#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:52:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179132 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/94/4309432.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_4309432
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            'C24 H21 Cl2 N6 Rh'
_chemical_formula_weight         567.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.024(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.216(3)
_cell_length_b                   10.2993(8)
_cell_length_c                   20.5772(19)
_cell_measurement_temperature    273(2)
_cell_volume                     4890.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18565
_diffrn_reflns_theta_full        29.06
_diffrn_reflns_theta_max         29.06
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  0.9118
_exptl_absorpt_correction_T_min  0.8564
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                4316
_reflns_number_total             6476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050551wsi20050409_021550.cif
_cod_data_source_block           scjp12bm
_cod_original_cell_volume        4890.1(7)
_cod_database_code               4309432
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.273115(8) 0.56568(2) 0.824689(11) 0.03349(7) Uani 1 1 d . . .
Cl1 Cl 0.32893(3) 0.45919(7) 0.94180(4) 0.04766(18) Uani 1 1 d . . .
Cl2 Cl 0.21820(3) 0.66182(6) 0.70303(4) 0.04237(16) Uani 1 1 d . . .
N3 N 0.31807(11) 0.4553(2) 0.77892(15) 0.0513(6) Uani 1 1 d . . .
H1A H 0.3307 0.3786 0.8032 0.062 Uiso 1 1 calc R . .
H1B H 0.2940 0.4403 0.7285 0.062 Uiso 1 1 calc R . .
N2 N 0.33616(9) 0.6862(2) 0.85255(12) 0.0443(6) Uani 1 1 d . . .
N1 N 0.34078(11) 0.7926(3) 0.88622(14) 0.0556(7) Uani 1 1 d . . .
C2 C 0.25292(12) 0.7067(3) 0.87284(14) 0.0398(6) Uani 1 1 d . . .
N4 N 0.20416(9) 0.4267(2) 0.78598(12) 0.0349(5) Uani 1 1 d . . .
H5A H 0.1765 0.4520 0.7385 0.042 Uiso 1 1 calc R . .
H5B H 0.2183 0.3513 0.7804 0.042 Uiso 1 1 calc R . .
N5 N 0.09859(10) 0.5373(2) 0.73688(13) 0.0434(6) Uani 1 1 d . . .
N6 N 0.05355(12) 0.5927(3) 0.72070(16) 0.0656(8) Uani 1 1 d . . .
C24 C -0.02077(14) 0.7388(4) 0.6373(2) 0.0805(12) Uani 1 1 d . . .
H24 H -0.0385 0.7203 0.6644 0.097 Uiso 1 1 calc R . .
C12 C 0.36616(13) 0.5344(4) 0.79219(19) 0.0574(9) Uani 1 1 d . . .
C11 C 0.40266(18) 0.4991(5) 0.7680(3) 0.0945(14) Uani 1 1 d . . .
H2 H 0.3969 0.4213 0.7420 0.113 Uiso 1 1 calc R . .
C10 C 0.4471(2) 0.5788(7) 0.7825(4) 0.146(3) Uani 1 1 d . . .
H3 H 0.4710 0.5548 0.7648 0.175 Uiso 1 1 calc R . .
C9 C 0.4581(2) 0.6925(7) 0.8218(4) 0.124(2) Uani 1 1 d . . .
H4 H 0.4898 0.7430 0.8318 0.149 Uiso 1 1 calc R . .
C8 C 0.42229(14) 0.7328(4) 0.8467(2) 0.0834(13) Uani 1 1 d . . .
H5 H 0.4288 0.8108 0.8727 0.100 Uiso 1 1 calc R . .
C7 C 0.37612(12) 0.6522(3) 0.83125(17) 0.0541(8) Uani 1 1 d . . .
C1 C 0.29487(14) 0.8058(3) 0.89875(16) 0.0505(8) Uani 1 1 d . . .
C6 C 0.29254(19) 0.9189(3) 0.93513(19) 0.0705(11) Uani 1 1 d . . .
H8 H 0.3211 0.9821 0.9517 0.085 Uiso 1 1 calc R . .
C5 C 0.2477(2) 0.9337(3) 0.9455(2) 0.0774(12) Uani 1 1 d . . .
H9 H 0.2451 1.0083 0.9690 0.093 Uiso 1 1 calc R . .
C4 C 0.20598(17) 0.8384(4) 0.92140(18) 0.0679(10) Uani 1 1 d . . .
H10 H 0.1757 0.8492 0.9296 0.081 Uiso 1 1 calc R . .
C3 C 0.20811(14) 0.7262(3) 0.88498(16) 0.0530(8) Uani 1 1 d . . .
H11 H 0.1792 0.6639 0.8687 0.064 Uiso 1 1 calc R . .
C13 C 0.17439(11) 0.3942(2) 0.82438(14) 0.0346(6) Uani 1 1 d . . .
C18 C 0.19755(12) 0.3045(3) 0.88324(15) 0.0420(6) Uani 1 1 d . . .
H13 H 0.2326 0.2643 0.8980 0.050 Uiso 1 1 calc R . .
C17 C 0.16935(13) 0.2742(3) 0.92002(16) 0.0529(8) Uani 1 1 d . . .
H14 H 0.1852 0.2131 0.9593 0.063 Uiso 1 1 calc R . .
C16 C 0.11712(13) 0.3344(3) 0.89887(17) 0.0577(8) Uani 1 1 d . . .
H15 H 0.0987 0.3152 0.9250 0.069 Uiso 1 1 calc R . .
C15 C 0.09270(13) 0.4222(3) 0.83946(17) 0.0505(8) Uani 1 1 d . . .
H16 H 0.0575 0.4613 0.8248 0.061 Uiso 1 1 calc R . .
C14 C 0.12096(11) 0.4523(3) 0.80144(15) 0.0405(6) Uani 1 1 d . . .
C19 C 0.03026(13) 0.6790(3) 0.65657(19) 0.0587(9) Uani 1 1 d . . .
C20 C 0.05698(14) 0.7064(4) 0.61626(19) 0.0656(9) Uani 1 1 d . . .
H19 H 0.0914 0.6653 0.6289 0.079 Uiso 1 1 calc R . .
C23 C -0.04583(16) 0.8273(4) 0.5773(2) 0.0872(13) Uani 1 1 d . . .
H20 H -0.0806 0.8674 0.5638 0.105 Uiso 1 1 calc R . .
C22 C -0.01973(17) 0.8552(4) 0.5382(2) 0.0808(12) Uani 1 1 d . . .
H21 H -0.0366 0.9152 0.4984 0.097 Uiso 1 1 calc R . .
C21 C 0.03136(16) 0.7961(4) 0.55681(19) 0.0785(12) Uani 1 1 d . . .
H22 H 0.0488 0.8161 0.5296 0.094 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'
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'
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 79.67(11) . . ?
N2 Rh1 N4 175.09(9) . . ?
C2 Rh1 N4 104.65(10) . . ?
N2 Rh1 N3 81.53(10) . . ?
C2 Rh1 N3 161.16(10) . . ?
N4 Rh1 N3 94.08(9) . . ?
N2 Rh1 Cl1 90.35(6) . . ?
C2 Rh1 Cl1 91.69(7) . . ?
N4 Rh1 Cl1 91.83(6) . . ?
N3 Rh1 Cl1 89.65(7) . . ?
N2 Rh1 Cl2 90.49(6) . . ?
C2 Rh1 Cl2 92.02(7) . . ?
N4 Rh1 Cl2 87.06(6) . . ?
N3 Rh1 Cl2 86.89(7) . . ?
Cl1 Rh1 Cl2 176.29(3) . . ?
C12 N3 Rh1 106.30(19) . . ?
N1 N2 C7 120.9(3) . . ?
N1 N2 Rh1 122.0(2) . . ?
C7 N2 Rh1 117.0(2) . . ?
N2 N1 C1 110.1(2) . . ?
C3 C2 C1 116.3(3) . . ?
C3 C2 Rh1 134.2(2) . . ?
C1 C2 Rh1 109.5(2) . . ?
C13 N4 Rh1 125.88(16) . . ?
N6 N5 C14 114.1(2) . . ?
N5 N6 C19 115.4(3) . . ?
C19 C24 C23 119.7(4) . . ?
C11 C12 C7 118.7(3) . . ?
C11 C12 N3 122.7(4) . . ?
C7 C12 N3 118.6(3) . . ?
C10 C11 C12 119.5(5) . . ?
C11 C10 C9 122.6(5) . . ?
C10 C9 C8 120.0(5) . . ?
C9 C8 C7 117.6(5) . . ?
C8 C7 C12 121.5(3) . . ?
C8 C7 N2 122.0(4) . . ?
C12 C7 N2 116.5(3) . . ?
C6 C1 C2 123.1(3) . . ?
C6 C1 N1 118.2(3) . . ?
C2 C1 N1 118.7(3) . . ?
C5 C6 C1 118.5(4) . . ?
C6 C5 C4 120.1(3) . . ?
C5 C4 C3 121.5(4) . . ?
C2 C3 C4 120.6(3) . . ?
C18 C13 C14 119.3(2) . . ?
C18 C13 N4 120.6(2) . . ?
C14 C13 N4 120.1(2) . . ?
C17 C18 C13 120.5(3) . . ?
C18 C17 C16 120.3(3) . . ?
C15 C16 C17 120.2(3) . . ?
C16 C15 C14 119.7(3) . . ?
C15 C14 C13 120.0(3) . . ?
C15 C14 N5 124.6(3) . . ?
C13 C14 N5 115.4(2) . . ?
C24 C19 C20 120.4(3) . . ?
C24 C19 N6 115.5(3) . . ?
C20 C19 N6 124.1(3) . . ?
C21 C20 C19 118.9(3) . . ?
C22 C23 C24 120.1(4) . . ?
C23 C22 C21 120.8(4) . . ?
C22 C21 C20 120.1(4) . . ?
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 1.942(2) . ?
Rh1 C2 1.993(3) . ?
Rh1 N4 2.150(2) . ?
Rh1 N3 2.213(2) . ?
Rh1 Cl1 2.3314(7) . ?
Rh1 Cl2 2.3480(7) . ?
N3 C12 1.439(4) . ?
N2 N1 1.267(3) . ?
N2 C7 1.415(4) . ?
N1 C1 1.410(4) . ?
C2 C3 1.383(4) . ?
C2 C1 1.409(4) . ?
N4 C13 1.439(3) . ?
N5 N6 1.227(3) . ?
N5 C14 1.430(3) . ?
N6 C19 1.430(4) . ?
C24 C19 1.372(4) . ?
C24 C23 1.388(5) . ?
C12 C11 1.375(5) . ?
C12 C7 1.400(5) . ?
C11 C10 1.358(7) . ?
C10 C9 1.363(8) . ?
C9 C8 1.384(7) . ?
C8 C7 1.395(4) . ?
C1 C6 1.403(4) . ?
C6 C5 1.354(6) . ?
C5 C4 1.379(5) . ?
C4 C3 1.395(4) . ?
C13 C18 1.382(4) . ?
C13 C14 1.402(4) . ?
C18 C17 1.369(4) . ?
C17 C16 1.392(4) . ?
C16 C15 1.376(4) . ?
C15 C14 1.392(4) . ?
C19 C20 1.391(5) . ?
C20 C21 1.390(5) . ?
C23 C22 1.355(5) . ?
C22 C21 1.374(5) . ?
