# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk-1
_database_code_depnum_ccdc_archive 'CCDC 2254126'
loop_
_audit_author_name
_audit_author_address
'Congqing Zhu'
;Nanjing University
China
;
_audit_update_record             
;
2023-07-25 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        123
_chemical_formula_moiety         'C20 H48 I2 N4 P2 U'
_chemical_formula_sum            'C20 H48 I2 N4 P2 U'
_chemical_formula_weight         898.39
_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 0.0137 0.0067 '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 0.0030 5.4350 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -3.9641 10.8496 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.9014(7)
_cell_length_b                   14.8611(12)
_cell_length_c                   11.4945(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.941(4)
_cell_angle_gamma                90
_cell_volume                     1509.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6786
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      53.86
_cell_measurement_theta_min      5.07
_shelx_estimated_absorpt_T_max   0.185
_shelx_estimated_absorpt_T_min   0.153
_exptl_absorpt_coefficient_mu    23.141
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0546 after correction.
The Ratio of minimum to maximum transmission is 0.7823.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9293
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.885
_diffrn_reflns_theta_min         5.066
_diffrn_ambient_temperature      193.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2555
_reflns_number_total             2740
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.093
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2740
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0269
_refine_ls_restrained_S_all      1.192
_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)+(0.0444P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0756
_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:
 C2(H2), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
C1 C 0.8935(6) 0.4123(4) 0.8324(5) 0.0478(13) Uani 1 1 d . . . . .
H1A H 0.847619 0.422883 0.904501 0.072 Uiso 1 1 calc R U . . .
H1B H 0.999345 0.394197 0.852335 0.072 Uiso 1 1 calc R U . . .
H1C H 0.838077 0.364410 0.786926 0.072 Uiso 1 1 calc R U . . .
U1 U 0.500000 0.500000 0.500000 0.02240(10) Uani 1 2 d S . P . .
P1 P 0.68543(12) 0.53775(8) 0.72719(9) 0.0282(2) Uani 1 1 d . . . . .
N1 N 0.6150(4) 0.6325(3) 0.3709(3) 0.0315(8) Uani 1 1 d . . . . .
I1 I 0.75574(3) 0.36112(2) 0.47538(3) 0.03701(12) Uani 1 1 d . . . . .
N2 N 0.6699(4) 0.5908(3) 0.5997(3) 0.0280(8) Uani 1 1 d . . . . .
C2 C 0.8864(6) 0.4989(3) 0.7595(5) 0.0329(12) Uani 1 1 d . . . . .
H2 H 0.918494 0.481505 0.682208 0.040 Uiso 1 1 calc R U . . .
C3 C 0.9979(6) 0.5696(4) 0.8095(5) 0.0418(12) Uani 1 1 d . . . . .
H3A H 0.991143 0.622125 0.757485 0.063 Uiso 1 1 calc R U . . .
H3B H 1.100679 0.544956 0.816103 0.063 Uiso 1 1 calc R U . . .
H3C H 0.974228 0.587730 0.887193 0.063 Uiso 1 1 calc R U . . .
C4 C 0.6772(7) 0.5797(5) 0.9642(5) 0.0549(15) Uani 1 1 d . . . . .
H4A H 0.606849 0.528949 0.964475 0.082 Uiso 1 1 calc R U . . .
H4B H 0.653872 0.624535 1.021834 0.082 Uiso 1 1 calc R U . . .
H4C H 0.781133 0.558105 0.984381 0.082 Uiso 1 1 calc R U . . .
C5 C 0.6611(6) 0.6225(3) 0.8417(4) 0.0357(11) Uani 1 1 d . . . . .
H5 H 0.742097 0.669047 0.840424 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5082(6) 0.6691(4) 0.8170(6) 0.0557(16) Uani 1 1 d . . . . .
H6A H 0.500260 0.698059 0.739905 0.084 Uiso 1 1 calc R U . . .
H6B H 0.498637 0.714613 0.877318 0.084 Uiso 1 1 calc R U . . .
H6C H 0.427176 0.624493 0.817807 0.084 Uiso 1 1 calc R U . . .
C7 C 0.7515(5) 0.6683(3) 0.5641(4) 0.0317(10) Uani 1 1 d . . . . .
H7A H 0.854223 0.650338 0.548190 0.038 Uiso 1 1 calc R U . . .
H7B H 0.761474 0.714141 0.626964 0.038 Uiso 1 1 calc R U . . .
C8 C 0.6632(6) 0.7061(3) 0.4543(4) 0.0345(10) Uani 1 1 d . . . . .
H8A H 0.573101 0.738669 0.474963 0.041 Uiso 1 1 calc R U . . .
H8B H 0.727090 0.749411 0.416921 0.041 Uiso 1 1 calc R U . . .
C9 C 0.5148(6) 0.6726(4) 0.2714(4) 0.0427(12) Uani 1 1 d . . . . .
H9A H 0.567576 0.722422 0.237980 0.064 Uiso 1 1 calc R U . . .
H9B H 0.422203 0.695083 0.299514 0.064 Uiso 1 1 calc R U . . .
H9C H 0.488704 0.626656 0.211166 0.064 Uiso 1 1 calc R U . . .
C10 C 0.7478(6) 0.5945(4) 0.3226(5) 0.0475(13) Uani 1 1 d . . . . .
H10A H 0.797375 0.641838 0.281689 0.071 Uiso 1 1 calc R U . . .
H10B H 0.714946 0.546084 0.267475 0.071 Uiso 1 1 calc R U . . .
H10C H 0.819233 0.570456 0.386615 0.071 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
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.532(7) . ?
U1 P1 2.9694(11) 3_666 ?
U1 P1 2.9694(11) . ?
U1 N1 2.737(4) 3_666 ?
U1 N1 2.737(4) . ?
U1 I1 3.1108(3) 3_666 ?
U1 I1 3.1109(3) . ?
U1 N2 2.237(4) 3_666 ?
U1 N2 2.237(4) . ?
P1 N2 1.656(4) . ?
P1 C2 1.874(6) . ?
P1 C5 1.854(5) . ?
N1 C8 1.484(6) . ?
N1 C9 1.487(6) . ?
N1 C10 1.478(6) . ?
N2 C7 1.446(6) . ?
C2 H2 1.0000 . ?
C2 C3 1.511(7) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 C5 1.536(7) . ?
C5 H5 1.0000 . ?
C5 C6 1.523(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.512(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
P1 U1 P1 180.0 3_666 . ?
P1 U1 I1 82.54(2) 3_666 3_666 ?
P1 U1 I1 97.46(2) . 3_666 ?
P1 U1 I1 82.54(2) . . ?
P1 U1 I1 97.46(2) 3_666 . ?
N1 U1 P1 82.16(9) 3_666 . ?
N1 U1 P1 97.84(9) . . ?
N1 U1 P1 97.84(9) 3_666 3_666 ?
N1 U1 P1 82.16(9) . 3_666 ?
N1 U1 N1 180.0 . 3_666 ?
N1 U1 I1 84.13(8) . 3_666 ?
N1 U1 I1 84.13(8) 3_666 . ?
N1 U1 I1 95.87(8) . . ?
N1 U1 I1 95.87(8) 3_666 3_666 ?
I1 U1 I1 180.0 3_666 . ?
N2 U1 P1 33.49(10) 3_666 3_666 ?
N2 U1 P1 33.49(10) . . ?
N2 U1 P1 146.51(10) 3_666 . ?
N2 U1 P1 146.51(10) . 3_666 ?
N2 U1 N1 115.49(13) . 3_666 ?
N2 U1 N1 64.51(13) . . ?
N2 U1 N1 115.49(13) 3_666 . ?
N2 U1 N1 64.51(13) 3_666 3_666 ?
N2 U1 I1 89.44(10) 3_666 3_666 ?
N2 U1 I1 89.44(10) . . ?
N2 U1 I1 90.56(10) 3_666 . ?
N2 U1 I1 90.56(10) . 3_666 ?
N2 U1 N2 180.0 . 3_666 ?
N2 P1 U1 48.19(13) . . ?
N2 P1 C2 107.4(2) . . ?
N2 P1 C5 107.5(2) . . ?
C2 P1 U1 122.15(17) . . ?
C5 P1 U1 130.76(16) . . ?
C5 P1 C2 105.0(2) . . ?
C8 N1 U1 106.2(3) . . ?
C8 N1 C9 107.5(4) . . ?
C9 N1 U1 118.5(3) . . ?
C10 N1 U1 107.3(3) . . ?
C10 N1 C8 110.0(4) . . ?
C10 N1 C9 107.3(4) . . ?
P1 N2 U1 98.32(17) . . ?
C7 N2 U1 131.8(3) . . ?
C7 N2 P1 129.7(3) . . ?
C1 C2 P1 110.1(4) . . ?
C1 C2 H2 105.8 . . ?
P1 C2 H2 105.8 . . ?
C3 C2 C1 113.3(5) . . ?
C3 C2 P1 115.4(3) . . ?
C3 C2 H2 105.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
P1 C5 H5 108.2 . . ?
C4 C5 P1 111.3(4) . . ?
C4 C5 H5 108.2 . . ?
C6 C5 P1 110.8(4) . . ?
C6 C5 C4 110.0(5) . . ?
C6 C5 H5 108.2 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 110.2 . . ?
N2 C7 H7B 110.2 . . ?
N2 C7 C8 107.7(4) . . ?
H7A C7 H7B 108.5 . . ?
C8 C7 H7A 110.2 . . ?
C8 C7 H7B 110.2 . . ?
N1 C8 C7 110.2(4) . . ?
N1 C8 H8A 109.6 . . ?
N1 C8 H8B 109.6 . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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
U1 P1 N2 C7 -175.9(5) . . . . ?
U1 P1 C2 C1 -98.8(4) . . . . ?
U1 P1 C2 C3 131.5(4) . . . . ?
U1 P1 C5 C4 131.9(3) . . . . ?
U1 P1 C5 C6 9.2(5) . . . . ?
U1 N1 C8 C7 46.1(4) . . . . ?
U1 N2 C7 C8 22.3(6) . . . . ?
P1 N2 C7 C8 -163.1(3) . . . . ?
N2 P1 C2 C1 -149.8(4) . . . . ?
N2 P1 C2 C3 80.5(4) . . . . ?
N2 P1 C5 C4 -178.8(4) . . . . ?
N2 P1 C5 C6 58.6(4) . . . . ?
N2 C7 C8 N1 -45.6(5) . . . . ?
C2 P1 N2 U1 117.93(18) . . . . ?
C2 P1 N2 C7 -58.0(5) . . . . ?
C2 P1 C5 C4 -64.7(4) . . . . ?
C2 P1 C5 C6 172.7(4) . . . . ?
C5 P1 N2 U1 -129.54(19) . . . . ?
C5 P1 N2 C7 54.5(5) . . . . ?
C5 P1 C2 C1 96.0(4) . . . . ?
C5 P1 C2 C3 -33.7(5) . . . . ?
C9 N1 C8 C7 173.8(4) . . . . ?
C10 N1 C8 C7 -69.7(5) . . . . ?


_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_lk-1_a
_database_code_depnum_ccdc_archive 'CCDC 2254127'
loop_
_audit_author_name
_audit_author_address
'Congqing Zhu'
;Nanjing University
China
;
_audit_update_record             
;
2023-07-25 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        2
_chemical_formula_moiety         'C29 H59 N5 P2 U'
_chemical_formula_sum            'C29 H59 N5 P2 U'
_chemical_formula_weight         777.78
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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      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                   10.0133(5)
_cell_length_b                   12.6600(6)
_cell_length_c                   14.4679(7)
_cell_angle_alpha                79.663(2)
_cell_angle_beta                 71.870(2)
_cell_angle_gamma                86.689(2)
_cell_volume                     1714.72(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6786
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      53.86
_cell_measurement_theta_min      5.07
_shelx_estimated_absorpt_T_max   0.511
_shelx_estimated_absorpt_T_min   0.476
_exptl_absorpt_coefficient_mu    4.851
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5872
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0546 after correction.
The Ratio of minimum to maximum transmission is 0.7823.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16048
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         2.140
_diffrn_ambient_temperature      193.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_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                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7267
_reflns_number_total             7817
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.094
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7817
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.033
_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)+(0.0502P)²+0.0770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0963
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C23(H23), C16(H16), C13(H13), C26(H26)
1.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C21(H21A,H21B), C1(H1A,H1B), C11(H11A,H11B), C12(H12A,H12B),
 C22(H22A,H22B)
1.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8)
1.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C), C19(H19A,H19B,
 H19C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C28(H28A,
 H28B,H28C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C),
 C14(H14A,H14B,H14C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.70778(2) 0.67801(2) 0.73439(2) 0.01851(6) Uani 1 1 d . . . . .
P1 P 0.74706(12) 0.86918(9) 0.84287(8) 0.0265(2) Uani 1 1 d . . . . .
P2 P 0.67745(12) 0.75696(8) 0.52419(7) 0.0221(2) Uani 1 1 d . . . . .
N2 N 0.8406(4) 0.8156(3) 0.7433(3) 0.0266(8) Uani 1 1 d . . . . .
N1 N 0.9865(4) 0.6731(3) 0.6297(3) 0.0277(8) Uani 1 1 d . . . . .
N3 N 0.4257(4) 0.7216(3) 0.8330(3) 0.0265(8) Uani 1 1 d . . . . .
N4 N 0.5803(4) 0.7694(3) 0.6391(2) 0.0246(7) Uani 1 1 d . . . . .
C23 C 0.6819(5) 0.8911(3) 0.4457(3) 0.0276(9) Uani 1 1 d . . . . .
H23 H 0.5868 0.9101 0.4429 0.033 Uiso 1 1 calc R U . . .
C2 C 0.7051(5) 0.5156(3) 0.6636(3) 0.0272(9) Uani 1 1 d . . . . .
H2A H 0.6371 0.5155 0.6283 0.033 Uiso 1 1 calc R U . . .
H2B H 0.7965 0.4889 0.6291 0.033 Uiso 1 1 calc R U . . .
C21 C 0.3949(5) 0.8217(4) 0.7751(3) 0.0326(10) Uani 1 1 d . . . . .
H21A H 0.4443 0.8804 0.7850 0.039 Uiso 1 1 calc R U . . .
H21B H 0.2950 0.8365 0.7979 0.039 Uiso 1 1 calc R U . . .
C1 C 0.6802(5) 0.5872(3) 0.9117(3) 0.0264(9) Uani 1 1 d . . . . .
H1A H 0.7105 0.6324 0.9489 0.032 Uiso 1 1 calc R U . . .
H1B H 0.5854 0.5616 0.9470 0.032 Uiso 1 1 calc R U . . .
C4 C 0.7680(5) 0.4449(3) 0.8112(3) 0.0249(8) Uani 1 1 d . . . . .
C3 C 0.7776(5) 0.5015(3) 0.8849(3) 0.0259(9) Uani 1 1 d . . . . .
C20 C 0.3407(5) 0.6325(4) 0.8280(4) 0.0359(11) Uani 1 1 d . . . . .
H20A H 0.3681 0.6184 0.7616 0.054 Uiso 1 1 calc R U . . .
H20B H 0.2430 0.6519 0.8477 0.054 Uiso 1 1 calc R U . . .
H20C H 0.3556 0.5693 0.8714 0.054 Uiso 1 1 calc R U . . .
C10 C 1.0256(6) 0.6212(5) 0.5428(4) 0.0405(13) Uani 1 1 d . . . . .
H10A H 1.0056 0.5458 0.5627 0.061 Uiso 1 1 calc R U . . .
H10B H 1.1242 0.6313 0.5090 0.061 Uiso 1 1 calc R U . . .
H10C H 0.9729 0.6524 0.4994 0.061 Uiso 1 1 calc R U . . .
C11 C 1.0242(5) 0.7883(4) 0.5984(3) 0.0332(10) Uani 1 1 d . . . . .
H11A H 0.9766 0.8212 0.5514 0.040 Uiso 1 1 calc R U . . .
H11B H 1.1247 0.7952 0.5660 0.040 Uiso 1 1 calc R U . . .
C29 C 0.5407(5) 0.3966(4) 0.8050(3) 0.0334(10) Uani 1 1 d . . . . .
H29A H 0.5014 0.3898 0.8754 0.050 Uiso 1 1 calc R U . . .
H29B H 0.5778 0.3285 0.7883 0.050 Uiso 1 1 calc R U . . .
H29C H 0.4690 0.4193 0.7745 0.050 Uiso 1 1 calc R U . . .
C19 C 0.3867(5) 0.7373(5) 0.9370(3) 0.0359(11) Uani 1 1 d . . . . .
H19A H 0.3974 0.6707 0.9780 0.054 Uiso 1 1 calc R U . . .
H19B H 0.2908 0.7607 0.9578 0.054 Uiso 1 1 calc R U . . .
H19C H 0.4468 0.7905 0.9428 0.054 Uiso 1 1 calc R U . . .
C12 C 0.9833(5) 0.8459(4) 0.6861(4) 0.0400(13) Uani 1 1 d . . . . .
H12A H 1.0458 0.8254 0.7258 0.048 Uiso 1 1 calc R U . . .
H12B H 0.9894 0.9229 0.6640 0.048 Uiso 1 1 calc R U . . .
C16 C 0.8431(6) 0.8312(4) 0.9379(4) 0.0374(11) Uani 1 1 d . . . . .
H16 H 0.8776 0.7579 0.9320 0.045 Uiso 1 1 calc R U . . .
C13 C 0.7743(6) 1.0171(3) 0.8081(4) 0.0355(11) Uani 1 1 d . . . . .
H13 H 0.8745 1.0326 0.7923 0.043 Uiso 1 1 calc R U . . .
C26 C 0.5709(5) 0.6744(3) 0.4776(3) 0.0270(9) Uani 1 1 d . . . . .
H26 H 0.5147 0.6264 0.5361 0.032 Uiso 1 1 calc R U . . .
C9 C 1.0663(5) 0.6211(4) 0.6958(4) 0.0392(11) Uani 1 1 d . . . . .
H9A H 1.0307 0.6450 0.7582 0.059 Uiso 1 1 calc R U . . .
H9B H 1.1638 0.6398 0.6667 0.059 Uiso 1 1 calc R U . . .
H9C H 1.0563 0.5446 0.7054 0.059 Uiso 1 1 calc R U . . .
C22 C 0.4393(5) 0.8150(4) 0.6654(3) 0.0317(10) Uani 1 1 d . . . . .
H22A H 0.3746 0.7698 0.6523 0.038 Uiso 1 1 calc R U . . .
H22B H 0.4388 0.8859 0.6267 0.038 Uiso 1 1 calc R U . . .
C25 C 0.7314(6) 0.9736(4) 0.4924(4) 0.0355(11) Uani 1 1 d . . . . .
H25A H 0.6672 0.9754 0.5571 0.053 Uiso 1 1 calc R U . . .
H25B H 0.7349 1.0431 0.4522 0.053 Uiso 1 1 calc R U . . .
H25C H 0.8233 0.9542 0.4973 0.053 Uiso 1 1 calc R U . . .
C5 C 0.8932(5) 0.4730(4) 0.9212(3) 0.0339(10) Uani 1 1 d . . . . .
H5 H 0.9070 0.5105 0.9672 0.041 Uiso 1 1 calc R U . . .
C24 C 0.7793(7) 0.8886(4) 0.3410(4) 0.0476(14) Uani 1 1 d . . . . .
H24A H 0.8727 0.8699 0.3432 0.071 Uiso 1 1 calc R U . . .
H24B H 0.7804 0.9581 0.3012 0.071 Uiso 1 1 calc R U . . .
H24C H 0.7459 0.8363 0.3130 0.071 Uiso 1 1 calc R U . . .
C28 C 0.6651(7) 0.6009(4) 0.4119(4) 0.0434(13) Uani 1 1 d . . . . .
H28A H 0.7201 0.6433 0.3515 0.065 Uiso 1 1 calc R U . . .
H28B H 0.6081 0.5516 0.3975 0.065 Uiso 1 1 calc R U . . .
H28C H 0.7264 0.5616 0.4453 0.065 Uiso 1 1 calc R U . . .
C18 C 0.7394(7) 0.8239(5) 1.0429(4) 0.0496(14) Uani 1 1 d . . . . .
H18A H 0.7104 0.8948 1.0558 0.074 Uiso 1 1 calc R U . . .
H18B H 0.7845 0.7892 1.0900 0.074 Uiso 1 1 calc R U . . .
H18C H 0.6586 0.7830 1.0484 0.074 Uiso 1 1 calc R U . . .
C6 C 0.8604(6) 0.3634(4) 0.7808(4) 0.0339(10) Uani 1 1 d . . . . .
H6 H 0.8494 0.3272 0.7331 0.041 Uiso 1 1 calc R U . . .
C7 C 0.9860(6) 0.3921(5) 0.8914(4) 0.0447(12) Uani 1 1 d . . . . .
H7 H 1.0595 0.3753 0.9180 0.054 Uiso 1 1 calc R U . . .
C17 C 0.9721(7) 0.8975(5) 0.9255(5) 0.0523(15) Uani 1 1 d . . . . .
H17A H 1.0424 0.8900 0.8644 0.078 Uiso 1 1 calc R U . . .
H17B H 1.0092 0.8725 0.9793 0.078 Uiso 1 1 calc R U . . .
H17C H 0.9459 0.9717 0.9251 0.078 Uiso 1 1 calc R U . . .
C8 C 0.9698(6) 0.3350(4) 0.8208(4) 0.0420(12) Uani 1 1 d . . . . .
H8 H 1.0309 0.2793 0.8013 0.050 Uiso 1 1 calc R U . . .
C15 C 0.6906(7) 1.0736(5) 0.8941(4) 0.0538(16) Uani 1 1 d . . . . .
H15A H 0.5928 1.0564 0.9119 0.081 Uiso 1 1 calc R U . . .
H15B H 0.7028 1.1499 0.8744 0.081 Uiso 1 1 calc R U . . .
H15C H 0.7241 1.0499 0.9499 0.081 Uiso 1 1 calc R U . . .
C14 C 0.7277(8) 1.0583(5) 0.7183(5) 0.0571(17) Uani 1 1 d . . . . .
H14A H 0.7812 1.0233 0.6646 0.086 Uiso 1 1 calc R U . . .
H14B H 0.7428 1.1344 0.6999 0.086 Uiso 1 1 calc R U . . .
H14C H 0.6297 1.0433 0.7332 0.086 Uiso 1 1 calc R U . . .
C27 C 0.4648(6) 0.7331(4) 0.4297(4) 0.0386(11) Uani 1 1 d . . . . .
H27A H 0.4061 0.7783 0.4727 0.058 Uiso 1 1 calc R U . . .
H27B H 0.4076 0.6816 0.4183 0.058 Uiso 1 1 calc R U . . .
H27C H 0.5141 0.7763 0.3680 0.058 Uiso 1 1 calc R U . . .
N5 N 0.6541(4) 0.4763(3) 0.7696(2) 0.0234(7) Uani 1 1 d . . . . .


_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 P1 3.2145(11) . ?
U1 P2 3.1286(11) . ?
U1 N2 2.297(3) . ?
U1 N1 2.734(4) . ?
U1 N3 2.813(4) . ?
U1 N4 2.285(4) . ?
U1 C2 2.461(4) . ?
U1 C1 2.553(4) . ?
U1 C4 3.056(4) . ?
U1 C3 3.040(4) . ?
U1 N5 2.568(3) . ?
P1 N2 1.688(4) . ?
P1 C16 1.891(5) . ?
P1 C13 1.863(4) . ?
P2 N4 1.675(4) . ?
P2 C23 1.861(4) . ?
P2 C26 1.875(4) . ?
N2 C12 1.444(5) . ?
N1 C10 1.458(6) . ?
N1 C11 1.481(5) . ?
N1 C9 1.474(6) . ?
N3 C21 1.462(6) . ?
N3 C20 1.477(6) . ?
N3 C19 1.480(6) . ?
N4 C22 1.457(6) . ?
C23 H23 0.9800 . ?
C23 C25 1.520(6) . ?
C23 C24 1.530(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 N5 1.459(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.527(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C3 1.439(6) . ?
C4 C3 1.415(6) . ?
C4 C6 1.384(7) . ?
C4 N5 1.453(5) . ?
C3 C5 1.417(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.511(6) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 N5 1.467(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C16 H16 0.9800 . ?
C16 C18 1.542(7) . ?
C16 C17 1.528(7) . ?
C13 H13 0.9800 . ?
C13 C15 1.538(7) . ?
C13 C14 1.511(8) . ?
C26 H26 0.9800 . ?
C26 C28 1.522(7) . ?
C26 C27 1.531(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C7 1.377(8) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C6 H6 0.9300 . ?
C6 C8 1.393(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.404(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C8 H8 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 U1 P1 113.76(3) . . ?
N2 U1 P1 30.22(9) . . ?
N2 U1 P2 99.68(10) . . ?
N2 U1 N1 64.59(12) . . ?
N2 U1 N3 107.27(12) . . ?
N2 U1 C2 146.30(14) . . ?
N2 U1 C1 93.21(13) . . ?
N2 U1 C4 120.81(13) . . ?
N2 U1 C3 100.08(13) . . ?
N2 U1 N5 149.07(13) . . ?
N1 U1 P1 93.52(8) . . ?
N1 U1 P2 82.45(9) . . ?
N1 U1 N3 170.16(11) . . ?
N1 U1 C4 81.91(12) . . ?
N1 U1 C3 86.03(12) . . ?
N3 U1 P1 79.48(8) . . ?
N3 U1 P2 93.98(8) . . ?
N3 U1 C4 107.60(11) . . ?
N3 U1 C3 101.29(12) . . ?
N4 U1 P1 98.46(10) . . ?
N4 U1 P2 31.41(9) . . ?
N4 U1 N2 100.16(14) . . ?
N4 U1 N1 111.12(12) . . ?
N4 U1 N3 63.65(12) . . ?
N4 U1 C2 90.73(15) . . ?
N4 U1 C1 140.98(14) . . ?
N4 U1 C4 138.13(12) . . ?
N4 U1 C3 157.74(12) . . ?
N4 U1 N5 110.50(12) . . ?
C2 U1 P1 170.70(12) . . ?
C2 U1 P2 73.69(10) . . ?
C2 U1 N1 81.73(13) . . ?
C2 U1 N3 106.15(13) . . ?
C2 U1 C1 98.13(13) . . ?
C2 U1 C4 50.58(13) . . ?
C2 U1 C3 77.40(13) . . ?
C2 U1 N5 33.65(12) . . ?
C1 U1 P1 75.61(9) . . ?
C1 U1 P2 166.21(10) . . ?
C1 U1 N1 107.75(14) . . ?
C1 U1 N3 77.40(13) . . ?
C1 U1 C4 51.24(13) . . ?
C1 U1 C3 28.13(13) . . ?
C1 U1 N5 65.53(12) . . ?
C4 U1 P1 121.00(8) . . ?
C4 U1 P2 123.61(8) . . ?
C3 U1 P1 94.36(8) . . ?
C3 U1 P2 150.09(8) . . ?
C3 U1 C4 26.85(11) . . ?
N5 U1 P1 141.11(8) . . ?
N5 U1 P2 104.27(8) . . ?
N5 U1 N1 99.34(12) . . ?
N5 U1 N3 90.42(11) . . ?
N5 U1 C4 28.28(11) . . ?
N5 U1 C3 50.65(11) . . ?
N2 P1 U1 43.24(11) . . ?
N2 P1 C16 106.2(2) . . ?
N2 P1 C13 106.5(2) . . ?
C16 P1 U1 115.26(15) . . ?
C13 P1 U1 136.06(16) . . ?
C13 P1 C16 102.5(2) . . ?
N4 P2 U1 45.29(14) . . ?
N4 P2 C23 107.1(2) . . ?
N4 P2 C26 106.24(19) . . ?
C23 P2 U1 134.00(14) . . ?
C23 P2 C26 103.1(2) . . ?
C26 P2 U1 118.62(13) . . ?
P1 N2 U1 106.54(17) . . ?
C12 N2 U1 129.2(3) . . ?
C12 N2 P1 123.8(3) . . ?
C10 N1 U1 117.6(3) . . ?
C10 N1 C11 109.0(4) . . ?
C10 N1 C9 107.9(4) . . ?
C11 N1 U1 103.1(3) . . ?
C9 N1 U1 109.3(3) . . ?
C9 N1 C11 109.6(4) . . ?
C21 N3 U1 104.1(3) . . ?
C21 N3 C20 110.8(4) . . ?
C21 N3 C19 107.5(4) . . ?
C20 N3 U1 107.2(3) . . ?
C20 N3 C19 108.2(3) . . ?
C19 N3 U1 119.0(3) . . ?
P2 N4 U1 103.31(19) . . ?
C22 N4 U1 131.4(3) . . ?
C22 N4 P2 124.7(3) . . ?
P2 C23 H23 109.0 . . ?
C25 C23 P2 108.7(3) . . ?
C25 C23 H23 109.0 . . ?
C25 C23 C24 110.9(4) . . ?
C24 C23 P2 110.2(4) . . ?
C24 C23 H23 109.0 . . ?
U1 C2 H2A 115.7 . . ?
U1 C2 H2B 115.7 . . ?
H2A C2 H2B 112.7 . . ?
N5 C2 U1 77.2(2) . . ?
N5 C2 H2A 115.7 . . ?
N5 C2 H2B 115.7 . . ?
N3 C21 H21A 109.4 . . ?
N3 C21 H21B 109.4 . . ?
N3 C21 C22 111.2(4) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
U1 C1 H1A 112.7 . . ?
U1 C1 H1B 112.7 . . ?
H1A C1 H1B 110.2 . . ?
C3 C1 U1 95.1(2) . . ?
C3 C1 H1A 112.7 . . ?
C3 C1 H1B 112.7 . . ?
C3 C4 U1 76.0(2) . . ?
C3 C4 N5 116.3(4) . . ?
C6 C4 U1 138.9(3) . . ?
C6 C4 C3 122.3(4) . . ?
C6 C4 N5 121.4(4) . . ?
N5 C4 U1 56.85(18) . . ?
C1 C3 U1 56.8(2) . . ?
C4 C3 U1 77.2(2) . . ?
C4 C3 C1 119.6(4) . . ?
C4 C3 C5 115.3(4) . . ?
C5 C3 U1 136.9(3) . . ?
C5 C3 C1 124.9(4) . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
N1 C11 C12 110.8(4) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N5 C29 H29A 109.5 . . ?
N5 C29 H29B 109.5 . . ?
N5 C29 H29C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C12 C11 107.6(3) . . ?
N2 C12 H12A 110.2 . . ?
N2 C12 H12B 110.2 . . ?
C11 C12 H12A 110.2 . . ?
C11 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
P1 C16 H16 105.7 . . ?
C18 C16 P1 110.4(4) . . ?
C18 C16 H16 105.7 . . ?
C17 C16 P1 117.3(4) . . ?
C17 C16 H16 105.7 . . ?
C17 C16 C18 111.1(4) . . ?
P1 C13 H13 109.0 . . ?
C15 C13 P1 110.3(3) . . ?
C15 C13 H13 109.0 . . ?
C14 C13 P1 109.5(3) . . ?
C14 C13 H13 109.0 . . ?
C14 C13 C15 109.9(5) . . ?
P2 C26 H26 105.4 . . ?
C28 C26 P2 110.8(3) . . ?
C28 C26 H26 105.4 . . ?
C28 C26 C27 111.1(4) . . ?
C27 C26 P2 117.7(3) . . ?
C27 C26 H26 105.4 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C22 C21 107.8(4) . . ?
N4 C22 H22A 110.2 . . ?
N4 C22 H22B 110.2 . . ?
C21 C22 H22A 110.2 . . ?
C21 C22 H22B 110.2 . . ?
H22A C22 H22B 108.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C3 C5 H5 118.6 . . ?
C7 C5 C3 122.8(4) . . ?
C7 C5 H5 118.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C4 C6 H6 119.7 . . ?
C4 C6 C8 120.6(4) . . ?
C8 C6 H6 119.7 . . ?
C5 C7 H7 119.9 . . ?
C5 C7 C8 120.1(5) . . ?
C8 C7 H7 119.9 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C6 C8 C7 118.7(5) . . ?
C6 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C2 N5 U1 69.1(2) . . ?
C2 N5 C29 117.4(3) . . ?
C4 N5 U1 94.9(2) . . ?
C4 N5 C2 112.2(4) . . ?
C4 N5 C29 112.1(3) . . ?
C29 N5 U1 144.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 P1 N2 C12 -173.1(5) . . . . ?
U1 P1 C16 C18 -106.3(3) . . . . ?
U1 P1 C16 C17 125.0(4) . . . . ?
U1 P1 C13 C15 141.1(4) . . . . ?
U1 P1 C13 C14 20.0(6) . . . . ?
U1 P2 N4 C22 -171.8(4) . . . . ?
U1 P2 C23 C25 10.0(4) . . . . ?
U1 P2 C23 C24 131.8(3) . . . . ?
U1 P2 C26 C28 -96.9(3) . . . . ?
U1 P2 C26 C27 133.7(3) . . . . ?
U1 N2 C12 C11 14.0(7) . . . . ?
U1 N1 C11 C12 53.3(4) . . . . ?
U1 N3 C21 C22 49.9(4) . . . . ?
U1 N4 C22 C21 16.2(5) . . . . ?
U1 C2 N5 C4 -86.7(3) . . . . ?
U1 C2 N5 C29 141.2(4) . . . . ?
U1 C1 C3 C4 -47.3(4) . . . . ?
U1 C1 C3 C5 127.4(4) . . . . ?
U1 C4 C3 C1 39.1(3) . . . . ?
U1 C4 C3 C5 -136.1(4) . . . . ?
U1 C4 C6 C8 105.4(6) . . . . ?
U1 C4 N5 C2 69.4(3) . . . . ?
U1 C4 N5 C29 -155.9(4) . . . . ?
U1 C3 C5 C7 -101.7(6) . . . . ?
P1 N2 C12 C11 -174.6(4) . . . . ?
P2 N4 C22 C21 -174.4(3) . . . . ?
N2 P1 C16 C18 -151.8(3) . . . . ?
N2 P1 C16 C17 79.6(4) . . . . ?
N2 P1 C13 C15 179.1(4) . . . . ?
N2 P1 C13 C14 58.0(5) . . . . ?
N1 C11 C12 N2 -47.6(6) . . . . ?
N3 C21 C22 N4 -46.6(5) . . . . ?
N4 P2 C23 C25 53.4(4) . . . . ?
N4 P2 C23 C24 175.2(4) . . . . ?
N4 P2 C26 C28 -144.4(3) . . . . ?
N4 P2 C26 C27 86.3(4) . . . . ?
C23 P2 N4 U1 -135.90(18) . . . . ?
C23 P2 N4 C22 52.3(4) . . . . ?
C23 P2 C26 C28 103.2(4) . . . . ?
C23 P2 C26 C27 -26.2(4) . . . . ?
C1 C3 C5 C7 -178.2(5) . . . . ?
C4 C3 C5 C7 -3.3(7) . . . . ?
C4 C6 C8 C7 -1.2(8) . . . . ?
C3 C4 C6 C8 -1.3(7) . . . . ?
C3 C4 N5 U1 49.8(4) . . . . ?
C3 C4 N5 C2 119.2(4) . . . . ?
C3 C4 N5 C29 -106.2(4) . . . . ?
C3 C5 C7 C8 1.0(8) . . . . ?
C20 N3 C21 C22 -65.0(5) . . . . ?
C10 N1 C11 C12 179.0(4) . . . . ?
C19 N3 C21 C22 177.0(4) . . . . ?
C16 P1 N2 U1 109.9(2) . . . . ?
C16 P1 N2 C12 -63.2(5) . . . . ?
C16 P1 C13 C15 -69.7(5) . . . . ?
C16 P1 C13 C14 169.3(4) . . . . ?
C13 P1 N2 U1 -141.4(2) . . . . ?
C13 P1 N2 C12 45.5(5) . . . . ?
C13 P1 C16 C18 96.7(4) . . . . ?
C13 P1 C16 C17 -31.9(5) . . . . ?
C26 P2 N4 U1 114.43(19) . . . . ?
C26 P2 N4 C22 -57.4(4) . . . . ?
C26 P2 C23 C25 165.2(3) . . . . ?
C26 P2 C23 C24 -73.0(4) . . . . ?
C9 N1 C11 C12 -63.0(5) . . . . ?
C5 C7 C8 C6 1.3(8) . . . . ?
C6 C4 C3 U1 139.5(4) . . . . ?
C6 C4 C3 C1 178.6(4) . . . . ?
C6 C4 C3 C5 3.4(6) . . . . ?
C6 C4 N5 U1 -130.9(4) . . . . ?
C6 C4 N5 C2 -61.5(5) . . . . ?
C6 C4 N5 C29 73.1(5) . . . . ?
N5 C4 C3 U1 -41.2(3) . . . . ?
N5 C4 C3 C1 -2.1(5) . . . . ?
N5 C4 C3 C5 -177.3(3) . . . . ?
N5 C4 C6 C8 179.5(4) . . . . ?

_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_lk-3_a
_database_code_depnum_ccdc_archive 'CCDC 2254128'
loop_
_audit_author_name
_audit_author_address
'Congqing Zhu'
;Nanjing University
China
;
_audit_update_record             
;
2023-07-25 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         'C40 H96 Cl6 N8 P4 Rh2 U2'
_chemical_formula_sum            'C40 H96 Cl6 N8 P4 Rh2 U2'
_chemical_formula_weight         1707.70
_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 0.0148 0.0070 '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 0.3294 0.5404 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2596 0.3354 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.0161 2.8414 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -5.2580 11.3041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.7929(4)
_cell_length_b                   26.3286(10)
_cell_length_c                   11.1451(4)
_cell_angle_alpha                90
_cell_angle_beta                 110.635(2)
_cell_angle_gamma                90
_cell_volume                     2963.83(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      53.89
_cell_measurement_theta_min      2.92
_shelx_estimated_absorpt_T_max   0.178
_shelx_estimated_absorpt_T_min   0.155
_exptl_absorpt_coefficient_mu    16.493
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1635 before and 0.0943 after correction.
The Ratio of minimum to maximum transmission is 0.5568.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellowish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29584
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.043
_diffrn_reflns_theta_min         2.920
_diffrn_ambient_temperature      193.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4530
_reflns_number_total             5437
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         3.093
_refine_diff_density_min         -2.238
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5437
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.026
_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)+(0.1010P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1402
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 2
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2.a Ternary CH refined with riding coordinates:
 C5(H5), C15(H15), C8(H8), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C4(H4A,H4B), C14(H14A,H14B), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C6(H6A,H6B,H6C),
 C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C12(H12A,H12B,H12C),
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.57898(3) 0.36668(2) 0.53057(2) 0.02440(14) Uani 1 1 d . . . . .
Rh1 Rh 0.51353(6) 0.45297(2) 0.37540(5) 0.02204(17) Uani 1 1 d . . . . .
Cl3 Cl 0.6506(2) 0.51184(7) 0.53838(18) 0.0306(5) Uani 1 1 d . . . . .
P1 P 0.6922(2) 0.42597(7) 0.33645(19) 0.0251(5) Uani 1 1 d . . . . .
P2 P 0.3627(2) 0.39429(7) 0.25900(19) 0.0258(5) Uani 1 1 d . . . . .
Cl1 Cl 0.5780(3) 0.41285(9) 0.7416(2) 0.0458(6) Uani 1 1 d . . . . .
Cl2 Cl 0.6286(3) 0.26718(8) 0.5125(2) 0.0476(6) Uani 1 1 d . . . . .
N4 N 0.3723(7) 0.3552(2) 0.3783(7) 0.0301(17) Uani 1 1 d . U . . .
N1 N 0.8287(9) 0.3576(3) 0.6994(8) 0.042(2) Uani 1 1 d . . . . .
N2 N 0.7464(7) 0.3813(3) 0.4457(7) 0.0376(18) Uani 1 1 d . . . . .
N3 N 0.3919(8) 0.3158(3) 0.6069(7) 0.0392(18) Uani 1 1 d . . . . .
C13 C 0.3180(10) 0.2848(3) 0.4924(8) 0.038(2) Uani 1 1 d . . . . .
H13A H 0.2427 0.2676 0.5064 0.046 Uiso 1 1 calc R U . . .
H13B H 0.3770 0.2585 0.4785 0.046 Uiso 1 1 calc R U . . .
C17 C 0.0823(9) 0.3912(4) 0.1145(9) 0.042(2) Uani 1 1 d . . . . .
H17A H 0.1011 0.3782 0.0403 0.063 Uiso 1 1 calc R U . . .
H17B H 0.0005 0.4112 0.0849 0.063 Uiso 1 1 calc R U . . .
H17C H 0.0716 0.3626 0.1665 0.063 Uiso 1 1 calc R U . . .
C5 C 0.8222(9) 0.4750(3) 0.3621(9) 0.034(2) Uani 1 1 d . . . . .
H5 H 0.8564 0.4809 0.4567 0.041 Uiso 1 1 calc R U . . .
C4 C 0.8842(11) 0.3657(3) 0.5043(12) 0.055(3) Uani 1 1 d . . . . .
H4A H 0.9417 0.3961 0.5269 0.065 Uiso 1 1 calc R U . . .
H4B H 0.9101 0.3452 0.4425 0.065 Uiso 1 1 calc R U . . .
C14 C 0.2668(9) 0.3190(3) 0.3747(8) 0.036(2) Uani 1 1 d . . . . .
H14A H 0.2422 0.2983 0.2956 0.044 Uiso 1 1 calc R U . . .
H14B H 0.1872 0.3377 0.3749 0.044 Uiso 1 1 calc R U . . .
C15 C 0.1968(8) 0.4246(3) 0.1953(8) 0.0302(19) Uani 1 1 d . . . . .
H15 H 0.1750 0.4350 0.2719 0.036 Uiso 1 1 calc R U . . .
C7 C 0.9457(10) 0.4603(4) 0.3310(10) 0.051(3) Uani 1 1 d . . . . .
H7A H 0.9721 0.4255 0.3601 0.077 Uiso 1 1 calc R U . . .
H7B H 1.0182 0.4837 0.3749 0.077 Uiso 1 1 calc R U . . .
H7C H 0.9254 0.4624 0.2382 0.077 Uiso 1 1 calc R U . . .
C3 C 0.9030(9) 0.3346(4) 0.6239(9) 0.047(3) Uani 1 1 d . . . . .
H3A H 0.8715 0.2995 0.5994 0.056 Uiso 1 1 calc R U . . .
H3B H 0.9984 0.3331 0.6769 0.056 Uiso 1 1 calc R U . . .
C8 C 0.6645(12) 0.4014(3) 0.1740(9) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.5761 0.3843 0.1481 0.057 Uiso 1 1 calc R U . . .
C11 C 0.3019(11) 0.3508(4) 0.6372(11) 0.054(3) Uani 1 1 d . . . . .
H11A H 0.3494 0.3683 0.7179 0.081 Uiso 1 1 calc R U . . .
H11B H 0.2275 0.3317 0.6457 0.081 Uiso 1 1 calc R U . . .
H11C H 0.2684 0.3758 0.5682 0.081 Uiso 1 1 calc R U . . .
C6 C 0.7732(11) 0.5259(3) 0.3051(11) 0.055(3) Uani 1 1 d . . . . .
H6A H 0.7572 0.5252 0.2130 0.082 Uiso 1 1 calc R U . . .
H6B H 0.8398 0.5518 0.3464 0.082 Uiso 1 1 calc R U . . .
H6C H 0.6905 0.5340 0.3188 0.082 Uiso 1 1 calc R U . . .
C2 C 0.8398(10) 0.3236(4) 0.8084(9) 0.051(3) Uani 1 1 d . . . . .
H2A H 0.7911 0.3383 0.8595 0.076 Uiso 1 1 calc R U . . .
H2B H 0.9333 0.3197 0.8622 0.076 Uiso 1 1 calc R U . . .
H2C H 0.8024 0.2903 0.7759 0.076 Uiso 1 1 calc R U . . .
C19 C 0.4558(11) 0.3053(3) 0.1706(9) 0.047(3) Uani 1 1 d . . . . .
H19A H 0.5446 0.3196 0.2114 0.071 Uiso 1 1 calc R U . . .
H19B H 0.4532 0.2851 0.0958 0.071 Uiso 1 1 calc R U . . .
H19C H 0.4343 0.2836 0.2319 0.071 Uiso 1 1 calc R U . . .
C1 C 0.8874(10) 0.4077(4) 0.7505(10) 0.056(3) Uani 1 1 d . . . . .
H1A H 0.8686 0.4320 0.6798 0.084 Uiso 1 1 calc R U . . .
H1B H 0.9834 0.4041 0.7927 0.084 Uiso 1 1 calc R U . . .
H1C H 0.8489 0.4200 0.8126 0.084 Uiso 1 1 calc R U . . .
C18 C 0.3547(10) 0.3484(4) 0.1277(9) 0.045(2) Uani 1 1 d . . . . .
H18 H 0.2680 0.3308 0.1101 0.054 Uiso 1 1 calc R U . . .
C12 C 0.4489(11) 0.2817(4) 0.7189(10) 0.052(3) Uani 1 1 d . . . . .
H12A H 0.5058 0.2564 0.6997 0.077 Uiso 1 1 calc R U . . .
H12B H 0.3772 0.2645 0.7374 0.077 Uiso 1 1 calc R U . . .
H12C H 0.5013 0.3018 0.7936 0.077 Uiso 1 1 calc R U . . .
C16 C 0.1983(11) 0.4738(4) 0.1218(10) 0.052(3) Uani 1 1 d . . . . .
H16A H 0.2659 0.4968 0.1769 0.078 Uiso 1 1 calc R U . . .
H16B H 0.1113 0.4902 0.0969 0.078 Uiso 1 1 calc R U . . .
H16C H 0.2186 0.4659 0.0449 0.078 Uiso 1 1 calc R U . . .
C20 C 0.3424(14) 0.3713(4) -0.0008(10) 0.062(3) Uani 1 1 d . . . . .
H20A H 0.3071 0.4058 -0.0066 0.093 Uiso 1 1 calc R U . . .
H20B H 0.2825 0.3505 -0.0698 0.093 Uiso 1 1 calc R U . . .
H20C H 0.4298 0.3723 -0.0091 0.093 Uiso 1 1 calc R U . . .
C10 C 0.7591(14) 0.3597(4) 0.1654(15) 0.081(4) Uani 1 1 d . U . . .
H10A H 0.8498 0.3729 0.1953 0.122 Uiso 1 1 calc R U . . .
H10B H 0.7345 0.3484 0.0762 0.122 Uiso 1 1 calc R U . . .
H10C H 0.7538 0.3309 0.2192 0.122 Uiso 1 1 calc R U . . .
C9 C 0.6463(15) 0.4428(5) 0.0770(10) 0.098(6) Uani 1 1 d . . . . .
H9A H 0.5846 0.4682 0.0875 0.146 Uiso 1 1 calc R U . . .
H9B H 0.6105 0.4283 -0.0094 0.146 Uiso 1 1 calc R U . . .
H9C H 0.7319 0.4588 0.0896 0.146 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Rh1 2.7910(6) . ?
U1 Cl1 2.651(2) . ?
U1 Cl2 2.696(2) . ?
U1 N4 2.298(7) . ?
U1 N1 2.700(8) . ?
U1 N2 2.348(7) . ?
U1 N3 2.793(8) . ?
Rh1 Cl3 2.473(2) 3_666 ?
Rh1 Cl3 2.4487(19) . ?
Rh1 P1 2.236(2) . ?
Rh1 P2 2.287(2) . ?
Cl3 Rh1 2.473(2) 3_666 ?
P1 N2 1.645(7) . ?
P1 C5 1.853(9) . ?
P1 C8 1.845(9) . ?
P2 N4 1.655(7) . ?
P2 C15 1.859(8) . ?
P2 C18 1.876(10) . ?
N4 C14 1.474(10) . ?
N1 C3 1.480(13) . ?
N1 C2 1.479(11) . ?
N1 C1 1.488(11) . ?
N2 C4 1.457(13) . ?
N3 C13 1.488(11) . ?
N3 C11 1.462(12) . ?
N3 C12 1.484(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.525(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 C15 1.526(11) . ?
C5 H5 1.0000 . ?
C5 C7 1.539(13) . ?
C5 C6 1.498(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.515(14) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 1.0000 . ?
C15 C16 1.536(13) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C8 H8 1.0000 . ?
C8 C10 1.526(15) . ?
C8 C9 1.497(14) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C18 1.529(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C20 1.516(14) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
Rh1 U1 N3 121.77(15) . . ?
Cl1 U1 Rh1 95.58(5) . . ?
Cl1 U1 Cl2 125.10(8) . . ?
Cl1 U1 N1 74.8(2) . . ?
Cl1 U1 N3 73.76(15) . . ?
Cl2 U1 Rh1 139.32(6) . . ?
Cl2 U1 N1 77.88(16) . . ?
Cl2 U1 N3 74.98(15) . . ?
N4 U1 Rh1 71.42(16) . . ?
N4 U1 Cl1 114.2(2) . . ?
N4 U1 Cl2 89.07(17) . . ?
N4 U1 N1 166.9(2) . . ?
N4 U1 N2 114.1(3) . . ?
N4 U1 N3 62.9(2) . . ?
N1 U1 Rh1 118.47(15) . . ?
N1 U1 N3 113.4(2) . . ?
N2 U1 Rh1 71.30(17) . . ?
N2 U1 Cl1 121.8(2) . . ?
N2 U1 Cl2 85.88(19) . . ?
N2 U1 N1 64.8(3) . . ?
N2 U1 N3 160.5(2) . . ?
Cl3 Rh1 U1 97.11(5) 3_666 . ?
Cl3 Rh1 U1 95.79(5) . . ?
Cl3 Rh1 Cl3 78.61(7) . 3_666 ?
P1 Rh1 U1 79.30(5) . . ?
P1 Rh1 Cl3 168.19(7) . 3_666 ?
P1 Rh1 Cl3 90.49(7) . . ?
P1 Rh1 P2 99.50(7) . . ?
P2 Rh1 U1 77.04(5) . . ?
P2 Rh1 Cl3 166.27(8) . . ?
P2 Rh1 Cl3 90.55(7) . 3_666 ?
Rh1 Cl3 Rh1 101.39(7) . 3_666 ?
N2 P1 Rh1 100.9(3) . . ?
N2 P1 C5 109.3(4) . . ?
N2 P1 C8 111.6(4) . . ?
C5 P1 Rh1 114.0(3) . . ?
C8 P1 Rh1 116.7(4) . . ?
C8 P1 C5 104.3(4) . . ?
N4 P2 Rh1 97.7(2) . . ?
N4 P2 C15 110.7(4) . . ?
N4 P2 C18 101.5(4) . . ?
C15 P2 Rh1 108.9(3) . . ?
C15 P2 C18 101.9(4) . . ?
C18 P2 Rh1 134.9(3) . . ?
P2 N4 U1 106.3(3) . . ?
C14 N4 U1 130.1(5) . . ?
C14 N4 P2 123.4(5) . . ?
C3 N1 U1 104.4(5) . . ?
C3 N1 C1 109.6(8) . . ?
C2 N1 U1 113.5(6) . . ?
C2 N1 C3 108.5(7) . . ?
C2 N1 C1 108.8(8) . . ?
C1 N1 U1 112.0(5) . . ?
P1 N2 U1 107.0(3) . . ?
C4 N2 U1 125.6(6) . . ?
C4 N2 P1 125.0(7) . . ?
C13 N3 U1 103.2(5) . . ?
C11 N3 U1 112.3(5) . . ?
C11 N3 C13 110.1(8) . . ?
C11 N3 C12 107.4(8) . . ?
C12 N3 U1 114.6(6) . . ?
C12 N3 C13 109.2(7) . . ?
N3 C13 H13A 109.7 . . ?
N3 C13 H13B 109.7 . . ?
N3 C13 C14 109.6(6) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
P1 C5 H5 104.5 . . ?
C7 C5 P1 117.4(6) . . ?
C7 C5 H5 104.5 . . ?
C6 C5 P1 115.0(7) . . ?
C6 C5 H5 104.5 . . ?
C6 C5 C7 109.5(8) . . ?
N2 C4 H4A 109.6 . . ?
N2 C4 H4B 109.6 . . ?
N2 C4 C3 110.2(9) . . ?
H4A C4 H4B 108.1 . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
N4 C14 C13 108.4(7) . . ?
N4 C14 H14A 110.0 . . ?
N4 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
P2 C15 H15 106.0 . . ?
C17 C15 P2 116.6(6) . . ?
C17 C15 H15 106.0 . . ?
C17 C15 C16 109.3(7) . . ?
C16 C15 P2 112.1(6) . . ?
C16 C15 H15 106.0 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C3 C4 110.4(8) . . ?
N1 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
P1 C8 H8 104.4 . . ?
C10 C8 P1 115.7(8) . . ?
C10 C8 H8 104.4 . . ?
C9 C8 P1 112.8(7) . . ?
C9 C8 H8 104.4 . . ?
C9 C8 C10 113.5(10) . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P2 C18 H18 103.5 . . ?
C19 C18 P2 113.8(6) . . ?
C19 C18 H18 103.5 . . ?
C20 C18 P2 116.5(7) . . ?
C20 C18 C19 113.9(9) . . ?
C20 C18 H18 103.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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
U1 N4 C14 C13 -3.0(11) . . . . ?
U1 N1 C3 C4 53.6(9) . . . . ?
U1 N2 C4 C3 4.6(12) . . . . ?
U1 N3 C13 C14 -53.9(8) . . . . ?
Rh1 P1 N2 U1 11.6(4) . . . . ?
Rh1 P1 N2 C4 -151.6(8) . . . . ?
Rh1 P1 C5 C7 -177.1(6) . . . . ?
Rh1 P1 C5 C6 -46.1(7) . . . . ?
Rh1 P1 C8 C10 -148.7(7) . . . . ?
Rh1 P1 C8 C9 78.2(9) . . . . ?
Rh1 P2 N4 U1 -25.7(3) . . . . ?
Rh1 P2 N4 C14 157.9(7) . . . . ?
Rh1 P2 C15 C17 -180.0(6) . . . . ?
Rh1 P2 C15 C16 52.9(7) . . . . ?
Rh1 P2 C18 C19 67.6(9) . . . . ?
Rh1 P2 C18 C20 -67.9(10) . . . . ?
P1 N2 C4 C3 164.7(7) . . . . ?
P2 N4 C14 C13 172.4(6) . . . . ?
N4 P2 C15 C17 -73.7(7) . . . . ?
N4 P2 C15 C16 159.2(6) . . . . ?
N4 P2 C18 C19 -45.6(8) . . . . ?
N4 P2 C18 C20 178.9(8) . . . . ?
N2 P1 C5 C7 70.8(8) . . . . ?
N2 P1 C5 C6 -158.2(7) . . . . ?
N2 P1 C8 C10 -33.4(9) . . . . ?
N2 P1 C8 C9 -166.5(9) . . . . ?
N2 C4 C3 N1 -42.1(11) . . . . ?
N3 C13 C14 N4 42.4(10) . . . . ?
C5 P1 N2 U1 132.0(4) . . . . ?
C5 P1 N2 C4 -31.1(10) . . . . ?
C5 P1 C8 C10 84.5(8) . . . . ?
C5 P1 C8 C9 -48.5(10) . . . . ?
C15 P2 N4 U1 -139.3(3) . . . . ?
C15 P2 N4 C14 44.4(8) . . . . ?
C15 P2 C18 C19 -159.8(7) . . . . ?
C15 P2 C18 C20 64.7(9) . . . . ?
C8 P1 N2 U1 -113.1(5) . . . . ?
C8 P1 N2 C4 83.7(9) . . . . ?
C8 P1 C5 C7 -48.6(8) . . . . ?
C8 P1 C5 C6 82.3(8) . . . . ?
C11 N3 C13 C14 66.1(10) . . . . ?
C2 N1 C3 C4 174.9(8) . . . . ?
C1 N1 C3 C4 -66.5(10) . . . . ?
C18 P2 N4 U1 113.2(4) . . . . ?
C18 P2 N4 C14 -63.1(8) . . . . ?
C18 P2 C15 C17 33.5(8) . . . . ?
C18 P2 C15 C16 -93.6(7) . . . . ?
C12 N3 C13 C14 -176.2(8) . . . . ?

_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_1_a
_database_code_depnum_ccdc_archive 'CCDC 2254129'
loop_
_audit_author_name
_audit_author_address
'Congqing Zhu'
;Nanjing University
China
;
_audit_update_record             
;
2023-07-25 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         'C20 H48 Cl2 N4 P2 U'
_chemical_formula_sum            'C20 H48 Cl2 N4 P2 U'
_chemical_formula_weight         715.49
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   22.444(6)
_cell_length_b                   8.321(2)
_cell_length_c                   16.158(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.132(8)
_cell_angle_gamma                90
_cell_volume                     2987.1(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   0.461
_shelx_estimated_absorpt_T_min   0.425
_exptl_absorpt_coefficient_mu    5.733
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4482
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.6012.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26266
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         2.582
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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                5316
_reflns_number_total             6741
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.850
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6741
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.021
_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)+(0.0125P)²+4.3050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0715
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C8(H8), C5(H5)
1.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B)
1.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C),
 C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C),
  C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.25253(2) 0.51196(2) 0.51462(2) 0.03005(6) Uani 1 1 d . . . . .
P2 P 0.37125(6) 0.37382(15) 0.58065(7) 0.0382(3) Uani 1 1 d . . . . .
P1 P 0.13030(6) 0.58177(16) 0.41970(7) 0.0399(3) Uani 1 1 d . . . . .
Cl2 Cl 0.24447(7) 0.24581(15) 0.41967(7) 0.0521(3) Uani 1 1 d . . . . .
Cl1 Cl 0.26240(7) 0.77575(16) 0.61174(8) 0.0558(4) Uani 1 1 d . . . . .
N4 N 0.30590(18) 0.3646(5) 0.6157(2) 0.0390(9) Uani 1 1 d . . . . .
N1 N 0.31728(18) 0.6752(5) 0.4138(2) 0.0394(9) Uani 1 1 d . . . . .
N3 N 0.18801(18) 0.3851(5) 0.6269(2) 0.0439(10) Uani 1 1 d . . . . .
N2 N 0.19832(18) 0.6484(5) 0.4098(2) 0.0406(9) Uani 1 1 d . . . . .
C15 C 0.4284(2) 0.4378(7) 0.6686(3) 0.0523(14) Uani 1 1 d . . . . .
H15 H 0.4336 0.3511 0.7100 0.063 Uiso 1 1 calc R . . . .
C4 C 0.2166(2) 0.7602(7) 0.3483(3) 0.0556(15) Uani 1 1 d . . . . .
H4A H 0.1895 0.8516 0.3412 0.067 Uiso 1 1 calc R . . . .
H4B H 0.2159 0.7074 0.2946 0.067 Uiso 1 1 calc R . . . .
C14 C 0.2867(3) 0.2752(7) 0.6858(3) 0.0551(15) Uani 1 1 d . . . . .
H14A H 0.3176 0.2791 0.7342 0.066 Uiso 1 1 calc R . . . .
H14B H 0.2789 0.1636 0.6705 0.066 Uiso 1 1 calc R . . . .
C1 C 0.3750(2) 0.7398(7) 0.4543(3) 0.0617(16) Uani 1 1 d . . . . .
H1A H 0.3683 0.8058 0.5008 0.092 Uiso 1 1 calc GR . . . .
H1B H 0.3930 0.8032 0.4148 0.092 Uiso 1 1 calc GR . . . .
H1C H 0.4014 0.6527 0.4736 0.092 Uiso 1 1 calc GR . . . .
C3 C 0.2796(2) 0.8145(6) 0.3812(3) 0.0546(14) Uani 1 1 d . . . . .
H3A H 0.2974 0.8660 0.3367 0.066 Uiso 1 1 calc R . . . .
H3B H 0.2783 0.8924 0.4255 0.066 Uiso 1 1 calc R . . . .
C18 C 0.3940(3) 0.1669(6) 0.5543(3) 0.0544(14) Uani 1 1 d . . . . .
H18 H 0.3564 0.1132 0.5312 0.065 Uiso 1 1 calc R . . . .
C8 C 0.1035(3) 0.4717(7) 0.3201(4) 0.0683(18) Uani 1 1 d . . . . .
H8 H 0.1403 0.4249 0.3039 0.082 Uiso 1 1 calc R . . . .
C5 C 0.0808(2) 0.7599(7) 0.4202(3) 0.0533(14) Uani 1 1 d . . . . .
H5 H 0.0781 0.8122 0.3655 0.064 Uiso 1 1 calc R . . . .
C2 C 0.3285(3) 0.5698(7) 0.3449(3) 0.0555(14) Uani 1 1 d . . . . .
H2A H 0.3553 0.4847 0.3663 0.083 Uiso 1 1 calc GR . . . .
H2B H 0.3466 0.6309 0.3045 0.083 Uiso 1 1 calc GR . . . .
H2C H 0.2912 0.5249 0.3187 0.083 Uiso 1 1 calc GR . . . .
C12 C 0.1613(3) 0.2336(7) 0.5930(3) 0.0636(17) Uani 1 1 d . . . . .
H12A H 0.1337 0.2550 0.5432 0.095 Uiso 1 1 calc GR . . . .
H12B H 0.1400 0.1836 0.6338 0.095 Uiso 1 1 calc GR . . . .
H12C H 0.1925 0.1630 0.5801 0.095 Uiso 1 1 calc GR . . . .
C13 C 0.2297(3) 0.3569(8) 0.7044(3) 0.0602(16) Uani 1 1 d . . . . .
H13A H 0.2102 0.2900 0.7418 0.072 Uiso 1 1 calc R . . . .
H13B H 0.2398 0.4587 0.7322 0.072 Uiso 1 1 calc R . . . .
C11 C 0.1389(3) 0.4909(7) 0.6489(4) 0.0654(17) Uani 1 1 d . . . . .
H11A H 0.1554 0.5931 0.6677 0.098 Uiso 1 1 calc GR . . . .
H11B H 0.1204 0.4415 0.6926 0.098 Uiso 1 1 calc GR . . . .
H11C H 0.1092 0.5061 0.6006 0.098 Uiso 1 1 calc GR . . . .
C9 C 0.0788(3) 0.5743(9) 0.2460(4) 0.087(2) Uani 1 1 d . . . . .
H9A H 0.0397 0.6140 0.2536 0.130 Uiso 1 1 calc GR . . . .
H9B H 0.0754 0.5109 0.1959 0.130 Uiso 1 1 calc GR . . . .
H9C H 0.1054 0.6632 0.2414 0.130 Uiso 1 1 calc GR . . . .
C20 C 0.4208(3) 0.0624(7) 0.6270(4) 0.080(2) Uani 1 1 d . . . . .
H20A H 0.4593 0.1047 0.6505 0.120 Uiso 1 1 calc GR . . . .
H20B H 0.4257 -0.0452 0.6076 0.120 Uiso 1 1 calc GR . . . .
H20C H 0.3945 0.0616 0.6689 0.120 Uiso 1 1 calc GR . . . .
C16 C 0.4066(3) 0.5873(8) 0.7099(4) 0.079(2) Uani 1 1 d . . . . .
H16A H 0.4009 0.6733 0.6700 0.118 Uiso 1 1 calc GR . . . .
H16B H 0.4360 0.6185 0.7562 0.118 Uiso 1 1 calc GR . . . .
H16C H 0.3691 0.5643 0.7296 0.118 Uiso 1 1 calc GR . . . .
C19 C 0.4316(3) 0.1709(8) 0.4830(4) 0.080(2) Uani 1 1 d . . . . .
H19A H 0.4099 0.2270 0.4362 0.120 Uiso 1 1 calc GR . . . .
H19B H 0.4397 0.0631 0.4667 0.120 Uiso 1 1 calc GR . . . .
H19C H 0.4689 0.2254 0.5010 0.120 Uiso 1 1 calc GR . . . .
C7 C 0.0177(3) 0.7126(9) 0.4346(5) 0.091(2) Uani 1 1 d . . . . .
H7A H 0.0016 0.6357 0.3931 0.136 Uiso 1 1 calc GR . . . .
H7B H -0.0076 0.8062 0.4306 0.136 Uiso 1 1 calc GR . . . .
H7C H 0.0192 0.6661 0.4892 0.136 Uiso 1 1 calc GR . . . .
C6 C 0.1080(3) 0.8790(8) 0.4863(4) 0.078(2) Uani 1 1 d . . . . .
H6A H 0.1120 0.8290 0.5403 0.117 Uiso 1 1 calc GR . . . .
H6B H 0.0822 0.9712 0.4857 0.117 Uiso 1 1 calc GR . . . .
H6C H 0.1469 0.9120 0.4745 0.117 Uiso 1 1 calc GR . . . .
C17 C 0.4893(3) 0.4699(9) 0.6392(5) 0.097(3) Uani 1 1 d . . . . .
H17A H 0.5033 0.3735 0.6157 0.145 Uiso 1 1 calc GR . . . .
H17B H 0.5178 0.5034 0.6860 0.145 Uiso 1 1 calc GR . . . .
H17C H 0.4848 0.5531 0.5977 0.145 Uiso 1 1 calc GR . . . .
C10 C 0.0661(4) 0.3300(9) 0.3346(4) 0.108(3) Uani 1 1 d . . . . .
H10A H 0.0876 0.2637 0.3775 0.163 Uiso 1 1 calc GR . . . .
H10B H 0.0575 0.2692 0.2839 0.163 Uiso 1 1 calc GR . . . .
H10C H 0.0291 0.3655 0.3520 0.163 Uiso 1 1 calc GR . . . .


_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 P2 2.9589(14) . ?
U1 P1 3.0042(14) . ?
U1 Cl2 2.6856(13) . ?
U1 Cl1 2.6890(13) . ?
U1 N4 2.248(4) . ?
U1 N1 2.698(4) . ?
U1 N3 2.691(4) . ?
U1 N2 2.249(4) . ?
P2 N4 1.647(4) . ?
P2 C15 1.852(5) . ?
P2 C18 1.862(5) . ?
P1 N2 1.653(4) . ?
P1 C8 1.876(5) . ?
P1 C5 1.853(5) . ?
N4 C14 1.469(6) . ?
N1 C1 1.467(6) . ?
N1 C3 1.486(6) . ?
N1 C2 1.468(6) . ?
N3 C12 1.468(6) . ?
N3 C13 1.473(6) . ?
N3 C11 1.493(7) . ?
N2 C4 1.462(6) . ?
C15 C16 1.525(8) . ?
C15 C17 1.532(8) . ?
C4 C3 1.508(7) . ?
C14 C13 1.517(7) . ?
C18 C20 1.515(7) . ?
C18 C19 1.523(8) . ?
C8 C9 1.511(8) . ?
C8 C10 1.484(9) . ?
C5 C7 1.520(7) . ?
C5 C6 1.519(7) . ?

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
P2 U1 P1 165.91(3) . . ?
Cl2 U1 P2 82.54(4) . . ?
Cl2 U1 P1 83.39(4) . . ?
Cl2 U1 Cl1 178.86(4) . . ?
Cl2 U1 N1 93.94(9) . . ?
Cl2 U1 N3 93.58(10) . . ?
Cl1 U1 P2 96.37(4) . . ?
Cl1 U1 P1 97.70(4) . . ?
Cl1 U1 N1 86.24(9) . . ?
Cl1 U1 N3 86.25(9) . . ?
N4 U1 P2 33.48(10) . . ?
N4 U1 P1 146.17(10) . . ?
N4 U1 Cl2 87.19(10) . . ?
N4 U1 Cl1 91.71(10) . . ?
N4 U1 N1 115.86(13) . . ?
N4 U1 N3 65.08(14) . . ?
N4 U1 N2 177.20(14) . . ?
N1 U1 P2 83.03(9) . . ?
N1 U1 P1 97.20(9) . . ?
N3 U1 P2 98.49(9) . . ?
N3 U1 P1 83.13(9) . . ?
N3 U1 N1 172.46(12) . . ?
N2 U1 P2 146.25(10) . . ?
N2 U1 P1 32.86(10) . . ?
N2 U1 Cl2 90.02(11) . . ?
N2 U1 Cl1 91.08(11) . . ?
N2 U1 N1 64.61(13) . . ?
N2 U1 N3 114.86(13) . . ?
N4 P2 U1 48.84(13) . . ?
N4 P2 C15 107.7(2) . . ?
N4 P2 C18 108.7(2) . . ?
C15 P2 U1 130.95(19) . . ?
C15 P2 C18 105.0(2) . . ?
C18 P2 U1 122.58(18) . . ?
N2 P1 U1 47.57(13) . . ?
N2 P1 C8 105.6(3) . . ?
N2 P1 C5 107.1(2) . . ?
C8 P1 U1 120.2(2) . . ?
C5 P1 U1 131.07(17) . . ?
C5 P1 C8 106.0(3) . . ?
P2 N4 U1 97.68(17) . . ?
C14 N4 U1 130.7(3) . . ?
C14 N4 P2 131.3(3) . . ?
C1 N1 U1 115.6(3) . . ?
C1 N1 C3 107.1(4) . . ?
C1 N1 C2 108.7(4) . . ?
C3 N1 U1 106.2(3) . . ?
C2 N1 U1 108.8(3) . . ?
C2 N1 C3 110.3(4) . . ?
C12 N3 U1 108.5(3) . . ?
C12 N3 C13 110.9(4) . . ?
C12 N3 C11 108.5(4) . . ?
C13 N3 U1 107.4(3) . . ?
C13 N3 C11 107.0(4) . . ?
C11 N3 U1 114.6(3) . . ?
P1 N2 U1 99.57(18) . . ?
C4 N2 U1 131.2(3) . . ?
C4 N2 P1 129.2(3) . . ?
C16 C15 P2 109.9(4) . . ?
C16 C15 C17 110.4(5) . . ?
C17 C15 P2 111.4(4) . . ?
N2 C4 C3 106.9(4) . . ?
N4 C14 C13 105.9(4) . . ?
N1 C3 C4 110.5(4) . . ?
C20 C18 P2 116.4(4) . . ?
C20 C18 C19 113.4(5) . . ?
C19 C18 P2 110.6(4) . . ?
C9 C8 P1 116.2(4) . . ?
C10 C8 P1 111.8(5) . . ?
C10 C8 C9 114.9(6) . . ?
C7 C5 P1 111.4(4) . . ?
C6 C5 P1 110.1(4) . . ?
C6 C5 C7 110.6(5) . . ?
N3 C13 C14 110.8(4) . . ?

_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_lk-1_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2254130'
loop_
_audit_author_name
_audit_author_address
'Congqing Zhu'
;Nanjing University
China
;
_audit_update_record             
;
2023-07-25 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         'C40 H96 Cl6 Ir2 N8 P4 U2, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H100 Cl10 Ir2 N8 P4 U2'
_chemical_formula_weight         2056.13
_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'
Ir Ir -1.4442 7.9887 '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'
P P 0.1023 0.0942 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.5738(6)
_cell_length_b                   16.9717(9)
_cell_length_c                   18.2716(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.101(2)
_cell_angle_gamma                90
_cell_volume                     3568.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.475
_shelx_estimated_absorpt_T_min   0.396
_exptl_absorpt_coefficient_mu    8.738
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0973 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.6560.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic orangish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31309
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.242
_diffrn_ambient_temperature      193.00
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6958
_reflns_number_total             8174
_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 V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.547
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         8174
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.044
_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)+(0.0205P)²+14.2056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0659
_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. Restrained distances
 Cl4-C21A \\sim Cl4-C21 \\sim Cl5A-C21A \\sim Cl5-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21A \\sim Cl4 \\sim C21 \\sim Cl5 \\sim Cl5A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(Cl5A)=1-FVAR(1)
 Sof(Cl5)=Sof(C21)=Sof(H21C)=Sof(H21D)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C5(H5), C8(H8), C18(H18)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B), C4(H4A,H4B), C3(H3A,H3B), C21A(H21A,H21B),
 C21(H21C,H21D)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C), C11(H11A,H11B,
 H11C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C10(H10A,H10B,
 H10C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C2(H2A,H2B,
 H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.73328(2) 0.57822(2) 0.36863(2) 0.01815(5) Uani 1 1 d . . . . .
Ir1 Ir 0.50907(2) 0.52468(2) 0.40025(2) 0.01639(5) Uani 1 1 d . . . . .
Cl3 Cl 0.49764(12) 0.41310(7) 0.48003(7) 0.0256(3) Uani 1 1 d . . . . .
P2 P 0.54527(11) 0.45051(8) 0.30340(7) 0.0200(3) Uani 1 1 d . . . . .
P1 P 0.48513(11) 0.64749(8) 0.35159(7) 0.0204(3) Uani 1 1 d . . . . .
Cl2 Cl 0.82782(12) 0.50921(8) 0.49011(7) 0.0319(3) Uani 1 1 d . . . . .
Cl1 Cl 0.79921(13) 0.66996(9) 0.25702(8) 0.0362(3) Uani 1 1 d . . . . .
Cl4 Cl 0.4969(3) 0.58980(15) 0.06129(12) 0.0857(8) Uani 1 1 d D U . . .
N4 N 0.6718(4) 0.4838(3) 0.2805(2) 0.0220(9) Uani 1 1 d . . . . .
N2 N 0.6149(3) 0.6859(2) 0.3746(2) 0.0210(9) Uani 1 1 d . . . . .
N1 N 0.8258(4) 0.7021(3) 0.4487(2) 0.0264(10) Uani 1 1 d . . . . .
C15 C 0.3771(5) 0.7036(3) 0.3989(3) 0.0289(12) Uani 1 1 d . . . . .
H15 H 0.4127 0.7103 0.4509 0.035 Uiso 1 1 calc R U . . .
N3 N 0.9133(4) 0.4982(3) 0.3137(3) 0.0302(10) Uani 1 1 d . . . . .
C5 C 0.5684(4) 0.3428(3) 0.3193(3) 0.0261(11) Uani 1 1 d . . . . .
H5 H 0.5963 0.3228 0.2729 0.031 Uiso 1 1 calc R U . . .
C8 C 0.4338(4) 0.4527(3) 0.2223(3) 0.0267(12) Uani 1 1 d . . . . .
H8 H 0.4374 0.5070 0.2015 0.032 Uiso 1 1 calc R U . . .
C18 C 0.4500(5) 0.6619(3) 0.2509(3) 0.0297(12) Uani 1 1 d . . . . .
H18 H 0.4946 0.6202 0.2273 0.036 Uiso 1 1 calc R U . . .
Cl5 Cl 0.7389(5) 0.5605(6) 0.0456(2) 0.158(3) Uani 0.758(10) 1 d D U P A 1
C16 C 0.2631(5) 0.6586(4) 0.4039(4) 0.0400(15) Uani 1 1 d . . . . .
H16A H 0.2183 0.6573 0.3553 0.060 Uiso 1 1 calc R U . . .
H16B H 0.2177 0.6851 0.4389 0.060 Uiso 1 1 calc R U . . .
H16C H 0.2806 0.6046 0.4206 0.060 Uiso 1 1 calc R U . . .
C12 C 0.7923(5) 0.7010(4) 0.5247(3) 0.0356(14) Uani 1 1 d . . . . .
H12A H 0.7078 0.6956 0.5232 0.053 Uiso 1 1 calc R U . . .
H12B H 0.8170 0.7502 0.5497 0.053 Uiso 1 1 calc R U . . .
H12C H 0.8300 0.6563 0.5516 0.053 Uiso 1 1 calc R U . . .
C7 C 0.6690(5) 0.3251(3) 0.3799(3) 0.0323(13) Uani 1 1 d . . . . .
H7A H 0.7075 0.3745 0.3961 0.049 Uiso 1 1 calc R U . . .
H7B H 0.7253 0.2900 0.3601 0.049 Uiso 1 1 calc R U . . .
H7C H 0.6380 0.2997 0.4218 0.049 Uiso 1 1 calc R U . . .
C11 C 0.9528(5) 0.7026(4) 0.4513(4) 0.0424(16) Uani 1 1 d . . . . .
H11A H 0.9841 0.6538 0.4743 0.064 Uiso 1 1 calc R U . . .
H11B H 0.9840 0.7479 0.4802 0.064 Uiso 1 1 calc R U . . .
H11C H 0.9752 0.7064 0.4012 0.064 Uiso 1 1 calc R U . . .
C9 C 0.3099(5) 0.4442(4) 0.2454(4) 0.0383(15) Uani 1 1 d . . . . .
H9A H 0.2531 0.4616 0.2051 0.057 Uiso 1 1 calc R U . . .
H9B H 0.3026 0.4766 0.2891 0.057 Uiso 1 1 calc R U . . .
H9C H 0.2953 0.3888 0.2568 0.057 Uiso 1 1 calc R U . . .
C6 C 0.4615(6) 0.2931(4) 0.3296(4) 0.0401(15) Uani 1 1 d . . . . .
H6A H 0.4179 0.3178 0.3666 0.060 Uiso 1 1 calc R U . . .
H6B H 0.4860 0.2402 0.3460 0.060 Uiso 1 1 calc R U . . .
H6C H 0.4121 0.2896 0.2827 0.060 Uiso 1 1 calc R U . . .
C14 C 0.6444(5) 0.7674(3) 0.3943(3) 0.0334(13) Uani 1 1 d . . . . .
H14A H 0.6070 0.7830 0.4384 0.040 Uiso 1 1 calc R U . . .
H14B H 0.6164 0.8031 0.3534 0.040 Uiso 1 1 calc R U . . .
C13 C 0.7760(5) 0.7732(3) 0.4101(3) 0.0305(12) Uani 1 1 d . . . . .
H13A H 0.8105 0.7798 0.3632 0.037 Uiso 1 1 calc R U . . .
H13B H 0.7962 0.8203 0.4409 0.037 Uiso 1 1 calc R U . . .
C20 C 0.4932(6) 0.7404(4) 0.2222(3) 0.0390(15) Uani 1 1 d . . . . .
H20A H 0.4822 0.7406 0.1683 0.059 Uiso 1 1 calc R U . . .
H20B H 0.5759 0.7469 0.2391 0.059 Uiso 1 1 calc R U . . .
H20C H 0.4491 0.7839 0.2410 0.059 Uiso 1 1 calc R U . . .
C10 C 0.4546(5) 0.3966(4) 0.1588(3) 0.0384(14) Uani 1 1 d . . . . .
H10A H 0.4438 0.3420 0.1742 0.058 Uiso 1 1 calc R U . . .
H10B H 0.5341 0.4035 0.1459 0.058 Uiso 1 1 calc R U . . .
H10C H 0.3993 0.4086 0.1159 0.058 Uiso 1 1 calc R U . . .
C19 C 0.3224(5) 0.6477(4) 0.2223(4) 0.0430(16) Uani 1 1 d . . . . .
H19A H 0.2759 0.6935 0.2339 0.064 Uiso 1 1 calc R U . . .
H19B H 0.2941 0.6007 0.2460 0.064 Uiso 1 1 calc R U . . .
H19C H 0.3155 0.6399 0.1689 0.064 Uiso 1 1 calc R U . . .
C4 C 0.7468(5) 0.4398(3) 0.2348(3) 0.0298(12) Uani 1 1 d . . . . .
H4A H 0.7102 0.4378 0.1833 0.036 Uiso 1 1 calc R U . . .
H4B H 0.7567 0.3851 0.2532 0.036 Uiso 1 1 calc R U . . .
C1 C 0.9487(5) 0.4255(4) 0.3543(4) 0.0379(14) Uani 1 1 d . . . . .
H1A H 0.9823 0.4390 0.4042 0.057 Uiso 1 1 calc R U . . .
H1B H 1.0067 0.3975 0.3287 0.057 Uiso 1 1 calc R U . . .
H1C H 0.8807 0.3916 0.3569 0.057 Uiso 1 1 calc R U . . .
C3 C 0.8656(5) 0.4799(4) 0.2373(3) 0.0322(13) Uani 1 1 d . . . . .
H3A H 0.9202 0.4449 0.2146 0.039 Uiso 1 1 calc R U . . .
H3B H 0.8579 0.5293 0.2083 0.039 Uiso 1 1 calc R U . . .
C17 C 0.3505(5) 0.7872(3) 0.3700(4) 0.0390(15) Uani 1 1 d . . . . .
H17A H 0.4233 0.8165 0.3690 0.059 Uiso 1 1 calc R U . . .
H17B H 0.3010 0.8142 0.4024 0.059 Uiso 1 1 calc R U . . .
H17C H 0.3101 0.7843 0.3201 0.059 Uiso 1 1 calc R U . . .
C2 C 1.0197(5) 0.5464(4) 0.3127(4) 0.0433(16) Uani 1 1 d . . . . .
H2A H 1.0007 0.5955 0.2859 0.065 Uiso 1 1 calc R U . . .
H2B H 1.0774 0.5169 0.2881 0.065 Uiso 1 1 calc R U . . .
H2C H 1.0515 0.5585 0.3633 0.065 Uiso 1 1 calc R U . . .
C21A C 0.6371(16) 0.584(4) 0.100(2) 0.106(4) Uani 0.242(10) 1 d D U P A 2
H21A H 0.6632 0.5285 0.1043 0.127 Uiso 0.242(10) 1 calc R U P A 2
H21B H 0.6462 0.6086 0.1493 0.127 Uiso 0.242(10) 1 calc R U P A 2
Cl5A Cl 0.7137(18) 0.6350(14) 0.0397(7) 0.133(5) Uani 0.242(10) 1 d D U P A 2
C21 C 0.6381(9) 0.6109(12) 0.0909(9) 0.108(3) Uani 0.758(10) 1 d D U P A 1
H21C H 0.6520 0.5987 0.1441 0.130 Uiso 0.758(10) 1 calc R U P A 1
H21D H 0.6506 0.6682 0.0850 0.130 Uiso 0.758(10) 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Ir1 2.8656(3) . ?
U1 Cl2 2.6419(13) . ?
U1 Cl1 2.7378(14) . ?
U1 N4 2.329(4) . ?
U1 N2 2.293(4) . ?
U1 N1 2.715(4) . ?
U1 N3 2.763(5) . ?
Ir1 Cl3 2.4019(12) . ?
Ir1 Cl3 2.4377(12) 3_666 ?
Ir1 P2 2.2471(13) . ?
Ir1 P1 2.2714(13) . ?
Cl3 Ir1 2.4375(12) 3_666 ?
P2 N4 1.664(4) . ?
P2 C5 1.865(6) . ?
P2 C8 1.859(5) . ?
P1 N2 1.650(4) . ?
P1 C15 1.857(6) . ?
P1 C18 1.858(5) . ?
Cl4 C21A 1.702(18) . ?
Cl4 C21 1.704(12) . ?
N4 C4 1.472(6) . ?
N2 C14 1.461(7) . ?
N1 C12 1.482(7) . ?
N1 C11 1.466(7) . ?
N1 C13 1.483(7) . ?
C15 H15 1.0000 . ?
C15 C16 1.536(7) . ?
C15 C17 1.533(7) . ?
N3 C1 1.475(8) . ?
N3 C3 1.479(7) . ?
N3 C2 1.480(7) . ?
C5 H5 1.0000 . ?
C5 C7 1.548(7) . ?
C5 C6 1.525(7) . ?
C8 H8 1.0000 . ?
C8 C9 1.544(8) . ?
C8 C10 1.539(7) . ?
C18 H18 1.0000 . ?
C18 C20 1.535(8) . ?
C18 C19 1.532(8) . ?
Cl5 C21 1.728(14) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.524(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.531(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C21A Cl5A 1.719(18) . ?
C21 H21C 0.9900 . ?
C21 H21D 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
Cl2 U1 Ir1 89.60(3) . . ?
Cl2 U1 Cl1 138.99(5) . . ?
Cl2 U1 N1 77.67(10) . . ?
Cl2 U1 N3 79.98(11) . . ?
Cl1 U1 Ir1 131.34(3) . . ?
Cl1 U1 N3 74.25(11) . . ?
N4 U1 Ir1 72.81(10) . . ?
N4 U1 Cl2 110.18(11) . . ?
N4 U1 Cl1 87.99(11) . . ?
N4 U1 N1 168.29(14) . . ?
N4 U1 N3 66.29(14) . . ?
N2 U1 Ir1 71.62(10) . . ?
N2 U1 Cl2 120.64(11) . . ?
N2 U1 Cl1 78.31(11) . . ?
N2 U1 N4 116.14(15) . . ?
N2 U1 N1 63.95(14) . . ?
N2 U1 N3 152.38(15) . . ?
N1 U1 Ir1 116.78(10) . . ?
N1 U1 Cl1 80.54(10) . . ?
N1 U1 N3 107.86(13) . . ?
N3 U1 Ir1 130.64(10) . . ?
Cl3 Ir1 U1 99.18(3) 3_666 . ?
Cl3 Ir1 U1 118.80(3) . . ?
Cl3 Ir1 Cl3 77.75(4) . 3_666 ?
P2 Ir1 U1 76.72(3) . . ?
P2 Ir1 Cl3 93.62(4) . . ?
P2 Ir1 Cl3 167.36(5) . 3_666 ?
P2 Ir1 P1 103.35(5) . . ?
P1 Ir1 U1 72.87(3) . . ?
P1 Ir1 Cl3 86.54(4) . 3_666 ?
P1 Ir1 Cl3 161.57(5) . . ?
Ir1 Cl3 Ir1 102.25(4) . 3_666 ?
N4 P2 Ir1 104.50(15) . . ?
N4 P2 C5 104.9(2) . . ?
N4 P2 C8 110.3(2) . . ?
C5 P2 Ir1 117.48(18) . . ?
C8 P2 Ir1 116.43(18) . . ?
C8 P2 C5 102.7(2) . . ?
N2 P1 Ir1 101.13(15) . . ?
N2 P1 C15 108.6(2) . . ?
N2 P1 C18 107.3(2) . . ?
C15 P1 Ir1 110.42(17) . . ?
C15 P1 C18 107.8(3) . . ?
C18 P1 Ir1 120.87(19) . . ?
P2 N4 U1 105.80(19) . . ?
C4 N4 U1 125.9(3) . . ?
C4 N4 P2 124.0(4) . . ?
P1 N2 U1 101.85(19) . . ?
C14 N2 U1 129.9(3) . . ?
C14 N2 P1 128.3(4) . . ?
C12 N1 U1 111.6(3) . . ?
C12 N1 C13 109.2(4) . . ?
C11 N1 U1 111.0(3) . . ?
C11 N1 C12 109.3(5) . . ?
C11 N1 C13 110.4(4) . . ?
C13 N1 U1 105.3(3) . . ?
P1 C15 H15 105.7 . . ?
C16 C15 P1 113.4(4) . . ?
C16 C15 H15 105.7 . . ?
C17 C15 P1 115.8(4) . . ?
C17 C15 H15 105.7 . . ?
C17 C15 C16 109.8(5) . . ?
C1 N3 U1 114.1(3) . . ?
C1 N3 C3 110.8(5) . . ?
C1 N3 C2 106.4(5) . . ?
C3 N3 U1 103.0(3) . . ?
C3 N3 C2 109.3(5) . . ?
C2 N3 U1 113.2(4) . . ?
P2 C5 H5 104.8 . . ?
C7 C5 P2 112.7(4) . . ?
C7 C5 H5 104.8 . . ?
C6 C5 P2 117.1(4) . . ?
C6 C5 H5 104.8 . . ?
C6 C5 C7 111.3(5) . . ?
P2 C8 H8 105.5 . . ?
C9 C8 P2 111.5(4) . . ?
C9 C8 H8 105.5 . . ?
C10 C8 P2 115.9(4) . . ?
C10 C8 H8 105.5 . . ?
C10 C8 C9 111.9(5) . . ?
P1 C18 H18 105.4 . . ?
C20 C18 P1 114.0(4) . . ?
C20 C18 H18 105.4 . . ?
C19 C18 P1 114.7(4) . . ?
C19 C18 H18 105.4 . . ?
C19 C18 C20 110.9(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C14 H14A 110.1 . . ?
N2 C14 H14B 110.1 . . ?
N2 C14 C13 108.1(5) . . ?
H14A C14 H14B 108.4 . . ?
C13 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
N1 C13 C14 111.5(4) . . ?
N1 C13 H13A 109.3 . . ?
N1 C13 H13B 109.3 . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C4 H4A 109.7 . . ?
N4 C4 H4B 109.7 . . ?
N4 C4 C3 109.8(4) . . ?
H4A C4 H4B 108.2 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
N3 C1 H1A 109.5 . . ?
N3 C1 H1B 109.5 . . ?
N3 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N3 C3 C4 111.4(4) . . ?
N3 C3 H3A 109.3 . . ?
N3 C3 H3B 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C2 H2A 109.5 . . ?
N3 C2 H2B 109.5 . . ?
N3 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Cl4 C21A H21A 111.0 . . ?
Cl4 C21A H21B 111.0 . . ?
Cl4 C21A Cl5A 103.8(16) . . ?
H21A C21A H21B 109.0 . . ?
Cl5A C21A H21A 111.0 . . ?
Cl5A C21A H21B 111.0 . . ?
Cl4 C21 Cl5 114.7(10) . . ?
Cl4 C21 H21C 108.6 . . ?
Cl4 C21 H21D 108.6 . . ?
Cl5 C21 H21C 108.6 . . ?
Cl5 C21 H21D 108.6 . . ?
H21C C21 H21D 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N4 C4 C3 -15.7(6) . . . . ?
U1 N2 C14 C13 1.6(7) . . . . ?
U1 N1 C13 C14 49.9(5) . . . . ?
U1 N3 C3 C4 -51.7(5) . . . . ?
Ir1 P2 N4 U1 4.0(2) . . . . ?
Ir1 P2 N4 C4 161.7(4) . . . . ?
Ir1 P2 C5 C7 -57.2(4) . . . . ?
Ir1 P2 C5 C6 73.9(4) . . . . ?
Ir1 P2 C8 C9 -45.7(5) . . . . ?
Ir1 P2 C8 C10 -175.2(4) . . . . ?
Ir1 P1 N2 U1 33.49(17) . . . . ?
Ir1 P1 N2 C14 -145.8(4) . . . . ?
Ir1 P1 C15 C16 -50.4(4) . . . . ?
Ir1 P1 C15 C17 -178.5(4) . . . . ?
Ir1 P1 C18 C20 -151.8(4) . . . . ?
Ir1 P1 C18 C19 78.8(5) . . . . ?
P2 N4 C4 C3 -168.9(4) . . . . ?
P1 N2 C14 C13 -179.4(4) . . . . ?
N4 P2 C5 C7 58.3(4) . . . . ?
N4 P2 C5 C6 -170.6(4) . . . . ?
N4 P2 C8 C9 -164.5(4) . . . . ?
N4 P2 C8 C10 65.9(5) . . . . ?
N4 C4 C3 N3 48.3(6) . . . . ?
N2 P1 C15 C16 -160.4(4) . . . . ?
N2 P1 C15 C17 71.4(5) . . . . ?
N2 P1 C18 C20 -36.8(5) . . . . ?
N2 P1 C18 C19 -166.3(4) . . . . ?
N2 C14 C13 N1 -37.8(6) . . . . ?
C15 P1 N2 U1 149.7(2) . . . . ?
C15 P1 N2 C14 -29.6(5) . . . . ?
C15 P1 C18 C20 79.9(5) . . . . ?
C15 P1 C18 C19 -49.5(5) . . . . ?
C5 P2 N4 U1 -120.2(2) . . . . ?
C5 P2 N4 C4 37.5(5) . . . . ?
C5 P2 C8 C9 84.1(4) . . . . ?
C5 P2 C8 C10 -45.4(5) . . . . ?
C8 P2 N4 U1 129.9(2) . . . . ?
C8 P2 N4 C4 -72.4(5) . . . . ?
C8 P2 C5 C7 173.6(4) . . . . ?
C8 P2 C5 C6 -55.2(5) . . . . ?
C18 P1 N2 U1 -94.0(2) . . . . ?
C18 P1 N2 C14 86.7(5) . . . . ?
C18 P1 C15 C16 83.6(5) . . . . ?
C18 P1 C15 C17 -44.5(5) . . . . ?
C12 N1 C13 C14 -70.0(6) . . . . ?
C11 N1 C13 C14 169.8(5) . . . . ?
C1 N3 C3 C4 70.8(6) . . . . ?
C2 N3 C3 C4 -172.3(5) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 46 electrons were 
found in a volume of 386Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[CH2Cl2] per Formula Unit 
which account for 42 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.000 192.8 23.3 '0.5 CH2Cl2'
2 0.500 0.000 0.500 192.8 23.3 '0.5 CH2Cl2'

_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_lk2023070602_0m
_database_code_depnum_ccdc_archive 'CCDC 2254132'
loop_
_audit_author_name
_audit_author_address
'Congqing Zhu'
;Nanjing University
China
;
_audit_update_record             
;
2023-07-25 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H56 N4 P2 U'
_chemical_formula_sum            'C32 H56 N4 P2 U'
_chemical_formula_weight         796.77
_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 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -3.9641 10.8496 '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                   11.1259(5)
_cell_length_b                   26.0312(11)
_cell_length_c                   12.8003(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.612(2)
_cell_angle_gamma                90
_cell_volume                     3492.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      53.818
_cell_measurement_theta_min      2.954
_shelx_estimated_absorpt_T_max   0.419
_shelx_estimated_absorpt_T_min   0.342
_exptl_absorpt_coefficient_mu    10.517
_exptl_absorpt_correction_T_max  0.3012
_exptl_absorpt_correction_T_min  0.1386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1505 before and 0.0799 after correction.
The Ratio of minimum to maximum transmission is 0.4602.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39278
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.932
_diffrn_reflns_theta_min         2.954
_diffrn_ambient_temperature      193.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4383
_reflns_number_total             6363
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         5.430
_refine_diff_density_min         -4.535
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6363
_refine_ls_number_restraints     1116
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0952
_refine_ls_restrained_S_all      1.036
_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)+123.8669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1996
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 P1B-C17B \\sim P1B-C17A
 with sigma of 0.02
 C17B-C18B \\sim C17A-C18A
 with sigma of 0.02
 C17B-C19B \\sim C17A-C19A
 with sigma of 0.02
 P2B-C30B \\sim P2B-C30A
 with sigma of 0.02
 C30B-C31B \\sim C30A-C31A
 with sigma of 0.02
 C30B-C32B \\sim C30A-C32A
 with sigma of 0.02
 P2B-C27B \\sim P2B-C27A
 with sigma of 0.02
 C27B-C28B \\sim C27A-C28A
 with sigma of 0.02
 C27B-C29B \\sim C27A-C29A
 with sigma of 0.02
 P1B-C20B \\sim P1B-C20A
 with sigma of 0.02
 C20B-C22B \\sim C20A-C22A
 with sigma of 0.02
 C20B-C21B \\sim C20A-C21A
 with sigma of 0.02
 P1B-N2A \\sim P1A-N2A
 with sigma of 0.02
 P1B-C17B \\sim P1A-C17B
 with sigma of 0.02
 P1B-C17A \\sim P1A-C17A
 with sigma of 0.02
 P1B-C20B \\sim P1A-C20B
 with sigma of 0.02
 P1B-C20A \\sim P1A-C20A
 with sigma of 0.02
 P2B-N3 \\sim P2A-N3
 with sigma of 0.02
 P2B-C27B \\sim P2A-C27B
 with sigma of 0.02
 P2B-C30B \\sim P2A-C30B
 with sigma of 0.02
 P2B-C30A \\sim P2A-C30A
 with sigma of 0.02
 P2B-C27A \\sim P2A-C27A
 with sigma of 0.02
 P2B-N3 \\sim P2B-N3A
 with sigma of 0.02
 N3-C26 \\sim N3A-C26
 with sigma of 0.02
 N3-P2A \\sim N3A-P2A
 with sigma of 0.02
 U1-N2A \\sim U1-N2B
 with sigma of 0.02
 P1B-N2A \\sim P1B-N2B
 with sigma of 0.02
 N2A-C16 \\sim N2B-C16
 with sigma of 0.02
 N2A-P1A \\sim N2B-P1A
 with sigma of 0.02
2. Rigid bond restraints
 N3, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17B \\sim C18B \\sim C19B \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27B
\\sim C28B \\sim C29B \\sim C30B \\sim C31B \\sim C32B \\sim C17A \\sim C18A
\\sim C19A \\sim C30A \\sim C31A \\sim C32A \\sim C28A \\sim C27A \\sim C29A
\\sim C20B \\sim C22B \\sim C21B \\sim C20A \\sim C22A \\sim C21A: within 3.8A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 3.8A
P1B \\sim P1A \\sim N2A \\sim N2B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(N3A) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(P2B) \\sim Ueq, Uanis(P2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(P1B)=Sof(P2B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(H26C)=
 Sof(H26D)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C29B)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30B)=Sof(H30B)=Sof(C31B)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32B)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C20B)=Sof(H20B)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C21B)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(N3A)=Sof(N2B)=1-FVAR(1)
 Sof(N2A)=Sof(N3)=Sof(H16A)=Sof(H16B)=Sof(H26A)=Sof(H26B)=Sof(C17A)=Sof(H17A)=
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C20A)=Sof(H20A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C21A)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(P1A)=Sof(P2A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C17B(H17B), C27B(H27B), C30B(H30B), C17A(H17A), C30A(H30A), C27A(H27A),
 C20B(H20B), C20A(H20A)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C16(H16C,H16D), C25(H25A,H25B), C26(H26A,
 H26B), C26(H26C,H26D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C18B(H18A,H18B,H18C), C19B(H19A,
 H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C28B(H28A,H28B,H28C),
 C29B(H29A,H29B,H29C), C31B(H31A,H31B,H31C), C32B(H32A,H32B,H32C), C18A(H18D,
 H18E,H18F), C19A(H19D,H19E,H19F), C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F),
 C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F), C22B(H22A,H22B,H22C), C21B(H21A,
 H21B,H21C), C22A(H22D,H22E,H22F), C21A(H21D,H21E,H21F)
;
_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
U1 U 0.28298(7) 0.62281(3) 0.68037(4) 0.0587(2) Uani 1 1 d D . . . .
P1B P 0.532(4) 0.6646(11) 0.840(2) 0.066(5) Uani 0.433(13) 1 d . U P A 2
P2B P 0.1284(14) 0.5741(5) 0.8029(12) 0.037(3) Uani 0.433(13) 1 d . U P A 2
N1 N 0.162(2) 0.7130(8) 0.6897(14) 0.093(6) Uani 1 1 d . . . . .
N2A N 0.399(2) 0.6764(9) 0.816(2) 0.070(5) Uani 0.567(13) 1 d D U P A 1
N3 N 0.202(3) 0.5541(8) 0.758(2) 0.056(7) Uani 0.567(13) 1 d D U P A 1
N4 N 0.395(2) 0.5306(7) 0.6651(12) 0.085(6) Uani 1 1 d . . . . .
C1 C 0.100(2) 0.6235(9) 0.5017(16) 0.085(4) Uani 1 1 d . U . . .
C2 C -0.035(2) 0.6186(9) 0.4804(18) 0.096(4) Uani 1 1 d . U . . .
H2 H -0.065019 0.610347 0.539915 0.116 Uiso 1 1 calc R U . . .
C3 C -0.126(2) 0.6259(10) 0.372(2) 0.103(5) Uani 1 1 d . U . . .
H3 H -0.213948 0.623287 0.362192 0.124 Uiso 1 1 calc R U . . .
C4 C -0.090(3) 0.6362(10) 0.285(2) 0.104(5) Uani 1 1 d . U . . .
H4 H -0.151544 0.641923 0.214238 0.125 Uiso 1 1 calc R U . . .
C5 C 0.037(2) 0.6383(9) 0.3008(18) 0.094(4) Uani 1 1 d . U . . .
H5 H 0.063013 0.644550 0.238640 0.113 Uiso 1 1 calc R U . . .
C6 C 0.131(2) 0.6314(9) 0.4056(16) 0.085(4) Uani 1 1 d . U . . .
C7 C 0.268(2) 0.6328(8) 0.4147(16) 0.079(4) Uani 1 1 d . U . . .
C8 C 0.309(2) 0.6283(9) 0.3202(17) 0.088(4) Uani 1 1 d . U . . .
H8 H 0.248926 0.622236 0.248294 0.106 Uiso 1 1 calc R U . . .
C9 C 0.440(2) 0.6332(8) 0.3375(18) 0.085(4) Uani 1 1 d . U . . .
H9 H 0.469154 0.632066 0.275515 0.101 Uiso 1 1 calc R U . . .
C10 C 0.523(2) 0.6392(9) 0.4357(18) 0.088(4) Uani 1 1 d . U . . .
H10 H 0.610671 0.641744 0.444237 0.105 Uiso 1 1 calc R U . . .
C11 C 0.488(2) 0.6418(9) 0.5256(18) 0.087(4) Uani 1 1 d . U . . .
H11 H 0.551740 0.646778 0.595791 0.105 Uiso 1 1 calc R U . . .
C12 C 0.359(2) 0.6375(8) 0.5212(15) 0.074(4) Uani 1 1 d . U . . .
C13 C 0.021(3) 0.7152(11) 0.658(2) 0.111(7) Uani 1 1 d . U . . .
H13A H -0.018063 0.708175 0.578743 0.166 Uiso 1 1 calc R U . . .
H13B H -0.004551 0.749469 0.674642 0.166 Uiso 1 1 calc R U . . .
H13C H -0.007615 0.689434 0.700556 0.166 Uiso 1 1 calc R U . . .
C14 C 0.202(2) 0.7466(9) 0.6149(18) 0.090(6) Uani 1 1 d . U . . .
H14A H 0.295489 0.746743 0.637222 0.135 Uiso 1 1 calc R U . . .
H14B H 0.171617 0.781611 0.618866 0.135 Uiso 1 1 calc R U . . .
H14C H 0.165963 0.733848 0.538637 0.135 Uiso 1 1 calc R U . . .
C15 C 0.211(3) 0.7288(10) 0.804(2) 0.109(7) Uani 1 1 d . U . . .
H15A H 0.179504 0.705204 0.849621 0.131 Uiso 1 1 calc R U . . .
H15B H 0.180245 0.763800 0.811329 0.131 Uiso 1 1 calc R U . . .
C16 C 0.350(3) 0.7284(10) 0.844(2) 0.105(6) Uani 1 1 d D U . . .
H16A H 0.382451 0.733771 0.925094 0.126 Uiso 0.567(13) 1 calc R U P A 1
H16B H 0.382021 0.756703 0.808680 0.126 Uiso 0.567(13) 1 calc R U P A 1
H16C H 0.381416 0.726663 0.925842 0.126 Uiso 0.433(13) 1 calc R U P A 2
H16D H 0.381269 0.760872 0.821923 0.126 Uiso 0.433(13) 1 calc R U P A 2
C17B C 0.661(7) 0.708(2) 0.795(5) 0.103(7) Uani 0.433(13) 1 d D U P A 2
H17B H 0.696073 0.733568 0.855284 0.124 Uiso 0.433(13) 1 calc R U P A 2
C18B C 0.607(7) 0.735(3) 0.697(5) 0.122(11) Uani 0.433(13) 1 d D U P A 2
H18A H 0.643172 0.723483 0.641303 0.182 Uiso 0.433(13) 1 calc R U P A 2
H18B H 0.624557 0.771866 0.711483 0.182 Uiso 0.433(13) 1 calc R U P A 2
H18C H 0.514327 0.729590 0.669650 0.182 Uiso 0.433(13) 1 calc R U P A 2
C19B C 0.772(6) 0.688(2) 0.768(5) 0.113(10) Uani 0.433(13) 1 d D U P A 2
H19A H 0.833450 0.671902 0.834551 0.170 Uiso 0.433(13) 1 calc R U P A 2
H19B H 0.813679 0.715787 0.742739 0.170 Uiso 0.433(13) 1 calc R U P A 2
H19C H 0.743228 0.661599 0.709564 0.170 Uiso 0.433(13) 1 calc R U P A 2
C23 C 0.522(3) 0.5294(10) 0.652(2) 0.107(7) Uani 1 1 d . U . . .
H23A H 0.517213 0.546654 0.582963 0.160 Uiso 1 1 calc R U . . .
H23B H 0.548104 0.493634 0.649985 0.160 Uiso 1 1 calc R U . . .
H23C H 0.583429 0.547069 0.714934 0.160 Uiso 1 1 calc R U . . .
C24 C 0.302(2) 0.5067(9) 0.5669(16) 0.086(5) Uani 1 1 d . U . . .
H24A H 0.215559 0.511391 0.569515 0.128 Uiso 1 1 calc R U . . .
H24B H 0.320435 0.469979 0.565978 0.128 Uiso 1 1 calc R U . . .
H24C H 0.307929 0.522956 0.499728 0.128 Uiso 1 1 calc R U . . .
C25 C 0.401(3) 0.5017(10) 0.769(2) 0.115(7) Uani 1 1 d . U . . .
H25A H 0.463693 0.518044 0.834855 0.138 Uiso 1 1 calc R U . . .
H25B H 0.427371 0.465764 0.764713 0.138 Uiso 1 1 calc R U . . .
C26 C 0.266(3) 0.5028(9) 0.781(2) 0.101(5) Uani 1 1 d D U . . .
H26A H 0.211164 0.477362 0.729317 0.121 Uiso 0.567(13) 1 calc R U P A 1
H26B H 0.273902 0.492153 0.857338 0.121 Uiso 0.567(13) 1 calc R U P A 1
H26C H 0.198795 0.487983 0.716318 0.121 Uiso 0.433(13) 1 calc R U P A 2
H26D H 0.263910 0.486905 0.850683 0.121 Uiso 0.433(13) 1 calc R U P A 2
C27B C 0.010(6) 0.524(2) 0.756(4) 0.087(6) Uani 0.433(13) 1 d D U P A 2
H27B H 0.047824 0.494142 0.806670 0.105 Uiso 0.433(13) 1 calc R U P A 2
C28B C -0.002(6) 0.503(2) 0.641(4) 0.091(9) Uani 0.433(13) 1 d D U P A 2
H28A H -0.031702 0.530385 0.585921 0.137 Uiso 0.433(13) 1 calc R U P A 2
H28B H -0.062587 0.474341 0.621646 0.137 Uiso 0.433(13) 1 calc R U P A 2
H28C H 0.081964 0.490846 0.641533 0.137 Uiso 0.433(13) 1 calc R U P A 2
C29B C -0.115(5) 0.529(3) 0.766(5) 0.098(9) Uani 0.433(13) 1 d D U P A 2
H29A H -0.113096 0.516396 0.838773 0.147 Uiso 0.433(13) 1 calc R U P A 2
H29B H -0.177695 0.509694 0.707466 0.147 Uiso 0.433(13) 1 calc R U P A 2
H29C H -0.138954 0.565677 0.759546 0.147 Uiso 0.433(13) 1 calc R U P A 2
C30B C 0.137(5) 0.579(2) 0.950(5) 0.090(7) Uani 0.433(13) 1 d D U P A 2
H30B H 0.170974 0.613836 0.972245 0.108 Uiso 0.433(13) 1 calc R U P A 2
C31B C 0.237(6) 0.544(2) 1.028(4) 0.097(9) Uani 0.433(13) 1 d D U P A 2
H31A H 0.217900 0.507728 1.003941 0.146 Uiso 0.433(13) 1 calc R U P A 2
H31B H 0.234808 0.547483 1.103228 0.146 Uiso 0.433(13) 1 calc R U P A 2
H31C H 0.321353 0.552771 1.026036 0.146 Uiso 0.433(13) 1 calc R U P A 2
C32B C 0.010(6) 0.576(3) 0.982(5) 0.104(9) Uani 0.433(13) 1 d D U P A 2
H32A H -0.027028 0.610918 0.976018 0.156 Uiso 0.433(13) 1 calc R U P A 2
H32B H 0.030824 0.563906 1.058062 0.156 Uiso 0.433(13) 1 calc R U P A 2
H32C H -0.051830 0.553152 0.931125 0.156 Uiso 0.433(13) 1 calc R U P A 2
C17A C 0.628(5) 0.7225(19) 0.831(4) 0.106(7) Uani 0.567(13) 1 d D U P A 1
H17A H 0.602688 0.739487 0.890659 0.128 Uiso 0.567(13) 1 calc R U P A 1
C18A C 0.761(4) 0.726(2) 0.869(4) 0.121(9) Uani 0.567(13) 1 d D U P A 1
H18D H 0.794865 0.714359 0.946060 0.182 Uiso 0.567(13) 1 calc R U P A 1
H18E H 0.786654 0.761517 0.863738 0.182 Uiso 0.567(13) 1 calc R U P A 1
H18F H 0.794902 0.703937 0.822857 0.182 Uiso 0.567(13) 1 calc R U P A 1
C19A C 0.556(5) 0.751(2) 0.728(4) 0.108(9) Uani 0.567(13) 1 d D U P A 1
H19D H 0.526825 0.727304 0.665818 0.163 Uiso 0.567(13) 1 calc R U P A 1
H19E H 0.611549 0.777237 0.713052 0.163 Uiso 0.567(13) 1 calc R U P A 1
H19F H 0.481920 0.768129 0.738659 0.163 Uiso 0.567(13) 1 calc R U P A 1
C30A C 0.113(4) 0.5639(18) 0.942(3) 0.089(6) Uani 0.567(13) 1 d D U P A 1
H30A H 0.098553 0.526755 0.953526 0.107 Uiso 0.567(13) 1 calc R U P A 1
C31A C 0.245(4) 0.5844(18) 1.008(3) 0.094(8) Uani 0.567(13) 1 d D U P A 1
H31D H 0.307684 0.571269 0.976958 0.141 Uiso 0.567(13) 1 calc R U P A 1
H31E H 0.267125 0.573178 1.085595 0.141 Uiso 0.567(13) 1 calc R U P A 1
H31F H 0.243554 0.622034 1.005323 0.141 Uiso 0.567(13) 1 calc R U P A 1
C32A C 0.028(5) 0.6036(17) 0.982(4) 0.102(8) Uani 0.567(13) 1 d D U P A 1
H32D H 0.064107 0.638184 0.985654 0.152 Uiso 0.567(13) 1 calc R U P A 1
H32E H 0.027702 0.593554 1.055686 0.152 Uiso 0.567(13) 1 calc R U P A 1
H32F H -0.059257 0.603338 0.929491 0.152 Uiso 0.567(13) 1 calc R U P A 1
C28A C -0.084(5) 0.4933(16) 0.768(3) 0.096(8) Uani 0.567(13) 1 d D U P A 1
H28D H -0.005440 0.473631 0.782270 0.144 Uiso 0.567(13) 1 calc R U P A 1
H28E H -0.155972 0.473991 0.717386 0.144 Uiso 0.567(13) 1 calc R U P A 1
H28F H -0.099862 0.499092 0.838229 0.144 Uiso 0.567(13) 1 calc R U P A 1
C27A C -0.072(5) 0.5455(15) 0.715(3) 0.090(6) Uani 0.567(13) 1 d D U P A 1
H27A H -0.066671 0.537409 0.640706 0.108 Uiso 0.567(13) 1 calc R U P A 1
C29A C -0.183(4) 0.5775(17) 0.696(3) 0.098(8) Uani 0.567(13) 1 d D U P A 1
H29D H -0.203999 0.580416 0.763855 0.148 Uiso 0.567(13) 1 calc R U P A 1
H29E H -0.255232 0.562236 0.637085 0.148 Uiso 0.567(13) 1 calc R U P A 1
H29F H -0.165515 0.611784 0.672280 0.148 Uiso 0.567(13) 1 calc R U P A 1
C20B C 0.604(8) 0.649(2) 0.986(6) 0.104(7) Uani 0.433(13) 1 d D U P A 2
H20B H 0.695990 0.656087 0.997004 0.125 Uiso 0.433(13) 1 calc R U P A 2
C22B C 0.585(6) 0.684(2) 1.070(4) 0.103(10) Uani 0.433(13) 1 d D U P A 2
H22A H 0.641942 0.713636 1.079238 0.154 Uiso 0.433(13) 1 calc R U P A 2
H22B H 0.603731 0.665874 1.140323 0.154 Uiso 0.433(13) 1 calc R U P A 2
H22C H 0.496116 0.695799 1.044403 0.154 Uiso 0.433(13) 1 calc R U P A 2
C21B C 0.609(7) 0.593(2) 1.005(5) 0.108(12) Uani 0.433(13) 1 d D U P A 2
H21A H 0.523009 0.579667 0.993294 0.162 Uiso 0.433(13) 1 calc R U P A 2
H21B H 0.664216 0.585029 1.080805 0.162 Uiso 0.433(13) 1 calc R U P A 2
H21C H 0.643729 0.575850 0.952350 0.162 Uiso 0.433(13) 1 calc R U P A 2
C20A C 0.647(5) 0.646(2) 0.977(5) 0.104(7) Uani 0.567(13) 1 d D U P A 1
H20A H 0.671641 0.680550 1.012466 0.124 Uiso 0.567(13) 1 calc R U P A 1
C22A C 0.557(5) 0.621(2) 1.024(3) 0.103(10) Uani 0.567(13) 1 d D U P A 1
H22D H 0.485744 0.644643 1.016773 0.155 Uiso 0.567(13) 1 calc R U P A 1
H22E H 0.601323 0.613664 1.102516 0.155 Uiso 0.567(13) 1 calc R U P A 1
H22F H 0.525325 0.589466 0.983714 0.155 Uiso 0.567(13) 1 calc R U P A 1
C21A C 0.764(5) 0.6139(18) 0.999(4) 0.115(9) Uani 0.567(13) 1 d D U P A 1
H21D H 0.742025 0.581723 0.957820 0.173 Uiso 0.567(13) 1 calc R U P A 1
H21E H 0.799713 0.606396 1.078968 0.173 Uiso 0.567(13) 1 calc R U P A 1
H21F H 0.827298 0.632621 0.976217 0.173 Uiso 0.567(13) 1 calc R U P A 1
P1A P 0.563(2) 0.6546(8) 0.8239(19) 0.067(5) Uani 0.567(13) 1 d . U P A 1
P2A P 0.0781(13) 0.5841(6) 0.7914(10) 0.058(3) Uani 0.567(13) 1 d . U P A 1
N3A N 0.263(3) 0.5597(8) 0.784(3) 0.044(8) Uani 0.433(13) 1 d D U P A 2
N2B N 0.405(3) 0.6825(12) 0.797(3) 0.070(6) Uani 0.433(13) 1 d D U P A 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 P1B 3.03(4) . ?
U1 P2B 2.973(16) . ?
U1 N1 2.73(2) . ?
U1 N2A 2.260(17) . ?
U1 N3 2.37(2) . ?
U1 N4 2.739(18) . ?
U1 C1 2.50(2) . ?
U1 C12 2.482(17) . ?
U1 P1A 3.15(3) . ?
U1 P2A 3.226(12) . ?
U1 N3A 2.16(3) . ?
U1 N2B 2.268(19) . ?
P1B C17B 2.05(7) . ?
P1B C20B 1.83(8) . ?
P1B N2B 1.41(4) . ?
P2B C27B 1.82(5) . ?
P2B C30B 1.85(6) . ?
P2B N3A 1.64(3) . ?
N1 C13 1.49(3) . ?
N1 C14 1.47(3) . ?
N1 C15 1.44(3) . ?
N2A C16 1.54(3) . ?
N2A P1A 1.88(4) . ?
N3 C26 1.50(3) . ?
N3 P2A 1.75(3) . ?
N4 C23 1.48(3) . ?
N4 C24 1.47(3) . ?
N4 C25 1.51(3) . ?
C1 C2 1.45(3) . ?
C1 C6 1.40(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.42(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.33(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.36(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.41(3) . ?
C6 C7 1.49(3) . ?
C7 C8 1.43(3) . ?
C7 C12 1.40(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.41(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.29(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.34(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.42(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.46(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 H16C 0.9900 . ?
C16 H16D 0.9900 . ?
C16 N2B 1.55(3) . ?
C17B H17B 1.0000 . ?
C17B C18B 1.40(6) . ?
C17B C19B 1.48(6) . ?
C18B H18A 0.9800 . ?
C18B H18B 0.9800 . ?
C18B H18C 0.9800 . ?
C19B H19A 0.9800 . ?
C19B H19B 0.9800 . ?
C19B H19C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.56(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 H26C 0.9900 . ?
C26 H26D 0.9900 . ?
C26 N3A 1.48(3) . ?
C27B H27B 1.0000 . ?
C27B C28B 1.53(4) . ?
C27B C29B 1.44(5) . ?
C28B H28A 0.9800 . ?
C28B H28B 0.9800 . ?
C28B H28C 0.9800 . ?
C29B H29A 0.9800 . ?
C29B H29B 0.9800 . ?
C29B H29C 0.9800 . ?
C30B H30B 1.0000 . ?
C30B C31B 1.52(4) . ?
C30B C32B 1.60(4) . ?
C31B H31A 0.9800 . ?
C31B H31B 0.9800 . ?
C31B H31C 0.9800 . ?
C32B H32A 0.9800 . ?
C32B H32B 0.9800 . ?
C32B H32C 0.9800 . ?
C17A H17A 1.0000 . ?
C17A C18A 1.40(5) . ?
C17A C19A 1.49(5) . ?
C17A P1A 1.90(5) . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C30A H30A 1.0000 . ?
C30A C31A 1.52(4) . ?
C30A C32A 1.60(4) . ?
C30A P2A 1.90(5) . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?
C28A C27A 1.54(4) . ?
C27A H27A 1.0000 . ?
C27A C29A 1.44(5) . ?
C27A P2A 1.91(4) . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C20B H20B 1.0000 . ?
C20B C22B 1.47(5) . ?
C20B C21B 1.49(5) . ?
C22B H22A 0.9800 . ?
C22B H22B 0.9800 . ?
C22B H22C 0.9800 . ?
C21B H21A 0.9800 . ?
C21B H21B 0.9800 . ?
C21B H21C 0.9800 . ?
C20A H20A 1.0000 . ?
C20A C22A 1.47(5) . ?
C20A C21A 1.49(5) . ?
C20A P1A 1.88(6) . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 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
P2B U1 P1B 110.9(7) . . ?
N1 U1 P1B 90.7(7) . . ?
N1 U1 P2B 87.9(5) . . ?
N1 U1 N4 177.6(6) . . ?
N1 U1 P1A 98.8(6) . . ?
N1 U1 P2A 79.5(5) . . ?
N2A U1 N1 66.3(7) . . ?
N2A U1 N3 110.1(12) . . ?
N2A U1 N4 116.1(7) . . ?
N2A U1 C1 140.9(9) . . ?
N2A U1 C12 105.7(11) . . ?
N2A U1 P1A 36.1(8) . . ?
N2A U1 P2A 99.3(10) . . ?
N3 U1 N1 111.6(7) . . ?
N3 U1 N4 67.4(7) . . ?
N3 U1 C1 94.7(8) . . ?
N3 U1 C12 138.2(8) . . ?
N3 U1 P1A 113.3(8) . . ?
N3 U1 P2A 32.0(6) . . ?
N4 U1 P1B 91.7(7) . . ?
N4 U1 P2B 91.2(5) . . ?
N4 U1 P1A 83.6(5) . . ?
N4 U1 P2A 99.3(5) . . ?
C1 U1 P1B 152.9(8) . . ?
C1 U1 P2B 92.8(5) . . ?
C1 U1 N1 76.8(7) . . ?
C1 U1 N4 101.0(7) . . ?
C1 U1 P1A 150.9(7) . . ?
C1 U1 P2A 85.8(5) . . ?
C12 U1 P1B 90.7(8) . . ?
C12 U1 P2B 156.2(5) . . ?
C12 U1 N1 102.2(6) . . ?
C12 U1 N4 77.8(6) . . ?
C12 U1 C1 69.1(7) . . ?
C12 U1 P1A 84.1(7) . . ?
C12 U1 P2A 153.5(5) . . ?
P1A U1 P2A 122.1(5) . . ?
N3A U1 P1B 96.8(11) . . ?
N3A U1 P2B 32.8(9) . . ?
N3A U1 N1 118.3(8) . . ?
N3A U1 N4 61.3(8) . . ?
N3A U1 C1 110.3(10) . . ?
N3A U1 C12 138.6(9) . . ?
N3A U1 N2B 106.1(15) . . ?
N2B U1 P1B 26.0(8) . . ?
N2B U1 P2B 105.6(12) . . ?
N2B U1 N1 64.9(8) . . ?
N2B U1 N4 117.5(8) . . ?
N2B U1 C1 136.3(11) . . ?
N2B U1 C12 98.2(13) . . ?
C17B P1B U1 125(2) . . ?
C20B P1B U1 127(3) . . ?
C20B P1B C17B 107(4) . . ?
N2B P1B U1 45.0(12) . . ?
N2B P1B C17B 115(3) . . ?
N2B P1B C20B 121(4) . . ?
C27B P2B U1 128.3(14) . . ?
C27B P2B C30B 99(2) . . ?
C30B P2B U1 132(2) . . ?
N3A P2B U1 45.4(10) . . ?
N3A P2B C27B 113(2) . . ?
N3A P2B C30B 115(2) . . ?
C13 N1 U1 120.9(16) . . ?
C14 N1 U1 102.9(14) . . ?
C14 N1 C13 108.8(19) . . ?
C15 N1 U1 105.5(15) . . ?
C15 N1 C13 106(2) . . ?
C15 N1 C14 113(2) . . ?
C16 N2A U1 124.4(16) . . ?
C16 N2A P1A 131(2) . . ?
P1A N2A U1 98.6(11) . . ?
C26 N3 U1 121.9(17) . . ?
C26 N3 P2A 136(2) . . ?
P2A N3 U1 102.0(10) . . ?
C23 N4 U1 120.1(14) . . ?
C23 N4 C25 109(2) . . ?
C24 N4 U1 103.1(14) . . ?
C24 N4 C23 108.5(17) . . ?
C24 N4 C25 110.8(19) . . ?
C25 N4 U1 105.0(14) . . ?
C2 C1 U1 130.4(15) . . ?
C6 C1 U1 116.4(16) . . ?
C6 C1 C2 113(2) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121(2) . . ?
C3 C2 H2 119.3 . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122(3) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 120.9 . . ?
C3 C4 C5 118(2) . . ?
C5 C4 H4 120.9 . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122(2) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C5 123(2) . . ?
C1 C6 C7 118.6(19) . . ?
C5 C6 C7 118.9(19) . . ?
C8 C7 C6 122.5(19) . . ?
C12 C7 C6 117.6(17) . . ?
C12 C7 C8 120(2) . . ?
C7 C8 H8 121.1 . . ?
C9 C8 C7 118(2) . . ?
C9 C8 H8 121.1 . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121(2) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 122(2) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 H11 118.5 . . ?
C10 C11 C12 123(2) . . ?
C12 C11 H11 118.5 . . ?
C7 C12 U1 116.8(13) . . ?
C7 C12 C11 115.8(17) . . ?
C11 C12 U1 126.6(14) . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.6 . . ?
N1 C15 H15B 109.6 . . ?
N1 C15 C16 110(2) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
N2A C16 H16A 109.7 . . ?
N2A C16 H16B 109.7 . . ?
C15 C16 N2A 110(2) . . ?
C15 C16 H16A 109.7 . . ?
C15 C16 H16B 109.7 . . ?
C15 C16 H16C 109.1 . . ?
C15 C16 H16D 109.1 . . ?
C15 C16 N2B 112(2) . . ?
H16A C16 H16B 108.2 . . ?
H16C C16 H16D 107.8 . . ?
N2B C16 H16C 109.1 . . ?
N2B C16 H16D 109.1 . . ?
P1B C17B H17B 106.3 . . ?
C18B C17B P1B 113(5) . . ?
C18B C17B H17B 106.3 . . ?
C18B C17B C19B 97(6) . . ?
C19B C17B P1B 126(5) . . ?
C19B C17B H17B 106.3 . . ?
C17B C18B H18A 109.5 . . ?
C17B C18B H18B 109.5 . . ?
C17B C18B H18C 109.5 . . ?
H18A C18B H18B 109.5 . . ?
H18A C18B H18C 109.5 . . ?
H18B C18B H18C 109.5 . . ?
C17B C19B H19A 109.5 . . ?
C17B C19B H19B 109.5 . . ?
C17B C19B H19C 109.5 . . ?
H19A C19B H19B 109.5 . . ?
H19A C19B H19C 109.5 . . ?
H19B C19B H19C 109.5 . . ?
N4 C23 H23A 109.5 . . ?
N4 C23 H23B 109.5 . . ?
N4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 H24A 109.5 . . ?
N4 C24 H24B 109.5 . . ?
N4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N4 C25 H25A 110.0 . . ?
N4 C25 H25B 110.0 . . ?
N4 C25 C26 108(2) . . ?
H25A C25 H25B 108.4 . . ?
C26 C25 H25A 110.0 . . ?
C26 C25 H25B 110.0 . . ?
N3 C26 C25 114(2) . . ?
N3 C26 H26A 108.7 . . ?
N3 C26 H26B 108.7 . . ?
C25 C26 H26A 108.7 . . ?
C25 C26 H26B 108.7 . . ?
C25 C26 H26C 113.2 . . ?
C25 C26 H26D 113.2 . . ?
H26A C26 H26B 107.6 . . ?
H26C C26 H26D 110.5 . . ?
N3A C26 C25 93(2) . . ?
N3A C26 H26C 113.2 . . ?
N3A C26 H26D 113.2 . . ?
P2B C27B H27B 103.6 . . ?
C28B C27B P2B 113(3) . . ?
C28B C27B H27B 103.6 . . ?
C29B C27B P2B 121(5) . . ?
C29B C27B H27B 103.6 . . ?
C29B C27B C28B 111(5) . . ?
C27B C28B H28A 109.5 . . ?
C27B C28B H28B 109.5 . . ?
C27B C28B H28C 109.5 . . ?
H28A C28B H28B 109.5 . . ?
H28A C28B H28C 109.5 . . ?
H28B C28B H28C 109.5 . . ?
C27B C29B H29A 109.5 . . ?
C27B C29B H29B 109.5 . . ?
C27B C29B H29C 109.5 . . ?
H29A C29B H29B 109.5 . . ?
H29A C29B H29C 109.5 . . ?
H29B C29B H29C 109.5 . . ?
P2B C30B H30B 103.8 . . ?
C31B C30B P2B 114(4) . . ?
C31B C30B H30B 103.8 . . ?
C31B C30B C32B 109(5) . . ?
C32B C30B P2B 121(4) . . ?
C32B C30B H30B 103.8 . . ?
C30B C31B H31A 109.5 . . ?
C30B C31B H31B 109.5 . . ?
C30B C31B H31C 109.5 . . ?
H31A C31B H31B 109.5 . . ?
H31A C31B H31C 109.5 . . ?
H31B C31B H31C 109.5 . . ?
C30B C32B H32A 109.5 . . ?
C30B C32B H32B 109.5 . . ?
C30B C32B H32C 109.5 . . ?
H32A C32B H32B 109.5 . . ?
H32A C32B H32C 109.5 . . ?
H32B C32B H32C 109.5 . . ?
C18A C17A H17A 104.2 . . ?
C18A C17A C19A 118(4) . . ?
C18A C17A P1A 115(4) . . ?
C19A C17A H17A 104.2 . . ?
C19A C17A P1A 110(3) . . ?
P1A C17A H17A 104.2 . . ?
C17A C18A H18D 109.5 . . ?
C17A C18A H18E 109.5 . . ?
C17A C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C17A C19A H19D 109.5 . . ?
C17A C19A H19E 109.5 . . ?
C17A C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C31A C30A H30A 115.5 . . ?
C31A C30A C32A 99(4) . . ?
C31A C30A P2A 108(3) . . ?
C32A C30A H30A 115.5 . . ?
C32A C30A P2A 102(3) . . ?
P2A C30A H30A 115.5 . . ?
C30A C31A H31D 109.5 . . ?
C30A C31A H31E 109.5 . . ?
C30A C31A H31F 109.5 . . ?
H31D C31A H31E 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C30A C32A H32D 109.5 . . ?
C30A C32A H32E 109.5 . . ?
C30A C32A H32F 109.5 . . ?
H32D C32A H32E 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C27A C28A H28D 109.5 . . ?
C27A C28A H28E 109.5 . . ?
C27A C28A H28F 109.5 . . ?
C28A C27A H27A 106.0 . . ?
C28A C27A P2A 116(3) . . ?
C29A C27A C28A 113(4) . . ?
C29A C27A H27A 106.0 . . ?
C29A C27A P2A 110(3) . . ?
P2A C27A H27A 106.0 . . ?
C27A C29A H29D 109.5 . . ?
C27A C29A H29E 109.5 . . ?
C27A C29A H29F 109.5 . . ?
H29D C29A H29E 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
P1B C20B H20B 100.3 . . ?
C22B C20B P1B 119(4) . . ?
C22B C20B H20B 100.3 . . ?
C22B C20B C21B 120(6) . . ?
C21B C20B P1B 111(5) . . ?
C21B C20B H20B 100.3 . . ?
C20B C22B H22A 109.5 . . ?
C20B C22B H22B 109.5 . . ?
C20B C22B H22C 109.5 . . ?
H22A C22B H22B 109.5 . . ?
H22A C22B H22C 109.5 . . ?
H22B C22B H22C 109.5 . . ?
C20B C21B H21A 109.5 . . ?
C20B C21B H21B 109.5 . . ?
C20B C21B H21C 109.5 . . ?
H21A C21B H21B 109.5 . . ?
H21A C21B H21C 109.5 . . ?
H21B C21B H21C 109.5 . . ?
C22A C20A H20A 109.2 . . ?
C22A C20A C21A 110(4) . . ?
C22A C20A P1A 108(4) . . ?
C21A C20A H20A 109.2 . . ?
C21A C20A P1A 111(3) . . ?
P1A C20A H20A 109.2 . . ?
C20A C22A H22D 109.5 . . ?
C20A C22A H22E 109.5 . . ?
C20A C22A H22F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C20A C21A H21D 109.5 . . ?
C20A C21A H21E 109.5 . . ?
C20A C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
N2A P1A U1 45.2(8) . . ?
N2A P1A C17A 94(2) . . ?
N2A P1A C20A 103(2) . . ?
C17A P1A U1 124.0(18) . . ?
C20A P1A U1 129(2) . . ?
C20A P1A C17A 91(2) . . ?
N3 P2A U1 46.0(8) . . ?
N3 P2A C30A 102.1(17) . . ?
N3 P2A C27A 105.4(18) . . ?
C30A P2A U1 126.5(13) . . ?
C30A P2A C27A 102.6(18) . . ?
C27A P2A U1 124.4(13) . . ?
P2B N3A U1 101.8(14) . . ?
C26 N3A U1 138(2) . . ?
C26 N3A P2B 105(2) . . ?
P1B N2B U1 109.1(15) . . ?
P1B N2B C16 126(2) . . ?
C16 N2B U1 123.7(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 P1B C20B C22B -98(6) . . . . ?
U1 P1B C20B C21B 49(6) . . . . ?
U1 P1B N2B C16 166(6) . . . . ?
U1 P2B C27B C28B 4(6) . . . . ?
U1 P2B C27B C29B -130(4) . . . . ?
U1 P2B C30B C31B -82(5) . . . . ?
U1 P2B C30B C32B 145(4) . . . . ?
U1 P2B N3A C26 -147(3) . . . . ?
U1 N1 C15 C16 51(2) . . . . ?
U1 N2A C16 C15 22(4) . . . . ?
U1 N2A P1A C17A 136.1(19) . . . . ?
U1 N2A P1A C20A -132(2) . . . . ?
U1 N3 C26 C25 10(3) . . . . ?
U1 N3 P2A C30A -129.8(16) . . . . ?
U1 N3 P2A C27A 123.4(15) . . . . ?
U1 N4 C25 C26 51(2) . . . . ?
U1 C1 C2 C3 172.7(19) . . . . ?
U1 C1 C6 C5 -173.0(18) . . . . ?
U1 C1 C6 C7 7(3) . . . . ?
N1 C15 C16 N2A -50(3) . . . . ?
N1 C15 C16 N2B -38(4) . . . . ?
N4 C25 C26 N3 -44(3) . . . . ?
N4 C25 C26 N3A -59(2) . . . . ?
C1 C2 C3 C4 2(4) . . . . ?
C1 C6 C7 C8 165(2) . . . . ?
C1 C6 C7 C12 -14(3) . . . . ?
C2 C1 C6 C5 5(4) . . . . ?
C2 C1 C6 C7 -175(2) . . . . ?
C2 C3 C4 C5 2(4) . . . . ?
C3 C4 C5 C6 -2(4) . . . . ?
C4 C5 C6 C1 -2(4) . . . . ?
C4 C5 C6 C7 178(2) . . . . ?
C5 C6 C7 C8 -15(3) . . . . ?
C5 C6 C7 C12 166(2) . . . . ?
C6 C1 C2 C3 -5(4) . . . . ?
C6 C7 C8 C9 176(2) . . . . ?
C6 C7 C12 U1 14(3) . . . . ?
C6 C7 C12 C11 -176(2) . . . . ?
C7 C8 C9 C10 3(4) . . . . ?
C8 C7 C12 U1 -164.9(16) . . . . ?
C8 C7 C12 C11 5(3) . . . . ?
C8 C9 C10 C11 -1(4) . . . . ?
C9 C10 C11 C12 1(4) . . . . ?
C10 C11 C12 U1 165.8(18) . . . . ?
C10 C11 C12 C7 -3(3) . . . . ?
C12 C7 C8 C9 -5(3) . . . . ?
C13 N1 C15 C16 -180(2) . . . . ?
C14 N1 C15 C16 -61(3) . . . . ?
C15 C16 N2B U1 0(4) . . . . ?
C15 C16 N2B P1B -164(4) . . . . ?
C16 N2A P1A U1 -154(4) . . . . ?
C16 N2A P1A C17A -18(4) . . . . ?
C16 N2A P1A C20A 74(4) . . . . ?
C17B P1B C20B C22B 91(6) . . . . ?
C17B P1B C20B C21B -123(6) . . . . ?
C17B P1B N2B U1 116(3) . . . . ?
C17B P1B N2B C16 -78(5) . . . . ?
C23 N4 C25 C26 -179.4(19) . . . . ?
C24 N4 C25 C26 -60(3) . . . . ?
C25 C26 N3A U1 56(4) . . . . ?
C25 C26 N3A P2B -177.0(19) . . . . ?
C26 N3 P2A U1 171(4) . . . . ?
C26 N3 P2A C30A 41(3) . . . . ?
C26 N3 P2A C27A -66(3) . . . . ?
C27B P2B C30B C31B 90(5) . . . . ?
C27B P2B C30B C32B -42(5) . . . . ?
C27B P2B N3A U1 122(2) . . . . ?
C27B P2B N3A C26 -25(3) . . . . ?
C30B P2B C27B C28B -169(4) . . . . ?
C30B P2B C27B C29B 57(5) . . . . ?
C30B P2B N3A U1 -125(2) . . . . ?
C30B P2B N3A C26 89(3) . . . . ?
C20B P1B N2B U1 -113(3) . . . . ?
C20B P1B N2B C16 53(6) . . . . ?
C22A C20A P1A U1 -1(5) . . . . ?
C22A C20A P1A N2A 42(4) . . . . ?
C22A C20A P1A C17A 136(4) . . . . ?
C21A C20A P1A U1 120(3) . . . . ?
C21A C20A P1A N2A 163(4) . . . . ?
C21A C20A P1A C17A -103(4) . . . . ?
P1A N2A C16 C15 170(3) . . . . ?
P2A N3 C26 C25 -159(2) . . . . ?
N3A P2B C27B C28B -46(5) . . . . ?
N3A P2B C27B C29B -180(4) . . . . ?
N3A P2B C30B C31B -30(5) . . . . ?
N3A P2B C30B C32B -163(4) . . . . ?
N2B P1B C20B C22B -43(7) . . . . ?
N2B P1B C20B C21B 103(6) . . . . ?

_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_lk-1_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2254131'
loop_
_audit_author_name
_audit_author_address
'Congqing Zhu'
;Nanjing University
China
;
_audit_update_record             
;
2023-07-25 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         'C40 H96 Cl8 N8 P4 Ru2 U2, 4(C4 H8 O)'
_chemical_formula_sum            'C56 H128 Cl8 N8 O4 P4 Ru2 U2'
_chemical_formula_weight         2063.34
_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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.973(3)
_cell_length_b                   12.2805(19)
_cell_length_c                   22.594(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.793(6)
_cell_angle_gamma                90
_cell_volume                     4051.2(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.518
_shelx_estimated_absorpt_T_min   0.483
_exptl_absorpt_coefficient_mu    4.737
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0973 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.6560.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic orangish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33633
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         2.167
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6594
_reflns_number_total             9177
_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 (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.697
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         9177
_refine_ls_number_restraints     131
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0717
_refine_ls_restrained_S_all      0.982
_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)+(0.1513P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2244
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C24
 1.55 with sigma of 0.001
 C27-C26 = C28-C25
 1.55 with sigma of 0.001
 C28-C27
 1.55 with sigma of 0.001
 O0AA-C26 = O0AA-C25
 1.4 with sigma of 0.01
 O0AA-C27
 2.31 with sigma of 0.001
 C23-C24
 1.55 with sigma of 0.001
 C21-C23
 1.55 with sigma of 0.001
 C22-C24 \\sim C23-C21 \\sim C24-C23
 with sigma of 0.02
 C14-C1 \\sim C17-C1
 with sigma of 0.02
 C17-C1 \\sim C14-C1 \\sim C3-C8 \\sim C9-C8 \\sim C6-C2 \\sim C12-C2 \\sim
C4-C16 \\sim C11-C4
 with sigma of 0.02
 C22-C29 \\sim C22-C24
 with sigma of 0.02
 C29-C23 \\sim C24-C23
 with sigma of 0.02
 C30-C26 \\sim C27-C26
 with sigma of 0.02
 C28-C30 \\sim C28-C27
 with sigma of 0.02
3. Rigid bond restraints
 O1, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O0AA) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(H22C)=Sof(H22D)=Sof(H23C)=Sof(H23D)=Sof(C29)=Sof(H29A)=Sof(H29B)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Sof(H26C)=Sof(H26D)=Sof(H28C)=Sof(H28D)=Sof(C30)=Sof(H30A)=Sof(H30B)=1-FVAR(2)
 Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H28A)=Sof(H28B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C8(H8)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C10(H10A,H10B), C13(H13A,H13B), C21(H21A,H21B),
 C22(H22A,H22B), C22(H22C,H22D), C23(H23C,H23D), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C26(H26A,H26B), C26(H26C,H26D), C27(H27A,H27B), C28(H28C,
 H28D), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.18675(2) 0.34062(3) 0.35337(2) 0.04304(16) Uani 1 1 d . . . . .
Ru1 Ru 0.39003(4) 0.43542(5) 0.46046(3) 0.02904(18) Uani 1 1 d . . . . .
Cl3 Cl 0.27710(14) 0.53042(16) 0.38844(10) 0.0400(5) Uani 1 1 d . . . . .
Cl4 Cl 0.51548(14) 0.39834(16) 0.54376(9) 0.0367(5) Uani 1 1 d . . . . .
P1 P 0.42281(16) 0.31615(18) 0.39445(10) 0.0344(5) Uani 1 1 d . . . . .
P2 P 0.29105(16) 0.33505(17) 0.50078(11) 0.0361(5) Uani 1 1 d . . . . .
Cl1 Cl 0.07964(18) 0.4929(2) 0.28558(13) 0.0588(7) Uani 1 1 d . . . . .
Cl2 Cl 0.1341(3) 0.1327(2) 0.33680(16) 0.0800(11) Uani 1 1 d . . . . .
N2 N 0.3310(6) 0.2841(6) 0.3412(3) 0.0417(19) Uani 1 1 d . . . . .
N4 N 0.1872(6) 0.3225(6) 0.4544(4) 0.0439(19) Uani 1 1 d . . . . .
C1 C 0.2872(7) 0.4278(8) 0.5667(4) 0.049(2) Uani 1 1 d D . . . .
H1 H 0.3511 0.4394 0.5877 0.059 Uiso 1 1 calc R U . . .
N1 N 0.1917(7) 0.3068(7) 0.2374(4) 0.058(3) Uani 1 1 d . . . . .
C2 C 0.4758(6) 0.1902(7) 0.4331(4) 0.046(2) Uani 1 1 d D . . . .
H2 H 0.4486 0.1833 0.4686 0.055 Uiso 1 1 calc R U . . .
C3 C 0.4015(6) 0.1907(9) 0.5869(4) 0.048(2) Uani 1 1 d D . . . .
H3A H 0.4508 0.2037 0.5669 0.072 Uiso 1 1 calc R U . . .
H3B H 0.4070 0.1186 0.6038 0.072 Uiso 1 1 calc R U . . .
H3C H 0.4041 0.2431 0.6188 0.072 Uiso 1 1 calc R U . . .
C4 C 0.5132(7) 0.3778(7) 0.3585(4) 0.041(2) Uani 1 1 d D . . . .
H4 H 0.5600 0.4053 0.3926 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3477(8) 0.2398(8) 0.2836(4) 0.052(3) Uani 1 1 d . . . . .
H5A H 0.3841 0.1739 0.2917 0.063 Uiso 1 1 calc R U . . .
H5B H 0.3818 0.2925 0.2654 0.063 Uiso 1 1 calc R U . . .
N3 N 0.0167(6) 0.3410(8) 0.3829(6) 0.076(4) Uani 1 1 d . . . . .
C6 C 0.5794(6) 0.1953(9) 0.4601(5) 0.052(3) Uani 1 1 d D . . . .
H6A H 0.6120 0.1786 0.4291 0.077 Uiso 1 1 calc R U . . .
H6B H 0.5954 0.1434 0.4925 0.077 Uiso 1 1 calc R U . . .
H6C H 0.5956 0.2672 0.4755 0.077 Uiso 1 1 calc R U . . .
C7 C 0.2573(9) 0.2146(9) 0.2397(5) 0.060(3) Uani 1 1 d . . . . .
H7A H 0.2680 0.2019 0.1994 0.072 Uiso 1 1 calc R U . . .
H7B H 0.2310 0.1489 0.2526 0.072 Uiso 1 1 calc R U . . .
C8 C 0.3098(6) 0.2013(7) 0.5409(4) 0.046(2) Uani 1 1 d D . . . .
H8 H 0.2635 0.1987 0.5655 0.056 Uiso 1 1 calc R U . . .
C9 C 0.2887(8) 0.1018(7) 0.4983(5) 0.057(3) Uani 1 1 d D . . . .
H9A H 0.2264 0.1056 0.4757 0.086 Uiso 1 1 calc R U . . .
H9B H 0.2974 0.0362 0.5219 0.086 Uiso 1 1 calc R U . . .
H9C H 0.3291 0.1018 0.4707 0.086 Uiso 1 1 calc R U . . .
C10 C 0.1084(8) 0.2925(11) 0.4823(6) 0.065(3) Uani 1 1 d . . . . .
H10A H 0.0915 0.3539 0.5046 0.078 Uiso 1 1 calc R U . . .
H10B H 0.1251 0.2321 0.5102 0.078 Uiso 1 1 calc R U . . .
C11 C 0.4794(8) 0.4793(8) 0.3197(4) 0.051(2) Uani 1 1 d D . . . .
H11A H 0.4393 0.4572 0.2823 0.076 Uiso 1 1 calc R U . . .
H11B H 0.5310 0.5175 0.3110 0.076 Uiso 1 1 calc R U . . .
H11C H 0.4470 0.5265 0.3416 0.076 Uiso 1 1 calc R U . . .
C12 C 0.4493(9) 0.0844(7) 0.3980(5) 0.062(3) Uani 1 1 d D . . . .
H12A H 0.3848 0.0719 0.3932 0.093 Uiso 1 1 calc R U . . .
H12B H 0.4827 0.0248 0.4200 0.093 Uiso 1 1 calc R U . . .
H12C H 0.4637 0.0899 0.3588 0.093 Uiso 1 1 calc R U . . .
C13 C 0.0281(8) 0.2604(11) 0.4305(6) 0.070(4) Uani 1 1 d . . . . .
H13A H 0.0399 0.1898 0.4145 0.084 Uiso 1 1 calc R U . . .
H13B H -0.0276 0.2551 0.4455 0.084 Uiso 1 1 calc R U . . .
C14 C 0.2517(8) 0.5387(8) 0.5419(5) 0.056(3) Uani 1 1 d D . . . .
H14A H 0.2907 0.5673 0.5172 0.085 Uiso 1 1 calc R U . . .
H14B H 0.2515 0.5875 0.5751 0.085 Uiso 1 1 calc R U . . .
H14C H 0.1906 0.5312 0.5179 0.085 Uiso 1 1 calc R U . . .
C15 C 0.1032(9) 0.2752(10) 0.1959(6) 0.082(5) Uani 1 1 d . . . . .
H15A H 0.0821 0.2077 0.2094 0.123 Uiso 1 1 calc R U . . .
H15B H 0.1122 0.2666 0.1554 0.123 Uiso 1 1 calc R U . . .
H15C H 0.0584 0.3309 0.1963 0.123 Uiso 1 1 calc R U . . .
C16 C 0.5648(9) 0.2992(10) 0.3247(5) 0.059(3) Uani 1 1 d D . . . .
H16A H 0.5700 0.2292 0.3440 0.089 Uiso 1 1 calc R U . . .
H16B H 0.6249 0.3274 0.3256 0.089 Uiso 1 1 calc R U . . .
H16C H 0.5317 0.2920 0.2833 0.089 Uiso 1 1 calc R U . . .
C17 C 0.2371(9) 0.3894(11) 0.6159(5) 0.063(3) Uani 1 1 d D . . . .
H17A H 0.1743 0.3739 0.5974 0.094 Uiso 1 1 calc R U . . .
H17B H 0.2399 0.4457 0.6457 0.094 Uiso 1 1 calc R U . . .
H17C H 0.2661 0.3248 0.6350 0.094 Uiso 1 1 calc R U . . .
C18 C 0.2277(9) 0.4030(10) 0.2117(5) 0.066(3) Uani 1 1 d . . . . .
H18A H 0.1796 0.4556 0.1998 0.098 Uiso 1 1 calc R U . . .
H18B H 0.2505 0.3818 0.1769 0.098 Uiso 1 1 calc R U . . .
H18C H 0.2765 0.4345 0.2416 0.098 Uiso 1 1 calc R U . . .
C19 C -0.0570(9) 0.3018(15) 0.3333(8) 0.102(6) Uani 1 1 d . . . . .
H19A H -0.0671 0.3536 0.3007 0.153 Uiso 1 1 calc R U . . .
H19B H -0.1122 0.2932 0.3478 0.153 Uiso 1 1 calc R U . . .
H19C H -0.0398 0.2330 0.3190 0.153 Uiso 1 1 calc R U . . .
C20 C -0.0059(9) 0.4480(14) 0.4035(8) 0.098(6) Uani 1 1 d . . . . .
H20A H 0.0468 0.4780 0.4307 0.148 Uiso 1 1 calc R U . . .
H20B H -0.0551 0.4411 0.4243 0.148 Uiso 1 1 calc R U . . .
H20C H -0.0245 0.4953 0.3692 0.148 Uiso 1 1 calc R U . . .
O1 O 0.0006(18) 0.1440(19) 0.5707(12) 0.197(8) Uani 1 1 d . U . . .
C21 C -0.0807(17) 0.096(2) 0.5462(14) 0.188(9) Uani 1 1 d D U . . .
H21A H -0.0855 0.0280 0.5673 0.225 Uiso 1 1 calc R U . . .
H21B H -0.0833 0.0789 0.5039 0.225 Uiso 1 1 calc R U . . .
C22 C -0.0161(13) 0.218(3) 0.6114(15) 0.190(9) Uani 1 1 d D U . . .
H22A H -0.0096 0.2918 0.5971 0.228 Uiso 0.61(4) 1 calc R U P A 1
H22B H 0.0262 0.2088 0.6503 0.228 Uiso 0.61(4) 1 calc R U P A 1
H22C H 0.0333 0.2708 0.6220 0.228 Uiso 0.39(4) 1 calc R U P A 2
H22D H -0.0259 0.1837 0.6480 0.228 Uiso 0.39(4) 1 calc R U P A 2
C23 C -0.1623(15) 0.171(2) 0.5507(11) 0.206(10) Uani 1 1 d D U . . .
H23C H -0.2029 0.1838 0.5115 0.247 Uiso 0.39(4) 1 calc R U P A 2
H23D H -0.1969 0.1432 0.5791 0.247 Uiso 0.39(4) 1 calc R U P A 2
H23A H -0.1690 0.2331 0.5238 0.247 Uiso 0.61(4) 1 calc R U P A 1
H23B H -0.2200 0.1321 0.5464 0.247 Uiso 0.61(4) 1 calc R U P A 1
C24 C -0.1159(15) 0.198(5) 0.6174(11) 0.201(11) Uani 0.61(4) 1 d D U P A 1
H24A H -0.1196 0.1373 0.6443 0.241 Uiso 0.61(4) 1 calc R U P A 1
H24B H -0.1424 0.2622 0.6316 0.241 Uiso 0.61(4) 1 calc R U P A 1
O0AA O 0.7381(17) 0.086(3) 0.3425(12) 0.344(15) Uani 1 1 d D U . . .
C25 C 0.6916(17) 0.030(2) 0.2909(15) 0.230(14) Uani 1 1 d D U . . .
H25A H 0.6780 0.0785 0.2564 0.276 Uiso 1 1 calc R U . . .
H25B H 0.6342 0.0015 0.2978 0.276 Uiso 1 1 calc R U . . .
C26 C 0.812(2) 0.015(3) 0.3631(8) 0.329(19) Uani 1 1 d D U . . .
H26A H 0.7917 -0.0503 0.3805 0.395 Uiso 0.64(4) 1 calc R U P B 1
H26B H 0.8594 0.0500 0.3932 0.395 Uiso 0.64(4) 1 calc R U P B 1
H26C H 0.8166 0.0059 0.4064 0.395 Uiso 0.36(4) 1 calc R U P B 2
H26D H 0.8665 0.0531 0.3586 0.395 Uiso 0.36(4) 1 calc R U P B 2
C27 C 0.8452(12) -0.011(2) 0.3045(10) 0.145(14) Uani 0.64(4) 1 d D U P B 1
H27A H 0.8570 0.0533 0.2825 0.174 Uiso 0.64(4) 1 calc R U P B 1
H27B H 0.8967 -0.0606 0.3108 0.174 Uiso 0.64(4) 1 calc R U P B 1
C28 C 0.7519(13) -0.0658(19) 0.2774(13) 0.195(12) Uani 1 1 d D U . . .
H28C H 0.7136 -0.1269 0.2605 0.235 Uiso 0.36(4) 1 calc R U P B 2
H28D H 0.7870 -0.0431 0.2483 0.235 Uiso 0.36(4) 1 calc R U P B 2
H28A H 0.7434 -0.0803 0.2344 0.235 Uiso 0.64(4) 1 calc R U P B 1
H28B H 0.7427 -0.1320 0.2988 0.235 Uiso 0.64(4) 1 calc R U P B 1
C29 C -0.104(2) 0.272(2) 0.5752(18) 0.085(14) Uani 0.39(4) 1 d D U P A 2
H29A H -0.0923 0.3164 0.5424 0.102 Uiso 0.39(4) 1 calc R U P A 2
H29B H -0.1337 0.3154 0.6011 0.102 Uiso 0.39(4) 1 calc R U P A 2
C30 C 0.816(3) -0.099(3) 0.3365(17) 0.11(2) Uani 0.36(4) 1 d D U P B 2
H30A H 0.8767 -0.1190 0.3318 0.131 Uiso 0.36(4) 1 calc R U P B 2
H30B H 0.7909 -0.1552 0.3583 0.131 Uiso 0.36(4) 1 calc R U 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 Ru1 3.6349(8) . ?
U1 Cl3 2.723(2) . ?
U1 Cl1 2.707(2) . ?
U1 Cl2 2.674(3) . ?
U1 N2 2.341(9) . ?
U1 N4 2.291(9) . ?
U1 N1 2.670(10) . ?
U1 N3 2.772(11) . ?
Ru1 Cl3 2.3769(19) . ?
Ru1 Cl4 2.498(2) 3_666 ?
Ru1 Cl4 2.3899(19) . ?
Ru1 P1 2.222(2) . ?
Ru1 P2 2.268(3) . ?
Cl4 Ru1 2.498(2) 3_666 ?
P1 N2 1.661(7) . ?
P1 C2 1.865(10) . ?
P1 C4 1.884(10) . ?
P2 N4 1.679(8) . ?
P2 C1 1.886(11) . ?
P2 C8 1.867(9) . ?
N2 C5 1.484(13) . ?
N4 C10 1.503(14) . ?
C1 H1 0.9800 . ?
C1 C14 1.522(11) . ?
C1 C17 1.545(11) . ?
N1 C7 1.492(14) . ?
N1 C15 1.495(13) . ?
N1 C18 1.471(16) . ?
C2 H2 0.9800 . ?
C2 C6 1.538(10) . ?
C2 C12 1.528(10) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C8 1.533(10) . ?
C4 H4 0.9800 . ?
C4 C11 1.544(10) . ?
C4 C16 1.541(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C7 1.523(15) . ?
N3 C13 1.442(16) . ?
N3 C19 1.468(17) . ?
N3 C20 1.459(19) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8 0.9800 . ?
C8 C9 1.545(11) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C13 1.533(16) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
O1 C21 1.36(3) . ?
O1 C22 1.36(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C23 1.5499(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C22 H22D 0.9700 . ?
C22 C24 1.5499(11) . ?
C22 C29 1.536(16) . ?
C23 H23C 0.9700 . ?
C23 H23D 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.5500(11) . ?
C23 C29 1.545(16) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
O0AA C25 1.403(10) . ?
O0AA C26 1.401(10) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C28 1.5499(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C26 H26D 0.9700 . ?
C26 C27 1.5499(10) . ?
C26 C30 1.532(19) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.5499(10) . ?
C28 H28C 0.9700 . ?
C28 H28D 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C30 1.517(19) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?

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
Cl3 U1 Ru1 40.83(4) . . ?
Cl3 U1 N3 110.6(2) . . ?
Cl1 U1 Ru1 117.34(6) . . ?
Cl1 U1 Cl3 76.55(7) . . ?
Cl1 U1 N3 71.0(2) . . ?
Cl2 U1 Ru1 125.20(8) . . ?
Cl2 U1 Cl3 165.95(9) . . ?
Cl2 U1 Cl1 117.45(9) . . ?
Cl2 U1 N3 77.1(2) . . ?
N2 U1 Ru1 60.99(16) . . ?
N2 U1 Cl3 82.90(18) . . ?
N2 U1 Cl1 125.79(19) . . ?
N2 U1 Cl2 87.2(2) . . ?
N2 U1 N1 67.2(3) . . ?
N2 U1 N3 161.6(3) . . ?
N4 U1 Ru1 63.3(2) . . ?
N4 U1 Cl3 84.3(2) . . ?
N4 U1 Cl1 120.1(2) . . ?
N4 U1 Cl2 89.0(2) . . ?
N4 U1 N2 106.8(3) . . ?
N4 U1 N1 165.4(3) . . ?
N4 U1 N3 63.9(3) . . ?
N1 U1 Ru1 120.1(2) . . ?
N1 U1 Cl3 107.4(2) . . ?
N1 U1 Cl1 72.2(2) . . ?
N1 U1 Cl2 77.6(2) . . ?
N1 U1 N3 117.6(3) . . ?
N3 U1 Ru1 121.2(3) . . ?
Cl3 Ru1 U1 48.52(5) . . ?
Cl3 Ru1 Cl4 84.02(7) . 3_666 ?
Cl3 Ru1 Cl4 161.54(7) . . ?
Cl4 Ru1 U1 149.25(5) . . ?
Cl4 Ru1 U1 129.37(5) 3_666 . ?
Cl4 Ru1 Cl4 80.37(7) . 3_666 ?
P1 Ru1 U1 67.59(6) . . ?
P1 Ru1 Cl3 95.36(8) . . ?
P1 Ru1 Cl4 107.58(9) . 3_666 ?
P1 Ru1 Cl4 98.69(8) . . ?
P1 Ru1 P2 99.93(9) . . ?
P2 Ru1 U1 64.40(6) . . ?
P2 Ru1 Cl3 96.47(8) . . ?
P2 Ru1 Cl4 152.33(9) . 3_666 ?
P2 Ru1 Cl4 92.85(8) . . ?
Ru1 Cl3 U1 90.65(7) . . ?
Ru1 Cl4 Ru1 99.63(7) . 3_666 ?
N2 P1 Ru1 111.8(3) . . ?
N2 P1 C2 109.9(4) . . ?
N2 P1 C4 110.0(4) . . ?
C2 P1 Ru1 111.5(3) . . ?
C2 P1 C4 105.3(4) . . ?
C4 P1 Ru1 108.1(3) . . ?
N4 P2 Ru1 113.3(3) . . ?
N4 P2 C1 111.3(5) . . ?
N4 P2 C8 104.0(4) . . ?
C1 P2 Ru1 97.2(3) . . ?
C8 P2 Ru1 129.2(3) . . ?
C8 P2 C1 100.1(4) . . ?
P1 N2 U1 118.8(4) . . ?
C5 N2 U1 123.5(6) . . ?
C5 N2 P1 116.6(7) . . ?
P2 N4 U1 114.3(4) . . ?
C10 N4 U1 127.8(6) . . ?
C10 N4 P2 117.7(7) . . ?
P2 C1 H1 105.8 . . ?
C14 C1 P2 108.7(7) . . ?
C14 C1 H1 105.8 . . ?
C14 C1 C17 110.6(9) . . ?
C17 C1 P2 119.2(8) . . ?
C17 C1 H1 105.8 . . ?
C7 N1 U1 104.2(6) . . ?
C7 N1 C15 108.0(9) . . ?
C15 N1 U1 116.3(9) . . ?
C18 N1 U1 110.8(7) . . ?
C18 N1 C7 109.1(11) . . ?
C18 N1 C15 108.2(9) . . ?
P1 C2 H2 104.1 . . ?
C6 C2 P1 116.0(7) . . ?
C6 C2 H2 104.1 . . ?
C12 C2 P1 115.3(6) . . ?
C12 C2 H2 104.1 . . ?
C12 C2 C6 111.3(9) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C8 C3 H3A 109.5 . . ?
C8 C3 H3B 109.5 . . ?
C8 C3 H3C 109.5 . . ?
P1 C4 H4 104.8 . . ?
C11 C4 P1 113.2(7) . . ?
C11 C4 H4 104.8 . . ?
C16 C4 P1 116.7(7) . . ?
C16 C4 H4 104.8 . . ?
C16 C4 C11 111.2(8) . . ?
N2 C5 H5A 109.6 . . ?
N2 C5 H5B 109.6 . . ?
N2 C5 C7 110.3(10) . . ?
H5A C5 H5B 108.1 . . ?
C7 C5 H5A 109.6 . . ?
C7 C5 H5B 109.6 . . ?
C13 N3 U1 102.4(7) . . ?
C13 N3 C19 106.8(10) . . ?
C13 N3 C20 112.2(13) . . ?
C19 N3 U1 113.0(11) . . ?
C20 N3 U1 111.6(7) . . ?
C20 N3 C19 110.5(11) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 C5 110.6(8) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
P2 C8 H8 104.7 . . ?
C3 C8 P2 114.8(6) . . ?
C3 C8 H8 104.7 . . ?
C3 C8 C9 112.6(9) . . ?
C9 C8 P2 113.9(6) . . ?
C9 C8 H8 104.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 H10A 110.3 . . ?
N4 C10 H10B 110.3 . . ?
N4 C10 C13 107.3(10) . . ?
H10A C10 H10B 108.5 . . ?
C13 C10 H10A 110.3 . . ?
C13 C10 H10B 110.3 . . ?
C4 C11 H11A 109.5 . . ?
C4 C11 H11B 109.5 . . ?
C4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C2 C12 H12A 109.5 . . ?
C2 C12 H12B 109.5 . . ?
C2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C10 109.6(9) . . ?
N3 C13 H13A 109.7 . . ?
N3 C13 H13B 109.7 . . ?
C10 C13 H13A 109.7 . . ?
C10 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C1 C14 H14A 109.5 . . ?
C1 C14 H14B 109.5 . . ?
C1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 C16 H16A 109.5 . . ?
C4 C16 H16B 109.5 . . ?
C4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 C17 H17A 109.5 . . ?
C1 C17 H17B 109.5 . . ?
C1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 O1 C22 107(2) . . ?
O1 C21 H21A 109.4 . . ?
O1 C21 H21B 109.4 . . ?
O1 C21 C23 111(2) . . ?
H21A C21 H21B 108.0 . . ?
C23 C21 H21A 109.4 . . ?
C23 C21 H21B 109.4 . . ?
O1 C22 H22A 110.5 . . ?
O1 C22 H22B 110.5 . . ?
O1 C22 H22C 111.6 . . ?
O1 C22 H22D 111.6 . . ?
O1 C22 C24 106(3) . . ?
O1 C22 C29 101(3) . . ?
H22A C22 H22B 108.7 . . ?
H22C C22 H22D 109.4 . . ?
C24 C22 H22A 110.5 . . ?
C24 C22 H22B 110.5 . . ?
C29 C22 H22C 111.6 . . ?
C29 C22 H22D 111.6 . . ?
C21 C23 H23C 112.5 . . ?
C21 C23 H23D 112.5 . . ?
C21 C23 H23A 113.6 . . ?
C21 C23 H23B 113.6 . . ?
H23C C23 H23D 110.0 . . ?
H23A C23 H23B 110.9 . . ?
C24 C23 C21 90(2) . . ?
C24 C23 H23A 113.6 . . ?
C24 C23 H23B 113.6 . . ?
C29 C23 C21 96(2) . . ?
C29 C23 H23C 112.5 . . ?
C29 C23 H23D 112.5 . . ?
C22 C24 H24A 111.7 . . ?
C22 C24 H24B 111.7 . . ?
C23 C24 C22 100.6(19) . . ?
C23 C24 H24A 111.7 . . ?
C23 C24 H24B 111.7 . . ?
H24A C24 H24B 109.4 . . ?
C26 O0AA C25 100(2) . . ?
O0AA C25 H25A 109.8 . . ?
O0AA C25 H25B 109.8 . . ?
O0AA C25 C28 110(2) . . ?
H25A C25 H25B 108.2 . . ?
C28 C25 H25A 109.8 . . ?
C28 C25 H25B 109.8 . . ?
O0AA C26 H26A 111.2 . . ?
O0AA C26 H26B 111.2 . . ?
O0AA C26 H26C 106.7 . . ?
O0AA C26 H26D 106.7 . . ?
O0AA C26 C27 102.9(5) . . ?
O0AA C26 C30 123(3) . . ?
H26A C26 H26B 109.1 . . ?
H26C C26 H26D 106.6 . . ?
C27 C26 H26A 111.2 . . ?
C27 C26 H26B 111.2 . . ?
C30 C26 H26C 106.7 . . ?
C30 C26 H26D 106.7 . . ?
C26 C27 H27A 113.7 . . ?
C26 C27 H27B 113.7 . . ?
H27A C27 H27B 111.0 . . ?
C28 C27 C26 90(2) . . ?
C28 C27 H27A 113.7 . . ?
C28 C27 H27B 113.7 . . ?
C25 C28 C27 96.1(18) . . ?
C25 C28 H28C 110.1 . . ?
C25 C28 H28D 110.1 . . ?
C25 C28 H28A 112.5 . . ?
C25 C28 H28B 112.5 . . ?
C27 C28 H28A 112.5 . . ?
C27 C28 H28B 112.5 . . ?
H28C C28 H28D 108.4 . . ?
H28A C28 H28B 110.0 . . ?
C30 C28 C25 108(3) . . ?
C30 C28 H28C 110.1 . . ?
C30 C28 H28D 110.1 . . ?
C22 C29 C23 101(2) . . ?
C22 C29 H29A 111.5 . . ?
C22 C29 H29B 111.5 . . ?
C23 C29 H29A 111.5 . . ?
C23 C29 H29B 111.5 . . ?
H29A C29 H29B 109.3 . . ?
C26 C30 H30A 113.4 . . ?
C26 C30 H30B 113.4 . . ?
C28 C30 C26 91(2) . . ?
C28 C30 H30A 113.4 . . ?
C28 C30 H30B 113.4 . . ?
H30A C30 H30B 110.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N2 C5 C7 -12.0(11) . . . . ?
U1 N4 C10 C13 7.5(14) . . . . ?
U1 N1 C7 C5 -53.3(11) . . . . ?
U1 N3 C13 C10 57.5(12) . . . . ?
Ru1 P1 N2 U1 -10.4(5) . . . . ?
Ru1 P1 N2 C5 158.1(6) . . . . ?
Ru1 P1 C2 C6 -83.1(8) . . . . ?
Ru1 P1 C2 C12 144.1(8) . . . . ?
Ru1 P1 C4 C11 -65.2(7) . . . . ?
Ru1 P1 C4 C16 163.9(7) . . . . ?
Ru1 P2 N4 U1 25.2(5) . . . . ?
Ru1 P2 N4 C10 -159.6(8) . . . . ?
Ru1 P2 C1 C14 60.2(7) . . . . ?
Ru1 P2 C1 C17 -172.0(8) . . . . ?
Ru1 P2 C8 C3 43.1(9) . . . . ?
Ru1 P2 C8 C9 -88.8(8) . . . . ?
P1 N2 C5 C7 180.0(7) . . . . ?
P2 N4 C10 C13 -167.0(8) . . . . ?
N2 P1 C2 C6 152.3(8) . . . . ?
N2 P1 C2 C12 19.6(10) . . . . ?
N2 P1 C4 C11 57.2(7) . . . . ?
N2 P1 C4 C16 -73.7(8) . . . . ?
N2 C5 C7 N1 46.2(12) . . . . ?
N4 P2 C1 C14 -58.4(8) . . . . ?
N4 P2 C1 C17 69.5(9) . . . . ?
N4 P2 C8 C3 179.9(8) . . . . ?
N4 P2 C8 C9 48.0(9) . . . . ?
N4 C10 C13 N3 -47.6(15) . . . . ?
C1 P2 N4 U1 133.5(4) . . . . ?
C1 P2 N4 C10 -51.3(9) . . . . ?
C1 P2 C8 C3 -65.0(8) . . . . ?
C1 P2 C8 C9 163.1(8) . . . . ?
C2 P1 N2 U1 114.0(5) . . . . ?
C2 P1 N2 C5 -77.5(8) . . . . ?
C2 P1 C4 C11 175.5(6) . . . . ?
C2 P1 C4 C16 44.6(8) . . . . ?
C4 P1 N2 U1 -130.6(4) . . . . ?
C4 P1 N2 C5 38.0(7) . . . . ?
C4 P1 C2 C6 33.9(9) . . . . ?
C4 P1 C2 C12 -98.8(9) . . . . ?
C8 P2 N4 U1 -119.6(5) . . . . ?
C8 P2 N4 C10 55.7(9) . . . . ?
C8 P2 C1 C14 -167.8(7) . . . . ?
C8 P2 C1 C17 -40.0(9) . . . . ?
C15 N1 C7 C5 -177.5(11) . . . . ?
C18 N1 C7 C5 65.1(12) . . . . ?
C19 N3 C13 C10 176.4(14) . . . . ?
C20 N3 C13 C10 -62.3(14) . . . . ?
O1 C21 C23 C24 -45(3) . . . . ?
O1 C21 C23 C29 7(3) . . . . ?
O1 C22 C24 C23 -38(4) . . . . ?
O1 C22 C29 C23 48(3) . . . . ?
C21 O1 C22 C24 9(4) . . . . ?
C21 O1 C22 C29 -44(3) . . . . ?
C21 C23 C24 C22 45(3) . . . . ?
C21 C23 C29 C22 -31(3) . . . . ?
C22 O1 C21 C23 24(4) . . . . ?
O0AA C25 C28 C27 -29(3) . . . . ?
O0AA C25 C28 C30 26(4) . . . . ?
O0AA C26 C27 C28 -64(3) . . . . ?
O0AA C26 C30 C28 24(4) . . . . ?
C25 O0AA C26 C27 47(4) . . . . ?
C25 O0AA C26 C30 -10(4) . . . . ?
C25 C28 C30 C26 -26(4) . . . . ?
C26 O0AA C25 C28 -10(4) . . . . ?
C26 C27 C28 C25 50(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
