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_1567569
_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 H86 N4 O4 U, F6 Sb, 3.5(C6 H6)'
_chemical_formula_sum            'C75 H107 F6 N4 O4 Sb U'
_chemical_formula_weight         1602.42
_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   mixed
_audit_creation_date             2019-11-20
_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                 113.0460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6848(8)
_cell_length_b                   12.0981(5)
_cell_length_c                   27.9247(11)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.41
_cell_volume                     7363.0(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            128434
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.598
_diffrn_reflns_theta_min         1.861
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1001 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.8537.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             3256
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         20670
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+13.8614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17059
_reflns_number_total             20670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02736d2.cif
_cod_data_source_block           jbh1908
_cod_database_code               1567569
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.635
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C53 \\sim C51A \\sim C52A \\sim C53A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
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
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C51A)
\\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(C53A) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
3. Others
 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(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)
4.a Riding coordinates:
 O4(H4)
4.b 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)
4.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)
4.d Fitted hexagon refined as free rotating group:
 C301(C302,C303,C304,C305,C306)
4.e Idealised Me refined as rotating group:
 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)
;
_shelx_res_checksum              2543
_shelx_hkl_checksum              54585
_olex2_submission_special_instructions 'No special instructions were received'