#------------------------------------------------------------------------------
#$Date: 2019-12-25 21:50:19 +0200 (Wed, 25 Dec 2019) $
#$Revision: 245799 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/13/2311329.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_2311329
loop_
_publ_author_name
'Suckert, Stefan'
'Wöhlert, Susanne'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 di-aqua-bis-(2,6-di-methyl-pyrazine-\kN)bis-(thio-cyanato-\kN)cobalt(II)
 2,5-di-methyl-pyrazine tris-olvate.
;
_journal_coeditor_code           WM5255
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              m269
_journal_page_last               70
_journal_paper_doi               10.1107/S2056989015024184
_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, 3(C6 H8 N2)'
_chemical_formula_sum            'C32 H44 Co N12 O2 S2'
_chemical_formula_weight         751.84
_chemical_name_systematic
'Diaquabis(2,6-dimethylpyrazine-κN)bis(thiocyanato-κN)cobalt(II) 2,5-dimethylpyrazine trisolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                103.231(9)
_cell_angle_beta                 111.888(9)
_cell_angle_gamma                104.123(9)
_cell_formula_units_Z            1
_cell_length_a                   9.3296(8)
_cell_length_b                   10.8407(8)
_cell_length_c                   11.3906(9)
_cell_measurement_reflns_used    8844
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      2.6
_cell_volume                     968.99(19)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 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      200(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.365
_diffrn_reflns_theta_min         2.619
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe, 2008)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       plate
_exptl_crystal_F_000             395
_exptl_crystal_size_max          0.1652
_exptl_crystal_size_mid          0.1291
_exptl_crystal_size_min          0.0617
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.786
_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     228
_refine_ls_number_reflns         4092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0772P)²+0.2726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                3540
_reflns_number_total             4092
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5255sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        968.99(15)
_cod_database_code               2311329
_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 0.02727(14) Uani d 1
N N1 0.4584(2) 0.32856(19) 0.34740(18) 0.0352(4) Uani d 1
C C1 0.4289(3) 0.2251(2) 0.2698(2) 0.0337(4) Uani d 1
S S1 0.38697(12) 0.08006(6) 0.15982(8) 0.0628(2) Uani d 1
N N10 0.2366(2) 0.47166(18) 0.40932(18) 0.0339(4) Uani d 1
C C10 0.1832(3) 0.5739(2) 0.4318(2) 0.0351(4) Uani d 1
H H10 0.2616 0.6618 0.4927 0.042 Uiso calc 1
C C11 0.0166(3) 0.5558(3) 0.3691(2) 0.0397(5) Uani d 1
C C12 -0.0429(3) 0.3307(3) 0.2646(3) 0.0492(6) Uani d 1
C C13 0.1238(3) 0.3506(2) 0.3258(2) 0.0416(5) Uani d 1
H H13 0.1579 0.2757 0.3073 0.050 Uiso calc 1
C C14 -0.0406(3) 0.6725(3) 0.3916(3) 0.0533(6) Uani d 1
H H14A -0.0693 0.6993 0.3118 0.080 Uiso calc 1
H H14B 0.0483 0.7496 0.4710 0.080 Uiso calc 1
H H14C -0.1384 0.6451 0.4069 0.080 Uiso calc 1
C C15 -0.1686(4) 0.1922(4) 0.1715(4) 0.0830(12) Uani d 1
H H15A -0.2500 0.1654 0.2047 0.125 Uiso calc 1
H H15B -0.1129 0.1265 0.1684 0.125 Uiso calc 1
H H15C -0.2252 0.1939 0.0804 0.125 Uiso calc 1
N N11 -0.0949(2) 0.4341(2) 0.2867(2) 0.0482(5) Uani d 1
C C20 0.8651(3) 0.4951(3) 0.9060(3) 0.0539(7) Uani d 1
H H20 0.7663 0.4936 0.8381 0.065 Uiso calc 1
N N20 0.8981(3) 0.3820(3) 0.8896(2) 0.0532(6) Uani d 1
C C24 1.0768(4) 0.2597(4) 0.9700(4) 0.0691(8) Uani d 1
H H24A 0.9786 0.1815 0.9460 0.104 Uiso calc 1
H H24B 1.1671 0.2702 1.0554 0.104 Uiso calc 1
H H24C 1.1115 0.2448 0.8982 0.104 Uiso calc 1
N N30 0.5186(3) 0.87945(19) 0.4487(2) 0.0425(4) Uani d 1
C C30 0.3732(3) 0.8941(2) 0.4031(2) 0.0431(5) Uani d 1
H H30 0.2788 0.8192 0.3329 0.052 Uiso calc 1
C C31 0.3532(3) 1.0149(2) 0.4541(2) 0.0423(5) Uani d 1
C C21 1.0360(3) 0.3855(3) 0.9857(3) 0.0515(6) Uani d 1
C C34 0.1905(4) 1.0312(3) 0.4020(4) 0.0596(7) Uani d 1
H H34A 0.1321 1.0032 0.4529 0.089 Uiso calc 1
H H34B 0.1241 0.9743 0.3059 0.089 Uiso calc 1
H H34C 0.2076 1.1267 0.4126 0.089 Uiso calc 1
N N40 0.4624(3) 0.4506(2) 0.86521(18) 0.0390(4) Uani d 1
C C40 0.4770(3) 0.5764(2) 0.9248(2) 0.0398(5) Uani d 1
H H40 0.4610 0.6333 0.8726 0.048 Uiso calc 1
C C41 0.5148(3) 0.6284(2) 1.0603(2) 0.0369(4) Uani d 1
C C44 0.5314(4) 0.7707(3) 1.1266(3) 0.0566(7) Uani d 1
H H44A 0.4322 0.7690 1.1384 0.085 Uiso calc 1
H H44B 0.5434 0.8240 1.0697 0.085 Uiso calc 1
H H44C 0.6294 0.8122 1.2152 0.085 Uiso calc 1
O O1 0.5467(2) 0.62397(14) 0.39186(14) 0.0351(3) Uani d 1
H H1O1 0.5451 0.7009 0.4059 0.053 Uiso d 1
H H2O1 0.5481 0.5992 0.3192 0.053 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'
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'
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
N1 Co1 N1 2_666 . 180.0
N1 Co1 O1 2_666 . 88.87(7)
N1 Co1 O1 . . 91.13(7)
N1 Co1 O1 2_666 2_666 91.13(7)
N1 Co1 O1 . 2_666 88.87(7)
O1 Co1 O1 . 2_666 180.0
N1 Co1 N10 2_666 2_666 91.60(7)
N1 Co1 N10 . 2_666 88.40(7)
O1 Co1 N10 . 2_666 88.71(7)
O1 Co1 N10 2_666 2_666 91.29(7)
N1 Co1 N10 2_666 . 88.40(7)
N1 Co1 N10 . . 91.60(7)
O1 Co1 N10 . . 91.29(7)
O1 Co1 N10 2_666 . 88.71(7)
N10 Co1 N10 2_666 . 180.0
C1 N1 Co1 . . 172.52(19)
N1 C1 S1 . . 179.6(2)
C13 N10 C10 . . 117.27(19)
C13 N10 Co1 . . 120.17(16)
C10 N10 Co1 . . 122.53(14)
N10 C10 C11 . . 122.0(2)
N10 C10 H10 . . 119.0
C11 C10 H10 . . 119.0
N11 C11 C10 . . 120.1(2)
N11 C11 C14 . . 118.6(2)
C10 C11 C14 . . 121.3(2)
N11 C12 C13 . . 121.0(2)
N11 C12 C15 . . 118.8(2)
C13 C12 C15 . . 120.3(3)
N10 C13 C12 . . 121.3(2)
N10 C13 H13 . . 119.3
C12 C13 H13 . . 119.3
C11 C14 H14A . . 109.5
C11 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C11 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
C12 C15 H15A . . 109.5
C12 C15 H15B . . 109.5
H15A C15 H15B . . 109.5
C12 C15 H15C . . 109.5
H15A C15 H15C . . 109.5
H15B C15 H15C . . 109.5
C11 N11 C12 . . 118.4(2)
N20 C20 C21 . 2_767 124.4(3)
N20 C20 H20 . . 117.8
C21 C20 H20 2_767 . 117.8
C20 N20 C21 . . 117.1(2)
C21 C24 H24A . . 109.5
C21 C24 H24B . . 109.5
H24A C24 H24B . . 109.5
C21 C24 H24C . . 109.5
H24A C24 H24C . . 109.5
H24B C24 H24C . . 109.5
C31 N30 C30 2_676 . 117.2(2)
N30 C30 C31 . . 122.6(2)
N30 C30 H30 . . 118.7
C31 C30 H30 . . 118.7
N30 C31 C30 2_676 . 120.3(2)
N30 C31 C34 2_676 . 117.4(2)
C30 C31 C34 . . 122.4(2)
N20 C21 C20 . 2_767 118.5(3)
N20 C21 C24 . . 118.3(3)
C20 C21 C24 2_767 . 123.2(3)
C31 C34 H34A . . 109.5
C31 C34 H34B . . 109.5
H34A C34 H34B . . 109.5
C31 C34 H34C . . 109.5
H34A C34 H34C . . 109.5
H34B C34 H34C . . 109.5
C40 N40 C41 . 2_667 118.11(19)
N40 C40 C41 . . 122.6(2)
N40 C40 H40 . . 118.7
C41 C40 H40 . . 118.7
N40 C41 C40 2_667 . 119.3(2)
N40 C41 C44 2_667 . 118.5(2)
C40 C41 C44 . . 122.2(2)
C41 C44 H44A . . 109.5
C41 C44 H44B . . 109.5
H44A C44 H44B . . 109.5
C41 C44 H44C . . 109.5
H44A C44 H44C . . 109.5
H44B C44 H44C . . 109.5
Co1 O1 H1O1 . . 125.2
Co1 O1 H2O1 . . 126.2
H1O1 O1 H2O1 . . 107.2
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 2.0718(18)
Co1 N1 . 2.0718(18)
Co1 O1 . 2.0942(15)
Co1 O1 2_666 2.0942(15)
Co1 N10 2_666 2.1895(18)
Co1 N10 . 2.1895(18)
N1 C1 . 1.153(3)
C1 S1 . 1.621(2)
N10 C13 . 1.320(3)
N10 C10 . 1.333(3)
C10 C11 . 1.387(3)
C10 H10 . 0.9500
C11 N11 . 1.320(3)
C11 C14 . 1.494(4)
C12 N11 . 1.335(4)
C12 C13 . 1.382(3)
C12 C15 . 1.497(4)
C13 H13 . 0.9500
C14 H14A . 0.9800
C14 H14B . 0.9800
C14 H14C . 0.9800
C15 H15A . 0.9800
C15 H15B . 0.9800
C15 H15C . 0.9800
C20 N20 . 1.325(4)
C20 C21 2_767 1.373(4)
C20 H20 . 0.9500
N20 C21 . 1.327(4)
C24 C21 . 1.494(5)
C24 H24A . 0.9800
C24 H24B . 0.9800
C24 H24C . 0.9800
N30 C31 2_676 1.316(3)
N30 C30 . 1.324(4)
C30 C31 . 1.393(3)
C30 H30 . 0.9500
C31 N30 2_676 1.316(3)
C31 C34 . 1.481(4)
C21 C20 2_767 1.373(4)
C34 H34A . 0.9800
C34 H34B . 0.9800
C34 H34C . 0.9800
N40 C40 . 1.326(3)
N40 C41 2_667 1.336(3)
C40 C41 . 1.386(3)
C40 H40 . 0.9500
C41 N40 2_667 1.336(3)
C41 C44 . 1.495(3)
C44 H44A . 0.9800
C44 H44B . 0.9800
C44 H44C . 0.9800
O1 H1O1 . 0.8175
O1 H2O1 . 0.8152
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 H1O1 N30 . 0.82 1.98 2.796(2) 172.2
O1 H2O1 N40 2_666 0.82 2.00 2.816(2) 174.2
