#------------------------------------------------------------------------------
#$Date: 2016-02-20 21:30:07 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/25/2222535.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2222535
loop_
_publ_author_name
'Vitze, Hannes'
'Lerner, Hans-Wolfram'
'Bolte, Michael'
_publ_section_title
;
 Dibromidotris(dimethylamine)magnesium(II)
;
_journal_coeditor_code           AT2830
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m888
_journal_paper_doi               10.1107/S1600536809024702
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mg Br2 (C2 H7 N)3]'
_chemical_formula_moiety         'C6 H21 Br2 Mg N3'
_chemical_formula_sum            'C6 H21 Br2 Mg N3'
_chemical_formula_weight         319.39
_chemical_name_systematic
;
Dibromidotris(dimethylamine)magnesium(II)
;
_space_group_IT_number           154
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.0951(7)
_cell_length_b                   9.0951(7)
_cell_length_c                   14.4544(12)
_cell_measurement_reflns_used    5127
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      3.8
_cell_volume                     1035.49(14)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe IPDSII two-circle'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5279
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         3.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.883
_exptl_absorpt_correction_T_max  0.3448
_exptl_absorpt_correction_T_min  0.3210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.335
_refine_ls_abs_structure_details 'Flack (1983), 517 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.012(17)
_refine_ls_extinction_coef       0.0106(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0217
_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)+(0.0277P)²+0.2606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                1223
_reflns_number_total             1285
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2830.cif
_cod_data_source_block           I
_cod_database_code               2222535
_cod_database_fobs_code          2222535
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'-x, -x+y, -z+2/3'
'x-y, -y, -z+1/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.39287(4) 0.37977(4) 0.318621(17) 0.03405(12) Uani d . 1 . .
Mg Mg1 0.41479(13) 0.41479(13) 0.5000 0.0231(3) Uani d S 1 . .
N N1 0.4463(3) 0.1927(3) 0.50042(15) 0.0301(5) Uani d . 1 . .
H H1 0.4887 0.1897 0.4423 0.036 Uiso calc R 1 . .
C C1 0.5661(5) 0.1872(5) 0.5683(2) 0.0441(9) Uani d . 1 . .
H H1A 0.6768 0.2910 0.5630 0.066 Uiso calc R 1 . .
H H1B 0.5789 0.0883 0.5556 0.066 Uiso calc R 1 . .
H H1C 0.5217 0.1787 0.6310 0.066 Uiso calc R 1 . .
C C2 0.2791(5) 0.0368(4) 0.5070(3) 0.0474(9) Uani d . 1 . .
H H2A 0.2012 0.0419 0.4620 0.071 Uiso calc R 1 . .
H H2B 0.2334 0.0270 0.5695 0.071 Uiso calc R 1 . .
H H2C 0.2916 -0.0621 0.4939 0.071 Uiso calc R 1 . .
N N2 0.6685(6) 0.6265(6) 0.5188(3) 0.0293(12) Uani d P 0.50 . .
H H2 0.7183 0.5896 0.5623 0.035 Uiso d PR 0.50 . .
C C3 0.6750(5) 0.7809(4) 0.5616(2) 0.0444(8) Uani d . 1 . .
H H3A 0.7933 0.8716 0.5684 0.067 Uiso d PR 0.50 A 1
H H3B 0.6206 0.7508 0.6226 0.067 Uiso d PR 0.50 A 1
H H3C 0.6143 0.8201 0.5218 0.067 Uiso d PR 0.50 A 1
H H3D 0.7715 0.8920 0.5457 0.067 Uiso d PR 0.50 A 2
H H3E 0.5785 0.7940 0.5803 0.067 Uiso d PR 0.50 A 2
H H3F 0.7063 0.7309 0.6125 0.067 Uiso d PR 0.50 A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.0453(2) 0.04152(19) 0.02015(14) 0.02533(16) 0.00289(12) -0.00057(12)
Mg1 0.0233(5) 0.0233(5) 0.0200(5) 0.0096(6) 0.0012(2) -0.0012(2)
N1 0.0368(15) 0.0336(14) 0.0232(12) 0.0199(12) 0.0007(12) -0.0026(11)
C1 0.055(2) 0.057(2) 0.0385(17) 0.041(2) -0.0087(17) -0.0075(17)
C2 0.048(2) 0.0276(17) 0.057(2) 0.0121(16) 0.0043(18) -0.0044(15)
N2 0.027(2) 0.027(3) 0.028(3) 0.010(2) -0.0027(19) 0.005(2)
C3 0.054(2) 0.0249(16) 0.0425(18) 0.0111(16) -0.0098(17) -0.0037(14)
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Mg1 N2 . 4_556 22.9(2) ?
N2 Mg1 N1 . . 104.45(16) ?
N2 Mg1 N1 4_556 . 122.07(17) ?
N2 Mg1 N1 . 4_556 122.07(17) ?
N2 Mg1 N1 4_556 4_556 104.45(16) ?
N1 Mg1 N1 . 4_556 133.08(16) ?
N2 Mg1 Br1 . 4_556 88.69(13) ?
N2 Mg1 Br1 4_556 4_556 102.44(14) ?
N1 Mg1 Br1 . 4_556 89.66(6) ?
N1 Mg1 Br1 4_556 4_556 85.86(6) ?
N2 Mg1 Br1 . . 102.44(14) ?
N2 Mg1 Br1 4_556 . 88.69(13) ?
N1 Mg1 Br1 . . 85.86(6) ?
N1 Mg1 Br1 4_556 . 89.66(6) ?
Br1 Mg1 Br1 4_556 . 168.72(5) ?
C2 N1 C1 . . 110.2(3) ?
C2 N1 Mg1 . . 110.0(2) ?
C1 N1 Mg1 . . 118.2(2) ?
C2 N1 H1 . . 105.9 ?
C1 N1 H1 . . 105.9 ?
Mg1 N1 H1 . . 105.9 ?
N1 C1 H1A . . 109.5 ?
N1 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
N1 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 H2A . . 109.5 ?
N1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
N1 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
N2 N2 C3 4_556 4_556 76.2(6) ?
N2 N2 C3 4_556 . 70.4(6) ?
C3 N2 C3 4_556 . 110.5(4) ?
N2 N2 Mg1 4_556 . 78.57(12) ?
C3 N2 Mg1 4_556 . 116.3(3) ?
C3 N2 Mg1 . . 114.1(3) ?
N2 N2 H2 4_556 . 175.2 ?
C3 N2 H2 4_556 . 104.6 ?
C3 N2 H2 . . 105.1 ?
Mg1 N2 H2 . . 105.0 ?
N2 C3 H3A 4_556 . 119.2 ?
N2 C3 H3A . . 109.9 ?
N2 C3 H3B 4_556 . 125.9 ?
N2 C3 H3B . . 109.2 ?
H3A C3 H3B . . 109.5 ?
N2 C3 H3C 4_556 . 76.1 ?
N2 C3 H3C . . 109.3 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
N2 C3 H3D 4_556 . 109.6 ?
N2 C3 H3D . . 117.5 ?
H3B C3 H3D . . 124.5 ?
H3C C3 H3D . . 82.1 ?
N2 C3 H3E 4_556 . 109.2 ?
N2 C3 H3E . . 127.2 ?
H3A C3 H3E . . 122.9 ?
H3B C3 H3E . . 55.2 ?
H3C C3 H3E . . 54.3 ?
H3D C3 H3E . . 109.5 ?
N2 C3 H3F 4_556 . 109.2 ?
N2 C3 H3F . . 76.2 ?
H3A C3 H3F . . 82.1 ?
H3B C3 H3F . . 54.4 ?
H3C C3 H3F . . 163.4 ?
H3D C3 H3F . . 109.7 ?
H3E C3 H3F . . 109.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Mg1 . 2.6365(4) ?
Mg1 N2 . 2.159(5) ?
Mg1 N2 4_556 2.159(5) ?
Mg1 N1 . 2.177(3) ?
Mg1 N1 4_556 2.177(3) ?
Mg1 Br1 4_556 2.6365(4) ?
N1 C2 . 1.475(4) ?
N1 C1 . 1.486(4) ?
N1 H1 . 0.9300 ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
N2 N2 4_556 0.856(9) ?
N2 C3 4_556 1.463(6) ?
N2 C3 . 1.508(6) ?
N2 H2 . 0.9300 ?
C3 N2 4_556 1.463(6) ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C3 H3D . 0.9788 ?
C3 H3E . 0.9803 ?
C3 H3F . 0.9780 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 Br1 5_655 0.93 2.90 3.638(2) 137.2
N2 H2 Br1 3_665 0.93 2.70 3.554(5) 153.3
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N2 Mg1 N1 C2 . . . . 168.6(2) ?
N2 Mg1 N1 C2 4_556 . . . -175.4(2) ?
N1 Mg1 N1 C2 4_556 . . . -3.95(19) ?
Br1 Mg1 N1 C2 4_556 . . . 80.0(2) ?
Br1 Mg1 N1 C2 . . . . -89.6(2) ?
N2 Mg1 N1 C1 . . . . 40.9(3) ?
N2 Mg1 N1 C1 4_556 . . . 56.8(3) ?
N1 Mg1 N1 C1 4_556 . . . -131.7(2) ?
Br1 Mg1 N1 C1 4_556 . . . -47.7(2) ?
Br1 Mg1 N1 C1 . . . . 142.7(2) ?
N1 Mg1 N2 N2 . . . 4_556 143.2(7) ?
N1 Mg1 N2 N2 4_556 . . 4_556 -43.2(8) ?
Br1 Mg1 N2 N2 4_556 . . 4_556 -127.5(7) ?
Br1 Mg1 N2 N2 . . . 4_556 54.3(8) ?
N2 Mg1 N2 C3 4_556 . . 4_556 -68.2(7) ?
N1 Mg1 N2 C3 . . . 4_556 75.0(3) ?
N1 Mg1 N2 C3 4_556 . . 4_556 -111.4(3) ?
Br1 Mg1 N2 C3 4_556 . . 4_556 164.3(3) ?
Br1 Mg1 N2 C3 . . . 4_556 -13.9(4) ?
N2 Mg1 N2 C3 4_556 . . . 62.2(7) ?
N1 Mg1 N2 C3 . . . . -154.6(3) ?
N1 Mg1 N2 C3 4_556 . . . 19.0(4) ?
Br1 Mg1 N2 C3 4_556 . . . -65.3(3) ?
Br1 Mg1 N2 C3 . . . . 116.5(3) ?
C3 N2 C3 N2 4_556 . . 4_556 66.2(5) ?
Mg1 N2 C3 N2 . . . 4_556 -67.0(4) ?
