Formation of <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediamine <i>via</i> coupling of the two charge reversed C-N bonds of Me<sub>3</sub>NO in the presence of an Eu(II) bis(trimethylsilyl)amide complex.
Li, Yangjuan; Gong, Yu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5342–5345; doi:10.1039/d4dt00061g

data_7715665
_publ_section_title
;
 Formation of
 <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediamine
 <i>via</i> coupling of the two charge reversed C-N bonds of
 Me<sub>3</sub>NO in the presence of an Eu(II) bis(trimethylsilyl)amide
 complex.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5342
_journal_page_last               5345
_journal_paper_doi               10.1039/d4dt00061g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H52 Eu N4 Si4'
_chemical_formula_sum            'C18 H52 Eu N4 Si4'
_chemical_formula_weight         588.95
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-11-08 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.988(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6046(2)
_cell_length_b                   17.8193(4)
_cell_length_c                   20.3916(4)
_cell_measurement_reflns_used    14728
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      31.0950
_cell_measurement_theta_min      2.0250
_cell_volume                     3058.41(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_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    -18.00  38.00   0.50    2.00    --    4.55 -99.00  30.00  112
  2  \w    -79.00   7.00   0.50    2.00    --   -6.43 -38.00 -60.00  172
  3  \w    -68.00 -43.00   0.50    2.00    --    4.55 -38.00-120.00   50
  4  \w     -9.00  78.00   0.50    2.00    --    4.55  38.00-150.00  174
  5  \w    -19.00  69.00   0.50    2.00    --   -6.43  19.00 120.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026082000
_diffrn_orient_matrix_UB_12      -0.0350508000
_diffrn_orient_matrix_UB_13      0.0162195000
_diffrn_orient_matrix_UB_21      0.0111648000
_diffrn_orient_matrix_UB_22      -0.0188027000
_diffrn_orient_matrix_UB_23      -0.0293297000
_diffrn_orient_matrix_UB_31      0.0834892000
_diffrn_orient_matrix_UB_32      0.0013939000
_diffrn_orient_matrix_UB_33      0.0118933000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18076
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.042
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.218
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.7551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3387
_reflns_number_total             3685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00061g2.cif
_cod_data_source_block           yj-569_auto
_cod_database_code               7715665
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         Eu1N1C1Si1H1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.878
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C5(H5A,
 H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              22643
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.151
_oxdiff_exptl_absorpt_empirical_full_min 0.858