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_7717146
_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         'C40 H58 Mg2 N6'
_chemical_formula_sum            'C40 H58 Mg2 N6'
_chemical_formula_weight         671.557
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_audit_creation_date             2024-09-04
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.08.07 svn.r83e07e25 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-09-24 deposited with the CCDC.	2024-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1364(2)
_cell_length_b                   15.1179(2)
_cell_length_c                   18.5001(2)
_cell_measurement_reflns_used    21729
_cell_measurement_temperature    99.97(19)
_cell_measurement_theta_max      67.4400
_cell_measurement_theta_min      4.7650
_cell_volume                     3953.71(9)
_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-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9953
_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    -44.00  25.00   0.50    1.80    --  -40.58  39.00 156.00  138
  2  \w    -72.00  30.00   0.50    1.80    --  -40.58  89.00 -77.00  204
  3  \w    -78.00   3.00   0.50    1.80    --  -40.58 106.00  11.00  162
  4  \w   -106.00 -25.00   0.50    1.80    --  -40.58 -39.00   1.00  162
  5  \w     25.00 107.00   0.50    1.80    --   40.58  39.00 156.00  164
  6  \w     19.00  78.00   0.50    1.80    --   40.58-106.00 -87.00  118
  7  \w    -21.00  72.00   0.50    1.80    --   40.58 -89.00 167.00  186
  8  \w    -25.00  44.00   0.50    1.80    --   40.58 -39.00   1.00  138
  9  \w    -83.00 -14.00   0.50    7.20    --  -82.50 106.00  11.00  138
 10  \w   -148.00 -67.00   0.50    7.20    --  -82.50 -39.00   1.00  162
 11  \w   -151.00 -82.00   0.50    7.20    --  -82.50-106.00 -87.00  138
 12  \w    -44.00 -16.00   0.50    7.20    --  -82.50  39.00 156.00   56
 13  \w     28.00 108.00   0.50    7.20    --   96.35-106.00 -87.00  160
 14  \w    104.00 165.00   0.50    7.20    --   96.35 106.00  11.00  122
 15  \w    100.00 167.00   0.50    7.20    --   96.35  89.00 -77.00  134
 16  \w     81.00 162.00   0.50    7.20    --   96.35  39.00 156.00  162
 17  \w     26.00 106.00   0.50    7.20    --   96.35 -89.00 167.00  160
 18  \w    -24.00  35.00   0.50    1.80    --  -40.58  12.00 -60.00  118
 19  \w   -108.00 -17.00   0.50    1.80    --  -40.58 -64.00-150.00  182
 20  \w    -24.00  35.00   0.50    1.80    --  -40.58  12.00-120.00  118
 21  \w     28.00  68.00   0.50    7.20    --   96.35 -59.00  90.00   80
 22  \w     30.00  57.00   0.50    7.20    --   96.35 -50.00   0.00   54
 23  \w     30.00  57.00   0.50    7.20    --   96.35 -50.00  60.00   54
 24  \w     30.00  57.00   0.50    7.20    --   96.35 -50.00-180.00   54
 25  \w    105.00 170.00   0.50    7.20    --   96.35  96.00  30.00  130
 26  \w     30.00  57.00   0.50    7.20    --   96.35 -50.00 150.00   54
 27  \w     28.00  68.00   0.50    7.20    --   96.35 -59.00 -30.00   80
 28  \w     28.00  68.00   0.50    7.20    --   96.35 -59.00 -90.00   80
 29  \w     99.00 160.00   0.50    7.20    --   96.35 117.00 -30.00  122
 30  \w     28.00  68.00   0.50    7.20    --   96.35 -59.00-120.00   80
 31  \w     29.00  83.00   0.50    7.20    --   96.35 -68.00  60.00  108
 32  \w     30.00  57.00   0.50    7.20    --   96.35 -50.00 -60.00   54
 33  \w   -108.00 -17.00   0.50    1.80    --  -40.58 -64.00-180.00  182
 34  \w   -109.00 -14.00   0.50    1.80    --  -40.58 -77.00  90.00  190
 35  \w   -109.00 -14.00   0.50    1.80    --  -40.58 -77.00 -90.00  190
 36  \w   -109.00 -14.00   0.50    1.80    --  -40.58 -77.00 150.00  190
 37  \w   -108.00 -17.00   0.50    1.80    --  -40.58 -64.00 -30.00  182
 38  \w   -109.00 -14.00   0.50    1.80    --  -40.58 -77.00  30.00  190
 39  \w   -109.00 -14.00   0.50    1.80    --  -40.58 -77.00 -60.00  190
 40  \w    -25.00  43.00   0.50    1.80    --   40.58 -38.00 -60.00  136
 41  \w     41.00 100.00   0.50    1.80    --   40.58-138.00-180.00  118
 42  \w   -150.00 -58.00   0.50    7.20    --  -82.50 -68.00  60.00  184
 43  \w   -151.00 -61.00   0.50    7.20    --  -82.50 -59.00 -60.00  180
 44  \w     33.00 110.00   0.50    7.20    --   96.35-117.00  90.00  154
 45  \w     72.00 164.00   0.50    7.20    --   96.35  68.00-120.00  184
 46  \w     80.00 164.00   0.50    7.20    --   96.35  42.00-150.00  168
 47  \w     75.00 125.00   0.50    7.20    --   96.35  59.00  60.00  100
 48  \w     77.00 163.00   0.50    7.20    --   96.35  50.00  90.00  172
 49  \w     70.00 165.00   0.50    7.20    --   96.35  77.00 150.00  190
 50  \w     72.00 164.00   0.50    7.20    --   96.35  68.00 -90.00  184
 51  \w     72.00 164.00   0.50    7.20    --   96.35  68.00 -30.00  184
 52  \w     75.00 165.00   0.50    7.20    --   96.35  59.00 120.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9953
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47379
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9953
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         4.78
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90020
_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    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             1461.304
_exptl_crystal_preparation       'solvent diffusion'
_exptl_crystal_recrystallization_method 'block red crystal'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.2842
_refine_diff_density_min         -0.1680
_refine_diff_density_rms         0.0418
_refine_ls_d_res_high            0.8301
_refine_ls_d_res_low             9.2500
_refine_ls_goodness_of_fit_ref   1.0804
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3601
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.0784
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+2.0117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3297
_reflns_number_total             3601
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02757d2.cif
_cod_data_source_block           dmesdmg_autocm_1
_cod_depositor_comments
'Adding full bibliography for 7717142--7717146.cif.'
_cod_database_code               7717146
_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. Restrained distances
 C20-H20a \\sim C20-H1
 with sigma of 0.02
 C20-H20b \\sim C20-H3
 with sigma of 0.02
 C20-H20c \\sim C20-H20d
 with sigma of 0.02
 C19-H19a \\sim C19-H4
 with sigma of 0.02
 C19-H19b \\sim C19-H5
 with sigma of 0.02
 C19-H19c \\sim C19-H19d
 with sigma of 0.02
3. Others
 Sof(H1)=Sof(H3)=Sof(H20d)=1-FVAR(1)
 Sof(H20a)=Sof(H20b)=Sof(H20c)=FVAR(1)
 Sof(H4)=Sof(H5)=Sof(H19d)=1-FVAR(2)
 Sof(H19a)=Sof(H19b)=Sof(H19c)=FVAR(2)
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
- for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 6.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-09-04_09-56-47
;
_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
;