#------------------------------------------------------------------------------
#$Date: 2022-12-03 04:00:33 +0200 (Sat, 03 Dec 2022) $
#$Revision: 279682 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/59/7245948.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7245948
loop_
_publ_author_name
'Tejero, Alvaro G.'
'Carmona, María'
'Rodríguez, Ricardo'
'Viguri, Fernando'
'Lahoz, Fernando J.'
'García-Orduña, Pilar'
'Carmona, Daniel'
_publ_section_title
;
 Synthesis of chiral-at-metal rhodium complexes from achiral tripodal
 tetradentate ligands: resolution and application to enantioselective
 Diels--Alder and 1,3-dipolar cycloadditions
;
_journal_issue                   53
_journal_name_full               'RSC Advances'
_journal_page_first              34704
_journal_page_last               34714
_journal_paper_doi               10.1039/D2RA06982B
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C37 H33 F3 N4 P Rh,2(F6 Sb),2(C H2 Cl2)'
_chemical_formula_sum            'C39 H37 Cl4 F15 N4 P Rh Sb2'
_chemical_formula_weight         1365.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-12 deposited with the CCDC.	2022-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                96.0690(10)
_cell_angle_beta                 102.032(2)
_cell_angle_gamma                92.269(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2805(9)
_cell_length_b                   13.6365(9)
_cell_length_c                   14.6021(10)
_cell_measurement_reflns_used    6927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.745
_cell_measurement_theta_min      2.340
_cell_volume                     2373.4(3)
_computing_cell_refinement       'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-3 (farrugia, 2012)'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32424
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.187
_diffrn_reflns_theta_min         1.436
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_T_max  0.8373
_exptl_absorpt_correction_T_min  0.7569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/acetone'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.977
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         12574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0526P)²+4.4625P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9063
_reflns_number_total             12574
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra06982b2.cif
_cod_data_source_block           cmpnd_2
_cod_database_code               7245948
_shelx_shelxl_version_number     2018/3
_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'
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
Rh Rh 0.72209(3) 0.74945(2) 0.25612(2) 0.01373(8) Uani 1 1 d . . . . .
P P 0.89969(9) 0.80996(8) 0.25739(7) 0.0132(2) Uani 1 1 d . . . . .
N1 N 0.6435(3) 0.8623(3) 0.1898(2) 0.0158(7) Uani 1 1 d . . . . .
N2 N 0.5550(3) 0.7069(3) 0.2538(2) 0.0168(7) Uani 1 1 d . . . . .
N3 N 0.7834(3) 0.6336(3) 0.3223(3) 0.0163(7) Uani 1 1 d . . . . .
N4 N 0.7065(3) 0.6605(3) 0.1212(3) 0.0188(8) Uani 1 1 d . . . . .
C1 C 1.0028(4) 0.8045(3) 0.3662(3) 0.0150(8) Uani 1 1 d . . . . .
C2 C 1.0037(4) 0.8702(3) 0.4467(3) 0.0201(9) Uani 1 1 d . . . . .
H2 H 0.951220 0.919654 0.444978 0.024 Uiso 1 1 calc R U . . .
C3 C 1.0810(4) 0.8629(4) 0.5287(3) 0.0246(10) Uani 1 1 d . . . . .
H3 H 1.081403 0.908159 0.582930 0.030 Uiso 1 1 calc R U . . .
C4 C 1.1573(4) 0.7919(4) 0.5336(3) 0.0261(11) Uani 1 1 d . . . . .
H4 H 1.209422 0.787362 0.590752 0.031 Uiso 1 1 calc R U . . .
C5 C 1.1574(4) 0.7271(4) 0.4544(3) 0.0276(11) Uani 1 1 d . . . . .
H5 H 1.210562 0.678212 0.457043 0.033 Uiso 1 1 calc R U . . .
C6 C 1.0806(4) 0.7324(3) 0.3707(3) 0.0202(9) Uani 1 1 d . . . . .
H6 H 1.081147 0.687137 0.316733 0.024 Uiso 1 1 calc R U . . .
C7 C 0.9632(4) 0.7487(3) 0.1668(3) 0.0163(9) Uani 1 1 d . . . . .
C8 C 1.0190(4) 0.8023(3) 0.1123(3) 0.0195(9) Uani 1 1 d . . . . .
H8 H 1.019498 0.872378 0.119484 0.023 Uiso 1 1 calc R U . . .
C9 C 1.0737(4) 0.7549(4) 0.0479(3) 0.0242(10) Uani 1 1 d . . . . .
H9 H 1.110297 0.792229 0.010512 0.029 Uiso 1 1 calc R U . . .
C10 C 1.0748(4) 0.6525(4) 0.0383(3) 0.0263(11) Uani 1 1 d . . . . .
H10 H 1.112824 0.619765 -0.005303 0.032 Uiso 1 1 calc R U . . .
C11 C 1.0208(4) 0.5983(4) 0.0920(3) 0.0236(10) Uani 1 1 d . . . . .
H11 H 1.022261 0.528319 0.085313 0.028 Uiso 1 1 calc R U . . .
C12 C 0.9643(4) 0.6450(3) 0.1557(3) 0.0177(9) Uani 1 1 d . . . . .
H12 H 0.926430 0.606964 0.191761 0.021 Uiso 1 1 calc R U . . .
C13 C 0.8996(4) 0.9380(3) 0.2338(3) 0.0154(8) Uani 1 1 d . . . . .
C14 C 0.9928(4) 1.0020(3) 0.2709(3) 0.0198(9) Uani 1 1 d . . . . .
H14 H 1.054900 0.979652 0.312127 0.024 Uiso 1 1 calc R U . . .
C15 C 0.9964(4) 1.0985(3) 0.2483(3) 0.0232(10) Uani 1 1 d . . . . .
H15 H 1.061384 1.141150 0.272683 0.028 Uiso 1 1 calc R U . . .
C16 C 0.9059(4) 1.1318(3) 0.1907(3) 0.0250(10) Uani 1 1 d . . . . .
H16 H 0.906904 1.198363 0.177131 0.030 Uiso 1 1 calc R U . . .
C17 C 0.8124(4) 1.0681(3) 0.1522(3) 0.0221(10) Uani 1 1 d . . . . .
H17 H 0.750549 1.091526 0.111607 0.026 Uiso 1 1 calc R U . . .
C18 C 0.8081(4) 0.9706(3) 0.1721(3) 0.0154(8) Uani 1 1 d . . . . .
C19 C 0.7058(4) 0.9053(3) 0.1238(3) 0.0171(9) Uani 1 1 d . . . . .
H19A H 0.654579 0.944286 0.082414 0.021 Uiso 1 1 calc R U . . .
H19B H 0.728577 0.850487 0.083250 0.021 Uiso 1 1 calc R U . . .
C20 C 0.5354(4) 0.8145(3) 0.1318(3) 0.0193(9) Uani 1 1 d . . . . .
H20A H 0.549160 0.773306 0.075866 0.023 Uiso 1 1 calc R U . . .
H20B H 0.484726 0.865886 0.109766 0.023 Uiso 1 1 calc R U . . .
C21 C 0.4825(4) 0.7514(3) 0.1910(3) 0.0184(9) Uani 1 1 d . . . . .
C22 C 0.3675(4) 0.7356(4) 0.1813(3) 0.0254(10) Uani 1 1 d . . . . .
H22 H 0.316682 0.766856 0.136946 0.030 Uiso 1 1 calc R U . . .
C23 C 0.3298(4) 0.6732(4) 0.2381(4) 0.0289(11) Uani 1 1 d . . . . .
H23 H 0.251946 0.660544 0.232513 0.035 Uiso 1 1 calc R U . . .
C24 C 0.4037(4) 0.6297(4) 0.3022(3) 0.0263(11) Uani 1 1 d . . . . .
H24 H 0.377863 0.586904 0.341501 0.032 Uiso 1 1 calc R U . . .
C25 C 0.5169(4) 0.6489(3) 0.3093(3) 0.0220(10) Uani 1 1 d . . . . .
H25 H 0.568596 0.619902 0.354941 0.026 Uiso 1 1 calc R U . . .
C26 C 0.6190(4) 0.9440(3) 0.2609(3) 0.0179(9) Uani 1 1 d . . . . .
H26A H 0.651105 1.008139 0.249456 0.021 Uiso 1 1 calc R U . . .
H26B H 0.537260 0.948222 0.252554 0.021 Uiso 1 1 calc R U . . .
C27 C 0.6673(4) 0.9242(3) 0.3596(3) 0.0160(9) Uani 1 1 d . . . . .
C28 C 0.7206(4) 0.8374(3) 0.3751(3) 0.0158(8) Uani 1 1 d . . . . .
C29 C 0.7560(4) 0.8155(4) 0.4677(3) 0.0197(9) Uani 1 1 d . . . . .
H29 H 0.791256 0.755993 0.479755 0.024 Uiso 1 1 calc R U . . .
C30 C 0.7390(4) 0.8817(4) 0.5422(3) 0.0219(10) Uani 1 1 d . . . . .
H30 H 0.762675 0.866778 0.605125 0.026 Uiso 1 1 calc R U . . .
C31 C 0.6882(4) 0.9685(3) 0.5259(3) 0.0174(9) Uani 1 1 d . . . . .
C32 C 0.6524(4) 0.9905(3) 0.4350(3) 0.0170(9) Uani 1 1 d . . . . .
H32 H 0.617631 1.050371 0.423731 0.020 Uiso 1 1 calc R U . . .
C33 C 0.6682(4) 1.0371(4) 0.6073(3) 0.0233(10) Uani 1 1 d . . . . .
C34 C 0.8128(4) 0.5655(4) 0.3531(3) 0.0218(10) Uani 1 1 d . . . . .
C35 C 0.8508(5) 0.4758(4) 0.3932(4) 0.0390(14) Uani 1 1 d . . . . .
H35A H 0.835985 0.477172 0.456714 0.059 Uiso 1 1 calc R U . . .
H35B H 0.931102 0.472444 0.396584 0.059 Uiso 1 1 calc R U . . .
H35C H 0.810837 0.417764 0.353248 0.059 Uiso 1 1 calc R U . . .
C36 C 0.7004(4) 0.6178(4) 0.0494(3) 0.0238(10) Uani 1 1 d . . . . .
C37 C 0.6971(5) 0.5660(4) -0.0437(4) 0.0351(13) Uani 1 1 d . . . . .
H37A H 0.699746 0.614217 -0.088544 0.053 Uiso 1 1 calc R U . . .
H37B H 0.628071 0.523722 -0.064206 0.053 Uiso 1 1 calc R U . . .
H37C H 0.761407 0.525191 -0.040997 0.053 Uiso 1 1 calc R U . . .
F1 F 0.7611(3) 1.0775(3) 0.6642(2) 0.0482(10) Uani 1 1 d . . . . .
F2 F 0.6072(3) 1.1130(2) 0.5810(2) 0.0421(8) Uani 1 1 d . . . . .
F3 F 0.6111(3) 0.9914(2) 0.6611(2) 0.0380(8) Uani 1 1 d . . . . .
Sb1 Sb 0.63158(3) 0.33762(3) 0.12407(2) 0.02973(10) Uani 1 1 d . . . . .
F4 F 0.6818(3) 0.2394(2) 0.0452(2) 0.0466(9) Uani 1 1 d . . . . .
F5 F 0.5811(3) 0.4369(3) 0.1996(3) 0.0610(11) Uani 1 1 d . . . . .
F6 F 0.5026(4) 0.2579(3) 0.1164(3) 0.0640(12) Uani 1 1 d . . . . .
F7 F 0.7598(3) 0.4183(3) 0.1264(3) 0.0504(9) Uani 1 1 d . . . . .
F8 F 0.5578(3) 0.3894(2) 0.0159(2) 0.0415(8) Uani 1 1 d . . . . .
F9 F 0.7031(3) 0.2826(3) 0.2312(2) 0.0514(10) Uani 1 1 d . . . . .
Sb2 Sb 0.85500(3) 0.60839(2) 0.69228(2) 0.02645(9) Uani 1 1 d . . . . .
F10 F 0.9615(3) 0.6504(3) 0.8000(3) 0.0658(13) Uani 1 1 d . . . . .
F11 F 0.7477(4) 0.5639(3) 0.5831(3) 0.0743(14) Uani 1 1 d . . . . .
F12 F 0.7668(4) 0.5515(3) 0.7631(3) 0.0632(12) Uani 1 1 d . . . . .
F13 F 0.9411(4) 0.6655(3) 0.6188(4) 0.0735(15) Uani 1 1 d . . . . .
F14 F 0.7828(3) 0.7262(2) 0.7033(2) 0.0342(7) Uani 1 1 d . . . . .
F15 F 0.9249(4) 0.4900(3) 0.6779(3) 0.0636(12) Uani 1 1 d . . . . .
C51 C 0.2881(6) 0.1190(4) 0.1510(4) 0.0419(15) Uani 1 1 d . . . . .
H51A H 0.271793 0.118343 0.214495 0.050 Uiso 1 1 calc R U . . .
H51B H 0.358037 0.160231 0.157295 0.050 Uiso 1 1 calc R U . . .
Cl1 Cl 0.30605(17) -0.00287(12) 0.10437(11) 0.0547(5) Uani 1 1 d . . . . .
Cl2 Cl 0.17804(14) 0.17068(13) 0.07729(10) 0.0458(4) Uani 1 1 d . . . . .
C52 C 0.5177(6) 0.6523(5) 0.6300(6) 0.061(2) Uani 1 1 d . . . . .
H52A H 0.525241 0.637491 0.695871 0.073 Uiso 1 1 calc R U . . .
H52B H 0.589060 0.638892 0.611070 0.073 Uiso 1 1 calc R U . . .
Cl3 Cl 0.41193(15) 0.57381(13) 0.55779(11) 0.0505(4) Uani 1 1 d . . . . .
Cl4 Cl 0.4951(2) 0.77580(16) 0.6257(2) 0.1011(10) Uani 1 1 d . . . . .
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'
Cl Cl 0.1484 0.1585 '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'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C28 Rh N3 95.16(16) . . ?
C28 Rh N1 84.30(16) . . ?
N3 Rh N1 174.12(15) . . ?
C28 Rh N2 86.84(16) . . ?
N3 Rh N2 94.02(15) . . ?
N1 Rh N2 80.10(15) . . ?
C28 Rh N4 173.81(16) . . ?
N3 Rh N4 89.56(14) . . ?
N1 Rh N4 90.59(14) . . ?
N2 Rh N4 88.84(14) . . ?
C28 Rh P 90.81(13) . . ?
N3 Rh P 90.69(11) . . ?
N1 Rh P 95.17(11) . . ?
N2 Rh P 174.91(11) . . ?
N4 Rh P 93.15(10) . . ?
C13 P C7 103.8(2) . . ?
C13 P C1 107.1(2) . . ?
C7 P C1 103.7(2) . . ?
C13 P Rh 110.56(15) . . ?
C7 P Rh 114.77(15) . . ?
C1 P Rh 115.88(14) . . ?
C19 N1 C20 107.5(3) . . ?
C19 N1 C26 110.0(3) . . ?
C20 N1 C26 109.1(3) . . ?
C19 N1 Rh 113.8(3) . . ?
C20 N1 Rh 104.7(3) . . ?
C26 N1 Rh 111.5(3) . . ?
C25 N2 C21 119.7(4) . . ?
C25 N2 Rh 127.7(3) . . ?
C21 N2 Rh 112.4(3) . . ?
C34 N3 Rh 174.8(4) . . ?
C36 N4 Rh 176.8(4) . . ?
C6 C1 C2 118.9(4) . . ?
C6 C1 P 120.0(3) . . ?
C2 C1 P 121.1(3) . . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 121.4(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 120.8(4) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.8(4) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
C8 C7 C12 118.6(4) . . ?
C8 C7 P 121.5(3) . . ?
C12 C7 P 119.7(3) . . ?
C9 C8 C7 121.0(4) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 119.7(5) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.7(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 119.9(4) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
C14 C13 C18 119.8(4) . . ?
C14 C13 P 120.3(3) . . ?
C18 C13 P 119.8(3) . . ?
C13 C14 C15 120.8(4) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 119.7(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 120.1(4) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 121.1(4) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C13 118.5(4) . . ?
C17 C18 C19 117.6(4) . . ?
C13 C18 C19 123.8(4) . . ?
N1 C19 C18 114.4(3) . . ?
N1 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
N1 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
N1 C20 C21 109.1(3) . . ?
N1 C20 H20A 109.9 . . ?
C21 C20 H20A 109.9 . . ?
N1 C20 H20B 109.9 . . ?
C21 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
N2 C21 C22 121.2(4) . . ?
N2 C21 C20 114.9(4) . . ?
C22 C21 C20 123.9(4) . . ?
C23 C22 C21 118.1(5) . . ?
C23 C22 H22 121.0 . . ?
C21 C22 H22 121.0 . . ?
C24 C23 C22 120.4(5) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 119.0(5) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
N2 C25 C24 121.6(5) . . ?
N2 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C27 C26 N1 110.8(3) . . ?
C27 C26 H26A 109.5 . . ?
N1 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
N1 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C28 C27 C32 120.9(4) . . ?
C28 C27 C26 119.6(4) . . ?
C32 C27 C26 119.4(4) . . ?
C27 C28 C29 118.9(4) . . ?
C27 C28 Rh 113.6(3) . . ?
C29 C28 Rh 127.1(3) . . ?
C30 C29 C28 119.4(4) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C31 C30 C29 121.0(4) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C32 C31 C30 120.1(4) . . ?
C32 C31 C33 120.0(4) . . ?
C30 C31 C33 119.8(4) . . ?
C31 C32 C27 119.6(4) . . ?
C31 C32 H32 120.2 . . ?
C27 C32 H32 120.2 . . ?
F1 C33 F3 106.4(4) . . ?
F1 C33 F2 105.7(4) . . ?
F3 C33 F2 104.7(4) . . ?
F1 C33 C31 113.5(4) . . ?
F3 C33 C31 112.2(4) . . ?
F2 C33 C31 113.7(4) . . ?
N3 C34 C35 179.7(6) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N4 C36 C37 177.2(6) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
F6 Sb1 F5 91.0(2) . . ?
F6 Sb1 F8 87.80(17) . . ?
F5 Sb1 F8 90.17(16) . . ?
F6 Sb1 F9 90.86(19) . . ?
F5 Sb1 F9 90.62(17) . . ?
F8 Sb1 F9 178.45(17) . . ?
F6 Sb1 F7 177.63(17) . . ?
F5 Sb1 F7 89.96(18) . . ?
F8 Sb1 F7 90.04(16) . . ?
F9 Sb1 F7 91.29(17) . . ?
F6 Sb1 F4 89.40(19) . . ?
F5 Sb1 F4 178.51(17) . . ?
F8 Sb1 F4 88.41(14) . . ?
F9 Sb1 F4 90.80(15) . . ?
F7 Sb1 F4 89.56(17) . . ?
F10 Sb2 F12 90.5(2) . . ?
F10 Sb2 F13 90.7(2) . . ?
F12 Sb2 F13 178.8(2) . . ?
F10 Sb2 F15 90.21(19) . . ?
F12 Sb2 F15 90.18(19) . . ?
F13 Sb2 F15 90.16(18) . . ?
F10 Sb2 F11 179.19(19) . . ?
F12 Sb2 F11 89.3(2) . . ?
F13 Sb2 F11 89.5(2) . . ?
F15 Sb2 F11 89.0(2) . . ?
F10 Sb2 F14 91.31(16) . . ?
F12 Sb2 F14 90.21(17) . . ?
F13 Sb2 F14 89.42(15) . . ?
F15 Sb2 F14 178.43(17) . . ?
F11 Sb2 F14 89.48(17) . . ?
Cl2 C51 Cl1 110.9(3) . . ?
Cl2 C51 H51A 109.5 . . ?
Cl1 C51 H51A 109.5 . . ?
Cl2 C51 H51B 109.5 . . ?
Cl1 C51 H51B 109.5 . . ?
H51A C51 H51B 108.0 . . ?
Cl4 C52 Cl3 113.6(4) . . ?
Cl4 C52 H52A 108.9 . . ?
Cl3 C52 H52A 108.9 . . ?
Cl4 C52 H52B 108.9 . . ?
Cl3 C52 H52B 108.9 . . ?
H52A C52 H52B 107.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh C28 2.007(4) . ?
Rh N3 2.028(4) . ?
Rh N1 2.069(4) . ?
Rh N2 2.102(4) . ?
Rh N4 2.170(4) . ?
Rh P 2.2968(12) . ?
P C13 1.815(4) . ?
P C7 1.818(4) . ?
P C1 1.823(4) . ?
N1 C19 1.499(6) . ?
N1 C20 1.500(5) . ?
N1 C26 1.524(5) . ?
N2 C25 1.329(6) . ?
N2 C21 1.350(6) . ?
N3 C34 1.114(6) . ?
N4 C36 1.131(6) . ?
C1 C6 1.395(6) . ?
C1 C2 1.399(6) . ?
C2 C3 1.379(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.371(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.395(6) . ?
C7 C12 1.407(6) . ?
C8 C9 1.387(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.389(6) . ?
C13 C18 1.405(6) . ?
C14 C15 1.390(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.510(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.502(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.395(6) . ?
C22 C23 1.380(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.362(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.497(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.393(6) . ?
C27 C32 1.397(6) . ?
C28 C29 1.399(6) . ?
C29 C30 1.394(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.379(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.377(6) . ?
C31 C33 1.500(6) . ?
C32 H32 0.9500 . ?
C33 F1 1.325(5) . ?
C33 F3 1.340(6) . ?
C33 F2 1.344(6) . ?
C34 C35 1.462(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.456(7) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
Sb1 F6 1.862(4) . ?
Sb1 F5 1.863(3) . ?
Sb1 F8 1.872(3) . ?
Sb1 F9 1.873(3) . ?
Sb1 F7 1.877(4) . ?
Sb1 F4 1.880(3) . ?
Sb2 F10 1.845(4) . ?
Sb2 F12 1.848(4) . ?
Sb2 F13 1.861(4) . ?
Sb2 F15 1.871(4) . ?
Sb2 F11 1.872(4) . ?
Sb2 F14 1.874(3) . ?
C51 Cl2 1.764(6) . ?
C51 Cl1 1.768(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 Cl4 1.723(7) . ?
C52 Cl3 1.740(7) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
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
C13 P C1 C6 -132.4(4) . . . . ?
C7 P C1 C6 -23.0(4) . . . . ?
Rh P C1 C6 103.7(4) . . . . ?
C13 P C1 C2 49.2(4) . . . . ?
C7 P C1 C2 158.6(4) . . . . ?
Rh P C1 C2 -74.7(4) . . . . ?
C6 C1 C2 C3 0.1(7) . . . . ?
P C1 C2 C3 178.5(4) . . . . ?
C1 C2 C3 C4 -0.5(7) . . . . ?
C2 C3 C4 C5 0.8(8) . . . . ?
C3 C4 C5 C6 -0.7(8) . . . . ?
C4 C5 C6 C1 0.4(8) . . . . ?
C2 C1 C6 C5 -0.1(7) . . . . ?
P C1 C6 C5 -178.5(4) . . . . ?
C13 P C7 C8 13.2(4) . . . . ?
C1 P C7 C8 -98.6(4) . . . . ?
Rh P C7 C8 134.0(3) . . . . ?
C13 P C7 C12 -171.9(3) . . . . ?
C1 P C7 C12 76.3(4) . . . . ?
Rh P C7 C12 -51.1(4) . . . . ?
C12 C7 C8 C9 0.6(6) . . . . ?
P C7 C8 C9 175.5(3) . . . . ?
C7 C8 C9 C10 -1.1(7) . . . . ?
C8 C9 C10 C11 0.6(7) . . . . ?
C9 C10 C11 C12 0.4(7) . . . . ?
C10 C11 C12 C7 -0.9(7) . . . . ?
C8 C7 C12 C11 0.4(6) . . . . ?
P C7 C12 C11 -174.6(3) . . . . ?
C7 P C13 C14 -85.6(4) . . . . ?
C1 P C13 C14 23.7(4) . . . . ?
Rh P C13 C14 150.8(3) . . . . ?
C7 P C13 C18 89.5(4) . . . . ?
C1 P C13 C18 -161.1(3) . . . . ?
Rh P C13 C18 -34.0(4) . . . . ?
C18 C13 C14 C15 0.6(6) . . . . ?
P C13 C14 C15 175.8(4) . . . . ?
C13 C14 C15 C16 1.7(7) . . . . ?
C14 C15 C16 C17 -2.4(7) . . . . ?
C15 C16 C17 C18 1.0(7) . . . . ?
C16 C17 C18 C13 1.3(7) . . . . ?
C16 C17 C18 C19 -177.3(4) . . . . ?
C14 C13 C18 C17 -2.1(6) . . . . ?
P C13 C18 C17 -177.3(3) . . . . ?
C14 C13 C18 C19 176.4(4) . . . . ?
P C13 C18 C19 1.2(6) . . . . ?
C20 N1 C19 C18 170.5(4) . . . . ?
C26 N1 C19 C18 51.8(5) . . . . ?
Rh N1 C19 C18 -74.1(4) . . . . ?
C17 C18 C19 N1 -121.1(4) . . . . ?
C13 C18 C19 N1 60.4(5) . . . . ?
C19 N1 C20 C21 167.4(3) . . . . ?
C26 N1 C20 C21 -73.4(4) . . . . ?
Rh N1 C20 C21 46.0(4) . . . . ?
C25 N2 C21 C22 -1.8(6) . . . . ?
Rh N2 C21 C22 -177.6(3) . . . . ?
C25 N2 C21 C20 -179.6(4) . . . . ?
Rh N2 C21 C20 4.5(5) . . . . ?
N1 C20 C21 N2 -34.5(5) . . . . ?
N1 C20 C21 C22 147.7(4) . . . . ?
N2 C21 C22 C23 0.2(7) . . . . ?
C20 C21 C22 C23 177.9(4) . . . . ?
C21 C22 C23 C24 0.7(7) . . . . ?
C22 C23 C24 C25 -0.1(8) . . . . ?
C21 N2 C25 C24 2.4(7) . . . . ?
Rh N2 C25 C24 177.6(3) . . . . ?
C23 C24 C25 N2 -1.5(7) . . . . ?
C19 N1 C26 C27 -122.3(4) . . . . ?
C20 N1 C26 C27 120.0(4) . . . . ?
Rh N1 C26 C27 4.9(4) . . . . ?
N1 C26 C27 C28 -3.1(6) . . . . ?
N1 C26 C27 C32 -179.2(4) . . . . ?
C32 C27 C28 C29 2.1(7) . . . . ?
C26 C27 C28 C29 -174.0(4) . . . . ?
C32 C27 C28 Rh 175.7(3) . . . . ?
C26 C27 C28 Rh -0.4(5) . . . . ?
C27 C28 C29 C30 -1.2(7) . . . . ?
Rh C28 C29 C30 -173.8(3) . . . . ?
C28 C29 C30 C31 -0.2(7) . . . . ?
C29 C30 C31 C32 0.7(7) . . . . ?
C29 C30 C31 C33 178.3(4) . . . . ?
C30 C31 C32 C27 0.2(7) . . . . ?
C33 C31 C32 C27 -177.4(4) . . . . ?
C28 C27 C32 C31 -1.7(7) . . . . ?
C26 C27 C32 C31 174.5(4) . . . . ?
C32 C31 C33 F1 -116.1(5) . . . . ?
C30 C31 C33 F1 66.3(6) . . . . ?
C32 C31 C33 F3 123.2(5) . . . . ?
C30 C31 C33 F3 -54.4(6) . . . . ?
C32 C31 C33 F2 4.6(6) . . . . ?
C30 C31 C33 F2 -172.9(4) . . . . ?
