Differential uranyl(v) oxo-group bonding between the uranium and metal cations from groups 1, 2, 4, and 12; a high energy resolution X-ray absorption, computational, and synthetic study
Zegke, Markus; Zhang, Xiaobin; Pidchenko, Ivan; Hlina, Johann A.; Lord, Rianne M.; Purkis, Jamie; Nichol, Gary S.; Magnani, Nicola; Schreckenbach, Georg; Vitova, Tonya; Love, Jason B.; Arnold, Polly L.; Chemical Science 10 (2019) 9740–; doi:10.1039/C8SC05717F

data_1554602
_publ_section_title
;
 Differential uranyl(v) oxo-group bonding between the uranium and metal
 cations from groups 1, 2, 4, and 12; a high energy resolution X-ray
 absorption, computational, and synthetic study
;
_journal_issue                   42
_journal_name_full               'Chemical Science'
_journal_page_first              9740
_journal_paper_doi               10.1039/C8SC05717F
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C62 H62 N12 O2 Rb U, 3(C5 H5 N)'
_chemical_formula_sum            'C77 H77 N15 O2 Rb U'
_chemical_formula_weight         1568.03
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6821(2)
_cell_length_b                   21.8875(3)
_cell_length_c                   24.2440(3)
_cell_measurement_reflns_used    80366
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      32.5830
_cell_measurement_theta_min      3.4820
_cell_volume                     7260.28(17)
_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)'
_computing_structure_solution    'ShelXS-1997 (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 0.998
_diffrn_measurement_details
;
  1 omega  -99.00  -13.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393  151.0000 -114.8201 172

  2 omega  -40.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -57.0000 -150.0000 178

  3 omega  -25.00   70.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -99.0000  150.0000 190

  4 omega    7.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   57.0000   90.0000 180

  5 omega  -45.00   73.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -19.0000  -90.0000 236

  6 omega  -96.00    4.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393  -77.0000  -30.0000 200

  7 omega  -46.00   43.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393   57.0000   60.0000 178

  8 omega -102.00  -34.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393 -179.0000  -60.0000 136

  9 omega   -2.00   99.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   77.0000 -180.0000 202

 10 omega   -2.00   99.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   77.0000   90.0000 202

 11 omega   34.00  105.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  179.0000  -90.0000 142

 12 omega    7.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   57.0000    0.0000 180

 13 omega   -2.00   99.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   77.0000  -90.0000 202

 14 omega  -25.00   70.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -99.0000   30.0000 190

 15 omega  -42.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -77.0000 -150.0000 202

 16 omega    3.00  101.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   37.0000 -150.0000 196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0107609000
_diffrn_orient_matrix_UB_12      0.0104059000
_diffrn_orient_matrix_UB_13      -0.0270435000
_diffrn_orient_matrix_UB_21      -0.0439954000
_diffrn_orient_matrix_UB_22      0.0171085000
_diffrn_orient_matrix_UB_23      -0.0002119000
_diffrn_orient_matrix_UB_31      0.0251670000
_diffrn_orient_matrix_UB_32      0.0254952000
_diffrn_orient_matrix_UB_33      0.0111724000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            216174
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.072
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.958
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.425
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       prism
_exptl_crystal_F_000             3156
_exptl_crystal_recrystallization_method 'from conc. pyridine-d5 solution'
_exptl_crystal_size_max          1.2579
_exptl_crystal_size_mid          0.8559
_exptl_crystal_size_min          0.5198
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 6849 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0820(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         16642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0206P)^2^+6.1773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15775
_reflns_number_total             16642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05717f2.cif
_cod_data_source_block           p15015ref
_cod_original_cell_volume        7260.27(18)
_cod_database_code               1554602
_chemical_oxdiff_formula         'C64 H64 N12 O2 Rb1 U1'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C36(H36), C38(H38), C39(H39), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C67(H), C78(HA), N4(H4),
 C69(HB), C2(H2), C3(H3), C5(H5), C7(H7), C12(H12), C15(H15), C17(H17),
 C18(H18), C25(H25), C27(H27), C29(H29), C34(H34), C44(H44), C45(H45), C46(H46),
  C47(H47), C64(HC), C65(HD), C66(HE), C68(HF), C70(HG), C71(HH), C72(HI),
 C73(HJ), N5(H5A), C74(HK), C75(HL), C76(HM), C77(HN)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C22(H22A,H22B,
 H22C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-02-05
_olex2_date_sample_submission    2015-02-05
_olex2_exptl_crystal_mounting_method 'glass fibre'
_olex2_submission_original_sample_id RML119
_olex2_submission_special_instructions 'No special instructions were received'