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_1566005
_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            'C58.39 H109.28 B4.72 La3 Na O14'
_chemical_formula_weight         1526.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.540(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6479(15)
_cell_length_b                   13.1522(9)
_cell_length_c                   25.776(2)
_cell_measurement_reflns_used    5279
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.255
_cell_volume                     6993.0(9)
_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      100(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.1091
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            61970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.139
_diffrn_reflns_theta_min         1.836
_exptl_absorpt_coefficient_mu    1.861
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.580
_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    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             3109
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.376
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         17094
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+19.5055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10861
_reflns_number_total             17094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120638.cif
_cod_data_source_block           9la
_cod_original_cell_volume        6993.1(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1566005
_shelx_estimated_absorpt_t_min   0.619
_shelx_estimated_absorpt_t_max   0.802