#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/95/2219568.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_2219568
loop_
_publ_author_name
'Lü, Yuanqi'
_publ_section_title
;
 Pentaaqua[5,5'-(m-phenylene)ditetrazolato-κN²]manganese(II)
 dihydrate
;
_journal_coeditor_code           EZ2139
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1255
_journal_paper_doi               10.1107/S1600536808028316
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Mn (C8 H4 N8)2 (H2 O)5] , 2H2 O'
_chemical_formula_moiety         'C8 H14 Mn N8 O5 , 2H2 O'
_chemical_formula_sum            'C8 H18 Mn N8 O7'
_chemical_formula_weight         393.24
_chemical_name_systematic
;
Pentaaqua[5,5'-(m-phenylene)ditetrazolato-κN²]manganese(II)
dihydrate
;
_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           'With SHELXTL software package'
_cell_angle_alpha                68.2960(10)
_cell_angle_beta                 77.213(3)
_cell_angle_gamma                77.280(5)
_cell_formula_units_Z            2
_cell_length_a                   6.59320(10)
_cell_length_b                   10.0711(2)
_cell_length_c                   12.9857(3)
_cell_measurement_reflns_used    3628
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.7
_cell_volume                     772.10(3)
_computing_cell_refinement       'SMART (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7710
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.7981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0380
_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)+(0.0414P)²+0.3671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                2846
_reflns_number_total             3704
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ez2139.cif
_cod_data_source_block           global
_cod_database_code               2219568
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
Mn Mn1 0.11390(6) 0.68638(4) 0.58413(3) 0.02732(12) Uani d . 1
O O1 0.3923(3) 0.7734(2) 0.57901(16) 0.0388(4) Uani d . 1
O O2 -0.1155(4) 0.8808(2) 0.58408(19) 0.0402(5) Uani d . 1
O O3 0.0794(3) 0.6043(2) 0.76359(15) 0.0361(4) Uani d . 1
O O4 -0.1679(4) 0.6027(2) 0.59456(18) 0.0411(5) Uani d . 1
O O5 0.3064(5) 0.4784(2) 0.5795(2) 0.0508(6) Uani d . 1
O O6 0.2643(3) 0.5392(2) 0.12086(18) 0.0370(4) Uani d . 1
O O7 0.6605(4) 0.3559(3) 0.11514(17) 0.0367(4) Uani d . 1
N N1 0.1613(3) 0.90491(19) 0.31988(14) 0.0244(4) Uani d . 1
N N2 0.1633(3) 0.76902(19) 0.39242(14) 0.0264(4) Uani d . 1
N N3 0.1980(3) 0.6792(2) 0.33621(15) 0.0300(4) Uani d . 1
N N4 0.2200(3) 0.75287(19) 0.22651(15) 0.0268(4) Uani d . 1
N N5 0.3286(3) 0.9471(2) -0.21040(15) 0.0276(4) Uani d . 1
N N6 0.3651(3) 0.9732(2) -0.32077(16) 0.0315(4) Uani d . 1
N N7 0.3610(3) 1.1128(2) -0.37435(16) 0.0318(4) Uani d . 1
N N8 0.3223(3) 1.1812(2) -0.29911(15) 0.0275(4) Uani d . 1
C C1 0.1974(3) 0.8914(2) 0.21865(17) 0.0205(4) Uani d . 1
C C2 0.2128(3) 1.0130(2) 0.11148(17) 0.0216(4) Uani d . 1
C C3 0.2001(4) 1.1526(2) 0.11091(19) 0.0306(5) Uani d . 1
H H3 0.1796 1.1699 0.1783 0.037 Uiso calc R 1
C C4 0.2177(4) 1.2662(2) 0.0105(2) 0.0380(6) Uani d . 1
H H4 0.2077 1.3597 0.0105 0.046 Uiso calc R 1
C C5 0.2501(4) 1.2411(2) -0.09028(19) 0.0311(5) Uani d . 1
H H5 0.2627 1.3178 -0.1576 0.037 Uiso calc R 1
C C6 0.2640(3) 1.1024(2) -0.09143(17) 0.0217(4) Uani d . 1
C C7 0.2443(3) 0.9883(2) 0.00989(17) 0.0214(4) Uani d . 1
H H7 0.2523 0.8950 0.0098 0.026 Uiso calc R 1
C C8 0.3031(3) 1.0766(2) -0.19900(17) 0.0224(4) Uani d . 1
H H1A 0.455(5) 0.808(3) 0.519(3) 0.044(9) Uiso d . 1
H H6A 0.254(5) 0.602(4) 0.148(3) 0.053(9) Uiso d . 1
H H4B -0.180(5) 0.511(4) 0.613(3) 0.063(10) Uiso d . 1
H H7A 0.659(5) 0.278(4) 0.135(3) 0.060(12) Uiso d . 1
H H5B 0.306(6) 0.402(4) 0.620(3) 0.068(12) Uiso d . 1
H H1B 0.378(5) 0.838(4) 0.608(3) 0.068(11) Uiso d . 1
H H2B -0.124(5) 0.933(4) 0.614(3) 0.052(10) Uiso d . 1
H H3B -0.018(5) 0.560(3) 0.800(3) 0.059(10) Uiso d . 1
H H3A 0.149(5) 0.615(4) 0.806(3) 0.065(11) Uiso d . 1
H H4A -0.261(6) 0.645(4) 0.597(3) 0.076(16) Uiso d . 1
H H2A -0.179(7) 0.908(5) 0.539(4) 0.105(18) Uiso d . 1
H H6B 0.286(8) 0.554(5) 0.070(4) 0.09(2) Uiso d . 1
H H7B 0.588(10) 0.394(6) 0.126(5) 0.11(3) Uiso d . 1
H H5A 0.396(10) 0.477(7) 0.567(5) 0.10(3) Uiso 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'
Mn Mn 0.3368 0.7283 '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
O3 Mn1 O4 88.99(8)
O3 Mn1 O1 89.37(8)
O4 Mn1 O1 177.83(8)
O3 Mn1 O2 92.33(8)
O4 Mn1 O2 81.61(9)
O1 Mn1 O2 97.05(8)
O3 Mn1 O5 89.42(8)
O4 Mn1 O5 90.03(11)
O1 Mn1 O5 91.36(10)
O2 Mn1 O5 171.42(11)
O3 Mn1 N2 177.82(7)
O4 Mn1 N2 92.24(8)
O1 Mn1 N2 89.44(7)
O2 Mn1 N2 89.63(8)
O5 Mn1 N2 88.78(8)
Mn1 O1 H1A 116(2)
Mn1 O1 H1B 118(2)
H1A O1 H1B 102(3)
Mn1 O2 H2B 131(3)
Mn1 O2 H2A 115(4)
H2B O2 H2A 113(4)
Mn1 O3 H3B 120(2)
Mn1 O3 H3A 129(2)
H3B O3 H3A 110(3)
Mn1 O4 H4B 127(2)
Mn1 O4 H4A 119(4)
H4B O4 H4A 113(4)
Mn1 O5 H5B 132(3)
Mn1 O5 H5A 117(7)
H5B O5 H5A 99(7)
H6A O6 H6B 119(5)
H7A O7 H7B 120(6)
C1 N1 N2 104.79(16)
N3 N2 N1 109.26(16)
N3 N2 Mn1 120.96(13)
N1 N2 Mn1 129.79(13)
N2 N3 N4 109.71(17)
N3 N4 C1 104.97(17)
N6 N5 C8 105.15(17)
N7 N6 N5 109.76(17)
N6 N7 N8 109.04(17)
C8 N8 N7 105.04(18)
N1 C1 N4 111.28(17)
N1 C1 C2 124.65(18)
N4 C1 C2 124.07(18)
C3 C2 C7 119.41(19)
C3 C2 C1 120.24(19)
C7 C2 C1 120.34(18)
C4 C3 C2 120.2(2)
C4 C3 H3 119.9
C2 C3 H3 119.9
C3 C4 C5 120.2(2)
C3 C4 H4 119.9
C5 C4 H4 119.9
C6 C5 C4 120.4(2)
C6 C5 H5 119.8
C4 C5 H5 119.8
C5 C6 C7 119.31(19)
C5 C6 C8 119.95(19)
C7 C6 C8 120.73(18)
C6 C7 C2 120.44(19)
C6 C7 H7 119.8
C2 C7 H7 119.8
N5 C8 N8 111.01(18)
N5 C8 C6 125.20(18)
N8 C8 C6 123.78(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 O3 2.1423(18)
Mn1 O4 2.162(2)
Mn1 O1 2.1797(19)
Mn1 O2 2.1946(19)
Mn1 O5 2.212(2)
Mn1 N2 2.2857(17)
O1 H1A 0.78(3)
O1 H1B 0.85(4)
O2 H2B 0.75(3)
O2 H2A 0.73(5)
O3 H3B 0.82(3)
O3 H3A 0.84(4)
O4 H4B 0.88(4)
O4 H4A 0.67(4)
O5 H5B 0.75(4)
O5 H5A 0.57(6)
O6 H6A 0.82(3)
O6 H6B 0.61(5)
O7 H7A 0.73(4)
O7 H7B 0.57(6)
N1 C1 1.335(3)
N1 N2 1.343(2)
N2 N3 1.314(2)
N3 N4 1.332(2)
N4 C1 1.338(3)
N5 N6 1.333(3)
N5 C8 1.336(3)
N6 N7 1.315(3)
N7 N8 1.343(3)
N8 C8 1.338(3)
C1 C2 1.476(3)
C2 C3 1.387(3)
C2 C7 1.394(3)
C3 C4 1.382(3)
C3 H3 0.9300
C4 C5 1.385(3)
C4 H4 0.9300
C5 C6 1.385(3)
C5 H5 0.9300
C6 C7 1.393(3)
C6 C8 1.472(3)
C7 H7 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
O7 H7B O6 . 0.57(6) 2.31(6) 2.852(3) 162(8)
O5 H5A O5 2_666 0.57(6) 2.41(5) 2.910(6) 148(9)
O6 H6B O7 2_665 0.61(5) 2.21(5) 2.814(3) 171(6)
O4 H4A O1 1_455 0.67(4) 2.38(4) 3.035(3) 167(5)
O3 H3A O7 2_666 0.84(4) 1.91(4) 2.747(3) 171(3)
O3 H3B O6 2_566 0.82(3) 1.98(3) 2.794(3) 176(3)
O2 H2B N1 2_576 0.75(3) 2.06(3) 2.800(3) 173(3)
O1 H1B N6 1_556 0.85(4) 1.89(4) 2.730(3) 176(3)
O5 H5B N8 1_546 0.75(4) 2.07(4) 2.810(3) 168(4)
O7 H7A N5 2_665 0.73(4) 2.10(4) 2.828(3) 173(4)
O4 H4B N3 2_566 0.88(4) 1.80(4) 2.681(3) 175(3)
O6 H6A N4 . 0.82(3) 2.07(4) 2.886(3) 176(3)
O1 H1A N7 2_675 0.78(3) 1.99(3) 2.771(3) 175(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
C1 N1 N2 N3 -0.3(2)
C1 N1 N2 Mn1 -179.63(15)
O4 Mn1 N2 N3 -62.82(18)
O1 Mn1 N2 N3 118.54(17)
O2 Mn1 N2 N3 -144.41(18)
O5 Mn1 N2 N3 27.16(18)
O3 Mn1 N2 N1 -119.2(19)
O4 Mn1 N2 N1 116.41(19)
O1 Mn1 N2 N1 -62.23(19)
O2 Mn1 N2 N1 34.82(19)
O5 Mn1 N2 N1 -153.6(2)
N1 N2 N3 N4 0.2(2)
Mn1 N2 N3 N4 179.52(14)
N2 N3 N4 C1 0.1(2)
C8 N5 N6 N7 -0.3(2)
N5 N6 N7 N8 0.4(3)
N6 N7 N8 C8 -0.2(2)
N2 N1 C1 N4 0.4(2)
N2 N1 C1 C2 -179.00(19)
N3 N4 C1 N1 -0.3(2)
N3 N4 C1 C2 179.09(19)
N1 C1 C2 C3 3.3(3)
N4 C1 C2 C3 -176.0(2)
N1 C1 C2 C7 -177.9(2)
N4 C1 C2 C7 2.7(3)
C7 C2 C3 C4 0.2(4)
C1 C2 C3 C4 179.0(2)
C2 C3 C4 C5 -0.6(4)
C3 C4 C5 C6 0.4(4)
C4 C5 C6 C7 0.2(4)
C4 C5 C6 C8 -178.7(2)
C5 C6 C7 C2 -0.5(3)
C8 C6 C7 C2 178.31(19)
C3 C2 C7 C6 0.3(3)
C1 C2 C7 C6 -178.46(19)
N6 N5 C8 N8 0.2(2)
N6 N5 C8 C6 -178.4(2)
N7 N8 C8 N5 0.0(2)
N7 N8 C8 C6 178.67(19)
C5 C6 C8 N5 176.9(2)
C7 C6 C8 N5 -1.9(3)
C5 C6 C8 N8 -1.6(3)
C7 C6 C8 N8 179.6(2)
