#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:57:47 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179086 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/48/4304895.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_4304895
loop_
_publ_author_name
'Laura L. Perissinotti'
'Gregory Leitus'
'Linda Shimon'
'Dario Estrin'
'Fabio Doctorovich'
_publ_section_title
;
A Unique Family of Stable and Water-Soluble S-Nitrosothiol Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4723
_journal_page_last               4733
_journal_paper_doi               10.1021/ic7024999
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C8 H12 Cl4 Ir K N4'
_chemical_formula_weight         537.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.5310(2)
_cell_length_b                   19.3820(6)
_cell_length_c                   23.7470(7)
_cell_measurement_reflns_used    5398
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.55
_cell_volume                     3466.25(17)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5045
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    8.549
_exptl_absorpt_correction_T_max  0.6745
_exptl_absorpt_correction_T_min  0.2797
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.003
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0413P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                3508
_reflns_number_total             5045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7024999-file003.cif
_cod_data_source_block           m664a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4304895
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
Ir1 Ir 0.18897(2) 0.228816(9) 0.125592(6) 0.02192(6) Uani 1 1 d . . .
Cl1 Cl 0.36724(13) 0.31324(5) 0.08353(4) 0.0244(2) Uani 1 1 d . . .
Cl2 Cl 0.20133(13) 0.16180(6) 0.04375(4) 0.0279(2) Uani 1 1 d . . .
Cl3 Cl -0.06374(13) 0.28678(6) 0.09113(4) 0.0293(2) Uani 1 1 d . . .
Cl4 Cl 0.44415(13) 0.17206(6) 0.15996(4) 0.0312(2) Uani 1 1 d . . .
N1 N 0.0302(4) 0.15898(19) 0.16131(14) 0.0281(8) Uani 1 1 d . . .
C1 C -0.0676(5) 0.1231(2) 0.18277(17) 0.0270(9) Uani 1 1 d . . .
C2 C -0.1907(5) 0.0784(3) 0.2115(2) 0.0339(11) Uani 1 1 d . . .
H2A H -0.1355 0.0332 0.2175 0.051 Uiso 1 1 calc R . .
H2B H -0.2980 0.0729 0.1886 0.051 Uiso 1 1 calc R . .
H2C H -0.2224 0.0987 0.2479 0.051 Uiso 1 1 calc R . .
N2 N 0.1783(4) 0.28446(19) 0.19728(14) 0.0221(8) Uani 1 1 d . . .
C3 C 0.1707(5) 0.3093(2) 0.23973(18) 0.0279(10) Uani 1 1 d . . .
C4 C 0.1638(6) 0.3420(3) 0.29446(19) 0.0371(12) Uani 1 1 d . . .
H4A H 0.2848 0.3522 0.3073 0.056 Uiso 1 1 calc R . .
H4B H 0.1060 0.3110 0.3214 0.056 Uiso 1 1 calc R . .
H4C H 0.0961 0.3851 0.2918 0.056 Uiso 1 1 calc R . .
N3 N 0.3390(6) 0.4660(3) 0.1995(2) 0.0599(14) Uani 1 1 d . . .
C5 C 0.2486(7) 0.4733(3) 0.1608(3) 0.0498(15) Uani 1 1 d . . .
C6 C 0.1370(10) 0.4830(4) 0.1127(3) 0.089(3) Uani 1 1 d . . .
H6A H 0.0134 0.4737 0.1230 0.134 Uiso 1 1 calc R . .
H6B H 0.1735 0.4514 0.0826 0.134 Uiso 1 1 calc R . .
H6C H 0.1478 0.5307 0.0994 0.134 Uiso 1 1 calc R . .
N4 N 0.7210(7) 0.0642(3) 0.0412(3) 0.077(2) Uani 1 1 d . . .
C7 C 0.7826(7) 0.0123(3) 0.0518(2) 0.0466(14) Uani 1 1 d . . .
C8 C 0.8613(7) -0.0527(3) 0.0685(2) 0.0525(15) Uani 1 1 d . . .
H8A H 0.9168 -0.0476 0.1056 0.079 Uiso 1 1 calc R . .
H8B H 0.9514 -0.0663 0.0409 0.079 Uiso 1 1 calc R . .
H8C H 0.7689 -0.0882 0.0703 0.079 Uiso 1 1 calc R . .
K5 K 0.62220(13) 0.20215(5) 0.03118(4) 0.0284(2) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ir Ir -1.4442 7.9887 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
K K 0.2009 0.2494 '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
_geom_angle_publ_flag
N1 Ir1 N2 88.86(14) . . ?
N1 Ir1 Cl2 90.02(10) . . ?
N2 Ir1 Cl2 178.60(10) . . ?
N1 Ir1 Cl1 178.11(10) . . ?
N2 Ir1 Cl1 90.53(10) . . ?
Cl2 Ir1 Cl1 90.62(4) . . ?
N1 Ir1 Cl3 89.26(10) . . ?
N2 Ir1 Cl3 90.35(9) . . ?
Cl2 Ir1 Cl3 90.48(4) . . ?
Cl1 Ir1 Cl3 88.95(4) . . ?
N1 Ir1 Cl4 91.42(10) . . ?
N2 Ir1 Cl4 89.41(10) . . ?
Cl2 Ir1 Cl4 89.78(4) . . ?
Cl1 Ir1 Cl4 90.37(4) . . ?
Cl3 Ir1 Cl4 179.28(4) . . ?
N1 Ir1 K5 123.29(10) . 3_455 ?
N2 Ir1 K5 127.13(10) . 3_455 ?
Cl2 Ir1 K5 54.25(3) . 3_455 ?
Cl1 Ir1 K5 55.90(3) . 3_455 ?
Cl3 Ir1 K5 54.13(3) . 3_455 ?
Cl4 Ir1 K5 125.59(3) . 3_455 ?
N1 Ir1 K5 129.84(10) . . ?
N2 Ir1 K5 125.15(9) . . ?
Cl2 Ir1 K5 55.18(3) . . ?
Cl1 Ir1 K5 51.83(3) . . ?
Cl3 Ir1 K5 121.78(3) . . ?
Cl4 Ir1 K5 57.89(3) . . ?
K5 Ir1 K5 67.803(14) 3_455 . ?
Ir1 Cl1 K5 92.31(4) . . ?
Ir1 Cl1 K5 88.19(3) . 3_455 ?
K5 Cl1 K5 87.32(3) . 3_455 ?
Ir1 Cl2 K5 89.83(4) . 3_455 ?
Ir1 Cl2 K5 88.95(3) . . ?
K5 Cl2 K5 86.19(3) 3_455 . ?
Ir1 Cl3 K5 120.35(5) . 1_455 ?
Ir1 Cl3 K5 89.65(3) . 3_455 ?
K5 Cl3 K5 87.40(3) 1_455 3_455 ?
Ir1 Cl4 K5 85.98(3) . . ?
C1 N1 Ir1 175.1(4) . . ?
N1 C1 C2 178.4(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 N2 Ir1 173.2(4) . . ?
N2 C3 C4 179.0(5) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 C6 179.3(8) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 N4 K5 168.0(6) . . ?
N4 C7 C8 176.8(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 K5 Cl1 141.95(12) . . ?
N4 K5 Cl3 104.81(13) . 1_655 ?
Cl1 K5 Cl3 85.68(4) . 1_655 ?
N4 K5 Cl3 104.85(15) . 3 ?
Cl1 K5 Cl3 92.60(4) . 3 ?
Cl3 K5 Cl3 133.14(4) 1_655 3 ?
N4 K5 Cl2 141.24(12) . 3 ?
Cl1 K5 Cl2 76.80(3) . 3 ?
Cl3 K5 Cl2 72.06(3) 1_655 3 ?
Cl3 K5 Cl2 62.07(3) 3 3 ?
N4 K5 Cl2 91.24(11) . . ?
Cl1 K5 Cl2 62.39(3) . . ?
Cl3 K5 Cl2 142.53(4) 1_655 . ?
Cl3 K5 Cl2 71.26(3) 3 . ?
Cl2 K5 Cl2 114.99(4) 3 . ?
N4 K5 Cl1 80.47(12) . 3 ?
Cl1 K5 Cl1 136.85(3) . 3 ?
Cl3 K5 Cl1 90.01(4) 1_655 3 ?
Cl3 K5 Cl1 60.46(3) 3 3 ?
Cl2 K5 Cl1 61.15(3) 3 3 ?
Cl2 K5 Cl1 126.41(4) . 3 ?
N4 K5 Cl4 82.16(12) . . ?
Cl1 K5 Cl4 61.26(3) . . ?
Cl3 K5 Cl4 88.81(3) 1_655 . ?
Cl3 K5 Cl4 130.61(4) 3 . ?
Cl2 K5 Cl4 135.16(4) 3 . ?
Cl2 K5 Cl4 59.63(3) . . ?
Cl1 K5 Cl4 161.67(4) 3 . ?
N4 K5 Ir1 111.60(13) . 3 ?
Cl1 K5 Ir1 102.50(3) . 3 ?
Cl3 K5 Ir1 98.61(3) 1_655 3 ?
Cl3 K5 Ir1 36.22(2) 3 3 ?
Cl2 K5 Ir1 35.92(2) 3 3 ?
Cl2 K5 Ir1 106.67(3) . 3 ?
Cl1 K5 Ir1 35.92(2) 3 3 ?
Cl4 K5 Ir1 161.77(3) . 3 ?
N4 K5 Ir1 107.14(11) . . ?
Cl1 K5 Ir1 35.86(2) . . ?
Cl3 K5 Ir1 106.67(3) 1_655 . ?
Cl3 K5 Ir1 98.17(3) 3 . ?
Cl2 K5 Ir1 110.72(3) 3 . ?
Cl2 K5 Ir1 35.87(2) . . ?
Cl1 K5 Ir1 158.63(3) 3 . ?
Cl4 K5 Ir1 36.13(2) . . ?
Ir1 K5 Ir1 125.72(2) 3 . ?
N4 K5 K5 130.88(13) . 3_455 ?
Cl1 K5 K5 47.85(3) . 3_455 ?
Cl3 K5 K5 123.90(4) 1_655 3_455 ?
Cl3 K5 K5 46.11(3) 3 3_455 ?
Cl2 K5 K5 68.49(3) 3 3_455 ?
Cl2 K5 K5 46.51(2) . 3_455 ?
Cl1 K5 K5 103.64(4) 3 3_455 ?
Cl4 K5 K5 92.13(3) . 3_455 ?
Ir1 K5 K5 69.89(3) 3 3_455 ?
Ir1 K5 K5 56.051(13) . 3_455 ?
N4 K5 K5 101.67(11) . 3 ?
Cl1 K5 K5 111.29(4) . 3 ?
Cl3 K5 K5 46.49(2) 1_655 3 ?
Cl3 K5 K5 92.29(4) 3 3 ?
Cl2 K5 K5 47.30(3) 3 3 ?
Cl2 K5 K5 161.37(4) . 3 ?
Cl1 K5 K5 44.83(3) 3 3 ?
Cl4 K5 K5 134.95(4) . 3 ?
Ir1 K5 K5 56.15(2) 3 3 ?
Ir1 K5 K5 145.51(4) . 3 ?
K5 K5 K5 115.55(4) 3_455 3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N1 1.995(4) . ?
Ir1 N2 2.017(4) . ?
Ir1 Cl2 2.3395(11) . ?
Ir1 Cl1 2.3405(10) . ?
Ir1 Cl3 2.3566(10) . ?
Ir1 Cl4 2.3599(10) . ?
Ir1 K5 3.9879(9) 3_455 ?
Ir1 K5 3.9924(10) . ?
Cl1 K5 3.1413(14) . ?
Cl1 K5 3.3037(13) 3_455 ?
Cl2 K5 3.2364(15) 3_455 ?
Cl2 K5 3.2783(14) . ?
Cl3 K5 3.2112(15) 1_455 ?
Cl3 K5 3.2317(14) 3_455 ?
Cl4 K5 3.3898(14) . ?
N1 C1 1.134(5) . ?
C1 C2 1.441(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N2 C3 1.119(5) . ?
C3 C4 1.447(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N3 C5 1.152(7) . ?
C5 C6 1.431(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N4 C7 1.136(7) . ?
N4 K5 2.785(6) . ?
C7 C8 1.448(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
K5 Cl3 3.2112(15) 1_655 ?
K5 Cl3 3.2316(14) 3 ?
K5 Cl2 3.2363(15) 3 ?
K5 Cl1 3.3036(13) 3 ?
K5 Ir1 3.9879(9) 3 ?
K5 K5 4.4511(10) 3_455 ?
K5 K5 4.4511(10) 3 ?
