#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:13:32 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179051 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/13/4301344.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_4301344
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 O4 Rh2'
_chemical_formula_weight         708.57
_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                 108.5270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7608(4)
_cell_length_b                   9.9032(3)
_cell_length_c                   20.8259(5)
_cell_measurement_reflns_used    9271
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.36
_cell_measurement_theta_min      2.50
_cell_volume                     3082.09(14)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-AXS, 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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41812
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.8976
_exptl_absorpt_correction_T_min  0.7018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.475
_refine_diff_density_min         -1.886
_refine_diff_density_rms         0.138
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         12275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0680P)²+6.4405P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                9217
_reflns_number_total             12275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801933b_si_002_1.cif
_cod_data_source_block           rf114_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               4301344
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
Rh1 Rh 0.479587(16) 0.18735(3) 0.223516(12) 0.02383(7) Uani 1 1 d . . .
Rh2 Rh 0.531347(14) -0.11116(2) 0.171344(12) 0.02182(6) Uani 1 1 d . . .
O1 O 0.36381(15) 0.0681(3) 0.19406(13) 0.0303(5) Uani 1 1 d . . .
O2 O 0.39281(15) -0.0992(3) 0.13136(13) 0.0330(5) Uani 1 1 d . . .
O3 O 0.52224(18) -0.1418(3) 0.26873(13) 0.0351(6) Uani 1 1 d . . .
O4 O 0.53512(19) 0.0691(3) 0.30955(12) 0.0373(6) Uani 1 1 d . . .
C1 C 0.5991(2) 0.2953(4) 0.23723(17) 0.0289(6) Uani 1 1 d . . .
H1A H 0.6547 0.2436 0.2609 0.035 Uiso 1 1 calc R . .
C2 C 0.6020(2) 0.3700(4) 0.17440(18) 0.0298(7) Uani 1 1 d . . .
H2A H 0.6607 0.3545 0.1678 0.036 Uiso 1 1 calc R . .
H2B H 0.5958 0.4681 0.1808 0.036 Uiso 1 1 calc R . .
C3 C 0.5270(2) 0.3231(3) 0.11090(16) 0.0251(6) Uani 1 1 d . . .
H3A H 0.5097 0.3990 0.0784 0.030 Uiso 1 1 calc R . .
H3B H 0.5499 0.2491 0.0889 0.030 Uiso 1 1 calc R . .
C4 C 0.4454(2) 0.2741(3) 0.12730(15) 0.0244(6) Uani 1 1 d . . .
H4A H 0.4036 0.2183 0.0908 0.029 Uiso 1 1 calc R . .
C5 C 0.4035(2) 0.3466(4) 0.16658(18) 0.0315(7) Uani 1 1 d . . .
H5A H 0.3374 0.3328 0.1533 0.038 Uiso 1 1 calc R . .
C6 C 0.4347(3) 0.4855(4) 0.1960(2) 0.0407(9) Uani 1 1 d . . .
H6A H 0.3822 0.5397 0.1965 0.049 Uiso 1 1 calc R . .
H6B H 0.4641 0.5324 0.1668 0.049 Uiso 1 1 calc R . .
C7 C 0.5008(3) 0.4758(4) 0.2687(2) 0.0419(9) Uani 1 1 d . . .
H7A H 0.5422 0.5537 0.2772 0.050 Uiso 1 1 calc R . .
H7B H 0.4670 0.4806 0.3014 0.050 Uiso 1 1 calc R . .
C8 C 0.5543(3) 0.3466(4) 0.28011(18) 0.0345(7) Uani 1 1 d . . .
H8A H 0.5838 0.3243 0.3290 0.041 Uiso 1 1 calc R . .
C9 C 0.5266(2) -0.1796(3) 0.07549(16) 0.0256(6) Uani 1 1 d . . .
H9A H 0.4647 -0.1982 0.0446 0.031 Uiso 1 1 calc R . .
C10 C 0.5917(2) -0.2936(3) 0.07962(17) 0.0289(6) Uani 1 1 d . . .
H10A H 0.6099 -0.2934 0.0383 0.035 Uiso 1 1 calc R . .
H10B H 0.5615 -0.3806 0.0812 0.035 Uiso 1 1 calc R . .
C11 C 0.6760(2) -0.2822(3) 0.14256(17) 0.0265(6) Uani 1 1 d . . .
H11A H 0.6988 -0.3738 0.1578 0.032 Uiso 1 1 calc R . .
H11B H 0.7233 -0.2329 0.1302 0.032 Uiso 1 1 calc R . .
C12 C 0.6560(2) -0.2085(3) 0.20030(16) 0.0235(6) Uani 1 1 d . . .
H12A H 0.6691 -0.2624 0.2430 0.028 Uiso 1 1 calc R . .
C13 C 0.66827(19) -0.0694(3) 0.21057(16) 0.0233(5) Uani 1 1 d . . .
H13A H 0.6888 -0.0415 0.2593 0.028 Uiso 1 1 calc R . .
C14 C 0.6997(2) 0.0223(3) 0.16459(17) 0.0265(6) Uani 1 1 d . . .
H14A H 0.7633 0.0028 0.1704 0.032 Uiso 1 1 calc R . .
H14B H 0.6955 0.1174 0.1780 0.032 Uiso 1 1 calc R . .
C15 C 0.6440(2) 0.0044(3) 0.08927(17) 0.0270(6) Uani 1 1 d . . .
H15A H 0.6414 0.0915 0.0654 0.032 Uiso 1 1 calc R . .
H15B H 0.6739 -0.0622 0.0682 0.032 Uiso 1 1 calc R . .
C16 C 0.5496(2) -0.0431(3) 0.08110(15) 0.0237(6) Uani 1 1 d . . .
H16A H 0.5014 0.0185 0.0536 0.028 Uiso 1 1 calc R . .
C17 C 0.3415(2) -0.0303(4) 0.15458(18) 0.0311(7) Uani 1 1 d . . .
C18 C 0.2428(2) -0.0710(4) 0.1312(2) 0.0390(9) Uani 1 1 d . . .
H18A H 0.2410 -0.1500 0.1009 0.047 Uiso 1 1 calc R . .
C19 C 0.1868(3) 0.0298(6) 0.0851(3) 0.0636(16) Uani 1 1 d . . .
H19A H 0.1258 -0.0089 0.0684 0.076 Uiso 1 1 calc R . .
H19B H 0.1833 0.1086 0.1134 0.076 Uiso 1 1 calc R . .
C20 C 0.2053(3) 0.0824(6) 0.0273(3) 0.0594(14) Uani 1 1 d . . .
H20A H 0.2070 0.0041 -0.0019 0.071 Uiso 1 1 calc R . .
H20B H 0.2668 0.1193 0.0436 0.071 Uiso 1 1 calc R . .
C21 C 0.1489(3) 0.1862(5) -0.0175(2) 0.0420(9) Uani 1 1 d . . .
H21A H 0.1707 0.2000 -0.0567 0.050 Uiso 1 1 calc R . .
H21B H 0.1565 0.2726 0.0076 0.050 Uiso 1 1 calc R . .
C22 C 0.0498(2) 0.1522(5) -0.0438(2) 0.0428(9) Uani 1 1 d . . .
H22A H 0.0174 0.2257 -0.0729 0.064 Uiso 1 1 calc R . .
H22B H 0.0270 0.1408 -0.0055 0.064 Uiso 1 1 calc R . .
H22C H 0.0412 0.0683 -0.0700 0.064 Uiso 1 1 calc R . .
C23 C 0.2154(3) -0.1295(7) 0.1863(3) 0.0746(19) Uani 1 1 d . . .
H23A H 0.1535 -0.1634 0.1664 0.089 Uiso 1 1 calc R . .
H23B H 0.2133 -0.0553 0.2177 0.089 Uiso 1 1 calc R . .
C24 C 0.2697(3) -0.2399(5) 0.2272(3) 0.0482(11) Uani 1 1 d . . .
H24A H 0.2432 -0.2686 0.2617 0.072 Uiso 1 1 calc R . .
H24B H 0.3308 -0.2078 0.2493 0.072 Uiso 1 1 calc R . .
H24C H 0.2709 -0.3164 0.1977 0.072 Uiso 1 1 calc R . .
C25 C 0.5295(3) -0.0564(5) 0.31513(19) 0.0405(9) Uani 1 1 d . . .
C26 C 0.5328(5) -0.1106(7) 0.3846(3) 0.081(2) Uani 1 1 d . . .
H26A H 0.5642 -0.0301 0.4104 0.097 Uiso 1 1 calc R . .
C27 C 0.6098(3) -0.2067(5) 0.4135(2) 0.0439(9) Uani 1 1 d . . .
H27A H 0.6098 -0.2336 0.4593 0.053 Uiso 1 1 calc R . .
H27B H 0.5982 -0.2891 0.3852 0.053 Uiso 1 1 calc R . .
C28 C 0.6956(6) -0.1602(14) 0.4187(5) 0.199(8) Uani 1 1 d . . .
H28A H 0.7219 -0.2407 0.4041 0.239 Uiso 1 1 calc R . .
H28B H 0.6826 -0.0974 0.3798 0.239 Uiso 1 1 calc R . .
C29 C 0.7643(6) -0.1060(15) 0.4600(6) 0.202(8) Uani 1 1 d . . .
H29A H 0.8117 -0.1651 0.4537 0.243 Uiso 1 1 calc R . .
H29B H 0.7683 -0.0226 0.4349 0.243 Uiso 1 1 calc R . .
C30 C 0.8011(8) -0.0674(8) 0.5190(4) 0.149(5) Uani 1 1 d . . .
H30A H 0.8596 -0.0283 0.5228 0.223 Uiso 1 1 calc R . .
H30B H 0.8090 -0.1444 0.5500 0.223 Uiso 1 1 calc R . .
H30C H 0.7636 0.0010 0.5309 0.223 Uiso 1 1 calc R . .
C31 C 0.4595(5) -0.0955(15) 0.4017(4) 0.175(7) Uani 1 1 d . . .
H31A H 0.4822 -0.0681 0.4499 0.211 Uiso 1 1 calc R . .
H31B H 0.4370 -0.1888 0.4019 0.211 Uiso 1 1 calc R . .
C32 C 0.3810(5) -0.0177(8) 0.3748(3) 0.084(2) Uani 1 1 d . . .
H32A H 0.3407 -0.0333 0.4014 0.125 Uiso 1 1 calc R . .
H32B H 0.3512 -0.0441 0.3277 0.125 Uiso 1 1 calc R . .
H32C H 0.3969 0.0782 0.3766 0.125 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'
Rh Rh -1.1178 0.9187 '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
O4 Rh1 C4 164.91(12) . . ?
O4 Rh1 C8 86.09(13) . . ?
C4 Rh1 C8 99.08(14) . . ?
O4 Rh1 O1 91.36(11) . . ?
C4 Rh1 O1 90.91(11) . . ?
C8 Rh1 O1 150.61(13) . . ?
O4 Rh1 C5 155.97(13) . . ?
C4 Rh1 C5 39.05(13) . . ?
C8 Rh1 C5 82.55(15) . . ?
O1 Rh1 C5 88.31(12) . . ?
O4 Rh1 C1 93.18(13) . . ?
C4 Rh1 C1 82.42(13) . . ?
C8 Rh1 C1 38.92(14) . . ?
O1 Rh1 C1 169.94(12) . . ?
C5 Rh1 C1 91.18(14) . . ?
O2 Rh2 C9 85.51(12) . . ?
O2 Rh2 C13 165.32(12) . . ?
C9 Rh2 C13 99.02(12) . . ?
O2 Rh2 C12 155.52(12) . . ?
C9 Rh2 C12 82.60(13) . . ?
C13 Rh2 C12 39.01(12) . . ?
O2 Rh2 O3 90.55(10) . . ?
C9 Rh2 O3 152.13(12) . . ?
C13 Rh2 O3 91.72(11) . . ?
C12 Rh2 O3 90.06(11) . . ?
O2 Rh2 C16 92.77(11) . . ?
C9 Rh2 C16 38.91(13) . . ?
C13 Rh2 C16 82.44(12) . . ?
C12 Rh2 C16 91.30(12) . . ?
O3 Rh2 C16 168.87(12) . . ?
C17 O1 Rh1 131.9(2) . . ?
C17 O2 Rh2 126.5(2) . . ?
C25 O3 Rh2 128.7(2) . . ?
C25 O4 Rh1 127.8(3) . . ?
C8 C1 C2 122.3(3) . . ?
C8 C1 Rh1 70.1(2) . . ?
C2 C1 Rh1 113.7(2) . . ?
C1 C2 C3 111.7(3) . . ?
C4 C3 C2 112.3(3) . . ?
C5 C4 C3 124.1(3) . . ?
C5 C4 Rh1 71.11(19) . . ?
C3 C4 Rh1 111.7(2) . . ?
C4 C5 C6 123.1(3) . . ?
C4 C5 Rh1 69.84(18) . . ?
C6 C5 Rh1 113.4(2) . . ?
C5 C6 C7 111.7(3) . . ?
C8 C7 C6 112.1(3) . . ?
C1 C8 C7 125.3(3) . . ?
C1 C8 Rh1 71.0(2) . . ?
C7 C8 Rh1 111.4(3) . . ?
C16 C9 C10 124.5(3) . . ?
C16 C9 Rh2 71.06(18) . . ?
C10 C9 Rh2 111.8(2) . . ?
C9 C10 C11 112.3(3) . . ?
C12 C11 C10 111.5(3) . . ?
C13 C12 C11 122.6(3) . . ?
C13 C12 Rh2 70.27(17) . . ?
C11 C12 Rh2 113.8(2) . . ?
C12 C13 C14 123.5(3) . . ?
C12 C13 Rh2 70.72(17) . . ?
C14 C13 Rh2 112.1(2) . . ?
C13 C14 C15 112.3(3) . . ?
C16 C15 C14 111.7(3) . . ?
C9 C16 C15 122.0(3) . . ?
C9 C16 Rh2 70.03(18) . . ?
C15 C16 Rh2 114.0(2) . . ?
O1 C17 O2 126.2(3) . . ?
O1 C17 C18 117.3(3) . . ?
O2 C17 C18 116.5(4) . . ?
C23 C18 C19 121.0(4) . . ?
C23 C18 C17 112.2(4) . . ?
C19 C18 C17 111.6(3) . . ?
C20 C19 C18 124.0(5) . . ?
C19 C20 C21 123.0(5) . . ?
C20 C21 C22 114.5(4) . . ?
C18 C23 C24 118.8(5) . . ?
O4 C25 O3 125.8(3) . . ?
O4 C25 C26 117.0(4) . . ?
O3 C25 C26 117.2(4) . . ?
C31 C26 C27 128.6(5) . . ?
C31 C26 C25 116.5(5) . . ?
C27 C26 C25 112.4(4) . . ?
C28 C27 C26 117.3(7) . . ?
C29 C28 C27 142.0(12) . . ?
C30 C29 C28 146.2(13) . . ?
C26 C31 C32 133.2(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
Rh1 O4 2.086(2) . ?
Rh1 C4 2.088(3) . ?
Rh1 C8 2.093(4) . ?
Rh1 O1 2.095(2) . ?
Rh1 C5 2.104(3) . ?
Rh1 C1 2.105(3) . ?
Rh2 O2 2.078(2) . ?
Rh2 C9 2.087(3) . ?
Rh2 C13 2.092(3) . ?
Rh2 C12 2.098(3) . ?
Rh2 O3 2.100(2) . ?
Rh2 C16 2.101(3) . ?
O1 C17 1.251(5) . ?
O2 C17 1.266(4) . ?
O3 C25 1.262(5) . ?
O4 C25 1.254(5) . ?
C1 C8 1.398(5) . ?
C1 C2 1.516(5) . ?
C2 C3 1.539(4) . ?
C3 C4 1.512(4) . ?
C4 C5 1.401(5) . ?
C5 C6 1.522(6) . ?
C6 C7 1.543(6) . ?
C7 C8 1.509(5) . ?
C9 C16 1.395(5) . ?
C9 C10 1.509(5) . ?
C10 C11 1.546(4) . ?
C11 C12 1.523(5) . ?
C12 C13 1.399(4) . ?
C13 C14 1.513(4) . ?
C14 C15 1.545(5) . ?
C15 C16 1.518(4) . ?
C17 C18 1.529(5) . ?
C18 C23 1.467(7) . ?
C18 C19 1.470(6) . ?
C19 C20 1.425(7) . ?
C20 C21 1.480(7) . ?
C21 C22 1.520(5) . ?
C23 C24 1.480(7) . ?
C25 C26 1.528(5) . ?
C26 C31 1.322(8) . ?
C26 C27 1.509(7) . ?
C27 C28 1.400(9) . ?
C28 C29 1.268(10) . ?
C29 C30 1.241(10) . ?
C31 C32 1.413(9) . ?
