#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:13:32 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179051 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/13/4301345.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_4301345
loop_
_publ_author_name
'William M. Alley'
'Chase W. Girard'
'Saim Özkar'
'Richard G. Finke'
_publ_contact_author_address
;Colorado State University
Chemistry Department
Fort Collins, CO 80523-1872
;
_publ_contact_author_email       rfinke@lamar.colostate.edu
_publ_contact_author_fax         '(970) 491-1801'
_publ_contact_author_name        'Richard G. Finke'
_publ_contact_author_phone       '(970) 491-2541'
_publ_section_title
;
Model Ziegler-Type Hydrogenation Catalyst Precursors,
[(1,5-COD)M(μ-O2C8H15)]2 (M = Ir and Rh): Synthesis, Characterization, and
Demonstration of Catalytic Activity En Route to Identifying the True
Industrial Hydrogenation Catalysts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1114
_journal_page_last               1121
_journal_paper_doi               10.1021/ic801933b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C32 H54 Ir2 O4'
_chemical_formula_weight         887.15
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'Bruker SHELXTL'
_cell_angle_alpha                90.00
_cell_angle_beta                 108.408(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7748(5)
_cell_length_b                   9.8962(3)
_cell_length_c                   20.8847(7)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.50
_cell_measurement_theta_min      2.50
_cell_volume                     3093.50(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Apex2 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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            124557
_diffrn_reflns_theta_full        40.25
_diffrn_reflns_theta_max         40.25
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    8.629
_exptl_absorpt_correction_T_max  0.2526
_exptl_absorpt_correction_T_min  0.1380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       cube/rods
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.180
_refine_diff_density_min         -3.720
_refine_diff_density_rms         0.215
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         19129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0095P)²+20.6990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                14679
_reflns_number_total             19129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801933b_si_002_2.cif
_cod_data_source_block           rf102r_0m
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301345
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.479760(9) 0.688710(16) 0.723127(7) 0.02319(3) Uani 1 1 d . . .
Ir2 Ir 0.530396(8) 0.395863(15) 0.671508(7) 0.02098(3) Uani 1 1 d . . .
O1 O 0.36301(19) 0.5716(3) 0.69508(16) 0.0305(6) Uani 1 1 d . . .
O2 O 0.39174(18) 0.4055(3) 0.63175(17) 0.0322(6) Uani 1 1 d . . .
O3 O 0.5198(2) 0.3621(4) 0.76800(17) 0.0365(7) Uani 1 1 d . . .
O4 O 0.5316(2) 0.5720(4) 0.80996(15) 0.0389(8) Uani 1 1 d . . .
C1 C 0.5995(3) 0.7950(4) 0.7362(2) 0.0286(7) Uani 1 1 d . . .
H1A H 0.6549 0.7429 0.7598 0.034 Uiso 1 1 calc R . .
C2 C 0.6027(3) 0.8709(4) 0.6739(2) 0.0296(8) Uani 1 1 d . . .
H2A H 0.6611 0.8546 0.6670 0.035 Uiso 1 1 calc R . .
H2B H 0.5975 0.9691 0.6811 0.035 Uiso 1 1 calc R . .
C3 C 0.5273(2) 0.8268(4) 0.61040(18) 0.0234(6) Uani 1 1 d . . .
H3A H 0.5094 0.9045 0.5792 0.028 Uiso 1 1 calc R . .
H3B H 0.5498 0.7548 0.5871 0.028 Uiso 1 1 calc R . .
C4 C 0.4465(2) 0.7751(4) 0.62725(18) 0.0229(6) Uani 1 1 d . . .
H4A H 0.4048 0.7192 0.5908 0.027 Uiso 1 1 calc R . .
C5 C 0.4041(3) 0.8482(5) 0.6673(2) 0.0305(8) Uani 1 1 d . . .
H5A H 0.3380 0.8344 0.6541 0.037 Uiso 1 1 calc R . .
C6 C 0.4354(4) 0.9878(5) 0.6959(3) 0.0386(10) Uani 1 1 d . . .
H6A H 0.3831 1.0419 0.6971 0.046 Uiso 1 1 calc R . .
H6B H 0.4637 1.0345 0.6660 0.046 Uiso 1 1 calc R . .
C7 C 0.5028(4) 0.9786(6) 0.7679(3) 0.0424(11) Uani 1 1 d . . .
H7A H 0.5454 1.0549 0.7750 0.051 Uiso 1 1 calc R . .
H7B H 0.4703 0.9869 0.8012 0.051 Uiso 1 1 calc R . .
C8 C 0.5540(3) 0.8474(5) 0.7795(2) 0.0346(9) Uani 1 1 d . . .
H8A H 0.5832 0.8251 0.8282 0.042 Uiso 1 1 calc R . .
C9 C 0.5260(2) 0.3272(4) 0.57620(19) 0.0251(7) Uani 1 1 d . . .
H9A H 0.4643 0.3094 0.5452 0.030 Uiso 1 1 calc R . .
C10 C 0.5911(3) 0.2129(4) 0.5798(2) 0.0280(7) Uani 1 1 d . . .
H10A H 0.6100 0.2147 0.5389 0.034 Uiso 1 1 calc R . .
H10B H 0.5608 0.1257 0.5806 0.034 Uiso 1 1 calc R . .
C11 C 0.6744(3) 0.2228(4) 0.6428(2) 0.0263(7) Uani 1 1 d . . .
H11A H 0.6966 0.1308 0.6576 0.032 Uiso 1 1 calc R . .
H11B H 0.7221 0.2720 0.6311 0.032 Uiso 1 1 calc R . .
C12 C 0.6537(2) 0.2959(4) 0.70055(19) 0.0248(7) Uani 1 1 d . . .
H12A H 0.6660 0.2417 0.7429 0.030 Uiso 1 1 calc R . .
C13 C 0.6669(2) 0.4374(4) 0.71107(18) 0.0232(6) Uani 1 1 d . . .
H13A H 0.6871 0.4654 0.7595 0.028 Uiso 1 1 calc R . .
C14 C 0.7004(2) 0.5267(4) 0.6652(2) 0.0256(7) Uani 1 1 d . . .
H14A H 0.7635 0.5041 0.6711 0.031 Uiso 1 1 calc R . .
H14B H 0.6981 0.6223 0.6786 0.031 Uiso 1 1 calc R . .
C15 C 0.6451(3) 0.5104(4) 0.5905(2) 0.0258(7) Uani 1 1 d . . .
H15A H 0.6436 0.5975 0.5669 0.031 Uiso 1 1 calc R . .
H15B H 0.6740 0.4427 0.5693 0.031 Uiso 1 1 calc R . .
C16 C 0.5499(2) 0.4655(4) 0.58249(18) 0.0227(6) Uani 1 1 d . . .
H16A H 0.5024 0.5281 0.5552 0.027 Uiso 1 1 calc R . .
C17 C 0.3403(2) 0.4726(5) 0.6552(2) 0.0305(8) Uani 1 1 d . . .
C18 C 0.2419(3) 0.4329(6) 0.6321(3) 0.0381(10) Uani 1 1 d . . .
H18A H 0.2446 0.3564 0.6016 0.046 Uiso 1 1 calc R . .
C19 C 0.1881(4) 0.5244(9) 0.5825(4) 0.090(3) Uani 1 1 d . . .
H19A H 0.1307 0.4763 0.5625 0.108 Uiso 1 1 calc R . .
H19B H 0.1748 0.5999 0.6089 0.108 Uiso 1 1 calc R . .
C20 C 0.2049(4) 0.5859(9) 0.5283(4) 0.074(3) Uani 1 1 d . . .
H20A H 0.2134 0.5111 0.4995 0.089 Uiso 1 1 calc R . .
H20B H 0.2640 0.6295 0.5472 0.089 Uiso 1 1 calc R . .
C21 C 0.1490(3) 0.6849(6) 0.4819(3) 0.0420(12) Uani 1 1 d . . .
H21A H 0.1714 0.6950 0.4429 0.050 Uiso 1 1 calc R . .
H21B H 0.1560 0.7733 0.5052 0.050 Uiso 1 1 calc R . .
C22 C 0.0496(3) 0.6509(6) 0.4553(2) 0.0408(11) Uani 1 1 d . . .
H22A H 0.0174 0.7243 0.4262 0.061 Uiso 1 1 calc R . .
H22B H 0.0264 0.6398 0.4934 0.061 Uiso 1 1 calc R . .
H22C H 0.0411 0.5667 0.4293 0.061 Uiso 1 1 calc R . .
C23 C 0.2181(4) 0.3608(13) 0.6805(6) 0.155(7) Uani 1 1 d . . .
H23A H 0.1621 0.3135 0.6554 0.186 Uiso 1 1 calc R . .
H23B H 0.2009 0.4301 0.7083 0.186 Uiso 1 1 calc R . .
C24 C 0.2692(3) 0.2634(6) 0.7278(3) 0.0445(12) Uani 1 1 d . . .
H24A H 0.2384 0.2419 0.7606 0.067 Uiso 1 1 calc R . .
H24B H 0.3284 0.3007 0.7514 0.067 Uiso 1 1 calc R . .
H24C H 0.2757 0.1811 0.7038 0.067 Uiso 1 1 calc R . .
C25 C 0.5264(4) 0.4461(6) 0.8147(2) 0.0434(13) Uani 1 1 d . . .
C26 C 0.5281(6) 0.3856(9) 0.8823(4) 0.095(4) Uani 1 1 d . . .
H26A H 0.5612 0.4656 0.9073 0.114 Uiso 1 1 calc R . .
C27 C 0.6070(4) 0.2956(5) 0.9121(2) 0.0418(11) Uani 1 1 d . . .
H27A H 0.6038 0.2608 0.9557 0.050 Uiso 1 1 calc R . .
H27B H 0.6019 0.2170 0.8818 0.050 Uiso 1 1 calc R . .
C28 C 0.6897(8) 0.3530(19) 0.9230(7) 0.249(13) Uani 1 1 d . . .
H28A H 0.7118 0.2973 0.8922 0.298 Uiso 1 1 calc R . .
H28B H 0.6719 0.4393 0.8985 0.298 Uiso 1 1 calc R . .
C29 C 0.7617(8) 0.387(2) 0.9643(8) 0.222(12) Uani 1 1 d . . .
H29A H 0.7927 0.2993 0.9676 0.266 Uiso 1 1 calc R . .
H29B H 0.7847 0.4401 0.9331 0.266 Uiso 1 1 calc R . .
C30 C 0.8091(10) 0.4354(10) 1.0162(6) 0.156(7) Uani 1 1 d . . .
H30A H 0.8719 0.4214 1.0195 0.233 Uiso 1 1 calc R . .
H30B H 0.7971 0.3914 1.0545 0.233 Uiso 1 1 calc R . .
H30C H 0.7971 0.5324 1.0170 0.233 Uiso 1 1 calc R . .
C31 C 0.4599(6) 0.4110(17) 0.9029(5) 0.163(8) Uani 1 1 d . . .
H31A H 0.4874 0.4496 0.9485 0.196 Uiso 1 1 calc R . .
H31B H 0.4386 0.3202 0.9105 0.196 Uiso 1 1 calc R . .
C32 C 0.3798(6) 0.4867(9) 0.8765(4) 0.077(3) Uani 1 1 d . . .
H32A H 0.3398 0.4677 0.9030 0.116 Uiso 1 1 calc R . .
H32B H 0.3505 0.4612 0.8294 0.116 Uiso 1 1 calc R . .
H32C H 0.3940 0.5833 0.8791 0.116 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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
C8 Ir1 C4 99.17(17) . . ?
C8 Ir1 O4 86.00(17) . . ?
C4 Ir1 O4 166.32(14) . . ?
C8 Ir1 C5 82.35(18) . . ?
C4 Ir1 C5 39.79(16) . . ?
O4 Ir1 C5 153.88(15) . . ?
C8 Ir1 O1 149.41(16) . . ?
C4 Ir1 O1 91.47(13) . . ?
O4 Ir1 O1 90.31(14) . . ?
C5 Ir1 O1 87.98(15) . . ?
C8 Ir1 C1 39.52(17) . . ?
C4 Ir1 C1 82.15(15) . . ?
O4 Ir1 C1 94.26(16) . . ?
C5 Ir1 C1 91.51(17) . . ?
O1 Ir1 C1 170.54(14) . . ?
O2 Ir2 C9 85.41(14) . . ?
O2 Ir2 C13 166.05(15) . . ?
C9 Ir2 C13 99.28(15) . . ?
O2 Ir2 C12 154.13(15) . . ?
C9 Ir2 C12 82.56(15) . . ?
C13 Ir2 C12 39.74(15) . . ?
O2 Ir2 C16 93.49(13) . . ?
C9 Ir2 C16 39.59(15) . . ?
C13 Ir2 C16 82.22(14) . . ?
C12 Ir2 C16 91.69(15) . . ?
O2 Ir2 O3 89.89(13) . . ?
C9 Ir2 O3 151.15(15) . . ?
C13 Ir2 O3 92.07(14) . . ?
C12 Ir2 O3 89.72(14) . . ?
C16 Ir2 O3 169.17(15) . . ?
C17 O1 Ir1 130.9(3) . . ?
C17 O2 Ir2 126.3(3) . . ?
C25 O3 Ir2 128.7(3) . . ?
C25 O4 Ir1 126.9(3) . . ?
C8 C1 C2 121.8(4) . . ?
C8 C1 Ir1 69.6(3) . . ?
C2 C1 Ir1 114.1(3) . . ?
C1 C2 C3 111.9(3) . . ?
C4 C3 C2 111.9(3) . . ?
C5 C4 C3 123.5(4) . . ?
C5 C4 Ir1 70.5(2) . . ?
C3 C4 Ir1 112.7(2) . . ?
C4 C5 C6 122.5(4) . . ?
C4 C5 Ir1 69.7(2) . . ?
C6 C5 Ir1 114.0(3) . . ?
C5 C6 C7 111.5(4) . . ?
C8 C7 C6 112.1(4) . . ?
C1 C8 C7 124.5(4) . . ?
C1 C8 Ir1 70.9(2) . . ?
C7 C8 Ir1 112.4(3) . . ?
C16 C9 C10 124.2(3) . . ?
C16 C9 Ir2 70.6(2) . . ?
C10 C9 Ir2 112.2(3) . . ?
C9 C10 C11 112.2(3) . . ?
C12 C11 C10 111.5(3) . . ?
C13 C12 C11 122.0(3) . . ?
C13 C12 Ir2 70.0(2) . . ?
C11 C12 Ir2 113.9(2) . . ?
C12 C13 C14 122.7(3) . . ?
C12 C13 Ir2 70.3(2) . . ?
C14 C13 Ir2 112.7(2) . . ?
C13 C14 C15 112.4(3) . . ?
C16 C15 C14 111.5(3) . . ?
C9 C16 C15 121.1(3) . . ?
C9 C16 Ir2 69.8(2) . . ?
C15 C16 Ir2 114.4(2) . . ?
O2 C17 O1 125.6(4) . . ?
O2 C17 C18 117.2(4) . . ?
O1 C17 C18 117.2(4) . . ?
C23 C18 C19 128.2(6) . . ?
C23 C18 C17 112.7(5) . . ?
C19 C18 C17 112.2(4) . . ?
C20 C19 C18 130.2(7) . . ?
C19 C20 C21 127.3(6) . . ?
C20 C21 C22 115.4(4) . . ?
C18 C23 C24 128.9(8) . . ?
O4 C25 O3 125.9(4) . . ?
O4 C25 C26 118.6(6) . . ?
O3 C25 C26 115.5(6) . . ?
C31 C26 C27 130.0(5) . . ?
C31 C26 C25 117.1(6) . . ?
C27 C26 C25 112.7(4) . . ?
C28 C27 C26 116.4(9) . . ?
C29 C28 C27 147.5(15) . . ?
C30 C29 C28 155.3(19) . . ?
C26 C31 C32 134.4(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C8 2.086(5) . ?
Ir1 C4 2.086(3) . ?
Ir1 O4 2.087(3) . ?
Ir1 C5 2.097(4) . ?
Ir1 O1 2.097(3) . ?
Ir1 C1 2.103(4) . ?
Ir2 O2 2.082(3) . ?
Ir2 C9 2.084(4) . ?
Ir2 C13 2.089(3) . ?
Ir2 C12 2.093(4) . ?
Ir2 C16 2.094(3) . ?
Ir2 O3 2.101(3) . ?
O1 C17 1.262(6) . ?
O2 C17 1.261(5) . ?
O3 C25 1.260(7) . ?
O4 C25 1.254(7) . ?
C1 C8 1.416(6) . ?
C1 C2 1.517(6) . ?
C2 C3 1.539(5) . ?
C3 C4 1.515(5) . ?
C4 C5 1.423(6) . ?
C5 C6 1.524(7) . ?
C6 C7 1.545(7) . ?
C7 C8 1.509(7) . ?
C9 C16 1.415(5) . ?
C9 C10 1.514(6) . ?
C10 C11 1.540(6) . ?
C11 C12 1.528(6) . ?
C12 C13 1.422(6) . ?
C13 C14 1.516(5) . ?
C14 C15 1.537(6) . ?
C15 C16 1.524(5) . ?
C17 C18 1.525(5) . ?
C18 C23 1.383(9) . ?
C18 C19 1.435(7) . ?
C19 C20 1.381(9) . ?
C20 C21 1.463(8) . ?
C21 C22 1.526(6) . ?
C23 C24 1.432(9) . ?
C25 C26 1.528(6) . ?
C26 C31 1.302(10) . ?
C26 C27 1.497(8) . ?
C27 C28 1.375(11) . ?
C28 C29 1.237(13) . ?
C29 C30 1.204(13) . ?
C31 C32 1.421(11) . ?
