# 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_Bak027
_database_code_depnum_ccdc_archive 'CCDC 1015594'
_audit_update_record             
;
2014-07-23 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N6 O4 Rh, Cl O4'
_chemical_formula_sum            'C16 H36 Cl N6 O8 Rh'
_chemical_formula_weight         578.87

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5412(7)
_cell_length_b                   9.4943(11)
_cell_length_c                   10.1892(12)
_cell_angle_alpha                68.6050(10)
_cell_angle_beta                 75.6380(10)
_cell_angle_gamma                83.364(2)
_cell_volume                     570.55(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4653
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      30.64

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.921
_shelx_estimated_absorpt_T_min   0.757
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_process_details   'BRUKER SADABS'

_exptl_special_details           
; 
A X-ray quality crystal was selected under ambient conditions
and covered with PARATONE oil
The crystal was mounted and centered in the X-ray beam by
using a video camera.The crystal evaluation and data
collection were performed on APEX-2 CCD diffractometer
with the detector to crystal distance of 5cm. 
The initial cell constants were obtained from three series of
OMEGA scans at different starting angles. Each series consisted
of 30 frames collected at intervals of 0.3 in a 10 range about
OMEGA with the exposure time of 10 seconds per frame. The 
obtained reflections were successfully indexed by an automated
indexing routine built to APEX2 program package. The final cell 
constants were calculated from a set of strong reflections from
the actual data collection.  

The data were collected using the full sphere routine by
collecting four sets of frames with 0.3 scans in ω with an
exposure time 10 sec per frame till resolution of 0.69 Å. 
Data were truncated to the resolution with  statistically 
reasonable R~σ~.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6453
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.202
_diffrn_reflns_theta_max         30.638
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3257
_reflns_number_gt                3222
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX2 Suite (Bruker AXS, 2013)'
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2013)'

_refine_special_details          
; 
The systematic absences in the diffraction data were consistent for the
stated space group. The position of almost all non-hydrogen atoms
were found by direct methods. The remaining atoms were located in an 
alternating series of least-squares cycles on difference Fourier maps.
All non-hydrogen atoms were refined in full-matrix anisotropic approximation.


All expected hydrogen atoms were placed on a calculated positions and were
 refined in isotropic approximation using "riding" model. The Uiso(H)
 values have been set at 1.2  - 1.5  times the Ueq value of the
 carrier atom.

Perchlorate counter-ion is disordered by inversion center and it was
geometrically restrained to make all CL - O and 
O - O distances equal. All displacement parameters were also restrained
 to be  the same for perchlorate oxygen atoms.

Final results were tested with CHECKCIF routine and all A-warnings (if any)
were addressed on the very top of this file.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0457P)²+0.5992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3257
_refine_ls_number_parameters     155
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0812
_refine_ls_wR_factor_gt          0.0807
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.5000 0.5000 0.0000 0.01578(7) Uani 1 2 d S . P . .
C1 C 0.6020(4) 0.2450(3) 0.2411(2) 0.0275(4) Uani 1 1 d . . . . .
H1A H 0.5528 0.1609 0.3327 0.033 Uiso 1 1 calc R U . . .
H1B H 0.7318 0.2847 0.2467 0.033 Uiso 1 1 calc R U . . .
C2 C 0.3973(4) 0.4527(3) 0.3201(2) 0.0230(4) Uani 1 1 d . . . . .
H2 H 0.5272 0.5093 0.3019 0.028 Uiso 1 1 calc R U . . .
C3 C 0.3508(5) 0.3457(3) 0.4771(3) 0.0371(6) Uani 1 1 d . . . . .
H3A H 0.2325 0.2821 0.4939 0.056 Uiso 1 1 calc R U . . .
H3B H 0.3142 0.4049 0.5413 0.056 Uiso 1 1 calc R U . . .
H3C H 0.4760 0.2814 0.4970 0.056 Uiso 1 1 calc R U . . .
C4 C 0.2136(3) 0.5669(3) 0.2913(2) 0.0243(4) Uani 1 1 d . . . . .
H4A H 0.1574 0.5936 0.3791 0.029 Uiso 1 1 calc R U . . .
H4B H 0.1003 0.5147 0.2796 0.029 Uiso 1 1 calc R U . . .
C5 C 0.2542(4) 0.7157(3) 0.1611(2) 0.0238(4) Uani 1 1 d . . . . .
C6 C 0.0540(4) 0.8170(3) 0.1675(3) 0.0360(6) Uani 1 1 d . . . . .
H6A H 0.0786 0.9137 0.0870 0.054 Uiso 1 1 calc R U . . .
H6B H 0.0189 0.8353 0.2593 0.054 Uiso 1 1 calc R U . . .
H6C H -0.0632 0.7666 0.1602 0.054 Uiso 1 1 calc R U . . .
C7 C 0.4353(4) 0.7994(3) 0.1679(3) 0.0300(5) Uani 1 1 d . . . . .
H7A H 0.5661 0.7382 0.1602 0.045 Uiso 1 1 calc R U . . .
H7B H 0.4031 0.8170 0.2599 0.045 Uiso 1 1 calc R U . . .
H7C H 0.4528 0.8967 0.0878 0.045 Uiso 1 1 calc R U . . .
C8 C 0.3524(4) 0.8110(2) -0.1149(2) 0.0266(4) Uani 1 1 d . . . . .
H8A H 0.4785 0.8596 -0.1152 0.032 Uiso 1 1 calc R U . . .
H8B H 0.2346 0.8869 -0.1235 0.032 Uiso 1 1 calc R U . . .
N1 N 0.4352(3) 0.3674(2) 0.21815(19) 0.0208(3) Uani 1 1 d . . . . .
H1 H 0.3101 0.3196 0.2356 0.025 Uiso 1 1 d . U . . .
N2 N 0.2949(3) 0.6796(2) 0.02303(19) 0.0206(3) Uani 1 1 d . . . . .
H2A H 0.1644 0.6512 0.0215 0.025 Uiso 1 1 d . U . . .
N3 N 0.7573(3) 0.5979(2) 0.0114(2) 0.0233(3) Uani 1 1 d . . . . .
O1 O 0.8470(3) 0.5359(2) 0.1133(2) 0.0315(4) Uani 1 1 d . . . . .
O2 O 0.8303(3) 0.7163(2) -0.0846(2) 0.0345(4) Uani 1 1 d . . . . .
Cl1 Cl 1.0202(3) 0.96650(15) 0.51439(19) 0.0395(3) Uani 0.5 1 d D . P A -1
O4 O 1.1249(11) 1.0063(7) 0.6024(7) 0.0735(8) Uani 0.5 1 d D . P A -1
O3 O 0.7927(10) 0.9806(7) 0.5703(7) 0.0735(8) Uani 0.5 1 d D . P A -1
O5 O 1.0760(11) 1.0689(7) 0.3687(7) 0.0735(8) Uani 0.5 1 d D . P A -1
O6 O 1.0783(11) 0.8122(7) 0.5261(7) 0.0735(8) Uani 0.5 1 d D . P A -1


_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 N3 2.0611(18) 2_665 ?
Rh1 N3 2.0611(18) . ?
Rh1 N1 2.0784(17) . ?
Rh1 N1 2.0784(17) 2_665 ?
Rh1 N2 2.0904(18) . ?
Rh1 N2 2.0905(18) 2_665 ?
C1 N1 1.494(3) . ?
C1 C8 1.515(3) 2_665 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.495(3) . ?
C2 C3 1.526(3) . ?
C2 C4 1.533(3) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.540(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.521(3) . ?
C5 C7 1.529(3) . ?
C5 C6 1.534(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N2 1.497(3) . ?
C8 C1 1.515(3) 2_665 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
N1 H1 0.9284 . ?
N2 H2A 0.9293 . ?
N3 O2 1.240(3) . ?
N3 O1 1.243(2) . ?
Cl1 O4 1.424(6) . ?
Cl1 O5 1.429(7) . ?
Cl1 O6 1.439(6) . ?
Cl1 O3 1.465(7) . ?

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
N3 Rh1 N3 180.0 2_665 . ?
N3 Rh1 N1 85.99(7) 2_665 . ?
N3 Rh1 N1 94.01(7) . . ?
N3 Rh1 N1 94.01(7) 2_665 2_665 ?
N3 Rh1 N1 85.99(7) . 2_665 ?
N1 Rh1 N1 180.0 . 2_665 ?
N3 Rh1 N2 86.71(7) 2_665 . ?
N3 Rh1 N2 93.29(7) . . ?
N1 Rh1 N2 95.74(7) . . ?
N1 Rh1 N2 84.27(7) 2_665 . ?
N3 Rh1 N2 93.29(7) 2_665 2_665 ?
N3 Rh1 N2 86.71(7) . 2_665 ?
N1 Rh1 N2 84.27(7) . 2_665 ?
N1 Rh1 N2 95.73(7) 2_665 2_665 ?
N2 Rh1 N2 180.0 . 2_665 ?
N1 C1 C8 108.14(18) . 2_665 ?
N1 C1 H1A 110.1 . . ?
C8 C1 H1A 110.1 2_665 . ?
N1 C1 H1B 110.1 . . ?
C8 C1 H1B 110.1 2_665 . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C3 111.25(19) . . ?
N1 C2 C4 109.38(17) . . ?
C3 C2 C4 110.41(19) . . ?
N1 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
C4 C2 H2 108.6 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 C5 118.87(18) . . ?
C2 C4 H4A 107.6 . . ?
C5 C4 H4A 107.6 . . ?
C2 C4 H4B 107.6 . . ?
C5 C4 H4B 107.6 . . ?
H4A C4 H4B 107.0 . . ?
N2 C5 C7 112.80(18) . . ?
N2 C5 C6 108.18(18) . . ?
C7 C5 C6 108.2(2) . . ?
N2 C5 C4 108.58(17) . . ?
C7 C5 C4 110.64(18) . . ?
C6 C5 C4 108.3(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C1 109.03(18) . 2_665 ?
N2 C8 H8A 109.9 . . ?
C1 C8 H8A 109.9 2_665 . ?
N2 C8 H8B 109.9 . . ?
C1 C8 H8B 109.9 2_665 . ?
H8A C8 H8B 108.3 . . ?
C1 N1 C2 114.83(17) . . ?
C1 N1 Rh1 107.72(13) . . ?
C2 N1 Rh1 115.24(13) . . ?
C1 N1 H1 106.1 . . ?
C2 N1 H1 106.1 . . ?
Rh1 N1 H1 106.1 . . ?
C8 N2 C5 115.64(17) . . ?
C8 N2 Rh1 106.63(13) . . ?
C5 N2 Rh1 119.95(13) . . ?
C8 N2 H2A 104.3 . . ?
C5 N2 H2A 104.3 . . ?
Rh1 N2 H2A 104.3 . . ?
O2 N3 O1 118.57(19) . . ?
O2 N3 Rh1 121.22(15) . . ?
O1 N3 Rh1 120.17(15) . . ?
O4 Cl1 O5 109.5(4) . . ?
O4 Cl1 O6 108.3(4) . . ?
O5 Cl1 O6 112.2(4) . . ?
O4 Cl1 O3 107.4(4) . . ?
O5 Cl1 O3 109.3(3) . . ?
O6 Cl1 O3 110.1(4) . . ?

_refine_diff_density_max         1.085
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.097

_shelxl_version_number           2014-3

