#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/28/2012892.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_2012892
loop_
_publ_author_name
'Freire, Eleonora'
'Baggio, Sergio'
'Muñoz, Juan Carlos'
'Baggio, Ricardo'
_publ_section_title
;Bis(1,10-phenanthroline)(thiosulfato)manganese(II) methanol solvate and
 catena-poly[[diaqua(2,9-dimethyl-1,10-phenanthroline)manganese(II)]-μ-thiosulfato]
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m455
_journal_page_last               m458
_journal_paper_doi               10.1107/S0108270102012404
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Mn (S2 O3) (C12 H8 N2)2 ], C H4 O1'
_chemical_formula_moiety         'Mn C24 H16 O3 N4 S2, C H4 O'
_chemical_formula_sum            'C25 H20 Mn N4 O4 S2'
_chemical_formula_weight         559.51
_chemical_name_systematic
;
bis(1,10-phenanthroline-κ²N,N')(thiosulfato-κ²O:S)manganese(II)
methanol solvate
;
_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                 109.180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9240(10)
_cell_length_b                   11.4120(10)
_cell_length_c                   17.0840(10)
_cell_measurement_reflns_used    84
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      1.73
_cell_volume                     2379.8(3)
_computing_cell_refinement       SMART-NT
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        'SAINT-NT (Bruker, 2000)'
_computing_molecular_graphics    'XP in SHELXTL-PC (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11546
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0728P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.119
_refine_ls_wR_factor_ref         0.125
_reflns_number_gt                3942
_reflns_number_total             5302
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob1070.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (21 time).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2379.9(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2012892
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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Mn 0.90273(3) 0.82197(3) 0.13372(2) 0.04316(14) Uani d . 1 . . Mn
S1 0.86129(5) 1.07293(6) 0.09745(4) 0.04631(18) Uani d . 1 . . S
S2 0.87452(6) 1.01075(7) 0.21088(4) 0.0564(2) Uani d . 1 . . S
O1 0.90030(15) 0.97408(16) 0.05753(10) 0.0523(4) Uani d . 1 . . O
O2 0.74816(15) 1.0993(2) 0.05129(11) 0.0676(6) Uani d . 1 . . O
O3 0.93141(18) 1.17420(17) 0.10435(15) 0.0733(6) Uani d . 1 . . O
N1A 1.08332(16) 0.79457(18) 0.16145(12) 0.0420(5) Uani d . 1 . . N
N2A 0.95801(16) 0.70514(18) 0.24681(12) 0.0433(5) Uani d . 1 . . N
C1A 1.1435(2) 0.8346(2) 0.11749(16) 0.0513(6) Uani d . 1 . . C
H1A 1.1099 0.8810 0.0713 0.062 Uiso calc R 1 . . H
C2A 1.2546(2) 0.8102(2) 0.13759(18) 0.0567(7) Uani d . 1 . . C
H2A 1.2934 0.8365 0.1038 0.068 Uiso calc R 1 . . H
C3A 1.3057(2) 0.7473(2) 0.20715(18) 0.0548(7) Uani d . 1 . . C
H3A 1.3804 0.7320 0.2221 0.066 Uiso calc R 1 . . H
C4A 1.2458(2) 0.7059(2) 0.25610(15) 0.0436(6) Uani d . 1 . . C
C5A 1.2943(2) 0.6408(2) 0.33134(16) 0.0516(6) Uani d . 1 . . C
H5A 1.3692 0.6258 0.3495 0.062 Uiso calc R 1 . . H
C6A 1.2330(2) 0.6013(2) 0.37586(16) 0.0506(6) Uani d . 1 . . C
H6A 1.2664 0.5612 0.4251 0.061 Uiso calc R 1 . . H
C7A 1.1170(2) 0.6202(2) 0.34879(14) 0.0444(6) Uani d . 1 . . C
C8A 1.0489(2) 0.5779(2) 0.39244(16) 0.0536(7) Uani d . 1 . . C
H8A 1.0787 0.5353 0.4411 0.064 Uiso calc R 1 . . H
C9A 0.9402(2) 0.5999(3) 0.36308(17) 0.0567(7) Uani d . 1 . . C
H9A 0.8945 0.5728 0.3914 0.068 Uiso calc R 1 . . H
C10A 0.8975(2) 0.6633(2) 0.29032(17) 0.0516(6) Uani d . 1 . . C
H10A 0.8224 0.6774 0.2708 0.062 Uiso calc R 1 . . H
C11A 1.06693(19) 0.68349(19) 0.27575(14) 0.0384(5) Uani d . 1 . . C
C12A 1.13361(18) 0.7289(2) 0.22955(14) 0.0383(5) Uani d . 1 . . C
N1B 0.86862(17) 0.69382(18) 0.02409(13) 0.0449(5) Uani d . 1 . . N
N2B 0.72489(17) 0.7690(2) 0.09821(13) 0.0494(5) Uani d . 1 . . N
C1B 0.9376(2) 0.6589(2) -0.01391(17) 0.0552(7) Uani d . 1 . . C
H1B 1.0105 0.6822 0.0079 0.066 Uiso calc R 1 . . H
C2B 0.9068(3) 0.5891(3) -0.08495(18) 0.0658(8) Uani d . 1 . . C
H2B 0.9581 0.5667 -0.1095 0.079 Uiso calc R 1 . . H
C3B 0.8010(3) 0.5544(2) -0.11757(18) 0.0645(8) Uani d . 1 . . C
H3B 0.7791 0.5083 -0.1651 0.077 Uiso calc R 1 . . H
C4B 0.7246(2) 0.5881(2) -0.07961(16) 0.0537(7) Uani d . 1 . . C
C5B 0.6121(3) 0.5572(3) -0.11106(19) 0.0676(9) Uani d . 1 . . C
H5B 0.5870 0.5109 -0.1584 0.081 Uiso calc R 1 . . H
C6B 0.5417(3) 0.5933(3) -0.0741(2) 0.0689(9) Uani d . 1 . . C
H6B 0.4685 0.5714 -0.0960 0.083 Uiso calc R 1 . . H
C7B 0.5760(2) 0.6645(2) -0.00190(18) 0.0569(7) Uani d . 1 . . C
C8B 0.5046(2) 0.7068(3) 0.0396(2) 0.0725(9) Uani d . 1 . . C
H8B 0.4306 0.6871 0.0202 0.087 Uiso calc R 1 . . H
C9B 0.5445(3) 0.7763(3) 0.1079(2) 0.0718(9) Uani d . 1 . . C
H9B 0.4984 0.8033 0.1359 0.086 Uiso calc R 1 . . H
C10B 0.6552(2) 0.8064(3) 0.1352(2) 0.0622(8) Uani d . 1 . . C
H10B 0.6815 0.8548 0.1813 0.075 Uiso calc R 1 . . H
C11B 0.6865(2) 0.6980(2) 0.03062(16) 0.0471(6) Uani d . 1 . . C
C12B 0.7623(2) 0.6587(2) -0.00875(15) 0.0453(6) Uani d . 1 . . C
O1XA 0.8929(4) 0.3714(5) 0.1854(3) 0.1215(14) Uani d PD 0.626(4) . . O
O1XB 0.7836(7) 0.3782(7) 0.0638(5) 0.1215(14) Uani d PD 0.374(4) . . O
C1X 0.8014(4) 0.4158(4) 0.1372(3) 0.1102(15) Uani d D 1 . . C
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
_geom_angle_publ_flag
O1 Mn N1A 92.71(7) y
O1 Mn N2B 103.93(8) y
N1A Mn N2B 156.20(8) y
O1 Mn N2A 157.67(7) y
N1A Mn N2A 73.92(7) y
N2B Mn N2A 94.57(8) y
O1 Mn N1B 93.40(7) y
N1A Mn N1B 89.49(7) y
N2B Mn N1B 72.88(8) y
N2A Mn N1B 104.06(8) y
O1 Mn S2 70.44(5) y
N1A Mn S2 108.42(5) y
N2B Mn S2 93.31(6) y
N2A Mn S2 96.45(5) y
N1B Mn S2 155.95(5) y
O2 S1 O3 111.79(14) y
O2 S1 O1 109.98(12) y
O3 S1 O1 110.15(12) y
O2 S1 S2 110.39(8) y
O3 S1 S2 110.43(10) y
O1 S1 S2 103.82(8) y
S1 S2 Mn 77.72(3) ?
S1 O1 Mn 105.81(9) ?
C1A N1A C12A 118.1(2) ?
C1A N1A Mn 126.44(17) ?
C12A N1A Mn 115.45(14) ?
C10A N2A C11A 117.5(2) ?
C10A N2A Mn 127.54(17) ?
C11A N2A Mn 114.75(15) ?
N1A C1A C2A 122.7(2) ?
N1A C1A H1A 118.6 ?
C2A C1A H1A 118.6 ?
C3A C2A C1A 119.2(2) ?
C3A C2A H2A 120.4 ?
C1A C2A H2A 120.4 ?
C2A C3A C4A 119.8(2) ?
C2A C3A H3A 120.1 ?
C4A C3A H3A 120.1 ?
C12A C4A C3A 117.6(2) ?
C12A C4A C5A 119.3(2) ?
C3A C4A C5A 123.1(2) ?
C6A C5A C4A 120.9(2) ?
C6A C5A H5A 119.5 ?
C4A C5A H5A 119.5 ?
C5A C6A C7A 121.1(2) ?
C5A C6A H6A 119.5 ?
C7A C6A H6A 119.5 ?
C11A C7A C8A 117.4(2) ?
C11A C7A C6A 119.5(2) ?
C8A C7A C6A 123.1(2) ?
C9A C8A C7A 119.5(2) ?
C9A C8A H8A 120.2 ?
C7A C8A H8A 120.2 ?
C8A C9A C10A 119.3(2) ?
C8A C9A H9A 120.4 ?
C10A C9A H9A 120.4 ?
N2A C10A C9A 123.6(3) ?
N2A C10A H10A 118.2 ?
C9A C10A H10A 118.2 ?
N2A C11A C7A 122.7(2) ?
N2A C11A C12A 118.1(2) ?
C7A C11A C12A 119.2(2) ?
N1A C12A C4A 122.5(2) ?
N1A C12A C11A 117.6(2) ?
C4A C12A C11A 119.9(2) ?
C1B N1B C12B 117.4(2) ?
C1B N1B Mn 127.57(18) ?
C12B N1B Mn 114.79(16) ?
C10B N2B C11B 118.6(2) ?
C10B N2B Mn 125.12(19) ?
C11B N2B Mn 116.20(16) ?
N1B C1B C2B 123.5(3) ?
N1B C1B H1B 118.3 ?
C2B C1B H1B 118.3 ?
C3B C2B C1B 119.1(3) ?
C3B C2B H2B 120.5 ?
C1B C2B H2B 120.5 ?
C2B C3B C4B 119.9(3) ?
C2B C3B H3B 120.1 ?
C4B C3B H3B 120.1 ?
C3B C4B C12B 117.4(3) ?
C3B C4B C5B 123.1(3) ?
C12B C4B C5B 119.4(3) ?
C6B C5B C4B 121.2(3) ?
C6B C5B H5B 119.4 ?
C4B C5B H5B 119.4 ?
C5B C6B C7B 121.4(3) ?
C5B C6B H6B 119.3 ?
C7B C6B H6B 119.3 ?
C11B C7B C8B 116.9(3) ?
C11B C7B C6B 119.1(3) ?
C8B C7B C6B 124.0(3) ?
C9B C8B C7B 120.0(3) ?
C9B C8B H8B 120.0 ?
C7B C8B H8B 120.0 ?
C8B C9B C10B 119.1(3) ?
C8B C9B H9B 120.4 ?
C10B C9B H9B 120.4 ?
N2B C10B C9B 122.9(3) ?
N2B C10B H10B 118.5 ?
C9B C10B H10B 118.5 ?
N2B C11B C7B 122.4(3) ?
N2B C11B C12B 118.0(2) ?
C7B C11B C12B 119.5(3) ?
N1B C12B C4B 122.8(3) ?
N1B C12B C11B 117.9(2) ?
C4B C12B C11B 119.3(2) ?
O1XB C1X O1XA 108.9(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
Mn O1 . 2.1637(18) y
Mn N1A . 2.246(2) y
Mn N2B . 2.258(2) y
Mn N2A . 2.261(2) y
Mn N1B . 2.302(2) y
Mn S2 . 2.6131(8) y
S1 O2 . 1.4466(18) y
S1 O3 . 1.449(2) y
S1 O1 . 1.4893(18) y
S1 S2 . 2.0175(9) y
N1A C1A . 1.327(3) ?
N1A C12A . 1.356(3) ?
N2A C10A . 1.332(3) ?
N2A C11A . 1.353(3) ?
C1A C2A . 1.391(4) ?
C1A H1A . 0.9300 ?
C2A C3A . 1.359(4) ?
C2A H2A . 0.9300 ?
C3A C4A . 1.395(4) ?
C3A H3A . 0.9300 ?
C4A C12A . 1.395(3) ?
C4A C5A . 1.438(4) ?
C5A C6A . 1.344(4) ?
C5A H5A . 0.9300 ?
C6A C7A . 1.432(3) ?
C6A H6A . 0.9300 ?
C7A C11A . 1.403(3) ?
C7A C8A . 1.412(4) ?
C8A C9A . 1.351(4) ?
C8A H8A . 0.9300 ?
C9A C10A . 1.387(4) ?
C9A H9A . 0.9300 ?
C10A H10A . 0.9300 ?
C11A C12A . 1.443(3) ?
N1B C1B . 1.325(3) ?
N1B C12B . 1.363(3) ?
N2B C10B . 1.329(3) ?
N2B C11B . 1.364(3) ?
C1B C2B . 1.396(4) ?
C1B H1B . 0.9300 ?
C2B C3B . 1.355(4) ?
C2B H2B . 0.9300 ?
C3B C4B . 1.401(4) ?
C3B H3B . 0.9300 ?
C4B C12B . 1.401(4) ?
C4B C5B . 1.420(4) ?
C5B C6B . 1.332(4) ?
C5B H5B . 0.9300 ?
C6B C7B . 1.420(4) ?
C6B H6B . 0.9300 ?
C7B C11B . 1.405(4) ?
C7B C8B . 1.421(4) ?
C8B C9B . 1.364(5) ?
C8B H8B . 0.9300 ?
C9B C10B . 1.395(4) ?
C9B H9B . 0.9300 ?
C10B H10B . 0.9300 ?
C11B C12B . 1.430(4) ?
O1XA C1X . 1.302(5) ?
O1XB C1X . 1.273(5) ?
