#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/61/2226172.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_2226172
loop_
_publ_author_name
'Wilseck, Zachary M.'
'LaDuca, Robert L.'
_publ_section_title
;
 Poly[[μ₄-bis(4-pyridylcarbonyl)piperazine-κ⁴N:N':O:O']bis(thiocyanato-κN)cobalt(II)]
;
_journal_coeditor_code           HY2308
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m713
_journal_paper_doi               10.1107/S160053681001915X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Co (N C S)2 (C16 H16 N4 O2)]'
_chemical_formula_moiety         'C18 H16 Co N6 O2 S2'
_chemical_formula_sum            'C18 H16 Co N6 O2 S2'
_chemical_formula_weight         471.44
_chemical_name_systematic
;
Poly[[μ₄-bis(4-pyridylcarbonyl)piperazine-
κ⁴N:N':O:O']bis(thiocyanato-
κN)cobalt(II)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.080(2)
_cell_angle_beta                 102.264(2)
_cell_angle_gamma                119.136(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7410(14)
_cell_length_b                   7.8943(15)
_cell_length_c                   9.801(3)
_cell_measurement_reflns_used    6955
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.27
_cell_volume                     479.58(19)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2007)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6955
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.9277
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             241
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.554
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0372
_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)+(0.0458P)²+0.1032P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                1646
_reflns_number_total             1753
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2308.cif
_cod_data_source_block           I
_cod_original_cell_volume        479.58(18)
_cod_database_code               2226172
_cod_database_fobs_code          2226172
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Co Co1 0.5000 0.5000 0.0000 0.03453(19) Uani d S 1 . .
S S1 0.75373(12) 1.06782(11) 0.44195(8) 0.0504(2) Uani d . 1 . .
N N1 0.2531(3) 0.5500(3) -0.0887(2) 0.0359(4) Uani d . 1 . .
N N2 -0.3493(3) 0.6090(3) -0.3539(2) 0.0384(5) Uani d . 1 . .
N N3 0.6324(3) 0.7503(3) 0.1850(2) 0.0409(5) Uani d . 1 . .
C C1 0.0560(4) 0.3911(4) -0.1764(3) 0.0391(5) Uani d . 1 . .
H H1 0.0304 0.2594 -0.2075 0.047 Uiso calc R 1 . .
C C2 -0.1098(4) 0.4140(4) -0.2225(3) 0.0389(5) Uani d . 1 . .
H H2 -0.2440 0.2996 -0.2828 0.047 Uiso calc R 1 . .
C C3 -0.0749(4) 0.6093(4) -0.1781(2) 0.0364(5) Uani d . 1 . .
C C4 0.1289(4) 0.7751(4) -0.0883(3) 0.0402(5) Uani d . 1 . .
H H4 0.1589 0.9085 -0.0564 0.048 Uiso calc R 1 . .
C C5 0.2849(4) 0.7384(4) -0.0476(3) 0.0402(5) Uani d . 1 . .
H H5 0.4208 0.8506 0.0119 0.048 Uiso calc R 1 . .
C C6 -0.2526(4) 0.6408(3) -0.2131(3) 0.0366(5) Uani d . 1 . .
C C7 -0.5284(4) 0.6312(4) -0.3955(3) 0.0418(6) Uani d . 1 . .
H H7A -0.4879 0.7492 -0.4281 0.050 Uiso calc R 1 . .
H H7B -0.5682 0.6550 -0.3099 0.050 Uiso calc R 1 . .
C C8 -0.2853(4) 0.5629(4) -0.4802(3) 0.0407(6) Uani d . 1 . .
H H8A -0.1706 0.5438 -0.4478 0.049 Uiso calc R 1 . .
H H8B -0.2349 0.6781 -0.5163 0.049 Uiso calc R 1 . .
C C9 0.6850(4) 0.8842(4) 0.2928(3) 0.0368(5) Uani d . 1 . .
O O1 -0.3046(2) 0.6962(2) -0.10853(17) 0.0385(4) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
N3 Co1 N3 2_665 . 180.0 ?
N3 Co1 N1 2_665 . 90.06(8) ?
N3 Co1 N1 . . 89.94(8) ?
N3 Co1 N1 2_665 2_665 89.94(8) ?
N3 Co1 N1 . 2_665 90.06(8) ?
N1 Co1 N1 . 2_665 180.00(9) ?
N3 Co1 O1 2_665 2_565 90.43(7) ?
N3 Co1 O1 . 2_565 89.57(7) ?
N1 Co1 O1 . 2_565 89.79(7) ?
N1 Co1 O1 2_665 2_565 90.21(7) ?
N3 Co1 O1 2_665 1_655 89.57(7) ?
N3 Co1 O1 . 1_655 90.43(7) ?
N1 Co1 O1 . 1_655 90.21(7) ?
N1 Co1 O1 2_665 1_655 89.79(7) ?
O1 Co1 O1 2_565 1_655 180.00(9) ?
C1 N1 C5 . . 116.8(2) ?
C1 N1 Co1 . . 121.35(15) ?
C5 N1 Co1 . . 121.59(15) ?
C6 N2 C7 . . 121.13(19) ?
C6 N2 C8 . . 125.8(2) ?
C7 N2 C8 . . 112.94(18) ?
C9 N3 Co1 . . 171.96(19) ?
N1 C1 C2 . . 123.1(2) ?
N1 C1 H1 . . 118.4 ?
C2 C1 H1 . . 118.4 ?
C1 C2 C3 . . 119.4(2) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C2 C3 C4 . . 118.0(2) ?
C2 C3 C6 . . 121.7(2) ?
C4 C3 C6 . . 120.1(2) ?
C5 C4 C3 . . 118.8(2) ?
C5 C4 H4 . . 120.6 ?
C3 C4 H4 . . 120.6 ?
N1 C5 C4 . . 123.9(2) ?
N1 C5 H5 . . 118.0 ?
C4 C5 H5 . . 118.0 ?
O1 C6 N2 . . 122.7(2) ?
O1 C6 C3 . . 118.7(2) ?
N2 C6 C3 . . 118.7(2) ?
N2 C7 C8 . 2_464 109.9(2) ?
N2 C7 H7A . . 109.7 ?
C8 C7 H7A 2_464 . 109.7 ?
N2 C7 H7B . . 109.7 ?
C8 C7 H7B 2_464 . 109.7 ?
H7A C7 H7B . . 108.2 ?
N2 C8 C7 . 2_464 109.98(19) ?
N2 C8 H8A . . 109.7 ?
C7 C8 H8A 2_464 . 109.7 ?
N2 C8 H8B . . 109.7 ?
C7 C8 H8B 2_464 . 109.7 ?
H8A C8 H8B . . 108.2 ?
N3 C9 S1 . . 179.0(2) ?
C6 O1 Co1 . 1_455 127.28(15) ?
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
Co1 N1 . 2.1739(19) y
Co1 N3 . 2.026(2) y
Co1 O1 2_565 2.2034(16) y
S1 C9 . 1.620(3) ?
N1 C1 . 1.343(3) ?
N1 C5 . 1.344(3) ?
N2 C6 . 1.331(3) ?
N2 C7 . 1.464(3) ?
N2 C8 . 1.475(3) ?
N3 C9 . 1.170(3) ?
C1 C2 . 1.377(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.388(3) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.391(3) ?
C3 C6 . 1.496(3) ?
C4 C5 . 1.372(4) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 O1 . 1.256(3) ?
C7 C8 2_464 1.515(3) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 C7 2_464 1.515(3) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
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
N3 Co1 N1 C1 2_665 . . . 32.05(18) ?
N3 Co1 N1 C1 . . . . -147.95(18) ?
O1 Co1 N1 C1 2_565 . . . -58.38(17) ?
O1 Co1 N1 C1 1_655 . . . 121.62(17) ?
N3 Co1 N1 C5 2_665 . . . -154.13(18) ?
N3 Co1 N1 C5 . . . . 25.87(18) ?
O1 Co1 N1 C5 2_565 . . . 115.44(18) ?
O1 Co1 N1 C5 1_655 . . . -64.56(18) ?
C5 N1 C1 C2 . . . . -0.9(3) ?
Co1 N1 C1 C2 . . . . 173.23(17) ?
N1 C1 C2 C3 . . . . 0.3(4) ?
C1 C2 C3 C4 . . . . 0.2(3) ?
C1 C2 C3 C6 . . . . -174.4(2) ?
C2 C3 C4 C5 . . . . -0.2(3) ?
C6 C3 C4 C5 . . . . 174.5(2) ?
C1 N1 C5 C4 . . . . 0.9(3) ?
Co1 N1 C5 C4 . . . . -173.16(18) ?
C3 C4 C5 N1 . . . . -0.4(4) ?
C7 N2 C6 O1 . . . . -1.9(4) ?
C8 N2 C6 O1 . . . . 174.0(2) ?
C7 N2 C6 C3 . . . . 178.1(2) ?
C8 N2 C6 C3 . . . . -6.1(3) ?
C2 C3 C6 O1 . . . . 110.4(3) ?
C4 C3 C6 O1 . . . . -64.0(3) ?
C2 C3 C6 N2 . . . . -69.5(3) ?
C4 C3 C6 N2 . . . . 116.0(3) ?
C6 N2 C7 C8 . . . 2_464 -126.9(2) ?
C8 N2 C7 C8 . . . 2_464 56.8(3) ?
C6 N2 C8 C7 . . . 2_464 127.0(2) ?
C7 N2 C8 C7 . . . 2_464 -56.8(3) ?
N2 C6 O1 Co1 . . . 1_455 100.8(2) ?
C3 C6 O1 Co1 . . . 1_455 -79.1(2) ?
