# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1417859'
_audit_update_record             
;
2015-08-10 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;
#=======================================================
_audit_creation_date             08-01-08
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title '1081416 Pn*Rh2(CO)4'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   12.3626(3)
_cell_length_b                   10.7476(3)
_cell_length_c                   14.5062(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.6252(12)
_cell_angle_gamma                90
_cell_volume                     1836.94(9)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062
5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C18 H18 O4 Rh2 
# Dc =      1.82 Fooo =    992.00 Mu =     18.14 M =    504.15
# Found Formula = C18 H18 O4 Rh2 
# Dc =      1.82 FOOO =    992.00 Mu =     18.14 M =    504.15

_chemical_formula_sum            'C18 H18 O4 Rh2'
_chemical_formula_moiety         'C18 H18 O4 Rh2'
_chemical_compound_source        SYN
_chemical_formula_weight         504.15


_cell_measurement_reflns_used    4319
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark orange'
_exptl_crystal_size_min          0.04
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_max          0.14

_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    1.814

# Sheldrick geometric approximatio 0.78 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.93
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            28297
_reflns_number_total             8089
_diffrn_reflns_av_R_equivalents  0.028
# Number of reflections with Friedels Law is 8089 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 4177 


_diffrn_reflns_theta_min         5.087
_diffrn_reflns_theta_max         27.397
_diffrn_measured_fraction_theta_max 0.990

_diffrn_reflns_theta_full        26.849
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -16
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   2.18
_oxford_diffrn_Wilson_scale      19.74

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -1.03
_refine_diff_density_max         0.96


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     0
_refine_ls_number_parameters     217
_oxford_refine_ls_R_factor_ref   0.0386
_refine_ls_wR_factor_ref         0.1005
_refine_ls_goodness_of_fit_ref   1.0293
_refine_ls_shift/su_max          0.000804


# The values computed from all data 
_oxford_reflns_number_all        4132
_refine_ls_R_factor_all          0.0568
_refine_ls_wR_factor_all         0.1140

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3346
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_gt          0.1038

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 6.86P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 0.8310(4) 0.6972(5) 0.8814(4) 0.0307 1.0000 Uani . . . . . . .
C2 C 0.8353(4) 0.5730(5) 0.9193(4) 0.0316 1.0000 Uani . . . . . . .
C3 C 0.7924(4) 0.5755(5) 1.0019(4) 0.0290 1.0000 Uani . . . . . . .
C4 C 0.7832(4) 0.7060(5) 1.0247(4) 0.0264 1.0000 Uani . . . . . . .
C5 C 0.7612(4) 0.7894(5) 1.0967(4) 0.0295 1.0000 Uani . . . . . . .
C6 C 0.7822(4) 0.9138(5) 1.0696(4) 0.0308 1.0000 Uani . . . . . . .
C7 C 0.7935(4) 0.9095(5) 0.9736(4) 0.0306 1.0000 Uani . . . . . . .
C8 C 0.8047(4) 0.7796(5) 0.9512(4) 0.0276 1.0000 Uani . . . . . . .
C9 C 0.8745(5) 0.7379(6) 0.7999(4) 0.0416 1.0000 Uani . . . . . . .
C10 C 0.8811(5) 0.4610(6) 0.8831(4) 0.0416 1.0000 Uani . . . . . . .
C11 C 0.7902(5) 0.4661(5) 1.0660(4) 0.0373 1.0000 Uani . . . . . . .
C12 C 0.7515(5) 0.7517(6) 1.1934(4) 0.0368 1.0000 Uani . . . . . . .
C13 C 0.7981(5) 1.0268(5) 1.1328(4) 0.0419 1.0000 Uani . . . . . . .
C14 C 0.8234(5) 1.0193(5) 0.9212(4) 0.0402 1.0000 Uani . . . . . . .
C15 C 0.5745(4) 0.6785(5) 0.7428(4) 0.0309 1.0000 Uani . . . . . . .
C16 C 0.5381(5) 0.5307(6) 0.8786(4) 0.0355 1.0000 Uani . . . . . . .
C17 C 0.4924(5) 0.8022(5) 1.0053(4) 0.0377 1.0000 Uani . . . . . . .
C18 C 0.5303(5) 0.9436(6) 0.8655(4) 0.0362 1.0000 Uani . . . . . . .
Rh19 Rh 0.65672(3) 0.62893(4) 0.86793(3) 0.0260 1.0000 Uani . . . . . . .
Rh20 Rh 0.61993(3) 0.85120(4) 0.96934(3) 0.0271 1.0000 Uani . . . . . . .
O21 O 0.5238(3) 0.7076(4) 0.6664(3) 0.0417 1.0000 Uani . . . . . . .
O22 O 0.4745(4) 1.0031(4) 0.8038(3) 0.0517 1.0000 Uani . . . . . . .
O23 O 0.4639(4) 0.4697(5) 0.8846(3) 0.0554 1.0000 Uani . . . . . . .
O24 O 0.4146(4) 0.7755(4) 1.0273(4) 0.0527 1.0000 Uani . . . . . . .
H91 H 0.8315 0.8080 0.7672 0.0629 1.0000 Uiso R . . . . . .
H92 H 0.9533 0.7613 0.8254 0.0629 1.0000 Uiso R . . . . . .
H93 H 0.8682 0.6709 0.7545 0.0631 1.0000 Uiso R . . . . . .
H101 H 0.8421 0.3883 0.8951 0.0599 1.0000 Uiso R . . . . . .
H102 H 0.9605 0.4535 0.9160 0.0599 1.0000 Uiso R . . . . . .
H103 H 0.8692 0.4694 0.8150 0.0600 1.0000 Uiso R . . . . . .
H111 H 0.7269 0.4753 1.0911 0.0539 1.0000 Uiso R . . . . . .
H112 H 0.8603 0.4632 1.1186 0.0541 1.0000 Uiso R . . . . . .
H113 H 0.7819 0.3905 1.0289 0.0541 1.0000 Uiso R . . . . . .
H121 H 0.7186 0.8192 1.2191 0.0561 1.0000 Uiso R . . . . . .
H122 H 0.8252 0.7326 1.2368 0.0560 1.0000 Uiso R . . . . . .
H123 H 0.7036 0.6797 1.1861 0.0559 1.0000 Uiso R . . . . . .
H131 H 0.7708 1.0993 1.0937 0.0609 1.0000 Uiso R . . . . . .
H132 H 0.8774 1.0365 1.1665 0.0610 1.0000 Uiso R . . . . . .
H133 H 0.7567 1.0168 1.1790 0.0610 1.0000 Uiso R . . . . . .
H141 H 0.7928 1.0071 0.8525 0.0571 1.0000 Uiso R . . . . . .
H142 H 0.9045 1.0271 0.9385 0.0570 1.0000 Uiso R . . . . . .
H143 H 0.7914 1.0938 0.9394 0.0571 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2307(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.439(8) yes
C1 . C8 . 1.454(7) yes
C1 . C9 . 1.504(7) yes
C1 . Rh19 . 2.228(5) yes
C2 . C3 . 1.450(7) yes
C2 . C10 . 1.491(8) yes
C2 . Rh19 . 2.190(5) yes
C3 . C4 . 1.453(7) yes
C3 . C11 . 1.504(7) yes
C3 . Rh19 . 2.224(5) yes
C4 . C5 . 1.462(7) yes
C4 . C8 . 1.417(7) yes
C4 . Rh19 . 2.480(5) yes
C4 . Rh20 . 2.484(5) yes
C5 . C6 . 1.439(7) yes
C5 . C12 . 1.500(7) yes
C5 . Rh20 . 2.225(5) yes
C6 . C7 . 1.442(7) yes
C6 . C13 . 1.498(7) yes
C6 . Rh20 . 2.196(5) yes
C7 . C8 . 1.449(7) yes
C7 . C14 . 1.508(7) yes
C7 . Rh20 . 2.219(5) yes
C8 . Rh19 . 2.468(5) yes
C8 . Rh20 . 2.499(5) yes
C9 . H91 . 0.961 no
C9 . H92 . 0.965 no
C9 . H93 . 0.963 no
C10 . H101 . 0.961 no
C10 . H102 . 0.957 no
C10 . H103 . 0.958 no
C11 . H111 . 0.963 no
C11 . H112 . 0.966 no
C11 . H113 . 0.962 no
C12 . H121 . 0.960 no
C12 . H122 . 0.960 no
C12 . H123 . 0.961 no
C13 . H131 . 0.963 no
C13 . H132 . 0.959 no
C13 . H133 . 0.965 no
C14 . H141 . 0.961 no
C14 . H142 . 0.961 no
C14 . H143 . 0.965 no
C15 . Rh19 . 1.870(6) yes
C15 . O21 . 1.139(6) yes
C16 . Rh19 . 1.851(5) yes
C16 . O23 . 1.152(7) yes
C17 . Rh20 . 1.880(6) yes
C17 . O24 . 1.138(7) yes
C18 . Rh20 . 1.863(6) yes
C18 . O22 . 1.146(7) yes
Rh19 . Rh20 . 2.9125(6) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C8 . 106.8(4) yes
C2 . C1 . C9 . 126.1(5) yes
C8 . C1 . C9 . 125.4(5) yes
C2 . C1 . Rh19 . 69.6(3) yes
C8 . C1 . Rh19 . 81.2(3) yes
C9 . C1 . Rh19 . 126.4(4) yes
C1 . C2 . C3 . 108.5(5) yes
C1 . C2 . C10 . 126.0(5) yes
C3 . C2 . C10 . 125.4(5) yes
C1 . C2 . Rh19 . 72.4(3) yes
C3 . C2 . Rh19 . 72.1(3) yes
C10 . C2 . Rh19 . 123.5(4) yes
C2 . C3 . C4 . 106.3(4) yes
C2 . C3 . C11 . 125.1(5) yes
C4 . C3 . C11 . 126.6(5) yes
C2 . C3 . Rh19 . 69.6(3) yes
C4 . C3 . Rh19 . 81.9(3) yes
C11 . C3 . Rh19 . 126.3(4) yes
C3 . C4 . C5 . 143.0(5) yes
C3 . C4 . C8 . 108.8(4) yes
C5 . C4 . C8 . 108.2(4) yes
C3 . C4 . Rh19 . 62.6(3) yes
C5 . C4 . Rh19 . 131.1(3) yes
C8 . C4 . Rh19 . 72.9(3) yes
C3 . C4 . Rh20 . 130.1(3) yes
C5 . C4 . Rh20 . 62.4(3) yes
C8 . C4 . Rh20 . 74.0(3) yes
Rh19 . C4 . Rh20 . 71.84(12) yes
C4 . C5 . C6 . 106.6(4) yes
C4 . C5 . C12 . 125.9(5) yes
C6 . C5 . C12 . 125.3(5) yes
C4 . C5 . Rh20 . 81.9(3) yes
C6 . C5 . Rh20 . 69.9(3) yes
C12 . C5 . Rh20 . 126.3(4) yes
C5 . C6 . C7 . 108.2(5) yes
C5 . C6 . C13 . 125.9(5) yes
C7 . C6 . C13 . 125.7(5) yes
C5 . C6 . Rh20 . 72.1(3) yes
C7 . C6 . Rh20 . 71.8(3) yes
C13 . C6 . Rh20 . 125.3(4) yes
C6 . C7 . C8 . 106.9(4) yes
C6 . C7 . C14 . 124.9(5) yes
C8 . C7 . C14 . 125.9(5) yes
C6 . C7 . Rh20 . 70.1(3) yes
C8 . C7 . Rh20 . 83.0(3) yes
C14 . C7 . Rh20 . 126.1(4) yes
C1 . C8 . C7 . 143.1(5) yes
C1 . C8 . C4 . 108.4(4) yes
C7 . C8 . C4 . 108.5(4) yes
C1 . C8 . Rh19 . 63.2(3) yes
C7 . C8 . Rh19 . 129.4(3) yes
C4 . C8 . Rh19 . 73.8(3) yes
C1 . C8 . Rh20 . 131.7(3) yes
C7 . C8 . Rh20 . 61.8(3) yes
C4 . C8 . Rh20 . 72.9(3) yes
Rh19 . C8 . Rh20 . 71.80(13) yes
C1 . C9 . H91 . 109.9 no
C1 . C9 . H92 . 109.5 no
H91 . C9 . H92 . 109.1 no
C1 . C9 . H93 . 110.3 no
H91 . C9 . H93 . 109.3 no
H92 . C9 . H93 . 108.7 no
C2 . C10 . H101 . 109.2 no
C2 . C10 . H102 . 109.5 no
H101 . C10 . H102 . 109.7 no
C2 . C10 . H103 . 109.4 no
H101 . C10 . H103 . 109.5 no
H102 . C10 . H103 . 109.6 no
C3 . C11 . H111 . 108.8 no
C3 . C11 . H112 . 109.5 no
H111 . C11 . H112 . 110.0 no
C3 . C11 . H113 . 109.5 no
H111 . C11 . H113 . 109.6 no
H112 . C11 . H113 . 109.5 no
C5 . C12 . H121 . 108.8 no
C5 . C12 . H122 . 110.0 no
H121 . C12 . H122 . 109.7 no
C5 . C12 . H123 . 109.6 no
H121 . C12 . H123 . 109.3 no
H122 . C12 . H123 . 109.4 no
C6 . C13 . H131 . 109.7 no
C6 . C13 . H132 . 108.9 no
H131 . C13 . H132 . 109.5 no
C6 . C13 . H133 . 109.6 no
H131 . C13 . H133 . 109.6 no
H132 . C13 . H133 . 109.5 no
C7 . C14 . H141 . 109.6 no
C7 . C14 . H142 . 109.4 no
H141 . C14 . H142 . 109.5 no
C7 . C14 . H143 . 109.1 no
H141 . C14 . H143 . 109.4 no
H142 . C14 . H143 . 109.8 no
Rh19 . C15 . O21 . 179.3(5) yes
Rh19 . C16 . O23 . 179.5(5) yes
Rh20 . C17 . O24 . 178.4(5) yes
Rh20 . C18 . O22 . 177.7(5) yes
C1 . Rh19 . C3 . 63.56(19) yes
C1 . Rh19 . C2 . 38.0(2) yes
C3 . Rh19 . C2 . 38.34(19) yes
C1 . Rh19 . C8 . 35.60(18) yes
C3 . Rh19 . C8 . 59.37(17) yes
C2 . Rh19 . C8 . 59.48(18) yes
C1 . Rh19 . C4 . 59.00(17) yes
C3 . Rh19 . C4 . 35.46(17) yes
C2 . Rh19 . C4 . 59.26(18) yes
C8 . Rh19 . C4 . 33.28(16) yes
C1 . Rh19 . C15 . 102.6(2) yes
C3 . Rh19 . C15 . 165.1(2) yes
C2 . Rh19 . C15 . 127.2(2) yes
C8 . Rh19 . C15 . 113.1(2) yes
C4 . Rh19 . C15 . 143.3(2) yes
C1 . Rh19 . C16 . 161.8(2) yes
C3 . Rh19 . C16 . 100.7(2) yes
C2 . Rh19 . C16 . 123.9(2) yes
C8 . Rh19 . C16 . 145.3(2) yes
C4 . Rh19 . C16 . 114.1(2) yes
C1 . Rh19 . Rh20 . 88.87(14) yes
C3 . Rh19 . Rh20 . 87.83(13) yes
C2 . Rh19 . Rh20 . 110.42(14) yes
C8 . Rh19 . Rh20 . 54.59(12) yes
C4 . Rh19 . Rh20 . 54.15(11) yes
C15 . Rh19 . C16 . 91.9(2) yes
C15 . Rh19 . Rh20 . 97.76(16) yes
C16 . Rh19 . Rh20 . 100.19(19) yes
C5 . Rh20 . C7 . 63.39(19) yes
C5 . Rh20 . C6 . 37.99(19) yes
C7 . Rh20 . C6 . 38.13(19) yes
C5 . Rh20 . Rh19 . 88.34(13) yes
C7 . Rh20 . Rh19 . 87.02(14) yes
C6 . Rh20 . Rh19 . 109.55(14) yes
C5 . Rh20 . C4 . 35.64(17) yes
C7 . Rh20 . C4 . 58.96(17) yes
C6 . Rh20 . C4 . 59.25(17) yes
Rh19 . Rh20 . C4 . 54.01(11) yes
C5 . Rh20 . C8 . 58.86(18) yes
C7 . Rh20 . C8 . 35.15(18) yes
C6 . Rh20 . C8 . 58.89(18) yes
Rh19 . Rh20 . C8 . 53.61(11) yes
C4 . Rh20 . C8 . 33.04(16) yes
C5 . Rh20 . C17 . 101.5(2) yes
C7 . Rh20 . C17 . 163.2(2) yes
C6 . Rh20 . C17 . 125.2(2) yes
Rh19 . Rh20 . C17 . 100.54(18) yes
C4 . Rh20 . C17 . 113.7(2) yes
C5 . Rh20 . C18 . 162.8(2) yes
C7 . Rh20 . C18 . 101.8(2) yes
C6 . Rh20 . C18 . 124.9(2) yes
Rh19 . Rh20 . C18 . 100.03(17) yes
C4 . Rh20 . C18 . 145.3(2) yes
C8 . Rh20 . C17 . 144.4(2) yes
C8 . Rh20 . C18 . 114.7(2) yes
C17 . Rh20 . C18 . 91.7(2) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C11 . H111 . O23 2_667 165 0.96 2.56 3.496(8) yes
C12 . H123 . O23 2_667 160 0.96 2.57 3.494(8) yes
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1417860'
_audit_update_record             
;
2015-08-10 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;
#==================================================

_audit_creation_date             2015-08-10
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '11251214 Pn*[Ir(CO)2]2'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'
_cell_length_a                   12.2542(3)
_cell_length_b                   10.8292(3)
_cell_length_c                   14.3587(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.9133(11)
_cell_angle_gamma                90
_cell_volume                     1823.03(8)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C18 H18 Ir2 O4 
# Dc =      2.49 Fooo =   1248.00 Mu =    146.02 M =    682.78
# Found Formula = C18 H18 Ir2 O4 
# Dc =      2.49 FOOO =   1248.00 Mu =    146.02 M =    682.78

_chemical_formula_sum            'C18 H18 Ir2 O4'
_chemical_formula_moiety         'C18 H18 Ir2 O4'
_chemical_compound_source        SYN
_chemical_formula_weight         682.78


_cell_measurement_reflns_used    4241
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.020
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_max          0.060

_exptl_crystal_density_diffrn    2.488
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    14.602

# Sheldrick geometric approximatio 0.56 0.75 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.75
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            7721
_reflns_number_total             4147
_diffrn_reflns_av_R_equivalents  0.033
# Number of reflections without Friedels Law is 4147 
# Number of reflections with Friedels Law is 0 
# Theoretical number of reflections is about 4185 


_diffrn_reflns_theta_min         5.126
_diffrn_reflns_theta_max         27.494
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.669
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   1.94
_oxford_diffrn_Wilson_scale      130.62

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.91
_refine_diff_density_max         1.77


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         3255
_refine_ls_number_restraints     0
_refine_ls_number_parameters     218
_oxford_refine_ls_R_factor_ref   0.0327
_refine_ls_wR_factor_ref         0.0768
_refine_ls_goodness_of_fit_ref   0.9982
_refine_ls_shift/su_max          0.0134608
_refine_ls_shift/su_mean         0.0004456


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4147
_refine_ls_R_factor_all          0.0459
_refine_ls_wR_factor_all         0.0855

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3453
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_gt          0.0793

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² +11.08P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ir1 Ir 0.34430(2) 0.62514(3) 0.63212(2) 0.0231 1.0000 Uani . . . . . .
Ir2 Ir 0.38214(2) 0.84786(3) 0.52960(2) 0.0236 1.0000 Uani . . . . . .
C3 C 0.4723(7) 0.9390(8) 0.6327(6) 0.0321 1.0000 Uani . . . . . .
O4 O 0.5266(5) 0.9986(6) 0.6954(4) 0.0437 1.0000 Uani . . . . . .
C5 C 0.2396(6) 0.7849(7) 0.4021(6) 0.0289 1.0000 Uani . . . . . .
C6 C 0.2200(6) 0.9097(7) 0.4315(5) 0.0270 1.0000 Uani . . . . . .
C7 C 0.2059(6) 0.9042(7) 0.5276(6) 0.0266 1.0000 Uani . . . . . .
C8 C 0.1927(6) 0.7752(7) 0.5486(5) 0.0235 1.0000 Uani . . . . . .
C9 C 0.2144(6) 0.7020(7) 0.4724(5) 0.0250 1.0000 Uani . . . . . .
C10 C 0.2072(6) 0.5722(7) 0.4971(5) 0.0242 1.0000 Uani . . . . . .
C11 C 0.1658(6) 0.5685(7) 0.5814(6) 0.0284 1.0000 Uani . . . . . .
C12 C 0.1678(6) 0.6921(7) 0.6199(5) 0.0253 1.0000 Uani . . . . . .
C13 C 0.1232(7) 0.7309(8) 0.7020(6) 0.0363 1.0000 Uani . . . . . .
C14 C 0.1176(7) 0.4566(8) 0.6173(7) 0.0386 1.0000 Uani . . . . . .
C15 C 0.2117(7) 0.4647(7) 0.4332(6) 0.0341 1.0000 Uani . . . . . .
C16 C 0.1759(7) 1.0132(8) 0.5803(6) 0.0364 1.0000 Uani . . . . . .
C17 C 0.2023(8) 1.0217(8) 0.3677(6) 0.0374 1.0000 Uani . . . . . .
C18 C 0.2496(7) 0.7498(8) 0.3039(5) 0.0323 1.0000 Uani . . . . . .
C19 C 0.5106(7) 0.8032(7) 0.4918(6) 0.0341 1.0000 Uani . . . . . .
O20 O 0.5888(5) 0.7798(6) 0.4677(5) 0.0465 1.0000 Uani . . . . . .
C21 C 0.4656(7) 0.5262(8) 0.6217(6) 0.0306 1.0000 Uani . . . . . .
O22 O 0.5369(5) 0.4627(6) 0.6147(5) 0.0466 1.0000 Uani . . . . . .
C23 C 0.4276(7) 0.6741(7) 0.7575(6) 0.0306 1.0000 Uani . . . . . .
O24 O 0.4758(5) 0.7034(6) 0.8347(4) 0.0365 1.0000 Uani . . . . . .
H131 H 0.1114 0.6598 0.7376 0.0560 1.0000 Uiso R . . . . .
H132 H 0.1744 0.7866 0.7441 0.0560 1.0000 Uiso R . . . . .
H133 H 0.0516 0.7718 0.6755 0.0559 1.0000 Uiso R . . . . .
H141 H 0.1254 0.4654 0.6851 0.0540 1.0000 Uiso R . . . . .
H142 H 0.1577 0.3844 0.6066 0.0539 1.0000 Uiso R . . . . .
H143 H 0.0390 0.4483 0.5836 0.0540 1.0000 Uiso R . . . . .
H151 H 0.2247 0.3904 0.4722 0.0510 1.0000 Uiso R . . . . .
H152 H 0.2750 0.4759 0.4070 0.0510 1.0000 Uiso R . . . . .
H153 H 0.1421 0.4577 0.3816 0.0511 1.0000 Uiso R . . . . .
H161 H 0.1915 0.9954 0.6479 0.0499 1.0000 Uiso R . . . . .
H162 H 0.2188 1.0843 0.5713 0.0499 1.0000 Uiso R . . . . .
H163 H 0.0968 1.0311 0.5549 0.0500 1.0000 Uiso R . . . . .
H171 H 0.2256 1.0936 0.4087 0.0580 1.0000 Uiso R . . . . .
H172 H 0.2496 1.0146 0.3253 0.0581 1.0000 Uiso R . . . . .
H173 H 0.1231 1.0283 0.3303 0.0581 1.0000 Uiso R . . . . .
H181 H 0.2974 0.6771 0.3112 0.0541 1.0000 Uiso R . . . . .
H182 H 0.2852 0.8162 0.2792 0.0540 1.0000 Uiso R . . . . .
H183 H 0.1748 0.7332 0.2596 0.0541 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       13(2)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.08690(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 . Ir2 . 2.9321(4) yes
Ir1 . C8 . 2.497(7) yes
Ir1 . C9 . 2.522(7) yes
Ir1 . C10 . 2.239(7) yes
Ir1 . C11 . 2.182(7) yes
Ir1 . C12 . 2.239(7) yes
Ir1 . C21 . 1.873(8) yes
Ir1 . C23 . 1.869(9) yes
Ir2 . C3 . 1.853(9) yes
Ir2 . C5 . 2.238(8) yes
Ir2 . C6 . 2.180(7) yes
Ir2 . C7 . 2.237(7) yes
Ir2 . C8 . 2.541(7) yes
Ir2 . C9 . 2.532(7) yes
Ir2 . C19 . 1.872(9) yes
C3 . O4 . 1.150(10) yes
C5 . C6 . 1.457(11) yes
C5 . C9 . 1.449(11) yes
C5 . C18 . 1.500(10) yes
C6 . C7 . 1.442(10) yes
C6 . C17 . 1.498(11) yes
C7 . C8 . 1.448(10) yes
C7 . C16 . 1.503(11) yes
C8 . C9 . 1.437(10) yes
C8 . C12 . 1.459(10) yes
C9 . C10 . 1.458(11) yes
C10 . C11 . 1.443(10) yes
C10 . C15 . 1.494(10) yes
C11 . C12 . 1.445(11) yes
C11 . C14 . 1.504(11) yes
C12 . C13 . 1.497(10) yes
C13 . H131 . 0.958 no
C13 . H132 . 0.950 no
C13 . H133 . 0.958 no
C14 . H141 . 0.955 no
C14 . H142 . 0.960 no
C14 . H143 . 0.948 no
C15 . H151 . 0.966 no
C15 . H152 . 0.964 no
C15 . H153 . 0.956 no
C16 . H161 . 0.953 no
C16 . H162 . 0.962 no
C16 . H163 . 0.951 no
C17 . H171 . 0.968 no
C17 . H172 . 0.959 no
C17 . H173 . 0.965 no
C18 . H181 . 0.968 no
C18 . H182 . 0.961 no
C18 . H183 . 0.968 no
C19 . O20 . 1.138(10) yes
C21 . O22 . 1.139(10) yes
C23 . O24 . 1.139(10) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ir2 . Ir1 . C8 . 55.11(16) yes
Ir2 . Ir1 . C9 . 54.70(17) yes
C8 . Ir1 . C9 . 33.3(2) yes
Ir2 . Ir1 . C10 . 87.94(19) yes
C8 . Ir1 . C10 . 59.0(3) yes
C9 . Ir1 . C10 . 35.0(3) yes
Ir2 . Ir1 . C11 . 110.7(2) yes
C8 . Ir1 . C11 . 59.3(3) yes
C9 . Ir1 . C11 . 58.9(3) yes
C10 . Ir1 . C11 . 38.1(3) yes
Ir2 . Ir1 . C12 . 89.11(19) yes
C8 . Ir1 . C12 . 35.4(2) yes
C9 . Ir1 . C12 . 58.8(2) yes
C10 . Ir1 . C12 . 63.3(3) yes
C11 . Ir1 . C12 . 38.1(3) yes
Ir2 . Ir1 . C21 . 100.7(2) yes
C8 . Ir1 . C21 . 146.2(3) yes
C9 . Ir1 . C21 . 115.0(3) yes
C10 . Ir1 . C21 . 101.4(3) yes
C11 . Ir1 . C21 . 123.7(3) yes
Ir2 . Ir1 . C23 . 97.4(2) yes
C8 . Ir1 . C23 . 113.5(3) yes
C9 . Ir1 . C23 . 143.6(3) yes
C10 . Ir1 . C23 . 165.5(3) yes
C11 . Ir1 . C23 . 127.9(3) yes
C12 . Ir1 . C21 . 161.8(3) yes
C12 . Ir1 . C23 . 103.2(3) yes
C21 . Ir1 . C23 . 90.9(3) yes
Ir1 . Ir2 . C3 . 100.5(2) yes
Ir1 . Ir2 . C5 . 87.7(2) yes
C3 . Ir2 . C5 . 163.3(3) yes
Ir1 . Ir2 . C6 . 109.2(2) yes
C3 . Ir2 . C6 . 124.9(3) yes
C5 . Ir2 . C6 . 38.5(3) yes
Ir1 . Ir2 . C7 . 86.4(2) yes
C3 . Ir2 . C7 . 102.4(3) yes
C5 . Ir2 . C7 . 63.4(3) yes
C6 . Ir2 . C7 . 38.1(3) yes
Ir1 . Ir2 . C8 . 53.71(16) yes
C3 . Ir2 . C8 . 115.5(3) yes
C5 . Ir2 . C8 . 58.2(3) yes
C6 . Ir2 . C8 . 58.3(3) yes
C7 . Ir2 . C8 . 34.6(3) yes
Ir1 . Ir2 . C9 . 54.38(16) yes
C3 . Ir2 . C9 . 146.1(3) yes
C5 . Ir2 . C9 . 34.7(3) yes
C6 . Ir2 . C9 . 58.7(3) yes
C7 . Ir2 . C9 . 58.4(3) yes
Ir1 . Ir2 . C19 . 101.7(2) yes
C3 . Ir2 . C19 . 90.7(4) yes
C5 . Ir2 . C19 . 101.9(3) yes
C6 . Ir2 . C19 . 125.3(3) yes
C7 . Ir2 . C19 . 163.2(3) yes
C8 . Ir2 . C9 . 32.9(2) yes
C8 . Ir2 . C19 . 145.4(3) yes
C9 . Ir2 . C19 . 114.6(3) yes
Ir2 . C3 . O4 . 178.0(8) yes
Ir2 . C5 . C6 . 68.6(4) yes
Ir2 . C5 . C9 . 83.8(4) yes
C6 . C5 . C9 . 106.6(7) yes
Ir2 . C5 . C18 . 126.1(5) yes
C6 . C5 . C18 . 124.9(7) yes
C9 . C5 . C18 . 126.2(7) yes
Ir2 . C6 . C5 . 72.9(4) yes
Ir2 . C6 . C7 . 73.1(4) yes
C5 . C6 . C7 . 108.4(7) yes
Ir2 . C6 . C17 . 125.9(6) yes
C5 . C6 . C17 . 125.6(7) yes
C7 . C6 . C17 . 125.6(7) yes
Ir2 . C7 . C6 . 68.8(4) yes
Ir2 . C7 . C8 . 84.3(4) yes
C6 . C7 . C8 . 106.9(7) yes
Ir2 . C7 . C16 . 125.7(5) yes
C6 . C7 . C16 . 124.3(7) yes
C8 . C7 . C16 . 126.5(7) yes
C7 . C8 . Ir1 . 128.0(5) yes
C7 . C8 . Ir2 . 61.2(4) yes
Ir1 . C8 . Ir2 . 71.18(18) yes
C7 . C8 . C9 . 108.5(6) yes
Ir1 . C8 . C9 . 74.3(4) yes
Ir2 . C8 . C9 . 73.2(4) yes
C7 . C8 . C12 . 143.1(7) yes
Ir1 . C8 . C12 . 62.6(4) yes
Ir2 . C8 . C12 . 130.5(5) yes
C9 . C8 . C12 . 108.5(6) yes
C5 . C9 . C8 . 108.3(7) yes
C5 . C9 . Ir1 . 129.2(5) yes
C8 . C9 . Ir1 . 72.4(4) yes
C5 . C9 . Ir2 . 61.5(4) yes
C8 . C9 . Ir2 . 73.9(4) yes
Ir1 . C9 . Ir2 . 70.92(18) yes
C5 . C9 . C10 . 143.7(7) yes
C8 . C9 . C10 . 108.0(6) yes
Ir1 . C9 . C10 . 61.8(4) yes
Ir2 . C9 . C10 . 128.6(5) yes
Ir1 . C10 . C9 . 83.1(4) yes
Ir1 . C10 . C11 . 68.8(4) yes
C9 . C10 . C11 . 107.0(6) yes
Ir1 . C10 . C15 . 125.4(5) yes
C9 . C10 . C15 . 125.9(7) yes
C11 . C10 . C15 . 125.3(7) yes
Ir1 . C11 . C10 . 73.1(4) yes
Ir1 . C11 . C12 . 73.1(4) yes
C10 . C11 . C12 . 108.9(6) yes
Ir1 . C11 . C14 . 124.6(5) yes
C10 . C11 . C14 . 125.4(7) yes
C12 . C11 . C14 . 125.4(7) yes
Ir1 . C12 . C8 . 82.0(4) yes
Ir1 . C12 . C11 . 68.8(4) yes
C8 . C12 . C11 . 106.7(6) yes
Ir1 . C12 . C13 . 126.5(5) yes
C8 . C12 . C13 . 125.3(7) yes
C11 . C12 . C13 . 126.3(7) yes
C12 . C13 . H131 . 109.9 no
C12 . C13 . H132 . 110.7 no
H131 . C13 . H132 . 110.2 no
C12 . C13 . H133 . 108.6 no
H131 . C13 . H133 . 108.8 no
H132 . C13 . H133 . 108.6 no
C11 . C14 . H141 . 109.7 no
C11 . C14 . H142 . 109.3 no
H141 . C14 . H142 . 109.9 no
C11 . C14 . H143 . 110.1 no
H141 . C14 . H143 . 108.5 no
H142 . C14 . H143 . 109.4 no
C10 . C15 . H151 . 108.8 no
C10 . C15 . H152 . 108.6 no
H151 . C15 . H152 . 108.4 no
C10 . C15 . H153 . 110.7 no
H151 . C15 . H153 . 110.1 no
H152 . C15 . H153 . 110.2 no
C7 . C16 . H161 . 110.3 no
C7 . C16 . H162 . 109.7 no
H161 . C16 . H162 . 110.1 no
C7 . C16 . H163 . 109.8 no
H161 . C16 . H163 . 108.2 no
H162 . C16 . H163 . 108.7 no
C6 . C17 . H171 . 108.4 no
C6 . C17 . H172 . 108.5 no
H171 . C17 . H172 . 109.0 no
C6 . C17 . H173 . 110.0 no
H171 . C17 . H173 . 110.5 no
H172 . C17 . H173 . 110.4 no
C5 . C18 . H181 . 108.4 no
C5 . C18 . H182 . 109.2 no
H181 . C18 . H182 . 108.8 no
C5 . C18 . H183 . 110.1 no
H181 . C18 . H183 . 110.3 no
H182 . C18 . H183 . 110.0 no
Ir2 . C19 . O20 . 177.7(7) yes
Ir1 . C21 . O22 . 177.7(7) yes
Ir1 . C23 . O24 . 178.2(7) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C15 . H152 . O22 2_666 163.2(2) 0.964 2.504 3.438(11) yes
C18 . H181 . O22 2_666 157.8(2) 0.968 2.509 3.425(11) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 10/08/15 at 15:18:28
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 10/08/15 at 15:18:28
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1417861'
_audit_update_record             
;
2015-08-10 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;
#================================================

_audit_creation_date             08-01-22
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title '1221031 Pn*Rh2(CO)3'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'
_cell_length_a                   10.5875(2)
_cell_length_b                   9.7143(2)
_cell_length_c                   15.3682(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.8887(7)
_cell_angle_gamma                90
_cell_volume                     1574.87(5)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062
5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C17 H18 O3 Rh2 
# Dc =      2.01 Fooo =    936.00 Mu =     21.04 M =    476.14
# Found Formula = C17 H18 O3 Rh2 
# Dc =      2.01 FOOO =    936.00 Mu =     21.04 M =    476.14

_chemical_formula_sum            'C17 H18 O3 Rh2'
_chemical_formula_moiety         'C17 H18 O3 Rh2'
_chemical_compound_source        SYN
_chemical_formula_weight         476.14


_cell_measurement_reflns_used    3797
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_max          0.04

_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    2.104

# Sheldrick geometric approximatio 0.92 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_T_max  0.96
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            31745
_reflns_number_total             7197
_diffrn_reflns_av_R_equivalents  0.023
# Number of reflections with Friedels Law is 7197 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 3616 


_diffrn_reflns_theta_min         5.251
_diffrn_reflns_theta_max         27.495
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        27.495
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   1.91
_oxford_diffrn_Wilson_scale      29.30

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.95
_refine_diff_density_max         0.95


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         3044
_refine_ls_number_restraints     0
_refine_ls_number_parameters     199
_oxford_refine_ls_R_factor_ref   0.0348
_refine_ls_wR_factor_ref         0.0823
_refine_ls_goodness_of_fit_ref   0.9857
_refine_ls_shift/su_max          0.001393


# The values computed from all data 
_oxford_reflns_number_all        3595
_refine_ls_R_factor_all          0.0414
_refine_ls_wR_factor_all         0.0866

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3131
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_gt          0.0839

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 4.88P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 0.6777(3) 0.6266(4) 0.4968(3) 0.0241 1.0000 Uani . . . . . . .
C2 C 0.6377(4) 0.6198(4) 0.5832(3) 0.0260 1.0000 Uani . . . . . . .
C3 C 0.6625(3) 0.4837(4) 0.6189(2) 0.0234 1.0000 Uani . . . . . . .
C4 C 0.7109(3) 0.4046(4) 0.5513(2) 0.0219 1.0000 Uani . . . . . . .
C5 C 1.2439(3) 0.7332(4) 0.4704(3) 0.0238 1.0000 Uani . . . . . . .
C6 C 1.2339(3) 0.7353(4) 0.5631(3) 0.0243 1.0000 Uani . . . . . . .
C7 C 1.2377(4) 0.5953(4) 0.5946(3) 0.0251 1.0000 Uani . . . . . . .
C8 C 0.7196(3) 0.4899(4) 0.4760(2) 0.0233 1.0000 Uani . . . . . . .
C9 C 0.6573(4) 0.7481(5) 0.4366(3) 0.0339 1.0000 Uani . . . . . . .
C10 C 0.5701(4) 0.7336(5) 0.6256(3) 0.0365 1.0000 Uani . . . . . . .
C11 C 0.6258(4) 0.4314(5) 0.7055(3) 0.0319 1.0000 Uani . . . . . . .
C12 C 1.2535(4) 0.8572(4) 0.4137(3) 0.0341 1.0000 Uani . . . . . . .
C13 C 1.2309(4) 0.8623(5) 0.6174(3) 0.0351 1.0000 Uani . . . . . . .
C14 C 1.2497(4) 0.5552(5) 0.6891(3) 0.0318 1.0000 Uani . . . . . . .
C15 C 0.9725(4) 0.6979(5) 0.4007(3) 0.0287 1.0000 Uani . . . . . . .
C16 C 0.9320(4) 0.5646(4) 0.7054(3) 0.0282 1.0000 Uani . . . . . . .
C17 C 0.9464(3) 0.7549(4) 0.5748(3) 0.0265 1.0000 Uani . . . . . . .
Rh1 Rh 1.06030(3) 0.64134(3) 0.505074(18) 0.0204 1.0000 Uani . . . . . . .
Rh2 Rh 0.84582(3) 0.58481(3) 0.596330(18) 0.0211 1.0000 Uani . . . . . . .
O3 O 0.9391(3) 0.8723(3) 0.5911(2) 0.0348 1.0000 Uani . . . . . . .
O4 O 0.9327(3) 0.7428(4) 0.3351(2) 0.0424 1.0000 Uani . . . . . . .
O5 O 0.9796(3) 0.5525(4) 0.77498(19) 0.0386 1.0000 Uani . . . . . . .
H91 H 0.6972 0.7318 0.3836 0.0502 1.0000 Uiso R . . . . . .
H92 H 0.6927 0.8294 0.4642 0.0501 1.0000 Uiso R . . . . . .
H93 H 0.5676 0.7616 0.4221 0.0502 1.0000 Uiso R . . . . . .
H101 H 0.5747 0.7201 0.6874 0.0540 1.0000 Uiso R . . . . . .
H102 H 0.6082 0.8207 0.6133 0.0540 1.0000 Uiso R . . . . . .
H103 H 0.4823 0.7349 0.6037 0.0542 1.0000 Uiso R . . . . . .
H111 H 0.6851 0.3628 0.7287 0.0471 1.0000 Uiso R . . . . . .
H112 H 0.6256 0.5065 0.7464 0.0471 1.0000 Uiso R . . . . . .
H113 H 0.5420 0.3920 0.6982 0.0472 1.0000 Uiso R . . . . . .
H121 H 1.2000 0.9289 0.4331 0.0493 1.0000 Uiso R . . . . . .
H122 H 1.3398 0.8890 0.4182 0.0491 1.0000 Uiso R . . . . . .
H123 H 1.2278 0.8348 0.3537 0.0491 1.0000 Uiso R . . . . . .
H131 H 1.1903 0.8429 0.6699 0.0511 1.0000 Uiso R . . . . . .
H132 H 1.3162 0.8944 0.6334 0.0510 1.0000 Uiso R . . . . . .
H133 H 1.1839 0.9328 0.5846 0.0509 1.0000 Uiso R . . . . . .
H141 H 1.2101 0.4679 0.6969 0.0459 1.0000 Uiso R . . . . . .
H142 H 1.3386 0.5487 0.7096 0.0460 1.0000 Uiso R . . . . . .
H143 H 1.2098 0.6234 0.7232 0.0459 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.18209(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.430(6) yes
C1 . C8 . 1.444(5) yes
C1 . C9 . 1.504(6) yes
C1 . Rh2 . 2.282(4) yes
C2 . C3 . 1.447(6) yes
C2 . C10 . 1.496(6) yes
C2 . Rh2 . 2.222(4) yes
C3 . C4 . 1.421(5) yes
C3 . C11 . 1.506(5) yes
C3 . Rh2 . 2.229(4) yes
C4 . C5 2_766 1.470(5) yes
C4 . Rh1 2_766 2.679(4) yes
C4 . C8 . 1.433(5) yes
C4 . Rh2 . 2.327(4) yes
C5 . C6 . 1.438(5) yes
C5 . C12 . 1.496(6) yes
C5 . Rh1 . 2.243(4) yes
C6 . C7 . 1.443(6) yes
C6 . C13 . 1.491(6) yes
C6 . Rh1 . 2.174(4) yes
C7 . C8 2_766 1.466(5) yes
C7 . C14 . 1.500(5) yes
C7 . Rh1 . 2.275(4) yes
C8 . Rh1 2_766 2.650(4) yes
C8 . Rh2 . 2.373(4) yes
C9 . H91 . 0.962 no
C9 . H92 . 0.958 no
C9 . H93 . 0.965 no
C10 . H101 . 0.956 no
C10 . H102 . 0.964 no
C10 . H103 . 0.962 no
C11 . H111 . 0.963 no
C11 . H112 . 0.963 no
C11 . H113 . 0.964 no
C12 . H121 . 0.961 no
C12 . H122 . 0.962 no
C12 . H123 . 0.964 no
C13 . H131 . 0.964 no
C13 . H132 . 0.967 no
C13 . H133 . 0.964 no
C14 . H141 . 0.958 no
C14 . H142 . 0.968 no
C14 . H143 . 0.965 no
C15 . Rh1 . 1.867(4) yes
C15 . O4 . 1.145(5) yes
C16 . Rh2 . 1.849(4) yes
C16 . O5 . 1.148(5) yes
C17 . Rh1 . 2.010(4) yes
C17 . Rh2 . 2.008(4) yes
C17 . O3 . 1.172(5) yes
Rh1 . Rh1 2_766 3.0268(6) yes
Rh1 . Rh2 2_766 2.9166(4) yes
Rh1 . Rh2 . 2.8228(4) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C8 . 106.5(3) yes
C2 . C1 . C9 . 124.7(4) yes
C8 . C1 . C9 . 128.1(4) yes
C2 . C1 . Rh2 . 69.2(2) yes
C8 . C1 . Rh2 . 75.4(2) yes
C9 . C1 . Rh2 . 127.9(3) yes
C1 . C2 . C3 . 109.5(3) yes
C1 . C2 . C10 . 124.2(4) yes
C3 . C2 . C10 . 126.1(4) yes
C1 . C2 . Rh2 . 73.8(2) yes
C3 . C2 . Rh2 . 71.3(2) yes
C10 . C2 . Rh2 . 125.5(3) yes
C2 . C3 . C4 . 106.4(3) yes
C2 . C3 . C11 . 126.2(4) yes
C4 . C3 . C11 . 126.8(4) yes
C2 . C3 . Rh2 . 70.8(2) yes
C4 . C3 . Rh2 . 75.6(2) yes
C11 . C3 . Rh2 . 125.4(3) yes
C5 2_766 C4 . C3 . 143.4(4) yes
C5 2_766 C4 . Rh1 2_766 56.87(18) yes
C3 . C4 . Rh1 2_766 135.9(3) yes
C5 2_766 C4 . C8 . 107.3(3) yes
C3 . C4 . C8 . 109.2(3) yes
Rh1 2_766 C4 . C8 . 73.3(2) yes
C5 2_766 C4 . Rh2 . 123.3(2) yes
C3 . C4 . Rh2 . 68.1(2) yes
Rh1 2_766 C4 . Rh2 . 70.88(9) yes
C8 . C4 . Rh2 . 74.0(2) yes
C4 2_766 C5 . C6 . 107.0(3) yes
C4 2_766 C5 . C12 . 124.1(3) yes
C6 . C5 . C12 . 125.5(4) yes
C4 2_766 C5 . Rh1 . 89.9(2) yes
C6 . C5 . Rh1 . 68.4(2) yes
C12 . C5 . Rh1 . 124.2(3) yes
C5 . C6 . C7 . 108.4(3) yes
C5 . C6 . C13 . 125.0(4) yes
C7 . C6 . C13 . 126.4(4) yes
C5 . C6 . Rh1 . 73.6(2) yes
C7 . C6 . Rh1 . 74.9(2) yes
C13 . C6 . Rh1 . 121.3(3) yes
C8 2_766 C7 . C6 . 106.6(3) yes
C8 2_766 C7 . C14 . 124.4(4) yes
C6 . C7 . C14 . 124.5(4) yes
C8 2_766 C7 . Rh1 . 87.4(2) yes
C6 . C7 . Rh1 . 67.3(2) yes
C14 . C7 . Rh1 . 129.4(3) yes
C7 2_766 C8 . C1 . 143.3(4) yes
C7 2_766 C8 . C4 . 108.5(3) yes
C1 . C8 . C4 . 108.1(3) yes
C7 2_766 C8 . Rh1 2_766 59.1(2) yes
C1 . C8 . Rh1 2_766 134.6(3) yes
C4 . C8 . Rh1 2_766 75.5(2) yes
C7 2_766 C8 . Rh2 . 127.4(3) yes
C1 . C8 . Rh2 . 68.5(2) yes
C4 . C8 . Rh2 . 70.5(2) yes
Rh1 2_766 C8 . Rh2 . 70.74(10) yes
C1 . C9 . H91 . 110.0 no
C1 . C9 . H92 . 110.2 no
H91 . C9 . H92 . 109.0 no
C1 . C9 . H93 . 109.6 no
H91 . C9 . H93 . 108.7 no
H92 . C9 . H93 . 109.3 no
C2 . C10 . H101 . 110.3 no
C2 . C10 . H102 . 109.9 no
H101 . C10 . H102 . 109.2 no
C2 . C10 . H103 . 109.9 no
H101 . C10 . H103 . 108.4 no
H102 . C10 . H103 . 109.1 no
C3 . C11 . H111 . 110.6 no
C3 . C11 . H112 . 109.7 no
H111 . C11 . H112 . 108.6 no
C3 . C11 . H113 . 109.6 no
H111 . C11 . H113 . 109.4 no
H112 . C11 . H113 . 108.9 no
C5 . C12 . H121 . 109.4 no
C5 . C12 . H122 . 109.1 no
H121 . C12 . H122 . 109.0 no
C5 . C12 . H123 . 110.4 no
H121 . C12 . H123 . 109.6 no
H122 . C12 . H123 . 109.3 no
C6 . C13 . H131 . 109.8 no
C6 . C13 . H132 . 110.1 no
H131 . C13 . H132 . 108.9 no
C6 . C13 . H133 . 109.2 no
H131 . C13 . H133 . 109.3 no
H132 . C13 . H133 . 109.4 no
C7 . C14 . H141 . 110.4 no
C7 . C14 . H142 . 109.4 no
H141 . C14 . H142 . 109.0 no
C7 . C14 . H143 . 110.1 no
H141 . C14 . H143 . 108.8 no
H142 . C14 . H143 . 109.1 no
Rh1 . C15 . O4 . 170.9(4) yes
Rh2 . C16 . O5 . 176.4(3) yes
Rh1 . C17 . Rh2 . 89.25(17) yes
Rh1 . C17 . O3 . 134.6(3) yes
Rh2 . C17 . O3 . 136.0(3) yes
C7 . Rh1 . Rh1 2_766 100.11(10) yes
C7 . Rh1 . C5 . 62.27(14) yes
Rh1 2_766 Rh1 . C5 . 135.95(10) yes
C7 . Rh1 . C6 . 37.75(15) yes
Rh1 2_766 Rh1 . C6 . 137.74(11) yes
C5 . Rh1 . C6 . 37.95(14) yes
C7 . Rh1 . Rh2 2_766 82.74(10) yes
Rh1 2_766 Rh1 . Rh2 2_766 56.674(11) yes
C5 . Rh1 . Rh2 2_766 80.28(10) yes
C6 . Rh1 . Rh2 2_766 102.76(10) yes
C7 . Rh1 . C17 . 106.70(15) yes
Rh1 2_766 Rh1 . C17 . 104.82(12) yes
C5 . Rh1 . C17 . 118.66(16) yes
C6 . Rh1 . C17 . 94.32(15) yes
Rh2 2_766 Rh1 . C17 . 161.00(12) yes
C7 . Rh1 . C8 2_766 33.55(13) yes
Rh1 2_766 Rh1 . C8 2_766 86.13(8) yes
C5 . Rh1 . C8 2_766 56.35(13) yes
C6 . Rh1 . C8 2_766 56.80(13) yes
Rh2 2_766 Rh1 . C8 2_766 50.19(8) yes
C7 . Rh1 . C4 2_766 55.98(13) yes
Rh1 2_766 Rh1 . C4 2_766 102.78(8) yes
C5 . Rh1 . C4 2_766 33.27(12) yes
C6 . Rh1 . C4 2_766 56.41(13) yes
Rh2 2_766 Rh1 . C4 2_766 48.92(8) yes
C7 . Rh1 . C15 . 154.41(15) yes
Rh1 2_766 Rh1 . C15 . 92.63(13) yes
C5 . Rh1 . C15 . 93.25(15) yes
C6 . Rh1 . C15 . 124.78(16) yes
Rh2 2_766 Rh1 . C15 . 85.98(13) yes
C7 . Rh1 . Rh2 . 108.59(10) yes
Rh1 2_766 Rh1 . Rh2 . 59.694(11) yes
C5 . Rh1 . Rh2 . 160.94(10) yes
C6 . Rh1 . Rh2 . 124.43(10) yes
Rh2 2_766 Rh1 . Rh2 . 116.368(12) yes
C17 . Rh1 . C8 2_766 140.13(14) yes
C17 . Rh1 . C4 2_766 149.79(14) yes
C8 2_766 Rh1 . C4 2_766 31.18(11) yes
C17 . Rh1 . C15 . 91.11(17) yes
C8 2_766 Rh1 . C15 . 127.18(14) yes
C4 2_766 Rh1 . C15 . 99.70(14) yes
C17 . Rh1 . Rh2 . 45.35(12) yes
C8 2_766 Rh1 . Rh2 . 126.09(8) yes
C4 2_766 Rh1 . Rh2 . 156.39(8) yes
C15 . Rh1 . Rh2 . 96.99(11) yes
C4 . Rh2 . C1 . 60.70(13) yes
C4 . Rh2 . C8 . 35.47(13) yes
C1 . Rh2 . C8 . 36.08(13) yes
C4 . Rh2 . C3 . 36.27(13) yes
C1 . Rh2 . C3 . 62.79(14) yes
C8 . Rh2 . C3 . 60.64(13) yes
C4 . Rh2 . C2 . 60.61(14) yes
C1 . Rh2 . C2 . 36.99(15) yes
C8 . Rh2 . C2 . 60.05(14) yes
C3 . Rh2 . C2 . 37.95(14) yes
C4 . Rh2 . Rh1 2_766 60.21(9) yes
C1 . Rh2 . Rh1 2_766 93.30(10) yes
C8 . Rh2 . Rh1 2_766 59.07(9) yes
C3 . Rh2 . Rh1 2_766 95.27(10) yes
C2 . Rh2 . Rh1 2_766 116.58(11) yes
C4 . Rh2 . Rh1 . 119.88(9) yes
C1 . Rh2 . Rh1 . 104.29(10) yes
C8 . Rh2 . Rh1 . 96.43(9) yes
C3 . Rh2 . Rh1 . 155.66(10) yes
C2 . Rh2 . Rh1 . 139.37(11) yes
C4 . Rh2 . C17 . 152.96(15) yes
C1 . Rh2 . C17 . 97.91(15) yes
C8 . Rh2 . C17 . 117.55(14) yes
C3 . Rh2 . C17 . 150.38(15) yes
C2 . Rh2 . C17 . 113.25(15) yes
C4 . Rh2 . C16 . 115.63(16) yes
C1 . Rh2 . C16 . 157.34(15) yes
C8 . Rh2 . C16 . 150.04(16) yes
C3 . Rh2 . C16 . 100.45(15) yes
C2 . Rh2 . C16 . 120.48(16) yes
Rh1 2_766 Rh2 . Rh1 . 63.632(12) yes
Rh1 2_766 Rh2 . C17 . 108.78(11) yes
Rh1 . Rh2 . C17 . 45.39(11) yes
Rh1 2_766 Rh2 . C16 . 103.89(13) yes
Rh1 . Rh2 . C16 . 96.61(12) yes
C17 . Rh2 . C16 . 90.51(17) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C12 . H121 . O3 2_776 153 0.96 2.44 3.322(6) yes
C14 . H141 . O4 2_766 160 0.96 2.57 3.482(6) yes

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
