# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Qpno_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 N4 O'
_chemical_formula_weight         448.55

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4903(8)
_cell_length_b                   10.9524(10)
_cell_length_c                   13.6734(12)
_cell_angle_alpha                70.137(5)
_cell_angle_beta                 70.544(5)
_cell_angle_gamma                77.237(4)
_cell_volume                     1251.02(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5810
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      23.46

_exptl_crystal_description       Rectangle
_exptl_crystal_colour            'Dark red'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             476
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19274
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         24.85
_reflns_number_total             4296
_reflns_number_gt                3107
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0887P)²+0.1230P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4296
_refine_ls_number_parameters     319
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1584
_refine_ls_wR_factor_gt          0.1430
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001

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
N1 N 0.24447(16) 0.45092(14) 0.65113(11) 0.0508(4) Uani 1 1 d . . .
H1A H 0.1638 0.4882 0.6324 0.061 Uiso 1 1 calc R . .
N8 N 0.05104(16) 0.63795(14) 0.70746(12) 0.0521(4) Uani 1 1 d . . .
N21 N 0.27994(17) 0.61871(14) 0.97921(12) 0.0554(4) Uani 1 1 d . . .
H21A H 0.3595 0.5832 0.9999 0.067 Uiso 1 1 calc R . .
O29 O 0.47233(15) 0.42686(14) 0.91848(11) 0.0706(4) Uani 1 1 d . . .
C2 C 0.26166(18) 0.48392(15) 0.73161(13) 0.0445(4) Uani 1 1 d . . .
C3 C 0.36860(19) 0.42976(16) 0.78552(13) 0.0501(4) Uani 1 1 d . . .
H3A H 0.4392 0.3619 0.7663 0.060 Uiso 1 1 calc R . .
C4 C 0.37549(19) 0.47334(17) 0.86939(14) 0.0497(4) Uani 1 1 d . . .
C5 C 0.26007(19) 0.58148(16) 0.90093(13) 0.0466(4) Uani 1 1 d . . .
C6 C 0.15146(19) 0.63282(16) 0.85005(13) 0.0473(4) Uani 1 1 d . . .
H6A H 0.0783 0.6978 0.8718 0.057 Uiso 1 1 calc R . .
C7 C 0.14525(18) 0.59080(15) 0.76434(13) 0.0441(4) Uani 1 1 d . . .
C9 C -0.06933(19) 0.73477(17) 0.73203(14) 0.0501(4) Uani 1 1 d . . .
C10 C -0.1804(2) 0.7140(2) 0.82791(17) 0.0709(6) Uani 1 1 d . . .
H10A H -0.1747 0.6351 0.8818 0.085 Uiso 1 1 calc R . .
C11 C -0.3007(2) 0.8084(2) 0.84581(19) 0.0776(6) Uani 1 1 d . . .
H11A H -0.3759 0.7912 0.9112 0.093 Uiso 1 1 calc R . .
C12 C -0.3124(2) 0.92725(19) 0.76959(19) 0.0658(5) Uani 1 1 d . . .
C13 C -0.2010(3) 0.9464(2) 0.67461(19) 0.0758(6) Uani 1 1 d . . .
H13A H -0.2052 1.0263 0.6217 0.091 Uiso 1 1 calc R . .
C14 C -0.0821(2) 0.85206(19) 0.65384(17) 0.0674(5) Uani 1 1 d . . .
H14A H -0.0102 0.8676 0.5867 0.081 Uiso 1 1 calc R . .
C15 C 0.3366(2) 0.36512(15) 0.59166(13) 0.0475(4) Uani 1 1 d . . .
C16 C 0.4912(2) 0.34661(17) 0.56705(14) 0.0532(5) Uani 1 1 d . . .
H16A H 0.5399 0.3853 0.5956 0.064 Uiso 1 1 calc R . .
C17 C 0.5736(2) 0.27063(17) 0.49994(15) 0.0596(5) Uani 1 1 d . . .
H17A H 0.6780 0.2583 0.4845 0.072 Uiso 1 1 calc R . .
C18 C 0.5070(3) 0.21270(18) 0.45525(16) 0.0653(5) Uani 1 1 d . . .
C19 C 0.3516(3) 0.2309(2) 0.48206(18) 0.0744(6) Uani 1 1 d . . .
H19A H 0.3029 0.1919 0.4538 0.089 Uiso 1 1 calc R . .
C20 C 0.2675(2) 0.30517(19) 0.54941(16) 0.0636(5) Uani 1 1 d . . .
H20A H 0.1630 0.3151 0.5667 0.076 Uiso 1 1 calc R . .
C22 C 0.1822(2) 0.71069(16) 1.03070(13) 0.0491(4) Uani 1 1 d . . .
C23 C 0.0288(2) 0.70912(17) 1.06661(14) 0.0547(5) Uani 1 1 d . . .
H23A H -0.0136 0.6487 1.0544 0.066 Uiso 1 1 calc R . .
C24 C -0.0623(2) 0.79649(18) 1.12050(15) 0.0590(5) Uani 1 1 d . . .
H24A H -0.1659 0.7948 1.1435 0.071 Uiso 1 1 calc R . .
C25 C -0.0031(2) 0.88676(17) 1.14115(15) 0.0595(5) Uani 1 1 d . . .
C26 C 0.1505(2) 0.88614(19) 1.10492(17) 0.0668(6) Uani 1 1 d . . .
H26A H 0.1934 0.9456 1.1178 0.080 Uiso 1 1 calc R . .
C27 C 0.2427(2) 0.80032(18) 1.05025(16) 0.0615(5) Uani 1 1 d . . .
H27A H 0.3462 0.8028 1.0264 0.074 Uiso 1 1 calc R . .
C28 C 0.5989(3) 0.1344(2) 0.3788(2) 0.0973(8) Uani 1 1 d . . .
H28A H 0.7039 0.1323 0.3701 0.146 Uiso 1 1 calc R . .
H28B H 0.5788 0.1740 0.3097 0.146 Uiso 1 1 calc R . .
H28C H 0.5726 0.0468 0.4078 0.146 Uiso 1 1 calc R . .
C30 C -0.1031(3) 0.9803(2) 1.2010(2) 0.0837(7) Uani 1 1 d . . .
H30A H -0.0430 1.0353 1.2076 0.126 Uiso 1 1 calc R . .
H30B H -0.1572 0.9321 1.2719 0.126 Uiso 1 1 calc R . .
H30C H -0.1733 1.0333 1.1619 0.126 Uiso 1 1 calc R . .
C31 C -0.4433(3) 1.0305(2) 0.7919(2) 0.0958(8) Uani 1 1 d . . .
H31A H -0.4330 1.1068 0.7302 0.144 Uiso 1 1 calc R . .
H31B H -0.4445 1.0532 0.8541 0.144 Uiso 1 1 calc R . .
H31C H -0.5357 0.9973 0.8055 0.144 Uiso 1 1 calc R . .
C33 C 0.8336(3) 0.3890(4) 0.6288(2) 0.0988(9) Uani 1 1 d . . .
C34 C 0.7921(6) 0.4655(5) 0.7002(3) 0.1134(11) Uani 1 1 d . . .
N32 N 0.8678(4) 0.3289(4) 0.5709(3) 0.1586(14) Uani 1 1 d . . .
H34C H 0.703(5) 0.534(4) 0.689(3) 0.165(16) Uiso 1 1 d . . .
H34B H 0.861(7) 0.516(6) 0.689(5) 0.26(3) Uiso 1 1 d . . .
H34A H 0.741(6) 0.425(5) 0.766(5) 0.22(2) Uiso 1 1 d . . .


_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
N1 C2 1.336(2) . ?
N1 C15 1.411(2) . ?
N8 C7 1.287(2) . ?
N8 C9 1.412(2) . ?
N21 C5 1.346(2) . ?
N21 C22 1.416(2) . ?
O29 C4 1.2355(19) . ?
C2 C3 1.364(2) . ?
C2 C7 1.499(2) . ?
C3 C4 1.408(2) . ?
C4 C5 1.499(2) . ?
C5 C6 1.348(2) . ?
C6 C7 1.419(2) . ?
C9 C10 1.365(3) . ?
C9 C14 1.376(3) . ?
C10 C11 1.377(3) . ?
C11 C12 1.373(3) . ?
C12 C13 1.359(3) . ?
C12 C31 1.508(3) . ?
C13 C14 1.375(3) . ?
C15 C16 1.375(3) . ?
C15 C20 1.377(3) . ?
C16 C17 1.378(2) . ?
C17 C18 1.369(3) . ?
C18 C19 1.382(3) . ?
C18 C28 1.503(3) . ?
C19 C20 1.371(3) . ?
C22 C27 1.376(2) . ?
C22 C23 1.375(3) . ?
C23 C24 1.377(2) . ?
C24 C25 1.383(3) . ?
C25 C26 1.374(3) . ?
C25 C30 1.497(3) . ?
C26 C27 1.373(3) . ?
C33 N32 1.120(4) . ?
C33 C34 1.402(5) . ?

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
C2 N1 C15 130.75(14) . . ?
C7 N8 C9 121.24(14) . . ?
C5 N21 C22 126.19(14) . . ?
N1 C2 C3 127.25(15) . . ?
N1 C2 C7 113.59(14) . . ?
C3 C2 C7 119.14(15) . . ?
C2 C3 C4 122.04(15) . . ?
O29 C4 C3 123.20(15) . . ?
O29 C4 C5 118.15(15) . . ?
C3 C4 C5 118.65(14) . . ?
N21 C5 C6 126.59(15) . . ?
N21 C5 C4 113.84(14) . . ?
C6 C5 C4 119.56(15) . . ?
C5 C6 C7 122.06(15) . . ?
N8 C7 C6 126.68(15) . . ?
N8 C7 C2 114.79(14) . . ?
C6 C7 C2 118.50(14) . . ?
C10 C9 C14 118.02(17) . . ?
C10 C9 N8 122.76(16) . . ?
C14 C9 N8 119.07(17) . . ?
C9 C10 C11 120.79(19) . . ?
C12 C11 C10 121.7(2) . . ?
C13 C12 C11 116.75(18) . . ?
C13 C12 C31 122.4(2) . . ?
C11 C12 C31 120.9(2) . . ?
C12 C13 C14 122.49(19) . . ?
C13 C14 C9 120.2(2) . . ?
C16 C15 C20 118.80(16) . . ?
C16 C15 N1 123.52(16) . . ?
C20 C15 N1 117.49(16) . . ?
C17 C16 C15 119.84(18) . . ?
C18 C17 C16 122.18(19) . . ?
C17 C18 C19 117.16(18) . . ?
C17 C18 C28 121.5(2) . . ?
C19 C18 C28 121.3(2) . . ?
C20 C19 C18 121.6(2) . . ?
C19 C20 C15 120.45(19) . . ?
C27 C22 C23 118.82(16) . . ?
C27 C22 N21 119.20(16) . . ?
C23 C22 N21 121.90(16) . . ?
C24 C23 C22 120.35(17) . . ?
C23 C24 C25 121.47(18) . . ?
C26 C25 C24 117.15(17) . . ?
C26 C25 C30 121.83(19) . . ?
C24 C25 C30 121.0(2) . . ?
C27 C26 C25 122.01(18) . . ?
C26 C27 C22 120.20(18) . . ?
N32 C33 C34 179.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        24.85
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.035
_database_code_depnum_ccdc_archive 'CCDC 979387'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1.EtOH

_audit_creation_method           SHELXL-97
_audit_creation_date             2012-03-08
_audit_block_code                WGT-PG-504-70
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_compound_source        'acetonitrile, ethanol'
_chemical_formula_moiety         'C27 H25 Cl2 N3 O Pd, C2 H6 O'
_chemical_formula_sum            'C29 H31 Cl2 N3 O2 Pd'
_chemical_formula_weight         630.87

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TRICLINIC
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-p 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.792(2)
_cell_length_b                   11.159(2)
_cell_length_c                   12.170(2)
_cell_angle_alpha                100.53(2)
_cell_angle_beta                 90.62(2)
_cell_angle_gamma                104.71(2)
_cell_volume                     1391.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27793
_cell_measurement_theta_min      2.6726
_cell_measurement_theta_max      31.9979

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.0700
1.00 0.00 0.00 0.0700
0.00 1.00 0.00 0.0800
0.00 -1.00 0.00 0.0800
0.00 0.00 -1.00 0.1400
1.00 0.00 3.00 0.1400
-1.00 0.00 -1.00 0.1200
1.00 0.00 -1.00 0.1300
-1.00 0.00 1.00 0.1400

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.69731
_exptl_absorpt_correction_T_max  0.82020

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 18.02
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26137
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         31.96
_reflns_number_total             9549
_reflns_number_gt                8583
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_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)+(0.0823P)²+1.1154P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9549
_refine_ls_number_parameters     347
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1309
_refine_ls_wR_factor_gt          0.1257
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_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
Pd1 Pd -0.014755(14) 0.621542(13) 0.267889(14) 0.01867(6) Uani 1 1 d . . .
Cl1 Cl 0.08276(6) 0.78928(5) 0.18967(6) 0.02903(13) Uani 1 1 d . . .
Cl2 Cl -0.13945(6) 0.73870(5) 0.36271(6) 0.02863(13) Uani 1 1 d . . .
N1 N -0.09480(18) 0.46216(17) 0.32353(17) 0.0201(3) Uani 1 1 d . . .
C2 C -0.0415(2) 0.36953(19) 0.2908(2) 0.0195(4) Uani 1 1 d . . .
C3 C -0.0687(2) 0.2537(2) 0.3316(2) 0.0221(4) Uani 1 1 d . . .
H3 H -0.1300 0.2389 0.3863 0.027 Uiso 1 1 calc R . .
C4 C -0.0057(2) 0.1647(2) 0.2913(2) 0.0226(4) Uani 1 1 d . . .
C5 C 0.0807(2) 0.1814(2) 0.1986(2) 0.0217(4) Uani 1 1 d . . .
C6 C 0.1185(2) 0.2968(2) 0.1672(2) 0.0221(4) Uani 1 1 d . . .
H6 H 0.1829 0.3109 0.1150 0.027 Uiso 1 1 calc R . .
C7 C 0.0616(2) 0.39418(19) 0.2122(2) 0.0203(4) Uani 1 1 d . . .
N8 N 0.09153(18) 0.50985(16) 0.19099(17) 0.0185(3) Uani 1 1 d . . .
C9 C 0.1932(2) 0.54497(18) 0.1193(2) 0.0196(4) Uani 1 1 d . . .
C10 C 0.1804(2) 0.4923(2) 0.0058(2) 0.0241(4) Uani 1 1 d . . .
H10 H 0.1027 0.4334 -0.0256 0.029 Uiso 1 1 calc R . .
C11 C 0.2820(2) 0.5259(2) -0.0619(2) 0.0248(4) Uani 1 1 d . . .
H11 H 0.2731 0.4891 -0.1394 0.030 Uiso 1 1 calc R . .
C12 C 0.3967(2) 0.6131(2) -0.0174(2) 0.0236(4) Uani 1 1 d . . .
C13 C 0.4060(2) 0.6660(2) 0.0964(2) 0.0262(4) Uani 1 1 d . . .
H13 H 0.4830 0.7258 0.1282 0.031 Uiso 1 1 calc R . .
C14 C 0.3052(2) 0.6332(2) 0.1643(2) 0.0238(4) Uani 1 1 d . . .
H14 H 0.3131 0.6713 0.2415 0.029 Uiso 1 1 calc R . .
C15 C -0.2038(2) 0.4391(2) 0.3903(2) 0.0205(4) Uani 1 1 d . . .
C16 C -0.3152(2) 0.3482(2) 0.3452(2) 0.0239(4) Uani 1 1 d . . .
H16 H -0.3197 0.3039 0.2702 0.029 Uiso 1 1 calc R . .
C17 C -0.4198(2) 0.3229(2) 0.4108(2) 0.0272(5) Uani 1 1 d . . .
H17 H -0.4961 0.2614 0.3797 0.033 Uiso 1 1 calc R . .
C18 C -0.4151(2) 0.3859(2) 0.5214(2) 0.0269(5) Uani 1 1 d . . .
C19 C -0.3041(3) 0.4786(2) 0.5634(2) 0.0273(5) Uani 1 1 d . . .
H19 H -0.2998 0.5237 0.6381 0.033 Uiso 1 1 calc R . .
C20 C -0.1991(2) 0.5066(2) 0.4988(2) 0.0242(4) Uani 1 1 d . . .
H20 H -0.1247 0.5714 0.5285 0.029 Uiso 1 1 calc R . .
N21 N 0.1210(2) 0.07867(17) 0.15489(19) 0.0239(4) Uani 1 1 d D . .
H21 H 0.085(3) 0.019(3) 0.189(3) 0.029 Uiso 1 1 d D . .
C22 C 0.1878(2) 0.0624(2) 0.0563(2) 0.0235(4) Uani 1 1 d . . .
C23 C 0.1639(2) 0.1131(2) -0.0367(2) 0.0277(5) Uani 1 1 d . . .
H23 H 0.1023 0.1610 -0.0339 0.033 Uiso 1 1 calc R . .
C24 C 0.2298(3) 0.0935(2) -0.1326(2) 0.0310(5) Uani 1 1 d . . .
H24 H 0.2148 0.1304 -0.1943 0.037 Uiso 1 1 calc R . .
C25 C 0.3175(3) 0.0209(2) -0.1399(2) 0.0303(5) Uani 1 1 d . . .
C26 C 0.3372(3) -0.0333(2) -0.0482(3) 0.0315(5) Uani 1 1 d . . .
H26 H 0.3945 -0.0858 -0.0530 0.038 Uiso 1 1 calc R . .
C27 C 0.2744(2) -0.0116(2) 0.0494(2) 0.0275(5) Uani 1 1 d . . .
H27 H 0.2905 -0.0473 0.1115 0.033 Uiso 1 1 calc R . .
C28 C -0.5277(3) 0.3540(3) 0.5927(3) 0.0357(6) Uani 1 1 d . . .
H28A H -0.5302 0.2744 0.6170 0.054 Uiso 1 1 calc R . .
H28B H -0.6074 0.3452 0.5490 0.054 Uiso 1 1 calc R . .
H28C H -0.5188 0.4216 0.6585 0.054 Uiso 1 1 calc R . .
O29 O -0.01396(18) 0.05946(15) 0.32921(17) 0.0273(4) Uani 1 1 d D . .
H29 H -0.053(3) 0.064(4) 0.391(2) 0.041 Uiso 1 1 d D . .
C30 C 0.3886(4) 0.0002(3) -0.2439(3) 0.0425(7) Uani 1 1 d . . .
H30A H 0.3322 -0.0639 -0.3015 0.064 Uiso 1 1 calc R . .
H30B H 0.4640 -0.0284 -0.2268 0.064 Uiso 1 1 calc R . .
H30C H 0.4162 0.0796 -0.2714 0.064 Uiso 1 1 calc R . .
C31 C 0.5093(2) 0.6475(3) -0.0885(2) 0.0301(5) Uani 1 1 d . . .
H31A H 0.5354 0.7393 -0.0830 0.045 Uiso 1 1 calc R . .
H31B H 0.4845 0.6064 -0.1667 0.045 Uiso 1 1 calc R . .
H31C H 0.5811 0.6192 -0.0620 0.045 Uiso 1 1 calc R . .
O50 O -0.12523(19) 0.07470(19) 0.51458(17) 0.0318(4) Uani 1 1 d D . .
H50 H -0.088(4) 0.115(4) 0.577(2) 0.048 Uiso 1 1 d D . .
C51 C -0.2397(3) -0.0097(3) 0.5402(3) 0.0326(5) Uani 1 1 d . . .
H51A H -0.2188 -0.0536 0.5988 0.039 Uiso 1 1 calc R . .
H51B H -0.2750 -0.0743 0.4725 0.039 Uiso 1 1 calc R . .
C52 C -0.3392(3) 0.0573(4) 0.5801(3) 0.0487(8) Uani 1 1 d . . .
H52A H -0.3096 0.1126 0.6528 0.073 Uiso 1 1 calc R . .
H52B H -0.4195 -0.0047 0.5877 0.073 Uiso 1 1 calc R . .
H52C H -0.3536 0.1081 0.5258 0.073 Uiso 1 1 calc R . .


_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
Pd1 N1 2.0101(18) . ?
Pd1 N8 2.0170(19) . ?
Pd1 Cl1 2.2781(7) . ?
Pd1 Cl2 2.2863(8) . ?
N1 C2 1.309(3) . ?
N1 C15 1.433(3) . ?
C2 C3 1.431(3) . ?
C2 C7 1.481(3) . ?
C3 C4 1.364(3) . ?
C4 O29 1.321(2) . ?
C4 C5 1.479(3) . ?
C5 N21 1.350(3) . ?
C5 C6 1.374(3) . ?
C6 C7 1.409(3) . ?
C7 N8 1.322(2) . ?
N8 C9 1.430(3) . ?
C9 C14 1.384(3) . ?
C9 C10 1.390(3) . ?
C10 C11 1.395(3) . ?
C11 C12 1.398(3) . ?
C12 C13 1.395(4) . ?
C12 C31 1.510(3) . ?
C13 C14 1.389(3) . ?
C15 C20 1.388(3) . ?
C15 C16 1.393(3) . ?
C16 C17 1.390(3) . ?
C17 C18 1.394(4) . ?
C18 C19 1.390(4) . ?
C18 C28 1.508(4) . ?
C19 C20 1.389(3) . ?
N21 C22 1.413(3) . ?
C22 C27 1.389(3) . ?
C22 C23 1.403(3) . ?
C23 C24 1.386(4) . ?
C24 C25 1.387(4) . ?
C25 C26 1.401(4) . ?
C25 C30 1.499(4) . ?
C26 C27 1.388(4) . ?
O50 C51 1.427(3) . ?
C51 C52 1.495(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
N1 Pd1 N8 80.49(8) . . ?
N1 Pd1 Cl1 174.04(6) . . ?
N8 Pd1 Cl1 94.01(5) . . ?
N1 Pd1 Cl2 95.85(6) . . ?
N8 Pd1 Cl2 176.19(5) . . ?
Cl1 Pd1 Cl2 89.69(3) . . ?
C2 N1 C15 117.97(18) . . ?
C2 N1 Pd1 114.60(15) . . ?
C15 N1 Pd1 127.40(14) . . ?
N1 C2 C3 125.1(2) . . ?
N1 C2 C7 115.62(18) . . ?
C3 C2 C7 119.11(19) . . ?
C4 C3 C2 119.4(2) . . ?
O29 C4 C3 125.0(2) . . ?
O29 C4 C5 114.26(19) . . ?
C3 C4 C5 120.70(19) . . ?
N21 C5 C6 125.2(2) . . ?
N21 C5 C4 114.75(18) . . ?
C6 C5 C4 120.0(2) . . ?
C5 C6 C7 120.1(2) . . ?
N8 C7 C6 125.9(2) . . ?
N8 C7 C2 114.72(19) . . ?
C6 C7 C2 119.34(18) . . ?
C7 N8 C9 119.23(18) . . ?
C7 N8 Pd1 114.42(15) . . ?
C9 N8 Pd1 126.35(13) . . ?
C14 C9 C10 120.0(2) . . ?
C14 C9 N8 119.1(2) . . ?
C10 C9 N8 120.9(2) . . ?
C9 C10 C11 119.9(2) . . ?
C10 C11 C12 120.9(2) . . ?
C13 C12 C11 118.0(2) . . ?
C13 C12 C31 120.3(2) . . ?
C11 C12 C31 121.7(2) . . ?
C14 C13 C12 121.5(2) . . ?
C9 C14 C13 119.8(2) . . ?
C20 C15 C16 120.1(2) . . ?
C20 C15 N1 120.7(2) . . ?
C16 C15 N1 119.3(2) . . ?
C17 C16 C15 119.5(2) . . ?
C16 C17 C18 121.3(2) . . ?
C19 C18 C17 118.1(2) . . ?
C19 C18 C28 121.3(3) . . ?
C17 C18 C28 120.6(2) . . ?
C20 C19 C18 121.5(2) . . ?
C15 C20 C19 119.5(2) . . ?
C5 N21 C22 126.35(19) . . ?
C27 C22 C23 119.3(2) . . ?
C27 C22 N21 118.8(2) . . ?
C23 C22 N21 121.9(2) . . ?
C24 C23 C22 120.2(2) . . ?
C23 C24 C25 120.9(3) . . ?
C24 C25 C26 118.4(3) . . ?
C24 C25 C30 120.7(3) . . ?
C26 C25 C30 120.9(3) . . ?
C27 C26 C25 121.2(2) . . ?
C26 C27 C22 119.9(2) . . ?
O50 C51 C52 112.1(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N21 H21 O29 0.863(18) 2.06(3) 2.597(3) 119(3) .
N21 H21 Cl1 0.863(18) 2.56(3) 3.2563(19) 139(3) 1_545
O29 H29 O50 0.866(18) 1.700(19) 2.566(3) 178(4) .
O50 H50 Cl2 0.845(18) 2.59(3) 3.237(2) 134(3) 2_566

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        31.96
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.253
_refine_diff_density_min         -4.017
_refine_diff_density_rms         0.158
_database_code_depnum_ccdc_archive 'CCDC 979388'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H27 Cl3 N2 P Rh'
_chemical_formula_weight         619.74

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.9397(5)
_cell_length_b                   9.5342(3)
_cell_length_c                   19.3761(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.7200(10)
_cell_angle_gamma                90.00
_cell_volume                     2695.87(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9968
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      25.39

_exptl_crystal_description       paralleopiped
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20744
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         25.48
_reflns_number_total             3730
_reflns_number_gt                3097
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0945P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3730
_refine_ls_number_parameters     312
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1331
_refine_ls_wR_factor_gt          0.1263
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_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
Rh Rh 0.37844(3) 1.25815(3) 0.02194(2) 0.02902(17) Uani 1 1 d . . .
Cl1 Cl 0.36944(9) 1.00709(12) 0.01945(7) 0.0456(3) Uani 1 1 d . . .
Cl2 Cl 0.36189(10) 1.27620(12) -0.10198(7) 0.0400(3) Uani 1 1 d . . .
Cl3 Cl 0.40421(8) 1.50189(11) 0.04505(7) 0.0391(3) Uani 1 1 d . . .
N10 N 0.4060(3) 1.2409(4) 0.1327(3) 0.0397(11) Uani 1 1 d . . .
C11 C 0.4331(5) 1.2294(6) 0.1946(4) 0.0508(14) Uani 1 1 d . . .
C12 C 0.4717(7) 1.2185(11) 0.2782(4) 0.097(3) Uani 1 1 d . . .
H12A H 0.5038 1.1311 0.2935 0.145 Uiso 1 1 calc R . .
H12B H 0.4229 1.2225 0.2952 0.145 Uiso 1 1 calc R . .
H12C H 0.5134 1.2948 0.2998 0.145 Uiso 1 1 calc R . .
N20 N 0.5230(3) 1.2426(3) 0.0467(3) 0.0349(9) Uani 1 1 d . . .
H20A H 0.5311 1.1656 0.0232 0.042 Uiso 1 1 calc R . .
H20B H 0.5380 1.3170 0.0254 0.042 Uiso 1 1 calc R . .
C21 C 0.5879(4) 1.2358(4) 0.1242(3) 0.0388(11) Uani 1 1 d . A .
C22 C 0.6124(4) 1.1082(5) 0.1602(3) 0.0487(13) Uani 1 1 d . . .
H22 H 0.5915 1.0251 0.1337 0.058 Uiso 1 1 calc R . .
C23 C 0.6682(5) 1.1055(6) 0.2361(4) 0.0627(16) Uani 1 1 d . A .
H23 H 0.6836 1.0194 0.2605 0.075 Uiso 1 1 calc R . .
C24 C 0.7017(5) 1.2252(7) 0.2764(4) 0.0640(17) Uani 1 1 d D . .
C25 C 0.6783(5) 1.3510(6) 0.2400(4) 0.0601(15) Uani 1 1 d . A .
H25 H 0.7011 1.4332 0.2668 0.072 Uiso 1 1 calc R . .
C26 C 0.6213(4) 1.3591(5) 0.1637(3) 0.0457(12) Uani 1 1 d . . .
H26 H 0.6059 1.4456 0.1396 0.055 Uiso 1 1 calc R A .
C27 C 0.747(4) 1.240(4) 0.3653(7) 0.090(7) Uani 0.46(5) 1 d PD A 1
H27A H 0.7615 1.1489 0.3878 0.135 Uiso 0.46(5) 1 calc PR A 1
H27B H 0.7044 1.2856 0.3819 0.135 Uiso 0.46(5) 1 calc PR A 1
H27C H 0.8016 1.2953 0.3801 0.135 Uiso 0.46(5) 1 calc PR A 1
C27' C 0.772(3) 1.203(4) 0.3610(9) 0.090(7) Uani 0.54(5) 1 d PD A 2
H27D H 0.7763 1.1053 0.3730 0.135 Uiso 0.54(5) 1 calc PR A 2
H27E H 0.7502 1.2530 0.3939 0.135 Uiso 0.54(5) 1 calc PR A 2
H27F H 0.8307 1.2387 0.3674 0.135 Uiso 0.54(5) 1 calc PR A 2
P30 P 0.22161(9) 1.27862(11) -0.01885(7) 0.0302(3) Uani 1 1 d . . .
C51 C 0.1769(3) 1.4575(4) -0.0422(2) 0.0340(9) Uani 1 1 d . . .
C52 C 0.2100(3) 1.5407(5) -0.0857(3) 0.0432(11) Uani 1 1 d . . .
H52 H 0.2537 1.5047 -0.1014 0.052 Uiso 1 1 calc R . .
C53 C 0.1778(4) 1.6764(5) -0.1054(3) 0.0492(12) Uani 1 1 d . . .
H53 H 0.2005 1.7315 -0.1336 0.059 Uiso 1 1 calc R . .
C54 C 0.1121(5) 1.7296(5) -0.0831(4) 0.0503(14) Uani 1 1 d . . .
H54 H 0.0904 1.8205 -0.0962 0.060 Uiso 1 1 calc R . .
C55 C 0.0793(4) 1.6478(5) -0.0417(3) 0.0521(12) Uani 1 1 d . . .
H55 H 0.0342 1.6833 -0.0275 0.063 Uiso 1 1 calc R . .
C56 C 0.1112(3) 1.5152(5) -0.0207(3) 0.0435(11) Uani 1 1 d . . .
H56 H 0.0886 1.4626 0.0084 0.052 Uiso 1 1 calc R . .
C41 C 0.1480(3) 1.1861(5) -0.1047(2) 0.0379(10) Uani 1 1 d . . .
C42 C 0.0543(4) 1.2236(5) -0.1394(3) 0.0452(12) Uani 1 1 d . . .
H42 H 0.0316 1.2929 -0.1178 0.054 Uiso 1 1 calc R . .
C43 C -0.0026(4) 1.1600(6) -0.2035(3) 0.0556(13) Uani 1 1 d . . .
H43 H -0.0640 1.1857 -0.2252 0.067 Uiso 1 1 calc R . .
C44 C 0.0295(4) 1.0567(6) -0.2374(3) 0.0564(14) Uani 1 1 d . . .
H44 H -0.0096 1.0148 -0.2821 0.068 Uiso 1 1 calc R . .
C45 C 0.1198(4) 1.0176(5) -0.2039(3) 0.0489(12) Uani 1 1 d . . .
H45 H 0.1417 0.9472 -0.2255 0.059 Uiso 1 1 calc R . .
C46 C 0.1789(3) 1.0821(5) -0.1379(3) 0.0428(11) Uani 1 1 d . . .
H46 H 0.2400 1.0547 -0.1160 0.051 Uiso 1 1 calc R . .
C31 C 0.1836(3) 1.2213(5) 0.0536(3) 0.0357(10) Uani 1 1 d . . .
C32 C 0.1312(3) 1.0989(5) 0.0444(3) 0.0445(11) Uani 1 1 d . . .
H32 H 0.1128 1.0472 0.0000 0.053 Uiso 1 1 calc R . .
C33 C 0.1073(4) 1.0560(6) 0.1029(3) 0.0580(14) Uani 1 1 d . . .
H33 H 0.0730 0.9747 0.0975 0.070 Uiso 1 1 calc R . .
C34 C 0.1335(4) 1.1313(6) 0.1676(3) 0.0601(15) Uani 1 1 d . . .
H34 H 0.1157 1.1024 0.2055 0.072 Uiso 1 1 calc R . .
C35 C 0.1871(6) 1.2522(5) 0.1776(4) 0.0577(18) Uani 1 1 d . . .
H35 H 0.2072 1.3018 0.2227 0.069 Uiso 1 1 calc R . .
C36 C 0.2094(4) 1.2961(5) 0.1191(3) 0.0439(11) Uani 1 1 d . . .
H36 H 0.2427 1.3785 0.1245 0.053 Uiso 1 1 calc R . .


_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
Rh N10 2.017(4) . ?
Rh N20 2.162(4) . ?
Rh P30 2.3070(13) . ?
Rh Cl2 2.3141(11) . ?
Rh Cl3 2.3710(11) . ?
Rh Cl1 2.3973(12) . ?
N10 C11 1.104(8) . ?
C11 C12 1.487(9) . ?
N20 C21 1.441(8) . ?
C21 C22 1.379(7) . ?
C21 C26 1.387(7) . ?
C22 C23 1.379(9) . ?
C23 C24 1.365(9) . ?
C24 C25 1.364(9) . ?
C24 C27' 1.581(13) . ?
C24 C27 1.583(14) . ?
C25 C26 1.392(9) . ?
P30 C31 1.822(4) . ?
P30 C41 1.831(5) . ?
P30 C51 1.833(4) . ?
C51 C56 1.386(6) . ?
C51 C52 1.407(6) . ?
C52 C53 1.387(7) . ?
C53 C54 1.380(8) . ?
C54 C55 1.365(8) . ?
C55 C56 1.362(7) . ?
C41 C46 1.377(6) . ?
C41 C42 1.415(8) . ?
C42 C43 1.352(8) . ?
C43 C44 1.391(8) . ?
C44 C45 1.371(8) . ?
C45 C46 1.390(7) . ?
C31 C36 1.368(7) . ?
C31 C32 1.404(6) . ?
C32 C33 1.395(6) . ?
C33 C34 1.356(8) . ?
C34 C35 1.401(8) . ?
C35 C36 1.383(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
N10 Rh N20 90.09(18) . . ?
N10 Rh P30 96.54(14) . . ?
N20 Rh P30 173.35(11) . . ?
N10 Rh Cl2 174.45(14) . . ?
N20 Rh Cl2 84.36(12) . . ?
P30 Rh Cl2 89.01(4) . . ?
N10 Rh Cl3 86.08(11) . . ?
N20 Rh Cl3 86.38(9) . . ?
P30 Rh Cl3 93.63(4) . . ?
Cl2 Rh Cl3 93.55(4) . . ?
N10 Rh Cl1 85.75(10) . . ?
N20 Rh Cl1 89.20(9) . . ?
P30 Rh Cl1 91.70(4) . . ?
Cl2 Rh Cl1 94.15(4) . . ?
Cl3 Rh Cl1 170.70(4) . . ?
C11 N10 Rh 170.5(5) . . ?
N10 C11 C12 177.9(8) . . ?
C21 N20 Rh 119.2(3) . . ?
C22 C21 C26 120.1(6) . . ?
C22 C21 N20 120.3(5) . . ?
C26 C21 N20 119.5(4) . . ?
C21 C22 C23 119.1(5) . . ?
C24 C23 C22 122.1(5) . . ?
C25 C24 C23 118.4(7) . . ?
C25 C24 C27' 125.7(15) . . ?
C23 C24 C27' 115.7(15) . . ?
C25 C24 C27 113.1(16) . . ?
C23 C24 C27 126.9(17) . . ?
C27' C24 C27 20.4(18) . . ?
C24 C25 C26 121.6(6) . . ?
C21 C26 C25 118.8(5) . . ?
C31 P30 C41 105.4(2) . . ?
C31 P30 C51 104.60(19) . . ?
C41 P30 C51 100.4(2) . . ?
C31 P30 Rh 111.18(18) . . ?
C41 P30 Rh 118.72(15) . . ?
C51 P30 Rh 115.06(15) . . ?
C56 C51 C52 117.8(4) . . ?
C56 C51 P30 124.2(3) . . ?
C52 C51 P30 118.0(3) . . ?
C53 C52 C51 120.3(4) . . ?
C54 C53 C52 120.0(4) . . ?
C55 C54 C53 119.5(5) . . ?
C56 C55 C54 121.3(5) . . ?
C55 C56 C51 121.1(4) . . ?
C46 C41 C42 117.9(4) . . ?
C46 C41 P30 123.6(4) . . ?
C42 C41 P30 118.5(3) . . ?
C43 C42 C41 120.8(5) . . ?
C42 C43 C44 120.9(5) . . ?
C45 C44 C43 119.0(5) . . ?
C44 C45 C46 120.6(4) . . ?
C41 C46 C45 120.7(5) . . ?
C36 C31 C32 119.6(4) . . ?
C36 C31 P30 119.3(3) . . ?
C32 C31 P30 121.1(4) . . ?
C33 C32 C31 118.9(5) . . ?
C34 C33 C32 120.9(5) . . ?
C33 C34 C35 120.5(4) . . ?
C36 C35 C34 118.6(6) . . ?
C31 C36 C35 121.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.745
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.740
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.098
_database_code_depnum_ccdc_archive 'CCDC 979389'
