#------------------------------------------------------------------------------
#$Date: 2015-12-13 04:36:31 +0200 (Sun, 13 Dec 2015) $
#$Revision: 171468 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/13/2241387.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_2241387
loop_
_publ_author_name
'Suckert, Stefan'
'Wöhlert, Susanne'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 diaquabis(2,6-dimethylpyrazine-κN⁴)bis(thiocyanato-κN)cobalt(II)
 2,5-dimethylpyrazine monosolvate
;
_journal_coeditor_code           WM5240
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m242
_journal_page_last               m243
_journal_paper_doi               10.1107/S2056989015021829
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Co (N C S)2 (C6 H8 N2)2 (H2 O)2], C6 H8 N2'
_chemical_formula_moiety         'C14 H20 Co N6 O2 S2, C6 H8 N2'
_chemical_formula_sum            'C20 H28 Co N8 O2 S2'
_chemical_formula_weight         535.55
_chemical_name_systematic
'Diaquabis(2,6-dimethylpyrazine-κN⁴)bis(thiocyanato-κN)cobalt(II) 2,5-dimethylpyrazine monosolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                96.640(4)
_cell_angle_beta                 105.820(4)
_cell_angle_gamma                116.070(4)
_cell_formula_units_Z            1
_cell_length_a                   8.3009(4)
_cell_length_b                   9.0466(5)
_cell_length_c                   10.4200(6)
_cell_measurement_reflns_used    10848
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      2.1
_cell_volume                     650.68(7)
_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) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.192
_diffrn_reflns_theta_min         2.926
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2008)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             279
_exptl_crystal_size_max          0.1503
_exptl_crystal_size_mid          0.0784
_exptl_crystal_size_min          0.0395
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0528P)²+0.1118P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                3175
_reflns_number_total             3447
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5240sup1.cif
_cod_data_source_block           I
_cod_database_code               2241387
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           .2013
loop_
_space_group_symop_operation_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_occupancy
Co Co1 0.5000 0.5000 0.5000 0.04299(10) Uani d 1
N N1 0.3328(2) 0.26365(19) 0.35238(16) 0.0590(3) Uani d 1
C C1 0.2857(2) 0.1399(2) 0.27093(18) 0.0558(4) Uani d 1
S S1 0.23050(11) -0.02995(8) 0.15745(7) 0.0943(2) Uani d 1
N N10 -0.05473(17) 0.39022(16) 0.65466(14) 0.0467(3) Uani d 1
C C10 -0.0663(2) 0.27462(19) 0.55572(16) 0.0476(3) Uani d 1
C C11 0.0930(2) 0.30432(19) 0.51972(16) 0.0470(3) Uani d 1
H H11 0.0815 0.2212 0.4508 0.056 Uiso calc 1
C C12 0.2717(2) 0.5600(2) 0.68289(16) 0.0496(3) Uani d 1
H H12 0.3881 0.6602 0.7301 0.059 Uiso calc 1
C C13 0.1150(2) 0.5321(2) 0.72101(16) 0.0472(3) Uani d 1
C C14 -0.2559(3) 0.1149(2) 0.4835(2) 0.0718(5) Uani d 1
H H14A -0.3458 0.1151 0.5251 0.108 Uiso calc 1
H H14B -0.2400 0.0171 0.4918 0.108 Uiso calc 1
H H14C -0.3038 0.1098 0.3873 0.108 Uiso calc 1
C C15 0.1285(3) 0.6597(3) 0.8350(2) 0.0706(5) Uani d 1
H H15A 0.0349 0.6942 0.7993 0.106 Uiso calc 1
H H15B 0.2551 0.7579 0.8702 0.106 Uiso calc 1
H H15C 0.1043 0.6087 0.9083 0.106 Uiso calc 1
N N11 0.26138(16) 0.44839(16) 0.58104(13) 0.0451(3) Uani d 1
N N20 0.4442(3) 0.5506(2) 0.10190(16) 0.0667(4) Uani d 1
C C20 0.5941(3) 0.6633(3) 0.07748(19) 0.0653(4) Uani d 1
C C21 0.6487(3) 0.6097(3) -0.0256(2) 0.0676(5) Uani d 1
H H21 0.7542 0.6894 -0.0414 0.081 Uiso calc 1
C C24 0.7003(5) 0.8448(3) 0.1628(3) 0.1000(9) Uani d 1
H H24A 0.6111 0.8861 0.1601 0.150 Uiso calc 1
H H24B 0.7935 0.9135 0.1263 0.150 Uiso calc 1
H H24C 0.7647 0.8517 0.2569 0.150 Uiso calc 1
O O1 0.40223(16) 0.61584(16) 0.35860(12) 0.0560(3) Uani d 1
H H1O1 0.2978 0.6105 0.3470 0.084 Uiso d 1
H H2O1 0.4074 0.6011 0.2810 0.084 Uiso 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'
Co Co 0.3494 0.9721 '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'
H H 0.0000 0.0000 '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
N1 Co1 N1 2_666 . 180.00(9)
N1 Co1 O1 2_666 . 89.38(6)
N1 Co1 O1 . . 90.62(6)
N1 Co1 O1 2_666 2_666 90.62(6)
N1 Co1 O1 . 2_666 89.38(6)
O1 Co1 O1 . 2_666 180.0
N1 Co1 N11 2_666 . 88.99(5)
N1 Co1 N11 . . 91.01(5)
O1 Co1 N11 . . 92.08(4)
O1 Co1 N11 2_666 . 87.92(4)
N1 Co1 N11 2_666 2_666 91.01(5)
N1 Co1 N11 . 2_666 88.99(5)
O1 Co1 N11 . 2_666 87.92(4)
O1 Co1 N11 2_666 2_666 92.08(4)
N11 Co1 N11 . 2_666 180.0
C1 N1 Co1 . . 162.42(13)
N1 C1 S1 . . 177.21(15)
C10 N10 C13 . . 118.09(12)
N10 C10 C11 . . 120.65(14)
N10 C10 C14 . . 117.78(13)
C11 C10 C14 . . 121.56(15)
N11 C11 C10 . . 122.01(13)
N11 C11 H11 . . 119.0
C10 C11 H11 . . 119.0
N11 C12 C13 . . 122.41(14)
N11 C12 H12 . . 118.8
C13 C12 H12 . . 118.8
N10 C13 C12 . . 120.37(14)
N10 C13 C15 . . 117.87(13)
C12 C13 C15 . . 121.76(15)
C10 C14 H14A . . 109.5
C10 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C10 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
C13 C15 H15A . . 109.5
C13 C15 H15B . . 109.5
H15A C15 H15B . . 109.5
C13 C15 H15C . . 109.5
H15A C15 H15C . . 109.5
H15B C15 H15C . . 109.5
C12 N11 C11 . . 116.38(12)
C12 N11 Co1 . . 123.72(10)
C11 N11 Co1 . . 119.73(9)
C21 N20 C20 2_665 . 118.15(15)
N20 C20 C21 . . 119.60(19)
N20 C20 C24 . . 118.75(18)
C21 C20 C24 . . 121.6(2)
N20 C21 C20 2_665 . 122.25(19)
N20 C21 H21 2_665 . 118.9
C20 C21 H21 . . 118.9
C20 C24 H24A . . 109.5
C20 C24 H24B . . 109.5
H24A C24 H24B . . 109.5
C20 C24 H24C . . 109.5
H24A C24 H24C . . 109.5
H24B C24 H24C . . 109.5
Co1 O1 H1O1 . . 119.4
Co1 O1 H2O1 . . 120.2
H1O1 O1 H2O1 . . 105.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 N1 2_666 2.0812(15)
Co1 N1 . 2.0812(15)
Co1 O1 . 2.0930(12)
Co1 O1 2_666 2.0930(12)
Co1 N11 . 2.2460(11)
Co1 N11 2_666 2.2460(11)
N1 C1 . 1.158(2)
C1 S1 . 1.6232(18)
N10 C10 . 1.3321(19)
N10 C13 . 1.336(2)
C10 C11 . 1.3935(18)
C10 C14 . 1.495(2)
C11 N11 . 1.3343(18)
C11 H11 . 0.9300
C12 N11 . 1.3342(18)
C12 C13 . 1.3893(18)
C12 H12 . 0.9300
C13 C15 . 1.501(2)
C14 H14A . 0.9600
C14 H14B . 0.9600
C14 H14C . 0.9600
C15 H15A . 0.9600
C15 H15B . 0.9600
C15 H15C . 0.9600
N20 C21 2_665 1.322(3)
N20 C20 . 1.330(3)
C20 C21 . 1.389(2)
C20 C24 . 1.493(3)
C21 N20 2_665 1.322(3)
C21 H21 . 0.9300
C24 H24A . 0.9600
C24 H24B . 0.9600
C24 H24C . 0.9600
O1 H1O1 . 0.8201
O1 H2O1 . 0.8200
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H2O1 N20 . 0.82 2.01 2.8193(17) 171.7
O1 H1O1 N10 2_566 0.82 2.01 2.8257(15) 172.6

_cod_database_fobs_code 2241387
