##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
# article from which it was obtained. #
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##############################################################################
data_I
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Dichloridobis[2-methylsulfanyl-4-(pyridin-2-yl)pyrimidine-
\k^2^N^3^,N^4^)cobalt(II)
;
_chemical_name_common ?
_chemical_formula_moiety 'C20 H18 Cl2 Co N6 S2'
_chemical_formula_sum 'C20 H18 Cl2 Co N6 S2'
_chemical_formula_iupac '[Co Cl2 (C10 H9 N3 S)2]'
_chemical_formula_weight 536.37
_chemical_melting_point ?
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
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'
_cell_length_a 8.709(11)
_cell_length_b 17.10(2)
_cell_length_c 15.328(19)
_cell_angle_alpha 90.00
_cell_angle_beta 102.34(3)
_cell_angle_gamma 90.00
_cell_volume 2230(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2588
_cell_measurement_theta_min 2.25
_cell_measurement_theta_max 25.50
_cell_measurement_temperature 298(2)
_exptl_crystal_description block
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.24
_exptl_crystal_density_diffrn 1.598
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1092
_exptl_absorpt_coefficient_mu 1.218
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2001)'
_exptl_absorpt_correction_T_min 0.671
_exptl_absorpt_correction_T_max 0.747
_exptl_special_details ?
_diffrn_ambient_temperature 298(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEXII CCD area-detector'
_diffrn_measurement_method '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 6138
_diffrn_reflns_av_R_equivalents 0.0522
_diffrn_reflns_av_sigmaI/netI 0.0915
_diffrn_reflns_theta_min 2.67
_diffrn_reflns_theta_max 28.36
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 20
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F^2^, conventional
R-factors R are based on F, with F set to zero for
negative F^2^. The threshold expression of F^2^ >
\s(F^2^) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F^2^ are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total 2586
_reflns_number_gt 1636
_reflns_threshold_expression I>2sigma(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0690
_refine_ls_R_factor_gt 0.0449
_refine_ls_wR_factor_gt 0.0568
_refine_ls_wR_factor_ref 0.0596
_refine_ls_goodness_of_fit_ref 0.928
_refine_ls_restrained_S_all 0.928
_refine_ls_number_reflns 2586
_refine_ls_number_parameters 141
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.329
_refine_diff_density_min -0.500
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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'
'S' 'S' 0.1246 0.1234
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'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'
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'SAINT-Plus (Bruker, 2007)'
_computing_data_reduction 'SAINT-Plus (Bruker, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.5000 0.29835(3) 0.2500 0.02888(15) Uani d S 1 2 . .
Cl Cl1 0.56198(8) 0.38235(4) 0.13403(4) 0.0435(2) Uani d . 1 1 . .
S S1 0.76922(8) 0.15867(5) 0.18274(4) 0.0419(2) Uani d . 1 1 . .
N N2 0.4663(2) 0.19418(12) 0.15296(11) 0.0274(5) Uani d . 1 1 . .
N N1 0.2595(2) 0.30314(13) 0.17840(12) 0.0309(5) Uani d . 1 1 . .
C C6 0.3142(3) 0.18317(15) 0.10981(14) 0.0279(6) Uani d . 1 1 . .
C C9 0.5705(3) 0.13805(16) 0.13928(15) 0.0314(7) Uani d . 1 1 . .
C C5 0.2020(3) 0.24704(16) 0.11833(14) 0.0288(6) Uani d . 1 1 . .
C C7 0.2671(3) 0.11737(17) 0.05868(16) 0.0389(7) Uani d . 1 1 . .
H H7A 0.1634 0.1105 0.0285 0.047 Uiso calc R 1 1 . .
C C1 0.1648(3) 0.36330(17) 0.18607(16) 0.0381(7) Uani d . 1 1 . .
H H1A 0.2041 0.4035 0.2255 0.046 Uiso calc R 1 1 . .
N N3 0.5331(3) 0.07212(14) 0.09342(13) 0.0402(6) Uani d . 1 1 . .
C C2 0.0109(3) 0.36861(17) 0.13814(17) 0.0422(8) Uani d . 1 1 . .
H H2A -0.0516 0.4109 0.1463 0.051 Uiso calc R 1 1 . .
C C8 0.3816(3) 0.06227(17) 0.05450(17) 0.0440(8) Uani d . 1 1 . .
H H8A 0.3519 0.0162 0.0232 0.053 Uiso calc R 1 1 . .
C C4 0.0501(3) 0.24955(17) 0.06704(15) 0.0364(7) Uani d . 1 1 . .
H H4A 0.0145 0.2105 0.0254 0.044 Uiso calc R 1 1 . .
C C10 0.8661(3) 0.07695(18) 0.14226(19) 0.0572(9) Uani d . 1 1 . .
H H10A 0.9779 0.0822 0.1622 0.086 Uiso calc R 1 1 . .
H H10B 0.8396 0.0762 0.0782 0.086 Uiso calc R 1 1 . .
H H10C 0.8323 0.0291 0.1649 0.086 Uiso calc R 1 1 . .
C C3 -0.0481(3) 0.31061(18) 0.07843(17) 0.0424(8) Uani d . 1 1 . .
H H3B -0.1516 0.3123 0.0464 0.051 Uiso calc R 1 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 0.0301(3) 0.0267(3) 0.0278(2) 0.000 0.0016(2) 0.000
Cl1 0.0447(5) 0.0451(5) 0.0379(4) -0.0040(4) 0.0027(3) 0.0098(3)
S1 0.0323(4) 0.0441(6) 0.0470(4) 0.0022(4) 0.0030(4) -0.0135(3)
N2 0.0295(13) 0.0292(14) 0.0223(9) 0.0010(11) 0.0029(10) 0.0001(9)
N1 0.0313(13) 0.0318(15) 0.0296(10) 0.0039(12) 0.0069(10) 0.0007(10)
C6 0.0299(16) 0.0316(18) 0.0211(11) -0.0022(13) 0.0029(12) -0.0015(11)
C9 0.0344(16) 0.0310(19) 0.0278(12) 0.0009(14) 0.0046(12) 0.0004(11)
C5 0.0316(16) 0.0309(17) 0.0233(12) -0.0039(14) 0.0044(12) 0.0029(11)
C7 0.0306(16) 0.045(2) 0.0376(15) -0.0031(16) -0.0006(13) -0.0075(13)
C1 0.0410(18) 0.037(2) 0.0349(14) 0.0062(16) 0.0057(14) -0.0009(12)
N3 0.0412(16) 0.0333(17) 0.0426(13) 0.0021(13) 0.0015(12) -0.0111(11)
C2 0.0423(19) 0.047(2) 0.0384(15) 0.0148(17) 0.0102(15) 0.0071(14)
C8 0.047(2) 0.033(2) 0.0492(17) -0.0070(17) 0.0031(16) -0.0157(14)
C4 0.0339(17) 0.041(2) 0.0322(14) -0.0013(15) 0.0022(13) 0.0014(13)
C10 0.0378(19) 0.059(2) 0.072(2) 0.0117(18) 0.0058(16) -0.0197(17)
C3 0.0294(16) 0.055(2) 0.0398(15) 0.0046(16) 0.0017(14) 0.0122(15)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
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_655 2.148(3) ?
Co1 N1 . 2.148(3) ?
Co1 N2 . 2.299(3) ?
Co1 N2 2_655 2.299(3) ?
Co1 Cl1 2_655 2.434(2) ?
Co1 Cl1 . 2.434(2) ?
S1 C9 . 1.752(3) ?
S1 C10 . 1.810(3) ?
N2 C6 . 1.361(3) ?
N2 C9 . 1.368(3) ?
N1 C5 . 1.350(3) ?
N1 C1 . 1.340(3) ?
C6 C7 . 1.382(4) ?
C6 C5 . 1.490(4) ?
C9 N3 . 1.332(3) ?
C5 C4 . 1.388(4) ?
C7 C8 . 1.383(4) ?
C7 H7A . 0.9300 ?
C1 C2 . 1.387(4) ?
C1 H1A . 0.9300 ?
N3 C8 . 1.337(3) ?
C2 C3 . 1.373(4) ?
C2 H2A . 0.9300 ?
C8 H8A . 0.9300 ?
C4 C3 . 1.384(4) ?
C4 H4A . 0.9300 ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C3 H3B . 0.9300 ?
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 Co1 N1 2_655 . 175.62(12) ?
N1 Co1 N2 2_655 . 109.62(8) ?
N1 Co1 N2 . . 73.94(8) ?
N1 Co1 N2 2_655 2_655 73.94(8) ?
N1 Co1 N2 . 2_655 109.62(8) ?
N2 Co1 N2 . 2_655 78.41(14) ?
N1 Co1 Cl1 2_655 2_655 87.05(8) ?
N1 Co1 Cl1 . 2_655 90.36(8) ?
N2 Co1 Cl1 . 2_655 155.81(5) ?
N2 Co1 Cl1 2_655 2_655 90.14(11) ?
N1 Co1 Cl1 2_655 . 90.36(8) ?
N1 Co1 Cl1 . . 87.05(8) ?
N2 Co1 Cl1 . . 90.14(11) ?
N2 Co1 Cl1 2_655 . 155.81(5) ?
Cl1 Co1 Cl1 2_655 . 107.66(10) ?
C9 S1 C10 . . 102.08(15) ?
C6 N2 C9 . . 115.9(2) ?
C6 N2 Co1 . . 113.46(15) ?
C9 N2 Co1 . . 130.23(17) ?
C5 N1 C1 . . 117.4(2) ?
C5 N1 Co1 . . 120.02(17) ?
C1 N1 Co1 . . 122.42(19) ?
N2 C6 C7 . . 121.9(2) ?
N2 C6 C5 . . 116.4(2) ?
C7 C6 C5 . . 121.7(3) ?
N3 C9 N2 . . 125.4(2) ?
N3 C9 S1 . . 118.8(2) ?
N2 C9 S1 . . 115.7(2) ?
N1 C5 C4 . . 122.3(2) ?
N1 C5 C6 . . 115.2(2) ?
C4 C5 C6 . . 122.5(2) ?
C8 C7 C6 . . 116.8(3) ?
C8 C7 H7A . . 121.6 ?
C6 C7 H7A . . 121.6 ?
N1 C1 C2 . . 123.2(3) ?
N1 C1 H1A . . 118.4 ?
C2 C1 H1A . . 118.4 ?
C9 N3 C8 . . 116.7(2) ?
C3 C2 C1 . . 119.2(3) ?
C3 C2 H2A . . 120.4 ?
C1 C2 H2A . . 120.4 ?
N3 C8 C7 . . 123.1(3) ?
N3 C8 H8A . . 118.5 ?
C7 C8 H8A . . 118.5 ?
C5 C4 C3 . . 119.4(3) ?
C5 C4 H4A . . 120.3 ?
C3 C4 H4A . . 120.3 ?
S1 C10 H10A . . 109.5 ?
S1 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
S1 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C4 C3 C2 . . 118.4(3) ?
C4 C3 H3B . . 120.8 ?
C2 C3 H3B . . 120.8 ?
data_global
_journal_date_recd_electronic 2011-07-22
_journal_date_accepted 2011-08-01
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2011
_journal_volume 67
_journal_issue 9
_journal_page_first m1193
_journal_page_last m1193
_journal_paper_category QM
_journal_coeditor_code VM2113
_publ_contact_author_name 'Wen-Na Yang'
_publ_contact_author_address
;
School of chemistry and chemical engineering
Southeast University, Nanjing 211189
P.R. China
;
_publ_contact_author_email 'yjs_seu@163.com'
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_section_title
;\
Dichloridobis[2-methylsulfanyl-4-(pyridin-2-yl)pyrimidine-\k^2^N^3^,\
N^4^)cobalt(II)
;
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Yang, Wen-Na' .
;
School of Chemistry and Chemical Engineering
Southeast University, Nanjing 211189
People's Republic of China
;