#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/12/2221286.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_2221286
loop_
_publ_author_name
'Wriedt, Mario'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
Poly[bis(cyanato-κN)bis(μ-pyrazine-κ²N:N')cobalt(II)]
_journal_coeditor_code           BT2872
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m431
_journal_paper_doi               10.1107/S1600536809005686
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Co (N C O)2 (C4 H4 N2)2]'
_chemical_formula_moiety         'C10 H8 Co N6 O2'
_chemical_formula_sum            'C10 H8 Co N6 O2'
_chemical_formula_weight         303.15
_chemical_name_systematic
Poly[bis(cyanato-κN)bis(μ-pyrazine-κ²N:N')cobalt(II)]
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.763(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.5712(17)
_cell_length_b                   10.1230(8)
_cell_length_c                   10.1863(7)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      14.1
_cell_volume                     2549.8(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2008)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11369
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0575P)²+18.631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                2058
_reflns_number_total             2684
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2872.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2221286
_cod_database_fobs_code          2221286
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.629290(19) 0.75059(4) 0.63502(4) 0.01326(17) Uani d . 1 . .
N N1 0.62838(13) 0.5943(3) 0.7846(3) 0.0162(6) Uani d . 1 . .
C C1 0.66193(17) 0.5983(3) 0.9072(4) 0.0224(8) Uani d . 1 . .
H H1 0.6868 0.6695 0.9297 0.027 Uiso calc R 1 . .
C C2 0.66194(17) 0.5014(4) 1.0044(3) 0.0224(8) Uani d . 1 . .
H H2 0.6864 0.5088 1.0916 0.027 Uiso calc R 1 . .
N N2 0.62829(13) 0.3981(3) 0.9778(3) 0.0171(6) Uani d . 1 . .
C C3 0.59444(17) 0.3935(4) 0.8537(3) 0.0230(8) Uani d . 1 . .
H H3 0.5700 0.3215 0.8305 0.028 Uiso calc R 1 . .
C C4 0.59412(17) 0.4920(4) 0.7578(4) 0.0225(8) Uani d . 1 . .
H H4 0.5690 0.4864 0.6714 0.027 Uiso calc R 1 . .
N N11 0.63140(13) 0.9093(3) 0.4902(3) 0.0163(6) Uani d . 1 . .
C C11 0.67047(17) 0.9151(4) 0.4247(4) 0.0228(8) Uani d . 1 . .
H H11 0.6992 0.8528 0.4461 0.027 Uiso calc R 1 . .
C C12 0.67008(17) 1.0102(3) 0.3260(4) 0.0222(8) Uani d . 1 . .
H H12 0.6984 1.0110 0.2810 0.027 Uiso calc R 1 . .
N N12 0.63094(13) 1.1005(3) 0.2930(3) 0.0167(6) Uani d . 1 . .
C C13 0.59214(17) 1.0958(4) 0.3588(4) 0.0259(9) Uani d . 1 . .
H H13 0.5637 1.1590 0.3381 0.031 Uiso calc R 1 . .
C C14 0.59239(18) 1.0000(4) 0.4575(4) 0.0259(9) Uani d . 1 . .
H H14 0.5641 0.9993 0.5025 0.031 Uiso calc R 1 . .
N N21 0.54684(14) 0.7557(3) 0.5817(3) 0.0238(7) Uani d . 1 . .
C C21 0.5047(3) 0.7083(8) 0.5445(8) 0.0347(16) Uani d P 0.75 A 1
O O21 0.4602(3) 0.6596(9) 0.5110(10) 0.109(4) Uani d P 0.75 A 1
O O21' 0.4627(6) 0.7506(17) 0.4184(18) 0.052(4) Uani d P 0.25 A 2
C C21' 0.5054(9) 0.7583(16) 0.498(2) 0.023(4) Uani d P 0.25 A 2
N N31 0.71251(14) 0.7443(3) 0.6873(3) 0.0218(7) Uani d . 1 . .
C C31 0.7539(3) 0.7288(7) 0.7698(8) 0.0250(15) Uani d P 0.70 A 1
O O31 0.7962(3) 0.7135(8) 0.8513(7) 0.074(3) Uani d P 0.70 A 1
C C31' 0.7530(9) 0.7621(19) 0.734(2) 0.030(6) Uiso d P 0.30 A 2
O O31' 0.8018(11) 0.771(2) 0.789(3) 0.098(8) Uiso d P 0.30 A 2
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'
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
N21 Co1 N31 . . 179.45(13) y
N21 Co1 N11 . . 90.19(12) y
N31 Co1 N11 . . 89.76(12) y
N21 Co1 N2 . 6_565 90.23(12) y
N31 Co1 N2 . 6_565 89.23(12) y
N11 Co1 N2 . 6_565 90.53(11) y
N21 Co1 N12 . 6_576 90.19(12) y
N31 Co1 N12 . 6_576 90.35(12) y
N11 Co1 N12 . 6_576 89.45(10) y
N2 Co1 N12 6_565 6_576 179.58(12) y
N21 Co1 N1 . . 90.57(12) y
N31 Co1 N1 . . 89.49(12) y
N11 Co1 N1 . . 178.55(11) y
N2 Co1 N1 6_565 . 90.70(10) y
N12 Co1 N1 6_576 . 89.32(10) y
C1 N1 C4 . . 116.7(3) ?
C1 N1 Co1 . . 120.9(2) ?
C4 N1 Co1 . . 122.5(2) ?
N1 C1 C2 . . 122.1(3) ?
N1 C1 H1 . . 118.9 ?
C2 C1 H1 . . 118.9 ?
N2 C2 C1 . . 121.5(3) ?
N2 C2 H2 . . 119.3 ?
C1 C2 H2 . . 119.3 ?
C2 N2 C3 . . 116.5(3) ?
C2 N2 Co1 . 6_566 120.1(2) ?
C3 N2 Co1 . 6_566 123.4(2) ?
N2 C3 C4 . . 121.6(3) ?
N2 C3 H3 . . 119.2 ?
C4 C3 H3 . . 119.2 ?
N1 C4 C3 . . 121.6(3) ?
N1 C4 H4 . . 119.2 ?
C3 C4 H4 . . 119.2 ?
C14 N11 C11 . . 116.8(3) ?
C14 N11 Co1 . . 121.8(2) ?
C11 N11 Co1 . . 121.2(2) ?
N11 C11 C12 . . 121.5(3) ?
N11 C11 H11 . . 119.2 ?
C12 C11 H11 . . 119.2 ?
N12 C12 C11 . . 121.6(3) ?
N12 C12 H12 . . 119.2 ?
C11 C12 H12 . . 119.2 ?
C13 N12 C12 . . 117.1(3) ?
C13 N12 Co1 . 6_575 121.0(2) ?
C12 N12 Co1 . 6_575 121.9(2) ?
N12 C13 C14 . . 121.3(3) ?
N12 C13 H13 . . 119.3 ?
C14 C13 H13 . . 119.3 ?
N11 C14 C13 . . 121.6(3) ?
N11 C14 H14 . . 119.2 ?
C13 C14 H14 . . 119.2 ?
C21 N21 C21' . . 34.7(8) ?
C21 N21 Co1 . . 153.4(5) ?
C21' N21 Co1 . . 150.6(11) ?
N21 C21 O21 . . 177.2(8) ?
N21 C21' O21' . . 174(2) ?
C31' N31 C31 . . 24.8(10) ?
C31' N31 Co1 . . 163.3(12) ?
C31 N31 Co1 . . 150.1(5) ?
N31 C31 O31 . . 178.7(10) ?
N31 C31' O31' . . 174(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
Co1 N21 . 2.039(3) y
Co1 N31 . 2.059(3) y
Co1 N11 . 2.191(3) y
Co1 N2 6_565 2.193(3) y
Co1 N12 6_576 2.197(3) y
Co1 N1 . 2.200(3) y
N1 C1 . 1.324(5) ?
N1 C4 . 1.339(5) ?
C1 C2 . 1.394(5) ?
C1 H1 . 0.9500 ?
C2 N2 . 1.337(5) ?
C2 H2 . 0.9500 ?
N2 C3 . 1.338(5) ?
N2 Co1 6_566 2.193(3) ?
C3 C4 . 1.395(5) ?
C3 H3 . 0.9500 ?
C4 H4 . 0.9500 ?
N11 C14 . 1.334(5) ?
N11 C11 . 1.337(5) ?
C11 C12 . 1.390(5) ?
C11 H11 . 0.9500 ?
C12 N12 . 1.333(5) ?
C12 H12 . 0.9500 ?
N12 C13 . 1.332(5) ?
N12 Co1 6_575 2.197(3) ?
C13 C14 . 1.397(5) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
N21 C21 . 1.151(8) ?
N21 C21' . 1.18(2) ?
C21 O21 . 1.206(9) ?
O21' C21' . 1.19(3) ?
N31 C31' . 1.04(2) ?
N31 C31 . 1.182(8) ?
C31 O31 . 1.195(9) ?
C31' O31' . 1.24(4) ?
