Magnesium catalyzed hydroamination of carbodiimides and hydroboration of cyanamides.
Das, Anubhab; Mukhopadhyay, Sayantan; Rajput, Sagrika; Nembenna, Sharanappa; Dalton transactions (Cambridge, England : 2003) 54 (2025) 17553–17563; doi:10.1039/d5dt02335a

data_7719777
_publ_section_title
;
 Magnesium catalyzed hydroamination of carbodiimides and hydroboration of
 cyanamides.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17553
_journal_page_last               17563
_journal_paper_doi               10.1039/d5dt02335a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C64 H82 Mg2 N6'
_chemical_formula_sum            'C64 H82 Mg2 N6'
_chemical_formula_weight         983.97
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-09-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-09-23 deposited with the CCDC.	2025-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                96.9060(10)
_cell_angle_beta                 105.6670(10)
_cell_angle_gamma                98.9370(10)
_cell_formula_units_Z            4
_cell_length_a                   13.32290(10)
_cell_length_b                   21.27950(10)
_cell_length_c                   21.37550(10)
_cell_measurement_reflns_used    72116
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      77.4710
_cell_measurement_theta_min      3.3150
_cell_volume                     5679.65(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_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 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_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    -67.00  28.00   0.38    0.35    --  -38.50  86.00 -67.00  250
  2  \w    -10.00  76.64   0.38    0.35    --   49.06 -86.00 173.00  228
  3  \w     39.00 134.00   0.38    1.40    --  106.83 -86.00 173.00  250
  4  \w    102.00 173.82   0.38    1.40    --  106.83  86.00 -67.00  189
  5  \w   -101.00 -28.04   0.38    0.35    --  -38.50 -57.00 150.00  192
  6  \w     28.00  96.78   0.38    0.35    --   49.06-125.00-180.00  181
  7  \w     38.00 110.96   0.38    0.35    --   49.06  57.00  30.00  192
  8  \w     38.00 110.96   0.38    0.35    --   49.06  57.00 -60.00  192
  9  \w    102.00 169.64   0.38    1.40    --  106.83  45.00 -90.00  178
 10  \w    104.00 173.92   0.38    1.40    --  106.83  30.00 150.00  184
 11  \w     42.00 109.64   0.38    1.40    --  106.83 -45.00-120.00  178
 12  \w     39.00 104.74   0.38    1.40    --  106.83 -94.00 -30.00  173
 13  \w     39.00 108.92   0.38    1.40    --  106.83 -30.00 120.00  184
 14  \w     39.00 115.00   0.38    1.40    --  106.83 -15.00 120.00  200
 15  \w     44.00 120.00   0.38    1.40    --  106.83 -61.00-150.00  200
 16  \w     42.00 109.64   0.38    1.40    --  106.83 -45.00 -30.00  178
 17  \w     39.00 104.74   0.38    1.40    --  106.83 -94.00   0.00  173
 18  \w     39.00 104.74   0.38    1.40    --  106.83 -94.00 120.00  173
 19  \w     39.00 104.74   0.38    1.40    --  106.83 -94.00  60.00  173
 20  \w     39.00 104.74   0.38    1.40    --  106.83 -94.00 150.00  173
 21  \w     94.00 170.00   0.38    1.40    --  106.83  61.00-120.00  200
 22  \w     39.00 108.92   0.38    1.40    --  106.83 -30.00 -60.00  184
 23  \w     38.00 110.96   0.38    0.35    --   49.06  57.00   0.00  192
 24  \w     38.00 110.96   0.38    0.35    --   49.06  57.00-180.00  192
 25  \w     38.00 110.96   0.38    0.35    --   49.06  57.00-120.00  192
 26  \w     38.00 110.96   0.38    0.35    --   49.06  57.00 -90.00  192
 27  \w     38.00 110.96   0.38    0.35    --   49.06  57.00  90.00  192
 28  \w     38.00 110.96   0.38    0.35    --   49.06  57.00 120.00  192
 29  \w    104.00 173.92   0.38    1.40    --  106.83  30.00  90.00  184
 30  \w     94.00 170.00   0.38    1.40    --  106.83  61.00-150.00  200
 31  \w    104.00 173.92   0.38    1.40    --  106.83  30.00 120.00  184
 32  \w     99.00 175.00   0.38    1.40    --  106.83  15.00 -30.00  200
 33  \w    104.00 173.92   0.38    1.40    --  106.83  30.00  60.00  184
 34  \w     94.00 170.00   0.38    1.40    --  106.83  61.00   0.00  200
 35  \w     94.00 170.00   0.38    1.40    --  106.83  61.00 -30.00  200
 36  \w     94.00 170.00   0.38    1.40    --  106.83  61.00 150.00  200
 37  \w     99.00 175.00   0.38    1.40    --  106.83  15.00-150.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            98358
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.100
_diffrn_reflns_theta_min         3.300
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.00024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1342
_refine_ls_number_reflns         22189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+3.7778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20733
_reflns_number_total             22189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02335a2.cif
_cod_data_source_block           compound_mg_2
_cod_depositor_comments
'Adding full bibliography for 7719777--7719779.cif.'
_cod_database_code               7719777
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.871
_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:
 C24(H24A,H24B), C26(H26A,H26B), C90(H90A,H90B), C30(H30A,H30B), C113(H11A,
 H11B), C117(H11C,H11D), C86(H86A,H86B), C59(H59A,H59B), C61(H61A,H61B),
 C28(H28A,H28B), C119(H11E,H11F), C88(H88A,H88B), C63(H63A,H63B), C115(H11J,
 H11K), C92(H92A,H92B), C65(H65A,H65B)
2.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C6(H6A), C10(H10), C14(H14), C2(H2), C22(H22), C37(H37), C33(H33),
 C57(H57), C49(H49), C98(H98), C34(H34), C131(H131), C141(H141), C55(H55),
 C21(H21), C48(H48), C97(H97), C20(H20), C56(H56), C139(H139), C125(H125),
 C96(H96), C138(H138), C134(H134), C123(H123), C142(H142), C130(H130), C36(H36),
  C84(H84), C133(H133), C122(H122), C83(H83), C82(H82), C111(H111), C126(H126),
 C110(H110), C109(H109), C70(H70), C71(H71), C69(H69), C44(H44), C42(H42),
 C43(H43)
2.c Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C78(H78A,H78B,H78C), C38(H38A,H38B,H38C), C51(H51A,H51B,
 H51C), C106(H10A,H10B,H10C), C105(H10D,H10E,H10F), C52(H52A,H52B,H52C),
 C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C91(H91A,H91B,H91C), C17(H17A,H17B,
 H17C), C27(H27A,H27B,H27C), C60(H60A,H60B,H60C), C120(H12A,H12B,H12C),
 C114(H11G,H11H,H11I), C128(H12D,H12E,H12F), C29(H29A,H29B,H29C), C144(H14A,
 H14B,H14C), C136(H13A,H13B,H13C), C87(H87A,H87B,H87C), C39(H39A,H39B,H39C),
 C89(H89A,H89B,H89C), C118(H11L,H11M,H11N), C64(H64A,H64B,H64C), C93(H93A,H93B,
 H93C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C), C116(H11O,H11P,H11Q)
;
_shelx_res_checksum              19444
_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
;