#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/65/2226516.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_2226516
loop_
_publ_author_name
'Wriedt, Mario'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Poly[tetrakis(selenocyanato-κN)bis(methanol-κO)tris(μ-pyrimidine-κ²N:N')dicobalt(II)]
;
_journal_coeditor_code           HY2313
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m742
_journal_paper_doi               10.1107/S160053681002060X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Co2 (C N Se)4 (C4 H4 N2)3 (C H4 O)2]'
_chemical_formula_moiety         'C9 H10 Co N5 O Se2'
_chemical_formula_sum            'C9 H10 Co N5 O Se2'
_chemical_formula_weight         421.07
_chemical_name_systematic
;
Poly[tetrakis(selenocyanato-κN)bis(methanol-κO)tris(μ-
pyrimidine-κ²N:N')dicobalt(II)]
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 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            16
_cell_length_a                   20.4069(8)
_cell_length_b                   33.0633(15)
_cell_length_c                   8.3750(3)
_cell_measurement_reflns_used    18545
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.35
_cell_volume                     5650.8(4)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'ω 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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18545
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.362
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.352
_refine_ls_abs_structure_details 'Flack (1983), 1579 Friedel pairs'
_refine_ls_abs_structure_Flack   0.057(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0380
_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)+(0.0286P)²+8.8704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                3067
_reflns_number_total             3391
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2313.cif
_cod_data_source_block           I
_cod_database_code               2226516
_cod_database_fobs_code          2226516
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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 0.60574(2) 0.227474(17) 0.78759(6) 0.03270(12) Uani d . 1 . .
N N1 0.55104(15) 0.27269(10) 0.6504(4) 0.0360(8) Uani d . 1 . .
N N2 0.47521(15) 0.28919(10) 0.4458(5) 0.0382(7) Uani d . 1 . .
C C1 0.50711(17) 0.26316(13) 0.5388(6) 0.0374(9) Uani d . 1 . .
H H1 0.4979 0.2358 0.5246 0.045 Uiso calc R 1 . .
C C2 0.4883(2) 0.32854(13) 0.4677(6) 0.0412(9) Uani d . 1 . .
H H2 0.4672 0.3477 0.4048 0.049 Uiso calc R 1 . .
C C3 0.5320(2) 0.34078(14) 0.5813(6) 0.0459(11) Uani d . 1 . .
H H3 0.5410 0.3681 0.5959 0.055 Uiso calc R 1 . .
C C4 0.5623(2) 0.31226(13) 0.6730(6) 0.0434(10) Uani d . 1 . .
H H4 0.5912 0.3204 0.7526 0.052 Uiso calc R 1 . .
N N11 0.69371(15) 0.24124(11) 0.6493(4) 0.0352(8) Uani d . 1 . .
C C11 0.7500 0.2500 0.7228(7) 0.0372(12) Uani d S 1 . .
H H11 0.7500 0.2500 0.8339 0.045 Uiso calc SR 1 . .
C C13 0.7500 0.2500 0.4059(8) 0.061(2) Uani d S 1 . .
H H13 0.7500 0.2500 0.2948 0.074 Uiso calc SR 1 . .
C C14 0.6944(2) 0.24140(17) 0.4914(6) 0.0499(12) Uani d . 1 . .
H H14 0.6559 0.2355 0.4366 0.060 Uiso calc R 1 . .
N N21 0.57994(17) 0.18287(12) 0.6270(5) 0.0434(8) Uani d . 1 . .
C C21 0.56005(17) 0.15562(13) 0.5553(5) 0.0381(9) Uani d . 1 . .
Se Se21 0.53008(3) 0.114405(17) 0.44108(7) 0.06121(16) Uani d . 1 . .
N N31 0.63231(16) 0.26940(12) 0.9575(5) 0.0428(8) Uani d . 1 . .
C C31 0.63448(17) 0.29139(13) 1.0643(5) 0.0373(9) Uani d . 1 . .
Se Se31 0.63665(3) 0.324181(19) 1.23170(7) 0.06461(17) Uani d . 1 . .
O O41 0.66187(15) 0.18255(10) 0.9111(4) 0.0522(8) Uani d . 1 . .
C C41 0.6758(4) 0.1790(2) 1.0749(8) 0.085(2) Uani d . 1 . .
H H41A 0.6359 0.1747 1.1328 0.127 Uiso calc R 1 . .
H H41B 0.6964 0.2034 1.1118 0.127 Uiso calc R 1 . .
H H41C 0.7048 0.1566 1.0918 0.127 Uiso calc R 1 . .
H H1O4 0.6862 0.1792 0.8352 0.127 Uiso d 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'
Se Se -0.0929 2.2259 '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'
O O 0.0106 0.0060 '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
N31 Co1 N21 . . 176.69(16) ?
N31 Co1 O41 . . 89.55(15) ?
N21 Co1 O41 . . 87.46(14) ?
N31 Co1 N11 . . 90.55(13) ?
N21 Co1 N11 . . 90.75(14) ?
O41 Co1 N11 . . 87.77(13) ?
N31 Co1 N2 . 6_655 87.12(14) ?
N21 Co1 N2 . 6_655 91.27(14) ?
O41 Co1 N2 . 6_655 86.37(13) ?
N11 Co1 N2 . 6_655 173.71(13) ?
N31 Co1 N1 . . 92.13(14) ?
N21 Co1 N1 . . 90.91(14) ?
O41 Co1 N1 . . 177.16(14) ?
N11 Co1 N1 . . 89.92(12) ?
N2 Co1 N1 6_655 . 96.00(13) ?
C1 N1 C4 . . 116.4(4) ?
C1 N1 Co1 . . 123.3(3) ?
C4 N1 Co1 . . 120.3(3) ?
C1 N2 C2 . . 116.8(4) ?
C1 N2 Co1 . 6_654 124.1(3) ?
C2 N2 Co1 . 6_654 118.5(3) ?
N2 C1 N1 . . 125.9(4) ?
N2 C1 H1 . . 117.0 ?
N1 C1 H1 . . 117.0 ?
N2 C2 C3 . . 120.8(4) ?
N2 C2 H2 . . 119.6 ?
C3 C2 H2 . . 119.6 ?
C4 C3 C2 . . 118.9(4) ?
C4 C3 H3 . . 120.6 ?
C2 C3 H3 . . 120.6 ?
N1 C4 C3 . . 121.2(4) ?
N1 C4 H4 . . 119.4 ?
C3 C4 H4 . . 119.4 ?
C14 N11 C11 . . 116.8(4) ?
C14 N11 Co1 . . 122.6(3) ?
C11 N11 Co1 . . 120.5(3) ?
N11 C11 N11 . 14_655 125.1(5) ?
N11 C11 H11 . . 117.5 ?
N11 C11 H11 14_655 . 117.5 ?
C14 C13 C14 . 14_655 117.1(6) ?
C14 C13 H13 . . 121.5 ?
C14 C13 H13 14_655 . 121.5 ?
N11 C14 C13 . . 122.1(4) ?
N11 C14 H14 . . 118.9 ?
C13 C14 H14 . . 118.9 ?
C21 N21 Co1 . . 169.9(4) ?
N21 C21 Se21 . . 178.7(4) ?
C31 N31 Co1 . . 166.0(3) ?
N31 C31 Se31 . . 178.4(4) ?
C41 O41 Co1 . . 129.6(4) ?
C41 O41 H1O4 . . 128.9 ?
Co1 O41 H1O4 . . 92.4 ?
O41 C41 H41A . . 109.5 ?
O41 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
O41 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
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
Co1 N1 . 2.191(3) y
Co1 N2 6_655 2.188(3) y
Co1 N11 . 2.184(3) y
Co1 N21 . 2.064(4) y
Co1 N31 . 2.059(4) y
Co1 O41 . 2.142(3) y
N1 C1 . 1.333(5) ?
N1 C4 . 1.342(5) ?
N2 C1 . 1.331(5) ?
N2 C2 . 1.341(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.366(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.364(7) ?
C3 H3 . 0.9300 ?
C4 H4 . 0.9300 ?
N11 C14 . 1.323(6) ?
N11 C11 . 1.335(4) ?
C11 N11 14_655 1.335(4) ?
C11 H11 . 0.9300 ?
C13 C14 . 1.372(6) ?
C13 C14 14_655 1.372(6) ?
C13 H13 . 0.9300 ?
C14 H14 . 0.9300 ?
N21 C21 . 1.157(5) ?
C21 Se21 . 1.774(5) ?
N31 C31 . 1.154(5) ?
C31 Se31 . 1.773(4) ?
O41 C41 . 1.405(7) ?
O41 H1O4 . 0.8139 ?
C41 H41A . 0.9600 ?
C41 H41B . 0.9600 ?
C41 H41C . 0.9600 ?
