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_7717144
_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         'C42 H58 Mg2 N6 O2 S4, 2.02[C7H8]'
_chemical_formula_sum            'C58.06 H77.94 Mg2 N6 O2.97 S4'
_chemical_formula_weight         1084.359
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                111.931(2)
_cell_angle_beta                 91.736(1)
_cell_angle_gamma                100.183(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9855(2)
_cell_length_b                   13.0705(2)
_cell_length_c                   13.5358(2)
_cell_measurement_reflns_used    17100
_cell_measurement_temperature    99.98(18)
_cell_measurement_theta_max      68.1510
_cell_measurement_theta_min      3.5260
_cell_volume                     1443.34(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.9898
_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    -76.00  19.00   0.50    0.31    --  -40.58 101.00 149.00  190
  2  \w      3.00  76.00   0.50    0.31    --   40.58-101.00  44.00  146
  3  \w   -154.00 -84.00   0.50    1.22    --  -82.50-101.00  44.00  140
  4  \w    -81.00 -11.00   0.50    1.22    --  -82.50 101.00 149.00  140
  5  \w     25.00 107.00   0.50    1.22    --   96.35-101.00  44.00  164
  6  \w    106.00 168.00   0.50    1.22    --   96.35 101.00 149.00  124
  7  \w    -96.00 -19.00   0.50    0.31    --  -40.58 138.00-120.00  154
  8  \w   -111.00 -26.00   0.50    0.31    --  -40.58 -25.00   0.00  170
  9  \w    -24.00  35.00   0.50    0.31    --  -40.58  12.00-150.00  118
 10  \w    -31.00  30.00   0.50    0.31    --  -40.58  25.00 -30.00  122
 11  \w    -24.00  35.00   0.50    0.31    --  -40.58  12.00 120.00  118
 12  \w    -24.00  35.00   0.50    0.31    --  -40.58  12.00 150.00  118
 13  \w    -29.00  31.00   0.50    0.31    --   40.58 -25.00-180.00  120
 14  \w     22.00 107.00   0.50    0.31    --   40.58  50.00-120.00  170
 15  \w     18.00  78.00   0.50    0.31    --   40.58-104.00-150.00  120
 16  \w     14.00 109.00   0.50    0.31    --   40.58  77.00 -30.00  190
 17  \w     12.00  43.00   0.50    0.31    --   40.58  83.00  90.16   62
 18  \w    -35.00  24.00   0.50    0.31    --   40.58 -12.00 -60.00  118
 19  \w   -153.00 -78.00   0.50    1.22    --  -82.50 -87.00 120.00  150
 20  \w   -151.00 -56.00   0.50    1.22    --  -82.50 -74.00 -18.36  190
 21  \w    -47.00 -15.00   0.50    1.22    --  -82.50  42.00  90.00   64
 22  \w   -156.00 -83.00   0.50    1.22    --  -82.50 -96.00 -60.00  146
 23  \w    -84.00 -18.00   0.50    1.22    --  -82.50 117.00-150.00  132
 24  \w    -47.00 -15.00   0.50    1.22    --  -82.50  42.00   0.00   64
 25  \w     28.00 105.00   0.50    1.22    --   96.35 -77.00 150.00  154
 26  \w     23.00 106.00   0.50    1.22    --   96.35 -96.00 120.00  166
 27  \w     30.00  57.00   0.50    1.22    --   96.35 -50.00  90.00   54
 28  \w     99.00 160.00   0.50    1.22    --   96.35 117.00-150.00  122
 29  \w     28.00 105.00   0.50    1.22    --   96.35 -77.00 -90.00  154
 30  \w     44.00 127.00   0.50    1.22    --   96.35-145.00 -60.00  166
 31  \w     83.00 164.00   0.50    1.22    --   96.35  33.00 120.00  162
 32  \w     99.00 160.00   0.50    1.22    --   96.35 117.00-120.00  122
 33  \w     83.00 164.00   0.50    1.22    --   96.35  33.00-150.00  162
 34  \w     81.00 167.00   0.50    1.22    --   96.35  25.00-180.00  172
 35  \w     70.00 165.00   0.50    1.22    --   96.35  77.00-150.00  190
 36  \w     29.00  83.00   0.50    1.22    --   96.35 -68.00  30.00  108
 37  \w     83.00 164.00   0.50    1.22    --   96.35  33.00 -30.00  162
 38  \w     99.00 160.00   0.50    1.22    --   96.35 117.00 -30.00  122
 39  \w     33.00 110.00   0.50    1.22    --   96.35-117.00   0.00  154
 40  \w     77.00 163.00   0.50    1.22    --   96.35  50.00-180.00  172
 41  \w     33.00 110.00   0.50    1.22    --   96.35-117.00 -60.00  154
 42  \w     33.00 110.00   0.50    1.22    --   96.35-117.00 120.00  154
 43  \w    105.00 170.00   0.50    1.22    --   96.35  96.00-180.00  130
 44  \w     44.00 127.00   0.50    1.22    --   96.35-145.00-150.00  166
 45  \w     23.00 106.00   0.50    1.22    --   96.35 -96.00   0.00  166
 46  \w     99.00 160.00   0.50    1.22    --   96.35 117.00 120.00  122
 47  \w     30.00  57.00   0.50    1.22    --   96.35 -50.00 150.00   54
 48  \w     28.00 105.00   0.50    1.22    --   96.35 -77.00-120.00  154
 49  \w     44.00 127.00   0.50    1.22    --   96.35-145.00-120.00  166
 50  \w    105.00 170.00   0.50    1.22    --   96.35  96.00  60.00  130
 51  \w   -109.00 -14.00   0.50    0.31    --  -40.58 -77.00-150.00  190
 52  \w   -107.00 -25.00   0.50    0.31    --  -40.58 -38.00  30.00  164
 53  \w     18.00 109.00   0.50    0.31    --   40.58  62.00 152.38  182
 54  \w     18.00 108.00   0.50    0.31    --   40.58  64.00 -60.00  180
 55  \w     14.00 109.00   0.50    0.31    --   40.58  77.00-180.00  190
 56  \w     14.00 109.00   0.50    0.31    --   40.58  77.00   0.00  190
 57  \w     18.00 108.00   0.50    0.31    --   40.58  64.00 -90.00  180
 58  \w     12.00  43.00   0.50    0.31    --   40.58  83.00 -70.99   62
 59  \w     14.00 109.00   0.50    0.31    --   40.58  77.00  60.00  190
 60  \w      7.00  35.00   0.50    0.31    --   40.58  94.00 116.58   56
 61  \w     14.00 109.00   0.50    0.31    --   40.58  77.00 150.00  190
 62  \w     18.00  78.00   0.50    0.31    --   40.58-104.00   0.00  120
 63  \w     14.00 109.00   0.50    0.31    --   40.58  77.00-120.00  190
 64  \w     18.00 108.00   0.50    0.31    --   40.58  64.00  60.00  180
 65  \w     25.00 107.00   0.50    0.31    --   40.58  38.00 150.00  164
 66  \w   -150.00 -57.00   0.50    1.22    --  -82.50 -70.00 -54.82  186
 67  \w   -151.00 -56.00   0.50    1.22    --  -82.50 -74.00  76.18  190
 68  \w   -151.00 -55.00   0.50    1.22    --  -82.50 -77.00 143.18  192
 69  \w   -151.00 -56.00   0.50    1.22    --  -82.50 -74.00  22.09  190
 70  \w     70.00 165.00   0.50    1.22    --   96.35  77.00-120.00  190
 71  \w     72.00 164.00   0.50    1.22    --   96.35  68.00 -90.00  184
 72  \w     72.00 164.00   0.50    1.22    --   96.35  68.00  60.00  184
 73  \w     77.00 163.00   0.50    1.22    --   96.35  50.00  30.00  172
;
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.9964
_diffrn_reflns_Laue_measured_fraction_max 0.9898
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28990
_diffrn_reflns_point_group_measured_fraction_full 0.9964
_diffrn_reflns_point_group_measured_fraction_max 0.9898
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         5.62
_exptl_absorpt_coefficient_mu    2.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             583.267
_exptl_crystal_preparation       'solvent diffusion'
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.5564
_refine_diff_density_min         -0.3785
_refine_diff_density_rms         0.0533
_refine_ls_d_res_high            0.8302
_refine_ls_d_res_low             7.8719
_refine_ls_goodness_of_fit_ref   1.0696
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    79
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.0530
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.7657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              14
_reflns_limit_k_min              -15
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4713
_reflns_number_total             5241
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02757d2.cif
_cod_data_source_block           dm_chh_mghcs2_auto
_cod_depositor_comments
'Adding full bibliography for 7717142--7717146.cif.'
_cod_database_code               7717144
_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
 C13-C14 = C14-C15 = C15-C16 = C16-C17 = C17-C18 = C18-C13
 1.39 with sigma of 0.01
 C24-C29 = C29-C31 = C31-C28 = C28-C32 = C32-C27 = C27-C24
 1.39 with sigma of 0.01
 C25-C23 = C23-C1b = C1b-C1a = C1a-C1c = C1c-C22 = C22-C25
 1.39 with sigma of 0.01
 C13-C15 \\sim C14-C16 \\sim C15-C17 \\sim C16-C18 \\sim C17-C13 \\sim C18-C14
 with sigma of 0.02
 C24-C31 \\sim C29-C28 \\sim C31-C32 \\sim C28-C27 \\sim C32-C24 \\sim C27-C29
 with sigma of 0.02
 C25-C1b \\sim C23-C1a \\sim C1b-C1c \\sim C1a-C22 \\sim C1c-C25 \\sim C22-C23
 with sigma of 0.02
3. Restrained planarity
 C13, C14, C15, C16, C17, C18
 with sigma of 0.1
 C24, C29, C31, C28, C32, C27
 with sigma of 0.1
 C25, C23, C1b, C1a, C1c, C22
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C27 \\sim C24 \\sim C29 \\sim C32 \\sim C31 \\sim C28: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C1c) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C1b) \\sim Ueq, Uanis(C1a) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C1c, C25, C22, C23, C1b, C1a
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(C30)=Sof(H30a)=
 Sof(H30b)=Sof(O26)=Sof(C35)=Sof(H35a)=Sof(H35b)=1-FVAR(1)
 Sof(C24)=Sof(H24)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=
 Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=FVAR(1)
 Fixed Sof: C25(0.5) H25(0.5) C22(0.5) H22(0.5) C23(0.5) H23(0.5) C1a(0.5)
 H1a(0.5) C1b(0.5) H1b(0.5) C1c(0.5) H1c(0.5)
7.a Ternary CH refined with riding coordinates:
 C2(H2)
7.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C6(H6a,H6b), C34(H34a,H34b), C33(H33a,H33b), C30(H30a,H30b),
 C35(H35a,H35b)
7.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C17(H17), C11(H11), C10(H10), C15(H15), C24(H24), C27(H27), C28(H28),
 C29(H29), C31(H31), C32(H32), C25(H25), C22(H22), C23(H23), C1a(H1a), C1b(H1b),
  C1c(H1c)
7.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C19(H19a,H19b,H19c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c),
 C20(H20a,H20b,H20c), C21(H21a,H21b,H21c)
;
_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
;