#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/87/2228754.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_2228754
loop_
_publ_author_name
'Dai, Jing'
'Chen, Xin-Yuan'
_publ_section_title
;
 Hexaaquamagnesium dibromide 5-(pyridinium-3-yl)tetrazol-1-ide
;
_journal_coeditor_code           HY2389
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m113
_journal_paper_doi               10.1107/S1600536810052992
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mg (H2 O)6] Br2, 2C6 H5 N5'
_chemical_formula_moiety         'H12 Mg O6 2+, 2(Br -), 2(C6 H5 N5)'
_chemical_formula_sum            'C12 H22 Br2 Mg N10 O6'
_chemical_formula_weight         586.53
_chemical_name_systematic
;
Hexaaquamagnesium dibromide 5-(pyridinium-3-yl)tetrazol-1-ide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.04(3)
_cell_angle_beta                 90.94(3)
_cell_angle_gamma                111.75(3)
_cell_formula_units_Z            1
_cell_length_a                   7.3439(15)
_cell_length_b                   8.7786(18)
_cell_length_c                   9.5863(19)
_cell_measurement_reflns_used    2627
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      3.10
_cell_volume                     572.0(2)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCXmini CCD'
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0497
_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       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5933
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    3.620
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.519
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0402
_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)+(0.0426P)²+0.1011P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                2172
_reflns_number_total             2627
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2389.cif
_cod_data_source_block           I
_cod_database_code               2228754
_cod_database_fobs_code          2228754
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
N N4 0.3716(3) 0.6009(3) 0.6076(3) 0.0347(6) Uani d . 1 . .
N N2 0.2637(3) 0.5318(3) 0.3932(2) 0.0315(5) Uani d . 1 . .
C C6 0.1639(4) 0.4135(3) 0.4740(3) 0.0263(6) Uani d . 1 . .
N N5 0.2266(3) 0.4528(3) 0.6073(2) 0.0328(5) Uani d . 1 . .
C C2 0.0038(4) 0.2612(3) 0.4229(3) 0.0272(6) Uani d . 1 . .
C C3 -0.1073(4) 0.1506(4) 0.5142(3) 0.0319(6) Uani d . 1 . .
H H3 -0.0792 0.1730 0.6101 0.038 Uiso calc R 1 . .
N N1 -0.1923(4) 0.0847(4) 0.2374(3) 0.0481(7) Uani d . 1 . .
H H1A -0.2202 0.0642 0.1489 0.058 Uiso calc R 1 . .
N N3 0.3947(3) 0.6479(3) 0.4800(3) 0.0360(6) Uani d . 1 . .
C C1 -0.0427(5) 0.2234(4) 0.2822(3) 0.0398(7) Uani d . 1 . .
H H1 0.0296 0.2941 0.2180 0.048 Uiso calc R 1 . .
C C5 -0.3000(5) -0.0234(4) 0.3232(4) 0.0464(8) Uani d . 1 . .
H H5 -0.4017 -0.1188 0.2873 0.056 Uiso calc R 1 . .
C C4 -0.2598(4) 0.0073(4) 0.4639(4) 0.0408(7) Uani d . 1 . .
H H4 -0.3335 -0.0668 0.5253 0.049 Uiso calc R 1 . .
Mg Mg1 0.5000 0.5000 1.0000 0.0303(3) Uani d S 1 . .
O O1W 0.2634(3) 0.3471(3) 0.8692(2) 0.0497(6) Uani d . 1 . .
H H1WA 0.2453 0.3674 0.7906 0.075 Uiso d R 1 . .
H H1WB 0.1806 0.2467 0.8849 0.075 Uiso d R 1 . .
O O2W 0.5507(3) 0.6851(2) 0.8697(2) 0.0465(6) Uani d . 1 . .
H H2WA 0.5117 0.6602 0.7829 0.070 Uiso d R 1 . .
H H2WB 0.6098 0.7777 0.8780 0.070 Uiso d R 1 . .
O O3W 0.3123(4) 0.5786(3) 1.1155(2) 0.0532(6) Uani d . 1 . .
H H3WA 0.2760 0.6585 1.0834 0.080 Uiso d R 1 . .
H H3WB 0.3030 0.5606 1.2130 0.080 Uiso d R 1 . .
Br Br1 0.79518(5) 0.08632(4) 0.89951(3) 0.04481(14) Uani d . 1 . .
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'
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'
O O 0.0106 0.0060 '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'
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
N3 N4 N5 . . 110.0(2) ?
N3 N2 C6 . . 105.2(2) ?
N5 C6 N2 . . 111.4(2) ?
N5 C6 C2 . . 124.2(2) ?
N2 C6 C2 . . 124.4(2) ?
C6 N5 N4 . . 104.5(2) ?
C1 C2 C3 . . 117.8(3) ?
C1 C2 C6 . . 120.7(3) ?
C3 C2 C6 . . 121.5(3) ?
C4 C3 C2 . . 120.7(3) ?
C4 C3 H3 . . 119.6 ?
C2 C3 H3 . . 119.6 ?
C5 N1 C1 . . 123.3(3) ?
C5 N1 H1A . . 118.3 ?
C1 N1 H1A . . 118.3 ?
N4 N3 N2 . . 108.8(2) ?
N1 C1 C2 . . 119.9(3) ?
N1 C1 H1 . . 120.1 ?
C2 C1 H1 . . 120.1 ?
N1 C5 C4 . . 119.4(3) ?
N1 C5 H5 . . 120.3 ?
C4 C5 H5 . . 120.3 ?
C5 C4 C3 . . 119.0(3) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
O2W Mg1 O2W 2_667 . 180.0000(10) ?
O2W Mg1 O3W 2_667 2_667 91.93(10) ?
O2W Mg1 O3W . 2_667 88.07(10) ?
O2W Mg1 O3W 2_667 . 88.07(10) ?
O2W Mg1 O3W . . 91.93(10) ?
O3W Mg1 O3W 2_667 . 180.0000(10) ?
O2W Mg1 O1W 2_667 . 89.55(9) ?
O2W Mg1 O1W . . 90.45(9) ?
O3W Mg1 O1W 2_667 . 90.10(11) ?
O3W Mg1 O1W . . 89.90(11) ?
O2W Mg1 O1W 2_667 2_667 90.45(9) ?
O2W Mg1 O1W . 2_667 89.55(9) ?
O3W Mg1 O1W 2_667 2_667 89.90(11) ?
O3W Mg1 O1W . 2_667 90.10(11) ?
O1W Mg1 O1W . 2_667 180.0000(10) ?
Mg1 O1W H1WA . . 122.5 ?
Mg1 O1W H1WB . . 126.6 ?
H1WA O1W H1WB . . 110.2 ?
Mg1 O2W H2WA . . 119.0 ?
Mg1 O2W H2WB . . 133.7 ?
H2WA O2W H2WB . . 107.0 ?
Mg1 O3W H3WA . . 118.6 ?
Mg1 O3W H3WB . . 118.7 ?
H3WA O3W H3WB . . 119.2 ?
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
N4 N3 . 1.312(4) ?
N4 N5 . 1.341(3) ?
N2 N3 . 1.336(3) ?
N2 C6 . 1.336(3) ?
C6 N5 . 1.329(3) ?
C6 C2 . 1.460(4) ?
C2 C1 . 1.373(4) ?
C2 C3 . 1.390(4) ?
C3 C4 . 1.386(4) ?
C3 H3 . 0.9300 ?
N1 C5 . 1.333(4) ?
N1 C1 . 1.339(4) ?
N1 H1A . 0.8600 ?
C1 H1 . 0.9300 ?
C5 C4 . 1.363(5) ?
C5 H5 . 0.9300 ?
C4 H4 . 0.9300 ?
Mg1 O2W 2_667 2.048(2) ?
Mg1 O2W . 2.048(2) ?
Mg1 O3W 2_667 2.061(2) ?
Mg1 O3W . 2.061(2) ?
Mg1 O1W . 2.087(2) ?
Mg1 O1W 2_667 2.087(2) ?
O1W H1WA . 0.8068 ?
O1W H1WB . 0.8907 ?
O2W H2WA . 0.8615 ?
O2W H2WB . 0.7636 ?
O3W H3WA . 0.9085 ?
O3W H3WB . 0.9576 ?
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
_geom_hbond_publ_flag
N1 H1A Br1 1_454 0.86 2.41 3.240(3) 161 y
O1W H1WA N5 . 0.81 1.98 2.780(3) 171 y
O1W H1WB Br1 1_455 0.89 2.66 3.382(3) 138 y
O2W H2WA N4 . 0.86 1.89 2.738(3) 167 y
O2W H2WB Br1 1_565 0.76 2.53 3.296(2) 178 y
O3W H3WA Br1 2_667 0.91 2.48 3.328(2) 156 y
O3W H3WB N2 1_556 0.96 1.78 2.730(3) 174 y
