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_7717145
_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         'C28 H38 Mg N4, 0.6[C6H6]'
_chemical_formula_sum            'C31.5 H42 Mg N4'
_chemical_formula_weight         501.017
_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'
_symmetry_Int_Tables_number      14
_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                 111.524(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6445(2)
_cell_length_b                   11.4598(1)
_cell_length_c                   18.6091(2)
_cell_measurement_reflns_used    20415
_cell_measurement_temperature    106(8)
_cell_measurement_theta_max      68.0540
_cell_measurement_theta_min      2.5800
_cell_volume                     2905.25(6)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      106.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.9971
_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    -75.00  23.00   0.50    0.60    --  -40.58 100.00  63.00  196
  2  \w     -1.00  76.00   0.50    0.60    --   40.58-100.00 -41.00  154
  3  \w   -154.00 -85.00   0.50    2.40    --  -82.50-100.00 -41.00  138
  4  \w    -81.00 -11.00   0.50    2.40    --  -82.50 100.00  63.00  140
  5  \w     25.00 106.00   0.50    2.40    --   96.35-100.00 -41.00  162
  6  \w    106.00 168.00   0.50    2.40    --   96.35 100.00  63.00  124
  7  \w    -57.00  26.00   0.50    0.60    --  -40.58  50.00  30.00  166
  8  \w    -24.00  35.00   0.50    0.60    --  -40.58  12.00 -30.00  118
  9  \w    -31.00  30.00   0.50    0.60    --  -40.58  25.00  90.00  122
 10  \w    -31.00  30.00   0.50    0.60    --  -40.58  25.00   0.00  122
 11  \w    -26.00  57.00   0.50    0.60    --   40.58 -50.00 -30.00  166
 12  \w    -35.00  24.00   0.50    0.60    --   40.58 -12.00 -60.00  118
 13  \w    -35.00  24.00   0.50    0.60    --   40.58 -12.00 150.00  118
 14  \w    -25.00  43.00   0.50    0.60    --   40.58 -38.00  30.00  136
 15  \w   -153.00 -68.00   0.50    2.40    --  -82.50 -25.00   0.00  170
 16  \w    -47.00 -15.00   0.50    2.40    --  -82.50  42.00-120.00   64
 17  \w    -47.00 -15.00   0.50    2.40    --  -82.50  42.00-150.00   64
 18  \w    -47.00 -15.00   0.50    2.40    --  -82.50  42.00   0.00   64
 19  \w     30.00  57.00   0.50    2.40    --   96.35 -50.00-180.00   54
 20  \w     81.00 165.00   0.50    2.40    --   96.35 145.00  30.00  168
 21  \w     30.00  57.00   0.50    2.40    --   96.35 -50.00  30.00   54
 22  \w     83.00 164.00   0.50    2.40    --   96.35  33.00-120.00  162
 23  \w     23.00 106.00   0.50    2.40    --   96.35 -96.00   0.00  166
 24  \w     30.00  57.00   0.50    2.40    --   96.35 -50.00 150.00   54
 25  \w     72.00 164.00   0.50    2.40    --   96.35  68.00  30.00  184
 26  \w     44.00 127.00   0.50    2.40    --   96.35-145.00-180.00  166
 27  \w     30.00  57.00   0.50    2.40    --   96.35 -50.00-150.00   54
 28  \w     44.00 127.00   0.50    2.40    --   96.35-145.00 150.00  166
 29  \w     28.00  68.00   0.50    2.40    --   96.35 -59.00-180.00   80
 30  \w     71.00 170.00   0.50    2.40    --   96.35  17.00 120.00  198
 31  \w     29.00  83.00   0.50    2.40    --   96.35 -68.00 -60.00  108
 32  \w     29.00  83.00   0.50    2.40    --   96.35 -68.00 150.00  108
 33  \w     28.00  68.00   0.50    2.40    --   96.35 -59.00   0.00   80
 34  \w     99.00 160.00   0.50    2.40    --   96.35 117.00 120.00  122
 35  \w     30.00  57.00   0.50    2.40    --   96.35 -50.00 -30.00   54
 36  \w   -109.00 -14.00   0.50    0.60    --  -40.58 -77.00 -30.00  190
 37  \w   -109.00 -14.00   0.50    0.60    --  -40.58 -77.00-120.00  190
 38  \w     18.00 108.00   0.50    0.60    --   40.58  64.00  60.00  180
 39  \w     14.00 109.00   0.50    0.60    --   40.58  77.00 120.00  190
 40  \w     18.00 108.00   0.50    0.60    --   40.58  64.00 -60.00  180
 41  \w     18.00  78.00   0.50    0.60    --   40.58-104.00-180.00  120
 42  \w     18.00 108.00   0.50    0.60    --   40.58  64.00   0.00  180
 43  \w     18.00 108.00   0.50    0.60    --   40.58  64.00-180.00  180
 44  \w     14.00 109.00   0.50    0.60    --   40.58  77.00  90.00  190
 45  \w    -29.00  31.00   0.50    0.60    --   40.58 -25.00  90.00  120
 46  \w     18.00 108.00   0.50    0.60    --   40.58  64.00-120.00  180
 47  \w     70.00 165.00   0.50    2.40    --   96.35  77.00 -90.00  190
 48  \w     77.00 163.00   0.50    2.40    --   96.35  50.00-180.00  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  0.0494
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.9971
_diffrn_reflns_Laue_measured_fraction_max 0.9953
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32463
_diffrn_reflns_point_group_measured_fraction_full 0.9971
_diffrn_reflns_point_group_measured_fraction_max 0.9953
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.15
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64710
_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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             1087.665
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.4092
_refine_diff_density_min         -0.2953
_refine_diff_density_rms         0.0413
_refine_ls_d_res_high            0.8306
_refine_ls_d_res_low             13.6233
_refine_ls_extinction_coef       0.00058(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0440
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    89
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5281
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.0127
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+1.3254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4654
_reflns_number_total             5281
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02757d2.cif
_cod_data_source_block           DMESDDH_auto
_cod_depositor_comments
'Adding full bibliography for 7717142--7717146.cif.'
_cod_database_code               7717145
_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
 C11-C12 \\sim C11-C12a
 with sigma of 0.02
 C12-C17 \\sim C12a-C17a
 with sigma of 0.02
 C12-C13 \\sim C12a-C13a
 with sigma of 0.02
 C17-C19 \\sim C17a-C19a
 with sigma of 0.02
 C17-C16 \\sim C17a-C16a
 with sigma of 0.02
 C13-C18 \\sim C13a-C18a
 with sigma of 0.02
 C13-C14 \\sim C13a-C14a
 with sigma of 0.02
 C14-C15 \\sim C14a-C15a
 with sigma of 0.02
 C16-C15 \\sim C16a-C15a
 with sigma of 0.02
 C15-C20a \\sim C15a-C20b
 with sigma of 0.02
 C11-C17 \\sim C11-C17a
 with sigma of 0.04
 C11-C13 \\sim C11-C13a
 with sigma of 0.04
 C12-C19 \\sim C12a-C19a
 with sigma of 0.04
 C12-C18 \\sim C12a-C18a
 with sigma of 0.04
 C12-C14 \\sim C12a-C14a
 with sigma of 0.04
 C12-C16 \\sim C12a-C16a
 with sigma of 0.04
 C17-C13 \\sim C17a-C13a
 with sigma of 0.04
 C17-C15 \\sim C17a-C15a
 with sigma of 0.04
 C13-C15 \\sim C13a-C15a
 with sigma of 0.04
 C19-C16 \\sim C19a-C16a
 with sigma of 0.04
 C18-C14 \\sim C18a-C14a
 with sigma of 0.04
 C14-C16 \\sim C14a-C16a
 with sigma of 0.04
 C14-C20a \\sim C14a-C20b
 with sigma of 0.04
 C16-C20a \\sim C16a-C20b
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C1a) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C1b) \\sim Ueq, Uanis(C31) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1a) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C1b) \\sim Ueq, Uanis(C31) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C12, C17, C13, C19, C18, C14, C16, C15, C20a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12a, C17a, C13a, C19a, C18a, C14a, C16a, C15a, C20b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1a, C33, C20, C30, C29, C1b, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C12a)=Sof(C17a)=Sof(C13a)=Sof(C19a)=Sof(H19d)=Sof(H19e)=Sof(H19f)=
 Sof(C18a)=Sof(H18d)=Sof(H18e)=Sof(H18f)=Sof(C14a)=Sof(H14a)=Sof(C16a)=
 Sof(H16a)=Sof(C15a)=Sof(C20b)=Sof(H20d)=Sof(H20e)=Sof(H20f)=1-FVAR(1)
 Sof(C12)=Sof(C17)=Sof(C13)=Sof(C19)=Sof(H19a)=Sof(H19b)=Sof(H19c)=Sof(C18)=
 Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(C14)=Sof(H14)=Sof(C16)=Sof(H16)=Sof(C15)=
 Sof(C20a)=Sof(H20a)=Sof(H20b)=Sof(H20c)=FVAR(1)
 Fixed Sof: H33(0.5) H29(0.5) H31(0.5) H30(0.5) H20(0.5) H1ba(0.5) H1bb(0.5)
 H1bc(0.5) C33(0.5) H33(0.5) C20(0.5) H20(0.5) C29(0.5) H29(0.5) C30(0.5)
 H30(0.5) C31(0.5) H31(0.5) C1a(0.5) C1b(0.5) H1ba(0.5) H1bb(0.5) H1bc(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C6(H6), C10(H10), C27(H27), C23(H23), C24(H24), C14(H14),
 C16(H16), C26(H26), C14a(H14a), C16a(H16a), C33(H33), C20(H20), C29(H29),
 C30(H30), C31(H31)
6.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C5(H5a,H5b,H5c),
 C18(H18a,H18b,H18c), C21(H21a,H21b,H21c), C28(H28a,H28b,H28c), C20a(H20a,H20b,
 H20c), C19a(H19d,H19e,H19f), C18a(H18d,H18e,H18f), C20b(H20d,H20e,H20f),
 C1b(H1ba,H1bb,H1bc)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.741