#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:45:22 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180052 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/46/7034659.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_7034659
loop_
_publ_author_name
'Das, Ujjwal'
'Ghorui, Tapas'
'Adhikari, Basab'
'Roy, Sima'
'Pramanik, Shuvam'
'Pramanik, Kausikisankar'
_publ_section_title
;
 Iridium-mediated C-S bond activation and transformation:
 organoiridium(iii) thioether, thiolato, sulfinato and thiyl radical
 compounds. Synthesis, mechanistic, spectral, electrochemical and
 theoretical aspects.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8625
_journal_page_last               8639
_journal_paper_doi               10.1039/c5dt00448a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H38 Cl Ir N2 O2 P2 S, (C H2 Cl2)'
_chemical_formula_sum            'C49 H40 Cl3 Ir N2 O2 P2 S'
_chemical_formula_weight         1081.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      36
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-30 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3746(18)
_cell_length_b                   18.420(2)
_cell_length_c                   17.336(2)
_cell_measurement_reflns_used    987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      1.73
_cell_volume                     4909.6(10)
_computing_cell_refinement       'SMART APEX II'
_computing_data_collection       'SMART APEX II (Bruker,2010)'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area-detector'
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25391
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs(Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         7289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0250
_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/[σ²(Fo²)+(0.0330P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                6571
_reflns_number_total             7289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00448a2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 7034657--7034660.cif.
;
_cod_original_cell_volume        4909.75(10)
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               7034659
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, 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'
'-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
Ir1 Ir 0.5000 0.041642(7) 0.248776(8) 0.02460(5) Uani 1 2 d S
Cl1 Cl 0.5000 0.01666(9) 0.38347(9) 0.0357(3) Uani 1 2 d S
S1 S 0.5000 0.16955(5) 0.24858(14) 0.02935(18) Uani 1 2 d S
P1 P 0.34499(5) 0.03754(4) 0.25719(10) 0.0297(2) Uani 1 1 d .
O1 O 0.57934(16) 0.20747(14) 0.27120(15) 0.0463(7) Uani 1 1 d .
N1 N 0.5000 0.0523(2) 0.1337(3) 0.0321(10) Uani 1 2 d S
N2 N 0.5000 -0.0030(3) 0.0896(3) 0.0378(12) Uani 1 2 d S
C1 C 0.5000 -0.0639(3) 0.2121(3) 0.0320(10) Uani 1 2 d S
C2 C 0.5000 -0.1320(2) 0.2460(7) 0.0398(10) Uani 1 2 d S
H2A H 0.5000 -0.1332 0.3008 0.048 Uiso 1 2 calc SR
C3 C 0.5000 -0.1953(3) 0.2103(4) 0.0559(16) Uani 1 2 d S
H3A H 0.5000 -0.2393 0.2390 0.067 Uiso 1 2 calc SR
C4 C 0.5000 -0.1965(3) 0.1310(4) 0.0601(18) Uani 1 2 d S
H4A H 0.5000 -0.2416 0.1044 0.072 Uiso 1 2 calc SR
C5 C 0.5000 -0.1333(3) 0.0908(4) 0.0496(15) Uani 1 2 d S
H5A H 0.5000 -0.1334 0.0360 0.059 Uiso 1 2 calc SR
C6 C 0.5000 -0.0686(3) 0.1316(3) 0.0360(11) Uani 1 2 d S
C7 C 0.5000 0.1211(3) 0.0973(3) 0.0350(11) Uani 1 2 d S
C8 C 0.5000 0.1304(4) 0.0180(4) 0.0563(16) Uani 1 2 d S
H8A H 0.5000 0.0894 -0.0153 0.068 Uiso 1 2 calc SR
C9 C 0.5000 0.2001(4) -0.0122(4) 0.0560(16) Uani 1 2 d S
H9A H 0.5000 0.2060 -0.0666 0.067 Uiso 1 2 calc SR
C10 C 0.5000 0.2575(4) 0.0312(4) 0.0544(18) Uani 1 2 d S
H10A H 0.5000 0.3044 0.0083 0.065 Uiso 1 2 calc SR
C11 C 0.5000 0.2504(3) 0.1128(3) 0.0403(12) Uani 1 2 d S
H11A H 0.5000 0.2920 0.1451 0.048 Uiso 1 2 calc SR
C12 C 0.5000 0.1797(3) 0.1447(3) 0.0343(11) Uani 1 2 d S
C13 C 0.3013(2) -0.05433(19) 0.2690(2) 0.0360(9) Uani 1 1 d .
C14 C 0.3263(3) -0.0912(2) 0.3358(2) 0.0483(10) Uani 1 1 d .
H14A H 0.3660 -0.0692 0.3707 0.058 Uiso 1 1 calc R
C15 C 0.2936(3) -0.1597(2) 0.3516(3) 0.0577(12) Uani 1 1 d .
H15A H 0.3101 -0.1837 0.3978 0.069 Uiso 1 1 calc R
C16 C 0.2383(3) -0.1931(3) 0.3017(3) 0.0610(13) Uani 1 1 d .
H16A H 0.2180 -0.2408 0.3121 0.073 Uiso 1 1 calc R
C17 C 0.2124(3) -0.1581(3) 0.2378(5) 0.0758(17) Uani 1 1 d .
H17A H 0.1721 -0.1807 0.2038 0.091 Uiso 1 1 calc R
C18 C 0.2444(3) -0.0877(3) 0.2204(3) 0.0637(13) Uani 1 1 d .
H18A H 0.2260 -0.0637 0.1747 0.076 Uiso 1 1 calc R
C19 C 0.2924(3) 0.0819(3) 0.3394(3) 0.0366(10) Uani 1 1 d .
C20 C 0.2020(3) 0.0717(3) 0.3471(3) 0.0601(12) Uani 1 1 d .
H20A H 0.1713 0.0449 0.3091 0.072 Uiso 1 1 calc R
C21 C 0.1574(3) 0.1004(3) 0.4096(3) 0.0778(17) Uani 1 1 d .
H21A H 0.0970 0.0913 0.4160 0.093 Uiso 1 1 calc R
C22 C 0.2020(5) 0.1424(4) 0.4626(4) 0.077(2) Uani 1 1 d .
H22A H 0.1712 0.1646 0.5038 0.093 Uiso 1 1 calc R
C23 C 0.2882(3) 0.1523(3) 0.4565(3) 0.0571(11) Uani 1 1 d .
H23A H 0.3184 0.1794 0.4947 0.069 Uiso 1 1 calc R
C24 C 0.3334(2) 0.1230(2) 0.3943(2) 0.0414(8) Uani 1 1 d .
H24A H 0.3942 0.1316 0.3899 0.050 Uiso 1 1 calc R
C25 C 0.2912(3) 0.0749(3) 0.1722(3) 0.0404(11) Uani 1 1 d .
C26 C 0.2975(3) 0.0389(2) 0.1025(3) 0.0527(11) Uani 1 1 d .
H26A H 0.3280 -0.0058 0.0988 0.063 Uiso 1 1 calc R
C27 C 0.2580(4) 0.0694(4) 0.0377(3) 0.0761(16) Uani 1 1 d .
H27A H 0.2608 0.0446 -0.0102 0.091 Uiso 1 1 calc R
C28 C 0.2173(5) 0.1316(4) 0.0417(4) 0.085(2) Uani 1 1 d .
H28A H 0.1909 0.1505 -0.0036 0.103 Uiso 1 1 calc R
C29 C 0.2113(4) 0.1704(3) 0.1085(4) 0.0825(17) Uani 1 1 d .
H29A H 0.1816 0.2155 0.1101 0.099 Uiso 1 1 calc R
C30 C 0.2511(3) 0.1410(2) 0.1760(3) 0.0585(12) Uani 1 1 d .
H30A H 0.2497 0.1673 0.2231 0.070 Uiso 1 1 calc R
C31 C 0.5000 0.3404(4) 0.3655(5) 0.082(2) Uani 1 2 d S
H31A H 0.4479 0.3277 0.3349 0.098 Uiso 0.50 1 calc PR
H31B H 0.5521 0.3277 0.3349 0.098 Uiso 0.50 1 calc PR
Cl2 Cl 0.5000 0.43702(19) 0.3855(2) 0.1734(19) Uani 1 2 d S
Cl3 Cl 0.5000 0.29144(19) 0.45064(17) 0.1190(11) Uani 1 2 d S
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'
P P 0.1023 0.0942 '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'
Ir Ir -1.4442 7.9887 '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
N1 Ir1 C1 77.5(2) . .
N1 Ir1 S1 84.30(14) . .
C1 Ir1 S1 161.79(16) . .
N1 Ir1 Cl1 174.47(15) . .
C1 Ir1 Cl1 96.98(16) . .
S1 Ir1 Cl1 101.23(7) . .
N1 Ir1 P1 93.66(4) . 3_655
C1 Ir1 P1 89.37(2) . 3_655
S1 Ir1 P1 91.818(18) . 3_655
Cl1 Ir1 P1 86.21(4) . 3_655
N1 Ir1 P1 93.66(4) . .
C1 Ir1 P1 89.37(2) . .
S1 Ir1 P1 91.818(18) . .
Cl1 Ir1 P1 86.21(4) . .
P1 Ir1 P1 172.11(8) 3_655 .
O1 S1 O1 113.4(2) 3_655 .
O1 S1 C12 102.58(16) 3_655 .
O1 S1 C12 102.58(16) . .
O1 S1 Ir1 118.57(11) 3_655 .
O1 S1 Ir1 118.57(11) . .
C12 S1 Ir1 96.01(18) . .
C25 P1 C19 105.07(16) . .
C25 P1 C13 105.8(2) . .
C19 P1 C13 99.4(2) . .
C25 P1 Ir1 113.02(16) . .
C19 P1 Ir1 118.30(17) . .
C13 P1 Ir1 113.70(11) . .
N2 N1 C7 116.7(5) . .
N2 N1 Ir1 121.3(4) . .
C7 N1 Ir1 122.1(4) . .
N1 N2 C6 112.1(5) . .
C2 C1 C6 111.6(6) . .
C2 C1 Ir1 136.7(6) . .
C6 C1 Ir1 111.6(4) . .
C3 C2 C1 127.0(10) . .
C3 C2 H2A 116.5 . .
C1 C2 H2A 116.5 . .
C2 C3 C4 118.8(7) . .
C2 C3 H3A 120.6 . .
C4 C3 H3A 120.6 . .
C5 C4 C3 120.0(6) . .
C5 C4 H4A 120.0 . .
C3 C4 H4A 120.0 . .
C4 C5 C6 118.5(6) . .
C4 C5 H5A 120.8 . .
C6 C5 H5A 120.8 . .
C5 C6 C1 124.1(5) . .
C5 C6 N2 118.3(5) . .
C1 C6 N2 117.5(5) . .
C12 C7 C8 120.2(5) . .
C12 C7 N1 116.3(5) . .
C8 C7 N1 123.5(5) . .
C7 C8 C9 119.3(6) . .
C7 C8 H8A 120.4 . .
C9 C8 H8A 120.4 . .
C10 C9 C8 122.4(6) . .
C10 C9 H9A 118.8 . .
C8 C9 H9A 118.8 . .
C9 C10 C11 120.1(6) . .
C9 C10 H10A 119.9 . .
C11 C10 H10A 119.9 . .
C12 C11 C10 118.3(5) . .
C12 C11 H11A 120.8 . .
C10 C11 H11A 120.8 . .
C7 C12 C11 119.7(5) . .
C7 C12 S1 121.3(4) . .
C11 C12 S1 118.9(4) . .
C18 C13 C14 118.1(4) . .
C18 C13 P1 125.7(3) . .
C14 C13 P1 116.1(3) . .
C15 C14 C13 120.4(4) . .
C15 C14 H14A 119.8 . .
C13 C14 H14A 119.8 . .
C16 C15 C14 120.9(5) . .
C16 C15 H15A 119.5 . .
C14 C15 H15A 119.5 . .
C17 C16 C15 119.6(4) . .
C17 C16 H16A 120.2 . .
C15 C16 H16A 120.2 . .
C16 C17 C18 120.7(5) . .
C16 C17 H17A 119.6 . .
C18 C17 H17A 119.6 . .
C13 C18 C17 120.3(5) . .
C13 C18 H18A 119.9 . .
C17 C18 H18A 119.9 . .
C24 C19 C20 117.5(4) . .
C24 C19 P1 125.7(4) . .
C20 C19 P1 116.8(4) . .
C21 C20 C19 120.8(5) . .
C21 C20 H20A 119.6 . .
C19 C20 H20A 119.6 . .
C22 C21 C20 119.1(5) . .
C22 C21 H21A 120.5 . .
C20 C21 H21A 120.5 . .
C23 C22 C21 120.9(5) . .
C23 C22 H22A 119.5 . .
C21 C22 H22A 119.5 . .
C22 C23 C24 120.1(5) . .
C22 C23 H23A 120.0 . .
C24 C23 H23A 120.0 . .
C19 C24 C23 121.5(4) . .
C19 C24 H24A 119.2 . .
C23 C24 H24A 119.2 . .
C30 C25 C26 120.0(5) . .
C30 C25 P1 120.2(4) . .
C26 C25 P1 119.6(4) . .
C25 C26 C27 118.7(5) . .
C25 C26 H26A 120.6 . .
C27 C26 H26A 120.6 . .
C28 C27 C26 121.3(6) . .
C28 C27 H27A 119.4 . .
C26 C27 H27A 119.4 . .
C27 C28 C29 122.4(6) . .
C27 C28 H28A 118.8 . .
C29 C28 H28A 118.8 . .
C28 C29 C30 118.0(5) . .
C28 C29 H29A 121.0 . .
C30 C29 H29A 121.0 . .
C25 C30 C29 119.5(5) . .
C25 C30 H30A 120.3 . .
C29 C30 H30A 120.3 . .
Cl3 C31 Cl2 110.4(5) . .
Cl3 C31 H31A 109.6 . .
Cl2 C31 H31A 109.6 . .
Cl3 C31 H31B 109.6 . .
Cl2 C31 H31B 109.6 . .
H31A C31 H31B 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 N1 2.004(5) .
Ir1 C1 2.045(5) .
Ir1 S1 2.3562(9) .
Ir1 Cl1 2.3799(16) .
Ir1 P1 2.3888(8) 3_655
Ir1 P1 2.3889(8) .
S1 O1 1.459(2) 3_655
S1 O1 1.459(2) .
S1 C12 1.811(5) .
P1 C25 1.824(5) .
P1 C19 1.831(5) .
P1 C13 1.832(3) .
N1 N2 1.274(6) .
N1 C7 1.417(7) .
N2 C6 1.409(8) .
C1 C2 1.385(8) .
C1 C6 1.398(7) .
C2 C3 1.321(9) .
C2 H2A 0.9500 .
C3 C4 1.376(10) .
C3 H3A 0.9500 .
C4 C5 1.357(9) .
C4 H4A 0.9500 .
C5 C6 1.386(7) .
C5 H5A 0.9500 .
C7 C12 1.356(7) .
C7 C8 1.385(8) .
C8 C9 1.386(9) .
C8 H8A 0.9500 .
C9 C10 1.298(10) .
C9 H9A 0.9500 .
C10 C11 1.421(9) .
C10 H10A 0.9500 .
C11 C12 1.414(7) .
C11 H11A 0.9500 .
C13 C18 1.360(5) .
C13 C14 1.397(5) .
C14 C15 1.386(6) .
C14 H14A 0.9500 .
C15 C16 1.359(7) .
C15 H15A 0.9500 .
C16 C17 1.342(8) .
C16 H16A 0.9500 .
C17 C18 1.420(6) .
C17 H17A 0.9500 .
C18 H18A 0.9500 .
C19 C24 1.370(6) .
C19 C20 1.409(6) .
C20 C21 1.387(7) .
C20 H20A 0.9500 .
C21 C22 1.384(9) .
C21 H21A 0.9500 .
C22 C23 1.342(8) .
C22 H22A 0.9500 .
C23 C24 1.392(5) .
C23 H23A 0.9500 .
C24 H24A 0.9500 .
C25 C30 1.368(7) .
C25 C26 1.382(7) .
C26 C27 1.395(7) .
C26 H26A 0.9500 .
C27 C28 1.307(9) .
C27 H27A 0.9500 .
C28 C29 1.364(9) .
C28 H28A 0.9500 .
C29 C30 1.425(7) .
C29 H29A 0.9500 .
C30 H30A 0.9500 .
C31 Cl3 1.729(9) .
C31 Cl2 1.813(9) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 1.022 0.152 148 50 ' '
2 0.000 -0.022 0.652 148 50 ' '
3 0.500 0.522 0.152 148 50 ' '
4 0.500 0.478 0.652 148 50 ' '
