#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:14:32 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180174 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/70/7107071.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7107071
loop_
_publ_author_name
'Motoshi Tamura'
'Kiyoshi Tsuge'
'Asako Igashira-Kamiyama'
'Takumi Konno'
_publ_section_title
;
 A bis-bipyridine osmium(II) complex with an N,S-chelating
 2-aminoethanesulfinate: photoinduced conversion of amine to imine donor
 group by air oxidation
;
_journal_name_full               Chem.Commun.
_journal_page_first              12464
_journal_paper_doi               10.1039/c1cc14342e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C22 H22 Cl2 N5 Na O10 Os S'
_chemical_formula_weight         832.60
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.6130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.5421(3)
_cell_length_b                   16.8001(7)
_cell_length_c                   34.0526(10)
_cell_measurement_reflns_used    19644
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.02
_cell_volume                     5422.6(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'Crystal Structure'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            26730
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    5.059
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.850
_refine_diff_density_min         -1.915
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6220
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0547P)²+44.8078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                5150
_reflns_number_total             6220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14342e.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7107071
loop_
_symmetry_equiv_pos_as_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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.27018(3) 0.471084(14) 0.118883(7) 0.03067(10) Uani 1 1 d . . .
S1 S 0.45253(19) 0.47616(10) 0.16691(5) 0.0387(4) Uani 1 1 d . . .
O1 O 0.4422(7) 0.4228(4) 0.20094(17) 0.0652(17) Uani 1 1 d . . .
O2 O 0.5067(6) 0.5538(3) 0.18211(16) 0.0498(12) Uani 1 1 d . . .
N1 N 0.4313(7) 0.4654(4) 0.07933(18) 0.0380(13) Uani 1 1 d . . .
H1 H 0.422(8) 0.495(5) 0.058(3) 0.046 Uiso 1 1 d . . .
H2 H 0.428(9) 0.426(5) 0.067(2) 0.046 Uiso 1 1 d . . .
C1 C 0.5898(8) 0.4360(5) 0.1415(2) 0.0545(19) Uani 1 1 d . . .
H3 H 0.6831 0.4489 0.1560 0.065 Uiso 1 1 calc R . .
H4 H 0.5807 0.3774 0.1396 0.065 Uiso 1 1 calc R . .
C2 C 0.5769(8) 0.4717(5) 0.1013(3) 0.054(2) Uani 1 1 d . . .
H5 H 0.6445 0.4449 0.0856 0.065 Uiso 1 1 calc R . .
H6 H 0.6037 0.5286 0.1036 0.065 Uiso 1 1 calc R . .
N2 N 0.1204(6) 0.4705(3) 0.15817(15) 0.0326(11) Uani 1 1 d . . .
C3 C 0.0564(8) 0.5358(4) 0.1713(2) 0.0432(16) Uani 1 1 d . . .
H7 H 0.0839 0.5868 0.1630 0.052 Uiso 1 1 calc R . .
C4 C -0.0441(8) 0.5310(4) 0.1956(2) 0.0454(17) Uani 1 1 d . . .
H8 H -0.0859 0.5781 0.2044 0.054 Uiso 1 1 calc R . .
C5 C -0.0870(8) 0.4576(5) 0.2080(2) 0.0467(17) Uani 1 1 d . . .
H9 H -0.1590 0.4533 0.2250 0.056 Uiso 1 1 calc R . .
C6 C -0.0227(7) 0.3907(5) 0.1951(2) 0.0428(16) Uani 1 1 d . . .
H10 H -0.0502 0.3395 0.2032 0.051 Uiso 1 1 calc R . .
C7 C 0.0825(7) 0.3977(4) 0.17024(19) 0.0374(14) Uani 1 1 d . . .
C8 C 0.1596(7) 0.3303(4) 0.15549(19) 0.0344(13) Uani 1 1 d . . .
C9 C 0.1367(8) 0.2521(4) 0.1657(2) 0.0411(15) Uani 1 1 d . . .
H11 H 0.0692 0.2394 0.1832 0.049 Uiso 1 1 calc R . .
C10 C 0.2128(8) 0.1931(4) 0.1502(2) 0.0494(18) Uani 1 1 d . . .
H12 H 0.1992 0.1390 0.1570 0.059 Uiso 1 1 calc R . .
C11 C 0.3086(9) 0.2126(4) 0.1248(2) 0.0494(18) Uani 1 1 d . . .
H13 H 0.3620 0.1722 0.1139 0.059 Uiso 1 1 calc R . .
C12 C 0.3272(8) 0.2911(4) 0.1153(2) 0.0452(17) Uani 1 1 d . . .
H14 H 0.3930 0.3042 0.0974 0.054 Uiso 1 1 calc R . .
N3 N 0.2546(6) 0.3504(3) 0.13071(15) 0.0335(11) Uani 1 1 d . . .
N4 N 0.2461(6) 0.5895(3) 0.10316(17) 0.0369(12) Uani 1 1 d . . .
C13 C 0.3325(8) 0.6500(4) 0.1160(2) 0.0429(16) Uani 1 1 d . . .
H15 H 0.4132 0.6389 0.1342 0.051 Uiso 1 1 calc R . .
C14 C 0.3080(9) 0.7276(4) 0.1035(3) 0.054(2) Uani 1 1 d . . .
H16 H 0.3711 0.7686 0.1134 0.064 Uiso 1 1 calc R . .
C15 C 0.1933(9) 0.7457(5) 0.0772(2) 0.0522(19) Uani 1 1 d . . .
H17 H 0.1766 0.7987 0.0682 0.063 Uiso 1 1 calc R . .
C16 C 0.1027(9) 0.6851(4) 0.0641(2) 0.0489(18) Uani 1 1 d . . .
H18 H 0.0216 0.6960 0.0460 0.059 Uiso 1 1 calc R . .
C17 C 0.1308(7) 0.6076(4) 0.07750(18) 0.0352(14) Uani 1 1 d . . .
C18 C 0.0450(8) 0.5395(5) 0.0629(2) 0.0416(16) Uani 1 1 d . . .
C19 C -0.0868(8) 0.5460(5) 0.0403(2) 0.0491(18) Uani 1 1 d . . .
H19 H -0.1266 0.5969 0.0342 0.059 Uiso 1 1 calc R . .
C20 C -0.1578(9) 0.4789(6) 0.0272(2) 0.057(2) Uani 1 1 d . . .
H20 H -0.2481 0.4826 0.0123 0.069 Uiso 1 1 calc R . .
C21 C -0.0966(8) 0.4053(6) 0.0358(2) 0.0513(19) Uani 1 1 d . . .
H21 H -0.1413 0.3579 0.0255 0.062 Uiso 1 1 calc R . .
C22 C 0.0307(8) 0.4018(5) 0.0596(2) 0.0442(16) Uani 1 1 d . . .
H22 H 0.0710 0.3512 0.0662 0.053 Uiso 1 1 calc R . .
N5 N 0.1002(6) 0.4678(3) 0.07379(15) 0.0330(12) Uani 1 1 d . . .
Na1 Na 0.5000 0.3363(2) 0.2500 0.0468(9) Uani 1 2 d S . .
Na2 Na 0.5000 0.5784(3) 0.2500 0.0590(11) Uani 1 2 d S . .
O3 O 0.2631(8) 0.2871(4) 0.2518(2) 0.092(3) Uani 1 1 d D . .
Cl1A Cl 0.2815(5) 0.2194(3) 0.27628(13) 0.0423(10) Uiso 0.50 1 d P . 1
O4A O 0.258(3) 0.1274(15) 0.2570(7) 0.116(8) Uiso 0.50 1 d P . 1
O5A O 0.4192(16) 0.2136(9) 0.2906(4) 0.083(4) Uiso 0.50 1 d P . 1
O6A O 0.1936(16) 0.2159(9) 0.3067(4) 0.076(4) Uiso 0.50 1 d P . 1
Cl1B Cl 0.2495(5) 0.2060(3) 0.26895(14) 0.0508(12) Uiso 0.50 1 d P . 2
O4B O 0.2455(18) 0.1513(8) 0.2487(4) 0.068(4) Uiso 0.50 1 d PD . 2
O5B O 0.3052(17) 0.2157(10) 0.3090(4) 0.098(5) Uiso 0.50 1 d PD . 2
O6B O 0.0936(15) 0.2092(11) 0.2685(5) 0.111(6) Uiso 0.50 1 d PD . 2
Cl2 Cl 0.0360(2) 0.15615(11) 0.01553(6) 0.0503(4) Uani 1 1 d . . .
O7 O 0.1097(11) 0.1616(5) -0.0176(3) 0.116(3) Uani 1 1 d . A .
O8A O 0.0176(14) 0.2389(8) 0.0267(4) 0.072(3) Uiso 0.50 1 d P A 1
O9A O 0.1139(17) 0.1175(11) 0.0487(5) 0.083(4) Uiso 0.50 1 d P A 1
O10A O -0.094(2) 0.1164(14) 0.0099(6) 0.121(6) Uiso 0.50 1 d P A 1
O8B O -0.1000(19) 0.1929(12) 0.0120(5) 0.100(5) Uiso 0.50 1 d P A 2
O9B O 0.124(2) 0.1713(13) 0.0499(5) 0.104(5) Uiso 0.50 1 d P A 2
O10B O 0.002(2) 0.0695(11) 0.0138(5) 0.102(5) Uiso 0.50 1 d P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 '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'
Os Os -1.2165 7.6030 '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'
Na Na 0.0362 0.0249 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N4 Os1 N2 96.2(2) . .
N4 Os1 N3 169.2(2) . .
N2 Os1 N3 78.4(2) . .
N4 Os1 N5 77.4(2) . .
N2 Os1 N5 86.6(2) . .
N3 Os1 N5 92.9(2) . .
N4 Os1 N1 86.9(2) . .
N2 Os1 N1 176.7(2) . .
N3 Os1 N1 98.6(2) . .
N5 Os1 N1 95.1(2) . .
N4 Os1 S1 101.86(17) . .
N2 Os1 S1 93.68(15) . .
N3 Os1 S1 87.86(15) . .
N5 Os1 S1 179.28(15) . .
N1 Os1 S1 84.74(18) . .
O2 S1 O1 108.3(3) . .
O2 S1 C1 104.9(4) . .
O1 S1 C1 105.7(4) . .
O2 S1 Os1 120.0(2) . .
O1 S1 Os1 115.6(2) . .
C1 S1 Os1 100.5(3) . .
O1 S1 Na2 70.0(3) . .
C1 S1 Na2 125.3(3) . .
Os1 S1 Na2 131.50(8) . .
S1 O1 Na1 161.4(4) . .
S1 O2 Na2 116.8(3) . .
C2 N1 Os1 111.8(4) . .
C2 N1 H1 112(5) . .
Os1 N1 H1 119(6) . .
C2 N1 H2 108(6) . .
Os1 N1 H2 112(6) . .
H1 N1 H2 92(8) . .
C2 C1 S1 107.9(6) . .
C2 C1 H3 110.1 . .
S1 C1 H3 110.1 . .
C2 C1 H4 110.1 . .
S1 C1 H4 110.1 . .
H3 C1 H4 108.4 . .
C1 C2 N1 113.8(6) . .
C1 C2 H5 108.8 . .
N1 C2 H5 108.8 . .
C1 C2 H6 108.8 . .
N1 C2 H6 108.8 . .
H5 C2 H6 107.7 . .
C7 N2 C3 118.9(6) . .
C7 N2 Os1 115.5(4) . .
C3 N2 Os1 125.5(5) . .
C4 C3 N2 122.5(7) . .
C4 C3 H7 118.7 . .
N2 C3 H7 118.7 . .
C3 C4 C5 120.1(7) . .
C3 C4 H8 120.0 . .
C5 C4 H8 120.0 . .
C6 C5 C4 118.2(7) . .
C6 C5 H9 120.9 . .
C4 C5 H9 120.9 . .
C5 C6 C7 120.3(7) . .
C5 C6 H10 119.8 . .
C7 C6 H10 119.8 . .
N2 C7 C6 120.0(6) . .
N2 C7 C8 115.5(6) . .
C6 C7 C8 124.5(6) . .
N3 C8 C9 122.1(6) . .
N3 C8 C7 114.7(5) . .
C9 C8 C7 123.2(6) . .
C10 C9 C8 119.0(7) . .
C10 C9 H11 120.5 . .
C8 C9 H11 120.5 . .
C11 C10 C9 119.5(7) . .
C11 C10 H12 120.3 . .
C9 C10 H12 120.3 . .
C10 C11 C12 119.6(7) . .
C10 C11 H13 120.2 . .
C12 C11 H13 120.2 . .
N3 C12 C11 121.9(7) . .
N3 C12 H14 119.1 . .
C11 C12 H14 119.1 . .
C8 N3 C12 118.0(6) . .
C8 N3 Os1 115.7(4) . .
C12 N3 Os1 126.3(5) . .
C13 N4 C17 117.3(6) . .
C13 N4 Os1 126.6(5) . .
C17 N4 Os1 116.1(5) . .
N4 C13 C14 122.4(7) . .
N4 C13 H15 118.8 . .
C14 C13 H15 118.8 . .
C15 C14 C13 120.3(8) . .
C15 C14 H16 119.8 . .
C13 C14 H16 119.8 . .
C14 C15 C16 118.4(7) . .
C14 C15 H17 120.8 . .
C16 C15 H17 120.8 . .
C15 C16 C17 119.5(7) . .
C15 C16 H18 120.2 . .
C17 C16 H18 120.2 . .
N4 C17 C16 122.0(7) . .
N4 C17 C18 115.1(6) . .
C16 C17 C18 122.7(6) . .
N5 C18 C19 121.2(7) . .
N5 C18 C17 114.8(6) . .
C19 C18 C17 124.0(7) . .
C20 C19 C18 119.8(8) . .
C20 C19 H19 120.1 . .
C18 C19 H19 120.1 . .
C19 C20 C21 119.1(8) . .
C19 C20 H20 120.4 . .
C21 C20 H20 120.4 . .
C22 C21 C20 118.9(8) . .
C22 C21 H21 120.6 . .
C20 C21 H21 120.6 . .
N5 C22 C21 122.5(7) . .
N5 C22 H22 118.7 . .
C21 C22 H22 118.7 . .
C18 N5 C22 118.3(6) . .
C18 N5 Os1 114.9(4) . .
C22 N5 Os1 126.0(5) . .
O1 Na1 O1 98.8(4) . 2_655
O1 Na1 O3 110.8(3) . 2_655
O1 Na1 O3 95.2(2) 2_655 2_655
O1 Na1 O3 95.2(2) . .
O1 Na1 O3 110.8(3) 2_655 .
O3 Na1 O3 140.0(4) 2_655 .
O1 Na1 O5A 100.2(4) . 2_655
O1 Na1 O5A 146.7(4) 2_655 2_655
O3 Na1 O5A 52.4(4) 2_655 2_655
O3 Na1 O5A 94.4(4) . 2_655
O1 Na1 O5A 146.7(4) . .
O1 Na1 O5A 100.2(4) 2_655 .
O3 Na1 O5A 94.4(4) 2_655 .
O3 Na1 O5A 52.4(4) . .
O5A Na1 O5A 77.7(7) 2_655 .
O1 Na1 Cl1A 121.07(18) . .
O1 Na1 Cl1A 108.4(2) 2_655 .
O3 Na1 Cl1A 117.3(3) 2_655 .
O3 Na1 Cl1A 26.47(18) . .
O5A Na1 Cl1A 84.4(4) 2_655 .
O5A Na1 Cl1A 26.0(3) . .
O1 Na1 Cl1A 108.4(2) . 2_655
O1 Na1 Cl1A 121.07(18) 2_655 2_655
O3 Na1 Cl1A 26.46(18) 2_655 2_655
O3 Na1 Cl1A 117.3(3) . 2_655
O5A Na1 Cl1A 26.0(3) 2_655 2_655
O5A Na1 Cl1A 84.4(4) . 2_655
Cl1A Na1 Cl1A 100.52(19) . 2_655
O1 Na1 Na2 49.42(19) . .
O1 Na1 Na2 49.42(19) 2_655 .
O3 Na1 Na2 110.0(2) 2_655 .
O3 Na1 Na2 110.0(2) . .
O5A Na1 Na2 141.2(3) 2_655 .
O5A Na1 Na2 141.2(3) . .
Cl1A Na1 Na2 129.74(10) . .
Cl1A Na1 Na2 129.74(10) 2_655 .
O2 Na2 O2 159.9(4) . 2_655
O2 Na2 O6B 111.2(4) . 3
O2 Na2 O6B 87.4(4) 2_655 3
O2 Na2 O6B 87.4(4) . 4
O2 Na2 O6B 111.2(4) 2_655 4
O6B Na2 O6B 50.3(8) 3 4
O2 Na2 O4A 90.8(5) . 3
O2 Na2 O4A 95.7(5) 2_655 3
O6B Na2 O4A 50.8(7) 3 3
O6B Na2 O4A 93.0(7) 4 3
O2 Na2 O4A 95.7(5) . 4
O2 Na2 O4A 90.8(5) 2_655 4
O6B Na2 O4A 93.0(7) 3 4
O6B Na2 O4A 50.8(7) 4 4
O4A Na2 O4A 142.7(12) 3 4
O2 Na2 O4B 102.8(4) . 4
O2 Na2 O4B 86.6(3) 2_655 4
O6B Na2 O4B 82.9(5) 3 4
O6B Na2 O4B 44.4(5) 4 4
O4A Na2 O4B 133.3(7) 3 4
O4A Na2 O4B 10.8(7) 4 4
O2 Na2 O4B 86.6(3) . 3
O2 Na2 O4B 102.8(4) 2_655 3
O6B Na2 O4B 44.4(5) 3 3
O6B Na2 O4B 82.9(5) 4 3
O4A Na2 O4B 10.8(7) 3 3
O4A Na2 O4B 133.3(7) 4 3
O4B Na2 O4B 124.9(7) 4 3
O2 Na2 Cl1B 102.14(18) . 3
O2 Na2 Cl1B 91.32(17) 2_655 3
O6B Na2 Cl1B 26.1(4) 3 3
O6B Na2 Cl1B 71.9(4) 4 3
O4A Na2 Cl1B 24.7(6) 3 3
O4A Na2 Cl1B 118.8(6) 4 3
O4B Na2 Cl1B 108.9(4) 4 3
O4B Na2 Cl1B 19.7(3) 3 3
O2 Na2 Cl1B 91.32(17) . 4
O2 Na2 Cl1B 102.14(18) 2_655 4
O6B Na2 Cl1B 71.9(4) 3 4
O6B Na2 Cl1B 26.1(4) 4 4
O4A Na2 Cl1B 118.8(6) 3 4
O4A Na2 Cl1B 24.7(6) 4 4
O4B Na2 Cl1B 19.7(3) 4 4
O4B Na2 Cl1B 108.9(4) 3 4
Cl1B Na2 Cl1B 96.3(2) 3 4
O2 Na2 S1 23.56(14) . .
O2 Na2 S1 137.3(2) 2_655 .
O6B Na2 S1 134.8(4) 3 .
O6B Na2 S1 103.8(4) 4 .
O4A Na2 S1 106.3(5) 3 .
O4A Na2 S1 93.0(5) 4 .
O4B Na2 S1 102.8(3) 4 .
O4B Na2 S1 105.1(3) 3 .
Cl1B Na2 S1 123.05(9) 3 .
Cl1B Na2 S1 98.62(9) 4 .
O2 Na2 S1 137.3(2) . 2_655
O2 Na2 S1 23.56(14) 2_655 2_655
O6B Na2 S1 103.8(4) 3 2_655
O6B Na2 S1 134.8(4) 4 2_655
O4A Na2 S1 93.0(5) 3 2_655
O4A Na2 S1 106.3(5) 4 2_655
O4B Na2 S1 105.1(3) 4 2_655
O4B Na2 S1 102.8(3) 3 2_655
Cl1B Na2 S1 98.62(9) 3 2_655
Cl1B Na2 S1 123.05(9) 4 2_655
S1 Na2 S1 117.21(16) . 2_655
Cl1A O3 Na1 103.8(4) . .
Cl1B O3 Na1 116.5(5) . .
O5A Cl1A O6A 111.6(9) . .
O5A Cl1A O3 108.7(8) . .
O6A Cl1A O3 115.2(7) . .
O5A Cl1A O4A 99.1(11) . .
O6A Cl1A O4A 100.6(11) . .
O3 Cl1A O4A 120.6(9) . .
O5A Cl1A Na1 59.1(7) . .
O6A Cl1A Na1 136.3(7) . .
O3 Cl1A Na1 49.7(3) . .
O4A Cl1A Na1 122.6(9) . .
Cl1A O4A Na2 114.5(12) . 3_445
Cl1A O5A Na1 94.9(8) . .
O4B Cl1B O5B 130.8(11) . .
O4B Cl1B O6B 93.4(12) . .
O5B Cl1B O6B 105.7(9) . .
O4B Cl1B O3 119.7(9) . .
O5B Cl1B O3 103.4(8) . .
O6B Cl1B O3 95.4(8) . .
O4B Cl1B Na2 51.1(9) . 3_445
O5B Cl1B Na2 117.2(7) . 3_445
O6B Cl1B Na2 46.0(7) . 3_445
O3 Cl1B Na2 128.8(4) . 3_445
Cl1B O4B Na2 109.2(11) . 3_445
Cl1B O6B Na2 107.9(10) . 3_445
O9B Cl2 O10A 130.1(12) . .
O9B Cl2 O7 111.1(9) . .
O10A Cl2 O7 116.0(9) . .
O9B Cl2 O8B 116.5(11) . .
O10A Cl2 O8B 54.2(11) . .
O7 Cl2 O8B 116.1(8) . .
O10A Cl2 O9A 105.2(11) . .
O7 Cl2 O9A 113.7(8) . .
O8B Cl2 O9A 130.1(9) . .
O9B Cl2 O8A 71.5(10) . .
O10A Cl2 O8A 111.1(11) . .
O7 Cl2 O8A 103.5(6) . .
O8B Cl2 O8A 58.3(9) . .
O9A Cl2 O8A 107.1(9) . .
O9B Cl2 O10B 108.6(11) . .
O10A Cl2 O10B 49.1(10) . .
O7 Cl2 O10B 99.1(8) . .
O8B Cl2 O10B 103.3(10) . .
O9A Cl2 O10B 71.2(10) . .
O8A Cl2 O10B 155.5(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 N4 2.066(5) .
Os1 N2 2.067(6) .
Os1 N3 2.076(5) .
Os1 N5 2.102(5) .
Os1 N1 2.160(6) .
Os1 S1 2.2481(18) .
S1 O2 1.476(6) .
S1 O1 1.477(6) .
S1 C1 1.784(8) .
S1 Na2 3.296(3) .
O1 Na1 2.236(6) .
O2 Na2 2.356(5) .
N1 C2 1.503(11) .
N1 H1 0.87(9) .
N1 H2 0.79(8) .
C1 C2 1.487(12) .
C1 H3 0.9900 .
C1 H4 0.9900 .
C2 H5 0.9900 .
C2 H6 0.9900 .
N2 C7 1.352(8) .
N2 C3 1.357(9) .
C3 C4 1.339(11) .
C3 H7 0.9500 .
C4 C5 1.380(11) .
C4 H8 0.9500 .
C5 C6 1.377(11) .
C5 H9 0.9500 .
C6 C7 1.390(9) .
C6 H10 0.9500 .
C7 C8 1.471(9) .
C8 N3 1.351(8) .
C8 C9 1.382(9) .
C9 C10 1.370(10) .
C9 H11 0.9500 .
C10 C11 1.367(11) .
C10 H12 0.9500 .
C11 C12 1.375(10) .
C11 H13 0.9500 .
C12 N3 1.353(9) .
C12 H14 0.9500 .
N4 C13 1.350(9) .
N4 C17 1.359(9) .
C13 C14 1.382(10) .
C13 H15 0.9500 .
C14 C15 1.366(12) .
C14 H16 0.9500 .
C15 C16 1.376(11) .
C15 H17 0.9500 .
C16 C17 1.397(10) .
C16 H18 0.9500 .
C17 C18 1.460(10) .
C18 N5 1.349(9) .
C18 C19 1.402(10) .
C19 C20 1.364(12) .
C19 H19 0.9500 .
C20 C21 1.385(12) .
C20 H20 0.9500 .
C21 C22 1.382(11) .
C21 H21 0.9500 .
C22 N5 1.352(9) .
C22 H22 0.9500 .
Na1 O1 2.236(6) 2_655
Na1 O3 2.414(7) 2_655
Na1 O3 2.414(7) .
Na1 O5A 2.645(16) 2_655
Na1 O5A 2.645(16) .
Na1 Cl1A 3.072(5) .
Na1 Cl1A 3.072(5) 2_655
Na1 Na2 4.067(6) .
Na2 O2 2.356(5) 2_655
Na2 O6B 2.429(18) 3
Na2 O6B 2.429(18) 4
Na2 O4A 2.58(3) 3
Na2 O4A 2.58(3) 4
Na2 O4B 2.649(16) 4
Na2 O4B 2.649(16) 3
Na2 Cl1B 3.214(7) 3
Na2 Cl1B 3.214(6) 4
Na2 S1 3.296(3) 2_655
O3 Cl1A 1.410(7) .
O3 Cl1B 1.494(8) .
Cl1A O5A 1.352(16) .
Cl1A O6A 1.408(15) .
Cl1A O4A 1.68(3) .
O4A Na2 2.58(3) 3_445
Cl1B O4B 1.147(13) .
Cl1B O5B 1.416(13) .
Cl1B O6B 1.487(15) .
Cl1B Na2 3.214(6) 3_445
O4B Na2 2.649(16) 3_445
O6B Na2 2.429(18) 3_445
Cl2 O9B 1.380(19) .
Cl2 O10A 1.40(2) .
Cl2 O7 1.400(8) .
Cl2 O8B 1.430(18) .
Cl2 O9A 1.435(16) .
Cl2 O8A 1.458(14) .
Cl2 O10B 1.490(19) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O10B 0.87(9) 2.17(9) 2.973(19) 153(7) 3
N1 H2 O7 0.79(8) 2.23(8) 2.989(10) 163(8) 7
N1 H1 O10A 0.87(9) 2.61(9) 3.46(2) 163(8) 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N4 Os1 S1 O2 8.1(3) . .
N2 Os1 S1 O2 -89.1(3) . .
N3 Os1 S1 O2 -167.3(3) . .
N1 Os1 S1 O2 93.8(3) . .
N4 Os1 S1 O1 140.7(4) . .
N2 Os1 S1 O1 43.6(4) . .
N3 Os1 S1 O1 -34.7(4) . .
N1 Os1 S1 O1 -133.6(4) . .
N4 Os1 S1 C1 -106.1(3) . .
N2 Os1 S1 C1 156.8(3) . .
N3 Os1 S1 C1 78.5(3) . .
N1 Os1 S1 C1 -20.4(4) . .
N4 Os1 S1 Na2 55.50(19) . .
N2 Os1 S1 Na2 -41.63(19) . .
N3 Os1 S1 Na2 -119.87(19) . .
N1 Os1 S1 Na2 141.2(2) . .
O2 S1 O1 Na1 -84.2(14) . .
C1 S1 O1 Na1 27.8(14) . .
Os1 S1 O1 Na1 137.9(12) . .
Na2 S1 O1 Na1 -94.7(13) . .
O1 S1 O2 Na2 -15.5(5) . .
C1 S1 O2 Na2 -128.0(4) . .
Os1 S1 O2 Na2 120.2(2) . .
N4 Os1 N1 C2 99.3(5) . .
N3 Os1 N1 C2 -89.9(5) . .
N5 Os1 N1 C2 176.4(5) . .
S1 Os1 N1 C2 -2.9(5) . .
O2 S1 C1 C2 -82.2(6) . .
O1 S1 C1 C2 163.4(6) . .
Os1 S1 C1 C2 42.9(6) . .
Na2 S1 C1 C2 -120.3(5) . .
S1 C1 C2 N1 -51.3(9) . .
Os1 N1 C2 C1 32.5(8) . .
N4 Os1 N2 C7 167.8(5) . .
N3 Os1 N2 C7 -2.8(4) . .
N5 Os1 N2 C7 90.8(5) . .
S1 Os1 N2 C7 -89.8(4) . .
N4 Os1 N2 C3 -10.1(6) . .
N3 Os1 N2 C3 179.3(6) . .
N5 Os1 N2 C3 -87.1(6) . .
S1 Os1 N2 C3 92.3(5) . .
C7 N2 C3 C4 -0.6(11) . .
Os1 N2 C3 C4 177.3(6) . .
N2 C3 C4 C5 -0.5(12) . .
C3 C4 C5 C6 0.8(12) . .
C4 C5 C6 C7 -0.1(11) . .
C3 N2 C7 C6 1.3(10) . .
Os1 N2 C7 C6 -176.8(5) . .
C3 N2 C7 C8 -178.4(6) . .
Os1 N2 C7 C8 3.5(7) . .
C5 C6 C7 N2 -1.0(11) . .
C5 C6 C7 C8 178.7(7) . .
N2 C7 C8 N3 -2.2(9) . .
C6 C7 C8 N3 178.1(6) . .
N2 C7 C8 C9 178.3(6) . .
C6 C7 C8 C9 -1.3(11) . .
N3 C8 C9 C10 0.0(11) . .
C7 C8 C9 C10 179.4(7) . .
C8 C9 C10 C11 -0.5(12) . .
C9 C10 C11 C12 0.0(12) . .
C10 C11 C12 N3 0.9(13) . .
C9 C8 N3 C12 0.9(10) . .
C7 C8 N3 C12 -178.6(6) . .
C9 C8 N3 Os1 179.3(5) . .
C7 C8 N3 Os1 -0.2(7) . .
C11 C12 N3 C8 -1.3(11) . .
C11 C12 N3 Os1 -179.5(6) . .
N4 Os1 N3 C8 -59.2(12) . .
N2 Os1 N3 C8 1.5(4) . .
N5 Os1 N3 C8 -84.3(5) . .
N1 Os1 N3 C8 -179.9(5) . .
S1 Os1 N3 C8 95.7(4) . .
N4 Os1 N3 C12 119.0(11) . .
N2 Os1 N3 C12 179.8(6) . .
N5 Os1 N3 C12 93.9(6) . .
N1 Os1 N3 C12 -1.6(6) . .
S1 Os1 N3 C12 -86.0(6) . .
N2 Os1 N4 C13 102.5(5) . .
N3 Os1 N4 C13 161.8(10) . .
N5 Os1 N4 C13 -172.5(6) . .
N1 Os1 N4 C13 -76.6(6) . .
S1 Os1 N4 C13 7.4(6) . .
N2 Os1 N4 C17 -77.1(4) . .
N3 Os1 N4 C17 -17.8(13) . .
N5 Os1 N4 C17 8.0(4) . .
N1 Os1 N4 C17 103.8(5) . .
S1 Os1 N4 C17 -172.2(4) . .
C17 N4 C13 C14 -0.8(10) . .
Os1 N4 C13 C14 179.6(6) . .
N4 C13 C14 C15 -0.3(12) . .
C13 C14 C15 C16 1.0(12) . .
C14 C15 C16 C17 -0.7(12) . .
C13 N4 C17 C16 1.2(9) . .
Os1 N4 C17 C16 -179.2(5) . .
C13 N4 C17 C18 176.9(6) . .
Os1 N4 C17 C18 -3.5(7) . .
C15 C16 C17 N4 -0.4(11) . .
C15 C16 C17 C18 -175.8(7) . .
N4 C17 C18 N5 -6.6(8) . .
C16 C17 C18 N5 169.1(6) . .
N4 C17 C18 C19 171.7(7) . .
C16 C17 C18 C19 -12.6(11) . .
N5 C18 C19 C20 -3.5(11) . .
C17 C18 C19 C20 178.3(7) . .
C18 C19 C20 C21 -1.3(12) . .
C19 C20 C21 C22 4.0(11) . .
C20 C21 C22 N5 -2.2(11) . .
C19 C18 N5 C22 5.4(10) . .
C17 C18 N5 C22 -176.3(5) . .
C19 C18 N5 Os1 -165.0(6) . .
C17 C18 N5 Os1 13.3(7) . .
C21 C22 N5 C18 -2.5(10) . .
C21 C22 N5 Os1 166.7(5) . .
N4 Os1 N5 C18 -11.6(5) . .
N2 Os1 N5 C18 85.5(5) . .
N3 Os1 N5 C18 163.7(5) . .
N1 Os1 N5 C18 -97.3(5) . .
N4 Os1 N5 C22 178.9(6) . .
N2 Os1 N5 C22 -84.0(6) . .
N3 Os1 N5 C22 -5.8(6) . .
N1 Os1 N5 C22 93.2(6) . .
S1 O1 Na1 O1 92.4(13) . 2_655
S1 O1 Na1 O3 -6.7(14) . 2_655
S1 O1 Na1 O3 -155.7(13) . .
S1 O1 Na1 O5A -60.2(14) . 2_655
S1 O1 Na1 O5A -143.3(12) . .
S1 O1 Na1 Cl1A -149.8(12) . .
S1 O1 Na1 Cl1A -34.7(14) . 2_655
S1 O1 Na1 Na2 92.4(13) . .
S1 O2 Na2 O2 23.6(3) . 2_655
S1 O2 Na2 O6B -179.9(5) . 3
S1 O2 Na2 O6B -134.6(5) . 4
S1 O2 Na2 O4A 132.4(7) . 3
S1 O2 Na2 O4A -84.4(7) . 4
S1 O2 Na2 O4B -92.7(5) . 4
S1 O2 Na2 O4B 142.3(5) . 3
S1 O2 Na2 Cl1B 154.5(3) . 3
S1 O2 Na2 Cl1B -108.8(3) . 4
S1 O2 Na2 S1 37.2(5) . 2_655
O1 S1 Na2 O2 164.4(5) . .
C1 S1 Na2 O2 68.9(5) . .
Os1 S1 Na2 O2 -88.7(4) . .
O2 S1 Na2 O2 -168.3(2) . 2_655
O1 S1 Na2 O2 -3.9(3) . 2_655
C1 S1 Na2 O2 -99.4(4) . 2_655
Os1 S1 Na2 O2 103.0(2) . 2_655
O2 S1 Na2 O6B 0.1(7) . 3
O1 S1 Na2 O6B 164.5(6) . 3
C1 S1 Na2 O6B 69.1(7) . 3
Os1 S1 Na2 O6B -88.6(5) . 3
O2 S1 Na2 O6B 47.1(5) . 4
O1 S1 Na2 O6B -148.6(5) . 4
C1 S1 Na2 O6B 116.0(5) . 4
Os1 S1 Na2 O6B -41.7(4) . 4
O2 S1 Na2 O4A -50.3(7) . 3
O1 S1 Na2 O4A 114.0(7) . 3
C1 S1 Na2 O4A 18.6(7) . 3
Os1 S1 Na2 O4A -139.1(6) . 3
O2 S1 Na2 O4A 97.3(7) . 4
O1 S1 Na2 O4A -98.3(6) . 4
C1 S1 Na2 O4A 166.3(7) . 4
Os1 S1 Na2 O4A 8.6(6) . 4
O2 S1 Na2 O4B 92.8(5) . 4
O1 S1 Na2 O4B -102.9(4) . 4
C1 S1 Na2 O4B 161.7(5) . 4
Os1 S1 Na2 O4B 4.0(4) . 4
O2 S1 Na2 O4B -39.2(5) . 3
O1 S1 Na2 O4B 125.2(5) . 3
C1 S1 Na2 O4B 29.7(5) . 3
Os1 S1 Na2 O4B -127.9(4) . 3
O2 S1 Na2 Cl1B -30.2(4) . 3
O1 S1 Na2 Cl1B 134.2(3) . 3
C1 S1 Na2 Cl1B 38.8(4) . 3
Os1 S1 Na2 Cl1B -118.89(14) . 3
O2 S1 Na2 Cl1B 73.2(4) . 4
O1 S1 Na2 Cl1B -122.5(3) . 4
C1 S1 Na2 Cl1B 142.1(4) . 4
Os1 S1 Na2 Cl1B -15.56(17) . 4
O2 S1 Na2 S1 -152.6(4) . 2_655
O1 S1 Na2 S1 11.8(3) . 2_655
C1 S1 Na2 S1 -83.6(4) . 2_655
Os1 S1 Na2 S1 118.72(11) . 2_655
O1 Na1 O3 Cl1A 168.7(5) . .
O1 Na1 O3 Cl1A -89.7(5) 2_655 .
O3 Na1 O3 Cl1A 37.3(4) 2_655 .
O5A Na1 O3 Cl1A 68.0(6) 2_655 .
O5A Na1 O3 Cl1A -2.7(5) . .
Cl1A Na1 O3 Cl1A 55.0(5) 2_655 .
Na2 Na1 O3 Cl1A -142.7(4) . .
O1 Na1 O3 Cl1B 156.9(5) . .
O1 Na1 O3 Cl1B -101.6(5) 2_655 .
O3 Na1 O3 Cl1B 25.4(4) 2_655 .
O5A Na1 O3 Cl1B 56.2(6) 2_655 .
O5A Na1 O3 Cl1B -14.6(5) . .
Cl1A Na1 O3 Cl1B -11.9(3) . .
Cl1A Na1 O3 Cl1B 43.1(5) 2_655 .
Na2 Na1 O3 Cl1B -154.6(4) . .
Cl1B O3 Cl1A O5A 145.1(14) . .
Na1 O3 Cl1A O5A 4.5(8) . .
Cl1B O3 Cl1A O6A -88.9(13) . .
Na1 O3 Cl1A O6A 130.5(8) . .
Cl1B O3 Cl1A O4A 32.0(13) . .
Na1 O3 Cl1A O4A -108.7(11) . .
Cl1B O3 Cl1A Na1 140.6(10) . .
O1 Na1 Cl1A O5A 171.8(8) . .
O1 Na1 Cl1A O5A -75.2(8) 2_655 .
O3 Na1 Cl1A O5A 30.9(8) 2_655 .
O3 Na1 Cl1A O5A -175.0(9) . .
O5A Na1 Cl1A O5A 73.2(10) 2_655 .
Cl1A Na1 Cl1A O5A 52.7(8) 2_655 .
Na2 Na1 Cl1A O5A -127.3(8) . .
O1 Na1 Cl1A O6A -98.5(10) . .
O1 Na1 Cl1A O6A 14.4(10) 2_655 .
O3 Na1 Cl1A O6A 120.6(10) 2_655 .
O3 Na1 Cl1A O6A -85.4(11) . .
O5A Na1 Cl1A O6A 162.9(10) 2_655 .
O5A Na1 Cl1A O6A 89.6(12) . .
Cl1A Na1 Cl1A O6A 142.4(10) 2_655 .
Na2 Na1 Cl1A O6A -37.6(10) . .
O1 Na1 Cl1A O3 -13.1(5) . .
O1 Na1 Cl1A O3 99.8(5) 2_655 .
O3 Na1 Cl1A O3 -154.0(4) 2_655 .
O5A Na1 Cl1A O3 -111.7(6) 2_655 .
O5A Na1 Cl1A O3 175.0(9) . .
Cl1A Na1 Cl1A O3 -132.2(5) 2_655 .
Na2 Na1 Cl1A O3 47.8(5) . .
O1 Na1 Cl1A O4A 91.3(11) . .
O1 Na1 Cl1A O4A -155.7(10) 2_655 .
O3 Na1 Cl1A O4A -49.6(11) 2_655 .
O3 Na1 Cl1A O4A 104.4(11) . .
O5A Na1 Cl1A O4A -7.3(11) 2_655 .
O5A Na1 Cl1A O4A -80.5(13) . .
Cl1A Na1 Cl1A O4A -27.8(10) 2_655 .
Na2 Na1 Cl1A O4A 152.2(10) . .
O5A Cl1A O4A Na2 156.2(11) . 3_445
O6A Cl1A O4A Na2 42.1(13) . 3_445
O3 Cl1A O4A Na2 -85.7(12) . 3_445
Na1 Cl1A O4A Na2 -144.8(6) . 3_445
O6A Cl1A O5A Na1 -132.0(7) . .
O3 Cl1A O5A Na1 -4.0(8) . .
O4A Cl1A O5A Na1 122.7(9) . .
O1 Na1 O5A Cl1A -12.8(13) . .
O1 Na1 O5A Cl1A 111.2(7) 2_655 .
O3 Na1 O5A Cl1A -152.7(7) 2_655 .
O3 Na1 O5A Cl1A 2.8(5) . .
O5A Na1 O5A Cl1A -102.7(9) 2_655 .
Cl1A Na1 O5A Cl1A -128.2(7) 2_655 .
Na2 Na1 O5A Cl1A 77.3(9) . .
Cl1A O3 Cl1B O4B -133.8(16) . .
Na1 O3 Cl1B O4B -90.3(11) . .
Cl1A O3 Cl1B O5B 21.6(11) . .
Na1 O3 Cl1B O5B 65.1(9) . .
Cl1A O3 Cl1B O6B 129.2(13) . .
Na1 O3 Cl1B O6B 172.7(8) . .
Cl1A O3 Cl1B Na2 164.2(13) . 3_445
Na1 O3 Cl1B Na2 -152.3(3) . 3_445
O5B Cl1B O4B Na2 94.6(14) . 3_445
O6B Cl1B O4B Na2 -19.6(10) . 3_445
O3 Cl1B O4B Na2 -117.8(8) . 3_445
O4B Cl1B O6B Na2 21.3(11) . 3_445
O5B Cl1B O6B Na2 -112.9(9) . 3_445
O3 Cl1B O6B Na2 141.5(7) . 3_445
