Cyclopentadienyl lanthanide borohydrides derived from the unsubstituted cyclopentadienyl ligand. Unprecedented structural diversity and ε-caprolactone polymerization
Bardonov, Daniil A.; Komarov, Pavel D.; Sadrtdinova, Guzelia I.; Besprozvannyh, Viktoria K.; Lyssenko, Konstantin A.; Gudovannyy, Alexei O.; Nifant'ev, Ilya E.; Minyaev, Mikhail E.; Roitershtein, Dmitrii M.; Inorganica Chimica Acta 529 (2022) 120638–; doi:10.1016/j.ica.2021.120638

data_1566004
_publ_section_title
;
 Cyclopentadienyl lanthanide borohydrides derived from the unsubstituted
 cyclopentadienyl ligand. Unprecedented structural diversity and
 \e-caprolactone polymerization
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120638
_journal_paper_doi               10.1016/j.ica.2021.120638
_journal_volume                  529
_journal_year                    2022
_chemical_formula_sum            'C32.5 H58.5 B1.5 Na O8 Tb'
_chemical_formula_weight         775.41
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.8128(19)
_cell_length_b                   13.8128(19)
_cell_length_c                   33.700(7)
_cell_measurement_reflns_used    7332
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      2.242
_cell_volume                     5568.3(16)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX3 (Bruker, 2019)
;
_computing_data_reduction
;
SAINT (Bruker, 2019), PLATON (Spek, 2020)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            53662
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.806
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.961
_exptl_absorpt_correction_T_max  0.6478
_exptl_absorpt_correction_T_min  0.3807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             2406
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.164
_refine_diff_density_max         1.555
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8520
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1589P)^2^+8.0819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2181
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7158
_reflns_number_total             8520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120638.cif
_cod_data_source_block           8tb
_cod_original_cell_volume        5568.4(19)
_cod_original_formula_sum        'C32.50 H58.50 B1.50 Na O8 Tb'
_cod_database_code               1566004
_shelx_estimated_absorpt_t_min   0.536
_shelx_estimated_absorpt_t_max   0.739