A complete series of uranium(iv) complexes with terminal hydrochalcogenido (EH) and chalcogenido (E) ligands E = O, S, Se, Te.
Rosenzweig, Michael W.; Hümmer, Julian; Scheurer, Andreas; Lamsfus, Carlos Alvarez; Heinemann, Frank W.; Maron, Laurent; Mazzanti, Marinella; Meyer, Karsten; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10853–10864; doi:10.1039/c9dt00530g

data_7049440
_publ_section_title
;
 A complete series of uranium(iv) complexes with terminal
 hydrochalcogenido (EH) and chalcogenido (E) ligands E = O, S, Se, Te.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10853
_journal_page_last               10864
_journal_paper_doi               10.1039/c9dt00530g
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H79 N3 O3 Se1 U1, 3.25(C4 H8 O)'
_chemical_formula_sum            'C73 H105 N3 O6.25 Se U'
_chemical_formula_weight         1441.58
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-01-25 deposited with the CCDC.    2019-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   20.3282(6)
_cell_length_b                   20.3282(6)
_cell_length_c                   18.6007(6)
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.28
_cell_volume                     6656.7(4)
_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-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Triumph curved graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            134384
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.617
_diffrn_reflns_theta_min         1.157
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0789 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.8540.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       prism
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
 Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         2.120
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 4851 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         12439
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+5.9766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                10689
_reflns_number_total             12439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00530g2.cif
_cod_data_source_block           mr1521sq
_cod_depositor_comments
'Adding full bibliography for 7049435--7049440.cif.'
_cod_database_code               7049440
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.453
_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 Se(H) groups
2. Restrained distances
 C101-C102 = C102-C103 = C103-C104
 1.54 with sigma of 0.02
 C201-C202 = C202-C203 = C203-C204
 1.54 with sigma of 0.02
3. Rigid bond restraints
 U1, Se1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 U2, Se2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: 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
Uanis(O100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O200) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq,
Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Se1) \\sim Ueq, Uanis(Se2) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
5. Same fragment restrains
{O200, C201, C202, C203, C204} sigma for 1-2: 0.02, 1-3: 0.04
as
{O100, C101, C102, C103, C104}
{O200, C204, C203, C202, C201} sigma for 1-2: 0.02, 1-3: 0.04
as
{O200, C201, C202, C203, C204}
6. Others
 Fixed Sof: H1(0.33333) H2(0.33333) O200(0.5) C201(0.5) H20D(0.5) H20E(0.5)
 C202(0.5) H20F(0.5) H20G(0.5) C203(0.5) H20H(0.5) H20I(0.5) C204(0.5)
 H20J(0.5) H20K(0.5)
7.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C31(H31), C32(H32), C33(H33)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C101(H10A,H10B),
 C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C201(H20D,H20E), C202(H20F,
 H20G), C203(H20H,H20I), C204(H20J,H20K)
7.c Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C40(H40A,H40B,H40C)
7.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C27(H27), C29(H29)
7.e Tetrahedral OH refined with riding coordinates:
 Se1(H1), Se2(H2)
;
_shelx_res_checksum              64407
_olex2_submission_special_instructions 'No special instructions were received'