#------------------------------------------------------------------------------
#$Date: 2016-03-25 04:00:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179691 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/16/2241615.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241615
loop_
_publ_author_name
'Sakate, Mika'
'Hosoda, Haruka'
'Suzuki, Takayoshi'
_publ_section_title
;
 Crystal structures of
 bis[2-(pyridin-2-yl)phenyl-κ²N,C¹]rhodium(III)
 complexes containing an acetonitrile or monodentate thyminate(1{-})
 ligand
;
_journal_coeditor_code           IS5448
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              543
_journal_page_last               547
_journal_paper_doi               10.1107/S2056989016004837
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Rh Cl (C11 H8 N)2 (C2 H3 N)]'
_chemical_formula_moiety         'C24 H19 Cl N3 Rh'
_chemical_formula_sum            'C24 H19 Cl N3 Rh'
_chemical_formula_weight         487.78
_chemical_name_systematic
(OC-6-42)-Acetonitrilechloridobis[2-(pyridin-2-yl)phenyl-κ²N,C¹]rhodium(III)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5415(9)
_cell_length_b                   14.6600(11)
_cell_length_c                   17.0026(12)
_cell_measurement_reflns_used    31949
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      3.02
_cell_volume                     4123.1(5)
_computing_cell_refinement
;
RAPID AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
CrystalStructure (Rigaku, 2010)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
Il Milione (Burla et al.,  2007)
;
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38163
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.026
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.8292
_exptl_absorpt_correction_T_min  0.6969
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Rigaku, 1999)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0309P)²+1.6125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                4327
_reflns_number_total             4709
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            is5448sup1.cif
_cod_data_source_block           1
_cod_database_code               2241615
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.697
_shelx_estimated_absorpt_t_max   0.829
_shelxl_version_number           .2013
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'x-1/2, y, -z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Rh Rh1 0.12078(2) 0.55701(2) 0.36161(2) 0.01986(5) Uani d 1
Cl Cl1 0.10904(2) 0.64708(3) 0.48498(2) 0.02906(9) Uani d 1
N N1 0.15175(8) 0.44472(8) 0.42460(8) 0.0238(3) Uani d 1
N N2 0.09842(8) 0.66466(9) 0.28773(8) 0.0235(3) Uani d 1
N N3 -0.00853(9) 0.53554(10) 0.36314(8) 0.0265(3) Uani d 1
C C1 0.09933(10) 0.38632(11) 0.45823(9) 0.0272(3) Uani d 1
H H1 0.0433 0.4006 0.4579 0.033 Uiso calc 1
C C2 0.12459(10) 0.30643(13) 0.49304(11) 0.0339(4) Uani d 1
H H2 0.0865 0.2662 0.5165 0.041 Uiso calc 1
C C3 0.20657(11) 0.28542(12) 0.49338(11) 0.0358(4) Uani d 1
H H3 0.2251 0.2298 0.5157 0.043 Uiso calc 1
C C4 0.26051(10) 0.34604(12) 0.46102(10) 0.0309(3) Uani d 1
H H4 0.3167 0.3329 0.4617 0.037 Uiso calc 1
C C5 0.23289(9) 0.42661(11) 0.42724(9) 0.0247(3) Uani d 1
C C6 0.28290(9) 0.49821(11) 0.39221(9) 0.0252(3) Uani d 1
C C7 0.36733(10) 0.49704(13) 0.39354(10) 0.0326(4) Uani d 1
H H7 0.3954 0.4472 0.4166 0.039 Uiso calc 1
C C8 0.40989(12) 0.56954(14) 0.36084(11) 0.0381(4) Uani d 1
H H8 0.4673 0.5693 0.3614 0.046 Uiso calc 1
C C9 0.36859(10) 0.64198(13) 0.32751(12) 0.0370(4) Uani d 1
H H9 0.3979 0.6915 0.3054 0.044 Uiso calc 1
C C10 0.28439(10) 0.64280(12) 0.32621(10) 0.0305(3) Uani d 1
H H10 0.2568 0.6929 0.3031 0.037 Uiso calc 1
C C11 0.24040(10) 0.57124(11) 0.35831(8) 0.0234(3) Uani d 1
C C12 0.07628(10) 0.74823(11) 0.31092(10) 0.0302(3) Uani d 1
H H12 0.0715 0.7604 0.3656 0.036 Uiso calc 1
C C13 0.06014(12) 0.81726(12) 0.25807(11) 0.0373(4) Uani d 1
H H13 0.0435 0.8758 0.2758 0.045 Uiso calc 1
C C14 0.06879(12) 0.79919(12) 0.17872(11) 0.0381(4) Uani d 1
H H14 0.0591 0.8459 0.1411 0.046 Uiso calc 1
C C15 0.09143(11) 0.71342(12) 0.15440(10) 0.0322(4) Uani d 1
H H15 0.0978 0.7007 0.1000 0.039 Uiso calc 1
C C16 0.10502(9) 0.64548(11) 0.20997(9) 0.0243(3) Uani d 1
C C17 0.12356(8) 0.54991(11) 0.19292(10) 0.0238(3) Uani d 1
C C18 0.12867(10) 0.51469(13) 0.11672(10) 0.0301(4) Uani d 1
H H18 0.1222 0.5540 0.0728 0.036 Uiso calc 1
C C19 0.14314(12) 0.42299(13) 0.10501(11) 0.0363(4) Uani d 1
H H19 0.1462 0.3990 0.0532 0.044 Uiso calc 1
C C20 0.15317(12) 0.36630(13) 0.16931(11) 0.0383(4) Uani d 1
H H20 0.1636 0.3033 0.1614 0.046 Uiso calc 1
C C21 0.14813(11) 0.40060(12) 0.24553(10) 0.0315(3) Uani d 1
H H21 0.1555 0.3607 0.2890 0.038 Uiso calc 1
C C22 0.13243(8) 0.49280(11) 0.25894(9) 0.0233(3) Uani d 1
C C23 -0.07658(11) 0.52843(12) 0.36004(9) 0.0285(3) Uani d 1
C C24 -0.16431(11) 0.51736(16) 0.35764(12) 0.0425(5) Uani d 1
H H24A -0.1903 0.5768 0.3653 0.051 Uiso calc 1
H H24B -0.1813 0.4756 0.3995 0.051 Uiso calc 1
H H24C -0.1802 0.4923 0.3065 0.051 Uiso calc 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rh Rh -1.1178 0.9187 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C11 Rh1 C22 85.91(6)
C11 Rh1 N1 81.31(6)
C22 Rh1 N1 93.13(6)
C11 Rh1 N2 94.67(6)
C22 Rh1 N2 81.05(6)
N1 Rh1 N2 173.19(5)
C11 Rh1 N3 177.47(6)
C22 Rh1 N3 92.15(5)
N1 Rh1 N3 97.20(5)
N2 Rh1 N3 86.62(5)
C11 Rh1 Cl1 92.62(4)
C22 Rh1 Cl1 176.01(5)
N1 Rh1 Cl1 90.30(4)
N2 Rh1 Cl1 95.40(4)
N3 Rh1 Cl1 89.42(4)
C1 N1 C5 119.62(14)
C1 N1 Rh1 125.26(11)
C5 N1 Rh1 114.97(10)
C12 N2 C16 119.94(14)
C12 N2 Rh1 124.99(11)
C16 N2 Rh1 115.03(11)
C23 N3 Rh1 175.44(14)
N1 C1 C2 121.87(15)
N1 C1 H1 119.1
C2 C1 H1 119.1
C1 C2 C3 119.09(16)
C1 C2 H2 120.5
C3 C2 H2 120.5
C4 C3 C2 119.22(16)
C4 C3 H3 120.4
C2 C3 H3 120.4
C3 C4 C5 120.08(15)
C3 C4 H4 120.0
C5 C4 H4 120.0
N1 C5 C4 120.04(15)
N1 C5 C6 113.69(14)
C4 C5 C6 126.28(15)
C7 C6 C11 121.09(15)
C7 C6 C5 123.36(15)
C11 C6 C5 115.52(14)
C8 C7 C6 119.36(17)
C8 C7 H7 120.3
C6 C7 H7 120.3
C9 C8 C7 120.01(17)
C9 C8 H8 120.0
C7 C8 H8 120.0
C8 C9 C10 120.43(17)
C8 C9 H9 119.8
C10 C9 H9 119.8
C11 C10 C9 120.75(17)
C11 C10 H10 119.6
C9 C10 H10 119.6
C10 C11 C6 118.35(15)
C10 C11 Rh1 127.68(13)
C6 C11 Rh1 113.96(11)
N2 C12 C13 122.19(16)
N2 C12 H12 118.9
C13 C12 H12 118.9
C12 C13 C14 118.37(16)
C12 C13 H13 120.8
C14 C13 H13 120.8
C15 C14 C13 119.78(16)
C15 C14 H14 120.1
C13 C14 H14 120.1
C14 C15 C16 119.62(16)
C14 C15 H15 120.2
C16 C15 H15 120.2
N2 C16 C15 120.05(15)
N2 C16 C17 114.12(14)
C15 C16 C17 125.79(15)
C18 C17 C22 120.88(15)
C18 C17 C16 123.39(15)
C22 C17 C16 115.67(15)
C19 C18 C17 120.29(17)
C19 C18 H18 119.9
C17 C18 H18 119.9
C18 C19 C20 119.47(17)
C18 C19 H19 120.3
C20 C19 H19 120.3
C19 C20 C21 120.76(17)
C19 C20 H20 119.6
C21 C20 H20 119.6
C20 C21 C22 120.86(16)
C20 C21 H21 119.6
C22 C21 H21 119.6
C21 C22 C17 117.72(14)
C21 C22 Rh1 128.23(12)
C17 C22 Rh1 114.05(12)
N3 C23 C24 178.48(19)
C23 C24 H24A 109.5
C23 C24 H24B 109.5
H24A C24 H24B 109.5
C23 C24 H24C 109.5
H24A C24 H24C 109.5
H24B C24 H24C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 C11 1.9904(16)
Rh1 C22 1.9926(15)
Rh1 N1 2.0296(13)
Rh1 N2 2.0507(13)
Rh1 N3 2.1621(14)
Rh1 Cl1 2.4862(4)
N1 C1 1.346(2)
N1 C5 1.369(2)
N2 C12 1.338(2)
N2 C16 1.356(2)
N3 C23 1.132(2)
C1 C2 1.377(2)
C1 H1 0.9500
C2 C3 1.391(2)
C2 H2 0.9500
C3 C4 1.374(2)
C3 H3 0.9500
C4 C5 1.391(2)
C4 H4 0.9500
C5 C6 1.463(2)
C6 C7 1.397(2)
C6 C11 1.405(2)
C7 C8 1.391(3)
C7 H7 0.9500
C8 C9 1.384(3)
C8 H8 0.9500
C9 C10 1.393(2)
C9 H9 0.9500
C10 C11 1.388(2)
C10 H10 0.9500
C12 C13 1.379(2)
C12 H12 0.9500
C13 C14 1.382(3)
C13 H13 0.9500
C14 C15 1.376(3)
C14 H14 0.9500
C15 C16 1.391(2)
C15 H15 0.9500
C16 C17 1.463(2)
C17 C18 1.397(2)
C17 C22 1.408(2)
C18 C19 1.380(3)
C18 H18 0.9500
C19 C20 1.383(3)
C19 H19 0.9500
C20 C21 1.393(2)
C20 H20 0.9500
C21 C22 1.395(2)
C21 H21 0.9500
C23 C24 1.461(3)
C24 H24A 0.9800
C24 H24B 0.9800
C24 H24C 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1 Cl1 5_566 0.95 2.79 3.613(2) 145
C14 H14 Cl1 3_564 0.95 2.78 3.452(2) 128
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C5 N1 C1 C2 -2.5(2)
Rh1 N1 C1 C2 173.05(13)
N1 C1 C2 C3 -0.1(3)
C1 C2 C3 C4 1.9(3)
C2 C3 C4 C5 -1.1(3)
C1 N1 C5 C4 3.2(2)
Rh1 N1 C5 C4 -172.74(12)
C1 N1 C5 C6 -176.83(14)
Rh1 N1 C5 C6 7.22(17)
C3 C4 C5 N1 -1.5(2)
C3 C4 C5 C6 178.60(16)
N1 C5 C6 C7 175.24(15)
C4 C5 C6 C7 -4.8(3)
N1 C5 C6 C11 -3.0(2)
C4 C5 C6 C11 176.96(16)
C11 C6 C7 C8 0.1(3)
C5 C6 C7 C8 -178.03(16)
C6 C7 C8 C9 0.1(3)
C7 C8 C9 C10 -0.2(3)
C8 C9 C10 C11 0.1(3)
C9 C10 C11 C6 0.1(2)
C9 C10 C11 Rh1 -178.98(14)
C7 C6 C11 C10 -0.2(2)
C5 C6 C11 C10 178.05(14)
C7 C6 C11 Rh1 179.01(13)
C5 C6 C11 Rh1 -2.72(17)
C16 N2 C12 C13 -0.5(2)
Rh1 N2 C12 C13 -178.34(13)
N2 C12 C13 C14 -1.2(3)
C12 C13 C14 C15 1.3(3)
C13 C14 C15 C16 0.3(3)
C12 N2 C16 C15 2.2(2)
Rh1 N2 C16 C15 -179.80(12)
C12 N2 C16 C17 -175.52(14)
Rh1 N2 C16 C17 2.54(16)
C14 C15 C16 N2 -2.1(3)
C14 C15 C16 C17 175.30(16)
N2 C16 C17 C18 176.48(14)
C15 C16 C17 C18 -1.0(2)
N2 C16 C17 C22 -0.54(19)
C15 C16 C17 C22 -178.06(15)
C22 C17 C18 C19 -0.5(2)
C16 C17 C18 C19 -177.33(15)
C17 C18 C19 C20 -0.5(3)
C18 C19 C20 C21 0.6(3)
C19 C20 C21 C22 0.3(3)
C20 C21 C22 C17 -1.3(2)
C20 C21 C22 Rh1 178.95(14)
C18 C17 C22 C21 1.3(2)
C16 C17 C22 C21 178.43(14)
C18 C17 C22 Rh1 -178.86(11)
C16 C17 C22 Rh1 -1.75(16)

_cod_database_fobs_code 2241615
