#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/84/2208452.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_2208452
loop_
_publ_author_name
'Kai-Long Zhong'
'Yi-Min Zhu'
'Wen-Jie Lu'
_publ_section_title
;Bis(1,10-phenanthroline-κ²N,N')(sulfato-κ²O,O')cobalt(II)
 1,2-ethanediol solvate
;
_journal_coeditor_code           WN6409
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m631
_journal_page_last               m633
_journal_paper_doi               10.1107/S1600536806002315
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co (S O4) (C12 H8 N2)2], C2 H6 O2'
_chemical_formula_moiety         'C24 H16 Co N4 O4 S, C2 H6 O2'
_chemical_formula_sum            'C26 H22 Co N4 O6 S'
_chemical_formula_weight         577.47
_chemical_name_systematic
;
Bis(1,10-phenanthroline-κ²N,N')(sulfato-κ²O,O')cobalt(II)
1,2-ethenediol solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 119.052(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.500(2)
_cell_length_b                   11.8612(12)
_cell_length_c                   12.8230(14)
_cell_measurement_reflns_used    4704
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      3.17
_cell_volume                     2459.7(5)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8438
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.7261
_exptl_absorpt_correction_T_min  0.6302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3065
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0359
_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)+(0.0624P)²+0.6033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                2656
_reflns_number_total             3065
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wn6409.cif
_cod_data_source_block           I
_cod_original_cell_volume        2459.8(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2208452
_cod_database_fobs_code          2208452
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Co Co1 0.5000 0.69577(3) 0.2500 0.03100(12) Uani d S 1 . .
S S1 0.5000 0.46760(5) 0.2500 0.03093(15) Uani d S 1 . .
O O1 0.55314(8) 0.54535(12) 0.34866(12) 0.0482(3) Uani d . 1 . .
O O2 0.55007(10) 0.39789(14) 0.21717(17) 0.0601(4) Uani d . 1 . .
N N1 0.59299(9) 0.80396(12) 0.37837(13) 0.0349(3) Uani d . 1 . .
N N2 0.58130(9) 0.71550(12) 0.17796(13) 0.0343(3) Uani d . 1 . .
C C1 0.60063(13) 0.84350(17) 0.48050(17) 0.0451(4) Uani d . 1 . .
H H1A 0.5584 0.8293 0.4984 0.054 Uiso calc R 1 . .
C C2 0.66924(15) 0.90543(18) 0.56193(19) 0.0522(5) Uani d . 1 . .
H H2B 0.6723 0.9311 0.6325 0.063 Uiso calc R 1 . .
C C3 0.73142(14) 0.92798(16) 0.53748(18) 0.0474(5) Uani d . 1 . .
H H3A 0.7771 0.9695 0.5910 0.057 Uiso calc R 1 . .
C C4 0.72630(11) 0.88829(15) 0.43090(16) 0.0381(4) Uani d . 1 . .
C C5 0.78880(12) 0.90643(17) 0.39792(19) 0.0464(5) Uani d . 1 . .
H H5A 0.8357 0.9475 0.4486 0.056 Uiso calc R 1 . .
C C6 0.78163(11) 0.86568(18) 0.29550(18) 0.0473(5) Uani d . 1 . .
H H6A 0.8230 0.8801 0.2759 0.057 Uiso calc R 1 . .
C C7 0.71101(11) 0.80035(15) 0.21625(17) 0.0386(4) Uani d . 1 . .
C C8 0.70114(12) 0.7523(2) 0.11033(19) 0.0509(5) Uani d . 1 . .
H H8A 0.7412 0.7636 0.0874 0.061 Uiso calc R 1 . .
C C9 0.63306(14) 0.68935(19) 0.04106(19) 0.0502(5) Uani d . 1 . .
H H9A 0.6256 0.6585 -0.0301 0.060 Uiso calc R 1 . .
C C10 0.57440(12) 0.67154(17) 0.07811(17) 0.0422(4) Uani d . 1 . .
H H10A 0.5286 0.6271 0.0310 0.051 Uiso calc R 1 . .
C C11 0.65563(10) 0.82575(14) 0.35436(15) 0.0317(3) Uani d . 1 . .
C C12 0.64855(10) 0.77977(14) 0.24615(15) 0.0313(3) Uani d . 1 . .
C C13 0.5282(3) 0.0910(3) 0.2291(5) 0.1123(14) Uani d D 1 . 1
H H13A 0.5808 0.0716 0.2975 0.135 Uiso calc R 1 . 1
H H13B 0.5130 0.0272 0.1752 0.135 Uiso calc R 1 . 1
O O3 0.5449(14) 0.1735(6) 0.1748(18) 0.090(6) Uani d PD 0.30 A 1
H H3 0.5601 0.2292 0.2180 0.135 Uiso calc PR 0.30 A 1
O O3" 0.5836(6) 0.1698(6) 0.2460(15) 0.078(3) Uani d PD 0.40 B 2
O O3' 0.563(2) 0.1794(8) 0.208(4) 0.127(12) Uani d PD 0.30 C 2
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'
Co Co 0.3494 0.9721 '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
N2 Co1 N2 2_655 . 167.36(8) ?
N2 Co1 O1 2_655 2_655 97.49(6) ?
N2 Co1 O1 . 2_655 93.09(6) ?
N2 Co1 O1 2_655 . 93.09(6) ?
N2 Co1 O1 . . 97.49(6) ?
O1 Co1 O1 2_655 . 66.32(7) yes
N2 Co1 N1 2_655 . 94.24(6) ?
N2 Co1 N1 . . 78.10(6) yes
O1 Co1 N1 2_655 . 157.94(5) ?
O1 Co1 N1 . . 94.52(5) ?
N2 Co1 N1 2_655 2_655 78.10(6) ?
N2 Co1 N1 . 2_655 94.24(6) ?
O1 Co1 N1 2_655 2_655 94.52(5) ?
O1 Co1 N1 . 2_655 157.94(6) ?
N1 Co1 N1 . 2_655 106.18(8) ?
N2 Co1 S1 2_655 . 96.32(4) ?
N2 Co1 S1 . . 96.32(4) ?
O1 Co1 S1 2_655 . 33.16(3) ?
O1 Co1 S1 . . 33.16(3) ?
N1 Co1 S1 . . 126.91(4) ?
N1 Co1 S1 2_655 . 126.91(4) ?
O2 S1 O2 2_655 . 110.38(14) yes
O2 S1 O1 2_655 . 111.02(10) ?
O2 S1 O1 . . 110.46(9) ?
O2 S1 O1 2_655 2_655 110.46(9) ?
O2 S1 O1 . 2_655 111.03(10) ?
O1 S1 O1 . 2_655 103.31(11) yes
O2 S1 Co1 2_655 . 124.81(7) ?
O2 S1 Co1 . . 124.81(7) ?
O1 S1 Co1 . . 51.66(5) ?
O1 S1 Co1 2_655 . 51.66(5) ?
S1 O1 Co1 . . 95.18(6) ?
C1 N1 C11 . . 117.39(16) ?
C1 N1 Co1 . . 129.06(13) ?
C11 N1 Co1 . . 113.28(11) ?
C10 N2 C12 . . 118.07(15) ?
C10 N2 Co1 . . 128.15(12) ?
C12 N2 Co1 . . 113.77(11) ?
N1 C1 C2 . . 122.94(18) ?
N1 C1 H1A . . 118.5 ?
C2 C1 H1A . . 118.5 ?
C3 C2 C1 . . 119.66(19) ?
C3 C2 H2B . . 120.2 ?
C1 C2 H2B . . 120.2 ?
C2 C3 C4 . . 119.62(18) ?
C2 C3 H3A . . 120.2 ?
C4 C3 H3A . . 120.2 ?
C3 C4 C11 . . 117.17(18) ?
C3 C4 C5 . . 123.80(17) ?
C11 C4 C5 . . 119.03(17) ?
C6 C5 C4 . . 121.70(17) ?
C6 C5 H5A . . 119.2 ?
C4 C5 H5A . . 119.2 ?
C5 C6 C7 . . 120.74(18) ?
C5 C6 H6A . . 119.6 ?
C7 C6 H6A . . 119.6 ?
C8 C7 C12 . . 117.19(16) ?
C8 C7 C6 . . 123.55(17) ?
C12 C7 C6 . . 119.24(18) ?
C9 C8 C7 . . 120.03(17) ?
C9 C8 H8A . . 120.0 ?
C7 C8 H8A . . 120.0 ?
C8 C9 C10 . . 119.18(19) ?
C8 C9 H9A . . 120.4 ?
C10 C9 H9A . . 120.4 ?
N2 C10 C9 . . 122.77(18) ?
N2 C10 H10A . . 118.6 ?
C9 C10 H10A . . 118.6 ?
N1 C11 C4 . . 123.21(16) ?
N1 C11 C12 . . 117.28(15) ?
C4 C11 C12 . . 119.50(16) ?
N2 C12 C7 . . 122.74(16) ?
N2 C12 C11 . . 117.47(14) ?
C7 C12 C11 . . 119.77(15) ?
O3 C13 C13 . 2_655 128.1(6) yes
O3 C13 H13A . . 105.3 ?
C13 C13 H13A 2_655 . 105.3 ?
O3 C13 H13B . . 105.3 ?
C13 C13 H13B 2_655 . 105.3 ?
H13A C13 H13B . . 106.0 ?
C13 O3 H3 . . 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
Co1 N2 2_655 2.1261(15) ?
Co1 N2 . 2.1261(15) yes
Co1 O1 2_655 2.1313(14) ?
Co1 O1 . 2.1313(14) yes
Co1 N1 . 2.1368(15) yes
Co1 N1 2_655 2.1368(14) ?
Co1 S1 . 2.7064(7) ?
S1 O2 2_655 1.4483(14) ?
S1 O2 . 1.4483(14) yes
S1 O1 . 1.4865(14) yes
S1 O1 2_655 1.4865(13) ?
N1 C1 . 1.332(2) ?
N1 C11 . 1.361(2) ?
N2 C10 . 1.330(2) ?
N2 C12 . 1.355(2) ?
C1 C2 . 1.398(3) ?
C1 H1A . 0.930 ?
C2 C3 . 1.358(3) ?
C2 H2B . 0.930 ?
C3 C4 . 1.405(3) ?
C3 H3A . 0.930 ?
C4 C11 . 1.406(2) ?
C4 C5 . 1.427(3) ?
C5 C6 . 1.344(3) ?
C5 H5A . 0.930 ?
C6 C7 . 1.432(3) ?
C6 H6A . 0.930 ?
C7 C8 . 1.400(3) ?
C7 C12 . 1.404(2) ?
C8 C9 . 1.359(3) ?
C8 H8A . 0.930 ?
C9 C10 . 1.396(3) ?
C9 H9A . 0.930 ?
C10 H10A . 0.930 ?
C11 C12 . 1.436(2) ?
C13 O3 . 1.320(6) yes
C13 C13 2_655 1.386(7) yes
C13 H13A . 0.970 ?
C13 H13B . 0.970 ?
O3 H3 . 0.820 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H3 O2 0.82 2.01 2.709(8) 143
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_3
_geom_torsion_site_symmetry_4
_geom_torsion
O3 C13 C13 O3 2_655 2_655 -40(3)
