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_7719779
_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         'C60 H88 Mg2 N8'
_chemical_formula_sum            'C60 H88 Mg2 N8'
_chemical_formula_weight         970.00
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_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                90
_cell_angle_beta                 102.311(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6329(3)
_cell_length_b                   15.0775(3)
_cell_length_c                   14.1556(3)
_cell_measurement_reflns_used    16518
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.5630
_cell_measurement_theta_min      4.3080
_cell_volume                     2842.78(11)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -61.00  26.00   0.50    0.49    --  -38.50  76.00-130.00  174
  2  \w    -15.00  72.00   0.50    0.49    --   49.31 -76.00 102.00  174
  3  \w     39.00 125.00   0.50    1.96    --  102.63 -76.00 102.00  172
  4  \w    103.00 167.00   0.50    1.96    --  102.63  76.00-130.00  128
  5  \w    -42.00  28.00   0.50    0.49    --  -38.50  37.00 -30.00  140
  6  \w    -42.00  28.00   0.50    0.49    --  -38.50  37.00  30.00  140
  7  \w     46.00 116.00   0.50    0.49    --   49.31  37.00 -30.00  140
  8  \w     35.00 106.00   0.50    1.96    --  102.63 -30.00 120.00  142
  9  \w     38.00 107.00   0.50    1.96    --  102.63 -45.00 150.00  138
 10  \w     40.00 112.00   0.50    1.96    --  102.63-125.00   0.00  144
 11  \w     97.00 166.00   0.50    1.96    --  102.63 125.00-180.00  138
 12  \w     34.00 111.00   0.50    1.96    --  102.63 -15.00  60.00  154
 13  \w     40.00 116.00   0.50    1.96    --  102.63 -61.00 -30.00  152
 14  \w    103.00 167.00   0.50    1.96    --  102.63  77.00-180.00  128
 15  \w    103.00 167.00   0.50    1.96    --  102.63  77.00 120.00  128
 16  \w     97.00 166.00   0.50    1.96    --  102.63 125.00-150.00  138
 17  \w     98.00 165.00   0.50    1.96    --  102.63  45.00 150.00  134
;
_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  0.0467
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21398
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         4.088
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76279
_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    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0944P)^2^+0.9349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4848
_reflns_number_total             5205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02335a2.cif
_cod_data_source_block           compound_mg_3
_cod_depositor_comments
'Adding full bibliography for 7719777--7719779.cif.'
_cod_original_cell_volume        2842.77(11)
_cod_database_code               7719779
_shelx_shelxl_version_number     2019/3
_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:
 C9(H9A,H9B), C32(H32A,H32B), C30(H30A,H30B), C28(H28A,H28B), C34(H34A,H34B),
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C26(H26), C12(H12), C24(H24), C25(H25), C13(H13), C11(H11)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C35(H35A,H35B,H35C), C10(H10A,H10B,H10C),
 C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              97601
_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
;