#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/11/4081157.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_4081157
loop_
_publ_author_name
'Huang, Da-wei'
'Lo, Ying-Hao'
'Liu, Yi-Hung'
'Peng, Shie-Ming'
'Liu, Shiuh-Tzung'
_publ_section_title
;
 Cyclometalation of Anthyridine-Based Ligands with Dirhodium Acetates:
 Structure and Catalytic Activity
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              4009
_journal_paper_doi               10.1021/om400508a
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C34.5 H28.5 Cl6 N3 O6 Rh2 S2'
_chemical_formula_weight         1063.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.515(2)
_cell_angle_beta                 98.669(2)
_cell_angle_gamma                115.686(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4138(3)
_cell_length_b                   12.6953(3)
_cell_length_c                   15.1813(4)
_cell_measurement_reflns_used    4989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3336
_cell_measurement_theta_min      2.9589
_cell_volume                     2058.81(10)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A'
_diffrn_measurement_method       CCD
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18406
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1057
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.185
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9329
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1838
_reflns_number_gt                6461
_reflns_number_total             9329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400508a_si_002.cif
_cod_data_source_block           ic15235
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2058.81(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34.50 H28.50 Cl6 N3 O6 Rh2 S2'
_cod_database_code               4081157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Rh1 Rh 1.38540(4) 0.58027(4) 0.78650(3) 0.02067(14) Uani 1 1 d .
Rh2 Rh 1.26296(4) 0.42621(4) 0.64187(3) 0.02078(14) Uani 1 1 d .
S1 S 1.67982(15) 0.72652(15) 1.05034(11) 0.0319(4) Uani 1 1 d .
S2 S 1.03577(17) 0.15553(16) 0.38526(14) 0.0424(5) Uani 1 1 d .
O1 O 1.2493(4) 0.4884(4) 0.8472(3) 0.0245(9) Uani 1 1 d .
O2 O 1.1318(4) 0.3493(4) 0.7116(3) 0.0265(9) Uani 1 1 d .
O3 O 1.2887(4) 0.6716(4) 0.7505(3) 0.0270(9) Uani 1 1 d .
O4 O 1.1845(4) 0.5335(4) 0.6119(3) 0.0264(9) Uani 1 1 d .
O5 O 1.5123(4) 0.6646(4) 0.7173(3) 0.0255(9) Uani 1 1 d .
O6 O 1.3997(4) 0.5184(4) 0.5828(3) 0.0273(9) Uani 1 1 d .
N2 N 1.3502(4) 0.3332(4) 0.6791(3) 0.0196(10) Uani 1 1 d .
N1 N 1.4706(4) 0.4816(4) 0.8135(3) 0.0197(10) Uani 1 1 d .
N3 N 1.2223(4) 0.1905(4) 0.5466(3) 0.0217(10) Uani 1 1 d .
C1 C 1.1530(6) 0.3952(5) 0.7966(4) 0.0240(13) Uani 1 1 d .
C2 C 1.0530(6) 0.3347(6) 0.8441(5) 0.0399(17) Uani 1 1 d .
H2A H 0.9833 0.2642 0.7995 0.060 Uiso 1 1 calc R
H2B H 1.0252 0.3920 0.8693 0.060 Uiso 1 1 calc R
H2C H 1.0856 0.3086 0.8943 0.060 Uiso 1 1 calc R
C3 C 1.2132(6) 0.6307(6) 0.6721(5) 0.0267(13) Uani 1 1 d .
C4 C 1.1537(7) 0.7059(7) 0.6460(5) 0.0395(17) Uani 1 1 d .
H4A H 1.0977 0.6657 0.5842 0.059 Uiso 1 1 calc R
H4B H 1.2176 0.7858 0.6461 0.059 Uiso 1 1 calc R
H4C H 1.1069 0.7151 0.6906 0.059 Uiso 1 1 calc R
C5 C 1.4939(6) 0.6169(6) 0.6320(4) 0.0264(13) Uani 1 1 d .
C6 C 1.5937(6) 0.6814(6) 0.5864(5) 0.0355(16) Uani 1 1 d .
H6A H 1.6597 0.7546 0.6312 0.053 Uiso 1 1 calc R
H6B H 1.5594 0.7036 0.5345 0.053 Uiso 1 1 calc R
H6C H 1.6273 0.6280 0.5639 0.053 Uiso 1 1 calc R
C7 C 1.5038(5) 0.6928(5) 0.9118(4) 0.0231(13) Uani 1 1 d .
C8 C 1.5372(6) 0.8036(6) 0.9740(4) 0.0294(14) Uani 1 1 d .
H8A H 1.5003 0.8537 0.9638 0.035 Uiso 1 1 calc R
C9 C 1.6282(7) 0.8321(6) 1.0510(5) 0.0358(16) Uani 1 1 d .
H9A H 1.6595 0.9031 1.0999 0.043 Uiso 1 1 calc R
C10 C 1.5747(5) 0.6406(5) 0.9445(4) 0.0247(13) Uani 1 1 d .
C11 C 1.5575(5) 0.5277(5) 0.8937(4) 0.0226(12) Uani 1 1 d .
C12 C 1.6208(6) 0.4631(6) 0.9207(4) 0.0274(14) Uani 1 1 d .
H12A H 1.6818 0.4959 0.9776 0.033 Uiso 1 1 calc R
C13 C 1.5943(6) 0.3548(5) 0.8653(4) 0.0272(13) Uani 1 1 d .
H13A H 1.6372 0.3122 0.8829 0.033 Uiso 1 1 calc R
C14 C 1.5012(5) 0.3056(5) 0.7803(4) 0.0216(12) Uani 1 1 d .
C15 C 1.4406(5) 0.3734(5) 0.7568(4) 0.0207(12) Uani 1 1 d .
C16 C 1.4700(5) 0.1941(5) 0.7199(4) 0.0234(13) Uani 1 1 d .
C17 C 1.3726(5) 0.1520(5) 0.6400(4) 0.0216(12) Uani 1 1 d .
C18 C 1.3162(5) 0.2226(5) 0.6219(4) 0.0228(12) Uani 1 1 d .
C19 C 1.3281(6) 0.0389(6) 0.5725(4) 0.0302(14) Uani 1 1 d .
H19A H 1.3646 -0.0122 0.5797 0.036 Uiso 1 1 calc R
C20 C 1.2338(6) 0.0061(6) 0.4989(4) 0.0297(14) Uani 1 1 d .
H20A H 1.2028 -0.0691 0.4546 0.036 Uiso 1 1 calc R
C21 C 1.1811(5) 0.0833(5) 0.4876(4) 0.0242(13) Uani 1 1 d .
C22 C 1.0802(6) 0.0495(5) 0.4089(4) 0.0243(13) Uani 1 1 d .
C23 C 1.0060(6) -0.0603(6) 0.3471(5) 0.0333(15) Uani 1 1 d .
H23A H 1.0147 -0.1306 0.3494 0.040 Uiso 1 1 calc R
C24 C 0.9156(6) -0.0594(6) 0.2797(5) 0.0390(17) Uani 1 1 d .
H24A H 0.8567 -0.1282 0.2318 0.047 Uiso 1 1 calc R
C25 C 0.9228(7) 0.0513(7) 0.2914(5) 0.0447(19) Uani 1 1 d .
H25A H 0.8703 0.0695 0.2515 0.054 Uiso 1 1 calc R
C26 C 1.5329(6) 0.1202(5) 0.7400(4) 0.0251(13) Uani 1 1 d .
C27 C 1.6540(6) 0.1587(6) 0.7386(5) 0.0352(16) Uani 1 1 d .
H27A H 1.7008 0.2356 0.7281 0.042 Uiso 1 1 calc R
C28 C 1.7080(7) 0.0866(7) 0.7524(6) 0.0432(18) Uani 1 1 d .
H28A H 1.7915 0.1128 0.7500 0.052 Uiso 1 1 calc R
C29 C 1.6406(7) -0.0247(7) 0.7698(5) 0.046(2) Uani 1 1 d .
H29A H 1.6784 -0.0741 0.7800 0.055 Uiso 1 1 calc R
C30 C 1.5215(7) -0.0626(6) 0.7724(5) 0.0399(17) Uani 1 1 d .
H30A H 1.4757 -0.1391 0.7838 0.048 Uiso 1 1 calc R
C31 C 1.4661(6) 0.0081(6) 0.7587(5) 0.0315(15) Uani 1 1 d .
H31A H 1.3828 -0.0186 0.7618 0.038 Uiso 1 1 calc R
Cl1 Cl 1.36679(18) -0.24527(19) 0.48424(16) 0.0542(5) Uani 1 1 d .
Cl2 Cl 1.2799(2) -0.4653(2) 0.34141(16) 0.0642(6) Uani 1 1 d .
Cl3 Cl 1.11090(19) -0.3768(2) 0.38519(16) 0.0627(6) Uani 1 1 d .
C32 C 1.2427(7) -0.3886(8) 0.4291(5) 0.049(2) Uani 1 1 d .
H32A H 1.2245 -0.4366 0.4759 0.058 Uiso 1 1 calc R
Cl4 Cl -0.2420(3) -0.8524(2) 0.0710(3) 0.0944(10) Uani 1 1 d .
Cl5 Cl -0.1485(2) -0.6594(4) -0.01880(17) 0.0935(11) Uani 1 1 d .
Cl6 Cl -0.0278(2) -0.6230(2) 0.16478(17) 0.0715(7) Uani 1 1 d .
C33 C -0.1725(7) -0.6968(7) 0.0833(5) 0.0437(18) Uani 1 1 d .
H33A H -0.2273 -0.6652 0.1057 0.052 Uiso 1 1 calc R
C34 C 1.8275(14) 0.7818(18) 0.8375(12) 0.053(4) Uani 0.50 1 d PU
H34A H 1.7503 0.7713 0.7999 0.079 Uiso 0.50 1 calc PR
H34B H 1.8096 0.7158 0.8679 0.079 Uiso 0.50 1 calc PR
H34C H 1.8827 0.7807 0.7980 0.079 Uiso 0.50 1 calc PR
C35 C 1.8757(19) 0.876(3) 0.8942(15) 0.094(7) Uani 0.50 1 d PU
H35A H 1.8068 0.8676 0.9227 0.112 Uiso 0.50 1 calc PR
H35B H 1.8785 0.9309 0.8545 0.112 Uiso 0.50 1 calc PR
C36 C 1.9729(17) 0.952(2) 0.9658(14) 0.095(6) Uani 0.50 1 d PU
H36B H 1.9789 0.8929 0.9983 0.114 Uiso 0.50 1 calc PR
H36D H 2.0396 0.9709 0.9330 0.114 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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
N1 Rh1 O5 89.44(17) .
N1 Rh1 O1 91.45(18) .
O5 Rh1 O1 175.97(16) .
N1 Rh1 C7 81.8(2) .
O5 Rh1 C7 91.6(2) .
O1 Rh1 C7 92.42(19) .
N1 Rh1 O3 175.84(18) .
O5 Rh1 O3 90.98(16) .
O1 Rh1 O3 87.85(17) .
C7 Rh1 O3 102.3(2) .
N1 Rh1 Rh2 88.40(14) .
O5 Rh1 Rh2 87.84(12) .
O1 Rh1 Rh2 88.26(12) .
C7 Rh1 Rh2 170.23(18) .
O3 Rh1 Rh2 87.47(12) .
N2 Rh2 O6 90.20(18) .
N2 Rh2 O2 91.69(17) .
O6 Rh2 O2 174.20(16) .
N2 Rh2 O4 175.34(18) .
O6 Rh2 O4 88.42(17) .
O2 Rh2 O4 89.26(17) .
N2 Rh2 Rh1 87.69(14) .
O6 Rh2 Rh1 87.71(12) .
O2 Rh2 Rh1 86.88(12) .
O4 Rh2 Rh1 87.80(12) .
C9 S1 C10 89.7(3) .
C25 S2 C22 91.0(3) .
C1 O1 Rh1 118.1(4) .
C1 O2 Rh2 119.4(4) .
C3 O3 Rh1 118.7(4) .
C3 O4 Rh2 119.0(4) .
C5 O5 Rh1 119.2(4) .
C5 O6 Rh2 119.2(4) .
C15 N2 C18 118.1(5) .
C15 N2 Rh2 123.9(4) .
C18 N2 Rh2 118.0(4) .
C11 N1 C15 121.4(5) .
C11 N1 Rh1 115.7(4) .
C15 N1 Rh1 122.8(4) .
C21 N3 C18 117.3(5) .
O2 C1 O1 127.3(6) .
O2 C1 C2 117.0(6) .
O1 C1 C2 115.7(5) .
O3 C3 O4 126.7(6) .
O3 C3 C4 116.7(6) .
O4 C3 C4 116.6(6) .
O5 C5 O6 126.0(5) .
O5 C5 C6 116.3(6) .
O6 C5 C6 117.7(6) .
C10 C7 C8 110.4(5) .
C10 C7 Rh1 108.2(4) .
C8 C7 Rh1 141.4(5) .
C9 C8 C7 113.4(6) .
C8 C9 S1 113.3(5) .
C7 C10 C11 120.9(6) .
C7 C10 S1 113.2(5) .
C11 C10 S1 125.8(5) .
N1 C11 C10 113.3(5) .
N1 C11 C12 120.2(5) .
C10 C11 C12 126.4(6) .
C13 C12 C11 120.2(6) .
C12 C13 C14 119.5(6) .
C16 C14 C15 119.9(5) .
C16 C14 C13 122.1(5) .
C15 C14 C13 118.0(5) .
N2 C15 N1 117.1(5) .
N2 C15 C14 122.2(5) .
N1 C15 C14 120.7(5) .
C14 C16 C17 117.0(5) .
C14 C16 C26 122.2(5) .
C17 C16 C26 120.8(5) .
C18 C17 C16 120.0(5) .
C18 C17 C19 116.2(5) .
C16 C17 C19 123.8(5) .
N3 C18 N2 112.8(5) .
N3 C18 C17 124.5(5) .
N2 C18 C17 122.8(5) .
C20 C19 C17 119.4(6) .
C19 C20 C21 120.1(6) .
N3 C21 C20 122.5(6) .
N3 C21 C22 116.8(5) .
C20 C21 C22 120.7(5) .
C23 C22 C21 129.6(6) .
C23 C22 S2 110.5(5) .
C21 C22 S2 119.8(4) .
C22 C23 C24 113.7(6) .
C25 C24 C23 111.6(6) .
C24 C25 S2 113.2(6) .
C27 C26 C31 119.3(6) .
C27 C26 C16 121.1(5) .
C31 C26 C16 119.6(6) .
C26 C27 C28 120.1(6) .
C27 C28 C29 120.1(7) .
C30 C29 C28 120.0(6) .
C29 C30 C31 120.7(7) .
C30 C31 C26 119.7(6) .
Cl1 C32 Cl3 110.5(5) .
Cl1 C32 Cl2 111.1(4) .
Cl3 C32 Cl2 110.8(4) .
Cl5 C33 Cl4 112.6(5) .
Cl5 C33 Cl6 107.6(4) .
Cl4 C33 Cl6 110.9(4) .
C34 C35 C36 147(3) .
C36 C36 C35 151(4) 2_977
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 2.011(5) .
Rh1 O5 2.035(4) .
Rh1 O1 2.045(4) .
Rh1 C7 2.064(6) .
Rh1 O3 2.074(4) .
Rh1 Rh2 2.4399(6) .
Rh2 N2 2.008(5) .
Rh2 O6 2.035(4) .
Rh2 O2 2.051(4) .
Rh2 O4 2.058(4) .
S1 C9 1.717(7) .
S1 C10 1.740(6) .
S2 C25 1.707(7) .
S2 C22 1.729(6) .
O1 C1 1.271(7) .
O2 C1 1.260(7) .
O3 C3 1.266(7) .
O4 C3 1.278(8) .
O5 C5 1.277(7) .
O6 C5 1.284(7) .
N2 C15 1.348(7) .
N2 C18 1.370(7) .
N1 C11 1.346(7) .
N1 C15 1.354(7) .
N3 C21 1.331(7) .
N3 C18 1.365(7) .
C1 C2 1.509(8) .
C3 C4 1.505(9) .
C5 C6 1.499(8) .
C7 C10 1.394(8) .
C7 C8 1.407(9) .
C8 C9 1.371(9) .
C10 C11 1.419(8) .
C11 C12 1.425(8) .
C12 C13 1.360(8) .
C13 C14 1.432(8) .
C14 C16 1.408(8) .
C14 C15 1.420(8) .
C16 C17 1.414(8) .
C16 C26 1.498(8) .
C17 C18 1.392(8) .
C17 C19 1.439(8) .
C19 C20 1.350(9) .
C20 C21 1.413(8) .
C21 C22 1.447(8) .
C22 C23 1.366(9) .
C23 C24 1.405(9) .
C24 C25 1.349(10) .
C26 C27 1.369(9) .
C26 C31 1.405(8) .
C27 C28 1.372(9) .
C28 C29 1.390(10) .
C29 C30 1.352(10) .
C30 C31 1.369(9) .
Cl1 C32 1.749(8) .
Cl2 C32 1.755(9) .
Cl3 C32 1.750(8) .
Cl4 C33 1.741(8) .
Cl5 C33 1.725(8) .
Cl6 C33 1.767(8) .
C34 C35 1.19(3) .
C35 C36 1.35(3) .
C36 C36 1.29(4) 2_977
