Uranium Tetrakis-Aryloxide Derivatives Supported by Tetraazacyclododecane: Synthesis of Air-Stable, Coordinatively-Unsaturated U(IV) and U(V) Complexes.
Hümmer, Julian; Heinemann, Frank W.; Meyer, Karsten; Inorganic chemistry 56 (2017) 3201–3206; doi:10.1021/acs.inorgchem.6b02123

data_4344931
_publ_section_title
;
 Uranium Tetrakis-Aryloxide Derivatives Supported by
 Tetraazacyclododecane: Synthesis of Air-Stable,
 Coordinatively-Unsaturated U(IV) and U(V) Complexes.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3201
_journal_page_last               3206
_journal_paper_doi               10.1021/acs.inorgchem.6b02123
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C44 H56 N4 O4 U, F6 Sb, C4 H8 O, C4 H10 O'
_chemical_formula_sum            'C52 H74 F6 N4 O6 Sb U'
_chemical_formula_weight         1324.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                102.392(2)
_cell_angle_beta                 99.172(2)
_cell_angle_gamma                92.988(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5028(13)
_cell_length_b                   13.2490(15)
_cell_length_c                   17.1043(19)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.38
_cell_volume                     2721.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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-2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            94508
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.899
_diffrn_reflns_theta_min         1.238
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.539
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0652 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.7990.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14094
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0153P)^2^+7.2058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12732
_reflns_number_total             14094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02123_si_003.cif
_cod_data_source_block           jbh1503
_cod_depositor_comments
'Adding full bibliography for 4344930--4344931.cif.'
_cod_database_code               4344931
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.460
_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. Restrained distances
 C214-C215
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C201 \\sim C202 \\sim O203 \\sim C204 \\sim C205 \\sim C211 \\sim C212 \\sim
O213 \\sim C214 \\sim C215: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C205: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C204: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O203: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C202: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq, Uanis(O203) \\sim Ueq,
Uanis(C204) \\sim Ueq, Uanis(C205) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C211) \\sim Ueq, Uanis(C212) \\sim Ueq, Uanis(O213) \\sim Ueq,
Uanis(C214) \\sim Ueq, Uanis(C215) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Same fragment restrains
{C201, C202, O203, C204, C205} sigma for 1-2: 0.02, 1-3: 0.04
as
{C211, C212, O213, C214, C215}
5. Others
 Sof(C211)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C212)=Sof(H21D)=Sof(H21E)=
 Sof(O213)=Sof(C214)=Sof(H21F)=Sof(H21G)=Sof(C215)=Sof(H21H)=Sof(H21I)=
 Sof(H21J)=1-FVAR(1)
 Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C202)=Sof(H20D)=Sof(H20E)=
 Sof(O203)=Sof(C204)=Sof(H20F)=Sof(H20G)=Sof(C205)=Sof(H20H)=Sof(H20I)=
 Sof(H20J)=FVAR(1)
6.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), C18(H18A,H18B), C27(H27A,H27B),
 C36(H36A,H36B), C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,
 H10H), C202(H20D,H20E), C204(H20F,H20G), C212(H21D,H21E), C214(H21F,H21G)
6.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C22(H22), C24(H24), C31(H31), C33(H33), C40(H40), C42(H42)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C201(H20A,H20B,H20C), C205(H20H,H20I,H20J), C211(H21A,H21B,H21C),
 C215(H21H,H21I,H21J)
;
_shelx_res_checksum              59824
_shelx_hkl_checksum              2734
_olex2_submission_special_instructions 'No special instructions were received'