#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/12/2211274.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_2211274
loop_
_publ_author_name
'Avila, Vanessa'
'Tiekink, Edward R. T.'
_publ_section_title
;catena-Poly[[bis(O,O'-diisopropyl
 dithiophosphato-κ²S,S')zinc(II)]-μ-1,2-bis(3-pyridylmethylene)hydrazine-κ²N:N']
;
_journal_coeditor_code           AT2170
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3530
_journal_page_last               m3531
_journal_paper_doi               10.1107/S160053680605001X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Zn (C6 H14 O2 P S2)2 (C12 H10 N4)]'
_chemical_formula_moiety         'C24 H38 N4 O4 P2 S4 Zn'
_chemical_formula_sum            'C24 H38 N4 O4 P2 S4 Zn'
_chemical_formula_weight         702.13
_chemical_name_systematic
;
catena-Poly[[bis(O,O'-diisopropyl dithiophosphato-κ²S,S')zinc(II)]-
μ-1,2-bis(3-pyridylmethylene)hydrazine-κ²N:N']
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 108.712(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.809(3)
_cell_length_b                   11.243(3)
_cell_length_c                   12.933(3)
_cell_measurement_reflns_used    5726
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     1626.3(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'PATTY in DIRDIF92 (Beurskens et al.,  1992)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  AFC12Κ/SATURN724
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.014
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34154
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.46
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.045
_refine_ls_R_factor_gt           0.044
_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)+(0.0527P)²+4.0311P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.108
_refine_ls_wR_factor_ref         0.109
_reflns_number_gt                2793
_reflns_number_total             2864
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2170.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2211274
_cod_database_fobs_code          2211274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Zn Zn 0.0000 0.0000 0.5000 0.01853(16) Uani d S 1
S S1 -0.19705(6) 0.06014(7) 0.52511(6) 0.02023(19) Uani d . 1
S S2 -0.05145(7) -0.19684(7) 0.57289(6) 0.0223(2) Uani d . 1
P P1 -0.18488(7) -0.10211(7) 0.59145(6) 0.0184(2) Uani d . 1
O O1 -0.1666(2) -0.0984(2) 0.71783(17) 0.0247(5) Uani d . 1
O O2 -0.31083(19) -0.1673(2) 0.54779(17) 0.0246(5) Uani d . 1
N N1 0.0971(2) 0.0659(2) 0.6675(2) 0.0190(5) Uani d . 1
N N2 0.4483(2) 0.0355(2) 0.9795(2) 0.0215(5) Uani d . 1
C C1 -0.2475(4) -0.0309(4) 0.7608(3) 0.0381(9) Uani d . 1
H H1 -0.2990 0.0233 0.7036 0.046 Uiso calc R 1
C C2 -0.1700(6) 0.0393(5) 0.8562(5) 0.0750(17) Uani d . 1
H H2A -0.1232 0.0974 0.8305 0.113 Uiso calc R 1
H H2B -0.1158 -0.0147 0.9086 0.113 Uiso calc R 1
H H2C -0.2205 0.0811 0.8916 0.113 Uiso calc R 1
C C3 -0.3229(5) -0.1198(6) 0.7965(5) 0.0791(18) Uani d . 1
H H3A -0.3738 -0.1630 0.7327 0.119 Uiso calc R 1
H H3B -0.3732 -0.0780 0.8321 0.119 Uiso calc R 1
H H3C -0.2708 -0.1761 0.8480 0.119 Uiso calc R 1
C C4 -0.3825(3) -0.1747(3) 0.4330(3) 0.0368(9) Uani d . 1
H H4 -0.3746 -0.0998 0.3942 0.044 Uiso calc R 1
C C5 -0.5110(4) -0.1869(6) 0.4376(5) 0.0735(17) Uani d . 1
H H5A -0.5312 -0.1163 0.4725 0.110 Uiso calc R 1
H H5B -0.5163 -0.2578 0.4799 0.110 Uiso calc R 1
H H5C -0.5671 -0.1944 0.3633 0.110 Uiso calc R 1
C C6 -0.3505(4) -0.2757(5) 0.3800(4) 0.0668(16) Uani d . 1
H H6A -0.2685 -0.2660 0.3787 0.100 Uiso calc R 1
H H6B -0.4053 -0.2816 0.3051 0.100 Uiso calc R 1
H H6C -0.3558 -0.3482 0.4202 0.100 Uiso calc R 1
C C7 0.1965(3) 0.0119(3) 0.7300(2) 0.0197(6) Uani d . 1
H H7 0.2192 -0.0610 0.7051 0.024 Uiso calc R 1
C C8 0.2683(3) 0.0572(3) 0.8298(2) 0.0200(6) Uani d . 1
C C9 0.2326(3) 0.1620(3) 0.8677(2) 0.0234(7) Uani d . 1
H H9 0.2789 0.1953 0.9356 0.028 Uiso calc R 1
C C10 0.1287(3) 0.2168(3) 0.8047(3) 0.0249(7) Uani d . 1
H H10 0.1017 0.2877 0.8292 0.030 Uiso calc R 1
C C11 0.0641(3) 0.1666(3) 0.7049(3) 0.0221(6) Uani d . 1
H H11 -0.0065 0.2056 0.6614 0.027 Uiso calc R 1
C C12 0.3795(3) -0.0047(3) 0.8897(3) 0.0223(7) Uani d . 1
H H12 0.4003 -0.0760 0.8607 0.027 Uiso calc R 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'
P P 0.1023 0.0942 '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'
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
S1 Zn S2 . . 81.23(3) y
S1 Zn N1 . . 89.65(7) y
S1 Zn S2 . 3_556 98.77(3) y
S1 Zn N1 3_556 . 90.35(7) y
S2 Zn N1 . . 92.20(7) y
S2 Zn N1 . 3_556 87.80(7) y
N1 Zn S2 . 3_556 87.80(7) ?
S1 Zn S2 . 3_556 98.77(3) ?
S1 Zn S1 3_556 . 180 ?
N1 Zn N1 3_556 . 180 ?
S2 Zn S2 . 3_556 180 ?
N1 Zn S2 3_556 3_556 92.20(7) ?
S1 Zn S2 3_556 3_556 81.23(3) ?
N1 Zn S1 3_556 3_556 89.65(7) ?
N1 Zn S1 . 3_556 90.35(7) ?
Zn S1 P1 . . 82.50(3) y
Zn S2 P1 . . 82.61(4) y
O1 P1 O2 . . 100.45(12) ?
O1 P1 S2 . . 106.86(9) ?
O2 P1 S2 . . 113.53(9) ?
O1 P1 S1 . . 112.75(9) ?
O2 P1 S1 . . 109.72(9) ?
S2 P1 S1 . . 112.89(5) ?
C1 O1 P1 . . 121.2(2) ?
C4 O2 P1 . . 124.0(2) ?
C11 N1 C7 . . 117.8(3) ?
C11 N1 Zn . . 120.94(19) ?
C7 N1 Zn . . 121.0(2) ?
C12 N2 N2 . 3_657 111.4(3) ?
O1 C1 C3 . . 107.2(4) ?
O1 C1 C2 . . 106.5(4) ?
C3 C1 C2 . . 111.2(4) ?
O1 C1 H1 . . 110.6 ?
C3 C1 H1 . . 110.6 ?
C2 C1 H1 . . 110.6 ?
C1 C2 H2A . . 109.5 ?
C1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
C1 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
C1 C3 H3A . . 109.5 ?
C1 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C1 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C6 C4 O2 . . 112.0(3) ?
C6 C4 C5 . . 111.1(4) ?
O2 C4 C5 . . 102.9(3) ?
C6 C4 H4 . . 110.2 ?
O2 C4 H4 . . 110.2 ?
C5 C4 H4 . . 110.2 ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
C4 C6 H6A . . 109.5 ?
C4 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C4 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N1 C7 C8 . . 123.3(3) ?
N1 C7 H7 . . 118.3 ?
C8 C7 H7 . . 118.3 ?
C7 C8 C9 . . 118.1(3) ?
C7 C8 C12 . . 119.4(3) ?
C9 C8 C12 . . 122.4(3) ?
C10 C9 C8 . . 118.8(3) ?
C10 C9 H9 . . 120.6 ?
C8 C9 H9 . . 120.6 ?
C9 C10 C11 . . 119.1(3) ?
C9 C10 H10 . . 120.5 ?
C11 C10 H10 . . 120.5 ?
N1 C11 C10 . . 122.8(3) ?
N1 C11 H11 . . 118.6 ?
C10 C11 H11 . . 118.6 ?
N2 C12 C8 . . 121.1(3) ?
N2 C12 H12 . . 119.5 ?
C8 C12 H12 . . 119.5 ?
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 S1 . 2.5420(9) y
Zn S2 . 2.5540(9) y
Zn N1 3_556 2.228(2) ?
Zn N1 . 2.228(2) y
Zn S1 3_556 2.5420(9) ?
Zn S2 3_556 2.5540(9) ?
S1 P1 . 2.0013(11) y
S2 P1 . 1.9792(11) y
P1 O1 . 1.579(2) ?
P1 O2 . 1.590(2) ?
O1 C1 . 1.462(4) ?
O2 C4 . 1.457(4) ?
N1 C11 . 1.337(4) ?
N1 C7 . 1.338(4) ?
N2 N2 3_657 1.412(5) y
N2 C12 . 1.268(4) y
C1 C3 . 1.506(7) ?
C1 C2 . 1.503(7) ?
C1 H1 . 1.0000 ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C4 C6 . 1.438(6) ?
C4 C5 . 1.543(6) ?
C4 H4 . 1.0000 ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 C8 . 1.393(4) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.393(4) ?
C8 C12 . 1.468(4) ?
C9 C10 . 1.381(5) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.391(4) ?
C10 H10 . 0.9500 ?
C11 H11 . 0.9500 ?
C12 H12 . 0.9500 ?
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
N1 Zn S1 P1 3_556 93.37(7)
N1 Zn S1 P1 . -86.63(7)
S2 Zn S1 P1 . 5.65(3)
S2 Zn S1 P1 3_556 -174.35(3)
N1 Zn S2 P1 3_556 -96.40(7)
N1 Zn S2 P1 . 83.59(7)
S1 Zn S2 P1 3_556 174.29(3)
S1 Zn S2 P1 . -5.71(3)
Zn S2 P1 O1 . -116.71(9)
Zn S2 P1 O2 . 133.49(10)
Zn S2 P1 S1 . 7.80(4)
Zn S1 P1 O1 . 113.39(10)
Zn S1 P1 O2 . -135.55(9)
Zn S1 P1 S2 . -7.83(4)
O2 P1 O1 C1 . -63.8(3)
S2 P1 O1 C1 . 177.5(2)
S1 P1 O1 C1 . 52.9(3)
O1 P1 O2 C4 . 167.9(3)
S2 P1 O2 C4 . -78.4(3)
S1 P1 O2 C4 . 49.0(3)
S1 Zn N1 C11 3_556 139.6(2)
S1 Zn N1 C11 . -40.4(2)
S2 Zn N1 C11 . -121.6(2)
S2 Zn N1 C11 3_556 58.4(2)
S1 Zn N1 C7 3_556 -34.3(2)
S1 Zn N1 C7 . 145.7(2)
S2 Zn N1 C7 . 64.4(2)
S2 Zn N1 C7 3_556 -115.6(2)
P1 O1 C1 C3 . 107.7(4)
P1 O1 C1 C2 . -133.2(3)
P1 O2 C4 C6 . 87.3(4)
P1 O2 C4 C5 . -153.3(3)
C11 N1 C7 C8 . -1.9(4)
Zn N1 C7 C8 . 172.2(2)
N1 C7 C8 C9 . 2.1(5)
N1 C7 C8 C12 . -176.4(3)
C7 C8 C9 C10 . -0.5(4)
C12 C8 C9 C10 . 177.9(3)
C8 C9 C10 C11 . -1.0(5)
C7 N1 C11 C10 . 0.3(4)
Zn N1 C11 C10 . -173.9(2)
C9 C10 C11 N1 . 1.2(5)
N2 N2 C12 C8 3_657 -177.8(3)
C7 C8 C12 N2 . 178.4(3)
C9 C8 C12 N2 . 0.0(5)
