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_7122025
_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 H34.54 B2.64 I0.36 O3 Tb'
_chemical_formula_sum            'C12 H34.54 B2.63 I0.37 O3 Tb'
_chemical_formula_weight         460.66
_chemical_name_systematic        '[Tb(BH4)3(THF)3]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-20
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1844(2)
_cell_length_b                   14.3006(3)
_cell_length_c                   14.7076(4)
_cell_measurement_reflns_used    8710
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      29.8080
_cell_measurement_theta_min      2.1950
_cell_volume                     1931.73(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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      N~2~
_diffrn_ambient_temperature      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -6.00  21.00   0.50    2.00    --   -7.80  21.00 -15.00   54
  2  \w    -43.00 -18.00   0.50    2.00    --   -7.80 -21.00 178.00   50
  3  \w    -94.00  31.00   0.50    2.00    --   -7.80 -38.00  30.00  250
  4  \w    -39.00  58.00   0.50    2.00    --   -7.80  57.00-150.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0273237000
_diffrn_orient_matrix_UB_12      0.0026061000
_diffrn_orient_matrix_UB_13      -0.0450381000
_diffrn_orient_matrix_UB_21      -0.0691189000
_diffrn_orient_matrix_UB_22      0.0134569000
_diffrn_orient_matrix_UB_23      0.0170663000
_diffrn_orient_matrix_UB_31      0.0210514000
_diffrn_orient_matrix_UB_32      0.0476628000
_diffrn_orient_matrix_UB_33      -0.0023407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12868
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.849
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.242
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1762
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0267
_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^)+6.1771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1731
_reflns_number_total             1762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05261a2.cif
_cod_data_source_block           1-Tb
_cod_depositor_comments
'Adding full bibliography for 7122025--7122029.cif.'
_cod_original_cell_volume        1931.72(8)
_cod_database_code               7122025
_manchester_internal_coll_name   rdpm80
_manchester_internal_coll_client CAPG/FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 2s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   18/11/17
_manchester_internal_process_user CAPG/FO
_manchester_internal_process_date 20/11/17
_manchester_internal_solution_user CAPG/FO
_manchester_internal_solution_date 20/11/17
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 20/11/17
_manchester_internal_validation_user FO
_manchester_internal_validation_date 20/11/17
_manchester_internal_archive_date 20/11/17
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     FO/CAPG
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All I(H) groups
2. Restrained distances
 B2-H2A = B2-H2B
 1.1 with sigma of 0.02
 B1-H1D = B1-H1A = B1-H1B = B1-H1C
 1.1 with sigma of 0.02
 H1D-H1A
 1.5 with sigma of 0.02
 H1D-H1C
 1.5 with sigma of 0.02
 H1A-H1B
 1.5 with sigma of 0.02
 H1D-H1B
 1.5 with sigma of 0.02
 Tb1-B1 \\sim Tb1-B2
 with sigma of 0.02
 Tb1-H1B \\sim Tb1-H1A \\sim Tb1-H1D
 with sigma of 0.02
 H1C-H1A \\sim H1C-H1B \\sim H1C-H1D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B1 \\sim I2A: 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(I2A)=1-FVAR(1)
 Sof(H1A)=Sof(H1B)=Sof(H1D)=Sof(B1)=Sof(H1C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1E,H1F), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              31685
_olex2_exptl_crystal_mounting_method 'in fomblin oil on micromount'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.132
_oxdiff_exptl_absorpt_empirical_full_min 0.646