#------------------------------------------------------------------------------
#$Date: 2014-10-25 20:23:10 +0300 (Sat, 25 Oct 2014) $
#$Revision: 125873 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/80/2018058.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_2018058
loop_
_publ_author_name
'Kochel, Andrzej'
'Ho\/ly\'nska, Ma\/lgorzata'
_publ_section_title
;
Diammonium hexakis(thiocyanato-\kN)rhenate(IV) dimethyl sulfone
tetrasolvate
;
_journal_coeditor_code FA3250
_journal_issue 5
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first m134
_journal_page_last m136
_journal_volume 67
_journal_year 2011
_chemical_formula_iupac '(N1 H4)2 [Re (N C S)6] , 4C2 H6 O2 S'
_chemical_formula_moiety '2(H4 N +), C6 N6 Re S6 2-, 4(C2 H6 O2 S)'
_chemical_formula_sum 'C14 H32 N8 O8 Re S10'
_chemical_formula_weight 947.28
_chemical_name_systematic
;
Diammonium hexakis(thiocyanato-\kN)rhenate(IV) dimethyl sulfone
tetrasolvate
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL97
_cell_angle_alpha 90.00
_cell_angle_beta 113.57(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 13.128(3)
_cell_length_b 9.493(3)
_cell_length_c 15.412(4)
_cell_measurement_reflns_used 3295
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.73
_cell_measurement_theta_min 2.88
_cell_volume 1760.5(9)
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2010) and SHELXTL (Sheldrick, 2008)
;
_computing_publication_material 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type 'Oxford KM-4 CCD area-detector'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0250
_diffrn_reflns_av_sigmaI/netI 0.0270
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 11719
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 28.73
_diffrn_reflns_theta_min 2.88
_exptl_absorpt_coefficient_mu 4.092
_exptl_absorpt_correction_T_max 0.956
_exptl_absorpt_correction_T_min 0.789
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.787
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 942
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.88
_refine_diff_density_min -0.74
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.004
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 191
_refine_ls_number_reflns 4234
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.004
_refine_ls_R_factor_all 0.0318
_refine_ls_R_factor_gt 0.0233
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0555
_refine_ls_wR_factor_ref 0.0571
_reflns_number_gt 3483
_reflns_number_total 4234
_reflns_threshold_expression I>2\s(I)
_[local]_cod_data_source_file fa3250.cif
_[local]_cod_data_source_block I
_[local]_cod_cif_authors_sg_H-M 'P 21/c'
_cod_original_cell_volume 1760.5(8)
_cod_database_code 2018058
_iucr_refine_instructions_details
;
TITL AKI.INS in P2(1)/c New: P21/c
CELL 0.71073 13.128 9.493 15.412 90.00 113.57 90.00
ZERR 2 0.003 0.003 0.004 0.00 0.03 0.00
LATT 1
SYMM - X , 0.50000 + Y , 0.50000 - Z
SFAC C H N O Re S
UNIT 28 64 16 16 2 20
L.S. 10
TEMP -173
EQIV $1 -x+1, y-1/2, -z+1/2
EQIV $2 -x, y-1/2, -z+1/2
EQIV $3 x, y-1, z
EQIV $4 -x, -y+1, -z
EQIV $5 x,y+1,z
HTAB N4 S1_$1
HTAB N4 O2_$2
HTAB N4 O4_$2
HTAB N4 O1_$3
HTAB N4 O1_$4
RTAB n S1 S3_$5
RTAB n S2 S2_$4
FMAP 2
PLAN 30
ACTA 50
HTAB 2
list 6
BOND $H
WGHT 0.035500
FVAR 1.84937
RE1 5 0.500000 0.500000 0.000000 10.50000 0.01127 0.01794 =
0.01593 0.00062 0.00376 0.00087
S1 6 0.684504 0.758361 0.287207 11.00000 0.02905 0.02389 =
0.02046 -0.00255 0.00000 0.00364
S2 6 0.141844 0.487635 0.015079 11.00000 0.01514 0.02849 =
0.02461 0.00050 0.01000 -0.00191
S3 6 0.606936 0.096918 0.201397 11.00000 0.02497 0.02337 =
0.03116 0.00915 0.00897 0.00135
N1 3 0.573619 0.611032 0.119764 11.00000 0.01325 0.02285 =
0.02077 0.00112 0.00430 0.00245
N2 3 0.353395 0.499899 0.014892 11.00000 0.01550 0.01962 =
0.02025 0.00081 0.00658 0.00109
N3 3 0.542920 0.322823 0.077205 11.00000 0.01495 0.02077 =
0.02177 0.00023 0.00540 0.00039
C1 1 0.620562 0.672175 0.191025 11.00000 0.01563 0.01866 =
0.02134 0.00496 0.00562 0.00431
C2 1 0.265543 0.493698 0.015716 11.00000 0.01934 0.01468 =
0.01416 0.00136 0.00479 0.00178
C3 1 0.569818 0.228511 0.130329 11.00000 0.01335 0.02248 =
0.02174 -0.00491 0.00554 -0.00130
S4 6 0.045997 0.824920 0.216102 11.00000 0.01472 0.02113 =
0.01335 0.00228 0.00570 -0.00015
O1 4 -0.009981 0.889094 0.123320 11.00000 0.01772 0.02724 =
0.01511 0.00559 0.00451 0.00017
O2 4 -0.019614 0.812132 0.272061 11.00000 0.02209 0.03665 =
0.02204 0.00859 0.01462 0.00404
C4 1 0.093728 0.658452 0.202120 11.00000 0.02280 0.02436 =
0.02282 -0.00325 0.00688 0.00181
AFIX 137
H4A 2 0.030312 0.598422 0.165528 11.00000 -1.50000
H4B 2 0.134734 0.616184 0.264466 11.00000 -1.50000
H4C 2 0.142946 0.667250 0.168512 11.00000 -1.50000
AFIX 0
C5 1 0.167401 0.921830 0.279105 11.00000 0.02225 0.02293 =
0.01889 -0.00221 0.00436 -0.00535
AFIX 137
H5A 2 0.210257 0.874519 0.339249 11.00000 -1.50000
H5B 2 0.147237 1.016768 0.291625 11.00000 -1.50000
H5C 2 0.212373 0.928214 0.241555 11.00000 -1.50000
AFIX 0
S5 6 0.252406 0.572693 0.515357 11.00000 0.01411 0.01862 =
0.01746 0.00253 0.00552 0.00068
O3 4 0.179118 0.543689 0.563401 11.00000 0.01993 0.02717 =
0.02332 0.00013 0.01118 -0.00280
O4 4 0.207919 0.665469 0.434808 11.00000 0.02700 0.02485 =
0.02117 0.00791 0.00842 0.00528
C6 1 0.291758 0.413292 0.479562 11.00000 0.02103 0.02267 =
0.02953 -0.00041 0.01100 0.00440
AFIX 137
H6A 2 0.342483 0.432726 0.448553 11.00000 -1.50000
H6B 2 0.225523 0.364865 0.435106 11.00000 -1.50000
H6C 2 0.329211 0.353402 0.535068 11.00000 -1.50000
AFIX 0
C7 1 0.375523 0.643869 0.598298 11.00000 0.01996 0.02765 =
0.02885 0.00102 0.00339 -0.00424
AFIX 137
H7A 2 0.359278 0.732700 0.622576 11.00000 -1.50000
H7B 2 0.427354 0.661425 0.568111 11.00000 -1.50000
H7C 2 0.409016 0.577419 0.650745 11.00000 -1.50000
AFIX 0
N4 3 0.033504 0.180376 0.068812 11.00000 0.01833 0.01754 =
0.01882 -0.00262 0.00920 -0.00012
AFIX 3
H1 2 0.106907 0.202528 0.098996 11.00000 -1.20000
H2 2 -0.007065 0.236977 0.090743 11.00000 -1.20000
H3 2 0.023980 0.088828 0.081764 11.00000 -1.20000
H4 2 0.011120 0.192614 0.005336 11.00000 -1.20000
rem dfix 0.91 0.003 N4 H1 N4 H2 N4 H3 N4 H4
rem dfix 1.5 0.01 H1 H2 H1 H3 H1 H4 H2 H3 H2 H4 H3 H4
HKLF 4
REM AKI.INS in P2(1)/c New: P21/c
REM R1 = 0.0233 for 3483 Fo > 4sig(Fo) and 0.0318 for all 4234 data
REM 191 parameters refined using 0 restraints
END
WGHT 0.0372 0.0000
REM Highest difference peak 0.882, deepest hole -0.741, 1-sigma level 0.115
Q1 1 0.4999 0.4987 0.0627 11.00000 0.05 0.88
Q2 1 0.6062 0.5017 0.1051 11.00000 0.05 0.82
Q3 1 0.3126 0.7582 0.7093 11.00000 0.05 0.81
Q4 1 0.2507 0.4326 0.5149 11.00000 0.05 0.80
Q5 1 0.5594 0.5032 0.0329 11.00000 0.05 0.72
Q6 1 0.6088 -0.0954 0.2000 11.00000 0.05 0.70
Q7 1 -0.0463 0.6750 0.2827 11.00000 0.05 0.68
Q8 1 0.5335 0.5600 0.0783 11.00000 0.05 0.55
Q9 1 0.0660 0.7364 0.2054 11.00000 0.05 0.55
Q10 1 0.5024 0.3920 0.0028 11.00000 0.05 0.53
Q11 1 0.3115 0.6159 0.5680 11.00000 0.05 0.52
Q12 1 0.4061 0.5076 0.0232 11.00000 0.05 0.48
Q13 1 0.2706 0.5004 0.4889 11.00000 0.05 0.48
Q14 1 0.4097 0.4200 -0.0080 11.00000 0.05 0.47
Q15 1 0.3401 0.4983 -0.0637 11.00000 0.05 0.47
Q16 1 0.2119 0.6424 0.4696 11.00000 0.05 0.45
Q17 1 0.4596 0.4250 0.0381 11.00000 0.05 0.44
Q18 1 0.5343 0.4470 0.0855 11.00000 0.05 0.44
Q19 1 0.6051 0.5864 0.1654 11.00000 0.05 0.44
Q20 1 -0.0165 0.8208 0.2328 11.00000 0.05 0.42
Q21 1 0.2314 0.5337 0.5632 11.00000 0.05 0.39
Q22 1 -0.0743 0.7813 0.2535 11.00000 0.05 0.39
Q23 1 0.6330 0.6833 0.2444 11.00000 0.05 0.39
Q24 1 0.2098 0.5004 0.0276 11.00000 0.05 0.39
Q25 1 0.2031 0.4233 0.0599 11.00000 0.05 0.38
Q26 1 0.5727 0.3673 0.1007 11.00000 0.05 0.36
Q27 1 0.6714 0.7412 0.2303 11.00000 0.05 0.36
Q28 1 0.2020 0.3368 0.4737 11.00000 0.05 0.36
Q29 1 0.6802 0.1004 0.2568 11.00000 0.05 0.36
Q30 1 0.4083 0.5881 -0.0107 11.00000 0.05 0.35
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re1 0.5000 0.5000 0.0000 0.01558(5) Uani d S 1 . .
S S1 0.68450(6) 0.75836(8) 0.28721(5) 0.02761(16) Uani d . 1 . .
S S2 0.14184(6) 0.48764(7) 0.01508(5) 0.02210(14) Uani d . 1 . .
S S3 0.60694(6) 0.09692(8) 0.20140(5) 0.02721(16) Uani d . 1 . .
N N1 0.57362(18) 0.6110(2) 0.11976(15) 0.0198(5) Uani d . 1 . .
N N2 0.3534(2) 0.4999(2) 0.01489(16) 0.0186(4) Uani d . 1 . .
N N3 0.54292(18) 0.3228(2) 0.07720(15) 0.0198(5) Uani d . 1 . .
C C1 0.6206(2) 0.6722(3) 0.19103(18) 0.0191(5) Uani d . 1 . .
C C2 0.2655(2) 0.4937(3) 0.01572(17) 0.0167(5) Uani d . 1 . .
C C3 0.5698(2) 0.2285(3) 0.13033(18) 0.0197(5) Uani d . 1 . .
S S4 0.04600(5) 0.82492(7) 0.21610(4) 0.01637(13) Uani d . 1 . .
O O1 -0.00998(14) 0.88909(19) 0.12332(12) 0.0207(4) Uani d . 1 . .
O O2 -0.01961(15) 0.8121(2) 0.27206(12) 0.0251(4) Uani d . 1 . .
C C4 0.0937(2) 0.6585(3) 0.20212(18) 0.0240(6) Uani d . 1 . .
H H4A 0.0303 0.5984 0.1655 0.036 Uiso calc R 1 . .
H H4B 0.1347 0.6162 0.2645 0.036 Uiso calc R 1 . .
H H4C 0.1429 0.6672 0.1685 0.036 Uiso calc R 1 . .
C C5 0.1674(2) 0.9218(3) 0.27910(18) 0.0226(6) Uani d . 1 . .
H H5A 0.2103 0.8745 0.3392 0.034 Uiso calc R 1 . .
H H5B 0.1472 1.0168 0.2916 0.034 Uiso calc R 1 . .
H H5C 0.2124 0.9282 0.2416 0.034 Uiso calc R 1 . .
S S5 0.25241(5) 0.57269(7) 0.51536(4) 0.01698(13) Uani d . 1 . .
O O3 0.17912(16) 0.5437(2) 0.56340(13) 0.0227(4) Uani d . 1 . .
O O4 0.20792(16) 0.6655(2) 0.43481(13) 0.0247(4) Uani d . 1 . .
C C6 0.2918(2) 0.4133(3) 0.47956(19) 0.0241(6) Uani d . 1 . .
H H6A 0.3425 0.4327 0.4486 0.036 Uiso calc R 1 . .
H H6B 0.2255 0.3649 0.4351 0.036 Uiso calc R 1 . .
H H6C 0.3292 0.3534 0.5351 0.036 Uiso calc R 1 . .
C C7 0.3755(2) 0.6439(3) 0.59830(19) 0.0275(6) Uani d . 1 . .
H H7A 0.3593 0.7327 0.6226 0.041 Uiso calc R 1 . .
H H7B 0.4274 0.6614 0.5681 0.041 Uiso calc R 1 . .
H H7C 0.4090 0.5774 0.6507 0.041 Uiso calc R 1 . .
N N4 0.03350(17) 0.1804(2) 0.06881(14) 0.0177(4) Uani d . 1 . .
H H1 0.1069 0.2025 0.0990 0.021 Uiso d R 1 . .
H H2 -0.0071 0.2370 0.0907 0.021 Uiso d R 1 . .
H H3 0.0240 0.0888 0.0818 0.021 Uiso d R 1 . .
H H4 0.0111 0.1926 0.0053 0.021 Uiso d R 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
Re1 0.01127(8) 0.01794(8) 0.01593(7) 0.00087(6) 0.00376(5) 0.00062(6)
S1 0.0290(4) 0.0239(4) 0.0205(3) 0.0036(3) 0.0000(3) -0.0025(3)
S2 0.0151(3) 0.0285(4) 0.0246(3) -0.0019(3) 0.0100(3) 0.0005(3)
S3 0.0250(4) 0.0234(4) 0.0312(4) 0.0013(3) 0.0090(3) 0.0092(3)
N1 0.0133(11) 0.0228(12) 0.0208(11) 0.0024(9) 0.0043(9) 0.0011(9)
N2 0.0155(11) 0.0196(11) 0.0203(11) 0.0011(10) 0.0066(8) 0.0008(9)
N3 0.0149(11) 0.0208(12) 0.0218(11) 0.0004(9) 0.0054(9) 0.0002(9)
C1 0.0156(13) 0.0187(14) 0.0213(12) 0.0043(11) 0.0056(10) 0.0050(11)
C2 0.0193(13) 0.0147(12) 0.0142(11) 0.0018(11) 0.0048(9) 0.0014(10)
C3 0.0133(13) 0.0225(14) 0.0217(13) -0.0013(11) 0.0055(10) -0.0049(11)
S4 0.0147(3) 0.0211(3) 0.0134(3) -0.0001(3) 0.0057(2) 0.0023(2)
O1 0.0177(10) 0.0272(11) 0.0151(8) 0.0002(8) 0.0045(7) 0.0056(8)
O2 0.0221(10) 0.0366(12) 0.0220(9) 0.0040(9) 0.0146(8) 0.0086(8)
C4 0.0228(15) 0.0244(15) 0.0228(13) 0.0018(12) 0.0069(11) -0.0032(11)
C5 0.0223(14) 0.0229(15) 0.0189(12) -0.0054(12) 0.0044(11) -0.0022(11)
S5 0.0141(3) 0.0186(3) 0.0175(3) 0.0007(3) 0.0055(2) 0.0025(3)
O3 0.0199(10) 0.0272(10) 0.0233(10) -0.0028(8) 0.0112(8) 0.0001(8)
O4 0.0270(11) 0.0249(11) 0.0212(9) 0.0053(9) 0.0084(8) 0.0079(8)
C6 0.0210(15) 0.0227(15) 0.0295(14) 0.0044(12) 0.0110(12) -0.0004(12)
C7 0.0200(15) 0.0277(16) 0.0288(14) -0.0042(12) 0.0034(12) 0.0010(12)
N4 0.0183(11) 0.0175(11) 0.0188(10) -0.0001(9) 0.0092(9) -0.0026(9)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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'
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 Re1 N1 . 3_665 180.0 ?
N1 Re1 N3 . . 88.69(8) yes
N1 Re1 N3 3_665 . 91.31(8) ?
N1 Re1 N3 . 3_665 91.31(8) ?
N1 Re1 N3 3_665 3_665 88.69(8) ?
N3 Re1 N3 . 3_665 180.0 ?
N1 Re1 N2 . . 91.49(9) yes
N1 Re1 N2 3_665 . 88.51(9) ?
N3 Re1 N2 . . 89.24(9) yes
N3 Re1 N2 3_665 . 90.76(9) ?
N1 Re1 N2 . 3_665 88.51(9) yes
N1 Re1 N2 3_665 3_665 91.49(9) ?
N3 Re1 N2 . 3_665 90.76(9) ?
N3 Re1 N2 3_665 3_665 89.24(9) ?
N2 Re1 N2 . 3_665 180.0 ?
C1 N1 Re1 . . 177.1(2) ?
C2 N2 Re1 . . 173.9(2) ?
C3 N3 Re1 . . 172.9(2) ?
N1 C1 S1 . . 178.9(2) ?
N2 C2 S2 . . 178.7(3) ?
N3 C3 S3 . . 178.7(2) ?
O2 S4 O1 . . 115.71(11) ?
O2 S4 C4 . . 109.05(13) ?
O1 S4 C4 . . 108.85(12) ?
O2 S4 C5 . . 109.81(13) ?
O1 S4 C5 . . 108.29(12) ?
C4 S4 C5 . . 104.54(14) ?
S4 C4 H4A . . 109.5 ?
S4 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
S4 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
S4 C5 H5A . . 109.5 ?
S4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
S4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
O4 S5 O3 . . 115.53(12) ?
O4 S5 C7 . . 109.37(14) ?
O3 S5 C7 . . 107.90(13) ?
O4 S5 C6 . . 108.93(13) ?
O3 S5 C6 . . 109.50(13) ?
C7 S5 C6 . . 105.11(14) ?
S5 C6 H6A . . 109.5 ?
S5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
S5 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
S5 C7 H7A . . 109.5 ?
S5 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
S5 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
H1 N4 H2 . . 109.3 ?
H1 N4 H3 . . 108.5 ?
H2 N4 H3 . . 109.2 ?
H1 N4 H4 . . 109.9 ?
H2 N4 H4 . . 109.8 ?
H3 N4 H4 . . 110.1 ?
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
Re1 N1 . 2.006(2) yes
Re1 N1 3_665 2.006(2) ?
Re1 N2 . 2.027(2) yes
Re1 N3 . 2.006(2) yes
Re1 N3 3_665 2.007(2) ?
Re1 N2 3_665 2.027(2) ?
S1 C1 . 1.605(3) yes
S2 C2 . 1.621(3) yes
S3 C3 . 1.603(3) yes
N1 C1 . 1.175(3) yes
N2 C2 . 1.160(4) yes
N3 C3 . 1.169(3) yes
S4 O1 . 1.4545(18) yes
S4 O2 . 1.4472(18) yes
S4 C4 . 1.745(3) ?
S4 C5 . 1.758(3) ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
S5 O4 . 1.4415(19) yes
S5 O3 . 1.456(2) yes
S5 C7 . 1.747(3) ?
S5 C6 . 1.758(3) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
N4 H1 . 0.9114 ?
N4 H2 . 0.9114 ?
N4 H3 . 0.9114 ?
N4 H4 . 0.9094 ?
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
N4 H2 O2 2_545 0.91 2.12 2.823(3) 133
N4 H2 O4 2_545 0.91 2.60 3.151(3) 120
N4 H3 O1 1_545 0.91 2.11 3.010(3) 172
N4 H4 O1 3_565 0.91 2.12 2.927(3) 147
_journal_paper_doi 10.1107/S0108270111010535