#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/07/2220791.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_2220791
loop_
_publ_author_name
'Wang, Zuoxiang'
'Gong, Ixaoning'
'Liu, Chunyi'
'Zhang, Xiaoming'
_publ_section_title
Di-μ-chlorido-bis{aquachlorido[3-ethyl-4-phenyl-5-(2-pyridyl)-4H-1,2,4-triazole-κ²N¹,N⁵]manganese(II)}
_journal_coeditor_code           HB2883
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m157
_journal_paper_doi               10.1107/S1600536808044103
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mn2 Cl4 (C15 H14 N4)2 (H2 O)2]'
_chemical_formula_moiety         'C30 H32 Cl4 Mn2 N8 O2'
_chemical_formula_sum            'C30 H32 Cl4 Mn2 N8 O2'
_chemical_formula_weight         788.32
_chemical_name_systematic
;
Di-μ-chlorido-bis{aquachlorido[3-ethyl-4-phenyl-5-(2-pyridyl)-4H-
1,2,4-triazole-κ^2^N^1^,N^^5^]manganese(II)}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.323(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9369(15)
_cell_length_b                   8.9369(13)
_cell_length_c                   19.642(3)
_cell_measurement_reflns_used    4766
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.50
_cell_volume                     1697.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8811
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0529
_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)+(0.04P)²+0.95P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                2364
_reflns_number_total             3329
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2883.cif
_cod_data_source_block           I
_cod_original_cell_volume        1697.3(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2220791
_cod_database_fobs_code          2220791
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Mn Mn1 0.52358(6) 0.80195(6) 0.52295(3) 0.03231(16) Uani d . 1 . .
Cl Cl1 0.32636(10) 0.98690(10) 0.50448(4) 0.0327(2) Uani d . 1 . .
Cl Cl2 0.46719(10) 0.68828(10) 0.40606(4) 0.0340(2) Uani d . 1 . .
C C1 0.5362(4) 0.9652(4) 0.67503(19) 0.0356(9) Uani d . 1 . .
H H1 0.4723 1.0295 0.6477 0.043 Uiso calc R 1 . .
C C2 0.5739(4) 0.9897(5) 0.7457(2) 0.0416(10) Uani d . 1 . .
H H2 0.5393 1.0715 0.7654 0.050 Uiso calc R 1 . .
C C3 0.6643(4) 0.8909(5) 0.78734(19) 0.0404(10) Uani d . 1 . .
H H3 0.6896 0.9038 0.8356 0.049 Uiso calc R 1 . .
C C4 0.7167(4) 0.7719(4) 0.75560(18) 0.0365(9) Uani d . 1 . .
H H4 0.7757 0.7025 0.7825 0.044 Uiso calc R 1 . .
C C5 0.6801(3) 0.7581(4) 0.68393(18) 0.0263(7) Uani d . 1 . .
C C6 0.7326(4) 0.6459(4) 0.64299(19) 0.0324(8) Uani d . 1 . .
C C7 0.8480(4) 0.4695(4) 0.60588(18) 0.0335(8) Uani d . 1 . .
C C8 0.9328(5) 0.3335(5) 0.60667(19) 0.0438(10) Uani d . 1 . .
H H8A 1.0122 0.3415 0.6459 0.053 Uiso calc R 1 . .
H H8B 0.8786 0.2488 0.6159 0.053 Uiso calc R 1 . .
C C9 0.9834(4) 0.2988(5) 0.5451(2) 0.0422(10) Uani d . 1 . .
H H9A 0.9074 0.2977 0.5047 0.063 Uiso calc R 1 . .
H H9B 1.0272 0.2024 0.5506 0.063 Uiso calc R 1 . .
H H9C 1.0492 0.3734 0.5390 0.063 Uiso calc R 1 . .
C C10 0.8737(4) 0.4760(4) 0.73627(18) 0.0368(9) Uani d . 1 . .
C C11 1.0054(4) 0.5134(5) 0.77226(18) 0.0390(9) Uani d . 1 . .
H H11 1.0620 0.5727 0.7517 0.047 Uiso calc R 1 . .
C C12 1.0518(4) 0.4594(5) 0.84098(19) 0.0397(10) Uani d . 1 . .
H H12 1.1397 0.4835 0.8670 0.048 Uiso calc R 1 . .
C C13 0.9654(4) 0.3702(5) 0.86918(19) 0.0420(10) Uani d . 1 . .
H H13 0.9960 0.3335 0.9144 0.050 Uiso calc R 1 . .
C C14 0.8336(5) 0.3345(5) 0.83126(19) 0.0421(10) Uani d . 1 . .
H H14 0.7758 0.2764 0.8517 0.051 Uiso calc R 1 . .
C C15 0.7878(5) 0.3844(5) 0.7637(2) 0.0443(10) Uani d . 1 . .
H H15 0.7012 0.3570 0.7372 0.053 Uiso calc R 1 . .
N N1 0.5877(3) 0.8514(3) 0.64330(14) 0.0303(7) Uani d . 1 . .
N N2 0.7055(3) 0.6526(3) 0.57301(15) 0.0322(7) Uani d . 1 . .
N N3 0.7784(3) 0.5400(3) 0.55068(15) 0.0329(7) Uani d . 1 . .
N N4 0.8223(3) 0.5325(3) 0.66508(14) 0.0313(7) Uani d . 1 . .
O O1 0.3944(3) 0.6254(3) 0.56175(12) 0.0321(6) Uani d . 1 . .
H H1A 0.4420 0.5461 0.5721 0.039 Uiso d R 1 . .
H H1C 0.3228 0.6062 0.5299 0.039 Uiso d R 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'
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'
Cl Cl 0.1484 0.1585 '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
O1 Mn1 N2 . . 84.37(10) ?
O1 Mn1 N1 . . 80.58(10) ?
N2 Mn1 N1 . . 70.80(10) ?
O1 Mn1 Cl2 . . 90.09(7) ?
N2 Mn1 Cl2 . . 98.54(8) ?
N1 Mn1 Cl2 . . 166.35(8) ?
O1 Mn1 Cl1 . . 91.32(7) ?
N2 Mn1 Cl1 . . 163.18(8) ?
N1 Mn1 Cl1 . . 92.47(8) ?
Cl2 Mn1 Cl1 . . 97.71(3) ?
O1 Mn1 Cl1 . 3_676 172.57(7) ?
N2 Mn1 Cl1 . 3_676 94.62(8) ?
N1 Mn1 Cl1 . 3_676 92.13(8) ?
Cl2 Mn1 Cl1 . 3_676 97.34(4) ?
Cl1 Mn1 Cl1 . 3_676 87.55(4) ?
Mn1 Cl1 Mn1 . 3_676 92.45(4) y
N1 C1 C2 . . 122.9(3) ?
N1 C1 H1 . . 118.6 ?
C2 C1 H1 . . 118.6 ?
C1 C2 C3 . . 119.1(4) ?
C1 C2 H2 . . 120.5 ?
C3 C2 H2 . . 120.5 ?
C2 C3 C4 . . 118.7(3) ?
C2 C3 H3 . . 120.6 ?
C4 C3 H3 . . 120.6 ?
C5 C4 C3 . . 119.2(4) ?
C5 C4 H4 . . 120.4 ?
C3 C4 H4 . . 120.4 ?
N1 C5 C4 . . 122.0(3) ?
N1 C5 C6 . . 112.3(3) ?
C4 C5 C6 . . 125.7(3) ?
N2 C6 N4 . . 108.9(3) ?
N2 C6 C5 . . 121.6(3) ?
N4 C6 C5 . . 129.2(3) ?
N3 C7 N4 . . 109.9(3) ?
N3 C7 C8 . . 126.7(3) ?
N4 C7 C8 . . 123.2(3) ?
C9 C8 C7 . . 118.3(3) ?
C9 C8 H8A . . 107.7 ?
C7 C8 H8A . . 107.7 ?
C9 C8 H8B . . 107.7 ?
C7 C8 H8B . . 107.7 ?
H8A C8 H8B . . 107.1 ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C11 C10 C15 . . 122.9(4) ?
C11 C10 N4 . . 119.2(4) ?
C15 C10 N4 . . 117.8(4) ?
C10 C11 C12 . . 118.2(4) ?
C10 C11 H11 . . 120.9 ?
C12 C11 H11 . . 120.9 ?
C13 C12 C11 . . 119.1(4) ?
C13 C12 H12 . . 120.4 ?
C11 C12 H12 . . 120.4 ?
C12 C13 C14 . . 121.1(4) ?
C12 C13 H13 . . 119.4 ?
C14 C13 H13 . . 119.4 ?
C15 C14 C13 . . 120.3(4) ?
C15 C14 H14 . . 119.8 ?
C13 C14 H14 . . 119.8 ?
C14 C15 C10 . . 118.3(4) ?
C14 C15 H15 . . 120.9 ?
C10 C15 H15 . . 120.9 ?
C1 N1 C5 . . 117.9(3) ?
C1 N1 Mn1 . . 124.2(2) ?
C5 N1 Mn1 . . 117.9(2) ?
C6 N2 N3 . . 107.5(3) ?
C6 N2 Mn1 . . 114.8(2) ?
N3 N2 Mn1 . . 135.8(2) ?
C7 N3 N2 . . 107.8(3) ?
C6 N4 C7 . . 105.9(3) ?
C6 N4 C10 . . 128.6(3) ?
C7 N4 C10 . . 125.3(3) ?
Mn1 O1 H1A . . 109.5 ?
Mn1 O1 H1C . . 109.5 ?
H1A O1 H1C . . 109.5 ?
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 O1 . 2.273(2) y
Mn1 N2 . 2.280(3) y
Mn1 N1 . 2.344(3) y
Mn1 Cl2 . 2.4544(11) y
Mn1 Cl1 . 2.5252(11) y
Mn1 Cl1 3_676 2.5387(11) y
Cl1 Mn1 3_676 2.5387(11) ?
C1 N1 . 1.353(5) ?
C1 C2 . 1.369(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.385(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.393(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.376(5) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.356(4) ?
C5 C6 . 1.455(5) ?
C6 N2 . 1.340(5) ?
C6 N4 . 1.354(5) ?
C7 N3 . 1.306(4) ?
C7 N4 . 1.368(4) ?
C7 C8 . 1.477(5) ?
C8 C9 . 1.447(5) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 C11 . 1.377(6) ?
C10 C15 . 1.379(6) ?
C10 N4 . 1.463(4) ?
C11 C12 . 1.407(5) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.378(6) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.387(6) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.374(5) ?
C14 H14 . 0.9300 ?
C15 H15 . 0.9300 ?
N2 N3 . 1.370(4) ?
O1 H1A . 0.8500 ?
O1 H1C . 0.8500 ?
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
O1 H1A Cl2 3_666 0.85 2.28 3.122(3) 170
O1 H1C N3 3_666 0.85 2.12 2.875(4) 148
