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_7709371
_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         'C46 H60 Mg N6, C3 H3'
_chemical_formula_sum            'C49 H63 Mg N6'
_chemical_formula_weight         760.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-12
_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                 96.658(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8797(11)
_cell_length_b                   21.1458(13)
_cell_length_c                   24.3580(15)
_cell_measurement_reflns_used    9455
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.103
_cell_measurement_theta_min      2.350
_cell_volume                     9147.2(10)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0885
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            86204
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.559
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1350 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.8676. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         10512
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0633P)^2^+11.8837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6675
_reflns_number_total             10512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03235f2.cif
_cod_data_source_block           t_CCDC1
_cod_database_code               7709371
_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. Rigid bond restraints
 C47, C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C47 \\sim C48 \\sim C49: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C47, C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C41(H41), C44(H44)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C14(H14), C15(H15), C16(H16), C26(H26),
 C27(H27), C28(H28), C32(H32), C37(H37), C38(H38), C39(H39)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              2069
_shelx_hkl_checksum              40983
_olex2_submission_special_instructions 'No special instructions were received'