The inverse-trans-influence in tetravalent lanthanide and actinide bis(carbene) complexes
Matthew Gregson; Erli Lu; David P. Mills; Floriana Tuna; Eric J. L. McInnes; Christoph Hennig; Andreas C. Scheinost; Jonathan McMaster; William Lewis; Alexander J. Blake; Andrew Kerridge; Stephen T. Liddle; Nature Communications 8 (2017) 14137–; doi:10.1038/ncomms14137

data_1548003
_publ_section_title
;
 The inverse-trans-influence in tetravalent lanthanide and actinide
 bis(carbene) complexes
;
_journal_name_full               'Nature Communications'
_journal_page_first              14137
_journal_paper_doi               10.1038/ncomms14137
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C62 H76 N4 P4 Si4 U, C6 H14'
_chemical_formula_sum            'C68 H90 N4 P4 Si4 U'
_chemical_formula_weight         1437.70
_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
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.968(3)
_cell_angle_beta                 101.233(3)
_cell_angle_gamma                109.178(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6142(6)
_cell_length_b                   13.8834(5)
_cell_length_c                   21.4347(8)
_cell_measurement_reflns_used    20206
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      75.5624
_cell_measurement_theta_min      3.4273
_cell_volume                     3419.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      90(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
  1 omega -115.00  -13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.2877  -77.0000    0.0000 102

  2 omega  -92.00   -7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.2877  125.0000   60.0000 85

  3 omega -112.00  -27.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.2877  -38.0000 -120.0000 85

  4 omega   68.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.2877 -125.0000 -150.0000 27

  5 omega  -17.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.2877  -38.0000 -180.0000 46

  6 omega    5.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.2877 -125.0000 -150.0000 27

  7 omega   97.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   45.0000  -60.0000 61

  8 omega   89.00  137.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -77.0000  -30.0000 48

  9 omega   49.00  115.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972 -118.0000  -92.0000 66

 10 omega   41.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000  150.0000 35

 11 omega   90.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   45.0000   60.0000 68

 12 omega   42.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000   60.0000 32

 13 omega   82.00  150.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   77.0000  -30.0000 68

 14 omega  105.00  152.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   77.0000    0.0000 47

 15 omega   66.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -95.0000  -10.0000 40

 16 omega   52.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -77.0000  120.0000 28

 17 omega  111.00  143.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   45.0000  150.0000 32

 18 omega  101.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   45.0000   90.0000 57

 19 omega   28.00  107.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -95.0000  -77.0000 79

 20 omega   28.00   65.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -95.0000  -10.0000 37

 21 omega   35.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972 -108.0000 -162.0000 64

 22 omega   39.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000  -60.0000 36

 23 omega   40.00   73.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000  -30.0000 33

 24 omega   39.00   65.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000   90.0000 26

 25 omega   87.00  133.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   45.0000 -120.0000 46

 26 omega   29.00   60.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -95.0000  -32.0000 31

 27 omega   76.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972 -132.0000  145.0000 48
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0001143000
_diffrn_orient_matrix_UB_12      -0.0614769000
_diffrn_orient_matrix_UB_13      -0.0641455000
_diffrn_orient_matrix_UB_21      0.1283914000
_diffrn_orient_matrix_UB_22      0.0159771000
_diffrn_orient_matrix_UB_23      0.0264130000
_diffrn_orient_matrix_UB_31      -0.0359347000
_diffrn_orient_matrix_UB_32      -0.1011778000
_diffrn_orient_matrix_UB_33      0.0271953000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27751
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.563
_diffrn_reflns_theta_min         3.427
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    8.554
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.377
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.3571
_exptl_crystal_size_mid          0.2299
_exptl_crystal_size_min          0.0812
_refine_diff_density_max         3.223
_refine_diff_density_min         -2.040
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         13610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+12.0334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11971
_reflns_number_total             13610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms14137-s7.cif
_cod_data_source_block           3U
_cod_original_cell_volume        3420.0(2)
_cod_database_code               1548003
_chemical_oxdiff_formula         'C68 H90 N4 P4 Si4 U'
_chemical_oxdiff_usercomment
'UDPMMH #9845 IN FOMBLIN FILM ON MICROMOUNT FOR DPM/STL'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C)
;
_shelx_res_checksum              61932
_shelx_hkl_checksum              17777
_shelx_fab_checksum              70535
_shelx_shelxl_version_number     2014/7