H01Z 109.5 . . ?
C48 C47 H 109.5 . . ?
C48 C47 HA 109.5 . . ?
C25 C27 H01Q 109.5 . . ?
C25 C27 H01R 109.5 . . ?
C25 C27 H01S 109.5 . . ?
H01Q C27 H01R 109.5 . . ?
H01Q C27 H01S 109.5 . . ?
H01R C27 H01S 109.5 . . ?
C28 C30 H01T 109.5 . . ?
C28 C30 H01U 109.5 . . ?
C28 C30 H01V 109.5 . . ?
H01T C30 H01U 109.5 . . ?
H01T C30 H01V 109.5 . . ?
H01U C30 H01V 109.5 . . ?
H01 C51 HB 109.5 . . ?
H01 C51 HC 109.5 . . ?
HB C51 HC 109.5 . . ?
C50 C51 H01 109.5 . . ?
C50 C51 HB 109.5 . . ?
C50 C51 HC 109.5 . . ?
C40 C42 H01W 109.5 . . ?
C40 C42 H01X 109.5 . . ?
C40 C42 H01Y 109.5 . . ?
H01W C42 H01X 109.5 . . ?
H01W C42 H01Y 109.5 . . ?
H01X C42 H01Y 109.5 . . ?
C47 C48 H0AA 108.9 . . ?
C47 C48 HD 108.9 . . ?
C47 C48 C49 113.4(16) . . ?
H0AA C48 HD 107.7 . . ?
C49 C48 H0AA 108.9 . . ?
C49 C48 HD 108.9 . . ?
C51 C50 H1AA 110.2 . . ?
C51 C50 HE 110.2 . . ?
H1AA C50 HE 108.5 . . ?
C49 C50 C51 108(2) . . ?
C49 C50 H1AA 110.2 . . ?
C49 C50 HE 110.2 . . ?
C48 C49 H2AA 109.0 . . ?
C48 C49 HF 109.0 . . ?
C50 C49 C48 113(2) . . ?
C50 C49 H2AA 109.0 . . ?
C50 C49 HF 109.0 . . ?
H2AA C49 HF 107.8 . . ?

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
Np1 O1 C46 C45 -161.9(6) . . . . ?
Np1 O1 C43 C44 -173.1(6) . . . . ?
Np1 N2 C14 C15 -174.9(7) . . . . ?
Np1 N2 C14 C13 7.7(14) . . . . ?
Np1 N2 C31 C32 -81.9(9) . . . . ?
Np1 N2 C31 C36 100.5(8) . . . . ?
Np1 C1 C6 C5 -63.7(8) . . . . ?
Np1 C1 C7 C12 -162.4(8) . . . . ?
Np1 C1 C7 C8 17.6(10) . . . . ?
Np1 C1 C2 C3 63.6(8) . . . . ?
Np1 C5 C6 C1 62.1(8) . . . . ?
Np1 C5 C4 C3 -66.3(8) . . . . ?
Np1 C5 C4 C13 109.4(8) . . . . ?
Np1 N1 C8 C9 170.4(7) . . . . ?
Np1 N1 C8 C7 -8.6(13) . . . . ?
Np1 N1 C19 C24 102.0(9) . . . . ?
Np1 N1 C19 C20 -80.7(9) . . . . ?
Np1 C3 C4 C5 67.8(8) . . . . ?
Np1 C3 C4 C13 -108.1(8) . . . . ?
Np1 C3 C2 C1 -63.0(8) . . . . ?
Np1 C4 C13 C14 -11.8(11) . . . . ?
Np1 C4 C13 C18 173.5(8) . . . . ?
O1 C46 C45 C44 -39.6(10) . . . . ?
O1 C43 C44 C45 -24.0(10) . . . . ?
N2 C14 C15 C16 179.7(10) . . . . ?
N2 C14 C13 C4 4.9(14) . . . . ?
N2 C14 C13 C18 179.6(10) . . . . ?
N2 C31 C32 C37 -3.2(14) . . . . ?
N2 C31 C32 C33 178.1(9) . . . . ?
N2 C31 C36 C40 2.0(14) . . . . ?
N2 C31 C36 C35 -180.0(8) . . . . ?
C5 C4 C13 C14 -102.1(11) . . . . ?
C5 C4 C13 C18 83.3(13) . . . . ?
N1 C8 C7 C1 -8.5(13) . . . . ?
N1 C8 C7 C12 171.5(9) . . . . ?
N1 C19 C24 C28 1.4(14) . . . . ?
N1 C19 C24 C23 -175.2(8) . . . . ?
N1 C19 C20 C21 174.4(8) . . . . ?
N1 C19 C20 C25 -10.3(14) . . . . ?
C3 C4 C13 C14 73.7(12) . . . . ?
C3 C4 C13 C18 -101.0(12) . . . . ?
C6 C1 C7 C12 -71.6(13) . . . . ?
C6 C1 C7 C8 108.4(10) . . . . ?
C6 C1 C2 Np1 -69.1(8) . . . . ?
C6 C1 C2 C3 -5.5(13) . . . . ?
C6 C5 C4 Np1 62.3(8) . . . . ?
C6 C5 C4 C3 -4.0(14) . . . . ?
C6 C5 C4 C13 171.7(9) . . . . ?
C9 C8 C7 C1 172.5(8) . . . . ?
C9 C8 C7 C12 -7.5(15) . . . . ?
C4 C5 C6 Np1 -61.7(8) . . . . ?
C4 C5 C6 C1 0.4(14) . . . . ?
C4 C3 C2 Np1 64.9(8) . . . . ?
C4 C3 C2 C1 1.9(14) . . . . ?
C4 C13 C18 C17 174.0(11) . . . . ?
C12 C11 C10 C9 -2.1(16) . . . . ?
C8 N1 C19 C24 -82.6(11) . . . . ?
C8 N1 C19 C20 94.7(10) . . . . ?
C8 C9 C10 C11 -1.9(16) . . . . ?
C46 O1 C43 C44 -0.5(10) . . . . ?
C46 C45 C44 C43 38.5(10) . . . . ?
C7 C1 C6 Np1 -109.3(8) . . . . ?
C7 C1 C6 C5 -173.0(9) . . . . ?
C7 C1 C2 Np1 108.4(8) . . . . ?
C7 C1 C2 C3 172.0(8) . . . . ?
C7 C12 C11 C10 1.2(15) . . . . ?
C2 C1 C6 Np1 68.1(7) . . . . ?
C2 C1 C6 C5 4.4(14) . . . . ?
C2 C1 C7 C12 111.0(11) . . . . ?
C2 C1 C7 C8 -69.0(12) . . . . ?
C2 C3 C4 Np1 -64.9(8) . . . . ?
C2 C3 C4 C5 2.9(14) . . . . ?
C2 C3 C4 C13 -173.0(8) . . . . ?
C11 C12 C7 C1 -176.1(9) . . . . ?
C11 C12 C7 C8 3.9(16) . . . . ?
C14 N2 C31 C32 99.7(10) . . . . ?
C14 N2 C31 C36 -77.9(11) . . . . ?
C14 C15 C16 C17 2.0(18) . . . . ?
C14 C13 C18 C17 -0.2(18) . . . . ?
C43 O1 C46 C45 25.3(10) . . . . ?
C19 N1 C8 C9 -4.5(14) . . . . ?
C19 N1 C8 C7 176.6(9) . . . . ?
C19 C24 C28 C29 -105.5(11) . . . . ?
C19 C24 C28 C30 127.2(10) . . . . ?
C19 C24 C23 C22 -1.8(14) . . . . ?
C19 C20 C21 C22 3.6(14) . . . . ?
C19 C20 C25 C26 139.8(10) . . . . ?
C19 C20 C25 C27 -97.3(11) . . . . ?
C15 C14 C13 C4 -172.8(9) . . . . ?
C15 C14 C13 C18 1.9(16) . . . . ?
C15 C16 C17 C18 -0.2(18) . . . . ?
C24 C19 C20 C21 -8.3(14) . . . . ?
C24 C19 C20 C25 167.0(9) . . . . ?
C31 N2 C14 C15 3.2(14) . . . . ?
C31 N2 C14 C13 -174.2(9) . . . . ?
C31 C32 C37 C39 -75.6(12) . . . . ?
C31 C32 C37 C38 162.9(9) . . . . ?
C31 C32 C33 C34 3.2(16) . . . . ?
C31 C36 C40 C41 -120.7(11) . . . . ?
C31 C36 C40 C42 119.8(11) . . . . ?
C31 C36 C35 C34 0.7(15) . . . . ?
C28 C24 C23 C22 -178.6(9) . . . . ?
C32 C31 C36 C40 -175.6(9) . . . . ?
C32 C31 C36 C35 2.4(13) . . . . ?
C32 C33 C34 C35 -0.1(18) . . . . ?
C37 C32 C33 C34 -175.6(10) . . . . ?
C23 C24 C28 C29 71.1(12) . . . . ?
C23 C24 C28 C30 -56.1(12) . . . . ?
C23 C22 C21 C20 2.0(15) . . . . ?
C36 C31 C32 C37 174.4(9) . . . . ?
C36 C31 C32 C33 -4.4(14) . . . . ?
C36 C35 C34 C33 -1.9(17) . . . . ?
C10 C9 C8 N1 -172.6(9) . . . . ?
C10 C9 C8 C7 6.4(14) . . . . ?
C40 C36 C35 C34 178.8(10) . . . . ?
C13 C14 C15 C16 -2.8(15) . . . . ?
C13 C18 C17 C16 -0.7(18) . . . . ?
C20 C19 C24 C28 -176.0(8) . . . . ?
C20 C19 C24 C23 7.4(14) . . . . ?
C35 C36 C40 C41 61.4(13) . . . . ?
C35 C36 C40 C42 -58.2(13) . . . . ?
C33 C32 C37 C39 103.2(12) . . . . ?
C33 C32 C37 C38 -18.3(14) . . . . ?
C21 C22 C23 C24 -2.9(15) . . . . ?
C21 C20 C25 C26 -45.0(13) . . . . ?
C21 C20 C25 C27 77.9(12) . . . . ?
C25 C20 C21 C22 -171.8(9) . . . . ?
C47 C48 C49 C50 -60(3) . . . . ?
C51 C50 C49 C48 173.2(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT360_3_Np                
;
PROBLEM: Short C(sp3)-C(sp3) Bond C01J - C01K . 1.33 Ang.
RESPONSE: These atoms are contained in disordered 
non-coordinated solvent within the lattice 
;
_vrf_PLAT971_3_Np                
;
PROBLEM: Check Calcd Resid. Dens. 0.94Ang From Np01 2.85 eA-3
RESPONSE: The residual density is attributed to absorption 
artefacts due to insufficient absorption correction due to Np 
atom
;
_vrf_PLAT973_3_Np                
;
PROBLEM: Check Calcd Positive Resid. Density on Np01 1.68 eA-3
RESPONSE: The residual density is attributed to absorption 
artefacts due to insufficient absorption correction due to Np 
atom
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_2_Np
_database_code_depnum_ccdc_archive 'CCDC 2238468'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_audit_creation_date             2021-02-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H66 Cl2 K N2 Np O4, C4 H9 O2'
_chemical_formula_sum            'C54 H75 Cl2 K N2 Np O6'
_chemical_formula_weight         1195.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         NpCl2KN2C50O6
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
Np Np -11.4937 4.1493 '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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.9304(14)
_cell_length_b                   12.0060(7)
_cell_length_c                   26.7063(18)
_cell_angle_alpha                90
_cell_angle_beta                 107.882(8)
_cell_angle_gamma                90
_cell_volume                     5471.4(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11223
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.6520
_cell_measurement_theta_min      2.0830
_shelx_estimated_absorpt_T_max   0.816
_shelx_estimated_absorpt_T_min   0.676
_exptl_absorpt_coefficient_mu    2.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2428
_exptl_crystal_preparation       'By AJG, JM, CAPG'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35831
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.876
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.26 122.26   0.50   60.00    --   28.00  73.75 -25.74  240
  2  ω      2.26 122.26   0.50   60.00    --   28.00  73.75  64.26  240
  3  ω    -53.74  65.76   0.50   60.00    --  -28.00  73.75 154.26  239
  4  ω    -53.74  65.76   0.50   60.00    --  -28.00  73.75-115.74  239
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0012990000
_diffrn_orient_matrix_UB_12      -0.0116774000
_diffrn_orient_matrix_UB_13      0.0262452000
_diffrn_orient_matrix_UB_21      -0.0344181000
_diffrn_orient_matrix_UB_22      -0.0328375000
_diffrn_orient_matrix_UB_23      -0.0093742000
_diffrn_orient_matrix_UB_31      0.0233492000
_diffrn_orient_matrix_UB_32      -0.0477512000
_diffrn_orient_matrix_UB_33      0.0000230000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8172
_reflns_number_total             11123
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         11123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.002
_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)+(0.0236P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0883
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C37(H37), C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B), C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C33(H33), C34(H34),
  C35(H35), C53(H53)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C14 C 0.8892(3) 0.2373(4) 0.28082(17) 0.0251(11) Uani 1 1 d . . . . .
Cl1 Cl 0.68862(8) 0.48087(12) 0.28236(5) 0.0392(3) Uani 1 1 d . . . . .
K1 K 0.58488(7) 0.17413(11) 0.44051(5) 0.0400(3) Uani 1 1 d . . . . .
N2 N 0.8381(2) 0.2275(3) 0.31033(15) 0.0250(9) Uani 1 1 d . . . . .
Np1 Np 0.79116(2) 0.37410(2) 0.35898(2) 0.02311(6) Uani 1 1 d . . . . .
O1 O 0.4403(2) 0.2648(3) 0.39778(15) 0.0477(10) Uani 1 1 d . . . . .
C15 C 0.9013(3) 0.1551(4) 0.24652(19) 0.0336(13) Uani 1 1 d . . . . .
H2 H 0.876268 0.084809 0.244783 0.040 Uiso 1 1 calc R U . . .
Cl2 Cl 0.69840(8) 0.21933(11) 0.38074(5) 0.0380(3) Uani 1 1 d . . . . .
N1 N 0.7790(2) 0.4742(3) 0.43792(14) 0.0247(9) Uani 1 1 d . . . . .
O2 O 0.4805(3) 0.0801(4) 0.34925(15) 0.0502(11) Uani 1 1 d . . . . .
C16 C 0.9489(3) 0.1743(4) 0.21533(18) 0.0320(13) Uani 1 1 d . . . . .
H3 H 0.955837 0.117026 0.192606 0.038 Uiso 1 1 calc R U . . .
O3 O 0.6024(2) 0.0766(3) 0.53770(15) 0.0479(11) Uani 1 1 d . . . . .
C17 C 0.9864(3) 0.2749(5) 0.2166(2) 0.0344(13) Uani 1 1 d . . . . .
H4 H 1.017074 0.288528 0.193844 0.041 Uiso 1 1 calc R U . . .
O4 O 0.6498(2) -0.0375(3) 0.46112(15) 0.0468(10) Uani 1 1 d . . . . .
C18 C 0.9787(3) 0.3549(4) 0.25119(19) 0.0315(12) Uani 1 1 d . . . . .
H5 H 1.005456 0.423816 0.252880 0.038 Uiso 1 1 calc R U . . .
C13 C 0.9326(3) 0.3375(4) 0.28398(18) 0.0266(12) Uani 1 1 d . . . . .
C4 C 0.9271(3) 0.4203(4) 0.32388(18) 0.0262(11) Uani 1 1 d . . . . .
C5 C 0.8849(3) 0.5194(4) 0.31167(19) 0.0294(12) Uani 1 1 d . . . . .
H8 H 0.864442 0.541902 0.275960 0.035 Uiso 1 1 calc R U . . .
C6 C 0.8722(3) 0.5855(4) 0.35083(18) 0.0272(12) Uani 1 1 d . . . . .
H9 H 0.843510 0.652928 0.341688 0.033 Uiso 1 1 calc R U . . .
C1 C 0.9013(3) 0.5539(4) 0.40366(18) 0.0256(11) Uani 1 1 d . . . . .
C2 C 0.9467(3) 0.4566(4) 0.41606(18) 0.0260(11) Uani 1 1 d . . . . .
H11 H 0.969005 0.435745 0.451883 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9595(3) 0.3909(4) 0.37734(17) 0.0247(11) Uani 1 1 d . . . . .
H12 H 0.990331 0.325276 0.386629 0.030 Uiso 1 1 calc R U . . .
C7 C 0.8796(3) 0.6157(4) 0.44551(17) 0.0253(11) Uani 1 1 d . . . . .
C12 C 0.9206(3) 0.7113(4) 0.46862(19) 0.0330(13) Uani 1 1 d . . . . .
H14 H 0.961580 0.739349 0.456516 0.040 Uiso 1 1 calc R U . . .
C11 C 0.9019(3) 0.7651(4) 0.5091(2) 0.0365(13) Uani 1 1 d . . . . .
H15 H 0.929254 0.830348 0.524698 0.044 Uiso 1 1 calc R U . . .
C10 C 0.8429(3) 0.7224(4) 0.52629(19) 0.0336(13) Uani 1 1 d . . . . .
H16 H 0.830190 0.758370 0.554289 0.040 Uiso 1 1 calc R U . . .
C9 C 0.8013(3) 0.6275(4) 0.50364(18) 0.0318(12) Uani 1 1 d . . . . .
H17 H 0.760649 0.600962 0.516421 0.038 Uiso 1 1 calc R U . . .
C8 C 0.8178(3) 0.5700(4) 0.46232(18) 0.0247(11) Uani 1 1 d . . . . .
C31 C 0.8034(3) 0.1172(4) 0.30730(18) 0.0271(11) Uani 1 1 d . . . . .
C32 C 0.8420(3) 0.0359(4) 0.34355(19) 0.0298(12) Uani 1 1 d . . . . .
C33 C 0.8075(4) -0.0699(5) 0.3404(2) 0.0404(14) Uani 1 1 d . . . . .
H21 H 0.833209 -0.126018 0.364712 0.048 Uiso 1 1 calc R U . . .
C34 C 0.7369(4) -0.0945(5) 0.3027(2) 0.0485(16) Uani 1 1 d . . . . .
H22 H 0.714112 -0.166229 0.301527 0.058 Uiso 1 1 calc R U . . .
C35 C 0.7002(4) -0.0146(5) 0.2671(2) 0.0409(14) Uani 1 1 d . . . . .
H23 H 0.652054 -0.031985 0.241164 0.049 Uiso 1 1 calc R U . . .
C36 C 0.7322(3) 0.0931(4) 0.26809(19) 0.0327(13) Uani 1 1 d . . . . .
C40 C 0.6902(3) 0.1794(5) 0.22750(19) 0.0357(13) Uani 1 1 d . . . . .
H25 H 0.721825 0.249485 0.234980 0.043 Uiso 1 1 calc R U . . .
C41 C 0.6081(3) 0.2066(5) 0.2301(2) 0.0452(15) Uani 1 1 d . . . . .
H26A H 0.576504 0.138469 0.224452 0.068 Uiso 1 1 calc R U . . .
H26B H 0.583208 0.261133 0.202778 0.068 Uiso 1 1 calc R U . . .
H26C H 0.612010 0.237650 0.264757 0.068 Uiso 1 1 calc R U . . .
C42 C 0.6852(4) 0.1413(5) 0.1715(2) 0.0516(17) Uani 1 1 d . . . . .
H27A H 0.738180 0.128530 0.169432 0.077 Uiso 1 1 calc R U . . .
H27B H 0.659331 0.199023 0.146230 0.077 Uiso 1 1 calc R U . . .
H27C H 0.655014 0.072005 0.163300 0.077 Uiso 1 1 calc R U . . .
C37 C 0.9183(3) 0.0613(4) 0.3864(2) 0.0325(13) Uani 1 1 d . . . . .
H28 H 0.936614 0.136469 0.379050 0.039 Uiso 1 1 calc R U . . .
C39 C 0.9049(4) 0.0662(7) 0.4400(2) 0.065(2) Uani 1 1 d . . . . .
H29A H 0.865266 0.122831 0.439349 0.098 Uiso 1 1 calc R U . . .
H29B H 0.954089 0.085376 0.466947 0.098 Uiso 1 1 calc R U . . .
H29C H 0.886652 -0.006595 0.448080 0.098 Uiso 1 1 calc R U . . .
C38 C 0.9823(4) -0.0218(5) 0.3877(3) 0.0564(18) Uani 1 1 d . . . . .
H30A H 0.967855 -0.095059 0.398045 0.085 Uiso 1 1 calc R U . . .
H30B H 1.031585 0.002629 0.413180 0.085 Uiso 1 1 calc R U . . .
H30C H 0.988986 -0.026943 0.352695 0.085 Uiso 1 1 calc R U . . .
C19 C 0.7227(3) 0.4377(4) 0.46255(18) 0.0247(11) Uani 1 1 d . . . . .
C20 C 0.6446(3) 0.4773(4) 0.44422(19) 0.0291(12) Uani 1 1 d . . . . .
C21 C 0.5934(3) 0.4488(4) 0.4731(2) 0.0341(13) Uani 1 1 d . . . . .
H33 H 0.541052 0.475581 0.461544 0.041 Uiso 1 1 calc R U . . .
C22 C 0.6166(3) 0.3840(5) 0.5172(2) 0.0378(14) Uani 1 1 d . . . . .
H34 H 0.581672 0.368747 0.536798 0.045 Uiso 1 1 calc R U . . .
C23 C 0.6925(3) 0.3403(4) 0.5330(2) 0.0333(13) Uani 1 1 d . . . . .
H35 H 0.707998 0.292131 0.562585 0.040 Uiso 1 1 calc R U . . .
C24 C 0.7459(3) 0.3658(4) 0.50623(18) 0.0287(12) Uani 1 1 d . . . . .
C28 C 0.8277(3) 0.3166(4) 0.52491(18) 0.0312(12) Uani 1 1 d . . . . .
H37 H 0.852712 0.328881 0.496669 0.037 Uiso 1 1 calc R U . . .
C30 C 0.8279(4) 0.1912(5) 0.5355(2) 0.0506(16) Uani 1 1 d . . . . .
H38A H 0.880144 0.160869 0.539360 0.076 Uiso 1 1 calc R U . . .
H38B H 0.789321 0.154406 0.505986 0.076 Uiso 1 1 calc R U . . .
H38C H 0.814490 0.178085 0.567910 0.076 Uiso 1 1 calc R U . . .
C29 C 0.8780(3) 0.3745(5) 0.5746(2) 0.0495(15) Uani 1 1 d . . . . .
H39A H 0.854021 0.364989 0.602778 0.074 Uiso 1 1 calc R U . . .
H39B H 0.881656 0.454100 0.567559 0.074 Uiso 1 1 calc R U . . .
H39C H 0.930559 0.341729 0.585544 0.074 Uiso 1 1 calc R U . . .
C25 C 0.6139(3) 0.5491(5) 0.3958(2) 0.0370(14) Uani 1 1 d . . . . .
H40 H 0.658804 0.564838 0.382079 0.044 Uiso 1 1 calc R U . . .
C26 C 0.5520(3) 0.4869(5) 0.3528(2) 0.0463(16) Uani 1 1 d . . . . .
H41A H 0.505491 0.474790 0.364060 0.069 Uiso 1 1 calc R U . . .
H41B H 0.573103 0.414854 0.346400 0.069 Uiso 1 1 calc R U . . .
H41C H 0.537655 0.531047 0.320403 0.069 Uiso 1 1 calc R U . . .
C27 C 0.5829(4) 0.6607(5) 0.4079(3) 0.0544(17) Uani 1 1 d . . . . .
H42A H 0.571778 0.708977 0.376884 0.082 Uiso 1 1 calc R U . . .
H42B H 0.622286 0.696185 0.437458 0.082 Uiso 1 1 calc R U . . .
H42C H 0.534679 0.648872 0.417181 0.082 Uiso 1 1 calc R U . . .
C43 C 0.3948(4) 0.3274(5) 0.4238(3) 0.0536(17) Uani 1 1 d . . . . .
H43A H 0.382916 0.400940 0.407333 0.080 Uiso 1 1 calc R U . . .
H43B H 0.424675 0.336209 0.461020 0.080 Uiso 1 1 calc R U . . .
H43C H 0.345851 0.287758 0.420692 0.080 Uiso 1 1 calc R U . . .
C44 C 0.3955(4) 0.2347(6) 0.3455(2) 0.0566(18) Uani 1 1 d . . . . .
H44A H 0.372091 0.302059 0.325425 0.068 Uiso 1 1 calc R U . . .
H44B H 0.352472 0.183848 0.346473 0.068 Uiso 1 1 calc R U . . .
C45 C 0.4479(4) 0.1782(5) 0.3193(2) 0.0542(18) Uani 1 1 d . . . . .
H45A H 0.417694 0.157094 0.282868 0.065 Uiso 1 1 calc R U . . .
H45B H 0.490548 0.229248 0.317779 0.065 Uiso 1 1 calc R U . . .
C46 C 0.5186(4) 0.0075(5) 0.3219(2) 0.0560(18) Uani 1 1 d . . . . .
H46A H 0.480854 -0.016026 0.288584 0.084 Uiso 1 1 calc R U . . .
H46B H 0.538763 -0.058132 0.343690 0.084 Uiso 1 1 calc R U . . .
H46C H 0.562070 0.047142 0.314890 0.084 Uiso 1 1 calc R U . . .
C47 C 0.5564(4) 0.1083(5) 0.5708(2) 0.0519(17) Uani 1 1 d . . . . .
H47A H 0.505311 0.071018 0.558844 0.078 Uiso 1 1 calc R U . . .
H47B H 0.548669 0.189174 0.569127 0.078 Uiso 1 1 calc R U . . .
H47C H 0.583642 0.086324 0.607217 0.078 Uiso 1 1 calc R U . . .
C48 C 0.6220(4) -0.0389(5) 0.5433(2) 0.0504(17) Uani 1 1 d . . . . .
H48A H 0.574229 -0.084306 0.528430 0.060 Uiso 1 1 calc R U . . .
H48B H 0.644402 -0.057703 0.581029 0.060 Uiso 1 1 calc R U . . .
C49 C 0.6799(4) -0.0644(5) 0.5153(2) 0.0514(17) Uani 1 1 d . . . . .
H49A H 0.728477 -0.021331 0.531381 0.062 Uiso 1 1 calc R U . . .
H49B H 0.693300 -0.144556 0.519194 0.062 Uiso 1 1 calc R U . . .
C50 C 0.7037(4) -0.0670(5) 0.4332(2) 0.0533(17) Uani 1 1 d . . . . .
H50A H 0.681607 -0.045719 0.396116 0.080 Uiso 1 1 calc R U . . .
H50B H 0.712788 -0.147598 0.435653 0.080 Uiso 1 1 calc R U . . .
H50C H 0.753417 -0.027896 0.448621 0.080 Uiso 1 1 calc R U . . .
O5 O 0.7770(2) 0.9589(3) 0.67483(15) 0.0490(11) Uani 1 1 d . . . . .
O6 O 0.7988(2) 0.7388(3) 0.63953(15) 0.0471(10) Uani 1 1 d . . . . .
C51 C 0.7597(4) 1.0741(5) 0.6677(2) 0.0516(17) Uani 1 1 d . . . . .
H51A H 0.741028 1.091048 0.629960 0.077 Uiso 1 1 calc R U . . .
H51B H 0.807070 1.117403 0.684438 0.077 Uiso 1 1 calc R U . . .
H51C H 0.718921 1.093345 0.683628 0.077 Uiso 1 1 calc R U . . .
C52 C 0.8402(3) 0.9263(5) 0.6568(2) 0.0445(15) Uani 1 1 d . . . . .
H52A H 0.886651 0.973021 0.673560 0.053 Uiso 1 1 calc R U . . .
H52B H 0.825834 0.936710 0.618204 0.053 Uiso 1 1 calc R U . . .
C53 C 0.8589(4) 0.8075(6) 0.6701(2) 0.0553(18) Uani 1 1 d . . . . .
H53 H 0.905050 0.781589 0.695800 0.066 Uiso 1 1 calc R U . . .
C54 C 0.8136(4) 0.6256(6) 0.6532(3) 0.0642(19) Uani 1 1 d . . . . .
H54A H 0.771890 0.579603 0.630068 0.096 Uiso 1 1 calc R U . . .
H54B H 0.815017 0.614502 0.689805 0.096 Uiso 1 1 calc R U . . .
H54C H 0.864096 0.603946 0.649081 0.096 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
C14 N2 1.384(6) . ?
C14 C15 1.408(6) . ?
C14 C13 1.422(7) . ?
Cl1 Np1 2.6268(13) . ?
K1 O1 2.718(4) . ?
K1 Cl2 2.9968(17) . ?
K1 O2 2.814(4) . ?
K1 O3 2.776(4) . ?
K1 O4 2.779(4) . ?
K1 C21 3.402(5) . ?
K1 C22 3.185(5) . ?
K1 C23 3.297(5) . ?
K1 C45 3.411(6) . ?
N2 Np1 2.483(4) . ?
N2 C31 1.454(6) . ?
Np1 Cl2 2.6740(13) . ?
Np1 N1 2.494(4) . ?
Np1 C4 2.921(5) . ?
Np1 C5 2.961(5) . ?
Np1 C6 2.966(5) . ?
Np1 C1 2.922(5) . ?
Np1 C2 2.911(5) . ?
Np1 C3 2.913(5) . ?
O1 C43 1.435(7) . ?
O1 C44 1.428(7) . ?
C15 H2 0.9500 . ?
C15 C16 1.382(7) . ?
N1 C8 1.398(6) . ?
N1 C19 1.432(6) . ?
O2 C45 1.443(7) . ?
O2 C46 1.437(7) . ?
C16 H3 0.9500 . ?
C16 C17 1.379(7) . ?
O3 C47 1.435(6) . ?
O3 C48 1.427(7) . ?
C17 H4 0.9500 . ?
C17 C18 1.369(7) . ?
O4 C49 1.418(6) . ?
O4 C50 1.435(6) . ?
C18 H5 0.9500 . ?
C18 C13 1.393(7) . ?
C13 C4 1.482(7) . ?
C4 C5 1.394(7) . ?
C4 C3 1.411(6) . ?
C5 H8 0.9500 . ?
C5 C6 1.386(6) . ?
C6 H9 0.9500 . ?
C6 C1 1.398(6) . ?
C1 C2 1.405(7) . ?
C1 C7 1.490(6) . ?
C2 H11 0.9500 . ?
C2 C3 1.375(6) . ?
C3 H12 0.9500 . ?
C7 C12 1.400(7) . ?
C7 C8 1.426(6) . ?
C12 H14 0.9500 . ?
C12 C11 1.387(7) . ?
C11 H15 0.9500 . ?
C11 C10 1.374(7) . ?
C10 H16 0.9500 . ?
C10 C9 1.393(7) . ?
C9 H17 0.9500 . ?
C9 C8 1.408(6) . ?
C31 C32 1.400(7) . ?
C31 C36 1.410(7) . ?
C32 C33 1.404(7) . ?
C32 C37 1.521(7) . ?
C33 H21 0.9500 . ?
C33 C34 1.387(8) . ?
C34 H22 0.9500 . ?
C34 C35 1.367(8) . ?
C35 H23 0.9500 . ?
C35 C36 1.412(7) . ?
C36 C40 1.521(7) . ?
C40 H25 1.0000 . ?
C40 C41 1.531(8) . ?
C40 C42 1.539(7) . ?
C41 H26A 0.9800 . ?
C41 H26B 0.9800 . ?
C41 H26C 0.9800 . ?
C42 H27A 0.9800 . ?
C42 H27B 0.9800 . ?
C42 H27C 0.9800 . ?
C37 H28 1.0000 . ?
C37 C39 1.522(7) . ?
C37 C38 1.514(7) . ?
C39 H29A 0.9800 . ?
C39 H29B 0.9800 . ?
C39 H29C 0.9800 . ?
C38 H30A 0.9800 . ?
C38 H30B 0.9800 . ?
C38 H30C 0.9800 . ?
C19 C20 1.416(7) . ?
C19 C24 1.408(7) . ?
C20 C21 1.411(7) . ?
C20 C25 1.510(7) . ?
C21 H33 0.9500 . ?
C21 C22 1.364(7) . ?
C22 H34 0.9500 . ?
C22 C23 1.397(7) . ?
C23 H35 0.9500 . ?
C23 C24 1.393(7) . ?
C24 C28 1.515(7) . ?
C28 H37 1.0000 . ?
C28 C30 1.532(7) . ?
C28 C29 1.525(7) . ?
C30 H38A 0.9800 . ?
C30 H38B 0.9800 . ?
C30 H38C 0.9800 . ?
C29 H39A 0.9800 . ?
C29 H39B 0.9800 . ?
C29 H39C 0.9800 . ?
C25 H40 1.0000 . ?
C25 C26 1.524(8) . ?
C25 C27 1.523(7) . ?
C26 H41A 0.9800 . ?
C26 H41B 0.9800 . ?
C26 H41C 0.9800 . ?
C27 H42A 0.9800 . ?
C27 H42B 0.9800 . ?
C27 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.496(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.485(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
O5 C51 1.417(7) . ?
O5 C52 1.417(6) . ?
O6 C53 1.404(7) . ?
O6 C54 1.411(7) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.484(8) . ?
C53 H53 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?

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
N2 C14 C15 124.9(5) . . ?
N2 C14 C13 119.0(4) . . ?
C15 C14 C13 116.1(4) . . ?
O1 K1 Cl2 114.82(10) . . ?
O1 K1 O2 60.14(12) . . ?
O1 K1 O3 112.40(12) . . ?
O1 K1 O4 137.47(13) . . ?
O1 K1 C21 71.42(13) . . ?
O1 K1 C22 84.96(14) . . ?
O1 K1 C23 109.59(14) . . ?
O1 K1 C45 43.94(14) . . ?
Cl2 K1 C21 88.65(9) . . ?
Cl2 K1 C22 100.52(10) . . ?
Cl2 K1 C23 87.26(10) . . ?
Cl2 K1 C45 84.29(11) . . ?
O2 K1 Cl2 89.50(9) . . ?
O2 K1 C21 125.20(13) . . ?
O2 K1 C22 144.50(14) . . ?
O2 K1 C23 166.42(14) . . ?
O2 K1 C45 24.48(13) . . ?
O3 K1 Cl2 132.39(10) . . ?
O3 K1 O2 119.65(12) . . ?
O3 K1 O4 60.58(12) . . ?
O3 K1 C21 100.74(12) . . ?
O3 K1 C22 77.66(13) . . ?
O3 K1 C23 71.52(13) . . ?
O3 K1 C45 137.33(14) . . ?
O4 K1 Cl2 87.67(9) . . ?
O4 K1 O2 86.07(13) . . ?
O4 K1 C21 148.48(13) . . ?
O4 K1 C22 127.93(14) . . ?
O4 K1 C23 106.96(13) . . ?
O4 K1 C45 109.69(14) . . ?
C21 K1 C45 101.06(15) . . ?
C22 K1 C21 23.61(12) . . ?
C22 K1 C23 24.81(13) . . ?
C22 K1 C45 122.22(16) . . ?
C23 K1 C21 41.57(13) . . ?
C23 K1 C45 141.94(15) . . ?
C14 N2 Np1 128.8(3) . . ?
C14 N2 C31 113.1(4) . . ?
C31 N2 Np1 117.8(3) . . ?
Cl1 Np1 Cl2 100.09(5) . . ?
Cl1 Np1 C4 96.37(10) . . ?
Cl1 Np1 C5 74.53(11) . . ?
Cl1 Np1 C6 76.51(10) . . ?
Cl1 Np1 C1 100.44(11) . . ?
Cl1 Np1 C2 124.81(10) . . ?
Cl1 Np1 C3 122.60(10) . . ?
N2 Np1 Cl1 101.95(9) . . ?
N2 Np1 Cl2 87.39(9) . . ?
N2 Np1 N1 156.29(13) . . ?
N2 Np1 C4 61.07(13) . . ?
N2 Np1 C5 82.32(13) . . ?
N2 Np1 C6 108.41(13) . . ?
N2 Np1 C1 116.24(13) . . ?
N2 Np1 C2 95.22(13) . . ?
N2 Np1 C3 68.70(13) . . ?
Cl2 Np1 C4 146.90(11) . . ?
Cl2 Np1 C5 167.03(10) . . ?
Cl2 Np1 C6 164.18(10) . . ?
Cl2 Np1 C1 144.31(9) . . ?
Cl2 Np1 C2 133.04(10) . . ?
Cl2 Np1 C3 133.87(10) . . ?
N1 Np1 Cl1 101.61(9) . . ?
N1 Np1 Cl2 85.94(9) . . ?
N1 Np1 C4 118.58(13) . . ?
N1 Np1 C5 106.59(13) . . ?
N1 Np1 C6 79.74(13) . . ?
N1 Np1 C1 61.49(13) . . ?
N1 Np1 C2 73.26(13) . . ?
N1 Np1 C3 100.36(13) . . ?
C4 Np1 C5 27.41(13) . . ?
C4 Np1 C6 48.55(14) . . ?
C4 Np1 C1 57.64(13) . . ?
C5 Np1 C6 27.05(13) . . ?
C1 Np1 C5 48.55(13) . . ?
C1 Np1 C6 27.46(12) . . ?
C2 Np1 C4 48.97(13) . . ?
C2 Np1 C5 56.29(14) . . ?
C2 Np1 C6 48.31(14) . . ?
C2 Np1 C1 27.86(13) . . ?
C2 Np1 C3 27.31(12) . . ?
C3 Np1 C4 28.00(12) . . ?
C3 Np1 C5 48.43(13) . . ?
C3 Np1 C6 56.45(14) . . ?
C3 Np1 C1 49.05(13) . . ?
C43 O1 K1 128.1(4) . . ?
C44 O1 K1 119.2(4) . . ?
C44 O1 C43 111.9(5) . . ?
C14 C15 H2 119.3 . . ?
C16 C15 C14 121.5(5) . . ?
C16 C15 H2 119.3 . . ?
Np1 Cl2 K1 144.21(6) . . ?
C8 N1 Np1 129.0(3) . . ?
C8 N1 C19 111.0(4) . . ?
C19 N1 Np1 119.9(3) . . ?
C45 O2 K1 101.6(3) . . ?
C46 O2 K1 112.9(3) . . ?
C46 O2 C45 112.8(4) . . ?
C15 C16 H3 119.4 . . ?
C17 C16 C15 121.2(5) . . ?
C17 C16 H3 119.4 . . ?
C47 O3 K1 122.9(3) . . ?
C48 O3 K1 117.4(3) . . ?
C48 O3 C47 111.3(4) . . ?
C16 C17 H4 120.6 . . ?
C18 C17 C16 118.8(4) . . ?
C18 C17 H4 120.6 . . ?
C49 O4 K1 114.5(3) . . ?
C49 O4 C50 111.7(5) . . ?
C50 O4 K1 115.5(3) . . ?
C17 C18 H5 119.3 . . ?
C17 C18 C13 121.4(5) . . ?
C13 C18 H5 119.3 . . ?
C14 C13 C4 117.0(4) . . ?
C18 C13 C14 120.7(4) . . ?
C18 C13 C4 122.3(5) . . ?
C13 C4 Np1 110.5(3) . . ?
C5 C4 Np1 77.9(3) . . ?
C5 C4 C13 123.7(4) . . ?
C5 C4 C3 118.4(4) . . ?
C3 C4 Np1 75.7(3) . . ?
C3 C4 C13 117.5(4) . . ?
Np1 C5 H8 120.1 . . ?
C4 C5 Np1 74.7(3) . . ?
C4 C5 H8 119.5 . . ?
C6 C5 Np1 76.7(3) . . ?
C6 C5 C4 121.0(5) . . ?
C6 C5 H8 119.5 . . ?
Np1 C6 H9 120.6 . . ?
C5 C6 Np1 76.3(3) . . ?
C5 C6 H9 119.7 . . ?
C5 C6 C1 120.6(5) . . ?
C1 C6 Np1 74.5(3) . . ?
C1 C6 H9 119.7 . . ?
C6 C1 Np1 78.0(3) . . ?
C6 C1 C2 118.3(4) . . ?
C6 C1 C7 121.3(5) . . ?
C2 C1 Np1 75.6(3) . . ?
C2 C1 C7 120.3(4) . . ?
C7 C1 Np1 112.0(3) . . ?
Np1 C2 H11 118.5 . . ?
C1 C2 Np1 76.5(3) . . ?
C1 C2 H11 119.4 . . ?
C3 C2 Np1 76.4(3) . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H11 119.4 . . ?
Np1 C3 H12 118.4 . . ?
C4 C3 Np1 76.3(3) . . ?
C4 C3 H12 119.8 . . ?
C2 C3 Np1 76.3(3) . . ?
C2 C3 C4 120.4(5) . . ?
C2 C3 H12 119.8 . . ?
C12 C7 C1 121.0(4) . . ?
C12 C7 C8 122.1(4) . . ?
C8 C7 C1 116.9(4) . . ?
C7 C12 H14 119.9 . . ?
C11 C12 C7 120.3(5) . . ?
C11 C12 H14 119.9 . . ?
C12 C11 H15 120.6 . . ?
C10 C11 C12 118.8(5) . . ?
C10 C11 H15 120.6 . . ?
C11 C10 H16 119.2 . . ?
C11 C10 C9 121.6(5) . . ?
C9 C10 H16 119.2 . . ?
C10 C9 H17 119.1 . . ?
C10 C9 C8 121.9(5) . . ?
C8 C9 H17 119.1 . . ?
N1 C8 C7 119.6(4) . . ?
N1 C8 C9 125.0(4) . . ?
C9 C8 C7 115.3(4) . . ?
C32 C31 N2 118.9(4) . . ?
C32 C31 C36 120.9(5) . . ?
C36 C31 N2 120.2(4) . . ?
C31 C32 C33 118.4(5) . . ?
C31 C32 C37 121.4(5) . . ?
C33 C32 C37 120.3(5) . . ?
C32 C33 H21 119.3 . . ?
C34 C33 C32 121.5(5) . . ?
C34 C33 H21 119.3 . . ?
C33 C34 H22 120.2 . . ?
C35 C34 C33 119.5(5) . . ?
C35 C34 H22 120.2 . . ?
C34 C35 H23 119.2 . . ?
C34 C35 C36 121.6(5) . . ?
C36 C35 H23 119.2 . . ?
C31 C36 C35 118.1(5) . . ?
C31 C36 C40 121.8(5) . . ?
C35 C36 C40 120.1(5) . . ?
C36 C40 H25 107.7 . . ?
C36 C40 C41 112.7(4) . . ?
C36 C40 C42 111.0(5) . . ?
C41 C40 H25 107.7 . . ?
C41 C40 C42 109.7(4) . . ?
C42 C40 H25 107.7 . . ?
C40 C41 H26A 109.5 . . ?
C40 C41 H26B 109.5 . . ?
C40 C41 H26C 109.5 . . ?
H26A C41 H26B 109.5 . . ?
H26A C41 H26C 109.5 . . ?
H26B C41 H26C 109.5 . . ?
C40 C42 H27A 109.5 . . ?
C40 C42 H27B 109.5 . . ?
C40 C42 H27C 109.5 . . ?
H27A C42 H27B 109.5 . . ?
H27A C42 H27C 109.5 . . ?
H27B C42 H27C 109.5 . . ?
C32 C37 H28 107.9 . . ?
C32 C37 C39 110.5(4) . . ?
C39 C37 H28 107.9 . . ?
C38 C37 C32 112.6(4) . . ?
C38 C37 H28 107.9 . . ?
C38 C37 C39 110.0(5) . . ?
C37 C39 H29A 109.5 . . ?
C37 C39 H29B 109.5 . . ?
C37 C39 H29C 109.5 . . ?
H29A C39 H29B 109.5 . . ?
H29A C39 H29C 109.5 . . ?
H29B C39 H29C 109.5 . . ?
C37 C38 H30A 109.5 . . ?
C37 C38 H30B 109.5 . . ?
C37 C38 H30C 109.5 . . ?
H30A C38 H30B 109.5 . . ?
H30A C38 H30C 109.5 . . ?
H30B C38 H30C 109.5 . . ?
C20 C19 N1 120.0(4) . . ?
C24 C19 N1 119.8(4) . . ?
C24 C19 C20 120.2(4) . . ?
C19 C20 C25 123.4(4) . . ?
C21 C20 C19 118.0(5) . . ?
C21 C20 C25 118.6(5) . . ?
K1 C21 H33 106.4 . . ?
C20 C21 K1 94.6(3) . . ?
C20 C21 H33 118.9 . . ?
C22 C21 K1 69.2(3) . . ?
C22 C21 C20 122.2(5) . . ?
C22 C21 H33 118.9 . . ?
K1 C22 H34 100.6 . . ?
C21 C22 K1 87.1(3) . . ?
C21 C22 H34 120.5 . . ?
C21 C22 C23 119.0(5) . . ?
C23 C22 K1 82.1(3) . . ?
C23 C22 H34 120.5 . . ?
K1 C23 H35 102.1 . . ?
C22 C23 K1 73.1(3) . . ?
C22 C23 H35 119.3 . . ?
C24 C23 K1 94.9(3) . . ?
C24 C23 C22 121.5(5) . . ?
C24 C23 H35 119.3 . . ?
C19 C24 C28 121.5(4) . . ?
C23 C24 C19 119.0(5) . . ?
C23 C24 C28 119.6(5) . . ?
C24 C28 H37 107.9 . . ?
C24 C28 C30 113.0(5) . . ?
C24 C28 C29 111.3(4) . . ?
C30 C28 H37 107.9 . . ?
C29 C28 H37 107.9 . . ?
C29 C28 C30 108.7(5) . . ?
C28 C30 H38A 109.5 . . ?
C28 C30 H38B 109.5 . . ?
C28 C30 H38C 109.5 . . ?
H38A C30 H38B 109.5 . . ?
H38A C30 H38C 109.5 . . ?
H38B C30 H38C 109.5 . . ?
C28 C29 H39A 109.5 . . ?
C28 C29 H39B 109.5 . . ?
C28 C29 H39C 109.5 . . ?
H39A C29 H39B 109.5 . . ?
H39A C29 H39C 109.5 . . ?
H39B C29 H39C 109.5 . . ?
C20 C25 H40 107.4 . . ?
C20 C25 C26 110.8(5) . . ?
C20 C25 C27 112.4(5) . . ?
C26 C25 H40 107.4 . . ?
C27 C25 H40 107.4 . . ?
C27 C25 C26 111.2(5) . . ?
C25 C26 H41A 109.5 . . ?
C25 C26 H41B 109.5 . . ?
C25 C26 H41C 109.5 . . ?
H41A C26 H41B 109.5 . . ?
H41A C26 H41C 109.5 . . ?
H41B C26 H41C 109.5 . . ?
C25 C27 H42A 109.5 . . ?
C25 C27 H42B 109.5 . . ?
C25 C27 H42C 109.5 . . ?
H42A C27 H42B 109.5 . . ?
H42A C27 H42C 109.5 . . ?
H42B C27 H42C 109.5 . . ?
O1 C43 H43A 109.5 . . ?
O1 C43 H43B 109.5 . . ?
O1 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O1 C44 H44A 109.9 . . ?
O1 C44 H44B 109.9 . . ?
O1 C44 C45 109.1(5) . . ?
H44A C44 H44B 108.3 . . ?
C45 C44 H44A 109.9 . . ?
C45 C44 H44B 109.9 . . ?
K1 C45 H45A 161.2 . . ?
K1 C45 H45B 73.0 . . ?
O2 C45 K1 53.9(3) . . ?
O2 C45 C44 108.4(5) . . ?
O2 C45 H45A 110.0 . . ?
O2 C45 H45B 110.0 . . ?
C44 C45 K1 86.3(3) . . ?
C44 C45 H45A 110.0 . . ?
C44 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
O2 C46 H46A 109.5 . . ?
O2 C46 H46B 109.5 . . ?
O2 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O3 C47 H47A 109.5 . . ?
O3 C47 H47B 109.5 . . ?
O3 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 C48 H48A 109.7 . . ?
O3 C48 H48B 109.7 . . ?
O3 C48 C49 109.6(5) . . ?
H48A C48 H48B 108.2 . . ?
C49 C48 H48A 109.7 . . ?
C49 C48 H48B 109.7 . . ?
O4 C49 C48 111.2(5) . . ?
O4 C49 H49A 109.4 . . ?
O4 C49 H49B 109.4 . . ?
C48 C49 H49A 109.4 . . ?
C48 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
O4 C50 H50A 109.5 . . ?
O4 C50 H50B 109.5 . . ?
O4 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 O5 C51 112.8(5) . . ?
C53 O6 C54 111.5(5) . . ?
O5 C51 H51A 109.5 . . ?
O5 C51 H51B 109.5 . . ?
O5 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O5 C52 H52A 109.8 . . ?
O5 C52 H52B 109.8 . . ?
O5 C52 C53 109.2(5) . . ?
H52A C52 H52B 108.3 . . ?
C53 C52 H52A 109.8 . . ?
C53 C52 H52B 109.8 . . ?
O6 C53 C52 110.4(5) . . ?
O6 C53 H53 124.8 . . ?
C52 C53 H53 124.8 . . ?
O6 C54 H54A 109.5 . . ?
O6 C54 H54B 109.5 . . ?
O6 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 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
C14 N2 C31 C32 89.3(5) . . . . ?
C14 N2 C31 C36 -90.2(5) . . . . ?
C14 C15 C16 C17 0.0(8) . . . . ?
C14 C13 C4 Np1 -17.5(5) . . . . ?
C14 C13 C4 C5 -106.3(5) . . . . ?
C14 C13 C4 C3 66.6(6) . . . . ?
K1 O1 C44 C45 -14.5(6) . . . . ?
K1 O2 C45 C44 -70.9(5) . . . . ?
K1 O3 C48 C49 39.8(6) . . . . ?
K1 O4 C49 C48 49.3(6) . . . . ?
K1 C21 C22 C23 79.3(5) . . . . ?
K1 C22 C23 C24 85.3(5) . . . . ?
K1 C23 C24 C19 73.5(5) . . . . ?
K1 C23 C24 C28 -107.0(4) . . . . ?
N2 C14 C15 C16 175.0(5) . . . . ?
N2 C14 C13 C18 -173.7(5) . . . . ?
N2 C14 C13 C4 7.1(7) . . . . ?
N2 C31 C32 C33 179.5(4) . . . . ?
N2 C31 C32 C37 1.3(7) . . . . ?
N2 C31 C36 C35 -179.2(4) . . . . ?
N2 C31 C36 C40 1.0(7) . . . . ?
Np1 N2 C31 C32 -96.1(4) . . . . ?
Np1 N2 C31 C36 84.4(5) . . . . ?
Np1 N1 C8 C7 -7.2(6) . . . . ?
Np1 N1 C8 C9 173.0(4) . . . . ?
Np1 N1 C19 C20 -86.5(5) . . . . ?
Np1 N1 C19 C24 95.9(5) . . . . ?
Np1 C4 C5 C6 63.7(4) . . . . ?
Np1 C4 C3 C2 -64.8(4) . . . . ?
Np1 C5 C6 C1 62.4(4) . . . . ?
Np1 C6 C1 C2 66.3(4) . . . . ?
Np1 C6 C1 C7 -108.6(4) . . . . ?
Np1 C1 C2 C3 64.7(4) . . . . ?
Np1 C1 C7 C12 -174.2(4) . . . . ?
Np1 C1 C7 C8 8.7(5) . . . . ?
Np1 C2 C3 C4 64.8(4) . . . . ?
O1 C44 C45 K1 10.0(4) . . . . ?
O1 C44 C45 O2 60.0(7) . . . . ?
C15 C14 N2 Np1 -167.3(4) . . . . ?
C15 C14 N2 C31 6.5(7) . . . . ?
C15 C14 C13 C18 5.4(7) . . . . ?
C15 C14 C13 C4 -173.8(4) . . . . ?
C15 C16 C17 C18 2.9(8) . . . . ?
N1 C19 C20 C21 -173.3(4) . . . . ?
N1 C19 C20 C25 6.1(7) . . . . ?
N1 C19 C24 C23 173.5(4) . . . . ?
N1 C19 C24 C28 -6.0(7) . . . . ?
C16 C17 C18 C13 -1.5(8) . . . . ?
O3 C48 C49 O4 -58.9(7) . . . . ?
C17 C18 C13 C14 -2.8(8) . . . . ?
C17 C18 C13 C4 176.4(5) . . . . ?
C18 C13 C4 Np1 163.4(4) . . . . ?
C18 C13 C4 C5 74.6(7) . . . . ?
C18 C13 C4 C3 -112.5(5) . . . . ?
C13 C14 N2 Np1 11.7(6) . . . . ?
C13 C14 N2 C31 -174.4(4) . . . . ?
C13 C14 C15 C16 -4.1(7) . . . . ?
C13 C4 C5 Np1 106.7(4) . . . . ?
C13 C4 C5 C6 170.4(5) . . . . ?
C13 C4 C3 Np1 -105.9(4) . . . . ?
C13 C4 C3 C2 -170.7(4) . . . . ?
C4 C5 C6 Np1 -62.7(4) . . . . ?
C4 C5 C6 C1 -0.3(7) . . . . ?
C5 C4 C3 Np1 67.4(4) . . . . ?
C5 C4 C3 C2 2.6(7) . . . . ?
C5 C6 C1 Np1 -63.3(4) . . . . ?
C5 C6 C1 C2 3.0(7) . . . . ?
C5 C6 C1 C7 -171.8(5) . . . . ?
C6 C1 C2 Np1 -67.6(4) . . . . ?
C6 C1 C2 C3 -2.9(7) . . . . ?
C6 C1 C7 C12 -85.1(6) . . . . ?
C6 C1 C7 C8 97.7(6) . . . . ?
C1 C2 C3 Np1 -64.7(4) . . . . ?
C1 C2 C3 C4 0.1(7) . . . . ?
C1 C7 C12 C11 -177.2(5) . . . . ?
C1 C7 C8 N1 -2.7(7) . . . . ?
C1 C7 C8 C9 177.1(4) . . . . ?
C2 C1 C7 C12 100.1(6) . . . . ?
C2 C1 C7 C8 -77.0(6) . . . . ?
C3 C4 C5 Np1 -66.2(4) . . . . ?
C3 C4 C5 C6 -2.5(7) . . . . ?
C7 C1 C2 Np1 107.3(4) . . . . ?
C7 C1 C2 C3 172.0(4) . . . . ?
C7 C12 C11 C10 0.6(8) . . . . ?
C12 C7 C8 N1 -179.8(4) . . . . ?
C12 C7 C8 C9 0.0(7) . . . . ?
C12 C11 C10 C9 -0.7(8) . . . . ?
C11 C10 C9 C8 0.5(8) . . . . ?
C10 C9 C8 N1 179.6(5) . . . . ?
C10 C9 C8 C7 -0.1(7) . . . . ?
C8 N1 C19 C20 90.3(5) . . . . ?
C8 N1 C19 C24 -87.3(5) . . . . ?
C8 C7 C12 C11 -0.2(8) . . . . ?
C31 C32 C33 C34 -0.2(8) . . . . ?
C31 C32 C37 C39 108.5(6) . . . . ?
C31 C32 C37 C38 -128.1(5) . . . . ?
C31 C36 C40 C41 -119.3(5) . . . . ?
C31 C36 C40 C42 117.2(5) . . . . ?
C32 C31 C36 C35 1.3(7) . . . . ?
C32 C31 C36 C40 -178.5(4) . . . . ?
C32 C33 C34 C35 0.9(9) . . . . ?
C33 C32 C37 C39 -69.8(6) . . . . ?
C33 C32 C37 C38 53.6(6) . . . . ?
C33 C34 C35 C36 -0.5(9) . . . . ?
C34 C35 C36 C31 -0.6(8) . . . . ?
C34 C35 C36 C40 179.3(5) . . . . ?
C35 C36 C40 C41 60.9(6) . . . . ?
C35 C36 C40 C42 -62.6(7) . . . . ?
C36 C31 C32 C33 -1.0(7) . . . . ?
C36 C31 C32 C37 -179.2(4) . . . . ?
C37 C32 C33 C34 178.1(5) . . . . ?
C19 N1 C8 C7 176.3(4) . . . . ?
C19 N1 C8 C9 -3.4(7) . . . . ?
C19 C20 C21 K1 -69.2(4) . . . . ?
C19 C20 C21 C22 -0.8(8) . . . . ?
C19 C20 C25 C26 113.7(5) . . . . ?
C19 C20 C25 C27 -121.1(5) . . . . ?
C19 C24 C28 C30 -133.0(5) . . . . ?
C19 C24 C28 C29 104.4(5) . . . . ?
C20 C19 C24 C23 -4.1(7) . . . . ?
C20 C19 C24 C28 176.4(4) . . . . ?
C20 C21 C22 K1 -82.2(5) . . . . ?
C20 C21 C22 C23 -2.8(8) . . . . ?
C21 C20 C25 C26 -66.8(6) . . . . ?
C21 C20 C25 C27 58.3(7) . . . . ?
C21 C22 C23 K1 -82.3(5) . . . . ?
C21 C22 C23 C24 3.1(8) . . . . ?
C22 C23 C24 C19 0.4(8) . . . . ?
C22 C23 C24 C28 179.8(5) . . . . ?
C23 C24 C28 C30 47.6(6) . . . . ?
C23 C24 C28 C29 -75.0(6) . . . . ?
C24 C19 C20 C21 4.3(7) . . . . ?
C24 C19 C20 C25 -176.3(5) . . . . ?
C25 C20 C21 K1 111.4(4) . . . . ?
C25 C20 C21 C22 179.7(5) . . . . ?
C43 O1 C44 C45 175.3(5) . . . . ?
C46 O2 C45 K1 -121.2(5) . . . . ?
C46 O2 C45 C44 167.9(5) . . . . ?
C47 O3 C48 C49 -170.9(5) . . . . ?
C50 O4 C49 C48 -177.0(5) . . . . ?
O5 C52 C53 O6 69.8(6) . . . . ?
C51 O5 C52 C53 174.9(5) . . . . ?
C54 O6 C53 C52 -177.4(5) . . . . ?

_LANL_internal_archive_date      ?
_LANL_internal_coll_client       CAPG/JM/AJG
_LANL_internal_coll_date         2/4/21
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_frame_time   60s
_LANL_internal_coll_frame_width  0.5
_LANL_internal_coll_name         ms0486
_LANL_internal_coll_type         custom
_LANL_internal_coll_user         CAPG
_LANL_internal_LA-UR             ?
_LANL_internal_process_date      2/5/21
_LANL_internal_process_user      CAPG
_LANL_internal_refinement_date   2/6/21
_LANL_internal_refinement_user   CAPG
_LANL_internal_solution_date     2/5/21
_LANL_internal_solution_user     CAPG
_LANL_internal_validation_date   ?
_LANL_internal_validation_user   ?
_olex2_exptl_crystal_mounting_method 
'Coated in NVH oil, mounted insisde a quartz capillary that was sealed at both ends with capillary wax. The outside of the capillary was then coated in Tough As Nails clear nail varnish to provide shatter resistance.'
_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 2.469
_oxdiff_exptl_absorpt_empirical_full_min 0.233
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_2_U
_database_code_depnum_ccdc_archive 'CCDC 2238469'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_2_U                 
;
PROBLEM: Check Calcd Resid. Dens.  1.11Ang From U1             -3.75 eA-3
RESPONSE: We attribute this to absorption artifacts due to insufficient absortion corrections caused by the high Z uranium center 
;
# Added during the CSD deposition process: Friday 27 January 2023 07:56 PM
# end Validation Reply Form

# end Validation Reply Form
_audit_creation_date             2023-01-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H65.73 Cl2 K N2 O2 U'
_chemical_formula_sum            'C50 H65.73 Cl2 K N2 O2 U'
_chemical_formula_weight         1074.80
_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 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3428(16)
_cell_length_b                   16.9863(19)
_cell_length_c                   25.645(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.263(4)
_cell_angle_gamma                90
_cell_volume                     5811.0(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9442
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.84
_shelx_estimated_absorpt_T_max   0.467
_shelx_estimated_absorpt_T_min   0.381
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.746072
_exptl_absorpt_correction_T_min  0.605955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 266824 reflections, Rint = 0.0591
 (103563 with I > 3sig(I), Rint = 0.0384)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2163
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34546
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.652
_diffrn_reflns_theta_min         1.941
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14382
_reflns_number_total             17753
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.350
_refine_diff_density_min         -2.759
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         17753
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0474
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+22.0423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0856
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O010-C01M \\sim O010-C7
 with sigma of 0.02
 C7-C13 \\sim C01M-C01K
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13 \\sim C01K: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C7 \\sim C01M: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Others
 Sof(C3AA)=Sof(H3AB)=Sof(H3AC)=Sof(H3AD)=1-FVAR(1)
 Sof(C01I)=Sof(H0AA)=Sof(HE)=Sof(HF)=FVAR(1)
 Sof(C4AA)=Sof(H4AB)=Sof(H4AC)=Sof(H4AD)=1-FVAR(2)
 Sof(H00Q)=Sof(C01J)=Sof(H1AA)=Sof(HG)=Sof(HH)=FVAR(2)
 Sof(C01M)=Sof(H4AA)=Sof(HL)=1-FVAR(3)
 Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(3)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(4)
 Sof(C01K)=Sof(H2AA)=Sof(HI)=Sof(HJ)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C00U(H00U), C00X(H00X), C01E(H01W)
5.b Secondary CH2 refined with riding coordinates:
 C016(H01D,H01E), C01D(H01U,H01V), C01L(H3AA,HK), C01M(H4AA,HL), C7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C008(H008), C009(H009), C00D(H00D), C00G(H00G), C00N(H00N), C00O(H00O),
 C00P(H00P), C00R(H00R), C00T(H00T), C00V(H00V), C00W(H00W), C00Y(H00Y),
 C00Z(H00Z), C011(H011), C013(H013), C014(H014), C015(H015), C018(H018)
5.d Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C), C017(H01F,H01G,H01H), C019(H01I,H01J,H01K), C01A(H01L,
 H01M,H01N), C01B(H01O,H01P,H01Q), C01C(H01R,H01S,H01T), C01F(H01X,H01Y,H),
 C01G(H01Z,HA,HB), C01H(H01,HC,HD), C01I(H0AA,HE,HF), C01J(H1AA,HG,HH),
 C01K(H2AA,HI,HJ), C4AA(H4AB,H4AC,H4AD), C3AA(H3AB,H3AC,H3AD), C13(H13A,H13B,
 H13C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.59593(2) 0.48287(2) 0.66404(2) 0.02187(4) Uani 1 1 d . . . . .
K1 K 0.64946(6) 0.17052(5) 0.71638(4) 0.03346(18) Uani 1 1 d . . . . .
Cl1 Cl 0.49198(7) 0.52919(6) 0.74635(4) 0.03021(19) Uani 1 1 d . . . . .
Cl2 Cl 0.67600(8) 0.34710(6) 0.69915(5) 0.0451(3) Uani 1 1 d . . . . .
N2 N 0.4693(2) 0.39624(17) 0.61854(11) 0.0224(6) Uani 1 1 d . . . . .
O1 O 0.7529(2) 0.17720(18) 0.80893(11) 0.0369(7) Uani 1 1 d . . . . .
N1 N 0.7590(2) 0.54462(18) 0.68242(12) 0.0256(6) Uani 1 1 d . . . . .
C5 C 0.4609(3) 0.6071(2) 0.62475(14) 0.0251(7) Uani 1 1 d . . . . .
H008 H 0.398293 0.617431 0.640336 0.030 Uiso 1 1 calc R . . . .
C6 C 0.5459(3) 0.6492(2) 0.64117(15) 0.0271(7) Uani 1 1 d . . . . .
H009 H 0.540612 0.687710 0.667849 0.032 Uiso 1 1 calc R . . . .
C19 C 0.8363(3) 0.4965(2) 0.70656(15) 0.0268(8) Uani 1 1 d . . . . .
C13 C 0.3803(3) 0.4998(2) 0.57218(13) 0.0233(7) Uani 1 1 d . . . . .
C8 C 0.7922(3) 0.6206(2) 0.67180(14) 0.0251(7) Uani 1 1 d . . . . .
C2 C 0.6440(3) 0.5806(2) 0.57719(14) 0.0254(7) Uani 1 1 d . . . . .
H00D H 0.705642 0.572618 0.560152 0.030 Uiso 1 1 calc R . . . .
C1 C 0.6388(3) 0.6352(2) 0.61866(15) 0.0259(7) Uani 1 1 d . . . . .
C4 C 0.4669(3) 0.5504(2) 0.58584(13) 0.0239(7) Uani 1 1 d . . . . .
C3 C 0.5594(3) 0.5386(2) 0.56120(14) 0.0257(7) Uani 1 1 d . . . . .
H00G H 0.563841 0.501670 0.533520 0.031 Uiso 1 1 calc R . . . .
C31 C 0.4691(3) 0.3135(2) 0.62865(14) 0.0247(7) Uani 1 1 d . . . . .
C7 C 0.7328(3) 0.6706(2) 0.63987(15) 0.0262(7) Uani 1 1 d . . . . .
C32 C 0.4172(3) 0.2828(2) 0.67184(15) 0.0277(8) Uani 1 1 d . . . . .
C20 C 0.8446(3) 0.4908(2) 0.76119(15) 0.0288(8) Uani 1 1 d . . . . .
C14 C 0.3868(3) 0.4201(2) 0.58838(13) 0.0241(7) Uani 1 1 d . . . . .
C24 C 0.9044(3) 0.4571(2) 0.67469(16) 0.0286(8) Uani 1 1 d . . . . .
C23 C 0.9809(3) 0.4128(2) 0.69855(18) 0.0346(9) Uani 1 1 d . . . . .
H00N H 1.027345 0.385826 0.677444 0.042 Uiso 1 1 calc R . . . .
C15 C 0.3054(3) 0.3711(2) 0.57332(15) 0.0300(8) Uani 1 1 d . . . . .
H00O H 0.307130 0.316714 0.582005 0.036 Uiso 1 1 calc R . . . .
C33 C 0.4154(3) 0.2013(2) 0.67946(16) 0.0312(8) Uani 1 1 d . . . . .
H00P H 0.381385 0.180474 0.708534 0.037 Uiso 1 1 calc R . . . .
C28 C 0.8961(3) 0.4617(2) 0.61566(17) 0.0324(9) Uani 1 1 d . . . . .
H00Q H 0.840(5) 0.482(4) 0.606(2) 0.039 Uiso 0.727(13) 1 d R . P A 4
C18 C 0.2965(3) 0.5287(3) 0.54522(14) 0.0314(8) Uani 1 1 d . . . . .
H00R H 0.294033 0.582670 0.535672 0.038 Uiso 1 1 calc R . . . .
C36 C 0.5180(3) 0.2610(2) 0.59534(15) 0.0292(8) Uani 1 1 d . . . . .
C9 C 0.8834(3) 0.6534(2) 0.69146(16) 0.0306(8) Uani 1 1 d . . . . .
H00T H 0.926059 0.622593 0.713486 0.037 Uiso 1 1 calc R . . . .
C25 C 0.7728(3) 0.5330(2) 0.79706(16) 0.0330(9) Uani 1 1 d . . . . .
H00U H 0.721811 0.560991 0.774694 0.040 Uiso 1 1 calc R . . . .
C22 C 0.9903(3) 0.4075(3) 0.75202(18) 0.0365(9) Uani 1 1 d . . . . .
H00V H 1.043444 0.377834 0.767525 0.044 Uiso 1 1 calc R . . . .
C21 C 0.9220(3) 0.4454(2) 0.78299(17) 0.0338(9) Uani 1 1 d . . . . .
H00W H 0.927869 0.440537 0.819829 0.041 Uiso 1 1 calc R . . . .
C40 C 0.3632(3) 0.3355(2) 0.70936(16) 0.0344(9) Uani 1 1 d . . . . .
H00X H 0.373199 0.391142 0.697793 0.041 Uiso 1 1 calc R . . . .
C12 C 0.7616(3) 0.7469(2) 0.62819(17) 0.0325(8) Uani 1 1 d . . . . .
H00Y H 0.718997 0.778799 0.606852 0.039 Uiso 1 1 calc R . . . .
C17 C 0.2168(3) 0.4799(3) 0.53209(15) 0.0349(9) Uani 1 1 d . . . . .
H00Z H 0.159266 0.499838 0.514019 0.042 Uiso 1 1 calc R . . . .
O2 O 0.7988(3) 0.0991(2) 0.66353(16) 0.0604(10) Uani 1 1 d D . . . .
C10 C 0.9110(3) 0.7293(2) 0.67908(18) 0.0355(9) Uani 1 1 d . . . . .
H011 H 0.972583 0.749448 0.692787 0.043 Uiso 1 1 calc R . . . .
C26 C 0.7171(3) 0.4738(3) 0.83095(18) 0.0431(10) Uani 1 1 d . . . . .
H01A H 0.683152 0.434898 0.808523 0.065 Uiso 1 1 calc GR . . . .
H01B H 0.667477 0.501538 0.851694 0.065 Uiso 1 1 calc GR . . . .
H01C H 0.765194 0.446927 0.854291 0.065 Uiso 1 1 calc GR . . . .
C35 C 0.5132(3) 0.1808(2) 0.60384(17) 0.0344(9) Uani 1 1 d . . . . .
H013 H 0.545489 0.145938 0.580641 0.041 Uiso 1 1 calc R . . . .
C34 C 0.4619(3) 0.1506(2) 0.64570(16) 0.0346(9) Uani 1 1 d . . . . .
H014 H 0.458806 0.095369 0.651119 0.042 Uiso 1 1 calc R . . . .
C11 C 0.8518(3) 0.7772(2) 0.64729(19) 0.0389(10) Uani 1 1 d . . . . .
H015 H 0.872311 0.829125 0.638833 0.047 Uiso 1 1 calc R . . . .
C45 C 0.7745(4) 0.2530(3) 0.83130(18) 0.0437(11) Uani 1 1 d . . . . .
H01D H 0.753584 0.294509 0.806204 0.052 Uiso 1 1 calc R . . . .
H01E H 0.847751 0.257930 0.837403 0.052 Uiso 1 1 calc R . . . .
C41 C 0.2498(4) 0.3196(3) 0.7090(2) 0.0522(13) Uani 1 1 d . . . . .
H01F H 0.222767 0.324405 0.673291 0.078 Uiso 1 1 calc GR . . . .
H01G H 0.216887 0.357994 0.731445 0.078 Uiso 1 1 calc GR . . . .
H01H H 0.237445 0.266333 0.722001 0.078 Uiso 1 1 calc GR . . . .
C16 C 0.2230(3) 0.4014(3) 0.54596(16) 0.0356(9) Uani 1 1 d . . . . .
H018 H 0.169287 0.367150 0.536532 0.043 Uiso 1 1 calc R . . . .
C43 C 0.7869(3) 0.0401(3) 0.8043(2) 0.0466(11) Uani 1 1 d . . . . .
H01I H 0.803553 0.044188 0.767363 0.070 Uiso 1 1 calc GR . . . .
H01J H 0.715057 0.029638 0.807363 0.070 Uiso 1 1 calc GR . . . .
H01K H 0.825291 -0.002988 0.820431 0.070 Uiso 1 1 calc GR . . . .
C42 C 0.4060(4) 0.3283(3) 0.76452(18) 0.0499(12) Uani 1 1 d . . . . .
H01L H 0.384844 0.278207 0.779664 0.075 Uiso 1 1 calc GR . . . .
H01M H 0.381368 0.371923 0.785765 0.075 Uiso 1 1 calc GR . . . .
H01N H 0.479334 0.330266 0.763735 0.075 Uiso 1 1 calc GR . . . .
C47 C 0.9065(4) 0.2024(3) 0.6942(2) 0.0564(14) Uani 1 1 d . . . . .
H01O H 0.862152 0.240958 0.677026 0.085 Uiso 1 1 calc GR . . . .
H01P H 0.975757 0.221443 0.693661 0.085 Uiso 1 1 calc GR . . . .
H01Q H 0.886266 0.195151 0.730370 0.085 Uiso 1 1 calc GR . . . .
C27 C 0.8258(3) 0.5940(3) 0.83093(18) 0.0436(11) Uani 1 1 d . . . . .
H01R H 0.874768 0.567879 0.854089 0.065 Uiso 1 1 calc GR . . . .
H01S H 0.776493 0.621889 0.851871 0.065 Uiso 1 1 calc GR . . . .
H01T H 0.860344 0.631782 0.808688 0.065 Uiso 1 1 calc GR . . . .
C44 C 0.8125(3) 0.1153(3) 0.83122(18) 0.0382(10) Uani 1 1 d . . . . .
H01U H 0.799230 0.110658 0.868922 0.046 Uiso 1 1 calc R . . . .
H01V H 0.884501 0.127283 0.827150 0.046 Uiso 1 1 calc R . . . .
C37 C 0.5737(4) 0.2913(3) 0.54783(17) 0.0405(10) Uani 1 1 d . . . . .
H01W H 0.579111 0.349894 0.550471 0.049 Uiso 1 1 calc R . . . .
C39 C 0.5160(5) 0.2710(4) 0.4976(2) 0.0605(15) Uani 1 1 d . . . . .
H01X H 0.511468 0.213676 0.493947 0.091 Uiso 1 1 calc GR . . . .
H01Y H 0.551074 0.292947 0.467702 0.091 Uiso 1 1 calc GR . . . .
H H 0.448375 0.293368 0.498779 0.091 Uiso 1 1 calc GR . . . .
C38 C 0.6798(4) 0.2569(4) 0.5461(2) 0.0683(18) Uani 1 1 d . . . . .
H01Z H 0.715261 0.267490 0.579238 0.102 Uiso 1 1 calc GR . . . .
HA H 0.716181 0.281241 0.517516 0.102 Uiso 1 1 calc GR . . . .
HB H 0.675771 0.199890 0.540480 0.102 Uiso 1 1 calc GR . . . .
C46 C 0.7223(6) 0.2660(3) 0.8818(2) 0.0728(19) Uani 1 1 d . . . . .
H01 H 0.649651 0.262257 0.875827 0.109 Uiso 1 1 calc GR . . . .
HC H 0.739208 0.318363 0.895375 0.109 Uiso 1 1 calc GR . . . .
HD H 0.743939 0.225869 0.907038 0.109 Uiso 1 1 calc GR . . . .
C30 C 0.9682(6) 0.5210(6) 0.5930(2) 0.046(2) Uani 0.727(18) 1 d . . P A 2
H0AA H 0.952977 0.573584 0.606290 0.070 Uiso 0.727(18) 1 calc GR . P A 2
HE H 0.961130 0.520860 0.554841 0.070 Uiso 0.727(18) 1 calc GR . P A 2
HF H 1.037096 0.506705 0.603092 0.070 Uiso 0.727(18) 1 calc GR . P A 2
C29 C 0.9167(6) 0.3806(4) 0.5892(3) 0.051(2) Uani 0.727(13) 1 d . . P A 4
H1AA H 0.987175 0.366037 0.595071 0.077 Uiso 0.727(13) 1 calc GR . P A 4
HG H 0.902410 0.384516 0.551669 0.077 Uiso 0.727(13) 1 calc GR . P A 4
HH H 0.873594 0.340246 0.604345 0.077 Uiso 0.727(13) 1 calc GR . P A 4
C50 C 0.6902(6) -0.0057(4) 0.6352(3) 0.062(2) Uani 0.793(14) 1 d D U P B 1
H2AA H 0.654729 0.032335 0.612721 0.093 Uiso 0.793(14) 1 calc GR . P B 1
HI H 0.657879 -0.008208 0.669062 0.093 Uiso 0.793(14) 1 calc GR . P B 1
HJ H 0.688060 -0.057772 0.618714 0.093 Uiso 0.793(14) 1 calc GR . P B 1
C48 C 0.8992(5) 0.1265(5) 0.6662(3) 0.091(2) Uani 1 1 d . . . . .
H3AA H 0.924511 0.132971 0.630493 0.109 Uiso 1 1 calc R . . . .
HK H 0.941747 0.086966 0.684479 0.109 Uiso 1 1 calc R . . . .
C49 C 0.7930(7) 0.0186(7) 0.6425(5) 0.075(4) Uani 0.76(2) 1 d D U P B 1
H4AA H 0.827339 0.016524 0.608657 0.090 Uiso 0.76(2) 1 calc R . P B 1
HL H 0.827798 -0.018051 0.666795 0.090 Uiso 0.76(2) 1 calc R . P B 1
C29b C 0.8294(15) 0.3991(10) 0.5943(7) 0.046(6) Uani 0.273(13) 1 d . . P A 3
H4AB H 0.856367 0.347429 0.604151 0.069 Uiso 0.273(13) 1 calc GR . P A 3
H4AC H 0.825540 0.403383 0.556222 0.069 Uiso 0.273(13) 1 calc GR . P A 3
H4AD H 0.762235 0.405262 0.608489 0.069 Uiso 0.273(13) 1 calc GR . P A 3
C30b C 0.9931(11) 0.4684(14) 0.5901(6) 0.037(5) Uani 0.273(18) 1 d . . P A 1
H3AB H 1.035082 0.506973 0.608749 0.056 Uiso 0.273(18) 1 calc GR . P A 1
H3AC H 0.982346 0.485619 0.553907 0.056 Uiso 0.273(18) 1 calc GR . P A 1
H3AD H 1.026727 0.417083 0.590478 0.056 Uiso 0.273(18) 1 calc GR . P A 1
C49b C 0.768(3) 0.0565(19) 0.6162(9) 0.085(10) Uani 0.24(2) 1 d D U P B 2
H7A H 0.693935 0.054254 0.612065 0.102 Uiso 0.24(2) 1 calc R . P B 2
H7B H 0.796753 0.080068 0.584592 0.102 Uiso 0.24(2) 1 calc R . P B 2
C50b C 0.809(4) -0.018(2) 0.627(2) 0.129(19) Uani 0.207(14) 1 d D U P B 2
H13A H 0.882051 -0.013962 0.631401 0.193 Uiso 0.207(14) 1 calc GR . P B 2
H13B H 0.793077 -0.054402 0.598214 0.193 Uiso 0.207(14) 1 calc GR . P B 2
H13C H 0.780840 -0.039095 0.659317 0.193 Uiso 0.207(14) 1 calc GR . P B 2


_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 Cl1 2.6697(9) . ?
U1 Cl2 2.6886(10) . ?
U1 N2 2.509(3) . ?
U1 N1 2.452(3) . ?
U1 C5 2.939(3) . ?
U1 C6 2.959(4) . ?
U1 C2 2.862(4) . ?
U1 C1 2.899(4) . ?
U1 C4 2.854(3) . ?
U1 C3 2.834(3) . ?
K1 Cl1 3.2120(13) 2_646 ?
K1 Cl2 3.0537(14) . ?
K1 O1 2.721(3) . ?
K1 C33 3.285(4) . ?
K1 O2 2.720(4) . ?
K1 C35 3.382(4) . ?
K1 C34 3.076(4) . ?
K1 C47 3.530(5) . ?
N2 C31 1.429(5) . ?
N2 C14 1.391(4) . ?
O1 C45 1.437(5) . ?
O1 C44 1.429(5) . ?
N1 C19 1.445(4) . ?
N1 C8 1.393(5) . ?
C5 C6 1.398(5) . ?
C5 C4 1.391(5) . ?
C6 C1 1.399(5) . ?
C19 C20 1.406(5) . ?
C19 C24 1.405(5) . ?
C13 C4 1.476(5) . ?
C13 C14 1.418(5) . ?
C13 C18 1.391(5) . ?
C8 C7 1.412(5) . ?
C8 C9 1.420(5) . ?
C2 C1 1.414(5) . ?
C2 C3 1.389(5) . ?
C1 C7 1.484(5) . ?
C4 C3 1.414(5) . ?
C31 C32 1.419(5) . ?
C31 C36 1.405(5) . ?
C7 C12 1.385(5) . ?
C32 C33 1.398(5) . ?
C32 C40 1.509(6) . ?
C20 C25 1.522(6) . ?
C20 C21 1.396(5) . ?
C14 C15 1.415(5) . ?
C24 C23 1.398(5) . ?
C24 C28 1.517(6) . ?
C23 C22 1.377(6) . ?
C15 C16 1.391(5) . ?
C33 C34 1.379(6) . ?
C28 C30 1.518(8) . ?
C28 C29 1.563(8) . ?
C28 C29b 1.482(15) . ?
C28 C30b 1.469(15) . ?
C18 C17 1.385(6) . ?
C36 C35 1.381(5) . ?
C36 C37 1.530(6) . ?
C9 C10 1.381(6) . ?
C25 C26 1.532(6) . ?
C25 C27 1.517(6) . ?
C22 C21 1.381(6) . ?
C40 C41 1.536(6) . ?
C40 C42 1.519(6) . ?
C12 C11 1.389(6) . ?
C17 C16 1.381(6) . ?
O2 C48 1.418(7) . ?
O2 C49 1.472(10) . ?
O2 C49b 1.466(18) . ?
C10 C11 1.386(6) . ?
C35 C34 1.384(6) . ?
C45 C46 1.499(7) . ?
C43 C44 1.488(6) . ?
C47 C48 1.477(9) . ?
C37 C39 1.526(7) . ?
C37 C38 1.533(7) . ?
C50 C49 1.441(11) . ?
C49b C50b 1.41(2) . ?

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
Cl1 U1 Cl2 101.39(4) . . ?
Cl1 U1 C5 74.58(8) . . ?
Cl1 U1 C6 75.91(8) . . ?
Cl1 U1 C2 125.00(8) . . ?
Cl1 U1 C1 99.49(8) . . ?
Cl1 U1 C4 96.97(7) . . ?
Cl1 U1 C3 123.76(8) . . ?
Cl2 U1 C5 165.24(8) . . ?
Cl2 U1 C6 166.33(8) . . ?
Cl2 U1 C2 131.61(8) . . ?
Cl2 U1 C1 145.04(8) . . ?
Cl2 U1 C4 143.98(8) . . ?
Cl2 U1 C3 131.07(8) . . ?
N2 U1 Cl1 100.62(7) . . ?
N2 U1 Cl2 84.90(7) . . ?
N2 U1 C5 81.98(10) . . ?
N2 U1 C6 108.75(10) . . ?
N2 U1 C2 97.95(10) . . ?
N2 U1 C1 118.27(10) . . ?
N2 U1 C4 61.27(10) . . ?
N2 U1 C3 70.30(10) . . ?
N1 U1 Cl1 101.32(8) . . ?
N1 U1 Cl2 87.60(7) . . ?
N1 U1 N2 157.81(10) . . ?
N1 U1 C5 107.07(10) . . ?
N1 U1 C6 79.91(10) . . ?
N1 U1 C2 71.85(10) . . ?
N1 U1 C1 60.88(10) . . ?
N1 U1 C4 118.83(10) . . ?
N1 U1 C3 99.77(11) . . ?
C5 U1 C6 27.43(10) . . ?
C2 U1 C5 57.50(10) . . ?
C2 U1 C6 49.09(10) . . ?
C2 U1 C1 28.41(10) . . ?
C1 U1 C5 49.17(10) . . ?
C1 U1 C6 27.60(10) . . ?
C4 U1 C5 27.74(10) . . ?
C4 U1 C6 49.26(10) . . ?
C4 U1 C2 50.37(10) . . ?
C4 U1 C1 58.72(10) . . ?
C3 U1 C5 49.43(10) . . ?
C3 U1 C6 57.54(10) . . ?
C3 U1 C2 28.22(10) . . ?
C3 U1 C1 50.20(11) . . ?
C3 U1 C4 28.77(10) . . ?
Cl1 K1 C33 69.14(7) 2_646 . ?
Cl1 K1 C35 89.10(8) 2_646 . ?
Cl1 K1 C47 137.89(10) 2_646 . ?
Cl2 K1 Cl1 147.99(4) . 2_646 ?
Cl2 K1 C33 85.08(8) . . ?
Cl2 K1 C35 83.54(7) . . ?
Cl2 K1 C34 96.78(8) . . ?
Cl2 K1 C47 73.13(9) . . ?
O1 K1 Cl1 93.53(7) . 2_646 ?
O1 K1 Cl2 91.55(7) . . ?
O1 K1 C33 134.85(10) . . ?
O1 K1 C35 174.25(10) . . ?
O1 K1 C34 155.35(11) . . ?
O1 K1 C47 70.04(12) . . ?
C33 K1 C35 41.92(10) . . ?
C33 K1 C47 148.17(12) . . ?
O2 K1 Cl1 104.89(9) . 2_646 ?
O2 K1 Cl2 106.08(10) . . ?
O2 K1 O1 95.17(11) . . ?
O2 K1 C33 129.03(12) . . ?
O2 K1 C35 89.08(12) . . ?
O2 K1 C34 104.65(12) . . ?
O2 K1 C47 42.52(13) . . ?
C35 K1 C47 111.12(13) . . ?
C34 K1 Cl1 67.52(8) . 2_646 ?
C34 K1 C33 24.75(11) . . ?
C34 K1 C35 24.16(11) . . ?
C34 K1 C47 134.61(13) . . ?
U1 Cl1 K1 140.75(4) . 2_656 ?
U1 Cl2 K1 147.62(4) . . ?
C31 N2 U1 119.8(2) . . ?
C14 N2 U1 127.2(2) . . ?
C14 N2 C31 112.5(3) . . ?
C45 O1 K1 118.6(3) . . ?
C44 O1 K1 125.8(3) . . ?
C44 O1 C45 113.2(3) . . ?
C19 N1 U1 117.5(2) . . ?
C8 N1 U1 130.1(2) . . ?
C8 N1 C19 112.4(3) . . ?
C6 C5 U1 77.1(2) . . ?
C4 C5 U1 72.74(19) . . ?
C4 C5 C6 120.7(3) . . ?
C5 C6 U1 75.5(2) . . ?
C5 C6 C1 120.6(3) . . ?
C1 C6 U1 73.8(2) . . ?
C20 C19 N1 120.3(3) . . ?
C24 C19 N1 119.0(3) . . ?
C24 C19 C20 120.6(3) . . ?
C14 C13 C4 116.3(3) . . ?
C18 C13 C4 121.9(3) . . ?
C18 C13 C14 121.7(3) . . ?
N1 C8 C7 119.6(3) . . ?
N1 C8 C9 124.6(3) . . ?
C7 C8 C9 115.8(3) . . ?
C1 C2 U1 77.3(2) . . ?
C3 C2 U1 74.8(2) . . ?
C3 C2 C1 120.4(3) . . ?
C6 C1 U1 78.6(2) . . ?
C6 C1 C2 118.7(3) . . ?
C6 C1 C7 122.0(3) . . ?
C2 C1 U1 74.3(2) . . ?
C2 C1 C7 119.1(3) . . ?
C7 C1 U1 112.8(2) . . ?
C5 C4 U1 79.5(2) . . ?
C5 C4 C13 121.1(3) . . ?
C5 C4 C3 118.9(3) . . ?
C13 C4 U1 112.9(2) . . ?
C3 C4 U1 74.81(19) . . ?
C3 C4 C13 119.9(3) . . ?
C2 C3 U1 77.0(2) . . ?
C2 C3 C4 120.5(3) . . ?
C4 C3 U1 76.4(2) . . ?
C32 C31 N2 120.4(3) . . ?
C36 C31 N2 120.7(3) . . ?
C36 C31 C32 118.8(3) . . ?
C8 C7 C1 115.3(3) . . ?
C12 C7 C8 122.3(4) . . ?
C12 C7 C1 122.4(3) . . ?
C31 C32 C40 121.9(3) . . ?
C33 C32 C31 118.9(4) . . ?
C33 C32 C40 119.2(4) . . ?
C19 C20 C25 122.2(3) . . ?
C21 C20 C19 118.5(4) . . ?
C21 C20 C25 119.2(4) . . ?
N2 C14 C13 118.9(3) . . ?
N2 C14 C15 125.0(3) . . ?
C15 C14 C13 116.1(3) . . ?
C19 C24 C28 121.5(3) . . ?
C23 C24 C19 118.5(4) . . ?
C23 C24 C28 120.1(4) . . ?
C22 C23 C24 121.4(4) . . ?
C16 C15 C14 120.9(4) . . ?
C32 C33 K1 100.3(2) . . ?
C34 C33 K1 69.1(2) . . ?
C34 C33 C32 121.4(4) . . ?
C24 C28 C29 112.2(4) . . ?
C30 C28 C24 112.5(4) . . ?
C29b C28 C24 111.2(7) . . ?
C30b C28 C24 113.8(7) . . ?
C17 C18 C13 121.0(4) . . ?
C31 C36 C37 120.7(3) . . ?
C35 C36 C31 120.4(4) . . ?
C35 C36 C37 118.8(4) . . ?
C10 C9 C8 121.1(4) . . ?
C20 C25 C26 110.7(3) . . ?
C27 C25 C20 112.1(3) . . ?
C27 C25 C26 110.5(4) . . ?
C23 C22 C21 119.7(4) . . ?
C22 C21 C20 121.3(4) . . ?
C32 C40 C41 112.1(4) . . ?
C32 C40 C42 111.8(4) . . ?
C42 C40 C41 110.0(4) . . ?
C7 C12 C11 120.8(4) . . ?
C16 C17 C18 118.2(4) . . ?
C48 O2 K1 122.1(4) . . ?
C48 O2 C49 111.4(5) . . ?
C48 O2 C49b 116.9(15) . . ?
C49 O2 K1 124.3(4) . . ?
C49b O2 K1 115.9(15) . . ?
C9 C10 C11 122.1(4) . . ?
C36 C35 K1 99.2(2) . . ?
C36 C35 C34 120.9(4) . . ?
C34 C35 K1 65.4(2) . . ?
C33 C34 K1 86.2(2) . . ?
C33 C34 C35 119.5(4) . . ?
C35 C34 K1 90.4(2) . . ?
C10 C11 C12 117.9(4) . . ?
O1 C45 C46 112.5(4) . . ?
C17 C16 C15 122.0(4) . . ?
C48 C47 K1 83.7(3) . . ?
O1 C44 C43 109.0(3) . . ?
C36 C37 C38 111.1(4) . . ?
C39 C37 C36 110.6(4) . . ?
C39 C37 C38 109.8(4) . . ?
O2 C48 C47 111.2(5) . . ?
C50 C49 O2 110.9(7) . . ?
C50b C49b O2 100(2) . . ?

_smtbx_masks_special_details     ?
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 -0.507 0.000 0.500 693.6 115.8 Hexane
2 -0.759 0.500 1.000 693.6 115.8 Hexane

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT972_u_anlg_0m_4a        
;
PROBLEM: Check Calcd Resid. Dens. 1.11Ang From U001 -3.77 eA-3
RESPONSE: We attribute this to absorption artifacts due to insufficient
absortion corrections caused by the high Z uranium center 
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_3_Ce
_database_code_depnum_ccdc_archive 'CCDC 2238470'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_audit_creation_date             2022-10-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H54 Ce I N2 O, C4 H10 O'
_chemical_formula_sum            'C50 H64 Ce I N2 O2'
_chemical_formula_weight         992.05
_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 0.0033 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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.4528(4)
_cell_length_b                   21.5419(9)
_cell_length_c                   18.1661(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.817(2)
_cell_angle_gamma                90
_cell_volume                     4428.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.719
_shelx_estimated_absorpt_T_min   0.332
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0782 before and 0.0579 after correction. The Ratio of minimum to maximum transmission is 0.9046. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            75264
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.557
_diffrn_reflns_theta_min         2.033
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10781
_reflns_number_total             13549
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.725
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         13549
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0303
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0324P)²+0.9560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0728
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00Q(H00Q), C00V(H00V), C00Z(H00Z), C011(H011)
2.b Secondary CH2 refined with riding coordinates:
 C010(H01A,H01B), C016(H01F,H01G), C01A(H01K,H01L), C01G(H01Z,HB), C01H(H01,
 HC), C01K(H2AA,HH)
2.c Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C00A(H00A), C00F(H00F), C00J(H00J), C00M(H00M),
 C00O(H00O), C00P(H00P), C00R(H00R), C00T(H00T), C00U(H00U), C00X(H00X),
 C00Y(H00Y), C012(H012), C013(H013), C014(H014), C017(H017), C018(H018)
2.d Idealised Me refined as rotating group:
 C00S(H00B,H00C,H00D), C015(H01C,H01D,H01E), C019(H01H,H01I,H01J), C01B(H01M,
 H01N,H01O), C01C(H01P,H01Q,H01R), C01D(H01S,H01T,H01U), C01E(H01V,H01W,H01X),
 C01F(H01Y,H,HA), C01I(H0AA,HD,HE), C01J(H1AA,HF,HG)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Ce00 Ce 0.53342(2) 0.71890(2) 0.67280(2) 0.01278(4) Uani 1 1 d . . . . .
I1 I 0.39305(2) 0.79783(2) 0.77040(2) 0.02183(4) Uani 1 1 d . . . . .
O1 O 0.66429(14) 0.66988(8) 0.77843(9) 0.0197(3) Uani 1 1 d . . . . .
N2 N 0.40795(16) 0.62719(8) 0.64974(10) 0.0149(4) Uani 1 1 d . . . . .
N1 N 0.70393(16) 0.78885(8) 0.65917(10) 0.0144(4) Uani 1 1 d . . . . .
C1 C 0.51274(19) 0.80718(10) 0.54784(12) 0.0136(4) Uani 1 1 d . . . . .
C3 C 0.4620(2) 0.70152(10) 0.50907(12) 0.0154(4) Uani 1 1 d . . . . .
H007 H 0.481619 0.663665 0.487073 0.019 Uiso 1 1 calc R . . . .
C6 C 0.4030(2) 0.81413(10) 0.56897(12) 0.0165(4) Uani 1 1 d . . . . .
H008 H 0.381249 0.852929 0.587731 0.020 Uiso 1 1 calc R . . . .
C19 C 0.81385(19) 0.78009(10) 0.70821(12) 0.0143(4) Uani 1 1 d . . . . .
C2 C 0.54118(19) 0.75030(10) 0.51591(12) 0.0150(4) Uani 1 1 d . . . . .
H00A H 0.615220 0.745633 0.499060 0.018 Uiso 1 1 calc R . . . .
C14 C 0.31378(19) 0.61009(10) 0.59582(12) 0.0153(4) Uani 1 1 d . . . . .
C4 C 0.3523(2) 0.70754(10) 0.53455(13) 0.0160(4) Uani 1 1 d . . . . .
C7 C 0.60489(19) 0.85549(10) 0.56097(12) 0.0143(4) Uani 1 1 d . . . . .
C13 C 0.27838(19) 0.65137(10) 0.53573(12) 0.0152(4) Uani 1 1 d . . . . .
C5 C 0.3225(2) 0.76415(11) 0.56300(13) 0.0183(5) Uani 1 1 d . . . . .
H00F H 0.247625 0.769271 0.578546 0.022 Uiso 1 1 calc R . . . .
C8 C 0.70565(19) 0.84107(10) 0.61398(12) 0.0147(4) Uani 1 1 d . . . . .
C31 C 0.4441(2) 0.58043(10) 0.70516(12) 0.0163(4) Uani 1 1 d . . . . .
C32 C 0.5247(2) 0.53400(11) 0.68998(13) 0.0200(5) Uani 1 1 d . . . . .
C18 C 0.1854(2) 0.63724(11) 0.48004(13) 0.0200(5) Uani 1 1 d . . . . .
H00J H 0.163230 0.665958 0.440692 0.024 Uiso 1 1 calc R . . . .
O2 O 1.08122(18) 0.94443(10) 0.64807(15) 0.0477(6) Uani 1 1 d . . . . .
C24 C 0.9064(2) 0.74599(11) 0.68399(13) 0.0196(5) Uani 1 1 d . . . . .
C9 C 0.7999(2) 0.88441(10) 0.61852(13) 0.0181(5) Uani 1 1 d . . . . .
H00M H 0.871496 0.876024 0.650898 0.022 Uiso 1 1 calc R . . . .
C20 C 0.8303(2) 0.80625(10) 0.78042(13) 0.0162(4) Uani 1 1 d . . . . .
C12 C 0.5959(2) 0.91051(10) 0.52086(13) 0.0186(5) Uani 1 1 d . . . . .
H00O H 0.525704 0.919129 0.487298 0.022 Uiso 1 1 calc R . . . .
C11 C 0.6879(2) 0.95325(11) 0.52893(13) 0.0213(5) Uani 1 1 d . . . . .
H00P H 0.680811 0.991372 0.502326 0.026 Uiso 1 1 calc R . . . .
C40 C 0.2996(2) 0.62184(11) 0.78889(13) 0.0214(5) Uani 1 1 d . . . . .
H00Q H 0.293430 0.657000 0.752547 0.026 Uiso 1 1 calc R . . . .
C33 C 0.5654(2) 0.49088(12) 0.74515(14) 0.0284(6) Uani 1 1 d . . . . .
H00R H 0.620817 0.460189 0.735695 0.034 Uiso 1 1 calc R . . . .
C41 C 0.3180(2) 0.64929(13) 0.86772(14) 0.0278(6) Uani 1 1 d . . . . .
H00B H 0.315668 0.615913 0.904126 0.042 Uiso 1 1 calc GR . . . .
H00C H 0.255248 0.679353 0.872126 0.042 Uiso 1 1 calc GR . . . .
H00D H 0.394915 0.670124 0.877279 0.042 Uiso 1 1 calc GR . . . .
C15 C 0.2518(2) 0.55350(11) 0.59423(14) 0.0208(5) Uani 1 1 d . . . . .
H00T H 0.274016 0.523819 0.632486 0.025 Uiso 1 1 calc R . . . .
C21 C 0.9403(2) 0.79925(12) 0.82539(14) 0.0216(5) Uani 1 1 d . . . . .
H00U H 0.952186 0.816676 0.874002 0.026 Uiso 1 1 calc R . . . .
C37 C 0.5588(2) 0.52809(11) 0.61177(13) 0.0213(5) Uani 1 1 d . . . . .
H00V H 0.488897 0.542030 0.575692 0.026 Uiso 1 1 calc R . . . .
C36 C 0.3993(2) 0.57979(10) 0.77357(13) 0.0184(5) Uani 1 1 d . . . . .
C10 C 0.7903(2) 0.93862(11) 0.57694(13) 0.0205(5) Uani 1 1 d . . . . .
H00X H 0.855420 0.966414 0.581442 0.025 Uiso 1 1 calc R . . . .
C23 C 1.0147(2) 0.74128(13) 0.73078(15) 0.0264(5) Uani 1 1 d . . . . .
H00Y H 1.077789 0.719495 0.714014 0.032 Uiso 1 1 calc R . . . .
C25 C 0.7334(2) 0.84237(12) 0.80994(14) 0.0230(5) Uani 1 1 d . . . . .
H00Z H 0.656375 0.823591 0.787254 0.028 Uiso 1 1 calc R . . . .
C46 C 0.6482(2) 0.67484(13) 0.85625(13) 0.0254(5) Uani 1 1 d . . . . .
H01A H 0.590785 0.643603 0.868560 0.031 Uiso 1 1 calc R . . . .
H01B H 0.619778 0.716742 0.867212 0.031 Uiso 1 1 calc R . . . .
C28 C 0.8935(2) 0.71617(12) 0.60733(15) 0.0249(5) Uani 1 1 d . . . . .
H011 H 0.807399 0.714546 0.586820 0.030 Uiso 1 1 calc R . . . .
C16 C 0.1592(2) 0.54024(12) 0.53815(14) 0.0246(5) Uani 1 1 d . . . . .
H012 H 0.118776 0.501794 0.538978 0.030 Uiso 1 1 calc R . . . .
C22 C 1.0321(2) 0.76754(12) 0.80073(15) 0.0266(6) Uani 1 1 d . . . . .
H013 H 1.106454 0.763922 0.831802 0.032 Uiso 1 1 calc R . . . .
C35 C 0.4427(2) 0.53523(11) 0.82690(14) 0.0250(5) Uani 1 1 d . . . . .
H014 H 0.413993 0.534651 0.873262 0.030 Uiso 1 1 calc R . . . .
C39 C 0.5836(2) 0.46048(12) 0.59207(15) 0.0293(6) Uani 1 1 d . . . . .
H01C H 0.654127 0.445612 0.624725 0.044 Uiso 1 1 calc GR . . . .
H01D H 0.596652 0.458182 0.540074 0.044 Uiso 1 1 calc GR . . . .
H01E H 0.515756 0.434528 0.598844 0.044 Uiso 1 1 calc GR . . . .
C45 C 0.7694(2) 0.66284(12) 0.89941(13) 0.0241(5) Uani 1 1 d . . . . .
H01F H 0.820525 0.700003 0.900448 0.029 Uiso 1 1 calc R . . . .
H01G H 0.765037 0.649625 0.951106 0.029 Uiso 1 1 calc R . . . .
C17 C 0.1241(2) 0.58164(12) 0.48097(14) 0.0236(5) Uani 1 1 d . . . . .
H017 H 0.059599 0.572314 0.443159 0.028 Uiso 1 1 calc R . . . .
C34 C 0.5262(3) 0.49213(12) 0.81371(15) 0.0308(6) Uani 1 1 d . . . . .
H018 H 0.556724 0.463393 0.851465 0.037 Uiso 1 1 calc R . . . .
C26 C 0.7387(3) 0.83933(13) 0.89453(16) 0.0365(7) Uani 1 1 d . . . . .
H01H H 0.747976 0.796055 0.911011 0.055 Uiso 1 1 calc GR . . . .
H01I H 0.665427 0.856219 0.908111 0.055 Uiso 1 1 calc GR . . . .
H01J H 0.806012 0.863777 0.918646 0.055 Uiso 1 1 calc GR . . . .
C43 C 0.7657(2) 0.62841(12) 0.77532(14) 0.0259(5) Uani 1 1 d . . . . .
H01K H 0.827223 0.649899 0.752084 0.031 Uiso 1 1 calc R . . . .
H01L H 0.740383 0.590816 0.745788 0.031 Uiso 1 1 calc R . . . .
C42 C 0.1821(2) 0.58618(13) 0.77644(16) 0.0319(6) Uani 1 1 d . . . . .
H01M H 0.186664 0.551008 0.810985 0.048 Uiso 1 1 calc GR . . . .
H01N H 0.166853 0.570844 0.725077 0.048 Uiso 1 1 calc GR . . . .
H01O H 0.117911 0.613913 0.785328 0.048 Uiso 1 1 calc GR . . . .
C29 C 0.9419(2) 0.64969(12) 0.60920(15) 0.0303(6) Uani 1 1 d . . . . .
H01P H 1.027798 0.650502 0.624463 0.045 Uiso 1 1 calc GR . . . .
H01Q H 0.923488 0.631177 0.559497 0.045 Uiso 1 1 calc GR . . . .
H01R H 0.905488 0.624939 0.644822 0.045 Uiso 1 1 calc GR . . . .
C38 C 0.6625(2) 0.56829(13) 0.59827(15) 0.0292(6) Uani 1 1 d . . . . .
H01S H 0.648104 0.611339 0.611874 0.044 Uiso 1 1 calc GR . . . .
H01T H 0.671232 0.566351 0.545501 0.044 Uiso 1 1 calc GR . . . .
H01U H 0.734880 0.553120 0.628737 0.044 Uiso 1 1 calc GR . . . .
C30 C 0.9552(3) 0.75455(13) 0.55396(16) 0.0335(6) Uani 1 1 d . . . . .
H01V H 0.918291 0.795641 0.547427 0.050 Uiso 1 1 calc GR . . . .
H01W H 0.947823 0.733496 0.505655 0.050 Uiso 1 1 calc GR . . . .
H01X H 1.038939 0.759159 0.574562 0.050 Uiso 1 1 calc GR . . . .
C27 C 0.7294(3) 0.90967(14) 0.78829(17) 0.0490(9) Uani 1 1 d . . . . .
H01Y H 0.803853 0.929709 0.809387 0.073 Uiso 1 1 calc GR . . . .
H H 0.663689 0.930027 0.807475 0.073 Uiso 1 1 calc GR . . . .
HA H 0.718018 0.913199 0.733878 0.073 Uiso 1 1 calc GR . . . .
C44 C 0.8129(3) 0.61117(15) 0.85496(15) 0.0364(7) Uani 1 1 d . . . . .
H01Z H 0.781244 0.570588 0.868211 0.044 Uiso 1 1 calc R . . . .
HB H 0.900278 0.609275 0.863179 0.044 Uiso 1 1 calc R . . . .
C48 C 1.1086(3) 0.9330(2) 0.7272(3) 0.0767(14) Uani 1 1 d . . . . .
H01 H 1.080776 0.891044 0.738513 0.092 Uiso 1 1 calc R . . . .
HC H 1.195264 0.934500 0.742813 0.092 Uiso 1 1 calc R . . . .
C47 C 1.0525(4) 0.9788(2) 0.7678(2) 0.0684(12) Uani 1 1 d . . . . .
H0AA H 0.966543 0.975326 0.754728 0.103 Uiso 1 1 calc GR . . . .
HD H 1.077624 1.020409 0.754809 0.103 Uiso 1 1 calc GR . . . .
HE H 1.075338 0.971978 0.821374 0.103 Uiso 1 1 calc GR . . . .
C50 C 1.0972(4) 0.91510(19) 0.5249(3) 0.0761(14) Uani 1 1 d . . . . .
H1AA H 1.142295 0.888147 0.496091 0.114 Uiso 1 1 calc GR . . . .
HF H 1.108109 0.958515 0.511337 0.114 Uiso 1 1 calc GR . . . .
HG H 1.013128 0.904372 0.513857 0.114 Uiso 1 1 calc GR . . . .
C49 C 1.1396(4) 0.9064(2) 0.6059(3) 0.0937(19) Uani 1 1 d . . . . .
H2AA H 1.127448 0.862614 0.619554 0.112 Uiso 1 1 calc R . . . .
HH H 1.225326 0.915260 0.616455 0.112 Uiso 1 1 calc R . . . .


_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
Ce00 I1 3.0810(2) . ?
Ce00 O1 2.4824(16) . ?
Ce00 N2 2.4409(18) . ?
Ce00 N1 2.5087(18) . ?
Ce00 C1 2.943(2) . ?
Ce00 C3 2.985(2) . ?
Ce00 C6 3.022(2) . ?
Ce00 C2 2.944(2) . ?
Ce00 C4 3.012(2) . ?
Ce00 C5 3.047(2) . ?
O1 C46 1.457(3) . ?
O1 C43 1.473(3) . ?
N2 C14 1.391(3) . ?
N2 C31 1.439(3) . ?
N1 C19 1.439(3) . ?
N1 C8 1.395(3) . ?
C1 C6 1.378(3) . ?
C1 C2 1.415(3) . ?
C1 C7 1.475(3) . ?
C3 H007 0.9500 . ?
C3 C2 1.381(3) . ?
C3 C4 1.411(3) . ?
C6 H008 0.9500 . ?
C6 C5 1.410(3) . ?
C19 C24 1.414(3) . ?
C19 C20 1.414(3) . ?
C2 H00A 0.9500 . ?
C14 C13 1.418(3) . ?
C14 C15 1.409(3) . ?
C4 C13 1.479(3) . ?
C4 C5 1.387(3) . ?
C7 C8 1.419(3) . ?
C7 C12 1.387(3) . ?
C13 C18 1.386(3) . ?
C5 H00F 0.9500 . ?
C8 C9 1.420(3) . ?
C31 C32 1.417(3) . ?
C31 C36 1.415(3) . ?
C32 C33 1.393(3) . ?
C32 C37 1.535(3) . ?
C18 H00J 0.9500 . ?
C18 C17 1.390(3) . ?
O2 C48 1.444(5) . ?
O2 C49 1.365(4) . ?
C24 C23 1.395(3) . ?
C24 C28 1.520(3) . ?
C9 H00M 0.9500 . ?
C9 C10 1.386(3) . ?
C20 C21 1.400(3) . ?
C20 C25 1.519(3) . ?
C12 H00O 0.9500 . ?
C12 C11 1.390(3) . ?
C11 H00P 0.9500 . ?
C11 C10 1.386(3) . ?
C40 H00Q 1.0000 . ?
C40 C41 1.534(3) . ?
C40 C36 1.516(3) . ?
C40 C42 1.536(4) . ?
C33 H00R 0.9500 . ?
C33 C34 1.388(4) . ?
C41 H00B 0.9800 . ?
C41 H00C 0.9800 . ?
C41 H00D 0.9800 . ?
C15 H00T 0.9500 . ?
C15 C16 1.383(3) . ?
C21 H00U 0.9500 . ?
C21 C22 1.385(3) . ?
C37 H00V 1.0000 . ?
C37 C39 1.536(3) . ?
C37 C38 1.519(3) . ?
C36 C35 1.400(3) . ?
C10 H00X 0.9500 . ?
C23 H00Y 0.9500 . ?
C23 C22 1.377(4) . ?
C25 H00Z 1.0000 . ?
C25 C26 1.530(4) . ?
C25 C27 1.501(4) . ?
C46 H01A 0.9900 . ?
C46 H01B 0.9900 . ?
C46 C45 1.509(3) . ?
C28 H011 1.0000 . ?
C28 C29 1.534(4) . ?
C28 C30 1.527(4) . ?
C16 H012 0.9500 . ?
C16 C17 1.381(4) . ?
C22 H013 0.9500 . ?
C35 H014 0.9500 . ?
C35 C34 1.380(4) . ?
C39 H01C 0.9800 . ?
C39 H01D 0.9800 . ?
C39 H01E 0.9800 . ?
C45 H01F 0.9900 . ?
C45 H01G 0.9900 . ?
C45 C44 1.504(4) . ?
C17 H017 0.9500 . ?
C34 H018 0.9500 . ?
C26 H01H 0.9800 . ?
C26 H01I 0.9800 . ?
C26 H01J 0.9800 . ?
C43 H01K 0.9900 . ?
C43 H01L 0.9900 . ?
C43 C44 1.511(4) . ?
C42 H01M 0.9800 . ?
C42 H01N 0.9800 . ?
C42 H01O 0.9800 . ?
C29 H01P 0.9800 . ?
C29 H01Q 0.9800 . ?
C29 H01R 0.9800 . ?
C38 H01S 0.9800 . ?
C38 H01T 0.9800 . ?
C38 H01U 0.9800 . ?
C30 H01V 0.9800 . ?
C30 H01W 0.9800 . ?
C30 H01X 0.9800 . ?
C27 H01Y 0.9800 . ?
C27 H 0.9800 . ?
C27 HA 0.9800 . ?
C44 H01Z 0.9900 . ?
C44 HB 0.9900 . ?
C48 H01 0.9900 . ?
C48 HC 0.9900 . ?
C48 C47 1.442(6) . ?
C47 H0AA 0.9800 . ?
C47 HD 0.9800 . ?
C47 HE 0.9800 . ?
C50 H1AA 0.9800 . ?
C50 HF 0.9800 . ?
C50 HG 0.9800 . ?
C50 C49 1.489(7) . ?
C49 H2AA 0.9900 . ?
C49 HH 0.9900 . ?

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 Ce00 I1 95.53(4) . . ?
O1 Ce00 N1 86.84(6) . . ?
O1 Ce00 C1 147.01(6) . . ?
O1 Ce00 C3 139.25(6) . . ?
O1 Ce00 C6 162.43(6) . . ?
O1 Ce00 C2 137.89(6) . . ?
O1 Ce00 C4 150.11(6) . . ?
O1 Ce00 C5 165.06(6) . . ?
N2 Ce00 I1 101.54(4) . . ?
N2 Ce00 O1 93.34(6) . . ?
N2 Ce00 N1 156.32(6) . . ?
N2 Ce00 C1 114.52(6) . . ?
N2 Ce00 C3 70.33(6) . . ?
N2 Ce00 C6 102.74(6) . . ?
N2 Ce00 C2 97.13(6) . . ?
N2 Ce00 C4 58.61(6) . . ?
N2 Ce00 C5 76.11(6) . . ?
N1 Ce00 I1 102.01(4) . . ?
N1 Ce00 C1 60.50(6) . . ?
N1 Ce00 C3 94.33(6) . . ?
N1 Ce00 C6 81.29(6) . . ?
N1 Ce00 C2 68.10(6) . . ?
N1 Ce00 C4 114.43(6) . . ?
N1 Ce00 C5 107.10(6) . . ?
C1 Ce00 I1 95.73(4) . . ?
C1 Ce00 C3 48.32(6) . . ?
C1 Ce00 C6 26.67(6) . . ?
C1 Ce00 C2 27.81(6) . . ?
C1 Ce00 C4 56.34(6) . . ?
C1 Ce00 C5 47.65(6) . . ?
C3 Ce00 I1 123.73(4) . . ?
C3 Ce00 C6 55.22(6) . . ?
C3 Ce00 C4 27.20(6) . . ?
C3 Ce00 C5 47.10(6) . . ?
C6 Ce00 I1 74.51(4) . . ?
C6 Ce00 C5 26.87(6) . . ?
C2 Ce00 I1 121.75(4) . . ?
C2 Ce00 C3 26.93(6) . . ?
C2 Ce00 C6 47.56(6) . . ?
C2 Ce00 C4 47.98(6) . . ?
C2 Ce00 C5 55.33(6) . . ?
C4 Ce00 I1 99.86(4) . . ?
C4 Ce00 C6 47.42(6) . . ?
C4 Ce00 C5 26.46(6) . . ?
C5 Ce00 I1 76.65(4) . . ?
C46 O1 Ce00 124.57(14) . . ?
C46 O1 C43 107.43(17) . . ?
C43 O1 Ce00 127.91(13) . . ?
C14 N2 Ce00 135.05(14) . . ?
C14 N2 C31 114.59(18) . . ?
C31 N2 Ce00 110.34(13) . . ?
C19 N1 Ce00 118.73(13) . . ?
C8 N1 Ce00 128.62(14) . . ?
C8 N1 C19 112.34(17) . . ?
C6 C1 Ce00 79.88(13) . . ?
C6 C1 C2 119.0(2) . . ?
C6 C1 C7 122.6(2) . . ?
C2 C1 Ce00 76.13(12) . . ?
C2 C1 C7 118.25(19) . . ?
C7 C1 Ce00 111.11(13) . . ?
Ce00 C3 H007 118.7 . . ?
C2 C3 Ce00 74.88(12) . . ?
C2 C3 H007 119.8 . . ?
C2 C3 C4 120.4(2) . . ?
C4 C3 Ce00 77.48(13) . . ?
C4 C3 H007 119.8 . . ?
Ce00 C6 H008 120.3 . . ?
C1 C6 Ce00 73.45(12) . . ?
C1 C6 H008 119.7 . . ?
C1 C6 C5 120.6(2) . . ?
C5 C6 Ce00 77.54(13) . . ?
C5 C6 H008 119.7 . . ?
C24 C19 N1 120.14(19) . . ?
C20 C19 N1 120.12(19) . . ?
C20 C19 C24 119.7(2) . . ?
Ce00 C2 H00A 116.7 . . ?
C1 C2 Ce00 76.06(12) . . ?
C1 C2 H00A 119.8 . . ?
C3 C2 Ce00 78.19(12) . . ?
C3 C2 C1 120.4(2) . . ?
C3 C2 H00A 119.8 . . ?
N2 C14 C13 118.38(19) . . ?
N2 C14 C15 125.3(2) . . ?
C15 C14 C13 116.3(2) . . ?
C3 C4 Ce00 75.31(13) . . ?
C3 C4 C13 118.05(19) . . ?
C13 C4 Ce00 112.14(14) . . ?
C5 C4 Ce00 78.16(13) . . ?
C5 C4 C3 119.0(2) . . ?
C5 C4 C13 122.7(2) . . ?
C8 C7 C1 116.26(19) . . ?
C12 C7 C1 121.6(2) . . ?
C12 C7 C8 122.0(2) . . ?
C14 C13 C4 115.32(19) . . ?
C18 C13 C14 121.4(2) . . ?
C18 C13 C4 123.1(2) . . ?
Ce00 C5 H00F 120.3 . . ?
C6 C5 Ce00 75.59(13) . . ?
C6 C5 H00F 119.8 . . ?
C4 C5 Ce00 75.38(13) . . ?
C4 C5 C6 120.4(2) . . ?
C4 C5 H00F 119.8 . . ?
N1 C8 C7 119.50(19) . . ?
N1 C8 C9 125.1(2) . . ?
C7 C8 C9 115.3(2) . . ?
C32 C31 N2 118.96(19) . . ?
C36 C31 N2 121.1(2) . . ?
C36 C31 C32 119.9(2) . . ?
C31 C32 C37 120.3(2) . . ?
C33 C32 C31 119.1(2) . . ?
C33 C32 C37 120.4(2) . . ?
C13 C18 H00J 119.5 . . ?
C13 C18 C17 120.9(2) . . ?
C17 C18 H00J 119.5 . . ?
C49 O2 C48 113.9(3) . . ?
C19 C24 C28 122.1(2) . . ?
C23 C24 C19 119.1(2) . . ?
C23 C24 C28 118.7(2) . . ?
C8 C9 H00M 119.1 . . ?
C10 C9 C8 121.7(2) . . ?
C10 C9 H00M 119.1 . . ?
C19 C20 C25 122.1(2) . . ?
C21 C20 C19 118.6(2) . . ?
C21 C20 C25 119.3(2) . . ?
C7 C12 H00O 119.4 . . ?
C7 C12 C11 121.1(2) . . ?
C11 C12 H00O 119.4 . . ?
C12 C11 H00P 121.0 . . ?
C10 C11 C12 118.1(2) . . ?
C10 C11 H00P 121.0 . . ?
C41 C40 H00Q 108.1 . . ?
C41 C40 C42 108.8(2) . . ?
C36 C40 H00Q 108.1 . . ?
C36 C40 C41 113.7(2) . . ?
C36 C40 C42 110.0(2) . . ?
C42 C40 H00Q 108.1 . . ?
C32 C33 H00R 119.5 . . ?
C34 C33 C32 120.9(2) . . ?
C34 C33 H00R 119.5 . . ?
C40 C41 H00B 109.5 . . ?
C40 C41 H00C 109.5 . . ?
C40 C41 H00D 109.5 . . ?
H00B C41 H00C 109.5 . . ?
H00B C41 H00D 109.5 . . ?
H00C C41 H00D 109.5 . . ?
C14 C15 H00T 119.3 . . ?
C16 C15 C14 121.4(2) . . ?
C16 C15 H00T 119.3 . . ?
C20 C21 H00U 119.2 . . ?
C22 C21 C20 121.6(2) . . ?
C22 C21 H00U 119.2 . . ?
C32 C37 H00V 106.9 . . ?
C32 C37 C39 112.1(2) . . ?
C39 C37 H00V 106.9 . . ?
C38 C37 C32 114.7(2) . . ?
C38 C37 H00V 106.9 . . ?
C38 C37 C39 109.0(2) . . ?
C31 C36 C40 122.7(2) . . ?
C35 C36 C31 118.4(2) . . ?
C35 C36 C40 118.7(2) . . ?
C9 C10 C11 121.6(2) . . ?
C9 C10 H00X 119.2 . . ?
C11 C10 H00X 119.2 . . ?
C24 C23 H00Y 119.3 . . ?
C22 C23 C24 121.4(2) . . ?
C22 C23 H00Y 119.3 . . ?
C20 C25 H00Z 107.1 . . ?
C20 C25 C26 114.5(2) . . ?
C26 C25 H00Z 107.1 . . ?
C27 C25 C20 113.4(2) . . ?
C27 C25 H00Z 107.1 . . ?
C27 C25 C26 107.4(2) . . ?
O1 C46 H01A 110.9 . . ?
O1 C46 H01B 110.9 . . ?
O1 C46 C45 104.37(19) . . ?
H01A C46 H01B 108.9 . . ?
C45 C46 H01A 110.9 . . ?
C45 C46 H01B 110.9 . . ?
C24 C28 H011 107.9 . . ?
C24 C28 C29 113.0(2) . . ?
C24 C28 C30 111.3(2) . . ?
C29 C28 H011 107.9 . . ?
C30 C28 H011 107.9 . . ?
C30 C28 C29 108.6(2) . . ?
C15 C16 H012 119.3 . . ?
C17 C16 C15 121.5(2) . . ?
C17 C16 H012 119.3 . . ?
C21 C22 H013 120.3 . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 H013 120.3 . . ?
C36 C35 H014 119.2 . . ?
C34 C35 C36 121.6(2) . . ?
C34 C35 H014 119.2 . . ?
C37 C39 H01C 109.5 . . ?
C37 C39 H01D 109.5 . . ?
C37 C39 H01E 109.5 . . ?
H01C C39 H01D 109.5 . . ?
H01C C39 H01E 109.5 . . ?
H01D C39 H01E 109.5 . . ?
C46 C45 H01F 111.4 . . ?
C46 C45 H01G 111.4 . . ?
H01F C45 H01G 109.3 . . ?
C44 C45 C46 101.6(2) . . ?
C44 C45 H01F 111.4 . . ?
C44 C45 H01G 111.4 . . ?
C18 C17 H017 120.8 . . ?
C16 C17 C18 118.5(2) . . ?
C16 C17 H017 120.8 . . ?
C33 C34 H018 120.1 . . ?
C35 C34 C33 119.8(2) . . ?
C35 C34 H018 120.1 . . ?
C25 C26 H01H 109.5 . . ?
C25 C26 H01I 109.5 . . ?
C25 C26 H01J 109.5 . . ?
H01H C26 H01I 109.5 . . ?
H01H C26 H01J 109.5 . . ?
H01I C26 H01J 109.5 . . ?
O1 C43 H01K 110.5 . . ?
O1 C43 H01L 110.5 . . ?
O1 C43 C44 106.30(19) . . ?
H01K C43 H01L 108.7 . . ?
C44 C43 H01K 110.5 . . ?
C44 C43 H01L 110.5 . . ?
C40 C42 H01M 109.5 . . ?
C40 C42 H01N 109.5 . . ?
C40 C42 H01O 109.5 . . ?
H01M C42 H01N 109.5 . . ?
H01M C42 H01O 109.5 . . ?
H01N C42 H01O 109.5 . . ?
C28 C29 H01P 109.5 . . ?
C28 C29 H01Q 109.5 . . ?
C28 C29 H01R 109.5 . . ?
H01P C29 H01Q 109.5 . . ?
H01P C29 H01R 109.5 . . ?
H01Q C29 H01R 109.5 . . ?
C37 C38 H01S 109.5 . . ?
C37 C38 H01T 109.5 . . ?
C37 C38 H01U 109.5 . . ?
H01S C38 H01T 109.5 . . ?
H01S C38 H01U 109.5 . . ?
H01T C38 H01U 109.5 . . ?
C28 C30 H01V 109.5 . . ?
C28 C30 H01W 109.5 . . ?
C28 C30 H01X 109.5 . . ?
H01V C30 H01W 109.5 . . ?
H01V C30 H01X 109.5 . . ?
H01W C30 H01X 109.5 . . ?
C25 C27 H01Y 109.5 . . ?
C25 C27 H 109.5 . . ?
C25 C27 HA 109.5 . . ?
H01Y C27 H 109.5 . . ?
H01Y C27 HA 109.5 . . ?
H C27 HA 109.5 . . ?
C45 C44 C43 103.5(2) . . ?
C45 C44 H01Z 111.1 . . ?
C45 C44 HB 111.1 . . ?
C43 C44 H01Z 111.1 . . ?
C43 C44 HB 111.1 . . ?
H01Z C44 HB 109.0 . . ?
O2 C48 H01 109.6 . . ?
O2 C48 HC 109.6 . . ?
H01 C48 HC 108.1 . . ?
C47 C48 O2 110.2(3) . . ?
C47 C48 H01 109.6 . . ?
C47 C48 HC 109.6 . . ?
C48 C47 H0AA 109.5 . . ?
C48 C47 HD 109.5 . . ?
C48 C47 HE 109.5 . . ?
H0AA C47 HD 109.5 . . ?
H0AA C47 HE 109.5 . . ?
HD C47 HE 109.5 . . ?
H1AA C50 HF 109.5 . . ?
H1AA C50 HG 109.5 . . ?
HF C50 HG 109.5 . . ?
C49 C50 H1AA 109.5 . . ?
C49 C50 HF 109.5 . . ?
C49 C50 HG 109.5 . . ?
O2 C49 C50 111.4(4) . . ?
O2 C49 H2AA 109.3 . . ?
O2 C49 HH 109.3 . . ?
C50 C49 H2AA 109.3 . . ?
C50 C49 HH 109.3 . . ?
H2AA C49 HH 108.0 . . ?

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
Ce00 O1 C46 C45 -156.65(15) . . . . ?
Ce00 O1 C43 C44 -179.14(17) . . . . ?
Ce00 N2 C14 C13 3.3(3) . . . . ?
Ce00 N2 C14 C15 -178.90(17) . . . . ?
Ce00 N2 C31 C32 -93.7(2) . . . . ?
Ce00 N2 C31 C36 87.2(2) . . . . ?
Ce00 N1 C19 C24 98.3(2) . . . . ?
Ce00 N1 C19 C20 -82.6(2) . . . . ?
Ce00 N1 C8 C7 -8.2(3) . . . . ?
Ce00 N1 C8 C9 168.59(16) . . . . ?
Ce00 C1 C6 C5 -64.1(2) . . . . ?
Ce00 C1 C2 C3 67.02(19) . . . . ?
Ce00 C1 C7 C8 20.3(2) . . . . ?
Ce00 C1 C7 C12 -162.94(17) . . . . ?
Ce00 C3 C2 C1 -65.90(18) . . . . ?
Ce00 C3 C4 C13 -107.57(19) . . . . ?
Ce00 C3 C4 C5 67.18(19) . . . . ?
Ce00 C6 C5 C4 -63.1(2) . . . . ?
Ce00 C4 C13 C14 -7.0(2) . . . . ?
Ce00 C4 C13 C18 177.02(17) . . . . ?
Ce00 C4 C5 C6 63.2(2) . . . . ?
O1 C46 C45 C44 -40.0(3) . . . . ?
O1 C43 C44 C45 -22.5(3) . . . . ?
N2 C14 C13 C4 3.8(3) . . . . ?
N2 C14 C13 C18 179.9(2) . . . . ?
N2 C14 C15 C16 -179.8(2) . . . . ?
N2 C31 C32 C33 176.2(2) . . . . ?
N2 C31 C32 C37 -8.8(3) . . . . ?
N2 C31 C36 C40 8.5(3) . . . . ?
N2 C31 C36 C35 -176.5(2) . . . . ?
N1 C19 C24 C23 176.1(2) . . . . ?
N1 C19 C24 C28 -1.6(3) . . . . ?
N1 C19 C20 C21 -177.1(2) . . . . ?
N1 C19 C20 C25 1.9(3) . . . . ?
N1 C8 C9 C10 -173.2(2) . . . . ?
C1 C6 C5 Ce00 62.02(19) . . . . ?
C1 C6 C5 C4 -1.1(3) . . . . ?
C1 C7 C8 N1 -11.1(3) . . . . ?
C1 C7 C8 C9 171.88(19) . . . . ?
C1 C7 C12 C11 -174.2(2) . . . . ?
C3 C4 C13 C14 77.7(3) . . . . ?
C3 C4 C13 C18 -98.3(3) . . . . ?
C3 C4 C5 Ce00 -65.64(19) . . . . ?
C3 C4 C5 C6 -2.4(3) . . . . ?
C6 C1 C2 Ce00 -69.87(18) . . . . ?
C6 C1 C2 C3 -2.8(3) . . . . ?
C6 C1 C7 C8 111.6(2) . . . . ?
C6 C1 C7 C12 -71.6(3) . . . . ?
C19 N1 C8 C7 178.44(19) . . . . ?
C19 N1 C8 C9 -4.8(3) . . . . ?
C19 C24 C23 C22 1.9(4) . . . . ?
C19 C24 C28 C29 -135.5(2) . . . . ?
C19 C24 C28 C30 102.0(3) . . . . ?
C19 C20 C21 C22 0.0(4) . . . . ?
C19 C20 C25 C26 150.9(2) . . . . ?
C19 C20 C25 C27 -85.3(3) . . . . ?
C2 C1 C6 Ce00 67.81(18) . . . . ?
C2 C1 C6 C5 3.7(3) . . . . ?
C2 C1 C7 C8 -64.9(3) . . . . ?
C2 C1 C7 C12 111.9(2) . . . . ?
C2 C3 C4 Ce00 -63.89(19) . . . . ?
C2 C3 C4 C13 -171.5(2) . . . . ?
C2 C3 C4 C5 3.3(3) . . . . ?
C14 N2 C31 C32 85.1(3) . . . . ?
C14 N2 C31 C36 -94.0(2) . . . . ?
C14 C13 C18 C17 -0.5(3) . . . . ?
C14 C15 C16 C17 0.5(4) . . . . ?
C4 C3 C2 Ce00 65.23(19) . . . . ?
C4 C3 C2 C1 -0.7(3) . . . . ?
C4 C13 C18 C17 175.2(2) . . . . ?
C7 C1 C6 Ce00 -108.7(2) . . . . ?
C7 C1 C6 C5 -172.8(2) . . . . ?
C7 C1 C2 Ce00 106.76(18) . . . . ?
C7 C1 C2 C3 173.78(19) . . . . ?
C7 C8 C9 C10 3.6(3) . . . . ?
C7 C12 C11 C10 1.6(3) . . . . ?
C13 C14 C15 C16 -2.0(3) . . . . ?
C13 C4 C5 Ce00 108.8(2) . . . . ?
C13 C4 C5 C6 172.1(2) . . . . ?
C13 C18 C17 C16 -1.0(4) . . . . ?
C5 C4 C13 C14 -96.9(3) . . . . ?
C5 C4 C13 C18 87.1(3) . . . . ?
C8 N1 C19 C24 -87.6(2) . . . . ?
C8 N1 C19 C20 91.6(2) . . . . ?
C8 C7 C12 C11 2.4(3) . . . . ?
C8 C9 C10 C11 0.1(4) . . . . ?
C31 N2 C14 C13 -175.08(19) . . . . ?
C31 N2 C14 C15 2.7(3) . . . . ?
C31 C32 C33 C34 1.4(4) . . . . ?
C31 C32 C37 C39 -147.4(2) . . . . ?
C31 C32 C37 C38 87.6(3) . . . . ?
C31 C36 C35 C34 -0.8(4) . . . . ?
C32 C31 C36 C40 -170.6(2) . . . . ?
C32 C31 C36 C35 4.4(3) . . . . ?
C32 C33 C34 C35 2.2(4) . . . . ?
C24 C19 C20 C21 2.1(3) . . . . ?
C24 C19 C20 C25 -178.9(2) . . . . ?
C24 C23 C22 C21 0.1(4) . . . . ?
C20 C19 C24 C23 -3.0(3) . . . . ?
C20 C19 C24 C28 179.3(2) . . . . ?
C20 C21 C22 C23 -1.1(4) . . . . ?
C12 C7 C8 N1 172.2(2) . . . . ?
C12 C7 C8 C9 -4.9(3) . . . . ?
C12 C11 C10 C9 -2.8(3) . . . . ?
C40 C36 C35 C34 174.4(2) . . . . ?
C33 C32 C37 C39 27.6(3) . . . . ?
C33 C32 C37 C38 -97.4(3) . . . . ?
C41 C40 C36 C31 -139.1(2) . . . . ?
C41 C40 C36 C35 46.0(3) . . . . ?
C15 C14 C13 C4 -174.1(2) . . . . ?
C15 C14 C13 C18 2.0(3) . . . . ?
C15 C16 C17 C18 1.0(4) . . . . ?
C21 C20 C25 C26 -30.0(3) . . . . ?
C21 C20 C25 C27 93.7(3) . . . . ?
C37 C32 C33 C34 -173.7(3) . . . . ?
C36 C31 C32 C33 -4.7(3) . . . . ?
C36 C31 C32 C37 170.4(2) . . . . ?
C36 C35 C34 C33 -2.5(4) . . . . ?
C23 C24 C28 C29 46.8(3) . . . . ?
C23 C24 C28 C30 -75.7(3) . . . . ?
C25 C20 C21 C22 -179.1(2) . . . . ?
C46 O1 C43 C44 -2.5(3) . . . . ?
C46 C45 C44 C43 37.8(3) . . . . ?
C28 C24 C23 C22 179.7(3) . . . . ?
C43 O1 C46 C45 26.6(3) . . . . ?
C42 C40 C36 C31 98.6(3) . . . . ?
C42 C40 C36 C35 -76.3(3) . . . . ?
C48 O2 C49 C50 173.1(3) . . . . ?
C49 O2 C48 C47 174.4(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_3_Pu
_database_code_depnum_ccdc_archive 'CCDC 2238472'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
# end Validation Reply Form
_audit_creation_date             2022-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C46 H54 I N2 O Pu, 0.67(C4 H8 O), 0.33(C4 H10 O)'
_chemical_formula_sum            'C50 H62.67 I N2 O2 Pu'
_chemical_formula_weight         1092.58
_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 0.0033 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'
I I -0.4742 1.8119 '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'
Pu Pu -9.4100 4.3056 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.8050(10)
_cell_length_b                   15.6334(12)
_cell_length_c                   21.9877(18)
_cell_angle_alpha                90
_cell_angle_beta                 108.057(3)
_cell_angle_gamma                90
_cell_volume                     4511.6(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   0.669
_shelx_estimated_absorpt_T_min   0.310
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1693 before and 0.0879 after correction. The Ratio of minimum to maximum transmission is 0.5446. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2159
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78010
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.026
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9488
_reflns_number_total             11214
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.837
_refine_diff_density_min         -2.460
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.00040(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   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         11214
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.054
_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)+(0.0526P)²+10.8321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0985
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C16, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C16, C17, C18, C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C14 \\sim C13 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C18 \\sim C13: within 0.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C13 \\sim C18: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C16 \\sim C15: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C17 \\sim C16: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C14 \\sim C15: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
4. Others
 Fixed Sof: O2(0.66666) C49(0.66666) H49A(0.66666) H49B(0.66666) C47(0.66666)
 H47A(0.66666) H47B(0.66666) C48(0.66666) H48A(0.66666) H48B(0.66666)
 C50(0.66666) H50A(0.66666) H50B(0.66666) C54(0.33333) H54A(0.33333)
 H54B(0.33333) H54C(0.33333) O3(0.33333) C53(0.33333) H53A(0.33333)
 H53B(0.33333) C51(0.33333) H51A(0.33333) H51B(0.33333) H51C(0.33333)
 C52(0.33333) H52A(0.33333) H52B(0.33333)
5.a Ternary CH refined with riding coordinates:
 C40(H40), C37(H37), C28(H28), C25(H25)
5.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C43(H43A,H43B), C45(H45A,H45B), C44(H44A,H44B), C49(H49A,
 H49B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B), C53(H53A,H53B),
 C52(H52A,H52B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C9(H9), C3(H3), C5(H5), C33(H33), C11(H11), C10(H10),
 C35(H35), C2(H2), C34(H34), C22(H22), C23(H23), C21(H21), C15(H15), C18(H18),
 C16(H16), C17(H17)
5.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,
 H27B,H27C), C54(H54A,H54B,H54C), C51(H51A,H51B,H51C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Pu1 Pu 0.35601(2) 0.29734(2) 0.60724(2) 0.01399(6) Uani 1 1 d . . . . .
I1 I 0.32257(2) 0.33256(2) 0.73465(2) 0.02605(8) Uani 1 1 d . . . . .
O1 O 0.4192(2) 0.15411(18) 0.64483(14) 0.0210(6) Uani 1 1 d . . . . .
N2 N 0.1969(3) 0.2330(2) 0.54339(17) 0.0178(7) Uani 1 1 d . . . . .
C1 C 0.3934(3) 0.4741(2) 0.5800(2) 0.0182(8) Uani 1 1 d . . . . .
C6 C 0.3190(3) 0.4841(2) 0.6101(2) 0.0203(8) Uani 1 1 d . . . . .
H6 H 0.334574 0.514358 0.649413 0.024 Uiso 1 1 calc R . . . .
N1 N 0.5336(3) 0.3452(2) 0.62714(17) 0.0171(7) Uani 1 1 d . . . . .
C12 C 0.5341(3) 0.5819(3) 0.6188(2) 0.0211(8) Uani 1 1 d . . . . .
H12 H 0.485245 0.626679 0.607887 0.025 Uiso 1 1 calc R . . . .
C9 C 0.6752(3) 0.4499(3) 0.6491(2) 0.0216(8) Uani 1 1 d . . . . .
H9 H 0.725078 0.405916 0.658109 0.026 Uiso 1 1 calc R . . . .
C31 C 0.6122(3) 0.2812(2) 0.6445(2) 0.0168(8) Uani 1 1 d . . . . .
C7 C 0.5010(3) 0.4973(2) 0.6102(2) 0.0181(8) Uani 1 1 d . . . . .
C32 C 0.6520(3) 0.2526(3) 0.7086(2) 0.0214(8) Uani 1 1 d . . . . .
C3 C 0.2701(4) 0.3994(3) 0.4929(2) 0.0259(10) Uani 1 1 d . . . . .
H3 H 0.253383 0.371363 0.452570 0.031 Uiso 1 1 calc R . . . .
C8 C 0.5713(3) 0.4282(3) 0.62895(18) 0.0172(8) Uani 1 1 d . . . . .
C46 C 0.3954(3) 0.1053(3) 0.6957(2) 0.0230(9) Uani 1 1 d . . . . .
H46A H 0.325952 0.080688 0.680003 0.028 Uiso 1 1 calc R . . . .
H46B H 0.400179 0.142140 0.733139 0.028 Uiso 1 1 calc R . . . .
C5 C 0.2214(3) 0.4500(3) 0.5826(2) 0.0268(10) Uani 1 1 d . . . . .
H5 H 0.171507 0.456881 0.603809 0.032 Uiso 1 1 calc R . . . .
C40 C 0.6249(4) 0.2962(3) 0.7626(2) 0.0235(9) Uani 1 1 d . . . . .
H40 H 0.561780 0.330763 0.743561 0.028 Uiso 1 1 calc R . . . .
C43 C 0.4756(4) 0.0963(3) 0.6144(2) 0.0267(10) Uani 1 1 d . . . . .
H43A H 0.544893 0.118703 0.619900 0.032 Uiso 1 1 calc R . . . .
H43B H 0.439308 0.090487 0.568051 0.032 Uiso 1 1 calc R . . . .
C33 C 0.7229(4) 0.1858(3) 0.7224(2) 0.0260(9) Uani 1 1 d . . . . .
H33 H 0.747941 0.164629 0.764921 0.031 Uiso 1 1 calc R . . . .
C4 C 0.1963(4) 0.4059(3) 0.5246(2) 0.0280(10) Uani 1 1 d . . . . .
C36 C 0.6520(3) 0.2479(3) 0.5974(2) 0.0190(8) Uani 1 1 d . . . . .
C11 C 0.6364(4) 0.6023(3) 0.6427(2) 0.0233(9) Uani 1 1 d . . . . .
H11 H 0.658247 0.660121 0.649737 0.028 Uiso 1 1 calc R . . . .
C10 C 0.7061(4) 0.5355(3) 0.6561(2) 0.0249(9) Uani 1 1 d . . . . .
H10 H 0.776802 0.548252 0.670439 0.030 Uiso 1 1 calc R . . . .
C45 C 0.4748(4) 0.0356(3) 0.7128(2) 0.0319(11) Uani 1 1 d . . . . .
H45A H 0.452401 -0.013284 0.733804 0.038 Uiso 1 1 calc R . . . .
H45B H 0.540800 0.057228 0.741057 0.038 Uiso 1 1 calc R . . . .
C35 C 0.7241(3) 0.1818(3) 0.6140(2) 0.0234(9) Uani 1 1 d . . . . .
H35 H 0.750562 0.158747 0.582439 0.028 Uiso 1 1 calc R . . . .
C37 C 0.6181(4) 0.2813(3) 0.5289(2) 0.0223(9) Uani 1 1 d . . . . .
H37 H 0.574186 0.332565 0.527486 0.027 Uiso 1 1 calc R . . . .
C41 C 0.6046(4) 0.2342(3) 0.8110(2) 0.0347(11) Uani 1 1 d . . . . .
H41A H 0.550355 0.194365 0.788805 0.052 Uiso 1 1 calc GR . . . .
H41B H 0.583586 0.266407 0.843023 0.052 Uiso 1 1 calc GR . . . .
H41C H 0.666886 0.202055 0.832190 0.052 Uiso 1 1 calc GR . . . .
C2 C 0.3670(4) 0.4332(3) 0.5194(2) 0.0224(9) Uani 1 1 d . . . . .
H2 H 0.415659 0.428943 0.497088 0.027 Uiso 1 1 calc R . . . .
C44 C 0.4812(5) 0.0113(3) 0.6475(3) 0.0366(12) Uani 1 1 d . . . . .
H44A H 0.546077 -0.018329 0.651017 0.044 Uiso 1 1 calc R . . . .
H44B H 0.423640 -0.026056 0.624398 0.044 Uiso 1 1 calc R . . . .
C34 C 0.7572(4) 0.1499(3) 0.6751(2) 0.0275(10) Uani 1 1 d . . . . .
H34 H 0.803618 0.103325 0.685017 0.033 Uiso 1 1 calc R . . . .
C19 C 0.1915(3) 0.1406(3) 0.5458(2) 0.0234(9) Uani 1 1 d . . . . .
C24 C 0.1459(4) 0.1001(3) 0.5868(2) 0.0337(11) Uani 1 1 d . . . . .
C42 C 0.7102(4) 0.3574(3) 0.7986(2) 0.0342(11) Uani 1 1 d . . . . .
H42A H 0.773669 0.325180 0.816173 0.051 Uiso 1 1 calc GR . . . .
H42B H 0.691773 0.384889 0.833480 0.051 Uiso 1 1 calc GR . . . .
H42C H 0.719747 0.401160 0.769034 0.051 Uiso 1 1 calc GR . . . .
C28 C 0.2744(4) 0.1347(3) 0.4555(3) 0.0360(12) Uani 1 1 d . . . . .
H28 H 0.315548 0.185052 0.477034 0.043 Uiso 1 1 calc R . . . .
C20 C 0.2306(4) 0.0926(3) 0.5043(3) 0.0310(11) Uani 1 1 d . . . . .
C25 C 0.0958(4) 0.1488(5) 0.6290(3) 0.0453(15) Uani 1 1 d . . . . .
H25 H 0.104402 0.211477 0.623358 0.054 Uiso 1 1 calc R . . . .
C38 C 0.5541(5) 0.2154(4) 0.4835(3) 0.0476(16) Uani 1 1 d . . . . .
H38A H 0.594543 0.163475 0.484894 0.071 Uiso 1 1 calc GR . . . .
H38B H 0.532358 0.238434 0.439945 0.071 Uiso 1 1 calc GR . . . .
H38C H 0.494059 0.201561 0.496424 0.071 Uiso 1 1 calc GR . . . .
C22 C 0.1819(5) -0.0369(3) 0.5460(3) 0.0558(19) Uani 1 1 d . . . . .
H22 H 0.178733 -0.097592 0.546298 0.067 Uiso 1 1 calc R . . . .
C23 C 0.1421(5) 0.0098(4) 0.5856(3) 0.0507(18) Uani 1 1 d . . . . .
H23 H 0.111229 -0.019349 0.612743 0.061 Uiso 1 1 calc R . . . .
C21 C 0.2259(5) 0.0033(3) 0.5065(3) 0.0488(16) Uani 1 1 d . . . . .
H21 H 0.254019 -0.029782 0.479851 0.059 Uiso 1 1 calc R . . . .
C39 C 0.7080(5) 0.3097(4) 0.5073(3) 0.0474(15) Uani 1 1 d . . . . .
H39A H 0.748109 0.352305 0.537321 0.071 Uiso 1 1 calc GR . . . .
H39B H 0.682653 0.334795 0.464452 0.071 Uiso 1 1 calc GR . . . .
H39C H 0.750928 0.260099 0.506301 0.071 Uiso 1 1 calc GR . . . .
C26 C 0.1407(5) 0.1268(5) 0.7002(3) 0.0497(16) Uani 1 1 d . . . . .
H26A H 0.132700 0.065437 0.706329 0.075 Uiso 1 1 calc GR . . . .
H26B H 0.104941 0.159319 0.724741 0.075 Uiso 1 1 calc GR . . . .
H26C H 0.213281 0.141608 0.714898 0.075 Uiso 1 1 calc GR . . . .
C30 C 0.1889(5) 0.1688(5) 0.3976(3) 0.0513(16) Uani 1 1 d . . . . .
H30A H 0.144778 0.121299 0.376633 0.077 Uiso 1 1 calc GR . . . .
H30B H 0.218852 0.195447 0.367324 0.077 Uiso 1 1 calc GR . . . .
H30C H 0.148615 0.211223 0.412082 0.077 Uiso 1 1 calc GR . . . .
C29 C 0.3431(5) 0.0791(5) 0.4304(4) 0.061(2) Uani 1 1 d . . . . .
H29A H 0.391531 0.048938 0.466118 0.091 Uiso 1 1 calc GR . . . .
H29B H 0.380433 0.114924 0.408710 0.091 Uiso 1 1 calc GR . . . .
H29C H 0.301770 0.037279 0.400092 0.091 Uiso 1 1 calc GR . . . .
O2 O 0.0355(6) 0.4467(5) 0.6550(4) 0.066(2) Uani 0.6667 1 d . . P A 2
C27 C -0.0192(5) 0.1282(8) 0.6097(4) 0.090(3) Uani 1 1 d . . . . .
H27A H -0.050738 0.140545 0.564079 0.135 Uiso 1 1 calc GR . . . .
H27B H -0.051296 0.163494 0.634900 0.135 Uiso 1 1 calc GR . . . .
H27C H -0.028618 0.067610 0.617717 0.135 Uiso 1 1 calc GR . . . .
C49 C -0.0278(10) 0.4120(9) 0.7395(7) 0.066(3) Uani 0.6667 1 d . . P A 2
H49A H -0.001356 0.397020 0.785409 0.079 Uiso 0.6667 1 calc R . P A 2
H49B H -0.094864 0.440261 0.730870 0.079 Uiso 0.6667 1 calc R . P A 2
C47 C -0.0315(11) 0.3758(9) 0.6377(7) 0.084(4) Uani 0.6667 1 d . . P A 2
H47A H -0.006148 0.334402 0.612126 0.101 Uiso 0.6667 1 calc R . P A 2
H47B H -0.100301 0.395004 0.611960 0.101 Uiso 0.6667 1 calc R . P A 2
C48 C -0.0352(14) 0.3352(9) 0.6986(8) 0.087(4) Uani 0.6667 1 d . . P A 2
H48A H -0.099972 0.304018 0.692607 0.105 Uiso 0.6667 1 calc R . P A 2
H48B H 0.022782 0.295739 0.716405 0.105 Uiso 0.6667 1 calc R . P A 2
C50 C 0.0471(9) 0.4689(10) 0.7196(8) 0.079(5) Uani 0.6667 1 d . . P A 2
H50A H 0.030898 0.530079 0.722971 0.095 Uiso 0.6667 1 calc R . P A 2
H50B H 0.117795 0.458133 0.747093 0.095 Uiso 0.6667 1 calc R . P A 2
C54 C 0.0003(18) 0.6284(17) 0.6814(10) 0.065(6) Uani 0.3333 1 d . . P B 1
H54A H 0.026678 0.659434 0.651104 0.097 Uiso 0.3333 1 calc GR . P B 1
H54B H 0.031641 0.651140 0.724553 0.097 Uiso 0.3333 1 calc GR . P B 1
H54C H -0.073752 0.635525 0.669169 0.097 Uiso 0.3333 1 calc GR . P B 1
O3 O -0.0148(13) 0.4837(11) 0.7187(8) 0.064(4) Uani 0.3333 1 d . . P B 1
C53 C 0.027(2) 0.5314(16) 0.6802(12) 0.067(6) Uani 0.3333 1 d . . P B 1
H53A H 0.000288 0.510024 0.635738 0.080 Uiso 0.3333 1 calc R . P B 1
H53B H 0.101459 0.524259 0.694815 0.080 Uiso 0.3333 1 calc R . P B 1
C51 C -0.0475(18) 0.3448(19) 0.7566(11) 0.067(6) Uani 0.3333 1 d . . P B 1
H51A H -0.121411 0.345834 0.735845 0.100 Uiso 0.3333 1 calc GR . P B 1
H51B H -0.031307 0.372157 0.798704 0.100 Uiso 0.3333 1 calc GR . P B 1
H51C H -0.023634 0.285452 0.761779 0.100 Uiso 0.3333 1 calc GR . P B 1
C52 C 0.006(3) 0.394(2) 0.7148(19) 0.098(12) Uani 0.3333 1 d . . P B 1
H52A H 0.080206 0.383439 0.730447 0.118 Uiso 0.3333 1 calc R . P B 1
H52B H -0.020486 0.374302 0.669840 0.118 Uiso 0.3333 1 calc R . P B 1
C13 C 0.0998(4) 0.3590(3) 0.4978(3) 0.0432(14) Uani 1 1 d . U . . .
C15 C 0.0148(4) 0.2234(3) 0.4758(3) 0.0340(10) Uani 1 1 d . U . . .
H15 H 0.015500 0.162745 0.478128 0.041 Uiso 1 1 calc R . . . .
C14 C 0.1046(3) 0.2697(3) 0.5069(2) 0.0248(9) Uani 1 1 d . U . . .
C18 C 0.0112(5) 0.3987(4) 0.4623(4) 0.0623(17) Uani 1 1 d . U . . .
H18 H 0.010282 0.459052 0.456810 0.075 Uiso 1 1 calc R . . . .
C16 C -0.0741(4) 0.2649(4) 0.4420(3) 0.0535(14) Uani 1 1 d . U . . .
H16 H -0.134273 0.232469 0.423754 0.064 Uiso 1 1 calc R . . . .
C17 C -0.0770(5) 0.3516(4) 0.4344(4) 0.0714(19) Uani 1 1 d . U . . .
H17 H -0.138161 0.379332 0.410427 0.086 Uiso 1 1 calc R . . . .


_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
Pu1 I1 3.0274(4) . ?
Pu1 O1 2.452(3) . ?
Pu1 N2 2.428(3) . ?
Pu1 C1 2.907(4) . ?
Pu1 C6 2.969(4) . ?
Pu1 N1 2.469(3) . ?
Pu1 C3 2.903(4) . ?
Pu1 C5 2.969(4) . ?
Pu1 C4 2.925(4) . ?
Pu1 C2 2.905(4) . ?
O1 C46 1.473(5) . ?
O1 C43 1.482(5) . ?
N2 C19 1.448(5) . ?
N2 C14 1.401(5) . ?
C1 C6 1.392(6) . ?
C1 C7 1.473(6) . ?
C1 C2 1.418(6) . ?
C6 C5 1.401(6) . ?
N1 C31 1.438(5) . ?
N1 C8 1.393(5) . ?
C12 C7 1.393(5) . ?
C12 C11 1.382(6) . ?
C9 C8 1.405(6) . ?
C9 C10 1.397(6) . ?
C31 C32 1.417(6) . ?
C31 C36 1.414(6) . ?
C7 C8 1.426(6) . ?
C32 C40 1.514(6) . ?
C32 C33 1.398(6) . ?
C3 C4 1.406(7) . ?
C3 C2 1.387(6) . ?
C46 C45 1.508(6) . ?
C5 C4 1.395(7) . ?
C40 C41 1.528(7) . ?
C40 C42 1.532(7) . ?
C43 C44 1.505(6) . ?
C33 C34 1.389(7) . ?
C4 C13 1.474(7) . ?
C36 C35 1.403(6) . ?
C36 C37 1.524(6) . ?
C11 C10 1.389(7) . ?
C45 C44 1.515(7) . ?
C35 C34 1.371(7) . ?
C37 C38 1.513(7) . ?
C37 C39 1.525(7) . ?
C19 C24 1.401(7) . ?
C19 C20 1.411(7) . ?
C24 C25 1.522(9) . ?
C24 C23 1.413(8) . ?
C28 C20 1.533(8) . ?
C28 C30 1.538(9) . ?
C28 C29 1.512(8) . ?
C20 C21 1.399(7) . ?
C25 C26 1.532(7) . ?
C25 C27 1.545(8) . ?
C22 C23 1.375(10) . ?
C22 C21 1.359(10) . ?
O2 C47 1.417(14) . ?
O2 C50 1.423(16) . ?
C49 C48 1.484(19) . ?
C49 C50 1.53(2) . ?
C47 C48 1.50(2) . ?
C54 C53 1.56(4) . ?
O3 C53 1.38(3) . ?
O3 C52 1.44(4) . ?
C51 C52 1.55(4) . ?
C13 C14 1.409(6) . ?
C13 C18 1.379(7) . ?
C15 C14 1.415(6) . ?
C15 C16 1.383(7) . ?
C18 C17 1.392(8) . ?
C16 C17 1.364(8) . ?

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 Pu1 I1 89.69(7) . . ?
O1 Pu1 C1 150.47(11) . . ?
O1 Pu1 C6 159.54(11) . . ?
O1 Pu1 N1 89.26(11) . . ?
O1 Pu1 C3 143.22(12) . . ?
O1 Pu1 C5 158.85(12) . . ?
O1 Pu1 C4 149.34(11) . . ?
O1 Pu1 C2 143.62(11) . . ?
N2 Pu1 I1 103.91(8) . . ?
N2 Pu1 O1 88.86(11) . . ?
N2 Pu1 C1 117.46(12) . . ?
N2 Pu1 C6 106.80(12) . . ?
N2 Pu1 N1 153.97(12) . . ?
N2 Pu1 C3 70.93(12) . . ?
N2 Pu1 C5 79.90(12) . . ?
N2 Pu1 C4 60.58(12) . . ?
N2 Pu1 C2 98.20(12) . . ?
C1 Pu1 I1 96.08(8) . . ?
C1 Pu1 C6 27.39(12) . . ?
C1 Pu1 C5 48.68(12) . . ?
C1 Pu1 C4 57.88(12) . . ?
C6 Pu1 I1 74.05(9) . . ?
C6 Pu1 C5 27.29(12) . . ?
N1 Pu1 I1 102.04(8) . . ?
N1 Pu1 C1 61.21(11) . . ?
N1 Pu1 C6 82.28(11) . . ?
N1 Pu1 C3 95.94(12) . . ?
N1 Pu1 C5 108.63(12) . . ?
N1 Pu1 C4 116.73(12) . . ?
N1 Pu1 C2 69.07(12) . . ?
C3 Pu1 I1 124.29(10) . . ?
C3 Pu1 C1 49.46(12) . . ?
C3 Pu1 C6 56.70(12) . . ?
C3 Pu1 C5 48.39(14) . . ?
C3 Pu1 C4 27.93(14) . . ?
C3 Pu1 C2 27.64(13) . . ?
C5 Pu1 I1 75.90(10) . . ?
C4 Pu1 I1 99.63(11) . . ?
C4 Pu1 C6 48.76(12) . . ?
C4 Pu1 C5 27.36(14) . . ?
C2 Pu1 I1 122.43(9) . . ?
C2 Pu1 C1 28.24(12) . . ?
C2 Pu1 C6 48.66(12) . . ?
C2 Pu1 C5 56.63(13) . . ?
C2 Pu1 C4 49.29(13) . . ?
C46 O1 Pu1 126.1(2) . . ?
C46 O1 C43 107.4(3) . . ?
C43 O1 Pu1 125.9(2) . . ?
C19 N2 Pu1 116.1(2) . . ?
C14 N2 Pu1 131.4(3) . . ?
C14 N2 C19 112.4(3) . . ?
C6 C1 Pu1 78.8(2) . . ?
C6 C1 C7 123.1(4) . . ?
C6 C1 C2 118.9(4) . . ?
C7 C1 Pu1 111.1(2) . . ?
C2 C1 Pu1 75.8(2) . . ?
C2 C1 C7 117.7(4) . . ?
C1 C6 Pu1 73.9(2) . . ?
C1 C6 C5 120.3(4) . . ?
C5 C6 Pu1 76.4(2) . . ?
C31 N1 Pu1 117.5(2) . . ?
C8 N1 Pu1 129.0(3) . . ?
C8 N1 C31 113.3(3) . . ?
C11 C12 C7 121.6(4) . . ?
C10 C9 C8 120.9(4) . . ?
C32 C31 N1 120.8(4) . . ?
C36 C31 N1 119.7(4) . . ?
C36 C31 C32 119.5(4) . . ?
C12 C7 C1 122.6(4) . . ?
C12 C7 C8 121.1(4) . . ?
C8 C7 C1 116.4(3) . . ?
C31 C32 C40 121.6(4) . . ?
C33 C32 C31 118.8(4) . . ?
C33 C32 C40 119.5(4) . . ?
C4 C3 Pu1 76.9(3) . . ?
C2 C3 Pu1 76.3(2) . . ?
C2 C3 C4 121.0(4) . . ?
N1 C8 C9 124.8(4) . . ?
N1 C8 C7 118.9(4) . . ?
C9 C8 C7 116.4(4) . . ?
O1 C46 C45 104.3(4) . . ?
C6 C5 Pu1 76.3(2) . . ?
C4 C5 Pu1 74.6(2) . . ?
C4 C5 C6 121.0(5) . . ?
C32 C40 C41 113.8(4) . . ?
C32 C40 C42 110.4(4) . . ?
C41 C40 C42 108.3(4) . . ?
O1 C43 C44 106.0(4) . . ?
C34 C33 C32 121.1(4) . . ?
C3 C4 Pu1 75.2(2) . . ?
C3 C4 C13 117.9(5) . . ?
C5 C4 Pu1 78.1(3) . . ?
C5 C4 C3 118.5(4) . . ?
C5 C4 C13 123.3(5) . . ?
C13 C4 Pu1 111.9(3) . . ?
C31 C36 C37 121.9(4) . . ?
C35 C36 C31 119.1(4) . . ?
C35 C36 C37 119.0(4) . . ?
C12 C11 C10 117.7(4) . . ?
C11 C10 C9 122.0(4) . . ?
C46 C45 C44 101.3(4) . . ?
C34 C35 C36 121.2(4) . . ?
C36 C37 C39 112.1(4) . . ?
C38 C37 C36 110.8(4) . . ?
C38 C37 C39 111.0(5) . . ?
C1 C2 Pu1 76.0(2) . . ?
C3 C2 Pu1 76.1(2) . . ?
C3 C2 C1 120.1(4) . . ?
C43 C44 C45 103.2(4) . . ?
C35 C34 C33 120.0(4) . . ?
C24 C19 N2 120.8(4) . . ?
C24 C19 C20 120.9(4) . . ?
C20 C19 N2 118.2(4) . . ?
C19 C24 C25 123.1(5) . . ?
C19 C24 C23 117.5(6) . . ?
C23 C24 C25 119.3(5) . . ?
C20 C28 C30 111.1(4) . . ?
C29 C28 C20 115.9(5) . . ?
C29 C28 C30 107.7(5) . . ?
C19 C20 C28 122.5(4) . . ?
C21 C20 C19 118.5(5) . . ?
C21 C20 C28 119.0(5) . . ?
C24 C25 C26 113.2(5) . . ?
C24 C25 C27 110.5(6) . . ?
C26 C25 C27 106.9(5) . . ?
C21 C22 C23 120.3(5) . . ?
C22 C23 C24 121.5(6) . . ?
C22 C21 C20 121.2(6) . . ?
C47 O2 C50 108.7(10) . . ?
C48 C49 C50 103.0(13) . . ?
O2 C47 C48 107.0(12) . . ?
C49 C48 C47 100.5(12) . . ?
O2 C50 C49 105.4(10) . . ?
C53 O3 C52 111(2) . . ?
O3 C53 C54 112.0(18) . . ?
O3 C52 C51 108(3) . . ?
C14 C13 C4 116.1(4) . . ?
C18 C13 C4 122.4(5) . . ?
C18 C13 C14 121.4(5) . . ?
C16 C15 C14 121.2(5) . . ?
N2 C14 C13 118.7(4) . . ?
N2 C14 C15 125.0(4) . . ?
C13 C14 C15 116.3(4) . . ?
C13 C18 C17 120.8(5) . . ?
C17 C16 C15 121.3(5) . . ?
C16 C17 C18 118.9(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT971_3_Pu                
;
PROBLEM: Check Calcd Resid. Dens. 0.89Ang From Pu1 3.06 eA-3
RESPONSE: The residual density is attributed to absorption 
artefacts due to insufficient absorption correction due to Pu 
atom
;
_vrf_PLAT972_3_Pu                
;
PROBLEM: Check Calcd Resid. Dens. 0.97Ang From Pu1 -2.72 eA-3
RESPONSE: The residual density is attributed to absorption 
artefacts due to insufficient absorption correction due to Pu 
atom
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_3_U
_database_code_depnum_ccdc_archive 'CCDC 2238473'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_audit_creation_date             2022-11-01
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H54 I N2 O U, 0.8(C4 H8 O), 0.2(C4 H10 O)'
_chemical_formula_sum            'C50 H62.40 I N2 O2 U'
_chemical_formula_weight         1088.35
_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 0.0033 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'
I I -0.4742 1.8119 '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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.7779(8)
_cell_length_b                   15.6184(10)
_cell_length_c                   21.8752(13)
_cell_angle_alpha                90
_cell_angle_beta                 107.8970(10)
_cell_angle_gamma                90
_cell_volume                     4479.5(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.529
_cell_measurement_theta_min      2.450
_shelx_estimated_absorpt_T_max   0.476
_shelx_estimated_absorpt_T_min   0.476
_exptl_absorpt_coefficient_mu    4.353
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1030 before and 0.0466 after correction. The Ratio of minimum to maximum transmission is 0.7228. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2150
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            134834
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.560
_diffrn_reflns_theta_min         1.957
_diffrn_ambient_temperature      100.02
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12929
_reflns_number_total             13721
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00015(2)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         13721
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0161
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0108P)²+4.7647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0353
_refine_ls_wR_factor_ref         0.0362
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C76-C3 \\sim O56-C5
 with sigma of 0.02
2. Others
 Fixed Sof: O56(0.8) C76(0.8) H76A(0.8) H76B(0.8) C3(0.8) H3A(0.8) H3B(0.8)
 C4(0.8) H4A(0.8) H4B(0.8) C5(0.8) H5A(0.8) H5B(0.8) O0AA(0.2) C1AA(0.2)
 H1AA(0.2) H1AB(0.2) C2AA(0.2) H2AA(0.2) H2AB(0.2) H2AC(0.2) C3AA(0.2)
 H3AA(0.2) H3AB(0.2) H3AC(0.2) C0AA(0.2) H0AA(0.2) H0AB(0.2)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C16(H16), C32(H32), C48(H48)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C40(H40A,H40B), C57(H57A,H57B), C76(H76A,
 H76B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C1AA(H1AA,H1AB), C0AA(H0AA,H0AB)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C21(H21), C23(H23), C24(H24), C27(H27), C28(H28), C35(H35),
 C36(H36), C37(H37), C41(H41), C43(H43), C46(H46), C47(H47), C49(H49), C58(H58),
  C61(H61), C65(H65), C79(H79)
3.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C54(H54A,H54B,
 H54C), C59(H59A,H59B,H59C), C70(H70A,H70B,H70C), C1(H1A,H1B,H1C), C2(H2A,H2B,
 H2C), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC)
;
_atom_sites_solution_hydrogens   geom
_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 0.14537(2) 0.20128(2) 0.39327(2) 0.01023(2) Uani 1 1 d . . . . .
I2 I 0.17837(2) 0.16745(2) 0.26361(2) 0.01883(2) Uani 1 1 d . . . . .
N1 N 0.30534(10) 0.26698(8) 0.45659(6) 0.0122(2) Uani 1 1 d . . . . .
N2 N -0.03405(10) 0.15381(8) 0.37380(6) 0.0117(2) Uani 1 1 d . . . . .
O1 O 0.08032(9) 0.34710(7) 0.35489(5) 0.0155(2) Uani 1 1 d . . . . .
C40 C -0.12538(13) 0.20186(10) 0.23785(7) 0.0176(3) Uani 1 1 d . . . . .
H9 H -0.062266 0.167268 0.257033 0.021 Uiso 1 1 calc R . . . .
C5 C 0.18202(12) 0.01694(9) 0.38946(8) 0.0149(3) Uani 1 1 d . . . . .
H10 H 0.166260 -0.012931 0.349775 0.018 Uiso 1 1 calc R . . . .
C14 C -0.07075(11) 0.07072(9) 0.37235(7) 0.0126(3) Uani 1 1 d . . . . .
C6 C 0.02344(13) 0.40410(10) 0.38511(8) 0.0187(3) Uani 1 1 d . . . . .
H13A H 0.059693 0.410307 0.431573 0.022 Uiso 1 1 calc R . . . .
H13B H -0.045553 0.380907 0.379759 0.022 Uiso 1 1 calc R . . . .
C43 C 0.10466(13) 0.39558(10) 0.30400(8) 0.0180(3) Uani 1 1 d . . . . .
H15A H 0.100967 0.358375 0.266708 0.022 Uiso 1 1 calc R . . . .
H15B H 0.173827 0.420735 0.319985 0.022 Uiso 1 1 calc R . . . .
C37 C -0.11821(12) 0.21862(10) 0.47235(7) 0.0157(3) Uani 1 1 d . . . . .
H16 H -0.075809 0.166312 0.473531 0.019 Uiso 1 1 calc R . . . .
C36 C -0.15237(12) 0.24601(10) 0.29226(7) 0.0142(3) Uani 1 1 d . . . . .
C32 C -0.15243(12) 0.25153(9) 0.40373(7) 0.0142(3) Uani 1 1 d . . . . .
C13 C -0.00018(12) 0.00220(9) 0.39016(7) 0.0129(3) Uani 1 1 d . . . . .
C35 C -0.22290(13) 0.31295(10) 0.27825(8) 0.0188(3) Uani 1 1 d . . . . .
H21 H -0.247659 0.333913 0.235490 0.023 Uiso 1 1 calc R . . . .
C1 C 0.30421(12) 0.09461(9) 0.47523(8) 0.0177(3) Uani 1 1 d . . . . .
C18 C -0.03168(13) -0.08254(10) 0.38173(7) 0.0158(3) Uani 1 1 d . . . . .
H23 H 0.017804 -0.126948 0.392284 0.019 Uiso 1 1 calc R . . . .
C46 C 0.28013(12) 0.05130(10) 0.41670(8) 0.0173(3) Uani 1 1 d . . . . .
H24 H 0.330086 0.045029 0.395236 0.021 Uiso 1 1 calc R . . . .
C24 C 0.26965(13) 0.40711(10) 0.49582(8) 0.0188(3) Uani 1 1 d . . . . .
C19 C 0.30977(11) 0.35864(9) 0.45436(7) 0.0144(3) Uani 1 1 d . . . . .
C34 C -0.25750(13) 0.34940(11) 0.32534(8) 0.0200(3) Uani 1 1 d . . . . .
H27 H -0.304116 0.395940 0.315173 0.024 Uiso 1 1 calc R . . . .
C3 C 0.13389(12) 0.06666(10) 0.48057(7) 0.0156(3) Uani 1 1 d . . . . .
H28 H 0.084957 0.070642 0.503001 0.019 Uiso 1 1 calc R . . . .
C31 C -0.11285(11) 0.21744(9) 0.35654(7) 0.0121(3) Uani 1 1 d . . . . .
C20 C 0.35562(13) 0.40034(11) 0.41314(8) 0.0200(3) Uani 1 1 d . . . . .
C28 C 0.22750(14) 0.36384(12) 0.54476(9) 0.0238(3) Uani 1 1 d . . . . .
H32 H 0.186627 0.313255 0.523234 0.029 Uiso 1 1 calc R . . . .
C4 C 0.10763(12) 0.02627(9) 0.42008(7) 0.0131(3) Uani 1 1 d . . . . .
C7 C 0.40141(13) 0.14106(10) 0.50265(9) 0.0218(3) Uani 1 1 d . . . . .
C9 C 0.48687(13) 0.27642(10) 0.52418(8) 0.0199(3) Uani 1 1 d . . . . .
H35 H 0.487187 0.336946 0.519956 0.024 Uiso 1 1 calc R . . . .
C16 C -0.20530(13) -0.03737(10) 0.34559(7) 0.0176(3) Uani 1 1 d . . . . .
H36 H -0.275988 -0.050724 0.331805 0.021 Uiso 1 1 calc R . . . .
C12 C 0.48905(16) 0.10086(12) 0.54008(13) 0.0425(6) Uani 1 1 d . . . . .
H37 H 0.489060 0.040615 0.546038 0.051 Uiso 1 1 calc R . . . .
C41 C -0.10460(16) 0.26325(13) 0.18931(8) 0.0262(4) Uani 1 1 d . . . . .
H38A H -0.167121 0.294716 0.167301 0.039 Uiso 1 1 calc GR . . . .
H38B H -0.082159 0.230789 0.157753 0.039 Uiso 1 1 calc GR . . . .
H38C H -0.051144 0.303780 0.211616 0.039 Uiso 1 1 calc GR . . . .
C42 C -0.21107(15) 0.14026(12) 0.20276(9) 0.0262(4) Uani 1 1 d . . . . .
H39A H -0.217593 0.095126 0.232369 0.039 Uiso 1 1 calc GR . . . .
H39B H -0.194908 0.114462 0.166215 0.039 Uiso 1 1 calc GR . . . .
H39C H -0.275466 0.171834 0.187266 0.039 Uiso 1 1 calc GR . . . .
C44 C 0.02480(15) 0.46447(11) 0.28599(8) 0.0228(3) Uani 1 1 d . . . . .
H40A H -0.040742 0.442171 0.257451 0.027 Uiso 1 1 calc R . . . .
H40B H 0.047194 0.513301 0.264786 0.027 Uiso 1 1 calc R . . . .
C15 C -0.17504(12) 0.04797(10) 0.35277(7) 0.0157(3) Uani 1 1 d . . . . .
H41 H -0.225356 0.091695 0.344373 0.019 Uiso 1 1 calc R . . . .
C26 C 0.35978(15) 0.37402(14) 0.29959(9) 0.0294(4) Uani 1 1 d . . . . .
H42A H 0.288203 0.356002 0.284840 0.044 Uiso 1 1 calc GR . . . .
H42B H 0.397653 0.343982 0.274800 0.044 Uiso 1 1 calc GR . . . .
H42C H 0.363932 0.435917 0.293472 0.044 Uiso 1 1 calc GR . . . .
C10 C 0.57465(14) 0.23511(12) 0.56049(11) 0.0326(4) Uani 1 1 d . . . . .
H43 H 0.634407 0.267709 0.579895 0.039 Uiso 1 1 calc R . . . .
C8 C 0.39729(12) 0.23054(10) 0.49345(7) 0.0156(3) Uani 1 1 d . . . . .
C2 C 0.23073(13) 0.10067(10) 0.50763(8) 0.0177(3) Uani 1 1 d . . . . .
H46 H 0.247441 0.128204 0.548270 0.021 Uiso 1 1 calc R . . . .
C21 C 0.35813(15) 0.49043(12) 0.41376(9) 0.0299(4) Uani 1 1 d . . . . .
H47 H 0.389046 0.519659 0.386468 0.036 Uiso 1 1 calc R . . . .
C25 C 0.40595(13) 0.35242(13) 0.37090(8) 0.0249(4) Uani 1 1 d . . . . .
H48 H 0.397234 0.289650 0.376558 0.030 Uiso 1 1 calc R . . . .
C17 C -0.13454(13) -0.10347(10) 0.35809(8) 0.0183(3) Uani 1 1 d . . . . .
H49 H -0.155837 -0.161426 0.350700 0.022 Uiso 1 1 calc R . . . .
C39 C -0.20805(16) 0.19296(17) 0.49504(10) 0.0381(5) Uani 1 1 d . . . . .
H54A H -0.250370 0.243364 0.495139 0.057 Uiso 1 1 calc GR . . . .
H54B H -0.182710 0.169444 0.538600 0.057 Uiso 1 1 calc GR . . . .
H54C H -0.248916 0.149566 0.465987 0.057 Uiso 1 1 calc GR . . . .
C45 C 0.01648(17) 0.48961(11) 0.35137(9) 0.0264(4) Uani 1 1 d . . . . .
H57A H 0.073040 0.527968 0.374520 0.032 Uiso 1 1 calc R . . . .
H57B H -0.049330 0.518268 0.347226 0.032 Uiso 1 1 calc R . . . .
C33 C -0.22374(12) 0.31762(10) 0.38735(8) 0.0173(3) Uani 1 1 d . . . . .
H58 H -0.249576 0.341216 0.419264 0.021 Uiso 1 1 calc R . . . .
C29 C 0.31247(18) 0.33072(16) 0.60287(10) 0.0363(5) Uani 1 1 d . . . . .
H59A H 0.353324 0.288241 0.588686 0.055 Uiso 1 1 calc GR . . . .
H59B H 0.282368 0.304131 0.633386 0.055 Uiso 1 1 calc GR . . . .
H59C H 0.356172 0.378551 0.623754 0.055 Uiso 1 1 calc GR . . . .
C11 C 0.57694(17) 0.14748(14) 0.56900(14) 0.0486(7) Uani 1 1 d . . . . .
H61 H 0.637373 0.119683 0.594113 0.058 Uiso 1 1 calc R . . . .
C23 C 0.27336(16) 0.49600(11) 0.49348(10) 0.0288(4) Uani 1 1 d . . . . .
H65 H 0.245244 0.528903 0.520444 0.035 Uiso 1 1 calc R . . . .
C27 C 0.52099(16) 0.3722(2) 0.39058(11) 0.0458(6) Uani 1 1 d . . . . .
H70A H 0.531022 0.433262 0.384156 0.069 Uiso 1 1 calc GR . . . .
H70B H 0.552683 0.338283 0.364164 0.069 Uiso 1 1 calc GR . . . .
H70C H 0.552447 0.357630 0.435959 0.069 Uiso 1 1 calc GR . . . .
C22 C 0.31685(17) 0.53708(12) 0.45296(10) 0.0337(5) Uani 1 1 d . . . . .
H79 H 0.318431 0.597867 0.451991 0.040 Uiso 1 1 calc R . . . .
O3 O 0.53669(16) 0.55189(13) 0.15391(10) 0.0400(4) Uiso 0.8 1 d D . P A 2
C53 C 0.4594(3) 0.6618(2) 0.19364(16) 0.0483(7) Uiso 0.8 1 d D . P A 2
H76A H 0.393021 0.690891 0.186690 0.058 Uiso 0.8 1 calc R . P A 2
H76B H 0.515189 0.703880 0.209777 0.058 Uiso 0.8 1 calc R . P A 2
C38 C -0.05174(19) 0.28425(14) 0.51712(9) 0.0385(5) Uani 1 1 d . . . . .
H1A H 0.005645 0.299538 0.501678 0.058 Uiso 1 1 calc GR . . . .
H1B H -0.025749 0.260105 0.560450 0.058 Uiso 1 1 calc GR . . . .
H1C H -0.092156 0.335553 0.518170 0.058 Uiso 1 1 calc GR . . . .
C30 C 0.15756(16) 0.42038(15) 0.57032(11) 0.0349(5) Uani 1 1 d . . . . .
H2A H 0.198485 0.463855 0.599260 0.052 Uiso 1 1 calc GR . . . .
H2B H 0.122273 0.384876 0.593765 0.052 Uiso 1 1 calc GR . . . .
H2C H 0.107245 0.448546 0.534250 0.052 Uiso 1 1 calc GR . . . .
C52 C 0.4713(2) 0.5868(2) 0.23893(15) 0.0393(6) Uiso 0.8 1 d D . P A 2
H3A H 0.405498 0.557059 0.232760 0.047 Uiso 0.8 1 calc R . P A 2
H3B H 0.499226 0.605071 0.284310 0.047 Uiso 0.8 1 calc R . P A 2
C51 C 0.5461(3) 0.5308(2) 0.21907(16) 0.0440(7) Uiso 0.8 1 d . . P A 2
H4A H 0.616499 0.541707 0.247035 0.053 Uiso 0.8 1 calc R . P A 2
H4B H 0.530001 0.469548 0.222634 0.053 Uiso 0.8 1 calc R . P A 2
C54 C 0.4651(3) 0.6192(2) 0.13390(16) 0.0477(7) Uiso 0.8 1 d D . P A 2
H5A H 0.397464 0.596277 0.109025 0.057 Uiso 0.8 1 calc R . P A 2
H5B H 0.487626 0.660338 0.106606 0.057 Uiso 0.8 1 calc R . P A 2
O2 O 0.4854(9) 0.5167(7) 0.2201(5) 0.057(2) Uiso 0.2 1 d . . P B 1
C49 C 0.5309(12) 0.4714(10) 0.1829(8) 0.057(4) Uiso 0.2 1 d . . P B 1
H1AA H 0.605859 0.478434 0.199886 0.069 Uiso 0.2 1 calc R . P B 1
H1AB H 0.507967 0.493812 0.138409 0.069 Uiso 0.2 1 calc R . P B 1
C50 C 0.5024(12) 0.3723(10) 0.1827(8) 0.058(4) Uiso 0.2 1 d . . P B 1
H2AA H 0.518460 0.351853 0.227066 0.086 Uiso 0.2 1 calc GR . P B 1
H2AB H 0.541763 0.339573 0.160302 0.086 Uiso 0.2 1 calc GR . P B 1
H2AC H 0.429355 0.364745 0.160676 0.086 Uiso 0.2 1 calc GR . P B 1
C47 C 0.4525(13) 0.6509(11) 0.2562(8) 0.063(4) Uiso 0.2 1 d . . P B 1
H3AA H 0.475955 0.710282 0.264451 0.095 Uiso 0.2 1 calc GR . P B 1
H3AB H 0.465049 0.620594 0.297107 0.095 Uiso 0.2 1 calc GR . P B 1
H3AC H 0.379344 0.650287 0.232939 0.095 Uiso 0.2 1 calc GR . P B 1
C48 C 0.5046(16) 0.6112(13) 0.2199(10) 0.073(5) Uiso 0.2 1 d . . P B 1
H0AA H 0.578575 0.622894 0.238092 0.088 Uiso 0.2 1 calc R . P B 1
H0AB H 0.481214 0.633332 0.175371 0.088 Uiso 0.2 1 calc R . P B 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 I2 3.05339(19) . ?
U1 N1 2.4398(13) . ?
U1 N2 2.4890(13) . ?
U1 O1 2.4965(11) . ?
U1 C5 2.9286(14) . ?
U1 C1 2.8928(15) . ?
U1 C46 2.9346(15) . ?
U1 C3 2.8773(15) . ?
U1 C4 2.8764(14) . ?
U1 C2 2.8814(15) . ?
N1 C19 1.4344(19) . ?
N1 C8 1.3968(19) . ?
N2 C14 1.3895(18) . ?
N2 C31 1.4343(18) . ?
O1 C6 1.4704(19) . ?
O1 C43 1.4679(18) . ?
C40 C36 1.517(2) . ?
C40 C41 1.522(2) . ?
C40 C42 1.534(2) . ?
C5 C46 1.405(2) . ?
C5 C4 1.394(2) . ?
C14 C13 1.418(2) . ?
C14 C15 1.413(2) . ?
C6 C45 1.515(2) . ?
C43 C44 1.502(2) . ?
C37 C32 1.518(2) . ?
C37 C39 1.522(2) . ?
C37 C38 1.516(3) . ?
C36 C35 1.396(2) . ?
C36 C31 1.415(2) . ?
C32 C31 1.412(2) . ?
C32 C33 1.394(2) . ?
C13 C18 1.387(2) . ?
C13 C4 1.476(2) . ?
C35 C34 1.384(2) . ?
C1 C46 1.395(2) . ?
C1 C7 1.478(2) . ?
C1 C2 1.406(2) . ?
C18 C17 1.390(2) . ?
C24 C19 1.418(2) . ?
C24 C28 1.524(3) . ?
C24 C23 1.391(2) . ?
C19 C20 1.409(2) . ?
C34 C33 1.384(2) . ?
C3 C4 1.409(2) . ?
C3 C2 1.388(2) . ?
C20 C21 1.408(3) . ?
C20 C25 1.513(3) . ?
C28 C29 1.529(3) . ?
C28 C30 1.534(3) . ?
C7 C12 1.384(2) . ?
C7 C8 1.411(2) . ?
C9 C10 1.385(2) . ?
C9 C8 1.407(2) . ?
C16 C15 1.391(2) . ?
C16 C17 1.388(2) . ?
C12 C11 1.388(3) . ?
C44 C45 1.521(2) . ?
C26 C25 1.530(2) . ?
C10 C11 1.380(3) . ?
C21 C22 1.374(3) . ?
C25 C27 1.541(3) . ?
C23 C22 1.372(3) . ?
O3 C51 1.430(4) . ?
O3 C54 1.416(4) . ?
C53 C52 1.510(4) . ?
C53 C54 1.490(5) . ?
C52 C51 1.514(4) . ?
O2 C49 1.368(18) . ?
O2 C48 1.50(2) . ?
C49 C50 1.60(2) . ?
C47 C48 1.37(2) . ?

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
N1 U1 I2 103.52(3) . . ?
N1 U1 N2 154.00(4) . . ?
N1 U1 O1 88.60(4) . . ?
N1 U1 C5 107.22(4) . . ?
N1 U1 C1 60.72(4) . . ?
N1 U1 C46 79.86(4) . . ?
N1 U1 C3 98.91(4) . . ?
N1 U1 C4 118.18(4) . . ?
N1 U1 C2 71.33(4) . . ?
N2 U1 I2 102.31(3) . . ?
N2 U1 O1 88.81(4) . . ?
N2 U1 C5 82.71(4) . . ?
N2 U1 C1 117.19(4) . . ?
N2 U1 C46 109.51(4) . . ?
N2 U1 C3 69.00(4) . . ?
N2 U1 C4 61.28(4) . . ?
N2 U1 C2 96.03(4) . . ?
O1 U1 I2 89.20(3) . . ?
O1 U1 C5 159.15(4) . . ?
O1 U1 C1 149.19(4) . . ?
O1 U1 C46 158.34(4) . . ?
O1 U1 C3 143.37(4) . . ?
O1 U1 C4 150.09(4) . . ?
O1 U1 C2 142.94(4) . . ?
C5 U1 I2 74.17(3) . . ?
C5 U1 C46 27.74(4) . . ?
C1 U1 I2 100.13(4) . . ?
C1 U1 C5 49.25(4) . . ?
C1 U1 C46 27.69(5) . . ?
C46 U1 I2 75.95(3) . . ?
C3 U1 I2 122.98(3) . . ?
C3 U1 C5 49.13(4) . . ?
C3 U1 C1 49.70(5) . . ?
C3 U1 C46 57.43(5) . . ?
C3 U1 C2 27.90(4) . . ?
C4 U1 I2 96.48(3) . . ?
C4 U1 C5 27.77(4) . . ?
C4 U1 C1 58.40(4) . . ?
C4 U1 C46 49.47(4) . . ?
C4 U1 C3 28.35(4) . . ?
C4 U1 C2 49.90(4) . . ?
C2 U1 I2 125.07(3) . . ?
C2 U1 C5 57.36(4) . . ?
C2 U1 C1 28.19(5) . . ?
C2 U1 C46 49.12(5) . . ?
C19 N1 U1 116.16(9) . . ?
C8 N1 U1 131.09(10) . . ?
C8 N1 C19 112.68(12) . . ?
C14 N2 U1 128.13(9) . . ?
C14 N2 C31 113.61(12) . . ?
C31 N2 U1 118.05(9) . . ?
C6 O1 U1 125.95(9) . . ?
C43 O1 U1 125.70(9) . . ?
C43 O1 C6 107.83(11) . . ?
C36 C40 C41 113.90(14) . . ?
C36 C40 C42 109.95(14) . . ?
C41 C40 C42 109.09(14) . . ?
C46 C5 U1 76.37(8) . . ?
C4 C5 U1 74.03(8) . . ?
C4 C5 C46 120.65(14) . . ?
N2 C14 C13 118.99(13) . . ?
N2 C14 C15 124.81(14) . . ?
C15 C14 C13 116.18(13) . . ?
O1 C6 C45 106.12(13) . . ?
O1 C43 C44 104.40(13) . . ?
C32 C37 C39 112.02(14) . . ?
C38 C37 C32 110.62(13) . . ?
C38 C37 C39 110.96(17) . . ?
C35 C36 C40 119.34(14) . . ?
C35 C36 C31 118.93(14) . . ?
C31 C36 C40 121.60(13) . . ?
C31 C32 C37 121.53(13) . . ?
C33 C32 C37 119.02(14) . . ?
C33 C32 C31 119.44(14) . . ?
C14 C13 C4 116.19(13) . . ?
C18 C13 C14 121.57(14) . . ?
C18 C13 C4 122.21(14) . . ?
C34 C35 C36 121.38(15) . . ?
C46 C1 U1 77.82(9) . . ?
C46 C1 C7 122.72(16) . . ?
C46 C1 C2 119.35(15) . . ?
C7 C1 U1 112.79(10) . . ?
C2 C1 U1 75.46(9) . . ?
C2 C1 C7 117.73(15) . . ?
C13 C18 C17 121.02(15) . . ?
C5 C46 U1 75.89(9) . . ?
C1 C46 U1 74.49(9) . . ?
C1 C46 C5 120.06(15) . . ?
C19 C24 C28 121.36(14) . . ?
C23 C24 C19 118.91(17) . . ?
C23 C24 C28 119.66(16) . . ?
C24 C19 N1 118.83(14) . . ?
C20 C19 N1 121.00(14) . . ?
C20 C19 C24 120.15(14) . . ?
C35 C34 C33 119.55(15) . . ?
C4 C3 U1 75.79(8) . . ?
C2 C3 U1 76.21(9) . . ?
C2 C3 C4 120.50(15) . . ?
C36 C31 N2 120.61(13) . . ?
C32 C31 N2 120.00(13) . . ?
C32 C31 C36 119.38(13) . . ?
C19 C20 C25 122.82(15) . . ?
C21 C20 C19 118.06(17) . . ?
C21 C20 C25 119.07(16) . . ?
C24 C28 C29 111.97(15) . . ?
C24 C28 C30 114.74(17) . . ?
C29 C28 C30 107.34(16) . . ?
C5 C4 U1 78.20(8) . . ?
C5 C4 C13 123.28(14) . . ?
C5 C4 C3 118.92(14) . . ?
C13 C4 U1 111.84(9) . . ?
C3 C4 U1 75.86(8) . . ?
C3 C4 C13 117.61(14) . . ?
C12 C7 C1 122.30(15) . . ?
C12 C7 C8 121.57(16) . . ?
C8 C7 C1 115.88(14) . . ?
C10 C9 C8 121.33(15) . . ?
C17 C16 C15 121.49(15) . . ?
C7 C12 C11 120.81(18) . . ?
C43 C44 C45 101.49(14) . . ?
C16 C15 C14 121.12(15) . . ?
C11 C10 C9 121.25(17) . . ?
N1 C8 C7 118.40(14) . . ?
N1 C8 C9 125.12(14) . . ?
C9 C8 C7 116.45(14) . . ?
C1 C2 U1 76.36(9) . . ?
C3 C2 U1 75.89(9) . . ?
C3 C2 C1 120.39(15) . . ?
C22 C21 C20 121.48(18) . . ?
C20 C25 C26 112.87(16) . . ?
C20 C25 C27 110.82(17) . . ?
C26 C25 C27 108.08(15) . . ?
C16 C17 C18 118.19(14) . . ?
C6 C45 C44 102.63(13) . . ?
C34 C33 C32 121.04(15) . . ?
C10 C11 C12 118.57(18) . . ?
C22 C23 C24 121.25(19) . . ?
C23 C22 C21 120.11(17) . . ?
C54 O3 C51 108.7(2) . . ?
C54 C53 C52 101.8(3) . . ?
C53 C52 C51 101.9(3) . . ?
O3 C51 C52 107.0(3) . . ?
O3 C54 C53 106.3(3) . . ?
C49 O2 C48 113.2(13) . . ?
O2 C49 C50 110.2(13) . . ?
C47 C48 O2 108.6(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2_Ce
_database_code_depnum_ccdc_archive 'CCDC 2238467'
loop_
_audit_author_name
_audit_author_address
'Jesse Murillo'
;Los Alamos National Labratory 
United States of America
;
_audit_update_record             
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_audit_creation_date             2023-01-20
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C100 H131.24 Ce2 Cl4 K2 N4 O5'
_chemical_formula_sum            'C100 H131.24 Ce2 Cl4 K2 N4 O5'
_chemical_formula_weight         1969.56
_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 0.0033 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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3524(4)
_cell_length_b                   16.9877(5)
_cell_length_c                   25.6828(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.9300(10)
_cell_angle_gamma                90
_cell_volume                     5824.8(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.489
_cell_measurement_theta_min      2.526
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.892
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0740 before and 0.0612 after correction. The Ratio of minimum to maximum transmission is 0.8270. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2042
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            240020
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_min         1.940
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14935
_reflns_number_total             17795
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         17795
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0272P)²+11.5017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1009
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Others
 Fixed Sof: C48(0.5) H2AA(0.5) H2AB(0.5) O3(0.5) O2(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) H1BD(0.5) H1BE(0.5) H1BF(0.5) O4(0.5) C53(0.5) H3AA(0.5) H3AB(0.5)
 C49(0.5) H4AA(0.5) H4AB(0.5) C52(0.5) H5AA(0.5) H5AB(0.5) C51(0.5) H9A(0.5)
 H9B(0.5) H9C(0.5) C47(0.5) H0AB(0.5) H0AC(0.5) H0AD(0.5)
 Fixed Uiso: H00A(0.032) H00C(0.034) H00I(0.044) H00J(0.034) H00L(0.038)
 H00N(0.033) H00Q(0.04) H00R(0.05) H00S(0.046) H00T(0.043) H00U(0.054)
 H00V(0.052) H00W(0.046) H00X(0.044) H00Y(0.044) H00Z(0.048) H010(0.053)
 H011(0.047) H012(0.053) H013(0.055) H014(0.047) H015(0.052) H01A(0.059)
 H01B(0.059) H01C(0.081) H01D(0.081) H01E(0.081) H01F(0.079) H01G(0.079)
 H01H(0.079) H01I(0.077) H01J(0.077) H01K(0.077) H01L(0.062) H01M(0.062)
 H01N(0.084) H01O(0.084) H01P(0.084) H01Q(0.082) H01R(0.082) H01S(0.082)
 H01T(0.097) H01U(0.097) H01V(0.097) H01W(0.107) H01X(0.107) H01Y(0.107)
 H01Z(0.136) H(0.136) HA(0.136) H01(0.083) HB(0.083) HC(0.083) H0AA(0.099)
 HD(0.099) HE(0.099) H3A(0.067) H3B(0.067) H3C(0.067) H4A(0.057) H4B(0.057)
 H4C(0.057) H2AA(0.082) H2AB(0.082) H1AA(0.103) H1AB(0.103) H1AC(0.103)
 H1BD(0.103) H1BE(0.103) H1BF(0.103) H3AA(0.125) H3AB(0.125) H4AA(0.094)
 H4AB(0.094) H5AA(0.127) H5AB(0.127) H9A(0.208) H9B(0.208) H9C(0.208)
 H0AB(0.175) H0AC(0.175) H0AD(0.175)
 Fixed X: H00A(0.396601) H00C(0.539028) H00I(0.383233) H00J(0.704228)
 H00L(0.29317) H00N(0.563348) H00Q(0.310004) H00R(1.025607) H00S(0.369722)
 H00T(0.159626) H00U(1.040788) H00V(0.926232) H00W(0.716325) H00X(0.925511)
 H00Y(0.171661) H00Z(0.553579) H010(0.721419) H012(0.585737) H013(0.86813)
 H014(0.465758) H015(0.970437) H01A(0.801702) H01B(0.887729) H01C(0.875044)
 H01D(0.777574) H01E(0.861318) H01F(0.387121) H01G(0.365021) H01H(0.471643)
 H01I(0.680013) H01J(0.666733) H01K(0.762839) H01L(0.762016) H01M(0.854326)
 H01N(0.221215) H01O(0.21294) H01P(0.235561) H01Q(0.806246) H01R(0.716103)
 H01S(0.824784) H01T(0.510852) H01U(0.557482) H01V(0.454636) H01W(0.716969)
 H01X(0.720599) H01Y(0.67619) H01Z(0.65618) H(0.750019) HA(0.745164)
 H01(0.95189) HB(0.960929) HC(1.036469) H0AA(0.991281) HD(0.894398)
 HE(0.885264) H3A(0.85967) H3B(0.814411) H3C(0.764403) H4A(1.030025)
 H4B(0.983886) H4C(1.030875) H2AA(0.766902) H2AB(0.818927) H1AA(0.879597)
 H1AB(0.966976) H1AC(0.931805) H1BD(0.86049) H1BE(0.976985) H1BF(0.894909)
 H3AA(0.946445) H3AB(0.929973) H4AA(0.901995) H4AB(0.93532) H5AA(0.836488)
 H5AB(0.836496) H9A(0.665877) H9B(0.692178) H9C(0.660927) H0AB(0.595812)
 H0AC(0.685082) H0AD(0.624201)
 Fixed Y: H00A(0.614268) H00C(0.684624) H00I(0.174047) H00J(0.569659)
 H00L(0.58022) H00N(0.499915) H00Q(0.312681) H00R(0.381769) H00S(0.384764)
 H00T(0.497264) H00U(0.372128) H00V(0.435234) H00W(0.776221) H00X(0.618254)
 H00Y(0.363311) H00Z(0.142363) H010(0.55701) H012(0.346875) H013(0.826411)
 H014(0.09042) H015(0.746554) H01A(0.103756) H01B(0.118893) H01C(0.562276)
 H01D(0.617102) H01E(0.626948) H01F(0.267228) H01G(0.358578) H01H(0.331463)
 H01I(0.432018) H01J(0.498561) H01K(0.442277) H01L(0.287763) H01M(0.249591)
 H01N(0.318668) H01O(0.347878) H01P(0.257287) H01Q(0.036148) H01R(0.023758)
 H01S(-0.010891) H01T(0.21542) H01U(0.292848) H01V(0.298145) H01W(0.256616)
 H01X(0.280226) H01Y(0.196658) H01Z(0.26056) H(0.310203) HA(0.217236)
 H01(0.571428) HB(0.517129) HC(0.504827) H0AA(0.368648) HD(0.380628)
 HE(0.334465) H3A(0.345013) H3B(0.40544) H3C(0.39764) H4A(0.509501)
 H4B(0.472199) H4C(0.416126) H2AA(0.073673) H2AB(-0.008362) H1AA(0.250505)
 H1AB(0.212324) H1AC(0.17036) H1BD(0.236761) H1BE(0.222681) H1BF(0.194914)
 H3AA(0.086529) H3AB(0.129106) H4AA(0.057288) H4AB(0.09867) H5AA(0.008986)
 H5AB(-0.02482) H9A(-0.016787) H9B(-0.062028) H9C(0.028891) H0AB(-0.033953)
 H0AC(-0.076438) H0AD(-0.006363)
 Fixed Z: H00A(0.641192) H00C(0.668607) H00I(0.705097) H00J(0.560857)
 H00L(0.537719) H00N(0.534004) H00Q(0.578413) H00R(0.676018) H00S(0.69477)
 H00T(0.514629) H00U(0.765892) H00V(0.818655) H00W(0.608031) H00X(0.711956)
 H00Y(0.534176) H00Z(0.579435) H010(0.774348) H012(0.550114) H013(0.641068)
 H014(0.648453) H015(0.692955) H01A(0.8669) H01B(0.825115) H01C(0.853671)
 H01D(0.85221) H01E(0.808812) H01F(0.774303) H01G(0.784107) H01H(0.762891)
 H01I(0.807895) H01J(0.851347) H01K(0.853124) H01L(0.804448) H01M(0.835914)
 H01N(0.66866) H01O(0.727674) H01P(0.715458) H01Q(0.765674) H01R(0.80516)
 H01S(0.818951) H01T(0.492291) H01U(0.466757) H01V(0.497705) H01W(0.57642)
 H01X(0.516158) H01Y(0.532942) H01Z(0.872646) H(0.894053) HA(0.903759)
 H01(0.603605) HB(0.552979) HC(0.601309) H0AA(0.58623) HD(0.549586)
 HE(0.603618) H3A(0.599084) H3B(0.557089) H3C(0.613062) H4A(0.605025)
 H4B(0.552687) H4C(0.596792) H2AA(0.586331) H2AB(0.602376) H1AA(0.703385)
 H1AB(0.669745) H1AC(0.722155) H1BD(0.675659) H1BE(0.68799) H1BF(0.728831)
 H3AA(0.685649) H3AB(0.630567) H4AA(0.677117) H4AB(0.623859) H5AA(0.608723)
 H5AB(0.667261) H9A(0.670139) H9B(0.617442) H9C(0.615661) H0AB(0.653481)
 H0AC(0.623581) H0AD(0.595998)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Ce1 Ce 0.59753(2) 0.47294(2) 0.66651(2) 0.02482(4) Uani 1 1 d . . . . .
K1 K 0.65406(5) 0.15924(4) 0.71490(3) 0.04320(15) Uani 1 1 d . . . . .
Cl1 Cl 0.48947(5) 0.52310(4) 0.74748(2) 0.03456(13) Uani 1 1 d . . . . .
Cl2 Cl 0.67414(6) 0.33724(4) 0.70327(4) 0.0508(2) Uani 1 1 d . . . . .
N2 N 0.46983(15) 0.39158(12) 0.61684(8) 0.0254(4) Uani 1 1 d . . . . .
N1 N 0.75876(15) 0.54110(12) 0.68167(9) 0.0303(4) Uani 1 1 d . . . . .
O1 O 0.75779(17) 0.16966(14) 0.80683(9) 0.0473(5) Uani 1 1 d . . . . .
C13 C 0.38004(18) 0.49664(15) 0.57246(9) 0.0267(4) Uani 1 1 d . . . . .
C4 C 0.46594(18) 0.54778(14) 0.58626(9) 0.0256(4) Uani 1 1 d . . . . .
C5 C 0.45926(18) 0.60426(14) 0.62549(10) 0.0268(5) Uani 1 1 d . . . . .
H00A H 0.396601 0.614268 0.641192 0.032 Uiso 1 1 calc R . . . .
C31 C 0.46968(18) 0.30831(14) 0.62629(10) 0.0278(5) Uani 1 1 d . . . . .
C6 C 0.54432(18) 0.64629(14) 0.64186(10) 0.0284(5) Uani 1 1 d . . . . .
H00C H 0.539028 0.684624 0.668607 0.034 Uiso 1 1 calc R . . . .
C32 C 0.41739(19) 0.27714(15) 0.66874(11) 0.0316(5) Uani 1 1 d . . . . .
C7 C 0.73033(18) 0.66723(15) 0.64043(11) 0.0305(5) Uani 1 1 d . . . . .
C19 C 0.83529(19) 0.49307(16) 0.70590(12) 0.0338(6) Uani 1 1 d . . . . .
C1 C 0.63702(18) 0.63215(14) 0.61906(10) 0.0281(5) Uani 1 1 d . . . . .
C8 C 0.79084(18) 0.61721(15) 0.67178(11) 0.0313(5) Uani 1 1 d . . . . .
C33 C 0.4178(2) 0.19558(16) 0.67636(12) 0.0364(6) Uani 1 1 d . . . . .
H00I H 0.383233 0.174047 0.705097 0.044 Uiso 1 1 calc R . . . .
C2 C 0.64239(18) 0.57785(15) 0.57781(10) 0.0286(5) Uani 1 1 d . . . . .
H00J H 0.704228 0.569659 0.560857 0.034 Uiso 1 1 calc R . . . .
C24 C 0.90339(19) 0.45301(16) 0.67373(12) 0.0363(6) Uani 1 1 d . . . . .
C18 C 0.29635(19) 0.52584(17) 0.54620(10) 0.0316(5) Uani 1 1 d . . . . .
H00L H 0.293170 0.580220 0.537719 0.038 Uiso 1 1 calc R . . . .
C36 C 0.5216(2) 0.25783(15) 0.59278(11) 0.0327(5) Uani 1 1 d . . . . .
C3 C 0.55859(18) 0.53650(14) 0.56183(9) 0.0272(5) Uani 1 1 d . . . . .
H00N H 0.563348 0.499915 0.534004 0.033 Uiso 1 1 calc R . . . .
C14 C 0.38776(17) 0.41626(15) 0.58724(9) 0.0265(4) Uani 1 1 d . . . . .
C20 C 0.8429(2) 0.48644(17) 0.76058(12) 0.0376(6) Uani 1 1 d . . . . .
C15 C 0.30735(19) 0.36742(17) 0.57096(11) 0.0334(5) Uani 1 1 d . . . . .
H00Q H 0.310004 0.312681 0.578413 0.040 Uiso 1 1 calc R . . . .
C23 C 0.9790(2) 0.40855(17) 0.69727(14) 0.0413(7) Uani 1 1 d . . . . .
H00R H 1.025607 0.381769 0.676018 0.050 Uiso 1 1 calc R . . . .
C37 C 0.3600(2) 0.32884(17) 0.70574(12) 0.0380(6) Uani 1 1 d . . . . .
H00S H 0.369722 0.384764 0.694770 0.046 Uiso 1 1 calc R . . . .
C17 C 0.21726(19) 0.47694(18) 0.53214(11) 0.0361(6) Uani 1 1 d . . . . .
H00T H 0.159626 0.497264 0.514629 0.043 Uiso 1 1 calc R . . . .
C22 C 0.9881(2) 0.40239(18) 0.75068(14) 0.0449(7) Uani 1 1 d . . . . .
H00U H 1.040788 0.372128 0.765892 0.054 Uiso 1 1 calc R . . . .
C21 C 0.9203(2) 0.44040(18) 0.78190(14) 0.0437(7) Uani 1 1 d . . . . .
H00V H 0.926232 0.435234 0.818655 0.052 Uiso 1 1 calc R . . . .
C12 C 0.7586(2) 0.74404(16) 0.62917(13) 0.0386(6) Uani 1 1 d . . . . .
H00W H 0.716325 0.776221 0.608031 0.046 Uiso 1 1 calc R . . . .
C9 C 0.88212(19) 0.64966(17) 0.69090(12) 0.0366(6) Uani 1 1 d . . . . .
H00X H 0.925511 0.618254 0.711956 0.044 Uiso 1 1 calc R . . . .
C16 C 0.2245(2) 0.39776(18) 0.54430(11) 0.0369(6) Uani 1 1 d . . . . .
H00Y H 0.171661 0.363311 0.534176 0.044 Uiso 1 1 calc R . . . .
C35 C 0.5189(2) 0.17678(17) 0.60205(12) 0.0399(6) Uani 1 1 d . . . . .
H00Z H 0.553579 0.142363 0.579435 0.048 Uiso 1 1 calc R . . . .
C25 C 0.7717(2) 0.5283(2) 0.79647(12) 0.0439(7) Uani 1 1 d . . . . .
H010 H 0.721419 0.557010 0.774348 0.053 Uiso 1 1 calc R . . . .
C28 C 0.8951(2) 0.45903(18) 0.61476(13) 0.0390(6) Uani 1 1 d . . . . .
H011 H 0.837(4) 0.492(3) 0.605(2) 0.047 Uiso 0.620(12) 1 d R . P A 1
C40 C 0.5781(3) 0.28860(18) 0.54627(13) 0.0443(7) Uani 1 1 d . . . . .
H012 H 0.585737 0.346875 0.550114 0.053 Uiso 1 1 calc R . . . .
C11 C 0.8485(2) 0.77396(18) 0.64871(14) 0.0459(7) Uani 1 1 d . . . . .
H013 H 0.868130 0.826411 0.641068 0.055 Uiso 1 1 calc R . . . .
C34 C 0.4673(2) 0.14573(16) 0.64306(12) 0.0391(6) Uani 1 1 d . . . . .
H014 H 0.465758 0.090420 0.648453 0.047 Uiso 1 1 calc R . . . .
C10 C 0.9090(2) 0.72627(18) 0.67943(14) 0.0435(7) Uani 1 1 d . . . . .
H015 H 0.970437 0.746554 0.692955 0.052 Uiso 1 1 calc R . . . .
C44 C 0.8155(2) 0.1079(2) 0.82924(14) 0.0493(8) Uani 1 1 d . . . . .
H01A H 0.801702 0.103756 0.866900 0.059 Uiso 1 1 calc R . . . .
H01B H 0.887729 0.118893 0.825115 0.059 Uiso 1 1 calc R . . . .
C27 C 0.8264(3) 0.5892(2) 0.83091(14) 0.0537(8) Uani 1 1 d . . . . .
H01C H 0.875044 0.562276 0.853671 0.081 Uiso 1 1 calc GR . . . .
H01D H 0.777574 0.617102 0.852210 0.081 Uiso 1 1 calc GR . . . .
H01E H 0.861318 0.626948 0.808812 0.081 Uiso 1 1 calc GR . . . .
C38 C 0.3995(3) 0.3208(2) 0.76181(13) 0.0527(8) Uani 1 1 d . . . . .
H01F H 0.387121 0.267228 0.774303 0.079 Uiso 1 1 calc GR . . . .
H01G H 0.365021 0.358578 0.784107 0.079 Uiso 1 1 calc GR . . . .
H01H H 0.471643 0.331463 0.762891 0.079 Uiso 1 1 calc GR . . . .
C26 C 0.7153(3) 0.4701(2) 0.83021(14) 0.0515(8) Uani 1 1 d . . . . .
H01I H 0.680013 0.432018 0.807895 0.077 Uiso 1 1 calc GR . . . .
H01J H 0.666733 0.498561 0.851347 0.077 Uiso 1 1 calc GR . . . .
H01K H 0.762839 0.442277 0.853124 0.077 Uiso 1 1 calc GR . . . .
C45 C 0.7811(3) 0.2459(2) 0.82955(14) 0.0515(8) Uani 1 1 d . . . . .
H01L H 0.762016 0.287763 0.804448 0.062 Uiso 1 1 calc R . . . .
H01M H 0.854326 0.249591 0.835914 0.062 Uiso 1 1 calc R . . . .
C39 C 0.2473(3) 0.3116(2) 0.70425(16) 0.0560(9) Uani 1 1 d . . . . .
H01N H 0.221215 0.318668 0.668660 0.084 Uiso 1 1 calc GR . . . .
H01O H 0.212940 0.347878 0.727674 0.084 Uiso 1 1 calc GR . . . .
H01P H 0.235561 0.257287 0.715458 0.084 Uiso 1 1 calc GR . . . .
C43 C 0.7883(3) 0.0328(2) 0.80246(16) 0.0545(9) Uani 1 1 d . . . . .
H01Q H 0.806246 0.036148 0.765674 0.082 Uiso 1 1 calc GR . . . .
H01R H 0.716103 0.023758 0.805160 0.082 Uiso 1 1 calc GR . . . .
H01S H 0.824784 -0.010891 0.818951 0.082 Uiso 1 1 calc GR . . . .
C42 C 0.5202(3) 0.2723(3) 0.49637(14) 0.0645(11) Uani 1 1 d . . . . .
H01T H 0.510852 0.215420 0.492291 0.097 Uiso 1 1 calc GR . . . .
H01U H 0.557482 0.292848 0.466757 0.097 Uiso 1 1 calc GR . . . .
H01V H 0.454636 0.298145 0.497705 0.097 Uiso 1 1 calc GR . . . .
C41 C 0.6823(3) 0.2523(3) 0.54262(16) 0.0714(12) Uani 1 1 d . . . . .
H01W H 0.716969 0.256616 0.576420 0.107 Uiso 1 1 calc GR . . . .
H01X H 0.720599 0.280226 0.516158 0.107 Uiso 1 1 calc GR . . . .
H01Y H 0.676190 0.196658 0.532942 0.107 Uiso 1 1 calc GR . . . .
C46 C 0.7287(5) 0.2597(3) 0.8792(2) 0.0908(17) Uani 1 1 d . . . . .
H01Z H 0.656180 0.260560 0.872646 0.136 Uiso 1 1 calc GR . . . .
H H 0.750019 0.310203 0.894053 0.136 Uiso 1 1 calc GR . . . .
HA H 0.745164 0.217236 0.903759 0.136 Uiso 1 1 calc GR . . . .
C30 C 0.9676(5) 0.5185(5) 0.5910(2) 0.055(2) Uani 0.620(12) 1 d . . P A 1
H01 H 0.951890 0.571428 0.603605 0.083 Uiso 0.620(12) 1 calc GR . P A 1
HB H 0.960929 0.517129 0.552979 0.083 Uiso 0.620(12) 1 calc GR . P A 1
HC H 1.036469 0.504827 0.601309 0.083 Uiso 0.620(12) 1 calc GR . P A 1
C29 C 0.9188(6) 0.3778(4) 0.5857(3) 0.066(2) Uani 0.580(9) 1 d . . P A 3
H0AA H 0.991281 0.368648 0.586230 0.099 Uiso 0.580(9) 1 calc GR . P A 3
HD H 0.894398 0.380628 0.549586 0.099 Uiso 0.580(9) 1 calc GR . P A 3
HE H 0.885264 0.334465 0.603618 0.099 Uiso 0.580(9) 1 calc GR . P A 3
C29b C 0.8277(6) 0.3965(5) 0.5943(3) 0.045(2) Uani 0.420(9) 1 d . . P A 4
H3A H 0.859670 0.345013 0.599084 0.067 Uiso 0.420(9) 1 calc GR . P A 4
H3B H 0.814411 0.405440 0.557089 0.067 Uiso 0.420(9) 1 calc GR . P A 4
H3C H 0.764403 0.397640 0.613062 0.067 Uiso 0.420(9) 1 calc GR . P A 4
C30b C 0.9931(6) 0.4647(6) 0.5903(3) 0.038(2) Uani 0.380(12) 1 d . . P A 2
H4A H 1.030025 0.509501 0.605025 0.057 Uiso 0.380(12) 1 calc GR . P A 2
H4B H 0.983886 0.472199 0.552687 0.057 Uiso 0.380(12) 1 calc GR . P A 2
H4C H 1.030875 0.416126 0.596792 0.057 Uiso 0.380(12) 1 calc GR . P A 2
C48 C 0.7925(8) 0.0419(6) 0.6160(4) 0.068(2) Uani 0.5 1 d D . P B 1
H2AA H 0.766902 0.073673 0.586331 0.082 Uiso 0.5 1 calc R . P B 1
H2AB H 0.818927 -0.008362 0.602376 0.082 Uiso 0.5 1 calc R . P B 1
O3 O 0.7186(5) 0.0281(4) 0.6502(3) 0.0723(18) Uani 0.5 1 d D . P B 1
O2 O 0.8377(5) 0.1574(4) 0.6630(3) 0.0744(17) Uani 0.5 1 d D . P B 1
C50 C 0.9095(3) 0.2010(3) 0.69177(19) 0.0685(11) Uani 1 1 d D . . . .
H1AA H 0.879597 0.250505 0.703385 0.103 Uiso 0.5 1 calc GR . P B 1
H1AB H 0.966976 0.212324 0.669745 0.103 Uiso 0.5 1 calc GR . P B 1
H1AC H 0.931805 0.170360 0.722155 0.103 Uiso 0.5 1 calc GR . P B 1
H1BD H 0.860490 0.236761 0.675659 0.103 Uiso 0.5 1 calc GR . P B 2
H1BE H 0.976985 0.222681 0.687990 0.103 Uiso 0.5 1 calc GR . P B 2
H1BF H 0.894909 0.194914 0.728831 0.103 Uiso 0.5 1 calc GR . P B 2
O4 O 0.8006(4) 0.0943(3) 0.6635(2) 0.0584(13) Uani 0.5 1 d D . P B 2
C53 C 0.9037(8) 0.1245(8) 0.6663(6) 0.104(5) Uani 0.5 1 d D . P B 2
H3AA H 0.946445 0.086529 0.685649 0.125 Uiso 0.5 1 calc R . P B 2
H3AB H 0.929973 0.129106 0.630567 0.125 Uiso 0.5 1 calc R . P B 2
C49 C 0.8779(8) 0.0885(6) 0.6468(5) 0.079(3) Uani 0.5 1 d D . P B 1
H4AA H 0.901995 0.057288 0.677117 0.094 Uiso 0.5 1 calc R . P B 1
H4AB H 0.935320 0.098670 0.623859 0.094 Uiso 0.5 1 calc R . P B 1
C52 C 0.8018(10) 0.0110(9) 0.6425(6) 0.106(5) Uani 0.5 1 d D U P B 2
H5AA H 0.836488 0.008986 0.608723 0.127 Uiso 0.5 1 calc R . P B 2
H5AB H 0.836496 -0.024820 0.667261 0.127 Uiso 0.5 1 calc R . P B 2
C51 C 0.6965(17) -0.0116(15) 0.6359(11) 0.139(13) Uani 0.5 1 d D U P B 2
H9A H 0.665877 -0.016787 0.670139 0.208 Uiso 0.5 1 calc GR . P B 2
H9B H 0.692178 -0.062028 0.617442 0.208 Uiso 0.5 1 calc GR . P B 2
H9C H 0.660927 0.028891 0.615661 0.208 Uiso 0.5 1 calc GR . P B 2
C47 C 0.651(2) -0.0262(13) 0.6293(9) 0.117(8) Uani 0.5 1 d . . P B 1
H0AB H 0.595812 -0.033953 0.653481 0.175 Uiso 0.5 1 calc GR . P B 1
H0AC H 0.685082 -0.076438 0.623581 0.175 Uiso 0.5 1 calc GR . P B 1
H0AD H 0.624201 -0.006363 0.595998 0.175 Uiso 0.5 1 calc GR . P B 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
Ce1 Cl1 2.6887(7) . ?
Ce1 Cl2 2.6870(7) . ?
Ce1 N2 2.525(2) . ?
Ce1 N1 2.470(2) . ?
Ce1 C4 2.972(2) . ?
Ce1 C5 3.071(2) . ?
Ce1 C6 3.092(2) . ?
Ce1 C1 3.016(2) . ?
Ce1 C2 2.961(2) . ?
Ce1 C3 2.936(2) . ?
K1 Cl1 3.1646(9) 2_646 ?
K1 Cl2 3.0509(10) . ?
K1 O1 2.724(2) . ?
K1 C33 3.348(3) . ?
K1 C35 3.402(3) . ?
K1 C34 3.086(3) . ?
K1 O3 2.918(6) . ?
K1 O2 2.810(7) . ?
K1 O4 2.621(5) . ?
N2 C31 1.435(3) . ?
N2 C14 1.388(3) . ?
N1 C19 1.441(3) . ?
N1 C8 1.387(3) . ?
O1 C44 1.418(4) . ?
O1 C45 1.453(4) . ?
C13 C4 1.477(3) . ?
C13 C18 1.387(3) . ?
C13 C14 1.421(3) . ?
C4 C5 1.395(3) . ?
C4 C3 1.409(3) . ?
C5 H00A 0.9500 . ?
C5 C6 1.400(3) . ?
C31 C32 1.408(4) . ?
C31 C36 1.405(4) . ?
C6 H00C 0.9500 . ?
C6 C1 1.399(3) . ?
C32 C33 1.399(4) . ?
C32 C37 1.511(4) . ?
C7 C1 1.479(3) . ?
C7 C8 1.415(4) . ?
C7 C12 1.390(4) . ?
C19 C24 1.413(4) . ?
C19 C20 1.411(4) . ?
C1 C2 1.407(4) . ?
C8 C9 1.418(4) . ?
C33 H00I 0.9500 . ?
C33 C34 1.380(4) . ?
C2 H00J 0.9500 . ?
C2 C3 1.378(3) . ?
C24 C23 1.392(4) . ?
C24 C28 1.520(4) . ?
C18 H00L 0.9500 . ?
C18 C17 1.387(4) . ?
C36 C35 1.398(4) . ?
C36 C40 1.516(4) . ?
C3 H00N 0.9500 . ?
C14 C15 1.415(3) . ?
C20 C21 1.400(4) . ?
C20 C25 1.512(4) . ?
C15 H00Q 0.9500 . ?
C15 C16 1.390(4) . ?
C23 H00R 0.9500 . ?
C23 C22 1.379(5) . ?
C37 H00S 1.0000 . ?
C37 C38 1.531(4) . ?
C37 C39 1.534(5) . ?
C17 H00T 0.9500 . ?
C17 C16 1.384(4) . ?
C22 H00U 0.9500 . ?
C22 C21 1.380(5) . ?
C21 H00V 0.9500 . ?
C12 H00W 0.9500 . ?
C12 C11 1.390(4) . ?
C9 H00X 0.9500 . ?
C9 C10 1.383(4) . ?
C16 H00Y 0.9500 . ?
C35 H00Z 0.9500 . ?
C35 C34 1.373(4) . ?
C25 H010 1.0000 . ?
C25 C27 1.538(4) . ?
C25 C26 1.522(5) . ?
C28 H011 0.98(6) . ?
C28 C30 1.533(7) . ?
C28 C29 1.602(7) . ?
C28 C29b 1.484(7) . ?
C28 C30b 1.464(8) . ?
C40 H012 1.0000 . ?
C40 C42 1.512(5) . ?
C40 C41 1.526(5) . ?
C11 H013 0.9500 . ?
C11 C10 1.382(5) . ?
C34 H014 0.9500 . ?
C10 H015 0.9500 . ?
C44 H01A 0.9900 . ?
C44 H01B 0.9900 . ?
C44 C43 1.492(5) . ?
C27 H01C 0.9800 . ?
C27 H01D 0.9800 . ?
C27 H01E 0.9800 . ?
C38 H01F 0.9800 . ?
C38 H01G 0.9800 . ?
C38 H01H 0.9800 . ?
C26 H01I 0.9800 . ?
C26 H01J 0.9800 . ?
C26 H01K 0.9800 . ?
C45 H01L 0.9900 . ?
C45 H01M 0.9900 . ?
C45 C46 1.484(6) . ?
C39 H01N 0.9800 . ?
C39 H01O 0.9800 . ?
C39 H01P 0.9800 . ?
C43 H01Q 0.9800 . ?
C43 H01R 0.9800 . ?
C43 H01S 0.9800 . ?
C42 H01T 0.9800 . ?
C42 H01U 0.9800 . ?
C42 H01V 0.9800 . ?
C41 H01W 0.9800 . ?
C41 H01X 0.9800 . ?
C41 H01Y 0.9800 . ?
C46 H01Z 0.9800 . ?
C46 H 0.9800 . ?
C46 HA 0.9800 . ?
C30 H01 0.9800 . ?
C30 HB 0.9800 . ?
C30 HC 0.9800 . ?
C29 H0AA 0.9800 . ?
C29 HD 0.9800 . ?
C29 HE 0.9800 . ?
C29b H3A 0.9800 . ?
C29b H3B 0.9800 . ?
C29b H3C 0.9800 . ?
C30b H4A 0.9800 . ?
C30b H4B 0.9800 . ?
C30b H4C 0.9800 . ?
C48 H2AA 0.9900 . ?
C48 H2AB 0.9900 . ?
C48 O3 1.352(11) . ?
C48 C49 1.590(17) . ?
O3 C47 1.39(3) . ?
O2 C50 1.410(8) . ?
O2 C49 1.356(10) . ?
C50 H1AA 0.9800 . ?
C50 H1AB 0.9800 . ?
C50 H1AC 0.9800 . ?
C50 H1BD 0.9800 . ?
C50 H1BE 0.9800 . ?
C50 H1BF 0.9800 . ?
C50 C53 1.456(11) . ?
O4 C53 1.470(11) . ?
O4 C52 1.516(13) . ?
C53 H3AA 0.9900 . ?
C53 H3AB 0.9900 . ?
C49 H4AA 0.9900 . ?
C49 H4AB 0.9900 . ?
C52 H5AA 0.9900 . ?
C52 H5AB 0.9900 . ?
C52 C51 1.46(2) . ?
C51 H9A 0.9800 . ?
C51 H9B 0.9800 . ?
C51 H9C 0.9800 . ?
C47 H0AB 0.9800 . ?
C47 H0AC 0.9800 . ?
C47 H0AD 0.9800 . ?

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
Cl1 Ce1 C4 94.71(5) . . ?
Cl1 Ce1 C5 73.02(5) . . ?
Cl1 Ce1 C6 74.47(5) . . ?
Cl1 Ce1 C1 97.34(5) . . ?
Cl1 Ce1 C2 121.47(5) . . ?
Cl1 Ce1 C3 120.16(5) . . ?
Cl2 Ce1 Cl1 101.90(3) . . ?
Cl2 Ce1 C4 145.89(5) . . ?
Cl2 Ce1 C5 165.23(5) . . ?
Cl2 Ce1 C6 166.85(5) . . ?
Cl2 Ce1 C1 147.47(5) . . ?
Cl2 Ce1 C2 134.91(5) . . ?
Cl2 Ce1 C3 134.26(5) . . ?
N2 Ce1 Cl1 101.41(5) . . ?
N2 Ce1 Cl2 87.59(5) . . ?
N2 Ce1 C4 59.80(7) . . ?
N2 Ce1 C5 80.04(6) . . ?
N2 Ce1 C6 105.47(6) . . ?
N2 Ce1 C1 114.06(7) . . ?
N2 Ce1 C2 94.82(7) . . ?
N2 Ce1 C3 68.31(7) . . ?
N1 Ce1 Cl1 101.94(6) . . ?
N1 Ce1 Cl2 91.20(5) . . ?
N1 Ce1 N2 156.36(7) . . ?
N1 Ce1 C4 114.38(7) . . ?
N1 Ce1 C5 103.37(7) . . ?
N1 Ce1 C6 77.45(7) . . ?
N1 Ce1 C1 59.05(7) . . ?
N1 Ce1 C2 69.66(7) . . ?
N1 Ce1 C3 96.48(7) . . ?
C4 Ce1 C5 26.63(6) . . ?
C4 Ce1 C6 47.11(7) . . ?
C4 Ce1 C1 56.05(7) . . ?
C5 Ce1 C6 26.26(6) . . ?
C1 Ce1 C5 47.01(7) . . ?
C1 Ce1 C6 26.43(7) . . ?
C2 Ce1 C4 48.22(7) . . ?
C2 Ce1 C5 55.03(7) . . ?
C2 Ce1 C6 47.00(7) . . ?
C2 Ce1 C1 27.22(7) . . ?
C3 Ce1 C4 27.59(6) . . ?
C3 Ce1 C5 47.32(6) . . ?
C3 Ce1 C6 54.94(7) . . ?
C3 Ce1 C1 47.92(7) . . ?
C3 Ce1 C2 27.02(7) . . ?
Cl1 K1 C33 69.68(5) 2_646 . ?
Cl1 K1 C35 90.49(6) 2_646 . ?
Cl2 K1 Cl1 143.98(3) . 2_646 ?
Cl2 K1 C33 82.66(5) . . ?
Cl2 K1 C35 82.88(5) . . ?
Cl2 K1 C34 94.97(5) . . ?
O1 K1 Cl1 94.87(5) . 2_646 ?
O1 K1 Cl2 88.63(6) . . ?
O1 K1 C33 135.05(8) . . ?
O1 K1 C35 171.11(7) . . ?
O1 K1 C34 156.59(8) . . ?
O1 K1 O3 113.13(16) . . ?
O1 K1 O2 88.63(16) . . ?
C33 K1 C35 41.22(8) . . ?
C34 K1 Cl1 68.95(6) . 2_646 ?
C34 K1 C33 24.33(8) . . ?
C34 K1 C35 23.79(8) . . ?
O3 K1 Cl1 78.57(16) . 2_646 ?
O3 K1 Cl2 132.36(16) . . ?
O3 K1 C33 104.94(16) . . ?
O3 K1 C35 74.87(16) . . ?
O3 K1 C34 81.12(16) . . ?
O2 K1 Cl1 132.38(13) . 2_646 ?
O2 K1 Cl2 83.45(13) . . ?
O2 K1 C33 133.42(15) . . ?
O2 K1 C35 92.99(16) . . ?
O2 K1 C34 114.75(16) . . ?
O2 K1 O3 56.9(2) . . ?
O4 K1 Cl1 107.87(12) . 2_646 ?
O4 K1 Cl2 107.48(12) . . ?
O4 K1 O1 95.20(14) . . ?
O4 K1 C33 129.50(14) . . ?
O4 K1 C35 89.88(14) . . ?
O4 K1 C34 105.67(14) . . ?
Ce1 Cl1 K1 143.41(3) . 2_656 ?
Ce1 Cl2 K1 148.34(3) . . ?
C31 N2 Ce1 117.18(14) . . ?
C14 N2 Ce1 129.20(16) . . ?
C14 N2 C31 112.77(19) . . ?
C19 N1 Ce1 114.38(16) . . ?
C8 N1 Ce1 132.78(16) . . ?
C8 N1 C19 112.8(2) . . ?
C44 O1 K1 124.7(2) . . ?
C44 O1 C45 112.6(3) . . ?
C45 O1 K1 120.60(19) . . ?
C18 C13 C4 121.5(2) . . ?
C18 C13 C14 121.9(2) . . ?
C14 C13 C4 116.6(2) . . ?
C13 C4 Ce1 111.27(15) . . ?
C5 C4 Ce1 80.64(13) . . ?
C5 C4 C13 121.3(2) . . ?
C5 C4 C3 118.8(2) . . ?
C3 C4 Ce1 74.76(13) . . ?
C3 C4 C13 119.8(2) . . ?
Ce1 C5 H00A 120.9 . . ?
C4 C5 Ce1 72.73(13) . . ?
C4 C5 H00A 119.8 . . ?
C4 C5 C6 120.4(2) . . ?
C6 C5 Ce1 77.71(13) . . ?
C6 C5 H00A 119.8 . . ?
C32 C31 N2 120.2(2) . . ?
C36 C31 N2 119.7(2) . . ?
C36 C31 C32 120.0(2) . . ?
Ce1 C6 H00C 121.6 . . ?
C5 C6 Ce1 76.02(13) . . ?
C5 C6 H00C 119.8 . . ?
C1 C6 Ce1 73.75(13) . . ?
C1 C6 C5 120.4(2) . . ?
C1 C6 H00C 119.8 . . ?
C31 C32 C37 122.1(2) . . ?
C33 C32 C31 118.7(3) . . ?
C33 C32 C37 119.2(3) . . ?
C8 C7 C1 116.0(2) . . ?
C12 C7 C1 122.1(2) . . ?
C12 C7 C8 121.8(2) . . ?
C24 C19 N1 118.6(3) . . ?
C20 C19 N1 121.0(2) . . ?
C20 C19 C24 120.4(2) . . ?
C6 C1 Ce1 79.81(14) . . ?
C6 C1 C7 121.4(2) . . ?
C6 C1 C2 118.9(2) . . ?
C7 C1 Ce1 111.30(15) . . ?
C2 C1 Ce1 74.21(14) . . ?
C2 C1 C7 119.4(2) . . ?
N1 C8 C7 119.3(2) . . ?
N1 C8 C9 124.4(2) . . ?
C7 C8 C9 116.3(2) . . ?
K1 C33 H00I 99.6 . . ?
C32 C33 K1 103.03(17) . . ?
C32 C33 H00I 119.3 . . ?
C34 C33 K1 67.13(16) . . ?
C34 C33 C32 121.4(3) . . ?
C34 C33 H00I 119.3 . . ?
Ce1 C2 H00J 116.9 . . ?
C1 C2 Ce1 78.57(14) . . ?
C1 C2 H00J 119.8 . . ?
C3 C2 Ce1 75.45(14) . . ?
C3 C2 C1 120.5(2) . . ?
C3 C2 H00J 119.8 . . ?
C19 C24 C28 120.8(2) . . ?
C23 C24 C19 118.5(3) . . ?
C23 C24 C28 120.7(3) . . ?
C13 C18 H00L 119.5 . . ?
C17 C18 C13 121.1(3) . . ?
C17 C18 H00L 119.5 . . ?
C31 C36 C40 121.9(2) . . ?
C35 C36 C31 118.9(3) . . ?
C35 C36 C40 119.2(3) . . ?
Ce1 C3 H00N 115.8 . . ?
C4 C3 Ce1 77.65(14) . . ?
C4 C3 H00N 119.6 . . ?
C2 C3 Ce1 77.52(14) . . ?
C2 C3 C4 120.8(2) . . ?
C2 C3 H00N 119.6 . . ?
N2 C14 C13 119.3(2) . . ?
N2 C14 C15 125.0(2) . . ?
C15 C14 C13 115.7(2) . . ?
C19 C20 C25 122.2(2) . . ?
C21 C20 C19 118.4(3) . . ?
C21 C20 C25 119.4(3) . . ?
C14 C15 H00Q 119.3 . . ?
C16 C15 C14 121.5(3) . . ?
C16 C15 H00Q 119.3 . . ?
C24 C23 H00R 119.2 . . ?
C22 C23 C24 121.7(3) . . ?
C22 C23 H00R 119.2 . . ?
C32 C37 H00S 107.8 . . ?
C32 C37 C38 111.7(2) . . ?
C32 C37 C39 112.4(3) . . ?
C38 C37 H00S 107.8 . . ?
C38 C37 C39 109.2(3) . . ?
C39 C37 H00S 107.8 . . ?
C18 C17 H00T 120.9 . . ?
C16 C17 C18 118.2(2) . . ?
C16 C17 H00T 120.9 . . ?
C23 C22 H00U 120.2 . . ?
C23 C22 C21 119.6(3) . . ?
C21 C22 H00U 120.2 . . ?
C20 C21 H00V 119.3 . . ?
C22 C21 C20 121.4(3) . . ?
C22 C21 H00V 119.3 . . ?
C7 C12 H00W 119.9 . . ?
C11 C12 C7 120.3(3) . . ?
C11 C12 H00W 119.9 . . ?
C8 C9 H00X 119.4 . . ?
C10 C9 C8 121.1(3) . . ?
C10 C9 H00X 119.4 . . ?
C15 C16 H00Y 119.2 . . ?
C17 C16 C15 121.6(3) . . ?
C17 C16 H00Y 119.2 . . ?
K1 C35 H00Z 102.1 . . ?
C36 C35 K1 102.51(18) . . ?
C36 C35 H00Z 119.2 . . ?
C34 C35 K1 65.08(17) . . ?
C34 C35 C36 121.6(3) . . ?
C34 C35 H00Z 119.2 . . ?
C20 C25 H010 107.8 . . ?
C20 C25 C27 111.7(3) . . ?
C20 C25 C26 111.3(3) . . ?
C27 C25 H010 107.8 . . ?
C26 C25 H010 107.8 . . ?
C26 C25 C27 110.1(3) . . ?
C24 C28 H011 109(3) . . ?
C24 C28 C30 113.8(3) . . ?
C24 C28 C29 113.2(4) . . ?
C30 C28 H011 92(3) . . ?
C29b C28 C24 109.9(4) . . ?
C30b C28 C24 112.4(4) . . ?
C36 C40 H012 108.3 . . ?
C36 C40 C41 112.0(3) . . ?
C42 C40 C36 110.5(3) . . ?
C42 C40 H012 108.3 . . ?
C42 C40 C41 109.2(3) . . ?
C41 C40 H012 108.3 . . ?
C12 C11 H013 120.5 . . ?
C10 C11 C12 119.0(3) . . ?
C10 C11 H013 120.5 . . ?
K1 C34 H014 90.3 . . ?
C33 C34 K1 88.53(17) . . ?
C33 C34 H014 120.3 . . ?
C35 C34 K1 91.13(18) . . ?
C35 C34 C33 119.4(3) . . ?
C35 C34 H014 120.3 . . ?
C9 C10 H015 119.3 . . ?
C11 C10 C9 121.4(3) . . ?
C11 C10 H015 119.3 . . ?
O1 C44 H01A 110.0 . . ?
O1 C44 H01B 110.0 . . ?
O1 C44 C43 108.6(3) . . ?
H01A C44 H01B 108.3 . . ?
C43 C44 H01A 110.0 . . ?
C43 C44 H01B 110.0 . . ?
C25 C27 H01C 109.5 . . ?
C25 C27 H01D 109.5 . . ?
C25 C27 H01E 109.5 . . ?
H01C C27 H01D 109.5 . . ?
H01C C27 H01E 109.5 . . ?
H01D C27 H01E 109.5 . . ?
C37 C38 H01F 109.5 . . ?
C37 C38 H01G 109.5 . . ?
C37 C38 H01H 109.5 . . ?
H01F C38 H01G 109.5 . . ?
H01F C38 H01H 109.5 . . ?
H01G C38 H01H 109.5 . . ?
C25 C26 H01I 109.5 . . ?
C25 C26 H01J 109.5 . . ?
C25 C26 H01K 109.5 . . ?
H01I C26 H01J 109.5 . . ?
H01I C26 H01K 109.5 . . ?
H01J C26 H01K 109.5 . . ?
O1 C45 H01L 109.1 . . ?
O1 C45 H01M 109.1 . . ?
O1 C45 C46 112.6(3) . . ?
H01L C45 H01M 107.8 . . ?
C46 C45 H01L 109.1 . . ?
C46 C45 H01M 109.1 . . ?
C37 C39 H01N 109.5 . . ?
C37 C39 H01O 109.5 . . ?
C37 C39 H01P 109.5 . . ?
H01N C39 H01O 109.5 . . ?
H01N C39 H01P 109.5 . . ?
H01O C39 H01P 109.5 . . ?
C44 C43 H01Q 109.5 . . ?
C44 C43 H01R 109.5 . . ?
C44 C43 H01S 109.5 . . ?
H01Q C43 H01R 109.5 . . ?
H01Q C43 H01S 109.5 . . ?
H01R C43 H01S 109.5 . . ?
C40 C42 H01T 109.5 . . ?
C40 C42 H01U 109.5 . . ?
C40 C42 H01V 109.5 . . ?
H01T C42 H01U 109.5 . . ?
H01T C42 H01V 109.5 . . ?
H01U C42 H01V 109.5 . . ?
C40 C41 H01W 109.5 . . ?
C40 C41 H01X 109.5 . . ?
C40 C41 H01Y 109.5 . . ?
H01W C41 H01X 109.5 . . ?
H01W C41 H01Y 109.5 . . ?
H01X C41 H01Y 109.5 . . ?
C45 C46 H01Z 109.5 . . ?
C45 C46 H 109.5 . . ?
C45 C46 HA 109.5 . . ?
H01Z C46 H 109.5 . . ?
H01Z C46 HA 109.5 . . ?
H C46 HA 109.5 . . ?
C28 C30 H01 109.5 . . ?
C28 C30 HB 109.5 . . ?
C28 C30 HC 109.5 . . ?
H01 C30 HB 109.5 . . ?
H01 C30 HC 109.5 . . ?
HB C30 HC 109.5 . . ?
C28 C29 H0AA 109.5 . . ?
C28 C29 HD 109.5 . . ?
C28 C29 HE 109.5 . . ?
H0AA C29 HD 109.5 . . ?
H0AA C29 HE 109.5 . . ?
HD C29 HE 109.5 . . ?
C28 C29b H3A 109.5 . . ?
C28 C29b H3B 109.5 . . ?
C28 C29b H3C 109.5 . . ?
H3A C29b H3B 109.5 . . ?
H3A C29b H3C 109.5 . . ?
H3B C29b H3C 109.5 . . ?
C28 C30b H4A 109.5 . . ?
C28 C30b H4B 109.5 . . ?
C28 C30b H4C 109.5 . . ?
H4A C30b H4B 109.5 . . ?
H4A C30b H4C 109.5 . . ?
H4B C30b H4C 109.5 . . ?
H2AA C48 H2AB 108.6 . . ?
O3 C48 H2AA 110.4 . . ?
O3 C48 H2AB 110.4 . . ?
O3 C48 C49 106.8(8) . . ?
C49 C48 H2AA 110.4 . . ?
C49 C48 H2AB 110.4 . . ?
C48 O3 K1 117.5(6) . . ?
C48 O3 C47 109.9(13) . . ?
C47 O3 K1 122.0(12) . . ?
C50 O2 K1 109.7(4) . . ?
C49 O2 K1 120.5(6) . . ?
C49 O2 C50 110.1(8) . . ?
O2 C50 H1AA 109.5 . . ?
O2 C50 H1AB 109.5 . . ?
O2 C50 H1AC 109.5 . . ?
H1AA C50 H1AB 109.5 . . ?
H1AA C50 H1AC 109.5 . . ?
H1AB C50 H1AC 109.5 . . ?
H1BD C50 H1BE 109.5 . . ?
H1BD C50 H1BF 109.5 . . ?
H1BE C50 H1BF 109.5 . . ?
C53 C50 H1BD 109.5 . . ?
C53 C50 H1BE 109.5 . . ?
C53 C50 H1BF 109.5 . . ?
C53 O4 K1 122.4(5) . . ?
C53 O4 C52 109.1(8) . . ?
C52 O4 K1 125.8(7) . . ?
C50 C53 O4 112.1(8) . . ?
C50 C53 H3AA 109.2 . . ?
C50 C53 H3AB 109.2 . . ?
O4 C53 H3AA 109.2 . . ?
O4 C53 H3AB 109.2 . . ?
H3AA C53 H3AB 107.9 . . ?
C48 C49 H4AA 110.2 . . ?
C48 C49 H4AB 110.3 . . ?
O2 C49 C48 107.3(8) . . ?
O2 C49 H4AA 110.3 . . ?
O2 C49 H4AB 110.3 . . ?
H4AA C49 H4AB 108.5 . . ?
O4 C52 H5AA 110.6 . . ?
O4 C52 H5AB 110.6 . . ?
H5AA C52 H5AB 108.7 . . ?
C51 C52 O4 105.7(13) . . ?
C51 C52 H5AA 110.6 . . ?
C51 C52 H5AB 110.6 . . ?
C52 C51 H9A 109.5 . . ?
C52 C51 H9B 109.5 . . ?
C52 C51 H9C 109.5 . . ?
H9A C51 H9B 109.5 . . ?
H9A C51 H9C 109.5 . . ?
H9B C51 H9C 109.5 . . ?
O3 C47 H0AB 109.5 . . ?
O3 C47 H0AC 109.5 . . ?
O3 C47 H0AD 109.5 . . ?
H0AB C47 H0AC 109.5 . . ?
H0AB C47 H0AD 109.5 . . ?
H0AC C47 H0AD 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
Ce1 N2 C31 C32 84.3(2) . . . . ?
Ce1 N2 C31 C36 -96.0(2) . . . . ?
Ce1 N2 C14 C13 14.1(3) . . . . ?
Ce1 N2 C14 C15 -164.25(19) . . . . ?
Ce1 N1 C19 C24 93.7(3) . . . . ?
Ce1 N1 C19 C20 -86.8(3) . . . . ?
Ce1 N1 C8 C7 -11.0(4) . . . . ?
Ce1 N1 C8 C9 169.3(2) . . . . ?
Ce1 C4 C5 C6 63.8(2) . . . . ?
Ce1 C4 C3 C2 -67.2(2) . . . . ?
Ce1 C5 C6 C1 61.3(2) . . . . ?
Ce1 C6 C1 C7 -108.8(2) . . . . ?
Ce1 C6 C1 C2 65.5(2) . . . . ?
Ce1 C1 C2 C3 65.4(2) . . . . ?
Ce1 C2 C3 C4 67.2(2) . . . . ?
K1 O1 C44 C43 -14.8(4) . . . . ?
K1 O1 C45 C46 113.7(4) . . . . ?
K1 C33 C34 C35 -90.5(3) . . . . ?
K1 C35 C34 C33 89.0(3) . . . . ?
K1 O2 C49 C48 49.4(10) . . . . ?
K1 O4 C53 C50 -11.0(16) . . . . ?
K1 O4 C52 C51 24.1(19) . . . . ?
N2 C31 C32 C33 179.2(2) . . . . ?
N2 C31 C32 C37 -0.1(4) . . . . ?
N2 C31 C36 C35 -178.8(2) . . . . ?
N2 C31 C36 C40 -0.2(4) . . . . ?
N2 C14 C15 C16 175.6(2) . . . . ?
N1 C19 C24 C23 178.1(2) . . . . ?
N1 C19 C24 C28 -1.2(4) . . . . ?
N1 C19 C20 C21 -178.5(3) . . . . ?
N1 C19 C20 C25 0.5(4) . . . . ?
N1 C8 C9 C10 -179.9(3) . . . . ?
C13 C4 C5 Ce1 109.3(2) . . . . ?
C13 C4 C5 C6 173.1(2) . . . . ?
C13 C4 C3 Ce1 -106.1(2) . . . . ?
C13 C4 C3 C2 -173.2(2) . . . . ?
C13 C18 C17 C16 -1.0(4) . . . . ?
C13 C14 C15 C16 -2.8(4) . . . . ?
C4 C13 C18 C17 178.2(2) . . . . ?
C4 C13 C14 N2 5.1(3) . . . . ?
C4 C13 C14 C15 -176.4(2) . . . . ?
C4 C5 C6 Ce1 -61.3(2) . . . . ?
C4 C5 C6 C1 0.0(4) . . . . ?
C5 C4 C3 Ce1 70.0(2) . . . . ?
C5 C4 C3 C2 2.8(3) . . . . ?
C5 C6 C1 Ce1 -62.5(2) . . . . ?
C5 C6 C1 C7 -171.3(2) . . . . ?
C5 C6 C1 C2 3.0(4) . . . . ?
C31 N2 C14 C13 -176.9(2) . . . . ?
C31 N2 C14 C15 4.7(3) . . . . ?
C31 C32 C33 K1 70.4(2) . . . . ?
C31 C32 C33 C34 -0.6(4) . . . . ?
C31 C32 C37 C38 -120.4(3) . . . . ?
C31 C32 C37 C39 116.5(3) . . . . ?
C31 C36 C35 K1 -68.5(3) . . . . ?
C31 C36 C35 C34 -0.3(4) . . . . ?
C31 C36 C40 C42 -104.2(3) . . . . ?
C31 C36 C40 C41 133.8(3) . . . . ?
C6 C1 C2 Ce1 -68.5(2) . . . . ?
C6 C1 C2 C3 -3.1(4) . . . . ?
C32 C31 C36 C35 0.9(4) . . . . ?
C32 C31 C36 C40 179.4(3) . . . . ?
C32 C33 C34 K1 91.7(3) . . . . ?
C32 C33 C34 C35 1.2(4) . . . . ?
C7 C1 C2 Ce1 105.9(2) . . . . ?
C7 C1 C2 C3 171.3(2) . . . . ?
C7 C8 C9 C10 0.4(4) . . . . ?
C7 C12 C11 C10 -0.1(5) . . . . ?
C19 N1 C8 C7 169.5(2) . . . . ?
C19 N1 C8 C9 -10.2(4) . . . . ?
C19 C24 C23 C22 0.6(4) . . . . ?
C19 C24 C28 C30 99.2(4) . . . . ?
C19 C24 C28 C29 -141.6(4) . . . . ?
C19 C24 C28 C29b -89.0(5) . . . . ?
C19 C24 C28 C30b 140.5(5) . . . . ?
C19 C20 C21 C22 0.2(5) . . . . ?
C19 C20 C25 C27 -116.3(3) . . . . ?
C19 C20 C25 C26 120.2(3) . . . . ?
C1 C7 C8 N1 -1.8(4) . . . . ?
C1 C7 C8 C9 177.9(2) . . . . ?
C1 C7 C12 C11 -177.9(3) . . . . ?
C1 C2 C3 Ce1 -67.0(2) . . . . ?
C1 C2 C3 C4 0.2(4) . . . . ?
C8 N1 C19 C24 -86.6(3) . . . . ?
C8 N1 C19 C20 92.9(3) . . . . ?
C8 C7 C1 Ce1 9.4(3) . . . . ?
C8 C7 C1 C6 100.3(3) . . . . ?
C8 C7 C1 C2 -74.0(3) . . . . ?
C8 C7 C12 C11 0.1(4) . . . . ?
C8 C9 C10 C11 -0.4(5) . . . . ?
C33 C32 C37 C38 60.4(4) . . . . ?
C33 C32 C37 C39 -62.8(3) . . . . ?
C24 C19 C20 C21 1.0(4) . . . . ?
C24 C19 C20 C25 180.0(3) . . . . ?
C24 C23 C22 C21 0.6(5) . . . . ?
C18 C13 C4 Ce1 163.74(19) . . . . ?
C18 C13 C4 C5 71.9(3) . . . . ?
C18 C13 C4 C3 -112.1(3) . . . . ?
C18 C13 C14 N2 -175.2(2) . . . . ?
C18 C13 C14 C15 3.3(4) . . . . ?
C18 C17 C16 C15 1.5(4) . . . . ?
C36 C31 C32 C33 -0.5(4) . . . . ?
C36 C31 C32 C37 -179.7(2) . . . . ?
C36 C35 C34 K1 -89.7(3) . . . . ?
C36 C35 C34 C33 -0.8(4) . . . . ?
C3 C4 C5 Ce1 -66.75(19) . . . . ?
C3 C4 C5 C6 -2.9(3) . . . . ?
C14 N2 C31 C32 -86.1(3) . . . . ?
C14 N2 C31 C36 93.5(3) . . . . ?
C14 C13 C4 Ce1 -16.5(3) . . . . ?
C14 C13 C4 C5 -108.4(3) . . . . ?
C14 C13 C4 C3 67.6(3) . . . . ?
C14 C13 C18 C17 -1.5(4) . . . . ?
C14 C15 C16 C17 0.5(4) . . . . ?
C20 C19 C24 C23 -1.4(4) . . . . ?
C20 C19 C24 C28 179.3(3) . . . . ?
C23 C24 C28 C30 -80.1(5) . . . . ?
C23 C24 C28 C29 39.1(5) . . . . ?
C23 C24 C28 C29b 91.7(5) . . . . ?
C23 C24 C28 C30b -38.8(6) . . . . ?
C23 C22 C21 C20 -1.1(5) . . . . ?
C37 C32 C33 K1 -110.3(2) . . . . ?
C37 C32 C33 C34 178.7(3) . . . . ?
C21 C20 C25 C27 62.7(4) . . . . ?
C21 C20 C25 C26 -60.8(4) . . . . ?
C12 C7 C1 Ce1 -172.5(2) . . . . ?
C12 C7 C1 C6 -81.6(3) . . . . ?
C12 C7 C1 C2 104.2(3) . . . . ?
C12 C7 C8 N1 -180.0(3) . . . . ?
C12 C7 C8 C9 -0.2(4) . . . . ?
C12 C11 C10 C9 0.2(5) . . . . ?
C35 C36 C40 C42 74.3(4) . . . . ?
C35 C36 C40 C41 -47.7(4) . . . . ?
C25 C20 C21 C22 -178.8(3) . . . . ?
C28 C24 C23 C22 179.9(3) . . . . ?
C40 C36 C35 K1 112.9(2) . . . . ?
C40 C36 C35 C34 -178.8(3) . . . . ?
C44 O1 C45 C46 -81.9(4) . . . . ?
C45 O1 C44 C43 -178.4(3) . . . . ?
O3 C48 C49 O2 -61.8(11) . . . . ?
C50 O2 C49 C48 178.8(6) . . . . ?
C53 O4 C52 C51 -174.3(16) . . . . ?
C49 C48 O3 K1 46.8(9) . . . . ?
C49 C48 O3 C47 -167.7(10) . . . . ?
C52 O4 C53 C50 -173.4(11) . . . . ?

_smtbx_masks_special_details     ?
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 -0.831 0.000 0.500 683.6 110.1 DME
2 -0.163 0.500 0.000 683.6 110.1 DME

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
