Synthesis and Reactivity of Magnesium Complexes Supported by Tris(2-dimethylaminoethyl)amine (Me6tren)
Guard, Louise M.; Hazari, Nilay; Organometallics 32 (2013) 2787–; doi:10.1021/om4002186

data_4080823
_publ_section_title
;
 Synthesis and Reactivity of Magnesium Complexes Supported by
 Tris(2-dimethylaminoethyl)amine (Me6tren)
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2787
_journal_paper_doi               10.1021/om4002186
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C14 H36 Mg N4'
_chemical_formula_sum            'C14 H36 Mg N4'
_chemical_formula_weight         284.78
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.555(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3141(3)
_cell_length_b                   11.5776(5)
_cell_length_c                   19.5193(14)
_cell_measurement_reflns_used    10387
_cell_measurement_temperature    223
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.3
_cell_volume                     1852.81(17)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      223
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -120.0000 - 60.0000
         Image width: 1.0000
            Exp time: 50.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 0.0000
                 XTD: 50.2626
              2theta: -28.5158
scan:
    Number of images: 180
               Slice: -120.0000 - 60.0000
         Image width: 1.0000
            Exp time: 50.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 120.0000
                 XTD: 50.2626
              2theta: -28.5158
scan:
    Number of images: 180
               Slice: -120.0000 - 60.0000
         Image width: 1.0000
            Exp time: 50.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 240.0000
                 XTD: 50.2626
              2theta: -28.5158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.010142
_diffrn_orient_matrix_UB_12      0.001574
_diffrn_orient_matrix_UB_13      -0.081373
_diffrn_orient_matrix_UB_21      -0.056174
_diffrn_orient_matrix_UB_22      -0.059203
_diffrn_orient_matrix_UB_23      -0.008147
_diffrn_orient_matrix_UB_31      -0.058894
_diffrn_orient_matrix_UB_32      0.056740
_diffrn_orient_matrix_UB_33      -0.006243
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36292
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_recrystallization_method 'ether/pentane at -30C'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4566
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.5807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                3617
_reflns_number_total             4566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002186_si_002.cif
_cod_data_source_block           '_Compound5'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.3.1 from 2005-06-27.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1852.80(16)
_cod_database_code               4080823
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H4A,H4B} of C4, {H7A,H7B} of C7, {H8A,H8B} of C8, {H11A,H11B} of C11A,
  {H3A,H3B} of C3, {H12A,H12B} of C12A, {H11C,H11D} of C11B, {H12C,H12D} of C12B
 At 1.5 times of:
  {H5A,H5B,H5C} of C5, {H6A,H6B,H6C} of C6, {H9A,H9B,H9C} of C9, {H10A,H10B,
  H10C} of C10, {H2A,H2B,H2C} of C2, {H1A,H1B,H1C} of C1, {H13A,H13B,H13C} of
  C13A, {H14A,H14B,H14C} of C14A, {H13D,H13E,H13F} of C13B, {H14D,H14E,H14F} of
  C14B
2. Rigid bond restraints
 N2, C11A, C12A, N4A, C13A, C14A, C11B, C12B, N4B, C13B, C14B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
N2 ~ C11A ~ C12A ~ N4A ~ C13A ~ C14A ~ C11B ~ C12B ~ N4B ~ C13B ~ C14B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Same fragment restrains
{N2, C11A, C12A, N4A, C14A, C13A}
{N2, C11B, C12B, N4B, C13B, C14B}
as
{N2, C11A, C12A, N4A, C13A, C14A}
5. Others
 Fixed Sof: C11A(0.31206) H11A(0.31206) H11B(0.31206) C12A(0.31206)
 H12A(0.31206) H12B(0.31206) N4A(0.31206) C13A(0.31206) H13A(0.31206)
 H13B(0.31206) H13C(0.31206) C14A(0.31206) H14A(0.31206) H14B(0.31206)
 H14C(0.31206) C11B(0.68794) H11C(0.68794) H11D(0.68794) C12B(0.68794)
 H12C(0.68794) H12D(0.68794) N4B(0.68794) C13B(0.68794) H13D(0.68794)
 H13E(0.68794) H13F(0.68794) C14B(0.68794) H14D(0.68794) H14E(0.68794)
 H14F(0.68794)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C11A(H11A,H11B),
 C12A(H12A,H12B), C11B(H11C,H11D), C12B(H12C,H12D)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C),
 C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F)
;