Unprecedented pairs of uranium (iv/v) hydroxido and (iv/v/vi) oxido complexes supported by a seven-coordinate cyclen-anchored tris-aryloxide ligand
Löffler, Sascha T.; Hümmer, Julian; Scheurer, Andreas; Heinemann, Frank W.; Meyer, Karsten; Chemical Science  (2022) –; doi:10.1039/D2SC02736D

data_1567571
_publ_section_title
;
 Unprecedented pairs of uranium (iv/v) hydroxido and (iv/v/vi) oxido
 complexes supported by a seven-coordinate cyclen-anchored tris-aryloxide
 ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02736D
_journal_year                    2022
_chemical_formula_moiety         'C54 H85 N4 O4 U, F6 Sb, 3.5(C6 H6)'
_chemical_formula_sum            'C75 H106 F6 N4 O4 Sb U'
_chemical_formula_weight         1601.41
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-08 deposited with the CCDC.	2022-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.169(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6833(13)
_cell_length_b                   12.0691(6)
_cell_length_c                   27.9262(13)
_cell_measurement_reflns_used    9451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.22
_cell_volume                     7338.5(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'Bruker APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ImuS Duo Photon II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS high brilliance micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            280430
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         2.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.636
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0859 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.9070.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       needle
_exptl_crystal_F_000             3252
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.876
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         18961
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0390
_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/[\s^2^(Fo^2^)+(0.0207P)^2^+23.9179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16039
_reflns_number_total             18961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02736d2.cif
_cod_data_source_block           jbh1907
_cod_original_cell_volume        7338.5(6)
_cod_database_code               1567571
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C50 \\sim C51 \\sim C52 \\sim C53 \\sim C50A \\sim C51A \\sim C52A \\sim C53A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C301 \\sim C302 \\sim C303 \\sim C304 \\sim C305 \\sim C306: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
3. Same fragment restrains
{C46, C47, C48, C49} sigma for 1-2: 0.02, 1-3: 0.04
as
{C50, C51, C52, C53}
{C46, C47, C48, C49} sigma for 1-2: 0.02, 1-3: 0.04
as
{C50A, C51A, C52A, C53A}
{C201, C202, C203, C204, C205, C206} sigma for 1-2: 0.02, 1-3: 0.04
as
{C101, C102, C103, C104, C105, C106}
{C201, C202, C203, C204, C205, C206} sigma for 1-2: 0.02, 1-3: 0.04
as
{C301, C302, C303, C304, C305, C306}
4. Others
 Sof(C50A)=Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52A)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(1)
 Sof(C50)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(1)
5.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), C24(H24A,H24B), C39(H39A,H39B)
5.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F), C53A(H53D,H53E,H53F), C54(H54A,
 H54B,H54C)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C28(H28), C30(H30), C43(H43), C45(H45), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C201(H201),
 C202(H202), C203(H203), C204(H204), C205(H205), C206(H206), C301(H301),
 C302(H302), C303(H303), C304(H304), C305(H305), C306(H306), C401(H401),
 C402(H402), C403(H403)
;
_shelx_res_checksum              40449
_shelx_hkl_checksum              46415
_olex2_submission_special_instructions 'No special instructions were received'