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_7122027
_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         'C34 H58 Tb, B C24 F20'
_chemical_formula_sum            'C58 H58 B F20 Tb'
_chemical_formula_weight         1304.77
_chemical_name_systematic        '[Tb(Cpttt)2][BArF20]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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
_audit_creation_date             2017-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                82.810(3)
_cell_angle_beta                 89.321(3)
_cell_angle_gamma                79.728(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7358(4)
_cell_length_b                   12.4581(4)
_cell_length_c                   19.9710(9)
_cell_measurement_reflns_used    3620
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.7890
_cell_measurement_theta_min      2.1940
_cell_volume                     2850.32(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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      150.00(10)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00  72.00   0.25    3.75  -8.00   0.00   0.00    --   288
  2  \f     72.00 144.00   0.25    3.75  -8.00   0.00  40.00    --   288
  3  \w    -12.00  23.00   0.25    3.75    --    5.00  57.00-120.00  140
  4  \w     49.00  75.00   0.25    3.75    --    5.00  57.00-180.00  104
  5  \w     -7.00  19.00   0.25    3.75    --    5.00  54.00 -49.16  104
  6  \w    -35.00  74.00   0.25    3.75    --   -7.70  57.00  30.00  436
  7  \w      1.00  82.00   0.25    3.75    --   -7.70  38.00 -30.00  324
  8  \w    -96.00  25.00   0.25    3.75    --   -7.70 -57.00-150.00  484
  9  \w    -84.00 -26.00   0.25    3.75    --   -7.70 -38.00  90.00  232
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35372
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.051
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.327
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         10291
_refine_ls_number_restraints     922
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0948P)^2^+20.8484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7152
_reflns_number_total             10291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05261a2.cif
_cod_data_source_block           3-Tb
_cod_depositor_comments
'Adding full bibliography for 7122025--7122029.cif.'
_cod_original_cell_volume        2850.33(19)
_cod_database_code               7122027
_manchester_internal_coll_name   rdpm83
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 3.75s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w & \f scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   20/11/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 20/11/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 20/11/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 26/11/17
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 29/4/18
_manchester_internal_archive_date 29/4/18
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.877
_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. Restrained distances
 C33A-C31 \\sim C31-C33B \\sim C32A-C31 \\sim C31-C32B \\sim C34A-C31 \\sim
C31-C34B
 with sigma of 0.008
 C32A-C33A \\sim C34A-C32A \\sim C32B-C33B \\sim C33B-C34B \\sim C34B-C32B
 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C32A \\sim C33A \\sim C34A \\sim C32B \\sim C33B \\sim C34B: within 2A with
sigma of 0.008 and sigma for terminal atoms of 0.016
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
6.a Me refined with riding coordinates:
 C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C32B(H32D,
 H32E,H32F), C33B(H33D,H33E,H33F), C34B(H34D,H34E,H34F)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
6.c 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), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              70993
_shelx_fab_checksum              78326
_olex2_date_sample_completion    2017-11-20
_olex2_date_sample_data_collection 2017-11-20
_olex2_date_sample_submission    2017-11-20
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id rdpm83
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;