#------------------------------------------------------------------------------
#$Date: 2021-12-03 22:48:57 +0200 (Fri, 03 Dec 2021) $
#$Revision: 271035 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/91/4519169.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_4519169
loop_
_publ_author_name
'Xue, Yuan'
'Park, Han Seul'
'Jiang, Chao'
'Yu, Jin-Quan'
_publ_section_title
;
 Palladium-Catalyzed β-C(sp3)--H Nitrooxylation of Ketones and Amides
 Using Practical Oxidants
;
_journal_issue                   22
_journal_name_full               'ACS Catalysis'
_journal_page_first              14188
_journal_page_last               14193
_journal_paper_doi               10.1021/acscatal.1c04188
_journal_volume                  11
_journal_year                    2021
_chemical_formula_sum            'C33 H28 F7 N2 O2 P Pd'
_chemical_formula_weight         754.94
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                102.4920(10)
_cell_angle_beta                 90.6450(10)
_cell_angle_gamma                99.7460(10)
_cell_formula_units_Z            4
_cell_length_a                   10.2240(3)
_cell_length_b                   15.6567(5)
_cell_length_c                   20.8337(7)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.30
_cell_volume                     3205.02(18)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23917
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.005
_exptl_absorpt_coefficient_mu    0.703
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         11187
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0290P)²+1.2850P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9179
_reflns_number_total             11187
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs1c04188_si_002.cif
_cod_data_source_block           20190905LI_NLG_JC3a_1_0m_a
_cod_database_code               4519169
_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.
;
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.939
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
C1 C 0.8313(5) 0.5291(3) 0.7518(3) 0.0557(13) Uani 1 1 d . . . . .
C2 C 0.8724(3) 0.6112(2) 0.7250(2) 0.0373(9) Uani 1 1 d . . . . .
C3 C 0.9545(3) 0.6113(2) 0.6727(2) 0.0348(9) Uani 1 1 d . . . . .
C4 C 0.9926(3) 0.6874(2) 0.64907(19) 0.0292(8) Uani 1 1 d . . . . .
C5 C 0.9524(3) 0.7672(2) 0.67567(18) 0.0256(7) Uani 1 1 d . . . . .
C6 C 0.8713(3) 0.7661(2) 0.72860(19) 0.0337(9) Uani 1 1 d . . . . .
C7 C 0.8334(3) 0.6906(2) 0.7523(2) 0.0381(9) Uani 1 1 d . . . . .
C8 C 1.0820(3) 0.9069(2) 0.68571(19) 0.0277(8) Uani 1 1 d . . . . .
C9 C 1.1325(3) 0.9834(2) 0.65357(19) 0.0313(8) Uani 1 1 d . . . . .
H9A H 1.057300 1.003520 0.636486 0.038 Uiso 1 1 calc R U . . .
H9B H 1.180747 1.032491 0.686543 0.038 Uiso 1 1 calc R U . . .
C10 C 1.2053(3) 0.8925(2) 0.49228(19) 0.0264(8) Uani 1 1 d . . . . .
C11 C 1.3491(3) 0.9283(2) 0.4870(2) 0.0420(10) Uani 1 1 d . . . . .
H11A H 1.357060 0.975797 0.464067 0.063 Uiso 1 1 calc R U . . .
H11B H 1.391801 0.881833 0.463297 0.063 Uiso 1 1 calc R U . . .
H11C H 1.390799 0.950353 0.530337 0.063 Uiso 1 1 calc R U . . .
C12 C 1.1206(3) 0.8334(2) 0.43456(19) 0.0311(8) Uani 1 1 d . . . . .
C13 C 1.1546(4) 0.8632(3) 0.3704(2) 0.0456(10) Uani 1 1 d . . . . .
H13A H 1.149832 0.925081 0.376061 0.068 Uiso 1 1 calc R U . . .
H13B H 1.092335 0.829035 0.335648 0.068 Uiso 1 1 calc R U . . .
H13C H 1.242805 0.854112 0.359251 0.068 Uiso 1 1 calc R U . . .
C14 C 1.1472(4) 0.7385(2) 0.4288(2) 0.0435(10) Uani 1 1 d . . . . .
H14A H 1.239984 0.737693 0.422827 0.065 Uiso 1 1 calc R U . . .
H14B H 1.095925 0.699479 0.391821 0.065 Uiso 1 1 calc R U . . .
H14C H 1.122326 0.718948 0.468312 0.065 Uiso 1 1 calc R U . . .
C15 C 0.9736(3) 0.8377(2) 0.44882(18) 0.0302(8) Uani 1 1 d . . . . .
H15A H 0.915930 0.786661 0.421845 0.036 Uiso 1 1 calc R U . . .
H15B H 0.950050 0.891248 0.439202 0.036 Uiso 1 1 calc R U . . .
C16 C 0.6605(3) 0.8363(2) 0.42941(18) 0.0260(8) Uani 1 1 d . . . . .
H16 H 0.712380 0.888534 0.452975 0.031 Uiso 1 1 calc R U . . .
C17 C 0.5884(3) 0.8375(2) 0.37376(19) 0.0313(8) Uani 1 1 d . . . . .
H17 H 0.591940 0.890513 0.359966 0.038 Uiso 1 1 calc R U . . .
C18 C 0.5102(3) 0.7602(2) 0.33787(19) 0.0350(9) Uani 1 1 d . . . . .
H18 H 0.461089 0.761081 0.300233 0.042 Uiso 1 1 calc R U . . .
C19 C 0.5064(3) 0.6822(2) 0.3589(2) 0.0376(9) Uani 1 1 d . . . . .
H19 H 0.454000 0.630168 0.335287 0.045 Uiso 1 1 calc R U . . .
C20 C 0.5793(3) 0.6801(2) 0.41461(19) 0.0317(8) Uani 1 1 d . . . . .
H20 H 0.576402 0.626810 0.427813 0.038 Uiso 1 1 calc R U . . .
C21 C 0.6572(3) 0.7576(2) 0.45114(18) 0.0241(7) Uani 1 1 d . . . . .
C22 C 0.8039(4) 0.5954(2) 0.4916(2) 0.0442(11) Uani 1 1 d . . . . .
H22 H 0.855229 0.618845 0.460811 0.053 Uiso 1 1 calc R U . . .
C23 C 0.7982(4) 0.5071(3) 0.4945(3) 0.0629(14) Uani 1 1 d . . . . .
H23 H 0.845501 0.471216 0.465561 0.076 Uiso 1 1 calc R U . . .
C24 C 0.7233(4) 0.4727(3) 0.5399(3) 0.0609(14) Uani 1 1 d . . . . .
H24 H 0.719118 0.413295 0.541366 0.073 Uiso 1 1 calc R U . . .
C25 C 0.6548(4) 0.5246(2) 0.5831(2) 0.0506(12) Uani 1 1 d . . . . .
H25 H 0.604958 0.500793 0.614136 0.061 Uiso 1 1 calc R U . . .
C26 C 0.6588(3) 0.6124(2) 0.5809(2) 0.0357(9) Uani 1 1 d . . . . .
H26 H 0.611859 0.647649 0.610498 0.043 Uiso 1 1 calc R U . . .
C27 C 0.7327(3) 0.6483(2) 0.53467(19) 0.0286(8) Uani 1 1 d . . . . .
C28 C 0.4913(3) 0.7735(2) 0.5768(2) 0.0409(10) Uani 1 1 d . . . . .
H28 H 0.461120 0.726837 0.541110 0.049 Uiso 1 1 calc R U . . .
C29 C 0.4014(4) 0.8076(3) 0.6196(2) 0.0515(12) Uani 1 1 d . . . . .
H29 H 0.311510 0.783128 0.613128 0.062 Uiso 1 1 calc R U . . .
C30 C 0.4436(4) 0.8760(3) 0.6708(2) 0.0657(15) Uani 1 1 d . . . . .
H30 H 0.382919 0.899264 0.699440 0.079 Uiso 1 1 calc R U . . .
C31 C 0.5758(4) 0.9114(3) 0.6806(3) 0.0787(18) Uani 1 1 d . . . . .
H31 H 0.604523 0.958844 0.715948 0.094 Uiso 1 1 calc R U . . .
C32 C 0.6675(4) 0.8773(3) 0.6384(2) 0.0493(12) Uani 1 1 d . . . . .
H32 H 0.757305 0.901611 0.645733 0.059 Uiso 1 1 calc R U . . .
C33 C 0.6259(3) 0.8080(2) 0.58612(18) 0.0272(8) Uani 1 1 d . . . . .
C34 C 0.3093(5) 0.4896(3) 0.7508(3) 0.0536(12) Uani 1 1 d . . . . .
C35 C 0.3073(3) 0.4069(2) 0.7760(2) 0.0341(9) Uani 1 1 d . . . . .
C36 C 0.3909(3) 0.4033(2) 0.8271(2) 0.0361(9) Uani 1 1 d . . . . .
C37 C 0.3899(3) 0.3268(2) 0.8497(2) 0.0325(8) Uani 1 1 d . . . . .
C38 C 0.3052(3) 0.2476(2) 0.82142(18) 0.0269(8) Uani 1 1 d . . . . .
C39 C 0.2225(3) 0.2514(2) 0.77007(19) 0.0304(8) Uani 1 1 d . . . . .
C40 C 0.2225(4) 0.3282(2) 0.74768(19) 0.0354(9) Uani 1 1 d . . . . .
C41 C 0.3697(3) 0.1109(2) 0.81153(18) 0.0266(8) Uani 1 1 d . . . . .
C42 C 0.3828(3) 0.0340(2) 0.84396(18) 0.0307(8) Uani 1 1 d . . . . .
H42A H 0.298881 0.014379 0.862014 0.037 Uiso 1 1 calc R U . . .
H42B H 0.403271 -0.015386 0.811063 0.037 Uiso 1 1 calc R U . . .
C43 C 0.5114(3) 0.1305(2) 1.00385(19) 0.0275(8) Uani 1 1 d . . . . .
C44 C 0.6426(3) 0.1019(2) 1.0092(2) 0.0360(9) Uani 1 1 d . . . . .
H44A H 0.668149 0.076061 0.966122 0.054 Uiso 1 1 calc R U . . .
H44B H 0.635568 0.058735 1.036039 0.054 Uiso 1 1 calc R U . . .
H44C H 0.708446 0.152482 1.028938 0.054 Uiso 1 1 calc R U . . .
C45 C 0.4532(3) 0.1866(2) 1.06101(19) 0.0300(8) Uani 1 1 d . . . . .
C46 C 0.5182(4) 0.2845(2) 1.0672(2) 0.0423(10) Uani 1 1 d . . . . .
H46A H 0.612732 0.290555 1.073677 0.063 Uiso 1 1 calc R U . . .
H46B H 0.484151 0.321018 1.104096 0.063 Uiso 1 1 calc R U . . .
H46C H 0.498271 0.303025 1.027713 0.063 Uiso 1 1 calc R U . . .
C47 C 0.4779(4) 0.1593(3) 1.1255(2) 0.0440(10) Uani 1 1 d . . . . .
H47A H 0.440894 0.097666 1.121135 0.066 Uiso 1 1 calc R U . . .
H47B H 0.436531 0.194581 1.160267 0.066 Uiso 1 1 calc R U . . .
H47C H 0.571758 0.168611 1.135556 0.066 Uiso 1 1 calc R U . . .
C48 C 0.3019(3) 0.1742(2) 1.04592(18) 0.0305(8) Uani 1 1 d . . . . .
H48A H 0.265867 0.223036 1.072383 0.037 Uiso 1 1 calc R U . . .
H48B H 0.257257 0.119155 1.055830 0.037 Uiso 1 1 calc R U . . .
C49 C 0.2237(4) 0.4041(2) 1.0177(2) 0.0517(12) Uani 1 1 d . . . . .
H49 H 0.253661 0.378207 1.049980 0.062 Uiso 1 1 calc R U . . .
C50 C 0.2666(4) 0.4935(3) 1.0205(3) 0.0677(16) Uani 1 1 d . . . . .
H50 H 0.325287 0.527767 1.054434 0.081 Uiso 1 1 calc R U . . .
C51 C 0.2219(4) 0.5315(3) 0.9725(3) 0.0631(16) Uani 1 1 d . . . . .
H51 H 0.249856 0.591791 0.974573 0.076 Uiso 1 1 calc R U . . .
C52 C 0.1366(4) 0.4815(3) 0.9219(2) 0.0524(12) Uani 1 1 d . . . . .
H52 H 0.107416 0.507579 0.889552 0.063 Uiso 1 1 calc R U . . .
C53 C 0.0940(4) 0.3920(2) 0.9190(2) 0.0416(10) Uani 1 1 d . . . . .
H53 H 0.036657 0.357890 0.884472 0.050 Uiso 1 1 calc R U . . .
C54 C 0.1363(3) 0.3526(2) 0.96718(19) 0.0299(8) Uani 1 1 d . . . . .
C55 C -0.0343(4) 0.1182(2) 0.8510(2) 0.0421(10) Uani 1 1 d . . . . .
H55 H 0.040519 0.091340 0.848383 0.051 Uiso 1 1 calc R U . . .
C56 C -0.1386(4) 0.0845(3) 0.8044(2) 0.0551(12) Uani 1 1 d . . . . .
H56 H -0.134104 0.034681 0.771348 0.066 Uiso 1 1 calc R U . . .
C57 C -0.2494(4) 0.1249(3) 0.8071(2) 0.0548(12) Uani 1 1 d . . . . .
H57 H -0.318608 0.103347 0.775356 0.066 Uiso 1 1 calc R U . . .
C58 C -0.2564(4) 0.1965(3) 0.8567(2) 0.0509(12) Uani 1 1 d . . . . .
H58 H -0.331268 0.223239 0.858809 0.061 Uiso 1 1 calc R U . . .
C59 C -0.1542(3) 0.2297(3) 0.9036(2) 0.0423(10) Uani 1 1 d . . . . .
H59 H -0.160982 0.278306 0.937324 0.051 Uiso 1 1 calc R U . . .
C60 C -0.0401(3) 0.1909(2) 0.90110(19) 0.0316(8) Uani 1 1 d . . . . .
C61 C -0.0409(3) 0.2962(2) 1.07723(19) 0.0344(9) Uani 1 1 d . . . . .
H61 H -0.029517 0.350712 1.065114 0.041 Uiso 1 1 calc R U . . .
C62 C -0.1067(4) 0.2862(3) 1.1333(2) 0.0439(10) Uani 1 1 d . . . . .
H62 H -0.142479 0.333225 1.157568 0.053 Uiso 1 1 calc R U . . .
C63 C -0.1199(3) 0.2072(3) 1.1538(2) 0.0460(11) Uani 1 1 d . . . . .
H63 H -0.160965 0.201467 1.192586 0.055 Uiso 1 1 calc R U . . .
C64 C -0.0714(3) 0.1367(3) 1.1159(2) 0.0425(10) Uani 1 1 d . . . . .
H64 H -0.080941 0.082967 1.128965 0.051 Uiso 1 1 calc R U . . .
C65 C -0.0090(3) 0.1454(2) 1.0587(2) 0.0347(9) Uani 1 1 d . . . . .
H65 H 0.021907 0.097048 1.033210 0.042 Uiso 1 1 calc R U . . .
C66 C 0.0083(3) 0.2260(2) 1.03874(18) 0.0270(8) Uani 1 1 d . . . . .
F1 F 0.6968(5) 0.5134(4) 0.7542(4) 0.079(2) Uani 0.618(12) 1 d . U P A 1
F2 F 0.8534(10) 0.4547(4) 0.7117(5) 0.092(3) Uani 0.618(12) 1 d . U P A 1
F3 F 0.8795(10) 0.5350(4) 0.8098(4) 0.091(3) Uani 0.618(12) 1 d . U P A 1
F4 F 0.7548(2) 0.69605(16) 0.80389(13) 0.0593(7) Uani 1 1 d . U . . .
F5 F 0.8305(2) 0.84093(13) 0.75855(12) 0.0480(6) Uani 1 1 d . U . . .
F6 F 1.07244(19) 0.68196(13) 0.59815(12) 0.0423(6) Uani 1 1 d . U . . .
F7 F 1.0002(2) 0.53801(13) 0.64349(13) 0.0525(6) Uani 1 1 d . U . . .
F8 F 0.4762(2) 0.47650(13) 0.85759(13) 0.0562(7) Uani 1 1 d . U . . .
F9 F 0.4755(2) 0.32889(14) 0.89939(13) 0.0485(6) Uani 1 1 d . U . . .
F10 F 0.1396(2) 0.17835(13) 0.73927(12) 0.0455(6) Uani 1 1 d . U . . .
F11 F 0.1381(2) 0.32513(14) 0.69707(13) 0.0573(7) Uani 1 1 d . U . . .
F14 F 0.1783(12) 0.5128(8) 0.7590(7) 0.063(3) Uani 0.372(12) 1 d . U P B 1
F12 F 0.3867(16) 0.5613(7) 0.7844(8) 0.072(4) Uani 0.372(12) 1 d . U P B 1
F13 F 0.3256(18) 0.4824(7) 0.6900(6) 0.058(4) Uani 0.372(12) 1 d . U P B 1
N1 N 0.9904(3) 0.84210(17) 0.64889(15) 0.0267(6) Uani 1 1 d . . . . .
N2 N 1.1440(2) 0.90636(16) 0.54511(15) 0.0249(6) Uani 1 1 d . . . . .
N3 N 0.3047(3) 0.17074(17) 0.84645(15) 0.0284(7) Uani 1 1 d . . . . .
N4 N 0.4391(2) 0.11301(16) 0.95097(15) 0.0253(6) Uani 1 1 d . . . . .
O1 O 1.1288(3) 0.90752(17) 0.74018(14) 0.0470(7) Uani 1 1 d . . . . .
O2 O 1.2185(2) 0.95933(14) 0.60062(13) 0.0322(6) Uani 1 1 d . . . . .
O3 O 0.4228(3) 0.11366(16) 0.75909(13) 0.0417(7) Uani 1 1 d . . . . .
O4 O 0.4859(2) 0.05994(14) 0.89586(12) 0.0303(6) Uani 1 1 d . . . . .
P1 P 0.74395(7) 0.76378(5) 0.52890(5) 0.02217(19) Uani 1 1 d . . . . .
P2 P 0.09360(8) 0.23401(5) 0.96374(5) 0.0252(2) Uani 1 1 d . . . . .
Pd1 Pd 0.95391(2) 0.83798(2) 0.54604(2) 0.02165(8) Uani 1 1 d . . . . .
Pd2 Pd 0.27489(2) 0.17138(2) 0.94860(2) 0.02328(8) Uani 1 1 d . . . . .
F12B F 0.326(2) 0.5618(11) 0.8031(9) 0.043(4) Uani 0.256(16) 1 d . U P B 3
F13B F 0.412(3) 0.5058(13) 0.7135(13) 0.055(5) Uani 0.256(16) 1 d . U P B 3
F14B F 0.201(2) 0.4926(12) 0.7210(17) 0.072(6) Uani 0.256(16) 1 d . U P B 3
F1' F 0.7571(14) 0.5416(7) 0.8040(7) 0.092(5) Uani 0.382(12) 1 d . U P A 2
F2' F 0.7787(13) 0.4639(8) 0.7109(7) 0.084(4) Uani 0.382(12) 1 d . U P A 2
F3' F 0.9435(10) 0.5071(7) 0.7757(7) 0.079(4) Uani 0.382(12) 1 d . U P A 2
F12A F 0.4443(13) 0.5260(10) 0.7425(9) 0.063(4) Uani 0.372(15) 1 d . U P B 2
F13A F 0.2488(16) 0.4753(8) 0.6900(8) 0.057(4) Uani 0.372(15) 1 d . U P B 2
F14A F 0.265(2) 0.5488(9) 0.7888(8) 0.072(5) Uani 0.372(15) 1 d . U P B 2
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'
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'
Pd Pd -0.9988 1.0072 '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'
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' C1 F1' 110.1(9) . . ?
F3 C1 F2 110.2(6) . . ?
F3 C1 F1 107.2(6) . . ?
F2 C1 F1 102.0(5) . . ?
F2' C1 F3' 106.1(8) . . ?
F1' C1 F3' 103.5(9) . . ?
F2' C1 C2 114.4(7) . . ?
F3 C1 C2 114.2(4) . . ?
F1' C1 C2 113.8(5) . . ?
F2 C1 C2 113.6(5) . . ?
F1 C1 C2 108.7(4) . . ?
F3' C1 C2 108.0(5) . . ?
C7 C2 C3 116.4(3) . . ?
C7 C2 C1 121.9(4) . . ?
C3 C2 C1 121.6(4) . . ?
F7 C3 C4 117.8(3) . . ?
F7 C3 C2 121.2(3) . . ?
C4 C3 C2 121.0(3) . . ?
F6 C4 C3 117.4(3) . . ?
F6 C4 C5 119.7(3) . . ?
C3 C4 C5 123.0(3) . . ?
C4 C5 C6 115.2(3) . . ?
C4 C5 N1 121.0(3) . . ?
C6 C5 N1 123.8(3) . . ?
F5 C6 C7 118.7(3) . . ?
F5 C6 C5 119.3(3) . . ?
C7 C6 C5 122.0(3) . . ?
F4 C7 C6 117.7(3) . . ?
F4 C7 C2 119.9(3) . . ?
C6 C7 C2 122.4(3) . . ?
O1 C8 N1 126.3(3) . . ?
O1 C8 C9 118.8(3) . . ?
N1 C8 C9 114.8(3) . . ?
O2 C9 C8 112.5(3) . . ?
O2 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
O2 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 C11 124.0(3) . . ?
N2 C10 C12 113.7(3) . . ?
C11 C10 C12 122.2(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 C14 107.6(3) . . ?
C10 C12 C13 111.4(3) . . ?
C14 C12 C13 109.5(3) . . ?
C10 C12 C15 107.9(3) . . ?
C14 C12 C15 110.5(3) . . ?
C13 C12 C15 109.9(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 Pd1 106.9(2) . . ?
C12 C15 H15A 110.3 . . ?
Pd1 C15 H15A 110.3 . . ?
C12 C15 H15B 110.3 . . ?
Pd1 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
C17 C16 C21 120.9(3) . . ?
C17 C16 H16 119.5 . . ?
C21 C16 H16 119.5 . . ?
C16 C17 C18 120.5(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 119.0(4) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 120.9(3) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C19 C20 C21 120.4(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C20 C21 C16 118.3(3) . . ?
C20 C21 P1 123.6(3) . . ?
C16 C21 P1 117.9(2) . . ?
C27 C22 C23 119.6(4) . . ?
C27 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 120.2(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 120.5(4) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C27 120.2(4) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C22 C27 C26 119.2(3) . . ?
C22 C27 P1 117.9(3) . . ?
C26 C27 P1 122.9(3) . . ?
C29 C28 C33 120.9(4) . . ?
C29 C28 H28 119.6 . . ?
C33 C28 H28 119.6 . . ?
C30 C29 C28 120.1(4) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 119.9(4) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 C32 120.7(4) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 120.0(4) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C28 118.4(3) . . ?
C32 C33 P1 120.8(3) . . ?
C28 C33 P1 120.7(3) . . ?
F13 C34 F12 109.9(8) . . ?
F14B C34 F13B 110.2(13) . . ?
F14A C34 F13A 109.5(9) . . ?
F14B C34 F12B 104.7(13) . . ?
F13B C34 F12B 104.8(11) . . ?
F14A C34 F12A 105.8(9) . . ?
F13A C34 F12A 104.4(8) . . ?
F13 C34 F14 103.7(8) . . ?
F12 C34 F14 102.5(8) . . ?
F14A C34 C35 114.0(7) . . ?
F13 C34 C35 116.1(6) . . ?
F14B C34 C35 114.1(9) . . ?
F12 C34 C35 116.0(6) . . ?
F13B C34 C35 113.1(8) . . ?
F13A C34 C35 114.0(6) . . ?
F12B C34 C35 109.1(9) . . ?
F12A C34 C35 108.4(6) . . ?
F14 C34 C35 106.9(5) . . ?
C36 C35 C40 116.1(3) . . ?
C36 C35 C34 122.4(4) . . ?
C40 C35 C34 121.5(4) . . ?
F8 C36 C37 117.7(3) . . ?
F8 C36 C35 120.1(3) . . ?
C37 C36 C35 122.2(3) . . ?
F9 C37 C36 118.4(3) . . ?
F9 C37 C38 119.6(3) . . ?
C36 C37 C38 122.0(3) . . ?
C39 C38 C37 115.5(3) . . ?
C39 C38 N3 123.8(3) . . ?
C37 C38 N3 120.7(3) . . ?
F10 C39 C40 117.7(3) . . ?
F10 C39 C38 119.6(3) . . ?
C40 C39 C38 122.6(3) . . ?
F11 C40 C39 118.1(3) . . ?
F11 C40 C35 120.3(3) . . ?
C39 C40 C35 121.5(4) . . ?
O3 C41 N3 127.3(3) . . ?
O3 C41 C42 118.7(3) . . ?
N3 C41 C42 113.9(3) . . ?
O4 C42 C41 111.4(3) . . ?
O4 C42 H42A 109.4 . . ?
C41 C42 H42A 109.4 . . ?
O4 C42 H42B 109.4 . . ?
C41 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
N4 C43 C44 124.2(3) . . ?
N4 C43 C45 112.9(3) . . ?
C44 C43 C45 122.9(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 C47 111.7(3) . . ?
C43 C45 C46 108.3(3) . . ?
C47 C45 C46 109.2(3) . . ?
C43 C45 C48 107.8(3) . . ?
C47 C45 C48 109.4(3) . . ?
C46 C45 C48 110.4(3) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 Pd2 107.2(2) . . ?
C45 C48 H48A 110.3 . . ?
Pd2 C48 H48A 110.3 . . ?
C45 C48 H48B 110.3 . . ?
Pd2 C48 H48B 110.3 . . ?
H48A C48 H48B 108.5 . . ?
C50 C49 C54 120.5(4) . . ?
C50 C49 H49 119.7 . . ?
C54 C49 H49 119.7 . . ?
C51 C50 C49 119.5(5) . . ?
C51 C50 H50 120.2 . . ?
C49 C50 H50 120.2 . . ?
C52 C51 C50 120.7(4) . . ?
C52 C51 H51 119.6 . . ?
C50 C51 H51 119.6 . . ?
C51 C52 C53 119.7(4) . . ?
C51 C52 H52 120.1 . . ?
C53 C52 H52 120.1 . . ?
C52 C53 C54 120.5(4) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C53 C54 C49 119.0(3) . . ?
C53 C54 P2 123.0(3) . . ?
C49 C54 P2 117.9(3) . . ?
C60 C55 C56 120.9(4) . . ?
C60 C55 H55 119.6 . . ?
C56 C55 H55 119.6 . . ?
C57 C56 C55 120.0(4) . . ?
C57 C56 H56 120.0 . . ?
C55 C56 H56 120.0 . . ?
C58 C57 C56 119.5(4) . . ?
C58 C57 H57 120.2 . . ?
C56 C57 H57 120.2 . . ?
C57 C58 C59 120.9(4) . . ?
C57 C58 H58 119.6 . . ?
C59 C58 H58 119.6 . . ?
C58 C59 C60 120.5(4) . . ?
C58 C59 H59 119.7 . . ?
C60 C59 H59 119.7 . . ?
C55 C60 C59 118.1(4) . . ?
C55 C60 P2 121.4(3) . . ?
C59 C60 P2 120.4(3) . . ?
C62 C61 C66 120.7(3) . . ?
C62 C61 H61 119.6 . . ?
C66 C61 H61 119.6 . . ?
C63 C62 C61 120.6(4) . . ?
C63 C62 H62 119.7 . . ?
C61 C62 H62 119.7 . . ?
C62 C63 C64 119.1(4) . . ?
C62 C63 H63 120.4 . . ?
C64 C63 H63 120.4 . . ?
C63 C64 C65 120.5(3) . . ?
C63 C64 H64 119.7 . . ?
C65 C64 H64 119.7 . . ?
C64 C65 C66 120.6(3) . . ?
C64 C65 H65 119.7 . . ?
C66 C65 H65 119.7 . . ?
C61 C66 C65 118.3(3) . . ?
C61 C66 P2 123.1(3) . . ?
C65 C66 P2 118.7(3) . . ?
C8 N1 C5 115.1(3) . . ?
C8 N1 Pd1 120.5(2) . . ?
C5 N1 Pd1 121.8(2) . . ?
C10 N2 O2 116.1(2) . . ?
C10 N2 Pd1 118.5(2) . . ?
O2 N2 Pd1 124.9(2) . . ?
C41 N3 C38 114.9(3) . . ?
C41 N3 Pd2 119.1(2) . . ?
C38 N3 Pd2 121.6(2) . . ?
C43 N4 O4 116.2(3) . . ?
C43 N4 Pd2 119.3(2) . . ?
O4 N4 Pd2 124.3(2) . . ?
N2 O2 C9 110.4(2) . . ?
N4 O4 C42 108.9(2) . . ?
C21 P1 C27 104.39(15) . . ?
C21 P1 C33 100.21(15) . . ?
C27 P1 C33 105.29(15) . . ?
C21 P1 Pd1 118.26(10) . . ?
C27 P1 Pd1 111.78(10) . . ?
C33 P1 Pd1 115.36(11) . . ?
C60 P2 C54 106.22(16) . . ?
C60 P2 C66 102.04(16) . . ?
C54 P2 C66 104.92(16) . . ?
C60 P2 Pd2 115.97(12) . . ?
C54 P2 Pd2 110.19(10) . . ?
C66 P2 Pd2 116.41(11) . . ?
C15 Pd1 N2 77.54(12) . . ?
C15 Pd1 N1 164.55(11) . . ?
N2 Pd1 N1 88.42(11) . . ?
C15 Pd1 P1 92.80(9) . . ?
N2 Pd1 P1 170.28(9) . . ?
N1 Pd1 P1 101.29(7) . . ?
C48 Pd2 N4 77.31(12) . . ?
C48 Pd2 N3 164.20(11) . . ?
N4 Pd2 N3 88.90(11) . . ?
C48 Pd2 P2 93.18(9) . . ?
N4 Pd2 P2 170.40(9) . . ?
N3 Pd2 P2 100.70(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
C1 F2' 1.218(13) . ?
C1 F3 1.279(7) . ?
C1 F1' 1.332(10) . ?
C1 F2 1.333(8) . ?
C1 F1 1.358(7) . ?
C1 F3' 1.371(11) . ?
C1 C2 1.508(5) . ?
C2 C7 1.377(5) . ?
C2 C3 1.383(5) . ?
C3 F7 1.338(4) . ?
C3 C4 1.383(5) . ?
C4 F6 1.343(4) . ?
C4 C5 1.386(5) . ?
C5 C6 1.389(5) . ?
C5 N1 1.404(4) . ?
C6 F5 1.338(4) . ?
C6 C7 1.376(5) . ?
C7 F4 1.346(4) . ?
C8 O1 1.224(4) . ?
C8 N1 1.349(4) . ?
C8 C9 1.516(4) . ?
C9 O2 1.445(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.269(4) . ?
C10 C11 1.497(4) . ?
C10 C12 1.509(5) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C14 1.536(5) . ?
C12 C13 1.533(5) . ?
C12 C15 1.545(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 Pd1 2.037(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.373(5) . ?
C16 C21 1.397(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.390(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.380(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.381(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.394(4) . ?
C20 H20 0.9300 . ?
C21 P1 1.814(4) . ?
C22 C27 1.386(5) . ?
C22 C23 1.389(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.367(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.360(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.385(5) . ?
C26 H26 0.9300 . ?
C27 P1 1.822(3) . ?
C28 C29 1.380(5) . ?
C28 C33 1.386(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.346(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.366(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.386(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.366(5) . ?
C32 H32 0.9300 . ?
C33 P1 1.821(3) . ?
C34 F14A 1.234(12) . ?
C34 F13 1.262(11) . ?
C34 F14B 1.278(18) . ?
C34 F12 1.313(11) . ?
C34 F13B 1.331(18) . ?
C34 F13A 1.360(13) . ?
C34 F12B 1.376(17) . ?
C34 F12A 1.429(13) . ?
C34 F14 1.449(12) . ?
C34 C35 1.497(5) . ?
C35 C36 1.373(5) . ?
C35 C40 1.389(5) . ?
C36 F8 1.346(4) . ?
C36 C37 1.378(5) . ?
C37 F9 1.339(4) . ?
C37 C38 1.394(5) . ?
C38 C39 1.374(5) . ?
C38 N3 1.410(4) . ?
C39 F10 1.334(4) . ?
C39 C40 1.381(5) . ?
C40 F11 1.342(4) . ?
C41 O3 1.231(4) . ?
C41 N3 1.333(4) . ?
C41 C42 1.526(4) . ?
C42 O4 1.444(4) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 N4 1.272(4) . ?
C43 C44 1.495(4) . ?
C43 C45 1.512(5) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C47 1.525(5) . ?
C45 C46 1.541(4) . ?
C45 C48 1.546(4) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 Pd2 2.033(4) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C50 1.384(5) . ?
C49 C54 1.387(5) . ?
C49 H49 0.9300 . ?
C50 C51 1.379(7) . ?
C50 H50 0.9300 . ?
C51 C52 1.371(7) . ?
C51 H51 0.9300 . ?
C52 C53 1.384(5) . ?
C52 H52 0.9300 . ?
C53 C54 1.386(5) . ?
C53 H53 0.9300 . ?
C54 P2 1.820(3) . ?
C55 C60 1.378(5) . ?
C55 C56 1.386(5) . ?
C55 H55 0.9300 . ?
C56 C57 1.385(6) . ?
C56 H56 0.9300 . ?
C57 C58 1.362(6) . ?
C57 H57 0.9300 . ?
C58 C59 1.375(6) . ?
C58 H58 0.9300 . ?
C59 C60 1.400(5) . ?
C59 H59 0.9300 . ?
C60 P2 1.815(4) . ?
C61 C62 1.379(5) . ?
C61 C66 1.386(5) . ?
C61 H61 0.9300 . ?
C62 C63 1.380(5) . ?
C62 H62 0.9300 . ?
C63 C64 1.379(6) . ?
C63 H63 0.9300 . ?
C64 C65 1.379(5) . ?
C64 H64 0.9300 . ?
C65 C66 1.397(4) . ?
C65 H65 0.9300 . ?
C66 P2 1.815(4) . ?
N1 Pd1 2.156(3) . ?
N2 O2 1.399(4) . ?
N2 Pd1 2.056(2) . ?
N3 Pd2 2.151(3) . ?
N4 O4 1.404(3) . ?
N4 Pd2 2.048(2) . ?
P1 Pd1 2.2459(8) . ?
P2 Pd2 2.2341(8) . ?
