#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/46/2224614.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_2224614
loop_
_publ_author_name
'Shi, Chong-Yu'
'Zhou, Xiao-Li'
'Wu, Bo'
'Zhu, Ni'
'Weia, Zhen-Shu'
_publ_section_title
catena-Poly[[diaquadichloridomanganese(II)]-μ-1,1'-bis(1H-1,2,4-triazol-1-ylmethyl)ferrocene]
_journal_coeditor_code           DN2521
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m96
_journal_paper_doi               10.1107/S1600536809053823
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Fe Mn (C8 H8 N3)2 Cl2 (H2 O)2]'
_chemical_formula_moiety         'C16 H20 Cl2 Fe Mn N6 O2'
_chemical_formula_sum            'C16 H20 Cl2 Fe Mn N6 O2'
_chemical_formula_weight         510.07
_chemical_name_systematic
;
catena-Poly[[diaquadichloridomanganese(II)]-μ-1,1'-bis(1H-
1,2,4-triazol-1-ylmethyl)ferrocene]
;
_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                98.963(2)
_cell_angle_beta                 101.076(2)
_cell_angle_gamma                103.939(2)
_cell_formula_units_Z            1
_cell_length_a                   5.9596(7)
_cell_length_b                   7.1630(8)
_cell_length_c                   12.4226(14)
_cell_measurement_reflns_used    1751
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      3.0
_cell_volume                     493.60(10)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_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  0.0074
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2618
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         3.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  0.8507
_exptl_absorpt_correction_T_min  0.6706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             259
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0274
_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)+(0.0350P)²+0.4359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                1655
_reflns_number_total             1751
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2521.cif
_cod_data_source_block           I
_cod_database_code               2224614
_cod_database_fobs_code          2224614
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
Fe Fe1 0.0000 0.5000 0.0000 0.02935(14) Uani d S 1 . .
Mn Mn1 0.5000 0.5000 0.5000 0.02631(14) Uani d S 1 . .
Cl Cl1 0.90203(9) 0.74119(8) 0.57695(5) 0.03530(16) Uani d . 1 . .
O O1 0.6247(3) 0.3669(2) 0.35390(13) 0.0326(4) Uani d . 1 . .
H H1W 0.7574 0.3523 0.3780 0.049 Uiso d R 1 . .
H H2W 0.5284 0.2583 0.3270 0.049 Uiso d R 1 . .
N N1 0.3881(3) 0.7148(3) 0.40001(16) 0.0314(4) Uani d . 1 . .
N N2 0.1856(3) 0.8317(3) 0.27483(15) 0.0290(4) Uani d . 1 . .
N N3 0.4163(4) 0.9406(3) 0.29279(18) 0.0372(5) Uani d . 1 . .
C C1 0.5298(4) 0.8646(3) 0.3686(2) 0.0343(5) Uani d . 1 . .
H H1 0.6935 0.9100 0.3982 0.041 Uiso calc R 1 . .
C C2 0.1739(4) 0.7009(3) 0.33907(19) 0.0316(5) Uani d . 1 . .
H H2 0.0340 0.6112 0.3413 0.038 Uiso calc R 1 . .
C C3 -0.0041(4) 0.8607(4) 0.19119(19) 0.0341(5) Uani d . 1 . .
H H3A 0.0119 1.0005 0.1998 0.041 Uiso calc R 1 . .
H H3B -0.1564 0.7989 0.2052 0.041 Uiso calc R 1 . .
C C4 -0.0033(4) 0.7779(3) 0.07253(19) 0.0291(5) Uani d . 1 . .
C C5 0.1944(5) 0.7898(3) 0.0235(2) 0.0374(6) Uani d . 1 . .
H H5 0.3535 0.8445 0.0611 0.045 Uiso calc R 1 . .
C C6 0.1073(6) 0.7037(4) -0.0928(2) 0.0472(7) Uani d . 1 . .
H H6 0.1995 0.6909 -0.1446 0.057 Uiso calc R 1 . .
C C7 -0.1441(6) 0.6408(4) -0.1162(2) 0.0477(7) Uani d . 1 . .
H H7 -0.2464 0.5801 -0.1860 0.057 Uiso calc R 1 . .
C C8 -0.2126(5) 0.6868(4) -0.0143(2) 0.0374(6) Uani d . 1 . .
H H8 -0.3681 0.6615 -0.0058 0.045 Uiso calc 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'
Fe Fe 0.3463 0.8444 '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
C6 Fe1 C6 . 2_565 180.00(11) ?
C6 Fe1 C7 . 2_565 139.78(13) ?
C6 Fe1 C7 2_565 2_565 40.22(13) ?
C6 Fe1 C7 . . 40.22(13) ?
C6 Fe1 C7 2_565 . 139.78(13) ?
C7 Fe1 C7 2_565 . 180.00(11) ?
C6 Fe1 C4 . . 67.93(10) ?
C6 Fe1 C4 2_565 . 112.07(10) ?
C7 Fe1 C4 2_565 . 112.05(10) ?
C7 Fe1 C4 . . 67.95(10) ?
C6 Fe1 C4 . 2_565 112.07(10) ?
C6 Fe1 C4 2_565 2_565 67.93(10) ?
C7 Fe1 C4 2_565 2_565 67.95(10) ?
C7 Fe1 C4 . 2_565 112.05(10) ?
C4 Fe1 C4 . 2_565 180.0 ?
C6 Fe1 C8 . 2_565 112.35(11) ?
C6 Fe1 C8 2_565 2_565 67.65(11) ?
C7 Fe1 C8 2_565 2_565 40.31(11) ?
C7 Fe1 C8 . 2_565 139.69(11) ?
C4 Fe1 C8 . 2_565 139.64(9) ?
C4 Fe1 C8 2_565 2_565 40.36(9) ?
C6 Fe1 C8 . . 67.65(11) ?
C6 Fe1 C8 2_565 . 112.35(11) ?
C7 Fe1 C8 2_565 . 139.69(11) ?
C7 Fe1 C8 . . 40.31(11) ?
C4 Fe1 C8 . . 40.36(9) ?
C4 Fe1 C8 2_565 . 139.64(9) ?
C8 Fe1 C8 2_565 . 180.0 ?
C6 Fe1 C5 . . 40.36(11) ?
C6 Fe1 C5 2_565 . 139.64(11) ?
C7 Fe1 C5 2_565 . 112.36(11) ?
C7 Fe1 C5 . . 67.64(11) ?
C4 Fe1 C5 . . 40.21(9) ?
C4 Fe1 C5 2_565 . 139.79(9) ?
C8 Fe1 C5 2_565 . 112.51(10) ?
C8 Fe1 C5 . . 67.49(10) ?
C6 Fe1 C5 . 2_565 139.64(11) ?
C6 Fe1 C5 2_565 2_565 40.36(11) ?
C7 Fe1 C5 2_565 2_565 67.64(11) ?
C7 Fe1 C5 . 2_565 112.36(11) ?
C4 Fe1 C5 . 2_565 139.79(9) ?
C4 Fe1 C5 2_565 2_565 40.21(9) ?
C8 Fe1 C5 2_565 2_565 67.49(10) ?
C8 Fe1 C5 . 2_565 112.51(10) ?
C5 Fe1 C5 . 2_565 180.0 ?
O1 Mn1 O1 2_666 . 180.00(5) ?
O1 Mn1 N1 2_666 2_666 89.33(6) ?
O1 Mn1 N1 . 2_666 90.67(6) ?
O1 Mn1 N1 2_666 . 90.67(6) ?
O1 Mn1 N1 . . 89.33(6) ?
N1 Mn1 N1 2_666 . 180.00(8) ?
O1 Mn1 Cl1 2_666 . 89.68(4) ?
O1 Mn1 Cl1 . . 90.32(4) ?
N1 Mn1 Cl1 2_666 . 90.62(5) ?
N1 Mn1 Cl1 . . 89.38(5) ?
O1 Mn1 Cl1 2_666 2_666 90.32(4) ?
O1 Mn1 Cl1 . 2_666 89.68(4) ?
N1 Mn1 Cl1 2_666 2_666 89.38(5) ?
N1 Mn1 Cl1 . 2_666 90.62(5) ?
Cl1 Mn1 Cl1 . 2_666 180.0 ?
Mn1 O1 H1W . . 108.5 ?
Mn1 O1 H2W . . 105.9 ?
H1W O1 H2W . . 109.2 ?
C2 N1 C1 . . 102.58(19) ?
C2 N1 Mn1 . . 128.23(16) ?
C1 N1 Mn1 . . 127.89(16) ?
C2 N2 N3 . . 109.41(19) ?
C2 N2 C3 . . 129.1(2) ?
N3 N2 C3 . . 121.46(19) ?
C1 N3 N2 . . 102.70(19) ?
N3 C1 N1 . . 114.4(2) ?
N3 C1 H1 . . 122.8 ?
N1 C1 H1 . . 122.8 ?
N2 C2 N1 . . 110.9(2) ?
N2 C2 H2 . . 124.5 ?
N1 C2 H2 . . 124.5 ?
N2 C3 C4 . . 113.50(18) ?
N2 C3 H3A . . 108.9 ?
C4 C3 H3A . . 108.9 ?
N2 C3 H3B . . 108.9 ?
C4 C3 H3B . . 108.9 ?
H3A C3 H3B . . 107.7 ?
C5 C4 C8 . . 107.6(2) ?
C5 C4 C3 . . 128.2(2) ?
C8 C4 C3 . . 124.0(2) ?
C5 C4 Fe1 . . 70.05(13) ?
C8 C4 Fe1 . . 69.72(12) ?
C3 C4 Fe1 . . 129.76(16) ?
C4 C5 C6 . . 108.2(2) ?
C4 C5 Fe1 . . 69.75(13) ?
C6 C5 Fe1 . . 69.51(15) ?
C4 C5 H5 . . 125.9 ?
C6 C5 H5 . . 125.9 ?
Fe1 C5 H5 . . 126.4 ?
C7 C6 C5 . . 108.0(2) ?
C7 C6 Fe1 . . 69.95(15) ?
C5 C6 Fe1 . . 70.13(14) ?
C7 C6 H6 . . 126.0 ?
C5 C6 H6 . . 126.0 ?
Fe1 C6 H6 . . 125.5 ?
C6 C7 C8 . . 107.9(2) ?
C6 C7 Fe1 . . 69.83(14) ?
C8 C7 Fe1 . . 69.84(13) ?
C6 C7 H7 . . 126.0 ?
C8 C7 H7 . . 126.0 ?
Fe1 C7 H7 . . 125.9 ?
C4 C8 C7 . . 108.3(2) ?
C4 C8 Fe1 . . 69.93(12) ?
C7 C8 Fe1 . . 69.85(14) ?
C4 C8 H8 . . 125.8 ?
C7 C8 H8 . . 125.8 ?
Fe1 C8 H8 . . 126.0 ?
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
Fe1 C6 . 2.056(3) ?
Fe1 C6 2_565 2.056(3) ?
Fe1 C7 2_565 2.057(2) ?
Fe1 C7 . 2.057(2) ?
Fe1 C4 . 2.060(2) ?
Fe1 C4 2_565 2.060(2) ?
Fe1 C8 2_565 2.057(2) ?
Fe1 C8 . 2.057(2) ?
Fe1 C5 . 2.064(2) ?
Fe1 C5 2_565 2.064(2) ?
Mn1 O1 2_666 2.2527(16) ?
Mn1 O1 . 2.2527(16) ?
Mn1 N1 2_666 2.2639(19) ?
Mn1 N1 . 2.2639(19) ?
Mn1 Cl1 . 2.5000(6) ?
Mn1 Cl1 2_666 2.5000(6) ?
O1 H1W . 0.8274 ?
O1 H2W . 0.8224 ?
N1 C2 . 1.326(3) ?
N1 C1 . 1.356(3) ?
N2 C2 . 1.320(3) ?
N2 N3 . 1.364(3) ?
N2 C3 . 1.460(3) ?
N3 C1 . 1.317(3) ?
C1 H1 . 0.9300 ?
C2 H2 . 0.9300 ?
C3 C4 . 1.502(3) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 C5 . 1.417(3) ?
C4 C8 . 1.420(3) ?
C5 C6 . 1.421(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.414(4) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.418(4) ?
C7 H7 . 0.9300 ?
C8 H8 . 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
O1 H1W Cl1 2_766 0.83 2.28 3.1021(17) 169.8
O1 H2W N3 1_545 0.82 2.16 2.921(3) 154.0
