Actinide covalency measured by pulsed electron paramagnetic resonance spectroscopy
Alasdair Formanuik; Ana-Maria Ariciu; Fabrizio Ortu; Reece Beekmeyer; Andrew Kerridge; Floriana Tuna; Eric J. L. McInnes; David P. Mills; Nature Chemistry 9 (2017) 578–583; doi:10.1038/nchem.2692

data_1552010
_publ_section_title
;
 Actinide covalency measured by pulsed electron paramagnetic resonance
 spectroscopy
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              578
_journal_page_last               583
_journal_paper_doi               10.1038/nchem.2692
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C39 H63 Cl U'
_chemical_formula_sum            'C39 H63 Cl U'
_chemical_formula_weight         805.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 118.596(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.100(2)
_cell_length_b                   21.4218(8)
_cell_length_c                   20.1165(15)
_cell_measurement_reflns_used    5433
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      26.0720
_cell_measurement_theta_min      3.5720
_cell_volume                     7605.1(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -87.00   -7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571  -57.0000   30.0000 80
  2 omega  -62.00   53.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571   19.0000   30.0000 115
  3 omega   21.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2946  -99.0000    0.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0363728000
_diffrn_orient_matrix_UB_12      -0.0057579000
_diffrn_orient_matrix_UB_13      -0.0035900000
_diffrn_orient_matrix_UB_21      -0.0169275000
_diffrn_orient_matrix_UB_22      0.0066636000
_diffrn_orient_matrix_UB_23      -0.0392600000
_diffrn_orient_matrix_UB_31      0.0030420000
_diffrn_orient_matrix_UB_32      -0.0318865000
_diffrn_orient_matrix_UB_33      -0.0075537000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30630
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.362
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.3894
_exptl_crystal_size_mid          0.2609
_exptl_crystal_size_min          0.1411
_refine_diff_density_max         2.384
_refine_diff_density_min         -1.832
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13880
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0262P)^2^+19.7610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8441
_reflns_number_total             13880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000003.cif
_cod_data_source_block           PCOD1000003
_cod_original_cell_volume        7605.0(12)
_cod_database_code               1552010
_chemical_oxdiff_formula         'U1 Cl1 C32 Si2 N1'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 2A with sigma of 0.006 and
sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C41(H41), C43(H43), C44(H44), C54(H54), C56(H56), C57(H57), C67(H67),
 C69(H69), C70(H70), C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18),
 C28(H28), C30(H30), C31(H31)
3.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,
 H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              14695
_shelx_hkl_checksum              72342