Lithium and magnesium complexes from the employment of pyridyl-pendanted unsymmetrical β-diketiminates: syntheses and utilization as catalysts for the hydroboration of carbonyl compounds
Li, Yafei; Pan, Huifen; Lu, Yanhua; Luo, Yanshu; Dang, Yan; Wang, Yalan; Xia, Shengwang; Li, Yahong; Xia, Yuanzhi; Dalton Transactions  (2022) –; doi:10.1039/D1DT03235F

data_7709370
_publ_section_title
;
 Lithium and magnesium complexes from the employment of pyridyl-pendanted
 unsymmetrical \b-diketiminates: syntheses and utilization as catalysts
 for the hydroboration of carbonyl compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03235F
_journal_year                    2022
_chemical_formula_moiety         'C44 H56 Li2 N6'
_chemical_formula_sum            'C44 H56 Li2 N6'
_chemical_formula_weight         682.82
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.665(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2500(8)
_cell_length_b                   17.6853(11)
_cell_length_c                   21.0440(15)
_cell_measurement_reflns_used    5735
_cell_measurement_temperature    189(2)
_cell_measurement_theta_max      26.808
_cell_measurement_theta_min      2.309
_cell_volume                     4178.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      189.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50327
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.932
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5367
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1433 before and 0.0832 after correction. The Ratio of minimum to maximum transmission is 0.7198. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0784P)^2^+0.0418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4510
_reflns_number_total             7330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03235f2.cif
_cod_data_source_block           t
_cod_database_code               7709370
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C31(H31), C37(H37)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15),
 C25(H25), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C43(H43), C44(H44)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C)
;
_shelx_res_checksum              82638
_shelx_hkl_checksum              21500
_olex2_submission_special_instructions 'No special instructions were received'