#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/67/4066787.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_4066787
loop_
_publ_author_name
'Nakai, Hidetaka'
'Nakano, Saori'
'Imai, Shunsuke'
'Isobe, Kiyoshi'
_publ_section_title
;
 Extraction of Hydrogen from Alcohols by a Methylene-Bridged Iridium(I)
 Dinuclear Complex Having a Short Ir−Ir Double Bond
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4210
_journal_paper_doi               10.1021/om100630g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C22 H36 Ir2 '
_chemical_formula_sum            'C22 H36 Ir2'
_chemical_formula_weight         684.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.245(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.1666(13)
_cell_length_b                   13.0931(15)
_cell_length_c                   14.6548(19)
_cell_measurement_reflns_used    6077
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2101.5(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22691
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    12.688
_exptl_absorpt_correction_T_max  0.218
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280.00
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.58
_refine_diff_density_min         -2.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4799
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0706P)²+24.3258P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                3719
_reflns_number_total             4799
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            om100630g_si_002.cif
_cod_data_source_block           '__Ir_dihydride'
_cod_original_formula_sum        'C22 H36 Ir2 '
_cod_database_code               4066787
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
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(1) Ir 0.55779(3) 0.85097(3) 0.18112(3) 0.02403(14) Uani 1.00 1 d .
Ir(2) Ir 0.43420(3) 0.83946(3) 0.31745(3) 0.02356(14) Uani 1.00 1 d .
C(1) C 0.6677(10) 0.7088(8) 0.1648(6) 0.034(2) Uani 1.00 1 d .
C(2) C 0.7322(9) 0.7983(7) 0.1472(8) 0.035(2) Uani 1.00 1 d .
C(3) C 0.6670(9) 0.8487(6) 0.0662(8) 0.033(2) Uani 1.00 1 d .
C(4) C 0.5585(10) 0.7963(8) 0.0380(7) 0.035(2) Uani 1.00 1 d .
C(5) C 0.5573(9) 0.7082(8) 0.0961(8) 0.036(2) Uani 1.00 1 d .
C(6) C 0.7128(12) 0.6281(9) 0.2363(8) 0.050(3) Uani 1.00 1 d .
C(7) C 0.8583(10) 0.8250(10) 0.1996(10) 0.056(3) Uani 1.00 1 d .
C(8) C 0.7102(11) 0.9405(8) 0.0244(9) 0.048(2) Uani 1.00 1 d .
C(9) C 0.4627(12) 0.8187(11) -0.0473(9) 0.058(3) Uani 1.00 1 d .
C(10) C 0.4571(12) 0.6261(10) 0.0777(11) 0.065(4) Uani 1.00 1 d .
C(11) C 0.4000(9) 0.6709(8) 0.3667(8) 0.033(2) Uani 1.00 1 d .
C(12) C 0.2856(8) 0.7218(8) 0.3323(7) 0.031(2) Uani 1.00 1 d .
C(13) C 0.2819(10) 0.8098(8) 0.3866(7) 0.035(2) Uani 1.00 1 d .
C(14) C 0.3964(9) 0.8146(8) 0.4565(7) 0.033(2) Uani 1.00 1 d .
C(15) C 0.4653(9) 0.7274(8) 0.4397(7) 0.032(2) Uani 1.00 1 d .
C(16) C 0.4303(10) 0.5669(9) 0.3335(8) 0.044(2) Uani 1.00 1 d .
C(17) C 0.1869(10) 0.6834(10) 0.2561(9) 0.052(3) Uani 1.00 1 d .
C(18) C 0.1738(10) 0.8816(8) 0.3831(9) 0.047(3) Uani 1.00 1 d .
C(19) C 0.4222(13) 0.8866(9) 0.5353(8) 0.053(3) Uani 1.00 1 d .
C(20) C 0.5857(9) 0.6985(10) 0.4962(8) 0.046(2) Uani 1.00 1 d .
C(21) C 0.6137(10) 0.8746(8) 0.3216(6) 0.034(2) Uani 1.00 1 d .
C(22) C 0.3739(9) 0.8698(9) 0.1770(6) 0.033(2) Uani 1.00 1 d .
H(1) H 0.7941 0.6469 0.2708 0.060 Uiso 1.00 1 c R
H(2) H 0.7175 0.5624 0.2052 0.060 Uiso 1.00 1 c R
H(3) H 0.6564 0.6224 0.2795 0.060 Uiso 1.00 1 c R
H(4) H 0.8865 0.8874 0.1734 0.067 Uiso 1.00 1 c R
H(5) H 0.9145 0.7689 0.1940 0.067 Uiso 1.00 1 c R
H(6) H 0.8560 0.8362 0.2653 0.067 Uiso 1.00 1 c R
H(7) H 0.6480 0.9627 -0.0287 0.058 Uiso 1.00 1 c R
H(8) H 0.7861 0.9248 0.0031 0.058 Uiso 1.00 1 c R
H(9) H 0.7252 0.9952 0.0708 0.058 Uiso 1.00 1 c R
H(10) H 0.3997 0.7657 -0.0549 0.070 Uiso 1.00 1 c R
H(11) H 0.5007 0.8197 -0.1022 0.070 Uiso 1.00 1 c R
H(12) H 0.4256 0.8854 -0.0404 0.070 Uiso 1.00 1 c R
H(13) H 0.4746 0.5731 0.1257 0.078 Uiso 1.00 1 c R
H(14) H 0.4551 0.5954 0.0164 0.078 Uiso 1.00 1 c R
H(15) H 0.3778 0.6574 0.0793 0.078 Uiso 1.00 1 c R
H(16) H 0.3626 0.5427 0.2854 0.053 Uiso 1.00 1 c R
H(17) H 0.4434 0.5190 0.3859 0.053 Uiso 1.00 1 c R
H(18) H 0.5047 0.5713 0.3075 0.053 Uiso 1.00 1 c R
H(19) H 0.1146 0.7270 0.2515 0.062 Uiso 1.00 1 c R
H(20) H 0.1658 0.6131 0.2699 0.062 Uiso 1.00 1 c R
H(21) H 0.2155 0.6848 0.1970 0.062 Uiso 1.00 1 c R
H(22) H 0.1916 0.9299 0.4351 0.057 Uiso 1.00 1 c R
H(23) H 0.1009 0.8418 0.3878 0.057 Uiso 1.00 1 c R
H(24) H 0.1594 0.9193 0.3242 0.057 Uiso 1.00 1 c R
H(25) H 0.5044 0.8739 0.5714 0.063 Uiso 1.00 1 c R
H(26) H 0.3623 0.8768 0.5753 0.063 Uiso 1.00 1 c R
H(27) H 0.4171 0.9568 0.5117 0.063 Uiso 1.00 1 c R
H(28) H 0.6176 0.6389 0.4682 0.055 Uiso 1.00 1 c R
H(29) H 0.5763 0.6817 0.5596 0.055 Uiso 1.00 1 c R
H(30) H 0.6426 0.7557 0.4981 0.055 Uiso 1.00 1 c R
H(31) H 0.6732 0.8242 0.3541 0.040 Uiso 1.00 1 c R
H(32) H 0.6372 0.9457 0.3399 0.040 Uiso 1.00 1 c R
H(33) H 0.3205 0.8169 0.1419 0.040 Uiso 1.00 1 c R
H(34) H 0.3423 0.9397 0.1622 0.040 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Ir Ir -1.444 7.990
;
International Tables for Crystallography
(1992, 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_publ_flag
Ir(2) Ir(1) C(1) 113.9(2) yes
Ir(2) Ir(1) C(2) 139.8(2) yes
Ir(2) Ir(1) C(3) 175.8(2) yes
Ir(2) Ir(1) C(4) 142.6(2) yes
Ir(2) Ir(1) C(5) 115.2(3) yes
Ir(2) Ir(1) C(21) 49.7(3) yes
Ir(2) Ir(1) C(22) 50.5(2) yes
C(1) Ir(1) C(2) 37.1(3) yes
C(1) Ir(1) C(3) 61.9(3) yes
C(1) Ir(1) C(4) 62.2(3) yes
C(1) Ir(1) C(5) 37.0(3) yes
C(1) Ir(1) C(21) 99.5(3) yes
C(1) Ir(1) C(22) 130.7(4) yes
C(2) Ir(1) C(3) 37.2(3) yes
C(2) Ir(1) C(4) 61.4(4) yes
C(2) Ir(1) C(5) 61.5(3) yes
C(2) Ir(1) C(21) 99.4(4) yes
C(2) Ir(1) C(22) 161.5(4) yes
C(3) Ir(1) C(4) 35.9(3) yes
C(3) Ir(1) C(5) 61.3(3) yes
C(3) Ir(1) C(21) 130.2(4) yes
C(3) Ir(1) C(22) 131.2(3) yes
C(4) Ir(1) C(5) 37.5(4) yes
C(4) Ir(1) C(21) 160.0(4) yes
C(4) Ir(1) C(22) 101.4(4) yes
C(5) Ir(1) C(21) 130.4(4) yes
C(5) Ir(1) C(22) 100.9(4) yes
C(21) Ir(1) C(22) 96.8(4) yes
Ir(1) Ir(2) C(11) 114.9(2) yes
Ir(1) Ir(2) C(12) 126.9(2) yes
Ir(1) Ir(2) C(13) 158.7(2) yes
Ir(1) Ir(2) C(14) 159.6(2) yes
Ir(1) Ir(2) C(15) 127.3(2) yes
Ir(1) Ir(2) C(21) 50.0(2) yes
Ir(1) Ir(2) C(22) 49.9(3) yes
C(11) Ir(2) C(12) 35.8(3) yes
C(11) Ir(2) C(13) 60.4(3) yes
C(11) Ir(2) C(14) 60.4(4) yes
C(11) Ir(2) C(15) 34.5(3) yes
C(11) Ir(2) C(21) 114.5(3) yes
C(11) Ir(2) C(22) 116.0(4) yes
C(12) Ir(2) C(13) 36.4(3) yes
C(12) Ir(2) C(14) 62.5(3) yes
C(12) Ir(2) C(15) 60.0(3) yes
C(12) Ir(2) C(21) 150.0(3) yes
C(12) Ir(2) C(22) 97.0(3) yes
C(13) Ir(2) C(14) 39.6(3) yes
C(13) Ir(2) C(15) 62.3(3) yes
C(13) Ir(2) C(21) 151.2(3) yes
C(13) Ir(2) C(22) 111.3(4) yes
C(14) Ir(2) C(15) 37.0(4) yes
C(14) Ir(2) C(21) 111.8(3) yes
C(14) Ir(2) C(22) 150.4(4) yes
C(15) Ir(2) C(21) 97.0(3) yes
C(15) Ir(2) C(22) 150.4(4) yes
C(21) Ir(2) C(22) 96.5(4) yes
Ir(1) C(1) C(2) 69.3(6) yes
Ir(1) C(1) C(5) 70.7(6) yes
Ir(1) C(1) C(6) 128.2(8) yes
C(2) C(1) C(5) 105.9(8) yes
C(2) C(1) C(6) 126.2(9) yes
C(5) C(1) C(6) 127.7(10) yes
Ir(1) C(2) C(1) 73.6(6) yes
Ir(1) C(2) C(3) 73.4(6) yes
Ir(1) C(2) C(7) 126.1(8) yes
C(1) C(2) C(3) 109.6(8) yes
C(1) C(2) C(7) 123.7(9) yes
C(3) C(2) C(7) 126.2(10) yes
Ir(1) C(3) C(2) 69.4(6) yes
Ir(1) C(3) C(4) 70.2(6) yes
Ir(1) C(3) C(8) 124.5(7) yes
C(2) C(3) C(4) 107.1(9) yes
C(2) C(3) C(8) 124.6(9) yes
C(4) C(3) C(8) 128.3(9) yes
Ir(1) C(4) C(3) 73.9(6) yes
Ir(1) C(4) C(5) 72.3(6) yes
Ir(1) C(4) C(9) 126.1(8) yes
C(3) C(4) C(5) 109.3(8) yes
C(3) C(4) C(9) 126.1(10) yes
C(5) C(4) C(9) 124.2(10) yes
Ir(1) C(5) C(1) 72.3(6) yes
Ir(1) C(5) C(4) 70.2(6) yes
Ir(1) C(5) C(10) 127.1(9) yes
C(1) C(5) C(4) 107.8(9) yes
C(1) C(5) C(10) 128.7(10) yes
C(4) C(5) C(10) 123.2(9) yes
Ir(2) C(11) C(12) 69.4(5) yes
Ir(2) C(11) C(15) 69.4(6) yes
Ir(2) C(11) C(16) 133.0(8) yes
C(12) C(11) C(15) 108.7(9) yes
C(12) C(11) C(16) 123.0(9) yes
C(15) C(11) C(16) 127.9(9) yes
Ir(2) C(12) C(11) 74.7(6) yes
Ir(2) C(12) C(13) 66.8(6) yes
Ir(2) C(12) C(17) 126.4(8) yes
C(11) C(12) C(13) 107.7(8) yes
C(11) C(12) C(17) 125.4(10) yes
C(13) C(12) C(17) 126.8(9) yes
Ir(2) C(13) C(12) 76.8(6) yes
Ir(2) C(13) C(14) 70.5(6) yes
Ir(2) C(13) C(18) 124.1(8) yes
C(12) C(13) C(14) 108.1(9) yes
C(12) C(13) C(18) 126.7(9) yes
C(14) C(13) C(18) 124.8(9) yes
Ir(2) C(14) C(13) 69.9(6) yes
Ir(2) C(14) C(15) 75.5(6) yes
Ir(2) C(14) C(19) 126.3(8) yes
C(13) C(14) C(15) 105.6(8) yes
C(13) C(14) C(19) 125.6(10) yes
C(15) C(14) C(19) 128.1(9) yes
Ir(2) C(15) C(11) 76.2(6) yes
Ir(2) C(15) C(14) 67.5(5) yes
Ir(2) C(15) C(20) 125.7(8) yes
C(11) C(15) C(14) 109.9(8) yes
C(11) C(15) C(20) 125.3(10) yes
C(14) C(15) C(20) 124.7(9) yes
Ir(1) C(21) Ir(2) 80.3(3) yes
Ir(1) C(22) Ir(2) 79.6(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ir(1) Ir(2) 2.6447(6) yes
Ir(1) C(1) 2.268(11) yes
Ir(1) C(2) 2.212(11) yes
Ir(1) C(3) 2.265(12) yes
Ir(1) C(4) 2.217(10) yes
Ir(1) C(5) 2.246(11) yes
Ir(1) C(21) 2.054(9) yes
Ir(1) C(22) 2.057(10) yes
Ir(2) C(11) 2.376(10) yes
Ir(2) C(12) 2.306(10) yes
Ir(2) C(13) 2.177(12) yes
Ir(2) C(14) 2.184(11) yes
Ir(2) C(15) 2.290(10) yes
Ir(2) C(21) 2.046(11) yes
Ir(2) C(22) 2.075(9) yes
C(1) C(2) 1.425(15) yes
C(1) C(5) 1.431(13) yes
C(1) C(6) 1.505(15) yes
C(2) C(3) 1.428(14) yes
C(2) C(7) 1.507(15) yes
C(3) C(4) 1.383(14) yes
C(3) C(8) 1.473(16) yes
C(4) C(5) 1.436(15) yes
C(4) C(9) 1.507(15) yes
C(5) C(10) 1.537(17) yes
C(11) C(12) 1.441(14) yes
C(11) C(15) 1.386(14) yes
C(11) C(16) 1.507(16) yes
C(12) C(13) 1.405(15) yes
C(12) C(17) 1.495(15) yes
C(13) C(14) 1.476(14) yes
C(13) C(18) 1.523(16) yes
C(14) C(15) 1.425(15) yes
C(14) C(19) 1.475(16) yes
C(15) C(20) 1.483(14) yes
