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_7049435
_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_formula_moiety         'C60 H79 N3 O4 U, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H95 N3 O6 U'
_chemical_formula_weight         1288.49
_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   mixed
_audit_creation_date             2019-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-25 deposited with the CCDC.    2019-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                75.002(3)
_cell_angle_beta                 83.542(3)
_cell_angle_gamma                80.041(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4689(11)
_cell_length_b                   12.8625(13)
_cell_length_c                   23.576(2)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.13
_cell_measurement_theta_min      2.23
_cell_volume                     3012.6(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-2016/6 (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 0.994
_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  0.0698
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.205
_diffrn_reflns_theta_min         1.658
_exptl_absorpt_coefficient_mu    2.748
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0697 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.8918.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.308
_refine_diff_density_min         -1.977
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         13383
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0252P)^2^+7.5131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11542
_reflns_number_total             13383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00530g2.cif
_cod_data_source_block           mr1522
_cod_depositor_comments
'Adding full bibliography for 7049435--7049440.cif.'
_cod_database_code               7049435
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.771
_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
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204 \\sim O210 \\sim C211 \\sim
C212 \\sim C213 \\sim C214: 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
{O200, C201, C202, C203, C204}
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O210, C211, C212, C213, C214}
4. Others
 Sof(O210)=Sof(C211)=Sof(H21C)=Sof(H21D)=Sof(C212)=Sof(H21E)=Sof(H21F)=
 Sof(C213)=Sof(H21G)=Sof(H21H)=Sof(C214)=Sof(H21I)=Sof(H21J)=1-FVAR(1)
 Sof(O200)=Sof(C201)=Sof(H20C)=Sof(H20D)=Sof(C202)=Sof(H20E)=Sof(H20F)=
 Sof(C203)=Sof(H20G)=Sof(H20H)=Sof(C204)=Sof(H20I)=Sof(H20J)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C33(H33), C34(H34), C35(H35), C51(H51),
 C52(H52), C53(H53)
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), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C36(H36A,H36B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,
 H43B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C101(H10A,H10B), C102(H10C,H10D), C103(H10E,
 H10F), C104(H10G,H10H), C201(H20C,H20D), C202(H20E,H20F), C203(H20G,H20H),
 C204(H20I,H20J), C211(H21C,H21D), C212(H21E,H21F), C213(H21G,H21H), C214(H21I,
 H21J)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C29(H29), C31(H31), C47(H47), C49(H49)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              33987
_olex2_submission_special_instructions 'No special instructions were received'