#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/94/2239444.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_2239444
loop_
_publ_author_name
'Rusanova, Julia A.'
'Semenaka, Valentyna V.'
'Zubatyuk, Roman I.'
_publ_section_title
;
 trans-Chloridobis(ethane-1,2-diamine-κ²N,N')(thiocyanato-κN)cobalt(III)
 diamminetetrakis(thiocyanato-κN)cromate(III)
;
_journal_coeditor_code           BR2236
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m110
_journal_page_last               m111
_journal_paper_doi               10.1107/S1600536814003869
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Co Cl (NCS) (C2 H8 N2)2] [Cr (N C S)4 (N H3)2]'
_chemical_formula_moiety         'C5 H16 Cl Co N5 S +, C4 H6 Cr N6 S4 -'
_chemical_formula_sum            'C9 H22 Cl Co Cr N11 S5'
_chemical_formula_weight         591.05
_chemical_name_systematic
;trans-Chloridobis(ethane-1,2-diamine-κ²N,N')(thiocyanato-κN)cobalt(III)
diamminetetrakis(thiocyanato-κN)cromate(III)
;
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                106.98(2)
_cell_angle_beta                 93.131(17)
_cell_angle_gamma                90.646(17)
_cell_formula_units_Z            2
_cell_length_a                   8.8290(15)
_cell_length_b                   10.745(3)
_cell_length_c                   13.275(3)
_cell_measurement_reflns_used    3528
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3220
_cell_measurement_theta_min      3.0540
_cell_volume                     1202.2(5)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8238
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.644
_diffrn_reflns_theta_min         2.894
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.2729
_exptl_crystal_size_mid          0.2415
_exptl_crystal_size_min          0.0746
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.723
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         8238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0800P)²+0.5674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                6185
_reflns_number_total             8238
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br2236sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1202.1(5)
_cod_database_code               2239444
_cod_database_fobs_code          2239444
#BEGIN Tags that were not found in dictionaries:
_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
#END Tags that were not found in dictionaries
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 0.54186(7) 0.40606(6) 0.75563(4) 0.02775(16) Uani d 1
Cr Cr1 0.08452(9) -0.07796(8) 0.76057(7) 0.0385(2) Uani d 1
Cl Cl1 0.40444(16) 0.35647(13) 0.87609(9) 0.0438(3) Uani d 1
S S1 0.78440(16) 0.49754(14) 0.48138(10) 0.0452(3) Uani d 1
S S2 0.0503(3) -0.3524(2) 0.9791(2) 0.1063(9) Uani d 1
S S3 0.0184(2) 0.2947(2) 0.6471(2) 0.0984(8) Uani d 1
S S4 0.55652(16) -0.22096(14) 0.61991(10) 0.0442(3) Uani d 1
S S5 -0.38612(16) 0.04575(16) 0.91039(11) 0.0518(4) Uani d 1
N N1 0.6708(5) 0.2569(4) 0.7487(3) 0.0370(9) Uani d 1
H H1A 0.7764 0.2817 0.7471 0.044 Uiso calc 1
H H1B 0.6599 0.2272 0.8104 0.044 Uiso calc 1
N N2 0.4114(4) 0.2859(4) 0.6452(3) 0.0343(9) Uani d 1
H H2A 0.3061 0.2971 0.6623 0.041 Uiso calc 1
H H2B 0.4225 0.3036 0.5783 0.041 Uiso calc 1
N N3 0.4130(5) 0.5558(4) 0.7636(3) 0.0371(9) Uani d 1
H H3A 0.4180 0.5815 0.6996 0.045 Uiso calc 1
H H3B 0.3084 0.5323 0.7701 0.045 Uiso calc 1
N N4 0.6745(5) 0.5263(4) 0.8661(3) 0.0367(9) Uani d 1
H H4A 0.6582 0.5137 0.9342 0.044 Uiso calc 1
H H4B 0.7801 0.5104 0.8513 0.044 Uiso calc 1
N N5 0.6529(5) 0.4460(4) 0.6499(3) 0.0362(9) Uani d 1
N N6 0.0981(6) -0.2081(5) 0.8404(4) 0.0603(14) Uani d 1
N N7 0.0637(6) 0.0593(5) 0.6873(4) 0.0561(13) Uani d 1
N N8 0.2839(5) -0.1270(4) 0.6994(4) 0.0461(11) Uani d 1
N N9 -0.1149(5) -0.0282(5) 0.8214(4) 0.0515(12) Uani d 1
N N10 -0.0200(6) -0.2146(5) 0.6325(4) 0.0695(15) Uani d 1
H H10A -0.1087 -0.2397 0.6501 0.104 Uiso calc 1
H H10B 0.0388 -0.2832 0.6125 0.104 Uiso calc 1
H H10C -0.0353 -0.1801 0.5796 0.104 Uiso calc 1
N N11 0.1914(5) 0.0620(4) 0.8881(3) 0.0472(11) Uani d 1
H H11A 0.1242 0.1198 0.9190 0.071 Uiso calc 1
H H11B 0.2652 0.1023 0.8656 0.071 Uiso calc 1
H H11C 0.2306 0.0238 0.9344 0.071 Uiso calc 1
C C1 0.6231(7) 0.1510(5) 0.6512(4) 0.0502(14) Uani d 1
H H1C 0.6687 0.1659 0.5908 0.060 Uiso calc 1
H H1D 0.6558 0.0677 0.6578 0.060 Uiso calc 1
C C2 0.4560(7) 0.1507(5) 0.6370(4) 0.0482(13) Uani d 1
H H2C 0.4101 0.1210 0.6910 0.058 Uiso calc 1
H H2D 0.4220 0.0926 0.5685 0.058 Uiso calc 1
C C3 0.4661(6) 0.6663(5) 0.8567(4) 0.0444(13) Uani d 1
H H3C 0.4223 0.6579 0.9200 0.053 Uiso calc 1
H H3D 0.4360 0.7484 0.8463 0.053 Uiso calc 1
C C4 0.6367(7) 0.6613(5) 0.8674(4) 0.0459(13) Uani d 1
H H4C 0.6814 0.6831 0.8093 0.055 Uiso calc 1
H H4D 0.6757 0.7230 0.9330 0.055 Uiso calc 1
C C5 0.7041(5) 0.4652(4) 0.5783(4) 0.0323(10) Uani d 1
C C6 0.0819(7) -0.2700(6) 0.8967(6) 0.0664(19) Uani d 1
C C7 0.0454(6) 0.1544(7) 0.6701(5) 0.0591(17) Uani d 1
C C8 0.3977(5) -0.1639(4) 0.6657(4) 0.0334(10) Uani d 1
C C9 -0.2279(6) 0.0020(5) 0.8567(4) 0.0374(11) Uani 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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
N1 Co1 Cl1 90.78(12)
N1 Co1 N3 179.61(17)
N1 Co1 N4 93.44(17)
N2 Co1 Cl1 88.77(12)
N2 Co1 N1 86.23(17)
N2 Co1 N3 94.07(17)
N2 Co1 N4 179.54(17)
N3 Co1 Cl1 88.98(13)
N3 Co1 N4 86.27(17)
N4 Co1 Cl1 91.54(12)
N5 Co1 Cl1 178.03(13)
N5 Co1 N1 89.78(17)
N5 Co1 N2 89.38(17)
N5 Co1 N3 90.47(17)
N5 Co1 N4 90.31(17)
N6 Cr1 N7 176.5(2)
N6 Cr1 N8 92.1(2)
N6 Cr1 N9 88.1(2)
N6 Cr1 N10 90.7(2)
N6 Cr1 N11 90.3(2)
N7 Cr1 N10 91.1(2)
N7 Cr1 N11 87.9(2)
N8 Cr1 N7 90.8(2)
N8 Cr1 N9 179.7(2)
N8 Cr1 N10 89.1(2)
N8 Cr1 N11 90.47(19)
N9 Cr1 N7 88.9(2)
N9 Cr1 N10 90.9(2)
N9 Cr1 N11 89.51(19)
N10 Cr1 N11 179.0(2)
Co1 N1 H1A 110.1
Co1 N1 H1B 110.1
H1A N1 H1B 108.4
C1 N1 Co1 108.2(3)
C1 N1 H1A 110.1
C1 N1 H1B 110.1
Co1 N2 H2A 109.9
Co1 N2 H2B 109.9
H2A N2 H2B 108.3
C2 N2 Co1 108.7(3)
C2 N2 H2A 109.9
C2 N2 H2B 109.9
Co1 N3 H3A 109.8
Co1 N3 H3B 109.8
H3A N3 H3B 108.2
C3 N3 Co1 109.4(3)
C3 N3 H3A 109.8
C3 N3 H3B 109.8
Co1 N4 H4A 110.2
Co1 N4 H4B 110.2
H4A N4 H4B 108.5
C4 N4 Co1 107.7(3)
C4 N4 H4A 110.2
C4 N4 H4B 110.2
C5 N5 Co1 171.6(4)
C6 N6 Cr1 166.2(5)
C7 N7 Cr1 163.2(5)
C8 N8 Cr1 175.0(4)
C9 N9 Cr1 179.0(5)
Cr1 N10 H10A 109.5
Cr1 N10 H10B 109.5
Cr1 N10 H10C 109.5
H10A N10 H10B 109.5
H10A N10 H10C 109.5
H10B N10 H10C 109.5
Cr1 N11 H11A 109.5
Cr1 N11 H11B 109.5
Cr1 N11 H11C 109.5
H11A N11 H11B 109.5
H11A N11 H11C 109.5
H11B N11 H11C 109.5
N1 C1 H1C 110.1
N1 C1 H1D 110.1
H1C C1 H1D 108.4
C2 C1 N1 108.0(4)
C2 C1 H1C 110.1
C2 C1 H1D 110.1
N2 C2 H2C 110.2
N2 C2 H2D 110.2
C1 C2 N2 107.6(4)
C1 C2 H2C 110.2
C1 C2 H2D 110.2
H2C C2 H2D 108.5
N3 C3 H3C 110.3
N3 C3 H3D 110.3
N3 C3 C4 107.1(4)
H3C C3 H3D 108.5
C4 C3 H3C 110.3
C4 C3 H3D 110.3
N4 C4 C3 107.1(4)
N4 C4 H4C 110.3
N4 C4 H4D 110.3
C3 C4 H4C 110.3
C3 C4 H4D 110.3
H4C C4 H4D 108.5
N5 C5 S1 176.7(5)
N6 C6 S2 176.6(6)
N7 C7 S3 179.0(7)
N8 C8 S4 177.7(5)
N9 C9 S5 178.3(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 Cl1 . 2.2378(14) ?
Co1 N1 . 1.960(4) ?
Co1 N2 . 1.954(4) ?
Co1 N3 . 1.962(4) ?
Co1 N4 . 1.965(4) ?
Co1 N5 . 1.900(4) ?
Cr1 N6 . 1.987(5) ?
Cr1 N7 . 1.995(5) ?
Cr1 N8 . 1.990(4) ?
Cr1 N9 . 1.990(5) ?
Cr1 N10 . 2.058(5) ?
Cr1 N11 . 2.080(4) ?
S1 C5 . 1.623(5) ?
S2 C6 . 1.629(7) ?
S3 C7 . 1.640(7) ?
S4 C8 . 1.615(5) ?
S5 C9 . 1.616(5) ?
S2 S2 2_547 3.489(3) yes
S5 S5 2_457 3.538(2) yes
N1 H1A . 0.9700 ?
N1 H1B . 0.9700 ?
N1 C1 . 1.489(7) ?
N2 H2A . 0.9700 ?
N2 H2B . 0.9700 ?
N2 C2 . 1.485(6) ?
N3 H3A . 0.9700 ?
N3 H3B . 0.9700 ?
N3 C3 . 1.492(6) ?
N4 H4A . 0.9700 ?
N4 H4B . 0.9700 ?
N4 C4 . 1.488(6) ?
N5 C5 . 1.144(6) ?
N6 C6 . 1.149(8) ?
N7 C7 . 1.122(8) ?
N8 C8 . 1.150(6) ?
N9 C9 . 1.135(6) ?
N10 H10A . 0.8900 ?
N10 H10B . 0.8900 ?
N10 H10C . 0.8900 ?
N11 H11A . 0.8900 ?
N11 H11B . 0.8900 ?
N11 H11C . 0.8900 ?
C1 H1C . 0.9700 ?
C1 H1D . 0.9700 ?
C1 C2 . 1.477(8) ?
C2 H2C . 0.9700 ?
C2 H2D . 0.9700 ?
C3 H3C . 0.9700 ?
C3 H3D . 0.9700 ?
C3 C4 . 1.508(8) ?
C4 H4C . 0.9700 ?
C4 H4D . 0.9700 ?
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
_geom_hbond_publ_flag
N1 H1A S3 1_655 0.9700 2.6000 3.485(5) 152.00 yes
N1 H1B S5 1_655 0.9700 2.7000 3.598(5) 154.00 yes
N2 H2A S3 . 0.9700 2.5400 3.473(4) 163.00 yes
N2 H2B S4 2_656 0.9700 2.5400 3.411(4) 150.00 yes
N4 H4A Cl1 2_667 0.9700 2.5900 3.398(4) 141.00 yes
N10 H10B S1 2_656 0.8900 2.8100 3.696(6) 171.00 yes
N11 H11C S5 2_557 0.8900 2.7000 3.578(5) 168.00 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Co1 N1 C1 C2 -38.5(5)
Co1 N2 C2 C1 -38.6(5)
Co1 N3 C3 C4 35.7(5)
Co1 N4 C4 C3 42.6(5)
N1 C1 C2 N2 50.6(5)
N3 C3 C4 N4 -51.3(5)
