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_4080824
_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         'Br2 Cl Mg, C12 H30 Br Mg N4'
_chemical_formula_sum            'C12 H30 Br3 Cl Mg2 N4'
_chemical_formula_weight         554.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                104.590(14)
_cell_angle_beta                 95.656(16)
_cell_angle_gamma                92.374(17)
_cell_formula_units_Z            2
_cell_length_a                   7.945(7)
_cell_length_b                   9.961(8)
_cell_length_c                   14.237(12)
_cell_measurement_reflns_used    2782
_cell_measurement_temperature    223
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.1
_cell_volume                     1082.5(16)
_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      223
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 6.8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -120.0000 - 60.0000
         Image width: 1.0000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 0.0000
                 XTD: 50.2731
              2theta: -28.5876
scan:
    Number of images: 180
               Slice: -120.0000 - 60.0000
         Image width: 1.0000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 120.0000
                 XTD: 50.2731
              2theta: -28.5876
scan:
    Number of images: 180
               Slice: -120.0000 - 60.0000
         Image width: 1.0000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 240.0000
                 XTD: 50.2731
              2theta: -28.5876
;
_diffrn_measurement_device
;
SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury275R CCD'
_diffrn_measurement_method       \w
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.104682
_diffrn_orient_matrix_UB_12      -0.014688
_diffrn_orient_matrix_UB_13      -0.047529
_diffrn_orient_matrix_UB_21      -0.071505
_diffrn_orient_matrix_UB_22      0.011790
_diffrn_orient_matrix_UB_23      0.055152
_diffrn_orient_matrix_UB_31      0.002079
_diffrn_orient_matrix_UB_32      0.102264
_diffrn_orient_matrix_UB_33      0.005939
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8439
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'Sealed Tube'
_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    5.773
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.616
_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    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                2718
_reflns_number_total             3682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002186_si_002.cif
_cod_data_source_block           '_Me6trenMgBrBr4Mg2Cl2'
_cod_original_cell_volume        1082.4(16)
_cod_database_code               4080824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1a,H1b} of C1, {H6a,H6b} of C6, {H10a,H10b} of C10, {H9a,H9b} of C9, {H5a,
  H5b} of C5, {H2a,H2b} of C2
 At 1.5 times of:
  {H12a,H12b,H12c} of C12, {H11a,H11b,H11c} of C11, {H8a,H8b,H8c} of C8, {H4a,
  H4b,H4c} of C4, {H3a,H3b,H3c} of C3, {H7a,H7b,H7c} of C7
2.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C9(H9a,H9b), C5(H5a,H5b), C2(H2a,H2b), C6(H6a,H6b), C10(H10a,H10b)
2.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C3(H3a,H3b,H3c), C12(H12a,H12b,H12c), C7(H7a,H7b,H7c),
 C11(H11a,H11b,H11c), C8(H8a,H8b,H8c)
;