#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/78/2217856.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_2217856
loop_
_publ_author_name
'Gallardo, Hugo'
'Molin, Fernando'
'Bortoluzzi, Adailton J.'
'Neves, Ademir'
_publ_section_title
;trans-Diaquabis{1,3-bis[5-(2-pyridyl)-2H-tetrazol-2-yl]propane}zinc(II)
 bis(perchlorate)
;
_journal_coeditor_code           BG2168
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m541
_journal_page_last               m542
_journal_paper_doi               10.1107/S1600536808006703
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Zn (C15 H14 N10) (H2 O)2] (Cl O4)2'
_chemical_formula_moiety         'C30 H32 N20 O2 Zn 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C30 H32 Cl2 N20 O10 Zn'
_chemical_formula_weight         969.03
_chemical_name_systematic
;
trans-Diaquabis{1,3-bis[5-(2-pyridyl)-2H-tetrazol-2-yl]propane}zinc(II)
bis(perchlorate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.25(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.378(3)
_cell_length_b                   13.354(3)
_cell_length_c                   20.764(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.35
_cell_measurement_theta_min      9.58
_cell_volume                     2019.2(10)
_computing_cell_refinement
;
SET4 in CAD-4 EXPRESS (Enraf--Nonius, 1994)
;
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'HELENA (Spek, 1996)'
_computing_molecular_graphics
;
PLATON (Spek, 2003) and Mercury (Macrae et al.,  2006)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3873
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North et al.,  1968)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.409
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3576
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0352
_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)+(0.0463P)²+1.2496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                2826
_reflns_number_total             3576
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg2168.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2217856
_cod_database_fobs_code          2217856
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Zn Zn1 0.0000 0.5000 0.5000 0.03313(13) Uani d S 1
O O1W 0.1357(3) 0.37083(13) 0.54150(8) 0.0414(4) Uani d . 1
H H1WA 0.2079 0.3821 0.5779 0.050 Uiso d R 1
H H1WB 0.0630 0.3224 0.5479 0.050 Uiso d R 1
C C1 0.2499(4) 0.4082(2) 0.26479(13) 0.0525(8) Uani d D 1
H H1C 0.3610 0.4474 0.2763 0.063 Uiso d PR 0.848(8)
H H1B 0.2857 0.3387 0.2618 0.063 Uiso d PR 0.848(8)
H H1A' 0.3789 0.4082 0.2838 0.063 Uiso d PR 0.152(8)
H H1B' 0.2230 0.3455 0.2416 0.063 Uiso d PR 0.152(8)
C C2 0.1502(6) 0.4409(3) 0.19841(17) 0.0478(12) Uani d PD 0.848(8)
H H2A 0.0335 0.4063 0.1884 0.057 Uiso d PR 0.848(8)
H H2B 0.2233 0.4235 0.1652 0.057 Uiso d PR 0.848(8)
C C2' 0.212(2) 0.5004(19) 0.2178(9) 0.062(9) Uani d PD 0.152(8)
H H2A' 0.3042 0.4990 0.1893 0.075 Uiso d PR 0.152(8)
H H2B' 0.2302 0.5620 0.2428 0.075 Uiso d PR 0.152(8)
C C3 0.1192(7) 0.5522(3) 0.19766(16) 0.0473(11) Uani d PD 0.848(8)
H H3A 0.0221 0.5680 0.2224 0.057 Uiso d PR 0.848(8)
H H3B 0.2299 0.5865 0.2177 0.057 Uiso d PR 0.848(8)
C C3' 0.031(2) 0.5010(16) 0.1744(9) 0.048(6) Uani d PD 0.152(8)
H H3A' -0.0017 0.4382 0.1521 0.058 Uiso d PR 0.152(8)
H H3B' -0.0640 0.5198 0.1994 0.058 Uiso d PR 0.152(8)
C C10 -0.2250(3) 0.36570(18) 0.40158(11) 0.0336(5) Uani d . 1
N N11 -0.2337(3) 0.40794(15) 0.46025(9) 0.0330(5) Uani d . 1
C C12 -0.3779(4) 0.3837(2) 0.48910(13) 0.0407(6) Uani d . 1
H H12 -0.3880 0.4129 0.5290 0.049 Uiso calc R 1
C C13 -0.5122(4) 0.3170(2) 0.46167(15) 0.0488(7) Uani d . 1
H H13 -0.6099 0.3013 0.4831 0.059 Uiso calc R 1
C C14 -0.4989(4) 0.2741(2) 0.40210(15) 0.0505(7) Uani d . 1
H H14 -0.5869 0.2285 0.3831 0.061 Uiso calc R 1
C C15 -0.3538(4) 0.2996(2) 0.37130(13) 0.0433(6) Uani d . 1
H H15 -0.3432 0.2727 0.3308 0.052 Uiso calc R 1
C C16 -0.0630(3) 0.39652(18) 0.37349(11) 0.0333(5) Uani d . 1
N N17 0.0622(3) 0.45884(16) 0.40591(10) 0.0351(5) Uani d . 1
N N18 0.1900(3) 0.47270(17) 0.36914(10) 0.0404(5) Uani d . 1
N N19 0.1370(3) 0.41780(17) 0.31670(10) 0.0395(5) Uani d . 1
N N20 -0.0198(3) 0.36842(17) 0.31667(10) 0.0414(5) Uani d . 1
C C20 0.1645(4) 0.6352(2) -0.02723(13) 0.0393(6) Uani d . 1
N N21 0.1096(3) 0.71610(16) -0.06368(11) 0.0429(5) Uani d . 1
C C22 0.1892(4) 0.7317(2) -0.11638(14) 0.0534(8) Uani d . 1
H H22 0.1536 0.7876 -0.1420 0.064 Uiso calc R 1
C C23 0.3205(5) 0.6698(3) -0.13475(16) 0.0654(9) Uani d . 1
H H23 0.3741 0.6845 -0.1712 0.078 Uiso calc R 1
C C24 0.3713(5) 0.5852(3) -0.09787(17) 0.0697(10) Uani d . 1
H H24 0.4573 0.5409 -0.1098 0.084 Uiso calc R 1
C C25 0.2923(4) 0.5676(2) -0.04327(15) 0.0552(8) Uani d . 1
H H25 0.3242 0.5113 -0.0176 0.066 Uiso calc R 1
C C26 0.0884(4) 0.62351(19) 0.03362(13) 0.0394(6) Uani d . 1
N N27 -0.0628(3) 0.66990(18) 0.04770(12) 0.0485(6) Uani d . 1
N N28 -0.0761(4) 0.64443(19) 0.10824(12) 0.0540(6) Uani d . 1
N N29 0.0649(4) 0.58592(19) 0.12805(12) 0.0539(6) Uani d D 1
N N30 0.1722(3) 0.56958(19) 0.08358(11) 0.0513(6) Uani d . 1
Cl Cl1 0.34362(10) 0.38846(6) 0.71439(3) 0.0497(2) Uani d . 1
O O11 0.3975(4) 0.4197(2) 0.65481(12) 0.0874(8) Uani d . 1
O O12 0.4636(4) 0.3152(2) 0.74296(16) 0.1075(11) Uani d . 1
O O13 0.1623(4) 0.3525(3) 0.70176(15) 0.1099(11) Uani d . 1
O O14 0.3557(5) 0.4722(3) 0.75703(19) 0.1274(13) 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
O1W Zn1 O1W 3_566 . 180.00(9)
O1W Zn1 N17 3_566 3_566 90.32(8)
O1W Zn1 N17 . 3_566 89.68(8)
O1W Zn1 N17 3_566 . 89.68(8)
O1W Zn1 N17 . . 90.32(8)
N17 Zn1 N17 3_566 . 180.00(4)
O1W Zn1 N11 3_566 3_566 89.32(8)
O1W Zn1 N11 . 3_566 90.68(8)
N17 Zn1 N11 3_566 3_566 77.40(8)
N17 Zn1 N11 . 3_566 102.60(8)
O1W Zn1 N11 3_566 . 90.68(8)
O1W Zn1 N11 . . 89.32(8)
N17 Zn1 N11 3_566 . 102.60(8)
N17 Zn1 N11 . . 77.40(8)
N11 Zn1 N11 3_566 . 180.00(9)
Zn1 O1W H1WA . . 113.6
Zn1 O1W H1WB . . 114.1
H1WA O1W H1WB . . 107.9
N19 C1 C2 . . 113.0(3)
N19 C1 C2' . . 108.8(8)
N19 C1 H1C . . 109.1
C2 C1 H1C . . 109.6
N19 C1 H1B . . 108.9
C2 C1 H1B . . 108.3
H1C C1 H1B . . 107.8
N19 C1 H1A' . . 109.6
C2' C1 H1A' . . 108.6
C2' C1 H1B' . . 111.6
H1A' C1 H1B' . . 108.1
C3 C2 C1 . . 110.2(3)
C3 C2 H2A . . 109.9
C1 C2 H2A . . 110.0
C3 C2 H2B . . 109.3
C1 C2 H2B . . 109.4
H2A C2 H2B . . 108.0
C3' C2' C1 . . 115.7(15)
C3' C2' H2A' . . 106.3
C1 C2' H2A' . . 106.9
C3' C2' H2B' . . 110.7
C1 C2' H2B' . . 109.7
H2A' C2' H2B' . . 107.1
C2 C3 N29 . . 108.8(3)
C2 C3 H3A . . 109.5
N29 C3 H3A . . 109.8
C2 C3 H3B . . 110.3
N29 C3 H3B . . 110.2
H3A C3 H3B . . 108.2
C2' C3' N29 . . 99.4(12)
C2' C3' H3A' . . 114.6
N29 C3' H3A' . . 113.1
C2' C3' H3B' . . 109.5
N29 C3' H3B' . . 110.4
H3A' C3' H3B' . . 109.4
N11 C10 C15 . . 123.4(2)
N11 C10 C16 . . 113.5(2)
C15 C10 C16 . . 123.0(2)
C12 N11 C10 . . 117.2(2)
C12 N11 Zn1 . . 127.24(17)
C10 N11 Zn1 . . 115.41(16)
N11 C12 C13 . . 122.5(3)
N11 C12 H12 . . 118.7
C13 C12 H12 . . 118.7
C14 C13 C12 . . 119.1(3)
C14 C13 H13 . . 120.5
C12 C13 H13 . . 120.5
C15 C14 C13 . . 119.1(3)
C15 C14 H14 . . 120.5
C13 C14 H14 . . 120.5
C10 C15 C14 . . 118.7(3)
C10 C15 H15 . . 120.7
C14 C15 H15 . . 120.7
N20 C16 N17 . . 112.2(2)
N20 C16 C10 . . 127.0(2)
N17 C16 C10 . . 120.9(2)
N18 N17 C16 . . 107.2(2)
N18 N17 Zn1 . . 140.15(17)
C16 N17 Zn1 . . 112.61(16)
N17 N18 N19 . . 104.8(2)
N18 N19 N20 . . 114.7(2)
N18 N19 C1 . . 121.8(2)
N20 N19 C1 . . 123.4(2)
C16 N20 N19 . . 101.1(2)
N21 C20 C25 . . 123.0(3)
N21 C20 C26 . . 116.6(2)
C25 C20 C26 . . 120.4(2)
C22 N21 C20 . . 116.9(2)
N21 C22 C23 . . 123.8(3)
N21 C22 H22 . . 118.1
C23 C22 H22 . . 118.1
C22 C23 C24 . . 118.6(3)
C22 C23 H23 . . 120.7
C24 C23 H23 . . 120.7
C25 C24 C23 . . 118.9(3)
C25 C24 H24 . . 120.6
C23 C24 H24 . . 120.6
C24 C25 C20 . . 118.8(3)
C24 C25 H25 . . 120.6
C20 C25 H25 . . 120.6
N30 C26 N27 . . 112.1(2)
N30 C26 C20 . . 122.2(2)
N27 C26 C20 . . 125.5(2)
N28 N27 C26 . . 106.2(2)
N29 N28 N27 . . 106.0(2)
N28 N29 N30 . . 114.3(2)
N28 N29 C3 . . 123.6(3)
N30 N29 C3 . . 121.5(3)
N28 N29 C3' . . 115.9(7)
N30 N29 C3' . . 119.4(9)
N29 N30 C26 . . 101.5(2)
O12 Cl1 O13 . . 111.2(2)
O12 Cl1 O14 . . 108.5(2)
O13 Cl1 O14 . . 110.3(2)
O12 Cl1 O11 . . 109.3(2)
O13 Cl1 O11 . . 109.19(18)
O14 Cl1 O11 . . 108.3(2)
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
Zn1 O1W 3_566 2.1079(18) ?
Zn1 O1W . 2.1079(18) y
Zn1 N17 3_566 2.149(2) ?
Zn1 N17 . 2.149(2) y
Zn1 N11 3_566 2.170(2) ?
Zn1 N11 . 2.170(2) y
O1W H1WA . 0.8646 ?
O1W H1WB . 0.8638 ?
C1 N19 . 1.470(3) ?
C1 C2 . 1.519(4) ?
C1 C2' . 1.569(17) ?
C1 H1C . 0.9700 ?
C1 H1B . 0.9700 ?
C1 H1A' . 0.9700 ?
C1 H1B' . 0.9700 ?
C2 C3 . 1.503(5) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9699 ?
C2' C3' . 1.485(17) ?
C2' H2A' . 0.9700 ?
C2' H2B' . 0.9700 ?
C3 N29 . 1.505(4) ?
C3 H3A . 0.9701 ?
C3 H3B . 0.9700 ?
C3' N29 . 1.534(14) ?
C3' H3A' . 0.9699 ?
C3' H3B' . 0.9700 ?
C10 N11 . 1.353(3) ?
C10 C15 . 1.373(4) ?
C10 C16 . 1.470(3) ?
N11 C12 . 1.342(3) ?
C12 C13 . 1.385(4) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.381(4) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.375(4) ?
C14 H14 . 0.9300 ?
C15 H15 . 0.9300 ?
C16 N20 . 1.325(3) ?
C16 N17 . 1.341(3) ?
N17 N18 . 1.319(3) ?
N18 N19 . 1.319(3) ?
N19 N20 . 1.331(3) ?
C20 N21 . 1.343(3) ?
C20 C25 . 1.385(4) ?
C20 C26 . 1.471(4) ?
N21 C22 . 1.339(4) ?
C22 C23 . 1.373(5) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.383(5) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.375(4) ?
C24 H24 . 0.9300 ?
C25 H25 . 0.9300 ?
C26 N30 . 1.331(3) ?
C26 N27 . 1.348(3) ?
N27 N28 . 1.321(3) ?
N28 N29 . 1.313(3) ?
N29 N30 . 1.327(3) ?
Cl1 O12 . 1.387(3) ?
Cl1 O13 . 1.406(3) ?
Cl1 O14 . 1.420(3) ?
Cl1 O11 . 1.421(3) ?
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
O1W H1WA O11 . 0.86 2.01 2.869(3) 172 y
O1W H1WB N21 2_545 0.86 1.97 2.833(3) 178 y
