# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1496354'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;

_audit_creation_date             2015-02-13T11:20:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H36 O4 P2 Rh2'
_chemical_formula_sum            'C20 H36 O4 P2 Rh2'
_chemical_formula_weight         608.25

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

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

_cell_length_a                   9.5370(15)
_cell_length_b                   9.7552(15)
_cell_length_c                   14.656(2)
_cell_angle_alpha                103.267(2)
_cell_angle_beta                 95.938(2)
_cell_angle_gamma                117.358(2)
_cell_volume                     1143.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3908
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      28.8

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

_exptl_crystal_description       prisms
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             616
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_T_max  0.786

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_number            12054
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.905
_reflns_number_total             5799
_reflns_number_gt                4355
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0111P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5799
_refine_ls_number_parameters     257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0862
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.078
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.15

#----------------------------------------------------------------------------#
#                   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'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.84166(4) 0.45007(4) 0.20821(2) 0.01831(9) Uani 1 1 d . . .
Rh2 Rh 1.11174(4) 0.27129(4) 0.27874(2) 0.01782(9) Uani 1 1 d . . .
P1 P 1.24047(12) 0.65016(13) 0.28276(8) 0.0218(2) Uani 1 1 d . . .
P2 P 0.97410(13) 0.22905(13) 0.05964(7) 0.0208(2) Uani 1 1 d . . .
O11 O 1.0762(3) 0.6292(3) 0.2928(2) 0.0269(7) Uani 1 1 d . . .
O12 O 1.2600(3) 0.5027(3) 0.2693(2) 0.0250(7) Uani 1 1 d . . .
C13 C 1.3853(5) 0.8040(6) 0.3929(3) 0.0378(12) Uani 1 1 d . . .
H131 H 1.359 0.7648 0.4481 0.057 Uiso 1 1 calc R . .
H132 H 1.3797 0.9038 0.4012 0.057 Uiso 1 1 calc R . .
H133 H 1.4953 0.8265 0.3888 0.057 Uiso 1 1 calc R . .
C14 C 1.2977(6) 0.7354(6) 0.1886(3) 0.0368(12) Uani 1 1 d . . .
H141 H 1.2954 0.8374 0.2014 0.055 Uiso 1 1 calc R . .
H142 H 1.2214 0.659 0.1268 0.055 Uiso 1 1 calc R . .
H143 H 1.4079 0.7569 0.1856 0.055 Uiso 1 1 calc R . .
O21 O 0.9412(3) 0.3635(3) 0.1046(2) 0.0240(6) Uani 1 1 d . . .
O22 O 1.0583(4) 0.1802(4) 0.12925(19) 0.0290(7) Uani 1 1 d . . .
C23 C 1.0958(5) 0.2911(6) -0.0236(3) 0.0308(10) Uani 1 1 d . . .
H231 H 1.1999 0.3894 0.0112 0.046 Uiso 1 1 calc R . .
H232 H 1.0386 0.3139 -0.0723 0.046 Uiso 1 1 calc R . .
H233 H 1.1158 0.2041 -0.0554 0.046 Uiso 1 1 calc R . .
C24 C 0.7886(5) 0.0484(5) -0.0114(3) 0.0335(11) Uani 1 1 d . . .
H241 H 0.7239 -0.0016 0.0316 0.05 Uiso 1 1 calc R . .
H242 H 0.8144 -0.0284 -0.0511 0.05 Uiso 1 1 calc R . .
H243 H 0.7264 0.0768 -0.0533 0.05 Uiso 1 1 calc R . .
C31 C 0.6150(5) 0.3375(5) 0.1121(3) 0.0292(10) Uani 1 1 d . . .
H31 H 0.616 0.299 0.0429 0.035 Uiso 1 1 calc R . .
C32 C 0.6198(5) 0.2350(5) 0.1666(3) 0.0264(10) Uani 1 1 d . . .
H32 H 0.6233 0.1379 0.1285 0.032 Uiso 1 1 calc R . .
C33 C 0.5372(5) 0.2089(5) 0.2485(3) 0.0307(10) Uani 1 1 d . . .
H331 H 0.5695 0.1452 0.2805 0.037 Uiso 1 1 calc R . .
H332 H 0.4179 0.1446 0.2219 0.037 Uiso 1 1 calc R . .
C34 C 0.5799(5) 0.3685(5) 0.3237(3) 0.0313(11) Uani 1 1 d . . .
H341 H 0.4958 0.3979 0.3084 0.038 Uiso 1 1 calc R . .
H342 H 0.5806 0.3538 0.3883 0.038 Uiso 1 1 calc R . .
C35 C 0.7452(5) 0.5052(5) 0.3255(3) 0.0231(9) Uani 1 1 d . . .
H35 H 0.8248 0.5567 0.3898 0.028 Uiso 1 1 calc R . .
C36 C 0.7658(5) 0.6099(5) 0.2727(3) 0.0292(10) Uani 1 1 d . . .
H36 H 0.8571 0.7233 0.3063 0.035 Uiso 1 1 calc R . .
C37 C 0.6294(5) 0.6004(6) 0.2032(4) 0.0398(13) Uani 1 1 d . . .
H371 H 0.6767 0.6803 0.1683 0.048 Uiso 1 1 calc R . .
H372 H 0.5603 0.629 0.2402 0.048 Uiso 1 1 calc R . .
C38 C 0.5231(5) 0.4278(6) 0.1290(3) 0.0397(13) Uani 1 1 d . . .
H381 H 0.4275 0.3649 0.1529 0.048 Uiso 1 1 calc R . .
H382 H 0.4829 0.437 0.067 0.048 Uiso 1 1 calc R . .
C41 C 0.9231(5) 0.0533(5) 0.2864(3) 0.0288(10) Uani 1 1 d . . .
H41 H 0.8381 -0.0161 0.2246 0.035 Uiso 1 1 calc R . .
C42 C 1.0688(5) 0.0472(5) 0.2885(3) 0.0256(10) Uani 1 1 d . . .
H42 H 1.0668 -0.0262 0.2276 0.031 Uiso 1 1 calc R . .
C43 C 1.1778(6) 0.0630(5) 0.3772(3) 0.0313(11) Uani 1 1 d . . .
H431 H 1.2788 0.0701 0.3613 0.038 Uiso 1 1 calc R . .
H432 H 1.1222 -0.0354 0.3971 0.038 Uiso 1 1 calc R . .
C44 C 1.2214(6) 0.2114(5) 0.4606(3) 0.0327(11) Uani 1 1 d . . .
H441 H 1.1433 0.1799 0.5017 0.039 Uiso 1 1 calc R . .
H442 H 1.3312 0.2523 0.5004 0.039 Uiso 1 1 calc R . .
C45 C 1.2191(5) 0.3456(5) 0.4271(3) 0.0223(9) Uani 1 1 d . . .
H45 H 1.3248 0.4505 0.4503 0.027 Uiso 1 1 calc R . .
C46 C 1.0804(5) 0.3637(5) 0.4136(3) 0.0236(9) Uani 1 1 d . . .
H46 H 1.106 0.4793 0.4292 0.028 Uiso 1 1 calc R . .
C47 C 0.9171(5) 0.2502(6) 0.4284(3) 0.0324(11) Uani 1 1 d . . .
H471 H 0.9268 0.2643 0.4983 0.039 Uiso 1 1 calc R . .
H472 H 0.8366 0.2804 0.4064 0.039 Uiso 1 1 calc R . .
C48 C 0.8556(6) 0.0735(6) 0.3747(3) 0.0373(12) Uani 1 1 d . . .
H481 H 0.7353 0.0153 0.3544 0.045 Uiso 1 1 calc R . .
H482 H 0.8869 0.0236 0.4187 0.045 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   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
Rh1 C32 2.077(4) . ?
Rh1 C31 2.084(4) . ?
Rh1 C36 2.086(4) . ?
Rh1 O21 2.089(3) . ?
Rh1 O11 2.105(3) . ?
Rh1 C35 2.109(4) . ?
Rh2 C42 2.074(4) . ?
Rh2 O22 2.076(3) . ?
Rh2 C46 2.088(4) . ?
Rh2 O12 2.089(3) . ?
Rh2 C41 2.099(4) . ?
Rh2 C45 2.106(4) . ?
P1 O12 1.506(3) . ?
P1 O11 1.512(3) . ?
P1 C14 1.778(4) . ?
P1 C13 1.813(4) . ?
P2 O21 1.509(3) . ?
P2 O22 1.522(3) . ?
P2 C23 1.786(4) . ?
P2 C24 1.797(4) . ?
C13 H131 0.98 . ?
C13 H132 0.98 . ?
C13 H133 0.98 . ?
C14 H141 0.98 . ?
C14 H142 0.98 . ?
C14 H143 0.98 . ?
C23 H231 0.98 . ?
C23 H232 0.98 . ?
C23 H233 0.98 . ?
C24 H241 0.98 . ?
C24 H242 0.98 . ?
C24 H243 0.98 . ?
C31 C32 1.429(6) . ?
C31 C38 1.503(6) . ?
C31 H31 1 . ?
C32 C33 1.509(6) . ?
C32 H32 1 . ?
C33 C34 1.530(6) . ?
C33 H331 0.99 . ?
C33 H332 0.99 . ?
C34 C35 1.519(5) . ?
C34 H341 0.99 . ?
C34 H342 0.99 . ?
C35 C36 1.375(6) . ?
C35 H35 1 . ?
C36 C37 1.520(6) . ?
C36 H36 1 . ?
C37 C38 1.552(6) . ?
C37 H371 0.99 . ?
C37 H372 0.99 . ?
C38 H381 0.99 . ?
C38 H382 0.99 . ?
C41 C42 1.415(6) . ?
C41 C48 1.516(6) . ?
C41 H41 1 . ?
C42 C43 1.509(5) . ?
C42 H42 1 . ?
C43 C44 1.513(6) . ?
C43 H431 0.99 . ?
C43 H432 0.99 . ?
C44 C45 1.508(6) . ?
C44 H441 0.99 . ?
C44 H442 0.99 . ?
C45 C46 1.413(6) . ?
C45 H45 1 . ?
C46 C47 1.515(6) . ?
C46 H46 1 . ?
C47 C48 1.513(6) . ?
C47 H471 0.99 . ?
C47 H472 0.99 . ?
C48 H481 0.99 . ?
C48 H482 0.99 . ?

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
C32 Rh1 C31 40.17(16) . . ?
C32 Rh1 C36 98.82(17) . . ?
C31 Rh1 C36 82.71(18) . . ?
C32 Rh1 O21 94.48(14) . . ?
C31 Rh1 O21 92.68(15) . . ?
C36 Rh1 O21 152.92(15) . . ?
C32 Rh1 O11 157.62(14) . . ?
C31 Rh1 O11 161.30(15) . . ?
C36 Rh1 O11 85.96(14) . . ?
O21 Rh1 O11 90.66(11) . . ?
C32 Rh1 C35 81.78(16) . . ?
C31 Rh1 C35 91.27(16) . . ?
C36 Rh1 C35 38.26(16) . . ?
O21 Rh1 C35 168.71(14) . . ?
O11 Rh1 C35 88.98(13) . . ?
C42 Rh2 O22 89.96(14) . . ?
C42 Rh2 C46 98.59(17) . . ?
O22 Rh2 C46 157.23(14) . . ?
C42 Rh2 O12 152.96(15) . . ?
O22 Rh2 O12 88.65(12) . . ?
C46 Rh2 O12 92.94(14) . . ?
C42 Rh2 C41 39.64(17) . . ?
O22 Rh2 C41 91.60(15) . . ?
C46 Rh2 C41 82.02(17) . . ?
O12 Rh2 C41 167.40(15) . . ?
C42 Rh2 C45 81.89(16) . . ?
O22 Rh2 C45 163.32(14) . . ?
C46 Rh2 C45 39.38(15) . . ?
O12 Rh2 C45 92.03(14) . . ?
C41 Rh2 C45 91.33(16) . . ?
O12 P1 O11 117.19(16) . . ?
O12 P1 C14 110.0(2) . . ?
O11 P1 C14 109.7(2) . . ?
O12 P1 C13 107.86(19) . . ?
O11 P1 C13 106.02(19) . . ?
C14 P1 C13 105.4(2) . . ?
O21 P2 O22 116.16(16) . . ?
O21 P2 C23 107.94(19) . . ?
O22 P2 C23 108.59(19) . . ?
O21 P2 C24 110.81(19) . . ?
O22 P2 C24 107.2(2) . . ?
C23 P2 C24 105.6(2) . . ?
P1 O11 Rh1 129.95(17) . . ?
P1 O12 Rh2 132.57(16) . . ?
P1 C13 H131 109.5 . . ?
P1 C13 H132 109.5 . . ?
H131 C13 H132 109.5 . . ?
P1 C13 H133 109.5 . . ?
H131 C13 H133 109.5 . . ?
H132 C13 H133 109.5 . . ?
P1 C14 H141 109.5 . . ?
P1 C14 H142 109.5 . . ?
H141 C14 H142 109.5 . . ?
P1 C14 H143 109.5 . . ?
H141 C14 H143 109.5 . . ?
H142 C14 H143 109.5 . . ?
P2 O21 Rh1 146.51(18) . . ?
P2 O22 Rh2 124.74(17) . . ?
P2 C23 H231 109.5 . . ?
P2 C23 H232 109.5 . . ?
H231 C23 H232 109.5 . . ?
P2 C23 H233 109.5 . . ?
H231 C23 H233 109.5 . . ?
H232 C23 H233 109.5 . . ?
P2 C24 H241 109.5 . . ?
P2 C24 H242 109.5 . . ?
H241 C24 H242 109.5 . . ?
P2 C24 H243 109.5 . . ?
H241 C24 H243 109.5 . . ?
H242 C24 H243 109.5 . . ?
C32 C31 C38 123.2(4) . . ?
C32 C31 Rh1 69.7(2) . . ?
C38 C31 Rh1 114.2(3) . . ?
C32 C31 H31 114.1 . . ?
C38 C31 H31 114.1 . . ?
Rh1 C31 H31 114.1 . . ?
C31 C32 C33 123.9(4) . . ?
C31 C32 Rh1 70.2(2) . . ?
C33 C32 Rh1 112.9(3) . . ?
C31 C32 H32 114.1 . . ?
C33 C32 H32 114.1 . . ?
Rh1 C32 H32 114.1 . . ?
C32 C33 C34 112.7(4) . . ?
C32 C33 H331 109.1 . . ?
C34 C33 H331 109.1 . . ?
C32 C33 H332 109.1 . . ?
C34 C33 H332 109.1 . . ?
H331 C33 H332 107.8 . . ?
C35 C34 C33 111.3(4) . . ?
C35 C34 H341 109.4 . . ?
C33 C34 H341 109.4 . . ?
C35 C34 H342 109.4 . . ?
C33 C34 H342 109.4 . . ?
H341 C34 H342 108 . . ?
C36 C35 C34 123.3(4) . . ?
C36 C35 Rh1 70.0(2) . . ?
C34 C35 Rh1 114.3(3) . . ?
C36 C35 H35 113.9 . . ?
C34 C35 H35 113.9 . . ?
Rh1 C35 H35 113.9 . . ?
C35 C36 C37 124.9(4) . . ?
C35 C36 Rh1 71.8(2) . . ?
C37 C36 Rh1 111.6(3) . . ?
C35 C36 H36 113.7 . . ?
C37 C36 H36 113.7 . . ?
Rh1 C36 H36 113.7 . . ?
C36 C37 C38 111.5(4) . . ?
C36 C37 H371 109.3 . . ?
C38 C37 H371 109.3 . . ?
C36 C37 H372 109.3 . . ?
C38 C37 H372 109.3 . . ?
H371 C37 H372 108 . . ?
C31 C38 C37 112.4(4) . . ?
C31 C38 H381 109.1 . . ?
C37 C38 H381 109.1 . . ?
C31 C38 H382 109.1 . . ?
C37 C38 H382 109.1 . . ?
H381 C38 H382 107.9 . . ?
C42 C41 C48 123.3(4) . . ?
C42 C41 Rh2 69.2(2) . . ?
C48 C41 Rh2 114.0(3) . . ?
C42 C41 H41 114.2 . . ?
C48 C41 H41 114.2 . . ?
Rh2 C41 H41 114.2 . . ?
C41 C42 C43 125.2(4) . . ?
C41 C42 Rh2 71.2(2) . . ?
C43 C42 Rh2 112.2(3) . . ?
C41 C42 H42 113.6 . . ?
C43 C42 H42 113.6 . . ?
Rh2 C42 H42 113.6 . . ?
C42 C43 C44 112.1(4) . . ?
C42 C43 H431 109.2 . . ?
C44 C43 H431 109.2 . . ?
C42 C43 H432 109.2 . . ?
C44 C43 H432 109.2 . . ?
H431 C43 H432 107.9 . . ?
C45 C44 C43 112.4(3) . . ?
C45 C44 H441 109.1 . . ?
C43 C44 H441 109.1 . . ?
C45 C44 H442 109.1 . . ?
C43 C44 H442 109.1 . . ?
H441 C44 H442 107.8 . . ?
C46 C45 C44 123.2(4) . . ?
C46 C45 Rh2 69.6(2) . . ?
C44 C45 Rh2 113.4(3) . . ?
C46 C45 H45 114.3 . . ?
C44 C45 H45 114.3 . . ?
Rh2 C45 H45 114.3 . . ?
C45 C46 C47 124.5(4) . . ?
C45 C46 Rh2 71.0(2) . . ?
C47 C46 Rh2 111.8(3) . . ?
C45 C46 H46 114 . . ?
C47 C46 H46 114 . . ?
Rh2 C46 H46 114 . . ?
C48 C47 C46 112.9(4) . . ?
C48 C47 H471 109 . . ?
C46 C47 H471 109 . . ?
C48 C47 H472 109 . . ?
C46 C47 H472 109 . . ?
H471 C47 H472 107.8 . . ?
C47 C48 C41 112.1(4) . . ?
C47 C48 H481 109.2 . . ?
C41 C48 H481 109.2 . . ?
C47 C48 H482 109.2 . . ?
C41 C48 H482 109.2 . . ?
H481 C48 H482 107.9 . . ?

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
O12 P1 O11 Rh1 -48.5(3) . . . . ?
C14 P1 O11 Rh1 77.8(3) . . . . ?
C13 P1 O11 Rh1 -168.9(2) . . . . ?
C32 Rh1 O11 P1 93.5(4) . . . . ?
C31 Rh1 O11 P1 -110.3(5) . . . . ?
C36 Rh1 O11 P1 -163.1(3) . . . . ?
O21 Rh1 O11 P1 -10.0(2) . . . . ?
C35 Rh1 O11 P1 158.7(2) . . . . ?
O11 P1 O12 Rh2 -9.2(3) . . . . ?
C14 P1 O12 Rh2 -135.3(2) . . . . ?
C13 P1 O12 Rh2 110.2(3) . . . . ?
C42 Rh2 O12 P1 -165.7(3) . . . . ?
O22 Rh2 O12 P1 107.0(2) . . . . ?
C46 Rh2 O12 P1 -50.3(3) . . . . ?
C41 Rh2 O12 P1 15.7(8) . . . . ?
C45 Rh2 O12 P1 -89.7(3) . . . . ?
O22 P2 O21 Rh1 -51.7(4) . . . . ?
C23 P2 O21 Rh1 -173.9(3) . . . . ?
C24 P2 O21 Rh1 70.9(3) . . . . ?
C32 Rh1 O21 P2 -50.5(3) . . . . ?
C31 Rh1 O21 P2 -90.7(3) . . . . ?
C36 Rh1 O21 P2 -169.9(3) . . . . ?
O11 Rh1 O21 P2 107.7(3) . . . . ?
C35 Rh1 O21 P2 19.6(8) . . . . ?
O21 P2 O22 Rh2 5.2(3) . . . . ?
C23 P2 O22 Rh2 127.1(2) . . . . ?
C24 P2 O22 Rh2 -119.2(2) . . . . ?
C42 Rh2 O22 P2 145.4(2) . . . . ?
C46 Rh2 O22 P2 32.8(5) . . . . ?
O12 Rh2 O22 P2 -61.6(2) . . . . ?
C41 Rh2 O22 P2 105.8(2) . . . . ?
C45 Rh2 O22 P2 -154.2(4) . . . . ?
C36 Rh1 C31 C32 -113.0(3) . . . . ?
O21 Rh1 C31 C32 93.8(3) . . . . ?
O11 Rh1 C31 C32 -166.2(4) . . . . ?
C35 Rh1 C31 C32 -75.6(3) . . . . ?
C32 Rh1 C31 C38 118.3(4) . . . . ?
C36 Rh1 C31 C38 5.3(3) . . . . ?
O21 Rh1 C31 C38 -147.9(3) . . . . ?
O11 Rh1 C31 C38 -47.9(6) . . . . ?
C35 Rh1 C31 C38 42.6(3) . . . . ?
C38 C31 C32 C33 -1.5(6) . . . . ?
Rh1 C31 C32 C33 104.8(4) . . . . ?
C38 C31 C32 Rh1 -106.3(4) . . . . ?
C36 Rh1 C32 C31 67.5(3) . . . . ?
O21 Rh1 C32 C31 -88.8(3) . . . . ?
O11 Rh1 C32 C31 168.4(3) . . . . ?
C35 Rh1 C32 C31 101.9(3) . . . . ?
C31 Rh1 C32 C33 -119.4(4) . . . . ?
C36 Rh1 C32 C33 -51.9(3) . . . . ?
O21 Rh1 C32 C33 151.7(3) . . . . ?
O11 Rh1 C32 C33 49.0(6) . . . . ?
C35 Rh1 C32 C33 -17.5(3) . . . . ?
C31 C32 C33 C34 -51.4(5) . . . . ?
Rh1 C32 C33 C34 29.4(5) . . . . ?
C32 C33 C34 C35 -26.6(5) . . . . ?
C33 C34 C35 C36 93.4(5) . . . . ?
C33 C34 C35 Rh1 12.2(5) . . . . ?
C32 Rh1 C35 C36 -115.7(3) . . . . ?
C31 Rh1 C35 C36 -76.5(3) . . . . ?
O21 Rh1 C35 C36 173.0(6) . . . . ?
O11 Rh1 C35 C36 84.8(2) . . . . ?
C32 Rh1 C35 C34 2.8(3) . . . . ?
C31 Rh1 C35 C34 41.9(3) . . . . ?
C36 Rh1 C35 C34 118.5(4) . . . . ?
O21 Rh1 C35 C34 -68.5(8) . . . . ?
O11 Rh1 C35 C34 -156.8(3) . . . . ?
C34 C35 C36 C37 -2.5(7) . . . . ?
Rh1 C35 C36 C37 104.1(4) . . . . ?
C34 C35 C36 Rh1 -106.6(4) . . . . ?
C32 Rh1 C36 C35 64.5(3) . . . . ?
C31 Rh1 C36 C35 101.4(3) . . . . ?
O21 Rh1 C36 C35 -177.0(2) . . . . ?
O11 Rh1 C36 C35 -93.5(2) . . . . ?
C32 Rh1 C36 C37 -56.7(3) . . . . ?
C31 Rh1 C36 C37 -19.7(3) . . . . ?
O21 Rh1 C36 C37 61.8(5) . . . . ?
O11 Rh1 C36 C37 145.3(3) . . . . ?
C35 Rh1 C36 C37 -121.2(4) . . . . ?
C35 C36 C37 C38 -52.1(6) . . . . ?
Rh1 C36 C37 C38 30.3(5) . . . . ?
C32 C31 C38 C37 90.8(5) . . . . ?
Rh1 C31 C38 C37 10.0(5) . . . . ?
C36 C37 C38 C31 -26.2(5) . . . . ?
O22 Rh2 C41 C42 88.0(2) . . . . ?
C46 Rh2 C41 C42 -113.9(3) . . . . ?
O12 Rh2 C41 C42 179.0(5) . . . . ?
C45 Rh2 C41 C42 -75.6(3) . . . . ?
C42 Rh2 C41 C48 118.3(4) . . . . ?
O22 Rh2 C41 C48 -153.7(3) . . . . ?
C46 Rh2 C41 C48 4.4(3) . . . . ?
O12 Rh2 C41 C48 -62.7(8) . . . . ?
C45 Rh2 C41 C48 42.7(3) . . . . ?
C48 C41 C42 C43 -1.3(6) . . . . ?
Rh2 C41 C42 C43 104.4(4) . . . . ?
C48 C41 C42 Rh2 -105.7(4) . . . . ?
O22 Rh2 C42 C41 -92.6(2) . . . . ?
C46 Rh2 C42 C41 66.3(3) . . . . ?
O12 Rh2 C42 C41 -179.5(3) . . . . ?
C45 Rh2 C42 C41 102.1(3) . . . . ?
O22 Rh2 C42 C43 146.2(3) . . . . ?
C46 Rh2 C42 C43 -55.0(3) . . . . ?
O12 Rh2 C42 C43 59.3(5) . . . . ?
C41 Rh2 C42 C43 -121.2(4) . . . . ?
C45 Rh2 C42 C43 -19.2(3) . . . . ?
C41 C42 C43 C44 -51.0(6) . . . . ?
Rh2 C42 C43 C44 31.0(5) . . . . ?
C42 C43 C44 C45 -27.5(6) . . . . ?
C43 C44 C45 C46 91.9(5) . . . . ?
C43 C44 C45 Rh2 11.7(5) . . . . ?
C42 Rh2 C45 C46 -114.3(3) . . . . ?
O22 Rh2 C45 C46 -175.8(4) . . . . ?
O12 Rh2 C45 C46 92.2(2) . . . . ?
C41 Rh2 C45 C46 -75.7(3) . . . . ?
C42 Rh2 C45 C44 4.1(3) . . . . ?
O22 Rh2 C45 C44 -57.4(6) . . . . ?
C46 Rh2 C45 C44 118.4(4) . . . . ?
O12 Rh2 C45 C44 -149.4(3) . . . . ?
C41 Rh2 C45 C44 42.7(3) . . . . ?
C44 C45 C46 C47 -1.4(6) . . . . ?
Rh2 C45 C46 C47 103.8(4) . . . . ?
C44 C45 C46 Rh2 -105.3(4) . . . . ?
C42 Rh2 C46 C45 65.9(3) . . . . ?
O22 Rh2 C46 C45 176.9(3) . . . . ?
O12 Rh2 C46 C45 -89.6(2) . . . . ?
C41 Rh2 C46 C45 102.0(3) . . . . ?
C42 Rh2 C46 C47 -54.7(3) . . . . ?
O22 Rh2 C46 C47 56.3(5) . . . . ?
O12 Rh2 C46 C47 149.9(3) . . . . ?
C41 Rh2 C46 C47 -18.5(3) . . . . ?
C45 Rh2 C46 C47 -120.5(4) . . . . ?
C45 C46 C47 C48 -51.5(6) . . . . ?
Rh2 C46 C47 C48 29.8(5) . . . . ?
C46 C47 C48 C41 -26.2(5) . . . . ?
C42 C41 C48 C47 90.7(5) . . . . ?
Rh2 C41 C48 C47 10.7(5) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1496355'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;

_audit_creation_date             2015-10-27T12:17:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C31 H42 N2 O4 P Rh'
_chemical_formula_sum            'C31 H42 N2 O4 P Rh'
_chemical_formula_weight         640.55
_chemical_absolute_configuration ad

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121
loop_
_symmetry_equiv_pos_as_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                   10.5240(14)
_cell_length_b                   15.865(2)
_cell_length_c                   19.108(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3190.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9911
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      29.5

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

_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_T_max  0.911

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_number            42996
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         29.69
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.952
_reflns_number_total             8401
_reflns_number_gt                7828
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8401
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0585
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881, 3610 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.006(14)
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.33
_refine_diff_density_rms         0.058

#----------------------------------------------------------------------------#
#                   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'
H H 0 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.336857(14) 0.265547(9) 0.219742(7) 0.01553(4) Uani 1 1 d . . .
C1 C 0.3269(2) 0.29337(12) 0.12767(10) 0.0222(4) Uani 1 1 d . . .
O1 O 0.31547(16) 0.31406(11) 0.07078(7) 0.0321(4) Uani 1 1 d . . .
C2 C 0.2619(2) 0.15931(13) 0.19666(11) 0.0237(4) Uani 1 1 d . . .
O2 O 0.22264(18) 0.09987(10) 0.17115(8) 0.0356(4) Uani 1 1 d . . .
N11 N 0.37415(14) 0.45716(10) 0.25000(8) 0.0146(3) Uani 1 1 d . . .
C12 C 0.42464(17) 0.38128(11) 0.23159(9) 0.0139(4) Uani 1 1 d . . .
N13 N 0.54354(14) 0.39960(9) 0.20906(8) 0.0139(3) Uani 1 1 d . . .
C14 C 0.56764(18) 0.48561(11) 0.21265(10) 0.0168(4) Uani 1 1 d . . .
H14 H 0.644 0.5135 0.1997 0.02 Uiso 1 1 calc R . .
C15 C 0.46162(18) 0.52140(12) 0.23797(9) 0.0175(4) Uani 1 1 d . . .
H15 H 0.4486 0.5798 0.2462 0.021 Uiso 1 1 calc R . .
C21 C 0.25818(17) 0.46856(11) 0.28907(10) 0.0154(4) Uani 1 1 d . . .
C22 C 0.27063(19) 0.48103(12) 0.36177(10) 0.0178(4) Uani 1 1 d . . .
C221 C 0.3986(2) 0.47991(13) 0.39897(10) 0.0204(4) Uani 1 1 d . . .
H221 H 0.4662 0.4727 0.3627 0.024 Uiso 1 1 calc R . .
C222 C 0.4064(2) 0.40508(14) 0.44925(10) 0.0269(5) Uani 1 1 d . . .
H222 H 0.3979 0.3524 0.4228 0.04 Uiso 1 1 calc R . .
H223 H 0.3377 0.409 0.4837 0.04 Uiso 1 1 calc R . .
H224 H 0.4886 0.4058 0.4734 0.04 Uiso 1 1 calc R . .
C223 C 0.4229(2) 0.56395(14) 0.43691(12) 0.0306(5) Uani 1 1 d . . .
H225 H 0.4187 0.6104 0.4032 0.046 Uiso 1 1 calc R . .
H226 H 0.5073 0.5628 0.4586 0.046 Uiso 1 1 calc R . .
H227 H 0.3583 0.5722 0.4732 0.046 Uiso 1 1 calc R . .
C23 C 0.1590(2) 0.49318(12) 0.39973(9) 0.0205(4) Uani 1 1 d . . .
H23 H 0.1638 0.5008 0.449 0.025 Uiso 1 1 calc R . .
C24 C 0.0416(2) 0.49433(13) 0.36738(11) 0.0218(4) Uani 1 1 d . . .
H24 H -0.0331 0.5029 0.3943 0.026 Uiso 1 1 calc R . .
C25 C 0.03284(19) 0.48298(13) 0.29537(10) 0.0208(4) Uani 1 1 d . . .
H25 H -0.0481 0.4847 0.2734 0.025 Uiso 1 1 calc R . .
C26 C 0.14108(18) 0.46915(12) 0.25503(10) 0.0159(4) Uani 1 1 d . . .
C261 C 0.12698(19) 0.45629(13) 0.17627(10) 0.0179(4) Uani 1 1 d . . .
H261 H 0.2122 0.4412 0.1568 0.021 Uiso 1 1 calc R . .
C262 C 0.0826(2) 0.53773(14) 0.14066(11) 0.0270(5) Uani 1 1 d . . .
H262 H 0.0718 0.5277 0.0904 0.04 Uiso 1 1 calc R . .
H263 H 0.1461 0.582 0.1479 0.04 Uiso 1 1 calc R . .
H264 H 0.0013 0.5555 0.1609 0.04 Uiso 1 1 calc R . .
C263 C 0.0353(2) 0.38411(14) 0.15996(11) 0.0255(5) Uani 1 1 d . . .
H265 H 0.0621 0.3334 0.1852 0.038 Uiso 1 1 calc R . .
H266 H 0.0358 0.3729 0.1095 0.038 Uiso 1 1 calc R . .
H267 H -0.0507 0.3998 0.1747 0.038 Uiso 1 1 calc R . .
C31 C 0.63692(17) 0.33571(12) 0.19323(10) 0.0151(4) Uani 1 1 d . . .
C32 C 0.68745(18) 0.28929(12) 0.24971(10) 0.0177(4) Uani 1 1 d . . .
C321 C 0.6516(2) 0.30901(12) 0.32560(9) 0.0190(4) Uani 1 1 d . . .
H321 H 0.561 0.3281 0.3261 0.023 Uiso 1 1 calc R . .
C322 C 0.6626(2) 0.23326(13) 0.37469(9) 0.0250(4) Uani 1 1 d . . .
H322 H 0.6172 0.1851 0.3545 0.037 Uiso 1 1 calc R . .
H323 H 0.6254 0.2474 0.4202 0.037 Uiso 1 1 calc R . .
H324 H 0.7524 0.2186 0.3809 0.037 Uiso 1 1 calc R . .
C323 C 0.7336(2) 0.38186(13) 0.35276(11) 0.0256(5) Uani 1 1 d . . .
H325 H 0.7221 0.4312 0.3226 0.038 Uiso 1 1 calc R . .
H326 H 0.8232 0.365 0.3524 0.038 Uiso 1 1 calc R . .
H327 H 0.7081 0.3959 0.4007 0.038 Uiso 1 1 calc R . .
C33 C 0.77710(18) 0.22735(13) 0.23430(10) 0.0218(4) Uani 1 1 d . . .
H33 H 0.813 0.195 0.2712 0.026 Uiso 1 1 calc R . .
C34 C 0.81478(19) 0.21228(12) 0.16570(10) 0.0225(4) Uani 1 1 d . . .
H34 H 0.8752 0.1694 0.1561 0.027 Uiso 1 1 calc R . .
C35 C 0.76468(18) 0.25949(13) 0.11129(10) 0.0207(4) Uani 1 1 d . . .
H35 H 0.7923 0.2493 0.0647 0.025 Uiso 1 1 calc R . .
C36 C 0.67418(19) 0.32180(11) 0.12408(9) 0.0163(4) Uani 1 1 d . . .
C361 C 0.6229(2) 0.37381(13) 0.06332(10) 0.0193(4) Uani 1 1 d . . .
H361 H 0.5456 0.4046 0.0799 0.023 Uiso 1 1 calc R . .
C362 C 0.7224(2) 0.43955(14) 0.04081(11) 0.0294(5) Uani 1 1 d . . .
H362 H 0.7396 0.4779 0.0799 0.044 Uiso 1 1 calc R . .
H363 H 0.6899 0.4718 0.0009 0.044 Uiso 1 1 calc R . .
H364 H 0.8011 0.4108 0.0273 0.044 Uiso 1 1 calc R . .
C363 C 0.5849(2) 0.31918(14) 0.00040(10) 0.0281(5) Uani 1 1 d . . .
H365 H 0.537 0.27 0.0168 0.042 Uiso 1 1 calc R . .
H366 H 0.6615 0.3003 -0.0242 0.042 Uiso 1 1 calc R . .
H367 H 0.5319 0.3523 -0.0316 0.042 Uiso 1 1 calc R . .
P41 P 0.25013(6) 0.18859(3) 0.36474(3) 0.02304(12) Uani 1 1 d . . .
O41 O 0.34288(14) 0.24726(8) 0.32583(6) 0.0223(3) Uani 1 1 d . . .
O42 O 0.21806(14) 0.10738(9) 0.33001(8) 0.0245(3) Uani 1 1 d . . .
C43 C 0.1081(3) 0.24846(14) 0.38151(17) 0.0459(7) Uani 1 1 d . . .
H431 H 0.0622 0.2574 0.3375 0.069 Uiso 1 1 calc R . .
H432 H 0.131 0.3031 0.4019 0.069 Uiso 1 1 calc R . .
H433 H 0.0538 0.2175 0.4143 0.069 Uiso 1 1 calc R . .
C44 C 0.3223(3) 0.17001(15) 0.44897(11) 0.0401(6) Uani 1 1 d . . .
H441 H 0.4034 0.1406 0.4426 0.06 Uiso 1 1 calc R . .
H442 H 0.2655 0.1353 0.4776 0.06 Uiso 1 1 calc R . .
H443 H 0.3372 0.224 0.4725 0.06 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   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
Rh1 C1 1.8169(19) . ?
Rh1 C2 1.913(2) . ?
Rh1 O41 2.0488(13) . ?
Rh1 C12 2.0679(18) . ?
C1 O1 1.142(2) . ?
C2 O2 1.139(3) . ?
N11 C12 1.362(2) . ?
N11 C15 1.393(2) . ?
N11 C21 1.442(2) . ?
C12 N13 1.355(2) . ?
N13 C14 1.390(2) . ?
N13 C31 1.444(2) . ?
C14 C15 1.342(3) . ?
C14 H14 0.95 . ?
C15 H15 0.95 . ?
C21 C26 1.394(3) . ?
C21 C22 1.409(3) . ?
C22 C23 1.394(3) . ?
C22 C221 1.523(3) . ?
C221 C222 1.529(3) . ?
C221 C223 1.539(3) . ?
C221 H221 1 . ?
C222 H222 0.98 . ?
C222 H223 0.98 . ?
C222 H224 0.98 . ?
C223 H225 0.98 . ?
C223 H226 0.98 . ?
C223 H227 0.98 . ?
C23 C24 1.382(3) . ?
C23 H23 0.95 . ?
C24 C25 1.391(3) . ?
C24 H24 0.95 . ?
C25 C26 1.393(3) . ?
C25 H25 0.95 . ?
C26 C261 1.526(2) . ?
C261 C263 1.529(3) . ?
C261 C262 1.533(3) . ?
C261 H261 1 . ?
C262 H262 0.98 . ?
C262 H263 0.98 . ?
C262 H264 0.98 . ?
C263 H265 0.98 . ?
C263 H266 0.98 . ?
C263 H267 0.98 . ?
C31 C36 1.396(2) . ?
C31 C32 1.411(3) . ?
C32 C33 1.394(3) . ?
C32 C321 1.531(3) . ?
C321 C322 1.529(3) . ?
C321 C323 1.533(3) . ?
C321 H321 1 . ?
C322 H322 0.98 . ?
C322 H323 0.98 . ?
C322 H324 0.98 . ?
C323 H325 0.98 . ?
C323 H326 0.98 . ?
C323 H327 0.98 . ?
C33 C34 1.390(3) . ?
C33 H33 0.95 . ?
C34 C35 1.386(3) . ?
C34 H34 0.95 . ?
C35 C36 1.394(3) . ?
C35 H35 0.95 . ?
C36 C361 1.523(3) . ?
C361 C363 1.535(3) . ?
C361 C362 1.540(3) . ?
C361 H361 1 . ?
C362 H362 0.98 . ?
C362 H363 0.98 . ?
C362 H364 0.98 . ?
C363 H365 0.98 . ?
C363 H366 0.98 . ?
C363 H367 0.98 . ?
P41 O42 1.4881(15) . ?
P41 O41 1.5401(14) . ?
P41 C43 1.800(2) . ?
P41 C44 1.804(2) . ?
C43 H431 0.98 . ?
C43 H432 0.98 . ?
C43 H433 0.98 . ?
C44 H441 0.98 . ?
C44 H442 0.98 . ?
C44 H443 0.98 . ?

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 Rh1 C2 88.11(9) . . ?
C1 Rh1 O41 173.87(8) . . ?
C2 Rh1 O41 96.67(7) . . ?
C1 Rh1 C12 85.18(8) . . ?
C2 Rh1 C12 172.77(8) . . ?
O41 Rh1 C12 90.21(6) . . ?
O1 C1 Rh1 176.1(2) . . ?
O2 C2 Rh1 167.92(18) . . ?
C12 N11 C15 110.26(15) . . ?
C12 N11 C21 125.08(15) . . ?
C15 N11 C21 123.59(15) . . ?
N13 C12 N11 104.65(15) . . ?
N13 C12 Rh1 124.63(13) . . ?
N11 C12 Rh1 129.70(13) . . ?
C12 N13 C14 111.32(15) . . ?
C12 N13 C31 123.00(15) . . ?
C14 N13 C31 125.13(15) . . ?
C15 C14 N13 106.35(16) . . ?
C15 C14 H14 126.8 . . ?
N13 C14 H14 126.8 . . ?
C14 C15 N11 107.43(16) . . ?
C14 C15 H15 126.3 . . ?
N11 C15 H15 126.3 . . ?
C26 C21 C22 122.78(17) . . ?
C26 C21 N11 120.50(16) . . ?
C22 C21 N11 116.69(16) . . ?
C23 C22 C21 117.00(17) . . ?
C23 C22 C221 120.25(16) . . ?
C21 C22 C221 122.74(17) . . ?
C22 C221 C222 110.47(17) . . ?
C22 C221 C223 110.91(17) . . ?
C222 C221 C223 111.57(17) . . ?
C22 C221 H221 107.9 . . ?
C222 C221 H221 107.9 . . ?
C223 C221 H221 107.9 . . ?
C221 C222 H222 109.5 . . ?
C221 C222 H223 109.5 . . ?
H222 C222 H223 109.5 . . ?
C221 C222 H224 109.5 . . ?
H222 C222 H224 109.5 . . ?
H223 C222 H224 109.5 . . ?
C221 C223 H225 109.5 . . ?
C221 C223 H226 109.5 . . ?
H225 C223 H226 109.5 . . ?
C221 C223 H227 109.5 . . ?
H225 C223 H227 109.5 . . ?
H226 C223 H227 109.5 . . ?
C24 C23 C22 121.51(17) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 120.01(18) . . ?
C23 C24 H24 120 . . ?
C25 C24 H24 120 . . ?
C24 C25 C26 120.91(18) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C21 117.77(17) . . ?
C25 C26 C261 119.17(17) . . ?
C21 C26 C261 123.06(17) . . ?
C26 C261 C263 111.25(17) . . ?
C26 C261 C262 110.77(17) . . ?
C263 C261 C262 110.37(17) . . ?
C26 C261 H261 108.1 . . ?
C263 C261 H261 108.1 . . ?
C262 C261 H261 108.1 . . ?
C261 C262 H262 109.5 . . ?
C261 C262 H263 109.5 . . ?
H262 C262 H263 109.5 . . ?
C261 C262 H264 109.5 . . ?
H262 C262 H264 109.5 . . ?
H263 C262 H264 109.5 . . ?
C261 C263 H265 109.5 . . ?
C261 C263 H266 109.5 . . ?
H265 C263 H266 109.5 . . ?
C261 C263 H267 109.5 . . ?
H265 C263 H267 109.5 . . ?
H266 C263 H267 109.5 . . ?
C36 C31 C32 122.40(17) . . ?
C36 C31 N13 120.02(17) . . ?
C32 C31 N13 117.57(16) . . ?
C33 C32 C31 117.49(17) . . ?
C33 C32 C321 120.75(17) . . ?
C31 C32 C321 121.67(16) . . ?
C322 C321 C32 113.68(16) . . ?
C322 C321 C323 109.99(16) . . ?
C32 C321 C323 109.61(17) . . ?
C322 C321 H321 107.8 . . ?
C32 C321 H321 107.8 . . ?
C323 C321 H321 107.8 . . ?
C321 C322 H322 109.5 . . ?
C321 C322 H323 109.5 . . ?
H322 C322 H323 109.5 . . ?
C321 C322 H324 109.5 . . ?
H322 C322 H324 109.5 . . ?
H323 C322 H324 109.5 . . ?
C321 C323 H325 109.5 . . ?
C321 C323 H326 109.5 . . ?
H325 C323 H326 109.5 . . ?
C321 C323 H327 109.5 . . ?
H325 C323 H327 109.5 . . ?
H326 C323 H327 109.5 . . ?
C34 C33 C32 120.90(18) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C35 C34 C33 120.40(18) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.78(18) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C31 118.02(17) . . ?
C35 C36 C361 119.51(16) . . ?
C31 C36 C361 122.44(17) . . ?
C36 C361 C363 112.55(17) . . ?
C36 C361 C362 109.79(17) . . ?
C363 C361 C362 109.94(17) . . ?
C36 C361 H361 108.1 . . ?
C363 C361 H361 108.1 . . ?
C362 C361 H361 108.1 . . ?
C361 C362 H362 109.5 . . ?
C361 C362 H363 109.5 . . ?
H362 C362 H363 109.5 . . ?
C361 C362 H364 109.5 . . ?
H362 C362 H364 109.5 . . ?
H363 C362 H364 109.5 . . ?
C361 C363 H365 109.5 . . ?
C361 C363 H366 109.5 . . ?
H365 C363 H366 109.5 . . ?
C361 C363 H367 109.5 . . ?
H365 C363 H367 109.5 . . ?
H366 C363 H367 109.5 . . ?
O42 P41 O41 116.86(8) . . ?
O42 P41 C43 110.37(11) . . ?
O41 P41 C43 107.06(10) . . ?
O42 P41 C44 110.60(10) . . ?
O41 P41 C44 105.23(10) . . ?
C43 P41 C44 106.08(14) . . ?
P41 O41 Rh1 122.93(8) . . ?
P41 C43 H431 109.5 . . ?
P41 C43 H432 109.5 . . ?
H431 C43 H432 109.5 . . ?
P41 C43 H433 109.5 . . ?
H431 C43 H433 109.5 . . ?
H432 C43 H433 109.5 . . ?
P41 C44 H441 109.5 . . ?
P41 C44 H442 109.5 . . ?
H441 C44 H442 109.5 . . ?
P41 C44 H443 109.5 . . ?
H441 C44 H443 109.5 . . ?
H442 C44 H443 109.5 . . ?

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
C1 Rh1 C2 O2 15.2(10) . . . . ?
O41 Rh1 C2 O2 -168.6(10) . . . . ?
C15 N11 C12 N13 0.65(19) . . . . ?
C21 N11 C12 N13 -167.83(15) . . . . ?
C15 N11 C12 Rh1 -167.97(13) . . . . ?
C21 N11 C12 Rh1 23.6(2) . . . . ?
C1 Rh1 C12 N13 -71.60(16) . . . . ?
O41 Rh1 C12 N13 112.45(15) . . . . ?
C1 Rh1 C12 N11 94.98(17) . . . . ?
O41 Rh1 C12 N11 -80.97(16) . . . . ?
N11 C12 N13 C14 -0.4(2) . . . . ?
Rh1 C12 N13 C14 168.93(13) . . . . ?
N11 C12 N13 C31 171.43(15) . . . . ?
Rh1 C12 N13 C31 -19.2(2) . . . . ?
C12 N13 C14 C15 0.1(2) . . . . ?
C31 N13 C14 C15 -171.60(16) . . . . ?
N13 C14 C15 N11 0.3(2) . . . . ?
C12 N11 C15 C14 -0.6(2) . . . . ?
C21 N11 C15 C14 168.04(16) . . . . ?
C12 N11 C21 C26 -85.0(2) . . . . ?
C15 N11 C21 C26 108.0(2) . . . . ?
C12 N11 C21 C22 96.6(2) . . . . ?
C15 N11 C21 C22 -70.4(2) . . . . ?
C26 C21 C22 C23 0.9(3) . . . . ?
N11 C21 C22 C23 179.19(16) . . . . ?
C26 C21 C22 C221 179.67(17) . . . . ?
N11 C21 C22 C221 -2.0(3) . . . . ?
C23 C22 C221 C222 64.3(2) . . . . ?
C21 C22 C221 C222 -114.4(2) . . . . ?
C23 C22 C221 C223 -59.9(2) . . . . ?
C21 C22 C221 C223 121.3(2) . . . . ?
C21 C22 C23 C24 -1.0(3) . . . . ?
C221 C22 C23 C24 -179.88(19) . . . . ?
C22 C23 C24 C25 0.2(3) . . . . ?
C23 C24 C25 C26 0.9(3) . . . . ?
C24 C25 C26 C21 -1.1(3) . . . . ?
C24 C25 C26 C261 179.49(18) . . . . ?
C22 C21 C26 C25 0.2(3) . . . . ?
N11 C21 C26 C25 -178.08(17) . . . . ?
C22 C21 C26 C261 179.57(18) . . . . ?
N11 C21 C26 C261 1.3(3) . . . . ?
C25 C26 C261 C263 -55.4(2) . . . . ?
C21 C26 C261 C263 125.20(19) . . . . ?
C25 C26 C261 C262 67.7(2) . . . . ?
C21 C26 C261 C262 -111.6(2) . . . . ?
C12 N13 C31 C36 110.5(2) . . . . ?
C14 N13 C31 C36 -78.8(2) . . . . ?
C12 N13 C31 C32 -69.6(2) . . . . ?
C14 N13 C31 C32 101.1(2) . . . . ?
C36 C31 C32 C33 -0.4(3) . . . . ?
N13 C31 C32 C33 179.68(16) . . . . ?
C36 C31 C32 C321 176.20(18) . . . . ?
N13 C31 C32 C321 -3.7(3) . . . . ?
C33 C32 C321 C322 -30.0(3) . . . . ?
C31 C32 C321 C322 153.51(18) . . . . ?
C33 C32 C321 C323 93.5(2) . . . . ?
C31 C32 C321 C323 -82.9(2) . . . . ?
C31 C32 C33 C34 0.0(3) . . . . ?
C321 C32 C33 C34 -176.64(19) . . . . ?
C32 C33 C34 C35 0.8(3) . . . . ?
C33 C34 C35 C36 -1.1(3) . . . . ?
C34 C35 C36 C31 0.7(3) . . . . ?
C34 C35 C36 C361 178.79(18) . . . . ?
C32 C31 C36 C35 0.0(3) . . . . ?
N13 C31 C36 C35 179.96(16) . . . . ?
C32 C31 C36 C361 -177.97(18) . . . . ?
N13 C31 C36 C361 2.0(3) . . . . ?
C35 C36 C361 C363 47.0(2) . . . . ?
C31 C36 C361 C363 -135.1(2) . . . . ?
C35 C36 C361 C362 -75.8(2) . . . . ?
C31 C36 C361 C362 102.1(2) . . . . ?
O42 P41 O41 Rh1 40.28(13) . . . . ?
C43 P41 O41 Rh1 -84.02(14) . . . . ?
C44 P41 O41 Rh1 163.42(11) . . . . ?
C2 Rh1 O41 P41 -26.52(12) . . . . ?
C12 Rh1 O41 P41 155.71(10) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1496356'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;

_audit_creation_date             2016-02-15T13:16:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C60 H84 N4 O6 P2 Rh2, 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H88 Cl4 N4 O6 P2 Rh2'
_chemical_formula_weight         1394.92

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.7954(8)
_cell_length_b                   17.1516(10)
_cell_length_c                   16.0830(10)
_cell_angle_alpha                90
_cell_angle_beta                 107.3960(10)
_cell_angle_gamma                90
_cell_volume                     3368.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5375
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      21.03

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

_exptl_crystal_description       prisms
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_T_max  0.894

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_number            82380
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.957
_reflns_number_total             8426
_reflns_number_gt                5954
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0238P)²+3.5643P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8426
_refine_ls_number_parameters     371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.089
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.101

#----------------------------------------------------------------------------#
#                   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'
H H 0 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.688001(19) 0.519631(14) 0.620889(15) 0.01924(7) Uani 1 1 d . . .
C1 C 0.7980(2) 0.57372(19) 0.60194(19) 0.0249(7) Uani 1 1 d . . .
O1 O 0.86384(19) 0.61122(14) 0.58458(15) 0.0354(6) Uani 1 1 d . . .
N11 N 0.80361(19) 0.47978(14) 0.80953(15) 0.0201(5) Uani 1 1 d . . .
C12 C 0.7841(2) 0.46482(17) 0.72307(19) 0.0194(6) Uani 1 1 d . . .
N13 N 0.8360(2) 0.39605(14) 0.72135(16) 0.0200(5) Uani 1 1 d . . .
C14 C 0.8867(3) 0.36912(18) 0.8051(2) 0.0250(7) Uani 1 1 d . . .
H14 H 0.9276 0.3223 0.8205 0.03 Uiso 1 1 calc R . .
C15 C 0.8670(3) 0.42144(18) 0.8600(2) 0.0255(7) Uani 1 1 d . . .
H15 H 0.8918 0.4192 0.9218 0.031 Uiso 1 1 calc R . .
C21 C 0.7804(3) 0.55231(18) 0.84744(19) 0.0251(7) Uani 1 1 d . . .
C22 C 0.6902(3) 0.55610(18) 0.8790(2) 0.0259(7) Uani 1 1 d . . .
C23 C 0.6806(3) 0.6242(2) 0.9240(2) 0.0348(8) Uani 1 1 d . . .
H23 H 0.6212 0.6291 0.9476 0.042 Uiso 1 1 calc R . .
C24 C 0.7545(3) 0.6841(2) 0.9351(2) 0.0410(9) Uani 1 1 d . . .
H24 H 0.7462 0.7292 0.9667 0.049 Uiso 1 1 calc R . .
C25 C 0.8410(3) 0.6792(2) 0.9006(2) 0.0364(9) Uani 1 1 d . . .
H25 H 0.8904 0.7217 0.9074 0.044 Uiso 1 1 calc R . .
C26 C 0.8567(3) 0.61283(19) 0.8561(2) 0.0276(7) Uani 1 1 d . . .
C31 C 0.8489(3) 0.36066(17) 0.64330(19) 0.0214(6) Uani 1 1 d . . .
C32 C 0.9399(3) 0.38256(18) 0.6179(2) 0.0249(7) Uani 1 1 d . . .
C33 C 0.9490(3) 0.34943(19) 0.5410(2) 0.0302(8) Uani 1 1 d . . .
H33 H 1.0094 0.3629 0.521 0.036 Uiso 1 1 calc R . .
C34 C 0.8711(3) 0.29712(19) 0.4934(2) 0.0321(8) Uani 1 1 d . . .
H34 H 0.8778 0.2759 0.4406 0.039 Uiso 1 1 calc R . .
C35 C 0.7843(3) 0.27585(19) 0.5222(2) 0.0306(8) Uani 1 1 d . . .
H35 H 0.7321 0.2396 0.4891 0.037 Uiso 1 1 calc R . .
C36 C 0.7711(3) 0.30615(18) 0.5985(2) 0.0243(7) Uani 1 1 d . . .
P41 P 0.43787(6) 0.45572(5) 0.58288(5) 0.02189(18) Uani 1 1 d . . .
O41 O 0.55577(16) 0.45985(12) 0.64114(13) 0.0246(5) Uani 1 1 d . . .
O42 O 0.42465(16) 0.43026(12) 0.48970(13) 0.0221(5) Uani 1 1 d . . .
C43 C 0.3693(3) 0.54695(18) 0.5844(2) 0.0255(7) Uani 1 1 d . . .
H431 H 0.4017 0.5872 0.5566 0.038 Uiso 1 1 calc R . .
H432 H 0.3776 0.5619 0.6448 0.038 Uiso 1 1 calc R . .
H433 H 0.2914 0.5414 0.5526 0.038 Uiso 1 1 calc R . .
C44 C 0.3690(3) 0.38650(19) 0.6318(2) 0.0288(7) Uani 1 1 d . . .
H441 H 0.405 0.3356 0.6355 0.043 Uiso 1 1 calc R . .
H442 H 0.2924 0.3819 0.5961 0.043 Uiso 1 1 calc R . .
H443 H 0.3722 0.4042 0.6904 0.043 Uiso 1 1 calc R . .
C221 C 0.6094(3) 0.4900(2) 0.8681(2) 0.0299(7) Uani 1 1 d . . .
H221 H 0.6177 0.4555 0.8203 0.036 Uiso 1 1 calc R . .
C222 C 0.6337(3) 0.4416(2) 0.9510(3) 0.0486(10) Uani 1 1 d . . .
H222 H 0.7074 0.4194 0.9643 0.073 Uiso 1 1 calc R . .
H223 H 0.5799 0.3993 0.9427 0.073 Uiso 1 1 calc R . .
H224 H 0.6292 0.4748 0.9994 0.073 Uiso 1 1 calc R . .
C223 C 0.4914(3) 0.5192(2) 0.8423(2) 0.0425(9) Uani 1 1 d . . .
H225 H 0.4774 0.5519 0.7901 0.064 Uiso 1 1 calc R . .
H226 H 0.4798 0.5499 0.8902 0.064 Uiso 1 1 calc R . .
H227 H 0.4413 0.4746 0.8301 0.064 Uiso 1 1 calc R . .
C261 C 0.9526(3) 0.6072(2) 0.8196(2) 0.0290(8) Uani 1 1 d . . .
H261 H 0.9341 0.5663 0.7731 0.035 Uiso 1 1 calc R . .
C262 C 0.9733(3) 0.6829(2) 0.7774(2) 0.0354(8) Uani 1 1 d . . .
H262 H 0.9044 0.7018 0.7372 0.053 Uiso 1 1 calc R . .
H263 H 1.0261 0.6735 0.7452 0.053 Uiso 1 1 calc R . .
H264 H 1.0028 0.7221 0.8226 0.053 Uiso 1 1 calc R . .
C263 C 1.0567(3) 0.5806(2) 0.8889(2) 0.0406(9) Uani 1 1 d . . .
H265 H 1.0422 0.5319 0.9153 0.061 Uiso 1 1 calc R . .
H266 H 1.0797 0.6208 0.934 0.061 Uiso 1 1 calc R . .
H267 H 1.115 0.5722 0.8619 0.061 Uiso 1 1 calc R . .
C321 C 1.0284(3) 0.43657(19) 0.6726(2) 0.0302(8) Uani 1 1 d . . .
H321 H 0.994 0.4698 0.7084 0.036 Uiso 1 1 calc R . .
C322 C 1.1206(3) 0.3896(2) 0.7360(2) 0.0384(9) Uani 1 1 d . . .
H322 H 1.0902 0.3581 0.7741 0.058 Uiso 1 1 calc R . .
H323 H 1.1758 0.4254 0.7714 0.058 Uiso 1 1 calc R . .
H324 H 1.1547 0.3552 0.7028 0.058 Uiso 1 1 calc R . .
C323 C 1.0780(3) 0.4910(2) 0.6194(3) 0.0408(9) Uani 1 1 d . . .
H325 H 1.0194 0.5203 0.5779 0.061 Uiso 1 1 calc R . .
H326 H 1.1181 0.4602 0.5876 0.061 Uiso 1 1 calc R . .
H327 H 1.1284 0.5275 0.6586 0.061 Uiso 1 1 calc R . .
C361 C 0.6803(3) 0.27780(19) 0.6341(2) 0.0272(7) Uani 1 1 d . . .
H361 H 0.6652 0.3199 0.672 0.033 Uiso 1 1 calc R . .
C362 C 0.5737(3) 0.2593(2) 0.5641(2) 0.0362(8) Uani 1 1 d . . .
H362 H 0.5481 0.3058 0.5284 0.054 Uiso 1 1 calc R . .
H363 H 0.5184 0.2433 0.5917 0.054 Uiso 1 1 calc R . .
H364 H 0.5859 0.217 0.5272 0.054 Uiso 1 1 calc R . .
C363 C 0.7191(3) 0.2056(2) 0.6911(2) 0.0375(9) Uani 1 1 d . . .
H365 H 0.7837 0.219 0.7397 0.056 Uiso 1 1 calc R . .
H366 H 0.7382 0.1643 0.6561 0.056 Uiso 1 1 calc R . .
H367 H 0.6604 0.1874 0.7138 0.056 Uiso 1 1 calc R . .
Cl51 Cl 0.33216(8) 0.27765(7) 0.86964(7) 0.0530(3) Uani 1 1 d . . .
C52 C 0.3981(3) 0.2075(2) 0.8245(3) 0.0463(10) Uani 1 1 d . . .
H521 H 0.3481 0.1903 0.7677 0.056 Uiso 1 1 calc R . .
H522 H 0.4154 0.1615 0.8634 0.056 Uiso 1 1 calc R . .
Cl53 Cl 0.51958(8) 0.24365(6) 0.80910(7) 0.0489(3) 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
Rh1 C1 1.786(3) . ?
Rh1 C12 1.972(3) . ?
Rh1 O41 2.086(2) . ?
Rh1 O42 2.109(2) 3_666 ?
C1 O1 1.158(4) . ?
N11 C12 1.362(4) . ?
N11 C15 1.387(4) . ?
N11 C21 1.455(4) . ?
C12 N13 1.358(4) . ?
N13 C14 1.388(4) . ?
N13 C31 1.448(4) . ?
C14 C15 1.334(4) . ?
C14 H14 0.95 . ?
C15 H15 0.95 . ?
C21 C22 1.395(4) . ?
C21 C26 1.403(4) . ?
C22 C23 1.398(4) . ?
C22 C221 1.508(5) . ?
C23 C24 1.371(5) . ?
C23 H23 0.95 . ?
C24 C25 1.380(5) . ?
C24 H24 0.95 . ?
C25 C26 1.391(4) . ?
C25 H25 0.95 . ?
C26 C261 1.513(4) . ?
C31 C32 1.395(4) . ?
C31 C36 1.399(4) . ?
C32 C33 1.397(4) . ?
C32 C321 1.523(5) . ?
C33 C34 1.389(5) . ?
C33 H33 0.95 . ?
C34 C35 1.374(5) . ?
C34 H34 0.95 . ?
C35 C36 1.390(4) . ?
C35 H35 0.95 . ?
C36 C361 1.520(4) . ?
P41 O42 1.521(2) . ?
P41 O41 1.521(2) . ?
P41 C44 1.794(3) . ?
P41 C43 1.797(3) . ?
O42 Rh1 2.109(2) 3_666 ?
C43 H431 0.98 . ?
C43 H432 0.98 . ?
C43 H433 0.98 . ?
C44 H441 0.98 . ?
C44 H442 0.98 . ?
C44 H443 0.98 . ?
C221 C222 1.523(5) . ?
C221 C223 1.526(5) . ?
C221 H221 1 . ?
C222 H222 0.98 . ?
C222 H223 0.98 . ?
C222 H224 0.98 . ?
C223 H225 0.98 . ?
C223 H226 0.98 . ?
C223 H227 0.98 . ?
C261 C262 1.526(4) . ?
C261 C263 1.528(5) . ?
C261 H261 1 . ?
C262 H262 0.98 . ?
C262 H263 0.98 . ?
C262 H264 0.98 . ?
C263 H265 0.98 . ?
C263 H266 0.98 . ?
C263 H267 0.98 . ?
C321 C323 1.527(4) . ?
C321 C322 1.537(5) . ?
C321 H321 1 . ?
C322 H322 0.98 . ?
C322 H323 0.98 . ?
C322 H324 0.98 . ?
C323 H325 0.98 . ?
C323 H326 0.98 . ?
C323 H327 0.98 . ?
C361 C362 1.520(4) . ?
C361 C363 1.532(5) . ?
C361 H361 1 . ?
C362 H362 0.98 . ?
C362 H363 0.98 . ?
C362 H364 0.98 . ?
C363 H365 0.98 . ?
C363 H366 0.98 . ?
C363 H367 0.98 . ?
Cl51 C52 1.748(4) . ?
C52 Cl53 1.758(4) . ?
C52 H521 0.99 . ?
C52 H522 0.99 . ?

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 Rh1 C12 93.63(12) . . ?
C1 Rh1 O41 177.92(12) . . ?
C12 Rh1 O41 88.17(10) . . ?
C1 Rh1 O42 91.10(11) . 3_666 ?
C12 Rh1 O42 174.82(10) . 3_666 ?
O41 Rh1 O42 87.15(8) . 3_666 ?
O1 C1 Rh1 175.1(3) . . ?
C12 N11 C15 111.0(2) . . ?
C12 N11 C21 126.2(2) . . ?
C15 N11 C21 121.9(2) . . ?
N13 C12 N11 104.0(2) . . ?
N13 C12 Rh1 125.7(2) . . ?
N11 C12 Rh1 129.8(2) . . ?
C12 N13 C14 111.0(2) . . ?
C12 N13 C31 124.4(2) . . ?
C14 N13 C31 124.1(2) . . ?
C15 C14 N13 107.0(3) . . ?
C15 C14 H14 126.5 . . ?
N13 C14 H14 126.5 . . ?
C14 C15 N11 106.9(3) . . ?
C14 C15 H15 126.5 . . ?
N11 C15 H15 126.5 . . ?
C22 C21 C26 123.8(3) . . ?
C22 C21 N11 119.2(3) . . ?
C26 C21 N11 116.8(3) . . ?
C21 C22 C23 115.9(3) . . ?
C21 C22 C221 122.4(3) . . ?
C23 C22 C221 121.7(3) . . ?
C24 C23 C22 122.0(3) . . ?
C24 C23 H23 119 . . ?
C22 C23 H23 119 . . ?
C23 C24 C25 120.5(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C26 120.8(3) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 117.0(3) . . ?
C25 C26 C261 120.7(3) . . ?
C21 C26 C261 122.3(3) . . ?
C32 C31 C36 123.9(3) . . ?
C32 C31 N13 117.6(3) . . ?
C36 C31 N13 118.5(3) . . ?
C31 C32 C33 116.6(3) . . ?
C31 C32 C321 122.4(3) . . ?
C33 C32 C321 121.0(3) . . ?
C34 C33 C32 121.0(3) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C35 C34 C33 120.3(3) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 121.5(3) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C35 C36 C31 116.7(3) . . ?
C35 C36 C361 121.5(3) . . ?
C31 C36 C361 121.8(3) . . ?
O42 P41 O41 114.70(12) . . ?
O42 P41 C44 108.51(14) . . ?
O41 P41 C44 106.69(14) . . ?
O42 P41 C43 110.62(13) . . ?
O41 P41 C43 110.44(14) . . ?
C44 P41 C43 105.36(15) . . ?
P41 O41 Rh1 128.92(12) . . ?
P41 O42 Rh1 124.10(12) . 3_666 ?
P41 C43 H431 109.5 . . ?
P41 C43 H432 109.5 . . ?
H431 C43 H432 109.5 . . ?
P41 C43 H433 109.5 . . ?
H431 C43 H433 109.5 . . ?
H432 C43 H433 109.5 . . ?
P41 C44 H441 109.5 . . ?
P41 C44 H442 109.5 . . ?
H441 C44 H442 109.5 . . ?
P41 C44 H443 109.5 . . ?
H441 C44 H443 109.5 . . ?
H442 C44 H443 109.5 . . ?
C22 C221 C222 110.8(3) . . ?
C22 C221 C223 111.9(3) . . ?
C222 C221 C223 110.0(3) . . ?
C22 C221 H221 108 . . ?
C222 C221 H221 108 . . ?
C223 C221 H221 108 . . ?
C221 C222 H222 109.5 . . ?
C221 C222 H223 109.5 . . ?
H222 C222 H223 109.5 . . ?
C221 C222 H224 109.5 . . ?
H222 C222 H224 109.5 . . ?
H223 C222 H224 109.5 . . ?
C221 C223 H225 109.5 . . ?
C221 C223 H226 109.5 . . ?
H225 C223 H226 109.5 . . ?
C221 C223 H227 109.5 . . ?
H225 C223 H227 109.5 . . ?
H226 C223 H227 109.5 . . ?
C26 C261 C262 112.8(3) . . ?
C26 C261 C263 111.6(3) . . ?
C262 C261 C263 110.4(3) . . ?
C26 C261 H261 107.3 . . ?
C262 C261 H261 107.3 . . ?
C263 C261 H261 107.3 . . ?
C261 C262 H262 109.5 . . ?
C261 C262 H263 109.5 . . ?
H262 C262 H263 109.5 . . ?
C261 C262 H264 109.5 . . ?
H262 C262 H264 109.5 . . ?
H263 C262 H264 109.5 . . ?
C261 C263 H265 109.5 . . ?
C261 C263 H266 109.5 . . ?
H265 C263 H266 109.5 . . ?
C261 C263 H267 109.5 . . ?
H265 C263 H267 109.5 . . ?
H266 C263 H267 109.5 . . ?
C32 C321 C323 114.2(3) . . ?
C32 C321 C322 110.8(3) . . ?
C323 C321 C322 109.0(3) . . ?
C32 C321 H321 107.5 . . ?
C323 C321 H321 107.5 . . ?
C322 C321 H321 107.5 . . ?
C321 C322 H322 109.5 . . ?
C321 C322 H323 109.5 . . ?
H322 C322 H323 109.5 . . ?
C321 C322 H324 109.5 . . ?
H322 C322 H324 109.5 . . ?
H323 C322 H324 109.5 . . ?
C321 C323 H325 109.5 . . ?
C321 C323 H326 109.5 . . ?
H325 C323 H326 109.5 . . ?
C321 C323 H327 109.5 . . ?
H325 C323 H327 109.5 . . ?
H326 C323 H327 109.5 . . ?
C36 C361 C362 113.9(3) . . ?
C36 C361 C363 109.6(3) . . ?
C362 C361 C363 109.5(3) . . ?
C36 C361 H361 107.9 . . ?
C362 C361 H361 107.9 . . ?
C363 C361 H361 107.9 . . ?
C361 C362 H362 109.5 . . ?
C361 C362 H363 109.5 . . ?
H362 C362 H363 109.5 . . ?
C361 C362 H364 109.5 . . ?
H362 C362 H364 109.5 . . ?
H363 C362 H364 109.5 . . ?
C361 C363 H365 109.5 . . ?
C361 C363 H366 109.5 . . ?
H365 C363 H366 109.5 . . ?
C361 C363 H367 109.5 . . ?
H365 C363 H367 109.5 . . ?
H366 C363 H367 109.5 . . ?
Cl51 C52 Cl53 111.9(2) . . ?
Cl51 C52 H521 109.2 . . ?
Cl53 C52 H521 109.2 . . ?
Cl51 C52 H522 109.2 . . ?
Cl53 C52 H522 109.2 . . ?
H521 C52 H522 107.9 . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1496357'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H38 O8 P4 Rh2'
_chemical_formula_weight         880.32

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'
O O 0.0106 0.0060 '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'

_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                   19.9476(11)
_cell_length_b                   9.3438(5)
_cell_length_c                   20.4044(11)
_cell_angle_alpha                90
_cell_angle_beta                 109.9100(10)
_cell_angle_gamma                90
_cell_volume                     3575.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      28.42

_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.149
_shelx_estimated_absorpt_T_min   0.762
_shelx_estimated_absorpt_T_max   0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21038
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.123
_diffrn_reflns_theta_max         28.597
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4308
_reflns_number_gt                3740
_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       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0274P)²+5.3938P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4308
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Rh1 Rh 0.41675(2) 0.00246(2) 0.66325(2) 0.01848(5) Uani 1 1 d . . . . .
C11 C 0.33505(11) 0.0720(2) 0.66870(10) 0.0245(4) Uani 1 1 d . . . . .
O12 O 0.28197(8) 0.11368(18) 0.67200(8) 0.0365(4) Uani 1 1 d . . . . .
P20 P 0.56212(3) -0.18548(5) 0.69531(3) 0.02278(11) Uani 1 1 d . . . . .
O21 O 0.50967(7) -0.07510(14) 0.65193(7) 0.0241(3) Uani 1 1 d . . . . .
O22 O 0.58061(8) -0.17626(14) 0.77361(7) 0.0242(3) Uani 1 1 d . . . . .
C23 C 0.64231(12) -0.1671(3) 0.67493(12) 0.0361(5) Uani 1 1 d . . . . .
H231 H 0.6317 -0.1827 0.6249 0.054 Uiso 1 1 calc R U . . .
H232 H 0.6773 -0.2380 0.7013 0.054 Uiso 1 1 calc R U . . .
H233 H 0.6618 -0.0707 0.6874 0.054 Uiso 1 1 calc R U . . .
C24 C 0.52854(14) -0.3614(2) 0.66871(11) 0.0348(5) Uani 1 1 d . . . . .
H241 H 0.5193 -0.3727 0.6186 0.052 Uiso 1 1 calc R U . . .
H242 H 0.4841 -0.3755 0.6784 0.052 Uiso 1 1 calc R U . . .
H243 H 0.5638 -0.4324 0.6945 0.052 Uiso 1 1 calc R U . . .
P30 P 0.41713(3) 0.17111(5) 0.58847(2) 0.01853(10) Uani 1 1 d . . . . .
C31 C 0.50458(10) 0.24582(19) 0.59953(10) 0.0204(4) Uani 1 1 d . . . . .
C32 C 0.51591(11) 0.3136(2) 0.54329(10) 0.0239(4) Uani 1 1 d . . . . .
H32 H 0.4781 0.3201 0.4999 0.029 Uiso 1 1 calc R U . . .
C33 C 0.58195(11) 0.3715(2) 0.55017(11) 0.0282(4) Uani 1 1 d . . . . .
H33 H 0.5894 0.4161 0.5114 0.034 Uiso 1 1 calc R U . . .
C34 C 0.63700(11) 0.3643(2) 0.61366(12) 0.0311(5) Uani 1 1 d . . . . .
H34 H 0.6821 0.4048 0.6185 0.037 Uiso 1 1 calc R U . . .
C35 C 0.62625(11) 0.2980(2) 0.67022(11) 0.0295(4) Uani 1 1 d . . . . .
H35 H 0.6641 0.2932 0.7137 0.035 Uiso 1 1 calc R U . . .
C36 C 0.56008(10) 0.2384(2) 0.66326(10) 0.0245(4) Uani 1 1 d . . . . .
H36 H 0.5528 0.1928 0.7019 0.029 Uiso 1 1 calc R U . . .
C41 C 0.36323(10) 0.3307(2) 0.58067(10) 0.0214(4) Uani 1 1 d . . . . .
C42 C 0.31504(10) 0.3768(2) 0.51736(10) 0.0237(4) Uani 1 1 d . . . . .
H42 H 0.3085 0.3224 0.4763 0.028 Uiso 1 1 calc R U . . .
C43 C 0.27616(11) 0.5026(2) 0.51385(12) 0.0280(4) Uani 1 1 d . . . . .
H43 H 0.2427 0.5331 0.4707 0.034 Uiso 1 1 calc R U . . .
C44 C 0.28654(12) 0.5820(2) 0.57323(13) 0.0349(5) Uani 1 1 d . . . . .
H44 H 0.2608 0.6686 0.5707 0.042 Uiso 1 1 calc R U . . .
C45 C 0.33405(13) 0.5371(3) 0.63665(13) 0.0417(6) Uani 1 1 d . . . . .
H45 H 0.3408 0.5924 0.6775 0.050 Uiso 1 1 calc R U . . .
C46 C 0.37176(12) 0.4109(2) 0.64030(12) 0.0342(5) Uani 1 1 d . . . . .
H46 H 0.4037 0.3790 0.6840 0.041 Uiso 1 1 calc R U . . .
O51 O 0.38888(7) 0.12068(14) 0.50793(7) 0.0236(3) Uani 1 1 d . . . . .
C52 C 0.40386(12) -0.0248(2) 0.49266(11) 0.0295(5) Uani 1 1 d . . . . .
H521 H 0.3906 -0.0369 0.4421 0.044 Uiso 1 1 calc R U . . .
H522 H 0.3762 -0.0914 0.5105 0.044 Uiso 1 1 calc R U . . .
H523 H 0.4548 -0.0444 0.5150 0.044 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C11 1.793(2) . ?
Rh1 O21 2.0749(13) . ?
Rh1 O22 2.0988(13) 2_656 ?
Rh1 P30 2.1953(5) . ?
C11 O12 1.151(2) . ?
P20 O22 1.5148(14) . ?
P20 O21 1.5202(14) . ?
P20 C24 1.788(2) . ?
P20 C23 1.793(2) . ?
O22 Rh1 2.0988(13) 2_656 ?
C23 H231 0.9800 . ?
C23 H232 0.9800 . ?
C23 H233 0.9800 . ?
C24 H241 0.9800 . ?
C24 H242 0.9800 . ?
C24 H243 0.9800 . ?
P30 O51 1.6154(14) . ?
P30 C41 1.8133(19) . ?
P30 C31 1.8202(19) . ?
C31 C36 1.393(3) . ?
C31 C32 1.395(3) . ?
C32 C33 1.386(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.389(3) . ?
C41 C42 1.390(3) . ?
C42 C43 1.397(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.375(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.387(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
O51 C52 1.448(2) . ?
C52 H521 0.9800 . ?
C52 H522 0.9800 . ?
C52 H523 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
C11 Rh1 O21 177.24(7) . . ?
C11 Rh1 O22 94.80(7) . 2_656 ?
O21 Rh1 O22 87.35(5) . 2_656 ?
C11 Rh1 P30 90.07(7) . . ?
O21 Rh1 P30 87.63(4) . . ?
O22 Rh1 P30 172.97(4) 2_656 . ?
O12 C11 Rh1 178.47(18) . . ?
O22 P20 O21 116.59(8) . . ?
O22 P20 C24 107.69(9) . . ?
O21 P20 C24 109.55(10) . . ?
O22 P20 C23 108.85(10) . . ?
O21 P20 C23 106.96(9) . . ?
C24 P20 C23 106.79(12) . . ?
P20 O21 Rh1 129.48(8) . . ?
P20 O22 Rh1 129.71(8) . 2_656 ?
P20 C23 H231 109.5 . . ?
P20 C23 H232 109.5 . . ?
H231 C23 H232 109.5 . . ?
P20 C23 H233 109.5 . . ?
H231 C23 H233 109.5 . . ?
H232 C23 H233 109.5 . . ?
P20 C24 H241 109.5 . . ?
P20 C24 H242 109.5 . . ?
H241 C24 H242 109.5 . . ?
P20 C24 H243 109.5 . . ?
H241 C24 H243 109.5 . . ?
H242 C24 H243 109.5 . . ?
O51 P30 C41 99.18(8) . . ?
O51 P30 C31 103.04(8) . . ?
C41 P30 C31 102.13(8) . . ?
O51 P30 Rh1 114.52(5) . . ?
C41 P30 Rh1 120.60(6) . . ?
C31 P30 Rh1 114.78(6) . . ?
C36 C31 C32 119.38(18) . . ?
C36 C31 P30 121.33(15) . . ?
C32 C31 P30 119.28(15) . . ?
C33 C32 C31 120.57(19) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 119.94(19) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.05(19) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 120.1(2) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C31 C36 C35 119.93(19) . . ?
C31 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C46 C41 C42 119.11(18) . . ?
C46 C41 P30 118.33(15) . . ?
C42 C41 P30 122.54(15) . . ?
C41 C42 C43 120.30(19) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 119.7(2) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 120.7(2) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C44 C45 C46 119.6(2) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 H45 120.2 . . ?
C45 C46 C41 120.6(2) . . ?
C45 C46 H46 119.7 . . ?
C41 C46 H46 119.7 . . ?
C52 O51 P30 117.81(12) . . ?
O51 C52 H521 109.5 . . ?
O51 C52 H522 109.5 . . ?
H521 C52 H522 109.5 . . ?
O51 C52 H523 109.5 . . ?
H521 C52 H523 109.5 . . ?
H522 C52 H523 109.5 . . ?

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
O22 P20 O21 Rh1 -41.62(14) . . . . ?
C24 P20 O21 Rh1 80.96(13) . . . . ?
C23 P20 O21 Rh1 -163.65(12) . . . . ?
O21 P20 O22 Rh1 -29.29(14) . . . 2_656 ?
C24 P20 O22 Rh1 -152.83(12) . . . 2_656 ?
C23 P20 O22 Rh1 91.74(13) . . . 2_656 ?
O51 P30 C31 C36 -148.41(15) . . . . ?
C41 P30 C31 C36 109.04(16) . . . . ?
Rh1 P30 C31 C36 -23.23(18) . . . . ?
O51 P30 C31 C32 32.50(17) . . . . ?
C41 P30 C31 C32 -70.05(17) . . . . ?
Rh1 P30 C31 C32 157.68(13) . . . . ?
C36 C31 C32 C33 0.9(3) . . . . ?
P30 C31 C32 C33 179.99(15) . . . . ?
C31 C32 C33 C34 -1.1(3) . . . . ?
C32 C33 C34 C35 0.6(3) . . . . ?
C33 C34 C35 C36 0.0(3) . . . . ?
C32 C31 C36 C35 -0.3(3) . . . . ?
P30 C31 C36 C35 -179.35(15) . . . . ?
C34 C35 C36 C31 -0.2(3) . . . . ?
O51 P30 C41 C46 -179.28(17) . . . . ?
C31 P30 C41 C46 -73.71(18) . . . . ?
Rh1 P30 C41 C46 54.98(18) . . . . ?
O51 P30 C41 C42 -0.55(17) . . . . ?
C31 P30 C41 C42 105.03(17) . . . . ?
Rh1 P30 C41 C42 -126.28(15) . . . . ?
C46 C41 C42 C43 0.4(3) . . . . ?
P30 C41 C42 C43 -178.29(15) . . . . ?
C41 C42 C43 C44 1.0(3) . . . . ?
C42 C43 C44 C45 -1.3(3) . . . . ?
C43 C44 C45 C46 0.2(4) . . . . ?
C44 C45 C46 C41 1.2(4) . . . . ?
C42 C41 C46 C45 -1.5(3) . . . . ?
P30 C41 C46 C45 177.3(2) . . . . ?
C41 P30 O51 C52 -163.71(14) . . . . ?
C31 P30 O51 C52 91.46(15) . . . . ?
Rh1 P30 O51 C52 -33.88(15) . . . . ?

_refine_diff_density_max         0.549
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.070

