Elemental Chalcogen Reactions of a Tetravalent Uranium Imidophosphorane Complex: Cleavage of Dioxygen
Aguirre Quintana, Luis M.; Rajeshkumar, Thayalan; Jiang, Ningxin; Niklas, Julie; Bacsa, John; Maron, Laurent; La Pierre, Henry Storms; Chemical Communications  (2022) –; doi:10.1039/D2CC05066H

data_7130939
_publ_section_title
;
 Elemental Chalcogen Reactions of a Tetravalent Uranium Imidophosphorane
 Complex: Cleavage of Dioxygen
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05066H
_journal_year                    2022
_chemical_formula_moiety         'C60 H120 N16 P4 Se2.688 U'
_chemical_formula_sum            'C72.5 H140 N16 O2 P4 Se2.69 U'
_chemical_formula_weight         1842.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-09-06
_audit_creation_method
;FinalCif V109 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-09-06 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.244(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4586(9)
_cell_length_b                   27.1124(13)
_cell_length_c                   22.5764(12)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.83
_cell_measurement_theta_min      2.36
_cell_volume                     8797.6(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2013)'
_computing_data_collection       'APEX2  v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1416
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            208409
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.917
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.080
_exptl_absorpt_correction_T_max  0.7417
_exptl_absorpt_correction_T_min  0.6190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1133 before and 0.1036 after correction.
The Ratio of minimum to maximum transmission is 0.8346.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       prism
_exptl_crystal_F_000             3786
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.446
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         14932
_refine_ls_number_restraints     3577
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0799
_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/[\s^2^(Fo^2^)+(0.0375P)^2^+156.1268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11981
_reflns_number_total             14932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05066h2.cif
_cod_data_source_block           laq-rad_se3
_cod_original_formula_sum        'C72.50 H140 N16 O2 P4 Se2.69 U'
_cod_database_code               7130939
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Shared sites
{U1A, U1B}
3. Restrained distances
 Se5-Se4
 2.323 with sigma of 0.01
 C5_21-C4_21 = C2_21-C1_21
 1.525 with sigma of 0.002
 C2_21-C1_21
 1.52 with sigma of 0.01
 C4_21-C3_21 = C3_21-C2_21 = C9_21-C8_21 = C8_21-C7_21 = C7_21-C6_21 = C9_21-
 C10_21
 1.525 with sigma of 0.002
 C5_25-C1_25
 2.535 with sigma of 0.01
 N2_1-P1_1
 1.72 with sigma of 0.02
 C1_1-C2_1 = C13_1-C14_1 = C4_1-C5_1 = C8_1-C9_1 = N1_1-P1_1
 1.53 with sigma of 0.02
 N4_1-P1_1
 1.68 with sigma of 0.02
 N3_1-P1_1
 1.69 with sigma of 0.02
 C1_1-N2_1 = C5_1-N2_1 = C6_1-N3_1
 1.48 with sigma of 0.02
 C10_1-N3_1 = C11_1-N4_1 = C15_1-N4_1
 1.46 with sigma of 0.02
 C10_1-C9_1 = C2_1-C3_1 = C3_1-C4_1 = C7_1-C8_1
 1.52 with sigma of 0.02
 C11_1-C12_1 = C14_1-C15_1 = C6_1-C7_1
 1.51 with sigma of 0.02
 C12_1-C11_1 = C15_1-C14_1 = C14_1-C13_1 = C13_1-C12_1
 1.525 with sigma of 0.002
 C12_1-C13_1
 1.54 with sigma of 0.02
 N3_22-C10_22 = N3_22-C6_22
 1.495 with sigma of 0.02
 H5A_22-H11A_24 = H11A_24-H11B_24
 -2.2 with sigma of 0.02
 H5A_24-C10_24
 -2.5 with sigma of 0.01
 C15_24-C11_24
 2.535 with sigma of 0.01
 C15_1-P1_1
 2.78 with sigma of 0.04
 C5_1-P1_1 = N1_1-N3_1
 2.69 with sigma of 0.04
 C1_1-P1_1 = N2_1-N4_1
 2.62 with sigma of 0.04
 C6_1-P1_1
 2.65 with sigma of 0.04
 C11_1-P1_1
 2.73 with sigma of 0.04
 C10_1-P1_1
 2.77 with sigma of 0.04
 N1_1-N2_1
 2.81 with sigma of 0.04
 N1_1-N4_1
 2.68 with sigma of 0.04
 C4_1-N2_1
 2.47 with sigma of 0.04
 N2_1-N3_1
 2.61 with sigma of 0.04
 N3_1-N4_1
 2.72 with sigma of 0.04
 C14_1-N4_1
 2.45 with sigma of 0.04
 C1_1-C3_1 = C10_1-C8_1 = C11_1-C13_1
 2.51 with sigma of 0.04
 C1_1-C5_1
 2.42 with sigma of 0.04
 C2_1-C4_1
 2.49 with sigma of 0.04
 C3_1-C5_1
 2.53 with sigma of 0.04
 C13_1-C15_1 = C6_1-C8_1 = C7_1-C9_1
 2.5 with sigma of 0.04
 C10_1-C6_1 = C11_1-C15_1
 2.43 with sigma of 0.04
 C12_1-C14_1
 2.52 with sigma of 0.04
 U1A-N1_25 \\sim U1B-N1_24
 with sigma of 0.002
 U1B-N1_24 \\sim U1A-N1_25
 with sigma of 0.02
 U1A-N1_21 \\sim U1B-N1_22
 with sigma of 0.002
 U1B-N1_23 \\sim U1A-N1_26
 with sigma of 0.002
 U1A-N1_25 \\sim U1B-N1_25
 with sigma of 0.002
 U1B-N1_25 \\sim U1A-N1_24
 with sigma of 0.003
 U1A-N1_1 \\sim U1B-N1_1
 with sigma of 0.002
 U1A-Se3 \\sim U1A-Se1
 with sigma of 0.003
 Se3-Se2 \\sim Se2-Se1
 with sigma of 0.002
 U1B-Se4 \\sim U1B-Se5
 with sigma of 0.003
 U1B-Se5 \\sim U1B-Se4
 with sigma of 0.002
 P1_25-N2_25 \\sim P1_26-N2_26 \\sim P1_1-N2_1 \\sim P1_21-N4_21
 with sigma of 0.002
 P1_22-N2_21 \\sim P1_23-N3_26
 with sigma of 0.002
 N3_21-C6_21 \\sim N3_21-C10_21 \\sim N2_21-C5_21 \\sim N2_21-C1_21 \\sim
N4_21-C15_21 \\sim N4_21-
 C11_21
 with sigma of 0.002
 P1_22-N2_22 \\sim P1_22-N2_21
 with sigma of 0.0002
 N2_21-C1_21 \\sim N2_21-C5_21 \\sim N4_21-C11_21 \\sim N2_1-C5_1 \\sim
N2_1-C1_1
 with sigma of 0.002
 N4_21-C11_21 \\sim N4_21-C15_21
 with sigma of 0.002
 P1_25-N4_24 \\sim P1_25-N4_25 \\sim P1_23-N3_23
 with sigma of 0.002
 P1_25-N2_25 \\sim P1_25-N4_25 \\sim P1_25-N3_25
 with sigma of 0.002
 P1_23-N3_23 \\sim P1_23-N3_26
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
Uanis(U1A) \\sim Ueq, Uanis(U1B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(U1B) \\sim Ueq, Uanis(U1A) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(U1A) \\sim Ueq, Uanis(N1_1) \\sim Ueq, Uanis(N1_21) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
Uanis(C5_22) \\sim Ueq, Uanis(C5_21) \\sim Ueq, Uanis(N2_22) \\sim Ueq,
Uanis(N2_21) \\sim Ueq, Uanis(C1_21) \\sim Ueq: with sigma of 0.002 and sigma
for terminal atoms of 0.004
Uanis(N1_26) \\sim Ueq, Uanis(N1_23) \\sim Ueq: with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(N4_26) \\sim Ueq, Uanis(N4_23) \\sim Ueq: with sigma of 0.002 and sigma
for terminal atoms of 0.004
Uanis(U1A) = Uanis(U1B)
Uanis(P1_21) = Uanis(P1_22)
Uanis(N1_21) = Uanis(N1_22)
Uanis(N2_22) = Uanis(N2_21)
Uanis(N3_21) = Uanis(N3_22)
Uanis(N4_21) = Uanis(N4_22)
Uanis(C2_22) = Uanis(C1_21)
Uanis(C3_22) = Uanis(C3_21)
Uanis(C4_21) = Uanis(C4_22)
Uanis(C5_22) = Uanis(C5_21)
Uanis(C6_21) = Uanis(C6_22)
Uanis(C7_21) = Uanis(C7_22)
Uanis(C8_21) = Uanis(C8_22)
Uanis(C9_21) = Uanis(C9_22)
Uanis(C10_21) = Uanis(C10_22)
Uanis(C11_21) = Uanis(C11_22)
Uanis(C12_21) = Uanis(C12_22)
Uanis(C13_21) = Uanis(C13_22)
Uanis(C14_21) = Uanis(C14_22)
Uanis(C15_21) = Uanis(C15_22)
Uanis(P1_24) = Uanis(P1_25)
Uanis(N1_24) = Uanis(N1_25)
Uanis(N2_24) = Uanis(N2_25)
Uanis(N3_24) = Uanis(N3_25)
Uanis(N4_24) = Uanis(N4_25)
Uanis(C1_24) = Uanis(C1_25)
Uanis(C2_24) = Uanis(C2_25)
Uanis(C3_24) = Uanis(C3_25)
Uanis(C4_24) = Uanis(C4_25)
Uanis(C5_24) = Uanis(C5_25)
Uanis(C6_24) = Uanis(C6_25)
Uanis(C7_24) = Uanis(C7_25)
Uanis(C8_24) = Uanis(C8_25)
Uanis(C9_24) = Uanis(C9_25)
Uanis(C10_24) = Uanis(C10_25)
Uanis(C11_24) = Uanis(C11_25)
Uanis(C12_25) = Uanis(C12_24)
Uanis(C13_25) = Uanis(C13_24)
Uanis(C14_25) = Uanis(C14_24) = Uanis(C13_24)
Uanis(C15_25) = Uanis(C15_24)
Uanis(P1_26) = Uanis(P1_23)
Uanis(N1_26) = Uanis(N1_23)
Uanis(N2_26) = Uanis(N2_23)
Uanis(N3_26) = Uanis(N3_23)
Uanis(N4_26) = Uanis(N4_23)
Uanis(C1_26) = Uanis(C1_23)
Uanis(C2_26) = Uanis(C2_23)
Uanis(C3_26) = Uanis(C3_23)
Uanis(C4_26) = Uanis(C4_23)
Uanis(C5_26) = Uanis(C5_23)
Uanis(C6_26) = Uanis(C6_23)
Uanis(C7_26) = Uanis(C7_23)
Uanis(C9_23) = Uanis(C9_26)
Uanis(C10_26) = Uanis(C10_23)
Uanis(C11_26) = Uanis(C11_23)
Uanis(C12_26) = Uanis(C12_23)
Uanis(C13_26) = Uanis(C13_23)
Uanis(C14_26) = Uanis(C14_23)
Uanis(C15_26) = Uanis(C15_23)
5. Rigid body (RIGU) restrains
 U1A, N4_24, Se1, C7_26, Se2, C8_24, Se3, N3_26, P1_1, C15_26, N1_1, C4_24,
 N2_1, C12_24, N3_1, N4_1, C3_26, C1_1, C11_26, C2_1, N2_24, C3_1, C2_24, C4_1,
 C6_24, C5_1, C10_24, C6_1, C14_24, C7_1, C8_1, N1_26, C9_1, C1_26, C10_1,
 C5_26, C11_1, C9_26, C12_1, C13_26, C13_1, N1_24, C14_1, N3_24, C15_1, C1_24,
 P1_21, C3_24, N1_21, C5_24, N2_21, C7_24, N3_21, C9_24, N4_21, C11_24, C1_21,
 C13_24, C2_21, C15_24, C3_21, C4_21, C5_21, P1_26, C6_21, N2_26, C7_21, N4_26,
 C8_21, C2_26, C9_21, C4_26, C10_21, C6_26, C11_21, C8_26, C12_21, C10_26,
 C13_21, C12_26, C14_21, C14_26, C15_21, P1_24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Se1, Se2, Se3
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 U1B, C12_23, P1_23, Se4, C13_25, Se5, C4_23, P1_22, C9_25, N1_22, N2_22,
 N4_23, N3_22, C8_23, N4_22, C7_25, C1_22, C11_25, C2_22, C15_25, C3_22, C4_22,
 N2_23, C5_22, C2_23, C6_22, C6_23, C7_22, C10_23, C8_22, C14_23, C9_22, C8_25,
 C10_22, C10_25, C11_22, C12_25, C12_22, C14_25, C13_22, C14_22, C15_22, P1_25,
 N1_23, N1_25, N3_23, N2_25, C1_23, N3_25, C3_23, N4_25, C5_23, C1_25, C7_23,
 C2_25, C9_23, C3_25, C11_23, C4_25, C13_23, C5_25, C15_23, C6_25
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 Se4, Se5
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 P1_22, N2_22
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{P1_25, N1_25, N2_25, N3_25, N4_25, C1_25, C2_25, C3_25, C4_25, C5_25, C6_25,
C7_25, C8_25, C9_25, C10_25, C11_25, C12_25, C13_25, C14_25, C15_25}
{P1_26, N1_26, N2_26, N3_26, N4_26, C1_26, C2_26, C3_26, C4_26, C5_26, C6_26,
C7_26, C8_26, C9_26, C10_26, C11_26, C12_26, C13_26, C14_26, C15_26}
{P1_1, N1_1, N2_1, N3_1, N4_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1,
C9_1, C10_1, C11_1, C12_1, C13_1, C14_1, C15_1}
{P1_22, N1_22, N2_22, N3_22, N4_22, C1_22, C2_22, C3_22, C4_22, C5_22, C6_22,
C7_22, C8_22, C9_22, C10_22, C11_22, C12_22, C13_22, C14_22, C15_22}
{P1_23, N1_23, N2_23, N3_23, N4_23, C1_23, C2_23, C3_23, C4_23, C5_23, C6_23,
C7_23, C8_23, C9_23, C10_23, C11_23, C12_23, C13_23, C14_23, C15_23}
{P1_24, N1_24, N2_24, N3_24, N4_24, C1_24, C2_24, C3_24, C4_24, C5_24, C6_24,
C7_24, C8_24, C9_24, C10_24, C11_24, C12_24, C13_24, C14_24, C15_24}
as
{P1_21, N1_21, N2_21, N3_21, N4_21, C1_21, C2_21, C3_21, C4_21, C5_21, C6_21,
C7_21, C8_21, C9_21, C10_21, C11_21, C12_21, C13_21, C14_21, C15_21} sigma for
1-2: 0.002 1-3: 0.002
7. Others
 Fixed Sof: U1A(0.68839) Se1(0.68839) Se2(0.68839) Se3(0.68839) U1B(0.31161)
 Se4(0.31161) Se5(0.31161) P1(0.68839) N1(0.68839) N2(0.68839) N3(0.68839)
 N4(0.68839) C1(0.68839) H1A(0.68839) H1B(0.68839) C2(0.68839) H2A(0.68839)
 H2B(0.68839) C3(0.68839) H3A(0.68839) H3B(0.68839) C4(0.68839) H4A(0.68839)
 H4B(0.68839) C5(0.68839) H5A(0.68839) H5B(0.68839) C6(0.68839) H6A(0.68839)
 H6B(0.68839) C7(0.68839) H7A(0.68839) H7B(0.68839) C8(0.68839) H8A(0.68839)
 H8B(0.68839) C9(0.68839) H9A(0.68839) H9B(0.68839) C10(0.68839) H10A(0.68839)
 H10B(0.68839) C11(0.68839) H11A(0.68839) H11B(0.68839) C12(0.68839)
 H12A(0.68839) H12B(0.68839) C13(0.68839) H13A(0.68839) H13B(0.68839)
 C14(0.68839) H14A(0.68839) H14B(0.68839) C15(0.68839) H15A(0.68839)
 H15B(0.68839) P1(0.68839) N1(0.68839) N2(0.68839) N3(0.68839) N4(0.68839)
 C1(0.68839) H1A(0.68839) H1B(0.68839) C2(0.68839) H2A(0.68839) H2B(0.68839)
 C3(0.68839) H3A(0.68839) H3B(0.68839) C4(0.68839) H4A(0.68839) H4B(0.68839)
 C5(0.68839) H5A(0.68839) H5B(0.68839) C6(0.68839) H6A(0.68839) H6B(0.68839)
 C7(0.68839) H7A(0.68839) H7B(0.68839) C8(0.68839) H8A(0.68839) H8B(0.68839)
 C9(0.68839) H9A(0.68839) H9B(0.68839) C10(0.68839) H10A(0.68839) H10B(0.68839)
 C11(0.68839) H11A(0.68839) H11B(0.68839) C12(0.68839) H12A(0.68839)
 H12B(0.68839) C13(0.68839) H13A(0.68839) H13B(0.68839) C14(0.68839)
 H14A(0.68839) H14B(0.68839) C15(0.68839) H15A(0.68839) H15B(0.68839)
 P1(0.68839) N1(0.68839) N2(0.68839) N3(0.68839) N4(0.68839) C1(0.68839)
 H1A(0.68839) H1B(0.68839) C2(0.68839) H2A(0.68839) H2B(0.68839) C3(0.68839)
 H3A(0.68839) H3B(0.68839) C4(0.68839) H4A(0.68839) H4B(0.68839) C5(0.68839)
 H5A(0.68839) H5B(0.68839) C6(0.68839) H6A(0.68839) H6B(0.68839) C7(0.68839)
 H7A(0.68839) H7B(0.68839) C8(0.68839) H8A(0.68839) H8B(0.68839) C9(0.68839)
 H9A(0.68839) H9B(0.68839) C10(0.68839) H10A(0.68839) H10B(0.68839)
 C11(0.68839) H11A(0.68839) H11B(0.68839) C12(0.68839) H12A(0.68839)
 H12B(0.68839) C13(0.68839) H13A(0.68839) H13B(0.68839) C14(0.68839)
 H14A(0.68839) H14B(0.68839) C15(0.68839) H15A(0.68839) H15B(0.68839)
 P1(0.31161) N1(0.31161) N2(0.31161) N3(0.31161) N4(0.31161) C1(0.31161)
 H1A(0.31161) H1B(0.31161) C2(0.31161) H2A(0.31161) H2B(0.31161) C3(0.31161)
 H3A(0.31161) H3B(0.31161) C4(0.31161) H4A(0.31161) H4B(0.31161) C5(0.31161)
 H5A(0.31161) H5B(0.31161) C6(0.31161) H6A(0.31161) H6B(0.31161) C7(0.31161)
 H7A(0.31161) H7B(0.31161) C8(0.31161) H8A(0.31161) H8B(0.31161) C9(0.31161)
 H9A(0.31161) H9B(0.31161) C10(0.31161) H10A(0.31161) H10B(0.31161)
 C11(0.31161) H11A(0.31161) H11B(0.31161) C12(0.31161) H12A(0.31161)
 H12B(0.31161) C13(0.31161) H13A(0.31161) H13B(0.31161) C14(0.31161)
 H14A(0.31161) H14B(0.31161) C15(0.31161) H15A(0.31161) H15B(0.31161)
 P1(0.31161) N1(0.31161) N2(0.31161) N3(0.31161) N4(0.31161) C1(0.31161)
 H1A(0.31161) H1B(0.31161) C2(0.31161) H2A(0.31161) H2B(0.31161) C3(0.31161)
 H3A(0.31161) H3B(0.31161) C4(0.31161) H4A(0.31161) H4B(0.31161) C5(0.31161)
 H5A(0.31161) H5B(0.31161) C6(0.31161) H6A(0.31161) H6B(0.31161) C7(0.31161)
 H7A(0.31161) H7B(0.31161) C8(0.31161) H8A(0.31161) H8B(0.31161) C9(0.31161)
 H9A(0.31161) H9B(0.31161) C10(0.31161) H10A(0.31161) H10B(0.31161)
 C11(0.31161) H11A(0.31161) H11B(0.31161) C12(0.31161) H12A(0.31161)
 H12B(0.31161) C13(0.31161) H13A(0.31161) H13B(0.31161) C14(0.31161)
 H14A(0.31161) H14B(0.31161) C15(0.31161) H15A(0.31161) H15B(0.31161)
 P1(0.31161) N1(0.31161) N2(0.31161) N3(0.31161) N4(0.31161) C1(0.31161)
 H1A(0.31161) H1B(0.31161) C2(0.31161) H2A(0.31161) H2B(0.31161) C3(0.31161)
 H3A(0.31161) H3B(0.31161) C4(0.31161) H4A(0.31161) H4B(0.31161) C5(0.31161)
 H5A(0.31161) H5B(0.31161) C6(0.31161) H6A(0.31161) H6B(0.31161) C7(0.31161)
 H7A(0.31161) H7B(0.31161) C8(0.31161) H8A(0.31161) H8B(0.31161) C9(0.31161)
 H9A(0.31161) H9B(0.31161) C10(0.31161) H10A(0.31161) H10B(0.31161)
 C11(0.31161) H11A(0.31161) H11B(0.31161) C12(0.31161) H12A(0.31161)
 H12B(0.31161) C13(0.31161) H13A(0.31161) H13B(0.31161) C14(0.31161)
 H14A(0.31161) H14B(0.31161) C15(0.31161) H15A(0.31161) H15B(0.31161)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,
 H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
  C15(H15A,H15B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,
 H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
  C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_estimated_absorpt_t_min   0.458
_shelx_estimated_absorpt_t_max   0.748
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              66732
_shelx_hkl_checksum              32810
_shelx_fab_checksum              99770