 
data_75
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C41 H35 N5 O8 U, C37 H34 N4 O9 U, C5 H5 N'
_chemical_formula_sum 
 'C83 H74 N10 O17 U2' 
_chemical_formula_weight          1959.58 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'U'  'U'  -9.6767   9.6646 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       triclinic 
_space_group_IT_number            2 
_space_group_name_H-M_alt         'P -1' 
_space_group_name_Hall            '-P 1' 
  
_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. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    13.7499(7) 
_cell_length_b                    16.0992(6) 
_cell_length_c                    18.3318(11) 
_cell_angle_alpha                 95.199(4) 
_cell_angle_beta                  104.557(5) 
_cell_angle_gamma                 90.954(4) 
_cell_volume                      3908.3(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     5382 
_cell_measurement_theta_min       2.9320 
_cell_measurement_theta_max       27.6290 
  
_exptl_crystal_description        tablets 
_exptl_crystal_colour             Orange 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.665 
_exptl_crystal_F_000              1924 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.247 
_exptl_crystal_size_mid           0.139 
_exptl_crystal_size_min           0.033 
_exptl_absorpt_coefficient_mu     4.214 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.561 
_exptl_absorpt_correction_T_max   0.879 
_exptl_absorpt_process_details     
; 
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
; 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'Enhance (Mo) X-ray Source' 
_diffrn_measurement_device_type   'Agilent Xcalibur 3 E' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  16.0382 
_diffrn_reflns_number             15451 
_diffrn_reflns_av_unetI/netI      0.1428 
_diffrn_reflns_av_R_equivalents   0.0563 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          2.543 
_diffrn_reflns_theta_max          28.242 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   0.792 
_diffrn_measured_fraction_theta_full  0.984 
_diffrn_reflns_Laue_measured_fraction_max    0.792 
_diffrn_reflns_Laue_measured_fraction_full   0.984 
_diffrn_reflns_point_group_measured_fraction_max   0.792 
_diffrn_reflns_point_group_measured_fraction_full  0.984 
_reflns_number_total              15451 
_reflns_number_gt                 8537 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
; 
  
_computing_data_collection        'CrysAlisPro, Rigaku OD' 
_computing_cell_refinement        'CrysAlisPro, Rigaku OD' 
_computing_data_reduction         'CrysAlisPro, Rigaku OD' 
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2017)' 
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'CIFTAB-2014 (Sheldrick, 2017)' 
_refine_special_details 
; 
 Refined as a 2-component twin. 
; 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0603P)²] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    mixed 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_number_reflns          15451 
_refine_ls_number_parameters      1019 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0978 
_refine_ls_R_factor_gt            0.0436 
_refine_ls_wR_factor_ref          0.1446 
_refine_ls_wR_factor_gt           0.1381 
_refine_ls_goodness_of_fit_ref    1.067 
_refine_ls_restrained_S_all       1.067 
_refine_ls_shift/su_max           0.008 
_refine_ls_shift/su_mean          0.000 
  
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 
U1A U 0.48760(3) 0.45216(3) 0.19483(2) 0.02275(13) Uani 1 1 d . . . . . 
N1A N 0.9020(6) 0.4019(6) 0.2424(5) 0.034(2) Uani 1 1 d . . . . . 
N2A N 0.8168(6) 0.3747(5) 0.2656(5) 0.028(2) Uani 1 1 d . . . . . 
C3A C 0.7348(7) 0.4156(7) 0.2353(6) 0.025(3) Uani 1 1 d . . . . . 
O3A O 0.6491(5) 0.4001(5) 0.2480(4) 0.0314(19) Uani 1 1 d . . . . . 
C4A C 0.7640(8) 0.4761(7) 0.1931(6) 0.028(3) Uani 1 1 d . . . . . 
C5A C 0.8694(8) 0.4609(7) 0.1994(6) 0.032(3) Uani 1 1 d . . . . . 
H5A H 0.910141 0.490686 0.174864 0.038 Uiso 1 1 calc R U . . . 
C6A C 0.8259(9) 0.3076(8) 0.3144(6) 0.040(3) Uani 1 1 d . . . . . 
H6A H 0.766602 0.307089 0.335818 0.048 Uiso 1 1 calc R U . . . 
H6B H 0.886166 0.319951 0.357122 0.048 Uiso 1 1 calc R U . . . 
C7A C 0.8338(8) 0.2229(7) 0.2771(6) 0.029(3) Uani 1 1 d . . . . . 
C8A C 0.7576(9) 0.1631(8) 0.2647(6) 0.038(3) Uani 1 1 d . . . . . 
H8A H 0.698583 0.176088 0.280714 0.046 Uiso 1 1 calc R U . . . 
C9A C 0.7642(9) 0.0846(9) 0.2297(6) 0.040(4) Uani 1 1 d . . . . . 
H9A H 0.710287 0.044367 0.221921 0.048 Uiso 1 1 calc R U . . . 
C10A C 0.8485(8) 0.0647(7) 0.2061(7) 0.033(3) Uani 1 1 d . . . . . 
C11A C 0.9242(9) 0.1254(8) 0.2155(7) 0.042(3) Uani 1 1 d . . . . . 
H11A H 0.981506 0.113914 0.196719 0.051 Uiso 1 1 calc R U . . . 
C12A C 0.9161(9) 0.2025(7) 0.2520(6) 0.037(3) Uani 1 1 d . . . . . 
H12A H 0.969848 0.242810 0.260008 0.045 Uiso 1 1 calc R U . . . 
O13A O 0.8481(7) -0.0144(6) 0.1728(5) 0.054(3) Uani 1 1 d . . . . . 
C14A C 0.9363(11) -0.0384(8) 0.1517(8) 0.061(4) Uani 1 1 d . . . . . 
H14A H 0.945968 -0.005399 0.111474 0.091 Uiso 1 1 calc R U . . . 
H14B H 0.929954 -0.097801 0.133224 0.091 Uiso 1 1 calc R U . . . 
H14C H 0.994288 -0.028611 0.195679 0.091 Uiso 1 1 calc R U . . . 
C15A C 0.6990(8) 0.5339(7) 0.1555(6) 0.026(3) Uani 1 1 d . . . . . 
O15A O 0.6052(5) 0.5289(4) 0.1499(4) 0.0295(19) Uani 1 1 d . . . . . 
C16A C 0.7360(8) 0.6030(6) 0.1208(6) 0.026(3) Uani 1 1 d . . . . . 
C17A C 0.8282(8) 0.6445(7) 0.1530(6) 0.035(3) Uani 1 1 d . . . . . 
H17A H 0.869399 0.626876 0.198279 0.042 Uiso 1 1 calc R U . . . 
C18A C 0.8618(9) 0.7098(7) 0.1219(7) 0.040(3) Uani 1 1 d . . . . . 
H18A H 0.925217 0.737238 0.145114 0.048 Uiso 1 1 calc R U . . . 
C19A C 0.8016(10) 0.7348(8) 0.0562(7) 0.049(4) Uani 1 1 d . . . . . 
H19A H 0.823402 0.780607 0.034234 0.059 Uiso 1 1 calc R U . . . 
C20A C 0.7127(9) 0.6954(7) 0.0227(6) 0.039(3) Uani 1 1 d . . . . . 
H20A H 0.673566 0.712530 -0.023558 0.047 Uiso 1 1 calc R U . . . 
C21A C 0.6767(8) 0.6301(7) 0.0545(6) 0.029(3) Uani 1 1 d . . . . . 
H21A H 0.612466 0.604232 0.031308 0.035 Uiso 1 1 calc R U . . . 
N31A N 0.0784(7) 0.4145(7) 0.0710(6) 0.051(3) Uani 1 1 d . . . . . 
N32A N 0.1527(6) 0.3930(6) 0.1319(5) 0.029(2) Uani 1 1 d . . . . . 
C33A C 0.2395(8) 0.4352(7) 0.1404(6) 0.030(3) Uani 1 1 d . . . . . 
O33A O 0.3183(5) 0.4244(4) 0.1937(4) 0.0285(18) Uani 1 1 d . . . . . 
C34A C 0.2248(7) 0.4899(7) 0.0816(6) 0.027(3) Uani 1 1 d . . . . . 
C35A C 0.1224(8) 0.4711(8) 0.0429(7) 0.039(3) Uani 1 1 d . . . . . 
H35A H 0.088798 0.497867 0.000030 0.047 Uiso 1 1 calc R U . . . 
C36A C 0.1311(9) 0.3313(7) 0.1804(7) 0.044(4) Uani 1 1 d . . . . . 
H36A H 0.062574 0.339560 0.187180 0.053 Uiso 1 1 calc R U . . . 
H36B H 0.178990 0.341602 0.230837 0.053 Uiso 1 1 calc R U . . . 
C37A C 0.1375(7) 0.2421(7) 0.1501(6) 0.026(3) Uani 1 1 d . U . . . 
C38A C 0.1970(8) 0.1867(9) 0.1921(7) 0.046(4) Uani 1 1 d . . . . . 
H38A H 0.237842 0.206554 0.240725 0.055 Uiso 1 1 calc R U . . . 
C39A C 0.2004(10) 0.1045(8) 0.1672(8) 0.055(4) Uani 1 1 d . . . . . 
H39A H 0.242277 0.068224 0.198160 0.067 Uiso 1 1 calc R U . . . 
C40A C 0.1417(9) 0.0747(8) 0.0961(7) 0.037(3) Uani 1 1 d . . . . . 
C41A C 0.0811(8) 0.1288(9) 0.0550(7) 0.041(3) Uani 1 1 d . . . . . 
H41A H 0.039152 0.109128 0.006747 0.049 Uiso 1 1 calc R U . . . 
C42A C 0.0789(8) 0.2099(8) 0.0810(7) 0.041(3) Uani 1 1 d . . . . . 
H42A H 0.035424 0.245576 0.050385 0.049 Uiso 1 1 calc R U . . . 
O43A O 0.1393(6) -0.0054(6) 0.0637(5) 0.052(2) Uani 1 1 d . . . . . 
C44A C 0.1987(11) -0.0646(9) 0.1058(8) 0.067(5) Uani 1 1 d . . . . . 
H44A H 0.200504 -0.115333 0.072325 0.101 Uiso 1 1 calc R U . . . 
H44B H 0.169320 -0.078415 0.146883 0.101 Uiso 1 1 calc R U . . . 
H44C H 0.267187 -0.041088 0.127109 0.101 Uiso 1 1 calc R U . . . 
C45A C 0.3004(7) 0.5452(6) 0.0726(6) 0.022(2) Uani 1 1 d . . . . . 
O45A O 0.3896(5) 0.5428(4) 0.1136(4) 0.0311(19) Uani 1 1 d . . . . . 
C46A C 0.2803(7) 0.6093(6) 0.0191(6) 0.022(2) Uani 1 1 d . . . . . 
C47A C 0.1881(8) 0.6480(7) -0.0019(6) 0.034(3) Uani 1 1 d . . . . . 
H47A H 0.134001 0.633539 0.018656 0.041 Uiso 1 1 calc R U . . . 
C48A C 0.1770(9) 0.7070(8) -0.0525(7) 0.048(4) Uani 1 1 d . . . . . 
H48A H 0.113737 0.731634 -0.067922 0.057 Uiso 1 1 calc R U . . . 
C49A C 0.2527(9) 0.7311(8) -0.0812(7) 0.043(3) Uani 1 1 d . . . . . 
H49A H 0.243901 0.773942 -0.114348 0.052 Uiso 1 1 calc R U . . . 
C50A C 0.3428(9) 0.6931(7) -0.0618(6) 0.037(3) Uani 1 1 d . . . . . 
H50A H 0.395566 0.709233 -0.083179 0.045 Uiso 1 1 calc R U . . . 
C51A C 0.3596(8) 0.6312(7) -0.0116(6) 0.030(3) Uani 1 1 d . . . . . 
H51A H 0.422282 0.605126 0.001070 0.036 Uiso 1 1 calc R U . . . 
N60A N 0.4721(6) 0.3302(6) 0.2728(5) 0.026(2) Uani 1 1 d . . . . . 
C61A C 0.4361(11) 0.3363(8) 0.3320(7) 0.058(4) Uani 1 1 d . . . . . 
H61A H 0.417803 0.389882 0.349093 0.069 Uiso 1 1 calc R U . . . 
C62A C 0.4226(11) 0.2703(10) 0.3717(8) 0.066(5) Uani 1 1 d . . . . . 
H62A H 0.395052 0.277571 0.414415 0.080 Uiso 1 1 calc R U . . . 
C63A C 0.4507(11) 0.1932(9) 0.3469(8) 0.057(4) Uani 1 1 d . . . . . 
H63A H 0.445247 0.146073 0.373487 0.068 Uiso 1 1 calc R U . . . 
C64A C 0.4855(9) 0.1857(7) 0.2855(8) 0.045(3) Uani 1 1 d . . . . . 
H64A H 0.503090 0.132854 0.266245 0.054 Uiso 1 1 calc R U . . . 
C65A C 0.4955(10) 0.2556(8) 0.2503(7) 0.048(4) Uani 1 1 d . . . . . 
H65A H 0.521268 0.249431 0.206750 0.058 Uiso 1 1 calc R U . . . 
O70A O 0.4704(5) 0.3794(5) 0.1153(4) 0.035(2) Uani 1 1 d . . . . . 
O80A O 0.5035(5) 0.5246(5) 0.2754(4) 0.0316(19) Uani 1 1 d . . . . . 
U1B U 0.49815(3) 0.91450(3) 0.29594(2) 0.02895(15) Uani 1 1 d . . . . . 
N1B N 0.9140(8) 0.9289(7) 0.3995(6) 0.052(3) Uani 1 1 d . . . . . 
N2B N 0.8363(6) 0.8903(6) 0.3407(6) 0.039(3) Uani 1 1 d . . . . . 
C3B C 0.7461(8) 0.9255(7) 0.3395(6) 0.031(3) Uani 1 1 d . . . . . 
O3B O 0.6665(5) 0.9001(5) 0.2902(4) 0.041(2) Uani 1 1 d . . . . . 
C4B C 0.7665(8) 0.9920(7) 0.3952(6) 0.029(3) Uani 1 1 d . . . . . 
C5B C 0.8744(9) 0.9903(8) 0.4286(7) 0.043(3) Uani 1 1 d . . . . . 
H5B H 0.910967 1.030236 0.467588 0.052 Uiso 1 1 calc R U . . . 
C6B C 0.8534(10) 0.8170(8) 0.2968(8) 0.049(4) Uani 1 1 d . . . . . 
H6C H 0.921729 0.822212 0.288800 0.059 Uiso 1 1 calc R U . . . 
H6D H 0.804837 0.813919 0.246506 0.059 Uiso 1 1 calc R U . . . 
C7B C 0.8443(9) 0.7363(9) 0.3310(7) 0.046(4) Uani 1 1 d . . . . . 
C8B C 0.7491(10) 0.7028(8) 0.3300(7) 0.050(4) Uani 1 1 d . . . . . 
H8B H 0.690263 0.730527 0.307425 0.060 Uiso 1 1 calc R U . . . 
C9B C 0.7413(10) 0.6290(9) 0.3620(8) 0.054(4) Uani 1 1 d . . . . . 
H9B H 0.676731 0.607320 0.362364 0.064 Uiso 1 1 calc R U . . . 
C10B C 0.8257(11) 0.5863(9) 0.3935(8) 0.053(4) Uani 1 1 d . . . . . 
C11B C 0.9201(12) 0.6186(10) 0.3939(8) 0.064(4) Uani 1 1 d . . . . . 
H11B H 0.978347 0.589906 0.415978 0.077 Uiso 1 1 calc R U . . . 
C12B C 0.9302(10) 0.6934(9) 0.3618(7) 0.053(4) Uani 1 1 d . . . . . 
H12B H 0.994853 0.714563 0.361044 0.064 Uiso 1 1 calc R U . . . 
O13B O 0.8256(9) 0.5123(7) 0.4257(6) 0.075(3) Uani 1 1 d . . . . . 
C14B C 0.7259(14) 0.4830(10) 0.4337(8) 0.092(6) Uani 1 1 d . . . . . 
H14D H 0.685256 0.458112 0.384475 0.138 Uiso 1 1 calc R U . . . 
H14E H 0.691418 0.530415 0.451601 0.138 Uiso 1 1 calc R U . . . 
H14F H 0.735382 0.441161 0.470247 0.138 Uiso 1 1 calc R U . . . 
C15B C 0.6902(9) 1.0434(7) 0.4113(6) 0.031(3) Uani 1 1 d . . . . . 
O15B O 0.5984(5) 1.0220(5) 0.3822(4) 0.037(2) Uani 1 1 d . . . . . 
C16B C 0.7128(10) 1.1226(8) 0.4612(7) 0.039(3) Uani 1 1 d . . . . . 
C17B C 0.7992(9) 1.1708(8) 0.4627(6) 0.039(3) Uani 1 1 d . . . . . 
H17B H 0.844061 1.151694 0.433522 0.047 Uiso 1 1 calc R U . . . 
C18B C 0.8186(10) 1.2470(8) 0.5073(7) 0.051(4) Uani 1 1 d . . . . . 
H18B H 0.876190 1.280594 0.507685 0.061 Uiso 1 1 calc R U . . . 
C19B C 0.7563(12) 1.2732(9) 0.5500(7) 0.057(4) Uani 1 1 d . . . . . 
H19B H 0.771079 1.324265 0.581658 0.068 Uiso 1 1 calc R U . . . 
C20B C 0.6677(11) 1.2239(9) 0.5476(8) 0.059(4) Uani 1 1 d . . . . . 
H20B H 0.622145 1.242196 0.576386 0.071 Uiso 1 1 calc R U . . . 
C21B C 0.6503(10) 1.1492(7) 0.5024(7) 0.042(4) Uani 1 1 d . . . . . 
H21B H 0.592070 1.115700 0.500663 0.050 Uiso 1 1 calc R U . . . 
N31B N 0.1034(7) 0.8117(7) 0.2803(6) 0.046(3) Uani 1 1 d . . . . . 
N32B N 0.1830(7) 0.7930(6) 0.2474(5) 0.035(2) Uani 1 1 d . . . . . 
C33B C 0.2583(8) 0.8511(7) 0.2702(7) 0.032(3) Uani 1 1 d . . . . . 
O33B O 0.3397(6) 0.8464(5) 0.2476(4) 0.038(2) Uani 1 1 d . . . . . 
C34B C 0.2282(8) 0.9124(7) 0.3182(6) 0.031(3) Uani 1 1 d . . . . . 
C35B C 0.1308(9) 0.8816(8) 0.3208(7) 0.043(3) Uani 1 1 d . . . . . 
H35B H 0.090609 0.909997 0.349450 0.051 Uiso 1 1 calc R U . . . 
C36B C 0.1790(9) 0.7140(8) 0.1996(7) 0.042(3) Uani 1 1 d . . . . . 
H36C H 0.232139 0.715642 0.171934 0.050 Uiso 1 1 calc R U . . . 
H36D H 0.113132 0.706891 0.161840 0.050 Uiso 1 1 calc R U . . . 
C37B C 0.1937(8) 0.6410(7) 0.2467(6) 0.033(3) Uani 1 1 d . . . . . 
C38B C 0.2867(9) 0.6177(7) 0.2858(7) 0.040(3) Uani 1 1 d . . . . . 
H38B H 0.344934 0.647657 0.281718 0.048 Uiso 1 1 calc R U . . . 
C39B C 0.2984(9) 0.5530(8) 0.3301(8) 0.051(4) Uani 1 1 d . . . . . 
H39B H 0.363909 0.538982 0.356280 0.061 Uiso 1 1 calc R U . . . 
C40B C 0.2153(9) 0.5077(8) 0.3371(7) 0.040(3) Uani 1 1 d . . . . . 
C41B C 0.1210(9) 0.5291(8) 0.2991(7) 0.045(3) Uani 1 1 d . . . . . 
H41B H 0.063086 0.498451 0.302783 0.054 Uiso 1 1 calc R U . . . 
C42B C 0.1112(9) 0.5956(8) 0.2554(7) 0.045(3) Uani 1 1 d . . . . . 
H42B H 0.045680 0.610764 0.230357 0.054 Uiso 1 1 calc R U . . . 
O43B O 0.2368(7) 0.4412(6) 0.3800(5) 0.063(3) Uani 1 1 d . . . . . 
C44B C 0.1481(13) 0.3987(10) 0.3913(8) 0.085(6) Uani 1 1 d . . . . . 
H44D H 0.101356 0.381721 0.342081 0.127 Uiso 1 1 calc R U . . . 
H44E H 0.115011 0.436482 0.421592 0.127 Uiso 1 1 calc R U . . . 
H44F H 0.168304 0.349130 0.417933 0.127 Uiso 1 1 calc R U . . . 
C45B C 0.2881(8) 0.9828(7) 0.3544(6) 0.028(3) Uani 1 1 d . . . . . 
O45B O 0.3805(6) 0.9899(5) 0.3523(4) 0.039(2) Uani 1 1 d . . . . . 
C46B C 0.2485(9) 1.0524(7) 0.3956(6) 0.034(3) Uani 1 1 d . . . . . 
C47B C 0.1495(11) 1.0764(8) 0.3716(7) 0.054(4) Uani 1 1 d . . . . . 
H47B H 0.106236 1.048310 0.327129 0.065 Uiso 1 1 calc R U . . . 
C48B C 0.1133(10) 1.1408(8) 0.4117(7) 0.051(4) Uani 1 1 d . . . . . 
H48B H 0.044794 1.154991 0.396776 0.062 Uiso 1 1 calc R U . . . 
C49B C 0.1803(10) 1.1848(7) 0.4749(7) 0.043(3) Uani 1 1 d . . . . . 
H49B H 0.157765 1.230639 0.501877 0.052 Uiso 1 1 calc R U . . . 
C50B C 0.2780(10) 1.1614(8) 0.4977(7) 0.042(3) Uani 1 1 d . . . . . 
H50B H 0.321764 1.190573 0.541294 0.050 Uiso 1 1 calc R U . . . 
C51B C 0.3143(9) 1.0972(7) 0.4592(6) 0.033(3) Uani 1 1 d . . . . . 
H51B H 0.382650 1.083052 0.475050 0.040 Uiso 1 1 calc R U . . . 
O60B O 0.5082(3) 0.8117(4) 0.1957(2) 0.040(2) Uani 1 1 d D . . . . 
H60B H 0.5441(4) 0.8276(6) 0.1641(2) 0.03(3) Uiso 1 1 d D . . . . 
C61B C 0.4931(10) 0.7246(7) 0.1859(9) 0.066(5) Uani 1 1 d . . . . . 
H61B H 0.420900 0.710194 0.173226 0.098 Uiso 1 1 calc R U . . . 
H61C H 0.526395 0.701162 0.232937 0.098 Uiso 1 1 calc R U . . . 
H61D H 0.521551 0.701552 0.144828 0.098 Uiso 1 1 calc R U . . . 
O70B O 0.5186(6) 0.8458(5) 0.3671(4) 0.041(2) Uani 1 1 d . . . . . 
O80B O 0.4761(6) 0.9840(5) 0.2247(4) 0.038(2) Uani 1 1 d . . . . . 
N91 N 0.5442(8) 0.8695(6) 0.0767(6) 0.044(3) Uani 1 1 d . . . . . 
C92 C 0.4718(10) 0.8716(9) 0.0120(10) 0.061(4) Uani 1 1 d . . . . . 
H92A H 0.405109 0.855685 0.012514 0.073 Uiso 1 1 calc R U . . . 
C93 C 0.4870(13) 0.8950(9) -0.0550(8) 0.066(5) Uani 1 1 d . . . . . 
H93A H 0.433536 0.893821 -0.099592 0.079 Uiso 1 1 calc R U . . . 
C94 C 0.5838(13) 0.9203(9) -0.0541(8) 0.065(4) Uani 1 1 d . . . . . 
H94A H 0.598860 0.935243 -0.099140 0.078 Uiso 1 1 calc R U . . . 
C95 C 0.6575(10) 0.9238(10) 0.0116(9) 0.063(4) Uani 1 1 d . . . . . 
H95A H 0.722994 0.945276 0.013505 0.075 Uiso 1 1 calc R U . . . 
C96 C 0.6372(10) 0.8963(8) 0.0746(8) 0.049(4) Uani 1 1 d . . . . . 
H96A H 0.690600 0.896030 0.119009 0.059 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 
U1A O70A 1.750(8) . ? 
U1A O80A 1.763(8) . ? 
U1A O33A 2.358(6) . ? 
U1A O15A 2.367(6) . ? 
U1A O45A 2.369(7) . ? 
U1A O3A 2.388(7) . ? 
U1A N60A 2.568(8) . ? 
N1A C5A 1.302(13) . ? 
N1A N2A 1.419(11) . ? 
N2A C3A 1.338(13) . ? 
N2A C6A 1.451(13) . ? 
C3A O3A 1.283(11) . ? 
C3A C4A 1.409(14) . ? 
C4A C15A 1.405(14) . ? 
C4A C5A 1.452(15) . ? 
C6A C7A 1.489(17) . ? 
C7A C12A 1.358(16) . ? 
C7A C8A 1.373(15) . ? 
C8A C9A 1.380(17) . ? 
C9A C10A 1.368(16) . ? 
C10A O13A 1.362(14) . ? 
C10A C11A 1.383(15) . ? 
C11A C12A 1.376(17) . ? 
O13A C14A 1.413(15) . ? 
C15A O15A 1.269(11) . ? 
C15A C16A 1.475(13) . ? 
C16A C17A 1.388(14) . ? 
C16A C21A 1.393(14) . ? 
C17A C18A 1.367(15) . ? 
C18A C19A 1.377(16) . ? 
C19A C20A 1.342(15) . ? 
C20A C21A 1.388(14) . ? 
N31A C35A 1.298(13) . ? 
N31A N32A 1.385(12) . ? 
N32A C33A 1.331(12) . ? 
N32A C36A 1.465(13) . ? 
C33A O33A 1.289(12) . ? 
C33A C34A 1.430(14) . ? 
C34A C45A 1.408(13) . ? 
C34A C35A 1.423(13) . ? 
C36A C37A 1.504(16) . ? 
C37A C42A 1.371(15) . ? 
C37A C38A 1.375(15) . ? 
C38A C39A 1.365(18) . ? 
C39A C40A 1.388(16) . ? 
C40A C41A 1.359(16) . ? 
C40A O43A 1.364(15) . ? 
C41A C42A 1.352(17) . ? 
O43A C44A 1.419(15) . ? 
C45A O45A 1.271(11) . ? 
C45A C46A 1.469(13) . ? 
C46A C51A 1.401(13) . ? 
C46A C47A 1.403(14) . ? 
C47A C48A 1.371(15) . ? 
C48A C49A 1.344(16) . ? 
C49A C50A 1.371(16) . ? 
C50A C51A 1.399(15) . ? 
N60A C61A 1.300(14) . ? 
N60A C65A 1.305(15) . ? 
C61A C62A 1.376(17) . ? 
C62A C63A 1.38(2) . ? 
C63A C64A 1.328(18) . ? 
C64A C65A 1.367(15) . ? 
U1B O70B 1.758(7) . ? 
U1B O80B 1.768(7) . ? 
U1B O33B 2.347(7) . ? 
U1B O3B 2.358(8) . ? 
U1B O60B 2.391(5) . ? 
U1B O15B 2.393(7) . ? 
U1B O45B 2.416(9) . ? 
N1B C5B 1.276(16) . ? 
N1B N2B 1.403(13) . ? 
N2B C3B 1.369(14) . ? 
N2B C6B 1.423(15) . ? 
C3B O3B 1.266(12) . ? 
C3B C4B 1.383(16) . ? 
C4B C15B 1.418(16) . ? 
C4B C5B 1.458(15) . ? 
C6B C7B 1.509(18) . ? 
C7B C12B 1.398(18) . ? 
C7B C8B 1.402(16) . ? 
C8B C9B 1.386(17) . ? 
C9B C10B 1.383(18) . ? 
C10B O13B 1.378(16) . ? 
C10B C11B 1.388(18) . ? 
C11B C12B 1.407(18) . ? 
O13B C14B 1.488(18) . ? 
C15B O15B 1.269(12) . ? 
C15B C16B 1.481(16) . ? 
C16B C21B 1.331(17) . ? 
C16B C17B 1.401(16) . ? 
C17B C18B 1.394(17) . ? 
C18B C19B 1.347(18) . ? 
C19B C20B 1.431(18) . ? 
C20B C21B 1.378(18) . ? 
N31B C35B 1.286(15) . ? 
N31B N32B 1.400(13) . ? 
N32B C33B 1.342(13) . ? 
N32B C36B 1.470(15) . ? 
C33B O33B 1.289(13) . ? 
C33B C34B 1.400(16) . ? 
C34B C45B 1.400(15) . ? 
C34B C35B 1.433(15) . ? 
C36B C37B 1.507(16) . ? 
C37B C38B 1.377(15) . ? 
C37B C42B 1.389(15) . ? 
C38B C39B 1.365(16) . ? 
C39B C40B 1.385(15) . ? 
C40B C41B 1.374(17) . ? 
C40B O43B 1.377(14) . ? 
C41B C42B 1.383(16) . ? 
O43B C44B 1.458(15) . ? 
C45B O45B 1.284(12) . ? 
C45B C46B 1.482(16) . ? 
C46B C47B 1.395(17) . ? 
C46B C51B 1.411(15) . ? 
C47B C48B 1.388(18) . ? 
C48B C49B 1.410(16) . ? 
C49B C50B 1.374(16) . ? 
C50B C51B 1.369(16) . ? 
O60B C61B 1.403(13) . ? 
N91 C92 1.347(16) . ? 
N91 C96 1.353(14) . ? 
C92 C93 1.381(19) . ? 
C93 C94 1.381(19) . ? 
C94 C95 1.361(18) . ? 
C95 C96 1.364(17) . ? 
  
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 
O70A U1A O80A 179.1(3) . . ? 
O70A U1A O33A 88.0(3) . . ? 
O80A U1A O33A 91.2(3) . . ? 
O70A U1A O15A 89.6(3) . . ? 
O80A U1A O15A 91.3(3) . . ? 
O33A U1A O15A 148.2(2) . . ? 
O70A U1A O45A 87.1(3) . . ? 
O80A U1A O45A 93.1(3) . . ? 
O33A U1A O45A 73.1(2) . . ? 
O15A U1A O45A 75.1(2) . . ? 
O70A U1A O3A 90.8(3) . . ? 
O80A U1A O3A 89.5(3) . . ? 
O33A U1A O3A 138.4(2) . . ? 
O15A U1A O3A 73.3(2) . . ? 
O45A U1A O3A 148.4(2) . . ? 
O70A U1A N60A 88.0(3) . . ? 
O80A U1A N60A 91.3(3) . . ? 
O33A U1A N60A 69.2(3) . . ? 
O15A U1A N60A 142.5(3) . . ? 
O45A U1A N60A 142.1(2) . . ? 
O3A U1A N60A 69.3(2) . . ? 
C5A N1A N2A 104.5(8) . . ? 
C3A N2A N1A 112.0(8) . . ? 
C3A N2A C6A 128.5(9) . . ? 
N1A N2A C6A 119.5(9) . . ? 
O3A C3A N2A 122.3(9) . . ? 
O3A C3A C4A 130.2(10) . . ? 
N2A C3A C4A 107.4(9) . . ? 
C3A O3A U1A 130.5(6) . . ? 
C15A C4A C3A 124.1(10) . . ? 
C15A C4A C5A 132.5(10) . . ? 
C3A C4A C5A 103.4(9) . . ? 
N1A C5A C4A 112.6(9) . . ? 
N2A C6A C7A 115.2(10) . . ? 
C12A C7A C8A 117.3(12) . . ? 
C12A C7A C6A 121.0(10) . . ? 
C8A C7A C6A 121.6(12) . . ? 
C7A C8A C9A 121.9(12) . . ? 
C10A C9A C8A 119.9(11) . . ? 
O13A C10A C9A 115.4(10) . . ? 
O13A C10A C11A 125.7(12) . . ? 
C9A C10A C11A 118.9(13) . . ? 
C12A C11A C10A 119.6(13) . . ? 
C7A C12A C11A 122.3(11) . . ? 
C10A O13A C14A 116.8(9) . . ? 
O15A C15A C4A 121.3(9) . . ? 
O15A C15A C16A 116.8(9) . . ? 
C4A C15A C16A 121.9(9) . . ? 
C15A O15A U1A 139.7(6) . . ? 
C17A C16A C21A 117.7(9) . . ? 
C17A C16A C15A 122.2(10) . . ? 
C21A C16A C15A 120.1(9) . . ? 
C18A C17A C16A 122.4(11) . . ? 
C17A C18A C19A 118.4(11) . . ? 
C20A C19A C18A 121.0(11) . . ? 
C19A C20A C21A 121.2(11) . . ? 
C20A C21A C16A 119.3(10) . . ? 
C35A N31A N32A 103.9(8) . . ? 
C33A N32A N31A 112.8(9) . . ? 
C33A N32A C36A 126.7(9) . . ? 
N31A N32A C36A 120.5(8) . . ? 
O33A C33A N32A 122.6(10) . . ? 
O33A C33A C34A 130.3(9) . . ? 
N32A C33A C34A 107.1(9) . . ? 
C33A O33A U1A 127.4(6) . . ? 
C45A C34A C35A 134.7(10) . . ? 
C45A C34A C33A 123.6(9) . . ? 
C35A C34A C33A 101.7(9) . . ? 
N31A C35A C34A 114.5(10) . . ? 
N32A C36A C37A 114.3(10) . . ? 
C42A C37A C38A 116.0(11) . . ? 
C42A C37A C36A 121.7(11) . . ? 
C38A C37A C36A 122.2(10) . . ? 
C39A C38A C37A 123.1(12) . . ? 
C38A C39A C40A 119.1(12) . . ? 
C41A C40A O43A 116.9(11) . . ? 
C41A C40A C39A 117.9(13) . . ? 
O43A C40A C39A 125.2(12) . . ? 
C42A C41A C40A 121.8(12) . . ? 
C41A C42A C37A 121.9(12) . . ? 
C40A O43A C44A 118.7(10) . . ? 
O45A C45A C34A 119.9(9) . . ? 
O45A C45A C46A 117.3(8) . . ? 
C34A C45A C46A 122.8(9) . . ? 
C45A O45A U1A 138.4(6) . . ? 
C51A C46A C47A 119.8(10) . . ? 
C51A C46A C45A 116.3(9) . . ? 
C47A C46A C45A 123.9(9) . . ? 
C48A C47A C46A 119.3(10) . . ? 
C49A C48A C47A 122.2(12) . . ? 
C48A C49A C50A 119.1(11) . . ? 
C49A C50A C51A 122.2(11) . . ? 
C50A C51A C46A 117.4(11) . . ? 
C61A N60A C65A 116.3(10) . . ? 
C61A N60A U1A 124.0(8) . . ? 
C65A N60A U1A 119.6(8) . . ? 
N60A C61A C62A 124.3(14) . . ? 
C61A C62A C63A 117.1(14) . . ? 
C64A C63A C62A 119.2(12) . . ? 
C63A C64A C65A 118.7(13) . . ? 
N60A C65A C64A 124.3(13) . . ? 
O70B U1B O80B 179.2(4) . . ? 
O70B U1B O33B 86.8(3) . . ? 
O80B U1B O33B 92.7(3) . . ? 
O70B U1B O3B 88.9(3) . . ? 
O80B U1B O3B 91.9(3) . . ? 
O33B U1B O3B 139.9(3) . . ? 
O70B U1B O60B 95.8(3) . . ? 
O80B U1B O60B 84.7(3) . . ? 
O33B U1B O60B 71.4(2) . . ? 
O3B U1B O60B 69.5(2) . . ? 
O70B U1B O15B 90.7(3) . . ? 
O80B U1B O15B 89.3(3) . . ? 
O33B U1B O15B 147.7(3) . . ? 
O3B U1B O15B 72.2(3) . . ? 
O60B U1B O15B 140.9(2) . . ? 
O70B U1B O45B 90.9(3) . . ? 
O80B U1B O45B 88.3(3) . . ? 
O33B U1B O45B 72.6(3) . . ? 
O3B U1B O45B 147.4(3) . . ? 
O60B U1B O45B 142.86(19) . . ? 
O15B U1B O45B 75.2(2) . . ? 
C5B N1B N2B 105.4(10) . . ? 
C3B N2B N1B 111.5(10) . . ? 
C3B N2B C6B 127.3(10) . . ? 
N1B N2B C6B 120.6(10) . . ? 
O3B C3B N2B 121.4(12) . . ? 
O3B C3B C4B 132.1(12) . . ? 
N2B C3B C4B 106.2(10) . . ? 
C3B O3B U1B 128.5(8) . . ? 
C3B C4B C15B 122.4(10) . . ? 
C3B C4B C5B 104.5(11) . . ? 
C15B C4B C5B 133.1(12) . . ? 
N1B C5B C4B 112.2(11) . . ? 
N2B C6B C7B 115.1(11) . . ? 
C12B C7B C8B 119.7(13) . . ? 
C12B C7B C6B 120.3(12) . . ? 
C8B C7B C6B 120.0(12) . . ? 
C9B C8B C7B 119.7(13) . . ? 
C10B C9B C8B 121.2(13) . . ? 
O13B C10B C9B 125.5(14) . . ? 
O13B C10B C11B 115.1(13) . . ? 
C9B C10B C11B 119.4(14) . . ? 
C10B C11B C12B 120.6(14) . . ? 
C7B C12B C11B 119.4(13) . . ? 
C10B O13B C14B 115.0(12) . . ? 
O15B C15B C4B 119.9(10) . . ? 
O15B C15B C16B 117.5(12) . . ? 
C4B C15B C16B 122.6(10) . . ? 
C15B O15B U1B 139.7(8) . . ? 
C21B C16B C17B 120.3(12) . . ? 
C21B C16B C15B 120.6(11) . . ? 
C17B C16B C15B 119.1(12) . . ? 
C18B C17B C16B 119.3(13) . . ? 
C19B C18B C17B 120.4(12) . . ? 
C18B C19B C20B 119.8(13) . . ? 
C21B C20B C19B 118.3(14) . . ? 
C16B C21B C20B 121.9(12) . . ? 
C35B N31B N32B 104.7(9) . . ? 
C33B N32B N31B 111.6(10) . . ? 
C33B N32B C36B 128.7(11) . . ? 
N31B N32B C36B 119.5(9) . . ? 
O33B C33B N32B 122.4(12) . . ? 
O33B C33B C34B 130.4(10) . . ? 
N32B C33B C34B 107.2(10) . . ? 
C33B O33B U1B 131.3(7) . . ? 
C45B C34B C33B 123.9(10) . . ? 
C45B C34B C35B 132.8(12) . . ? 
C33B C34B C35B 103.3(10) . . ? 
N31B C35B C34B 113.2(12) . . ? 
N32B C36B C37B 111.0(9) . . ? 
C38B C37B C42B 116.3(11) . . ? 
C38B C37B C36B 123.2(10) . . ? 
C42B C37B C36B 120.4(11) . . ? 
C39B C38B C37B 122.4(11) . . ? 
C38B C39B C40B 120.4(12) . . ? 
C41B C40B O43B 125.9(11) . . ? 
C41B C40B C39B 119.0(12) . . ? 
O43B C40B C39B 115.1(12) . . ? 
C40B C41B C42B 119.5(11) . . ? 
C41B C42B C37B 122.4(12) . . ? 
C40B O43B C44B 113.9(11) . . ? 
O45B C45B C34B 120.8(11) . . ? 
O45B C45B C46B 117.0(9) . . ? 
C34B C45B C46B 122.2(10) . . ? 
C45B O45B U1B 138.7(7) . . ? 
C47B C46B C51B 119.5(12) . . ? 
C47B C46B C45B 121.7(11) . . ? 
C51B C46B C45B 118.8(11) . . ? 
C48B C47B C46B 120.9(12) . . ? 
C47B C48B C49B 118.6(13) . . ? 
C50B C49B C48B 120.0(12) . . ? 
C51B C50B C49B 121.8(12) . . ? 
C50B C51B C46B 119.0(12) . . ? 
C61B O60B U1B 132.5(7) . . ? 
C92 N91 C96 115.7(11) . . ? 
N91 C92 C93 125.0(13) . . ? 
C94 C93 C92 116.7(13) . . ? 
C95 C94 C93 119.8(13) . . ? 
C94 C95 C96 119.8(13) . . ? 
N91 C96 C95 122.9(12) . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
 _geom_hbond_publ_flag 
O60B H60B N91  0.9000(1) 1.794(11) 2.601(11) 147.9(7) . yes 
  
_refine_diff_density_max    2.583 
_refine_diff_density_min   -1.186 
_refine_diff_density_rms    0.152 
  
  
  
#===END

