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_1551966
_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         'C51 H112 As K N6 O6 Si3 U, 0.25(C6H14)'
_chemical_formula_sum            'C52.5 H115.5 As K N6 O6 Si3 U'
_chemical_formula_weight         1363.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   'geom, As-H from difmap'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                88.3008(13)
_cell_angle_beta                 89.3347(14)
_cell_angle_gamma                68.8052(19)
_cell_formula_units_Z            4
_cell_length_a                   15.3188(3)
_cell_length_b                   18.8965(4)
_cell_length_c                   24.8556(3)
_cell_measurement_reflns_used    31824
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3130
_cell_measurement_theta_min      3.1050
_cell_volume                     6705.3(2)
_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)'
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_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 0.997
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;

  1 omega  -94.00  -11.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  125.0000  -60.0000 83

  2 omega  -26.00   25.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000   38.0000 -120.0000 51

  3 omega  -42.00   29.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000   38.0000 -150.0000 71

  4 omega  -37.00  -12.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  125.0000 -150.0000 25

  5 omega -111.00  -19.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  -38.0000   60.0000 92

  6 omega   55.00   81.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -       43.3152 -125.0000 -120.0000 26

  7 omega   57.00  117.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322 -125.0000 -150.0000 60

  8 omega   32.00   70.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -30.0000  -60.0000 38

  9 omega   40.00   66.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -30.0000  120.0000 26

 10 omega   82.00  175.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322   30.0000 -180.0000 93

 11 omega   39.00   96.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -45.0000   60.0000 57

 12 omega   26.00  109.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -95.0000 -150.0000 83

 13 omega  151.00  177.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  125.0000 -120.0000 26

 14 omega   34.00   91.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -30.0000 -120.0000 57

 15 omega   31.00   89.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -30.0000    0.0000 58

 16 omega   40.00   66.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -30.0000  150.0000 26

 17 omega  102.00  128.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  125.0000   90.0000 26

 18 omega   56.00  115.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322 -125.0000   30.0000 59

 19 omega   84.00  119.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322 -125.0000   90.0000 35

 20 omega  139.00  178.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  125.0000   60.0000 39

 21 omega   61.00  160.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322   15.0000  -60.0000 99

 22 omega   36.00  103.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -61.0000    0.0000 67

 23 omega   36.00   89.00   1.0000    5.0000

omega____ theta____ kappa____ phi______ frames

    -      106.1322  -61.0000 -150.0000 53

 24 omega -112.00   -7.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  -77.0000 -120.0000 105

 25 omega  -50.00   34.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000   38.0000  150.0000 84

 26 omega -109.00  -12.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -      -38.5000  -57.0000  -30.0000 97

 27 omega   17.00   60.00   1.0000    1.2500

omega____ theta____ kappa____ phi______ frames

    -       43.3152   57.0000 -180.0000 43

;
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.1047289000
_diffrn_orient_matrix_UB_12      -0.0111843000
_diffrn_orient_matrix_UB_13      -0.0009703000
_diffrn_orient_matrix_UB_21      0.0253083000
_diffrn_orient_matrix_UB_22      -0.0855352000
_diffrn_orient_matrix_UB_23      -0.0085519000
_diffrn_orient_matrix_UB_31      -0.0050752000
_diffrn_orient_matrix_UB_32      0.0145003000
_diffrn_orient_matrix_UB_33      -0.0614076000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            64713
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.776
_diffrn_reflns_theta_min         3.094
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    8.776
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.116
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plank
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.6148
_exptl_crystal_size_mid          0.1607
_exptl_crystal_size_min          0.1377
_refine_diff_density_max         7.034
_refine_diff_density_min         -2.772
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1520
_refine_ls_number_reflns         26670
_refine_ls_number_restraints     1514
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+(0.0947P)^2^+26.6612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                23895
_reflns_number_total             26670
_reflns_threshold_expression     'I > 2s(I)'
_cod_data_source_file            nchem.2279-s6.cif
_cod_data_source_block           5
_cod_depositor_comments
;

2022-12-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C105 H231 As2 K2 N12 O12 Si6 U2'
_cod_original_formula_weight         2726.63
_cod_original_formula_moiety         '2(C51 H112 As K N6 O6 Si3 U), 0.5(C6H14)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        6705.4(2)
_cod_database_code               1551966
_chemical_oxdiff_formula         C102H222As2K2N12O12Si6U2
_chemical_oxdiff_usercomment
'UBMGOJ #13825 SN-216 for BMG/STL in fomblin oil on micromount'
_reflns_odcompleteness_completeness 99.73
_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, All As(H) groups

2. Restrained distances

 As1-H1

 1.58 with sigma of 0.01

 As2-H2

 1.58 with sigma of 0.01

 As2-H2 sim As1-H1

 with sigma of 0.02

 U1-H1 sim U2-H2

 with sigma of 0.02

 C97-C85 sim C97-C91 sim C85-C91

 with sigma of 0.02

 C102-C96 sim C102-C90 sim C90-C96

 with sigma of 0.02

 C103-C115 sim C103-C109 sim C115-C109 sim C108-C120

 with sigma of 0.02

 C89-C90 sim C103-C104 sim C108-C107 sim C86-C85

 with sigma of 0.02

 O14-C107 sim O7-C86 sim O13-C104 sim O8-C89

 with sigma of 0.02

 O15-C110 sim O12-C101 sim O16-C113 sim O18-C119 sim O11-C98 sim

O9-C92 sim O17-C116 sim O10-

 C95

 with sigma of 0.02

 O15-C111 sim O10-C94 sim O12-C100 sim O16-C112 sim O18-C118 sim

O11-C99 sim O9-C93 sim O17-

 C117

 with sigma of 0.02

 C99-C100 sim C118-C117 sim C94-C93 sim C112-C111

 with sigma of 0.02

 N12-C102 sim N12-C90 sim N12-C96 sim N14-C108 sim N14-C120 sim

N11-C85 sim N11-C97 sim N11-

 C91 sim N13-C103 sim N13-C115 sim N13-C109

 with sigma of 0.02

 C116-C115 sim C110-C109 sim C95-C96 sim C102-C101 sim C120-C119 sim

C97-C98 sim C92-C91

 with sigma of 0.02

 O14-C106 sim O13-C105 sim O8-C88

 with sigma of 0.02

 O7-C87 sim O8-C88 sim O14-C106 sim O13-C105

 with sigma of 0.02

 C88-C87 sim C106-C105

 with sigma of 0.02

3. Uiso/Uaniso restraints and constraints

C65 sim C63 sim C64: within 1.7A with sigma of 0.005 and sigma for terminal

atoms of 0.01

K2 sim C110 sim C101 sim O10 sim O9 sim N11 sim C95 sim O11 sim

C93 sim N14 sim O17 sim O12 sim C97 sim C92 sim O18 sim N13 sim

O8 sim O7 sim C96 sim O14 sim O13 sim C117 sim C100 sim C91 sim

N12 sim C104 sim C90 sim C89 sim C85 sim C103 sim C86 sim C108

sim C107 sim C102 sim C106 sim C115 sim C105 sim C114 sim C119

sim C98 sim C116 sim O15 sim C113 sim C111 sim C109 sim C99 sim

C120 sim C88 sim O16 sim C94 sim C118 sim C112 sim C87: within 1.7A

with sigma of 0.005 and sigma for terminal atoms of 0.01

4. Rigid body (RIGU) restrains

 C65, C63, C64

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

 K2, C110, C101, O10, O9, N11, C95, O11, C93, N14, O17, O12, C97, C92, O18,

 N13, O8, O7, C96, O14, O13, C117, C100, C91, N12, C104, C90, C89, C85, C103,

 C86, C108, C107, C102, C106, C115, C105, C114, C119, C98, C116, O15, C113,

 C111, C109, C99, C120, C88, O16, C94, C118, C112, C87

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

5. Others

 Sof(N13)=Sof(C103)=Sof(H10G)=Sof(H10H)=Sof(C104)=Sof(H10I)=Sof(H10J)=Sof(O13)=

 Sof(C105)=Sof(H10K)=Sof(H10L)=Sof(C106)=Sof(H10M)=Sof(H10N)=Sof(O14)=Sof(C107)=

 Sof(H10O)=Sof(H10P)=Sof(C108)=Sof(H10Q)=Sof(H10R)=Sof(C109)=Sof(H10S)=

 Sof(H10T)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(O15)=Sof(C111)=Sof(H11C)=Sof(H11D)=

 Sof(C112)=Sof(H11E)=Sof(H11F)=Sof(O16)=Sof(C113)=Sof(H11G)=Sof(H11H)=Sof(C114)=

 Sof(H11I)=Sof(H11J)=Sof(C115)=Sof(H11K)=Sof(H11L)=Sof(C116)=Sof(H11M)=

 Sof(H11N)=Sof(O17)=Sof(C117)=Sof(H11O)=Sof(H11P)=Sof(C118)=Sof(H11Q)=Sof(H11R)=

 Sof(O18)=Sof(C119)=Sof(H11S)=Sof(H11T)=Sof(C120)=Sof(H12A)=Sof(H12B)=Sof(N14)=

 1-FVAR(1)

 Sof(N11)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(O7)=

 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(O8)=Sof(C89)=

 Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=Sof(H91B)=

 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(O9)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=

 Sof(H94A)=Sof(H94B)=Sof(O10)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=

 Sof(H96B)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(O11)=

 Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(O12)=Sof(C101)=

 Sof(H10C)=Sof(H10D)=Sof(C102)=Sof(H10E)=Sof(H10F)=Sof(N12)=FVAR(1)

6.a Ternary CH refined with riding coordinates:

 C2(H2A), C4(H4), C7(H7), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26),

 C29(H29), C52(H52), C55(H55), C58(H58), C63(H63), C66(H66), C69(H69), C74(H74),

  C77(H77), C80(H80)

6.b Secondary CH2 refined with riding coordinates:

 C10(H10U,H10V), C11(H11U,H11V), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,

 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),

 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),

  C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,

 H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),

 C51(H51A,H51B), C61(H61A,H61B), C62(H62A,H62B), C72(H72A,H72B), C73(H73A,H73B),

  C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,

 H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B),

 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B),

  C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B), C101(H10C,

 H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J), C105(H10K,H10L),

 C106(H10M,H10N), C107(H10O,H10P), C108(H10Q,H10R), C109(H10S,H10T), C110(H11A,

 H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H), C114(H11I,H11J),

 C115(H11K,H11L), C116(H11M,H11N), C117(H11O,H11P), C118(H11Q,H11R), C119(H11S,

 H11T), C120(H12A,H12B)

6.c Idealised Me refined as rotating group:

 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,

 H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,

 H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),

 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,

 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C53(H53A,H53B,H53C), C54(H54A,

 H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),

 C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,

 H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C75(H75A,

 H75B,H75C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),

 C81(H81A,H81B,H81C), C82(H82A,H82B,H82C)

;