##############################################################################
### ###
### Electronic paper (Acta Crystallographica Section E) ###
### ###
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# #
# This CIF contains the data in a paper accepted for publication in Acta #
# Crystallographica Section E. It conforms to the requirements of Notes #
# for Authors for Section E, and has been peer reviewed under the auspices #
# of the IUCr Commission on Journals. #
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# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. #
# #
# Software is freely available for graphical display of the structure(s) in #
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data_I
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
5-(Pyridinium-3-yl)tetrazol-1-ide hexaaquamagnesium dichloride
;
_chemical_name_common ?
_chemical_formula_moiety 'H12 Mg O6 2+, 2(Cl -), C12 H10 N10'
_chemical_formula_sum 'C12 H22 Cl2 Mg N10 O6'
_chemical_formula_iupac '(C6 H5 N5)2 [Mg (H2 O)6] Cl2'
_chemical_formula_weight 497.61
_chemical_melting_point ?
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.4354(15)
_cell_length_b 8.4232(17)
_cell_length_c 9.5817(19)
_cell_angle_alpha 94.06(3)
_cell_angle_beta 90.71(3)
_cell_angle_gamma 110.67(3)
_cell_volume 559.60(19)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 2552
_cell_measurement_theta_min 3.15
_cell_measurement_theta_max 27.48
_cell_measurement_temperature 298(2)
_exptl_crystal_description 'Block'
_exptl_crystal_colour 'colourless'
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.05
_exptl_crystal_density_diffrn 1.477
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 258
_exptl_absorpt_coefficient_mu 0.369
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(CrystalClear; Rigaku, 2005)'
_exptl_absorpt_correction_T_min 0.89
_exptl_absorpt_correction_T_max 0.95
_exptl_special_details
;
;
_diffrn_ambient_temperature 298(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku SCXmini diffractometer'
_diffrn_measurement_method 'CCD_Profile_fitting'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number 5836
_diffrn_reflns_av_R_equivalents 0.0291
_diffrn_reflns_av_sigmaI/netI 0.0368
_diffrn_reflns_theta_min 3.15
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F^2^, conventional
R-factors R are based on F, with F set to zero for
negative F^2^. The threshold expression of F^2^ >
\s(F^2^) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F^2^ are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total 2552
_reflns_number_gt 2086
_reflns_threshold_expression I>2sigma(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0533
_refine_ls_R_factor_gt 0.0405
_refine_ls_wR_factor_gt 0.0946
_refine_ls_wR_factor_ref 0.1007
_refine_ls_goodness_of_fit_ref 1.094
_refine_ls_restrained_S_all 1.092
_refine_ls_number_reflns 2552
_refine_ls_number_parameters 142
_refine_ls_number_restraints 6
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.1577P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.268
_refine_diff_density_min -0.249
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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'
'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'
'Mg' 'Mg' 0.0486 0.0363
'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'
_computing_data_collection 'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement 'CrystalClear (Rigaku, 2005)'
_computing_data_reduction 'CrystalClear (Rigaku, 2005)'
_computing_structure_solution 'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
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
Mg Mg1 0.0000 0.5000 0.5000 0.0313(2) Uani d S 1 . .
O O1W 0.0599(2) 0.69394(16) 0.36976(13) 0.0459(4) Uani d D 1 . .
H H1WA 0.0113 0.6775 0.2869 0.069 Uiso d RD 1 . .
H H1WB 0.1228 0.7998 0.3859 0.069 Uiso d RD 1 . .
O O2W 0.2487(2) 0.64382(19) 0.62087(14) 0.0528(4) Uani d D 1 . .
H H2WA 0.2766 0.6238 0.7025 0.079 Uiso d RD 1 . .
H H2WB 0.3531 0.7163 0.5961 0.079 Uiso d RD 1 . .
N N2 0.2278(2) 0.46353(18) 0.10243(15) 0.0317(3) Uani d . 1 . .
C C6 0.3333(2) 0.5845(2) 0.02382(17) 0.0263(3) Uani d . 1 . .
C C2 0.4917(2) 0.7372(2) 0.07879(18) 0.0299(4) Uani d . 1 . .
N N3 0.1006(2) 0.34796(18) 0.01273(16) 0.0357(3) Uani d . 1 . .
N N4 0.1310(2) 0.39758(19) -0.11389(16) 0.0362(4) Uani d . 1 . .
N N5 0.2776(2) 0.54786(18) -0.11105(15) 0.0336(3) Uani d . 1 . .
O O3W 0.1562(2) 0.3929(2) 0.37477(15) 0.0565(4) Uani d D 1 . .
H H3WA 0.1824 0.4149 0.2906 0.085 Uiso d RD 1 . .
H H3WB 0.1934 0.3113 0.3914 0.085 Uiso d RD 1 . .
C C3 0.6097(3) 0.8510(2) -0.0093(2) 0.0370(4) Uani d . 1 . .
H H3 0.5879 0.8315 -0.1058 0.044 Uiso calc R 1 . .
C C1 0.5289(3) 0.7704(2) 0.2209(2) 0.0416(5) Uani d . 1 . .
H H1 0.4520 0.6969 0.2821 0.050 Uiso calc R 1 . .
N N1 0.6760(3) 0.9086(2) 0.2710(2) 0.0528(5) Uani d . 1 . .
H H1A 0.6978 0.9268 0.3602 0.063 Uiso calc R 1 . .
C C4 0.7593(3) 0.9931(2) 0.0469(3) 0.0490(5) Uani d . 1 . .
H H4 0.8379 1.0697 -0.0117 0.059 Uiso calc R 1 . .
C C5 0.7908(3) 1.0201(3) 0.1877(3) 0.0543(6) Uani d . 1 . .
H H5 0.8912 1.1151 0.2264 0.065 Uiso calc R 1 . .
Cl Cl1 0.31120(8) 0.08959(6) 0.40654(6) 0.05028(17) Uani d . 1 . .
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
Mg1 0.0380(5) 0.0285(4) 0.0220(4) 0.0051(3) 0.0002(3) 0.0023(3)
O1W 0.0647(9) 0.0284(7) 0.0290(7) -0.0025(6) -0.0112(6) 0.0042(5)
O2W 0.0463(8) 0.0564(9) 0.0343(7) -0.0092(7) -0.0087(6) 0.0112(6)
N2 0.0320(7) 0.0299(7) 0.0284(7) 0.0051(6) 0.0011(6) 0.0025(6)
C6 0.0244(8) 0.0257(8) 0.0266(8) 0.0066(6) 0.0011(6) 0.0009(6)
C2 0.0260(8) 0.0260(8) 0.0358(9) 0.0079(7) -0.0005(7) -0.0019(7)
N3 0.0304(8) 0.0296(8) 0.0405(9) 0.0030(6) -0.0007(6) 0.0004(6)
N4 0.0322(8) 0.0347(8) 0.0363(8) 0.0065(6) -0.0073(6) -0.0022(6)
N5 0.0328(8) 0.0335(8) 0.0285(8) 0.0043(6) -0.0026(6) 0.0032(6)
O3W 0.0863(12) 0.0675(10) 0.0347(8) 0.0479(9) 0.0192(8) 0.0157(7)
C3 0.0323(9) 0.0317(9) 0.0450(11) 0.0082(8) 0.0038(8) 0.0052(8)
C1 0.0380(10) 0.0383(10) 0.0391(10) 0.0037(8) -0.0024(8) -0.0062(8)
N1 0.0490(10) 0.0494(11) 0.0477(10) 0.0071(8) -0.0102(8) -0.0201(8)
C4 0.0358(10) 0.0284(10) 0.0754(16) 0.0023(8) 0.0065(10) 0.0041(9)
C5 0.0372(11) 0.0329(11) 0.0798(17) 0.0004(9) -0.0046(11) -0.0158(10)
Cl1 0.0557(3) 0.0341(3) 0.0536(3) 0.0067(2) -0.0008(2) 0.0045(2)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
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
Mg1 O1W . 2.0526(14) ?
Mg1 O1W 2_566 2.0526(14) ?
Mg1 O3W 2_566 2.0552(15) ?
Mg1 O3W . 2.0552(15) ?
Mg1 O2W . 2.0965(16) ?
Mg1 O2W 2_566 2.0965(16) ?
O1W H1WA . 0.8500 ?
O1W H1WB . 0.8499 ?
O2W H2WA . 0.8500 ?
O2W H2WB . 0.8499 ?
N2 C6 . 1.334(2) ?
N2 N3 . 1.339(2) ?
C6 N5 . 1.333(2) ?
C6 C2 . 1.462(2) ?
C2 C1 . 1.375(3) ?
C2 C3 . 1.393(3) ?
N3 N4 . 1.308(2) ?
N4 N5 . 1.346(2) ?
O3W H3WA . 0.8500 ?
O3W H3WB . 0.8499 ?
C3 C4 . 1.383(3) ?
C3 H3 . 0.9300 ?
C1 N1 . 1.338(2) ?
C1 H1 . 0.9300 ?
N1 C5 . 1.344(3) ?
N1 H1A . 0.8600 ?
C4 C5 . 1.356(3) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
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
O1W Mg1 O1W . 2_566 180.00(5) ?
O1W Mg1 O3W . 2_566 91.30(6) ?
O1W Mg1 O3W 2_566 2_566 88.70(6) ?
O1W Mg1 O3W . . 88.70(6) ?
O1W Mg1 O3W 2_566 . 91.30(6) ?
O3W Mg1 O3W 2_566 . 180.0000(10)
?
O1W Mg1 O2W . . 88.73(6) ?
O1W Mg1 O2W 2_566 . 91.27(6) ?
O3W Mg1 O2W 2_566 . 89.27(7) ?
O3W Mg1 O2W . . 90.73(7) ?
O1W Mg1 O2W . 2_566 91.27(6) ?
O1W Mg1 O2W 2_566 2_566 88.73(6) ?
O3W Mg1 O2W 2_566 2_566 90.73(7) ?
O3W Mg1 O2W . 2_566 89.27(7) ?
O2W Mg1 O2W . 2_566 180.0 ?
Mg1 O1W H1WA . . 121.5 ?
Mg1 O1W H1WB . . 130.3 ?
H1WA O1W H1WB . . 107.9 ?
Mg1 O2W H2WA . . 125.4 ?
Mg1 O2W H2WB . . 129.5 ?
H2WA O2W H2WB . . 103.6 ?
C6 N2 N3 . . 105.15(14) ?
N5 C6 N2 . . 111.57(14) ?
N5 C6 C2 . . 124.30(15) ?
N2 C6 C2 . . 124.13(15) ?
C1 C2 C3 . . 118.19(17) ?
C1 C2 C6 . . 120.00(16) ?
C3 C2 C6 . . 121.80(16) ?
N4 N3 N2 . . 109.00(14) ?
N3 N4 N5 . . 110.09(14) ?
C6 N5 N4 . . 104.18(14) ?
Mg1 O3W H3WA . . 124.6 ?
Mg1 O3W H3WB . . 127.9 ?
H3WA O3W H3WB . . 107.1 ?
C4 C3 C2 . . 120.02(19) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
N1 C1 C2 . . 120.00(19) ?
N1 C1 H1 . . 120.0 ?
C2 C1 H1 . . 120.0 ?
C1 N1 C5 . . 122.59(19) ?
C1 N1 H1A . . 118.7 ?
C5 N1 H1A . . 118.7 ?
C5 C4 C3 . . 119.6(2) ?
C5 C4 H4 . . 120.2 ?
C3 C4 H4 . . 120.2 ?
N1 C5 C4 . . 119.60(18) ?
N1 C5 H5 . . 120.2 ?
C4 C5 H5 . . 120.2 ?
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
O1W H1WA N4 2_565 0.85 1.90 2.737(2) 169
O1W H1WB Cl1 1_565 0.85 2.34 3.1848(17) 174
O2W H2WA N5 1_556 0.85 1.94 2.775(2) 167
O2W H2WB Cl1 2_666 0.85 2.46 3.2764(19) 163
N1 H1A Cl1 2_666 0.86 2.25 3.088(2) 165
O3W H3WA N2 . 0.85 1.89 2.735(2) 177
O3W H3WB Cl1 . 0.85 2.34 3.1822(17) 172
data_global
_journal_date_recd_electronic 2010-12-11
_journal_date_accepted 2010-12-25
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2011
_journal_volume 67
_journal_issue 2
_journal_page_first m171
_journal_page_last m171
_journal_paper_category QM
_journal_coeditor_code BX2339
_publ_contact_author_name 'Jing Dai'
_publ_contact_author_address
;
Ordered Matter Science Research Center, College of Chemistry and Chemical
Engineering, Southeast UniVersity,
Nanjing 210096, People's Republic of China
;
_publ_contact_author_email fudavid88@yahoo.com.cn
_publ_contact_author_fax '862552090626'
_publ_contact_author_phone '862552090626'
_publ_section_title
;
5-(Pyridinium-3-yl)tetrazol-1-ide hexaaquamagnesium dichloride
;
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Jing Dai' .
;
Ordered Matter Science Research Center,
College of Chemistry and Chemical Engineering, Southeast University,
Nanjing 210096, People's Republic of China
;
'Xin-Yuan Chen' .
;
Ordered Matter Science Research Center,
College of Chemistry and Chemical Engineering, Southeast University,
Nanjing 210096, People's Republic of China
;
_publ_section_synopsis .