#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/91/2229168.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_2229168
loop_
_publ_author_name
'Liu, Hong'
'Qin, Hui'
'Zhang, Yun-Jie'
'Yang, Hong-Wei'
'Zhang, Jian'
_publ_section_title
;
 Triaqua(1,10-phenanthroline-κ²N,N')(sulfato-κO)zinc(II)
;
_journal_coeditor_code           NG5108
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m280
_journal_page_last               m281
_journal_paper_doi               10.1107/S1600536811003138
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Zn (S O4) (C12 H8 N2) (H2 O)3]'
_chemical_formula_moiety         'C12 H14 N2 O7 S Zn'
_chemical_formula_sum            'C12 H14 N2 O7 S Zn'
_chemical_formula_weight         395.71
_chemical_name_systematic
;
Triaqua(1,10-phenanthroline-κ²N,N')(sulfato-
κO)zinc(II)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0011(4)
_cell_length_b                   9.6006(4)
_cell_length_c                   19.1606(9)
_cell_measurement_reflns_used    1025
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      1.50
_cell_volume                     1471.83(12)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ'
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7397
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.360
_refine_ls_abs_structure_details 'Flack (1983), 1165 Friedel pairs'
_refine_ls_abs_structure_Flack   0.005(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0213
_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)+(0.0161P)²+0.0050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                2667
_reflns_number_total             2793
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng5108.cif
_cod_data_source_block           I
_cod_database_code               2229168
_cod_database_fobs_code          2229168
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'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
Zn Zn 0.35962(3) 0.46528(2) 0.682343(13) 0.02381(7) Uani d . 1 . .
S S 0.75438(7) 0.43014(5) 0.72471(3) 0.02418(13) Uani d . 1 . .
O O1 0.59078(18) 0.36372(14) 0.70689(8) 0.0256(4) Uani d . 1 . .
O O2 0.8188(2) 0.50361(18) 0.66363(10) 0.0400(5) Uani d . 1 . .
O O3 0.7288(2) 0.52839(19) 0.78257(9) 0.0405(4) Uani d . 1 . .
O O4 0.8701(2) 0.31908(16) 0.74536(10) 0.0368(4) Uani d . 1 . .
O O5 0.13662(19) 0.58142(15) 0.67227(9) 0.0360(4) Uani d . 1 . .
H H51 0.0345 0.5516 0.6719 0.043 Uiso d R 1 . .
H H52 0.1259 0.6578 0.6961 0.043 Uiso d R 1 . .
O O6 0.3974(2) 0.57293(15) 0.77750(9) 0.0323(4) Uani d . 1 . .
H H61 0.3775 0.6643 0.7869 0.039 Uiso d R 1 . .
H H62 0.5003 0.5579 0.7908 0.039 Uiso d R 1 . .
O O7 0.2180(2) 0.31186(16) 0.73196(10) 0.0371(4) Uani d . 1 . .
H H71 0.2385 0.2140 0.7387 0.044 Uiso d R 1 . .
H H72 0.1156 0.3184 0.7392 0.044 Uiso d R 1 . .
N N1 0.4592(2) 0.62126(19) 0.61251(10) 0.0264(4) Uani d . 1 . .
N N2 0.3537(3) 0.35890(18) 0.58398(10) 0.0291(4) Uani d . 1 . .
C C1 0.3124(3) 0.2282(3) 0.57089(15) 0.0384(6) Uani d . 1 . .
H H1 0.2798 0.1720 0.6080 0.046 Uiso calc R 1 . .
C C2 0.3153(4) 0.1707(3) 0.50423(16) 0.0489(8) Uani d . 1 . .
H H2 0.2882 0.0775 0.4975 0.059 Uiso calc R 1 . .
C C3 0.3584(4) 0.2526(3) 0.44882(16) 0.0491(7) Uani d . 1 . .
H H3 0.3586 0.2159 0.4039 0.059 Uiso calc R 1 . .
C C4 0.4539(4) 0.4834(4) 0.40547(14) 0.0534(8) Uani d . 1 . .
H H4 0.4550 0.4519 0.3596 0.064 Uiso calc R 1 . .
C C5 0.5013(4) 0.6158(4) 0.41983(16) 0.0560(8) Uani d . 1 . .
H H5 0.5333 0.6740 0.3834 0.067 Uiso calc R 1 . .
C C6 0.5501(4) 0.8055(3) 0.50634(16) 0.0513(8) Uani d . 1 . .
H H6 0.5799 0.8678 0.4713 0.062 Uiso calc R 1 . .
C C7 0.5510(4) 0.8461(3) 0.57495(17) 0.0478(7) Uani d . 1 . .
H H7 0.5808 0.9366 0.5870 0.057 Uiso calc R 1 . .
C C8 0.5069(3) 0.7504(3) 0.62626(15) 0.0356(6) Uani d . 1 . .
H H8 0.5112 0.7786 0.6727 0.043 Uiso calc R 1 . .
C C9 0.4024(3) 0.3920(3) 0.45999(14) 0.0385(6) Uani d . 1 . .
C C10 0.5032(4) 0.6680(3) 0.48954(14) 0.0401(6) Uani d . 1 . .
C C11 0.4028(3) 0.4397(2) 0.52967(12) 0.0270(5) Uani d . 1 . .
C C12 0.4559(3) 0.5801(2) 0.54475(13) 0.0274(5) Uani d . 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 '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'
O O 0.0106 0.0060 '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'
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'
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
O7 Zn O5 . . 87.46(6) n
O7 Zn O6 . . 91.71(7) n
O5 Zn O6 . . 86.66(6) n
O7 Zn O1 . . 92.72(6) n
O5 Zn O1 . . 171.49(6) n
O6 Zn O1 . . 84.83(6) n
O7 Zn N2 . . 92.99(7) n
O5 Zn N2 . . 98.77(7) n
O6 Zn N2 . . 172.97(7) n
O1 Zn N2 . . 89.73(7) n
O7 Zn N1 . . 166.26(7) n
O5 Zn N1 . . 83.64(6) n
O6 Zn N1 . . 98.18(7) n
O1 Zn N1 . . 97.64(6) n
N2 Zn N1 . . 78.11(7) n
O2 S O4 . . 110.15(10) n
O2 S O3 . . 110.09(11) n
O4 S O3 . . 110.55(11) n
O2 S O1 . . 109.39(10) n
O4 S O1 . . 107.69(9) n
O3 S O1 . . 108.91(10) n
S O1 Zn . . 127.69(8) n
Zn O5 H51 . . 128.6 n
Zn O5 H52 . . 118.8 n
H51 O5 H52 . . 101.0 n
Zn O6 H61 . . 128.0 n
Zn O6 H62 . . 107.7 n
H61 O6 H62 . . 105.5 n
Zn O7 H71 . . 131.1 n
Zn O7 H72 . . 123.8 n
H71 O7 H72 . . 102.6 n
C8 N1 C12 . . 118.0(2) n
C8 N1 Zn . . 129.22(18) n
C12 N1 Zn . . 112.53(14) n
C1 N2 C11 . . 118.0(2) n
C1 N2 Zn . . 128.65(18) n
C11 N2 Zn . . 113.30(14) n
N2 C1 C2 . . 123.1(3) n
N2 C1 H1 . . 118.4 n
C2 C1 H1 . . 118.4 n
C3 C2 C1 . . 119.3(2) n
C3 C2 H2 . . 120.3 n
C1 C2 H2 . . 120.3 n
C2 C3 C9 . . 119.7(3) n
C2 C3 H3 . . 120.2 n
C9 C3 H3 . . 120.2 n
C5 C4 C9 . . 120.7(3) n
C5 C4 H4 . . 119.7 n
C9 C4 H4 . . 119.7 n
C4 C5 C10 . . 121.5(3) n
C4 C5 H5 . . 119.2 n
C10 C5 H5 . . 119.2 n
C7 C6 C10 . . 119.2(3) n
C7 C6 H6 . . 120.4 n
C10 C6 H6 . . 120.4 n
C6 C7 C8 . . 119.2(3) n
C6 C7 H7 . . 120.4 n
C8 C7 H7 . . 120.4 n
N1 C8 C7 . . 123.5(3) n
N1 C8 H8 . . 118.3 n
C7 C8 H8 . . 118.3 n
C3 C9 C11 . . 117.1(2) n
C3 C9 C4 . . 123.3(3) n
C11 C9 C4 . . 119.5(2) n
C12 C10 C6 . . 117.5(2) n
C12 C10 C5 . . 119.4(3) n
C6 C10 C5 . . 123.1(3) n
N2 C11 C9 . . 122.6(2) n
N2 C11 C12 . . 117.8(2) n
C9 C11 C12 . . 119.6(2) n
N1 C12 C10 . . 122.7(2) n
N1 C12 C11 . . 118.0(2) n
C10 C12 C11 . . 119.3(2) n
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
Zn O7 . 2.0874(16) y
Zn O5 . 2.1128(15) y
Zn O6 . 2.1175(16) y
Zn O1 . 2.1431(15) y
Zn N2 . 2.1442(19) y
Zn N1 . 2.1605(19) y
S O2 . 1.4605(18) n
S O4 . 1.4663(16) n
S O3 . 1.4698(18) n
S O1 . 1.4955(15) n
O5 H51 . 0.8655 n
O5 H52 . 0.8678 n
O6 H61 . 0.9094 n
O6 H62 . 0.8738 n
O7 H71 . 0.9628 n
O7 H72 . 0.8331 n
N1 C8 . 1.324(3) n
N1 C12 . 1.357(3) n
N2 C1 . 1.322(3) n
N2 C11 . 1.356(3) n
C1 C2 . 1.392(4) n
C1 H1 . 0.9300 n
C2 C3 . 1.365(4) n
C2 H2 . 0.9300 n
C3 C9 . 1.400(4) n
C3 H3 . 0.9300 n
C4 C5 . 1.355(5) n
C4 C9 . 1.425(4) n
C4 H4 . 0.9300 n
C5 C10 . 1.427(4) n
C5 H5 . 0.9300 n
C6 C7 . 1.371(4) n
C6 C10 . 1.409(4) n
C6 H6 . 0.9300 n
C7 C8 . 1.392(4) n
C7 H7 . 0.9300 n
C8 H8 . 0.9300 n
C9 C11 . 1.412(3) n
C10 C12 . 1.405(3) n
C11 C12 . 1.442(3) n
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
O5 H51 O2 1_455 0.87 1.79 2.655(2) 174
O5 H52 O4 3_656 0.87 1.91 2.775(2) 172
O6 H61 O1 3_656 0.91 1.93 2.809(2) 161
O6 H62 O3 . 0.87 1.86 2.688(2) 158
O7 H71 O3 3_646 0.96 1.85 2.769(3) 160
O7 H72 O4 1_455 0.83 1.97 2.797(2) 173
C1 H1 O3 3_646 0.93 2.51 3.416(3) 165
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
O2 S O1 Zn . . . . -66.81(14) n
O4 S O1 Zn . . . . 173.47(11) n
O3 S O1 Zn . . . . 53.56(15) n
O7 Zn O1 S . . . . -144.44(12) n
O6 Zn O1 S . . . . -52.97(12) n
N2 Zn O1 S . . . . 122.58(13) n
N1 Zn O1 S . . . . 44.62(13) n
O7 Zn N1 C8 . . . . 127.7(3) n
O5 Zn N1 C8 . . . . 77.8(2) n
O6 Zn N1 C8 . . . . -7.9(2) n
O1 Zn N1 C8 . . . . -93.7(2) n
N2 Zn N1 C8 . . . . 178.2(2) n
O7 Zn N1 C12 . . . . -45.9(4) n
O5 Zn N1 C12 . . . . -95.77(15) n
O6 Zn N1 C12 . . . . 178.55(15) n
O1 Zn N1 C12 . . . . 92.71(15) n
N2 Zn N1 C12 . . . . 4.61(15) n
O7 Zn N2 C1 . . . . -15.4(2) n
O5 Zn N2 C1 . . . . -103.3(2) n
O1 Zn N2 C1 . . . . 77.3(2) n
N1 Zn N2 C1 . . . . 175.2(2) n
O7 Zn N2 C11 . . . . 165.96(15) n
O5 Zn N2 C11 . . . . 78.08(16) n
O1 Zn N2 C11 . . . . -101.33(16) n
N1 Zn N2 C11 . . . . -3.46(15) n
C11 N2 C1 C2 . . . . -0.7(4) n
Zn N2 C1 C2 . . . . -179.3(2) n
N2 C1 C2 C3 . . . . -1.8(5) n
C1 C2 C3 C9 . . . . 1.4(5) n
C9 C4 C5 C10 . . . . 0.7(5) n
C10 C6 C7 C8 . . . . 0.4(5) n
C12 N1 C8 C7 . . . . 1.1(4) n
Zn N1 C8 C7 . . . . -172.2(2) n
C6 C7 C8 N1 . . . . -1.8(5) n
C2 C3 C9 C11 . . . . 1.3(4) n
C2 C3 C9 C4 . . . . 178.0(3) n
C5 C4 C9 C3 . . . . -177.4(3) n
C5 C4 C9 C11 . . . . -0.8(4) n
C7 C6 C10 C12 . . . . 1.4(4) n
C7 C6 C10 C5 . . . . -178.9(3) n
C4 C5 C10 C12 . . . . 0.4(5) n
C4 C5 C10 C6 . . . . -179.3(3) n
C1 N2 C11 C9 . . . . 3.6(3) n
Zn N2 C11 C9 . . . . -177.59(18) n
C1 N2 C11 C12 . . . . -176.9(2) n
Zn N2 C11 C12 . . . . 1.9(3) n
C3 C9 C11 N2 . . . . -3.9(4) n
C4 C9 C11 N2 . . . . 179.3(2) n
C3 C9 C11 C12 . . . . 176.6(2) n
C4 C9 C11 C12 . . . . -0.2(4) n
C8 N1 C12 C10 . . . . 1.0(3) n
Zn N1 C12 C10 . . . . 175.37(19) n
C8 N1 C12 C11 . . . . -179.6(2) n
Zn N1 C12 C11 . . . . -5.2(2) n
C6 C10 C12 N1 . . . . -2.2(4) n
C5 C10 C12 N1 . . . . 178.1(3) n
C6 C10 C12 C11 . . . . 178.4(3) n
C5 C10 C12 C11 . . . . -1.3(4) n
N2 C11 C12 N1 . . . . 2.3(3) n
C9 C11 C12 N1 . . . . -178.2(2) n
N2 C11 C12 C10 . . . . -178.2(2) n
C9 C11 C12 C10 . . . . 1.3(3) n
