#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:52:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179132 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/94/4309433.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_4309433
loop_
_publ_author_name
'Jahar lal Pratihar'
'Nilkamal Maiti'
'Surajit Chattopadhyay'
_publ_section_title
;
Reactions of 2-(Arylazo) Aniline with RhCl3: Synthesis and Structure of
New Cyclometalated Complexes of Rh(III) and Recognition of RhCl3 Assisted
Azo (NN) Cleavage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6111
_journal_page_last               6114
_journal_paper_doi               10.1021/ic050551w
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C36 H34 Cl4 N8 O Rh2'
_chemical_formula_weight         942.33
_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                91.21(2)
_cell_angle_beta                 98.51(2)
_cell_angle_gamma                101.85(3)
_cell_formula_units_Z            2
_cell_length_a                   12.251(12)
_cell_length_b                   12.438(12)
_cell_length_c                   13.836(13)
_cell_measurement_temperature    273(2)
_cell_volume                     2038(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.809
_diffrn_measured_fraction_theta_max 0.809
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15326
_diffrn_reflns_theta_full        28.63
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  0.8691
_exptl_absorpt_correction_T_min  0.6972
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0396
_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)+(0.0433P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                5764
_reflns_number_total             8466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050551wsi20050409_021713.cif
_cod_data_source_block           scjp13m
_cod_database_code               4309433
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.25477(3) 0.52663(2) 0.059007(18) 0.03178(10) Uani 1 1 d . . .
Rh2 Rh 0.24888(3) 0.86820(2) 0.559468(18) 0.03375(10) Uani 1 1 d . . .
Cl1 Cl 0.39120(11) 0.41869(9) 0.09619(7) 0.0512(3) Uani 1 1 d . . .
Cl2 Cl 0.11743(10) 0.63339(7) 0.01591(7) 0.0431(3) Uani 1 1 d . . .
Cl3 Cl 0.10900(11) 0.70427(7) 0.51589(7) 0.0477(3) Uani 1 1 d . . .
Cl4 Cl 0.38419(12) 1.03543(8) 0.59592(7) 0.0548(3) Uani 1 1 d . . .
C2 C 0.1870(4) 0.4734(3) 0.1779(2) 0.0340(9) Uani 1 1 d . . .
N1 N 0.3214(3) 0.6447(2) 0.2434(2) 0.0403(9) Uani 1 1 d . . .
N2 N 0.3401(3) 0.6440(2) 0.15409(19) 0.0341(8) Uani 1 1 d . . .
N3 N 0.3655(3) 0.6258(2) -0.03802(19) 0.0369(8) Uani 1 1 d . . .
H4A H 0.4120 0.5860 -0.0588 0.044 Uiso 1 1 calc R . .
H4B H 0.3230 0.6457 -0.0906 0.044 Uiso 1 1 calc R . .
N4 N 0.1578(3) 0.3966(2) -0.0417(2) 0.0417(9) Uani 1 1 d . . .
H5A H 0.1688 0.3319 -0.0187 0.050 Uiso 1 1 calc R . .
H5B H 0.0841 0.3972 -0.0443 0.050 Uiso 1 1 calc R . .
C20 C 0.1785(4) 0.8923(3) 0.6783(2) 0.0375(10) Uani 1 1 d . . .
N5 N 0.3159(3) 0.7823(2) 0.7429(2) 0.0407(8) Uani 1 1 d . . .
N6 N 0.3355(3) 0.7896(2) 0.65447(19) 0.0355(8) Uani 1 1 d . . .
N7 N 0.3655(3) 0.8181(2) 0.4630(2) 0.0397(8) Uani 1 1 d . . .
H9A H 0.3255 0.7793 0.4091 0.048 Uiso 1 1 calc R . .
H9B H 0.4111 0.8779 0.4445 0.048 Uiso 1 1 calc R . .
N8 N 0.1509(3) 0.9524(2) 0.4587(2) 0.0447(9) Uani 1 1 d . . .
H10A H 0.0777 0.9191 0.4542 0.054 Uiso 1 1 calc R . .
H10B H 0.1584 1.0217 0.4829 0.054 Uiso 1 1 calc R . .
C3 C 0.1100(4) 0.3788(3) 0.1958(3) 0.0437(11) Uani 1 1 d . . .
H1 H 0.0774 0.3269 0.1448 0.052 Uiso 1 1 calc R . .
C4 C 0.0812(4) 0.3612(3) 0.2895(3) 0.0509(12) Uani 1 1 d . . .
H2 H 0.0299 0.2979 0.3002 0.061 Uiso 1 1 calc R . .
C5 C 0.1294(4) 0.4386(3) 0.3669(3) 0.0536(13) Uani 1 1 d . . .
H3 H 0.1096 0.4268 0.4288 0.064 Uiso 1 1 calc R . .
C6 C 0.2070(4) 0.5331(3) 0.3518(3) 0.0452(11) Uani 1 1 d . . .
H4 H 0.2386 0.5848 0.4032 0.054 Uiso 1 1 calc R . .
C1 C 0.2372(4) 0.5499(3) 0.2582(2) 0.0347(9) Uani 1 1 d . . .
C7 C 0.4201(4) 0.7312(3) 0.1212(3) 0.0393(10) Uani 1 1 d . . .
C8 C 0.4847(4) 0.8209(3) 0.1817(3) 0.0505(12) Uani 1 1 d . . .
H7 H 0.4765 0.8268 0.2473 0.061 Uiso 1 1 calc R . .
C9 C 0.5621(5) 0.9023(4) 0.1425(3) 0.0672(16) Uani 1 1 d . . .
H8 H 0.6070 0.9603 0.1830 0.081 Uiso 1 1 calc R . .
C10 C 0.5714(5) 0.8961(3) 0.0440(3) 0.0651(16) Uani 1 1 d . . .
H9 H 0.6203 0.9514 0.0181 0.078 Uiso 1 1 calc R . .
C11 C 0.5077(4) 0.8073(3) -0.0163(3) 0.0521(13) Uani 1 1 d . . .
H10 H 0.5156 0.8030 -0.0820 0.062 Uiso 1 1 calc R . .
C12 C 0.4307(4) 0.7232(3) 0.0214(2) 0.0373(9) Uani 1 1 d . . .
C13 C 0.1856(4) 0.4040(3) -0.1406(3) 0.0444(11) Uani 1 1 d . . .
C18 C 0.2742(6) 0.3615(5) -0.1660(3) 0.0831(19) Uani 1 1 d . . .
H13 H 0.3146 0.3243 -0.1208 0.100 Uiso 1 1 calc R . .
C17 C 0.3028(7) 0.3751(7) -0.2604(4) 0.124(3) Uani 1 1 d . . .
H14 H 0.3610 0.3452 -0.2782 0.149 Uiso 1 1 calc R . .
C16 C 0.2445(7) 0.4329(6) -0.3271(4) 0.096(2) Uani 1 1 d . . .
H15 H 0.2657 0.4452 -0.3884 0.115 Uiso 1 1 calc R . .
C15 C 0.1547(7) 0.4720(5) -0.3013(4) 0.087(2) Uani 1 1 d . . .
H16 H 0.1122 0.5064 -0.3473 0.104 Uiso 1 1 calc R . .
C14 C 0.1267(5) 0.4610(4) -0.2077(3) 0.0631(14) Uani 1 1 d . . .
H17 H 0.0688 0.4916 -0.1901 0.076 Uiso 1 1 calc R . .
C21 C 0.0970(4) 0.9491(3) 0.6968(3) 0.0518(12) Uani 1 1 d . . .
H18 H 0.0631 0.9855 0.6465 0.062 Uiso 1 1 calc R . .
C22 C 0.0640(5) 0.9534(4) 0.7900(3) 0.0585(13) Uani 1 1 d . . .
H19 H 0.0081 0.9909 0.8003 0.070 Uiso 1 1 calc R . .
C23 C 0.1159(5) 0.9005(3) 0.8671(3) 0.0550(13) Uani 1 1 d . . .
H20 H 0.0956 0.9045 0.9291 0.066 Uiso 1 1 calc R . .
C24 C 0.1969(4) 0.8427(3) 0.8511(3) 0.0473(12) Uani 1 1 d . . .
H21 H 0.2301 0.8064 0.9017 0.057 Uiso 1 1 calc R . .
C19 C 0.2292(4) 0.8389(3) 0.7579(2) 0.0375(10) Uani 1 1 d . . .
C25 C 0.4183(4) 0.7381(3) 0.6205(3) 0.0399(10) Uani 1 1 d . . .
C26 C 0.4833(5) 0.6766(3) 0.6807(3) 0.0535(12) Uani 1 1 d . . .
H24 H 0.4739 0.6683 0.7458 0.064 Uiso 1 1 calc R . .
C27 C 0.5609(5) 0.6288(4) 0.6422(3) 0.0673(15) Uani 1 1 d . . .
H25 H 0.6048 0.5893 0.6819 0.081 Uiso 1 1 calc R . .
C28 C 0.5739(5) 0.6396(4) 0.5441(3) 0.0657(15) Uani 1 1 d . . .
H26 H 0.6254 0.6061 0.5184 0.079 Uiso 1 1 calc R . .
C29 C 0.5101(4) 0.7001(3) 0.4845(3) 0.0526(13) Uani 1 1 d . . .
H27 H 0.5195 0.7071 0.4193 0.063 Uiso 1 1 calc R . .
C30 C 0.4318(4) 0.7505(3) 0.5220(2) 0.0372(10) Uani 1 1 d . . .
C31 C 0.1812(5) 0.9567(4) 0.3610(3) 0.0527(13) Uani 1 1 d . . .
C36 C 0.1416(6) 0.8663(4) 0.2970(3) 0.0734(18) Uani 1 1 d . . .
H30 H 0.0950 0.8043 0.3162 0.088 Uiso 1 1 calc R . .
C35 C 0.1713(7) 0.8675(6) 0.2029(4) 0.100(3) Uani 1 1 d . . .
H31 H 0.1443 0.8068 0.1591 0.120 Uiso 1 1 calc R . .
C34 C 0.2406(8) 0.9596(9) 0.1765(5) 0.133(3) Uani 1 1 d . . .
H32 H 0.2601 0.9607 0.1140 0.159 Uiso 1 1 calc R . .
C33 C 0.2820(8) 1.0496(8) 0.2392(5) 0.150(4) Uani 1 1 d . . .
H33 H 0.3302 1.1105 0.2201 0.180 Uiso 1 1 calc R . .
C32 C 0.2508(6) 1.0491(5) 0.3335(4) 0.092(2) Uani 1 1 d . . .
H34 H 0.2769 1.1104 0.3766 0.111 Uiso 1 1 calc R . .
O1 O 0.1088(5) 0.1749(3) 0.5376(4) 0.1119(16) Uani 1 1 d . . .
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'
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'
O O 0.0106 0.0060 '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
N2 Rh1 C2 81.32(14) . . ?
N2 Rh1 N4 178.15(13) . . ?
C2 Rh1 N4 96.88(15) . . ?
N2 Rh1 N3 80.48(13) . . ?
C2 Rh1 N3 161.72(12) . . ?
N4 Rh1 N3 101.33(13) . . ?
N2 Rh1 Cl1 91.65(12) . . ?
C2 Rh1 Cl1 89.32(12) . . ?
N4 Rh1 Cl1 88.75(11) . . ?
N3 Rh1 Cl1 89.47(11) . . ?
N2 Rh1 Cl2 89.80(11) . . ?
C2 Rh1 Cl2 92.21(12) . . ?
N4 Rh1 Cl2 89.84(11) . . ?
N3 Rh1 Cl2 89.46(11) . . ?
Cl1 Rh1 Cl2 178.03(4) . . ?
N6 Rh2 C20 80.56(15) . . ?
N6 Rh2 N8 178.36(14) . . ?
C20 Rh2 N8 98.01(16) . . ?
N6 Rh2 N7 80.75(14) . . ?
C20 Rh2 N7 161.16(13) . . ?
N8 Rh2 N7 100.72(13) . . ?
N6 Rh2 Cl4 92.23(11) . . ?
C20 Rh2 Cl4 91.50(12) . . ?
N8 Rh2 Cl4 88.60(12) . . ?
N7 Rh2 Cl4 86.92(10) . . ?
N6 Rh2 Cl3 90.54(11) . . ?
C20 Rh2 Cl3 89.59(12) . . ?
N8 Rh2 Cl3 88.65(12) . . ?
N7 Rh2 Cl3 92.89(10) . . ?
Cl4 Rh2 Cl3 177.15(4) . . ?
C3 C2 C1 118.0(3) . . ?
C3 C2 Rh1 133.6(3) . . ?
C1 C2 Rh1 108.3(3) . . ?
N2 N1 C1 110.6(3) . . ?
N1 N2 C7 120.9(3) . . ?
N1 N2 Rh1 120.4(2) . . ?
C7 N2 Rh1 118.6(2) . . ?
C12 N3 Rh1 106.5(2) . . ?
C13 N4 Rh1 114.1(2) . . ?
C21 C20 C19 117.3(3) . . ?
C21 C20 Rh2 133.9(3) . . ?
C19 C20 Rh2 108.8(3) . . ?
N6 N5 C19 110.6(3) . . ?
N5 N6 C25 121.4(3) . . ?
N5 N6 Rh2 120.8(3) . . ?
C25 N6 Rh2 117.7(2) . . ?
C30 N7 Rh2 106.1(2) . . ?
C31 N8 Rh2 114.7(3) . . ?
C2 C3 C4 120.9(3) . . ?
C5 C4 C3 120.2(4) . . ?
C6 C5 C4 120.3(4) . . ?
C5 C6 C1 119.5(4) . . ?
C6 C1 C2 121.0(3) . . ?
C6 C1 N1 119.7(3) . . ?
C2 C1 N1 119.3(3) . . ?
C8 C7 C12 120.4(4) . . ?
C8 C7 N2 123.9(3) . . ?
C12 C7 N2 115.7(3) . . ?
C7 C8 C9 119.7(4) . . ?
C10 C9 C8 120.3(4) . . ?
C9 C10 C11 120.2(4) . . ?
C10 C11 C12 120.7(4) . . ?
C7 C12 C11 118.7(3) . . ?
C7 C12 N3 118.5(3) . . ?
C11 C12 N3 122.8(3) . . ?
C14 C13 C18 120.0(4) . . ?
C14 C13 N4 118.9(4) . . ?
C18 C13 N4 121.0(4) . . ?
C13 C18 C17 119.7(5) . . ?
C16 C17 C18 120.2(7) . . ?
C15 C16 C17 119.2(6) . . ?
C16 C15 C14 121.1(5) . . ?
C13 C14 C15 119.6(5) . . ?
C20 C21 C22 121.7(4) . . ?
C23 C22 C21 119.7(4) . . ?
C24 C23 C22 120.1(4) . . ?
C23 C24 C19 119.8(4) . . ?
C24 C19 N5 119.4(3) . . ?
C24 C19 C20 121.4(4) . . ?
N5 C19 C20 119.1(3) . . ?
C30 C25 C26 120.5(4) . . ?
C30 C25 N6 116.5(3) . . ?
C26 C25 N6 123.0(3) . . ?
C27 C26 C25 119.5(4) . . ?
C26 C27 C28 120.4(4) . . ?
C29 C28 C27 120.2(5) . . ?
C28 C29 C30 120.5(4) . . ?
C29 C30 C25 118.8(4) . . ?
C29 C30 N7 122.5(3) . . ?
C25 C30 N7 118.7(4) . . ?
C36 C31 C32 120.5(5) . . ?
C36 C31 N8 119.0(4) . . ?
C32 C31 N8 120.5(4) . . ?
C31 C36 C35 120.2(6) . . ?
C34 C35 C36 118.9(6) . . ?
C33 C34 C35 121.9(6) . . ?
C34 C33 C32 119.2(7) . . ?
C31 C32 C33 119.3(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 N2 1.959(3) . ?
Rh1 C2 2.014(4) . ?
Rh1 N4 2.143(3) . ?
Rh1 N3 2.255(3) . ?
Rh1 Cl1 2.357(2) . ?
Rh1 Cl2 2.3672(19) . ?
Rh2 N6 1.969(3) . ?
Rh2 C20 2.010(4) . ?
Rh2 N8 2.136(3) . ?
Rh2 N7 2.260(4) . ?
Rh2 Cl4 2.371(2) . ?
Rh2 Cl3 2.380(2) . ?
C2 C3 1.401(5) . ?
C2 C1 1.425(5) . ?
N1 N2 1.289(4) . ?
N1 C1 1.439(5) . ?
N2 C7 1.436(5) . ?
N3 C12 1.466(5) . ?
N4 C13 1.458(5) . ?
C20 C21 1.386(6) . ?
C20 C19 1.428(5) . ?
N5 N6 1.283(4) . ?
N5 C19 1.425(5) . ?
N6 C25 1.434(6) . ?
N7 C30 1.464(5) . ?
N8 C31 1.453(5) . ?
C3 C4 1.404(5) . ?
C4 C5 1.399(6) . ?
C5 C6 1.393(6) . ?
C6 C1 1.407(5) . ?
C7 C8 1.405(5) . ?
C7 C12 1.408(5) . ?
C8 C9 1.414(6) . ?
C9 C10 1.387(6) . ?
C10 C11 1.393(6) . ?
C11 C12 1.422(6) . ?
C13 C14 1.387(6) . ?
C13 C18 1.387(7) . ?
C18 C17 1.406(8) . ?
C17 C16 1.386(9) . ?
C16 C15 1.379(9) . ?
C15 C14 1.391(7) . ?
C21 C22 1.409(6) . ?
C22 C23 1.406(6) . ?
C23 C24 1.379(7) . ?
C24 C19 1.405(5) . ?
C25 C30 1.405(5) . ?
C25 C26 1.412(5) . ?
C26 C27 1.382(7) . ?
C27 C28 1.396(6) . ?
C28 C29 1.390(6) . ?
C29 C30 1.401(6) . ?
C31 C36 1.374(6) . ?
C31 C32 1.380(7) . ?
C36 C35 1.402(8) . ?
C35 C34 1.370(11) . ?
C34 C33 1.363(11) . ?
C33 C32 1.413(9) . ?
