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_1566000
_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            'C26 H50 B2 Na Nd O7'
_chemical_formula_weight         663.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.842(5)
_cell_length_b                   14.238(3)
_cell_length_c                   18.216(4)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.152
_cell_volume                     6443(2)
_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      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31148
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.430
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.662
_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            blue
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.130
_exptl_transmission_factor_max   0.813
_exptl_transmission_factor_min   0.542
_refine_diff_density_max         1.071
_refine_diff_density_min         -1.814
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 4396 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         14920
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0223P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.690
_reflns_Friedel_fraction_full    0.729
_reflns_Friedel_fraction_max     0.733
_reflns_number_gt                12690
_reflns_number_total             14920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120638.cif
_cod_data_source_block           5Nd
_cod_depositor_comments
;

2022-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H100 B4 Na2 Nd2 O14'
_cod_original_formula_weight         1327.01
_cod_original_formula_units_Z            4
_cod_database_code               1566000
_shelx_estimated_absorpt_t_min   0.542
_shelx_estimated_absorpt_t_max   0.813