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_7717143
_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         'C29 H38 I Mg N5, 1[C4H8O]'
_chemical_formula_sum            'C33 H46 I Mg N5 O'
_chemical_formula_weight         679.96
_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
_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                 106.939(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2666(2)
_cell_length_b                   21.1640(3)
_cell_length_c                   15.6557(2)
_cell_measurement_reflns_used    22983
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      68.0330
_cell_measurement_theta_min      3.5960
_cell_volume                     3571.09(10)
_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 (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    '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 0.995
_diffrn_measured_fraction_theta_max 0.986
_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    -79.00   0.00   0.50    1.24    --  -40.58 109.00 -62.00  158
  2  \w     22.00  80.00   0.50    1.24    --   40.58-109.00-158.00  116
  3  \w   -150.00 -81.00   0.50    4.97    --  -82.50-109.00-158.00  138
  4  \w    -82.00 -15.00   0.50    4.97    --  -82.50 109.00 -62.00  134
  5  \w     29.00 108.00   0.50    4.97    --   96.35-109.00-158.00  158
  6  \w    103.00 164.00   0.50    4.97    --   96.35 109.00 -62.00  122
  7  \w    -24.00  35.00   0.50    1.24    --  -40.58  12.00-120.00  118
  8  \w    -31.00  30.00   0.50    1.24    --  -40.58  25.00   0.00  122
  9  \w    -43.00  26.00   0.50    1.24    --  -40.58  38.00 -60.00  138
 10  \w   -107.00 -21.00   0.50    1.24    --  -40.58 -50.00-180.00  172
 11  \w    -24.00  35.00   0.50    1.24    --  -40.58  12.00 120.00  118
 12  \w     41.00 100.00   0.50    1.24    --   40.58-138.00-120.00  118
 13  \w     41.00 100.00   0.50    1.24    --   40.58-138.00 120.00  118
 14  \w    -35.00  24.00   0.50    1.24    --   40.58 -12.00  90.00  118
 15  \w    -47.00 -15.00   0.50    4.97    --  -82.50  42.00  90.00   64
 16  \w    -57.00 -16.00   0.50    4.97    --  -82.50  50.00-120.00   82
 17  \w   -149.00 -63.00   0.50    4.97    --  -82.50 -50.00-120.00  172
 18  \w    -47.00 -15.00   0.50    4.97    --  -82.50  42.00 -30.00   64
 19  \w     29.00  83.00   0.50    4.97    --   96.35 -68.00 -90.00  108
 20  \w     83.00 164.00   0.50    4.97    --   96.35  33.00 120.00  162
 21  \w     30.00  57.00   0.50    4.97    --   96.35 -50.00  60.00   54
 22  \w     81.00 165.00   0.50    4.97    --   96.35 145.00  90.00  168
 23  \w     30.00  57.00   0.50    4.97    --   96.35 -50.00 -90.00   54
 24  \w     29.00  83.00   0.50    4.97    --   96.35 -68.00-120.00  108
 25  \w     30.00  57.00   0.50    4.97    --   96.35 -50.00  90.00   54
 26  \w     26.00 127.00   0.50    4.97    --   96.35 -87.00-150.00  202
 27  \w     33.00 110.00   0.50    4.97    --   96.35-117.00 -90.00  154
 28  \w     81.00 167.00   0.50    4.97    --   96.35  25.00 -60.00  172
 29  \w     71.00 170.00   0.50    4.97    --   96.35  17.00-120.00  198
 30  \w     30.00  57.00   0.50    4.97    --   96.35 -50.00-180.00   54
 31  \w     70.00 165.00   0.50    4.97    --   96.35  77.00  30.00  190
 32  \w     30.00  57.00   0.50    4.97    --   96.35 -50.00 -30.00   54
 33  \w     28.00  68.00   0.50    4.97    --   96.35 -59.00 120.00   80
 34  \w     30.00  57.00   0.50    4.97    --   96.35 -50.00-120.00   54
 35  \w     30.00  57.00   0.50    4.97    --   96.35 -50.00 -60.00   54
 36  \w   -107.00 -21.00   0.50    1.24    --  -40.58 -50.00 -30.00  172
 37  \w   -108.00 -17.00   0.50    1.24    --  -40.58 -64.00 -90.00  182
 38  \w   -109.00 -14.00   0.50    1.24    --  -40.58 -77.00  60.00  190
 39  \w   -109.00 -14.00   0.50    1.24    --  -40.58 -77.00 150.00  190
 40  \w   -108.00 -17.00   0.50    1.24    --  -40.58 -64.00  90.00  182
 41  \w   -109.00 -14.00   0.50    1.24    --  -40.58 -77.00-150.00  190
 42  \w   -109.00 -14.00   0.50    1.24    --  -40.58 -77.00 -30.00  190
 43  \w   -109.00 -14.00   0.50    1.24    --  -40.58 -77.00  30.00  190
 44  \w   -109.00 -14.00   0.50    1.24    --  -40.58 -77.00 -90.00  190
 45  \w   -109.00 -14.00   0.50    1.24    --  -40.58 -77.00  90.00  190
 46  \w    -96.00 -19.00   0.50    1.24    --  -40.58 138.00  30.00  154
 47  \w     72.00 164.00   0.50    4.97    --   96.35  68.00 150.00  184
 48  \w     28.00 105.00   0.50    4.97    --   96.35 -77.00  30.00  154
 49  \w     70.00 121.00   0.50    4.97    --   96.35  77.00  60.00  102
 50  \w     80.00 164.00   0.50    4.97    --   96.35  42.00   0.00  168
;
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41954
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.333
_diffrn_reflns_theta_min         3.615
_exptl_absorpt_coefficient_mu    7.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55126
_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    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.916
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0521
_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^)+(0.1090P)^2^+1.5465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5601
_reflns_number_total             6464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02757d2.cif
_cod_data_source_block           dm_cmmghbenz_auto
_cod_depositor_comments
'Adding full bibliography for 7717142--7717146.cif.'
_cod_database_code               7717143
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.449
_shelx_estimated_absorpt_t_min   0.368
_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:
 C3(H3A,H3B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C28(H28), C27(H27), C25(H25), C8(H8), C10(H10), C26(H26), C9(H9),
 C18(H18), C15(H15)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C),
 C5(H5A,H5B,H5C), C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 154 electrons were 
found in a volume of 998\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O] per Formula Unit 
which account for 160 electrons 
per unit cell.
;
_shelx_res_checksum              42609
_shelx_hkl_checksum              45373
_shelx_fab_checksum              45704
_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
;