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_4344930
_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, 5(C4 H8 O)'
_chemical_formula_sum            'C64 H96 N4 O9 U'
_chemical_formula_weight         1303.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 119.4543(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.123(4)
_cell_length_b                   12.1958(14)
_cell_length_c                   17.838(2)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.43
_cell_volume                     6274.5(13)
_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      180.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            103302
_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         28.719
_diffrn_reflns_theta_min         1.412
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.644
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0510 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.8772.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         8103
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0512P)^2^+5.2625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7388
_reflns_number_total             8103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02123_si_002.cif
_cod_data_source_block           jbh1501
_cod_depositor_comments
'Adding full bibliography for 4344930--4344931.cif.'
_cod_original_cell_volume        6274.5(12)
_cod_database_code               4344930
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.742
_shelx_estimated_absorpt_t_min   0.662
_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
 C101-C102 = C102-C103 = C103-C104
 1.54 with sigma of 0.01
 O100-C101 = O100-C104
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C301) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O200, C201, C202, C203, C204}
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C14(H14A,
 H14B), C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H),
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C301(H30A,
 H30B), C302(H30C,H30D)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C18(H18), C20(H20)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              90647
_shelx_hkl_checksum              36046
_olex2_submission_special_instructions 'No special instructions were received'