Control of oxo-group functionalization and reduction of the uranyl ion.
Arnold, Polly L.; Pécharman, Anne-Frédérique; Lord, Rianne M.; Jones, Guy M.; Hollis, Emmalina; Nichol, Gary S.; Maron, Laurent; Fang, Jian; Davin, Thomas; Love, Jason B.; Inorganic chemistry 54 (2015) 3702–3710; doi:10.1021/acs.inorgchem.5b00420

data_4342717
_publ_section_title
;
 Control of oxo-group functionalization and reduction of the uranyl ion.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3702
_journal_page_last               3710
_journal_paper_doi               10.1021/acs.inorgchem.5b00420
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C56 H59 I2 N10 O3 U Zn2, 3(C4 H8 O)'
_chemical_formula_sum            'C68 H83 I2 N10 O6 U Zn2'
_chemical_formula_weight         1759.01
_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   geom
_audit_creation_date             2015-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                95.7370(10)
_cell_angle_beta                 106.8540(10)
_cell_angle_gamma                111.132(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7534(2)
_cell_length_b                   15.2777(2)
_cell_length_c                   20.2051(3)
_cell_measurement_reflns_used    42729
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      73.5960
_cell_measurement_theta_min      2.3453
_cell_volume                     3420.90(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.1574
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_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega -101.00  -56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega  -95.00  -48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -94.00  -32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  122.0000  -18.0000 62

  4 omega  -65.00   27.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914   37.0000  -60.0000 92

  5 omega  -26.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  122.0000  -18.0000 27

  6 omega -107.00  -15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   95.00  121.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1914  179.0000  -90.0000 26

  8 omega  101.00  156.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
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  9 omega   40.00  132.00   1.0000    7.5000
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 10 omega  111.00  168.00   1.0000    7.5000
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    -      108.1200  125.0000   30.0000 57

 11 omega   85.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   45.0000 -150.0000 93

 12 omega  103.00  145.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  125.0000   60.0000 42

 13 omega   81.00  175.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   45.0000  150.0000 94

 14 omega   72.00  138.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  -77.0000   90.0000 66

 15 omega   30.00  131.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  -77.0000    0.0000 101

 16 omega   29.00   62.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  -77.0000   90.0000 33

 17 omega   84.00  112.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200 -122.0000 -100.0000 28

 18 omega   38.00   65.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  -45.0000  120.0000 27

 19 omega   45.00   71.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  -15.0000  -60.0000 26

 20 omega  109.00  163.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  -15.0000  -60.0000 54

 21 omega   92.00  117.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200 -116.0000   80.0000 25

 22 omega   31.00   69.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200 -116.0000   80.0000 38

 23 omega -119.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  -77.0000   90.0000 112

 24 omega -119.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  -77.0000 -120.0000 112

 25 omega -116.00  -56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914 -151.0000   98.0000 60

 26 omega -119.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  -77.0000    0.0000 112

 27 omega -119.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  -77.0000  150.0000 112

 28 omega   56.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1914  179.0000 -120.0000 74

 29 omega -140.00  -28.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -76.0000  -15.0000 112

 30 omega -140.00  -28.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000 -150.0000 112

 31 omega -140.00  -28.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000  -90.0000 112

 32 omega -140.00  -28.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000  150.0000 112

 33 omega -140.00  -28.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000   60.0000 112

 34 omega   47.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   15.0000   60.0000 131

 35 omega   33.00   77.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200  -45.0000  150.0000 44

 36 omega   74.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   77.0000  150.0000 104

 37 omega   74.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   77.0000   60.0000 104

 38 omega   74.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   77.0000 -120.0000 104

 39 omega   81.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   45.0000  120.0000 97

 40 omega   81.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.1200   45.0000  -60.0000 97

 41 omega -116.00  -36.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  -37.0000  -60.0000 80

 42 omega -116.00  -14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1914  -37.0000 -120.0000 102

 43 omega   56.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1914  179.0000  -30.0000 74

 44 omega   14.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1914   37.0000  -30.0000 102

 45 omega   21.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1914 -122.0000   18.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0468964000
_diffrn_orient_matrix_UB_12      -0.1048593000
_diffrn_orient_matrix_UB_13      -0.0413185000
_diffrn_orient_matrix_UB_21      -0.0435319000
_diffrn_orient_matrix_UB_22      0.0295225000
_diffrn_orient_matrix_UB_23      -0.0701615000
_diffrn_orient_matrix_UB_31      0.1226278000
_diffrn_orient_matrix_UB_32      0.0216193000
_diffrn_orient_matrix_UB_33      -0.0082843000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69699
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.758
_diffrn_reflns_theta_min         2.347
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) 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    1.708
_exptl_crystal_description       block
_exptl_crystal_F_000             1734
_refine_diff_density_max         1.774
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         13587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0398P)^2^+13.1432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12464
_reflns_number_total             13587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00420_si_006.cif
_cod_data_source_block           po0028
_cod_depositor_comments          'Adding full bibliography for 4342717.cif.'
_cod_original_cell_volume        3420.89(10)
_cod_database_code               4342717
_chemical_oxdiff_formula         'C49 H57 I2 N8 O3 Si U Zn2'
_chemical_oxdiff_usercomment     'PO0028 8621 AFP/POA Cu'
_reflns_odcompleteness_completeness 99.98
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C61(H61A,
 H61B), C66(H66A,H66B), C62(H62A,H62B), C59(H59A,H59B), C57(H57A,H57B),
 C65(H65A,H65B), C64(H64A,H64B), C60(H60A,H60B), C68(H68A,H68B), C67(H67A,H67B),
  C58(H58A,H58B), C63(H63A,H63B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C14(H14), C15(H15), C17(H17), C19(H19),
 C24(H24), C26(H26), C28(H28), C29(H29), C35(H35), C36(H36), C38(H38), C40(H40),
  C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), N6(H6)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,
 H42B,H42C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'