#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/54/2225414.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_2225414
loop_
_publ_author_name
'Zhong, Kai-Long'
_publ_section_title
;Bis(1,10-phenanthroline-κ²N,N')(sulfato-κ²O,O')cobalt(II)
 propane-1,3-diol solvate
;
_journal_coeditor_code           ZQ2024
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m247
_journal_paper_doi               10.1107/S1600536810003478
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Co (S O4) (C12 H8 N2)2], C3 H8 O2'
_chemical_formula_moiety         'C24 H16 Co N4 O4 S, C3 H8 O2'
_chemical_formula_sum            'C27 H24 Co N4 O6 S'
_chemical_formula_weight         591.49
_chemical_name_systematic
;
Bis(1,10-phenanthroline-κ²N,N')(sulfato-
κ²O,O')cobalt(II) propane-1,3-diol 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                 121.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.285(4)
_cell_length_b                   12.422(3)
_cell_length_c                   13.211(3)
_cell_measurement_reflns_used    3592
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      27.4623
_cell_measurement_theta_min      3.1955
_cell_volume                     2549.7(13)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7099
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB: Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.451
_refine_ls_extinction_coef       0.0057(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2898
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0616P)²+1.0504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                2540
_reflns_number_total             2898
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            zq2024.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2225414
_cod_database_fobs_code          2225414
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 0.81835(3) 0.2500 0.02201(14) Uani d S 1 . .
S S1 0.5000 1.03618(5) 0.2500 0.02331(17) Uani d S 1 . .
O O1 0.44793(9) 0.96187(12) 0.14805(12) 0.0329(3) Uani d . 1 . .
C C11 0.34382(12) 0.68292(14) 0.14757(16) 0.0224(4) Uani d . 1 . .
N N2 0.40420(10) 0.71189(13) 0.12195(14) 0.0238(3) Uani d . 1 . .
C C10 0.39507(13) 0.67410(16) 0.02169(18) 0.0284(4) Uani d . 1 . .
H H10A 0.4356 0.6935 0.0028 0.034 Uiso calc R 1 . .
C C8 0.26687(13) 0.57717(16) -0.03144(17) 0.0304(4) Uani d . 1 . .
H H8A 0.2213 0.5328 -0.0832 0.036 Uiso calc R 1 . .
O O2 0.55612(10) 1.10269(14) 0.22920(16) 0.0446(4) Uani d . 1 . .
C C6 0.21399(13) 0.58852(17) 0.10868(18) 0.0310(4) Uani d . 1 . .
H H6A 0.1679 0.5434 0.0604 0.037 Uiso calc R 1 . .
C C12 0.35267(11) 0.72718(15) 0.25388(16) 0.0223(4) Uani d . 1 . .
C C7 0.27424(12) 0.61511(16) 0.07446(17) 0.0264(4) Uani d . 1 . .
C C4 0.29234(12) 0.69936(16) 0.28497(17) 0.0270(4) Uani d . 1 . .
C C9 0.32726(14) 0.60646(18) -0.05671(18) 0.0331(4) Uani d . 1 . .
H H9A 0.3235 0.5817 -0.1257 0.040 Uiso calc R 1 . .
C C5 0.22322(12) 0.62810(18) 0.21042(18) 0.0322(5) Uani d . 1 . .
H H5A 0.1841 0.6086 0.2319 0.039 Uiso calc R 1 . .
N N1 0.41806(10) 0.79727(13) 0.31789(14) 0.0250(3) Uani d . 1 . .
C C1 0.42581(13) 0.84107(17) 0.41526(18) 0.0291(4) Uani d . 1 . .
H H1A 0.4706 0.8892 0.4597 0.035 Uiso calc R 1 . .
C C2 0.36899(14) 0.81726(18) 0.45310(19) 0.0335(5) Uani d . 1 . .
H H2A 0.3762 0.8491 0.5215 0.040 Uiso calc R 1 . .
C C3 0.30319(13) 0.74709(18) 0.38888(18) 0.0335(5) Uani d . 1 . .
H H3A 0.2653 0.7306 0.4135 0.040 Uiso calc R 1 . .
O O3 0.56334(16) 1.31539(16) 0.1809(2) 0.0659(6) Uani d D 1 . .
H H3B 0.5610 1.2514 0.1944 0.099 Uiso calc R 1 . .
C C14 0.5000 1.4456(3) 0.2500 0.0562(10) Uani d SDU 1 . .
C C13 0.5774(2) 1.3764(3) 0.2780(3) 0.0723(9) Uani d DU 1 . .
H H13A 0.6268 1.4227 0.3033 0.087 Uiso calc R 1 . .
H H13B 0.5907 1.3286 0.3436 0.087 Uiso calc R 1 . .
H H14 0.496(3) 1.442(4) 0.174(2) 0.143(19) Uiso d D 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'
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
N1 Co1 N1 2_655 . 165.87(9) ?
N1 Co1 O1 2_655 2_655 100.94(6) ?
N1 Co1 O1 . 2_655 90.91(6) ?
N1 Co1 O1 2_655 . 90.91(6) ?
N1 Co1 O1 . . 100.94(6) ?
O1 Co1 O1 2_655 . 66.54(8) ?
N1 Co1 N2 2_655 . 93.19(6) ?
N1 Co1 N2 . . 77.99(6) ?
O1 Co1 N2 2_655 . 157.72(6) ?
O1 Co1 N2 . . 96.36(6) ?
N1 Co1 N2 2_655 2_655 77.99(6) ?
N1 Co1 N2 . 2_655 93.19(6) ?
O1 Co1 N2 2_655 2_655 96.36(6) ?
O1 Co1 N2 . 2_655 157.72(6) ?
N2 Co1 N2 . 2_655 103.42(9) ?
N1 Co1 S1 2_655 . 97.06(5) ?
N1 Co1 S1 . . 97.06(5) ?
O1 Co1 S1 2_655 . 33.27(4) ?
O1 Co1 S1 . . 33.27(4) ?
N2 Co1 S1 . . 128.29(5) ?
N2 Co1 S1 2_655 . 128.29(5) ?
O2 S1 O2 . 2_655 110.64(15) ?
O2 S1 O1 . . 111.10(9) ?
O2 S1 O1 2_655 . 110.18(9) ?
O2 S1 O1 . 2_655 110.18(9) ?
O2 S1 O1 2_655 2_655 111.10(9) ?
O1 S1 O1 . 2_655 103.45(12) ?
O2 S1 Co1 . . 124.68(7) ?
O2 S1 Co1 2_655 . 124.68(7) ?
O1 S1 Co1 . . 51.72(6) ?
O1 S1 Co1 2_655 . 51.72(6) ?
S1 O1 Co1 . . 95.01(7) ?
N2 C11 C7 . . 123.19(17) ?
N2 C11 C12 . . 116.97(16) ?
C7 C11 C12 . . 119.82(17) ?
C10 N2 C11 . . 117.47(17) ?
C10 N2 Co1 . . 128.88(13) ?
C11 N2 Co1 . . 113.62(12) ?
N2 C10 C9 . . 123.06(18) ?
N2 C10 H10A . . 118.5 ?
C9 C10 H10A . . 118.5 ?
C9 C8 C7 . . 119.17(19) ?
C9 C8 H8A . . 120.4 ?
C7 C8 H8A . . 120.4 ?
C5 C6 C7 . . 120.98(18) ?
C5 C6 H6A . . 119.5 ?
C7 C6 H6A . . 119.5 ?
N1 C12 C4 . . 123.01(17) ?
N1 C12 C11 . . 117.63(16) ?
C4 C12 C11 . . 119.33(17) ?
C11 C7 C8 . . 117.41(18) ?
C11 C7 C6 . . 119.39(18) ?
C8 C7 C6 . . 123.19(18) ?
C12 C4 C3 . . 116.81(18) ?
C12 C4 C5 . . 119.71(18) ?
C3 C4 C5 . . 123.45(18) ?
C8 C9 C10 . . 119.69(19) ?
C8 C9 H9A . . 120.2 ?
C10 C9 H9A . . 120.2 ?
C6 C5 C4 . . 120.73(18) ?
C6 C5 H5A . . 119.6 ?
C4 C5 H5A . . 119.6 ?
C1 N1 C12 . . 118.30(16) ?
C1 N1 Co1 . . 127.99(14) ?
C12 N1 Co1 . . 113.67(12) ?
N1 C1 C2 . . 122.42(19) ?
N1 C1 H1A . . 118.8 ?
C2 C1 H1A . . 118.8 ?
C3 C2 C1 . . 119.41(19) ?
C3 C2 H2A . . 120.3 ?
C1 C2 H2A . . 120.3 ?
C2 C3 C4 . . 120.05(18) ?
C2 C3 H3A . . 120.0 ?
C4 C3 H3A . . 120.0 ?
C13 O3 H3B . . 109.5 ?
C13 C14 C13 2_655 . 111.4(3) ?
C13 C14 H14 2_655 . 100(3) ?
C13 C14 H14 . . 77(3) ?
O3 C13 C14 . . 112.8(2) ?
O3 C13 H13A . . 109.0 ?
C14 C13 H13A . . 109.0 ?
O3 C13 H13B . . 109.0 ?
C14 C13 H13B . . 109.0 ?
H13A C13 H13B . . 107.8 ?
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 N1 2_655 2.1295(16) ?
Co1 N1 . 2.1295(16) ?
Co1 O1 2_655 2.1323(15) ?
Co1 O1 . 2.1323(15) ?
Co1 N2 . 2.1341(17) ?
Co1 N2 2_655 2.1341(17) ?
Co1 S1 . 2.7058(9) ?
S1 O2 . 1.4519(15) ?
S1 O2 2_655 1.4519(15) ?
S1 O1 . 1.4901(15) ?
S1 O1 2_655 1.4901(15) ?
C11 N2 . 1.363(2) ?
C11 C7 . 1.402(3) ?
C11 C12 . 1.436(3) ?
N2 C10 . 1.330(2) ?
C10 C9 . 1.401(3) ?
C10 H10A . 0.9300 ?
C8 C9 . 1.361(3) ?
C8 C7 . 1.414(3) ?
C8 H8A . 0.9300 ?
C6 C5 . 1.356(3) ?
C6 C7 . 1.432(3) ?
C6 H6A . 0.9300 ?
C12 N1 . 1.355(3) ?
C12 C4 . 1.408(3) ?
C4 C3 . 1.410(3) ?
C4 C5 . 1.428(3) ?
C9 H9A . 0.9300 ?
C5 H5A . 0.9300 ?
N1 C1 . 1.334(3) ?
C1 C2 . 1.401(3) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.360(3) ?
C2 H2A . 0.9300 ?
C3 H3A . 0.9300 ?
O3 C13 . 1.392(3) ?
O3 H3B . 0.8200 ?
C14 C13 2_655 1.525(4) ?
C14 C13 . 1.525(4) ?
C14 H14 . 0.97(3) ?
C13 H13A . 0.9700 ?
C13 H13B . 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
O3 H3B O2 . 0.82 1.92 2.737(3) 178.8
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 Co1 S1 O2 2_655 . . . -9.86(10) ?
N1 Co1 S1 O2 . . . . 170.14(10) ?
O1 Co1 S1 O2 2_655 . . . 89.33(12) ?
O1 Co1 S1 O2 . . . . -90.67(12) ?
N2 Co1 S1 O2 . . . . -109.61(10) ?
N2 Co1 S1 O2 2_655 . . . 70.39(10) ?
N1 Co1 S1 O2 2_655 . . 2_655 170.14(10) ?
N1 Co1 S1 O2 . . . 2_655 -9.86(10) ?
O1 Co1 S1 O2 2_655 . . 2_655 -90.67(12) ?
O1 Co1 S1 O2 . . . 2_655 89.33(12) ?
N2 Co1 S1 O2 . . . 2_655 70.39(10) ?
N2 Co1 S1 O2 2_655 . . 2_655 -109.61(10) ?
N1 Co1 S1 O1 2_655 . . . 80.81(9) ?
N1 Co1 S1 O1 . . . . -99.19(9) ?
O1 Co1 S1 O1 2_655 . . . 180.0 ?
N2 Co1 S1 O1 . . . . -18.94(9) ?
N2 Co1 S1 O1 2_655 . . . 161.06(9) ?
N1 Co1 S1 O1 2_655 . . 2_655 -99.19(9) ?
N1 Co1 S1 O1 . . . 2_655 80.81(9) ?
O1 Co1 S1 O1 . . . 2_655 180.0 ?
N2 Co1 S1 O1 . . . 2_655 161.06(9) ?
N2 Co1 S1 O1 2_655 . . 2_655 -18.94(9) ?
O2 S1 O1 Co1 . . . . 118.19(9) ?
O2 S1 O1 Co1 2_655 . . . -118.83(9) ?
O1 S1 O1 Co1 2_655 . . . 0.0 ?
N1 Co1 O1 S1 2_655 . . . -101.54(8) ?
N1 Co1 O1 S1 . . . . 86.20(8) ?
O1 Co1 O1 S1 2_655 . . . 0.0 ?
N2 Co1 O1 S1 . . . . 165.15(7) ?
N2 Co1 O1 S1 2_655 . . . -42.22(19) ?
C7 C11 N2 C10 . . . . 0.7(3) ?
C12 C11 N2 C10 . . . . -177.90(17) ?
C7 C11 N2 Co1 . . . . 178.87(14) ?
C12 C11 N2 Co1 . . . . 0.2(2) ?
N1 Co1 N2 C10 2_655 . . . -14.97(17) ?
N1 Co1 N2 C10 . . . . 176.18(18) ?
O1 Co1 N2 C10 2_655 . . . 114.64(19) ?
O1 Co1 N2 C10 . . . . 76.30(17) ?
N2 Co1 N2 C10 2_655 . . . -93.38(17) ?
S1 Co1 N2 C10 . . . . 86.62(17) ?
N1 Co1 N2 C11 2_655 . . . 167.15(13) ?
N1 Co1 N2 C11 . . . . -1.71(12) ?
O1 Co1 N2 C11 2_655 . . . -63.2(2) ?
O1 Co1 N2 C11 . . . . -101.58(13) ?
N2 Co1 N2 C11 2_655 . . . 88.74(13) ?
S1 Co1 N2 C11 . . . . -91.26(13) ?
C11 N2 C10 C9 . . . . -0.4(3) ?
Co1 N2 C10 C9 . . . . -178.16(15) ?
N2 C11 C12 N1 . . . . 2.5(3) ?
C7 C11 C12 N1 . . . . -176.19(17) ?
N2 C11 C12 C4 . . . . -179.60(17) ?
C7 C11 C12 C4 . . . . 1.7(3) ?
N2 C11 C7 C8 . . . . -1.0(3) ?
C12 C11 C7 C8 . . . . 177.62(17) ?
N2 C11 C7 C6 . . . . 179.73(18) ?
C12 C11 C7 C6 . . . . -1.7(3) ?
C9 C8 C7 C11 . . . . 0.8(3) ?
C9 C8 C7 C6 . . . . -179.9(2) ?
C5 C6 C7 C11 . . . . 0.1(3) ?
C5 C6 C7 C8 . . . . -179.1(2) ?
N1 C12 C4 C3 . . . . -0.9(3) ?
C11 C12 C4 C3 . . . . -178.66(17) ?
N1 C12 C4 C5 . . . . 177.55(18) ?
C11 C12 C4 C5 . . . . -0.2(3) ?
C7 C8 C9 C10 . . . . -0.5(3) ?
N2 C10 C9 C8 . . . . 0.3(3) ?
C7 C6 C5 C4 . . . . 1.4(3) ?
C12 C4 C5 C6 . . . . -1.3(3) ?
C3 C4 C5 C6 . . . . 177.0(2) ?
C4 C12 N1 C1 . . . . 0.6(3) ?
C11 C12 N1 C1 . . . . 178.38(17) ?
C4 C12 N1 Co1 . . . . 178.28(14) ?
C11 C12 N1 Co1 . . . . -3.9(2) ?
N1 Co1 N1 C1 2_655 . . . 128.19(17) ?
O1 Co1 N1 C1 2_655 . . . -19.01(17) ?
O1 Co1 N1 C1 . . . . -85.28(18) ?
N2 Co1 N1 C1 . . . . -179.54(18) ?
N2 Co1 N1 C1 2_655 . . . 77.41(18) ?
S1 Co1 N1 C1 . . . . -51.81(17) ?
N1 Co1 N1 C12 2_655 . . . -49.27(13) ?
O1 Co1 N1 C12 2_655 . . . 163.52(13) ?
O1 Co1 N1 C12 . . . . 97.25(14) ?
N2 Co1 N1 C12 . . . . 2.99(13) ?
N2 Co1 N1 C12 2_655 . . . -100.06(14) ?
S1 Co1 N1 C12 . . . . 130.73(13) ?
C12 N1 C1 C2 . . . . -0.1(3) ?
Co1 N1 C1 C2 . . . . -177.43(15) ?
N1 C1 C2 C3 . . . . -0.1(3) ?
C1 C2 C3 C4 . . . . -0.3(3) ?
C12 C4 C3 C2 . . . . 0.7(3) ?
C5 C4 C3 C2 . . . . -177.6(2) ?
C13 C14 C13 O3 2_655 . . . 64.6(2) ?
