#------------------------------------------------------------------------------
#$Date: 2020-09-24 02:14:04 +0300 (Thu, 24 Sep 2020) $
#$Revision: 256681 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/88/4038832.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_4038832
loop_
_publ_author_name
'Moritz, Jan-Ole'
'Chakrabortty, Soumyadeep'
'Müller, Bernd H'
'Spannenberg, Anke'
'Kamer, Paul C. J.'
_publ_section_title
;
 P-chirogenic Diphosphazanes with Axially Chiral Substituents and their
 Use in Rh-catalyzed Asymmetric Hydrogenation.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01108
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H54 N2 O4 P4 Rh, B F4'
_chemical_formula_sum            'C40 H54 B F4 N2 O4 P4 Rh'
_chemical_formula_weight         940.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.2616(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8041(6)
_cell_length_b                   15.3336(8)
_cell_length_c                   13.3346(7)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      4.19
_cell_volume                     2158.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24957
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.687
_diffrn_reflns_theta_max         66.687
_diffrn_reflns_theta_min         3.392
_exptl_absorpt_coefficient_mu    5.100
_exptl_absorpt_correction_T_max  0.41
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 3495 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0460P)²+0.9520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                7502
_reflns_number_total             7515
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo0c01108_si_005.cif
_cod_data_source_block           AX1794
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4038832
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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
B1 B 0.0349(4) 0.3223(2) 0.1477(3) 0.0365(10) Uani 1 1 d D . . . .
C1 C 0.4991(3) 0.4684(3) 0.9870(3) 0.0258(7) Uani 1 1 d . . . . .
H1 H 0.4182 0.4840 1.0076 0.031 Uiso 1 1 calc R U . . .
C2 C 0.6057(3) 0.5139(3) 1.0618(2) 0.0260(7) Uani 1 1 d D . . . .
C3 C 0.5954(4) 0.6024(3) 1.0813(3) 0.0324(8) Uani 1 1 d D . . . .
H3 H 0.5220 0.6333 1.0479 0.039 Uiso 1 1 calc R U . . .
C4 C 0.6907(4) 0.6464(3) 1.1489(3) 0.0382(9) Uani 1 1 d . . . . .
H4 H 0.6818 0.7069 1.1614 0.046 Uiso 1 1 calc R U . . .
C5 C 0.7984(4) 0.6025(3) 1.1981(3) 0.0355(9) Uani 1 1 d . . . . .
H5 H 0.8642 0.6326 1.2436 0.043 Uiso 1 1 calc R U . . .
C6 C 0.8091(3) 0.5142(3) 1.1801(3) 0.0348(8) Uani 1 1 d . . . . .
H6 H 0.8824 0.4834 1.2139 0.042 Uiso 1 1 calc R U . . .
C7 C 0.7128(4) 0.4700(3) 1.1125(3) 0.0299(8) Uani 1 1 d D . . . .
H7 H 0.7209 0.4093 1.1014 0.036 Uiso 1 1 calc R U . . .
C8 C 0.5081(4) 0.3693(3) 0.9885(3) 0.0326(8) Uani 1 1 d . . . . .
H8A H 0.4348 0.3448 0.9407 0.049 Uiso 1 1 calc R U . . .
H8B H 0.5092 0.3480 1.0580 0.049 Uiso 1 1 calc R U . . .
H8C H 0.5860 0.3513 0.9678 0.049 Uiso 1 1 calc R U . . .
C9 C 0.2719(4) 0.6162(3) 0.8015(3) 0.0272(8) Uani 1 1 d . . . . .
C10 C 0.2365(5) 0.6225(3) 0.9063(3) 0.0410(11) Uani 1 1 d . . . . .
H10A H 0.3128 0.6156 0.9605 0.061 Uiso 1 1 calc R U . . .
H10B H 0.1758 0.5763 0.9124 0.061 Uiso 1 1 calc R U . . .
H10C H 0.1982 0.6795 0.9131 0.061 Uiso 1 1 calc R U . . .
C11 C 0.1509(4) 0.6178(3) 0.7168(3) 0.0333(9) Uani 1 1 d . . . . .
H11A H 0.0951 0.5699 0.7278 0.050 Uiso 1 1 calc R U . . .
H11B H 0.1733 0.6109 0.6498 0.050 Uiso 1 1 calc R U . . .
H11C H 0.1072 0.6735 0.7188 0.050 Uiso 1 1 calc R U . . .
C12 C 0.3576(4) 0.6927(3) 0.7869(4) 0.0381(9) Uani 1 1 d . . . . .
H12A H 0.3117 0.7477 0.7885 0.057 Uiso 1 1 calc R U . . .
H12B H 0.3823 0.6869 0.7206 0.057 Uiso 1 1 calc R U . . .
H12C H 0.4335 0.6925 0.8422 0.057 Uiso 1 1 calc R U . . .
C13 C 0.2447(4) 0.4272(3) 0.7855(2) 0.0250(8) Uani 1 1 d D . . . .
C14 C 0.1942(4) 0.4057(3) 0.8707(3) 0.0330(9) Uani 1 1 d D . . . .
H14 H 0.2260 0.4331 0.9348 0.040 Uiso 1 1 calc R U . . .
C15 C 0.0981(4) 0.3446(3) 0.8620(3) 0.0383(10) Uani 1 1 d . . . . .
H15 H 0.0663 0.3288 0.9207 0.046 Uiso 1 1 calc R U . . .
C16 C 0.0481(4) 0.3064(3) 0.7679(4) 0.0385(9) Uani 1 1 d . . . . .
H16 H -0.0210 0.2669 0.7613 0.046 Uiso 1 1 calc R U . . .
C17 C 0.0987(4) 0.3258(3) 0.6841(3) 0.0364(9) Uani 1 1 d . . . . .
H17 H 0.0658 0.2985 0.6200 0.044 Uiso 1 1 calc R U . . .
C18 C 0.1972(3) 0.3847(3) 0.6928(3) 0.0285(8) Uani 1 1 d D . . . .
H18 H 0.2329 0.3965 0.6350 0.034 Uiso 1 1 calc R U . . .
C19 C 0.8135(4) 0.5770(4) 0.9138(3) 0.0405(11) Uani 1 1 d . . . . .
H19A H 0.8162 0.5807 0.9884 0.049 Uiso 1 1 calc R U . . .
H19B H 0.8791 0.6162 0.8970 0.049 Uiso 1 1 calc R U . . .
C20 C 0.8344(4) 0.4847(4) 0.8832(4) 0.0423(11) Uani 1 1 d . . . . .
H20A H 0.8781 0.4838 0.8250 0.051 Uiso 1 1 calc R U . . .
H20B H 0.8867 0.4525 0.9414 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4604(3) 0.5181(3) 0.3211(2) 0.0211(6) Uani 1 1 d . . . . .
H21 H 0.5435 0.5395 0.3092 0.025 Uiso 1 1 calc R U . . .
C22 C 0.3578(2) 0.57353(15) 0.25336(17) 0.0283(8) Uani 1 1 d G . . . .
C23 C 0.2512(2) 0.53536(15) 0.19243(19) 0.0396(9) Uani 1 1 d G . . . .
H23 H 0.2405 0.4739 0.1930 0.047 Uiso 1 1 calc R U . . .
C24 C 0.1602(2) 0.5872(2) 0.13068(19) 0.0500(13) Uani 1 1 d G . . . .
H24 H 0.0873 0.5611 0.0890 0.060 Uiso 1 1 calc R U . . .
C25 C 0.1758(3) 0.6771(2) 0.1299(2) 0.0570(16) Uani 1 1 d G . . . .
H25 H 0.1135 0.7125 0.0876 0.068 Uiso 1 1 calc R U . . .
C26 C 0.2824(3) 0.71528(14) 0.1908(2) 0.0542(14) Uani 1 1 d G . . . .
H26 H 0.2930 0.7768 0.1902 0.065 Uiso 1 1 calc R U . . .
C27 C 0.3734(2) 0.66349(16) 0.2525(2) 0.0399(10) Uani 1 1 d G . . . .
H27 H 0.4463 0.6896 0.2942 0.048 Uiso 1 1 calc R U . . .
C28 C 0.4529(4) 0.4215(3) 0.2938(3) 0.0287(8) Uani 1 1 d . . . . .
H28A H 0.5202 0.3899 0.3406 0.043 Uiso 1 1 calc R U . . .
H28B H 0.4634 0.4140 0.2231 0.043 Uiso 1 1 calc R U . . .
H28C H 0.3702 0.3985 0.3001 0.043 Uiso 1 1 calc R U . . .
C29 C 0.6770(4) 0.6427(3) 0.5345(3) 0.0277(8) Uani 1 1 d . . . . .
C30 C 0.7238(5) 0.6648(3) 0.4371(3) 0.0424(11) Uani 1 1 d . . . . .
H30A H 0.7529 0.7255 0.4403 0.064 Uiso 1 1 calc R U . . .
H30B H 0.6544 0.6571 0.3771 0.064 Uiso 1 1 calc R U . . .
H30C H 0.7940 0.6260 0.4313 0.064 Uiso 1 1 calc R U . . .
C31 C 0.7911(5) 0.6384(4) 0.6244(4) 0.0486(12) Uani 1 1 d . . . . .
H31A H 0.8497 0.5932 0.6110 0.073 Uiso 1 1 calc R U . . .
H31B H 0.7624 0.6241 0.6874 0.073 Uiso 1 1 calc R U . . .
H31C H 0.8343 0.6949 0.6324 0.073 Uiso 1 1 calc R U . . .
C32 C 0.5842(5) 0.7134(3) 0.5535(4) 0.0458(11) Uani 1 1 d . . . . .
H32A H 0.5577 0.7012 0.6179 0.069 Uiso 1 1 calc R U . . .
H32B H 0.5099 0.7137 0.4967 0.069 Uiso 1 1 calc R U . . .
H32C H 0.6259 0.7705 0.5580 0.069 Uiso 1 1 calc R U . . .
C33 C 0.6949(3) 0.4484(2) 0.5135(2) 0.0225(7) Uani 1 1 d D . . . .
C34 C 0.7005(4) 0.3767(2) 0.5788(3) 0.0283(8) Uani 1 1 d D . . . .
H34 H 0.6613 0.3797 0.6360 0.034 Uiso 1 1 calc R U . . .
C35 C 0.7628(4) 0.3012(3) 0.5609(3) 0.0362(9) Uani 1 1 d . . . . .
H35 H 0.7655 0.2525 0.6053 0.043 Uiso 1 1 calc R U . . .
C36 C 0.8211(4) 0.2970(3) 0.4781(3) 0.0342(9) Uani 1 1 d . . . . .
H36 H 0.8626 0.2448 0.4652 0.041 Uiso 1 1 calc R U . . .
C37 C 0.8193(4) 0.3678(3) 0.4143(3) 0.0307(8) Uani 1 1 d . . . . .
H37 H 0.8610 0.3647 0.3584 0.037 Uiso 1 1 calc R U . . .
C38 C 0.7566(3) 0.4437(3) 0.4313(3) 0.0283(8) Uani 1 1 d D . . . .
H38 H 0.7556 0.4924 0.3872 0.034 Uiso 1 1 calc R U . . .
C39 C 0.1211(4) 0.5508(4) 0.4031(4) 0.0518(15) Uani 1 1 d . . . . .
H39A H 0.1070 0.5689 0.3303 0.062 Uiso 1 1 calc R U . . .
H39B H 0.0478 0.5702 0.4311 0.062 Uiso 1 1 calc R U . . .
C40 C 0.1352(5) 0.4543(4) 0.4117(4) 0.0560(15) Uani 1 1 d . . . . .
H40A H 0.0816 0.4309 0.4571 0.067 Uiso 1 1 calc R U . . .
H40B H 0.1083 0.4270 0.3432 0.067 Uiso 1 1 calc R U . . .
F1 F 0.1579(4) 0.3159(3) 0.2046(4) 0.0971(15) Uani 1 1 d D . . . .
F2 F 0.0150(4) 0.2511(3) 0.0851(3) 0.0777(11) Uani 1 1 d D . . . .
F3 F -0.0462(4) 0.3232(2) 0.2148(3) 0.0783(11) Uani 1 1 d D . . . .
F4 F 0.0278(3) 0.3992(2) 0.0939(3) 0.0700(9) Uani 1 1 d D . . . .
N1 N 0.4894(3) 0.50126(18) 0.8800(2) 0.0226(7) Uani 1 1 d . . . . .
N2 N 0.4623(2) 0.5323(2) 0.43276(18) 0.0185(5) Uani 1 1 d . . . . .
O1 O 0.6877(3) 0.60092(19) 0.8546(2) 0.0300(6) Uani 1 1 d . . . . .
O2 O 0.7092(3) 0.4456(2) 0.8534(2) 0.0301(6) Uani 1 1 d . . . . .
O3 O 0.2359(3) 0.5889(2) 0.4606(2) 0.0328(7) Uani 1 1 d . . . . .
O4 O 0.2661(3) 0.43528(19) 0.4535(2) 0.0322(7) Uani 1 1 d . . . . .
P1 P 0.35748(7) 0.51449(7) 0.78139(6) 0.01966(18) Uani 1 1 d . . . . .
P2 P 0.60241(7) 0.51814(7) 0.81298(6) 0.01998(17) Uani 1 1 d . . . . .
P3 P 0.59220(7) 0.53724(6) 0.53477(6) 0.01858(19) Uani 1 1 d . . . . .
P4 P 0.34777(6) 0.51955(7) 0.49928(5) 0.01785(16) Uani 1 1 d . . . . .
Rh1 Rh 0.47348(2) 0.52290(2) 0.65672(2) 0.01742(8) 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 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh 0.0927 3.6045 '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
F2 B1 F4 112.6(4) . . ?
F2 B1 F3 111.5(3) . . ?
F4 B1 F3 110.9(3) . . ?
F2 B1 F1 106.7(4) . . ?
F4 B1 F1 106.7(3) . . ?
F3 B1 F1 108.2(4) . . ?
N1 C1 C8 109.9(3) . . ?
N1 C1 C2 111.1(3) . . ?
C8 C1 C2 114.3(3) . . ?
N1 C1 H1 107.0 . . ?
C8 C1 H1 107.0 . . ?
C2 C1 H1 107.0 . . ?
C7 C2 C3 118.3(4) . . ?
C7 C2 C1 122.3(4) . . ?
C3 C2 C1 119.4(3) . . ?
C2 C3 C4 121.2(4) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.1(4) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C7 120.5(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C2 C7 C6 120.6(4) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C1 C8 H8A 109.5 . . ?
C1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C12 110.1(4) . . ?
C10 C9 C11 109.4(3) . . ?
C12 C9 C11 109.7(3) . . ?
C10 C9 P1 114.4(3) . . ?
C12 C9 P1 106.9(3) . . ?
C11 C9 P1 106.1(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 118.3(4) . . ?
C18 C13 P1 116.1(3) . . ?
C14 C13 P1 125.2(3) . . ?
C15 C14 C13 120.4(4) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 120.2(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 119.8(4) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.3(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 120.8(3) . . ?
C17 C18 H18 119.6 . . ?
C13 C18 H18 119.6 . . ?
O1 C19 C20 105.3(4) . . ?
O1 C19 H19A 110.7 . . ?
C20 C19 H19A 110.7 . . ?
O1 C19 H19B 110.7 . . ?
C20 C19 H19B 110.7 . . ?
H19A C19 H19B 108.8 . . ?
O2 C20 C19 106.1(4) . . ?
O2 C20 H20A 110.5 . . ?
C19 C20 H20A 110.5 . . ?
O2 C20 H20B 110.5 . . ?
C19 C20 H20B 110.5 . . ?
H20A C20 H20B 108.7 . . ?
N2 C21 C28 111.6(3) . . ?
N2 C21 C22 111.2(2) . . ?
C28 C21 C22 113.8(3) . . ?
N2 C21 H21 106.6 . . ?
C28 C21 H21 106.6 . . ?
C22 C21 H21 106.6 . . ?
C23 C22 C27 120.0 . . ?
C23 C22 C21 121.2(2) . . ?
C27 C22 C21 118.8(2) . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C22 120.0 . . ?
C26 C27 H27 120.0 . . ?
C22 C27 H27 120.0 . . ?
C21 C28 H28A 109.5 . . ?
C21 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C21 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31 C29 C30 108.6(3) . . ?
C31 C29 C32 110.4(4) . . ?
C30 C29 C32 109.2(4) . . ?
C31 C29 P3 106.0(3) . . ?
C30 C29 P3 116.5(3) . . ?
C32 C29 P3 105.9(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 118.8(3) . . ?
C34 C33 P3 116.2(2) . . ?
C38 C33 P3 124.6(3) . . ?
C35 C34 C33 120.7(3) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C36 C35 C34 119.8(4) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C37 C36 C35 120.5(4) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 120.2(3) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C33 120.0(3) . . ?
C37 C38 H38 120.0 . . ?
C33 C38 H38 120.0 . . ?
O3 C39 C40 107.5(4) . . ?
O3 C39 H39A 110.2 . . ?
C40 C39 H39A 110.2 . . ?
O3 C39 H39B 110.2 . . ?
C40 C39 H39B 110.2 . . ?
H39A C39 H39B 108.5 . . ?
O4 C40 C39 107.9(4) . . ?
O4 C40 H40A 110.1 . . ?
C39 C40 H40A 110.1 . . ?
O4 C40 H40B 110.1 . . ?
C39 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?
C1 N1 P2 130.4(2) . . ?
C1 N1 P1 130.0(2) . . ?
P2 N1 P1 98.76(15) . . ?
C21 N2 P4 130.5(2) . . ?
C21 N2 P3 128.5(2) . . ?
P4 N2 P3 98.90(13) . . ?
C19 O1 P2 112.9(3) . . ?
C20 O2 P2 111.4(3) . . ?
C39 O3 P4 114.0(3) . . ?
C40 O4 P4 113.5(3) . . ?
N1 P1 C13 109.84(16) . . ?
N1 P1 C9 110.01(16) . . ?
C13 P1 C9 104.83(16) . . ?
N1 P1 Rh1 93.93(10) . . ?
C13 P1 Rh1 122.49(11) . . ?
C9 P1 Rh1 115.02(13) . . ?
C13 P1 P2 132.76(13) . . ?
C9 P1 P2 118.68(15) . . ?
O1 P2 O2 96.48(14) . . ?
O1 P2 N1 111.64(16) . . ?
O2 P2 N1 105.41(16) . . ?
O1 P2 Rh1 119.63(12) . . ?
O2 P2 Rh1 126.26(12) . . ?
N1 P2 Rh1 96.92(10) . . ?
O1 P2 P1 124.59(13) . . ?
O2 P2 P1 132.37(13) . . ?
N2 P3 C33 105.30(15) . . ?
N2 P3 C29 110.66(17) . . ?
C33 P3 C29 109.55(18) . . ?
N2 P3 Rh1 94.07(9) . . ?
C33 P3 Rh1 119.49(11) . . ?
C29 P3 Rh1 115.88(13) . . ?
C33 P3 P4 121.62(12) . . ?
C29 P3 P4 124.97(14) . . ?
O3 P4 O4 95.45(17) . . ?
O3 P4 N2 109.95(16) . . ?
O4 P4 N2 107.40(15) . . ?
O3 P4 Rh1 123.23(13) . . ?
O4 P4 Rh1 123.14(13) . . ?
N2 P4 Rh1 97.11(9) . . ?
O3 P4 P3 130.91(13) . . ?
O4 P4 P3 127.38(12) . . ?
P4 Rh1 P2 176.66(5) . . ?
P4 Rh1 P3 69.91(3) . . ?
P2 Rh1 P3 109.37(3) . . ?
P4 Rh1 P1 111.22(3) . . ?
P2 Rh1 P1 69.63(3) . . ?
P3 Rh1 P1 177.50(4) . . ?
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
B1 F2 1.363(4) . ?
B1 F4 1.374(4) . ?
B1 F3 1.379(4) . ?
B1 F1 1.387(4) . ?
C1 N1 1.496(4) . ?
C1 C8 1.522(5) . ?
C1 C2 1.524(5) . ?
C1 H1 1.0000 . ?
C2 C7 1.385(4) . ?
C2 C3 1.390(5) . ?
C3 C4 1.391(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.398(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.527(5) . ?
C9 C12 1.532(6) . ?
C9 C11 1.535(5) . ?
C9 P1 1.862(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.395(5) . ?
C13 C14 1.401(4) . ?
C13 P1 1.818(4) . ?
C14 C15 1.385(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 O1 1.466(5) . ?
C19 C20 1.504(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 O2 1.456(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 N2 1.500(4) . ?
C21 C28 1.523(5) . ?
C21 C22 1.530(4) . ?
C21 H21 1.0000 . ?
C22 C23 1.3900 . ?
C22 C27 1.3900 . ?
C23 C24 1.3900 . ?
C23 H23 0.9500 . ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25 0.9500 . ?
C26 C27 1.3900 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C31 1.527(6) . ?
C29 C30 1.529(5) . ?
C29 C32 1.534(6) . ?
C29 P3 1.860(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.395(4) . ?
C33 C38 1.401(4) . ?
C33 P3 1.816(4) . ?
C34 C35 1.386(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.377(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 O3 1.436(6) . ?
C39 C40 1.489(9) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 O4 1.437(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
N1 P2 1.679(3) . ?
N1 P1 1.733(3) . ?
N2 P4 1.680(2) . ?
N2 P3 1.736(3) . ?
O1 P2 1.597(3) . ?
O2 P2 1.610(3) . ?
O3 P4 1.610(3) . ?
O4 P4 1.610(3) . ?
P1 Rh1 2.2883(7) . ?
P1 P2 2.5904(10) . ?
P2 Rh1 2.2483(8) . ?
P3 Rh1 2.2855(8) . ?
P3 P4 2.5964(10) . ?
P4 Rh1 2.2457(7) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C7 -114.0(4) . . . . ?
C8 C1 C2 C7 11.1(5) . . . . ?
N1 C1 C2 C3 66.9(4) . . . . ?
C8 C1 C2 C3 -168.0(3) . . . . ?
C7 C2 C3 C4 1.0(6) . . . . ?
C1 C2 C3 C4 -179.9(4) . . . . ?
C2 C3 C4 C5 0.1(7) . . . . ?
C3 C4 C5 C6 -0.9(7) . . . . ?
C4 C5 C6 C7 0.5(6) . . . . ?
C3 C2 C7 C6 -1.4(5) . . . . ?
C1 C2 C7 C6 179.5(3) . . . . ?
C5 C6 C7 C2 0.6(6) . . . . ?
C18 C13 C14 C15 -1.0(6) . . . . ?
P1 C13 C14 C15 172.6(3) . . . . ?
C13 C14 C15 C16 -2.2(6) . . . . ?
C14 C15 C16 C17 3.5(7) . . . . ?
C15 C16 C17 C18 -1.6(7) . . . . ?
C16 C17 C18 C13 -1.7(7) . . . . ?
C14 C13 C18 C17 2.9(6) . . . . ?
P1 C13 C18 C17 -171.2(3) . . . . ?
O1 C19 C20 O2 -27.9(4) . . . . ?
N2 C21 C22 C23 -111.3(3) . . . . ?
C28 C21 C22 C23 15.7(3) . . . . ?
N2 C21 C22 C27 69.5(3) . . . . ?
C28 C21 C22 C27 -163.6(2) . . . . ?
C27 C22 C23 C24 0.0 . . . . ?
C21 C22 C23 C24 -179.2(2) . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C26 C27 C22 0.0 . . . . ?
C23 C22 C27 C26 0.0 . . . . ?
C21 C22 C27 C26 179.3(2) . . . . ?
C38 C33 C34 C35 -1.9(6) . . . . ?
P3 C33 C34 C35 171.7(3) . . . . ?
C33 C34 C35 C36 0.6(6) . . . . ?
C34 C35 C36 C37 1.0(6) . . . . ?
C35 C36 C37 C38 -1.3(6) . . . . ?
C36 C37 C38 C33 -0.1(6) . . . . ?
C34 C33 C38 C37 1.6(5) . . . . ?
P3 C33 C38 C37 -171.4(3) . . . . ?
O3 C39 C40 O4 -12.9(6) . . . . ?
C8 C1 N1 P2 -81.1(4) . . . . ?
C2 C1 N1 P2 46.5(4) . . . . ?
C8 C1 N1 P1 85.8(4) . . . . ?
C2 C1 N1 P1 -146.6(3) . . . . ?
C28 C21 N2 P4 -70.7(4) . . . . ?
C22 C21 N2 P4 57.5(4) . . . . ?
C28 C21 N2 P3 89.5(4) . . . . ?
C22 C21 N2 P3 -142.3(3) . . . . ?
C20 C19 O1 P2 19.7(4) . . . . ?
C19 C20 O2 P2 26.8(4) . . . . ?
C40 C39 O3 P4 9.2(5) . . . . ?
C39 C40 O4 P4 12.2(5) . . . . ?
C1 N1 P1 C13 -36.0(3) . . . . ?
P2 N1 P1 C13 133.96(16) . . . . ?
C1 N1 P1 C9 78.9(3) . . . . ?
P2 N1 P1 C9 -111.15(19) . . . . ?
C1 N1 P1 Rh1 -162.7(3) . . . . ?
P2 N1 P1 Rh1 7.29(13) . . . . ?
C1 N1 P1 P2 -169.9(4) . . . . ?
C18 C13 P1 N1 -131.2(3) . . . . ?
C14 C13 P1 N1 55.1(4) . . . . ?
C18 C13 P1 C9 110.6(3) . . . . ?
C14 C13 P1 C9 -63.0(4) . . . . ?
C18 C13 P1 Rh1 -22.8(4) . . . . ?
C14 C13 P1 Rh1 163.6(3) . . . . ?
C18 C13 P1 P2 -92.3(3) . . . . ?
C14 C13 P1 P2 94.0(4) . . . . ?
C10 C9 P1 N1 -54.1(4) . . . . ?
C12 C9 P1 N1 68.1(3) . . . . ?
C11 C9 P1 N1 -174.8(3) . . . . ?
C10 C9 P1 C13 64.0(3) . . . . ?
C12 C9 P1 C13 -173.9(3) . . . . ?
C11 C9 P1 C13 -56.8(3) . . . . ?
C10 C9 P1 Rh1 -158.6(3) . . . . ?
C12 C9 P1 Rh1 -36.4(3) . . . . ?
C11 C9 P1 Rh1 80.7(3) . . . . ?
C10 C9 P1 P2 -97.0(3) . . . . ?
C12 C9 P1 P2 25.2(3) . . . . ?
C11 C9 P1 P2 142.3(2) . . . . ?
C19 O1 P2 O2 -4.0(3) . . . . ?
C19 O1 P2 N1 105.4(3) . . . . ?
C19 O1 P2 Rh1 -142.6(2) . . . . ?
C19 O1 P2 P1 150.4(2) . . . . ?
C20 O2 P2 O1 -14.0(3) . . . . ?
C20 O2 P2 N1 -128.6(3) . . . . ?
C20 O2 P2 Rh1 120.4(3) . . . . ?
C20 O2 P2 P1 -165.3(2) . . . . ?
C1 N1 P2 O1 -71.8(3) . . . . ?
P1 N1 P2 O1 118.27(17) . . . . ?
C1 N1 P2 O2 31.8(3) . . . . ?
P1 N1 P2 O2 -138.12(16) . . . . ?
C1 N1 P2 Rh1 162.4(3) . . . . ?
P1 N1 P2 Rh1 -7.46(13) . . . . ?
C1 N1 P2 P1 169.9(4) . . . . ?
C21 N2 P3 C33 -43.5(3) . . . . ?
P4 N2 P3 C33 121.40(16) . . . . ?
C21 N2 P3 C29 74.8(4) . . . . ?
P4 N2 P3 C29 -120.31(18) . . . . ?
C21 N2 P3 Rh1 -165.6(3) . . . . ?
P4 N2 P3 Rh1 -0.68(15) . . . . ?
C21 N2 P3 P4 -164.9(4) . . . . ?
C34 C33 P3 N2 -107.4(3) . . . . ?
C38 C33 P3 N2 65.8(3) . . . . ?
C34 C33 P3 C29 133.5(3) . . . . ?
C38 C33 P3 C29 -53.2(3) . . . . ?
C34 C33 P3 Rh1 -3.6(3) . . . . ?
C38 C33 P3 Rh1 169.6(3) . . . . ?
C34 C33 P3 P4 -67.6(3) . . . . ?
C38 C33 P3 P4 105.6(3) . . . . ?
C31 C29 P3 N2 -178.0(3) . . . . ?
C30 C29 P3 N2 -57.0(4) . . . . ?
C32 C29 P3 N2 64.7(3) . . . . ?
C31 C29 P3 C33 -62.3(3) . . . . ?
C30 C29 P3 C33 58.7(4) . . . . ?
C32 C29 P3 C33 -179.6(3) . . . . ?
C31 C29 P3 Rh1 76.5(3) . . . . ?
C30 C29 P3 Rh1 -162.5(3) . . . . ?
C32 C29 P3 Rh1 -40.8(3) . . . . ?
C31 C29 P3 P4 139.6(3) . . . . ?
C30 C29 P3 P4 -99.4(3) . . . . ?
C32 C29 P3 P4 22.3(4) . . . . ?
C39 O3 P4 O4 -2.0(3) . . . . ?
C39 O3 P4 N2 108.7(3) . . . . ?
C39 O3 P4 Rh1 -138.0(3) . . . . ?
C39 O3 P4 P3 150.8(3) . . . . ?
C40 O4 P4 O3 -6.3(3) . . . . ?
C40 O4 P4 N2 -119.2(3) . . . . ?
C40 O4 P4 Rh1 129.7(3) . . . . ?
C40 O4 P4 P3 -160.6(3) . . . . ?
C21 N2 P4 O3 -65.6(4) . . . . ?
P3 N2 P4 O3 129.95(17) . . . . ?
C21 N2 P4 O4 37.1(4) . . . . ?
P3 N2 P4 O4 -127.36(17) . . . . ?
C21 N2 P4 Rh1 165.1(3) . . . . ?
P3 N2 P4 Rh1 0.69(15) . . . . ?
C21 N2 P4 P3 164.4(4) . . . . ?
