#------------------------------------------------------------------------------
#$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $
#$Revision: 32112 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/22/33/2223379.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_2223379
loop_
_publ_author_name
'Lu, Jing'
_publ_section_title
;
 Tris(ethylenediamine)manganese(II) sulfate
;
_journal_coeditor_code           HB5060
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1187
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mn (C2 H8 N2 )3] S O4'
_chemical_formula_moiety         'C6 H24 Mn N6 +, O4 S -'
_chemical_formula_sum            'C6 H24 Mn N6 O4 S'
_chemical_formula_weight         331.31
_chemical_name_systematic
;
Tris(ethylenediamine)manganese(II) sulfate
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.9460(13)
_cell_length_b                   8.9460(13)
_cell_length_c                   9.6230(19)
_cell_measurement_reflns_used    2640
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.63
_cell_volume                     666.96(19)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (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 CCD'
_diffrn_measurement_method       \w
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2640
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.630
_refine_ls_extinction_coef       0.051(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXS97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.549
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         402
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.894
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0575
_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/[\s^2^(Fo^2^)+(0.0637P)^2^+1.2291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                386
_reflns_number_total             402
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    hb5060.cif
_[local]_cod_data_source_block   I
_cod_error_flag                  retracted
_cod_error_source                original
_cod_error_description
;
    This file does not describe any real compound and was retracted by
    the publisher. The previously deposited coordinates can be reviewed
    in older revisions of this file or in the COD database retracted/
    subdirectory, http://www.crystallography.net/retracted/.

    The precise reasons for the retraction and other circumstances are
    extensively discussed in the Acta Cryst. E editorial:

    William T. A. Harrison, Jim Simpson and Matthias Weil, Acta
    Cryst. E 66 (2010) e1--e2

    http://journals.iucr.org/e/issues/2010/01/00/me0406/index.html
    http://journals.iucr.org/e/issues/2010/01/00/me0406/me0406.pdf
    doi:10.1107/S1600536809051757
    (http://dx.doi.org/10.1107/S1600536809051757)

    Saulius Gra\<zulis
    2011-04-19
;
_cod_database_code               2223379
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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_group
Mn Mn1 0.3333 0.6667 0.7500 0.0200(8) Uani d SU 1 .
S S1 0.3333 0.6667 0.2500 0.0332(10) Uani d S 1 .
O O1 0.489(3) 0.813(4) 0.186(2) 0.051(4) Uani d P 0.220(12) 1
O O2 0.489(3) 0.721(6) 0.163(3) 0.051(4) Uani d P 0.210(13) 2
O O3 0.373(6) 0.799(3) 0.146(3) 0.051(4) Uani d P 0.203(14) 3
O O4 0.3333 0.6667 0.114(9) 0.051(4) Uani d SP 0.10(2) 4
N N1 0.3136(7) 0.4590(8) 0.8712(6) 0.0427(14) Uani d U 1 .
H H1A 0.4072 0.4479 0.8581 0.051 Uiso calc R 1 .
H H1B 0.3070 0.4791 0.9621 0.051 Uiso calc R 1 .
C C1 0.1570(9) 0.3007(9) 0.8275(8) 0.0491(18) Uani d . 1 .
H H1C 0.0561 0.2960 0.8692 0.059 Uiso calc R 1 .
H H1D 0.1626 0.2002 0.8578 0.059 Uiso calc R 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
Mn1 0.0208(9) 0.0208(9) 0.0184(12) 0.0104(5) 0.000 0.000
S1 0.0327(13) 0.0327(13) 0.034(2) 0.0163(7) 0.000 0.000
O1 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8)
O2 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8)
O3 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8)
O4 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8)
N1 0.041(3) 0.051(3) 0.040(3) 0.026(3) 0.008(2) 0.000(2)
C1 0.051(4) 0.053(4) 0.054(4) 0.035(3) 0.002(3) -0.006(3)
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'
S S 0.1246 0.1234 '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
N1 Mn1 N1 6_566 3_565 81.6(3) ?
N1 Mn1 N1 6_566 2_665 93.5(3) ?
N1 Mn1 N1 3_565 2_665 92.7(2) ?
N1 Mn1 N1 6_566 5_556 92.7(2) ?
N1 Mn1 N1 3_565 5_556 93.5(3) ?
N1 Mn1 N1 2_665 5_556 171.8(3) ?
N1 Mn1 N1 6_566 4_666 92.7(2) ?
N1 Mn1 N1 3_565 4_666 171.8(3) ?
N1 Mn1 N1 2_665 4_666 81.6(3) ?
N1 Mn1 N1 5_556 4_666 92.7(2) ?
N1 Mn1 N1 6_566 . 171.8(3) ?
N1 Mn1 N1 3_565 . 92.7(2) ?
N1 Mn1 N1 2_665 . 92.7(2) ?
N1 Mn1 N1 5_556 . 81.6(3) y
N1 Mn1 N1 4_666 . 93.5(3) ?
O4 S1 O4 . 4_665 180.000(19) ?
O4 S1 O3 . 5 133.7(10) ?
O4 S1 O3 4_665 5 46.3(10) ?
O4 S1 O3 . 2_665 46.3(10) ?
O4 S1 O3 4_665 2_665 133.7(10) ?
O3 S1 O3 5 2_665 156(4) ?
O4 S1 O3 . . 46.3(10) ?
O4 S1 O3 4_665 . 133.7(10) ?
O3 S1 O3 5 . 90(2) ?
O3 S1 O3 2_665 . 77.5(15) ?
O4 S1 O3 . 4_665 133.7(10) ?
O4 S1 O3 4_665 4_665 46.3(10) ?
O3 S1 O3 5 4_665 77.5(15) ?
O3 S1 O3 2_665 4_665 90(2) ?
O3 S1 O3 . 4_665 121(3) ?
O4 S1 O3 . 3_565 46.3(10) ?
O4 S1 O3 4_665 3_565 133.7(10) ?
O3 S1 O3 5 3_565 121(3) ?
O3 S1 O3 2_665 3_565 77.5(15) ?
O3 S1 O3 . 3_565 77.5(15) ?
O3 S1 O3 4_665 3_565 156(4) ?
O4 S1 O3 . 6_565 133.7(10) ?
O4 S1 O3 4_665 6_565 46.3(10) ?
O3 S1 O3 5 6_565 77.5(15) ?
O3 S1 O3 2_665 6_565 121(3) ?
O3 S1 O3 . 6_565 156(4) ?
O3 S1 O3 4_665 6_565 77.5(15) ?
O3 S1 O3 3_565 6_565 90(2) ?
O4 S1 O2 . 2_665 55.7(10) ?
O4 S1 O2 4_665 2_665 124.3(10) ?
O3 S1 O2 5 2_665 97(2) ?
O3 S1 O2 2_665 2_665 62.4(15) ?
O3 S1 O2 . 2_665 30.1(12) ?
O3 S1 O2 4_665 2_665 94(3) ?
O3 S1 O2 3_565 2_665 99.3(13) ?
O3 S1 O2 6_565 2_665 170.3(17) ?
O4 S1 O2 . 5 124.3(10) ?
O4 S1 O2 4_665 5 55.7(10) ?
O3 S1 O2 5 5 62.4(15) ?
O3 S1 O2 2_665 5 97(2) ?
O3 S1 O2 . 5 94(3) ?
O3 S1 O2 4_665 5 30.1(12) ?
O3 S1 O2 3_565 5 170.3(17) ?
O3 S1 O2 6_565 5 99.3(13) ?
O2 S1 O2 2_665 5 71(2) ?
O4 S1 O2 . 6_565 124.3(11) ?
O4 S1 O2 4_665 6_565 55.7(10) ?
O3 S1 O2 5 6_565 30.1(12) ?
O3 S1 O2 2_665 6_565 170.3(18) ?
O3 S1 O2 . 6_565 97(2) ?
O3 S1 O2 4_665 6_565 99.3(13) ?
O3 S1 O2 3_565 6_565 94(3) ?
O3 S1 O2 6_565 6_565 62.4(15) ?
O2 S1 O2 2_665 6_565 116(3) ?
O2 S1 O2 5 6_565 91.3(15) ?
O4 S1 O2 . 3_565 55.7(10) ?
O4 S1 O2 4_665 3_565 124.3(10) ?
O3 S1 O2 5 3_565 170.3(17) ?
O3 S1 O2 2_665 3_565 30.1(12) ?
O3 S1 O2 . 3_565 99.3(13) ?
O3 S1 O2 4_665 3_565 97(2) ?
O3 S1 O2 3_565 3_565 62.4(15) ?
O3 S1 O2 6_565 3_565 94(3) ?
O2 S1 O2 2_665 3_565 91.3(15) ?
O2 S1 O2 5 3_565 116(3) ?
O2 S1 O2 6_565 3_565 147(4) ?
S1 O1 O1 . 6_565 54.1(11) ?
S1 O2 O2 . 6_565 54.5(12) ?
S1 O3 O3 . 2_665 51.2(7) ?
S1 O3 O3 . 3_565 51.2(7) ?
O3 O3 O3 2_665 3_565 60.0000(10) ?
C1 N1 Mn1 . . 107.9(4) ?
C1 N1 H1A . . 110.1 ?
Mn1 N1 H1A . . 110.1 ?
C1 N1 H1B . . 110.1 ?
Mn1 N1 H1B . . 110.1 ?
H1A N1 H1B . . 108.4 ?
N1 C1 C1 . 5_556 108.9(5) ?
N1 C1 H1C . . 109.9 ?
C1 C1 H1C 5_556 . 109.9 ?
N1 C1 H1D . . 109.9 ?
C1 C1 H1D 5_556 . 109.9 ?
H1C C1 H1D . . 108.3 ?
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 N1 6_566 2.125(6) ?
Mn1 N1 3_565 2.125(6) ?
Mn1 N1 2_665 2.125(6) ?
Mn1 N1 5_556 2.125(6) ?
Mn1 N1 4_666 2.125(6) ?
Mn1 N1 . 2.125(6) y
S1 O4 . 1.30(9) ?
S1 O4 4_665 1.30(9) ?
S1 O3 5 1.45(3) ?
S1 O3 2_665 1.45(3) ?
S1 O3 . 1.45(3) ?
S1 O3 4_665 1.45(3) ?
S1 O3 3_565 1.45(3) ?
S1 O3 6_565 1.45(3) ?
S1 O2 2_665 1.48(3) ?
S1 O2 5 1.48(3) ?
S1 O2 6_565 1.48(3) ?
S1 O2 3_565 1.48(3) ?
O1 O1 6_565 1.74(5) ?
O2 O2 6_565 1.72(6) ?
O3 O3 2_665 1.82(4) ?
O3 O3 3_565 1.82(4) ?
N1 C1 . 1.471(9) ?
N1 H1A . 0.9000 ?
N1 H1B . 0.9000 ?
C1 C1 5_556 1.496(15) ?
C1 H1C . 0.9700 ?
C1 H1D . 0.9700 ?
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
_geom_hbond_publ_flag
N1 H1A O1 9_656 0.90 2.28 3.16(3) 166 yes
N1 H1A O1 12_656 0.90 2.43 3.15(3) 138 yes
N1 H1B O1 3_566 0.90 2.17 3.06(2) 170 yes
N1 H1B O2 3_566 0.90 2.11 3.00(2) 167 yes
N1 H1A O2 7_666 0.90 2.14 2.95(5) 148 yes
N1 H1A O3 9_656 0.90 1.92 2.80(3) 166 yes
N1 H1B O3 3_566 0.90 2.15 2.96(3) 150 yes
N1 H1B O3 2_666 0.90 2.36 3.18(3) 152 yes
N1 H1B O4 1_556 0.90 2.15 2.94(7) 146 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O4 S1 O1 O1 . 6_565 -129(2)
O4 S1 O1 O1 4_665 6_565 51(2)
O3 S1 O1 O1 5 6_565 65.8(19)
O3 S1 O1 O1 2_665 6_565 -140(3)
O3 S1 O1 O1 . 6_565 179(3)
O3 S1 O1 O1 4_665 6_565 100(3)
O3 S1 O1 O1 3_565 6_565 -77(2)
O3 S1 O1 O1 6_565 6_565 0(2)
O2 S1 O1 O1 2_665 6_565 171(2)
O2 S1 O1 O1 5 6_565 112.2(18)
O2 S1 O1 O1 6_565 6_565 34.5(19)
O2 S1 O1 O1 3_565 6_565 -108(3)
O4 S1 O2 O2 . 6_565 163(4)
O4 S1 O2 O2 4_665 6_565 -17(4)
O3 S1 O2 O2 5 6_565 20(2)
O3 S1 O2 O2 2_665 6_565 179(4)
O3 S1 O2 O2 . 6_565 109(4)
O3 S1 O2 O2 4_665 6_565 -0E1(2)
O3 S1 O2 O2 3_565 6_565 -136(5)
O3 S1 O2 O2 6_565 6_565 -58(2)
O2 S1 O2 O2 2_665 6_565 117(4)
O2 S1 O2 O2 5 6_565 61(2)
O2 S1 O2 O2 3_565 6_565 -151(4)
O4 S1 O3 O3 . 2_665 39.9(5)
O4 S1 O3 O3 4_665 2_665 -140.1(5)
O3 S1 O3 O3 5 2_665 -159(3)
O3 S1 O3 O3 4_665 2_665 -83(2)
O3 S1 O3 O3 3_565 2_665 79.8(10)
O3 S1 O3 O3 6_565 2_665 141.8(18)
O2 S1 O3 O3 2_665 2_665 -55(3)
O2 S1 O3 O3 5 2_665 -96(3)
O2 S1 O3 O3 6_565 2_665 172(3)
O2 S1 O3 O3 3_565 2_665 20.9(16)
O4 S1 O3 O3 . 3_565 -39.9(5)
O4 S1 O3 O3 4_665 3_565 140.1(5)
O3 S1 O3 O3 5 3_565 122(4)
O3 S1 O3 O3 2_665 3_565 -79.8(10)
O3 S1 O3 O3 4_665 3_565 -163(2)
O3 S1 O3 O3 6_565 3_565 62(2)
O2 S1 O3 O3 2_665 3_565 -135(3)
O2 S1 O3 O3 5 3_565 -176(3)
O2 S1 O3 O3 6_565 3_565 92(3)
O2 S1 O3 O3 3_565 3_565 -58.9(16)
N1 Mn1 N1 C1 6_566 . 32.2(4)
N1 Mn1 N1 C1 3_565 . 78.5(5)
N1 Mn1 N1 C1 2_665 . 171.4(4)
N1 Mn1 N1 C1 5_556 . -14.7(3)
N1 Mn1 N1 C1 4_666 . -106.9(4)
Mn1 N1 C1 C1 . 5_556 41.5(7)