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_4080822
_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         '4(C12 H30 Br Mg N4), 2(Br4 Mg), C7 H8'
_chemical_formula_sum            'C55 H128 Br12 Mg6 N16'
_chemical_formula_weight         2118.51
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 113.437(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1927(3)
_cell_length_b                   19.9755(4)
_cell_length_c                   15.9698(11)
_cell_measurement_reflns_used    68335
_cell_measurement_temperature    93
_cell_measurement_theta_max      65.9
_cell_measurement_theta_min      2.2
_cell_volume                     4446.7(4)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -48.0000 - 132.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 15.0000
                 Phi: 0.0000
                 XTD: 50.0000
              2theta: 42.0000
scan:
    Number of images: 360
               Slice: -48.0000 - 132.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 30.0000
                 Phi: 90.0000
                 XTD: 50.0000
              2theta: 42.0000
scan:
    Number of images: 342
               Slice: -48.0000 - 123.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 45.0000
                 Phi: 90.0000
                 XTD: 50.0000
              2theta: 42.0000
scan:
    Number of images: 330
               Slice: -48.0000 - 117.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 15.0000
                 Phi: 90.0000
                 XTD: 50.0000
              2theta: 42.0000
scan:
    Number of images: 344
               Slice: -48.0000 - 124.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 30.0000
                 Phi: 180.0000
                 XTD: 50.0000
              2theta: 42.0000
scan:
    Number of images: 360
               Slice: -48.0000 - 132.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 45.0000
                 Phi: 180.0000
                 XTD: 50.0000
              2theta: 42.0000
scan:
    Number of images: 180
               Slice: -25.0000 - 65.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 45.0000
                 Phi: 0.0000
                 XTD: 50.0000
              2theta: 42.0000
scan:
    Number of images: 360
               Slice: 0.0000 - 180.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 15.0000
                 Phi: 90.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 360
               Slice: 0.0000 - 180.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 30.0000
                 Phi: 0.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 360
               Slice: 0.0000 - 180.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 30.0000
                 Phi: 90.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 360
               Slice: 0.0000 - 180.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 300
               Slice: 0.0000 - 150.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 45.0000
                 Phi: 0.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 318
               Slice: 0.0000 - 159.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 45.0000
                 Phi: 90.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 324
               Slice: 0.0000 - 162.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 15.0000
                 Phi: 0.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 360
               Slice: 0.0000 - 180.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 30.0000
                 Phi: 180.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 280
               Slice: 0.0000 - 140.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 15.0000
                 Phi: 180.0000
                 XTD: 50.0000
              2theta: 90.0000
scan:
    Number of images: 300
               Slice: 0.0000 - 150.0000
         Image width: 0.5000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 45.0000
                 Phi: 180.0000
                 XTD: 50.0000
              2theta: 90.0000
;
_diffrn_measurement_device
;
AFC11 (Left): Eulerian 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.050687
_diffrn_orient_matrix_UB_12      -0.024455
_diffrn_orient_matrix_UB_13      -0.051241
_diffrn_orient_matrix_UB_21      -0.004998
_diffrn_orient_matrix_UB_22      -0.033641
_diffrn_orient_matrix_UB_23      0.044276
_diffrn_orient_matrix_UB_31      -0.050522
_diffrn_orient_matrix_UB_32      0.027863
_diffrn_orient_matrix_UB_33      0.008482
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            72247
_diffrn_reflns_theta_full        65.86
_diffrn_reflns_theta_max         65.86
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_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    7.154
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_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    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7629
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+7.4602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                7364
_reflns_number_total             7629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002186_si_002.cif
_cod_data_source_block           '_Compound4'
_cod_original_cell_volume        4446.7(3)
_cod_database_code               4080822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H12A,H12B} of C12, {H11A,H11B} of C11, {H10A,H10B} of C10, {H9A,H9B} of C9,
   {H7A,H7B} of C7, {H8A,H8B} of C8, H6S of C6S, H5S of C5S, H4S of C4S, H3S of
  C3S, H2S of C2S, {H24A,H24B} of C24, {H23A,H23B} of C23, {H22A,H22B} of C22,
  {H21A,H21B} of C21, {H20A,H20B} of C20, {H19A,H19B} of C19
 At 1.5 times of:
  {H6A,H6B,H6C} of C6, {H7SA,H7SB,H7SC} of C7S, {H13A,H13B,H13C} of C13,
  {H14A,H14B,H14C} of C14, {H15A,H15B,H15C} of C15, {H16A,H16B,H16C} of C16,
  {H17A,H17B,H17C} of C17, {H18A,H18B,H18C} of C18, {H1A,H1B,H1C} of C1, {H2A,
  H2B,H2C} of C2, {H3A,H3B,H3C} of C3, {H4A,H4B,H4C} of C4, {H5A,H5B,H5C} of C5
2. Rigid bond restraints
 C7S, C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C7S ~ C1S ~ C2S ~ C3S ~ C4S ~ C5S ~ C6S: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{C7S, C1S, C6S, C5S, C4S, C3S, C2S}
as
{C7S, C1S, C2S, C3S, C4S, C5S, C6S}
5. Others
 Fixed Sof: C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5) C1S(0.5) C2S(0.5) H2S(0.5)
 C3S(0.5) H3S(0.5) C4S(0.5) H4S(0.5) C5S(0.5) H5S(0.5) C6S(0.5) H6S(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C7S(H7SA,H7SB,H7SC)
;