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_7719778
_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 H80 Mg2 N4 O2'
_chemical_formula_sum            'C64 H80 Mg2 N4 O2'
_chemical_formula_weight         985.94
_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   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                90
_cell_angle_beta                 100.1610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4339(2)
_cell_length_b                   17.9921(2)
_cell_length_c                   13.7145(2)
_cell_measurement_reflns_used    14839
_cell_measurement_temperature    99.98(14)
_cell_measurement_theta_max      77.3880
_cell_measurement_theta_min      3.9330
_cell_volume                     2777.09(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 0.969
_diffrn_measured_fraction_theta_max 0.968
_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    -62.00  26.00   0.50    0.79    --  -38.50  78.00 113.00  176
  2  \w    -16.00  73.00   0.50    0.79    --   49.06 -78.00 -11.00  178
  3  \w    103.00 172.00   0.50    3.09    --  106.83  78.00 113.00  138
  4  \w    105.00 131.00   0.50    3.09    --  106.83  30.00  30.00   52
  5  \w    -42.00  28.00   0.50    0.79    --  -38.50  38.00-120.00  140
  6  \w    -50.00  24.00   0.50    0.79    --  -38.50  57.00-150.00  148
  7  \w     46.00 115.00   0.50    0.79    --   49.06  38.00 -60.00  138
  8  \w     38.00 112.00   0.50    0.79    --   49.06  57.00-180.00  148
  9  \w    105.00 175.00   0.50    3.09    --  106.83  30.00  30.00  140
 10  \w    150.00 175.00   0.50    3.09    --  106.83  30.00  30.00   50
 11  \w     43.00  73.00   0.50    3.09    --  106.83 -30.00   0.00   60
 12  \w     75.00 108.00   0.50    3.09    --  106.83 -45.00  30.00   66
 13  \w     80.00 110.00   0.50    3.09    --  106.83 -30.00   0.00   60
 14  \w     43.00 104.00   0.50    3.09    --  106.83 -94.00-120.00  122
 15  \w    100.00 169.00   0.50    3.09    --  106.83  61.00 150.00  138
 16  \w     56.00 106.00   0.50    3.09    --  106.83 -94.00 120.00  100
 17  \w     66.00 101.00   0.50    3.09    --  106.83 -94.00 -90.00   70
 18  \w    117.00 171.00   0.50    3.09    --  106.83  77.00  60.00  108
 19  \w    105.00 168.00   0.50    3.09    --  106.83 125.00 -30.00  126
 20  \w    136.00 168.00   0.50    3.09    --  106.83  77.00-180.00   64
;
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18031
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         4.094
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45610
_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    1.179
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0595P)^2^+3.0922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4630
_reflns_number_total             4932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02335a2.cif
_cod_data_source_block           compound_mg_4
_cod_depositor_comments
'Adding full bibliography for 7719777--7719779.cif.'
_cod_database_code               7719778
_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:
 C00H(H00E,H00G), C00I(H00H,H00I), C00U(H00U,H00V), C00Z(H2,HD)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C00D(H00D), C00F(H00F), C00J(H00J), C00K(H00K), C00M(H00M),
 C00N(H00N), C00O(H00O), C00R(H00R), C00S(H00S), C00T(H00T), C00W(H00Z)
2.c Idealised Me refined as rotating group:
 C00G(H00A,H00B,H00C), C00P(H00L,H00P,H00Q), C00V(H00W,H00X,H00Y), C00X(H00,H,
 HA), C00Y(H1,HB,HC), C010(H01A,H01B,H01C)
;
_shelx_res_checksum              4976
_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
;