Terbocenium: completing a heavy lanthanide metallocenium cation family with an alternative anion abstraction strategy.
Goodwin, Conrad A. P.; Reta, Daniel; Ortu, Fabrizio; Liu, Jingjing; Chilton, Nicholas F.; Mills, David P.; Chemical communications (Cambridge, England) 54 (2018) 9182–9185; doi:10.1039/c8cc05261a

data_7122026
_publ_section_title
;
 Terbocenium: completing a heavy lanthanide metallocenium cation family
 with an alternative anion abstraction strategy.
;
_journal_issue                   66
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9182
_journal_page_last               9185
_journal_paper_doi               10.1039/c8cc05261a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C12 H34.42 B2.61 I0.39 O3 Y'
_chemical_formula_sum            'C12 H34.42 B2.61 I0.4 O3 Y'
_chemical_formula_weight         394.01
_chemical_name_systematic        '[Y(BH4)3(THF)3]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.122(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9188(2)
_cell_length_b                   12.5674(3)
_cell_length_c                   16.2017(4)
_cell_measurement_reflns_used    11904
_cell_measurement_temperature    150.11(2)
_cell_measurement_theta_max      74.5737
_cell_measurement_theta_min      2.7256
_cell_volume                     1815.64(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.11(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   60.71  247.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.8669  249.2094 187

  2 omega   50.71  237.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   73.8669  114.2094 187

  3 phi   -205.79  153.43   1.0006    5.0000
omega____ theta____ kappa____ phi______ frames
 128.8997  110.5000   73.8669     -     359

  4 omega   81.21  268.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8669    4.2094 187

  5 omega  -13.14  161.86   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0000   73.8669   19.2094 175

  6 phi     51.88  326.22   1.0012    5.0000
omega____ theta____ kappa____ phi______ frames
 224.2097  111.0000   73.8669     -     274

  7 omega   80.71  267.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8669  314.2094 187

  8 omega   30.71  217.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   73.8669  -20.7900 187

  9 omega   80.71  267.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8669   54.2081 187

 10 omega   81.83  192.80   0.9997    5.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8669  254.2100 111

 11 omega   60.71  247.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.8669   29.2100 187

 12 omega   83.21  268.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  194.2088 185

 13 omega   68.21  153.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   73.8669  279.2081 85

 14 omega  106.91  183.91   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  319.2094 77

 15 omega   83.30  172.30   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  169.2088 89

 16 omega  110.03  232.03   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8669  184.2094 122

 17 omega  -91.38   84.62   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.0000   73.8669  104.2088 176

 18 omega   71.24  254.24   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   73.8669  234.2081 183

 19 omega  -58.78  119.22   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   73.8669  124.2088 178
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0852507000
_diffrn_orient_matrix_UB_12      0.0207515000
_diffrn_orient_matrix_UB_13      -0.0819751000
_diffrn_orient_matrix_UB_21      0.1273353000
_diffrn_orient_matrix_UB_22      -0.0536174000
_diffrn_orient_matrix_UB_23      -0.0474988000
_diffrn_orient_matrix_UB_31      -0.0796743000
_diffrn_orient_matrix_UB_32      -0.1083621000
_diffrn_orient_matrix_UB_33      0.0078451000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1426
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27112
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         4.453
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.781
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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_primary    colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.009
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3328
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+10.0720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2578
_reflns_number_total             3328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05261a2.cif
_cod_data_source_block           1-Y
_cod_depositor_comments
'Adding full bibliography for 7122025--7122029.cif.'
_cod_original_cell_volume        1815.64(8)
_cod_original_formula_sum        'C12 H34.42 B2.61 I0.40 O3 Y'
_cod_database_code               7122026
_manchester_internal_coll_name   xdpm42
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 5s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w and \p scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   12/08/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 13/08/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 13/08/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 18/05/2018
_manchester_internal_validation_user FO
_manchester_internal_validation_date 18/05/2018
_manchester_internal_archive_date 18/05/2018
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.828
_reflns_odcompleteness_completeness 97.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.57
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H,H,H,H,H,H) groups,
   All I(H,H,H,H) groups
2. Restrained distances
 B2-H2D = B2-H2C = B2-H2E = B2-H2F
 1 with sigma of 0.008
 B3-H3A = B3-H3C = B3-H3D = B3-H3B
 1 with sigma of 0.02
 Y1-B2 \\sim Y1-B3 \\sim Y1-B1
 with sigma of 0.02
 H1D-H1A \\sim H1D-H1B \\sim H1D-H1C
 with sigma of 0.02
 H1A-H1B \\sim H1A-H1C \\sim H1B-H1C
 with sigma of 0.02
 C2-C1 \\sim C2A-C1 \\sim C4-C3 \\sim C6-C5 \\sim C8-C7 \\sim C12-C11 \\sim
C9-C10
 with sigma of 0.02
 C3-C2A \\sim C3-C2 \\sim C7-C6 \\sim C11-C10
 with sigma of 0.02
 H2C-H2D \\sim H2C-H2E \\sim H2C-H2F \\sim H2D-H2E \\sim H2D-H2F \\sim H2E-H2F
 with sigma of 0.02
 I3-Y1 \\sim I2-Y1
 with sigma of 0.02
 H3A-H3B \\sim H3A-H3C \\sim H3A-H3D \\sim H3B-H3C \\sim H3B-H3D \\sim H3C-H3D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B3 \\sim I3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(I2)=1-FVAR(1)
 Sof(B2)=Sof(H2C)=Sof(H2D)=Sof(H2E)=Sof(H2F)=FVAR(1)
 Sof(I3)=1-FVAR(2)
 Sof(B3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(H3D)=FVAR(2)
 Sof(H1BC)=Sof(H1BD)=Sof(H3BC)=Sof(H3BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(3)
 Sof(H1AA)=Sof(H1AB)=Sof(H3AA)=Sof(H3AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(3)
 Fixed U11: Y1(0.025014)
 Fixed U12: Y1(-0.002091)
 Fixed U13: Y1(-0.001939)
 Fixed U22: Y1(0.02856)
 Fixed U23: Y1(0.00514)
 Fixed U33: Y1(0.02905)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C2(H2A,H2B), C2A(H2AA,H2AB)
;
_shelx_res_checksum              30379
_olex2_submission_special_instructions 'No special instructions were received'