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_1567568
_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, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H102 N4 O6 U'
_chemical_formula_weight         1237.50
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-09-24
_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                 90.093(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7445(6)
_cell_length_b                   16.3263(9)
_cell_length_c                   37.618(2)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.33
_cell_volume                     6598.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            165247
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.737
_diffrn_reflns_theta_min         1.083
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.506
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0745 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.8517.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             2568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran, n-hexane'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.610
_refine_diff_density_min         -2.972
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         17052
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0357
_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/[\s^2^(Fo^2^)+(0.0292P)^2^+11.8956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14244
_reflns_number_total             17052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02736d2.cif
_cod_data_source_block           jbh1802_sq
_cod_database_code               1567568
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.530
_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
C21 \\sim C22 \\sim C23 \\sim C21A \\sim C22A \\sim C23A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim O110 \\sim C110 \\sim
C112 \\sim C113 \\sim C114: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
3. Same fragment restrains
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O110, C110, C112, C113, C114}
4. Others
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(O110)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(C112)=Sof(H11C)=Sof(H11D)=
 Sof(C113)=Sof(H11E)=Sof(H11F)=Sof(C114)=Sof(H11G)=Sof(H11H)=1-FVAR(2)
 Sof(O100)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(C102)=Sof(H10C)=Sof(H10D)=
 Sof(C103)=Sof(H10E)=Sof(H10F)=Sof(C104)=Sof(H10G)=Sof(H10H)=FVAR(2)
5.a Riding coordinates:
 O4(H4)
5.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),
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C110(H11A,
 H11B), C112(H11C,H11D), C113(H11E,H11F), C114(H11G,H11H), C201(H20A,H20B),
 C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H)
5.c 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), C21A(H21D,H21E,H21F),
 C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), 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), C54(H54A,H54B,
 H54C)
5.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C28(H28), C30(H30), C43(H43), C45(H45)
;
_shelx_res_checksum              43888
_shelx_hkl_checksum              82650
_shelx_fab_checksum              52042
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'