# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4BF4
_database_code_depnum_ccdc_archive 'CCDC 1556215'
_audit_update_record             
;
2017-06-15 deposited with the CCDC.
2017-07-07 downloaded from the CCDC.
;

_audit_creation_date             2016-04-12T17:38:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C35 H35 B1 Cl F4 N3 P Rh'
_chemical_formula_moiety         'C35 H35 Cl N3 P Rh, B F4'
_chemical_formula_weight         753.80
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2988(2)
_cell_length_b                   13.2821(3)
_cell_length_c                   14.5983(3)
_cell_angle_alpha                81.8530(10)
_cell_angle_beta                 73.4020(10)
_cell_angle_gamma                72.6490(10)
_cell_volume                     1646.10(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.44
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_crystal_description       cube
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.7147
_exptl_absorpt_correction_T_max  0.7465


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_number            96636
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.446
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             6735
_reflns_number_gt                6237
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

__atom_sites_solution_primary    direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0191P)²+1.2191P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6735
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0189
_refine_ls_wR_factor_ref         0.0487
_refine_ls_wR_factor_gt          0.0469
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.056

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.75171(17) 0.35419(11) 0.89525(10) 0.0121(3) Uani 1 1 d . . . . .
H1 H 0.68 0.3389 0.8678 0.014 Uiso 1 1 calc R U . . .
C2 C 0.85666(18) 0.39303(13) 0.99904(11) 0.0161(3) Uani 1 1 d . . . . .
H2 H 0.8698 0.4097 1.0568 0.019 Uiso 1 1 calc R U . . .
C3 C 0.96419(18) 0.37985(12) 0.91411(11) 0.0151(3) Uani 1 1 d . . . . .
H3 H 1.0676 0.3858 0.9008 0.018 Uiso 1 1 calc R U . . .
C4 C 0.97515(17) 0.33167(11) 0.74843(10) 0.0108(3) Uani 1 1 d . . . . .
H4 H 1.0511 0.3751 0.7242 0.013 Uiso 1 1 calc R U . . .
C5 C 0.57940(17) 0.37760(12) 1.05642(11) 0.0133(3) Uani 1 1 d . . . . .
C6 C 0.56359(19) 0.39219(13) 1.15091(11) 0.0181(3) Uani 1 1 d . . . . .
H6 H 0.6458 0.4032 1.1712 0.022 Uiso 1 1 calc R U . . .
C7 C 0.4217(2) 0.38998(14) 1.21467(12) 0.0223(4) Uani 1 1 d . . . . .
H7 H 0.4045 0.3997 1.2806 0.027 Uiso 1 1 calc R U . . .
C8 C 0.3055(2) 0.37352(13) 1.18188(12) 0.0221(4) Uani 1 1 d . . . . .
H8 H 0.2073 0.3721 1.2244 0.027 Uiso 1 1 calc R U . . .
C9 C 0.33593(19) 0.35923(13) 1.08545(12) 0.0209(3) Uani 1 1 d . . . . .
H9 H 0.2565 0.347 1.0631 0.025 Uiso 1 1 calc R U . . .
C11 C 0.86152(17) 0.36361(12) 0.68628(10) 0.0122(3) Uani 1 1 d . . . . .
C12 C 0.75986(17) 0.30436(12) 0.68753(11) 0.0149(3) Uani 1 1 d . . . . .
H12 H 0.7552 0.2448 0.7316 0.018 Uiso 1 1 calc R U . . .
C13 C 0.66531(18) 0.33246(14) 0.62436(11) 0.0195(3) Uani 1 1 d . . . . .
H13 H 0.5952 0.2925 0.6258 0.023 Uiso 1 1 calc R U . . .
C14 C 0.67322(19) 0.41854(14) 0.55936(12) 0.0214(4) Uani 1 1 d . . . . .
H14 H 0.6104 0.4366 0.5152 0.026 Uiso 1 1 calc R U . . .
C15 C 0.77274(19) 0.47847(13) 0.55868(11) 0.0188(3) Uani 1 1 d . . . . .
H15 H 0.7768 0.5381 0.5146 0.023 Uiso 1 1 calc R U . . .
C16 C 0.86636(18) 0.45168(12) 0.62210(11) 0.0149(3) Uani 1 1 d . . . . .
H16 H 0.9337 0.4933 0.6218 0.018 Uiso 1 1 calc R U . . .
C21 C 1.22954(16) 0.17629(12) 0.80756(10) 0.0113(3) Uani 1 1 d . . . . .
C22 C 1.25550(17) 0.09021(12) 0.87290(11) 0.0145(3) Uani 1 1 d . . . . .
H22 H 1.2006 0.0382 0.8812 0.017 Uiso 1 1 calc R U . . .
C23 C 1.36209(18) 0.08046(13) 0.92604(11) 0.0185(3) Uani 1 1 d . . . . .
H23 H 1.3819 0.0207 0.9694 0.022 Uiso 1 1 calc R U . . .
C24 C 1.43939(18) 0.15710(13) 0.91619(12) 0.0186(3) Uani 1 1 d . . . . .
H24 H 1.5098 0.151 0.954 0.022 Uiso 1 1 calc R U . . .
C25 C 1.41382(18) 0.24295(13) 0.85087(11) 0.0171(3) Uani 1 1 d . . . . .
H25 H 1.4668 0.2957 0.8441 0.02 Uiso 1 1 calc R U . . .
C26 C 1.31160(17) 0.25204(12) 0.79550(11) 0.0142(3) Uani 1 1 d . . . . .
H26 H 1.2972 0.3097 0.7493 0.017 Uiso 1 1 calc R U . . .
C31 C 1.21404(17) 0.19276(12) 0.61408(10) 0.0127(3) Uani 1 1 d . . . . .
C32 C 1.37497(19) 0.14584(13) 0.59638(12) 0.0190(3) Uani 1 1 d . . . . .
H32 H 1.4194 0.1154 0.6484 0.023 Uiso 1 1 calc R U . . .
C33 C 1.4701(2) 0.14336(15) 0.50365(12) 0.0254(4) Uani 1 1 d . . . . .
H33 H 1.579 0.1112 0.4927 0.031 Uiso 1 1 calc R U . . .
C34 C 1.4077(2) 0.18725(15) 0.42719(12) 0.0249(4) Uani 1 1 d . . . . .
H34 H 1.4734 0.1862 0.3639 0.03 Uiso 1 1 calc R U . . .
C35 C 1.2489(2) 0.23271(13) 0.44333(11) 0.0188(3) Uani 1 1 d . . . . .
H35 H 1.2056 0.263 0.3909 0.023 Uiso 1 1 calc R U . . .
C36 C 1.15225(18) 0.23444(12) 0.53562(11) 0.0142(3) Uani 1 1 d . . . . .
H36 H 1.043 0.2642 0.5456 0.017 Uiso 1 1 calc R U . . .
C41 C 0.9401(2) -0.09807(13) 0.84706(12) 0.0190(3) Uani 1 1 d . . . . .
C42 C 1.0813(2) -0.17847(13) 0.79458(13) 0.0271(4) Uani 1 1 d . . . . .
H42A H 1.0585 -0.248 0.8042 0.032 Uiso 1 1 calc R U . . .
H42B H 1.1693 -0.1853 0.8226 0.032 Uiso 1 1 calc R U . . .
C43 C 1.1312(2) -0.14986(14) 0.68643(13) 0.0276(4) Uani 1 1 d . . . . .
H43A H 1.2435 -0.1848 0.6616 0.033 Uiso 1 1 calc R U . . .
H43B H 1.0726 -0.1772 0.6533 0.033 Uiso 1 1 calc R U . . .
C44 C 1.1024(2) -0.03117(13) 0.66355(12) 0.0204(3) Uani 1 1 d . . . . .
C45 C 0.9676(2) 0.03555(14) 0.64167(11) 0.0202(3) Uani 1 1 d . . . . .
C46 C 0.8240(2) 0.00379(16) 0.64162(13) 0.0283(4) Uani 1 1 d . . . . .
H46A H 0.8437 -0.0296 0.5812 0.034 Uiso 1 1 calc R U . . .
H46B H 0.7357 0.0681 0.6435 0.034 Uiso 1 1 calc R U . . .
C47 C 0.7780(2) -0.07306(16) 0.72632(13) 0.0279(4) Uani 1 1 d . . . . .
H47A H 0.6659 -0.0681 0.7383 0.033 Uiso 1 1 calc R U . . .
H47B H 0.838 -0.1462 0.7098 0.033 Uiso 1 1 calc R U . . .
C48 C 0.8084(2) -0.04951(13) 0.81646(12) 0.0193(3) Uani 1 1 d . . . . .
F1 F 0.30437(11) 0.60586(7) 0.67331(7) 0.0196(2) Uani 1 1 d . . . . .
F2 F 0.14578(14) 0.53633(9) 0.79920(7) 0.0314(3) Uani 1 1 d . . . . .
F3 F 0.05262(11) 0.62283(8) 0.67295(8) 0.0260(2) Uani 1 1 d . . . . .
F4 F 0.23141(12) 0.46210(7) 0.65529(6) 0.0205(2) Uani 1 1 d . . . . .
P1 P 1.09150(4) 0.18785(3) 0.73737(3) 0.00964(8) Uani 1 1 d . . . . .
Cl1 Cl 0.85140(4) 0.12312(3) 0.93900(2) 0.01427(8) Uani 1 1 d . . . . .
Rh1 Rh 0.96152(2) 0.06004(2) 0.78285(2) 0.01087(4) Uani 1 1 d . . . . .
N1 N 0.72304(14) 0.37744(10) 0.98571(9) 0.0119(2) Uani 1 1 d . . . . .
N2 N 0.89638(14) 0.35592(10) 0.84973(9) 0.0111(2) Uani 1 1 d . . . . .
N3 N 0.47157(15) 0.36168(11) 1.02179(9) 0.0175(3) Uani 1 1 d . . . . .
B1 B 0.1850(2) 0.55771(15) 0.69879(13) 0.0173(4) Uani 1 1 d . . . . .
H41 H 0.938(2) -0.0926(16) 0.9113(15) 0.029 Uiso 1 1 d . U . . .
H44 H 1.196(2) -0.0103(16) 0.6398(15) 0.03 Uiso 1 1 d . U . . .
H45 H 0.979(3) 0.0972(18) 0.6024(16) 0.036 Uiso 1 1 d . U . . .
H48 H 0.720(2) -0.0106(16) 0.8596(14) 0.025 Uiso 1 1 d . U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N2 1.3248(19) . ?
C1 N1 1.3325(19) . ?
C1 H1 0.95 . ?
C2 C3 1.348(2) . ?
C2 N1 1.3883(19) . ?
C2 H2 0.95 . ?
C3 N2 1.3873(19) . ?
C3 H3 0.95 . ?
C4 N2 1.4841(18) . ?
C4 C11 1.5135(19) . ?
C4 P1 1.8974(15) . ?
C4 H4 1 . ?
C5 N3 1.324(2) . ?
C5 C6 1.380(2) . ?
C5 N1 1.4356(19) . ?
C6 C7 1.386(2) . ?
C6 H6 0.95 . ?
C7 C8 1.383(3) . ?
C7 H7 0.95 . ?
C8 C9 1.383(2) . ?
C8 H8 0.95 . ?
C9 N3 1.342(2) . ?
C9 H9 0.95 . ?
C11 C12 1.394(2) . ?
C11 C16 1.395(2) . ?
C12 C13 1.390(2) . ?
C12 H12 0.95 . ?
C13 C14 1.384(2) . ?
C13 H13 0.95 . ?
C14 C15 1.386(2) . ?
C14 H14 0.95 . ?
C15 C16 1.387(2) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C21 C22 1.390(2) . ?
C21 C26 1.399(2) . ?
C21 P1 1.8194(15) . ?
C22 C23 1.391(2) . ?
C22 H22 0.95 . ?
C23 C24 1.382(2) . ?
C23 H23 0.95 . ?
C24 C25 1.388(2) . ?
C24 H24 0.95 . ?
C25 C26 1.384(2) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C31 C36 1.398(2) . ?
C31 C32 1.401(2) . ?
C31 P1 1.8389(15) . ?
C32 C33 1.388(2) . ?
C32 H32 0.95 . ?
C33 C34 1.381(3) . ?
C33 H33 0.95 . ?
C34 C35 1.381(2) . ?
C34 H34 0.95 . ?
C35 C36 1.389(2) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C41 C48 1.369(2) . ?
C41 C42 1.508(2) . ?
C41 Rh1 2.2166(16) . ?
C41 H41 0.95(2) . ?
C42 C43 1.539(3) . ?
C42 H42A 0.99 . ?
C42 H42B 0.99 . ?
C43 C44 1.523(2) . ?
C43 H43A 0.99 . ?
C43 H43B 0.99 . ?
C44 C45 1.394(3) . ?
C44 Rh1 2.1367(16) . ?
C44 H44 0.95(2) . ?
C45 C46 1.516(2) . ?
C45 Rh1 2.1140(16) . ?
C45 H45 0.94(2) . ?
C46 C47 1.534(3) . ?
C46 H46A 0.99 . ?
C46 H46B 0.99 . ?
C47 C48 1.514(2) . ?
C47 H47A 0.99 . ?
C47 H47B 0.99 . ?
C48 Rh1 2.2402(15) . ?
C48 H48 0.94(2) . ?
F1 B1 1.379(2) . ?
F2 B1 1.414(2) . ?
F3 B1 1.394(2) . ?
F4 B1 1.395(2) . ?
P1 Rh1 2.2868(4) . ?
Cl1 Rh1 2.3755(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 N1 108.97(13) . . ?
N2 C1 H1 125.5 . . ?
N1 C1 H1 125.5 . . ?
C3 C2 N1 106.65(13) . . ?
C3 C2 H2 126.7 . . ?
N1 C2 H2 126.7 . . ?
C2 C3 N2 107.51(13) . . ?
C2 C3 H3 126.2 . . ?
N2 C3 H3 126.2 . . ?
N2 C4 C11 111.80(11) . . ?
N2 C4 P1 111.72(9) . . ?
C11 C4 P1 111.75(10) . . ?
N2 C4 H4 107.1 . . ?
C11 C4 H4 107.1 . . ?
P1 C4 H4 107.1 . . ?
N3 C5 C6 125.80(14) . . ?
N3 C5 N1 113.79(13) . . ?
C6 C5 N1 120.40(14) . . ?
C5 C6 C7 116.66(15) . . ?
C5 C6 H6 121.7 . . ?
C7 C6 H6 121.7 . . ?
C8 C7 C6 119.67(15) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 118.20(15) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
N3 C9 C8 123.58(16) . . ?
N3 C9 H9 118.2 . . ?
C8 C9 H9 118.2 . . ?
C12 C11 C16 119.59(14) . . ?
C12 C11 C4 122.02(13) . . ?
C16 C11 C4 118.28(13) . . ?
C13 C12 C11 120.04(15) . . ?
C13 C12 H12 120 . . ?
C11 C12 H12 120 . . ?
C14 C13 C12 120.09(15) . . ?
C14 C13 H13 120 . . ?
C12 C13 H13 120 . . ?
C13 C14 C15 120.05(15) . . ?
C13 C14 H14 120 . . ?
C15 C14 H14 120 . . ?
C14 C15 C16 120.25(15) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 119.95(15) . . ?
C15 C16 H16 120 . . ?
C11 C16 H16 120 . . ?
C22 C21 C26 119.63(13) . . ?
C22 C21 P1 119.55(11) . . ?
C26 C21 P1 120.81(11) . . ?
C21 C22 C23 119.77(14) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 120.49(15) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 119.78(14) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 120.33(15) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 119.94(14) . . ?
C25 C26 H26 120 . . ?
C21 C26 H26 120 . . ?
C36 C31 C32 118.06(14) . . ?
C36 C31 P1 122.74(11) . . ?
C32 C31 P1 119.02(12) . . ?
C33 C32 C31 120.64(15) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 120.55(16) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C33 C34 C35 119.52(15) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C36 120.51(15) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 120.69(15) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
C48 C41 C42 126.03(16) . . ?
C48 C41 Rh1 73.05(9) . . ?
C42 C41 Rh1 107.15(11) . . ?
C48 C41 H41 118.9(13) . . ?
C42 C41 H41 114.0(13) . . ?
Rh1 C41 H41 101.2(13) . . ?
C41 C42 C43 113.29(15) . . ?
C41 C42 H42A 108.9 . . ?
C43 C42 H42A 108.9 . . ?
C41 C42 H42B 108.9 . . ?
C43 C42 H42B 108.9 . . ?
H42A C42 H42B 107.7 . . ?
C44 C43 C42 112.47(14) . . ?
C44 C43 H43A 109.1 . . ?
C42 C43 H43A 109.1 . . ?
C44 C43 H43B 109.1 . . ?
C42 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
C45 C44 C43 124.75(16) . . ?
C45 C44 Rh1 69.98(9) . . ?
C43 C44 Rh1 113.35(11) . . ?
C45 C44 H44 118.0(13) . . ?
C43 C44 H44 112.8(13) . . ?
Rh1 C44 H44 108.1(13) . . ?
C44 C45 C46 126.12(16) . . ?
C44 C45 Rh1 71.74(9) . . ?
C46 C45 Rh1 109.97(11) . . ?
C44 C45 H45 116.6(13) . . ?
C46 C45 H45 113.3(13) . . ?
Rh1 C45 H45 108.8(13) . . ?
C45 C46 C47 113.19(15) . . ?
C45 C46 H46A 108.9 . . ?
C47 C46 H46A 108.9 . . ?
C45 C46 H46B 108.9 . . ?
C47 C46 H46B 108.9 . . ?
H46A C46 H46B 107.8 . . ?
C48 C47 C46 111.84(14) . . ?
C48 C47 H47A 109.2 . . ?
C46 C47 H47A 109.2 . . ?
C48 C47 H47B 109.2 . . ?
C46 C47 H47B 109.2 . . ?
H47A C47 H47B 107.9 . . ?
C41 C48 C47 124.99(16) . . ?
C41 C48 Rh1 71.17(9) . . ?
C47 C48 Rh1 110.97(11) . . ?
C41 C48 H48 118.8(12) . . ?
C47 C48 H48 114.6(12) . . ?
Rh1 C48 H48 100.9(12) . . ?
C21 P1 C31 102.02(7) . . ?
C21 P1 C4 102.03(7) . . ?
C31 P1 C4 100.70(7) . . ?
C21 P1 Rh1 112.26(5) . . ?
C31 P1 Rh1 118.50(5) . . ?
C4 P1 Rh1 118.77(5) . . ?
C45 Rh1 C44 38.29(7) . . ?
C45 Rh1 C41 97.03(6) . . ?
C44 Rh1 C41 81.38(6) . . ?
C45 Rh1 C48 80.97(6) . . ?
C44 Rh1 C48 88.13(6) . . ?
C41 Rh1 C48 35.78(6) . . ?
C45 Rh1 P1 94.64(5) . . ?
C44 Rh1 P1 92.88(5) . . ?
C41 Rh1 P1 152.63(5) . . ?
C48 Rh1 P1 171.55(5) . . ?
C45 Rh1 Cl1 157.09(5) . . ?
C44 Rh1 Cl1 163.44(5) . . ?
C41 Rh1 Cl1 87.80(4) . . ?
C48 Rh1 Cl1 90.40(4) . . ?
P1 Rh1 Cl1 90.998(13) . . ?
C1 N1 C2 108.56(12) . . ?
C1 N1 C5 123.65(13) . . ?
C2 N1 C5 127.65(13) . . ?
C1 N2 C3 108.31(12) . . ?
C1 N2 C4 125.96(12) . . ?
C3 N2 C4 125.67(12) . . ?
C5 N3 C9 116.09(14) . . ?
F1 B1 F3 111.04(14) . . ?
F1 B1 F4 110.46(14) . . ?
F3 B1 F4 109.40(13) . . ?
F1 B1 F2 109.27(13) . . ?
F3 B1 F2 108.37(14) . . ?
F4 B1 F2 108.23(14) . . ?

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
N1 C2 C3 N2 -0.27(17) . . . . ?
N3 C5 C6 C7 -0.1(2) . . . . ?
N1 C5 C6 C7 -179.25(14) . . . . ?
C5 C6 C7 C8 0.1(2) . . . . ?
C6 C7 C8 C9 0.3(3) . . . . ?
C7 C8 C9 N3 -0.8(3) . . . . ?
N2 C4 C11 C12 -76.25(17) . . . . ?
P1 C4 C11 C12 49.82(17) . . . . ?
N2 C4 C11 C16 107.58(15) . . . . ?
P1 C4 C11 C16 -126.35(12) . . . . ?
C16 C11 C12 C13 0.7(2) . . . . ?
C4 C11 C12 C13 -175.41(14) . . . . ?
C11 C12 C13 C14 0.8(2) . . . . ?
C12 C13 C14 C15 -1.6(2) . . . . ?
C13 C14 C15 C16 0.9(2) . . . . ?
C14 C15 C16 C11 0.6(2) . . . . ?
C12 C11 C16 C15 -1.4(2) . . . . ?
C4 C11 C16 C15 174.90(13) . . . . ?
C26 C21 C22 C23 0.4(2) . . . . ?
P1 C21 C22 C23 179.36(12) . . . . ?
C21 C22 C23 C24 1.7(2) . . . . ?
C22 C23 C24 C25 -1.8(2) . . . . ?
C23 C24 C25 C26 -0.1(2) . . . . ?
C24 C25 C26 C21 2.2(2) . . . . ?
C22 C21 C26 C25 -2.3(2) . . . . ?
P1 C21 C26 C25 178.75(12) . . . . ?
C36 C31 C32 C33 1.5(2) . . . . ?
P1 C31 C32 C33 176.78(13) . . . . ?
C31 C32 C33 C34 0.1(3) . . . . ?
C32 C33 C34 C35 -0.8(3) . . . . ?
C33 C34 C35 C36 0.0(3) . . . . ?
C34 C35 C36 C31 1.7(2) . . . . ?
C32 C31 C36 C35 -2.4(2) . . . . ?
P1 C31 C36 C35 -177.46(12) . . . . ?
C48 C41 C42 C43 42.8(2) . . . . ?
Rh1 C41 C42 C43 -38.41(18) . . . . ?
C41 C42 C43 C44 34.3(2) . . . . ?
C42 C43 C44 C45 -92.9(2) . . . . ?
C42 C43 C44 Rh1 -11.7(2) . . . . ?
C43 C44 C45 C46 3.3(3) . . . . ?
Rh1 C44 C45 C46 -101.80(16) . . . . ?
C43 C44 C45 Rh1 105.11(16) . . . . ?
C44 C45 C46 C47 41.3(2) . . . . ?
Rh1 C45 C46 C47 -40.23(19) . . . . ?
C45 C46 C47 C48 35.8(2) . . . . ?
C42 C41 C48 C47 3.7(3) . . . . ?
Rh1 C41 C48 C47 102.87(16) . . . . ?
C42 C41 C48 Rh1 -99.18(16) . . . . ?
C46 C47 C48 C41 -95.3(2) . . . . ?
C46 C47 C48 Rh1 -14.2(2) . . . . ?
C22 C21 P1 C31 -121.94(12) . . . . ?
C26 C21 P1 C31 57.05(13) . . . . ?
C22 C21 P1 C4 134.21(12) . . . . ?
C26 C21 P1 C4 -46.80(13) . . . . ?
C22 C21 P1 Rh1 5.97(13) . . . . ?
C26 C21 P1 Rh1 -175.04(10) . . . . ?
C36 C31 P1 C21 -159.03(13) . . . . ?
C32 C31 P1 C21 25.93(14) . . . . ?
C36 C31 P1 C4 -54.13(14) . . . . ?
C32 C31 P1 C4 130.83(13) . . . . ?
C36 C31 P1 Rh1 77.16(13) . . . . ?
C32 C31 P1 Rh1 -97.87(12) . . . . ?
N2 C4 P1 C21 -59.82(11) . . . . ?
C11 C4 P1 C21 174.06(10) . . . . ?
N2 C4 P1 C31 -164.71(10) . . . . ?
C11 C4 P1 C31 69.18(11) . . . . ?
N2 C4 P1 Rh1 64.16(10) . . . . ?
C11 C4 P1 Rh1 -61.95(11) . . . . ?
N2 C1 N1 C2 -1.04(17) . . . . ?
N2 C1 N1 C5 -176.93(13) . . . . ?
C3 C2 N1 C1 0.80(17) . . . . ?
C3 C2 N1 C5 176.48(14) . . . . ?
N3 C5 N1 C1 -5.7(2) . . . . ?
C6 C5 N1 C1 173.55(14) . . . . ?
N3 C5 N1 C2 179.21(14) . . . . ?
C6 C5 N1 C2 -1.5(2) . . . . ?
N1 C1 N2 C3 0.87(17) . . . . ?
N1 C1 N2 C4 178.32(13) . . . . ?
C2 C3 N2 C1 -0.36(17) . . . . ?
C2 C3 N2 C4 -177.82(13) . . . . ?
C11 C4 N2 C1 32.28(19) . . . . ?
P1 C4 N2 C1 -93.81(15) . . . . ?
C11 C4 N2 C3 -150.70(14) . . . . ?
P1 C4 N2 C3 83.21(15) . . . . ?
C6 C5 N3 C9 -0.4(2) . . . . ?
N1 C5 N3 C9 178.85(13) . . . . ?
C8 C9 N3 C5 0.8(2) . . . . ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1556217'
_audit_update_record             
;
2017-06-15 deposited with the CCDC.
2017-07-07 downloaded from the CCDC.
;

_audit_creation_date             2017-06-15T09:14:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C27 H22 Br2 N3 Ni P'
_chemical_formula_sum            'C27 H22 Br2 N3 Ni P'
_chemical_formula_weight         637.97

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.7320(11)
_cell_length_b                   7.9816(6)
_cell_length_c                   23.4948(18)
_cell_angle_alpha                90
_cell_angle_beta                 96.728(3)
_cell_angle_gamma                90
_cell_volume                     2557.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9856
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      60.669

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Plates
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
        wR2(int) was 0.1340 before and 0.0616 after correction.
        The Ratio of minimum to maximum transmission is 0.5784.
        The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_correction_T_min  0.4349
_exptl_absorpt_correction_T_max  0.7519
_shelx_estimated_absorpt_T_min   0.311
_shelx_estimated_absorpt_T_max   0.76

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      273.15
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_type           GaK\a
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_number            42082
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.819
_diffrn_reflns_theta_max         60.638
_diffrn_reflns_theta_full        53.594
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             5881
_reflns_number_gt                5679
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'XT (Sheldrick, 2015)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²+1.9737P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5881
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_restrained_S_all      1.07
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.094

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.015 0.007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.95 1.041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.025 0.014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -1.341 3.29 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.26 0.335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Br1 Br 0.34464(2) 0.90506(3) 0.58191(2) 0.02311(7) Uani 1 1 d . . . . .
Br2 Br 0.08843(2) 0.81207(3) 0.62115(2) 0.02159(7) Uani 1 1 d . . . . .
Ni1 Ni 0.23662(2) 0.67508(3) 0.57222(2) 0.01927(8) Uani 1 1 d . . . . .
P1 P 0.32553(4) 0.51799(6) 0.63206(2) 0.01950(10) Uani 1 1 d . . . . .
N3 N 0.17033(12) 0.7196(2) 0.49165(7) 0.0203(3) Uani 1 1 d . . . . .
N1 N 0.12546(12) 0.4496(2) 0.50465(7) 0.0206(3) Uani 1 1 d . . . . .
N2 N 0.18687(13) 0.3264(2) 0.58244(7) 0.0211(3) Uani 1 1 d . . . . .
C9 C 0.17336(16) 0.8597(3) 0.46041(9) 0.0243(4) Uani 1 1 d . . . . .
H9 H 0.2074 0.952 0.4766 0.029 Uiso 1 1 calc R U . . .
C8 C 0.12732(17) 0.8716(3) 0.40464(9) 0.0281(4) Uani 1 1 d . . . . .
H8 H 0.1306 0.9702 0.3839 0.034 Uiso 1 1 calc R U . . .
C7 C 0.07635(16) 0.7338(3) 0.38037(9) 0.0286(4) Uani 1 1 d . . . . .
H7 H 0.0451 0.7396 0.3431 0.034 Uiso 1 1 calc R U . . .
C6 C 0.07218(15) 0.5871(3) 0.41202(9) 0.0241(4) Uani 1 1 d . . . . .
H6 H 0.0387 0.4931 0.3968 0.029 Uiso 1 1 calc R U . . .
C5 C 0.12016(14) 0.5878(3) 0.46709(8) 0.0208(4) Uani 1 1 d . . . . .
C1 C 0.18105(14) 0.4745(3) 0.55553(8) 0.0207(4) Uani 1 1 d . . . . .
C2 C 0.09536(15) 0.2815(3) 0.50012(9) 0.0227(4) Uani 1 1 d . . . . .
H2 H 0.0567 0.2322 0.4695 0.027 Uiso 1 1 calc R U . . .
C3 C 0.13376(15) 0.2055(3) 0.54910(9) 0.0224(4) Uani 1 1 d . . . . .
H3 H 0.1262 0.0936 0.5587 0.027 Uiso 1 1 calc R U . . .
C4 C 0.25497(15) 0.3141(2) 0.63560(8) 0.0206(4) Uani 1 1 d . . . . .
H4 H 0.2997 0.2198 0.6323 0.025 Uiso 1 1 calc R U . . .
C11 C 0.20425(15) 0.2914(3) 0.68866(8) 0.0220(4) Uani 1 1 d . . . . .
C16 C 0.13407(15) 0.4054(3) 0.70325(9) 0.0241(4) Uani 1 1 d . . . . .
H16 H 0.1177 0.4979 0.68 0.029 Uiso 1 1 calc R U . . .
C15 C 0.08868(16) 0.3807(3) 0.75246(9) 0.0277(4) Uani 1 1 d . . . . .
H15 H 0.0418 0.4566 0.7619 0.033 Uiso 1 1 calc R U . . .
C14 C 0.11284(19) 0.2444(3) 0.78724(10) 0.0355(5) Uani 1 1 d . . . . .
H14 H 0.082 0.2279 0.82 0.043 Uiso 1 1 calc R U . . .
C13 C 0.1831(2) 0.1321(4) 0.77338(12) 0.0439(6) Uani 1 1 d . . . . .
H13 H 0.1999 0.0408 0.7971 0.053 Uiso 1 1 calc R U . . .
C12 C 0.22871(19) 0.1551(3) 0.72402(11) 0.0330(5) Uani 1 1 d . . . . .
H12 H 0.2756 0.0789 0.7148 0.04 Uiso 1 1 calc R U . . .
C31 C 0.36313(15) 0.5697(3) 0.70605(8) 0.0221(4) Uani 1 1 d . . . . .
C32 C 0.31156(17) 0.6900(3) 0.73314(9) 0.0270(4) Uani 1 1 d . . . . .
H32 H 0.2629 0.7531 0.7123 0.032 Uiso 1 1 calc R U . . .
C33 C 0.33376(19) 0.7147(3) 0.79193(10) 0.0339(5) Uani 1 1 d . . . . .
H33 H 0.2993 0.7943 0.8105 0.041 Uiso 1 1 calc R U . . .
C34 C 0.40687(19) 0.6214(3) 0.82287(10) 0.0336(5) Uani 1 1 d . . . . .
H34 H 0.4209 0.6382 0.8621 0.04 Uiso 1 1 calc R U . . .
C35 C 0.45917(18) 0.5036(3) 0.79580(10) 0.0316(5) Uani 1 1 d . . . . .
H35 H 0.509 0.4428 0.8167 0.038 Uiso 1 1 calc R U . . .
C36 C 0.43707(16) 0.4762(3) 0.73729(9) 0.0273(4) Uani 1 1 d . . . . .
H36 H 0.4714 0.3959 0.719 0.033 Uiso 1 1 calc R U . . .
C21 C 0.43585(15) 0.4591(3) 0.60155(8) 0.0229(4) Uani 1 1 d . . . . .
C26 C 0.52199(16) 0.5505(3) 0.61522(9) 0.0280(4) Uani 1 1 d . . . . .
H26 H 0.5244 0.6359 0.6423 0.034 Uiso 1 1 calc R U . . .
C25 C 0.60453(17) 0.5132(3) 0.58807(10) 0.0350(5) Uani 1 1 d . . . . .
H25 H 0.6623 0.5732 0.5972 0.042 Uiso 1 1 calc R U . . .
C24 C 0.60023(18) 0.3867(3) 0.54739(10) 0.0367(6) Uani 1 1 d . . . . .
H24 H 0.6552 0.3626 0.5292 0.044 Uiso 1 1 calc R U . . .
C23 C 0.51510(18) 0.2961(3) 0.53366(10) 0.0326(5) Uani 1 1 d . . . . .
H23 H 0.513 0.211 0.5065 0.039 Uiso 1 1 calc R U . . .
C22 C 0.43261(17) 0.3319(3) 0.56033(9) 0.0264(4) Uani 1 1 d . . . . .
H22 H 0.3751 0.2714 0.5508 0.032 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Br1 Ni1 2.3542(4) . ?
Br2 Ni1 2.6845(4) . ?
Ni1 C1 1.797(2) . ?
Ni1 N3 2.0333(16) . ?
Ni1 P1 2.1534(6) . ?
P1 C31 1.802(2) . ?
P1 C21 1.812(2) . ?
P1 C4 1.901(2) . ?
N3 C9 1.341(3) . ?
N3 C5 1.349(3) . ?
N1 C1 1.356(2) . ?
N1 C2 1.404(3) . ?
N1 C5 1.409(3) . ?
N2 C1 1.338(3) . ?
N2 C3 1.394(3) . ?
N2 C4 1.473(2) . ?
C9 C8 1.390(3) . ?
C9 H9 0.93 . ?
C8 C7 1.389(3) . ?
C8 H8 0.93 . ?
C7 C6 1.392(3) . ?
C7 H7 0.93 . ?
C6 C5 1.382(3) . ?
C6 H6 0.93 . ?
C2 C3 1.352(3) . ?
C2 H2 0.93 . ?
C3 H3 0.93 . ?
C4 C11 1.508(3) . ?
C4 H4 0.98 . ?
C11 C12 1.386(3) . ?
C11 C16 1.397(3) . ?
C16 C15 1.390(3) . ?
C16 H16 0.93 . ?
C15 C14 1.378(3) . ?
C15 H15 0.93 . ?
C14 C13 1.383(4) . ?
C14 H14 0.93 . ?
C13 C12 1.393(3) . ?
C13 H13 0.93 . ?
C12 H12 0.93 . ?
C31 C32 1.390(3) . ?
C31 C36 1.397(3) . ?
C32 C33 1.393(3) . ?
C32 H32 0.93 . ?
C33 C34 1.386(4) . ?
C33 H33 0.93 . ?
C34 C35 1.383(4) . ?
C34 H34 0.93 . ?
C35 C36 1.390(3) . ?
C35 H35 0.93 . ?
C36 H36 0.93 . ?
C21 C26 1.395(3) . ?
C21 C22 1.400(3) . ?
C26 C25 1.396(3) . ?
C26 H26 0.93 . ?
C25 C24 1.387(4) . ?
C25 H25 0.93 . ?
C24 C23 1.380(4) . ?
C24 H24 0.93 . ?
C23 C22 1.387(3) . ?
C23 H23 0.93 . ?
C22 H22 0.93 . ?

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
C1 Ni1 N3 79.64(8) . . ?
C1 Ni1 P1 79.48(6) . . ?
N3 Ni1 P1 150.14(5) . . ?
C1 Ni1 Br1 164.24(6) . . ?
N3 Ni1 Br1 99.33(5) . . ?
P1 Ni1 Br1 95.063(18) . . ?
C1 Ni1 Br2 97.61(6) . . ?
N3 Ni1 Br2 92.77(5) . . ?
P1 Ni1 Br2 110.965(18) . . ?
Br1 Ni1 Br2 98.143(13) . . ?
C31 P1 C21 106.42(10) . . ?
C31 P1 C4 104.12(9) . . ?
C21 P1 C4 104.43(10) . . ?
C31 P1 Ni1 124.94(7) . . ?
C21 P1 Ni1 109.21(7) . . ?
C4 P1 Ni1 105.91(6) . . ?
C9 N3 C5 117.58(17) . . ?
C9 N3 Ni1 128.03(14) . . ?
C5 N3 Ni1 114.35(13) . . ?
C1 N1 C2 109.70(17) . . ?
C1 N1 C5 114.84(17) . . ?
C2 N1 C5 135.01(17) . . ?
C1 N2 C3 110.35(16) . . ?
C1 N2 C4 117.17(16) . . ?
C3 N2 C4 131.92(17) . . ?
N3 C9 C8 122.2(2) . . ?
N3 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C7 C8 C9 119.0(2) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C8 C7 C6 119.78(19) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C5 C6 C7 116.9(2) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 H6 121.6 . . ?
N3 C5 C6 124.54(19) . . ?
N3 C5 N1 110.86(17) . . ?
C6 C5 N1 124.58(19) . . ?
N2 C1 N1 106.47(17) . . ?
N2 C1 Ni1 133.11(15) . . ?
N1 C1 Ni1 120.25(15) . . ?
C3 C2 N1 106.38(17) . . ?
C3 C2 H2 126.8 . . ?
N1 C2 H2 126.8 . . ?
C2 C3 N2 107.08(18) . . ?
C2 C3 H3 126.5 . . ?
N2 C3 H3 126.5 . . ?
N2 C4 C11 113.58(17) . . ?
N2 C4 P1 100.46(13) . . ?
C11 C4 P1 115.19(14) . . ?
N2 C4 H4 109.1 . . ?
C11 C4 H4 109.1 . . ?
P1 C4 H4 109.1 . . ?
C12 C11 C16 119.3(2) . . ?
C12 C11 C4 119.10(19) . . ?
C16 C11 C4 121.58(18) . . ?
C15 C16 C11 120.1(2) . . ?
C15 C16 H16 120 . . ?
C11 C16 H16 120 . . ?
C14 C15 C16 120.3(2) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C11 C12 C13 120.1(2) . . ?
C11 C12 H12 120 . . ?
C13 C12 H12 120 . . ?
C32 C31 C36 120.40(19) . . ?
C32 C31 P1 119.73(16) . . ?
C36 C31 P1 119.51(16) . . ?
C31 C32 C33 119.2(2) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C34 C33 C32 120.3(2) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C35 C34 C33 120.5(2) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 119.8(2) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 119.8(2) . . ?
C35 C36 H36 120.1 . . ?
C31 C36 H36 120.1 . . ?
C26 C21 C22 119.7(2) . . ?
C26 C21 P1 119.94(17) . . ?
C22 C21 P1 120.09(16) . . ?
C21 C26 C25 119.7(2) . . ?
C21 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C24 C25 C26 119.9(2) . . ?
C24 C25 H25 120 . . ?
C26 C25 H25 120 . . ?
C23 C24 C25 120.6(2) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C23 C22 120.0(2) . . ?
C24 C23 H23 120 . . ?
C22 C23 H23 120 . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120 . . ?
C21 C22 H22 120 . . ?

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
C5 N3 C9 C8 -0.2(3) . . . . ?
Ni1 N3 C9 C8 177.55(16) . . . . ?
N3 C9 C8 C7 0.0(3) . . . . ?
C9 C8 C7 C6 0.0(3) . . . . ?
C8 C7 C6 C5 0.1(3) . . . . ?
C9 N3 C5 C6 0.3(3) . . . . ?
Ni1 N3 C5 C6 -177.74(16) . . . . ?
C9 N3 C5 N1 178.76(17) . . . . ?
Ni1 N3 C5 N1 0.7(2) . . . . ?
C7 C6 C5 N3 -0.2(3) . . . . ?
C7 C6 C5 N1 -178.51(19) . . . . ?
C1 N1 C5 N3 -2.1(2) . . . . ?
C2 N1 C5 N3 -173.5(2) . . . . ?
C1 N1 C5 C6 176.33(19) . . . . ?
C2 N1 C5 C6 5.0(4) . . . . ?
C3 N2 C1 N1 -0.7(2) . . . . ?
C4 N2 C1 N1 171.73(16) . . . . ?
C3 N2 C1 Ni1 -175.88(17) . . . . ?
C4 N2 C1 Ni1 -3.4(3) . . . . ?
C2 N1 C1 N2 0.5(2) . . . . ?
C5 N1 C1 N2 -173.05(17) . . . . ?
C2 N1 C1 Ni1 176.37(14) . . . . ?
C5 N1 C1 Ni1 2.9(2) . . . . ?
N3 Ni1 C1 N2 172.8(2) . . . . ?
P1 Ni1 C1 N2 14.22(19) . . . . ?
Br1 Ni1 C1 N2 85.1(3) . . . . ?
Br2 Ni1 C1 N2 -95.8(2) . . . . ?
N3 Ni1 C1 N1 -1.86(15) . . . . ?
P1 Ni1 C1 N1 -160.40(17) . . . . ?
Br1 Ni1 C1 N1 -89.5(3) . . . . ?
Br2 Ni1 C1 N1 89.58(16) . . . . ?
C1 N1 C2 C3 0.0(2) . . . . ?
C5 N1 C2 C3 171.6(2) . . . . ?
N1 C2 C3 N2 -0.4(2) . . . . ?
C1 N2 C3 C2 0.7(2) . . . . ?
C4 N2 C3 C2 -170.2(2) . . . . ?
C1 N2 C4 C11 112.0(2) . . . . ?
C3 N2 C4 C11 -77.5(3) . . . . ?
C1 N2 C4 P1 -11.5(2) . . . . ?
C3 N2 C4 P1 158.93(19) . . . . ?
N2 C4 C11 C12 124.3(2) . . . . ?
P1 C4 C11 C12 -120.6(2) . . . . ?
N2 C4 C11 C16 -56.3(3) . . . . ?
P1 C4 C11 C16 58.8(2) . . . . ?
C12 C11 C16 C15 -0.7(3) . . . . ?
C4 C11 C16 C15 179.97(19) . . . . ?
C11 C16 C15 C14 0.3(3) . . . . ?
C16 C15 C14 C13 0.4(4) . . . . ?
C15 C14 C13 C12 -0.8(4) . . . . ?
C16 C11 C12 C13 0.4(4) . . . . ?
C4 C11 C12 C13 179.7(2) . . . . ?
C14 C13 C12 C11 0.3(4) . . . . ?
C21 P1 C31 C32 149.00(18) . . . . ?
C4 P1 C31 C32 -100.99(18) . . . . ?
Ni1 P1 C31 C32 20.4(2) . . . . ?
C21 P1 C31 C36 -37.8(2) . . . . ?
C4 P1 C31 C36 72.21(19) . . . . ?
Ni1 P1 C31 C36 -166.42(14) . . . . ?
C36 C31 C32 C33 -0.7(3) . . . . ?
P1 C31 C32 C33 172.41(18) . . . . ?
C31 C32 C33 C34 0.5(4) . . . . ?
C32 C33 C34 C35 0.5(4) . . . . ?
C33 C34 C35 C36 -1.2(4) . . . . ?
C34 C35 C36 C31 1.0(4) . . . . ?
C32 C31 C36 C35 0.0(3) . . . . ?
P1 C31 C36 C35 -173.15(18) . . . . ?
C31 P1 C21 C26 -41.53(19) . . . . ?
C4 P1 C21 C26 -151.31(16) . . . . ?
Ni1 P1 C21 C26 95.77(16) . . . . ?
C31 P1 C21 C22 144.28(16) . . . . ?
C4 P1 C21 C22 34.50(18) . . . . ?
Ni1 P1 C21 C22 -78.42(17) . . . . ?
C22 C21 C26 C25 -0.6(3) . . . . ?
P1 C21 C26 C25 -174.84(17) . . . . ?
C21 C26 C25 C24 0.5(3) . . . . ?
C26 C25 C24 C23 -0.4(3) . . . . ?
C25 C24 C23 C22 0.4(3) . . . . ?
C24 C23 C22 C21 -0.5(3) . . . . ?
C26 C21 C22 C23 0.6(3) . . . . ?
P1 C21 C22 C23 174.83(16) . . . . ?



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1556216'
_audit_update_record             
;
2017-06-15 deposited with the CCDC.
2017-07-07 downloaded from the CCDC.
;

_audit_creation_date             2017-05-01T16:08:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C34 H30 I3 N3 P Rh'
_chemical_formula_moiety         'C27 H22 I3 N3 P Rh, C7 H8'
_chemical_formula_weight         995.19

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9780(3)
_cell_length_b                   15.1277(3)
_cell_length_c                   17.3050(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.2880(10)
_cell_angle_gamma                90
_cell_volume                     3394.74(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      1.80
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#


_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_T_max  0.7469

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.013
_diffrn_reflns_number            119877
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_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         2.356
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             6940
_reflns_number_gt                6448
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0195P)²+10.9637P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6940
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_ref         0.056
_refine_ls_wR_factor_gt          0.0525
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.91
_refine_diff_density_rms         0.102

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.2969(2) 0.62058(19) 0.49468(18) 0.0165(6) Uani 1 1 d . . . . .
C2 C 0.3127(2) 0.4866(2) 0.54883(19) 0.0218(7) Uani 1 1 d . . . . .
H2 H 0.3315 0.4266 0.5572 0.026 Uiso 1 1 calc R U . . .
C3 C 0.2574(2) 0.5374(2) 0.59538(19) 0.0218(7) Uani 1 1 d . . . . .
H3 H 0.2295 0.52 0.643 0.026 Uiso 1 1 calc R U . . .
C4 C 0.1927(2) 0.6999(2) 0.58430(17) 0.0187(6) Uani 1 1 d . . . . .
H4 H 0.2268 0.7229 0.6331 0.022 Uiso 1 1 calc R U . . .
C5 C 0.3917(2) 0.5253(2) 0.41806(18) 0.0193(6) Uani 1 1 d . . . . .
C6 C 0.4354(3) 0.4452(2) 0.4000(2) 0.0262(7) Uani 1 1 d . . . . .
H6 H 0.427 0.3944 0.4313 0.031 Uiso 1 1 calc R U . . .
C7 C 0.4920(3) 0.4425(2) 0.3340(2) 0.0305(8) Uani 1 1 d . . . . .
H7 H 0.5236 0.3887 0.3192 0.037 Uiso 1 1 calc R U . . .
C8 C 0.5028(3) 0.5173(2) 0.2897(2) 0.0286(8) Uani 1 1 d . . . . .
H8 H 0.5435 0.5162 0.2452 0.034 Uiso 1 1 calc R U . . .
C9 C 0.4534(2) 0.5943(2) 0.31075(19) 0.0230(7) Uani 1 1 d . . . . .
H9 H 0.4596 0.6456 0.2796 0.028 Uiso 1 1 calc R U . . .
C11 C 0.0824(3) 0.6775(2) 0.60049(18) 0.0197(6) Uani 1 1 d . . . . .
C12 C 0.0400(3) 0.7068(2) 0.66835(19) 0.0274(7) Uani 1 1 d . . . . .
H12 H 0.0816 0.738 0.7056 0.033 Uiso 1 1 calc R U . . .
C13 C -0.0637(3) 0.6903(2) 0.6818(2) 0.0351(9) Uani 1 1 d . . . . .
H13 H -0.0932 0.7124 0.7273 0.042 Uiso 1 1 calc R U . . .
C14 C -0.1230(3) 0.6424(3) 0.6295(3) 0.0378(9) Uani 1 1 d . . . . .
H14 H -0.1933 0.6309 0.6389 0.045 Uiso 1 1 calc R U . . .
C15 C -0.0801(3) 0.6106(3) 0.5626(2) 0.0340(8) Uani 1 1 d . . . . .
H15 H -0.1208 0.5764 0.5268 0.041 Uiso 1 1 calc R U . . .
C16 C 0.0219(3) 0.6285(2) 0.5479(2) 0.0246(7) Uani 1 1 d . . . . .
H16 H 0.0506 0.6073 0.5018 0.03 Uiso 1 1 calc R U . . .
C21 C 0.2743(2) 0.8796(2) 0.55132(18) 0.0180(6) Uani 1 1 d . . . . .
C22 C 0.3253(2) 0.9391(2) 0.5046(2) 0.0226(7) Uani 1 1 d . . . . .
H22 H 0.3291 0.9281 0.4508 0.027 Uiso 1 1 calc R U . . .
C23 C 0.3707(3) 1.0146(2) 0.5366(2) 0.0271(7) Uani 1 1 d . . . . .
H23 H 0.4067 1.0543 0.5049 0.033 Uiso 1 1 calc R U . . .
C24 C 0.3635(3) 1.0320(2) 0.6147(2) 0.0280(7) Uani 1 1 d . . . . .
H24 H 0.3955 1.0831 0.6367 0.034 Uiso 1 1 calc R U . . .
C25 C 0.3093(3) 0.9746(2) 0.6608(2) 0.0270(7) Uani 1 1 d . . . . .
H25 H 0.302 0.9878 0.714 0.032 Uiso 1 1 calc R U . . .
C26 C 0.2659(3) 0.8983(2) 0.62974(19) 0.0232(7) Uani 1 1 d . . . . .
H26 H 0.2303 0.8587 0.6619 0.028 Uiso 1 1 calc R U . . .
C31 C 0.0884(2) 0.83185(19) 0.47633(18) 0.0177(6) Uani 1 1 d . . . . .
C32 C 0.0581(3) 0.8454(2) 0.39940(19) 0.0230(7) Uani 1 1 d . . . . .
H32 H 0.1006 0.826 0.3593 0.028 Uiso 1 1 calc R U . . .
C33 C -0.0355(3) 0.8878(2) 0.3815(2) 0.0305(8) Uani 1 1 d . . . . .
H33 H -0.0562 0.8981 0.3289 0.037 Uiso 1 1 calc R U . . .
C34 C -0.0978(3) 0.9147(2) 0.4394(2) 0.0327(8) Uani 1 1 d . . . . .
H34 H -0.1621 0.942 0.4266 0.039 Uiso 1 1 calc R U . . .
C35 C -0.0676(3) 0.9023(2) 0.5159(2) 0.0289(7) Uani 1 1 d . . . . .
H35 H -0.1111 0.9211 0.5556 0.035 Uiso 1 1 calc R U . . .
C36 C 0.0255(3) 0.8628(2) 0.5346(2) 0.0242(7) Uani 1 1 d . . . . .
H36 H 0.0474 0.8564 0.5874 0.029 Uiso 1 1 calc R U . . .
C41 C 0.1874(3) 0.3904(3) 0.7487(2) 0.0320(8) Uani 1 1 d . . . . .
C42 C 0.1868(3) 0.3387(3) 0.6813(2) 0.0348(8) Uani 1 1 d . . . . .
H42 H 0.1343 0.3475 0.6421 0.042 Uiso 1 1 calc R U . . .
C43 C 0.2614(3) 0.2754(3) 0.6711(3) 0.0394(9) Uani 1 1 d . . . . .
H43 H 0.2605 0.241 0.6251 0.047 Uiso 1 1 calc R U . . .
C44 C 0.3376(4) 0.2621(3) 0.7281(3) 0.0454(10) Uani 1 1 d . . . . .
H44 H 0.3892 0.2186 0.721 0.054 Uiso 1 1 calc R U . . .
C45 C 0.3392(4) 0.3116(3) 0.7954(3) 0.0476(11) Uani 1 1 d . . . . .
H45 H 0.391 0.3018 0.8348 0.057 Uiso 1 1 calc R U . . .
C46 C 0.2645(3) 0.3755(3) 0.8046(3) 0.0399(9) Uani 1 1 d . . . . .
H46 H 0.2662 0.41 0.8504 0.048 Uiso 1 1 calc R U . . .
C47 C 0.1047(3) 0.4584(3) 0.7603(3) 0.0422(10) Uani 1 1 d . . . . .
H47A H 0.0536 0.4346 0.7949 0.063 Uiso 1 1 calc R U . . .
H47B H 0.0709 0.473 0.7102 0.063 Uiso 1 1 calc R U . . .
H47C H 0.1358 0.5118 0.7832 0.063 Uiso 1 1 calc R U . . .
N1 N 0.3372(2) 0.53913(17) 0.48534(15) 0.0184(5) Uani 1 1 d . . . . .
N2 N 0.2484(2) 0.62102(17) 0.56070(15) 0.0176(5) Uani 1 1 d . . . . .
N3 N 0.39731(19) 0.59832(17) 0.37381(15) 0.0190(5) Uani 1 1 d . . . . .
P1 P 0.21363(6) 0.78505(5) 0.50268(4) 0.01456(15) Uani 1 1 d . . . . .
Rh1 Rh 0.30905(2) 0.70853(2) 0.41765(2) 0.01373(6) Uani 1 1 d . . . . .
I1 I 0.48804(2) 0.75901(2) 0.48562(2) 0.02193(6) Uani 1 1 d . . . . .
I2 I 0.32982(2) 0.82398(2) 0.29689(2) 0.02269(6) Uani 1 1 d . . . . .
I3 I 0.14751(2) 0.63048(2) 0.34502(2) 0.01770(5) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N2 1.326(4) . ?
C1 N1 1.351(4) . ?
C1 Rh1 1.894(3) . ?
C2 C3 1.342(5) . ?
C2 N1 1.403(4) . ?
C2 H2 0.95 . ?
C3 N2 1.403(4) . ?
C3 H3 0.95 . ?
C4 N2 1.462(4) . ?
C4 C11 1.508(4) . ?
C4 P1 1.939(3) . ?
C4 H4 1 . ?
C5 N3 1.347(4) . ?
C5 C6 1.379(4) . ?
C5 N1 1.401(4) . ?
C6 C7 1.382(5) . ?
C6 H6 0.95 . ?
C7 C8 1.379(6) . ?
C7 H7 0.95 . ?
C8 C9 1.385(5) . ?
C8 H8 0.95 . ?
C9 N3 1.337(4) . ?
C9 H9 0.95 . ?
C11 C12 1.389(4) . ?
C11 C16 1.392(5) . ?
C12 C13 1.397(5) . ?
C12 H12 0.95 . ?
C13 C14 1.373(6) . ?
C13 H13 0.95 . ?
C14 C15 1.390(6) . ?
C14 H14 0.95 . ?
C15 C16 1.384(5) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C21 C26 1.395(4) . ?
C21 C22 1.396(4) . ?
C21 P1 1.822(3) . ?
C22 C23 1.389(5) . ?
C22 H22 0.95 . ?
C23 C24 1.382(5) . ?
C23 H23 0.95 . ?
C24 C25 1.390(5) . ?
C24 H24 0.95 . ?
C25 C26 1.383(5) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C31 C32 1.388(4) . ?
C31 C36 1.403(5) . ?
C31 P1 1.814(3) . ?
C32 C33 1.397(5) . ?
C32 H32 0.95 . ?
C33 C34 1.374(5) . ?
C33 H33 0.95 . ?
C34 C35 1.379(5) . ?
C34 H34 0.95 . ?
C35 C36 1.376(5) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C41 C46 1.382(6) . ?
C41 C42 1.405(6) . ?
C41 C47 1.505(6) . ?
C42 C43 1.378(6) . ?
C42 H42 0.95 . ?
C43 C44 1.384(7) . ?
C43 H43 0.95 . ?
C44 C45 1.384(7) . ?
C44 H44 0.95 . ?
C45 C46 1.383(6) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C47 H47A 0.98 . ?
C47 H47B 0.98 . ?
C47 H47C 0.98 . ?
N3 Rh1 2.176(3) . ?
P1 Rh1 2.2769(8) . ?
Rh1 I1 2.6729(3) . ?
Rh1 I3 2.6755(3) . ?
Rh1 I2 2.7450(3) . ?

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
N2 C1 N1 107.9(3) . . ?
N2 C1 Rh1 131.2(2) . . ?
N1 C1 Rh1 120.9(2) . . ?
C3 C2 N1 106.8(3) . . ?
C3 C2 H2 126.6 . . ?
N1 C2 H2 126.6 . . ?
C2 C3 N2 107.3(3) . . ?
C2 C3 H3 126.4 . . ?
N2 C3 H3 126.4 . . ?
N2 C4 C11 110.6(2) . . ?
N2 C4 P1 104.67(19) . . ?
C11 C4 P1 116.5(2) . . ?
N2 C4 H4 108.2 . . ?
C11 C4 H4 108.2 . . ?
P1 C4 H4 108.2 . . ?
N3 C5 C6 124.0(3) . . ?
N3 C5 N1 113.0(3) . . ?
C6 C5 N1 123.0(3) . . ?
C5 C6 C7 116.8(3) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 H6 121.6 . . ?
C8 C7 C6 120.2(3) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.1(3) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
N3 C9 C8 121.7(3) . . ?
N3 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C12 C11 C16 119.4(3) . . ?
C12 C11 C4 119.7(3) . . ?
C16 C11 C4 120.8(3) . . ?
C11 C12 C13 120.0(3) . . ?
C11 C12 H12 120 . . ?
C13 C12 H12 120 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.0(4) . . ?
C13 C14 H14 120 . . ?
C15 C14 H14 120 . . ?
C16 C15 C14 120.2(4) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 120.1(3) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
C26 C21 C22 119.3(3) . . ?
C26 C21 P1 124.0(2) . . ?
C22 C21 P1 116.5(2) . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.1(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.8(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 120.1(3) . . ?
C25 C26 H26 120 . . ?
C21 C26 H26 120 . . ?
C32 C31 C36 119.3(3) . . ?
C32 C31 P1 121.0(2) . . ?
C36 C31 P1 119.4(2) . . ?
C31 C32 C33 119.4(3) . . ?
C31 C32 H32 120.3 . . ?
C33 C32 H32 120.3 . . ?
C34 C33 C32 120.3(3) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C31 120.4(3) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C46 C41 C42 118.0(4) . . ?
C46 C41 C47 121.3(4) . . ?
C42 C41 C47 120.7(4) . . ?
C43 C42 C41 120.8(4) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
C42 C43 C44 119.8(4) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C43 C44 C45 120.5(4) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C46 C45 C44 119.2(5) . . ?
C46 C45 H45 120.4 . . ?
C44 C45 H45 120.4 . . ?
C41 C46 C45 121.7(4) . . ?
C41 C46 H46 119.1 . . ?
C45 C46 H46 119.1 . . ?
C41 C47 H47A 109.5 . . ?
C41 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C41 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C1 N1 C5 116.5(3) . . ?
C1 N1 C2 108.8(3) . . ?
C5 N1 C2 134.8(3) . . ?
C1 N2 C3 109.3(3) . . ?
C1 N2 C4 120.1(2) . . ?
C3 N2 C4 130.5(3) . . ?
C9 N3 C5 118.1(3) . . ?
C9 N3 Rh1 129.1(2) . . ?
C5 N3 Rh1 112.9(2) . . ?
C31 P1 C21 100.15(14) . . ?
C31 P1 C4 106.97(14) . . ?
C21 P1 C4 104.80(14) . . ?
C31 P1 Rh1 122.74(11) . . ?
C21 P1 Rh1 117.48(10) . . ?
C4 P1 Rh1 103.22(10) . . ?
C1 Rh1 N3 76.52(12) . . ?
C1 Rh1 P1 80.78(10) . . ?
N3 Rh1 P1 157.24(7) . . ?
C1 Rh1 I1 89.20(9) . . ?
N3 Rh1 I1 84.95(7) . . ?
P1 Rh1 I1 93.20(2) . . ?
C1 Rh1 I3 86.28(9) . . ?
N3 Rh1 I3 84.93(7) . . ?
P1 Rh1 I3 95.26(2) . . ?
I1 Rh1 I3 169.643(11) . . ?
C1 Rh1 I2 174.88(9) . . ?
N3 Rh1 I2 98.80(7) . . ?
P1 Rh1 I2 103.94(2) . . ?
I1 Rh1 I2 92.474(9) . . ?
I3 Rh1 I2 91.267(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
N1 C2 C3 N2 -0.2(3) . . . . ?
N3 C5 C6 C7 3.1(5) . . . . ?
N1 C5 C6 C7 -176.3(3) . . . . ?
C5 C6 C7 C8 0.0(5) . . . . ?
C6 C7 C8 C9 -2.1(5) . . . . ?
C7 C8 C9 N3 1.3(5) . . . . ?
N2 C4 C11 C12 131.5(3) . . . . ?
P1 C4 C11 C12 -109.1(3) . . . . ?
N2 C4 C11 C16 -49.1(4) . . . . ?
P1 C4 C11 C16 70.2(4) . . . . ?
C16 C11 C12 C13 -2.8(5) . . . . ?
C4 C11 C12 C13 176.6(3) . . . . ?
C11 C12 C13 C14 2.4(6) . . . . ?
C12 C13 C14 C15 -0.5(6) . . . . ?
C13 C14 C15 C16 -1.2(6) . . . . ?
C14 C15 C16 C11 0.8(6) . . . . ?
C12 C11 C16 C15 1.1(5) . . . . ?
C4 C11 C16 C15 -178.2(3) . . . . ?
C26 C21 C22 C23 2.5(5) . . . . ?
P1 C21 C22 C23 177.8(3) . . . . ?
C21 C22 C23 C24 -1.4(5) . . . . ?
C22 C23 C24 C25 -1.1(5) . . . . ?
C23 C24 C25 C26 2.6(5) . . . . ?
C24 C25 C26 C21 -1.5(5) . . . . ?
C22 C21 C26 C25 -1.0(5) . . . . ?
P1 C21 C26 C25 -176.0(3) . . . . ?
C36 C31 C32 C33 -1.5(5) . . . . ?
P1 C31 C32 C33 -175.1(3) . . . . ?
C31 C32 C33 C34 -1.0(5) . . . . ?
C32 C33 C34 C35 1.7(6) . . . . ?
C33 C34 C35 C36 0.0(6) . . . . ?
C34 C35 C36 C31 -2.4(5) . . . . ?
C32 C31 C36 C35 3.2(5) . . . . ?
P1 C31 C36 C35 176.9(3) . . . . ?
C46 C41 C42 C43 -0.4(5) . . . . ?
C47 C41 C42 C43 -178.9(4) . . . . ?
C41 C42 C43 C44 0.4(6) . . . . ?
C42 C43 C44 C45 0.3(6) . . . . ?
C43 C44 C45 C46 -0.9(7) . . . . ?
C42 C41 C46 C45 -0.3(6) . . . . ?
C47 C41 C46 C45 178.3(4) . . . . ?
C44 C45 C46 C41 0.9(7) . . . . ?
N2 C1 N1 C5 179.8(2) . . . . ?
Rh1 C1 N1 C5 2.8(4) . . . . ?
N2 C1 N1 C2 -0.1(3) . . . . ?
Rh1 C1 N1 C2 -177.1(2) . . . . ?
N3 C5 N1 C1 1.8(4) . . . . ?
C6 C5 N1 C1 -178.7(3) . . . . ?
N3 C5 N1 C2 -178.3(3) . . . . ?
C6 C5 N1 C2 1.2(5) . . . . ?
C3 C2 N1 C1 0.2(3) . . . . ?
C3 C2 N1 C5 -179.7(3) . . . . ?
N1 C1 N2 C3 0.0(3) . . . . ?
Rh1 C1 N2 C3 176.5(2) . . . . ?
N1 C1 N2 C4 -177.0(2) . . . . ?
Rh1 C1 N2 C4 -0.5(4) . . . . ?
C2 C3 N2 C1 0.2(3) . . . . ?
C2 C3 N2 C4 176.8(3) . . . . ?
C11 C4 N2 C1 125.4(3) . . . . ?
P1 C4 N2 C1 -0.9(3) . . . . ?
C11 C4 N2 C3 -50.9(4) . . . . ?
P1 C4 N2 C3 -177.2(3) . . . . ?
C8 C9 N3 C5 1.5(5) . . . . ?
C8 C9 N3 Rh1 -178.0(2) . . . . ?
C6 C5 N3 C9 -3.9(5) . . . . ?
N1 C5 N3 C9 175.6(3) . . . . ?
C6 C5 N3 Rh1 175.7(2) . . . . ?
N1 C5 N3 Rh1 -4.8(3) . . . . ?
C32 C31 P1 C21 113.5(3) . . . . ?
C36 C31 P1 C21 -60.1(3) . . . . ?
C32 C31 P1 C4 -137.4(3) . . . . ?
C36 C31 P1 C4 48.9(3) . . . . ?
C32 C31 P1 Rh1 -18.7(3) . . . . ?
C36 C31 P1 Rh1 167.6(2) . . . . ?
C26 C21 P1 C31 87.3(3) . . . . ?
C22 C21 P1 C31 -87.7(3) . . . . ?
C26 C21 P1 C4 -23.4(3) . . . . ?
C22 C21 P1 C4 161.5(2) . . . . ?
C26 C21 P1 Rh1 -137.2(2) . . . . ?
C22 C21 P1 Rh1 47.7(3) . . . . ?
N2 C1 Rh1 N3 179.8(3) . . . . ?
N1 C1 Rh1 N3 -4.1(2) . . . . ?
N2 C1 Rh1 P1 1.4(3) . . . . ?
N1 C1 Rh1 P1 177.5(2) . . . . ?
N2 C1 Rh1 I1 94.8(3) . . . . ?
N1 C1 Rh1 I1 -89.1(2) . . . . ?
N2 C1 Rh1 I3 -94.6(3) . . . . ?
N1 C1 Rh1 I3 81.6(2) . . . . ?

