#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/50/2205016.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_2205016
loop_
_publ_author_name
'Ma, Zhi-Jie'
'Tao, Jun'
'Huang, Rong-Bin'
'Zheng, Lan-Sun'
_publ_section_title
;
 Hexaaquamanganese(II) 5,5'-(1,4-phenylene)ditetrazolate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m361
_journal_page_last               m363
_journal_paper_doi               10.1107/S1600536805001418
_journal_volume                  61
_journal_year                    2005
_chemical_formula_moiety         'H12 Mn O6 2+, C8 H4 N8 2-'
_chemical_formula_sum            'C8 H16 Mn N8 O6'
_chemical_formula_weight         375.23
_chemical_name_systematic
;
  Hexaaquamanganese(II) 5,5'-(1,4-phenylene)bis-tetrazolate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.1490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.0587(3)
_cell_length_b                   13.4343(7)
_cell_length_c                   11.4989(6)
_cell_measurement_reflns_used    4474
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.282
_cell_measurement_theta_min      2.339
_cell_volume                     776.97(7)
_computing_cell_refinement       'SAINT (Bruker 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX 2000'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6205
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.8701
_exptl_absorpt_correction_T_min  0.7629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1674
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0463P)²+0.2423P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                1599
_reflns_number_total             1674
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bv6009.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2205016
_cod_database_fobs_code          2205016
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_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_type_symbol
Mn1 0.5000 0.0000 0.5000 0.02655(13) Uani d S 1 Mn
O1W 0.2304(2) -0.05949(8) 0.35326(9) 0.0292(2) Uani d D 1 O
H1WA 0.188(5) -0.0190(10) 0.2980(10) 0.043(6) Uiso d D 1 H
H1WB 0.262(4) -0.1166(8) 0.3270(10) 0.039(5) Uiso d D 1 H
O2W 0.1917(2) 0.10825(8) 0.52315(11) 0.0339(3) Uani d D 1 O
H2WA 0.256(4) 0.1650(10) 0.5440(10) 0.045(6) Uiso d D 1 H
H2WB 0.078(4) 0.09380(10) 0.5690(10) 0.055(7) Uiso d D 1 H
O3W 0.3422(2) -0.11100(10) 0.60910(10) 0.0448(3) Uani d D 1 O
H3WA 0.446(3) -0.1410(10) 0.6590(10) 0.063(7) Uiso d D 1 H
H3WB 0.183(2) -0.126(2) 0.613(2) 0.084(9) Uiso d D 1 H
N1 0.9034(3) -0.08910(10) 0.80080(10) 0.0333(3) Uani d . 1 N
N2 0.7609(3) -0.16970(10) 0.76600(10) 0.0365(3) Uani d . 1 N
N3 0.8643(3) -0.24720(10) 0.82030(10) 0.0385(3) Uani d . 1 N
N4 1.0771(3) -0.21960(10) 0.89290(10) 0.0362(3) Uani d . 1 N
C1 1.0958(3) -0.12210(10) 0.87890(10) 0.0278(3) Uani d . 1 C
C2 1.3018(3) -0.05950(10) 0.94110(10) 0.0291(3) Uani d . 1 C
C3 1.3321(4) 0.03930(10) 0.90910(10) 0.0397(4) Uani d . 1 C
H3A 1.2194 0.0662 0.8479 0.048 Uiso calc R 1 H
C4 1.4719(4) -0.09770(10) 1.03260(10) 0.0398(4) Uani d . 1 C
H4A 1.4539 -0.1636 1.0551 0.048 Uiso calc R 1 H
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
Mn1 0.02300(10) 0.0260(2) 0.0295(2) -0.00010(10) -0.00210(10) -0.00130(10)
O1W 0.0343(5) 0.0220(5) 0.0295(6) 0.0022(4) -0.0046(4) 0.0003(4)
O2W 0.0273(5) 0.0287(6) 0.0454(7) -0.0021(4) 0.0022(5) -0.0083(5)
O3W 0.0301(6) 0.0591(8) 0.0433(7) -0.0072(6) -0.0049(5) 0.0190(6)
N1 0.0363(7) 0.0248(6) 0.0361(7) -0.0037(5) -0.0088(5) 0.0050(5)
N2 0.0378(7) 0.0282(7) 0.0400(8) -0.0055(5) -0.0115(6) 0.0049(6)
N3 0.0409(7) 0.0251(6) 0.0455(8) -0.0056(6) -0.0129(6) 0.0042(6)
N4 0.0374(7) 0.0238(6) 0.0440(8) -0.0030(5) -0.0116(6) 0.0040(5)
C1 0.0307(7) 0.0229(7) 0.0289(7) -0.0002(5) -0.0010(6) 0.0021(5)
C2 0.0299(7) 0.0248(7) 0.0315(8) -0.0022(6) -0.0020(6) 0.0015(6)
C3 0.0447(9) 0.0281(8) 0.0420(9) -0.0040(7) -0.0161(7) 0.0077(7)
C4 0.0457(9) 0.0242(7) 0.0457(9) -0.0068(6) -0.0132(7) 0.0096(7)
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'
Mn Mn 0.3368 0.7283 '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
O3W Mn1 O3W . 3_656 180.0 ?
O3W Mn1 O2W . . 94.38(5) yes
O3W Mn1 O2W 3_656 . 85.62(5) ?
O3W Mn1 O2W . 3_656 85.62(5) ?
O3W Mn1 O2W 3_656 3_656 94.38(5) ?
O2W Mn1 O2W . 3_656 180.00(6) ?
O3W Mn1 O1W . 3_656 92.44(5) ?
O3W Mn1 O1W 3_656 3_656 87.56(5) ?
O2W Mn1 O1W . 3_656 93.27(4) ?
O2W Mn1 O1W 3_656 3_656 86.73(4) ?
O3W Mn1 O1W . . 87.56(5) yes
O3W Mn1 O1W 3_656 . 92.44(5) ?
O2W Mn1 O1W . . 86.73(4) yes
O2W Mn1 O1W 3_656 . 93.27(4) ?
O1W Mn1 O1W 3_656 . 180.0 ?
Mn1 O1W H1WA . . 116.0(10) ?
Mn1 O1W H1WB . . 118.0(10) ?
H1WA O1W H1WB . . 110.0(10) ?
Mn1 O2W H2WA . . 112.0(10) ?
Mn1 O2W H2WB . . 117.0(10) ?
H2WA O2W H2WB . . 108.0(10) ?
Mn1 O3W H3WA . . 119.0(10) ?
Mn1 O3W H3WB . . 128(2) ?
H3WA O3W H3WB . . 113.0(10) ?
C1 N1 N2 . . 105.30(10) yes
N3 N2 N1 . . 109.20(10) yes
N2 N3 N4 . . 109.50(10) yes
C1 N4 N3 . . 105.00(10) yes
N4 C1 N1 . . 110.90(10) yes
N4 C1 C2 . . 124.40(10) ?
N1 C1 C2 . . 124.70(10) ?
C4 C2 C3 . . 118.50(10) ?
C4 C2 C1 . . 120.60(10) ?
C3 C2 C1 . . 120.80(10) ?
C4 C3 C2 3_857 . 120.50(10) ?
C4 C3 H3A 3_857 . 119.7 ?
C2 C3 H3A . . 119.7 ?
C3 C4 C2 3_857 . 120.90(10) ?
C3 C4 H4A 3_857 . 119.5 ?
C2 C4 H4A . . 119.5 ?
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
Mn1 O3W . 2.1560(10) yes
Mn1 O3W 3_656 2.1560(10) ?
Mn1 O2W . 2.1700(10) yes
Mn1 O2W 3_656 2.1700(10) ?
Mn1 O1W 3_656 2.2030(10) ?
Mn1 O1W . 2.2030(10) yes
O1W H1WA . 0.847(9) ?
O1W H1WB . 0.845(9) ?
O2W H2WA . 0.854(9) ?
O2W H2WB . 0.850(9) ?
O3W H3WA . 0.838(9) ?
O3W H3WB . 0.840(10) ?
N1 C1 . 1.328(2) yes
N1 N2 . 1.3390(10) yes
N2 N3 . 1.2950(10) yes
N3 N4 . 1.342(2) yes
N4 C1 . 1.325(2) yes
C1 C2 . 1.465(2) yes
C2 C4 . 1.384(2) yes
C2 C3 . 1.390(2) yes
C3 C4 3_857 1.381(2) ?
C3 H3A . 0.9300 ?
C4 C3 3_857 1.381(2) ?
C4 H4A . 0.9300 ?
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
O3W H3WA N2 . 0.838(9) 1.940(10) 2.746(2) 160(2)
O1W H1WA N1 3_656 0.847(9) 1.872(9) 2.7060(10) 168(2)
O2W H2WA N4 2_656 0.854(9) 1.870(10) 2.720(2) 172(2)
O1W H1WB N3 4 0.845(9) 1.905(9) 2.721(2) 162.0(10)
