Amine–Boranes Reactions Promoted by Lanthanide(II) Ions
Kirkina, Vladislava A.; Kissel, Alexander; Selikhov, Alexander N.; Nelyubina, Yulia V.; Filippov, Oleg A.; Belkova, Natalia; Trifonov, Alexander; Shubina, Elena; Chemical Communications  (2022) –; doi:10.1039/D1CC06401K

data_7129411
_publ_section_title
;
 Amine--Boranes Reactions Promoted by Lanthanide(II) Ions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06401K
_journal_year                    2022
_chemical_formula_moiety         'C28 H104 B8 N12 Sm4'
_chemical_formula_sum            'C28 H104 B8 N12 Sm4'
_chemical_formula_weight         1297.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-10-23 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                104.319(4)
_cell_angle_beta                 107.514(4)
_cell_angle_gamma                108.505(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7159(17)
_cell_length_b                   13.065(2)
_cell_length_c                   13.542(2)
_cell_measurement_reflns_used    1064
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1438.5(4)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1301
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_number            5650
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.704
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.051
_exptl_absorpt_correction_T_max  0.023686
_exptl_absorpt_correction_T_min  0.004570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/2 (Bruker,2010) was used for absorption correction.

Final HKLF 4 output contains 67884 reflections, Rint = 0.2642
 (14434 with I > 3sig(I), Rint = 0.1301)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_gt           0.0815
_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^)+(0.0803P)^2^+28.2984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.2077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3809
_reflns_number_total             5650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06401k2.cif
_cod_data_source_block           SmDMAB
_cod_original_cell_volume        1438.6(4)
_cod_database_code               7129411
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.582
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 B1(H1D,H1E,H1F), B2(H2D,H2E,H2F), B3(H3D,H3E,H3F), B4(H4D,H4E,H4F)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,H11C,
 H11B), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              80692
_olex2_submission_special_instructions 'No special instructions were received'