#------------------------------------------------------------------------------
#$Date: 2016-03-21 12:17:54 +0100 (lun 21 de mar de 2016) $
#$Revision: 178697 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/08/4080824.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4080824
loop_
_publ_author_name
'Guard, Louise M.'
'Hazari, Nilay'
_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       ω
_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/[σ²(Fo²)+(0.0612P)²+0.0000P] where P=(Fo²+2Fc²)/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
#BEGIN Tags that were not found in dictionaries:
_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)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br2 Br 0.41139(10) 0.17565(8) 0.73329(5) 0.0671(3) Uani 1 1 d .
Br1 Br 1.13323(7) 0.29463(7) 0.04051(4) 0.0465(2) Uani 1 1 d .
Br3 Br 0.40241(8) 0.31782(6) 0.49133(5) 0.0521(2) Uani 1 1 d .
Mg1 Mg 0.9596(2) 0.31425(18) 0.17627(12) 0.0307(4) Uani 1 1 d .
Cl1 Cl 0.7458(2) 0.06680(17) 0.54048(12) 0.0599(5) Uani 1 1 d .
Mg2 Mg 0.4482(3) 0.1249(2) 0.56171(14) 0.0435(5) Uani 1 1 d .
N2 N 1.0343(5) 0.1300(5) 0.2213(3) 0.0344(11) Uani 1 1 d .
N3 N 0.7087(6) 0.3003(5) 0.0988(3) 0.0447(12) Uani 1 1 d .
N1 N 0.8132(5) 0.3322(5) 0.2983(3) 0.0356(11) Uani 1 1 d .
N4 N 1.0562(6) 0.5204(4) 0.2613(3) 0.0368(11) Uani 1 1 d .
C1 C 0.8128(8) 0.2009(7) 0.3274(4) 0.0467(16) Uani 1 1 d .
H1A H 0.7273 0.1345 0.2853 0.056 Uiso 1 1 calc R
H1B H 0.7854 0.2167 0.3941 0.056 Uiso 1 1 calc R
C4 C 1.2165(8) 0.1054(7) 0.2234(5) 0.0529(17) Uani 1 1 d .
H4A H 1.2511 0.0965 0.1595 0.079 Uiso 1 1 calc R
H4B H 1.2360 0.0214 0.2431 0.079 Uiso 1 1 calc R
H4C H 1.2810 0.1822 0.2691 0.079 Uiso 1 1 calc R
C9 C 0.8923(8) 0.4455(6) 0.3773(4) 0.0488(16) Uani 1 1 d .
H9A H 0.9893 0.4138 0.4105 0.059 Uiso 1 1 calc R
H9B H 0.8122 0.4760 0.4243 0.059 Uiso 1 1 calc R
C5 C 0.6397(7) 0.3584(7) 0.2666(5) 0.0503(16) Uani 1 1 d .
H5A H 0.6328 0.4565 0.2703 0.060 Uiso 1 1 calc R
H5B H 0.5633 0.3335 0.3096 0.060 Uiso 1 1 calc R
C2 C 0.9824(8) 0.1444(7) 0.3198(4) 0.0456(15) Uani 1 1 d .
H2A H 1.0652 0.2061 0.3676 0.055 Uiso 1 1 calc R
H2B H 0.9795 0.0543 0.3342 0.055 Uiso 1 1 calc R
C3 C 0.9434(8) 0.0103(6) 0.1524(5) 0.0517(16) Uani 1 1 d .
H3A H 0.8236 0.0185 0.1536 0.078 Uiso 1 1 calc R
H3B H 0.9742 -0.0729 0.1702 0.078 Uiso 1 1 calc R
H3C H 0.9724 0.0062 0.0879 0.078 Uiso 1 1 calc R
C6 C 0.5882(7) 0.2760(8) 0.1654(5) 0.0550(18) Uani 1 1 d .
H6A H 0.5805 0.1780 0.1637 0.066 Uiso 1 1 calc R
H6B H 0.4769 0.3004 0.1434 0.066 Uiso 1 1 calc R
C12 C 1.2276(7) 0.5021(7) 0.3023(5) 0.0548(17) Uani 1 1 d .
H12A H 1.2242 0.4261 0.3324 0.082 Uiso 1 1 calc R
H12B H 1.2711 0.5857 0.3502 0.082 Uiso 1 1 calc R
H12C H 1.2999 0.4823 0.2510 0.082 Uiso 1 1 calc R
C10 C 0.9483(8) 0.5643(6) 0.3388(5) 0.0503(16) Uani 1 1 d .
H10A H 0.8495 0.6041 0.3138 0.060 Uiso 1 1 calc R
H10B H 1.0099 0.6358 0.3916 0.060 Uiso 1 1 calc R
C7 C 0.6833(9) 0.4358(7) 0.0786(6) 0.067(2) Uani 1 1 d .
H7A H 0.6986 0.5073 0.1388 0.101 Uiso 1 1 calc R
H7B H 0.5705 0.4352 0.0472 0.101 Uiso 1 1 calc R
H7C H 0.7640 0.4535 0.0365 0.101 Uiso 1 1 calc R
C11 C 1.0724(9) 0.6290(6) 0.2097(5) 0.0587(19) Uani 1 1 d .
H11A H 1.1468 0.6016 0.1601 0.088 Uiso 1 1 calc R
H11B H 1.1180 0.7142 0.2551 0.088 Uiso 1 1 calc R
H11C H 0.9628 0.6426 0.1799 0.088 Uiso 1 1 calc R
C8 C 0.6780(9) 0.1921(8) 0.0070(5) 0.069(2) Uani 1 1 d .
H8A H 0.7536 0.2102 -0.0376 0.104 Uiso 1 1 calc R
H8B H 0.5629 0.1917 -0.0208 0.104 Uiso 1 1 calc R
H8C H 0.6975 0.1032 0.0193 0.104 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Mg1 Br1 98.46(13) . .
N3 Mg1 Br1 100.30(15) . .
N3 Mg1 N2 116.2(2) . .
N3 Mg1 N4 115.8(2) . .
N1 Mg1 Br1 178.43(14) . .
N1 Mg1 N2 80.83(17) . .
N1 Mg1 N3 81.28(19) . .
N1 Mg1 N4 81.09(19) . .
N4 Mg1 Br1 98.13(14) . .
N4 Mg1 N2 120.83(18) . .
Mg2 Cl1 Mg2 70.79(10) 2_656 .
Br2 Mg2 Cl1 113.50(10) . 2_656
Br2 Mg2 Cl1 109.05(9) . .
Br2 Mg2 Mg2 128.72(11) . 2_656
Br3 Mg2 Br2 113.70(9) . .
Br3 Mg2 Cl1 105.94(9) . .
Br3 Mg2 Cl1 105.09(10) . 2_656
Br3 Mg2 Mg2 117.51(12) . 2_656
Cl1 Mg2 Cl1 109.21(10) 2_656 .
Cl1 Mg2 Mg2 54.17(8) . 2_656
Cl1 Mg2 Mg2 55.04(9) 2_656 2_656
C4 N2 Mg1 115.9(3) . .
C2 N2 Mg1 106.7(3) . .
C2 N2 C4 109.2(4) . .
C3 N2 Mg1 107.5(3) . .
C3 N2 C4 107.0(5) . .
C3 N2 C2 110.5(5) . .
C6 N3 Mg1 106.8(3) . .
C6 N3 C7 109.1(5) . .
C7 N3 Mg1 107.0(4) . .
C8 N3 Mg1 115.4(4) . .
C8 N3 C6 109.4(5) . .
C8 N3 C7 108.9(5) . .
C1 N1 Mg1 108.9(3) . .
C9 N1 Mg1 107.7(3) . .
C9 N1 C1 110.7(5) . .
C9 N1 C5 111.8(5) . .
C5 N1 Mg1 108.0(3) . .
C5 N1 C1 109.5(5) . .
C12 N4 Mg1 104.8(3) . .
C10 N4 Mg1 107.5(4) . .
C10 N4 C12 110.6(5) . .
C10 N4 C11 109.4(5) . .
C11 N4 Mg1 117.7(4) . .
C11 N4 C12 106.6(5) . .
N1 C1 C2 109.5(5) . .
N1 C9 C10 110.4(5) . .
N1 C5 C6 110.2(5) . .
N2 C2 C1 111.3(4) . .
N3 C6 C5 111.8(5) . .
N4 C10 C9 111.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br2 Mg2 2.416(3) .
Br1 Mg1 2.456(2) .
Br3 Mg2 2.405(3) .
Mg1 N2 2.177(5) .
Mg1 N3 2.163(5) .
Mg1 N1 2.159(5) .
Mg1 N4 2.169(5) .
Cl1 Mg2 2.487(3) .
Cl1 Mg2 2.460(3) 2_656
Mg2 Cl1 2.460(3) 2_656
Mg2 Mg2 2.865(4) 2_656
N2 C4 1.477(7) .
N2 C2 1.475(7) .
N2 C3 1.450(7) .
N3 C6 1.466(7) .
N3 C7 1.466(8) .
N3 C8 1.460(8) .
N1 C1 1.467(7) .
N1 C9 1.448(7) .
N1 C5 1.463(7) .
N4 C12 1.464(7) .
N4 C10 1.455(7) .
N4 C11 1.461(7) .
C1 C2 1.485(8) .
C9 C10 1.494(9) .
C5 C6 1.476(9) .
