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_7129412
_publ_section_title
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 Amine--Boranes Reactions Promoted by Lanthanide(II) Ions
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06401K
_journal_year                    2022
_chemical_formula_moiety         'C12 H44 B4 N4 O2 Yb'
_chemical_formula_sum            'C12 H44 B4 N4 O2 Yb'
_chemical_formula_weight         492.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_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.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3781(4)
_cell_length_b                   12.5474(4)
_cell_length_c                   17.7027(6)
_cell_measurement_reflns_used    8236
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      2.30
_cell_volume                     2305.21(14)
_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      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26967
_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         28.976
_diffrn_reflns_theta_min         2.301
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.066
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.2842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1092 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.6564.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       needle
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0164
_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^)+(0.0132P)^2^+2.1371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2129
_reflns_number_total             3063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06401k2.cif
_cod_data_source_block           YbDME_DMAB
_cod_database_code               7129412
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.330
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, 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(H2B,H2A)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2C,
 H2D,H2E)
;
_shelx_res_checksum              36623
_olex2_submission_special_instructions 'No special instructions were received'