#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:56:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178674 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/85/4078569.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_4078569
loop_
_publ_author_name
'Lin, Cheng-Huei'
'Chiu, Yuan-Chieh'
'Chi, Yun'
'Tao, Yu-Tai'
'Liao, Liang-Sheng'
'Tseng, Meu-Rurng'
'Lee, Gene-Hsiang'
_publ_section_title
;
 Mechanistic Investigation of Improved Syntheses of Iridium(III)-Based
 OLED Phosphors
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4349
_journal_paper_doi               10.1021/om300325y
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C84 H82 Cl4 Ir2 P4 S2'
_chemical_formula_weight         1805.70
_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                 103.151(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.3581(17)
_cell_length_b                   8.8949(3)
_cell_length_c                   19.2344(7)
_cell_measurement_reflns_used    6069
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.34
_cell_volume                     7223.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       '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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27074
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    4.022
_exptl_absorpt_correction_T_max  0.4329
_exptl_absorpt_correction_T_min  0.3989
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0266P)²+10.3881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                7696
_reflns_number_total             8308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300325y_si_001.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4078569
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
Ir Ir 0.603572(2) 0.527266(13) 0.579310(6) 0.01427(4) Uani 1 1 d .
Cl1 Cl 0.626074(17) 0.40963(9) 0.48667(4) 0.02188(15) Uani 1 1 d .
Cl2 Cl 0.601041(17) 0.27470(8) 0.62663(4) 0.02184(15) Uani 1 1 d .
S1 S 0.550195(18) 0.49515(9) 0.50547(4) 0.02024(16) Uani 1 1 d .
P1 P 0.604700(17) 0.75607(9) 0.53102(4) 0.01522(15) Uani 1 1 d .
P2 P 0.649080(17) 0.56593(9) 0.66722(4) 0.01623(15) Uani 1 1 d .
C1 C 0.57809(7) 0.6358(4) 0.64282(15) 0.0193(6) Uani 1 1 d .
C2 C 0.56258(8) 0.5592(4) 0.68862(17) 0.0248(7) Uani 1 1 d .
H2 H 0.5651 0.4534 0.6937 0.030 Uiso 1 1 calc R
C3 C 0.54370(9) 0.6339(5) 0.7267(2) 0.0362(9) Uani 1 1 d .
H3 H 0.5332 0.5788 0.7569 0.043 Uiso 1 1 calc R
C4 C 0.53998(9) 0.7880(5) 0.7210(2) 0.0388(9) Uani 1 1 d .
H4 H 0.5276 0.8396 0.7483 0.047 Uiso 1 1 calc R
C5 C 0.55448(8) 0.8658(4) 0.67534(18) 0.0288(7) Uani 1 1 d .
H5 H 0.5516 0.9715 0.6703 0.035 Uiso 1 1 calc R
C6 C 0.57325(7) 0.7916(4) 0.63650(15) 0.0201(6) Uani 1 1 d .
C7 C 0.59001(7) 0.8844(3) 0.58998(16) 0.0204(6) Uani 1 1 d .
H7A H 0.6078 0.9406 0.6201 0.024 Uiso 1 1 calc R
H7B H 0.5751 0.9575 0.5615 0.024 Uiso 1 1 calc R
C8 C 0.64057(7) 0.8405(3) 0.51477(15) 0.0173(6) Uani 1 1 d .
C9 C 0.66529(7) 0.7530(4) 0.50120(16) 0.0219(6) Uani 1 1 d .
H9 H 0.6653 0.6471 0.5077 0.026 Uiso 1 1 calc R
C10 C 0.68984(7) 0.8227(4) 0.47815(18) 0.0262(7) Uani 1 1 d .
H10 H 0.7069 0.7643 0.4696 0.031 Uiso 1 1 calc R
C11 C 0.68959(8) 0.9755(4) 0.46762(18) 0.0262(7) Uani 1 1 d .
H11 H 0.7062 1.0215 0.4503 0.031 Uiso 1 1 calc R
C12 C 0.66531(8) 1.0628(4) 0.48204(17) 0.0244(7) Uani 1 1 d .
H12 H 0.6654 1.1686 0.4754 0.029 Uiso 1 1 calc R
C13 C 0.64103(8) 0.9954(3) 0.50609(17) 0.0215(7) Uani 1 1 d .
H13 H 0.6246 1.0553 0.5168 0.026 Uiso 1 1 calc R
C14 C 0.57916(7) 0.7796(3) 0.44194(15) 0.0182(6) Uani 1 1 d .
C15 C 0.59151(8) 0.7522(4) 0.38199(17) 0.0251(7) Uani 1 1 d .
H15 H 0.6128 0.7199 0.3878 0.030 Uiso 1 1 calc R
C16 C 0.57263(9) 0.7722(4) 0.31412(18) 0.0327(8) Uani 1 1 d .
H16 H 0.5812 0.7557 0.2734 0.039 Uiso 1 1 calc R
C17 C 0.54152(9) 0.8159(5) 0.30554(19) 0.0381(9) Uani 1 1 d .
H17 H 0.5286 0.8288 0.2589 0.046 Uiso 1 1 calc R
C18 C 0.52887(8) 0.8412(5) 0.3643(2) 0.0378(9) Uani 1 1 d .
H18 H 0.5073 0.8704 0.3580 0.045 Uiso 1 1 calc R
C19 C 0.54770(7) 0.8238(4) 0.43268(18) 0.0260(7) Uani 1 1 d .
H19 H 0.5391 0.8421 0.4731 0.031 Uiso 1 1 calc R
C20 C 0.70723(7) 0.4013(4) 0.80901(16) 0.0233(7) Uani 1 1 d .
H20 H 0.7097 0.3423 0.7695 0.028 Uiso 1 1 calc R
C21 C 0.73275(8) 0.4222(4) 0.86632(18) 0.0290(7) Uani 1 1 d .
H21 H 0.7527 0.3795 0.8654 0.035 Uiso 1 1 calc R
C22 C 0.72926(8) 0.5048(4) 0.92467(18) 0.0274(8) Uani 1 1 d .
H22 H 0.7469 0.5199 0.9637 0.033 Uiso 1 1 calc R
C23 C 0.70023(8) 0.5653(4) 0.92631(17) 0.0279(7) Uani 1 1 d .
H23 H 0.6976 0.6201 0.9670 0.033 Uiso 1 1 calc R
C24 C 0.67479(8) 0.5464(4) 0.86868(17) 0.0230(7) Uani 1 1 d .
H24 H 0.6549 0.5891 0.8702 0.028 Uiso 1 1 calc R
C25 C 0.67789(7) 0.4660(3) 0.80866(16) 0.0188(6) Uani 1 1 d .
C26 C 0.64994(7) 0.4460(3) 0.74652(16) 0.0194(6) Uani 1 1 d .
H26A H 0.6304 0.4655 0.7635 0.023 Uiso 1 1 calc R
H26B H 0.6493 0.3395 0.7312 0.023 Uiso 1 1 calc R
C27 C 0.68702(7) 0.5086(4) 0.64931(17) 0.0196(6) Uani 1 1 d .
C28 C 0.68761(7) 0.3660(4) 0.61978(16) 0.0222(7) Uani 1 1 d .
H28 H 0.6683 0.3132 0.6025 0.027 Uiso 1 1 calc R
C29 C 0.71622(8) 0.3004(4) 0.61552(17) 0.0277(7) Uani 1 1 d .
H29 H 0.7164 0.2024 0.5959 0.033 Uiso 1 1 calc R
C30 C 0.74426(8) 0.3763(4) 0.63946(19) 0.0337(8) Uani 1 1 d .
H30 H 0.7637 0.3306 0.6365 0.040 Uiso 1 1 calc R
C31 C 0.74411(8) 0.5184(4) 0.6676(2) 0.0347(9) Uani 1 1 d .
H31 H 0.7634 0.5721 0.6829 0.042 Uiso 1 1 calc R
C32 C 0.71562(7) 0.5836(4) 0.67374(19) 0.0276(7) Uani 1 1 d .
H32 H 0.7157 0.6803 0.6948 0.033 Uiso 1 1 calc R
C33 C 0.65358(7) 0.7540(3) 0.70557(16) 0.0195(6) Uani 1 1 d .
C34 C 0.63660(8) 0.7875(4) 0.75732(16) 0.0247(7) Uani 1 1 d .
H34 H 0.6233 0.7131 0.7706 0.030 Uiso 1 1 calc R
C35 C 0.63890(9) 0.9271(4) 0.78938(18) 0.0331(8) Uani 1 1 d .
H35 H 0.6272 0.9482 0.8245 0.040 Uiso 1 1 calc R
C36 C 0.65799(10) 1.0354(4) 0.7707(2) 0.0376(9) Uani 1 1 d .
H36 H 0.6602 1.1300 0.7943 0.045 Uiso 1 1 calc R
C37 C 0.67409(10) 1.0072(4) 0.7177(2) 0.0336(9) Uani 1 1 d .
H37 H 0.6867 1.0839 0.7037 0.040 Uiso 1 1 calc R
C38 C 0.67194(8) 0.8677(4) 0.68498(17) 0.0246(7) Uani 1 1 d .
H38 H 0.6830 0.8491 0.6484 0.029 Uiso 1 1 calc R
C39 C 0.54940(8) 0.4075(4) 0.41965(17) 0.0296(8) Uani 1 1 d .
H39A H 0.5316 0.4468 0.3825 0.036 Uiso 1 1 calc R
H39B H 0.5694 0.4265 0.4047 0.036 Uiso 1 1 calc R
C40 C 0.54521(10) 0.2408(5) 0.4316(2) 0.0437(10) Uani 1 1 d .
H40A H 0.5654 0.1956 0.4578 0.052 Uiso 1 1 calc R
H40B H 0.5381 0.1879 0.3854 0.052 Uiso 1 1 calc R
C41 C 0.52013(9) 0.2300(5) 0.4754(2) 0.0429(10) Uani 1 1 d .
H41A H 0.4991 0.2568 0.4457 0.051 Uiso 1 1 calc R
H41B H 0.5191 0.1263 0.4934 0.051 Uiso 1 1 calc R
C42 C 0.52951(7) 0.3387(4) 0.53710(18) 0.0278(7) Uani 1 1 d .
H42A H 0.5436 0.2887 0.5784 0.033 Uiso 1 1 calc R
H42B H 0.5105 0.3757 0.5521 0.033 Uiso 1 1 calc R
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'
P P 0.1023 0.0942 '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'
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
C1 Ir P1 83.44(9)
C1 Ir P2 88.87(8)
P1 Ir P2 94.16(3)
C1 Ir Cl2 97.73(9)
P1 Ir Cl2 177.45(3)
P2 Ir Cl2 88.13(3)
C1 Ir S1 80.49(8)
P1 Ir S1 88.42(3)
P2 Ir S1 168.70(3)
Cl2 Ir S1 89.55(3)
C1 Ir Cl1 170.01(8)
P1 Ir Cl1 92.09(3)
P2 Ir Cl1 100.39(3)
Cl2 Ir Cl1 86.40(3)
S1 Ir Cl1 90.49(3)
C39 S1 C42 93.79(16)
C39 S1 Ir 113.45(12)
C42 S1 Ir 111.50(11)
C8 P1 C7 106.39(14)
C8 P1 C14 98.69(13)
C7 P1 C14 106.78(14)
C8 P1 Ir 123.13(10)
C7 P1 Ir 105.47(10)
C14 P1 Ir 115.24(10)
C33 P2 C27 108.32(14)
C33 P2 C26 102.43(14)
C27 P2 C26 98.29(14)
C33 P2 Ir 115.31(9)
C27 P2 Ir 118.37(10)
C26 P2 Ir 111.70(10)
C2 C1 C6 116.8(3)
C2 C1 Ir 122.9(2)
C6 C1 Ir 120.0(2)
C3 C2 C1 121.7(3)
C4 C3 C2 120.4(3)
C5 C4 C3 119.1(3)
C4 C5 C6 120.8(3)
C5 C6 C1 121.1(3)
C5 C6 C7 118.4(3)
C1 C6 C7 120.4(3)
C6 C7 P1 108.0(2)
C13 C8 C9 119.9(3)
C13 C8 P1 117.9(2)
C9 C8 P1 121.7(2)
C10 C9 C8 119.2(3)
C11 C10 C9 120.5(3)
C10 C11 C12 120.4(3)
C13 C12 C11 119.7(3)
C12 C13 C8 120.3(3)
C19 C14 C15 119.4(3)
C19 C14 P1 121.3(2)
C15 C14 P1 119.3(2)
C16 C15 C14 120.0(3)
C17 C16 C15 120.1(3)
C16 C17 C18 120.5(3)
C17 C18 C19 119.9(3)
C18 C19 C14 120.0(3)
C21 C20 C25 120.7(3)
C22 C21 C20 120.3(3)
C23 C22 C21 119.8(3)
C22 C23 C24 120.0(3)
C23 C24 C25 121.2(3)
C24 C25 C20 117.9(3)
C24 C25 C26 120.5(3)
C20 C25 C26 121.5(3)
C25 C26 P2 116.5(2)
C32 C27 C28 118.4(3)
C32 C27 P2 125.0(3)
C28 C27 P2 115.6(2)
C29 C28 C27 120.4(3)
C30 C29 C28 120.5(3)
C29 C30 C31 120.0(3)
C30 C31 C32 120.0(3)
C27 C32 C31 120.7(3)
C34 C33 C38 118.3(3)
C34 C33 P2 117.3(2)
C38 C33 P2 124.4(3)
C35 C34 C33 120.9(3)
C36 C35 C34 120.1(4)
C35 C36 C37 120.1(3)
C36 C37 C38 120.3(4)
C37 C38 C33 120.2(3)
C40 C39 S1 105.1(3)
C39 C40 C41 105.7(3)
C42 C41 C40 107.2(3)
C41 C42 S1 106.8(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ir C1 2.064(3)
Ir P1 2.2423(8)
Ir P2 2.3136(7)
Ir Cl2 2.4358(7)
Ir S1 2.4411(8)
Ir Cl1 2.4521(7)
S1 C39 1.819(3)
S1 C42 1.833(3)
P1 C8 1.817(3)
P1 C7 1.823(3)
P1 C14 1.828(3)
P2 C33 1.821(3)
P2 C27 1.828(3)
P2 C26 1.855(3)
C1 C2 1.401(4)
C1 C6 1.403(4)
C2 C3 1.386(5)
C3 C4 1.381(6)
C4 C5 1.378(5)
C5 C6 1.390(4)
C6 C7 1.518(4)
C8 C13 1.389(4)
C8 C9 1.396(4)
C9 C10 1.389(4)
C10 C11 1.373(5)
C11 C12 1.386(5)
C12 C13 1.379(5)
C14 C19 1.392(4)
C14 C15 1.399(4)
C15 C16 1.385(4)
C16 C17 1.377(5)
C17 C18 1.383(5)
C18 C19 1.389(4)
C20 C21 1.385(4)
C20 C25 1.395(4)
C21 C22 1.378(5)
C22 C23 1.376(5)
C23 C24 1.385(4)
C24 C25 1.390(4)
C25 C26 1.507(4)
C27 C32 1.392(4)
C27 C28 1.393(5)
C28 C29 1.390(4)
C29 C30 1.375(5)
C30 C31 1.376(6)
C31 C32 1.393(5)
C33 C34 1.398(5)
C33 C38 1.399(4)
C34 C35 1.380(5)
C35 C36 1.370(6)
C36 C37 1.383(6)
C37 C38 1.386(5)
C39 C40 1.517(5)
C40 C41 1.523(5)
C41 C42 1.513(5)
