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_7049439
_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 O3 Te U, 3(C1 H2 Cl2)'
_chemical_formula_sum            'C63 H85 Cl6 N3 O3 Te U'
_chemical_formula_weight         1510.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90.534(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3450(4)
_cell_length_b                   25.1895(11)
_cell_length_c                   23.6311(9)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.29
_cell_volume                     6157.7(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(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            110112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.128
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.408
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8206.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.317
_refine_diff_density_min         -3.020
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         12556
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0502P)^2^+67.7713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9464
_reflns_number_total             12556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00530g2.cif
_cod_data_source_block           mr1528
_cod_depositor_comments
'Adding full bibliography for 7049435--7049440.cif.'
_cod_database_code               7049439
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.508
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9966(4)
 0.0034(4)
2. 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 Te(H) groups
3. Uiso/Uaniso restraints and constraints
C1 \\sim C6 \\sim N1: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C100 \\sim Cl11 \\sim Cl12 \\sim C101 \\sim Cl13 \\sim Cl14: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C200 \\sim Cl21 \\sim Cl22 \\sim C201 \\sim Cl23 \\sim Cl24: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C300 \\sim Cl31 \\sim Cl32 \\sim C301 \\sim Cl33 \\sim Cl34: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(Cl31) \\sim Ueq, Uanis(Cl32) \\sim Ueq, Uanis(Cl33) \\sim Ueq,
Uanis(Cl34) \\sim Ueq, Uanis(Cl24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Same fragment restrains
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C101, Cl13, Cl14}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C200, Cl21, Cl22}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C201, Cl23, Cl24}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C300, Cl31, Cl32}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C301, Cl33, Cl34}
5. Others
 Sof(C301)=Sof(H30C)=Sof(H30D)=Sof(Cl33)=Sof(Cl34)=1-FVAR(1)
 Sof(C300)=Sof(H30A)=Sof(H30B)=Sof(Cl31)=Sof(Cl32)=FVAR(1)
 Sof(C201)=Sof(H20E)=Sof(H20F)=Sof(Cl23)=Sof(Cl24)=1-FVAR(2)
 Sof(C200)=Sof(H20C)=Sof(H20D)=Sof(Cl21)=Sof(Cl22)=FVAR(2)
 Sof(C101)=Sof(H10C)=Sof(H10D)=Sof(Cl13)=Sof(Cl14)=1-FVAR(3)
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(Cl11)=Sof(Cl12)=FVAR(3)
6.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)
6.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), C100(H10A,H10B), C101(H10C,H10D), C200(H20C,
 H20D), C201(H20E,H20F), C300(H30A,H30B), C301(H30C,H30D)
6.c Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C60(H60A,H60B,H60C)
6.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C29(H29), C31(H31), C47(H47), C49(H49)
6.e Idealised tetrahedral OH refined as rotating group:
 Te1(H1)
;
_shelx_res_checksum              55149
_olex2_submission_special_instructions 'No special instructions were received'