Synthesis and reactivity of a heteroleptic magnesium hydride on a dearomatized picolyl-based NNN-chelator.
Mandal, Chhotan; Sarkar, Subham; Panda, Sourav; Mallick, Dibyendu; Mukherjee, Debabrata; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17343–17350; doi:10.1039/d4dt02757d

data_7717142
_publ_section_title
;
 Synthesis and reactivity of a heteroleptic magnesium hydride on a
 dearomatized picolyl-based NNN-chelator.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17343
_journal_page_last               17350
_journal_paper_doi               10.1039/d4dt02757d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H37 Mg N3'
_chemical_formula_sum            'C24 H37 Mg N3'
_chemical_formula_weight         391.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-09-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-24 deposited with the CCDC.	2024-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.866(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2110(3)
_cell_length_b                   11.1972(3)
_cell_length_c                   17.5444(5)
_cell_measurement_reflns_used    12024
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      67.7880
_cell_measurement_theta_min      3.9760
_cell_volume                     2328.92(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00 -47.00   0.50    1.50    --  -40.58-165.00  84.00  126
  2  \w    -83.00  -6.00   0.50    1.50    --  -40.58 117.00 -39.00  154
  3  \w     54.00 115.00   0.50    1.50    --   40.58-165.00  84.00  122
  4  \w   -138.00 -47.00   0.50    8.00    --  -82.50-165.00  84.00  182
  5  \w   -146.00 -78.00   0.50    8.00    --  -82.50-117.00-127.00  136
  6  \w     54.00 140.00   0.50    8.00    --   96.35-165.00  84.00  172
  7  \w     33.00 110.00   0.50    8.00    --   96.35-117.00-127.00  154
  8  \w    -31.00  30.00   0.50    1.50    --  -40.58  25.00-120.00  122
  9  \w    -24.00  35.00   0.50    1.50    --  -40.58  12.00 -30.00  118
 10  \w   -108.00 -17.00   0.50    1.50    --  -40.58 -64.00  30.00  182
 11  \w    -31.00  30.00   0.50    1.50    --  -40.58  25.00-180.00  122
 12  \w   -114.00 -32.00   0.50    1.50    --  -40.58 165.00 108.00  164
 13  \w    -57.00  26.00   0.50    1.50    --  -40.58  50.00-120.00  166
 14  \w    -28.00  68.00   0.50    1.50    --   40.58 -77.00  60.00  192
 15  \w    -47.00 -15.00   0.50    8.00    --  -82.50  42.00-150.00   64
 16  \w    -68.00 -14.00   0.50    8.00    --  -82.50  59.00   0.00  108
 17  \w   -149.00 -63.00   0.50    8.00    --  -82.50 -50.00 -90.00  172
 18  \w     28.00  68.00   0.50    8.00    --   96.35 -59.00 120.00   80
 19  \w     28.00  68.00   0.50    8.00    --   96.35 -59.00 -60.00   80
 20  \w     29.00  83.00   0.50    8.00    --   96.35 -68.00 -90.00  108
 21  \w     44.00 127.00   0.50    8.00    --   96.35-145.00  30.00  166
 22  \w     81.00 167.00   0.50    8.00    --   96.35  25.00 150.00  172
 23  \w     80.00 164.00   0.50    8.00    --   96.35  42.00-120.00  168
 24  \w     28.00 105.00   0.50    8.00    --   96.35 -77.00-150.00  154
 25  \w     30.00  57.00   0.50    8.00    --   96.35 -50.00   0.00   54
 26  \w     28.00  68.00   0.50    8.00    --   96.35 -59.00-120.00   80
 27  \w     30.00  57.00   0.50    8.00    --   96.35 -50.00  90.00   54
 28  \w     83.00 164.00   0.50    8.00    --   96.35  33.00 -60.00  162
 29  \w     30.00  57.00   0.50    8.00    --   96.35 -50.00 -30.00   54
 30  \w    105.00 170.00   0.50    8.00    --   96.35  96.00 -60.00  130
 31  \w     99.00 160.00   0.50    8.00    --   96.35 117.00  60.00  122
 32  \w     83.00 164.00   0.50    8.00    --   96.35  33.00 -30.00  162
 33  \w     28.00  68.00   0.50    8.00    --   96.35 -59.00-150.00   80
 34  \w     28.00 105.00   0.50    8.00    --   96.35 -77.00-180.00  154
 35  \w     99.00 160.00   0.50    8.00    --   96.35 117.00 -39.00  122
 36  \w   -109.00 -58.00   0.50    1.50    --  -40.58 -77.00-150.00  102
 37  \w   -109.00 -14.00   0.50    1.50    --  -40.58 -77.00-120.00  190
 38  \w   -107.00 -21.00   0.50    1.50    --  -40.58 -50.00 -60.00  172
 39  \w   -108.00 -17.00   0.50    1.50    --  -40.58 -64.00  90.00  182
 40  \w   -109.00 -14.00   0.50    1.50    --  -40.58 -77.00 -60.00  190
 41  \w   -109.00 -14.00   0.50    1.50    --  -40.58 -77.00   0.00  190
 42  \w   -109.00 -14.00   0.50    1.50    --  -40.58 -77.00  90.00  190
 43  \w    -78.00   4.00   0.50    1.50    --  -40.58 104.00  90.00  164
 44  \w   -109.00 -14.00   0.50    1.50    --  -40.58 -77.00-180.00  190
 45  \w    -29.00  31.00   0.50    1.50    --   40.58 -25.00 -90.00  120
 46  \w     18.00 108.00   0.50    1.50    --   40.58  64.00-180.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.996
_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       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23984
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.371
_diffrn_reflns_theta_min         4.000
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_preparation       'solvent diffusion'
_exptl_crystal_recrystallization_method 'block crystal'
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1508P)^2^+0.2598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3642
_reflns_number_total             4230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02757d2.cif
_cod_data_source_block           cm-mg08_autocm_01
_cod_depositor_comments
'Adding full bibliography for 7717142--7717146.cif.'
_cod_database_code               7717142
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C16(H16), C9(H9), C10(H10), C8(H8), C14(H14)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C6(H6A,H6B,H6C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              84483
_shelx_hkl_checksum              16457
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;