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_1567565
_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_absolute_configuration ad
_chemical_formula_moiety         'C54 H85 Cl N4 O3 U, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H101 Cl N4 O5 U'
_chemical_formula_weight         1255.94
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-17
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.083(3)
_cell_length_b                   17.018(3)
_cell_length_c                   24.513(5)
_cell_measurement_reflns_used    9181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.32
_cell_measurement_theta_min      2.14
_cell_volume                     6292(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_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  0.1095
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            179377
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.450
_diffrn_reflns_theta_min         1.457
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.670
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1214 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.7618.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         6.097
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Flack x determined using 4901 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         14173
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0738P)^2^+10.0893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                12099
_reflns_number_total             14173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02736d2.cif
_cod_data_source_block           jbh1704
_cod_database_code               1567565
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.604
_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
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim O110 \\sim C111 \\sim
C112 \\sim C113 \\sim C114: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
3. Same fragment restrains
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O110, C111, C112, C113, C114}
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O200, C201, C202, C203, C204}
4. Others
 Sof(O110)=Sof(C111)=Sof(H11A)=Sof(H11B)=Sof(C112)=Sof(H11C)=Sof(H11D)=
 Sof(C113)=Sof(H11E)=Sof(H11F)=Sof(C114)=Sof(H11G)=Sof(H11H)=1-FVAR(1)
 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(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),
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C111(H11A,
 H11B), C112(H11C,H11D), C113(H11E,H11F), C114(H11G,H11H), C201(H20A,H20B),
 C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C28(H28), C30(H30), C43(H43), C45(H45)
5.c 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), C54(H54A,
 H54B,H54C)
;
_shelx_res_checksum              89486
_shelx_hkl_checksum              10236
_olex2_submission_special_instructions 'No special instructions were received'