#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/16/2211626.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_2211626
loop_
_publ_author_name
'Wang, Xiao-Xia'
'Sun, Feng'
'Zhan, Qing-Guang'
'Wu, Jian-Zhong'
_publ_section_title
;Tetraaqua(1,10-phenanthroline-5,6-dione-κ²N,N')manganese(II)
 sulfate dihydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3380
_journal_page_last               m3382
_journal_paper_doi               10.1107/S160053680604774X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C12 H14 Mn N2 O6, O4 S, H4 O2'
_chemical_formula_sum            'C12 H18 Mn N2 O12 S'
_chemical_formula_weight         469.28
_chemical_name_systematic
;
Tetraaqua-(1,10-phenanthroline-5,6-dione-N,N')manganese(II) sulfate
hydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 97.317(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6237(4)
_cell_length_b                   13.9117(6)
_cell_length_c                   13.8744(6)
_cell_measurement_reflns_used    3587
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.59
_cell_volume                     1842.41(14)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10376
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2205
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0445P)²+3.5719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                1906
_reflns_number_total             2205
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj2162.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2211626
_cod_database_fobs_code          2211626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
O O8 0.2157(8) 0.0851(6) 0.3649(11) 0.126(10) Uani d PD 0.35(2) A 1
O O8' 0.2004(12) 0.0320(11) 0.3953(5) 0.084(8) Uani d P 0.331(14) . 2
O O8'' 0.261(3) 0.1095(8) 0.3231(11) 0.181(11) Uani d P 0.319(15) A 3
C C1 0.1513(3) 0.69232(19) 0.2146(2) 0.0415(6) Uani d . 1 . .
H H1 0.2263 0.7225 0.2515 0.050 Uiso calc R 1 . .
C C2 0.0481(3) 0.7495(2) 0.1646(2) 0.0485(7) Uani d . 1 . .
H H2 0.0547 0.8162 0.1669 0.058 Uiso calc R 1 . .
C C3 -0.0641(3) 0.7050(2) 0.1116(2) 0.0443(6) Uani d . 1 . .
H H3 -0.1350 0.7413 0.0772 0.053 Uiso calc R 1 . .
C C4 -0.0705(2) 0.60576(18) 0.10989(16) 0.0328(5) Uani d . 1 . .
C C5 0.0386(2) 0.55302(16) 0.16119(15) 0.0270(4) Uani d . 1 . .
C C6 -0.1905(3) 0.5552(2) 0.05441(17) 0.0391(6) Uani d . 1 . .
Mn Mn 0.31165(5) 0.5000 0.29690(4) 0.03150(18) Uani d S 1 . .
N N 0.1488(2) 0.59675(14) 0.21260(14) 0.0312(4) Uani d . 1 . .
O O1 -0.2848(2) 0.59738(19) 0.00612(16) 0.0621(6) Uani d . 1 . .
O O2 0.4378(3) 0.5000 0.17485(18) 0.0450(7) Uani d S 1 . .
H H21 0.5285 0.5000 0.1820 0.054 Uiso d SR 1 . .
H H22 0.4095 0.5000 0.1153 0.054 Uiso d SR 1 . .
O O3 0.1880(3) 0.5000 0.4152(2) 0.0668(10) Uani d S 1 . .
H H31 0.0915 0.5000 0.4069 0.080 Uiso d SR 1 . .
H H32 0.2126 0.5000 0.4776 0.080 Uiso d SR 1 . .
O O4 0.4434(2) 0.61274(16) 0.35852(17) 0.0592(6) Uani d . 1 . .
H H41 0.4188 0.6661 0.3883 0.071 Uiso d R 1 . .
H H42 0.5197 0.6022 0.3749 0.071 Uiso d R 1 . .
S S 0.27286(9) 0.0000 0.32154(6) 0.0395(2) Uani d SD 1 . .
O O6 0.4203(3) 0.0000 0.3394(3) 0.111(2) Uani d SD 1 A .
O O7 0.2144(3) 0.0000 0.22185(19) 0.0980(18) Uani d SD 1 A .
O O5 0.3641(3) 0.77055(19) 0.4503(2) 0.0797(8) Uani d . 1 . .
H H51 0.3290 0.8285 0.4209 0.096 Uiso d R 1 . .
H H52 0.4510 0.7977 0.4760 0.096 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'
S S 0.1246 0.1234 '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
O8' O8' S 6 . 71.3(6)
N C1 C2 . . 123.6(3)
N C1 H1 . . 118.2
C2 C1 H1 . . 118.2
C3 C2 C1 . . 118.3(3)
C3 C2 H2 . . 120.9
C1 C2 H2 . . 120.9
C2 C3 C4 . . 119.2(2)
C2 C3 H3 . . 120.4
C4 C3 H3 . . 120.4
C3 C4 C5 . . 119.1(2)
C3 C4 C6 . . 120.8(2)
C5 C4 C6 . . 120.0(2)
N C5 C4 . . 121.5(2)
N C5 C5 . 6_565 116.87(13)
C4 C5 C5 . 6_565 121.64(14)
O1 C6 C4 . . 122.6(3)
O1 C6 C6 . 6_565 118.99(18)
C4 C6 C6 . 6_565 118.32(14)
O4 Mn O4 . 6_565 95.04(13)
O4 Mn O3 . . 93.02(8)
O4 Mn O3 6_565 . 93.02(8)
O4 Mn O2 . . 87.15(8)
O4 Mn O2 6_565 . 87.15(8)
O3 Mn O2 . . 179.73(10)
O4 Mn N . 6_565 168.55(8)
O4 Mn N 6_565 6_565 96.13(8)
O3 Mn N . 6_565 88.88(8)
O2 Mn N . 6_565 90.90(7)
O4 Mn N . . 96.13(8)
O4 Mn N 6_565 . 168.55(8)
O3 Mn N . . 88.88(8)
O2 Mn N . . 90.90(7)
N Mn N 6_565 . 72.61(10)
C1 N C5 . . 118.3(2)
C1 N Mn . . 124.89(17)
C5 N Mn . . 116.76(15)
Mn O2 H21 . . 123.9
Mn O2 H22 . . 128.1
H21 O2 H22 . . 108.0
Mn O3 H31 . . 123.6
Mn O3 H32 . . 130.9
H31 O3 H32 . . 105.4
Mn O4 H41 . . 128.1
Mn O4 H42 . . 119.0
H41 O4 H42 . . 109.0
O8' S O6 . . 117.5(5)
O8' S O6 6 . 117.5(5)
O8' S O7 . . 123.0(4)
O8' S O7 6 . 123.0(4)
O6 S O7 . . 115.7(2)
O8' S O8 6 . 72.8(10)
O6 S O8 . . 110.5(4)
O7 S O8 . . 106.0(6)
O8' S O8 . 6 72.8(10)
O6 S O8 . 6 110.5(3)
O7 S O8 . 6 106.0(6)
O8 S O8 . 6 107.6(10)
O8' S O8'' . 6 105.3(10)
O8' S O8'' 6 6 67.9(14)
O6 S O8'' . 6 94.1(11)
O7 S O8'' . 6 89.6(4)
O8 S O8'' . 6 140.0(13)
O8' S O8'' . . 67.9(14)
O8' S O8'' 6 . 105.3(10)
O6 S O8'' . . 94.1(11)
O7 S O8'' . . 89.6(4)
O8 S O8'' 6 . 140.0(13)
O8'' S O8'' 6 . 171(2)
H51 O5 H52 . . 94.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O8 S . 1.467(3)
O8' O8' 6 0.89(3)
O8' S . 1.383(8)
O8'' S . 1.528(11)
C1 N . 1.330(3)
C1 C2 . 1.387(4)
C1 H1 . 0.9300
C2 C3 . 1.374(4)
C2 H2 . 0.9300
C3 C4 . 1.382(4)
C3 H3 . 0.9300
C4 C5 . 1.399(3)
C4 C6 . 1.481(3)
C5 N . 1.346(3)
C5 C5 6_565 1.475(4)
C6 O1 . 1.209(3)
C6 C6 6_565 1.537(6)
Mn O4 . 2.127(2)
Mn O4 6_565 2.127(2)
Mn O3 . 2.146(3)
Mn O2 . 2.206(2)
Mn N 6_565 2.273(2)
Mn N . 2.273(2)
O2 H21 . 0.8662
O2 H22 . 0.8361
O3 H31 . 0.9211
O3 H32 . 0.8680
O4 H41 . 0.8955
O4 H42 . 0.7549
S O8' 6 1.383(8)
S O6 . 1.409(3)
S O7 . 1.425(3)
S O8 6 1.467(3)
S O8'' 6 1.528(11)
O5 H51 . 0.9464
O5 H52 . 0.9460
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
O4 H41 O5 . 0.90 1.80 2.697(3) 177.7
O2 H21 O7 3 0.87 1.80 2.659(4) 168.8
O3 H31 O6 3_455 0.92 1.79 2.656(4) 155.8
O3 H32 O8' 4_556 0.87 1.91 2.747(8) 162.7
O3 H32 O8' 7_556 0.87 1.91 2.747(8) 162.7
O4 H42 O8 3 0.75 1.92 2.639(8) 158.1
O4 H42 O8' 3 0.75 1.98 2.705(9) 160.1
O5 H51 O8'' 6_565 0.95 1.67 2.537(13) 150.7
O5 H51 O8 6_565 0.95 1.74 2.654(8) 161.9
O5 H52 O5 2_656 0.95 1.97 2.798(5) 144.6
