Triamidoamine uranium(IV)-arsenic complexes containing one-, two- and threefold U-As bonding interactions
Benedict M. Gardner; Gabor Balazs; Manfred Scheer; Floriana Tuna; Eric J. L. McInnes; Jonathan McMaster; William Lewis; Alexander J. Blake; Stephen T. Liddle; Nature Chemistry 7 (2015) 582–590; doi:10.1038/nchem.2279

data_1551967
_publ_section_title
;
 Triamidoamine uranium(IV)-arsenic complexes containing one-, two- and
 threefold U-As bonding interactions
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              582
_journal_page_last               590
_journal_paper_doi               10.1038/nchem.2279
_journal_volume                  7
_journal_year                    2015
_chemical_formula_moiety
'C66 H150 As3 N8 Si6 U2, C28 H40 K O10, C7 H8'
_chemical_formula_sum            'C101 H198 As3 K N8 O10 Si6 U2'
_chemical_formula_weight         2593.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.065(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1907(4)
_cell_length_b                   20.1898(5)
_cell_length_c                   22.7981(6)
_cell_measurement_reflns_used    20980
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4140
_cell_measurement_theta_min      4.0060
_cell_volume                     5862.9(3)
_computing_cell_refinement
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)

(compiled Jan 14 2014,18:38:05)

;
_computing_data_collection
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)

(compiled Jan 14 2014,18:38:05)

;
_computing_data_reduction
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)

(compiled Jan 14 2014,18:38:05)

;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;

  1 omega  -77.00  -51.00   1.0000   20.0000

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  125.0000  -30.0000 26

  2 omega  -50.00   34.00   1.0000   20.0000

omega____ theta____ kappa____ phi______ frames

    -      -38.5000   38.0000  -30.0000 84

  3 omega -109.00  -12.00   1.0000   20.0000

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  -57.0000 -180.0000 97

  4 omega  -41.00   -9.00   1.0000   20.0000

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  125.0000  -30.0000 32

  5 omega   53.00   80.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -30.0000   60.0000 27

  6 omega   41.00  134.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -77.0000  150.0000 93

  7 omega   36.00  119.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -77.0000  -60.0000 83

  8 omega   75.00  169.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322   15.0000 -150.0000 94

  9 omega   51.00   77.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -45.0000    0.0000 26

 10 omega   38.00   91.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -45.0000  150.0000 53

 11 omega   83.00  175.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322   45.0000   90.0000 92

 12 omega -109.00  -12.00   1.0000   20.0000

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  -57.0000   60.0000 97

 13 omega   17.00  113.00   1.0000   20.0000

omega____ theta____ kappa____ phi______ frames

    -       43.3152   57.0000    0.0000 96

 14 omega  -29.00   66.00   1.0000   20.0000

omega____ theta____ kappa____ phi______ frames

    -       43.3152  -38.0000   60.0000 95

 15 omega   35.00   60.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322 -125.0000  150.0000 25

 16 omega   82.00  177.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322   45.0000   30.0000 95

 17 omega   61.00  178.00   1.0000   80.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322   15.0000  -30.0000 117

;
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0314015000
_diffrn_orient_matrix_UB_12      -0.0464945000
_diffrn_orient_matrix_UB_13      -0.0458790000
_diffrn_orient_matrix_UB_21      0.0362389000
_diffrn_orient_matrix_UB_22      -0.0524078000
_diffrn_orient_matrix_UB_23      0.0502318000
_diffrn_orient_matrix_UB_31      -0.1109950000
_diffrn_orient_matrix_UB_32      -0.0302994000
_diffrn_orient_matrix_UB_33      -0.0164334000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43935
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.635
_diffrn_reflns_theta_min         3.528
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    9.986
_exptl_absorpt_correction_T_max  0.575
_exptl_absorpt_correction_T_min  0.108
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)

(compiled Jan 14 2014,18:38:05)

Numerical absorption correction based on gaussian integration over

a multifaceted crystal model

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       needle
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.2893
_exptl_crystal_size_mid          0.0429
_exptl_crystal_size_min          0.0343
_refine_diff_density_max         5.841
_refine_diff_density_min         -3.399
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         11750
_refine_ls_number_restraints     2196
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0839P)^2^+56.3575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10067
_reflns_number_total             11750
_reflns_threshold_expression     'I > 2s(I)'
_cod_data_source_file            nchem.2279-s7.cif
_cod_data_source_block           6
_cod_database_code               1551967
_chemical_oxdiff_formula         C66H150As3KN8O10Si6U2
_chemical_oxdiff_usercomment
'UBMGOI #13809 SN-227 for BMG/STL in fomblin oil on micromount'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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

 H21A-H17D

 -2 with sigma of 0.02

 H22B-H16F

 -2 with sigma of 0.02

 Si1-N1 sim Si1A-N1

 with sigma of 0.02

 Si1-C1 sim Si1A-C1A sim Si1-C7 sim Si1A-C7A sim Si1-C4 sim Si1A-C4A

 with sigma of 0.02

 C3-C1 sim C3A-C1A sim C2-C1 sim C8A-C7A sim C8-C7 sim C9A-C7A sim

C9-C7 sim C5-C4 sim C5A-C4A

 sim C6-C4 sim C6A-C4A

 with sigma of 0.02

 Si2A-C18A sim Si2-C18 sim Si2A-C15A sim Si2-C15 sim Si2A-C12A sim

Si2-C12

 with sigma of 0.02

 C19-C18 sim C20-C18 sim C19A-C18A sim C20A-C18A sim C14A-C12A sim

C14-C12 sim C13-C12

 C13A-C12A sim C16-C15 sim C17-C15 sim C16A-C15A sim C17A-C15A

 with sigma of 0.02

 C47-C42 sim C47A-C42A

 with sigma of 0.02

 C47-C46 sim C47A-C46A sim C43-C42 sim C43A-C42A

 with sigma of 0.02

 C46-C45 sim C46A-C45A sim C44-C43 sim C44A-C43A

 with sigma of 0.02

 C45-C44 sim C45A-C44A

 with sigma of 0.02

 O1-C47 sim O1A-C47A sim O5-C42 sim O5A-C42A

 with sigma of 0.02

 O1A-C34A sim O1-C34 sim O5-C41 sim O5A-C41A

 with sigma of 0.02

 C41A-C40A sim C41-C40 sim C35A-C34A sim C35-C34

 with sigma of 0.02

 O2A-C35A sim O2-C35 sim O4-C40 sim O4A-C40A

 with sigma of 0.02

 O4-C39 sim O4A-C39A sim O2A-C36A sim O2-C36

 with sigma of 0.02

 C37A-C36A sim C37-C36 sim C39-C38 sim C39A-C38A

 with sigma of 0.02

 O3-C38 sim O3A-C38A sim O3-C37 sim O3A-C37A

 with sigma of 0.02

3. Uiso/Uaniso restraints and constraints

All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma

for terminal atoms of 0.08

4. Rigid body (RIGU) restrains

 All non-hydrogen atoms

 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004

5. Others

 Sof(Si1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=

 Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=

 Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7A)=Sof(C8A)=

 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)

 Sof(Si1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=

 Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=

 Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=

 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)

 Sof(Si2A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=

 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15A)=Sof(C16A)=

 Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=

 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=

 Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(2)

 Sof(Si2)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=

 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=

 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)=Sof(C19)=

 Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(2)

 Sof(O1A)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(O2A)=

 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(O3A)=Sof(C38A)=

 Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(O4A)=Sof(C40A)=Sof(H40C)=

 Sof(H40D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(O5A)=Sof(C42A)=Sof(C43A)=Sof(H43A)=

 Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=1-FVAR(3)

 Sof(O1)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O2)=

 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(O3)=Sof(C38)=

 Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(O4)=Sof(C40)=Sof(H40A)=

 Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(O5)=Sof(C42)=Sof(C43)=Sof(H43)=

 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=FVAR(3)

 Fixed Sof: C49(0.5) H49(0.5) H50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C51(0.5)

 H51(0.5) C53(0.5)

6.a Ternary CH refined with riding coordinates:

 C1(H1), C1A(H1A), C4(H4), C4A(H4A), C7(H7), C7A(H7A), C12(H12), C12A(H12A),

 C15(H15), C15A(H15A), C18(H18), C18A(H18A), C23(H23), C26(H26), C29(H29)

6.b Secondary CH2 refined with riding coordinates:

 C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,

 H32B), C33(H33A,H33B), C34(H34A,H34B), C34A(H34C,H34D), C35(H35A,H35B),

 C35A(H35C,H35D), C36(H36A,H36B), C36A(H36C,H36D), C37(H37A,H37B), C37A(H37C,

 H37D), C38(H38A,H38B), C38A(H38C,H38D), C39(H39A,H39B), C39A(H39C,H39D),

 C40(H40A,H40B), C40A(H40C,H40D), C41(H41A,H41B), C41A(H41C,H41D)

6.c Aromatic/amide H refined with riding coordinates:

 C43(H43), C43A(H43A), C44(H44), C44A(H44A), C45(H45), C45A(H45A), C46(H46),

 C46A(H46A), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)

6.d Idealised Me refined as rotating group:

 C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC),

 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC),

 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),

 C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,H14E,

 H14F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C17(H17A,H17B,H17C),

 C17A(H17D,H17E,H17F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,

 H20C), C20A(H20D,H20E,H20F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),

 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,

 H31C), C50(H50A,H50B,H50C)

;