#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/39/2223948.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_2223948
loop_
_publ_author_name
'Wang, Shi'
'Ding, Xuehua'
'He, Wenrui'
'Huang, Wei'
_publ_section_title
;
 cis-Diaquabis(2,2',2''-tripyridylamine)zinc(II)
 bis(perchlorate)
;
_journal_coeditor_code           NK2005
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1424
_journal_paper_doi               10.1107/S1600536809042688
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Zn (C15 H12 N4)2 (H2 O)2] (Cl O4)2'
_chemical_formula_moiety         'C30 H28 N8 O2 Zn 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C30 H28 Cl2 N8 O10 Zn'
_chemical_formula_weight         796.89
_chemical_name_systematic
;
cis-Diaquabis(2,2',2''-tripyridylamine)zinc(II) bis(perchlorate)
;
_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                 121.689(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.687(3)
_cell_length_b                   19.305(4)
_cell_length_c                   10.8910(19)
_cell_measurement_reflns_used    7889
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.8955
_cell_measurement_theta_min      2.1845
_cell_volume                     3343.2(11)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7752
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.413
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2940
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0705P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                1861
_reflns_number_total             2940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nk2005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2223948
_cod_database_fobs_code          2223948
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
N N1 0.5518(2) 0.28833(19) 0.9789(4) 0.0386(9) Uani d . 1 . .
C C1 0.5611(3) 0.2247(2) 1.0527(5) 0.0419(12) Uani d . 1 . .
C C2 0.5981(3) 0.2230(3) 1.1989(5) 0.0560(15) Uani d . 1 . .
H H2 0.6182 0.2634 1.2530 0.067 Uiso calc R 1 . .
C C3 0.6054(4) 0.1604(3) 1.2652(6) 0.0726(19) Uani d . 1 . .
H H3 0.6305 0.1579 1.3648 0.087 Uiso calc R 1 . .
C C4 0.5750(4) 0.1018(3) 1.1816(7) 0.0750(19) Uani d . 1 . .
H H4 0.5783 0.0591 1.2237 0.090 Uiso calc R 1 . .
C C5 0.5400(4) 0.1072(3) 1.0366(6) 0.0612(16) Uani d . 1 . .
H H5 0.5209 0.0671 0.9811 0.073 Uiso calc R 1 . .
N N2 0.5317(2) 0.16820(19) 0.9694(4) 0.0428(10) Uani d . 1 . .
C C6 0.6036(3) 0.2977(2) 0.9218(5) 0.0382(11) Uani d . 1 . .
C C7 0.6595(3) 0.3515(3) 0.9666(5) 0.0533(14) Uani d . 1 . .
H H7 0.6629 0.3836 1.0331 0.064 Uiso calc R 1 . .
C C8 0.7103(3) 0.3570(3) 0.9116(6) 0.0670(17) Uani d . 1 . .
H H8 0.7474 0.3940 0.9378 0.080 Uiso calc R 1 . .
C C9 0.7060(3) 0.3072(3) 0.8166(6) 0.0598(16) Uani d . 1 . .
H H9 0.7410 0.3096 0.7799 0.072 Uiso calc R 1 . .
C C10 0.6500(3) 0.2550(3) 0.7783(5) 0.0455(12) Uani d . 1 . .
H H10 0.6476 0.2211 0.7155 0.055 Uiso calc R 1 . .
N N3 0.5972(2) 0.25002(18) 0.8277(4) 0.0350(9) Uani d . 1 . .
Zn Zn1 0.5000 0.17445(4) 0.7500 0.0376(3) Uani d S 1 . .
O O1W 0.4117(3) 0.0899(2) 0.7028(5) 0.0598(10) Uani d D 1 . .
H H1W 0.387(4) 0.066(3) 0.626(5) 0.10(3) Uiso d D 1 . .
H H2W 0.384(4) 0.088(3) 0.742(6) 0.10(3) Uiso d D 1 . .
C C11 0.5002(3) 0.3407(2) 0.9806(5) 0.0416(12) Uani d . 1 . .
N N4 0.4849(3) 0.3960(2) 0.8930(4) 0.0573(12) Uani d . 1 . .
C C12 0.4310(3) 0.4453(3) 0.8870(6) 0.0569(15) Uani d . 1 . .
H H12 0.4197 0.4841 0.8288 0.068 Uiso calc R 1 . .
C C13 0.3930(4) 0.4387(3) 0.9659(7) 0.0664(17) Uani d . 1 . .
H H13 0.3549 0.4717 0.9595 0.080 Uiso calc R 1 . .
C C14 0.4128(4) 0.3824(3) 1.0536(6) 0.0696(17) Uani d . 1 . .
H H14 0.3890 0.3776 1.1097 0.084 Uiso calc R 1 . .
C C15 0.4662(3) 0.3336(2) 1.0602(5) 0.0494(13) Uani d . 1 . .
H H15 0.4790 0.2953 1.1200 0.059 Uiso calc R 1 . .
Cl Cl1 0.79396(8) 0.44302(7) 0.37729(14) 0.0488(4) Uani d . 1 . .
O O2 0.8198(5) 0.3778(3) 0.3894(6) 0.200(4) Uani d . 1 . .
O O3 0.7209(4) 0.4465(5) 0.3674(8) 0.222(4) Uani d . 1 . .
O O4 0.8513(5) 0.4778(3) 0.4996(5) 0.159(3) Uani d . 1 . .
O O5 0.7854(3) 0.4721(3) 0.2524(4) 0.1048(17) Uani 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
C11 N1 C6 . . 123.2(4) ?
C11 N1 C1 . . 119.6(4) ?
C6 N1 C1 . . 116.7(4) ?
N2 C1 C2 . . 123.2(5) ?
N2 C1 N1 . . 115.8(4) ?
C2 C1 N1 . . 121.0(5) ?
C1 C2 C3 . . 118.9(5) ?
C1 C2 H2 . . 120.6 ?
C3 C2 H2 . . 120.6 ?
C4 C3 C2 . . 118.9(5) ?
C4 C3 H3 . . 120.6 ?
C2 C3 H3 . . 120.6 ?
C5 C4 C3 . . 119.0(5) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
N2 C5 C4 . . 123.0(5) ?
N2 C5 H5 . . 118.5 ?
C4 C5 H5 . . 118.5 ?
C1 N2 C5 . . 116.9(4) ?
C1 N2 Zn1 . . 119.0(3) ?
C5 N2 Zn1 . . 122.6(3) ?
N3 C6 C7 . . 122.7(5) ?
N3 C6 N1 . . 116.3(4) ?
C7 C6 N1 . . 120.9(5) ?
C8 C7 C6 . . 118.6(5) ?
C8 C7 H7 . . 120.7 ?
C6 C7 H7 . . 120.7 ?
C7 C8 C9 . . 119.5(5) ?
C7 C8 H8 . . 120.2 ?
C9 C8 H8 . . 120.2 ?
C10 C9 C8 . . 118.7(5) ?
C10 C9 H9 . . 120.6 ?
C8 C9 H9 . . 120.6 ?
N3 C10 C9 . . 122.5(5) ?
N3 C10 H10 . . 118.7 ?
C9 C10 H10 . . 118.7 ?
C6 N3 C10 . . 117.8(4) ?
C6 N3 Zn1 . . 119.5(3) ?
C10 N3 Zn1 . . 122.6(3) ?
N3 Zn1 N3 . 2_656 93.45(19) ?
N3 Zn1 N2 . 2_656 99.25(14) ?
N3 Zn1 N2 2_656 2_656 85.21(14) ?
N3 Zn1 N2 . . 85.21(14) ?
N3 Zn1 N2 2_656 . 99.25(14) ?
N2 Zn1 N2 2_656 . 173.5(2) ?
N3 Zn1 O1W . . 171.28(15) ?
N3 Zn1 O1W 2_656 . 92.16(15) ?
N2 Zn1 O1W 2_656 . 87.87(16) ?
N2 Zn1 O1W . . 87.30(16) ?
N3 Zn1 O1W . 2_656 92.16(15) ?
N3 Zn1 O1W 2_656 2_656 171.28(15) ?
N2 Zn1 O1W 2_656 2_656 87.30(16) ?
N2 Zn1 O1W . 2_656 87.87(16) ?
O1W Zn1 O1W . 2_656 83.1(2) ?
Zn1 O1W H1W . . 126(4) ?
Zn1 O1W H2W . . 120(5) ?
H1W O1W H2W . . 109(6) ?
C15 C11 N4 . . 123.1(4) ?
C15 C11 N1 . . 120.2(4) ?
N4 C11 N1 . . 116.7(4) ?
C11 N4 C12 . . 117.4(4) ?
N4 C12 C13 . . 121.1(5) ?
N4 C12 H12 . . 119.5 ?
C13 C12 H12 . . 119.5 ?
C14 C13 C12 . . 118.0(5) ?
C14 C13 H13 . . 121.0 ?
C12 C13 H13 . . 121.0 ?
C15 C14 C13 . . 121.2(5) ?
C15 C14 H14 . . 119.4 ?
C13 C14 H14 . . 119.4 ?
C11 C15 C14 . . 119.3(5) ?
C11 C15 H15 . . 120.4 ?
C14 C15 H15 . . 120.4 ?
O3 Cl1 O2 . . 111.4(6) ?
O3 Cl1 O4 . . 107.6(5) ?
O2 Cl1 O4 . . 108.1(4) ?
O3 Cl1 O5 . . 108.4(4) ?
O2 Cl1 O5 . . 109.0(4) ?
O4 Cl1 O5 . . 112.4(3) ?
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
N1 C11 . 1.404(5) ?
N1 C6 . 1.411(6) ?
N1 C1 . 1.428(5) ?
C1 N2 . 1.338(6) ?
C1 C2 . 1.364(6) ?
C2 C3 . 1.376(7) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.374(8) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.359(7) ?
C4 H4 . 0.9300 ?
C5 N2 . 1.352(6) ?
C5 H5 . 0.9300 ?
N2 Zn1 . 2.142(4) ?
C6 N3 . 1.335(5) ?
C6 C7 . 1.368(7) ?
C7 C8 . 1.366(7) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.384(8) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.352(7) ?
C9 H9 . 0.9300 ?
C10 N3 . 1.352(5) ?
C10 H10 . 0.9300 ?
N3 Zn1 . 2.128(4) ?
Zn1 N3 2_656 2.128(4) ?
Zn1 N2 2_656 2.142(4) ?
Zn1 O1W . 2.182(4) ?
Zn1 O1W 2_656 2.182(4) ?
O1W H1W . 0.85(4) ?
O1W H2W . 0.83(2) ?
C11 C15 . 1.325(6) ?
C11 N4 . 1.358(6) ?
N4 C12 . 1.364(6) ?
C12 C13 . 1.379(7) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.364(8) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.346(7) ?
C14 H14 . 0.9300 ?
C15 H15 . 0.9300 ?
Cl1 O3 . 1.314(5) ?
Cl1 O2 . 1.330(5) ?
Cl1 O4 . 1.369(5) ?
Cl1 O5 . 1.401(4) ?
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
_geom_hbond_publ_flag
C3 H3 O2 7_657 0.93 2.43 3.336(8) 165.5 n
O1W H2W O5 8_456 0.83(2) 2.23(4) 2.939(6) 143(6) y
O1W H1W O4 3_445 0.85(4) 2.07(5) 2.868(6) 158(6) y
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
C11 N1 C1 N2 . . . . 115.9(5) ?
C6 N1 C1 N2 . . . . -71.3(5) ?
C11 N1 C1 C2 . . . . -64.4(6) ?
C6 N1 C1 C2 . . . . 108.4(5) ?
N2 C1 C2 C3 . . . . -0.5(8) ?
N1 C1 C2 C3 . . . . 179.8(5) ?
C1 C2 C3 C4 . . . . -0.1(9) ?
C2 C3 C4 C5 . . . . 1.1(9) ?
C3 C4 C5 N2 . . . . -1.6(9) ?
C2 C1 N2 C5 . . . . 0.1(7) ?
N1 C1 N2 C5 . . . . 179.8(4) ?
C2 C1 N2 Zn1 . . . . -166.8(4) ?
N1 C1 N2 Zn1 . . . . 12.9(5) ?
C4 C5 N2 C1 . . . . 1.0(8) ?
C4 C5 N2 Zn1 . . . . 167.3(4) ?
C11 N1 C6 N3 . . . . -129.6(4) ?
C1 N1 C6 N3 . . . . 57.8(5) ?
C11 N1 C6 C7 . . . . 53.0(6) ?
C1 N1 C6 C7 . . . . -119.5(5) ?
N3 C6 C7 C8 . . . . 0.7(7) ?
N1 C6 C7 C8 . . . . 177.9(4) ?
C6 C7 C8 C9 . . . . -2.2(8) ?
C7 C8 C9 C10 . . . . 1.5(8) ?
C8 C9 C10 N3 . . . . 0.9(8) ?
C7 C6 N3 C10 . . . . 1.6(7) ?
N1 C6 N3 C10 . . . . -175.7(4) ?
C7 C6 N3 Zn1 . . . . -174.0(3) ?
N1 C6 N3 Zn1 . . . . 8.7(5) ?
C9 C10 N3 C6 . . . . -2.4(7) ?
C9 C10 N3 Zn1 . . . . 173.1(4) ?
C6 N3 Zn1 N3 . . . 2_656 56.2(3) ?
C10 N3 Zn1 N3 . . . 2_656 -119.1(4) ?
C6 N3 Zn1 N2 . . . 2_656 141.9(3) ?
C10 N3 Zn1 N2 . . . 2_656 -33.4(4) ?
C6 N3 Zn1 N2 . . . . -42.8(3) ?
C10 N3 Zn1 N2 . . . . 141.9(4) ?
C6 N3 Zn1 O1W . . . 2_656 -130.5(3) ?
C10 N3 Zn1 O1W . . . 2_656 54.2(4) ?
C1 N2 Zn1 N3 . . . . 30.8(3) ?
C5 N2 Zn1 N3 . . . . -135.2(4) ?
C1 N2 Zn1 N3 . . . 2_656 -61.9(3) ?
C5 N2 Zn1 N3 . . . 2_656 132.0(4) ?
C1 N2 Zn1 O1W . . . . -153.6(4) ?
C5 N2 Zn1 O1W . . . . 40.3(4) ?
C1 N2 Zn1 O1W . . . 2_656 123.2(4) ?
C5 N2 Zn1 O1W . . . 2_656 -42.9(4) ?
C6 N1 C11 C15 . . . . -166.6(5) ?
C1 N1 C11 C15 . . . . 5.8(7) ?
C6 N1 C11 N4 . . . . 16.3(6) ?
C1 N1 C11 N4 . . . . -171.4(4) ?
C15 C11 N4 C12 . . . . -0.8(7) ?
N1 C11 N4 C12 . . . . 176.2(4) ?
C11 N4 C12 C13 . . . . -0.7(8) ?
N4 C12 C13 C14 . . . . 1.9(9) ?
C12 C13 C14 C15 . . . . -1.7(9) ?
N4 C11 C15 C14 . . . . 1.0(8) ?
N1 C11 C15 C14 . . . . -175.9(5) ?
C13 C14 C15 C11 . . . . 0.3(9) ?
