Potential precursors for terminal ytterbium(II) imide complexes bearing the tris(3-tert-butyl-5-methylpyrazolyl)hydroborato ligand
Katzenmayer, Markus; Kracht, Felix; Maichle-Moessmer, Caecilia; Anwander, Reiner; Dalton Transactions  (2023) –; doi:10.1039/D3DT00861D

data_7712803
_publ_section_title
;
 Potential precursors for terminal ytterbium(II) imide complexes bearing
 the tris(3-tert-butyl-5-methylpyrazolyl)hydroborato ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00861D
_journal_year                    2023
_chemical_formula_sum            'C43 H67 B F6 N7 O2 Yb'
_chemical_formula_weight         1011.88
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-03-14 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                100.123(3)
_cell_angle_beta                 107.912(3)
_cell_angle_gamma                90.396(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6419(9)
_cell_length_b                   12.1357(10)
_cell_length_c                   17.4345(14)
_cell_measurement_reflns_used    180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.75
_cell_measurement_theta_min      2.298
_cell_volume                     2302.4(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'APEX3 v2019.11-0'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.1091
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54467
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.505
_diffrn_reflns_theta_min         1.249
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       needle
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.049
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6236
_refine_diff_density_max         2.236
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.486(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         18830
_refine_ls_number_restraints     2338
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                14115
_reflns_number_total             18830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00861d2.cif
_cod_data_source_block           3-thf_mo_MK174_2_0m_p1
_cod_database_code               7712803
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.629
_shelx_estimated_absorpt_t_max   0.904
_shelx_res_checksum              65226
_shelx_hkl_checksum              34455