# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1059873'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-06-26 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
"{bis(μ₂-Iodo)-bis(N,N'-bis(2,6-dimethylphenyl)pentane-2,4-diiminato-N,N')-diphenyl-di-rhodium(II) toluene solvate"
_chemical_name_common            ?
_chemical_formula_moiety         'C42 H62 I2 N4 Rh2, C7'
_chemical_formula_sum            'C49 H62 I2 N4 Rh2'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene, hexane, THF'
_chemical_melting_point          ?

_exptl_crystal_description       'a irregular fragment'
_exptl_crystal_colour            'dark green'

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1166.65

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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_int_tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_chemical_absolute_configuration ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x, y, -z'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   19.268(7)
_cell_length_b                   11.773(4)
_cell_length_c                   14.410(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 131.886(6)
_cell_angle_gamma                90.00
_cell_volume                     2433.4(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9848
_cell_measurement_theta_min      2.840
_cell_measurement_theta_max      30.095
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8094
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker D8 three-circle diffractometer with an APEX-II CCD detector'
_diffrn_measurement_method       'area detector φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9067
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2396
_reflns_number_gt                2256
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 software suite'
_computing_cell_refinement       'APEX2 software suite'
_computing_data_reduction        'APEX2 software suite'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0577P)²+3.7955P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00062(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2396
_refine_ls_number_parameters     150
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0897
_refine_ls_wR_factor_gt          0.0870
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.08292(2) 0.5000 0.45998(3) 0.03848(14) Uani 1 2 d S . .
I1 I -0.095636(19) 0.5000 0.34555(3) 0.06044(16) Uani 1 2 d S . .
C11 C 0.3704(3) 0.5000 0.6115(5) 0.0693(14) Uani 1 2 d S . .
H111 H 0.3913 0.5305 0.5721 0.104 Uiso 1 1 calc R . .
H112 H 0.3929 0.4236 0.6383 0.104 Uiso 1 1 calc R . .
H113 H 0.3939 0.5458 0.6824 0.104 Uiso 1 1 calc R . .
C12 C 0.2654(3) 0.5000 0.5203(4) 0.0491(10) Uani 1 2 d S . .
C13 C 0.2199(4) 0.5000 0.3954(5) 0.0564(12) Uani 1 2 d S . .
H13 H 0.2582 0.5000 0.3775 0.068 Uiso 1 2 calc SR . .
C14 C 0.1255(3) 0.5000 0.2934(4) 0.0483(10) Uani 1 2 d S . .
C15 C 0.0952(4) 0.5000 0.1667(4) 0.0643(13) Uani 1 2 d S . .
H151 H 0.1457 0.5257 0.1734 0.096 Uiso 1 1 calc R . .
H152 H 0.0428 0.5499 0.1125 0.096 Uiso 1 1 calc R . .
H153 H 0.0778 0.4244 0.1332 0.096 Uiso 1 1 calc R . .
N1 N 0.2208(2) 0.5000 0.5613(3) 0.0420(8) Uani 1 2 d S . .
N2 N 0.0613(3) 0.5000 0.3030(3) 0.0452(8) Uani 1 2 d S . .
C21 C 0.2798(3) 0.5000 0.6958(4) 0.0481(10) Uani 1 2 d S . .
C22 C 0.3060(2) 0.3964(4) 0.7577(4) 0.0690(10) Uani 1 1 d . . .
C23 C 0.3621(3) 0.4003(7) 0.8872(4) 0.106(2) Uani 1 1 d . . .
H23 H 0.3814 0.3328 0.9317 0.127 Uiso 1 1 calc R . .
C24 C 0.3888(6) 0.5000 0.9488(7) 0.133(5) Uani 1 2 d S . .
H24 H 0.4260 0.5000 1.0349 0.160 Uiso 1 2 calc SR . .
C27 C 0.2744(4) 0.2869(4) 0.6881(6) 0.0990(17) Uani 1 1 d . . .
H271 H 0.2078 0.2878 0.6219 0.148 Uiso 1 1 calc R . .
H272 H 0.2921 0.2253 0.7439 0.148 Uiso 1 1 calc R . .
H273 H 0.3029 0.2770 0.6538 0.148 Uiso 1 1 calc R . .
C31 C -0.0351(3) 0.5000 0.1863(4) 0.0550(12) Uani 1 2 d S . .
C32 C -0.0795(3) 0.6043(4) 0.1342(3) 0.0736(11) Uani 1 1 d . . .
C33 C -0.1739(3) 0.6011(7) 0.0241(4) 0.111(2) Uani 1 1 d . . .
H33 H -0.2058 0.6688 -0.0141 0.134 Uiso 1 1 calc R . .
C34 C -0.2199(5) 0.5000 -0.0280(7) 0.125(4) Uani 1 2 d S . .
H34 H -0.2829 0.5000 -0.0995 0.150 Uiso 1 2 calc SR . .
C37 C -0.0307(4) 0.7140(4) 0.1933(5) 0.0929(15) Uani 1 1 d . . .
H371 H 0.0020 0.7114 0.2806 0.139 Uiso 1 1 calc R . .
H372 H -0.0754 0.7746 0.1547 0.139 Uiso 1 1 calc R . .
H373 H 0.0130 0.7269 0.1829 0.139 Uiso 1 1 calc R . .
C91 C 0.0000 0.1719(12) 0.5000 0.159(4) Uiso 1 2 d SD . .
C92 C 0.0692(8) 0.0998(7) 0.6028(10) 0.108(3) Uiso 0.50 1 d PD . .
C93 C 0.0736(5) -0.0209(6) 0.6098(7) 0.080(2) Uiso 0.50 1 d PD . .
C94 C 0.0000 -0.0733(12) 0.5000 0.088(4) Uiso 0.50 2 d SPD . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 N1 2.003(4) . ?
Rh1 N2 2.008(4) . ?
Rh1 I1 2.6420(11) . ?
Rh1 I1 2.6449(9) 5_566 ?
I1 Rh1 2.6449(9) 5_566 ?
C11 C12 1.507(6) . ?
C11 H111 0.9600 . ?
C11 H112 0.9600 . ?
C11 H113 0.9600 . ?
C12 N1 1.328(6) . ?
C12 C13 1.379(7) . ?
C13 C14 1.379(7) . ?
C13 H13 0.9300 . ?
C14 N2 1.332(6) . ?
C14 C15 1.500(6) . ?
C15 H151 0.9600 . ?
C15 H152 0.9600 . ?
C15 H153 0.9600 . ?
N1 C21 1.451(5) . ?
N2 C31 1.452(6) . ?
C21 C22 1.392(4) . ?
C21 C22 1.392(4) 2_565 ?
C22 C23 1.399(6) . ?
C22 C27 1.490(7) . ?
C23 C24 1.349(7) . ?
C23 H23 0.9300 . ?
C24 C23 1.349(7) 2_565 ?
C24 H24 0.9300 . ?
C27 H271 0.9600 . ?
C27 H272 0.9600 . ?
C27 H273 0.9600 . ?
C31 C32 1.394(5) 2_565 ?
C31 C32 1.394(5) . ?
C32 C33 1.405(6) . ?
C32 C37 1.486(7) . ?
C33 C34 1.370(8) . ?
C33 H33 0.9300 . ?
C34 C33 1.370(8) 2_565 ?
C34 H34 0.9300 . ?
C37 H371 0.9600 . ?
C37 H372 0.9600 . ?
C37 H373 0.9600 . ?
C91 C94 1.161(16) 5_556 ?
C91 C92 1.434(8) . ?
C91 C92 1.434(8) 6_556 ?
C92 C93 0.931(13) 2 ?
C92 C94 1.197(11) 5_556 ?
C92 C93 1.423(8) . ?
C93 C93 0.493(15) 2 ?
C93 C92 0.931(13) 2 ?
C93 C94 1.378(7) . ?
C93 C94 1.658(13) 5_556 ?
C94 C91 1.161(16) 5_556 ?
C94 C92 1.197(11) 2 ?
C94 C92 1.197(11) 5_556 ?
C94 C93 1.378(7) 6_556 ?
C94 C93 1.658(13) 5_556 ?
C94 C93 1.658(13) 2 ?
C94 C94 1.73(3) 5_556 ?

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
N1 Rh1 N2 89.85(15) . . ?
N1 Rh1 I1 174.83(10) . . ?
N2 Rh1 I1 95.33(11) . . ?
N1 Rh1 I1 95.07(10) . 5_566 ?
N2 Rh1 I1 175.08(11) . 5_566 ?
I1 Rh1 I1 79.756(19) . 5_566 ?
Rh1 I1 Rh1 100.24(2) . 5_566 ?
C12 C11 H111 109.5 . . ?
C12 C11 H112 109.5 . . ?
H111 C11 H112 109.5 . . ?
C12 C11 H113 109.5 . . ?
H111 C11 H113 109.5 . . ?
H112 C11 H113 109.5 . . ?
N1 C12 C13 123.0(4) . . ?
N1 C12 C11 120.1(4) . . ?
C13 C12 C11 116.9(4) . . ?
C12 C13 C14 128.8(4) . . ?
C12 C13 H13 115.6 . . ?
C14 C13 H13 115.6 . . ?
N2 C14 C13 123.0(4) . . ?
N2 C14 C15 119.5(4) . . ?
C13 C14 C15 117.4(4) . . ?
C14 C15 H151 109.5 . . ?
C14 C15 H152 109.5 . . ?
H151 C15 H152 109.5 . . ?
C14 C15 H153 109.5 . . ?
H151 C15 H153 109.5 . . ?
H152 C15 H153 109.5 . . ?
C12 N1 C21 115.6(4) . . ?
C12 N1 Rh1 127.8(3) . . ?
C21 N1 Rh1 116.6(3) . . ?
C14 N2 C31 116.0(4) . . ?
C14 N2 Rh1 127.5(3) . . ?
C31 N2 Rh1 116.5(3) . . ?
C22 C21 C22 122.5(5) . 2_565 ?
C22 C21 N1 118.8(2) . . ?
C22 C21 N1 118.8(2) 2_565 . ?
C21 C22 C23 116.8(5) . . ?
C21 C22 C27 121.1(4) . . ?
C23 C22 C27 122.0(5) . . ?
C24 C23 C22 121.5(6) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C23 120.9(7) . 2_565 ?
C23 C24 H24 119.6 . . ?
C23 C24 H24 119.6 2_565 . ?
C22 C27 H271 109.5 . . ?
C22 C27 H272 109.5 . . ?
H271 C27 H272 109.5 . . ?
C22 C27 H273 109.5 . . ?
H271 C27 H273 109.5 . . ?
H272 C27 H273 109.5 . . ?
C32 C31 C32 123.4(5) 2_565 . ?
C32 C31 N2 118.3(3) 2_565 . ?
C32 C31 N2 118.3(3) . . ?
C31 C32 C33 116.7(5) . . ?
C31 C32 C37 122.1(4) . . ?
C33 C32 C37 121.2(5) . . ?
C34 C33 C32 121.2(6) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C33 120.6(7) 2_565 . ?
C33 C34 H34 119.7 2_565 . ?
C33 C34 H34 119.7 . . ?
C32 C37 H371 109.5 . . ?
C32 C37 H372 109.5 . . ?
H371 C37 H372 109.5 . . ?
C32 C37 H373 109.5 . . ?
H371 C37 H373 109.5 . . ?
H372 C37 H373 109.5 . . ?
C94 C91 C92 53.7(6) 5_556 . ?
C94 C91 C92 53.7(6) 5_556 6_556 ?
C92 C91 C92 107.4(13) . 6_556 ?
C93 C92 C94 79.6(10) 2 5_556 ?
C93 C92 C93 1.6(3) 2 . ?
C94 C92 C93 78.0(8) 5_556 . ?
C93 C92 C91 131.0(14) 2 . ?
C94 C92 C91 51.4(9) 5_556 . ?
C93 C92 C91 129.4(11) . . ?
C93 C93 C92 175.3(9) 2 2 ?
C93 C93 C94 116.6(6) 2 . ?
C92 C93 C94 58.7(8) 2 . ?
C93 C93 C92 3.1(6) 2 . ?
C92 C93 C92 172.2(14) 2 . ?
C94 C93 C92 113.5(10) . . ?
C93 C93 C94 48.0(5) 2 5_556 ?
C92 C93 C94 127.3(11) 2 5_556 ?
C94 C93 C94 68.6(10) . 5_556 ?
C92 C93 C94 44.9(6) . 5_556 ?
C91 C94 C92 74.9(7) 5_556 2 ?
C91 C94 C92 74.9(7) 5_556 5_556 ?
C92 C94 C92 149.8(14) 2 5_556 ?
C91 C94 C93 116.6(6) 5_556 6_556 ?
C92 C94 C93 168.5(12) 2 6_556 ?
C92 C94 C93 41.7(6) 5_556 6_556 ?
C91 C94 C93 116.6(6) 5_556 . ?
C92 C94 C93 41.7(6) 2 . ?
C92 C94 C93 168.5(12) 5_556 . ?
C93 C94 C93 126.8(12) 6_556 . ?
C91 C94 C93 132.0(5) 5_556 5_556 ?
C92 C94 C93 153.1(12) 2 5_556 ?
C92 C94 C93 57.1(4) 5_556 5_556 ?
C93 C94 C93 15.4(4) 6_556 5_556 ?
C93 C94 C93 111.4(10) . 5_556 ?
C91 C94 C93 132.0(5) 5_556 2 ?
C92 C94 C93 57.1(4) 2 2 ?
C92 C94 C93 153.1(12) 5_556 2 ?
C93 C94 C93 111.4(10) 6_556 2 ?
C93 C94 C93 15.4(4) . 2 ?
C93 C94 C93 96.0(10) 5_556 2 ?
C91 C94 C94 179.997(1) 5_556 5_556 ?
C92 C94 C94 105.1(7) 2 5_556 ?
C92 C94 C94 105.1(7) 5_556 5_556 ?
C93 C94 C94 63.4(6) 6_556 5_556 ?
C93 C94 C94 63.4(6) . 5_556 ?
C93 C94 C94 48.0(5) 5_556 5_556 ?
C93 C94 C94 48.0(5) 2 5_556 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.108

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1059874'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-06-26 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
"bis(μ₂-Bromo)-bis(N,N'-bis(2,6-dimethylphenyl)pentane-2,4-diiminato-N,N')-diphenyl-di-rhodium(II) toluene solvate"
_chemical_name_common            ?
_chemical_formula_moiety         'C42 H62 Br2 N4 Rh2, C7'
_chemical_formula_sum            'C49 H62 Br2 N4 Rh2'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene, hexane, thf'
_chemical_melting_point          ?

_exptl_crystal_description       'a irregular block'
_exptl_crystal_colour            deep-green

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1072.67

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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_int_tables_number      12
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  '-C 2y'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x, y, -z'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.862(7)
_cell_length_b                   11.848(5)
_cell_length_c                   14.220(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 131.564(13)
_cell_angle_gamma                90.00
_cell_volume                     2377.7(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9409
_cell_measurement_theta_min      2.8855
_cell_measurement_theta_max      29.988
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    2.411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7724
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker D8 three-circle diffractometer with an APEX-II CCD detector'
_diffrn_measurement_method       'area detector φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8868
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2336
_reflns_number_gt                2251
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 software suite'
_computing_cell_refinement       'APEX2 software suite'
_computing_data_reduction        'APEX2 software suite'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0639P)²+5.9921P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2336
_refine_ls_number_parameters     151
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.11750(2) 0.5000 0.03682(3) 0.03854(19) Uani 1 2 d S . .
Br1 Br 0.05639(3) 0.5000 0.14746(4) 0.0615(2) Uani 1 2 d S . .
C11 C 0.2543(4) 0.5000 -0.1190(6) 0.0703(17) Uani 1 2 d S . .
H111 H 0.3140 0.5343 -0.0816 0.106 Uiso 1 1 calc R . .
H112 H 0.2040 0.5420 -0.1922 0.106 Uiso 1 1 calc R . .
H113 H 0.2535 0.4237 -0.1425 0.106 Uiso 1 1 calc R . .
C12 C 0.2409(4) 0.5000 -0.0253(5) 0.0502(11) Uani 1 2 d S . .
C13 C 0.3229(4) 0.5000 0.1007(5) 0.0599(14) Uani 1 2 d S . .
H13 H 0.3800 0.5000 0.1183 0.072 Uiso 1 2 calc SR . .
C14 C 0.3288(3) 0.5000 0.2035(5) 0.0535(12) Uani 1 2 d S . .
C15 C 0.4263(4) 0.5000 0.3312(5) 0.0677(16) Uani 1 2 d S . .
H151 H 0.4272 0.5473 0.3867 0.102 Uiso 1 1 calc R . .
H152 H 0.4708 0.5283 0.3250 0.102 Uiso 1 1 calc R . .
H153 H 0.4435 0.4244 0.3637 0.102 Uiso 1 1 calc R . .
N1 N 0.1543(3) 0.5000 -0.0661(4) 0.0410(8) Uani 1 2 d S . .
N2 N 0.2540(3) 0.5000 0.1938(4) 0.0433(9) Uani 1 2 d S . .
C21 C 0.0770(4) 0.5000 -0.2003(5) 0.0532(13) Uani 1 2 d S . .
C22 C 0.0413(3) 0.6030(5) -0.2622(5) 0.0834(16) Uani 1 1 d . . .
C23 C -0.0327(5) 0.5978(10) -0.3933(6) 0.136(4) Uani 1 1 d . . .
H23 H -0.0585 0.6647 -0.4387 0.163 Uiso 1 1 calc R . .
C24 C -0.0669(8) 0.5000 -0.4541(9) 0.181(10) Uani 1 2 d S . .
H24 H -0.1158 0.5000 -0.5410 0.218 Uiso 1 2 calc SR . .
C27 C 0.0795(6) 0.7109(5) -0.1930(8) 0.127(3) Uani 1 1 d . . .
H271 H 0.0687 0.7160 -0.1360 0.191 Uiso 1 1 calc R . .
H272 H 0.0483 0.7726 -0.2515 0.191 Uiso 1 1 calc R . .
H273 H 0.1463 0.7144 -0.1465 0.191 Uiso 1 1 calc R . .
C31 C 0.2727(3) 0.5000 0.3099(4) 0.0520(12) Uani 1 2 d S . .
C32 C 0.2804(3) 0.3965(5) 0.3629(4) 0.0691(12) Uani 1 1 d . . .
C33 C 0.2963(4) 0.4013(7) 0.4749(5) 0.099(2) Uani 1 1 d . . .
H33 H 0.3022 0.3344 0.5137 0.119 Uiso 1 1 calc R . .
C34 C 0.3031(6) 0.5000 0.5270(7) 0.116(4) Uani 1 2 d S . .
H34 H 0.3127 0.5000 0.6001 0.139 Uiso 1 2 calc SR . .
C37 C 0.2708(4) 0.2876(5) 0.3029(5) 0.0955(18) Uani 1 1 d . . .
H371 H 0.2190 0.2926 0.2138 0.143 Uiso 1 1 calc R . .
H372 H 0.2591 0.2278 0.3365 0.143 Uiso 1 1 calc R . .
H373 H 0.3283 0.2724 0.3197 0.143 Uiso 1 1 calc R . .
C81 C 0.0000 0.1817(19) 0.0000 0.14(2) Uiso 0.50 2 d SPD . .
C82 C 0.0000 0.0650(12) 0.0000 0.086(4) Uiso 0.50 2 d SPD . .
C83 C -0.0334(7) 0.0000 -0.1030(8) 0.097(2) Uiso 1 2 d SD . .
C84 C -0.0349(10) -0.1119(7) -0.1087(13) 0.106(4) Uiso 0.50 1 d PD . .
C85 C 0.0000 -0.164(3) 0.0000 0.16(3) Uiso 0.50 2 d SPD . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 N1 1.993(4) . ?
Rh1 N2 1.996(4) . ?
Rh1 Br1 2.4921(9) . ?
Rh1 Br1 2.4939(11) 5_565 ?
Br1 Rh1 2.4939(11) 5_565 ?
C11 C12 1.512(7) . ?
C11 H111 0.9600 . ?
C11 H112 0.9600 . ?
C11 H113 0.9600 . ?
C12 N1 1.321(7) . ?
C12 C13 1.388(8) . ?
C13 C14 1.390(8) . ?
C13 H13 0.9300 . ?
C14 N2 1.322(7) . ?
C14 C15 1.500(7) . ?
C15 H151 0.9600 . ?
C15 H152 0.9600 . ?
C15 H153 0.9600 . ?
N1 C21 1.441(6) . ?
N2 C31 1.442(6) . ?
C21 C22 1.390(6) . ?
C21 C22 1.390(6) 2_565 ?
C22 C23 1.405(8) . ?
C22 C27 1.478(9) . ?
C23 C24 1.329(11) . ?
C23 H23 0.9300 . ?
C24 C23 1.329(11) 2_565 ?
C24 H24 0.9300 . ?
C27 H271 0.9600 . ?
C27 H272 0.9600 . ?
C27 H273 0.9600 . ?
C31 C32 1.396(5) . ?
C31 C32 1.396(5) 2_565 ?
C32 C33 1.412(7) . ?
C32 C37 1.490(8) . ?
C33 C34 1.343(8) . ?
C33 H33 0.9300 . ?
C34 C33 1.343(8) 2_565 ?
C34 H34 0.9300 . ?
C37 H371 0.9600 . ?
C37 H372 0.9600 . ?
C37 H373 0.9600 . ?
C81 C85 0.21(4) 5 ?
C81 C82 1.383(16) . ?
C81 C84 1.469(18) 5 ?
C81 C84 1.469(18) 2 ?
C82 C85 1.18(3) 5 ?
C82 C84 1.335(13) 5 ?
C82 C84 1.335(13) 2 ?
C82 C83 1.382(8) . ?
C82 C83 1.382(8) 5 ?
C82 C82 1.54(3) 5 ?
C83 C84 1.327(9) . ?
C83 C84 1.327(9) 2 ?
C83 C82 1.382(8) 5 ?
C84 C82 1.335(13) 5 ?
C84 C85 1.364(9) . ?
C84 C81 1.469(18) 5 ?
C85 C81 0.21(4) 5 ?
C85 C82 1.18(3) 5 ?
C85 C84 1.364(9) 6 ?

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
N1 Rh1 N2 90.07(17) . . ?
N1 Rh1 Br1 174.88(11) . . ?
N2 Rh1 Br1 95.05(12) . . ?
N1 Rh1 Br1 94.86(12) . 5_565 ?
N2 Rh1 Br1 175.07(11) . 5_565 ?
Br1 Rh1 Br1 80.02(4) . 5_565 ?
Rh1 Br1 Rh1 99.98(4) . 5_565 ?
C12 C11 H111 109.5 . . ?
C12 C11 H112 109.5 . . ?
H111 C11 H112 109.5 . . ?
C12 C11 H113 109.5 . . ?
H111 C11 H113 109.5 . . ?
H112 C11 H113 109.5 . . ?
N1 C12 C13 124.1(5) . . ?
N1 C12 C11 119.6(5) . . ?
C13 C12 C11 116.3(5) . . ?
C12 C13 C14 126.9(5) . . ?
C12 C13 H13 116.5 . . ?
C14 C13 H13 116.5 . . ?
N2 C14 C13 123.6(5) . . ?
N2 C14 C15 119.5(5) . . ?
C13 C14 C15 116.8(5) . . ?
C14 C15 H151 109.5 . . ?
C14 C15 H152 109.5 . . ?
H151 C15 H152 109.5 . . ?
C14 C15 H153 109.5 . . ?
H151 C15 H153 109.5 . . ?
H152 C15 H153 109.5 . . ?
C12 N1 C21 116.8(4) . . ?
C12 N1 Rh1 127.5(3) . . ?
C21 N1 Rh1 115.6(3) . . ?
C14 N2 C31 116.5(4) . . ?
C14 N2 Rh1 127.7(3) . . ?
C31 N2 Rh1 115.7(3) . . ?
C22 C21 C22 122.8(6) . 2_565 ?
C22 C21 N1 118.6(3) . . ?
C22 C21 N1 118.6(3) 2_565 . ?
C21 C22 C23 116.1(7) . . ?
C21 C22 C27 121.4(5) . . ?
C23 C22 C27 122.5(7) . . ?
C24 C23 C22 121.8(9) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C23 121.4(9) 2_565 . ?
C23 C24 H24 119.3 2_565 . ?
C23 C24 H24 119.3 . . ?
C22 C27 H271 109.5 . . ?
C22 C27 H272 109.5 . . ?
H271 C27 H272 109.5 . . ?
C22 C27 H273 109.5 . . ?
H271 C27 H273 109.5 . . ?
H272 C27 H273 109.5 . . ?
C32 C31 C32 122.9(5) . 2_565 ?
C32 C31 N2 118.5(3) . . ?
C32 C31 N2 118.5(3) 2_565 . ?
C31 C32 C33 116.2(5) . . ?
C31 C32 C37 121.4(4) . . ?
C33 C32 C37 122.4(5) . . ?
C34 C33 C32 121.9(6) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C33 120.9(7) . 2_565 ?
C33 C34 H34 119.5 . . ?
C33 C34 H34 119.5 2_565 . ?
C32 C37 H371 109.5 . . ?
C32 C37 H372 109.5 . . ?
H371 C37 H372 109.5 . . ?
C32 C37 H373 109.5 . . ?
H371 C37 H373 109.5 . . ?
H372 C37 H373 109.5 . . ?
C85 C81 C82 0.013(7) 5 . ?
C85 C81 C84 55.7(7) 5 5 ?
C82 C81 C84 55.7(7) . 5 ?
C85 C81 C84 55.7(7) 5 2 ?
C82 C81 C84 55.7(7) . 2 ?
C84 C81 C84 111.5(14) 5 2 ?
C85 C82 C84 65.4(6) 5 5 ?
C85 C82 C84 65.4(6) 5 2 ?
C84 C82 C84 130.8(13) 5 2 ?
C85 C82 C81 0.002(1) 5 . ?
C84 C82 C81 65.4(6) 5 . ?
C84 C82 C81 65.4(6) 2 . ?
C85 C82 C83 123.9(6) 5 . ?
C84 C82 C83 170.7(12) 5 . ?
C84 C82 C83 58.4(4) 2 . ?
C81 C82 C83 123.8(6) . . ?
C85 C82 C83 123.8(6) 5 5 ?
C84 C82 C83 58.4(4) 5 5 ?
C84 C82 C83 170.7(12) 2 5 ?
C81 C82 C83 123.8(6) . 5 ?
C83 C82 C83 112.3(12) . 5 ?
C85 C82 C82 179.996(1) 5 5 ?
C84 C82 C82 114.6(6) 5 5 ?
C84 C82 C82 114.6(6) 2 5 ?
C81 C82 C82 180.0 . 5 ?
C83 C82 C82 56.2(6) . 5 ?
C83 C82 C82 56.2(6) 5 5 ?
C84 C83 C84 174.3(14) . 2 ?
C84 C83 C82 126.7(11) . . ?
C84 C83 C82 59.0(7) 2 . ?
C84 C83 C82 59.0(7) . 5 ?
C84 C83 C82 126.7(11) 2 5 ?
C82 C83 C82 67.7(12) . 5 ?
C83 C84 C82 62.6(6) . 5 ?
C83 C84 C85 114(2) . . ?
C82 C84 C85 51.7(17) 5 . ?
C83 C84 C81 121.4(11) . 5 ?
C82 C84 C81 58.9(7) 5 5 ?
C85 C84 C81 7.2(13) . 5 ?
C81 C85 C82 179.984(7) 5 5 ?
C81 C85 C84 117.1(14) 5 . ?
C82 C85 C84 62.9(14) 5 . ?
C81 C85 C84 117.1(14) 5 6 ?
C82 C85 C84 62.9(14) 5 6 ?
C84 C85 C84 126(3) . 6 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.095

_exptl_crystal_preparation       'Magnetic properties'
