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_1551965
_publ_section_title
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 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         'C44 H75 As K2 N4 Si3 U, 5/4(C6 H6)'
_chemical_formula_sum            'C40.4 H82.5 As K2 N4 Si3 U'
_chemical_formula_weight         1101.02
_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'
_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                 97.2734(9)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.84985(19)
_cell_length_b                   34.2192(3)
_cell_length_c                   32.8697(3)
_cell_measurement_temperature    120(2)
_cell_volume                     19915.5(3)
_computing_cell_refinement
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)

(compiled Mar 27 2014,17:12:48)

;
_computing_data_collection
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)

(compiled Mar 27 2014,17:12:48)

;
_computing_data_reduction
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)

(compiled Mar 27 2014,17:12:48)

;
_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_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       'w scans'
_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  0.1087
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            254309
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.315
_diffrn_reflns_theta_min         2.685
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    12.301
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)

(compiled Mar 27 2014,17:12:48).

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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             8936
_exptl_crystal_size_max          0.4068
_exptl_crystal_size_mid          0.3045
_exptl_crystal_size_min          0.2171
_refine_diff_density_max         14.993
_refine_diff_density_min         -6.455
_refine_diff_density_rms         0.362
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1755
_refine_ls_number_reflns         40034
_refine_ls_number_restraints     2793
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.1266
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+(0.1685P)^2^+875.8348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3242
_refine_ls_wR_factor_ref         0.3264
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                37904
_reflns_number_total             40034
_reflns_threshold_expression     'I > 2s(I)'
_cod_data_source_file            nchem.2279-s5.cif
_cod_data_source_block           4
_cod_depositor_comments
;

2022-12-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C162 H330 As4 K8 N16 Si12 U4'
_cod_original_formula_weight         4404.08
_cod_original_formula_moiety         'C132 H300 As4 K8 N16 Si12 U4, 5(C6 H6)'
_cod_original_formula_units_Z            4
_cod_database_code               1551965
_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

 H10f-H91b

 -2.2 with sigma of 0.01

 H85b-H86b

 -2.2 with sigma of 0.01

 C117-C118

 -1.5 with sigma of 0.01

 C142-C141 sim C140-C141 sim C140-C139 sim C139-C144 sim C144-C143

sim C142-C143

 with sigma of 0.001

 C141-C143 sim C143-C139

 with sigma of 0.001

 C142-C144 sim C144-C140

 with sigma of 0.001

 C136-C137 sim C138-C137 sim C138-C133 sim C133-C134 sim C135-C134

sim C135-C136

 with sigma of 0.001

 C156-C155 sim C156-C151 sim C152-C151 sim C153-C152 sim C154-C153

sim C155-C154

 with sigma of 0.001

 C144-C139 sim C140-C139 sim C141-C140 sim C142-C141 sim C143-C142

sim C144-C143

 with sigma of 0.001

3. Restrained planarity

 C143, C144, C139, C140, C141, C142

 with sigma of 0.1

4. Uiso/Uaniso restraints and constraints

All non-hydrogen atoms have similar U: within 2A with sigma of 0.003 and sigma

for terminal atoms of 0.006

Uanis(K4) sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01

5. 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

6. Others

 Sof(K2A)=1-FVAR(1)

 Sof(K2)=FVAR(1)

 Sof(K6A)=1-FVAR(2)

 Sof(K6)=FVAR(2)

7.a Ternary CH refined with riding coordinates:

 C1(H1), C4(H4), C7(H7), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26),

 C29(H29), C34(H34), C37(H37), C40(H40), C45(H45), C48(H48), C51(H51), C56(H56),

  C59(H59), C62(H62), C67(H67), C70(H70), C73(H73), C78(H78), C81(H81),

 C84(H84), C89(H89), C92(H92), C95(H95), C100(H100), C103(H103), C106(H106),

 C111(H111), C114(H114), C117(H117), C122(H122), C125(H125), C128(H128)

7.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), C43(H43a,H43b), C44(H44a,H44b), C54(H54a,H54b),

 C55(H55a,H55b), C65(H65a,H65b), C66(H66a,H66b), C76(H76a,H76b), C77(H77a,H77b),

  C87(H87a,H87b), C88(H88a,H88b), C98(H98a,H98b), C99(H99a,H99b), C109(H10u,

 H10v), C110(H11c,H11d), C120(H12a,H12b), C121(H12c,H12d), C131(H13g,H13h),

 C132(H13i,H13j)

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

 C133(H133), C134(H134), C135(H135), C136(H136), C137(H137), C138(H138),

 C143(H143), C142(H142), C141(H141), C140(H140), C139(H139), C144(H144),

 C156(H156), C155(H155), C154(H154), C153(H153), C152(H152), C151(H151)

7.d Fitted hexagon refined as free rotating group:

 C143(C142,C141,C140,C139,C144), C156(C155,C154,C153,C152,C151)

7.e Idealised Me refined as rotating group:

 C2(H2a,H2b,H2c), 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), C35(H35a,H35b,H35c), C36(H36a,

 H36b,H36c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C41(H41a,H41b,H41c),

 C42(H42a,H42b,H42c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C49(H49a,H49b,

 H49c), C50(H50a,H50b,H50c), C52(H52a,H52b,H52c), C53(H53a,H53b,H53c), C57(H57a,

 H57b,H57c), C58(H58a,H58b,H58c), C60(H60a,H60b,H60c), C61(H61a,H61b,H61c),

 C63(H63a,H63b,H63c), C64(H64a,H64b,H64c), C68(H68a,H68b,H68c), C69(H69a,H69b,

 H69c), C71(H71a,H71b,H71c), C72(H72a,H72b,H72c), C74(H74a,H74b,H74c), C75(H75a,

 H75b,H75c), C79(H79a,H79b,H79c), C80(H80a,H80b,H80c), C82(H82a,H82b,H82c),

 C83(H83a,H83b,H83c), C85(H85a,H85b,H85c), C86(H86a,H86b,H86c), C90(H90a,H90b,

 H90c), C91(H91a,H91b,H91c), C93(H93a,H93b,H93c), C94(H94a,H94b,H94c), C96(H96a,

 H96b,H96c), C97(H97a,H97b,H97c), C101(H10c,H10d,H10e), C102(H10f,H10g,H10h),

 C104(H10i,H10j,H10k), C105(H10l,H10m,H10n), C107(H10o,H10p,H10q), C108(H10r,

 H10s,H10t), C112(H11e,H11f,H11g), C113(H11h,H11i,H11j), C115(H11k,H11l,H11m),

 C116(H11n,H11o,H11p), C118(H11q,H11r,H11s), C119(H11t,H11u,H11v), C123(H12e,

 H12f,H12g), C124(H12h,H12i,H12j), C126(H12k,H12l,H12m), C127(H12n,H12o,H12p),

 C129(H12q,H12r,H12s), C130(H13d,H13e,H13f)

;