#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/67/2226794.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_2226794
loop_
_publ_author_name
'Reinert, Thorben'
'Boeckmann, Jan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 catena-Poly[[μ₃-hydroxido-tetra-μ₂-pyridazine-1:2κ⁴N:N';1:3κ²N:N';2:3κ²N:N'-tetrakis(selenocyanato)-1κN,2κN,3κ²N-trizinc(II)]-μ-cyanido-1:2'κ²C:N]
;
_journal_coeditor_code           BT5302
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1018
_journal_page_last               m1019
_journal_paper_doi               10.1107/S1600536810029107
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Zn3 (C N Se)4 (O H) (C N) (C4 H4 N2)4]'
_chemical_formula_moiety         'C21 H17 N13 O Se4 Zn3'
_chemical_formula_sum            'C21 H17 N13 O Se4 Zn3'
_chemical_formula_weight         979.43
_chemical_name_systematic
;
catena-Poly[[μ₃-hydroxido-tetra-μ₂-pyridazine-
1:2κ⁴N:N';1:3κ²N:N';
2:3κ²N:N'-tetrakis(selenocyanato)-
1κN,2κN,3κ²N-
trizinc(II)]-μ-cyanido-1:2'κ²C:N]
;
_space_group_IT_number           40
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2a'
_symmetry_space_group_name_H-M   'A m a 2'
_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                   15.6156(12)
_cell_length_b                   22.6489(16)
_cell_length_c                   8.6626(5)
_cell_measurement_reflns_used    8001
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.5
_cell_volume                     3063.8(4)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2010)
;
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi 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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22283
_diffrn_reflns_theta_full        28.11
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.123
_exptl_absorpt_correction_T_max  0.5032
_exptl_absorpt_correction_T_min  0.1961
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-Shape and X-Red32 ;Stoe, 2008)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.652
_refine_ls_abs_structure_details 'Flack  (1983), 1747 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.012(10)
_refine_ls_extinction_coef       0.00122(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3752
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0346P)²+4.6032P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                3588
_reflns_number_total             3752
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt5302.cif
_cod_data_source_block           I
_cod_database_code               2226794
_cod_database_fobs_code          2226794
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-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
Zn Zn1 0.7500 0.69593(2) 0.31561(6) 0.01454(11) Uani d S 1 . .
Zn Zn2 0.63959(2) 0.565314(15) 0.35942(4) 0.01401(9) Uani d . 1 . .
O O1 0.7500 0.61613(13) 0.4136(4) 0.0124(6) Uani d S 1 . .
H H1 0.7500 0.619(4) 0.500(12) 0.05(3) Uiso d S 1 . .
Se Se1 0.7500 0.70340(2) -0.25158(6) 0.02447(12) Uani d S 1 . .
C C1 0.7500 0.6962(2) -0.0473(6) 0.0211(10) Uani d S 1 . .
N N1 0.7500 0.6936(2) 0.0866(6) 0.0283(10) Uani d S 1 . .
Se Se2 0.7500 0.89017(2) 0.57363(7) 0.02695(13) Uani d S 1 . .
C C2 0.7500 0.8214(2) 0.4730(6) 0.0180(9) Uani d S 1 . .
N N2 0.7500 0.77724(17) 0.4100(5) 0.0209(9) Uani d S 1 . .
Se Se3 0.45849(2) 0.591502(15) 0.83059(4) 0.02298(9) Uani d . 1 . .
C C3 0.5344(2) 0.58566(15) 0.6754(4) 0.0198(7) Uani d . 1 . .
N N3 0.58164(18) 0.58100(13) 0.5733(4) 0.0210(6) Uani d . 1 . .
N N11 0.60825(17) 0.69737(12) 0.3112(4) 0.0203(6) Uani d . 1 . .
N N12 0.56988(17) 0.64629(12) 0.2776(3) 0.0161(5) Uani d . 1 . .
C C11 0.4879(2) 0.64663(16) 0.2356(5) 0.0244(7) Uani d . 1 . .
H H11 0.4619 0.6103 0.2074 0.029 Uiso calc R 1 . .
C C12 0.4386(2) 0.69777(17) 0.2312(6) 0.0334(10) Uani d . 1 . .
H H12 0.3799 0.6964 0.2026 0.040 Uiso calc R 1 . .
C C13 0.4770(2) 0.74982(17) 0.2690(7) 0.0410(12) Uani d . 1 . .
H H13 0.4463 0.7860 0.2689 0.049 Uiso calc R 1 . .
C C14 0.5641(2) 0.74755(16) 0.3081(6) 0.0339(10) Uani d . 1 . .
H H14 0.5927 0.7833 0.3334 0.041 Uiso calc R 1 . .
N N21 0.70660(17) 0.48500(12) 0.4454(3) 0.0160(5) Uani d . 1 . .
C C21 0.6652(2) 0.43725(16) 0.4926(5) 0.0242(7) Uani d . 1 . .
H H21 0.6043 0.4381 0.4938 0.029 Uiso calc R 1 . .
C C22 0.7066(2) 0.38574(17) 0.5405(5) 0.0302(8) Uani d . 1 . .
H H22 0.6751 0.3519 0.5720 0.036 Uiso calc R 1 . .
N N31 0.70651(16) 0.55138(11) 0.1423(3) 0.0140(5) Uani d . 1 . .
C C31 0.6645(2) 0.54118(15) 0.0115(4) 0.0198(6) Uani d . 1 . .
H H31 0.6037 0.5408 0.0133 0.024 Uiso calc R 1 . .
C C32 0.7064(2) 0.53091(16) -0.1289(4) 0.0222(7) Uani d . 1 . .
H H32 0.6750 0.5242 -0.2211 0.027 Uiso calc R 1 . .
N N41 0.53181(18) 0.51316(13) 0.2907(4) 0.0168(6) Uani d P 0.50 . .
C C41 0.53181(18) 0.51316(13) 0.2907(4) 0.0168(6) Uani d P 0.50 . .
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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 Zn1 O1 . . 113.64(18) y
N1 Zn1 N2 . . 115.5(2) y
O1 Zn1 N2 . . 130.90(17) y
N1 Zn1 N11 . 4_655 89.03(9) y
O1 Zn1 N11 . 4_655 91.19(7) y
N2 Zn1 N11 . 4_655 89.64(7) y
N1 Zn1 N11 . . 89.03(9) y
O1 Zn1 N11 . . 91.19(7) y
N2 Zn1 N11 . . 89.64(7) y
N11 Zn1 N11 4_655 . 177.39(16) y
N3 Zn2 O1 . . 93.64(12) y
N3 Zn2 N41 . . 89.99(12) y
O1 Zn2 N41 . . 176.37(13) y
N3 Zn2 N31 . . 176.69(11) y
O1 Zn2 N31 . . 83.09(12) y
N41 Zn2 N31 . . 93.28(11) y
N3 Zn2 N21 . . 92.62(11) y
O1 Zn2 N21 . . 89.28(10) y
N41 Zn2 N21 . . 90.67(11) y
N31 Zn2 N21 . . 86.85(10) y
N3 Zn2 N12 . . 86.05(11) y
O1 Zn2 N12 . . 91.18(10) y
N41 Zn2 N12 . . 88.96(11) y
N31 Zn2 N12 . . 94.50(10) y
N21 Zn2 N12 . . 178.62(10) y
Zn1 O1 Zn2 . . 113.35(11) y
Zn1 O1 Zn2 . 4_655 113.35(11) y
Zn2 O1 Zn2 . 4_655 108.42(14) y
Zn1 O1 H1 . . 110(6) ?
Zn2 O1 H1 . . 106(3) ?
Zn2 O1 H1 4_655 . 106(3) ?
N1 C1 Se1 . . 177.7(5) ?
C1 N1 Zn1 . . 175.6(5) ?
N2 C2 Se2 . . 179.4(4) ?
C2 N2 Zn1 . . 175.3(4) ?
N3 C3 Se3 . . 178.2(3) ?
C3 N3 Zn2 . . 165.6(3) ?
C14 N11 N12 . . 120.3(3) ?
C14 N11 Zn1 . . 122.1(2) ?
N12 N11 Zn1 . . 116.09(19) ?
C11 N12 N11 . . 119.1(3) ?
C11 N12 Zn2 . . 123.8(2) ?
N11 N12 Zn2 . . 114.92(19) ?
N12 C11 C12 . . 123.0(3) ?
N12 C11 H11 . . 118.5 ?
C12 C11 H11 . . 118.5 ?
C13 C12 C11 . . 118.0(3) ?
C13 C12 H12 . . 121.0 ?
C11 C12 H12 . . 121.0 ?
C12 C13 C14 . . 117.0(3) ?
C12 C13 H13 . . 121.5 ?
C14 C13 H13 . . 121.5 ?
N11 C14 C13 . . 122.6(3) ?
N11 C14 H14 . . 118.7 ?
C13 C14 H14 . . 118.7 ?
C21 N21 N21 . 4_655 119.2(2) ?
C21 N21 Zn2 . . 122.7(2) y
N21 N21 Zn2 4_655 . 118.03(7) ?
N21 C21 C22 . . 123.2(3) ?
N21 C21 H21 . . 118.4 ?
C22 C21 H21 . . 118.4 ?
C22 C22 C21 4_655 . 117.6(2) ?
C22 C22 H22 4_655 . 121.2 ?
C21 C22 H22 . . 121.2 ?
C31 N31 N31 . 4_655 119.55(18) ?
C31 N31 Zn2 . . 121.7(2) y
N31 N31 Zn2 4_655 . 118.72(7) ?
N31 C31 C32 . . 122.6(3) ?
N31 C31 H31 . . 118.7 ?
C32 C31 H31 . . 118.7 ?
C32 C32 C31 4_655 . 117.84(19) ?
C32 C32 H32 4_655 . 121.1 ?
C31 C32 H32 . . 121.1 ?
C41 N41 N41 2_665 2_665 0.0(4) ?
C41 N41 Zn2 2_665 . 163.36(12) ?
N41 N41 Zn2 2_665 . 163.36(12) y
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 N1 . 1.985(5) y
Zn1 O1 . 1.997(3) y
Zn1 N2 . 2.015(4) y
Zn1 N11 4_655 2.214(3) ?
Zn1 N11 . 2.214(3) y
Zn2 N3 . 2.092(3) y
Zn2 O1 . 2.1254(19) y
Zn2 N41 . 2.141(3) y
Zn2 N31 . 2.174(3) y
Zn2 N21 . 2.227(3) y
Zn2 N12 . 2.247(3) y
O1 Zn2 4_655 2.1254(19) ?
O1 H1 . 0.75(10) ?
Se1 C1 . 1.777(5) ?
C1 N1 . 1.161(7) ?
Se2 C2 . 1.784(5) ?
C2 N2 . 1.140(7) ?
Se3 C3 . 1.797(4) ?
C3 N3 . 1.157(5) ?
N11 C14 . 1.330(4) ?
N11 N12 . 1.335(4) ?
N12 C11 . 1.331(4) ?
C11 C12 . 1.392(5) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.363(5) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.402(5) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
N21 C21 . 1.325(4) ?
N21 N21 4_655 1.355(5) ?
C21 C22 . 1.398(5) ?
C21 H21 . 0.9500 ?
C22 C22 4_655 1.355(8) ?
C22 H22 . 0.9500 ?
N31 C31 . 1.330(4) ?
N31 N31 4_655 1.358(5) ?
C31 C32 . 1.400(5) ?
C31 H31 . 0.9500 ?
C32 C32 4_655 1.363(7) ?
C32 H32 . 0.9500 ?
N41 C41 2_665 1.159(6) ?
N41 N41 2_665 1.159(6) ?
