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_1548006
_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 Ag N4 P4 Si4 Tb, C7 H8'
_chemical_formula_sum            'C69 H84 Ag N4 P4 Si4 Tb'
_chemical_formula_weight         1472.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.683(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.786(3)
_cell_length_b                   12.9185(7)
_cell_length_c                   24.1821(12)
_cell_measurement_reflns_used    7343
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8380
_cell_measurement_theta_min      3.5420
_cell_volume                     13836.3(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega   51.00  109.00   2.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  150.0000 29

  2 omega   31.00   71.00   2.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   30.0000 20

  3 omega   27.00  105.00   2.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -30.0000 39

  4 omega   43.00  107.00   2.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -120.0000 32

  5 omega   36.00   64.00   2.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -15.0000 -150.0000 14

  6 omega   99.00  157.00   2.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   61.0000  -30.0000 29

  7 omega   78.00  168.00   2.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000   30.0000 45

  8 omega   26.00  112.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6804   38.0000  120.0000 43

  9 omega   -7.00   21.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 14

 10 omega  -46.00  -22.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 12

 11 omega  -27.00   65.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6804  -57.0000  -30.0000 46
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0077253000
_diffrn_orient_matrix_UB_12      -0.1131887000
_diffrn_orient_matrix_UB_13      -0.0105887000
_diffrn_orient_matrix_UB_21      -0.0339020000
_diffrn_orient_matrix_UB_22      -0.0256316000
_diffrn_orient_matrix_UB_23      -0.0197041000
_diffrn_orient_matrix_UB_31      0.0001487000
_diffrn_orient_matrix_UB_32      0.0276193000
_diffrn_orient_matrix_UB_33      -0.0619200000
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27389
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.164
_diffrn_reflns_theta_min         3.564
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    9.092
_exptl_absorpt_correction_T_max  0.314
_exptl_absorpt_correction_T_min  0.163
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             6032
_exptl_crystal_size_max          0.3431
_exptl_crystal_size_mid          0.2418
_exptl_crystal_size_min          0.216
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         13618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+2.9283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12320
_reflns_number_total             13618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms14137-s12.cif
_cod_data_source_block           6Tb
_cod_original_cell_volume        13836.2(13)
_cod_database_code               1548006
_chemical_oxdiff_formula         'C69 H84 Ag N4 P4 Si4 Tb'
_reflns_odcompleteness_completeness 99.70
_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), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
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), C63(H63A,H63B,H63C)
;
_olex2_submission_special_instructions 'No special instructions were received'