#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:58:54 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178927 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/56/4115678.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_4115678
loop_
_publ_author_name
'Rachel C. Linck'
'Robert J. Pafford'
'Thomas B. Rauchfuss'
_publ_section_title
;
 Heterolytic and Homolytic Activation of Dihydrogen at an Unusual Iridium
 (II) Sulfide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8856
_journal_page_last               8857
_journal_paper_doi               10.1021/ja010603q
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C76 H66 Ir2 N2 P4 S2'
_chemical_formula_weight         1579.71
_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                 112.6350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6333(11)
_cell_length_b                   13.1125(7)
_cell_length_c                   24.0252(12)
_cell_measurement_temperature    193(2)
_cell_volume                     6581.0(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21290
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.246
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prism
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0
_exptl_crystal_size_mid          0
_exptl_crystal_size_min          0
_refine_diff_density_max         2.205
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0426P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                5660
_reflns_number_total             7956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010603q_1.cif
_cod_data_source_block           h10j80fa
_cod_database_code               4115678
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
Ir1 Ir 0.439938(8) 0.515961(13) 0.204435(8) 0.02947(7) Uani 1 1 d .
S1 S 0.53224(6) 0.56781(9) 0.19680(5) 0.0371(3) Uani 1 1 d .
P1 P 0.37135(6) 0.59296(9) 0.12014(5) 0.0305(3) Uani 1 1 d .
P2 P 0.37605(6) 0.39641(9) 0.22112(5) 0.0309(3) Uani 1 1 d .
N1 N 0.0463(6) 0.3331(10) 0.0306(4) 0.195(6) Uani 1 1 d .
C1 C 0.3882(2) 0.7312(4) 0.1251(2) 0.0376(12) Uani 1 1 d .
C2 C 0.4126(2) 0.7764(3) 0.1816(2) 0.0353(11) Uani 1 1 d .
H2A H 0.4247 0.7350 0.2167 0.042 Uiso 1 1 calc R
C3 C 0.4193(2) 0.8818(4) 0.1874(2) 0.0426(13) Uani 1 1 d .
H3A H 0.4356 0.9120 0.2263 0.051 Uiso 1 1 calc R
C4 C 0.4027(3) 0.9416(4) 0.1376(3) 0.0537(15) Uani 1 1 d .
H4A H 0.4062 1.0137 0.1416 0.064 Uiso 1 1 calc R
C5 C 0.3809(3) 0.8980(4) 0.0815(3) 0.073(2) Uani 1 1 d .
H5A H 0.3706 0.9399 0.0468 0.088 Uiso 1 1 calc R
C6 C 0.3737(3) 0.7932(4) 0.0749(3) 0.0603(18) Uani 1 1 d .
H6A H 0.3587 0.7637 0.0358 0.072 Uiso 1 1 calc R
C7 C 0.3714(2) 0.5543(4) 0.0466(2) 0.0366(11) Uani 1 1 d .
C8 C 0.4223(3) 0.4977(4) 0.0438(3) 0.0479(14) Uani 1 1 d .
H8A H 0.4575 0.4806 0.0799 0.058 Uiso 1 1 calc R
C9 C 0.4218(3) 0.4661(5) -0.0118(3) 0.0619(17) Uani 1 1 d .
H9A H 0.4562 0.4263 -0.0134 0.074 Uiso 1 1 calc R
C10 C 0.3718(4) 0.4923(5) -0.0642(3) 0.0630(19) Uani 1 1 d .
H10A H 0.3719 0.4720 -0.1021 0.076 Uiso 1 1 calc R
C11 C 0.3213(3) 0.5485(4) -0.0614(2) 0.0582(17) Uani 1 1 d .
H11A H 0.2866 0.5666 -0.0976 0.070 Uiso 1 1 calc R
C12 C 0.3207(3) 0.5785(4) -0.0069(2) 0.0442(13) Uani 1 1 d .
H12A H 0.2854 0.6161 -0.0056 0.053 Uiso 1 1 calc R
C13 C 0.2855(2) 0.5932(3) 0.10297(19) 0.0310(10) Uani 1 1 d .
C14 C 0.2524(3) 0.6762(4) 0.1111(2) 0.0442(13) Uani 1 1 d .
H14A H 0.2743 0.7392 0.1238 0.053 Uiso 1 1 calc R
C15 C 0.1882(3) 0.6703(4) 0.1014(3) 0.0534(15) Uani 1 1 d .
H15A H 0.1665 0.7288 0.1074 0.064 Uiso 1 1 calc R
C16 C 0.1552(3) 0.5792(4) 0.0827(2) 0.0488(14) Uani 1 1 d .
H16A H 0.1112 0.5745 0.0765 0.059 Uiso 1 1 calc R
C17 C 0.1872(3) 0.4961(4) 0.0734(2) 0.0458(13) Uani 1 1 d .
H17A H 0.1650 0.4337 0.0599 0.055 Uiso 1 1 calc R
C18 C 0.2513(2) 0.5025(3) 0.0835(2) 0.0386(12) Uani 1 1 d .
H18A H 0.2727 0.4441 0.0771 0.046 Uiso 1 1 calc R
C19 C 0.3398(2) 0.3107(3) 0.1564(2) 0.0368(12) Uani 1 1 d .
C20 C 0.3763(3) 0.2869(4) 0.1238(2) 0.0467(14) Uani 1 1 d .
H20A H 0.4176 0.3163 0.1349 0.056 Uiso 1 1 calc R
C21 C 0.3540(3) 0.2208(5) 0.0751(3) 0.0600(17) Uani 1 1 d .
H21A H 0.3792 0.2065 0.0522 0.072 Uiso 1 1 calc R
C22 C 0.2954(4) 0.1767(4) 0.0603(3) 0.0640(19) Uani 1 1 d .
H22A H 0.2808 0.1288 0.0282 0.077 Uiso 1 1 calc R
C23 C 0.2572(3) 0.2003(4) 0.0910(3) 0.0585(17) Uani 1 1 d .
H23A H 0.2156 0.1712 0.0791 0.070 Uiso 1 1 calc R
C24 C 0.2794(3) 0.2669(4) 0.1398(2) 0.0457(13) Uani 1 1 d .
H24A H 0.2535 0.2824 0.1617 0.055 Uiso 1 1 calc R
C25 C 0.3107(2) 0.4347(3) 0.2440(2) 0.0335(11) Uani 1 1 d .
C26 C 0.2939(3) 0.5369(4) 0.2416(2) 0.0444(13) Uani 1 1 d .
H26A H 0.3172 0.5864 0.2295 0.053 Uiso 1 1 calc R
C27 C 0.2438(3) 0.5669(4) 0.2565(3) 0.0571(16) Uani 1 1 d .
H27A H 0.2334 0.6373 0.2552 0.069 Uiso 1 1 calc R
C28 C 0.2086(3) 0.4975(4) 0.2733(3) 0.0552(16) Uani 1 1 d .
H28A H 0.1730 0.5190 0.2822 0.066 Uiso 1 1 calc R
C29 C 0.2255(3) 0.3963(4) 0.2772(2) 0.0465(13) Uani 1 1 d .
H29A H 0.2016 0.3474 0.2891 0.056 Uiso 1 1 calc R
C30 C 0.2766(3) 0.3655(4) 0.2639(2) 0.0409(12) Uani 1 1 d .
H30A H 0.2888 0.2957 0.2685 0.049 Uiso 1 1 calc R
C31 C 0.4169(2) 0.3026(3) 0.2806(2) 0.0346(11) Uani 1 1 d .
C32 C 0.4329(3) 0.3282(4) 0.3407(2) 0.0415(13) Uani 1 1 d .
H32A H 0.4234 0.3945 0.3508 0.050 Uiso 1 1 calc R
C33 C 0.4629(3) 0.2579(4) 0.3867(2) 0.0463(14) Uani 1 1 d .
H33A H 0.4732 0.2760 0.4276 0.056 Uiso 1 1 calc R
C34 C 0.4775(3) 0.1616(4) 0.3720(3) 0.0465(14) Uani 1 1 d .
H34A H 0.4984 0.1137 0.4031 0.056 Uiso 1 1 calc R
C35 C 0.4622(3) 0.1353(4) 0.3136(2) 0.0496(14) Uani 1 1 d .
H35A H 0.4719 0.0688 0.3040 0.059 Uiso 1 1 calc R
C36 C 0.4323(3) 0.2049(4) 0.2677(2) 0.0451(13) Uani 1 1 d .
H36A H 0.4222 0.1856 0.2270 0.054 Uiso 1 1 calc R
C37 C 0.0655(5) 0.3223(7) 0.1396(4) 0.108(3) Uani 1 1 d .
H37A H 0.0918 0.3808 0.1602 0.162 Uiso 1 1 calc R
H37B H 0.0883 0.2589 0.1564 0.162 Uiso 1 1 calc R
H37C H 0.0248 0.3239 0.1452 0.162 Uiso 1 1 calc R
C38 C 0.0534(5) 0.3272(7) 0.0777(4) 0.101(3) 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
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'
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
P1 Ir1 S1 97.46(4) . .
P1 Ir1 P2 101.66(4) . .
S1 Ir1 P2 152.78(4) . .
P1 Ir1 S1 127.61(5) . 2_655
S1 Ir1 S1 95.70(5) . 2_655
P2 Ir1 S1 87.84(4) . 2_655
P1 Ir1 Ir1 146.99(3) . 2_655
S1 Ir1 Ir1 53.66(3) . 2_655
P2 Ir1 Ir1 111.11(3) . 2_655
S1 Ir1 Ir1 52.33(3) 2_655 2_655
Ir1 S1 Ir1 74.01(4) . 2_655
C13 P1 C7 100.2(2) . .
C13 P1 C1 100.9(2) . .
C7 P1 C1 104.8(2) . .
C13 P1 Ir1 120.52(15) . .
C7 P1 Ir1 118.95(17) . .
C1 P1 Ir1 109.09(15) . .
C25 P2 C19 105.8(2) . .
C25 P2 C31 99.9(2) . .
C19 P2 C31 100.1(2) . .
C25 P2 Ir1 120.36(15) . .
C19 P2 Ir1 112.39(17) . .
C31 P2 Ir1 115.74(16) . .
C6 C1 C2 118.2(4) . .
C6 C1 P1 123.1(4) . .
C2 C1 P1 118.5(4) . .
C1 C2 C3 120.7(4) . .
C4 C3 C2 120.2(5) . .
C3 C4 C5 120.0(5) . .
C4 C5 C6 120.5(5) . .
C1 C6 C5 120.4(5) . .
C12 C7 C8 118.7(5) . .
C12 C7 P1 121.4(4) . .
C8 C7 P1 119.9(4) . .
C9 C8 C7 120.1(6) . .
C10 C9 C8 120.3(6) . .
C9 C10 C11 119.6(6) . .
C12 C11 C10 120.6(6) . .
C11 C12 C7 120.7(6) . .
C14 C13 C18 117.2(5) . .
C14 C13 P1 124.0(4) . .
C18 C13 P1 118.6(4) . .
C13 C14 C15 121.7(5) . .
C14 C15 C16 120.2(5) . .
C17 C16 C15 118.9(5) . .
C16 C17 C18 120.5(5) . .
C17 C18 C13 121.4(5) . .
C20 C19 C24 118.8(5) . .
C20 C19 P2 116.7(4) . .
C24 C19 P2 124.5(4) . .
C19 C20 C21 121.3(6) . .
C22 C21 C20 119.2(6) . .
C21 C22 C23 121.1(5) . .
C22 C23 C24 119.7(6) . .
C23 C24 C19 119.9(6) . .
C26 C25 C30 117.7(5) . .
C26 C25 P2 119.4(4) . .
C30 C25 P2 122.9(4) . .
C27 C26 C25 120.5(5) . .
C28 C27 C26 121.3(5) . .
C27 C28 C29 118.9(6) . .
C28 C29 C30 120.4(5) . .
C29 C30 C25 121.1(5) . .
C32 C31 C36 117.7(4) . .
C32 C31 P2 119.9(4) . .
C36 C31 P2 122.4(4) . .
C31 C32 C33 121.1(5) . .
C34 C33 C32 119.4(5) . .
C35 C34 C33 120.3(5) . .
C34 C35 C36 120.5(5) . .
C35 C36 C31 120.9(5) . .
N1 C38 C37 177.1(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 P1 2.2606(12) .
Ir1 S1 2.2706(13) .
Ir1 P2 2.2705(13) .
Ir1 S1 2.3106(12) 2_655
Ir1 Ir1 2.7575(3) 2_655
S1 Ir1 2.3106(12) 2_655
P1 C13 1.823(5) .
P1 C7 1.838(5) .
P1 C1 1.847(5) .
P2 C25 1.835(5) .
P2 C19 1.836(5) .
P2 C31 1.841(5) .
N1 C38 1.084(10) .
C1 C6 1.384(7) .
C1 C2 1.386(6) .
C2 C3 1.392(7) .
C3 C4 1.358(7) .
C4 C5 1.369(8) .
C5 C6 1.386(7) .
C7 C12 1.389(6) .
C7 C8 1.396(7) .
C8 C9 1.394(8) .
C9 C10 1.374(9) .
C10 C11 1.382(9) .
C11 C12 1.374(7) .
C13 C14 1.379(7) .
C13 C18 1.397(6) .
C14 C15 1.383(7) .
C15 C16 1.388(8) .
C16 C17 1.374(8) .
C17 C18 1.379(7) .
C19 C20 1.377(7) .
C19 C24 1.391(7) .
C20 C21 1.386(7) .
C21 C22 1.363(9) .
C22 C23 1.372(9) .
C23 C24 1.391(7) .
C25 C26 1.388(7) .
C25 C30 1.391(7) .
C26 C27 1.372(8) .
C27 C28 1.369(8) .
C28 C29 1.374(7) .
C29 C30 1.374(7) .
C31 C32 1.388(7) .
C31 C36 1.394(7) .
C32 C33 1.398(7) .
C33 C34 1.385(8) .
C34 C35 1.353(7) .
C35 C36 1.391(7) .
C37 C38 1.405(10) .
