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_1552008
_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 Th'
_chemical_formula_sum            'C39 H63 Th'
_chemical_formula_weight         763.93
_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
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 104.847(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7341(3)
_cell_length_b                   19.6772(6)
_cell_length_c                   17.8417(5)
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      28.3780
_cell_measurement_theta_min      3.5900
_cell_volume                     3642.65(19)
_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(11)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -40.00   15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571   57.0000 -150.0000 55
  2 omega  -30.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509    0.0000  -60.0000 103
  3 omega   -7.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509  -99.0000  -60.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0448360000
_diffrn_orient_matrix_UB_12      -0.0109931000
_diffrn_orient_matrix_UB_13      -0.0205315000
_diffrn_orient_matrix_UB_21      -0.0070009000
_diffrn_orient_matrix_UB_22      -0.0339717000
_diffrn_orient_matrix_UB_23      0.0116478000
_diffrn_orient_matrix_UB_31      -0.0510845000
_diffrn_orient_matrix_UB_32      -0.0050661000
_diffrn_orient_matrix_UB_33      -0.0336698000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14197
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.323
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.117
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.654
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.4787
_exptl_crystal_size_mid          0.3526
_exptl_crystal_size_min          0.3258
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0178P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5506
_reflns_number_total             6642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000001.cif
_cod_data_source_block           PCOD1000001
_cod_database_code               1552008
_chemical_oxdiff_formula         'C39 Th1 '
_reflns_odcompleteness_completeness 99.74
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C28(H28), C30(H30),
 C31(H31)
2.b Idealised Me refined as rotating group:
 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              2345
_shelx_hkl_checksum              21294
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'