The addition of Grignard reagents to carbodiimides. The synthesis, structure and potential utilization of magnesium amidinates.
Chlupatý, Tomáš; Bílek, Michal; Merna, Jan; Brus, Jiří; RůŽičková, Zdeňka; Strassner, Thomas; RůŽička, Aleš; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5335–5342; doi:10.1039/c9dt00880b

data_7049473
_publ_section_title
;
 The addition of Grignard reagents to carbodiimides. The synthesis,
 structure and potential utilization of magnesium amidinates.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5335
_journal_page_last               5342
_journal_paper_doi               10.1039/c9dt00880b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C25 H40 I2 Mg2 N2 O2'
_chemical_formula_sum            'C25 H40 I2 Mg2 N2 O2'
_chemical_formula_weight         703.01
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2019-02-21 deposited with the CCDC.    2019-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.168(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.361(2)
_cell_length_b                   8.5970(9)
_cell_length_c                   26.456(3)
_cell_measurement_reflns_used    32656
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     6368.1(11)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 25.035
_diffrn_measured_fraction_theta_max 26.372
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30794
_diffrn_reflns_point_group_measured_fraction_full 25.035
_diffrn_reflns_point_group_measured_fraction_max 26.372
_diffrn_reflns_theta_full        25.035
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         4.076
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.036
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0525 before and 0.0238 after correction.
The Ratio of minimum to maximum transmission is 0.6000.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0387P)^2^+41.7826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8352
_reflns_number_total             11280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00880b2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7049472--7049477.cif.'
_cod_database_code               7049473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H12F,H12G,H12H} of C122, {H12A,H12B,H12C} of C120, {H11I,
  H11J,H11K} of C118, {H11D,H11E,H11F} of C116, {H11A,H11B,H11C} of C115, {H10A,
  H10B,H10C} of C108, {H12K,H12L,H12M} of C124, {H20A,H20B,H20C} of C20, {H18A,
  H18B,H18C} of C18, {H16A,H16B,H16C} of C16, {H15A,H15B,H15C} of C15, {H22A,
  H22B,H22C} of C22, {H24A,H24B,H24C} of C24, {H8A,H8B,H8C} of C8, All C(H,H)
  groups
 At 1.5 times of:
  {H12N,H12O,H12P} of C125, {H25A,H25B,H25C} of C25
2.a Riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8A,H8B,H8C), C10(H10), C11(H11), C13(H13),
  C14(H14), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B), C18(H18A,
 H18B,H18C), C19(H19A,H19B), C20(H20A,H20B,H20C), C21(H21A,H21B), C22(H22A,H22B,
 H22C), C23(H23A,H23B), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C103(H103),
 C104(H104), C106(H106), C107(H107), C108(H10A,H10B,H10C), C110(H110),
 C111(H111), C113(H113), C114(H114), C115(H11A,H11B,H11C), C116(H11D,H11E,H11F),
  C117(H11G,H11H), C118(H11I,H11J,H11K), C119(H11L,H11M), C120(H12A,H12B,H12C),
 C121(H12D,H12E), C122(H12F,H12G,H12H), C123(H12I,H12J), C124(H12K,H12L,H12M),
 C125(H12N,H12O,H12P)
;