#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/46/7034658.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_7034658
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 P2 S, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H42 Cl5 Ir N2 P2 S'
_chemical_formula_weight         1134.31
_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                   14.995(10)
_cell_length_b                   18.277(12)
_cell_length_c                   17.451(11)
_cell_measurement_reflns_used    34021
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.76
_cell_volume                     4783(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34021
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  0.433
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs(Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         2.419
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.125(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         7084
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0262
_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)+(0.0328P)²+1.8808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                6860
_reflns_number_total             7084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00448a2.cif
_cod_data_source_block           3
_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_sg_symbol_Hall     C2c-2
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               7034658
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 0.0000 0.034630(6) 0.409151(8) 0.01417(4) Uani 1 2 d S
Cl1 Cl 0.0000 0.00607(7) 0.27451(7) 0.0232(3) Uani 1 2 d S
S1 S 0.0000 0.16992(5) 0.40360(12) 0.0194(2) Uani 1 2 d S
P1 P 0.15902(5) 0.03323(3) 0.40198(10) 0.0185(2) Uani 1 1 d .
N1 N 0.0000 0.05070(19) 0.5215(2) 0.0166(7) Uani 1 2 d S
N2 N 0.0000 -0.0043(3) 0.5695(3) 0.0245(10) Uani 1 2 d S
C1 C 0.0000 -0.0702(2) 0.4486(3) 0.0210(8) Uani 1 2 d S
C2 C 0.0000 -0.1404(2) 0.4134(5) 0.0271(9) Uani 1 2 d S
H2 H 0.0000 -0.1434 0.3602 0.033 Uiso 1 2 calc SR
C3 C 0.0000 -0.2045(3) 0.4559(3) 0.0356(12) Uani 1 2 d S
H3 H 0.0000 -0.2493 0.4307 0.043 Uiso 1 2 calc SR
C4 C 0.0000 -0.2029(3) 0.5358(3) 0.0347(12) Uani 1 2 d S
H4 H 0.0000 -0.2465 0.5633 0.042 Uiso 1 2 calc SR
C5 C 0.0000 -0.1367(3) 0.5745(3) 0.0289(10) Uani 1 2 d S
H5 H 0.0000 -0.1350 0.6277 0.035 Uiso 1 2 calc SR
C6 C 0.0000 -0.0712(2) 0.5301(3) 0.0207(8) Uani 1 2 d S
C7 C 0.0000 0.1227(2) 0.5550(3) 0.0191(8) Uani 1 2 d S
C8 C 0.0000 0.1330(3) 0.6348(3) 0.0280(10) Uani 1 2 d S
H8 H 0.0000 0.0927 0.6674 0.034 Uiso 1 2 calc SR
C9 C 0.0000 0.2027(3) 0.6648(3) 0.0353(12) Uani 1 2 d S
H9 H 0.0000 0.2099 0.7176 0.042 Uiso 1 2 calc SR
C10 C 0.0000 0.2639(3) 0.6137(3) 0.0281(12) Uani 1 2 d S
H10 H 0.0000 0.3112 0.6333 0.034 Uiso 1 2 calc SR
C11 C 0.0000 0.2531(2) 0.5355(3) 0.0216(8) Uani 1 2 d S
H11 H 0.0000 0.2934 0.5030 0.026 Uiso 1 2 calc SR
C12 C 0.0000 0.1822(2) 0.5040(2) 0.0175(8) Uani 1 2 d S
C13 C 0.2114(3) 0.0806(3) 0.3201(3) 0.0241(9) Uani 1 1 d .
C14 C 0.3034(3) 0.0713(3) 0.3073(3) 0.0411(9) Uani 1 1 d .
H14 H 0.3367 0.0428 0.3409 0.049 Uiso 1 1 calc R
C15 C 0.3455(3) 0.1044(3) 0.2447(3) 0.0529(12) Uani 1 1 d .
H15 H 0.4063 0.0980 0.2370 0.063 Uiso 1 1 calc R
C16 C 0.2953(4) 0.1473(3) 0.1934(3) 0.0431(13) Uani 1 1 d .
H16 H 0.3228 0.1689 0.1514 0.052 Uiso 1 1 calc R
C17 C 0.2058(3) 0.1571(2) 0.2056(2) 0.0338(8) Uani 1 1 d .
H17 H 0.1731 0.1858 0.1717 0.041 Uiso 1 1 calc R
C18 C 0.1626(2) 0.12434(18) 0.26822(19) 0.0265(7) Uani 1 1 d .
H18 H 0.1018 0.1315 0.2755 0.032 Uiso 1 1 calc R
C19 C 0.2094(2) -0.05862(17) 0.39116(17) 0.0239(7) Uani 1 1 d .
C20 C 0.2715(3) -0.0884(2) 0.4417(3) 0.0453(10) Uani 1 1 d .
H20 H 0.2899 -0.0618 0.4844 0.054 Uiso 1 1 calc R
C21 C 0.3063(4) -0.1584(3) 0.4283(3) 0.0625(17) Uani 1 1 d .
H21 H 0.3463 -0.1785 0.4632 0.075 Uiso 1 1 calc R
C22 C 0.2823(4) -0.1979(3) 0.3647(3) 0.0534(13) Uani 1 1 d .
H22 H 0.3074 -0.2436 0.3557 0.064 Uiso 1 1 calc R
C23 C 0.2206(3) -0.1692(2) 0.3143(3) 0.0435(10) Uani 1 1 d .
H23 H 0.2033 -0.1962 0.2716 0.052 Uiso 1 1 calc R
C24 C 0.1838(3) -0.0997(2) 0.3268(2) 0.0335(8) Uani 1 1 d .
H24 H 0.1424 -0.0808 0.2925 0.040 Uiso 1 1 calc R
C25 C 0.2120(3) 0.0736(3) 0.4867(3) 0.0230(8) Uani 1 1 d .
C26 C 0.2529(3) 0.1424(2) 0.4830(2) 0.0353(8) Uani 1 1 d .
H26 H 0.2567 0.1669 0.4364 0.042 Uiso 1 1 calc R
C27 C 0.2882(3) 0.1747(3) 0.5496(3) 0.0512(11) Uani 1 1 d .
H27 H 0.3138 0.2210 0.5474 0.061 Uiso 1 1 calc R
C28 C 0.2847(5) 0.1369(4) 0.6190(3) 0.0514(16) Uani 1 1 d .
H28 H 0.3103 0.1571 0.6627 0.062 Uiso 1 1 calc R
C29 C 0.2429(3) 0.0692(3) 0.6229(2) 0.0480(11) Uani 1 1 d .
H29 H 0.2392 0.0449 0.6697 0.058 Uiso 1 1 calc R
C30 C 0.2068(3) 0.0374(2) 0.5577(2) 0.0328(8) Uani 1 1 d .
H30 H 0.1791 -0.0080 0.5610 0.039 Uiso 1 1 calc R
C31 C 0.5000 0.0491(5) 0.5447(6) 0.066(2) Uani 1 2 d S
H31A H 0.5522 0.0701 0.5691 0.080 Uiso 0.50 1 calc PR
H31B H 0.4478 0.0701 0.5691 0.080 Uiso 0.50 1 calc PR
C32 C 0.5000 0.8555(5) 0.2933(5) 0.069(2) Uani 1 2 d S
H32A H 0.4478 0.8485 0.3253 0.083 Uiso 0.50 1 calc PR
H32B H 0.5522 0.8485 0.3253 0.083 Uiso 0.50 1 calc PR
Cl2 Cl 0.5000 -0.04406(16) 0.5608(2) 0.0967(11) Uani 1 2 d S
Cl3 Cl 0.5000 0.07406(16) 0.44864(15) 0.0819(7) Uani 1 2 d S
Cl4 Cl 0.5000 0.78924(11) 0.22169(12) 0.0593(5) Uani 1 2 d S
Cl5 Cl 0.5000 0.9400(2) 0.2609(3) 0.191(3) 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'
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 78.75(17) . .
N1 Ir1 P1 93.06(4) . .
C1 Ir1 P1 90.44(2) . .
N1 Ir1 P1 93.06(4) . 3
C1 Ir1 P1 90.44(2) . 3
P1 Ir1 P1 173.87(8) . 3
N1 Ir1 Cl1 175.99(11) . .
C1 Ir1 Cl1 97.24(14) . .
P1 Ir1 Cl1 86.93(4) . .
P1 Ir1 Cl1 86.93(4) 3 .
N1 Ir1 S1 83.73(11) . .
C1 Ir1 S1 162.48(14) . .
P1 Ir1 S1 90.494(15) . .
P1 Ir1 S1 90.494(15) 3 .
Cl1 Ir1 S1 100.28(6) . .
C12 S1 Ir1 95.06(15) . .
C25 P1 C13 104.52(14) . .
C25 P1 C19 105.71(19) . .
C13 P1 C19 99.96(19) . .
C25 P1 Ir1 112.71(15) . .
C13 P1 Ir1 117.39(16) . .
C19 P1 Ir1 115.02(11) . .
N2 N1 C7 116.2(4) . .
N2 N1 Ir1 121.3(3) . .
C7 N1 Ir1 122.5(3) . .
N1 N2 C6 110.9(4) . .
C2 C1 C6 114.9(5) . .
C2 C1 Ir1 134.6(5) . .
C6 C1 Ir1 110.5(3) . .
C3 C2 C1 122.1(8) . .
C3 C2 H2 119.0 . .
C1 C2 H2 119.0 . .
C2 C3 C4 121.1(5) . .
C2 C3 H3 119.4 . .
C4 C3 H3 119.4 . .
C5 C4 C3 120.3(5) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C4 C5 C6 118.0(5) . .
C4 C5 H5 121.0 . .
C6 C5 H5 121.0 . .
N2 C6 C1 118.6(4) . .
N2 C6 C5 117.8(4) . .
C1 C6 C5 123.6(4) . .
C8 C7 C12 121.7(4) . .
C8 C7 N1 121.6(4) . .
C12 C7 N1 116.7(4) . .
C9 C8 C7 120.0(4) . .
C9 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C8 C9 C10 119.1(5) . .
C8 C9 H9 120.5 . .
C10 C9 H9 120.5 . .
C11 C10 C9 120.4(5) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C10 C11 C12 121.2(4) . .
C10 C11 H11 119.4 . .
C12 C11 H11 119.4 . .
C7 C12 C11 117.7(4) . .
C7 C12 S1 122.0(3) . .
C11 C12 S1 120.3(3) . .
C14 C13 C18 118.3(4) . .
C14 C13 P1 118.9(4) . .
C18 C13 P1 122.8(3) . .
C15 C14 C13 120.9(4) . .
C15 C14 H14 119.6 . .
C13 C14 H14 119.6 . .
C14 C15 C16 119.8(4) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
C17 C16 C15 119.9(4) . .
C17 C16 H16 120.1 . .
C15 C16 H16 120.1 . .
C16 C17 C18 121.1(4) . .
C16 C17 H17 119.5 . .
C18 C17 H17 119.5 . .
C17 C18 C13 120.1(4) . .
C17 C18 H18 120.0 . .
C13 C18 H18 120.0 . .
C20 C19 C24 118.7(3) . .
C20 C19 P1 124.2(3) . .
C24 C19 P1 117.1(3) . .
C19 C20 C21 119.9(4) . .
C19 C20 H20 120.0 . .
C21 C20 H20 120.0 . .
C22 C21 C20 121.2(4) . .
C22 C21 H21 119.4 . .
C20 C21 H21 119.4 . .
C21 C22 C23 119.5(4) . .
C21 C22 H22 120.2 . .
C23 C22 H22 120.2 . .
C22 C23 C24 120.5(4) . .
C22 C23 H23 119.8 . .
C24 C23 H23 119.8 . .
C23 C24 C19 120.2(4) . .
C23 C24 H24 119.9 . .
C19 C24 H24 119.9 . .
C26 C25 C30 119.1(4) . .
C26 C25 P1 121.0(3) . .
C30 C25 P1 119.8(3) . .
C25 C26 C27 120.3(4) . .
C25 C26 H26 119.9 . .
C27 C26 H26 119.9 . .
C28 C27 C26 119.7(5) . .
C28 C27 H27 120.1 . .
C26 C27 H27 120.1 . .
C29 C28 C27 120.0(5) . .
C29 C28 H28 120.0 . .
C27 C28 H28 120.0 . .
C30 C29 C28 120.6(4) . .
C30 C29 H29 119.7 . .
C28 C29 H29 119.7 . .
C29 C30 C25 120.3(4) . .
C29 C30 H30 119.9 . .
C25 C30 H30 119.9 . .
Cl2 C31 Cl3 114.6(6) . .
Cl2 C31 H31A 108.6 . .
Cl3 C31 H31A 108.6 . .
Cl2 C31 H31B 108.6 . .
Cl3 C31 H31B 108.6 . .
H31A C31 H31B 107.6 . .
Cl5 C32 Cl4 114.0(5) . .
Cl5 C32 H32A 108.8 . .
Cl4 C32 H32A 108.8 . .
Cl5 C32 H32B 108.8 . .
Cl4 C32 H32B 108.8 . .
H32A C32 H32B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 N1 1.982(4) .
Ir1 C1 2.036(4) .
Ir1 P1 2.3880(17) .
Ir1 P1 2.3880(17) 3
Ir1 Cl1 2.4069(19) .
Ir1 S1 2.4746(18) .
S1 C12 1.766(5) .
P1 C25 1.833(5) .
P1 C13 1.846(5) .
P1 C19 1.851(3) .
N1 N2 1.308(5) .
N1 C7 1.440(5) .
N2 C6 1.403(7) .
C1 C2 1.423(7) .
C1 C6 1.423(6) .
C2 C3 1.386(8) .
C2 H2 0.9300 .
C3 C4 1.396(8) .
C3 H3 0.9300 .
C4 C5 1.385(8) .
C4 H4 0.9300 .
C5 C6 1.425(6) .
C5 H5 0.9300 .
C7 C8 1.406(6) .
C7 C12 1.406(6) .
C8 C9 1.378(7) .
C8 H8 0.9300 .
C9 C10 1.431(9) .
C9 H9 0.9300 .
C10 C11 1.378(8) .
C10 H10 0.9300 .
C11 C12 1.408(6) .
C11 H11 0.9300 .
C13 C14 1.409(6) .
C13 C18 1.412(6) .
C14 C15 1.398(6) .
C14 H14 0.9300 .
C15 C16 1.407(8) .
C15 H15 0.9300 .
C16 C17 1.370(8) .
C16 H16 0.9300 .
C17 C18 1.405(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C20 1.393(5) .
C19 C24 1.404(5) .
C20 C21 1.403(6) .
C20 H20 0.9300 .
C21 C22 1.371(7) .
C21 H21 0.9300 .
C22 C23 1.381(7) .
C22 H22 0.9300 .
C23 C24 1.401(5) .
C23 H23 0.9300 .
C24 H24 0.9300 .
C25 C26 1.400(6) .
C25 C30 1.408(6) .
C26 C27 1.407(5) .
C26 H26 0.9300 .
C27 C28 1.396(8) .
C27 H27 0.9300 .
C28 C29 1.389(8) .
C28 H28 0.9300 .
C29 C30 1.388(6) .
C29 H29 0.9300 .
C30 H30 0.9300 .
C31 Cl2 1.726(9) .
C31 Cl3 1.737(10) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 Cl5 1.645(10) .
C32 Cl4 1.740(8) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
