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_4343123
_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_absolute_configuration unk
_chemical_formula_moiety         'C47 H47 N9 O2 U, 2(C4 H8 O)'
_chemical_formula_sum            'C55 H63 N9 O4 U'
_chemical_formula_weight         1152.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3655(3)
_cell_length_b                   14.7033(3)
_cell_length_c                   26.6592(8)
_cell_measurement_reflns_used    5586
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      22.6150
_cell_measurement_theta_min      3.3420
_cell_volume                     5239.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      170.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -95.00  -34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955 -179.0000  -30.0000 61

  2 omega  -25.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000    0.0000 89

  3 omega  -22.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   19.0000 -150.0000 117

  4 omega  -88.00  -47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -57.0000  -30.0000 41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0020431000
_diffrn_orient_matrix_UB_12      -0.0348017000
_diffrn_orient_matrix_UB_13      0.0183955000
_diffrn_orient_matrix_UB_21      0.0194926000
_diffrn_orient_matrix_UB_22      0.0315494000
_diffrn_orient_matrix_UB_23      0.0175934000
_diffrn_orient_matrix_UB_31      -0.0493286000
_diffrn_orient_matrix_UB_32      0.0110175000
_diffrn_orient_matrix_UB_33      0.0077119000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         3.056
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.2007
_exptl_crystal_size_mid          0.0975
_exptl_crystal_size_min          0.0789
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.451(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8900
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0172P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7398
_reflns_number_total             8900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00420_si_004.cif
_cod_data_source_block           p15122ref
_cod_database_code               4343123
_chemical_oxdiff_formula         C44H44Cl1N8O2U1Zn1
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.549(9) 0.451(9)
2. 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
3. Restrained distances
 C48-C49
 1.42 with sigma of 0.02
 C51-C50
 1.42 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C45) = Uanis(C47)
Uanis(C44) = Uanis(C43)
5. Rigid body (RIGU) restrains
 C48, C49, C50, C51, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B)
6.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16), C17(H17),
 C23(H23), C24(H24), C26(H26), C28(H28), C33(H33), C35(H35), C37(H37), C38(H38),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), N4(H4), N5(H5A)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              63859
_shelx_hkl_checksum              97737
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'