#------------------------------------------------------------------------------
#$Date: 2020-11-04 03:15:21 +0200 (Wed, 04 Nov 2020) $
#$Revision: 258696 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/81/4518119.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_4518119
loop_
_publ_author_name
'Takaya, Jun'
'Ogawa, Koki'
'Nakaya, Ryota'
'Iwasawa, Nobuharu'
_publ_section_title
;
 Rhodium-Catalyzed Chemoselective Hydrosilylation of Nitriles to an Imine
 Oxidation Level Enabled by a Pincer-type Group 13 Metallylene Ligand
;
_journal_issue                   20
_journal_name_full               'ACS Catalysis'
_journal_page_first              12223
_journal_page_last               12228
_journal_paper_doi               10.1021/acscatal.0c02779
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C39H29N3P2AlCl4Rh, 2(C3H7NO), 2(CH4O)'
_chemical_formula_sum            'C47 H51 Al Cl4 N5 O4 P2 Rh'
_chemical_formula_weight         1083.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 111.781(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4262(3)
_cell_length_b                   17.0323(3)
_cell_length_c                   19.6403(4)
_cell_measurement_reflns_used    31110
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.2770
_cell_measurement_theta_min      2.4660
_cell_volume                     4791.96(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    Yadokari-XG
_computing_publication_material  Yadokari-XG
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    Sir-2014
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.225
_diffrn_reflns_theta_min         1.858
_diffrn_source                   'rotating anode X-ray generator'
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.60592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       prism
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         14609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0469P)²+10.1745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11782
_reflns_number_total             14609
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs0c02779_si_002.cif
_cod_data_source_block           2-Al
_cod_depositor_comments
'Adding full bibliography for 4518119--4518122.cif.'
_cod_original_cell_volume        4791.95(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518119
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.965
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.22346(2) 0.24067(2) 0.34513(2) 0.01706(6) Uani 1 1 d . . . . .
Al1 Al 0.37807(6) 0.19618(5) 0.42202(4) 0.01794(16) Uani 1 1 d . . . . .
Cl1 Cl 0.18501(5) 0.36100(4) 0.28798(4) 0.02492(15) Uani 1 1 d . . . . .
Cl2 Cl 0.24213(5) 0.11500(4) 0.39833(4) 0.02129(13) Uani 1 1 d . . . . .
Cl3 Cl 0.46862(5) 0.29654(4) 0.42498(4) 0.02523(15) Uani 1 1 d . . . . .
P1 P 0.21148(5) 0.29277(4) 0.44935(4) 0.01789(14) Uani 1 1 d . . . . .
P2 P 0.24561(5) 0.18452(4) 0.24605(4) 0.01838(14) Uani 1 1 d . . . . .
N1 N 0.36938(16) 0.21261(14) 0.52192(12) 0.0183(4) Uani 1 1 d . . . . .
N2 N 0.47957(16) 0.12928(14) 0.48445(12) 0.0181(4) Uani 1 1 d . . . . .
N3 N 0.40640(16) 0.12890(14) 0.34693(12) 0.0183(4) Uani 1 1 d . . . . .
C1 C 0.30015(19) 0.25137(16) 0.53254(15) 0.0197(5) Uani 1 1 d . . . . .
C2 C 0.2988(2) 0.25969(18) 0.60323(15) 0.0229(6) Uani 1 1 d . . . . .
H1 H 0.2500 0.2879 0.6108 0.027 Uiso 1 1 calc R U . . .
C3 C 0.3702(2) 0.22578(19) 0.66197(16) 0.0251(6) Uani 1 1 d . . . . .
H2 H 0.3708 0.2311 0.7103 0.030 Uiso 1 1 calc R U . . .
C4 C 0.4400(2) 0.18460(17) 0.65009(15) 0.0221(6) Uani 1 1 d . . . . .
H3 H 0.4883 0.1603 0.6897 0.027 Uiso 1 1 calc R U . . .
C5 C 0.43840(19) 0.17930(16) 0.57929(14) 0.0184(5) Uani 1 1 d . . . . .
C6 C 0.50554(19) 0.13506(16) 0.55767(14) 0.0180(5) Uani 1 1 d . . . . .
C7 C 0.5876(2) 0.10032(17) 0.60373(16) 0.0226(6) Uani 1 1 d . . . . .
H4 H 0.6069 0.1048 0.6555 0.027 Uiso 1 1 calc R U . . .
C8 C 0.6410(2) 0.05899(18) 0.57268(16) 0.0246(6) Uani 1 1 d . . . . .
H5 H 0.6978 0.0354 0.6035 0.030 Uiso 1 1 calc R U . . .
C9 C 0.61243(19) 0.05165(17) 0.49678(16) 0.0220(6) Uani 1 1 d . . . . .
H6 H 0.6480 0.0224 0.4751 0.026 Uiso 1 1 calc R U . . .
C10 C 0.53014(19) 0.08864(17) 0.45407(15) 0.0191(5) Uani 1 1 d . . . . .
C11 C 0.48587(19) 0.08582(17) 0.37361(15) 0.0195(5) Uani 1 1 d . . . . .
C12 C 0.5159(2) 0.04031(18) 0.32865(16) 0.0217(5) Uani 1 1 d . . . . .
H7 H 0.5729 0.0119 0.3480 0.026 Uiso 1 1 calc R U . . .
C13 C 0.4611(2) 0.03684(19) 0.25413(16) 0.0244(6) Uani 1 1 d . . . . .
H8 H 0.4802 0.0060 0.2219 0.029 Uiso 1 1 calc R U . . .
C14 C 0.3784(2) 0.07890(19) 0.22750(16) 0.0242(6) Uani 1 1 d . . . . .
H9 H 0.3395 0.0761 0.1771 0.029 Uiso 1 1 calc R U . . .
C15 C 0.35291(19) 0.12515(17) 0.27531(15) 0.0188(5) Uani 1 1 d . . . . .
C16 C 0.2287(2) 0.39707(17) 0.47062(15) 0.0210(5) Uani 1 1 d . . . . .
C17 C 0.2898(2) 0.43902(18) 0.44728(16) 0.0239(6) Uani 1 1 d . . . . .
H10 H 0.3199 0.4139 0.4188 0.029 Uiso 1 1 calc R U . . .
C18 C 0.3068(2) 0.51786(19) 0.46577(17) 0.0299(7) Uani 1 1 d . . . . .
H11 H 0.3482 0.5466 0.4494 0.036 Uiso 1 1 calc R U . . .
C19 C 0.2641(3) 0.5548(2) 0.50759(19) 0.0345(8) Uani 1 1 d . . . . .
H12 H 0.2752 0.6089 0.5192 0.041 Uiso 1 1 calc R U . . .
C20 C 0.2050(3) 0.5128(2) 0.5326(2) 0.0366(8) Uani 1 1 d . . . . .
H13 H 0.1768 0.5378 0.5624 0.044 Uiso 1 1 calc R U . . .
C21 C 0.1868(2) 0.4338(2) 0.51396(18) 0.0295(7) Uani 1 1 d . . . . .
H14 H 0.1459 0.4050 0.5308 0.035 Uiso 1 1 calc R U . . .
C22 C 0.1001(2) 0.26784(18) 0.45454(16) 0.0217(5) Uani 1 1 d . . . . .
C23 C 0.0218(2) 0.3090(2) 0.40780(17) 0.0264(6) Uani 1 1 d . . . . .
H15 H 0.0295 0.3516 0.3794 0.032 Uiso 1 1 calc R U . . .
C24 C -0.0668(2) 0.2872(2) 0.40319(19) 0.0338(7) Uani 1 1 d . . . . .
H16 H -0.1200 0.3149 0.3716 0.041 Uiso 1 1 calc R U . . .
C25 C -0.0777(2) 0.2246(3) 0.4448(2) 0.0388(8) Uani 1 1 d . . . . .
H17 H -0.1385 0.2100 0.4419 0.047 Uiso 1 1 calc R U . . .
C26 C -0.0009(3) 0.1837(2) 0.4903(2) 0.0370(8) Uani 1 1 d . . . . .
H18 H -0.0089 0.1409 0.5184 0.044 Uiso 1 1 calc R U . . .
C27 C 0.0881(2) 0.2046(2) 0.49519(17) 0.0290(7) Uani 1 1 d . . . . .
H19 H 0.1408 0.1760 0.5262 0.035 Uiso 1 1 calc R U . . .
C28 C 0.2677(2) 0.24459(18) 0.17755(16) 0.0234(6) Uani 1 1 d . . . . .
C29 C 0.2276(3) 0.2323(2) 0.10176(17) 0.0327(7) Uani 1 1 d . . . . .
H20 H 0.1812 0.1931 0.0822 0.039 Uiso 1 1 calc R U . . .
C30 C 0.2563(3) 0.2779(2) 0.0557(2) 0.0438(10) Uani 1 1 d . . . . .
H21 H 0.2286 0.2703 0.0042 0.053 Uiso 1 1 calc R U . . .
C31 C 0.3242(3) 0.3338(2) 0.0837(2) 0.0443(10) Uani 1 1 d . . . . .
H22 H 0.3440 0.3641 0.0515 0.053 Uiso 1 1 calc R U . . .
C32 C 0.3638(3) 0.3465(2) 0.1583(2) 0.0399(8) Uani 1 1 d . . . . .
H23 H 0.4104 0.3857 0.1773 0.048 Uiso 1 1 calc R U . . .
C33 C 0.3357(2) 0.3022(2) 0.20510(19) 0.0330(7) Uani 1 1 d . . . . .
H24 H 0.3629 0.3111 0.2565 0.040 Uiso 1 1 calc R U . . .
C34 C 0.1556(2) 0.11438(18) 0.19707(15) 0.0214(6) Uani 1 1 d . . . . .
C35 C 0.0713(2) 0.1432(2) 0.14709(19) 0.0328(7) Uani 1 1 d . . . . .
H25 H 0.0639 0.1980 0.1373 0.039 Uiso 1 1 calc R U . . .
C36 C -0.0016(2) 0.0925(2) 0.1117(2) 0.0409(9) Uani 1 1 d . . . . .
H26 H -0.0586 0.1123 0.0773 0.049 Uiso 1 1 calc R U . . .
C37 C 0.0084(3) 0.0129(2) 0.1263(2) 0.0392(8) Uani 1 1 d . . . . .
H27 H -0.0418 -0.0219 0.1022 0.047 Uiso 1 1 calc R U . . .
C38 C 0.0919(2) -0.0163(2) 0.17621(19) 0.0325(7) Uani 1 1 d . . . . .
H28 H 0.0987 -0.0710 0.1860 0.039 Uiso 1 1 calc R U . . .
C39 C 0.1652(2) 0.03423(18) 0.21172(16) 0.0245(6) Uani 1 1 d . . . . .
H29 H 0.2221 0.0141 0.2461 0.029 Uiso 1 1 calc R U . . .
Cl4 Cl 0.65255(6) -0.06414(5) 0.24030(5) 0.03291(17) Uani 1 1 d . . . . .
C40 C 0.1583(3) 0.3100(3) 0.8125(2) 0.0465(10) Uani 1 1 d . . . . .
H30 H 0.1562 0.3537 0.7818 0.056 Uiso 1 1 calc R U . . .
O1 O 0.1733(2) 0.3237(2) 0.87680(16) 0.0572(8) Uani 1 1 d . . . . .
N4 N 0.1444(3) 0.2394(2) 0.78142(19) 0.0452(8) Uani 1 1 d . . . . .
C41 C 0.1447(5) 0.1702(3) 0.8234(3) 0.0675(15) Uani 1 1 d . . . . .
H31 H 0.1531 0.1853 0.8736 0.101 Uiso 1 1 calc R U . . .
H32 H 0.1960 0.1358 0.8243 0.101 Uiso 1 1 calc R U . . .
H33 H 0.0852 0.1424 0.8008 0.101 Uiso 1 1 calc R U . . .
C42 C 0.1312(4) 0.2284(3) 0.7054(2) 0.0580(12) Uani 1 1 d . . . . .
H34 H 0.1348 0.2793 0.6833 0.087 Uiso 1 1 calc R U . . .
H35 H 0.0699 0.2048 0.6792 0.087 Uiso 1 1 calc R U . . .
H36 H 0.1801 0.1937 0.7020 0.087 Uiso 1 1 calc R U . . .
C43 C 0.0817(3) 1.0160(3) 0.6749(3) 0.0514(11) Uani 1 1 d . . . . .
H37 H 0.1386 1.0446 0.6908 0.062 Uiso 1 1 calc R U . . .
O2 O 0.0150(3) 1.0449(3) 0.6261(2) 0.0788(12) Uani 1 1 d . . . . .
N5 N 0.0815(2) 0.9484(2) 0.7073(2) 0.0459(8) Uani 1 1 d . . . . .
C44 C 0.1621(3) 0.9186(4) 0.7624(3) 0.0724(17) Uani 1 1 d . . . . .
H38 H 0.1771 0.8670 0.7476 0.109 Uiso 1 1 calc R U . . .
H39 H 0.1510 0.9135 0.8082 0.109 Uiso 1 1 calc R U . . .
H40 H 0.2144 0.9546 0.7699 0.109 Uiso 1 1 calc R U . . .
C45 C -0.0010(3) 0.9009(3) 0.6872(3) 0.0563(12) Uani 1 1 d . . . . .
H41 H -0.0512 0.9258 0.6464 0.084 Uiso 1 1 calc R U . . .
H42 H -0.0202 0.8958 0.7293 0.084 Uiso 1 1 calc R U . . .
H43 H 0.0120 0.8488 0.6721 0.084 Uiso 1 1 calc R U . . .
C46 C 0.0079(4) 0.4201(5) 0.5923(3) 0.082(2) Uani 1 1 d . . . . .
H44 H -0.0077 0.4751 0.5786 0.123 Uiso 1 1 calc R U . . .
H45 H -0.0333 0.3996 0.6159 0.123 Uiso 1 1 calc R U . . .
H46 H -0.0002 0.3891 0.5483 0.123 Uiso 1 1 calc R U . . .
O3 O 0.1002(2) 0.41490(19) 0.64071(16) 0.0514(7) Uani 1 1 d . . . . .
H50 H 0.1119 0.4521 0.6708 0.077 Uiso 1 1 calc R U . . .
C47 C 0.3073(3) 0.5072(3) 0.9461(3) 0.0491(10) Uani 1 1 d . . . . .
H47 H 0.3597 0.5263 0.9339 0.074 Uiso 1 1 calc R U . . .
H48 H 0.2905 0.4541 0.9266 0.074 Uiso 1 1 calc R U . . .
H49 H 0.3255 0.5063 0.9995 0.074 Uiso 1 1 calc R U . . .
O4 O 0.22885(18) 0.55831(16) 0.91457(14) 0.0371(6) Uani 1 1 d . . . . .
H51 H 0.2170 0.5630 0.8694 0.056 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
O O 0.0106 0.0060 '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
P1 Rh1 P2 175.85(3) . . ?
P1 Rh1 Cl1 89.96(3) . . ?
P2 Rh1 Cl1 92.85(3) . . ?
P1 Rh1 Cl2 89.59(3) . . ?
P2 Rh1 Cl2 88.01(3) . . ?
Cl1 Rh1 Cl2 172.71(3) . . ?
P1 Rh1 Al1 87.22(3) . . ?
P2 Rh1 Al1 88.65(3) . . ?
Cl1 Rh1 Al1 126.67(3) . . ?
Cl2 Rh1 Al1 60.56(3) . . ?
N2 Al1 N1 78.44(10) . . ?
N2 Al1 N3 77.85(10) . . ?
N1 Al1 N3 152.03(10) . . ?
N2 Al1 Cl3 94.79(8) . . ?
N1 Al1 Cl3 97.83(8) . . ?
N3 Al1 Cl3 98.73(8) . . ?
N2 Al1 Cl2 102.92(8) . . ?
N1 Al1 Cl2 84.33(7) . . ?
N3 Al1 Cl2 86.71(7) . . ?
Cl3 Al1 Cl2 162.21(5) . . ?
N2 Al1 Rh1 161.17(8) . . ?
N1 Al1 Rh1 98.99(7) . . ?
N3 Al1 Rh1 98.66(7) . . ?
Cl3 Al1 Rh1 104.03(4) . . ?
Cl2 Al1 Rh1 58.27(3) . . ?
Rh1 Cl2 Al1 61.17(3) . . ?
C22 P1 C16 106.08(14) . . ?
C22 P1 C1 105.60(14) . . ?
C16 P1 C1 99.97(13) . . ?
C22 P1 Rh1 110.55(10) . . ?
C16 P1 Rh1 121.81(10) . . ?
C1 P1 Rh1 111.34(9) . . ?
C34 P2 C28 107.15(14) . . ?
C34 P2 C15 103.08(13) . . ?
C28 P2 C15 98.40(13) . . ?
C34 P2 Rh1 113.40(10) . . ?
C28 P2 Rh1 121.20(10) . . ?
C15 P2 Rh1 111.24(9) . . ?
C1 N1 C5 120.3(2) . . ?
C1 N1 Al1 124.11(19) . . ?
C5 N1 Al1 115.58(19) . . ?
C10 N2 C6 121.5(2) . . ?
C10 N2 Al1 119.04(18) . . ?
C6 N2 Al1 118.60(19) . . ?
C15 N3 C11 119.7(2) . . ?
C15 N3 Al1 124.83(19) . . ?
C11 N3 Al1 115.48(18) . . ?
N1 C1 C2 120.7(3) . . ?
N1 C1 P1 115.2(2) . . ?
C2 C1 P1 124.1(2) . . ?
C3 C2 C1 118.7(3) . . ?
C3 C2 H1 120.6 . . ?
C1 C2 H1 120.6 . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H2 120.0 . . ?
C2 C3 H2 120.0 . . ?
C3 C4 C5 118.7(3) . . ?
C3 C4 H3 120.6 . . ?
C5 C4 H3 120.6 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 113.3(2) . . ?
C4 C5 C6 125.0(3) . . ?
N2 C6 C7 120.2(3) . . ?
N2 C6 C5 112.7(2) . . ?
C7 C6 C5 127.1(3) . . ?
C8 C7 C6 118.6(3) . . ?
C8 C7 H4 120.7 . . ?
C6 C7 H4 120.7 . . ?
C7 C8 C9 120.8(3) . . ?
C7 C8 H5 119.6 . . ?
C9 C8 H5 119.6 . . ?
C10 C9 C8 117.5(3) . . ?
C10 C9 H6 121.3 . . ?
C8 C9 H6 121.3 . . ?
N2 C10 C9 121.3(3) . . ?
N2 C10 C11 112.4(2) . . ?
C9 C10 C11 126.2(3) . . ?
N3 C11 C12 121.8(3) . . ?
N3 C11 C10 113.0(2) . . ?
C12 C11 C10 125.0(3) . . ?
C11 C12 C13 118.6(3) . . ?
C11 C12 H7 120.7 . . ?
C13 C12 H7 120.7 . . ?
C14 C13 C12 119.3(3) . . ?
C14 C13 H8 120.3 . . ?
C12 C13 H8 120.3 . . ?
C13 C14 C15 119.3(3) . . ?
C13 C14 H9 120.3 . . ?
C15 C14 H9 120.3 . . ?
N3 C15 C14 121.1(3) . . ?
N3 C15 P2 115.7(2) . . ?
C14 C15 P2 123.2(2) . . ?
C17 C16 C21 119.7(3) . . ?
C17 C16 P1 119.0(2) . . ?
C21 C16 P1 121.1(2) . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H10 120.2 . . ?
C18 C17 H10 120.2 . . ?
C19 C18 C17 120.7(3) . . ?
C19 C18 H11 119.7 . . ?
C17 C18 H11 119.7 . . ?
C18 C19 C20 119.9(3) . . ?
C18 C19 H12 120.0 . . ?
C20 C19 H12 120.0 . . ?
C19 C20 C21 119.9(3) . . ?
C19 C20 H13 120.0 . . ?
C21 C20 H13 120.0 . . ?
C16 C21 C20 120.0(3) . . ?
C16 C21 H14 120.0 . . ?
C20 C21 H14 120.0 . . ?
C27 C22 C23 119.7(3) . . ?
C27 C22 P1 123.0(2) . . ?
C23 C22 P1 116.8(2) . . ?
C24 C23 C22 119.8(3) . . ?
C24 C23 H15 120.1 . . ?
C22 C23 H15 120.1 . . ?
C23 C24 C25 119.9(3) . . ?
C23 C24 H16 120.1 . . ?
C25 C24 H16 120.1 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H17 119.8 . . ?
C24 C25 H17 119.8 . . ?
C25 C26 C27 120.3(3) . . ?
C25 C26 H18 119.8 . . ?
C27 C26 H18 119.8 . . ?
C26 C27 C22 119.9(3) . . ?
C26 C27 H19 120.1 . . ?
C22 C27 H19 120.1 . . ?
C33 C28 C29 119.4(3) . . ?
C33 C28 P2 115.5(2) . . ?
C29 C28 P2 124.8(3) . . ?
C30 C29 C28 119.2(4) . . ?
C30 C29 H20 120.4 . . ?
C28 C29 H20 120.4 . . ?
C31 C30 C29 120.7(4) . . ?
C31 C30 H21 119.6 . . ?
C29 C30 H21 119.6 . . ?
C30 C31 C32 120.4(4) . . ?
C30 C31 H22 119.8 . . ?
C32 C31 H22 119.8 . . ?
C33 C32 C31 119.9(4) . . ?
C33 C32 H23 120.1 . . ?
C31 C32 H23 120.1 . . ?
C32 C33 C28 120.4(3) . . ?
C32 C33 H24 119.8 . . ?
C28 C33 H24 119.8 . . ?
C39 C34 C35 119.4(3) . . ?
C39 C34 P2 122.3(2) . . ?
C35 C34 P2 118.1(2) . . ?
C36 C35 C34 120.3(3) . . ?
C36 C35 H25 119.8 . . ?
C34 C35 H25 119.8 . . ?
C37 C36 C35 120.1(3) . . ?
C37 C36 H26 120.0 . . ?
C35 C36 H26 120.0 . . ?
C36 C37 C38 120.0(3) . . ?
C36 C37 H27 120.0 . . ?
C38 C37 H27 120.0 . . ?
C39 C38 C37 120.2(3) . . ?
C39 C38 H28 119.9 . . ?
C37 C38 H28 119.9 . . ?
C38 C39 C34 120.0(3) . . ?
C38 C39 H29 120.0 . . ?
C34 C39 H29 120.0 . . ?
O1 C40 N4 125.8(4) . . ?
O1 C40 H30 117.1 . . ?
N4 C40 H30 117.1 . . ?
C40 N4 C41 120.9(4) . . ?
C40 N4 C42 122.0(4) . . ?
C41 N4 C42 117.1(4) . . ?
N4 C41 H31 109.5 . . ?
N4 C41 H32 109.5 . . ?
H31 C41 H32 109.5 . . ?
N4 C41 H33 109.5 . . ?
H31 C41 H33 109.5 . . ?
H32 C41 H33 109.5 . . ?
N4 C42 H34 109.5 . . ?
N4 C42 H35 109.5 . . ?
H34 C42 H35 109.5 . . ?
N4 C42 H36 109.5 . . ?
H34 C42 H36 109.5 . . ?
H35 C42 H36 109.5 . . ?
O2 C43 N5 125.5(5) . . ?
O2 C43 H37 117.3 . . ?
N5 C43 H37 117.3 . . ?
C43 N5 C44 121.9(4) . . ?
C43 N5 C45 121.3(4) . . ?
C44 N5 C45 116.8(4) . . ?
N5 C44 H38 109.5 . . ?
N5 C44 H39 109.5 . . ?
H38 C44 H39 109.5 . . ?
N5 C44 H40 109.5 . . ?
H38 C44 H40 109.5 . . ?
H39 C44 H40 109.5 . . ?
N5 C45 H41 109.5 . . ?
N5 C45 H42 109.5 . . ?
H41 C45 H42 109.5 . . ?
N5 C45 H43 109.5 . . ?
H41 C45 H43 109.5 . . ?
H42 C45 H43 109.5 . . ?
O3 C46 H44 109.5 . . ?
O3 C46 H45 109.5 . . ?
H44 C46 H45 109.5 . . ?
O3 C46 H46 109.5 . . ?
H44 C46 H46 109.5 . . ?
H45 C46 H46 109.5 . . ?
C46 O3 H50 109.5 . . ?
O4 C47 H47 109.5 . . ?
O4 C47 H48 109.5 . . ?
H47 C47 H48 109.5 . . ?
O4 C47 H49 109.5 . . ?
H47 C47 H49 109.5 . . ?
H48 C47 H49 109.5 . . ?
C47 O4 H51 109.5 . . ?
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 P1 2.3004(7) . ?
Rh1 P2 2.3048(7) . ?
Rh1 Cl1 2.3060(7) . ?
Rh1 Cl2 2.3523(7) . ?
Rh1 Al1 2.4230(8) . ?
Al1 N2 1.957(2) . ?
Al1 N1 2.035(2) . ?
Al1 N3 2.039(2) . ?
Al1 Cl3 2.1946(11) . ?
Al1 Cl2 2.4086(11) . ?
P1 C22 1.809(3) . ?
P1 C16 1.822(3) . ?
P1 C1 1.838(3) . ?
P2 C34 1.813(3) . ?
P2 C28 1.820(3) . ?
P2 C15 1.840(3) . ?
N1 C1 1.336(4) . ?
N1 C5 1.354(3) . ?
N2 C10 1.338(4) . ?
N2 C6 1.345(3) . ?
N3 C15 1.342(3) . ?
N3 C11 1.356(4) . ?
C1 C2 1.404(4) . ?
C2 C3 1.391(4) . ?
C2 H1 0.9500 . ?
C3 C4 1.375(4) . ?
C3 H2 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H3 0.9500 . ?
C5 C6 1.465(4) . ?
C6 C7 1.387(4) . ?
C7 C8 1.385(4) . ?
C7 H4 0.9500 . ?
C8 C9 1.394(4) . ?
C8 H5 0.9500 . ?
C9 C10 1.386(4) . ?
C9 H6 0.9500 . ?
C10 C11 1.471(4) . ?
C11 C12 1.379(4) . ?
C12 C13 1.394(4) . ?
C12 H7 0.9500 . ?
C13 C14 1.386(4) . ?
C13 H8 0.9500 . ?
C14 C15 1.389(4) . ?
C14 H9 0.9500 . ?
C16 C17 1.389(4) . ?
C16 C21 1.394(4) . ?
C17 C18 1.390(4) . ?
C17 H10 0.9500 . ?
C18 C19 1.380(5) . ?
C18 H11 0.9500 . ?
C19 C20 1.384(5) . ?
C19 H12 0.9500 . ?
C20 C21 1.396(5) . ?
C20 H13 0.9500 . ?
C21 H14 0.9500 . ?
C22 C27 1.393(4) . ?
C22 C23 1.403(4) . ?
C23 C24 1.387(4) . ?
C23 H15 0.9500 . ?
C24 C25 1.390(5) . ?
C24 H16 0.9500 . ?
C25 C26 1.381(5) . ?
C25 H17 0.9500 . ?
C26 C27 1.387(5) . ?
C26 H18 0.9500 . ?
C27 H19 0.9500 . ?
C28 C33 1.391(5) . ?
C28 C29 1.400(4) . ?
C29 C30 1.383(5) . ?
C29 H20 0.9500 . ?
C30 C31 1.372(6) . ?
C30 H21 0.9500 . ?
C31 C32 1.379(6) . ?
C31 H22 0.9500 . ?
C32 C33 1.378(5) . ?
C32 H23 0.9500 . ?
C33 H24 0.9500 . ?
C34 C39 1.392(4) . ?
C34 C35 1.397(4) . ?
C35 C36 1.384(5) . ?
C35 H25 0.9500 . ?
C36 C37 1.383(6) . ?
C36 H26 0.9500 . ?
C37 C38 1.389(5) . ?
C37 H27 0.9500 . ?
C38 C39 1.386(4) . ?
C38 H28 0.9500 . ?
C39 H29 0.9500 . ?
C40 O1 1.219(5) . ?
C40 N4 1.330(6) . ?
C40 H30 0.9500 . ?
N4 C41 1.437(6) . ?
N4 C42 1.443(5) . ?
C41 H31 0.9800 . ?
C41 H32 0.9800 . ?
C41 H33 0.9800 . ?
C42 H34 0.9800 . ?
C42 H35 0.9800 . ?
C42 H36 0.9800 . ?
C43 O2 1.221(5) . ?
C43 N5 1.317(6) . ?
C43 H37 0.9500 . ?
N5 C44 1.405(6) . ?
N5 C45 1.434(5) . ?
C44 H38 0.9800 . ?
C44 H39 0.9800 . ?
C44 H40 0.9800 . ?
C45 H41 0.9800 . ?
C45 H42 0.9800 . ?
C45 H43 0.9800 . ?
C46 O3 1.390(6) . ?
C46 H44 0.9800 . ?
C46 H45 0.9800 . ?
C46 H46 0.9800 . ?
O3 H50 0.8400 . ?
C47 O4 1.432(5) . ?
C47 H47 0.9800 . ?
C47 H48 0.9800 . ?
C47 H49 0.9800 . ?
O4 H51 0.8400 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 1.4(4) . . . . ?
Al1 N1 C1 C2 179.5(2) . . . . ?
C5 N1 C1 P1 -179.7(2) . . . . ?
Al1 N1 C1 P1 -1.6(3) . . . . ?
C22 P1 C1 N1 134.3(2) . . . . ?
C16 P1 C1 N1 -115.7(2) . . . . ?
Rh1 P1 C1 N1 14.3(2) . . . . ?
C22 P1 C1 C2 -46.8(3) . . . . ?
C16 P1 C1 C2 63.2(3) . . . . ?
Rh1 P1 C1 C2 -166.8(2) . . . . ?
N1 C1 C2 C3 -1.0(4) . . . . ?
P1 C1 C2 C3 -179.8(2) . . . . ?
C1 C2 C3 C4 -0.4(5) . . . . ?
C2 C3 C4 C5 1.4(5) . . . . ?
C1 N1 C5 C4 -0.4(4) . . . . ?
Al1 N1 C5 C4 -178.7(2) . . . . ?
C1 N1 C5 C6 176.5(2) . . . . ?
Al1 N1 C5 C6 -1.8(3) . . . . ?
C3 C4 C5 N1 -1.0(4) . . . . ?
C3 C4 C5 C6 -177.5(3) . . . . ?
C10 N2 C6 C7 1.8(4) . . . . ?
Al1 N2 C6 C7 -167.7(2) . . . . ?
C10 N2 C6 C5 -177.6(2) . . . . ?
Al1 N2 C6 C5 13.0(3) . . . . ?
N1 C5 C6 N2 -6.8(3) . . . . ?
C4 C5 C6 N2 170.0(3) . . . . ?
N1 C5 C6 C7 174.0(3) . . . . ?
C4 C5 C6 C7 -9.3(5) . . . . ?
N2 C6 C7 C8 -0.9(4) . . . . ?
C5 C6 C7 C8 178.3(3) . . . . ?
C6 C7 C8 C9 -0.7(4) . . . . ?
C7 C8 C9 C10 1.4(4) . . . . ?
C6 N2 C10 C9 -1.0(4) . . . . ?
Al1 N2 C10 C9 168.4(2) . . . . ?
C6 N2 C10 C11 176.3(2) . . . . ?
Al1 N2 C10 C11 -14.3(3) . . . . ?
C8 C9 C10 N2 -0.6(4) . . . . ?
C8 C9 C10 C11 -177.5(3) . . . . ?
C15 N3 C11 C12 2.8(4) . . . . ?
Al1 N3 C11 C12 -177.1(2) . . . . ?
C15 N3 C11 C10 -172.8(2) . . . . ?
Al1 N3 C11 C10 7.4(3) . . . . ?
N2 C10 C11 N3 3.9(3) . . . . ?
C9 C10 C11 N3 -179.0(3) . . . . ?
N2 C10 C11 C12 -171.5(3) . . . . ?
C9 C10 C11 C12 5.6(5) . . . . ?
N3 C11 C12 C13 -2.1(4) . . . . ?
C10 C11 C12 C13 172.9(3) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C12 C13 C14 C15 1.5(5) . . . . ?
C11 N3 C15 C14 -1.2(4) . . . . ?
Al1 N3 C15 C14 178.7(2) . . . . ?
C11 N3 C15 P2 178.7(2) . . . . ?
Al1 N3 C15 P2 -1.4(3) . . . . ?
C13 C14 C15 N3 -0.9(5) . . . . ?
C13 C14 C15 P2 179.2(2) . . . . ?
C34 P2 C15 N3 -128.0(2) . . . . ?
C28 P2 C15 N3 122.1(2) . . . . ?
Rh1 P2 C15 N3 -6.2(2) . . . . ?
C34 P2 C15 C14 51.9(3) . . . . ?
C28 P2 C15 C14 -58.0(3) . . . . ?
Rh1 P2 C15 C14 173.7(2) . . . . ?
C22 P1 C16 C17 -158.1(2) . . . . ?
C1 P1 C16 C17 92.3(2) . . . . ?
Rh1 P1 C16 C17 -30.6(3) . . . . ?
C22 P1 C16 C21 26.3(3) . . . . ?
C1 P1 C16 C21 -83.2(3) . . . . ?
Rh1 P1 C16 C21 153.8(2) . . . . ?
C21 C16 C17 C18 -1.7(4) . . . . ?
P1 C16 C17 C18 -177.3(2) . . . . ?
C16 C17 C18 C19 0.5(5) . . . . ?
C17 C18 C19 C20 1.1(5) . . . . ?
C18 C19 C20 C21 -1.6(5) . . . . ?
C17 C16 C21 C20 1.2(5) . . . . ?
P1 C16 C21 C20 176.7(3) . . . . ?
C19 C20 C21 C16 0.4(5) . . . . ?
C16 P1 C22 C27 -129.3(3) . . . . ?
C1 P1 C22 C27 -23.8(3) . . . . ?
Rh1 P1 C22 C27 96.7(3) . . . . ?
C16 P1 C22 C23 58.8(3) . . . . ?
C1 P1 C22 C23 164.3(2) . . . . ?
Rh1 P1 C22 C23 -75.2(2) . . . . ?
C27 C22 C23 C24 0.9(5) . . . . ?
P1 C22 C23 C24 173.1(3) . . . . ?
C22 C23 C24 C25 -0.1(5) . . . . ?
C23 C24 C25 C26 -0.5(6) . . . . ?
C24 C25 C26 C27 0.2(6) . . . . ?
C25 C26 C27 C22 0.6(6) . . . . ?
C23 C22 C27 C26 -1.2(5) . . . . ?
P1 C22 C27 C26 -172.9(3) . . . . ?
C34 P2 C28 C33 -179.8(2) . . . . ?
C15 P2 C28 C33 -73.3(3) . . . . ?
Rh1 P2 C28 C33 47.9(3) . . . . ?
C34 P2 C28 C29 -5.3(3) . . . . ?
C15 P2 C28 C29 101.2(3) . . . . ?
Rh1 P2 C28 C29 -137.6(3) . . . . ?
C33 C28 C29 C30 -0.1(5) . . . . ?
P2 C28 C29 C30 -174.4(3) . . . . ?
C28 C29 C30 C31 0.9(6) . . . . ?
C29 C30 C31 C32 -1.2(6) . . . . ?
C30 C31 C32 C33 0.6(6) . . . . ?
C31 C32 C33 C28 0.2(6) . . . . ?
C29 C28 C33 C32 -0.5(5) . . . . ?
P2 C28 C33 C32 174.4(3) . . . . ?
C28 P2 C34 C39 129.3(3) . . . . ?
C15 P2 C34 C39 26.1(3) . . . . ?
Rh1 P2 C34 C39 -94.3(3) . . . . ?
C28 P2 C34 C35 -55.7(3) . . . . ?
C15 P2 C34 C35 -158.9(3) . . . . ?
Rh1 P2 C34 C35 80.7(3) . . . . ?
C39 C34 C35 C36 -0.9(5) . . . . ?
P2 C34 C35 C36 -176.0(3) . . . . ?
C34 C35 C36 C37 0.8(6) . . . . ?
C35 C36 C37 C38 -0.5(6) . . . . ?
C36 C37 C38 C39 0.3(6) . . . . ?
C37 C38 C39 C34 -0.4(5) . . . . ?
C35 C34 C39 C38 0.7(5) . . . . ?
P2 C34 C39 C38 175.6(2) . . . . ?
O1 C40 N4 C41 1.0(7) . . . . ?
O1 C40 N4 C42 -177.1(5) . . . . ?
O2 C43 N5 C44 179.0(5) . . . . ?
O2 C43 N5 C45 -0.1(8) . . . . ?
