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_1565999
_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_moiety         'C14 H22 B Nd O'
_chemical_formula_sum            'C14 H22 B Nd O'
_chemical_formula_weight         361.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 106.9970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.01650(10)
_cell_length_b                   14.09950(10)
_cell_length_c                   13.6640(2)
_cell_measurement_reflns_used    24318
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.2960
_cell_measurement_theta_min      4.6150
_cell_volume                     1476.96(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -120.00 -72.75   0.35    0.23    --  -48.51-128.00 107.00  135
  2  \w    -99.00 -22.00   0.35    0.23    --  -48.51 142.00  -7.00  220
  3  \w   -120.00 -62.95   0.35    0.23    --  -48.51-142.00 -63.00  163
  4  \w    -88.00 -14.85   0.35    0.23    --  -48.51 128.00-178.00  209
  5  \w     36.00  95.85   0.35    0.23    --   48.51-128.00 107.00  171
  6  \w     44.00 103.85   0.35    0.23    --   48.51-142.00 -63.00  171
  7  \w   -155.00 -63.30   0.35    0.75    --  -90.00-142.00 -63.00  262
  8  \w   -161.00 -73.15   0.35    0.75    --  -90.00-128.00 107.00  251
  9  \w    -88.00 -18.00   0.35    0.75    --  -90.00 128.00-178.00  200
 10  \w     84.00 171.15   0.35    0.75    --  111.50 142.00  -7.00  249
 11  \w     40.00 113.15   0.35    0.75    --  111.50-128.00 107.00  209
 12  \w     93.00 177.00   0.35    0.75    --  111.50 128.00-178.00  240
 13  \w     44.00 123.10   0.35    0.75    --  111.50-142.00 -63.00  226
 14  \w    -26.00  25.10   0.35    0.23    --  -48.51  19.00 -30.00  146
 15  \w   -120.00 -74.15   0.35    0.23    --  -48.51-125.00 -30.00  131
 16  \w   -120.00 -35.30   0.35    0.23    --  -48.51 -57.00  30.00  242
 17  \w    -26.00  25.10   0.35    0.23    --  -48.51  19.00-180.00  146
 18  \w    -26.00  25.10   0.35    0.23    --  -48.51  19.00 -60.00  146
 19  \w   -120.00 -74.15   0.35    0.23    --  -48.51-125.00   0.00  131
 20  \w    -26.00  25.10   0.35    0.23    --  -48.51  19.00 150.00  146
 21  \w    -25.00  25.05   0.35    0.23    --   48.51 -19.00  90.00  143
 22  \w    -98.00 -22.75   0.35    0.75    --  -90.00 142.00  -7.00  215
 23  \w     40.00  69.75   0.35    0.75    --  111.50 -61.00 150.00   85
 24  \w     40.00 110.00   0.35    0.75    --  111.50-125.00 -30.00  200
 25  \w     40.00 110.00   0.35    0.75    --  111.50-125.00-180.00  200
 26  \w     96.00 176.85   0.35    0.75    --  111.50  61.00-120.00  231
 27  \w     40.00  69.75   0.35    0.75    --  111.50 -61.00-120.00   85
 28  \w     40.00  69.75   0.35    0.75    --  111.50 -61.00  90.00   85
 29  \w     40.00 106.85   0.35    0.75    --  111.50-109.00 169.68  191
 30  \w     40.00 110.00   0.35    0.75    --  111.50-125.00-120.00  200
 31  \w     40.00 103.70   0.35    0.75    --  111.50 -77.00-150.00  182
 32  \w     44.00 124.15   0.35    0.75    --  111.50-143.00 165.58  229
 33  \w     40.00 110.00   0.35    0.75    --  111.50-125.00 -60.00  200
 34  \w     95.00 176.90   0.35    0.75    --  111.50 125.00  90.00  234
 35  \w     40.00 110.00   0.35    0.75    --  111.50-125.00-150.00  200
 36  \w     42.00 121.10   0.35    0.75    --  111.50-138.00  95.52  226
 37  \w     40.00 106.85   0.35    0.75    --  111.50-110.00-107.24  191
 38  \w    101.00 178.00   0.35    0.75    --  111.50  45.00 -60.00  220
 39  \w     40.00 106.15   0.35    0.75    --  111.50-107.00 -21.62  189
 40  \w     93.00 177.00   0.35    0.75    --  111.50  69.00  49.91  240
 41  \w    101.00 178.00   0.35    0.75    --  111.50  45.00 -90.00  220
 42  \w    101.00 178.00   0.35    0.75    --  111.50  30.00 150.00  220
 43  \w     96.00 176.85   0.35    0.75    --  111.50  61.00   0.00  231
 44  \w     40.00 106.85   0.35    0.75    --  111.50-109.00   4.31  191
 45  \w     96.00 176.85   0.35    0.75    --  111.50  61.00  90.00  231
 46  \w     40.00 106.15   0.35    0.75    --  111.50-106.00 106.43  189
 47  \w     40.00 103.70   0.35    0.75    --  111.50 -77.00-180.00  182
 48  \w     95.00 176.90   0.35    0.75    --  111.50 125.00 150.00  234
 49  \w     95.00 176.90   0.35    0.75    --  111.50 125.00  30.00  234
 50  \w     40.00 103.70   0.35    0.75    --  111.50 -77.00 150.00  182
 51  \w     45.00 124.10   0.35    0.75    --  111.50-144.00  56.42  226
 52  \w     40.00 103.70   0.35    0.75    --  111.50 -77.00 120.00  182
 53  \w     40.00 105.10   0.35    0.75    --  111.50-100.00  60.29  186
 54  \w    101.00 178.00   0.35    0.75    --  111.50  30.00  90.00  220
 55  \w     43.00 122.10   0.35    0.75    --  111.50-140.00-100.48  226
 56  \w     40.00 105.10   0.35    0.75    --  111.50 -99.00  -7.94  186
 57  \w     40.00 106.15   0.35    0.75    --  111.50-108.00  35.39  189
 58  \w     40.00 110.00   0.35    0.75    --  111.50-120.00 130.24  200
 59  \w     40.00  69.75   0.35    0.75    --  111.50 -61.00 -90.00   85
 60  \w     95.00 176.90   0.35    0.75    --  111.50 125.00  60.00  234
 61  \w    102.00 177.25   0.35    0.75    --  111.50  15.00 120.00  215
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0205945000
_diffrn_orient_matrix_UB_12      -0.0614130000
_diffrn_orient_matrix_UB_13      -0.0960424000
_diffrn_orient_matrix_UB_21      0.0574469000
_diffrn_orient_matrix_UB_22      -0.0881197000
_diffrn_orient_matrix_UB_23      0.0681864000
_diffrn_orient_matrix_UB_31      -0.1915021000
_diffrn_orient_matrix_UB_32      -0.0198467000
_diffrn_orient_matrix_UB_33      -0.0053726000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40069
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.769
_diffrn_reflns_theta_min         4.614
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    26.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.714
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.00045(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+1.3831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3076
_reflns_number_total             3188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120638.cif
_cod_data_source_block           nd5-bh4
_cod_database_code               1565999
_chemical_oxdiff_formula         'Nd C14 H22 B Nd O'
_chemical_oxdiff_usercomment     ND5_BH4
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.158
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. Fixed Uiso
 At 1 times of:
  All C(H) groups
;