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#  experimental, refinement, atomic coordinates,
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#  as required by the journal to which it was submitted.
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data_delta-(R)-3

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C39 H40 N3 O4 Rh), 3(C H2 Cl2)'
_chemical_formula_sum            'C81 H86 Cl6 N6 O8 Rh2'
_chemical_formula_weight         1690.07

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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.919(6)
_cell_length_b                   19.144(9)
_cell_length_c                   28.616(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7625(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9357
_cell_measurement_theta_min      2.3020
_cell_measurement_theta_max      25.7262

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             3480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.704
_shelx_estimated_absorpt_T_min   0.747
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            64188
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.302
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14187
_reflns_number_gt                12148
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'BRUKER APEX2'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  ?

_refine_special_details          
; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0255P)²+4.1982P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 4954 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.020(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         14187
_refine_ls_number_parameters     996
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.027
_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_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
C2 C 0.6924(4) 0.7451(3) 0.39041(17) 0.0161(12) Uani 1 1 d . . . . .
C4 C 0.7118(4) 0.6344(3) 0.40030(17) 0.0153(12) Uani 1 1 d . . . . .
C5 C 0.7481(4) 0.5692(3) 0.40752(17) 0.0199(13) Uani 1 1 d . . . . .
H5 H 0.8142 0.5611 0.4136 0.024 Uiso 1 1 calc R U . . .
C6 C 0.6808(4) 0.5153(3) 0.40531(16) 0.0201(12) Uani 1 1 d . . . . .
H6 H 0.7027 0.4687 0.4097 0.024 Uiso 1 1 calc R U . . .
C7 C 0.5836(4) 0.5261(2) 0.39703(16) 0.0167(12) Uani 1 1 d . . . . .
C8 C 0.5498(4) 0.5941(2) 0.39020(15) 0.0134(11) Uani 1 1 d . . . . .
H8 H 0.4836 0.6031 0.3849 0.016 Uiso 1 1 calc R U . . .
C9 C 0.6155(4) 0.6472(2) 0.39142(16) 0.0135(11) Uani 1 1 d . . . . .
C10 C 0.7073(4) 0.8188(2) 0.38485(16) 0.0148(11) Uani 1 1 d . . . . .
C11 C 0.6204(3) 0.8529(2) 0.37417(17) 0.0144(11) Uani 1 1 d . . . . .
C12 C 0.6273(4) 0.9250(3) 0.36825(17) 0.0166(11) Uani 1 1 d . . . . .
H12 H 0.5710 0.9511 0.3614 0.020 Uiso 1 1 calc R U . . .
C13 C 0.7144(4) 0.9592(3) 0.37213(18) 0.0210(12) Uani 1 1 d . . . . .
H13 H 0.7166 1.0085 0.3682 0.025 Uiso 1 1 calc R U . . .
C14 C 0.7984(4) 0.9235(3) 0.38161(18) 0.0204(12) Uani 1 1 d . . . . .
H14 H 0.8577 0.9479 0.3836 0.024 Uiso 1 1 calc R U . . .
C15 C 0.7958(4) 0.8523(3) 0.38815(17) 0.0197(12) Uani 1 1 d . . . . .
H15 H 0.8527 0.8267 0.3947 0.024 Uiso 1 1 calc R U . . .
C16 C 0.5110(4) 0.4666(2) 0.39814(17) 0.0229(13) Uani 1 1 d . . . . .
C17 C 0.4410(5) 0.4719(3) 0.3563(2) 0.0364(17) Uani 1 1 d . . . . .
H17A H 0.3991 0.4308 0.3558 0.055 Uiso 1 1 calc R U . . .
H17B H 0.4777 0.4742 0.3271 0.055 Uiso 1 1 calc R U . . .
H17C H 0.4018 0.5142 0.3595 0.055 Uiso 1 1 calc R U . . .
C18 C 0.4541(4) 0.4716(3) 0.44382(19) 0.0273(13) Uani 1 1 d . . . . .
H18A H 0.4047 0.4352 0.4444 0.041 Uiso 1 1 calc R U . . .
H18B H 0.4235 0.5176 0.4459 0.041 Uiso 1 1 calc R U . . .
H18C H 0.4978 0.4652 0.4704 0.041 Uiso 1 1 calc R U . . .
C19 C 0.5602(4) 0.3949(3) 0.3968(2) 0.0310(15) Uani 1 1 d . . . . .
H19A H 0.5113 0.3582 0.3954 0.047 Uiso 1 1 calc R U . . .
H19B H 0.5992 0.3888 0.4250 0.047 Uiso 1 1 calc R U . . .
H19C H 0.6015 0.3920 0.3691 0.047 Uiso 1 1 calc R U . . .
C21 C 0.4326(3) 0.8772(2) 0.29836(17) 0.0140(11) Uani 1 1 d . . . . .
C23 C 0.3382(4) 0.9625(3) 0.31674(18) 0.0165(12) Uani 1 1 d . . . . .
C24 C 0.2779(4) 1.0183(3) 0.31575(19) 0.0242(13) Uani 1 1 d . . . . .
H24 H 0.2641 1.0428 0.2877 0.029 Uiso 1 1 calc R U . . .
C25 C 0.2377(4) 1.0372(3) 0.35848(19) 0.0251(14) Uani 1 1 d . . . . .
H25 H 0.1936 1.0751 0.3593 0.030 Uiso 1 1 calc R U . . .
C26 C 0.2596(4) 1.0026(3) 0.40038(18) 0.0221(12) Uani 1 1 d . . . . .
C27 C 0.3261(4) 0.9481(3) 0.39970(19) 0.0207(13) Uani 1 1 d . . . . .
H27 H 0.3457 0.9260 0.4279 0.025 Uiso 1 1 calc R U . . .
C28 C 0.3631(4) 0.9269(3) 0.35696(17) 0.0145(12) Uani 1 1 d . . . . .
C29 C 0.4896(4) 0.8283(2) 0.27229(15) 0.0131(10) Uani 1 1 d . . . . .
C30 C 0.5360(4) 0.7800(2) 0.30143(15) 0.0131(10) Uani 1 1 d . . . . .
C31 C 0.5898(4) 0.7290(3) 0.27870(18) 0.0191(12) Uani 1 1 d . . . . .
H31 H 0.6232 0.6951 0.2967 0.023 Uiso 1 1 calc R U . . .
C32 C 0.5961(4) 0.7266(3) 0.23027(18) 0.0208(12) Uani 1 1 d . . . . .
H32 H 0.6320 0.6903 0.2159 0.025 Uiso 1 1 calc R U . . .
C33 C 0.5509(4) 0.7759(3) 0.20268(18) 0.0224(12) Uani 1 1 d . . . . .
H33 H 0.5570 0.7743 0.1696 0.027 Uiso 1 1 calc R U . . .
C34 C 0.4970(4) 0.8274(2) 0.22359(16) 0.0194(11) Uani 1 1 d . . . . .
H34 H 0.4653 0.8618 0.2052 0.023 Uiso 1 1 calc R U . . .
C35 C 0.2099(4) 1.0219(3) 0.4469(2) 0.0317(15) Uani 1 1 d . . . . .
C36 C 0.1717(5) 0.9572(3) 0.4708(2) 0.0408(17) Uani 1 1 d . . . . .
H36A H 0.1401 0.9703 0.5001 0.061 Uiso 1 1 calc R U . . .
H36B H 0.2250 0.9253 0.4775 0.061 Uiso 1 1 calc R U . . .
H36C H 0.1253 0.9339 0.4503 0.061 Uiso 1 1 calc R U . . .
C37 C 0.2835(5) 1.0550(3) 0.4809(2) 0.0395(17) Uani 1 1 d . . . . .
H37A H 0.2515 1.0669 0.5104 0.059 Uiso 1 1 calc R U . . .
H37B H 0.3103 1.0975 0.4669 0.059 Uiso 1 1 calc R U . . .
H37C H 0.3355 1.0217 0.4870 0.059 Uiso 1 1 calc R U . . .
C38 C 0.1302(6) 1.0744(4) 0.4400(2) 0.064(3) Uani 1 1 d . . . . .
H38A H 0.1008 1.0853 0.4702 0.097 Uiso 1 1 calc R U . . .
H38B H 0.0815 1.0548 0.4190 0.097 Uiso 1 1 calc R U . . .
H38C H 0.1566 1.1171 0.4262 0.097 Uiso 1 1 calc R U . . .
N39 N 0.4487(3) 0.7942(2) 0.44018(13) 0.0157(9) Uani 1 1 d . U . . .
H39 H 0.4535 0.8431 0.4523 0.019 Uiso 1 1 calc R U . . .
C40 C 0.3457(4) 0.7741(3) 0.43794(19) 0.0276(14) Uani 1 1 d . U . . .
H40 H 0.3129 0.8175 0.4269 0.033 Uiso 1 1 calc R U . A 1
C41 C 0.3045(9) 0.7621(7) 0.4842(4) 0.020(3) Uani 0.56(2) 1 d . U P B 1
H41A H 0.2538 0.7258 0.4835 0.024 Uiso 0.56(2) 1 calc R U P B 1
H41B H 0.2783 0.8056 0.4979 0.024 Uiso 0.56(2) 1 calc R U P B 1
C42 C 0.3940(13) 0.7372(9) 0.5100(6) 0.029(4) Uani 0.56(2) 1 d . U P B 1
H42A H 0.3864 0.6875 0.5191 0.035 Uiso 0.56(2) 1 calc R U P B 1
H42B H 0.4031 0.7650 0.5389 0.035 Uiso 0.56(2) 1 calc R U P B 1
C41A C 0.3429(16) 0.7274(12) 0.4892(5) 0.032(5) Uani 0.44(2) 1 d . U P B 2
H41C H 0.2875 0.7423 0.5085 0.039 Uiso 0.44(2) 1 calc R U P B 2
H41D H 0.3361 0.6769 0.4825 0.039 Uiso 0.44(2) 1 calc R U P B 2
C42A C 0.4360(17) 0.7407(11) 0.5153(7) 0.029(4) Uani 0.44(2) 1 d . U P B 2
H42C H 0.4347 0.7845 0.5337 0.035 Uiso 0.44(2) 1 calc R U P B 2
H42D H 0.4555 0.7010 0.5353 0.035 Uiso 0.44(2) 1 calc R U P B 2
C43 C 0.4897(5) 0.7461(3) 0.47529(17) 0.0359(15) Uani 1 1 d . U . . .
H43A H 0.5449 0.7672 0.4920 0.043 Uiso 0.56(2) 1 calc R U P B 1
H43B H 0.5094 0.7011 0.4612 0.043 Uiso 0.56(2) 1 calc R U P B 1
H43C H 0.4960 0.6991 0.4611 0.043 Uiso 0.44(2) 1 calc R U P B 2
H43D H 0.5550 0.7624 0.4837 0.043 Uiso 0.44(2) 1 calc R U P B 2
C44 C 0.3271(4) 0.7214(3) 0.39873(18) 0.0171(12) Uani 1 1 d . . . . .
C48 C -0.1117(4) 0.5411(3) 0.32105(17) 0.0174(12) Uani 1 1 d . . . . .
C50 C -0.1153(4) 0.6505(3) 0.30194(18) 0.0190(12) Uani 1 1 d . . . . .
C51 C -0.1389(4) 0.7140(3) 0.28378(18) 0.0247(13) Uani 1 1 d . . . . .
H51 H -0.1961 0.7212 0.2663 0.030 Uiso 1 1 calc R U . . .
C52 C -0.0747(4) 0.7669(3) 0.29228(18) 0.0205(13) Uani 1 1 d . . . . .
H52 H -0.0886 0.8120 0.2803 0.025 Uiso 1 1 calc R U . . .
C53 C 0.0103(4) 0.7576(2) 0.31771(16) 0.0166(11) Uani 1 1 d . . . . .
C54 C 0.0309(4) 0.6919(2) 0.33656(16) 0.0158(11) Uani 1 1 d . . . . .
H54 H 0.0877 0.6842 0.3542 0.019 Uiso 1 1 calc R U . . .
C55 C -0.0342(4) 0.6382(2) 0.32873(16) 0.0152(11) Uani 1 1 d . . . . .
C56 C -0.1338(4) 0.4686(3) 0.32447(17) 0.0157(12) Uani 1 1 d . . . . .
C57 C -0.0652(3) 0.4322(3) 0.35001(17) 0.0141(11) Uani 1 1 d . . . . .
C58 C -0.0818(4) 0.3610(3) 0.35493(18) 0.0219(13) Uani 1 1 d . . . . .
H58 H -0.0370 0.3333 0.3718 0.026 Uiso 1 1 calc R U . . .
C59 C -0.1624(4) 0.3295(3) 0.3357(2) 0.0279(14) Uani 1 1 d . . . . .
H59 H -0.1724 0.2808 0.3399 0.033 Uiso 1 1 calc R U . . .
C60 C -0.2287(4) 0.3682(3) 0.31050(19) 0.0231(13) Uani 1 1 d . . . . .
H60 H -0.2830 0.3460 0.2970 0.028 Uiso 1 1 calc R U . . .
C61 C -0.2157(4) 0.4382(3) 0.30514(17) 0.0198(12) Uani 1 1 d . . . . .
H61 H -0.2612 0.4656 0.2886 0.024 Uiso 1 1 calc R U . . .
C62 C 0.0824(4) 0.8164(3) 0.32462(18) 0.0216(13) Uani 1 1 d . . . . .
C63 C 0.0510(4) 0.8843(3) 0.3005(2) 0.0323(15) Uani 1 1 d . . . . .
H63A H 0.0988 0.9209 0.3065 0.048 Uiso 1 1 calc R U . . .
H63B H -0.0114 0.8991 0.3129 0.048 Uiso 1 1 calc R U . . .
H63C H 0.0457 0.8764 0.2668 0.048 Uiso 1 1 calc R U . . .
C64 C 0.0944(4) 0.8305(3) 0.3775(2) 0.0286(13) Uani 1 1 d . . . . .
H64A H 0.1440 0.8661 0.3822 0.043 Uiso 1 1 calc R U . . .
H64B H 0.1134 0.7873 0.3933 0.043 Uiso 1 1 calc R U . . .
H64C H 0.0333 0.8471 0.3904 0.043 Uiso 1 1 calc R U . . .
C65 C 0.1798(4) 0.7952(3) 0.30436(18) 0.0240(12) Uani 1 1 d . . . . .
H65A H 0.2256 0.8336 0.3084 0.036 Uiso 1 1 calc R U . . .
H65B H 0.1726 0.7847 0.2710 0.036 Uiso 1 1 calc R U . . .
H65C H 0.2035 0.7536 0.3207 0.036 Uiso 1 1 calc R U . . .
C66 C 0.1058(4) 0.3672(3) 0.44711(18) 0.0187(12) Uani 1 1 d . . . . .
C67 C 0.1599(3) 0.3751(2) 0.3761(2) 0.0209(12) Uani 1 1 d . . . . .
C69 C 0.1689(4) 0.3126(3) 0.4397(2) 0.0246(13) Uani 1 1 d . . . . .
C70 C 0.1911(5) 0.2646(3) 0.4729(2) 0.0351(16) Uani 1 1 d . . . . .
H70 H 0.2342 0.2271 0.4670 0.042 Uiso 1 1 calc R U . . .
C71 C 0.1471(4) 0.2735(3) 0.5159(2) 0.0355(16) Uani 1 1 d . . . . .
H71 H 0.1602 0.2405 0.5398 0.043 Uiso 1 1 calc R U . . .
C72 C 0.0842(4) 0.3288(3) 0.52602(19) 0.0248(13) Uani 1 1 d . . . . .
C73 C 0.0616(4) 0.3754(3) 0.49006(18) 0.0196(12) Uani 1 1 d . . . . .
H73 H 0.0168 0.4121 0.4950 0.023 Uiso 1 1 calc R U . . .
C74 C 0.1750(4) 0.4034(3) 0.33054(19) 0.0225(13) Uani 1 1 d . . . . .
C75 C 0.1224(4) 0.4654(3) 0.32439(19) 0.0188(13) Uani 1 1 d . . . . .
C76 C 0.1353(4) 0.4995(3) 0.28204(17) 0.0241(13) Uani 1 1 d . . . . .
H76 H 0.1023 0.5421 0.2763 0.029 Uiso 1 1 calc R U . . .
C77 C 0.1956(4) 0.4724(3) 0.24778(19) 0.0310(15) Uani 1 1 d . . . . .
H77 H 0.2034 0.4971 0.2192 0.037 Uiso 1 1 calc R U . . .
C78 C 0.2447(4) 0.4100(3) 0.2543(2) 0.0338(16) Uani 1 1 d . . . . .
H78 H 0.2841 0.3915 0.2303 0.041 Uiso 1 1 calc R U . . .
C79 C 0.2353(4) 0.3758(3) 0.2960(2) 0.0296(15) Uani 1 1 d . . . . .
H79 H 0.2695 0.3336 0.3014 0.036 Uiso 1 1 calc R U . . .
C80 C 0.0390(4) 0.3360(3) 0.57430(19) 0.0268(13) Uani 1 1 d . . . . .
C81 C 0.0188(5) 0.4135(3) 0.58579(18) 0.0330(15) Uani 1 1 d . . . . .
H81A H -0.0088 0.4170 0.6172 0.050 Uiso 1 1 calc R U . . .
H81B H -0.0267 0.4325 0.5630 0.050 Uiso 1 1 calc R U . . .
H81C H 0.0789 0.4400 0.5845 0.050 Uiso 1 1 calc R U . . .
C82 C -0.0565(4) 0.2966(3) 0.5746(2) 0.0325(15) Uani 1 1 d . . . . .
H82A H -0.0899 0.3053 0.6042 0.049 Uiso 1 1 calc R U . . .
H82B H -0.0444 0.2464 0.5712 0.049 Uiso 1 1 calc R U . . .
H82C H -0.0965 0.3129 0.5486 0.049 Uiso 1 1 calc R U . . .
C83 C 0.1042(4) 0.3084(3) 0.6132(2) 0.0381(16) Uani 1 1 d . . . . .
H83A H 0.0756 0.3191 0.6436 0.057 Uiso 1 1 calc R U . . .
H83B H 0.1674 0.3306 0.6109 0.057 Uiso 1 1 calc R U . . .
H83C H 0.1113 0.2577 0.6099 0.057 Uiso 1 1 calc R U . . .
C85 C 0.0826(4) 0.5963(3) 0.45562(18) 0.0230(13) Uani 1 1 d . U . . .
H85A H 0.0720 0.6465 0.4474 0.028 Uiso 0.59 1 calc R U P C 1
H85B H 0.0720 0.6465 0.4474 0.028 Uiso 0.41 1 calc R U P D 2
C86 C 0.1494(5) 0.5928(4) 0.4977(2) 0.0478(18) Uani 1 1 d . U . . .
H86A H 0.1887 0.6357 0.5003 0.057 Uiso 0.59 1 calc R U P E 1
H86B H 0.1126 0.5863 0.5270 0.057 Uiso 0.59 1 calc R U P E 1
H86C H 0.1233 0.5601 0.5213 0.057 Uiso 0.41 1 calc R U P F 2
H86D H 0.1555 0.6395 0.5122 0.057 Uiso 0.41 1 calc R U P F 2
C87 C 0.2046(8) 0.5368(6) 0.4886(3) 0.036(3) Uani 0.59 1 d . U P G 1
H87A H 0.1714 0.4938 0.4991 0.043 Uiso 0.59 1 calc R U P G 1
H87B H 0.2660 0.5406 0.5059 0.043 Uiso 0.59 1 calc R U P G 1
C87A C 0.2527(11) 0.5660(8) 0.4798(5) 0.025(3) Uani 0.41 1 d . U P G 2
H87C H 0.2975 0.6054 0.4745 0.031 Uiso 0.41 1 calc R U P G 2
H87D H 0.2819 0.5325 0.5020 0.031 Uiso 0.41 1 calc R U P G 2
C88 C 0.2249(4) 0.5322(3) 0.43592(19) 0.0279(13) Uani 1 1 d . U . . .
H88A H 0.2816 0.5606 0.4271 0.033 Uiso 0.59 1 calc R U P G 1
H88B H 0.2351 0.4833 0.4259 0.033 Uiso 0.59 1 calc R U P G 1
H88C H 0.2160 0.4816 0.4415 0.033 Uiso 0.41 1 calc R U P G 2
H88D H 0.2776 0.5378 0.4129 0.033 Uiso 0.41 1 calc R U P G 2
C89 C -0.0146(4) 0.5627(2) 0.46595(16) 0.0180(12) Uani 1 1 d . . . . .
Rh1 Rh 0.50582(3) 0.79109(2) 0.36935(2) 0.01180(9) Uani 1 1 d . . . . .
Rh2 Rh 0.03815(3) 0.49117(2) 0.37824(2) 0.01284(9) Uani 1 1 d . . . . .
N1 N 0.6063(3) 0.7196(2) 0.38602(13) 0.0130(9) Uani 1 1 d . . . . .
N20 N 0.4233(3) 0.8719(2) 0.34371(14) 0.0137(9) Uani 1 1 d . . . . .
N47 N -0.0344(3) 0.5672(2) 0.34099(13) 0.0144(9) Uani 1 1 d . . . . .
N66 N 0.1022(3) 0.4058(2) 0.40577(14) 0.0171(10) Uani 1 1 d . . . . .
N84 N 0.1353(3) 0.5615(2) 0.41597(14) 0.0148(9) Uani 1 1 d . U . . .
H84 H 0.1545 0.5991 0.3936 0.018 Uiso 1 1 calc R U . . .
O3 O 0.7612(2) 0.69747(18) 0.39963(12) 0.0187(8) Uani 1 1 d . . . . .
O22 O 0.3844(3) 0.93061(17) 0.27889(11) 0.0179(8) Uani 1 1 d . . . . .
O45 O 0.3896(2) 0.71835(16) 0.36596(11) 0.0137(7) Uani 1 1 d . . . . .
O46 O 0.2520(3) 0.68703(18) 0.40018(12) 0.0203(9) Uani 1 1 d . . . . .
O49 O -0.1654(2) 0.58789(18) 0.29722(12) 0.0208(8) Uani 1 1 d . . . . .
O68 O 0.2040(3) 0.31767(18) 0.39393(13) 0.0274(10) Uani 1 1 d . . . . .
O90 O -0.0441(2) 0.51402(16) 0.43921(10) 0.0132(7) Uani 1 1 d . . . . .
O91 O -0.0598(3) 0.58452(18) 0.50029(12) 0.0267(9) Uani 1 1 d . . . . .
C1L C 0.3583(6) 0.6229(4) 0.2659(3) 0.065(2) Uani 1 1 d . . . . .
H02C H 0.3915 0.6617 0.2820 0.078 Uiso 1 1 calc R U . . .
H02D H 0.3235 0.5953 0.2897 0.078 Uiso 1 1 calc R U . . .
C3L C 0.4850(5) 0.3335(3) 0.6873(2) 0.0510(19) Uani 1 1 d . . . . .
H02A H 0.4277 0.3257 0.6675 0.061 Uiso 1 1 calc R U . . .
H02B H 0.4724 0.3126 0.7183 0.061 Uiso 1 1 calc R U . . .
Cl1 Cl 0.44372(14) 0.56974(9) 0.23897(6) 0.0526(5) Uani 1 1 d . . . . .
Cl2 Cl 0.27530(16) 0.65754(10) 0.22609(7) 0.0634(6) Uani 1 1 d . . . . .
Cl5 Cl 0.58584(13) 0.29202(8) 0.66156(6) 0.0437(4) Uani 1 1 d . . . . .
Cl6 Cl 0.50418(15) 0.42284(9) 0.69356(6) 0.0593(5) Uani 1 1 d . . . . .
C2L C 0.3925(8) 0.3401(5) 0.5319(3) 0.039(2) Uani 0.764(9) 1 d D U P H 1
H2LA H 0.4589 0.3510 0.5220 0.047 Uiso 0.764(9) 1 calc R U P H 1
H2LB H 0.3526 0.3366 0.5034 0.047 Uiso 0.764(9) 1 calc R U P H 1
Cl3 Cl 0.3515(2) 0.40658(14) 0.56423(17) 0.0618(13) Uani 0.764(9) 1 d D U P H 1
Cl4 Cl 0.3926(2) 0.25844(14) 0.55993(10) 0.0450(10) Uani 0.764(9) 1 d D U P H 1
C4L C 0.353(3) 0.360(2) 0.5447(12) 0.119(19) Uani 0.236(9) 1 d D U P H 2
H4LA H 0.2870 0.3444 0.5373 0.143 Uiso 0.236(9) 1 calc R U P H 2
H4LB H 0.3702 0.3980 0.5228 0.143 Uiso 0.236(9) 1 calc R U P H 2
Cl7 Cl 0.4294(11) 0.2931(11) 0.5376(7) 0.121(8) Uani 0.236(9) 1 d D U P H 2
Cl8 Cl 0.3572(9) 0.3911(7) 0.6017(7) 0.091(6) Uani 0.236(9) 1 d D U P H 2


_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
C2 N1 1.300(6) . ?
C2 O3 1.349(6) . ?
C2 C10 1.434(7) . ?
C4 C5 1.361(7) . ?
C4 C9 1.387(7) . ?
C4 O3 1.390(6) . ?
C5 C6 1.395(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(6) . ?
C7 C16 1.523(7) . ?
C8 C9 1.368(7) . ?
C8 H8 0.9500 . ?
C9 N1 1.400(6) . ?
C10 C15 1.392(7) . ?
C10 C11 1.408(7) . ?
C11 C12 1.394(7) . ?
C11 Rh1 1.991(5) . ?
C12 C13 1.384(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C18 1.531(8) . ?
C16 C19 1.535(7) . ?
C16 C17 1.547(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 N20 1.308(6) . ?
C21 O22 1.344(6) . ?
C21 C29 1.436(7) . ?
C23 C24 1.359(7) . ?
C23 C28 1.382(7) . ?
C23 O22 1.400(6) . ?
C24 C25 1.393(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.404(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.395(7) . ?
C26 C35 1.546(7) . ?
C27 C28 1.387(7) . ?
C27 H27 0.9500 . ?
C28 N20 1.399(6) . ?
C29 C34 1.397(6) . ?
C29 C30 1.402(6) . ?
C30 C31 1.392(7) . ?
C30 Rh1 2.000(4) . ?
C31 C32 1.389(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(7) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C38 1.509(9) . ?
C35 C36 1.512(8) . ?
C35 C37 1.549(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N39 C43 1.478(6) . ?
N39 C40 1.486(7) . ?
N39 Rh1 2.178(4) . ?
N39 H39 1.0000 . ?
C40 C41 1.461(11) . ?
C40 C44 1.530(7) . ?
C40 C41A 1.719(19) . ?
C40 H40 1.0000 . ?
C41 C42 1.526(17) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.671(17) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C41A C42A 1.52(2) . ?
C41A H41C 0.9900 . ?
C41A H41D 0.9900 . ?
C42A C43 1.37(2) . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 H43C 0.9900 . ?
C43 H43D 0.9900 . ?
C44 O46 1.237(6) . ?
C44 O45 1.280(6) . ?
C48 N47 1.316(7) . ?
C48 O49 1.351(6) . ?
C48 C56 1.426(7) . ?
C50 C51 1.361(7) . ?
C50 C55 1.386(7) . ?
C50 O49 1.394(6) . ?
C51 C52 1.371(7) . ?
C51 H51 0.9500 . ?
C52 C53 1.400(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.398(6) . ?
C53 C62 1.521(7) . ?
C54 C55 1.388(7) . ?
C54 H54 0.9500 . ?
C55 N47 1.404(6) . ?
C56 C57 1.390(7) . ?
C56 C61 1.394(7) . ?
C57 C58 1.389(7) . ?
C57 Rh2 2.000(5) . ?
C58 C59 1.387(8) . ?
C58 H58 0.9500 . ?
C59 C60 1.386(8) . ?
C59 H59 0.9500 . ?
C60 C61 1.360(7) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C62 C65 1.529(8) . ?
C62 C63 1.536(7) . ?
C62 C64 1.546(7) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 C73 1.383(7) . ?
C66 C69 1.383(7) . ?
C66 N66 1.395(6) . ?
C67 N66 1.309(6) . ?
C67 O68 1.359(6) . ?
C67 C74 1.426(8) . ?
C69 C70 1.357(8) . ?
C69 O68 1.401(7) . ?
C70 C71 1.385(9) . ?
C70 H70 0.9500 . ?
C71 C72 1.404(8) . ?
C71 H71 0.9500 . ?
C72 C73 1.398(7) . ?
C72 C80 1.524(8) . ?
C73 H73 0.9500 . ?
C74 C79 1.401(8) . ?
C74 C75 1.406(7) . ?
C75 C76 1.388(7) . ?
C75 Rh2 1.998(5) . ?
C76 C77 1.391(7) . ?
C76 H76 0.9500 . ?
C77 C78 1.387(8) . ?
C77 H77 0.9500 . ?
C78 C79 1.366(8) . ?
C78 H78 0.9500 . ?
C79 H79 0.9500 . ?
C80 C82 1.529(8) . ?
C80 C83 1.529(8) . ?
C80 C81 1.545(7) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C85 N84 1.507(6) . ?
C85 C86 1.523(8) . ?
C85 C89 1.528(7) . ?
C85 H85A 1.0000 . ?
C85 H85B 1.0000 . ?
C86 C87 1.345(13) . ?
C86 C87A 1.610(16) . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C86 H86C 0.9900 . ?
C86 H86D 0.9900 . ?
C87 C88 1.536(12) . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C87A C88 1.465(14) . ?
C87A H87C 0.9900 . ?
C87A H87D 0.9900 . ?
C88 N84 1.482(7) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88 H88C 0.9900 . ?
C88 H88D 0.9900 . ?
C89 O91 1.239(6) . ?
C89 O90 1.273(5) . ?
Rh1 N1 2.014(4) . ?
Rh1 N20 2.061(4) . ?
Rh1 O45 2.137(3) . ?
Rh2 N66 2.022(4) . ?
Rh2 N47 2.067(4) . ?
Rh2 O90 2.132(3) . ?
Rh2 N84 2.192(4) . ?
N84 H84 1.0000 . ?
C1L Cl1 1.743(7) . ?
C1L Cl2 1.753(8) . ?
C1L H02C 0.9900 . ?
C1L H02D 0.9900 . ?
C3L Cl6 1.740(6) . ?
C3L Cl5 1.773(7) . ?
C3L H02A 0.9900 . ?
C3L H02B 0.9900 . ?
C2L Cl3 1.673(10) . ?
C2L Cl4 1.757(8) . ?
C2L H2LA 0.9900 . ?
C2L H2LB 0.9900 . ?
C4L Cl7 1.68(3) . ?
C4L Cl8 1.74(3) . ?
C4L H4LA 0.9900 . ?
C4L H4LB 0.9900 . ?

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 C2 O3 114.8(4) . . ?
N1 C2 C10 119.5(5) . . ?
O3 C2 C10 125.7(5) . . ?
C5 C4 C9 123.2(5) . . ?
C5 C4 O3 128.0(5) . . ?
C9 C4 O3 108.8(4) . . ?
C4 C5 C6 115.0(5) . . ?
C4 C5 H5 122.5 . . ?
C6 C5 H5 122.5 . . ?
C7 C6 C5 123.4(5) . . ?
C7 C6 H6 118.3 . . ?
C5 C6 H6 118.3 . . ?
C6 C7 C8 119.4(5) . . ?
C6 C7 C16 122.1(4) . . ?
C8 C7 C16 118.4(5) . . ?
C9 C8 C7 117.7(5) . . ?
C9 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?
C8 C9 C4 121.3(4) . . ?
C8 C9 N1 132.3(5) . . ?
C4 C9 N1 106.5(4) . . ?
C15 C10 C11 124.1(4) . . ?
C15 C10 C2 125.0(5) . . ?
C11 C10 C2 110.9(4) . . ?
C12 C11 C10 115.3(4) . . ?
C12 C11 Rh1 129.4(4) . . ?
C10 C11 Rh1 115.3(3) . . ?
C13 C12 C11 121.3(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C14 C13 C12 121.5(5) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C15 C14 C13 119.6(5) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C10 118.1(5) . . ?
C14 C15 H15 120.9 . . ?
C10 C15 H15 120.9 . . ?
C7 C16 C18 108.3(4) . . ?
C7 C16 C19 111.8(5) . . ?
C18 C16 C19 107.9(4) . . ?
C7 C16 C17 110.7(4) . . ?
C18 C16 C17 109.3(5) . . ?
C19 C16 C17 108.7(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N20 C21 O22 114.9(4) . . ?
N20 C21 C29 121.2(4) . . ?
O22 C21 C29 123.8(4) . . ?
C24 C23 C28 124.0(5) . . ?
C24 C23 O22 127.6(5) . . ?
C28 C23 O22 108.3(4) . . ?
C23 C24 C25 115.8(5) . . ?
C23 C24 H24 122.1 . . ?
C25 C24 H24 122.1 . . ?
C24 C25 C26 122.6(5) . . ?
C24 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C27 C26 C25 119.0(5) . . ?
C27 C26 C35 119.2(5) . . ?
C25 C26 C35 121.7(5) . . ?
C28 C27 C26 118.5(5) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 120.7 . . ?
C23 C28 C27 119.8(5) . . ?
C23 C28 N20 107.2(4) . . ?
C27 C28 N20 133.0(5) . . ?
C34 C29 C30 123.5(4) . . ?
C34 C29 C21 124.5(4) . . ?
C30 C29 C21 112.0(4) . . ?
C31 C30 C29 115.6(4) . . ?
C31 C30 Rh1 129.9(4) . . ?
C29 C30 Rh1 114.3(3) . . ?
C32 C31 C30 121.6(5) . . ?
C32 C31 H31 119.2 . . ?
C30 C31 H31 119.2 . . ?
C33 C32 C31 121.2(5) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C34 C33 C32 119.3(5) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C29 118.8(5) . . ?
C33 C34 H34 120.6 . . ?
C29 C34 H34 120.6 . . ?
C38 C35 C36 110.3(6) . . ?
C38 C35 C26 112.0(5) . . ?
C36 C35 C26 110.6(5) . . ?
C38 C35 C37 107.3(5) . . ?
C36 C35 C37 106.5(5) . . ?
C26 C35 C37 110.0(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C43 N39 C40 103.9(4) . . ?
C43 N39 Rh1 118.3(3) . . ?
C40 N39 Rh1 107.7(3) . . ?
C43 N39 H39 108.8 . . ?
C40 N39 H39 108.8 . . ?
Rh1 N39 H39 108.8 . . ?
C41 C40 N39 112.4(6) . . ?
C41 C40 C44 119.7(6) . . ?
N39 C40 C44 111.5(4) . . ?
N39 C40 C41A 96.9(8) . . ?
C44 C40 C41A 106.2(7) . . ?
C41 C40 H40 103.8 . . ?
N39 C40 H40 103.8 . . ?
C44 C40 H40 103.8 . . ?
C40 C41 C42 99.6(9) . . ?
C40 C41 H41A 111.8 . . ?
C42 C41 H41A 111.8 . . ?
C40 C41 H41B 111.8 . . ?
C42 C41 H41B 111.8 . . ?
H41A C41 H41B 109.6 . . ?
C41 C42 C43 109.3(10) . . ?
C41 C42 H42A 109.8 . . ?
C43 C42 H42A 109.8 . . ?
C41 C42 H42B 109.8 . . ?
C43 C42 H42B 109.8 . . ?
H42A C42 H42B 108.3 . . ?
C42A C41A C40 108.2(12) . . ?
C42A C41A H41C 110.1 . . ?
C40 C41A H41C 110.1 . . ?
C42A C41A H41D 110.1 . . ?
C40 C41A H41D 110.1 . . ?
H41C C41A H41D 108.4 . . ?
C43 C42A C41A 93.9(14) . . ?
C43 C42A H42C 112.9 . . ?
C41A C42A H42C 112.9 . . ?
C43 C42A H42D 112.9 . . ?
C41A C42A H42D 112.9 . . ?
H42C C42A H42D 110.4 . . ?
C42A C43 N39 113.8(11) . . ?
N39 C43 C42 99.3(7) . . ?
N39 C43 H43A 111.9 . . ?
C42 C43 H43A 111.9 . . ?
N39 C43 H43B 111.9 . . ?
C42 C43 H43B 111.9 . . ?
H43A C43 H43B 109.6 . . ?
C42A C43 H43C 108.8 . . ?
N39 C43 H43C 108.8 . . ?
C42A C43 H43D 108.8 . . ?
N39 C43 H43D 108.8 . . ?
H43C C43 H43D 107.7 . . ?
O46 C44 O45 125.0(5) . . ?
O46 C44 C40 118.0(5) . . ?
O45 C44 C40 116.9(5) . . ?
N47 C48 O49 114.9(4) . . ?
N47 C48 C56 121.0(5) . . ?
O49 C48 C56 124.1(5) . . ?
C51 C50 C55 124.0(5) . . ?
C51 C50 O49 127.6(5) . . ?
C55 C50 O49 108.3(4) . . ?
C50 C51 C52 115.7(5) . . ?
C50 C51 H51 122.1 . . ?
C52 C51 H51 122.1 . . ?
C51 C52 C53 123.3(5) . . ?
C51 C52 H52 118.3 . . ?
C53 C52 H52 118.3 . . ?
C54 C53 C52 119.2(5) . . ?
C54 C53 C62 118.7(5) . . ?
C52 C53 C62 122.1(4) . . ?
C55 C54 C53 118.1(5) . . ?
C55 C54 H54 121.0 . . ?
C53 C54 H54 121.0 . . ?
C50 C55 C54 119.6(4) . . ?
C50 C55 N47 107.6(4) . . ?
C54 C55 N47 132.7(5) . . ?
C57 C56 C61 124.1(5) . . ?
C57 C56 C48 112.1(5) . . ?
C61 C56 C48 123.8(5) . . ?
C58 C57 C56 115.5(5) . . ?
C58 C57 Rh2 129.3(4) . . ?
C56 C57 Rh2 115.0(4) . . ?
C59 C58 C57 121.4(5) . . ?
C59 C58 H58 119.3 . . ?
C57 C58 H58 119.3 . . ?
C60 C59 C58 120.8(5) . . ?
C60 C59 H59 119.6 . . ?
C58 C59 H59 119.6 . . ?
C61 C60 C59 119.8(5) . . ?
C61 C60 H60 120.1 . . ?
C59 C60 H60 120.1 . . ?
C60 C61 C56 118.4(5) . . ?
C60 C61 H61 120.8 . . ?
C56 C61 H61 120.8 . . ?
C53 C62 C65 109.8(4) . . ?
C53 C62 C63 112.4(5) . . ?
C65 C62 C63 107.9(5) . . ?
C53 C62 C64 109.1(4) . . ?
C65 C62 C64 108.8(4) . . ?
C63 C62 C64 108.8(4) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C62 C65 H65A 109.5 . . ?
C62 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C62 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C73 C66 C69 120.3(5) . . ?
C73 C66 N66 132.7(5) . . ?
C69 C66 N66 107.0(5) . . ?
N66 C67 O68 113.3(5) . . ?
N66 C67 C74 120.9(5) . . ?
O68 C67 C74 125.7(5) . . ?
C70 C69 C66 123.3(6) . . ?
C70 C69 O68 128.5(5) . . ?
C66 C69 O68 108.2(5) . . ?
C69 C70 C71 115.9(6) . . ?
C69 C70 H70 122.0 . . ?
C71 C70 H70 122.0 . . ?
C70 C71 C72 123.6(5) . . ?
C70 C71 H71 118.2 . . ?
C72 C71 H71 118.2 . . ?
C73 C72 C71 118.0(5) . . ?
C73 C72 C80 121.1(5) . . ?
C71 C72 C80 120.8(5) . . ?
C66 C73 C72 118.8(5) . . ?
C66 C73 H73 120.6 . . ?
C72 C73 H73 120.6 . . ?
C79 C74 C75 122.8(6) . . ?
C79 C74 C67 126.2(5) . . ?
C75 C74 C67 111.0(5) . . ?
C76 C75 C74 116.0(5) . . ?
C76 C75 Rh2 129.3(4) . . ?
C74 C75 Rh2 114.7(4) . . ?
C75 C76 C77 121.2(5) . . ?
C75 C76 H76 119.4 . . ?
C77 C76 H76 119.4 . . ?
C78 C77 C76 121.5(6) . . ?
C78 C77 H77 119.3 . . ?
C76 C77 H77 119.3 . . ?
C79 C78 C77 119.0(5) . . ?
C79 C78 H78 120.5 . . ?
C77 C78 H78 120.5 . . ?
C78 C79 C74 119.4(6) . . ?
C78 C79 H79 120.3 . . ?
C74 C79 H79 120.3 . . ?
C72 C80 C82 108.6(5) . . ?
C72 C80 C83 112.6(5) . . ?
C82 C80 C83 110.0(4) . . ?
C72 C80 C81 110.8(4) . . ?
C82 C80 C81 108.3(5) . . ?
C83 C80 C81 106.6(5) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C80 C83 H83A 109.5 . . ?
C80 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C80 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
N84 C85 C86 106.2(5) . . ?
N84 C85 C89 112.9(4) . . ?
C86 C85 C89 111.6(4) . . ?
N84 C85 H85A 108.6 . . ?
C86 C85 H85A 108.6 . . ?
C89 C85 H85A 108.6 . . ?
N84 C85 H85B 108.6 . . ?
C86 C85 H85B 108.6 . . ?
C89 C85 H85B 108.6 . . ?
C87 C86 C85 103.3(6) . . ?
C85 C86 C87A 107.9(6) . . ?
C87 C86 H86A 111.1 . . ?
C85 C86 H86A 111.1 . . ?
C87 C86 H86B 111.1 . . ?
C85 C86 H86B 111.1 . . ?
H86A C86 H86B 109.1 . . ?
C85 C86 H86C 110.1 . . ?
C87A C86 H86C 110.1 . . ?
C85 C86 H86D 110.1 . . ?
C87A C86 H86D 110.1 . . ?
H86C C86 H86D 108.4 . . ?
C86 C87 C88 110.0(8) . . ?
C86 C87 H87A 109.7 . . ?
C88 C87 H87A 109.7 . . ?
C86 C87 H87B 109.7 . . ?
C88 C87 H87B 109.7 . . ?
H87A C87 H87B 108.2 . . ?
C88 C87A C86 100.3(9) . . ?
C88 C87A H87C 111.7 . . ?
C86 C87A H87C 111.7 . . ?
C88 C87A H87D 111.7 . . ?
C86 C87A H87D 111.7 . . ?
H87C C87A H87D 109.5 . . ?
C87A C88 N84 112.7(7) . . ?
N84 C88 C87 101.6(6) . . ?
N84 C88 H88A 111.4 . . ?
C87 C88 H88A 111.4 . . ?
N84 C88 H88B 111.4 . . ?
C87 C88 H88B 111.4 . . ?
H88A C88 H88B 109.3 . . ?
C87A C88 H88C 109.1 . . ?
N84 C88 H88C 109.1 . . ?
C87A C88 H88D 109.1 . . ?
N84 C88 H88D 109.1 . . ?
H88C C88 H88D 107.8 . . ?
O91 C89 O90 124.1(5) . . ?
O91 C89 C85 117.4(4) . . ?
O90 C89 C85 118.5(4) . . ?
C11 Rh1 C30 87.85(19) . . ?
C11 Rh1 N1 80.28(17) . . ?
C30 Rh1 N1 90.71(18) . . ?
C11 Rh1 N20 91.42(18) . . ?
C30 Rh1 N20 81.41(18) . . ?
N1 Rh1 N20 168.81(16) . . ?
C11 Rh1 O45 175.64(16) . . ?
C30 Rh1 O45 92.61(16) . . ?
N1 Rh1 O45 95.37(14) . . ?
N20 Rh1 O45 92.94(14) . . ?
C11 Rh1 N39 102.21(18) . . ?
C30 Rh1 N39 169.74(18) . . ?
N1 Rh1 N39 92.97(15) . . ?
N20 Rh1 N39 96.14(15) . . ?
O45 Rh1 N39 77.52(13) . . ?
C75 Rh2 C57 88.4(2) . . ?
C75 Rh2 N66 80.9(2) . . ?
C57 Rh2 N66 91.02(19) . . ?
C75 Rh2 N47 93.59(19) . . ?
C57 Rh2 N47 80.67(18) . . ?
N66 Rh2 N47 170.21(15) . . ?
C75 Rh2 O90 175.40(18) . . ?
C57 Rh2 O90 93.45(16) . . ?
N66 Rh2 O90 94.81(15) . . ?
N47 Rh2 O90 90.88(14) . . ?
C75 Rh2 N84 99.73(18) . . ?
C57 Rh2 N84 171.73(17) . . ?
N66 Rh2 N84 91.87(16) . . ?
N47 Rh2 N84 97.08(16) . . ?
O90 Rh2 N84 78.59(14) . . ?
C2 N1 C9 106.1(4) . . ?
C2 N1 Rh1 114.0(3) . . ?
C9 N1 Rh1 139.6(3) . . ?
C21 N20 C28 105.6(4) . . ?
C21 N20 Rh1 110.9(3) . . ?
C28 N20 Rh1 143.4(3) . . ?
C48 N47 C55 105.1(4) . . ?
C48 N47 Rh2 110.9(3) . . ?
C55 N47 Rh2 144.0(3) . . ?
C67 N66 C66 107.0(4) . . ?
C67 N66 Rh2 112.3(4) . . ?
C66 N66 Rh2 140.7(4) . . ?
C88 N84 C85 106.7(4) . . ?
C88 N84 Rh2 118.5(3) . . ?
C85 N84 Rh2 110.1(3) . . ?
C88 N84 H84 107.0 . . ?
C85 N84 H84 107.0 . . ?
Rh2 N84 H84 107.0 . . ?
C2 O3 C4 103.8(4) . . ?
C21 O22 C23 103.9(4) . . ?
C44 O45 Rh1 116.8(3) . . ?
C48 O49 C50 104.2(4) . . ?
C67 O68 C69 104.5(4) . . ?
C89 O90 Rh2 118.0(3) . . ?
Cl1 C1L Cl2 112.6(4) . . ?
Cl1 C1L H02C 109.1 . . ?
Cl2 C1L H02C 109.1 . . ?
Cl1 C1L H02D 109.1 . . ?
Cl2 C1L H02D 109.1 . . ?
H02C C1L H02D 107.8 . . ?
Cl6 C3L Cl5 111.2(4) . . ?
Cl6 C3L H02A 109.4 . . ?
Cl5 C3L H02A 109.4 . . ?
Cl6 C3L H02B 109.4 . . ?
Cl5 C3L H02B 109.4 . . ?
H02A C3L H02B 108.0 . . ?
Cl3 C2L Cl4 115.2(5) . . ?
Cl3 C2L H2LA 108.5 . . ?
Cl4 C2L H2LA 108.5 . . ?
Cl3 C2L H2LB 108.5 . . ?
Cl4 C2L H2LB 108.5 . . ?
H2LA C2L H2LB 107.5 . . ?
Cl7 C4L Cl8 110.7(19) . . ?
Cl7 C4L H4LA 109.5 . . ?
Cl8 C4L H4LA 109.5 . . ?
Cl7 C4L H4LB 109.5 . . ?
Cl8 C4L H4LB 109.5 . . ?
H4LA C4L H4LB 108.1 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 C6 0.1(7) . . . . ?
O3 C4 C5 C6 -178.8(5) . . . . ?
C4 C5 C6 C7 -0.8(7) . . . . ?
C5 C6 C7 C8 0.4(7) . . . . ?
C5 C6 C7 C16 -175.7(5) . . . . ?
C6 C7 C8 C9 0.9(7) . . . . ?
C16 C7 C8 C9 177.1(4) . . . . ?
C7 C8 C9 C4 -1.6(7) . . . . ?
C7 C8 C9 N1 179.9(5) . . . . ?
C5 C4 C9 C8 1.2(8) . . . . ?
O3 C4 C9 C8 -179.7(4) . . . . ?
C5 C4 C9 N1 180.0(5) . . . . ?
O3 C4 C9 N1 -0.9(5) . . . . ?
N1 C2 C10 C15 -179.2(5) . . . . ?
O3 C2 C10 C15 0.1(8) . . . . ?
N1 C2 C10 C11 -1.0(7) . . . . ?
O3 C2 C10 C11 178.3(4) . . . . ?
C15 C10 C11 C12 -2.0(7) . . . . ?
C2 C10 C11 C12 179.8(4) . . . . ?
C15 C10 C11 Rh1 177.7(4) . . . . ?
C2 C10 C11 Rh1 -0.6(5) . . . . ?
C10 C11 C12 C13 0.9(7) . . . . ?
Rh1 C11 C12 C13 -178.7(4) . . . . ?
C11 C12 C13 C14 0.6(8) . . . . ?
C12 C13 C14 C15 -1.1(8) . . . . ?
C13 C14 C15 C10 0.1(8) . . . . ?
C11 C10 C15 C14 1.5(8) . . . . ?
C2 C10 C15 C14 179.6(5) . . . . ?
C6 C7 C16 C18 104.4(5) . . . . ?
C8 C7 C16 C18 -71.7(5) . . . . ?
C6 C7 C16 C19 -14.4(6) . . . . ?
C8 C7 C16 C19 169.5(4) . . . . ?
C6 C7 C16 C17 -135.8(5) . . . . ?
C8 C7 C16 C17 48.2(6) . . . . ?
C28 C23 C24 C25 -2.4(8) . . . . ?
O22 C23 C24 C25 176.7(5) . . . . ?
C23 C24 C25 C26 1.8(8) . . . . ?
C24 C25 C26 C27 1.7(8) . . . . ?
C24 C25 C26 C35 -176.6(5) . . . . ?
C25 C26 C27 C28 -4.5(8) . . . . ?
C35 C26 C27 C28 173.7(5) . . . . ?
C24 C23 C28 C27 -0.5(8) . . . . ?
O22 C23 C28 C27 -179.7(5) . . . . ?
C24 C23 C28 N20 178.1(5) . . . . ?
O22 C23 C28 N20 -1.2(5) . . . . ?
C26 C27 C28 C23 4.0(8) . . . . ?
C26 C27 C28 N20 -174.1(5) . . . . ?
N20 C21 C29 C34 174.9(5) . . . . ?
O22 C21 C29 C34 -4.2(8) . . . . ?
N20 C21 C29 C30 -3.8(7) . . . . ?
O22 C21 C29 C30 177.0(4) . . . . ?
C34 C29 C30 C31 -1.1(7) . . . . ?
C21 C29 C30 C31 177.7(4) . . . . ?
C34 C29 C30 Rh1 -176.7(4) . . . . ?
C21 C29 C30 Rh1 2.1(5) . . . . ?
C29 C30 C31 C32 -0.4(7) . . . . ?
Rh1 C30 C31 C32 174.3(4) . . . . ?
C30 C31 C32 C33 1.8(8) . . . . ?
C31 C32 C33 C34 -1.5(8) . . . . ?
C32 C33 C34 C29 0.1(7) . . . . ?
C30 C29 C34 C33 1.3(8) . . . . ?
C21 C29 C34 C33 -177.3(5) . . . . ?
C27 C26 C35 C38 -171.6(6) . . . . ?
C25 C26 C35 C38 6.6(8) . . . . ?
C27 C26 C35 C36 -48.2(7) . . . . ?
C25 C26 C35 C36 130.0(6) . . . . ?
C27 C26 C35 C37 69.2(7) . . . . ?
C25 C26 C35 C37 -112.6(6) . . . . ?
C43 N39 C40 C41 43.3(8) . . . . ?
Rh1 N39 C40 C41 169.6(7) . . . . ?
C43 N39 C40 C44 -94.2(5) . . . . ?
Rh1 N39 C40 C44 32.1(5) . . . . ?
C43 N39 C40 C41A 16.4(8) . . . . ?
Rh1 N39 C40 C41A 142.7(8) . . . . ?
N39 C40 C41 C42 -29.8(13) . . . . ?
C44 C40 C41 C42 103.8(10) . . . . ?
C41A C40 C41 C42 33.6(14) . . . . ?
C40 C41 C42 C43 6.9(15) . . . . ?
C41 C40 C41A C42A -113(2) . . . . ?
N39 C40 C41A C42A 10.7(16) . . . . ?
C44 C40 C41A C42A 125.4(14) . . . . ?
C40 C41A C42A C43 -34.0(17) . . . . ?
C41A C42A C43 N39 50.0(17) . . . . ?
C41A C42A C43 C42 4(3) . . . . ?
C40 N39 C43 C42A -46.9(12) . . . . ?
Rh1 N39 C43 C42A -166.3(11) . . . . ?
C40 N39 C43 C42 -32.5(8) . . . . ?
Rh1 N39 C43 C42 -151.8(7) . . . . ?
C41 C42 C43 C42A 155(5) . . . . ?
C41 C42 C43 N39 16.5(14) . . . . ?
C41 C40 C44 O46 27.9(10) . . . . ?
N39 C40 C44 O46 161.9(4) . . . . ?
C41A C40 C44 O46 57.5(10) . . . . ?
C41 C40 C44 O45 -154.5(8) . . . . ?
N39 C40 C44 O45 -20.5(7) . . . . ?
C41A C40 C44 O45 -124.9(9) . . . . ?
C55 C50 C51 C52 2.0(8) . . . . ?
O49 C50 C51 C52 -177.5(5) . . . . ?
C50 C51 C52 C53 0.2(8) . . . . ?
C51 C52 C53 C54 -1.5(8) . . . . ?
C51 C52 C53 C62 177.0(5) . . . . ?
C52 C53 C54 C55 0.6(7) . . . . ?
C62 C53 C54 C55 -178.0(4) . . . . ?
C51 C50 C55 C54 -2.9(8) . . . . ?
O49 C50 C55 C54 176.7(4) . . . . ?
C51 C50 C55 N47 -180.0(5) . . . . ?
O49 C50 C55 N47 -0.4(5) . . . . ?
C53 C54 C55 C50 1.5(7) . . . . ?
C53 C54 C55 N47 177.7(5) . . . . ?
N47 C48 C56 C57 -0.5(7) . . . . ?
O49 C48 C56 C57 178.4(4) . . . . ?
N47 C48 C56 C61 178.4(5) . . . . ?
O49 C48 C56 C61 -2.7(8) . . . . ?
C61 C56 C57 C58 1.0(7) . . . . ?
C48 C56 C57 C58 180.0(5) . . . . ?
C61 C56 C57 Rh2 -174.7(4) . . . . ?
C48 C56 C57 Rh2 4.2(6) . . . . ?
C56 C57 C58 C59 -0.6(7) . . . . ?
Rh2 C57 C58 C59 174.5(4) . . . . ?
C57 C58 C59 C60 0.7(8) . . . . ?
C58 C59 C60 C61 -1.2(8) . . . . ?
C59 C60 C61 C56 1.6(8) . . . . ?
C57 C56 C61 C60 -1.6(8) . . . . ?
C48 C56 C61 C60 179.6(5) . . . . ?
C54 C53 C62 C65 58.0(6) . . . . ?
C52 C53 C62 C65 -120.6(5) . . . . ?
C54 C53 C62 C63 178.0(5) . . . . ?
C52 C53 C62 C63 -0.5(7) . . . . ?
C54 C53 C62 C64 -61.2(6) . . . . ?
C52 C53 C62 C64 120.3(5) . . . . ?
C73 C66 C69 C70 0.3(8) . . . . ?
N66 C66 C69 C70 179.2(5) . . . . ?
C73 C66 C69 O68 -178.9(5) . . . . ?
N66 C66 C69 O68 0.0(6) . . . . ?
C66 C69 C70 C71 -0.7(9) . . . . ?
O68 C69 C70 C71 178.3(5) . . . . ?
C69 C70 C71 C72 -0.9(9) . . . . ?
C70 C71 C72 C73 2.9(9) . . . . ?
C70 C71 C72 C80 -179.3(6) . . . . ?
C69 C66 C73 C72 1.8(8) . . . . ?
N66 C66 C73 C72 -176.8(5) . . . . ?
C71 C72 C73 C66 -3.3(8) . . . . ?
C80 C72 C73 C66 179.0(5) . . . . ?
N66 C67 C74 C79 179.5(5) . . . . ?
O68 C67 C74 C79 2.1(8) . . . . ?
N66 C67 C74 C75 1.0(7) . . . . ?
O68 C67 C74 C75 -176.4(5) . . . . ?
C79 C74 C75 C76 -1.5(8) . . . . ?
C67 C74 C75 C76 177.0(4) . . . . ?
C79 C74 C75 Rh2 177.8(4) . . . . ?
C67 C74 C75 Rh2 -3.8(6) . . . . ?
C74 C75 C76 C77 1.1(7) . . . . ?
Rh2 C75 C76 C77 -178.1(4) . . . . ?
C75 C76 C77 C78 0.6(8) . . . . ?
C76 C77 C78 C79 -1.9(9) . . . . ?
C77 C78 C79 C74 1.4(8) . . . . ?
C75 C74 C79 C78 0.3(8) . . . . ?
C67 C74 C79 C78 -178.0(5) . . . . ?
C73 C72 C80 C82 87.1(6) . . . . ?
C71 C72 C80 C82 -90.6(6) . . . . ?
C73 C72 C80 C83 -150.9(5) . . . . ?
C71 C72 C80 C83 31.4(7) . . . . ?
C73 C72 C80 C81 -31.7(7) . . . . ?
C71 C72 C80 C81 150.6(5) . . . . ?
N84 C85 C86 C87 -25.7(8) . . . . ?
C89 C85 C86 C87 97.8(7) . . . . ?
N84 C85 C86 C87A 9.7(9) . . . . ?
C89 C85 C86 C87A 133.1(7) . . . . ?
C85 C86 C87 C88 36.0(9) . . . . ?
C87A C86 C87 C88 -66.3(12) . . . . ?
C87 C86 C87A C88 66.5(12) . . . . ?
C85 C86 C87A C88 -21.0(11) . . . . ?
C86 C87A C88 N84 25.7(11) . . . . ?
C86 C87A C88 C87 -51.9(11) . . . . ?
C86 C87 C88 C87A 80.5(14) . . . . ?
C86 C87 C88 N84 -32.5(9) . . . . ?
N84 C85 C89 O91 174.7(4) . . . . ?
C86 C85 C89 O91 55.1(7) . . . . ?
N84 C85 C89 O90 -5.0(7) . . . . ?
C86 C85 C89 O90 -124.6(5) . . . . ?
O3 C2 N1 C9 -1.7(6) . . . . ?
C10 C2 N1 C9 177.7(4) . . . . ?
O3 C2 N1 Rh1 -177.3(3) . . . . ?
C10 C2 N1 Rh1 2.0(6) . . . . ?
C8 C9 N1 C2 -179.9(5) . . . . ?
C4 C9 N1 C2 1.5(5) . . . . ?
C8 C9 N1 Rh1 -6.0(9) . . . . ?
C4 C9 N1 Rh1 175.4(4) . . . . ?
O22 C21 N20 C28 -0.1(5) . . . . ?
C29 C21 N20 C28 -179.3(4) . . . . ?
O22 C21 N20 Rh1 -177.3(3) . . . . ?
C29 C21 N20 Rh1 3.5(6) . . . . ?
C23 C28 N20 C21 0.8(5) . . . . ?
C27 C28 N20 C21 179.1(6) . . . . ?
C23 C28 N20 Rh1 176.4(4) . . . . ?
C27 C28 N20 Rh1 -5.3(10) . . . . ?
O49 C48 N47 C55 -1.4(6) . . . . ?
C56 C48 N47 C55 177.6(5) . . . . ?
O49 C48 N47 Rh2 177.8(3) . . . . ?
C56 C48 N47 Rh2 -3.2(6) . . . . ?
C50 C55 N47 C48 1.0(5) . . . . ?
C54 C55 N47 C48 -175.5(5) . . . . ?
C50 C55 N47 Rh2 -177.7(4) . . . . ?
C54 C55 N47 Rh2 5.8(9) . . . . ?
O68 C67 N66 C66 -0.1(6) . . . . ?
C74 C67 N66 C66 -177.9(5) . . . . ?
O68 C67 N66 Rh2 179.8(3) . . . . ?
C74 C67 N66 Rh2 2.1(6) . . . . ?
C73 C66 N66 C67 178.8(6) . . . . ?
C69 C66 N66 C67 0.1(6) . . . . ?
C73 C66 N66 Rh2 -1.1(10) . . . . ?
C69 C66 N66 Rh2 -179.9(4) . . . . ?
C87A C88 N84 C85 -21.3(9) . . . . ?
C87 C88 N84 C85 13.7(6) . . . . ?
C87A C88 N84 Rh2 -146.0(7) . . . . ?
C87 C88 N84 Rh2 -111.0(5) . . . . ?
C86 C85 N84 C88 5.7(6) . . . . ?
C89 C85 N84 C88 -117.0(5) . . . . ?
C86 C85 N84 Rh2 135.5(4) . . . . ?
C89 C85 N84 Rh2 12.8(5) . . . . ?
N1 C2 O3 C4 1.1(5) . . . . ?
C10 C2 O3 C4 -178.2(5) . . . . ?
C5 C4 O3 C2 179.0(5) . . . . ?
C9 C4 O3 C2 0.0(5) . . . . ?
N20 C21 O22 C23 -0.6(5) . . . . ?
C29 C21 O22 C23 178.6(4) . . . . ?
C24 C23 O22 C21 -178.2(5) . . . . ?
C28 C23 O22 C21 1.1(5) . . . . ?
O46 C44 O45 Rh1 174.2(4) . . . . ?
C40 C44 O45 Rh1 -3.2(6) . . . . ?
N47 C48 O49 C50 1.1(6) . . . . ?
C56 C48 O49 C50 -177.8(5) . . . . ?
C51 C50 O49 C48 179.2(5) . . . . ?
C55 C50 O49 C48 -0.4(5) . . . . ?
N66 C67 O68 C69 0.1(6) . . . . ?
C74 C67 O68 C69 177.7(5) . . . . ?
C70 C69 O68 C67 -179.2(6) . . . . ?
C66 C69 O68 C67 -0.1(5) . . . . ?
O91 C89 O90 Rh2 174.1(4) . . . . ?
C85 C89 O90 Rh2 -6.3(6) . . . . ?

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
N39 H39 O91 1.00 1.95 2.881(5) 154.1 4_566
N84 H84 O46 1.00 2.17 2.937(5) 132.2 .

_refine_diff_density_max         0.569
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.073

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1027144'
#######################################################################
#
#                 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_delta-Rh


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C38 H38 N4 O2 Rh, F6 P, C H2 Cl2'
_chemical_formula_sum            'C39 H40 Cl2 F6 N4 O2 P Rh'
_chemical_formula_weight         915.53

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'
F F 0.0171 0.0103 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.1445(5)
_cell_length_b                   13.6427(6)
_cell_length_c                   22.5166(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4037.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9096
_cell_measurement_theta_min      2.3340
_cell_measurement_theta_max      27.4834

_exptl_crystal_description       nugget
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.662
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            39009
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.345
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9272
_reflns_number_gt                8540
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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       'BRUKER APEX2'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  ?

_refine_special_details          
; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0230P)²+1.5302P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 3570 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.033(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9272
_refine_ls_number_parameters     590
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0579
_refine_ls_wR_factor_gt          0.0560
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.043
_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_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
C2 C 0.9380(2) 0.4133(3) 0.58141(13) 0.0193(7) Uani 1 1 d . . . . .
C4 C 0.9731(2) 0.3630(2) 0.67024(13) 0.0194(7) Uani 1 1 d . . . . .
C5 C 1.0194(3) 0.3437(3) 0.72335(14) 0.0241(8) Uani 1 1 d . . . . .
H5 H 1.0880 0.3611 0.7312 0.029 Uiso 1 1 calc R U . . .
C6 C 0.9586(3) 0.2969(3) 0.76475(14) 0.0238(8) Uani 1 1 d . . . . .
H6 H 0.9875 0.2815 0.8023 0.029 Uiso 1 1 calc R U . . .
C7 C 0.8567(3) 0.2706(3) 0.75467(13) 0.0204(7) Uani 1 1 d . . . . .
C8 C 0.8127(2) 0.2927(3) 0.69979(13) 0.0180(7) Uani 1 1 d . . . . .
H8 H 0.7440 0.2762 0.6915 0.022 Uiso 1 1 calc R U . . .
C9 C 0.8726(2) 0.3396(2) 0.65773(13) 0.0174(7) Uani 1 1 d . . . . .
C10 C 0.9451(2) 0.4570(3) 0.52343(13) 0.0194(7) Uani 1 1 d . . . . .
C11 C 0.8497(2) 0.4588(2) 0.49439(13) 0.0166(7) Uani 1 1 d . . . . .
C12 C 0.8473(3) 0.5022(2) 0.43849(14) 0.0190(7) Uani 1 1 d . . . . .
H12 H 0.7847 0.5067 0.4176 0.023 Uiso 1 1 calc R U . . .
C13 C 0.9361(3) 0.5392(3) 0.41266(15) 0.0240(8) Uani 1 1 d . . . . .
H13 H 0.9327 0.5686 0.3745 0.029 Uiso 1 1 calc R U . . .
C14 C 1.0284(3) 0.5338(3) 0.44160(15) 0.0268(8) Uani 1 1 d . . . . .
H14 H 1.0882 0.5576 0.4229 0.032 Uiso 1 1 calc R U . . .
C15 C 1.0337(3) 0.4937(3) 0.49787(15) 0.0251(8) Uani 1 1 d . . . . .
H15 H 1.0965 0.4912 0.5187 0.030 Uiso 1 1 calc R U . . .
C16 C 0.7975(3) 0.2210(3) 0.80466(14) 0.0227(8) Uani 1 1 d . . . . .
C17 C 0.8507(3) 0.1251(3) 0.82232(16) 0.0327(9) Uani 1 1 d . . . . .
H17A H 0.8155 0.0959 0.8563 0.049 Uiso 1 1 calc R U . . .
H17B H 0.9215 0.1389 0.8331 0.049 Uiso 1 1 calc R U . . .
H17C H 0.8491 0.0793 0.7888 0.049 Uiso 1 1 calc R U . . .
C18 C 0.7943(3) 0.2904(3) 0.85839(15) 0.0335(9) Uani 1 1 d . . . . .
H18A H 0.7563 0.2593 0.8908 0.050 Uiso 1 1 calc R U . . .
H18B H 0.7606 0.3517 0.8471 0.050 Uiso 1 1 calc R U . . .
H18C H 0.8638 0.3044 0.8716 0.050 Uiso 1 1 calc R U . . .
C19 C 0.6878(3) 0.1972(3) 0.78641(17) 0.0325(10) Uani 1 1 d . . . . .
H19A H 0.6532 0.1637 0.8192 0.049 Uiso 1 1 calc R U . . .
H19B H 0.6885 0.1545 0.7514 0.049 Uiso 1 1 calc R U . . .
H19C H 0.6517 0.2581 0.7770 0.049 Uiso 1 1 calc R U . . .
C21 C 0.6472(2) 0.3340(2) 0.43079(13) 0.0163(7) Uani 1 1 d . . . . .
C23 C 0.5287(2) 0.4278(2) 0.39510(13) 0.0181(7) Uani 1 1 d . . . . .
C24 C 0.4502(3) 0.4680(3) 0.36293(14) 0.0225(7) Uani 1 1 d . . . . .
H24 H 0.4261 0.4388 0.3273 0.027 Uiso 1 1 calc R U . . .
C25 C 0.4082(3) 0.5535(3) 0.38529(15) 0.0231(7) Uani 1 1 d . . . . .
H25 H 0.3536 0.5832 0.3643 0.028 Uiso 1 1 calc R U . . .
C26 C 0.4432(2) 0.5982(3) 0.43795(14) 0.0201(7) Uani 1 1 d . . . . .
C27 C 0.5246(2) 0.5563(2) 0.46838(14) 0.0187(7) Uani 1 1 d . . . . .
H27 H 0.5516 0.5865 0.5030 0.022 Uiso 1 1 calc R U . . .
C28 C 0.5653(2) 0.4697(2) 0.44703(13) 0.0166(7) Uani 1 1 d . . . . .
C29 C 0.7201(2) 0.2574(2) 0.43945(13) 0.0156(6) Uani 1 1 d . . . . .
C30 C 0.7763(2) 0.2709(2) 0.49268(13) 0.0166(6) Uani 1 1 d . . . . .
C31 C 0.8485(3) 0.2003(3) 0.50598(15) 0.0229(7) Uani 1 1 d . . . . .
H31 H 0.8880 0.2059 0.5411 0.027 Uiso 1 1 calc R U . . .
C32 C 0.8634(3) 0.1212(3) 0.46811(15) 0.0286(8) Uani 1 1 d . . . . .
H32 H 0.9127 0.0731 0.4783 0.034 Uiso 1 1 calc R U . . .
C33 C 0.8086(2) 0.1102(3) 0.41581(14) 0.0238(7) Uani 1 1 d . . . . .
H33 H 0.8212 0.0560 0.3904 0.029 Uiso 1 1 calc R U . . .
C34 C 0.7359(3) 0.1786(2) 0.40126(12) 0.0190(6) Uani 1 1 d . . . . .
H34 H 0.6973 0.1722 0.3658 0.023 Uiso 1 1 calc R U . . .
C35 C 0.3887(2) 0.6891(3) 0.46178(17) 0.0244(7) Uani 1 1 d . . . . .
C36 C 0.4333(3) 0.7241(3) 0.52029(18) 0.0360(10) Uani 1 1 d . . . . .
H36A H 0.4275 0.6718 0.5500 0.054 Uiso 1 1 calc R U . . .
H36B H 0.3960 0.7820 0.5340 0.054 Uiso 1 1 calc R U . . .
H36C H 0.5051 0.7409 0.5146 0.054 Uiso 1 1 calc R U . . .
C37 C 0.3950(4) 0.7734(3) 0.41653(19) 0.0415(11) Uani 1 1 d . . . . .
H37A H 0.4663 0.7923 0.4110 0.062 Uiso 1 1 calc R U . . .
H37B H 0.3563 0.8297 0.4313 0.062 Uiso 1 1 calc R U . . .
H37C H 0.3665 0.7518 0.3785 0.062 Uiso 1 1 calc R U . . .
C38 C 0.2764(3) 0.6645(3) 0.47257(15) 0.0325(9) Uani 1 1 d . . . . .
H38A H 0.2714 0.6103 0.5010 0.049 Uiso 1 1 calc R U . . .
H38B H 0.2446 0.6453 0.4350 0.049 Uiso 1 1 calc R U . . .
H38C H 0.2415 0.7222 0.4886 0.049 Uiso 1 1 calc R U . . .
C40 C 0.5650(3) 0.2627(3) 0.60902(14) 0.0200(7) Uani 1 1 d . . . . .
C41 C 0.4883(3) 0.2022(3) 0.63783(17) 0.0310(9) Uani 1 1 d . . . . .
H01A H 0.4548 0.2401 0.6692 0.047 Uiso 1 1 calc R U . . .
H01B H 0.5208 0.1442 0.6552 0.047 Uiso 1 1 calc R U . . .
H01C H 0.4376 0.1815 0.6085 0.047 Uiso 1 1 calc R U . . .
C43 C 0.6479(3) 0.5755(3) 0.61529(17) 0.0375(10) Uani 1 1 d . . . . .
C44 C 0.5979(4) 0.6512(5) 0.6514(2) 0.079(2) Uani 1 1 d . . . . .
H01D H 0.6474 0.6799 0.6789 0.119 Uiso 1 1 calc R U . . .
H01E H 0.5420 0.6217 0.6740 0.119 Uiso 1 1 calc R U . . .
H01F H 0.5709 0.7025 0.6253 0.119 Uiso 1 1 calc R U . . .
N1 N 0.8532(2) 0.3740(2) 0.59967(10) 0.0177(6) Uani 1 1 d . . . . .
N20 N 0.64055(17) 0.40659(19) 0.46873(10) 0.0154(5) Uani 1 1 d . . . . .
N39 N 0.6252(2) 0.3097(2) 0.58661(11) 0.0190(6) Uani 1 1 d . . . . .
N42 N 0.6851(2) 0.5182(2) 0.58665(12) 0.0243(7) Uani 1 1 d . . . . .
O3 O 1.01489(16) 0.41047(19) 0.62104(9) 0.0222(5) Uani 1 1 d . . . . .
O22 O 0.58146(17) 0.34091(17) 0.38453(9) 0.0189(5) Uani 1 1 d . . . . .
F1 F 0.0907(12) 0.5002(8) 0.2920(7) 0.041(3) Uani 0.55(3) 1 d D U P A 1
F2 F 0.0651(10) 0.5806(9) 0.2057(4) 0.045(3) Uani 0.55(3) 1 d D U P A 1
F3 F 0.1609(13) 0.7056(10) 0.2374(7) 0.032(2) Uani 0.55(3) 1 d D U P A 1
F4 F 0.1879(10) 0.6250(12) 0.3256(5) 0.043(2) Uani 0.55(3) 1 d D U P A 1
F5 F 0.0296(8) 0.6528(9) 0.2927(6) 0.030(2) Uani 0.55(3) 1 d D U P A 1
F6 F 0.2257(9) 0.5538(7) 0.2354(7) 0.051(3) Uani 0.55(3) 1 d D U P A 1
P1 P 0.1279(9) 0.6021(9) 0.2653(5) 0.0274(9) Uani 0.55(3) 1 d D U P A 1
F1A F 0.1095(17) 0.5073(13) 0.3066(9) 0.060(4) Uani 0.45(3) 1 d D U P A 2
F2A F 0.1008(16) 0.5522(12) 0.2111(5) 0.061(3) Uani 0.45(3) 1 d D U P A 2
F3A F 0.1804(19) 0.6968(14) 0.2363(10) 0.050(5) Uani 0.45(3) 1 d D U P A 2
F4A F 0.1844(15) 0.6520(15) 0.3296(7) 0.060(4) Uani 0.45(3) 1 d D U P A 2
F5A F 0.0369(13) 0.6550(15) 0.2821(10) 0.061(5) Uani 0.45(3) 1 d D U P A 2
F6A F 0.2485(9) 0.5516(9) 0.2603(9) 0.054(3) Uani 0.45(3) 1 d D U P A 2
P1A P 0.1407(11) 0.6016(11) 0.2705(6) 0.0274(9) Uani 0.45(3) 1 d D U P A 2
Rh1 Rh 0.73792(2) 0.39113(2) 0.53888(2) 0.01450(6) Uani 1 1 d . . . . .
C1L C 0.7125(7) 0.4493(8) 0.2782(3) 0.074(3) Uani 0.815(4) 1 d D U P B 1
H7A H 0.7230 0.3919 0.3044 0.089 Uiso 0.815(4) 1 calc R U P B 1
H7B H 0.6715 0.4978 0.3006 0.089 Uiso 0.815(4) 1 calc R U P B 1
Cl1 Cl 0.64481(16) 0.41288(17) 0.21759(10) 0.0461(5) Uani 0.815(4) 1 d D U P B
1
Cl2 Cl 0.83155(10) 0.50147(11) 0.26207(6) 0.0420(4) Uani 0.815(4) 1 d D U P B 1
C1LA C 0.687(2) 0.3590(17) 0.2563(12) 0.066(8) Uani 0.185(4) 1 d D U P B 2
H5A H 0.7280 0.3115 0.2330 0.079 Uiso 0.185(4) 1 calc R U P B 2
H5B H 0.6407 0.3215 0.2823 0.079 Uiso 0.185(4) 1 calc R U P B 2
Cl1A Cl 0.7674(8) 0.4296(7) 0.2994(4) 0.073(3) Uani 0.185(4) 1 d D U P B 2
Cl2A Cl 0.6174(11) 0.4311(10) 0.2087(7) 0.107(6) Uani 0.185(4) 1 d D U P B 2


_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
C2 N1 1.304(4) . ?
C2 O3 1.349(4) . ?
C2 C10 1.439(4) . ?
C4 C5 1.367(4) . ?
C4 C9 1.388(4) . ?
C4 O3 1.396(4) . ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.405(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(4) . ?
C7 C16 1.527(5) . ?
C8 C9 1.388(5) . ?
C8 H8 0.9500 . ?
C9 N1 1.412(4) . ?
C10 C15 1.391(5) . ?
C10 C11 1.414(4) . ?
C11 C12 1.391(4) . ?
C11 Rh1 2.004(3) . ?
C12 C13 1.398(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C19 1.533(5) . ?
C16 C18 1.537(5) . ?
C16 C17 1.537(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 N20 1.310(4) . ?
C21 O22 1.356(4) . ?
C21 C29 1.432(4) . ?
C23 C24 1.375(4) . ?
C23 C28 1.388(4) . ?
C23 O22 1.394(4) . ?
C24 C25 1.385(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.411(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.394(4) . ?
C26 C35 1.529(5) . ?
C27 C28 1.383(5) . ?
C27 H27 0.9500 . ?
C28 N20 1.399(4) . ?
C29 C34 1.392(4) . ?
C29 C30 1.420(4) . ?
C30 C31 1.385(5) . ?
C30 Rh1 2.007(3) . ?
C31 C32 1.389(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.375(5) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.519(5) . ?
C35 C38 1.532(5) . ?
C35 C37 1.538(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C40 N39 1.136(4) . ?
C40 C41 1.456(5) . ?
C41 H01A 0.9800 . ?
C41 H01B 0.9800 . ?
C41 H01C 0.9800 . ?
C43 N42 1.125(5) . ?
C43 C44 1.469(6) . ?
C44 H01D 0.9800 . ?
C44 H01E 0.9800 . ?
C44 H01F 0.9800 . ?
N1 Rh1 2.056(2) . ?
N20 Rh1 2.044(2) . ?
N39 Rh1 2.142(3) . ?
N42 Rh1 2.155(3) . ?
F1 P1 1.592(10) . ?
F2 P1 1.602(10) . ?
F3 P1 1.605(11) . ?
F4 P1 1.601(10) . ?
F5 P1 1.590(10) . ?
F6 P1 1.593(10) . ?
F1A P1A 1.577(14) . ?
F2A P1A 1.588(13) . ?
F3A P1A 1.598(14) . ?
F4A P1A 1.605(13) . ?
F5A P1A 1.569(14) . ?
F6A P1A 1.589(12) . ?
C1L Cl1 1.704(8) . ?
C1L Cl2 1.758(7) . ?
C1L H7A 0.9900 . ?
C1L H7B 0.9900 . ?
C1LA Cl2A 1.721(19) . ?
C1LA Cl1A 1.73(2) . ?
C1LA H5A 0.9900 . ?
C1LA H5B 0.9900 . ?

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 C2 O3 114.9(3) . . ?
N1 C2 C10 120.8(3) . . ?
O3 C2 C10 124.3(3) . . ?
C5 C4 C9 123.8(3) . . ?
C5 C4 O3 127.5(3) . . ?
C9 C4 O3 108.7(3) . . ?
C4 C5 C6 114.9(3) . . ?
C4 C5 H5 122.5 . . ?
C6 C5 H5 122.5 . . ?
C5 C6 C7 124.0(3) . . ?
C5 C6 H6 118.0 . . ?
C7 C6 H6 118.0 . . ?
C8 C7 C6 118.8(3) . . ?
C8 C7 C16 122.5(3) . . ?
C6 C7 C16 118.7(3) . . ?
C9 C8 C7 117.9(3) . . ?
C9 C8 H8 121.0 . . ?
C7 C8 H8 121.0 . . ?
C8 C9 C4 120.5(3) . . ?
C8 C9 N1 133.0(3) . . ?
C4 C9 N1 106.5(3) . . ?
C15 C10 C11 123.0(3) . . ?
C15 C10 C2 125.4(3) . . ?
C11 C10 C2 111.7(3) . . ?
C12 C11 C10 116.5(3) . . ?
C12 C11 Rh1 129.2(3) . . ?
C10 C11 Rh1 114.3(2) . . ?
C11 C12 C13 120.7(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 121.2(3) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C10 118.6(3) . . ?
C14 C15 H15 120.7 . . ?
C10 C15 H15 120.7 . . ?
C7 C16 C19 112.1(3) . . ?
C7 C16 C18 108.7(3) . . ?
C19 C16 C18 108.4(3) . . ?
C7 C16 C17 109.6(3) . . ?
C19 C16 C17 108.5(3) . . ?
C18 C16 C17 109.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N20 C21 O22 114.0(3) . . ?
N20 C21 C29 120.5(3) . . ?
O22 C21 C29 125.5(3) . . ?
C24 C23 C28 122.7(3) . . ?
C24 C23 O22 128.5(3) . . ?
C28 C23 O22 108.8(3) . . ?
C23 C24 C25 116.3(3) . . ?
C23 C24 H24 121.8 . . ?
C25 C24 H24 121.8 . . ?
C24 C25 C26 122.7(3) . . ?
C24 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C27 C26 C25 119.1(3) . . ?
C27 C26 C35 121.3(3) . . ?
C25 C26 C35 119.5(3) . . ?
C28 C27 C26 118.5(3) . . ?
C28 C27 H27 120.8 . . ?
C26 C27 H27 120.8 . . ?
C27 C28 C23 120.7(3) . . ?
C27 C28 N20 132.7(3) . . ?
C23 C28 N20 106.6(3) . . ?
C34 C29 C30 122.9(3) . . ?
C34 C29 C21 125.5(3) . . ?
C30 C29 C21 111.6(3) . . ?
C31 C30 C29 116.7(3) . . ?
C31 C30 Rh1 129.0(2) . . ?
C29 C30 Rh1 114.4(2) . . ?
C30 C31 C32 120.3(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 122.1(3) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C29 118.7(3) . . ?
C33 C34 H34 120.6 . . ?
C29 C34 H34 120.6 . . ?
C36 C35 C26 112.2(3) . . ?
C36 C35 C38 107.6(3) . . ?
C26 C35 C38 109.3(3) . . ?
C36 C35 C37 108.6(3) . . ?
C26 C35 C37 110.4(3) . . ?
C38 C35 C37 108.7(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N39 C40 C41 179.7(4) . . ?
C40 C41 H01A 109.5 . . ?
C40 C41 H01B 109.5 . . ?
H01A C41 H01B 109.5 . . ?
C40 C41 H01C 109.5 . . ?
H01A C41 H01C 109.5 . . ?
H01B C41 H01C 109.5 . . ?
N42 C43 C44 178.6(5) . . ?
C43 C44 H01D 109.5 . . ?
C43 C44 H01E 109.5 . . ?
H01D C44 H01E 109.5 . . ?
C43 C44 H01F 109.5 . . ?
H01D C44 H01F 109.5 . . ?
H01E C44 H01F 109.5 . . ?
C2 N1 C9 105.9(3) . . ?
C2 N1 Rh1 111.9(2) . . ?
C9 N1 Rh1 141.9(2) . . ?
C21 N20 C28 106.5(2) . . ?
C21 N20 Rh1 112.6(2) . . ?
C28 N20 Rh1 140.9(2) . . ?
C40 N39 Rh1 175.8(3) . . ?
C43 N42 Rh1 170.0(3) . . ?
C2 O3 C4 104.1(2) . . ?
C21 O22 C23 104.2(2) . . ?
F5 P1 F1 89.0(8) . . ?
F5 P1 F6 177.8(9) . . ?
F1 P1 F6 92.6(8) . . ?
F5 P1 F4 89.2(8) . . ?
F1 P1 F4 90.0(8) . . ?
F6 P1 F4 92.3(7) . . ?
F5 P1 F2 89.2(7) . . ?
F1 P1 F2 89.9(7) . . ?
F6 P1 F2 89.3(6) . . ?
F4 P1 F2 178.4(9) . . ?
F5 P1 F3 89.4(8) . . ?
F1 P1 F3 177.8(10) . . ?
F6 P1 F3 88.9(8) . . ?
F4 P1 F3 91.6(8) . . ?
F2 P1 F3 88.4(8) . . ?
F5A P1A F1A 93.8(12) . . ?
F5A P1A F2A 92.9(10) . . ?
F1A P1A F2A 90.1(9) . . ?
F5A P1A F6A 177.3(12) . . ?
F1A P1A F6A 87.5(11) . . ?
F2A P1A F6A 89.5(8) . . ?
F5A P1A F3A 89.3(11) . . ?
F1A P1A F3A 175.7(13) . . ?
F2A P1A F3A 92.7(11) . . ?
F6A P1A F3A 89.3(10) . . ?
F5A P1A F4A 88.5(11) . . ?
F1A P1A F4A 90.8(10) . . ?
F2A P1A F4A 178.3(12) . . ?
F6A P1A F4A 89.1(9) . . ?
F3A P1A F4A 86.3(12) . . ?
C11 Rh1 C30 86.14(13) . . ?
C11 Rh1 N20 91.45(11) . . ?
C30 Rh1 N20 80.87(11) . . ?
C11 Rh1 N1 81.06(12) . . ?
C30 Rh1 N1 93.81(12) . . ?
N20 Rh1 N1 171.14(10) . . ?
C11 Rh1 N39 175.89(13) . . ?
C30 Rh1 N39 90.58(12) . . ?
N20 Rh1 N39 90.47(10) . . ?
N1 Rh1 N39 96.71(10) . . ?
C11 Rh1 N42 96.61(12) . . ?
C30 Rh1 N42 175.76(12) . . ?
N20 Rh1 N42 95.80(10) . . ?
N1 Rh1 N42 89.81(11) . . ?
N39 Rh1 N42 86.81(11) . . ?
Cl1 C1L Cl2 114.6(4) . . ?
Cl1 C1L H7A 108.6 . . ?
Cl2 C1L H7A 108.6 . . ?
Cl1 C1L H7B 108.6 . . ?
Cl2 C1L H7B 108.6 . . ?
H7A C1L H7B 107.6 . . ?
Cl2A C1LA Cl1A 110.9(14) . . ?
Cl2A C1LA H5A 109.5 . . ?
Cl1A C1LA H5A 109.5 . . ?
Cl2A C1LA H5B 109.5 . . ?
Cl1A C1LA H5B 109.5 . . ?
H5A C1LA H5B 108.1 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 C6 0.9(5) . . . . ?
O3 C4 C5 C6 178.9(3) . . . . ?
C4 C5 C6 C7 -0.4(5) . . . . ?
C5 C6 C7 C8 -0.1(5) . . . . ?
C5 C6 C7 C16 -178.8(3) . . . . ?
C6 C7 C8 C9 0.1(5) . . . . ?
C16 C7 C8 C9 178.8(3) . . . . ?
C7 C8 C9 C4 0.3(5) . . . . ?
C7 C8 C9 N1 -178.5(3) . . . . ?
C5 C4 C9 C8 -0.9(5) . . . . ?
O3 C4 C9 C8 -179.2(3) . . . . ?
C5 C4 C9 N1 178.2(3) . . . . ?
O3 C4 C9 N1 -0.1(4) . . . . ?
N1 C2 C10 C15 -174.5(3) . . . . ?
O3 C2 C10 C15 6.6(6) . . . . ?
N1 C2 C10 C11 5.5(5) . . . . ?
O3 C2 C10 C11 -173.4(3) . . . . ?
C15 C10 C11 C12 -1.7(5) . . . . ?
C2 C10 C11 C12 178.2(3) . . . . ?
C15 C10 C11 Rh1 175.2(3) . . . . ?
C2 C10 C11 Rh1 -4.8(4) . . . . ?
C10 C11 C12 C13 1.7(5) . . . . ?
Rh1 C11 C12 C13 -174.8(3) . . . . ?
C11 C12 C13 C14 0.1(5) . . . . ?
C12 C13 C14 C15 -1.9(6) . . . . ?
C13 C14 C15 C10 1.8(6) . . . . ?
C11 C10 C15 C14 0.1(6) . . . . ?
C2 C10 C15 C14 -179.9(3) . . . . ?
C8 C7 C16 C19 1.5(5) . . . . ?
C6 C7 C16 C19 -179.9(3) . . . . ?
C8 C7 C16 C18 -118.4(4) . . . . ?
C6 C7 C16 C18 60.3(4) . . . . ?
C8 C7 C16 C17 122.0(3) . . . . ?
C6 C7 C16 C17 -59.4(4) . . . . ?
C28 C23 C24 C25 -0.4(5) . . . . ?
O22 C23 C24 C25 177.0(3) . . . . ?
C23 C24 C25 C26 0.3(5) . . . . ?
C24 C25 C26 C27 1.3(5) . . . . ?
C24 C25 C26 C35 -176.3(3) . . . . ?
C25 C26 C27 C28 -2.7(5) . . . . ?
C35 C26 C27 C28 174.8(3) . . . . ?
C26 C27 C28 C23 2.7(5) . . . . ?
C26 C27 C28 N20 -174.9(3) . . . . ?
C24 C23 C28 C27 -1.1(5) . . . . ?
O22 C23 C28 C27 -178.9(3) . . . . ?
C24 C23 C28 N20 177.0(3) . . . . ?
O22 C23 C28 N20 -0.8(3) . . . . ?
N20 C21 C29 C34 -178.0(3) . . . . ?
O22 C21 C29 C34 1.0(5) . . . . ?
N20 C21 C29 C30 1.9(4) . . . . ?
O22 C21 C29 C30 -179.2(3) . . . . ?
C34 C29 C30 C31 -0.9(5) . . . . ?
C21 C29 C30 C31 179.3(3) . . . . ?
C34 C29 C30 Rh1 179.7(2) . . . . ?
C21 C29 C30 Rh1 -0.1(3) . . . . ?
C29 C30 C31 C32 0.2(5) . . . . ?
Rh1 C30 C31 C32 179.5(3) . . . . ?
C30 C31 C32 C33 0.8(5) . . . . ?
C31 C32 C33 C34 -1.2(5) . . . . ?
C32 C33 C34 C29 0.5(5) . . . . ?
C30 C29 C34 C33 0.5(5) . . . . ?
C21 C29 C34 C33 -179.6(3) . . . . ?
C27 C26 C35 C36 -0.5(4) . . . . ?
C25 C26 C35 C36 177.1(3) . . . . ?
C27 C26 C35 C38 -119.8(3) . . . . ?
C25 C26 C35 C38 57.8(4) . . . . ?
C27 C26 C35 C37 120.8(4) . . . . ?
C25 C26 C35 C37 -61.7(4) . . . . ?
O3 C2 N1 C9 -0.4(4) . . . . ?
C10 C2 N1 C9 -179.4(3) . . . . ?
O3 C2 N1 Rh1 175.6(2) . . . . ?
C10 C2 N1 Rh1 -3.4(4) . . . . ?
C8 C9 N1 C2 179.2(4) . . . . ?
C4 C9 N1 C2 0.3(4) . . . . ?
C8 C9 N1 Rh1 5.3(6) . . . . ?
C4 C9 N1 Rh1 -173.7(3) . . . . ?
O22 C21 N20 C28 -0.8(3) . . . . ?
C29 C21 N20 C28 178.3(3) . . . . ?
O22 C21 N20 Rh1 178.31(19) . . . . ?
C29 C21 N20 Rh1 -2.7(4) . . . . ?
C27 C28 N20 C21 178.7(3) . . . . ?
C23 C28 N20 C21 0.9(3) . . . . ?
C27 C28 N20 Rh1 0.1(6) . . . . ?
C23 C28 N20 Rh1 -177.7(2) . . . . ?
N1 C2 O3 C4 0.3(4) . . . . ?
C10 C2 O3 C4 179.2(3) . . . . ?
C5 C4 O3 C2 -178.3(3) . . . . ?
C9 C4 O3 C2 -0.1(3) . . . . ?
N20 C21 O22 C23 0.3(3) . . . . ?
C29 C21 O22 C23 -178.7(3) . . . . ?
C24 C23 O22 C21 -177.3(3) . . . . ?
C28 C23 O22 C21 0.4(3) . . . . ?

_refine_diff_density_max         0.511
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.059

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1027145'
#######################################################################
#
#                 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_5d


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H18 N2 O5'
_chemical_formula_sum            'C14 H18 N2 O5'
_chemical_formula_weight         294.30

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   5.4571(2)
_cell_length_b                   15.3289(6)
_cell_length_c                   17.4084(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1456.24(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4862
_cell_measurement_theta_min      2.3399
_cell_measurement_theta_max      27.1255

_exptl_crystal_description       Needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.103
_shelx_estimated_absorpt_T_min   0.955
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            11088
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.340
_diffrn_reflns_theta_max         25.488
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2707
_reflns_number_gt                2478
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'BRUKER APEX2'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  ?

_refine_special_details          
; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+0.2015P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 961 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.3(4)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         2707
_refine_ls_number_parameters     194
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0646
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
C1 C 0.8650(4) 0.44471(13) 0.44074(11) 0.0143(4) Uani 1 1 d . . . . .
C2 C 0.7628(4) 0.40594(13) 0.51374(11) 0.0140(4) Uani 1 1 d . . . . .
H2A H 0.8910 0.4083 0.5539 0.017 Uiso 1 1 calc R U . . .
H2B H 0.7243 0.3437 0.5044 0.017 Uiso 1 1 calc R U . . .
C3 C 0.5332(4) 0.45112(13) 0.54396(11) 0.0140(4) Uani 1 1 d . . . . .
H3 H 0.4157 0.4548 0.5000 0.017 Uiso 1 1 calc R U . . .
C4 C 0.4095(4) 0.39540(13) 0.60593(12) 0.0175(5) Uani 1 1 d . . . . .
H4A H 0.2667 0.4265 0.6263 0.026 Uiso 1 1 calc R U . . .
H4B H 0.5260 0.3842 0.6476 0.026 Uiso 1 1 calc R U . . .
H4C H 0.3567 0.3398 0.5835 0.026 Uiso 1 1 calc R U . . .
C5 C 1.0745(4) 0.39691(13) 0.40693(11) 0.0147(4) Uani 1 1 d . . . . .
C7 C 1.3982(4) 0.36787(13) 0.33707(12) 0.0180(5) Uani 1 1 d . . . . .
H7 H 1.5284 0.3711 0.3010 0.022 Uiso 1 1 calc R U . . .
C8 C 1.3512(4) 0.30125(13) 0.38729(12) 0.0182(5) Uani 1 1 d . . . . .
H8 H 1.4459 0.2494 0.3912 0.022 Uiso 1 1 calc R U . . .
C10 C 1.2085(4) 0.51382(13) 0.31185(12) 0.0232(5) Uani 1 1 d . . . . .
H10A H 1.3417 0.5187 0.2743 0.035 Uiso 1 1 calc R U . . .
H10B H 1.2253 0.5599 0.3505 0.035 Uiso 1 1 calc R U . . .
H10C H 1.0507 0.5200 0.2856 0.035 Uiso 1 1 calc R U . . .
C11 C 0.5822(4) 0.54524(12) 0.57049(11) 0.0132(4) Uani 1 1 d . . . . .
H11 H 0.6876 0.5721 0.5299 0.016 Uiso 1 1 calc R U . . .
C12 C 0.7250(4) 0.55347(12) 0.64473(11) 0.0154(4) Uani 1 1 d . . . . .
C14 C 0.5853(4) 0.70400(13) 0.64554(12) 0.0188(5) Uani 1 1 d . . . . .
C16 C 0.3500(4) 0.59880(13) 0.57233(11) 0.0155(4) Uani 1 1 d . . . . .
C17 C 0.7422(4) 0.74769(13) 0.58537(13) 0.0210(5) Uani 1 1 d . . . . .
H17A H 0.6545 0.7980 0.5642 0.031 Uiso 1 1 calc R U . . .
H17B H 0.7780 0.7061 0.5441 0.031 Uiso 1 1 calc R U . . .
H17C H 0.8960 0.7673 0.6088 0.031 Uiso 1 1 calc R U . . .
C18 C 0.5160(5) 0.76403(15) 0.71055(14) 0.0293(6) Uani 1 1 d . . . . .
H18A H 0.4210 0.8132 0.6904 0.044 Uiso 1 1 calc R U . . .
H18B H 0.6649 0.7859 0.7354 0.044 Uiso 1 1 calc R U . . .
H18C H 0.4172 0.7320 0.7481 0.044 Uiso 1 1 calc R U . . .
N6 N 1.2201(3) 0.42861(10) 0.34942(9) 0.0153(4) Uani 1 1 d . . . . .
N9 N 1.1499(3) 0.31928(10) 0.43096(10) 0.0172(4) Uani 1 1 d . . . . .
O1 O 0.7853(3) 0.51138(8) 0.41140(8) 0.0182(3) Uani 1 1 d . . . . .
O12 O 0.8432(3) 0.49683(9) 0.67424(8) 0.0202(3) Uani 1 1 d . . . . .
O13 O 0.7110(3) 0.63175(8) 0.68082(8) 0.0201(4) Uani 1 1 d . . . . .
O15 O 0.3564(3) 0.67425(9) 0.61291(8) 0.0200(3) Uani 1 1 d . . . . .
O16 O 0.1627(3) 0.57962(9) 0.54018(8) 0.0207(4) Uani 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
C1 O1 1.222(2) . ?
C1 C5 1.480(3) . ?
C1 C2 1.510(3) . ?
C2 C3 1.525(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.533(3) . ?
C3 C11 1.538(3) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N9 1.327(3) . ?
C5 N6 1.368(3) . ?
C7 N6 1.363(3) . ?
C7 C8 1.369(3) . ?
C7 H7 0.9500 . ?
C8 N9 1.364(3) . ?
C8 H8 0.9500 . ?
C10 N6 1.462(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C16 1.510(3) . ?
C11 C12 1.514(3) . ?
C11 H11 1.0000 . ?
C12 O12 1.197(2) . ?
C12 O13 1.357(2) . ?
C14 O13 1.440(3) . ?
C14 O15 1.446(3) . ?
C14 C18 1.507(3) . ?
C14 C17 1.510(3) . ?
C16 O16 1.202(2) . ?
C16 O15 1.356(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

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
O1 C1 C5 121.51(18) . . ?
O1 C1 C2 123.33(18) . . ?
C5 C1 C2 115.16(17) . . ?
C1 C2 C3 114.52(17) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 C4 110.58(16) . . ?
C2 C3 C11 112.73(16) . . ?
C4 C3 C11 112.83(16) . . ?
C2 C3 H3 106.7 . . ?
C4 C3 H3 106.7 . . ?
C11 C3 H3 106.7 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N9 C5 N6 111.67(17) . . ?
N9 C5 C1 123.94(18) . . ?
N6 C5 C1 124.34(17) . . ?
N6 C7 C8 105.98(18) . . ?
N6 C7 H7 127.0 . . ?
C8 C7 H7 127.0 . . ?
N9 C8 C7 110.84(18) . . ?
N9 C8 H8 124.6 . . ?
C7 C8 H8 124.6 . . ?
N6 C10 H10A 109.5 . . ?
N6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 111.62(16) . . ?
C16 C11 C3 111.72(16) . . ?
C12 C11 C3 115.07(16) . . ?
C16 C11 H11 105.9 . . ?
C12 C11 H11 105.9 . . ?
C3 C11 H11 105.9 . . ?
O12 C12 O13 118.24(18) . . ?
O12 C12 C11 125.66(18) . . ?
O13 C12 C11 116.09(17) . . ?
O13 C14 O15 109.66(15) . . ?
O13 C14 C18 105.59(18) . . ?
O15 C14 C18 105.71(18) . . ?
O13 C14 C17 111.54(18) . . ?
O15 C14 C17 110.94(18) . . ?
C18 C14 C17 113.12(18) . . ?
O16 C16 O15 118.25(18) . . ?
O16 C16 C11 124.80(18) . . ?
O15 C16 C11 116.95(17) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C7 N6 C5 106.69(16) . . ?
C7 N6 C10 124.80(17) . . ?
C5 N6 C10 128.29(17) . . ?
C5 N9 C8 104.82(17) . . ?
C12 O13 C14 120.64(15) . . ?
C16 O15 C14 119.73(16) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 6.2(3) . . . . ?
C5 C1 C2 C3 -174.80(16) . . . . ?
C1 C2 C3 C4 166.64(17) . . . . ?
C1 C2 C3 C11 -66.0(2) . . . . ?
O1 C1 C5 N9 -171.78(19) . . . . ?
C2 C1 C5 N9 9.2(3) . . . . ?
O1 C1 C5 N6 11.0(3) . . . . ?
C2 C1 C5 N6 -167.99(18) . . . . ?
N6 C7 C8 N9 -0.5(2) . . . . ?
C2 C3 C11 C16 159.09(17) . . . . ?
C4 C3 C11 C16 -74.8(2) . . . . ?
C2 C3 C11 C12 -72.3(2) . . . . ?
C4 C3 C11 C12 53.9(2) . . . . ?
C16 C11 C12 O12 145.5(2) . . . . ?
C3 C11 C12 O12 16.8(3) . . . . ?
C16 C11 C12 O13 -33.0(2) . . . . ?
C3 C11 C12 O13 -161.70(16) . . . . ?
C12 C11 C16 O16 -147.7(2) . . . . ?
C3 C11 C16 O16 -17.2(3) . . . . ?
C12 C11 C16 O15 32.9(2) . . . . ?
C3 C11 C16 O15 163.32(16) . . . . ?
C8 C7 N6 C5 0.6(2) . . . . ?
C8 C7 N6 C10 175.56(19) . . . . ?
N9 C5 N6 C7 -0.5(2) . . . . ?
C1 C5 N6 C7 176.95(18) . . . . ?
N9 C5 N6 C10 -175.25(19) . . . . ?
C1 C5 N6 C10 2.2(3) . . . . ?
N6 C5 N9 C8 0.2(2) . . . . ?
C1 C5 N9 C8 -177.27(18) . . . . ?
C7 C8 N9 C5 0.2(2) . . . . ?
O12 C12 O13 C14 175.80(19) . . . . ?
C11 C12 O13 C14 -5.6(3) . . . . ?
O15 C14 O13 C12 44.0(2) . . . . ?
C18 C14 O13 C12 157.41(18) . . . . ?
C17 C14 O13 C12 -79.3(2) . . . . ?
O16 C16 O15 C14 -173.51(18) . . . . ?
C11 C16 O15 C14 6.0(3) . . . . ?
O13 C14 O15 C16 -44.0(2) . . . . ?
C18 C14 O15 C16 -157.37(17) . . . . ?
C17 C14 O15 C16 79.7(2) . . . . ?

_refine_diff_density_max         0.146
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.035

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1027146'
#######################################################################
#
#                 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.
# 
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#  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_5f


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            w234b
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H26 N2 O4'
_chemical_formula_sum            'C22 H26 N2 O4'
_chemical_formula_weight         382.45

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1905(5)
_cell_length_b                   11.5731(6)
_cell_length_c                   17.4203(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.5045(16)
_cell_angle_gamma                90
_cell_volume                     2036.88(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9754
_cell_measurement_theta_min      2.3585
_cell_measurement_theta_max      27.4950

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.086
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            47435
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.118
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4679
_reflns_number_gt                3939
_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       'BRUKER APEX2'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  ?

_refine_special_details          
; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0574P)²+0.6490P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4679
_refine_ls_number_parameters     258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1004
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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
C1 C 0.21092(13) 0.34740(11) 0.48117(7) 0.0194(3) Uani 1 1 d . . . . .
C2 C 0.30438(14) 0.37209(11) 0.42221(7) 0.0218(3) Uani 1 1 d . . . . .
H2A H 0.3941 0.3865 0.4499 0.026 Uiso 1 1 calc R U . . .
H2B H 0.2750 0.4434 0.3936 0.026 Uiso 1 1 calc R U . . .
C3 C 0.31207(13) 0.27380(11) 0.36402(7) 0.0194(3) Uani 1 1 d . . . . .
H3 H 0.2244 0.2336 0.3569 0.023 Uiso 1 1 calc R U . . .
C4 C 0.33720(12) 0.32174(11) 0.28458(7) 0.0173(2) Uani 1 1 d . . . . .
C5 C 0.34956(12) 0.22095(11) 0.22694(7) 0.0175(3) Uani 1 1 d . . . . .
C6 C 0.46918(12) 0.24108(10) 0.18959(7) 0.0166(2) Uani 1 1 d . . . . .
C7 C 0.51388(12) 0.17753(11) 0.12994(7) 0.0186(3) Uani 1 1 d . . . . .
H7 H 0.4671 0.1113 0.1090 0.022 Uiso 1 1 calc R U . . .
C8 C 0.62802(13) 0.21385(11) 0.10231(7) 0.0221(3) Uani 1 1 d . . . . .
H8 H 0.6606 0.1727 0.0615 0.027 Uiso 1 1 calc R U . . .
C9 C 0.69578(13) 0.31128(12) 0.13434(8) 0.0239(3) Uani 1 1 d . . . . .
H9 H 0.7740 0.3353 0.1147 0.029 Uiso 1 1 calc R U . . .
C10 C 0.65182(12) 0.37381(11) 0.19408(7) 0.0203(3) Uani 1 1 d . . . . .
H10 H 0.6994 0.4393 0.2156 0.024 Uiso 1 1 calc R U . . .
C11 C 0.53613(12) 0.33789(10) 0.22157(7) 0.0168(2) Uani 1 1 d . . . . .
C12 C 0.46703(12) 0.39203(11) 0.28426(7) 0.0185(3) Uani 1 1 d . . . . .
H12A H 0.4472 0.4744 0.2726 0.022 Uiso 1 1 calc R U . . .
H12B H 0.5228 0.3866 0.3351 0.022 Uiso 1 1 calc R U . . .
C13 C 0.19358(12) 0.44430(11) 0.53375(7) 0.0175(3) Uani 1 1 d . . . . .
C15 C 0.11292(13) 0.55579(11) 0.61768(7) 0.0205(3) Uani 1 1 d . . . . .
H15 H 0.0609 0.5862 0.6544 0.025 Uiso 1 1 calc R U . . .
C16 C 0.21861(13) 0.60779(11) 0.59095(7) 0.0213(3) Uani 1 1 d . . . . .
H16 H 0.2524 0.6818 0.6068 0.026 Uiso 1 1 calc R U . . .
C18 C -0.00127(13) 0.36553(12) 0.59573(8) 0.0235(3) Uani 1 1 d . . . . .
H18A H -0.0712 0.4026 0.6206 0.035 Uiso 1 1 calc R U . . .
H18B H 0.0412 0.3052 0.6298 0.035 Uiso 1 1 calc R U . . .
H18C H -0.0398 0.3310 0.5466 0.035 Uiso 1 1 calc R U . . .
C19 C 0.41680(14) 0.18588(12) 0.39667(8) 0.0267(3) Uani 1 1 d . . . . .
H19A H 0.3957 0.1570 0.4465 0.040 Uiso 1 1 calc R U . . .
H19B H 0.5039 0.2230 0.4041 0.040 Uiso 1 1 calc R U . . .
H19C H 0.4179 0.1213 0.3604 0.040 Uiso 1 1 calc R U . . .
C20 C 0.21652(12) 0.39176(11) 0.24849(7) 0.0192(3) Uani 1 1 d . . . . .
C22 C 0.14827(13) 0.52571(11) 0.14079(7) 0.0207(3) Uani 1 1 d . . . . .
C23 C 0.13181(17) 0.62899(13) 0.19245(9) 0.0328(3) Uani 1 1 d . . . . .
H23A H 0.2192 0.6584 0.2138 0.049 Uiso 1 1 calc R U . . .
H23B H 0.0833 0.6054 0.2349 0.049 Uiso 1 1 calc R U . . .
H23C H 0.0824 0.6898 0.1620 0.049 Uiso 1 1 calc R U . . .
C24 C 0.01731(14) 0.46780(13) 0.11242(9) 0.0303(3) Uani 1 1 d . . . . .
H24A H -0.0262 0.4446 0.1569 0.045 Uiso 1 1 calc R U . . .
H24B H 0.0332 0.3994 0.0818 0.045 Uiso 1 1 calc R U . . .
H24C H -0.0396 0.5220 0.0802 0.045 Uiso 1 1 calc R U . . .
C25 C 0.22027(15) 0.55797(13) 0.07284(8) 0.0292(3) Uani 1 1 d . . . . .
H25A H 0.3068 0.5911 0.0921 0.044 Uiso 1 1 calc R U . . .
H25B H 0.1679 0.6149 0.0403 0.044 Uiso 1 1 calc R U . . .
H25C H 0.2326 0.4888 0.0422 0.044 Uiso 1 1 calc R U . . .
N14 N 0.09708(10) 0.45169(9) 0.58118(6) 0.0176(2) Uani 1 1 d . . . . .
N17 N 0.26887(11) 0.53899(9) 0.53846(6) 0.0206(2) Uani 1 1 d . . . . .
O1 O 0.15165(10) 0.25630(8) 0.48425(6) 0.0278(2) Uani 1 1 d . . . . .
O5 O 0.27226(9) 0.14132(8) 0.21652(5) 0.0251(2) Uani 1 1 d . . . . .
O20 O 0.11369(10) 0.39777(9) 0.27515(6) 0.0316(3) Uani 1 1 d . . . . .
O21 O 0.24198(9) 0.44233(8) 0.18336(5) 0.0207(2) Uani 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
C1 O1 1.2197(16) . ?
C1 C13 1.4731(17) . ?
C1 C2 1.5163(17) . ?
C2 C3 1.5323(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C19 1.5295(17) . ?
C3 C4 1.5431(17) . ?
C3 H3 1.0000 . ?
C4 C20 1.5370(17) . ?
C4 C12 1.5537(17) . ?
C4 C5 1.5549(17) . ?
C5 O5 1.2106(15) . ?
C5 C6 1.4733(16) . ?
C6 C11 1.3899(17) . ?
C6 C7 1.3972(17) . ?
C7 C8 1.3811(18) . ?
C7 H7 0.9500 . ?
C8 C9 1.3996(19) . ?
C8 H8 0.9500 . ?
C9 C10 1.3889(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.3927(17) . ?
C10 H10 0.9500 . ?
C11 C12 1.5107(16) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N17 1.3341(17) . ?
C13 N14 1.3673(15) . ?
C15 N14 1.3619(17) . ?
C15 C16 1.3674(19) . ?
C15 H15 0.9500 . ?
C16 N17 1.3619(16) . ?
C16 H16 0.9500 . ?
C18 N14 1.4593(17) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 O20 1.2025(15) . ?
C20 O21 1.3319(15) . ?
C22 O21 1.4860(15) . ?
C22 C24 1.5172(18) . ?
C22 C25 1.5185(18) . ?
C22 C23 1.5186(19) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?

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
O1 C1 C13 122.03(12) . . ?
O1 C1 C2 123.45(11) . . ?
C13 C1 C2 114.50(11) . . ?
C1 C2 C3 113.52(11) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C19 C3 C2 109.95(11) . . ?
C19 C3 C4 112.53(10) . . ?
C2 C3 C4 110.80(10) . . ?
C19 C3 H3 107.8 . . ?
C2 C3 H3 107.8 . . ?
C4 C3 H3 107.8 . . ?
C20 C4 C3 109.80(10) . . ?
C20 C4 C12 111.02(10) . . ?
C3 C4 C12 115.63(10) . . ?
C20 C4 C5 105.03(10) . . ?
C3 C4 C5 110.26(10) . . ?
C12 C4 C5 104.46(9) . . ?
O5 C5 C6 127.87(11) . . ?
O5 C5 C4 124.19(11) . . ?
C6 C5 C4 107.94(10) . . ?
C11 C6 C7 122.12(11) . . ?
C11 C6 C5 109.98(10) . . ?
C7 C6 C5 127.89(11) . . ?
C8 C7 C6 118.05(12) . . ?
C8 C7 H7 121.0 . . ?
C6 C7 H7 121.0 . . ?
C7 C8 C9 120.02(12) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 121.86(12) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C11 118.19(12) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C6 C11 C10 119.74(11) . . ?
C6 C11 C12 111.92(10) . . ?
C10 C11 C12 128.34(11) . . ?
C11 C12 C4 105.24(10) . . ?
C11 C12 H12A 110.7 . . ?
C4 C12 H12A 110.7 . . ?
C11 C12 H12B 110.7 . . ?
C4 C12 H12B 110.7 . . ?
H12A C12 H12B 108.8 . . ?
N17 C13 N14 111.38(11) . . ?
N17 C13 C1 123.29(11) . . ?
N14 C13 C1 125.28(11) . . ?
N14 C15 C16 106.32(11) . . ?
N14 C15 H15 126.8 . . ?
C16 C15 H15 126.8 . . ?
N17 C16 C15 110.69(12) . . ?
N17 C16 H16 124.7 . . ?
C15 C16 H16 124.7 . . ?
N14 C18 H18A 109.5 . . ?
N14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C3 C19 H19A 109.5 . . ?
C3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O20 C20 O21 125.47(12) . . ?
O20 C20 C4 124.30(11) . . ?
O21 C20 C4 110.22(10) . . ?
O21 C22 C24 110.87(10) . . ?
O21 C22 C25 101.78(10) . . ?
C24 C22 C25 110.41(11) . . ?
O21 C22 C23 109.20(11) . . ?
C24 C22 C23 112.34(12) . . ?
C25 C22 C23 111.75(11) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C15 N14 C13 106.66(11) . . ?
C15 N14 C18 124.45(11) . . ?
C13 N14 C18 128.80(11) . . ?
C13 N17 C16 104.95(11) . . ?
C20 O21 C22 121.77(10) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 2.93(18) . . . . ?
C13 C1 C2 C3 -175.27(11) . . . . ?
C1 C2 C3 C19 -87.08(14) . . . . ?
C1 C2 C3 C4 147.89(11) . . . . ?
C19 C3 C4 C20 169.77(11) . . . . ?
C2 C3 C4 C20 -66.67(13) . . . . ?
C19 C3 C4 C12 -63.67(14) . . . . ?
C2 C3 C4 C12 59.89(14) . . . . ?
C19 C3 C4 C5 54.51(14) . . . . ?
C2 C3 C4 C5 178.07(10) . . . . ?
C20 C4 C5 O5 -69.79(15) . . . . ?
C3 C4 C5 O5 48.44(16) . . . . ?
C12 C4 C5 O5 173.28(12) . . . . ?
C20 C4 C5 C6 110.39(11) . . . . ?
C3 C4 C5 C6 -131.38(10) . . . . ?
C12 C4 C5 C6 -6.54(12) . . . . ?
O5 C5 C6 C11 -175.69(12) . . . . ?
C4 C5 C6 C11 4.12(13) . . . . ?
O5 C5 C6 C7 5.3(2) . . . . ?
C4 C5 C6 C7 -174.89(12) . . . . ?
C11 C6 C7 C8 -0.39(18) . . . . ?
C5 C6 C7 C8 178.50(12) . . . . ?
C6 C7 C8 C9 0.39(19) . . . . ?
C7 C8 C9 C10 0.1(2) . . . . ?
C8 C9 C10 C11 -0.7(2) . . . . ?
C7 C6 C11 C10 -0.14(18) . . . . ?
C5 C6 C11 C10 -179.21(11) . . . . ?
C7 C6 C11 C12 179.28(11) . . . . ?
C5 C6 C11 C12 0.20(14) . . . . ?
C9 C10 C11 C6 0.66(18) . . . . ?
C9 C10 C11 C12 -178.65(12) . . . . ?
C6 C11 C12 C4 -4.39(14) . . . . ?
C10 C11 C12 C4 174.97(12) . . . . ?
C20 C4 C12 C11 -106.26(11) . . . . ?
C3 C4 C12 C11 127.80(11) . . . . ?
C5 C4 C12 C11 6.44(12) . . . . ?
O1 C1 C13 N17 171.20(12) . . . . ?
C2 C1 C13 N17 -10.57(17) . . . . ?
O1 C1 C13 N14 -11.49(19) . . . . ?
C2 C1 C13 N14 166.74(11) . . . . ?
N14 C15 C16 N17 0.24(15) . . . . ?
C3 C4 C20 O20 -6.85(18) . . . . ?
C12 C4 C20 O20 -135.97(13) . . . . ?
C5 C4 C20 O20 111.69(14) . . . . ?
C3 C4 C20 O21 174.26(10) . . . . ?
C12 C4 C20 O21 45.15(13) . . . . ?
C5 C4 C20 O21 -67.20(12) . . . . ?
C16 C15 N14 C13 0.02(13) . . . . ?
C16 C15 N14 C18 176.93(11) . . . . ?
N17 C13 N14 C15 -0.27(14) . . . . ?
C1 C13 N14 C15 -177.86(11) . . . . ?
N17 C13 N14 C18 -177.01(12) . . . . ?
C1 C13 N14 C18 5.4(2) . . . . ?
N14 C13 N17 C16 0.41(14) . . . . ?
C1 C13 N17 C16 178.05(11) . . . . ?
C15 C16 N17 C13 -0.40(14) . . . . ?
O20 C20 O21 C22 7.9(2) . . . . ?
C4 C20 O21 C22 -173.25(10) . . . . ?
C24 C22 O21 C20 -62.63(15) . . . . ?
C25 C22 O21 C20 179.93(11) . . . . ?
C23 C22 O21 C20 61.67(15) . . . . ?

_refine_diff_density_max         0.353
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.085

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1027147'
#######################################################################
#
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#                                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_w261_0m_sq

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C49 H48 N4 O3 Rh, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C51 H52 Cl4 F6 N4 O3 P Rh'
_chemical_formula_weight         1158.64

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'
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'
F F 0.0171 0.0103 '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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   17.7761(6)
_cell_length_b                   22.9437(8)
_cell_length_c                   13.1111(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5347.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9841
_cell_measurement_theta_min      2.4575
_cell_measurement_theta_max      25.2916

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_F_000             2368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.615
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            56957
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.113
_diffrn_reflns_theta_max         25.329
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             9643
_reflns_number_gt                8691
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_max     0.974
_reflns_Friedel_fraction_full    0.978

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _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       'BRUKER APEX2 2014.1-1'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  ?

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+3.7850P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 3767 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.015(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9643
_refine_ls_number_parameters     705
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0889
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.013
_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
C2 C 0.7586(3) 0.5353(2) 0.1040(4) 0.0152(10) Uani 1 1 d . . . . .
C4 C 0.8392(3) 0.5018(2) -0.0047(4) 0.0154(10) Uani 1 1 d . . . . .
C5 C 0.8915(3) 0.4952(2) -0.0811(4) 0.0218(12) Uani 1 1 d . . . . .
H5 H 0.9081 0.5270 -0.1218 0.026 Uiso 1 1 calc R U . . .
C6 C 0.9184(3) 0.4391(2) -0.0947(4) 0.0220(12) Uani 1 1 d . . . . .
H6 H 0.9550 0.4325 -0.1462 0.026 Uiso 1 1 calc R U . . .
C7 C 0.8940(3) 0.3912(2) -0.0358(4) 0.0226(12) Uani 1 1 d . . . . .
C8 C 0.8412(3) 0.3998(2) 0.0410(4) 0.0176(11) Uani 1 1 d . . . . .
H8 H 0.8241 0.3684 0.0821 0.021 Uiso 1 1 calc R U . . .
C9 C 0.8143(3) 0.4564(2) 0.0555(4) 0.0154(10) Uani 1 1 d . . . . .
C10 C 0.7104(3) 0.5723(2) 0.1630(4) 0.0165(10) Uani 1 1 d . . . . .
C11 C 0.6708(2) 0.54103(19) 0.2388(6) 0.0156(9) Uani 1 1 d . . . . .
C12 C 0.6222(3) 0.5728(2) 0.3011(4) 0.0189(11) Uani 1 1 d . . . . .
H12 H 0.5940 0.5535 0.3525 0.023 Uiso 1 1 calc R U . . .
C13 C 0.6149(3) 0.6328(2) 0.2884(4) 0.0245(12) Uani 1 1 d . . . . .
H13 H 0.5820 0.6539 0.3319 0.029 Uiso 1 1 calc R U . . .
C14 C 0.6547(3) 0.6623(2) 0.2139(4) 0.0234(12) Uani 1 1 d . . . . .
H14 H 0.6491 0.7032 0.2067 0.028 Uiso 1 1 calc R U . . .
C15 C 0.7026(3) 0.6321(2) 0.1499(4) 0.0220(11) Uani 1 1 d . . . . .
H15 H 0.7297 0.6519 0.0979 0.026 Uiso 1 1 calc R U . . .
C16 C 0.9270(3) 0.3307(2) -0.0585(5) 0.0262(12) Uani 1 1 d . . . . .
C17 C 1.0134(3) 0.3333(3) -0.0468(5) 0.0356(15) Uani 1 1 d . . . . .
H17A H 1.0349 0.2950 -0.0618 0.053 Uiso 1 1 calc R U . . .
H17B H 1.0261 0.3445 0.0233 0.053 Uiso 1 1 calc R U . . .
H17C H 1.0340 0.3622 -0.0943 0.053 Uiso 1 1 calc R U . . .
C18 C 0.9076(4) 0.3139(3) -0.1681(5) 0.0361(15) Uani 1 1 d . . . . .
H18A H 0.9288 0.2754 -0.1834 0.054 Uiso 1 1 calc R U . . .
H18B H 0.9288 0.3428 -0.2151 0.054 Uiso 1 1 calc R U . . .
H18C H 0.8528 0.3127 -0.1762 0.054 Uiso 1 1 calc R U . . .
C19 C 0.8977(4) 0.2837(2) 0.0155(5) 0.0371(15) Uani 1 1 d . . . . .
H19A H 0.9224 0.2465 0.0007 0.056 Uiso 1 1 calc R U . . .
H19B H 0.8432 0.2794 0.0069 0.056 Uiso 1 1 calc R U . . .
H19C H 0.9087 0.2954 0.0858 0.056 Uiso 1 1 calc R U . . .
C21 C 0.5525(3) 0.4274(2) 0.3204(4) 0.0158(11) Uani 1 1 d . . . . .
C23 C 0.5405(3) 0.4278(3) 0.4853(5) 0.0198(13) Uani 1 1 d . . . . .
C24 C 0.5139(3) 0.4247(2) 0.5833(4) 0.0232(12) Uani 1 1 d . . . . .
H24 H 0.4629 0.4161 0.5986 0.028 Uiso 1 1 calc R U . . .
C25 C 0.5672(3) 0.4353(3) 0.6583(4) 0.0271(12) Uani 1 1 d . . . . .
H25 H 0.5514 0.4343 0.7275 0.033 Uiso 1 1 calc R U . . .
C26 C 0.6429(3) 0.4473(3) 0.6378(4) 0.0290(14) Uani 1 1 d . . . . .
C27 C 0.6663(3) 0.4514(2) 0.5362(4) 0.0226(12) Uani 1 1 d . . . . .
H27 H 0.7166 0.4614 0.5193 0.027 Uiso 1 1 calc R U . . .
C28 C 0.6139(3) 0.4402(3) 0.4616(4) 0.0162(12) Uani 1 1 d . . . . .
C29 C 0.5403(3) 0.4258(2) 0.2125(4) 0.0174(12) Uani 1 1 d . . . . .
C30 C 0.6060(3) 0.4409(2) 0.1580(4) 0.0157(11) Uani 1 1 d . . . . .
C31 C 0.6014(3) 0.4413(3) 0.0522(5) 0.0232(13) Uani 1 1 d . . . . .
H31 H 0.6439 0.4522 0.0127 0.028 Uiso 1 1 calc R U . . .
C32 C 0.5338(4) 0.4257(3) 0.0037(5) 0.0298(16) Uani 1 1 d . . . . .
H32 H 0.5316 0.4255 -0.0687 0.036 Uiso 1 1 calc R U . . .
C33 C 0.4708(3) 0.4107(3) 0.0587(5) 0.0291(13) Uani 1 1 d . . . . .
H33 H 0.4257 0.4004 0.0243 0.035 Uiso 1 1 calc R U . . .
C34 C 0.4734(3) 0.4106(2) 0.1645(4) 0.0229(11) Uani 1 1 d . . . . .
H34 H 0.4302 0.4003 0.2033 0.028 Uiso 1 1 calc R U . . .
C35 C 0.6985(3) 0.4569(3) 0.7261(5) 0.0418(19) Uani 1 1 d D U . . .
C36 C 0.6728(4) 0.5066(4) 0.7927(6) 0.0333(19) Uani 0.75 1 d D U P A 1
H36A H 0.7059 0.5096 0.8523 0.050 Uiso 0.75 1 calc R U P A 1
H36B H 0.6211 0.4995 0.8153 0.050 Uiso 0.75 1 calc R U P A 1
H36C H 0.6748 0.5431 0.7538 0.050 Uiso 0.75 1 calc R U P A 1
C37 C 0.6982(4) 0.4000(4) 0.7950(6) 0.039(2) Uani 0.75 1 d D U P A 1
H37A H 0.7339 0.4049 0.8513 0.058 Uiso 0.75 1 calc R U P A 1
H37B H 0.7129 0.3663 0.7537 0.058 Uiso 0.75 1 calc R U P A 1
H37C H 0.6476 0.3938 0.8226 0.058 Uiso 0.75 1 calc R U P A 1
C38 C 0.7783(4) 0.4663(6) 0.6904(6) 0.051(3) Uani 0.75 1 d D U P A 1
H38A H 0.8118 0.4687 0.7496 0.077 Uiso 0.75 1 calc R U P A 1
H38B H 0.7813 0.5026 0.6513 0.077 Uiso 0.75 1 calc R U P A 1
H38C H 0.7937 0.4336 0.6470 0.077 Uiso 0.75 1 calc R U P A 1
C36A C 0.6682(16) 0.4691(15) 0.8285(16) 0.062(8) Uani 0.25 1 d D U P A 2
H36D H 0.7095 0.4705 0.8778 0.094 Uiso 0.25 1 calc R U P A 2
H36E H 0.6328 0.4383 0.8479 0.094 Uiso 0.25 1 calc R U P A 2
H36F H 0.6420 0.5067 0.8278 0.094 Uiso 0.25 1 calc R U P A 2
C37A C 0.7601(16) 0.4121(12) 0.7173(19) 0.062(8) Uani 0.25 1 d D U P A 2
H37D H 0.7921 0.4138 0.7781 0.093 Uiso 0.25 1 calc R U P A 2
H37E H 0.7905 0.4203 0.6566 0.093 Uiso 0.25 1 calc R U P A 2
H37F H 0.7379 0.3732 0.7115 0.093 Uiso 0.25 1 calc R U P A 2
C38A C 0.7422(17) 0.5168(10) 0.693(2) 0.064(7) Uani 0.25 1 d D U P A 2
H38D H 0.7776 0.5279 0.7470 0.096 Uiso 0.25 1 calc R U P A 2
H38E H 0.7054 0.5481 0.6832 0.096 Uiso 0.25 1 calc R U P A 2
H38F H 0.7698 0.5102 0.6294 0.096 Uiso 0.25 1 calc R U P A 2
C40 C 0.7940(3) 0.3591(2) 0.3124(4) 0.0164(10) Uani 1 1 d . . . . .
C42 C 0.7603(2) 0.27462(19) 0.2489(6) 0.0238(10) Uani 1 1 d . . . . .
H42 H 0.7580 0.2343 0.2330 0.029 Uiso 1 1 calc R U . . .
C43 C 0.7129(3) 0.3168(2) 0.2137(4) 0.0228(12) Uani 1 1 d . . . . .
H43 H 0.6714 0.3108 0.1692 0.027 Uiso 1 1 calc R U . . .
C44 C 0.8258(3) 0.4094(2) 0.3660(4) 0.0153(10) Uani 1 1 d . . . . .
C45 C 0.8871(3) 0.4061(2) 0.4389(4) 0.0194(11) Uani 1 1 d . . . . .
H45 H 0.9137 0.3704 0.4472 0.023 Uiso 1 1 calc R U . . .
C46 C 0.9066(3) 0.4526(2) 0.4948(4) 0.0163(10) Uani 1 1 d . . . . .
H46 H 0.8803 0.4877 0.4808 0.020 Uiso 1 1 calc R U . . .
C47 C 0.9636(3) 0.4555(2) 0.5745(4) 0.0171(11) Uani 1 1 d . . . . .
C48 C 1.0075(3) 0.4078(2) 0.6027(4) 0.0193(11) Uani 1 1 d . . . . .
H48 H 1.0005 0.3713 0.5700 0.023 Uiso 1 1 calc R U . . .
C49 C 1.0617(3) 0.4136(2) 0.6788(4) 0.0219(12) Uani 1 1 d . . . . .
H49 H 1.0912 0.3809 0.6978 0.026 Uiso 1 1 calc R U . . .
C50 C 1.0728(3) 0.4669(2) 0.7272(4) 0.0246(14) Uani 1 1 d . . . . .
H50 H 1.1101 0.4706 0.7787 0.030 Uiso 1 1 calc R U . . .
C51 C 1.0290(3) 0.5147(2) 0.6996(4) 0.0216(11) Uani 1 1 d . . . . .
H51 H 1.0362 0.5510 0.7329 0.026 Uiso 1 1 calc R U . . .
C52 C 0.9750(3) 0.5094(2) 0.6236(4) 0.0198(11) Uani 1 1 d . . . . .
H52 H 0.9456 0.5422 0.6047 0.024 Uiso 1 1 calc R U . . .
C53 C 0.8667(3) 0.2686(2) 0.3748(5) 0.0277(13) Uani 1 1 d . . . . .
H53 H 0.9133 0.2928 0.3814 0.033 Uiso 1 1 calc R U . . .
C54 C 0.8876(4) 0.2110(3) 0.3239(7) 0.0475(19) Uani 1 1 d . . . . .
H54A H 0.8980 0.2178 0.2515 0.071 Uiso 1 1 calc R U . . .
H54B H 0.8456 0.1836 0.3307 0.071 Uiso 1 1 calc R U . . .
H54C H 0.9323 0.1948 0.3570 0.071 Uiso 1 1 calc R U . . .
C55 C 0.8331(4) 0.2603(3) 0.4801(6) 0.052(2) Uani 1 1 d . . . . .
H55A H 0.8241 0.2985 0.5113 0.078 Uiso 1 1 calc R U . . .
H55B H 0.8681 0.2380 0.5226 0.078 Uiso 1 1 calc R U . . .
H55C H 0.7854 0.2392 0.4744 0.078 Uiso 1 1 calc R U . . .
C102 C 0.6065(6) 0.2754(5) 0.5710(11) 0.050(3) Uani 0.75 1 d . U P B 1
H10C H 0.6161 0.3176 0.5623 0.060 Uiso 0.75 1 calc R U P B 1
H10D H 0.6160 0.2559 0.5049 0.060 Uiso 0.75 1 calc R U P B 1
C103 C 0.611(2) 0.2476(17) 0.560(4) 0.061(11) Uani 0.25 1 d . U P B 2
H10A H 0.6377 0.2234 0.6108 0.073 Uiso 0.25 1 calc R U P B 2
H10B H 0.6078 0.2249 0.4956 0.073 Uiso 0.25 1 calc R U P B 2
N1 N 0.7628(2) 0.47930(18) 0.1247(3) 0.0133(8) Uani 1 1 d . . . . .
N20 N 0.6194(2) 0.4402(2) 0.3555(4) 0.0157(10) Uani 1 1 d . . . . .
N39 N 0.73465(19) 0.36858(16) 0.2526(4) 0.0160(8) Uani 1 1 d . . . . .
N41 N 0.8116(2) 0.30101(17) 0.3112(4) 0.0185(9) Uani 1 1 d . . . . .
O2 O 0.79427(18) 0.45752(14) 0.3474(3) 0.0144(8) Uani 1 1 d . . . . .
O3 O 0.80303(19) 0.55200(15) 0.0255(3) 0.0180(8) Uani 1 1 d . . . . .
O22 O 0.50022(19) 0.41915(16) 0.3949(3) 0.0203(8) Uani 1 1 d . . . . .
F1 F 0.6169(2) 0.20441(17) 0.1901(3) 0.0454(10) Uani 1 1 d . . . . .
F2 F 0.50195(19) 0.17047(17) 0.2378(4) 0.0518(9) Uani 1 1 d . . . . .
F3 F 0.5476(2) 0.1505(3) 0.3934(4) 0.0771(16) Uani 1 1 d . . . . .
F4 F 0.5601(2) 0.24118(19) 0.3286(4) 0.0615(13) Uani 1 1 d . . . . .
F5 F 0.6615(2) 0.18410(18) 0.3464(3) 0.0488(10) Uani 1 1 d . . . . .
F6 F 0.6046(2) 0.11396(15) 0.2530(5) 0.0628(12) Uani 1 1 d . . . . .
P1 P 0.58229(9) 0.17759(8) 0.29215(14) 0.0368(4) Uani 1 1 d . . . . .
Rh1 Rh 0.69601(2) 0.45559(2) 0.24407(3) 0.01252(10) Uani 1 1 d . . . . .
C100 C 0.2026(5) 0.3587(6) 0.0292(10) 0.060(3) Uani 0.75 1 d D U P C 1
H10E H 0.1642 0.3705 0.0798 0.073 Uiso 0.75 1 calc R U P C 1
H10F H 0.1873 0.3206 0.0004 0.073 Uiso 0.75 1 calc R U P C 1
Cl1 Cl 0.20605(10) 0.41002(10) -0.06767(17) 0.0595(6) Uani 1 1 d D U . . .
Cl2 Cl 0.28857(11) 0.35112(12) 0.0895(2) 0.0555(7) Uani 0.75 1 d D U P C 1
C101 C 0.2229(19) 0.3384(10) -0.021(3) 0.085(9) Uani 0.25 1 d D U P C 2
H10G H 0.2769 0.3378 -0.0024 0.102 Uiso 0.25 1 calc R U P C 2
H10H H 0.1951 0.3363 0.0445 0.102 Uiso 0.25 1 calc R U P C 2
Cl2A Cl 0.2065(5) 0.2717(6) -0.0801(14) 0.125(5) Uani 0.25 1 d D U P C 2
Cl3 Cl 0.51385(12) 0.26466(10) 0.6067(2) 0.0796(8) Uani 1 1 d . U . . .
Cl4 Cl 0.66813(16) 0.24692(12) 0.6647(2) 0.0630(7) Uani 0.75 1 d . U P B 1
Cl5 Cl 0.6607(6) 0.3097(4) 0.5383(10) 0.090(3) Uani 0.25 1 d . U P B 2


_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
C2 N1 1.316(6) . ?
C2 O3 1.353(6) . ?
C2 C10 1.432(7) . ?
C4 C5 1.375(7) . ?
C4 O3 1.377(6) . ?
C4 C9 1.379(7) . ?
C5 C6 1.384(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.412(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.390(7) . ?
C7 C16 1.535(8) . ?
C8 C9 1.397(7) . ?
C8 H8 0.9500 . ?
C9 N1 1.392(6) . ?
C10 C15 1.391(7) . ?
C10 C11 1.412(8) . ?
C11 C12 1.395(8) . ?
C11 Rh1 2.012(4) . ?
C12 C13 1.392(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C18 1.527(8) . ?
C16 C19 1.542(8) . ?
C16 C17 1.544(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 N20 1.309(7) . ?
C21 O22 1.362(6) . ?
C21 C29 1.431(8) . ?
C23 C24 1.371(8) . ?
C23 C28 1.372(8) . ?
C23 O22 1.398(7) . ?
C24 C25 1.387(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.399(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.399(8) . ?
C26 C35 1.538(8) . ?
C27 C28 1.374(8) . ?
C27 H27 0.9500 . ?
C28 N20 1.395(7) . ?
C29 C34 1.391(7) . ?
C29 C30 1.411(7) . ?
C30 C31 1.390(8) . ?
C30 Rh1 1.987(6) . ?
C31 C32 1.406(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.375(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(8) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36A 1.474(16) . ?
C35 C37A 1.507(16) . ?
C35 C36 1.508(10) . ?
C35 C38 1.510(9) . ?
C35 C37 1.587(10) . ?
C35 C38A 1.637(18) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?
C37A H37D 0.9800 . ?
C37A H37E 0.9800 . ?
C37A H37F 0.9800 . ?
C38A H38D 0.9800 . ?
C38A H38E 0.9800 . ?
C38A H38F 0.9800 . ?
C40 N39 1.332(6) . ?
C40 N41 1.369(7) . ?
C40 C44 1.465(7) . ?
C42 C43 1.364(7) . ?
C42 N41 1.366(7) . ?
C42 H42 0.9500 . ?
C43 N39 1.349(7) . ?
C43 H43 0.9500 . ?
C44 O2 1.262(6) . ?
C44 C45 1.452(7) . ?
C45 C46 1.341(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.457(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.393(7) . ?
C47 C52 1.409(7) . ?
C48 C49 1.392(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.391(8) . ?
C49 H49 0.9500 . ?
C50 C51 1.393(8) . ?
C50 H50 0.9500 . ?
C51 C52 1.390(7) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 N41 1.486(7) . ?
C53 C55 1.517(9) . ?
C53 C54 1.525(8) . ?
C53 H53 1.0000 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C102 Cl3 1.729(10) . ?
C102 Cl4 1.771(13) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C103 Cl5 1.70(4) . ?
C103 Cl3 1.88(4) . ?
C103 H10A 0.9900 . ?
C103 H10B 0.9900 . ?
N1 Rh1 2.038(4) . ?
N20 Rh1 2.028(5) . ?
N39 Rh1 2.114(4) . ?
O2 Rh1 2.211(3) . ?
F1 P1 1.596(4) . ?
F2 P1 1.604(4) . ?
F3 P1 1.591(4) . ?
F4 P1 1.585(5) . ?
F5 P1 1.585(4) . ?
F6 P1 1.597(4) . ?
C100 Cl2 1.729(10) . ?
C100 Cl1 1.733(10) . ?
C100 H10E 0.9900 . ?
C100 H10F 0.9900 . ?
Cl1 C101 1.78(2) . ?
C101 Cl2A 1.74(3) . ?
C101 H10G 0.9900 . ?
C101 H10H 0.9900 . ?

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 C2 O3 113.6(4) . . ?
N1 C2 C10 120.0(4) . . ?
O3 C2 C10 126.4(4) . . ?
C5 C4 O3 128.1(5) . . ?
C5 C4 C9 123.4(5) . . ?
O3 C4 C9 108.5(4) . . ?
C4 C5 C6 115.4(5) . . ?
C4 C5 H5 122.3 . . ?
C6 C5 H5 122.3 . . ?
C5 C6 C7 123.2(5) . . ?
C5 C6 H6 118.4 . . ?
C7 C6 H6 118.4 . . ?
C8 C7 C6 119.5(5) . . ?
C8 C7 C16 121.9(5) . . ?
C6 C7 C16 118.7(5) . . ?
C7 C8 C9 117.6(5) . . ?
C7 C8 H8 121.2 . . ?
C9 C8 H8 121.2 . . ?
C4 C9 N1 107.4(4) . . ?
C4 C9 C8 120.9(5) . . ?
N1 C9 C8 131.7(5) . . ?
C15 C10 C11 122.6(5) . . ?
C15 C10 C2 125.2(5) . . ?
C11 C10 C2 112.2(4) . . ?
C12 C11 C10 117.0(4) . . ?
C12 C11 Rh1 128.8(5) . . ?
C10 C11 Rh1 114.1(4) . . ?
C13 C12 C11 120.3(5) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 121.3(5) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C15 C14 C13 120.0(5) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C10 118.7(5) . . ?
C14 C15 H15 120.7 . . ?
C10 C15 H15 120.7 . . ?
C18 C16 C7 108.9(5) . . ?
C18 C16 C19 109.8(5) . . ?
C7 C16 C19 112.4(5) . . ?
C18 C16 C17 109.2(5) . . ?
C7 C16 C17 109.1(4) . . ?
C19 C16 C17 107.5(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N20 C21 O22 113.5(5) . . ?
N20 C21 C29 119.4(5) . . ?
O22 C21 C29 127.1(4) . . ?
C24 C23 C28 123.4(5) . . ?
C24 C23 O22 127.6(5) . . ?
C28 C23 O22 108.9(5) . . ?
C23 C24 C25 114.8(5) . . ?
C23 C24 H24 122.6 . . ?
C25 C24 H24 122.6 . . ?
C24 C25 C26 123.7(5) . . ?
C24 C25 H25 118.2 . . ?
C26 C25 H25 118.2 . . ?
C27 C26 C25 118.9(5) . . ?
C27 C26 C35 121.1(5) . . ?
C25 C26 C35 120.1(5) . . ?
C28 C27 C26 117.6(5) . . ?
C28 C27 H27 121.2 . . ?
C26 C27 H27 121.2 . . ?
C23 C28 C27 121.5(5) . . ?
C23 C28 N20 107.0(5) . . ?
C27 C28 N20 131.5(5) . . ?
C34 C29 C30 122.7(5) . . ?
C34 C29 C21 125.6(5) . . ?
C30 C29 C21 111.6(5) . . ?
C31 C30 C29 117.3(5) . . ?
C31 C30 Rh1 127.8(4) . . ?
C29 C30 Rh1 114.9(4) . . ?
C30 C31 C32 120.0(6) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 121.5(6) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C32 C33 C34 119.8(5) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C33 C34 C29 118.6(5) . . ?
C33 C34 H34 120.7 . . ?
C29 C34 H34 120.7 . . ?
C36A C35 C37A 117.7(13) . . ?
C36 C35 C38 110.9(7) . . ?
C36A C35 C26 118.6(12) . . ?
C37A C35 C26 108.2(12) . . ?
C36 C35 C26 110.5(5) . . ?
C38 C35 C26 113.0(6) . . ?
C36 C35 C37 106.9(6) . . ?
C38 C35 C37 107.3(6) . . ?
C26 C35 C37 108.0(6) . . ?
C36A C35 C38A 104.7(14) . . ?
C37A C35 C38A 101.9(12) . . ?
C26 C35 C38A 103.1(11) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C36A H36D 109.5 . . ?
C35 C36A H36E 109.5 . . ?
H36D C36A H36E 109.5 . . ?
C35 C36A H36F 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 109.5 . . ?
C35 C37A H37D 109.5 . . ?
C35 C37A H37E 109.5 . . ?
H37D C37A H37E 109.5 . . ?
C35 C37A H37F 109.5 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?
C35 C38A H38D 109.5 . . ?
C35 C38A H38E 109.5 . . ?
H38D C38A H38E 109.5 . . ?
C35 C38A H38F 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?
N39 C40 N41 109.4(4) . . ?
N39 C40 C44 117.4(4) . . ?
N41 C40 C44 133.2(4) . . ?
C43 C42 N41 107.5(4) . . ?
C43 C42 H42 126.3 . . ?
N41 C42 H42 126.3 . . ?
N39 C43 C42 108.7(5) . . ?
N39 C43 H43 125.7 . . ?
C42 C43 H43 125.7 . . ?
O2 C44 C45 120.5(5) . . ?
O2 C44 C40 115.1(4) . . ?
C45 C44 C40 124.3(5) . . ?
C46 C45 C44 120.8(5) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 127.4(5) . . ?
C45 C46 H46 116.3 . . ?
C47 C46 H46 116.3 . . ?
C48 C47 C52 119.2(5) . . ?
C48 C47 C46 123.0(5) . . ?
C52 C47 C46 117.8(4) . . ?
C49 C48 C47 120.2(5) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C50 C49 C48 120.6(5) . . ?
C50 C49 H49 119.7 . . ?
C48 C49 H49 119.7 . . ?
C49 C50 C51 119.6(5) . . ?
C49 C50 H50 120.2 . . ?
C51 C50 H50 120.2 . . ?
C52 C51 C50 120.3(5) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 C47 120.2(5) . . ?
C51 C52 H52 119.9 . . ?
C47 C52 H52 119.9 . . ?
N41 C53 C55 108.2(5) . . ?
N41 C53 C54 110.4(5) . . ?
C55 C53 C54 112.7(6) . . ?
N41 C53 H53 108.5 . . ?
C55 C53 H53 108.5 . . ?
C54 C53 H53 108.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
Cl3 C102 Cl4 110.4(7) . . ?
Cl3 C102 H10C 109.6 . . ?
Cl4 C102 H10C 109.6 . . ?
Cl3 C102 H10D 109.6 . . ?
Cl4 C102 H10D 109.6 . . ?
H10C C102 H10D 108.1 . . ?
Cl5 C103 Cl3 111(2) . . ?
Cl5 C103 H10A 109.5 . . ?
Cl3 C103 H10A 109.5 . . ?
Cl5 C103 H10B 109.5 . . ?
Cl3 C103 H10B 109.5 . . ?
H10A C103 H10B 108.0 . . ?
C2 N1 C9 105.7(4) . . ?
C2 N1 Rh1 112.7(3) . . ?
C9 N1 Rh1 141.5(3) . . ?
C21 N20 C28 106.7(5) . . ?
C21 N20 Rh1 113.3(4) . . ?
C28 N20 Rh1 139.9(4) . . ?
C40 N39 C43 107.8(4) . . ?
C40 N39 Rh1 116.3(3) . . ?
C43 N39 Rh1 135.9(3) . . ?
C42 N41 C40 106.6(4) . . ?
C42 N41 C53 123.6(4) . . ?
C40 N41 C53 129.2(4) . . ?
C44 O2 Rh1 116.9(3) . . ?
C2 O3 C4 104.8(4) . . ?
C21 O22 C23 103.9(4) . . ?
F4 P1 F5 90.0(2) . . ?
F4 P1 F3 90.7(3) . . ?
F5 P1 F3 90.4(2) . . ?
F4 P1 F1 89.6(2) . . ?
F5 P1 F1 89.9(2) . . ?
F3 P1 F1 179.6(3) . . ?
F4 P1 F6 178.8(3) . . ?
F5 P1 F6 90.5(2) . . ?
F3 P1 F6 90.4(3) . . ?
F1 P1 F6 89.3(3) . . ?
F4 P1 F2 90.3(2) . . ?
F5 P1 F2 179.5(3) . . ?
F3 P1 F2 89.2(2) . . ?
F1 P1 F2 90.6(2) . . ?
F6 P1 F2 89.2(2) . . ?
C30 Rh1 C11 88.1(2) . . ?
C30 Rh1 N20 80.7(2) . . ?
C11 Rh1 N20 92.6(2) . . ?
C30 Rh1 N1 94.52(19) . . ?
C11 Rh1 N1 81.0(2) . . ?
N20 Rh1 N1 172.12(18) . . ?
C30 Rh1 N39 97.54(19) . . ?
C11 Rh1 N39 173.79(15) . . ?
N20 Rh1 N39 90.90(18) . . ?
N1 Rh1 N39 95.95(17) . . ?
C30 Rh1 O2 170.97(18) . . ?
C11 Rh1 O2 100.22(17) . . ?
N20 Rh1 O2 95.33(16) . . ?
N1 Rh1 O2 90.29(15) . . ?
N39 Rh1 O2 74.32(14) . . ?
Cl2 C100 Cl1 111.8(5) . . ?
Cl2 C100 H10E 109.2 . . ?
Cl1 C100 H10E 109.2 . . ?
Cl2 C100 H10F 109.2 . . ?
Cl1 C100 H10F 109.2 . . ?
H10E C100 H10F 107.9 . . ?
Cl2A C101 Cl1 129(2) . . ?
Cl2A C101 H10G 105.0 . . ?
Cl1 C101 H10G 105.0 . . ?
Cl2A C101 H10H 105.0 . . ?
Cl1 C101 H10H 105.0 . . ?
H10G C101 H10H 105.9 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C4 C5 C6 -179.7(5) . . . . ?
C9 C4 C5 C6 0.1(7) . . . . ?
C4 C5 C6 C7 0.6(8) . . . . ?
C5 C6 C7 C8 -0.9(8) . . . . ?
C5 C6 C7 C16 179.3(5) . . . . ?
C6 C7 C8 C9 0.5(7) . . . . ?
C16 C7 C8 C9 -179.8(5) . . . . ?
C5 C4 C9 N1 179.2(4) . . . . ?
O3 C4 C9 N1 -0.9(5) . . . . ?
C5 C4 C9 C8 -0.5(8) . . . . ?
O3 C4 C9 C8 179.4(4) . . . . ?
C7 C8 C9 C4 0.2(7) . . . . ?
C7 C8 C9 N1 -179.5(5) . . . . ?
N1 C2 C10 C15 178.4(5) . . . . ?
O3 C2 C10 C15 -1.2(8) . . . . ?
N1 C2 C10 C11 -1.1(7) . . . . ?
O3 C2 C10 C11 179.3(5) . . . . ?
C15 C10 C11 C12 0.3(8) . . . . ?
C2 C10 C11 C12 179.8(4) . . . . ?
C15 C10 C11 Rh1 -177.7(4) . . . . ?
C2 C10 C11 Rh1 1.8(6) . . . . ?
C10 C11 C12 C13 -0.8(8) . . . . ?
Rh1 C11 C12 C13 176.9(4) . . . . ?
C11 C12 C13 C14 0.6(8) . . . . ?
C12 C13 C14 C15 0.3(8) . . . . ?
C13 C14 C15 C10 -0.7(8) . . . . ?
C11 C10 C15 C14 0.5(8) . . . . ?
C2 C10 C15 C14 -179.0(5) . . . . ?
C8 C7 C16 C18 119.4(6) . . . . ?
C6 C7 C16 C18 -60.9(6) . . . . ?
C8 C7 C16 C19 -2.5(7) . . . . ?
C6 C7 C16 C19 177.3(5) . . . . ?
C8 C7 C16 C17 -121.6(6) . . . . ?
C6 C7 C16 C17 58.2(7) . . . . ?
C28 C23 C24 C25 0.0(9) . . . . ?
O22 C23 C24 C25 179.9(5) . . . . ?
C23 C24 C25 C26 -1.0(9) . . . . ?
C24 C25 C26 C27 2.7(10) . . . . ?
C24 C25 C26 C35 -178.4(6) . . . . ?
C25 C26 C27 C28 -3.3(9) . . . . ?
C35 C26 C27 C28 177.8(6) . . . . ?
C24 C23 C28 C27 -0.8(9) . . . . ?
O22 C23 C28 C27 179.3(5) . . . . ?
C24 C23 C28 N20 -179.2(5) . . . . ?
O22 C23 C28 N20 0.8(6) . . . . ?
C26 C27 C28 C23 2.4(9) . . . . ?
C26 C27 C28 N20 -179.5(6) . . . . ?
N20 C21 C29 C34 177.2(5) . . . . ?
O22 C21 C29 C34 -5.6(9) . . . . ?
N20 C21 C29 C30 -1.9(8) . . . . ?
O22 C21 C29 C30 175.3(5) . . . . ?
C34 C29 C30 C31 1.3(8) . . . . ?
C21 C29 C30 C31 -179.5(5) . . . . ?
C34 C29 C30 Rh1 -176.0(4) . . . . ?
C21 C29 C30 Rh1 3.1(6) . . . . ?
C29 C30 C31 C32 -1.6(9) . . . . ?
Rh1 C30 C31 C32 175.4(5) . . . . ?
C30 C31 C32 C33 1.2(10) . . . . ?
C31 C32 C33 C34 -0.3(10) . . . . ?
C32 C33 C34 C29 0.0(9) . . . . ?
C30 C29 C34 C33 -0.5(8) . . . . ?
C21 C29 C34 C33 -179.6(6) . . . . ?
C27 C26 C35 C36A 162.4(16) . . . . ?
C25 C26 C35 C36A -16.5(17) . . . . ?
C27 C26 C35 C37A -60.1(14) . . . . ?
C25 C26 C35 C37A 121.0(13) . . . . ?
C27 C26 C35 C36 120.8(7) . . . . ?
C25 C26 C35 C36 -58.1(8) . . . . ?
C27 C26 C35 C38 -4.1(10) . . . . ?
C25 C26 C35 C38 177.0(7) . . . . ?
C27 C26 C35 C37 -122.6(6) . . . . ?
C25 C26 C35 C37 58.5(8) . . . . ?
C27 C26 C35 C38A 47.3(13) . . . . ?
C25 C26 C35 C38A -131.6(13) . . . . ?
N41 C42 C43 N39 0.5(7) . . . . ?
N39 C40 C44 O2 -1.8(6) . . . . ?
N41 C40 C44 O2 179.8(5) . . . . ?
N39 C40 C44 C45 175.7(5) . . . . ?
N41 C40 C44 C45 -2.6(8) . . . . ?
O2 C44 C45 C46 6.3(7) . . . . ?
C40 C44 C45 C46 -171.2(5) . . . . ?
C44 C45 C46 C47 176.5(5) . . . . ?
C45 C46 C47 C48 0.8(8) . . . . ?
C45 C46 C47 C52 179.9(5) . . . . ?
C52 C47 C48 C49 0.2(7) . . . . ?
C46 C47 C48 C49 179.3(5) . . . . ?
C47 C48 C49 C50 -0.2(8) . . . . ?
C48 C49 C50 C51 0.4(8) . . . . ?
C49 C50 C51 C52 -0.6(8) . . . . ?
C50 C51 C52 C47 0.5(8) . . . . ?
C48 C47 C52 C51 -0.4(7) . . . . ?
C46 C47 C52 C51 -179.5(5) . . . . ?
O3 C2 N1 C9 0.4(5) . . . . ?
C10 C2 N1 C9 -179.3(4) . . . . ?
O3 C2 N1 Rh1 179.5(3) . . . . ?
C10 C2 N1 Rh1 -0.2(6) . . . . ?
C4 C9 N1 C2 0.3(5) . . . . ?
C8 C9 N1 C2 180.0(5) . . . . ?
C4 C9 N1 Rh1 -178.3(4) . . . . ?
C8 C9 N1 Rh1 1.3(9) . . . . ?
O22 C21 N20 C28 0.8(6) . . . . ?
C29 C21 N20 C28 178.3(5) . . . . ?
O22 C21 N20 Rh1 -177.7(3) . . . . ?
C29 C21 N20 Rh1 -0.2(7) . . . . ?
C23 C28 N20 C21 -0.9(6) . . . . ?
C27 C28 N20 C21 -179.2(6) . . . . ?
C23 C28 N20 Rh1 176.9(5) . . . . ?
C27 C28 N20 Rh1 -1.3(11) . . . . ?
N41 C40 N39 C43 0.8(6) . . . . ?
C44 C40 N39 C43 -177.9(4) . . . . ?
N41 C40 N39 Rh1 179.1(3) . . . . ?
C44 C40 N39 Rh1 0.4(6) . . . . ?
C42 C43 N39 C40 -0.8(6) . . . . ?
C42 C43 N39 Rh1 -178.7(4) . . . . ?
C43 C42 N41 C40 -0.1(6) . . . . ?
C43 C42 N41 C53 171.9(5) . . . . ?
N39 C40 N41 C42 -0.4(6) . . . . ?
C44 C40 N41 C42 178.0(5) . . . . ?
N39 C40 N41 C53 -171.8(5) . . . . ?
C44 C40 N41 C53 6.6(9) . . . . ?
C55 C53 N41 C42 -93.8(7) . . . . ?
C54 C53 N41 C42 29.9(7) . . . . ?
C55 C53 N41 C40 76.2(7) . . . . ?
C54 C53 N41 C40 -160.0(5) . . . . ?
C45 C44 O2 Rh1 -175.3(3) . . . . ?
C40 C44 O2 Rh1 2.3(5) . . . . ?
N1 C2 O3 C4 -0.9(5) . . . . ?
C10 C2 O3 C4 178.7(5) . . . . ?
C5 C4 O3 C2 -179.0(5) . . . . ?
C9 C4 O3 C2 1.1(5) . . . . ?
N20 C21 O22 C23 -0.3(6) . . . . ?
C29 C21 O22 C23 -177.6(5) . . . . ?
C24 C23 O22 C21 179.7(6) . . . . ?
C28 C23 O22 C21 -0.4(6) . . . . ?
Cl2 C100 Cl1 C101 81(3) . . . . ?
C100 Cl1 C101 Cl2A 137(4) . . . . ?
Cl4 C102 Cl3 C103 -74(5) . . . . ?
Cl5 C103 Cl3 C102 -9(3) . . . . ?

_refine_diff_density_max         1.123
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.070

_shelxl_version_number           2014-3




_database_code_depnum_ccdc_archive 'CCDC 1028075'
#######################################################################
#
#                 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_c75_0m

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H43 Ir N4 O3, C H2 Cl2'
_chemical_formula_sum            'C47 H45 Cl2 Ir N4 O3'
_chemical_formula_weight         976.97

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'
Ir Ir -1.4442 7.9887 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   38.9286(14)
_cell_length_b                   13.3583(5)
_cell_length_c                   17.0015(7)
_cell_angle_alpha                90
_cell_angle_beta                 111.4793(12)
_cell_angle_gamma                90
_cell_volume                     8227.1(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    9838
_cell_measurement_theta_min      2.2883
_cell_measurement_theta_max      25.2832

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_F_000             3920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.423
_shelx_estimated_absorpt_T_min   0.665
_shelx_estimated_absorpt_T_max   0.935
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      105(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            86572
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.197
_diffrn_reflns_theta_max         25.304
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7482
_reflns_number_gt                6105
_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       'BRUKER APEX2 2014.1-1'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  ?

_refine_special_details          
; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0237P)²+38.6963P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7482
_refine_ls_number_parameters     568
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0636
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.003
_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
C2 C 0.46804(12) 0.4476(3) 0.5670(3) 0.0247(10) Uani 1 1 d . . . . .
C4 C 0.47271(12) 0.6093(3) 0.5708(3) 0.0285(10) Uani 1 1 d . . . . .
C5 C 0.48502(13) 0.7066(4) 0.5853(3) 0.0387(13) Uani 1 1 d . . . . .
H5 H 0.5100 0.7227 0.6176 0.046 Uiso 1 1 calc R U . . .
C6 C 0.45860(13) 0.7792(3) 0.5498(3) 0.0333(11) Uani 1 1 d . . . . .
H6 H 0.4659 0.8475 0.5579 0.040 Uiso 1 1 calc R U . . .
C7 C 0.42165(11) 0.7573(3) 0.5023(3) 0.0212(9) Uani 1 1 d . . . . .
C8 C 0.41018(11) 0.6577(3) 0.4891(2) 0.0178(9) Uani 1 1 d . . . . .
H8 H 0.3853 0.6407 0.4569 0.021 Uiso 1 1 calc R U . . .
C9 C 0.43648(11) 0.5845(3) 0.5247(3) 0.0185(9) Uani 1 1 d . . . . .
C10 C 0.47557(12) 0.3420(3) 0.5755(3) 0.0259(10) Uani 1 1 d . . . . .
C11 C 0.44327(12) 0.2867(3) 0.5309(3) 0.0222(10) Uani 1 1 d . . . . .
C12 C 0.44818(13) 0.1821(3) 0.5334(3) 0.0315(11) Uani 1 1 d . . . . .
H12 H 0.4278 0.1403 0.5041 0.038 Uiso 1 1 calc R U . . .
C13 C 0.48207(14) 0.1391(4) 0.5777(3) 0.0430(13) Uani 1 1 d . . . . .
H13 H 0.4844 0.0683 0.5778 0.052 Uiso 1 1 calc R U . . .
C14 C 0.51272(14) 0.1963(4) 0.6217(4) 0.0465(14) Uani 1 1 d . . . . .
H14 H 0.5357 0.1651 0.6524 0.056 Uiso 1 1 calc R U . . .
C15 C 0.50956(13) 0.2989(4) 0.6206(3) 0.0394(13) Uani 1 1 d . . . . .
H15 H 0.5303 0.3396 0.6502 0.047 Uiso 1 1 calc R U . . .
C16 C 0.39343(12) 0.8419(3) 0.4682(3) 0.0250(10) Uani 1 1 d D U . . .
C17 C 0.36770(15) 0.8434(4) 0.5209(4) 0.0292(15) Uani 0.812(6) 1 d D U P A 1
H17A H 0.3483 0.8937 0.4975 0.044 Uiso 0.812(6) 1 calc R U P A 1
H17B H 0.3823 0.8601 0.5799 0.044 Uiso 0.812(6) 1 calc R U P A 1
H17C H 0.3564 0.7773 0.5184 0.044 Uiso 0.812(6) 1 calc R U P A 1
C18 C 0.36854(17) 0.8188(4) 0.3766(4) 0.0306(15) Uani 0.812(6) 1 d D U P A 1
H18A H 0.3508 0.8735 0.3546 0.046 Uiso 0.812(6) 1 calc R U P A 1
H18B H 0.3552 0.7561 0.3749 0.046 Uiso 0.812(6) 1 calc R U P A 1
H18C H 0.3837 0.8121 0.3419 0.046 Uiso 0.812(6) 1 calc R U P A 1
C19 C 0.41039(16) 0.9422(4) 0.4728(4) 0.0300(15) Uani 0.812(6) 1 d D U P A 1
H19A H 0.3909 0.9924 0.4494 0.045 Uiso 0.812(6) 1 calc R U P A 1
H19B H 0.4265 0.9420 0.4401 0.045 Uiso 0.812(6) 1 calc R U P A 1
H19C H 0.4249 0.9585 0.5319 0.045 Uiso 0.812(6) 1 calc R U P A 1
C17A C 0.3963(6) 0.9182(16) 0.5375(12) 0.031(5) Uani 0.188(6) 1 d D U P A 2
H17D H 0.3838 0.9803 0.5116 0.046 Uiso 0.188(6) 1 calc R U P A 2
H17E H 0.4224 0.9323 0.5702 0.046 Uiso 0.188(6) 1 calc R U P A 2
H17F H 0.3846 0.8910 0.5750 0.046 Uiso 0.188(6) 1 calc R U P A 2
C18A C 0.4063(6) 0.9084(17) 0.4030(14) 0.033(5) Uani 0.188(6) 1 d D U P A 2
H18D H 0.3902 0.9669 0.3843 0.049 Uiso 0.188(6) 1 calc R U P A 2
H18E H 0.4047 0.8676 0.3539 0.049 Uiso 0.188(6) 1 calc R U P A 2
H18F H 0.4319 0.9307 0.4319 0.049 Uiso 0.188(6) 1 calc R U P A 2
C19A C 0.3556(5) 0.8123(17) 0.4152(17) 0.035(6) Uani 0.188(6) 1 d D U P A 2
H19D H 0.3415 0.8719 0.3884 0.052 Uiso 0.188(6) 1 calc R U P A 2
H19E H 0.3438 0.7800 0.4504 0.052 Uiso 0.188(6) 1 calc R U P A 2
H19F H 0.3564 0.7655 0.3715 0.052 Uiso 0.188(6) 1 calc R U P A 2
C21 C 0.36097(11) 0.2234(3) 0.3547(3) 0.0203(9) Uani 1 1 d . . . . .
C23 C 0.32388(11) 0.1206(3) 0.3833(2) 0.0200(9) Uani 1 1 d . . . . .
C24 C 0.29903(11) 0.0474(3) 0.3813(3) 0.0234(10) Uani 1 1 d . . . . .
H24 H 0.2892 0.0030 0.3347 0.028 Uiso 1 1 calc R U . . .
C25 C 0.28898(11) 0.0419(3) 0.4515(3) 0.0236(10) Uani 1 1 d . . . . .
H25 H 0.2715 -0.0074 0.4523 0.028 Uiso 1 1 calc R U . . .
C26 C 0.30344(11) 0.1061(3) 0.5215(3) 0.0219(9) Uani 1 1 d . . . . .
C27 C 0.32909(11) 0.1787(3) 0.5214(2) 0.0186(9) Uani 1 1 d . . . . .
H27 H 0.3397 0.2223 0.5682 0.022 Uiso 1 1 calc R U . . .
C28 C 0.33867(10) 0.1852(3) 0.4508(2) 0.0164(9) Uani 1 1 d . . . . .
C29 C 0.38158(11) 0.2781(3) 0.3142(3) 0.0207(9) Uani 1 1 d . . . . .
C30 C 0.40135(11) 0.3573(3) 0.3663(3) 0.0204(9) Uani 1 1 d . . . . .
C31 C 0.42212(11) 0.4166(3) 0.3319(3) 0.0217(9) Uani 1 1 d . . . . .
H31 H 0.4360 0.4712 0.3637 0.026 Uiso 1 1 calc R U . . .
C32 C 0.42285(11) 0.3973(3) 0.2525(3) 0.0256(10) Uani 1 1 d . . . . .
H32 H 0.4372 0.4391 0.2312 0.031 Uiso 1 1 calc R U . . .
C33 C 0.40313(12) 0.3183(3) 0.2031(3) 0.0289(11) Uani 1 1 d . . . . .
H33 H 0.4043 0.3057 0.1492 0.035 Uiso 1 1 calc R U . . .
C34 C 0.38185(12) 0.2584(3) 0.2336(3) 0.0265(10) Uani 1 1 d . . . . .
H34 H 0.3677 0.2050 0.2005 0.032 Uiso 1 1 calc R U . . .
C35 C 0.29022(12) 0.0942(3) 0.5958(3) 0.0272(10) Uani 1 1 d . . . . .
C36 C 0.24838(12) 0.1159(4) 0.5648(3) 0.0356(12) Uani 1 1 d . . . . .
H36A H 0.2394 0.1023 0.6105 0.053 Uiso 1 1 calc R U . . .
H36B H 0.2354 0.0730 0.5163 0.053 Uiso 1 1 calc R U . . .
H36C H 0.2439 0.1863 0.5479 0.053 Uiso 1 1 calc R U . . .
C37 C 0.29770(13) -0.0135(4) 0.6300(3) 0.0371(12) Uani 1 1 d . . . . .
H37A H 0.2893 -0.0212 0.6773 0.056 Uiso 1 1 calc R U . . .
H37B H 0.3242 -0.0273 0.6494 0.056 Uiso 1 1 calc R U . . .
H37C H 0.2844 -0.0607 0.5850 0.056 Uiso 1 1 calc R U . . .
C38 C 0.30972(13) 0.1661(4) 0.6673(3) 0.0366(12) Uani 1 1 d . . . . .
H38A H 0.3010 0.1553 0.7138 0.055 Uiso 1 1 calc R U . . .
H38B H 0.3044 0.2351 0.6469 0.055 Uiso 1 1 calc R U . . .
H38C H 0.3364 0.1544 0.6874 0.055 Uiso 1 1 calc R U . . .
C40 C 0.39982(12) 0.3354(3) 0.6727(3) 0.0259(10) Uani 1 1 d . . . . .
H40 H 0.4188 0.2865 0.6918 0.031 Uiso 1 1 calc R U . . .
C41 C 0.38091(13) 0.3736(3) 0.7179(3) 0.0301(11) Uani 1 1 d . . . . .
H41 H 0.3840 0.3564 0.7743 0.036 Uiso 1 1 calc R U . . .
C43 C 0.36086(11) 0.4449(3) 0.5918(3) 0.0206(9) Uani 1 1 d . . . . .
C44 C 0.34182(11) 0.5010(3) 0.5124(3) 0.0200(9) Uani 1 1 d . . . . .
C45 C 0.31914(11) 0.5799(3) 0.5084(3) 0.0234(10) Uani 1 1 d . . . . .
H45 H 0.3176 0.6010 0.5603 0.028 Uiso 1 1 calc R U . . .
C46 C 0.29709(11) 0.6352(3) 0.4334(3) 0.0240(9) Uani 1 1 d . . . . .
C47 C 0.29270(11) 0.6073(3) 0.3509(3) 0.0239(10) Uani 1 1 d . . . . .
H47 H 0.3053 0.5501 0.3419 0.029 Uiso 1 1 calc R U . . .
C48 C 0.27026(12) 0.6623(3) 0.2824(3) 0.0293(11) Uani 1 1 d . . . . .
H48 H 0.2678 0.6421 0.2270 0.035 Uiso 1 1 calc R U . . .
C49 C 0.25135(13) 0.7459(3) 0.2924(3) 0.0336(11) Uani 1 1 d . . . . .
H49 H 0.2358 0.7824 0.2447 0.040 Uiso 1 1 calc R U . . .
C50 C 0.25556(12) 0.7750(3) 0.3732(3) 0.0347(12) Uani 1 1 d . . . . .
H50 H 0.2428 0.8324 0.3813 0.042 Uiso 1 1 calc R U . . .
C51 C 0.27823(12) 0.7214(3) 0.4430(3) 0.0299(11) Uani 1 1 d . . . . .
H51 H 0.2810 0.7434 0.4981 0.036 Uiso 1 1 calc R U . . .
C52 C 0.33088(13) 0.5002(4) 0.6956(3) 0.0349(12) Uani 1 1 d . . . . .
H52A H 0.3055 0.4896 0.6563 0.052 Uiso 1 1 calc R U . . .
H52B H 0.3370 0.5715 0.6970 0.052 Uiso 1 1 calc R U . . .
H52C H 0.3331 0.4784 0.7523 0.052 Uiso 1 1 calc R U . . .
C53 C 0.4444(2) 0.0229(8) 0.2342(6) 0.148(4) Uani 1 1 d D U . . .
H53A H 0.4420 0.0764 0.1923 0.177 Uiso 0.8 1 calc R U P B 1
H53B H 0.4653 -0.0201 0.2354 0.177 Uiso 0.8 1 calc R U P B 1
H53C H 0.4589 -0.0389 0.2550 0.177 Uiso 0.2 1 calc R U P C 2
H53D H 0.4352 0.0176 0.1718 0.177 Uiso 0.2 1 calc R U P C 2
N1 N 0.43448(9) 0.4796(2) 0.5243(2) 0.0188(8) Uani 1 1 d . . . . .
N20 N 0.36279(9) 0.2497(2) 0.4307(2) 0.0178(7) Uani 1 1 d . . . . .
N39 N 0.38699(9) 0.3795(2) 0.5941(2) 0.0211(8) Uani 1 1 d . . . . .
N42 N 0.35626(10) 0.4423(3) 0.6677(2) 0.0250(8) Uani 1 1 d . . . . .
O2 O 0.34989(7) 0.4666(2) 0.44858(17) 0.0187(6) Uani 1 1 d . . . . .
O3 O 0.49296(8) 0.5214(2) 0.5982(2) 0.0338(8) Uani 1 1 d . . . . .
O22 O 0.33821(8) 0.1445(2) 0.32177(17) 0.0222(6) Uani 1 1 d . . . . .
Ir1 Ir 0.39698(2) 0.36764(2) 0.48084(2) 0.01662(5) Uani 1 1 d . . . . .
Cl1 Cl 0.45608(6) 0.07809(15) 0.33096(16) 0.0732(8) Uani 0.754(3) 1 d D U P D 1
Cl2 Cl 0.40650(6) -0.04579(18) 0.19909(17) 0.0677(8) Uani 0.689(3) 1 d D U P D
1
Cl3 Cl 0.4737(2) 0.1010(6) 0.2520(5) 0.159(3) Uani 0.428(3) 1 d D U P D 2
Cl4 Cl 0.4066(3) 0.0012(10) 0.2549(9) 0.0677(8) Uani 0.128(2) 1 d D U P D 2


_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
C2 N1 1.312(5) . ?
C2 O3 1.348(5) . ?
C2 C10 1.437(6) . ?
C4 C5 1.375(6) . ?
C4 C9 1.380(6) . ?
C4 O3 1.396(5) . ?
C5 C6 1.382(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.399(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.395(6) . ?
C7 C16 1.535(6) . ?
C8 C9 1.384(6) . ?
C8 H8 0.9500 . ?
C9 N1 1.404(5) . ?
C10 C15 1.388(6) . ?
C10 C11 1.416(6) . ?
C11 C12 1.408(6) . ?
C11 Ir1 2.004(4) . ?
C12 C13 1.382(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C19A 1.471(15) . ?
C16 C19 1.483(6) . ?
C16 C17A 1.531(15) . ?
C16 C18 1.534(7) . ?
C16 C17 1.570(7) . ?
C16 C18A 1.636(16) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C21 N20 1.314(5) . ?
C21 O22 1.359(5) . ?
C21 C29 1.434(6) . ?
C23 C24 1.367(6) . ?
C23 C28 1.381(5) . ?
C23 O22 1.392(5) . ?
C24 C25 1.387(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.405(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.393(6) . ?
C26 C35 1.538(6) . ?
C27 C28 1.384(5) . ?
C27 H27 0.9500 . ?
C28 N20 1.406(5) . ?
C29 C34 1.400(6) . ?
C29 C30 1.413(6) . ?
C30 C31 1.404(6) . ?
C30 Ir1 2.021(4) . ?
C31 C32 1.384(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.391(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C38 1.517(6) . ?
C35 C37 1.539(6) . ?
C35 C36 1.545(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C40 C41 1.344(6) . ?
C40 N39 1.376(5) . ?
C40 H40 0.9500 . ?
C41 N42 1.375(6) . ?
C41 H41 0.9500 . ?
C43 N39 1.331(5) . ?
C43 N42 1.366(5) . ?
C43 C44 1.485(6) . ?
C44 O2 1.318(5) . ?
C44 C45 1.360(6) . ?
C45 C46 1.452(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.400(6) . ?
C46 C51 1.406(6) . ?
C47 C48 1.384(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.381(6) . ?
C48 H48 0.9500 . ?
C49 C50 1.380(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.390(6) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 N42 1.464(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 Cl3 1.494(8) . ?
C53 Cl2 1.651(7) . ?
C53 Cl4 1.656(12) . ?
C53 Cl1 1.705(9) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 H53C 0.9900 . ?
C53 H53D 0.9900 . ?
N1 Ir1 2.031(3) . ?
N20 Ir1 2.037(3) . ?
N39 Ir1 2.105(3) . ?
O2 Ir1 2.161(3) . ?
Cl3 Cl3 2.072(15) 2_655 ?

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 C2 O3 114.0(4) . . ?
N1 C2 C10 120.0(4) . . ?
O3 C2 C10 126.0(4) . . ?
C5 C4 C9 123.0(4) . . ?
C5 C4 O3 128.2(4) . . ?
C9 C4 O3 108.8(4) . . ?
C4 C5 C6 115.5(4) . . ?
C4 C5 H5 122.3 . . ?
C6 C5 H5 122.3 . . ?
C5 C6 C7 123.2(4) . . ?
C5 C6 H6 118.4 . . ?
C7 C6 H6 118.4 . . ?
C8 C7 C6 119.6(4) . . ?
C8 C7 C16 119.9(4) . . ?
C6 C7 C16 120.4(4) . . ?
C9 C8 C7 117.5(4) . . ?
C9 C8 H8 121.3 . . ?
C7 C8 H8 121.3 . . ?
C4 C9 C8 121.2(4) . . ?
C4 C9 N1 106.6(4) . . ?
C8 C9 N1 132.2(4) . . ?
C15 C10 C11 124.0(4) . . ?
C15 C10 C2 125.5(4) . . ?
C11 C10 C2 110.5(4) . . ?
C12 C11 C10 114.7(4) . . ?
C12 C11 Ir1 129.7(3) . . ?
C10 C11 Ir1 115.5(3) . . ?
C13 C12 C11 121.4(4) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 121.8(5) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 119.2(5) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C10 118.9(5) . . ?
C14 C15 H15 120.6 . . ?
C10 C15 H15 120.6 . . ?
C19A C16 C17A 115.1(13) . . ?
C19 C16 C18 109.8(4) . . ?
C19A C16 C7 116.8(10) . . ?
C19 C16 C7 113.7(4) . . ?
C17A C16 C7 111.0(9) . . ?
C18 C16 C7 109.6(4) . . ?
C19 C16 C17 108.8(4) . . ?
C18 C16 C17 106.5(4) . . ?
C7 C16 C17 108.1(4) . . ?
C19A C16 C18A 102.6(13) . . ?
C17A C16 C18A 101.8(12) . . ?
C7 C16 C18A 107.5(8) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C17A H17D 109.5 . . ?
C16 C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
C16 C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
C16 C18A H18D 109.5 . . ?
C16 C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
C16 C18A H18F 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C16 C19A H19D 109.5 . . ?
C16 C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C16 C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
N20 C21 O22 113.9(4) . . ?
N20 C21 C29 119.8(4) . . ?
O22 C21 C29 126.3(4) . . ?
C24 C23 C28 122.9(4) . . ?
C24 C23 O22 128.4(4) . . ?
C28 C23 O22 108.7(3) . . ?
C23 C24 C25 115.8(4) . . ?
C23 C24 H24 122.1 . . ?
C25 C24 H24 122.1 . . ?
C24 C25 C26 123.0(4) . . ?
C24 C25 H25 118.5 . . ?
C26 C25 H25 118.5 . . ?
C27 C26 C25 119.3(4) . . ?
C27 C26 C35 121.9(4) . . ?
C25 C26 C35 118.8(4) . . ?
C28 C27 C26 117.7(4) . . ?
C28 C27 H27 121.1 . . ?
C26 C27 H27 121.1 . . ?
C23 C28 C27 121.2(4) . . ?
C23 C28 N20 107.1(3) . . ?
C27 C28 N20 131.7(4) . . ?
C34 C29 C30 123.8(4) . . ?
C34 C29 C21 125.5(4) . . ?
C30 C29 C21 110.6(4) . . ?
C31 C30 C29 115.2(4) . . ?
C31 C30 Ir1 128.9(3) . . ?
C29 C30 Ir1 115.9(3) . . ?
C32 C31 C30 121.5(4) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C31 C32 C33 121.7(4) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C34 C33 C32 119.2(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C29 118.6(4) . . ?
C33 C34 H34 120.7 . . ?
C29 C34 H34 120.7 . . ?
C38 C35 C26 111.9(4) . . ?
C38 C35 C37 108.7(4) . . ?
C26 C35 C37 109.4(4) . . ?
C38 C35 C36 108.1(4) . . ?
C26 C35 C36 109.2(4) . . ?
C37 C35 C36 109.6(4) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41 C40 N39 108.2(4) . . ?
C41 C40 H40 125.9 . . ?
N39 C40 H40 125.9 . . ?
C40 C41 N42 107.6(4) . . ?
C40 C41 H41 126.2 . . ?
N42 C41 H41 126.2 . . ?
N39 C43 N42 108.6(4) . . ?
N39 C43 C44 118.7(4) . . ?
N42 C43 C44 132.7(4) . . ?
O2 C44 C45 125.2(4) . . ?
O2 C44 C43 112.5(4) . . ?
C45 C44 C43 122.3(4) . . ?
C44 C45 C46 127.0(4) . . ?
C44 C45 H45 116.5 . . ?
C46 C45 H45 116.5 . . ?
C47 C46 C51 117.1(4) . . ?
C47 C46 C45 124.1(4) . . ?
C51 C46 C45 118.8(4) . . ?
C48 C47 C46 120.7(4) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C49 C48 C47 121.8(4) . . ?
C49 C48 H48 119.1 . . ?
C47 C48 H48 119.1 . . ?
C50 C49 C48 118.4(5) . . ?
C50 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
C49 C50 C51 120.8(4) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 H50 119.6 . . ?
C50 C51 C46 121.3(4) . . ?
C50 C51 H51 119.4 . . ?
C46 C51 H51 119.4 . . ?
N42 C52 H52A 109.5 . . ?
N42 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N42 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
Cl3 C53 Cl4 138.7(10) . . ?
Cl2 C53 Cl1 118.5(6) . . ?
Cl2 C53 H53A 107.7 . . ?
Cl1 C53 H53A 107.7 . . ?
Cl2 C53 H53B 107.7 . . ?
Cl1 C53 H53B 107.7 . . ?
H53A C53 H53B 107.1 . . ?
Cl3 C53 H53C 102.4 . . ?
Cl4 C53 H53C 102.4 . . ?
Cl3 C53 H53D 102.4 . . ?
Cl4 C53 H53D 102.4 . . ?
H53C C53 H53D 104.9 . . ?
C2 N1 C9 106.3(3) . . ?
C2 N1 Ir1 113.5(3) . . ?
C9 N1 Ir1 140.2(3) . . ?
C21 N20 C28 105.9(3) . . ?
C21 N20 Ir1 114.2(3) . . ?
C28 N20 Ir1 139.8(3) . . ?
C43 N39 C40 108.1(3) . . ?
C43 N39 Ir1 114.7(3) . . ?
C40 N39 Ir1 137.2(3) . . ?
C43 N42 C41 107.5(4) . . ?
C43 N42 C52 129.1(4) . . ?
C41 N42 C52 123.5(4) . . ?
C44 O2 Ir1 116.1(2) . . ?
C2 O3 C4 104.3(3) . . ?
C21 O22 C23 104.4(3) . . ?
C11 Ir1 C30 89.56(16) . . ?
C11 Ir1 N1 80.09(15) . . ?
C30 Ir1 N1 95.62(15) . . ?
C11 Ir1 N20 96.24(16) . . ?
C30 Ir1 N20 79.40(15) . . ?
N1 Ir1 N20 173.90(13) . . ?
C11 Ir1 N39 95.20(15) . . ?
C30 Ir1 N39 174.58(14) . . ?
N1 Ir1 N39 87.77(13) . . ?
N20 Ir1 N39 97.47(13) . . ?
C11 Ir1 O2 169.97(14) . . ?
C30 Ir1 O2 99.21(13) . . ?
N1 Ir1 O2 94.13(12) . . ?
N20 Ir1 O2 90.18(12) . . ?
N39 Ir1 O2 76.27(11) . . ?
C53 Cl3 Cl3 133.2(6) . 2_655 ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 C6 -0.7(8) . . . . ?
O3 C4 C5 C6 179.7(5) . . . . ?
C4 C5 C6 C7 0.3(8) . . . . ?
C5 C6 C7 C8 -0.2(7) . . . . ?
C5 C6 C7 C16 177.2(5) . . . . ?
C6 C7 C8 C9 0.3(6) . . . . ?
C16 C7 C8 C9 -177.0(4) . . . . ?
C5 C4 C9 C8 0.8(7) . . . . ?
O3 C4 C9 C8 -179.5(4) . . . . ?
C5 C4 C9 N1 -179.4(5) . . . . ?
O3 C4 C9 N1 0.3(5) . . . . ?
C7 C8 C9 C4 -0.6(6) . . . . ?
C7 C8 C9 N1 179.7(4) . . . . ?
N1 C2 C10 C15 -178.4(5) . . . . ?
O3 C2 C10 C15 3.0(8) . . . . ?
N1 C2 C10 C11 1.9(6) . . . . ?
O3 C2 C10 C11 -176.7(4) . . . . ?
C15 C10 C11 C12 -1.6(7) . . . . ?
C2 C10 C11 C12 178.2(4) . . . . ?
C15 C10 C11 Ir1 174.3(4) . . . . ?
C2 C10 C11 Ir1 -6.0(5) . . . . ?
C10 C11 C12 C13 1.0(7) . . . . ?
Ir1 C11 C12 C13 -174.2(4) . . . . ?
C11 C12 C13 C14 0.3(8) . . . . ?
C12 C13 C14 C15 -0.9(9) . . . . ?
C13 C14 C15 C10 0.3(9) . . . . ?
C11 C10 C15 C14 1.0(8) . . . . ?
C2 C10 C15 C14 -178.8(5) . . . . ?
C8 C7 C16 C19A -5.8(14) . . . . ?
C6 C7 C16 C19A 176.9(14) . . . . ?
C8 C7 C16 C19 -169.2(4) . . . . ?
C6 C7 C16 C19 13.5(6) . . . . ?
C8 C7 C16 C17A 129.0(10) . . . . ?
C6 C7 C16 C17A -48.3(11) . . . . ?
C8 C7 C16 C18 -45.9(6) . . . . ?
C6 C7 C16 C18 136.8(5) . . . . ?
C8 C7 C16 C17 69.8(5) . . . . ?
C6 C7 C16 C17 -107.5(5) . . . . ?
C8 C7 C16 C18A -120.4(10) . . . . ?
C6 C7 C16 C18A 62.3(11) . . . . ?
C28 C23 C24 C25 0.6(6) . . . . ?
O22 C23 C24 C25 -178.6(4) . . . . ?
C23 C24 C25 C26 -0.8(6) . . . . ?
C24 C25 C26 C27 -0.1(6) . . . . ?
C24 C25 C26 C35 179.5(4) . . . . ?
C25 C26 C27 C28 1.1(6) . . . . ?
C35 C26 C27 C28 -178.5(4) . . . . ?
C24 C23 C28 C27 0.4(6) . . . . ?
O22 C23 C28 C27 179.8(3) . . . . ?
C24 C23 C28 N20 -179.8(4) . . . . ?
O22 C23 C28 N20 -0.4(4) . . . . ?
C26 C27 C28 C23 -1.2(6) . . . . ?
C26 C27 C28 N20 179.0(4) . . . . ?
N20 C21 C29 C34 -179.5(4) . . . . ?
O22 C21 C29 C34 -0.5(7) . . . . ?
N20 C21 C29 C30 -0.8(5) . . . . ?
O22 C21 C29 C30 178.2(4) . . . . ?
C34 C29 C30 C31 -0.4(6) . . . . ?
C21 C29 C30 C31 -179.1(3) . . . . ?
C34 C29 C30 Ir1 -178.9(3) . . . . ?
C21 C29 C30 Ir1 2.4(4) . . . . ?
C29 C30 C31 C32 -0.2(6) . . . . ?
Ir1 C30 C31 C32 178.1(3) . . . . ?
C30 C31 C32 C33 -0.1(6) . . . . ?
C31 C32 C33 C34 0.9(7) . . . . ?
C32 C33 C34 C29 -1.5(6) . . . . ?
C30 C29 C34 C33 1.3(6) . . . . ?
C21 C29 C34 C33 179.8(4) . . . . ?
C27 C26 C35 C38 -2.8(6) . . . . ?
C25 C26 C35 C38 177.6(4) . . . . ?
C27 C26 C35 C37 -123.3(4) . . . . ?
C25 C26 C35 C37 57.1(5) . . . . ?
C27 C26 C35 C36 116.8(4) . . . . ?
C25 C26 C35 C36 -62.8(5) . . . . ?
N39 C40 C41 N42 -0.3(5) . . . . ?
N39 C43 C44 O2 9.7(5) . . . . ?
N42 C43 C44 O2 -167.1(4) . . . . ?
N39 C43 C44 C45 -169.4(4) . . . . ?
N42 C43 C44 C45 13.8(7) . . . . ?
O2 C44 C45 C46 5.9(7) . . . . ?
C43 C44 C45 C46 -175.1(4) . . . . ?
C44 C45 C46 C47 7.8(7) . . . . ?
C44 C45 C46 C51 -173.4(4) . . . . ?
C51 C46 C47 C48 -0.9(6) . . . . ?
C45 C46 C47 C48 178.0(4) . . . . ?
C46 C47 C48 C49 -0.2(7) . . . . ?
C47 C48 C49 C50 0.8(7) . . . . ?
C48 C49 C50 C51 -0.2(7) . . . . ?
C49 C50 C51 C46 -1.0(7) . . . . ?
C47 C46 C51 C50 1.5(6) . . . . ?
C45 C46 C51 C50 -177.4(4) . . . . ?
O3 C2 N1 C9 1.1(5) . . . . ?
C10 C2 N1 C9 -177.7(4) . . . . ?
O3 C2 N1 Ir1 -178.2(3) . . . . ?
C10 C2 N1 Ir1 3.0(5) . . . . ?
C4 C9 N1 C2 -0.8(5) . . . . ?
C8 C9 N1 C2 178.9(4) . . . . ?
C4 C9 N1 Ir1 178.2(3) . . . . ?
C8 C9 N1 Ir1 -2.1(8) . . . . ?
O22 C21 N20 C28 -1.4(5) . . . . ?
C29 C21 N20 C28 177.6(3) . . . . ?
O22 C21 N20 Ir1 179.8(2) . . . . ?
C29 C21 N20 Ir1 -1.1(5) . . . . ?
C23 C28 N20 C21 1.1(4) . . . . ?
C27 C28 N20 C21 -179.1(4) . . . . ?
C23 C28 N20 Ir1 179.4(3) . . . . ?
C27 C28 N20 Ir1 -0.9(7) . . . . ?
N42 C43 N39 C40 -1.0(4) . . . . ?
C44 C43 N39 C40 -178.5(3) . . . . ?
N42 C43 N39 Ir1 177.7(2) . . . . ?
C44 C43 N39 Ir1 0.2(4) . . . . ?
C41 C40 N39 C43 0.8(5) . . . . ?
C41 C40 N39 Ir1 -177.5(3) . . . . ?
N39 C43 N42 C41 0.8(4) . . . . ?
C44 C43 N42 C41 177.9(4) . . . . ?
N39 C43 N42 C52 -180.0(4) . . . . ?
C44 C43 N42 C52 -2.9(7) . . . . ?
C40 C41 N42 C43 -0.3(5) . . . . ?
C40 C41 N42 C52 -179.6(4) . . . . ?
C45 C44 O2 Ir1 164.5(3) . . . . ?
C43 C44 O2 Ir1 -14.6(4) . . . . ?
N1 C2 O3 C4 -0.9(5) . . . . ?
C10 C2 O3 C4 177.8(4) . . . . ?
C5 C4 O3 C2 180.0(5) . . . . ?
C9 C4 O3 C2 0.3(5) . . . . ?
N20 C21 O22 C23 1.2(4) . . . . ?
C29 C21 O22 C23 -177.8(4) . . . . ?
C24 C23 O22 C21 179.0(4) . . . . ?
C28 C23 O22 C21 -0.4(4) . . . . ?
Cl2 C53 Cl3 Cl3 -121(4) . . . 2_655 ?
Cl4 C53 Cl3 Cl3 161.3(11) . . . 2_655 ?
Cl1 C53 Cl3 Cl3 126.4(9) . . . 2_655 ?

_refine_diff_density_max         0.849
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.104

_shelxl_version_number           2014-3

_database_code_depnum_ccdc_archive 'CCDC 1014508'
