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_7715667
_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         'C32 H88 N4 O3 Si8 Sm2'
_chemical_formula_sum            'C32 H88 N4 O3 Si8 Sm2'
_chemical_formula_weight         1102.48
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-05 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                119.001(3)
_cell_angle_beta                 102.554(2)
_cell_angle_gamma                91.310(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8990(3)
_cell_length_b                   12.0887(3)
_cell_length_c                   12.2407(3)
_cell_measurement_reflns_used    23183
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.8100
_cell_measurement_theta_min      1.9300
_cell_volume                     1361.20(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -71.00  17.00   0.50    0.60    --    4.55 -19.00 150.00  176
  2  \w    -68.00  18.00   0.50    0.60    --    4.55 -38.00  90.00  172
  3  \w    -18.00  38.00   0.50    0.60    --    4.55 -99.00 -90.00  112
  4  \w    -18.00  38.00   0.50    0.60    --    4.55 -99.00 -30.00  112
  5  \w    -18.00  27.00   0.50    0.60    --   -6.43 -99.00   0.00   90
  6  \w    -27.00  66.00   0.50    0.60    --   -6.43  72.00 -57.00  186
  7  \w    -79.00 -51.00   0.50    0.60    --   -6.43 -57.00 -90.00   56
  8  \w    -79.00   7.00   0.50    0.60    --   -6.43 -38.00   0.00  172
  9  \w    -79.00  14.00   0.50    0.60    --   -6.43 -72.00 173.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0287130000
_diffrn_orient_matrix_UB_12      -0.0006426000
_diffrn_orient_matrix_UB_13      0.0575041000
_diffrn_orient_matrix_UB_21      0.0460414000
_diffrn_orient_matrix_UB_22      -0.0351507000
_diffrn_orient_matrix_UB_23      -0.0295930000
_diffrn_orient_matrix_UB_31      0.0400464000
_diffrn_orient_matrix_UB_32      0.0580385000
_diffrn_orient_matrix_UB_33      0.0229917000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28184
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         1.936
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5560
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0436P)^2^+1.8272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5210
_reflns_number_total             5560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00061g2.cif
_cod_data_source_block           yj-670-2_auto
_cod_original_cell_volume        1361.20(7)
_cod_database_code               7715667
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Sm1C1N1Si1O1
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.751
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C),
  C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              70015
_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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.802