#------------------------------------------------------------------------------
#$Date: 2015-05-20 05:40:45 +0300 (Wed, 20 May 2015) $
#$Revision: 137007 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/07/2240743.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_2240743
loop_
_publ_author_name
'Moon, Dohyun'
'Choi, Jong-Ha'
_publ_section_title
;
 Crystal structure of
 trans-bis(ethane-1,2-diamine-κ²N,N')bis(thiocyanato-κN)chromium(III)
 perchlorate from synchrotron data
;
_journal_coeditor_code           SJ5459
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              650
_journal_page_last               653
_journal_paper_doi               10.1107/S2056989015009184
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cr (N C S)2 (C2 H8 N2)2] Cl O4'
_chemical_formula_moiety         'C6 H16  Cr N6 S2 +, Cl O4 -'
_chemical_formula_sum            'C6 H16 Cl Cr N6 O4 S2'
_chemical_formula_weight         387.82
_chemical_name_systematic
'trans-Bis(ethane-1,2-diamine-κ²N,N')bis(thiocyanato-κN)chromium(III) perchlorate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.599(3)
_cell_length_b                   7.4440(15)
_cell_length_c                   13.792(3)
_cell_measurement_reflns_used    46962
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     1540.8(6)
_computing_cell_refinement
;
HKL3000sm (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
PAL ADSC Quantum-210 ADX Program (Arvai & Nielsen, 1983)
;
_computing_data_reduction
;
HKL3000sm (Otwinowski & Minor,1997)
;
_computing_molecular_graphics
;
DIAMOND (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8172
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.707
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(HKL3000sm SCALEAPCK; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.735
_refine_diff_density_min         -1.119
_refine_ls_extinction_coef       0.045(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0599
_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)+(0.1146P)²+2.4721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                2019
_reflns_number_total             2121
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj5459sup1.cf
_cod_data_source_block           I
_cod_database_code               2240743
_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.
;
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.897
loop_
_space_group_symop_operation_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr Cr1 0.2500 0.2500 0.5000 0.0273(3) Uani d 1 . .
S S1 0.21080(8) 0.77661(11) 0.67477(8) 0.0586(3) Uani d 1 . .
N N1 0.24831(15) 0.4775(3) 0.57426(17) 0.0433(5) Uani d 1 . .
C C1 0.23290(16) 0.6026(3) 0.61573(17) 0.0363(5) Uani d 1 . .
N N2A 0.3423(12) 0.1308(19) 0.6213(13) 0.036(2) Uani d 0.522(16) A 1
H H2A1 0.3272 0.1503 0.6781 0.043 Uiso calc 0.522(16) A 1
H H2A2 0.3442 0.0127 0.6118 0.043 Uiso calc 0.522(16) A 1
N N3A 0.3624(11) 0.337(2) 0.4641(10) 0.043(3) Uani d 0.522(16) A 1
H H3A1 0.3553 0.3266 0.3981 0.052 Uiso calc 0.522(16) A 1
H H3A2 0.3722 0.4525 0.4807 0.052 Uiso calc 0.522(16) A 1
C C2A 0.4311(5) 0.2126(10) 0.6277(8) 0.057(2) Uani d 0.522(16) A 1
H H2A3 0.4784 0.1375 0.6678 0.068 Uiso calc 0.522(16) A 1
H H2A4 0.4355 0.3305 0.6587 0.068 Uiso calc 0.522(16) A 1
C C3A 0.4385(5) 0.2274(14) 0.5199(10) 0.066(3) Uani d 0.522(16) A 1
H H3A3 0.4943 0.2842 0.5191 0.079 Uiso calc 0.522(16) A 1
H H3A4 0.4362 0.1092 0.4897 0.079 Uiso calc 0.522(16) A 1
N N2B 0.3570(13) 0.164(2) 0.6143(14) 0.041(3) Uani d 0.478(16) A 2
H H2B1 0.3654 0.2382 0.6667 0.049 Uiso calc 0.478(16) A 2
H H2B2 0.3464 0.0548 0.6342 0.049 Uiso calc 0.478(16) A 2
N N3B 0.3502(13) 0.341(3) 0.4378(9) 0.040(2) Uani d 0.478(16) A 2
H H3B1 0.3527 0.2732 0.3856 0.048 Uiso calc 0.478(16) A 2
H H3B2 0.3396 0.4543 0.4167 0.048 Uiso calc 0.478(16) A 2
C C2B 0.4369(4) 0.1614(15) 0.5773(8) 0.056(2) Uani d 0.478(16) A 2
H H2B3 0.4355 0.0582 0.5339 0.067 Uiso calc 0.478(16) A 2
H H2B4 0.4902 0.1541 0.6334 0.067 Uiso calc 0.478(16) A 2
C C3B 0.4370(5) 0.3297(19) 0.5203(7) 0.060(3) Uani d 0.478(16) A 2
H H3B3 0.4869 0.3303 0.4911 0.072 Uiso calc 0.478(16) A 2
H H3B4 0.4427 0.4322 0.5651 0.072 Uiso calc 0.478(16) A 2
Cl Cl1B 0.5000 0.7072(3) 0.7500 0.0989(7) Uani d 0.5 B 1
O O1B 0.4393(4) 0.5672(9) 0.7711(5) 0.0762(16) Uani d 0.5 B 1
O O2B 0.4350(6) 0.7462(8) 0.6376(6) 0.159(3) Uani d 0.5 B 1
Cl Cl1C 0.5000 0.7072(3) 0.7500 0.0989(7) Uani d 0.5 C 2
O O1C 0.4350(6) 0.7462(8) 0.6376(6) 0.159(3) Uani d 0.5 C 2
O O2C 0.4488(11) 0.8416(15) 0.7860(8) 0.152(5) Uani d 0.5 C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 '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 0.0050 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1020 0.0980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1230 0.1260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.2900 0.4910 '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 Cr1 N1 . 7_556 180.0
N1 Cr1 N3A . 7_556 90.8(5)
N1 Cr1 N3A 7_556 7_556 89.2(5)
N1 Cr1 N3A . . 89.2(5)
N1 Cr1 N3A 7_556 . 90.8(5)
N3A Cr1 N3A 7_556 . 180.0
N1 Cr1 N2B . . 89.5(5)
N1 Cr1 N2B 7_556 . 90.5(5)
N1 Cr1 N2B . 7_556 90.5(5)
N1 Cr1 N2B 7_556 7_556 89.5(5)
N2B Cr1 N2B . 7_556 180.0(9)
N1 Cr1 N2A . 7_556 87.0(4)
N1 Cr1 N2A 7_556 7_556 93.0(5)
N3A Cr1 N2A 7_556 7_556 83.1(5)
N3A Cr1 N2A . 7_556 96.9(5)
N1 Cr1 N2A . . 93.0(4)
N1 Cr1 N2A 7_556 . 87.0(4)
N3A Cr1 N2A 7_556 . 96.9(5)
N3A Cr1 N2A . . 83.1(5)
N2A Cr1 N2A 7_556 . 180.0
N1 Cr1 N3B . 7_556 87.1(5)
N1 Cr1 N3B 7_556 7_556 92.9(5)
N2B Cr1 N3B . 7_556 97.2(5)
N2B Cr1 N3B 7_556 7_556 82.8(5)
N1 Cr1 N3B . . 92.9(5)
N1 Cr1 N3B 7_556 . 87.1(5)
N2B Cr1 N3B . . 82.8(5)
N2B Cr1 N3B 7_556 . 97.2(5)
N3B Cr1 N3B 7_556 . 180.0
C1 N1 Cr1 . . 168.7(2)
N1 C1 S1 . . 179.3(3)
C2A N2A Cr1 . . 107.5(7)
C2A N2A H2A1 . . 110.2
Cr1 N2A H2A1 . . 110.2
C2A N2A H2A2 . . 110.2
Cr1 N2A H2A2 . . 110.2
H2A1 N2A H2A2 . . 108.5
C3A N3A Cr1 . . 108.5(8)
C3A N3A H3A1 . . 110.0
Cr1 N3A H3A1 . . 110.0
C3A N3A H3A2 . . 110.0
Cr1 N3A H3A2 . . 110.0
H3A1 N3A H3A2 . . 108.4
N2A C2A C3A . . 106.7(9)
N2A C2A H2A3 . . 110.4
C3A C2A H2A3 . . 110.4
N2A C2A H2A4 . . 110.4
C3A C2A H2A4 . . 110.4
H2A3 C2A H2A4 . . 108.6
N3A C3A C2A . . 106.5(10)
N3A C3A H3A3 . . 110.4
C2A C3A H3A3 . . 110.4
N3A C3A H3A4 . . 110.4
C2A C3A H3A4 . . 110.4
H3A3 C3A H3A4 . . 108.6
C2B N2B Cr1 . . 109.0(9)
C2B N2B H2B1 . . 109.9
Cr1 N2B H2B1 . . 109.9
C2B N2B H2B2 . . 109.9
Cr1 N2B H2B2 . . 109.9
H2B1 N2B H2B2 . . 108.3
C3B N3B Cr1 . . 106.7(8)
C3B N3B H3B1 . . 110.4
Cr1 N3B H3B1 . . 110.4
C3B N3B H3B2 . . 110.4
Cr1 N3B H3B2 . . 110.4
H3B1 N3B H3B2 . . 108.6
N2B C2B C3B . . 107.1(10)
N2B C2B H2B3 . . 110.3
C3B C2B H2B3 . . 110.3
N2B C2B H2B4 . . 110.3
C3B C2B H2B4 . . 110.3
H2B3 C2B H2B4 . . 108.5
C2B C3B N3B . . 108.6(10)
C2B C3B H3B3 . . 110.0
N3B C3B H3B3 . . 110.0
C2B C3B H3B4 . . 110.0
N3B C3B H3B4 . . 110.0
H3B3 C3B H3B4 . . 108.4
O1B Cl1B O1B 2_656 . 91.2(5)
O1B Cl1B O2B 2_656 2_656 92.7(4)
O1B Cl1B O2B . 2_656 101.7(3)
O1B Cl1B O2B 2_656 . 101.7(3)
O1B Cl1B O2B . . 92.7(4)
O2B Cl1B O2B 2_656 . 159.4(5)
O2C Cl1C O2C 2_656 . 92.7(9)
O2C Cl1C O1C 2_656 2_656 86.8(6)
O2C Cl1C O1C . 2_656 79.0(6)
O2C Cl1C O1C 2_656 . 79.0(6)
O2C Cl1C O1C . . 86.8(6)
O1C Cl1C O1C 2_656 . 159.4(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cr1 N1 . 1.983(2)
Cr1 N1 7_556 1.983(2)
Cr1 N3A 7_556 2.053(16)
Cr1 N3A . 2.053(16)
Cr1 N2B . 2.06(2)
Cr1 N2B 7_556 2.06(2)
Cr1 N2A 7_556 2.085(19)
Cr1 N2A . 2.085(19)
Cr1 N3B 7_556 2.09(2)
Cr1 N3B . 2.09(2)
S1 C1 . 1.617(3)
N1 C1 . 1.152(3)
N2A C2A . 1.493(15)
N2A H2A1 . 0.8900
N2A H2A2 . 0.8900
N3A C3A . 1.475(16)
N3A H3A1 . 0.8900
N3A H3A2 . 0.8900
C2A C3A . 1.527(17)
C2A H2A3 . 0.9700
C2A H2A4 . 0.9700
C3A H3A3 . 0.9700
C3A H3A4 . 0.9700
N2B C2B . 1.471(18)
N2B H2B1 . 0.8900
N2B H2B2 . 0.8900
N3B C3B . 1.514(17)
N3B H3B1 . 0.8900
N3B H3B2 . 0.8900
C2B C3B . 1.479(17)
C2B H2B3 . 0.9700
C2B H2B4 . 0.9700
C3B H3B3 . 0.9700
C3B H3B4 . 0.9700
Cl1B O1B 2_656 1.489(6)
Cl1B O1B . 1.489(6)
Cl1B O2B 2_656 1.630(8)
Cl1B O2B . 1.630(8)
Cl1C O2C 2_656 1.450(13)
Cl1C O2C . 1.450(13)
Cl1C O1C 2_656 1.630(8)
Cl1C O1C . 1.630(8)
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
N2A H2A1 S1 4_546 0.89 2.45 3.324(17) 166.9
N2A H2A2 O2B 1_545 0.89 2.41 3.187(19) 146.4
N3A H3A1 O1B 6_565 0.89 2.58 3.282(16) 136.2
N2B H2B1 S1 4_546 0.89 2.77 3.459(17) 134.8
N3B H3B1 O2C 6_565 0.89 2.45 3.22(2) 145.2
N3B H3B2 S1 7_566 0.89 2.38 3.255(18) 166.3
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
Cr1 N2A C2A C3A -42.0(11)
Cr1 N3A C3A C2A -44.8(13)
N2A C2A C3A N3A 57.9(14)
Cr1 N2B C2B C3B 44.2(13)
N2B C2B C3B N3B -56.3(15)
Cr1 N3B C3B C2B 40.2(12)

_cod_database_fobs_code 2240743
