# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
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data_cu_cxy0207_0m_4
_database_code_depnum_ccdc_archive 'CCDC 1825616'
_audit_update_record
;
2018-02-25 deposited with the CCDC.
2018-04-27 downloaded from the CCDC.
;
_audit_creation_date 2017-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C23 H19 N4 Pd, 2(F3 P0.5), C3 H7 N O'
_chemical_formula_sum 'C26 H26 F6 N5 O P Pd'
_chemical_formula_weight 675.89
_chemical_melting_point ?
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'
F F 0.0727 0.0534 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 6.5861(5)
_cell_length_b 12.6581(10)
_cell_length_c 17.1310(14)
_cell_angle_alpha 109.005(3)
_cell_angle_beta 99.386(3)
_cell_angle_gamma 92.908(4)
_cell_volume 1323.96(18)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 4494
_cell_measurement_temperature 100
_cell_measurement_theta_max 65.236
_cell_measurement_theta_min 2.779
_shelx_estimated_absorpt_T_max 0.820
_shelx_estimated_absorpt_T_min 0.217
_exptl_absorpt_coefficient_mu 6.887
_exptl_absorpt_correction_T_max 0.75
_exptl_absorpt_correction_T_min 0.38
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
For component 1:
wR2(int) was 0.1379 before and 0.0816 after correction.
The Ratio of minimum to maximum transmission not present.
The \l/2 correction factor is Not present
For component 2:
wR2(int) was 0.1293 before and 0.0798 after correction.
The Ratio of minimum to maximum transmission is 0.51.
The \l/2 correction factor is Not present
Final HKLF 4 output contains 20596 reflections, Rint = 0.0834
(14272 with I > 3sig(I), Rint = 0.0776)
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.695
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_unetI/netI 0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 4324
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full 65.356
_diffrn_reflns_theta_max 65.356
_diffrn_reflns_theta_min 2.779
_diffrn_ambient_temperature 100
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3376
_reflns_number_total 4324
_reflns_special_details
;
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.550
_refine_diff_density_min -1.439
_refine_diff_density_rms 0.199
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.992
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 344
_refine_ls_number_reflns 4324
_refine_ls_number_restraints 232
_refine_ls_R_factor_all 0.1205
_refine_ls_R_factor_gt 0.0999
_refine_ls_restrained_S_all 0.978
_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/[\s^2^(Fo^2^)+(0.1000P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2463
_refine_ls_wR_factor_ref 0.2670
_refine_special_details
;
Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.393(5)
0.607(5)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Restrained distances
N5-C26 = N5-C25
1.45 with sigma of 0.02
N5-C24
1.45 with sigma of 0.02
O1-C24
1.25 with sigma of 0.02
H26B-C24
2.46 with sigma of 0.02
C24-C25 \\sim C24-C26
with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
5.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
C15(H15), C16(H16), C20(H20), C21(H21), C24(H24)
5.b Idealised Me refined as rotating group:
C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
H26C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
Pd1 Pd 0.24819(16) 0.50022(8) 0.49541(6) 0.0443(3) Uani 1 1 d . U . . .
N1 N 0.2791(16) 0.6388(9) 0.4614(7) 0.046(3) Uani 1 1 d . U . . .
N2 N 0.1866(18) 0.4291(10) 0.3709(6) 0.047(2) Uani 1 1 d . U . . .
N3 N 0.407(2) 0.5948(12) 0.8351(8) 0.063(3) Uani 1 1 d . U . . .
N4 N 0.420(2) 0.7628(12) 0.8288(8) 0.063(3) Uani 1 1 d . U . . .
C1 C 0.1987(18) 0.3364(11) 0.4853(9) 0.045(3) Uani 1 1 d . U . . .
C2 C 0.211(2) 0.2874(14) 0.5471(10) 0.058(3) Uani 1 1 d . U . . .
H2 H 0.2448 0.3349 0.6043 0.070 Uiso 1 1 calc R . . . .
C3 C 0.176(2) 0.1737(13) 0.5297(10) 0.056(3) Uani 1 1 d . U . . .
H3 H 0.1834 0.1439 0.5742 0.068 Uiso 1 1 calc R . . . .
C4 C 0.130(2) 0.1041(13) 0.4487(12) 0.060(4) Uani 1 1 d . U . . .
H4 H 0.0988 0.0257 0.4369 0.072 Uiso 1 1 calc R . . . .
C5 C 0.126(2) 0.1453(12) 0.3816(11) 0.061(4) Uani 1 1 d . U . . .
H5 H 0.1037 0.0951 0.3253 0.073 Uiso 1 1 calc R . . . .
C6 C 0.157(2) 0.2632(12) 0.3994(10) 0.055(3) Uani 1 1 d . U . . .
C7 C 0.153(2) 0.3172(13) 0.3399(10) 0.054(3) Uani 1 1 d . U . . .
C8 C 0.109(2) 0.2665(15) 0.2528(10) 0.066(4) Uani 1 1 d . U . . .
H8 H 0.0825 0.1870 0.2288 0.079 Uiso 1 1 calc R . . . .
C9 C 0.103(3) 0.3312(15) 0.2003(9) 0.065(4) Uani 1 1 d . U . . .
H9 H 0.0742 0.2963 0.1408 0.078 Uiso 1 1 calc R . . . .
C10 C 0.140(2) 0.4478(15) 0.2367(9) 0.064(4) Uani 1 1 d . U . . .
H10 H 0.1326 0.4938 0.2024 0.077 Uiso 1 1 calc R . . . .
C11 C 0.186(2) 0.4955(14) 0.3229(9) 0.055(3) Uani 1 1 d . U . . .
C12 C 0.234(2) 0.6169(14) 0.3748(10) 0.061(3) Uani 1 1 d . U . . .
C13 C 0.247(2) 0.7037(15) 0.3398(11) 0.066(4) Uani 1 1 d . U . . .
H13 H 0.2241 0.6868 0.2807 0.079 Uiso 1 1 calc R . . . .
C14 C 0.293(3) 0.8143(14) 0.3944(12) 0.069(4) Uani 1 1 d . U . . .
H14 H 0.2957 0.8738 0.3721 0.083 Uiso 1 1 calc R . . . .
C15 C 0.334(2) 0.8380(13) 0.4775(11) 0.057(3) Uani 1 1 d . U . . .
H15 H 0.3713 0.9139 0.5133 0.068 Uiso 1 1 calc R . . . .
C16 C 0.322(2) 0.7546(10) 0.5123(10) 0.052(3) Uani 1 1 d . U . . .
H16 H 0.3439 0.7747 0.5717 0.063 Uiso 1 1 calc R . . . .
C17 C 0.310(2) 0.5682(13) 0.6187(8) 0.053(3) Uani 1 1 d . U . . .
C18 C 0.344(3) 0.6067(14) 0.6933(9) 0.060(3) Uani 1 1 d . U . . .
C19 C 0.387(2) 0.6534(14) 0.7830(10) 0.059(3) Uani 1 1 d . U . . .
C20 C 0.461(3) 0.7704(16) 0.9124(9) 0.070(4) Uani 1 1 d . U . . .
H20 H 0.4948 0.8380 0.9593 0.084 Uiso 1 1 calc R . . . .
C21 C 0.447(3) 0.6697(15) 0.9157(10) 0.069(4) Uani 1 1 d . U . . .
H21 H 0.4616 0.6509 0.9655 0.083 Uiso 1 1 calc R . . . .
C22 C 0.383(3) 0.4740(14) 0.8119(11) 0.074(5) Uani 1 1 d . U . . .
H22A H 0.4859 0.4513 0.8497 0.110 Uiso 1 1 calc GR . . . .
H22B H 0.4028 0.4400 0.7539 0.110 Uiso 1 1 calc GR . . . .
H22C H 0.2434 0.4487 0.8163 0.110 Uiso 1 1 calc GR . . . .
C23 C 0.410(3) 0.8573(15) 0.7972(12) 0.074(5) Uani 1 1 d . U . . .
H23A H 0.5462 0.9011 0.8130 0.111 Uiso 1 1 calc GR . . . .
H23B H 0.3082 0.9054 0.8216 0.111 Uiso 1 1 calc GR . . . .
H23C H 0.3682 0.8286 0.7358 0.111 Uiso 1 1 calc GR . . . .
P2 P 0.0000 0.0000 0.0000 0.0754(18) Uani 1 2 d S TU P . .
F4 F -0.0158(18) -0.1297(8) -0.0107(8) 0.093(3) Uani 1 1 d . U . . .
F5 F 0.069(3) 0.0290(11) 0.0955(9) 0.157(7) Uani 1 1 d . U . . .
F6 F -0.227(2) 0.0000(10) 0.0110(13) 0.161(8) Uani 1 1 d . U . . .
P1 P 0.0000 0.5000 0.0000 0.0727(17) Uani 1 2 d S TU P . .
F1 F 0.0460(19) 0.5822(9) 0.0968(6) 0.089(3) Uani 1 1 d . U . . .
F2 F -0.2448(16) 0.5030(9) -0.0030(7) 0.096(4) Uani 1 1 d . U . . .
F3 F 0.0051(17) 0.6049(9) -0.0311(6) 0.082(3) Uani 1 1 d . U . . .
N5 N 0.610(4) -0.155(3) 0.1867(18) 0.174(9) Uiso 1 1 d D U . . .
C24 C 0.688(5) -0.090(3) 0.274(2) 0.188(12) Uiso 1 1 d D U . . .
H24 H 0.8207 -0.0940 0.3035 0.225 Uiso 1 1 calc R . . A 1
C25 C 0.387(4) -0.164(3) 0.1566(19) 0.178(13) Uiso 1 1 d D U . . .
H25A H 0.3206 -0.1234 0.2032 0.267 Uiso 1 1 calc GR . . . .
H25B H 0.3305 -0.2433 0.1346 0.267 Uiso 1 1 calc GR . . . .
H25C H 0.3602 -0.1312 0.1119 0.267 Uiso 1 1 calc GR . . . .
C26 C 0.759(6) -0.202(3) 0.136(2) 0.205(16) Uiso 1 1 d D U . . .
H26A H 0.7319 -0.2843 0.1152 0.308 Uiso 1 1 calc GR . . . .
H26B H 0.8991 -0.1795 0.1705 0.308 Uiso 1 1 calc DGR . . . .
H26C H 0.7492 -0.1748 0.0885 0.308 Uiso 1 1 calc GR . . . .
O1 O 0.560(6) -0.026(3) 0.308(2) 0.273(15) Uiso 1 1 d D U . B 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0417(5) 0.0437(6) 0.0452(5) 0.0146(5) 0.0034(4) 0.0028(4)
N1 0.031(5) 0.044(6) 0.061(6) 0.007(5) 0.023(5) 0.015(4)
N2 0.038(5) 0.061(6) 0.038(5) 0.018(5) -0.002(5) -0.001(5)
N3 0.058(7) 0.075(8) 0.052(6) 0.021(6) 0.007(6) -0.003(6)
N4 0.058(7) 0.068(8) 0.058(7) 0.018(6) 0.006(6) -0.005(6)
C1 0.029(6) 0.045(7) 0.061(7) 0.029(6) -0.006(5) -0.008(5)
C2 0.052(7) 0.060(8) 0.070(8) 0.039(7) 0.001(6) -0.003(6)
C3 0.041(7) 0.066(8) 0.078(8) 0.039(7) 0.017(6) 0.020(6)
C4 0.035(6) 0.042(7) 0.103(10) 0.025(7) 0.008(7) 0.010(6)
C5 0.052(8) 0.045(8) 0.074(9) 0.002(7) 0.017(7) 0.002(6)
C6 0.045(7) 0.049(7) 0.056(7) 0.003(6) 0.005(6) -0.005(6)
C7 0.039(6) 0.054(7) 0.061(7) 0.017(6) -0.007(6) 0.001(6)
C8 0.055(8) 0.065(9) 0.061(8) 0.002(7) 0.008(7) 0.000(7)
C9 0.046(7) 0.089(10) 0.043(7) 0.003(7) 0.004(6) 0.013(7)
C10 0.047(7) 0.087(10) 0.052(7) 0.021(7) 0.004(6) 0.000(7)
C11 0.042(6) 0.073(8) 0.049(6) 0.022(6) 0.003(5) 0.001(6)
C12 0.048(7) 0.074(8) 0.062(7) 0.024(6) 0.008(6) 0.004(6)
C13 0.057(8) 0.079(9) 0.073(9) 0.039(7) 0.012(7) 0.012(7)
C14 0.066(9) 0.062(8) 0.089(10) 0.040(8) 0.008(8) 0.006(7)
C15 0.036(6) 0.053(7) 0.087(9) 0.028(7) 0.012(6) 0.026(5)
C16 0.057(7) 0.033(6) 0.062(7) 0.013(6) 0.009(6) -0.017(5)
C17 0.037(6) 0.075(9) 0.037(6) 0.006(6) 0.002(6) 0.008(6)
C18 0.048(7) 0.071(9) 0.054(7) 0.016(7) 0.004(6) 0.005(6)
C19 0.040(6) 0.067(8) 0.067(7) 0.021(6) 0.005(6) 0.005(6)
C20 0.073(9) 0.078(9) 0.044(7) 0.004(7) 0.008(7) 0.004(8)
C21 0.080(9) 0.072(10) 0.049(7) 0.018(7) 0.005(7) 0.000(8)
C22 0.086(12) 0.063(11) 0.062(10) 0.018(8) 0.001(9) -0.006(9)
C23 0.074(11) 0.073(11) 0.073(11) 0.015(9) 0.029(9) 0.014(9)
P2 0.073(4) 0.062(4) 0.073(4) 0.004(3) 0.006(3) -0.005(3)
F4 0.111(9) 0.057(6) 0.097(8) 0.010(5) 0.014(7) 0.006(6)
F5 0.253(18) 0.077(9) 0.091(9) -0.013(7) -0.019(11) 0.026(10)
F6 0.099(10) 0.078(9) 0.27(2) -0.009(11) 0.073(12) 0.006(8)
P1 0.083(4) 0.085(5) 0.056(3) 0.033(3) 0.013(3) 0.008(3)
F1 0.118(9) 0.086(7) 0.062(6) 0.028(5) 0.009(6) 0.007(6)
F2 0.085(8) 0.115(10) 0.100(9) 0.048(7) 0.027(6) 0.012(7)
F3 0.101(8) 0.081(7) 0.073(6) 0.033(5) 0.024(6) 0.022(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.032(12) . ?
Pd1 N2 1.989(10) . ?
Pd1 C1 2.029(12) . ?
Pd1 C17 1.967(12) . ?
N1 C12 1.394(19) . ?
N1 C16 1.426(17) . ?
N2 C7 1.333(18) . ?
N2 C11 1.353(18) . ?
N3 C19 1.328(19) . ?
N3 C21 1.37(2) . ?
N3 C22 1.44(2) . ?
N4 C19 1.34(2) . ?
N4 C20 1.38(2) . ?
N4 C23 1.46(2) . ?
C1 C2 1.384(18) . ?
C1 C6 1.43(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.37(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.35(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.41(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.42(2) . ?
C6 C7 1.40(2) . ?
C7 C8 1.39(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.40(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.39(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.38(2) . ?
C11 C12 1.49(2) . ?
C12 C13 1.42(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.39(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.33(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.375(19) . ?
C16 H16 0.9500 . ?
C17 C18 1.188(18) . ?
C18 C19 1.43(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.29(2) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
P2 F4 1.587(10) 2 ?
P2 F4 1.587(10) . ?
P2 F5 1.539(14) 2 ?
P2 F5 1.539(14) . ?
P2 F6 1.537(12) . ?
P2 F6 1.537(12) 2 ?
P1 F1 1.614(10) 2_565 ?
P1 F1 1.614(10) . ?
P1 F2 1.608(10) . ?
P1 F2 1.608(10) 2_565 ?
P1 F3 1.585(10) 2_565 ?
P1 F3 1.585(10) . ?
N5 C24 1.448(18) . ?
N5 C25 1.458(18) . ?
N5 C26 1.445(18) . ?
C24 H24 0.9500 . ?
C24 O1 1.266(19) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N1 79.9(5) . . ?
N2 Pd1 C1 80.1(5) . . ?
C1 Pd1 N1 160.0(5) . . ?
C17 Pd1 N1 100.9(6) . . ?
C17 Pd1 N2 179.1(6) . . ?
C17 Pd1 C1 99.0(6) . . ?
C12 N1 Pd1 114.2(10) . . ?
C12 N1 C16 115.6(13) . . ?
C16 N1 Pd1 129.9(10) . . ?
C7 N2 Pd1 117.0(9) . . ?
C7 N2 C11 124.0(12) . . ?
C11 N2 Pd1 119.0(10) . . ?
C19 N3 C21 107.8(15) . . ?
C19 N3 C22 126.6(14) . . ?
C21 N3 C22 125.5(14) . . ?
C19 N4 C20 106.9(14) . . ?
C19 N4 C23 126.9(14) . . ?
C20 N4 C23 126.2(15) . . ?
C2 C1 Pd1 130.2(12) . . ?
C2 C1 C6 117.7(13) . . ?
C6 C1 Pd1 112.0(10) . . ?
C1 C2 H2 118.4 . . ?
C3 C2 C1 123.2(15) . . ?
C3 C2 H2 118.4 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.6(14) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 119.3 . . ?
C3 C4 C5 121.5(14) . . ?
C5 C4 H4 119.3 . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.0(15) . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C1 119.0(14) . . ?
C7 C6 C1 115.1(13) . . ?
C7 C6 C5 125.8(15) . . ?
N2 C7 C6 115.7(14) . . ?
N2 C7 C8 117.5(14) . . ?
C8 C7 C6 126.7(15) . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.9(16) . . ?
C9 C8 H8 119.6 . . ?
C8 C9 H9 120.6 . . ?
C10 C9 C8 118.7(14) . . ?
C10 C9 H9 120.6 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.2(16) . . ?
C11 C10 H10 120.4 . . ?
N2 C11 C10 119.7(15) . . ?
N2 C11 C12 112.0(13) . . ?
C10 C11 C12 128.3(15) . . ?
N1 C12 C11 114.7(13) . . ?
N1 C12 C13 121.9(15) . . ?
C13 C12 C11 123.2(16) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 C12 118.3(17) . . ?
C14 C13 H13 120.8 . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.0(15) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.2(15) . . ?
C16 C15 H15 119.4 . . ?
N1 C16 H16 119.2 . . ?
C15 C16 N1 121.7(14) . . ?
C15 C16 H16 119.2 . . ?
C18 C17 Pd1 178.0(15) . . ?
C17 C18 C19 179.3(18) . . ?
N3 C19 N4 108.4(14) . . ?
N3 C19 C18 125.5(15) . . ?
N4 C19 C18 126.1(15) . . ?
N4 C20 H20 125.8 . . ?
C21 C20 N4 108.4(15) . . ?
C21 C20 H20 125.8 . . ?
N3 C21 H21 125.8 . . ?
C20 C21 N3 108.3(15) . . ?
C20 C21 H21 125.8 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 H23A 109.5 . . ?
N4 C23 H23B 109.5 . . ?
N4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
F4 P2 F4 180.0 . 2 ?
F5 P2 F4 89.3(7) . . ?
F5 P2 F4 89.3(7) 2 2 ?
F5 P2 F4 90.7(7) 2 . ?
F5 P2 F4 90.7(7) . 2 ?
F5 P2 F5 180.0 2 . ?
F6 P2 F4 88.7(7) . . ?
F6 P2 F4 91.3(7) . 2 ?
F6 P2 F4 91.3(7) 2 . ?
F6 P2 F4 88.7(7) 2 2 ?
F6 P2 F5 89.6(11) . . ?
F6 P2 F5 90.4(11) 2 . ?
F6 P2 F5 89.6(11) 2 2 ?
F6 P2 F5 90.4(11) . 2 ?
F6 P2 F6 180.0 2 . ?
F1 P1 F1 180.0 . 2_565 ?
F2 P1 F1 89.7(6) 2_565 . ?
F2 P1 F1 90.3(6) 2_565 2_565 ?
F2 P1 F1 90.3(6) . . ?
F2 P1 F1 89.7(6) . 2_565 ?
F2 P1 F2 180.0 2_565 . ?
F3 P1 F1 89.2(5) 2_565 . ?
F3 P1 F1 90.8(5) 2_565 2_565 ?
F3 P1 F1 89.2(5) . 2_565 ?
F3 P1 F1 90.8(5) . . ?
F3 P1 F2 90.5(5) . 2_565 ?
F3 P1 F2 90.5(5) 2_565 . ?
F3 P1 F2 89.5(5) . . ?
F3 P1 F2 89.5(5) 2_565 2_565 ?
F3 P1 F3 180.0(8) . 2_565 ?
C24 N5 C25 117.1(19) . . ?
C26 N5 C24 117.2(19) . . ?
C26 N5 C25 126(3) . . ?
N5 C24 H24 123.4 . . ?
O1 C24 N5 113(3) . . ?
O1 C24 H24 123.4 . . ?
N5 C25 H25A 109.5 . . ?
N5 C25 H25B 109.5 . . ?
N5 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 H26A 109.5 . . ?
N5 C26 H26B 109.5 . . ?
N5 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
_shelx_res_file
;
cu_cxy0207_0m_4.res created by SHELXL-2014/7
TITL cu_cxy0207_0m_4_a.res in P-1
REM Old TITL cu_cxy0207_0m_4 in P-1
REM SHELXT solution in P-1
REM R1 0.253, Rweak 0.017, Alpha 0.090, Orientation as input
REM Formula found by SHELXT: C31 N8 Pt
CELL 1.54178 6.5861 12.6581 17.131 109.005 99.386 92.908
ZERR 2 0.0005 0.001 0.0014 0.003 0.003 0.004
LATT 1
SFAC C H F N O P Pd
UNIT 52 52 12 10 2 2 2
DFIX 1.45 N5 C26 N5 C25
DFIX 1.45 N5 C24
DFIX 1.25 O1 C24
DFIX 2.46 H26b C24
SADI C24 C25 C24 C26
SIMU 0.02 0.04 2
L.S. 40 0 0
PLAN 50
SIZE 0.32 0.04 0.03
TEMP -173.15
BOND $H
list 4
fmap 2 53
ACTA
OMIT -4 0 6
REM
REM
REM
WGHT 0.100000 20.000000
BASF 0.60743
FVAR 0.31453
PD1 7 0.248192 0.500216 0.495407 11.00000 0.04169 0.04372 =
0.04517 0.01464 0.00341 0.00278
N1 4 0.279073 0.638837 0.461394 11.00000 0.03070 0.04409 =
0.06080 0.00741 0.02332 0.01490
N2 4 0.186602 0.429140 0.370892 11.00000 0.03821 0.06119 =
0.03782 0.01778 -0.00196 -0.00134
N3 4 0.406841 0.594850 0.835085 11.00000 0.05791 0.07468 =
0.05228 0.02091 0.00698 -0.00347
N4 4 0.419824 0.762812 0.828803 11.00000 0.05794 0.06793 =
0.05773 0.01763 0.00634 -0.00494
C1 1 0.198735 0.336354 0.485332 11.00000 0.02851 0.04485 =
0.06148 0.02850 -0.00615 -0.00751
C2 1 0.210654 0.287390 0.547085 11.00000 0.05194 0.06025 =
0.07028 0.03873 0.00106 -0.00289
AFIX 43
H2 2 0.244824 0.334868 0.604273 11.00000 -1.20000
AFIX 0
C3 1 0.175546 0.173720 0.529726 11.00000 0.04065 0.06616 =
0.07768 0.03947 0.01738 0.01992
AFIX 43
H3 2 0.183438 0.143927 0.574231 11.00000 -1.20000
AFIX 0
C4 1 0.129514 0.104118 0.448689 11.00000 0.03459 0.04186 =
0.10251 0.02481 0.00757 0.00969
AFIX 43
H4 2 0.098849 0.025710 0.436912 11.00000 -1.20000
AFIX 0
C5 1 0.126112 0.145346 0.381624 11.00000 0.05233 0.04483 =
0.07396 0.00241 0.01742 0.00151
AFIX 43
H5 2 0.103662 0.095073 0.325273 11.00000 -1.20000
AFIX 0
C6 1 0.156739 0.263229 0.399420 11.00000 0.04490 0.04914 =
0.05640 0.00308 0.00475 -0.00517
C7 1 0.153268 0.317212 0.339921 11.00000 0.03853 0.05385 =
0.06134 0.01721 -0.00726 0.00051
C8 1 0.108964 0.266546 0.252808 11.00000 0.05545 0.06518 =
0.06135 0.00225 0.00755 -0.00020
AFIX 43
H8 2 0.082545 0.186997 0.228794 11.00000 -1.20000
AFIX 0
C9 1 0.102853 0.331164 0.200254 11.00000 0.04638 0.08861 =
0.04317 0.00272 0.00414 0.01315
AFIX 43
H9 2 0.074220 0.296267 0.140849 11.00000 -1.20000
AFIX 0
C10 1 0.139572 0.447783 0.236671 11.00000 0.04682 0.08749 =
0.05204 0.02061 0.00394 -0.00029
AFIX 43
H10 2 0.132562 0.493782 0.202395 11.00000 -1.20000
AFIX 0
C11 1 0.186103 0.495472 0.322882 11.00000 0.04184 0.07332 =
0.04901 0.02164 0.00305 0.00115
C12 1 0.233631 0.616941 0.374838 11.00000 0.04751 0.07407 =
0.06210 0.02426 0.00814 0.00369
C13 1 0.246533 0.703686 0.339847 11.00000 0.05662 0.07917 =
0.07259 0.03927 0.01243 0.01151
AFIX 43
H13 2 0.224054 0.686783 0.280653 11.00000 -1.20000
AFIX 0
C14 1 0.292991 0.814339 0.394405 11.00000 0.06575 0.06156 =
0.08896 0.04002 0.00815 0.00607
AFIX 43
H14 2 0.295697 0.873841 0.372072 11.00000 -1.20000
AFIX 0
C15 1 0.333709 0.838018 0.477464 11.00000 0.03614 0.05271 =
0.08703 0.02806 0.01191 0.02570
AFIX 43
H15 2 0.371279 0.913883 0.513283 11.00000 -1.20000
AFIX 0
C16 1 0.322343 0.754646 0.512289 11.00000 0.05698 0.03275 =
0.06227 0.01335 0.00888 -0.01740
AFIX 43
H16 2 0.343852 0.774700 0.571735 11.00000 -1.20000
AFIX 0
C17 1 0.310193 0.568181 0.618719 11.00000 0.03690 0.07461 =
0.03662 0.00637 0.00173 0.00834
C18 1 0.343801 0.606727 0.693340 11.00000 0.04789 0.07146 =
0.05436 0.01621 0.00368 0.00468
C19 1 0.386986 0.653406 0.783032 11.00000 0.04042 0.06697 =
0.06679 0.02075 0.00482 0.00521
C20 1 0.461353 0.770401 0.912360 11.00000 0.07311 0.07835 =
0.04391 0.00435 0.00850 0.00369
AFIX 43
H20 2 0.494774 0.838024 0.959293 11.00000 -1.20000
AFIX 0
C21 1 0.446931 0.669738 0.915711 11.00000 0.08002 0.07230 =
0.04896 0.01792 0.00532 0.00015
AFIX 43
H21 2 0.461615 0.650922 0.965537 11.00000 -1.20000
AFIX 0
C22 1 0.382814 0.474038 0.811889 11.00000 0.08601 0.06346 =
0.06238 0.01824 0.00075 -0.00614
AFIX 137
H22A 2 0.485861 0.451329 0.849696 11.00000 -1.50000
H22B 2 0.402812 0.440040 0.753866 11.00000 -1.50000
H22C 2 0.243446 0.448666 0.816344 11.00000 -1.50000
AFIX 0
C23 1 0.409797 0.857274 0.797214 11.00000 0.07434 0.07326 =
0.07261 0.01501 0.02874 0.01385
AFIX 137
H23A 2 0.546239 0.901065 0.813041 11.00000 -1.50000
H23B 2 0.308217 0.905392 0.821648 11.00000 -1.50000
H23C 2 0.368224 0.828578 0.735814 11.00000 -1.50000
AFIX 0
P2 6 0.000000 0.000000 0.000000 10.50000 0.07260 0.06187 =
0.07332 0.00373 0.00618 -0.00501
F4 3 -0.015777 -0.129662 -0.010651 11.00000 0.11068 0.05668 =
0.09693 0.00976 0.01412 0.00609
F5 3 0.069398 0.029049 0.095519 11.00000 0.25286 0.07737 =
0.09077 -0.01299 -0.01913 0.02625
F6 3 -0.226971 0.000029 0.011031 11.00000 0.09922 0.07783 =
0.26828 -0.00914 0.07256 0.00582
P1 6 0.000000 0.500000 0.000000 10.50000 0.08316 0.08484 =
0.05634 0.03251 0.01330 0.00808
F1 3 0.046004 0.582162 0.096803 11.00000 0.11800 0.08600 =
0.06186 0.02790 0.00940 0.00726
F2 3 -0.244820 0.503017 -0.003035 11.00000 0.08534 0.11467 =
0.09960 0.04844 0.02664 0.01218
F3 3 0.005077 0.604941 -0.031107 11.00000 0.10125 0.08098 =
0.07297 0.03290 0.02377 0.02246
N5 4 0.609532 -0.154588 0.186685 11.00000 0.17390
C24 1 0.687526 -0.089613 0.274336 11.00000 0.18778
PART 1
AFIX 43
H24 2 0.820664 -0.094047 0.303538 11.00000 -1.20000
AFIX 0
PART 0
C25 1 0.386962 -0.163881 0.156648 11.00000 0.17810
AFIX 137
H25A 2 0.320568 -0.123415 0.203217 11.00000 -1.50000
H25B 2 0.330501 -0.243295 0.134644 11.00000 -1.50000
H25C 2 0.360169 -0.131183 0.111888 11.00000 -1.50000
AFIX 0
C26 1 0.759497 -0.202126 0.136144 11.00000 0.20531
AFIX 137
H26A 2 0.731944 -0.284310 0.115242 11.00000 -1.50000
H26B 2 0.899117 -0.179531 0.170455 11.00000 -1.50000
H26C 2 0.749156 -0.174783 0.088450 11.00000 -1.50000
AFIX 0
PART 1
O1 5 0.560388 -0.026287 0.308140 11.00000 0.27306
HKLF 5
REM cu_cxy0207_0m_4_a.res in P-1
REM R1 = 0.0999 for 3376 Fo > 4sig(Fo) and 0.1205 for all 4324 data
REM 344 parameters refined using 232 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 1.550, deepest hole -1.439, 1-sigma level 0.199
Q1 1 0.1171 0.5183 0.4832 11.00000 0.05 1.55
Q2 1 0.1731 -0.0827 0.2482 11.00000 0.05 1.48
Q3 1 0.3044 0.5936 0.5039 11.00000 0.05 1.45
Q4 1 0.3964 0.4966 0.5011 11.00000 0.05 1.42
Q5 1 0.1903 0.4010 0.4895 11.00000 0.05 1.42
Q6 1 0.3237 0.5344 0.5623 11.00000 0.05 1.04
Q7 1 0.2442 0.3629 0.5331 11.00000 0.05 1.00
Q8 1 0.4868 0.7532 0.5274 11.00000 0.05 0.93
Q9 1 -0.0840 0.3386 0.4432 11.00000 0.05 0.93
Q10 1 0.6494 -0.0848 0.2599 11.00000 0.05 0.89
Q11 1 0.2644 0.5165 0.5375 11.00000 0.05 0.89
Q12 1 1.0062 -0.1402 0.1842 11.00000 0.05 0.86
Q13 1 0.8619 -0.1420 0.1996 11.00000 0.05 0.85
Q14 1 0.1769 0.7425 0.5029 11.00000 0.05 0.84
Q15 1 0.4407 0.3542 0.4605 11.00000 0.05 0.83
Q16 1 -0.1257 0.0456 0.0884 11.00000 0.05 0.83
Q17 1 0.5576 -0.1352 0.1993 11.00000 0.05 0.82
Q18 1 0.2760 0.5013 0.4626 11.00000 0.05 0.80
Q19 1 0.1849 0.5585 0.5949 11.00000 0.05 0.77
Q20 1 0.4790 0.6023 0.5580 11.00000 0.05 0.76
Q21 1 0.2563 0.4018 0.4028 11.00000 0.05 0.71
Q22 1 0.5885 -0.1986 0.1147 11.00000 0.05 0.70
Q23 1 0.1635 0.4672 0.4223 11.00000 0.05 0.70
Q24 1 0.1591 -0.1318 0.1879 11.00000 0.05 0.68
Q25 1 0.5444 0.8317 0.5235 11.00000 0.05 0.68
Q26 1 -0.0292 0.1767 0.4854 11.00000 0.05 0.67
Q27 1 0.2939 0.4219 0.4039 11.00000 0.05 0.66
Q28 1 0.1919 0.0240 0.0618 11.00000 0.05 0.65
Q29 1 0.5586 0.6244 0.6006 11.00000 0.05 0.64
Q30 1 0.0591 0.2555 0.4530 11.00000 0.05 0.64
Q31 1 0.2202 0.4797 0.4412 11.00000 0.05 0.63
Q32 1 -0.0158 0.3988 0.5250 11.00000 0.05 0.63
Q33 1 0.5167 0.5876 0.4512 11.00000 0.05 0.62
Q34 1 0.2912 0.3993 0.5580 11.00000 0.05 0.61
Q35 1 0.0266 0.4405 0.2505 11.00000 0.05 0.60
Q36 1 0.0239 0.3969 0.4364 11.00000 0.05 0.58
Q37 1 0.0272 0.1347 0.5598 11.00000 0.05 0.57
Q38 1 0.2651 0.3188 0.4802 11.00000 0.05 0.57
Q39 1 0.5711 0.8626 0.5337 11.00000 0.05 0.57
Q40 1 0.4046 0.2734 0.3549 11.00000 0.05 0.56
Q41 1 0.0591 0.6222 0.6000 11.00000 0.05 0.56
Q42 1 -0.1280 0.2668 0.3438 11.00000 0.05 0.55
Q43 1 0.2673 0.2169 0.5623 11.00000 0.05 0.55
Q44 1 0.3336 0.7276 0.4650 11.00000 0.05 0.54
Q45 1 0.3987 0.6245 0.2856 11.00000 0.05 0.52
Q46 1 -0.2736 0.1005 0.0548 11.00000 0.05 0.52
Q47 1 0.5418 0.8267 0.6061 11.00000 0.05 0.52
Q48 1 0.2814 0.3713 0.4576 11.00000 0.05 0.51
Q49 1 0.3730 0.6861 0.5448 11.00000 0.05 0.51
Q50 1 0.4143 0.9243 0.5613 11.00000 0.05 0.51
;
_shelx_res_checksum 42647
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.393(5)
2 0.607(5)
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_cxy0264_0m
_database_code_depnum_ccdc_archive 'CCDC 1825617'
_audit_update_record
;
2018-02-25 deposited with the CCDC.
2018-04-27 downloaded from the CCDC.
;
_audit_creation_date 2017-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C23 H19 N4 Pd, F6 P'
_chemical_formula_sum 'C23 H19 F6 N4 P Pd'
_chemical_formula_weight 602.79
_chemical_melting_point ?
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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.2664(11)
_cell_length_b 11.9680(15)
_cell_length_c 12.4012(16)
_cell_angle_alpha 73.332(4)
_cell_angle_beta 73.511(4)
_cell_angle_gamma 74.085(4)
_cell_volume 1101.9(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9933
_cell_measurement_temperature 100
_cell_measurement_theta_max 27.53
_cell_measurement_theta_min 2.63
_shelx_estimated_absorpt_T_max 0.770
_shelx_estimated_absorpt_T_min 0.694
_exptl_absorpt_coefficient_mu 0.986
_exptl_absorpt_correction_T_max 0.2617
_exptl_absorpt_correction_T_min 0.2187
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1308 before and 0.0644 after correction. The Ratio of minimum to maximum transmission is 0.8357. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.817
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 600
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.28
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0478
_diffrn_reflns_av_unetI/netI 0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 11570
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.533
_diffrn_reflns_theta_min 2.628
_diffrn_ambient_temperature 100
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4632
_reflns_number_total 5010
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.693
_refine_diff_density_min -0.525
_refine_diff_density_rms 0.102
_refine_ls_extinction_coef 0.0113(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 319
_refine_ls_number_reflns 5010
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0351
_refine_ls_R_factor_gt 0.0314
_refine_ls_restrained_S_all 1.035
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+1.3189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0777
_refine_ls_wR_factor_ref 0.0799
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
C15(H15), C16(H16), C19(H19), C20(H20)
2.b Idealised Me refined as rotating group:
C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
Pd1 Pd 0.23027(2) 0.31683(2) 0.52093(2) 0.01155(8) Uani 1 1 d . . . . .
N1 N 0.0591(3) 0.38165(18) 0.64949(17) 0.0129(4) Uani 1 1 d . . . . .
N2 N 0.2759(3) 0.49306(18) 0.48493(18) 0.0147(4) Uani 1 1 d . . . . .
N3 N 0.6288(3) 0.06315(19) 0.19479(18) 0.0169(4) Uani 1 1 d . . . . .
N4 N 0.7307(3) 0.22386(18) 0.14345(18) 0.0159(4) Uani 1 1 d . . . . .
C1 C -0.0479(3) 0.3113(2) 0.7224(2) 0.0134(5) Uani 1 1 d . . . . .
C2 C -0.1792(3) 0.3573(2) 0.8074(2) 0.0169(5) Uani 1 1 d . . . . .
H2 H -0.2580 0.3105 0.8585 0.020 Uiso 1 1 calc R . . . .
C3 C -0.1924(3) 0.4725(2) 0.8161(2) 0.0183(5) Uani 1 1 d . . . . .
H3 H -0.2798 0.5042 0.8746 0.022 Uiso 1 1 calc R . . . .
C4 C -0.0795(3) 0.5422(2) 0.7403(2) 0.0170(5) Uani 1 1 d . . . . .
H4 H -0.0884 0.6211 0.7465 0.020 Uiso 1 1 calc R . . . .
C5 C 0.0462(3) 0.4940(2) 0.6557(2) 0.0141(5) Uani 1 1 d . . . . .
C6 C 0.1731(3) 0.5556(2) 0.5645(2) 0.0140(5) Uani 1 1 d . . . . .
C7 C 0.3899(3) 0.5456(2) 0.3986(2) 0.0159(5) Uani 1 1 d . . . . .
H7 H 0.4600 0.5027 0.3421 0.019 Uiso 1 1 calc R . . . .
C8 C 0.4100(3) 0.6594(2) 0.3883(2) 0.0179(5) Uani 1 1 d . . . . .
H8 H 0.4930 0.6937 0.3264 0.021 Uiso 1 1 calc R . . . .
C9 C 0.3072(3) 0.7225(2) 0.4698(2) 0.0193(5) Uani 1 1 d . . . . .
H9 H 0.3193 0.8005 0.4652 0.023 Uiso 1 1 calc R . . . .
C10 C 0.1865(3) 0.6704(2) 0.5580(2) 0.0178(5) Uani 1 1 d . . . . .
H10 H 0.1131 0.7131 0.6138 0.021 Uiso 1 1 calc R . . . .
C11 C -0.0093(3) 0.1933(2) 0.6956(2) 0.0142(5) Uani 1 1 d . . . . .
C12 C 0.1262(3) 0.1743(2) 0.5980(2) 0.0145(5) Uani 1 1 d . . . . .
C13 C 0.1635(3) 0.0647(2) 0.5687(2) 0.0194(5) Uani 1 1 d . . . . .
H13 H 0.2533 0.0492 0.5039 0.023 Uiso 1 1 calc R . . . .
C14 C 0.0700(4) -0.0226(2) 0.6336(3) 0.0230(6) Uani 1 1 d . . . . .
H14 H 0.0966 -0.0967 0.6120 0.028 Uiso 1 1 calc R . . . .
C15 C -0.0606(3) -0.0035(2) 0.7288(2) 0.0209(5) Uani 1 1 d . . . . .
H15 H -0.1218 -0.0643 0.7729 0.025 Uiso 1 1 calc R . . . .
C16 C -0.1016(3) 0.1053(2) 0.7594(2) 0.0174(5) Uani 1 1 d . . . . .
H16 H -0.1926 0.1198 0.8240 0.021 Uiso 1 1 calc R . . . .
C17 C 0.4921(3) 0.2104(2) 0.3147(2) 0.0167(5) Uani 1 1 d . . . . .
C18 C 0.6118(3) 0.1677(2) 0.2213(2) 0.0148(5) Uani 1 1 d . . . . .
C19 C 0.8241(3) 0.1533(2) 0.0667(2) 0.0215(5) Uani 1 1 d . . . . .
H19 H 0.9163 0.1716 0.0031 0.026 Uiso 1 1 calc R . . . .
C20 C 0.7605(3) 0.0539(2) 0.0986(2) 0.0210(5) Uani 1 1 d . . . . .
H20 H 0.7994 -0.0111 0.0615 0.025 Uiso 1 1 calc R . . . .
C22 C 0.5238(4) -0.0250(2) 0.2575(3) 0.0236(6) Uani 1 1 d . . . . .
H22A H 0.5814 -0.0841 0.3154 0.035 Uiso 1 1 calc GR . . . .
H22B H 0.5086 -0.0650 0.2034 0.035 Uiso 1 1 calc GR . . . .
H22C H 0.4108 0.0147 0.2960 0.035 Uiso 1 1 calc GR . . . .
C23 C 0.7460(4) 0.3445(2) 0.1371(2) 0.0238(6) Uani 1 1 d . . . . .
H23A H 0.6534 0.4026 0.1041 0.036 Uiso 1 1 calc GR . . . .
H23B H 0.8581 0.3583 0.0882 0.036 Uiso 1 1 calc GR . . . .
H23C H 0.7369 0.3535 0.2149 0.036 Uiso 1 1 calc GR . . . .
C24 C 0.3924(3) 0.2490(2) 0.3950(2) 0.0154(5) Uani 1 1 d . . . . .
P1 P 0.31767(8) 0.28745(6) -0.03627(6) 0.01840(15) Uani 1 1 d . . . . .
F1 F 0.1508(2) 0.3731(2) 0.02045(19) 0.0467(6) Uani 1 1 d . . . . .
F2 F 0.3112(3) 0.1909(2) 0.0810(2) 0.0673(7) Uani 1 1 d . . . . .
F3 F 0.1991(2) 0.22761(17) -0.07576(19) 0.0400(5) Uani 1 1 d . . . . .
F4 F 0.3260(3) 0.38562(17) -0.15441(17) 0.0430(5) Uani 1 1 d . . . . .
F5 F 0.4383(2) 0.34778(18) 0.00071(17) 0.0386(5) Uani 1 1 d . . . . .
F6 F 0.4866(2) 0.20508(15) -0.09675(17) 0.0344(4) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01228(11) 0.01047(11) 0.01201(12) -0.00432(7) -0.00148(7) -0.00197(7)
N1 0.0139(9) 0.0124(9) 0.0133(10) -0.0037(8) -0.0046(8) -0.0015(8)
N2 0.0159(10) 0.0137(10) 0.0152(10) -0.0041(8) -0.0059(8) -0.0013(8)
N3 0.0181(10) 0.0163(10) 0.0168(11) -0.0064(9) -0.0024(8) -0.0030(8)
N4 0.0143(10) 0.0178(10) 0.0133(10) -0.0022(8) -0.0013(8) -0.0027(8)
C1 0.0139(11) 0.0142(11) 0.0126(11) -0.0025(9) -0.0064(9) -0.0009(9)
C2 0.0172(12) 0.0185(12) 0.0131(12) -0.0020(10) -0.0022(10) -0.0037(10)
C3 0.0192(12) 0.0210(12) 0.0127(12) -0.0067(10) -0.0013(10) -0.0002(10)
C4 0.0209(12) 0.0144(11) 0.0176(12) -0.0076(10) -0.0061(10) -0.0006(9)
C5 0.0149(11) 0.0139(11) 0.0139(11) -0.0039(9) -0.0044(9) -0.0015(9)
C6 0.0151(11) 0.0142(11) 0.0132(11) -0.0047(9) -0.0047(9) -0.0006(9)
C7 0.0160(11) 0.0184(12) 0.0134(12) -0.0024(10) -0.0054(9) -0.0027(9)
C8 0.0195(12) 0.0190(12) 0.0161(12) 0.0012(10) -0.0073(10) -0.0075(10)
C9 0.0246(13) 0.0157(12) 0.0200(13) -0.0018(10) -0.0096(11) -0.0058(10)
C10 0.0221(12) 0.0157(12) 0.0182(12) -0.0054(10) -0.0069(10) -0.0043(10)
C11 0.0145(11) 0.0139(11) 0.0150(12) -0.0020(9) -0.0070(9) -0.0017(9)
C12 0.0138(11) 0.0130(11) 0.0175(12) -0.0019(10) -0.0060(9) -0.0030(9)
C13 0.0209(12) 0.0169(12) 0.0205(13) -0.0086(11) -0.0012(10) -0.0032(10)
C14 0.0271(14) 0.0158(12) 0.0295(15) -0.0082(11) -0.0071(12) -0.0060(11)
C15 0.0200(12) 0.0188(12) 0.0237(14) -0.0011(11) -0.0051(11) -0.0077(10)
C16 0.0167(12) 0.0182(12) 0.0164(12) -0.0019(10) -0.0043(10) -0.0040(10)
C17 0.0184(12) 0.0155(11) 0.0176(12) -0.0047(10) -0.0033(10) -0.0057(10)
C18 0.0137(11) 0.0156(11) 0.0147(12) -0.0034(10) -0.0033(9) -0.0025(9)
C19 0.0149(12) 0.0282(14) 0.0157(12) -0.0060(11) -0.0023(10) 0.0043(10)
C20 0.0199(12) 0.0226(13) 0.0186(13) -0.0111(11) -0.0042(10) 0.0052(10)
C22 0.0250(14) 0.0185(13) 0.0309(15) -0.0087(12) -0.0064(12) -0.0069(11)
C23 0.0254(14) 0.0229(13) 0.0226(14) -0.0031(11) -0.0016(11) -0.0101(11)
C24 0.0175(12) 0.0114(11) 0.0189(12) -0.0038(10) -0.0043(10) -0.0048(9)
P1 0.0144(3) 0.0235(3) 0.0181(3) -0.0078(3) -0.0004(3) -0.0053(3)
F1 0.0174(8) 0.0738(15) 0.0575(13) -0.0468(12) 0.0008(8) 0.0007(9)
F2 0.0600(15) 0.0844(18) 0.0397(13) 0.0327(12) -0.0130(11) -0.0339(14)
F3 0.0257(9) 0.0392(10) 0.0676(14) -0.0254(10) -0.0136(9) -0.0094(8)
F4 0.0560(13) 0.0312(10) 0.0353(11) 0.0029(8) -0.0105(9) -0.0094(9)
F5 0.0205(8) 0.0580(12) 0.0508(12) -0.0386(10) -0.0041(8) -0.0064(8)
F6 0.0213(8) 0.0291(9) 0.0571(12) -0.0263(9) -0.0050(8) 0.0014(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 1.993(2) . ?
Pd1 N2 2.142(2) . ?
Pd1 C12 1.992(2) . ?
Pd1 C24 1.959(3) . ?
N1 C1 1.351(3) . ?
N1 C5 1.342(3) . ?
N2 C6 1.363(3) . ?
N2 C7 1.340(3) . ?
N3 C18 1.344(3) . ?
N3 C20 1.376(3) . ?
N3 C22 1.456(3) . ?
N4 C18 1.342(3) . ?
N4 C19 1.379(3) . ?
N4 C23 1.462(3) . ?
C1 C2 1.396(3) . ?
C1 C11 1.473(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.386(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.389(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(3) . ?
C5 C6 1.482(3) . ?
C6 C10 1.386(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.421(3) . ?
C11 C16 1.391(3) . ?
C12 C13 1.391(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.394(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.412(3) . ?
C17 C24 1.214(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.343(4) . ?
C20 H20 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
P1 F1 1.5925(18) . ?
P1 F2 1.575(2) . ?
P1 F3 1.6035(18) . ?
P1 F4 1.5909(19) . ?
P1 F5 1.6036(18) . ?
P1 F6 1.5998(17) . ?
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
N1 Pd1 N2 78.27(8) . . ?
C12 Pd1 N1 81.94(9) . . ?
C12 Pd1 N2 160.20(9) . . ?
C24 Pd1 N1 177.72(8) . . ?
C24 Pd1 N2 103.73(9) . . ?
C24 Pd1 C12 96.03(10) . . ?
C1 N1 Pd1 117.19(16) . . ?
C5 N1 Pd1 119.69(17) . . ?
C5 N1 C1 122.9(2) . . ?
C6 N2 Pd1 112.55(16) . . ?
C7 N2 Pd1 129.00(17) . . ?
C7 N2 C6 118.4(2) . . ?
C18 N3 C20 108.8(2) . . ?
C18 N3 C22 125.3(2) . . ?
C20 N3 C22 125.9(2) . . ?
C18 N4 C19 108.8(2) . . ?
C18 N4 C23 124.5(2) . . ?
C19 N4 C23 126.4(2) . . ?
N1 C1 C2 118.9(2) . . ?
N1 C1 C11 112.3(2) . . ?
C2 C1 C11 128.8(2) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.8(2) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.4(2) . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 120.1(2) . . ?
N1 C5 C6 113.6(2) . . ?
C4 C5 C6 126.3(2) . . ?
N2 C6 C5 115.8(2) . . ?
N2 C6 C10 121.3(2) . . ?
C10 C6 C5 123.0(2) . . ?
N2 C7 H7 118.6 . . ?
N2 C7 C8 122.8(2) . . ?
C8 C7 H7 118.6 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.8(2) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 119.0(2) . . ?
C10 C9 H9 120.5 . . ?
C6 C10 H10 120.2 . . ?
C9 C10 C6 119.6(2) . . ?
C9 C10 H10 120.2 . . ?
C12 C11 C1 116.2(2) . . ?
C16 C11 C1 122.7(2) . . ?
C16 C11 C12 121.1(2) . . ?
C11 C12 Pd1 112.28(17) . . ?
C13 C12 Pd1 129.96(19) . . ?
C13 C12 C11 117.7(2) . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.5(2) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.3 . . ?
C15 C14 C13 121.3(2) . . ?
C15 C14 H14 119.3 . . ?
C14 C15 H15 120.3 . . ?
C14 C15 C16 119.4(2) . . ?
C16 C15 H15 120.3 . . ?
C11 C16 H16 120.0 . . ?
C15 C16 C11 119.9(2) . . ?
C15 C16 H16 120.0 . . ?
C24 C17 C18 178.1(3) . . ?
N3 C18 C17 126.4(2) . . ?
N4 C18 N3 107.6(2) . . ?
N4 C18 C17 126.1(2) . . ?
N4 C19 H19 126.3 . . ?
C20 C19 N4 107.3(2) . . ?
C20 C19 H19 126.3 . . ?
N3 C20 H20 126.2 . . ?
C19 C20 N3 107.5(2) . . ?
C19 C20 H20 126.2 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 H23A 109.5 . . ?
N4 C23 H23B 109.5 . . ?
N4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C24 Pd1 178.0(2) . . ?
F1 P1 F3 90.54(10) . . ?
F1 P1 F5 90.12(10) . . ?
F1 P1 F6 178.09(12) . . ?
F2 P1 F1 91.17(14) . . ?
F2 P1 F3 91.00(13) . . ?
F2 P1 F4 179.28(13) . . ?
F2 P1 F5 89.87(13) . . ?
F2 P1 F6 90.66(13) . . ?
F3 P1 F5 178.90(11) . . ?
F4 P1 F1 88.93(12) . . ?
F4 P1 F3 89.71(11) . . ?
F4 P1 F5 89.42(11) . . ?
F4 P1 F6 89.23(11) . . ?
F6 P1 F3 89.95(10) . . ?
F6 P1 F5 89.36(9) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C1 C2 -174.55(17) . . . . ?
Pd1 N1 C1 C11 3.4(3) . . . . ?
Pd1 N1 C5 C4 175.91(18) . . . . ?
Pd1 N1 C5 C6 -2.8(3) . . . . ?
Pd1 N2 C6 C5 -2.8(3) . . . . ?
Pd1 N2 C6 C10 178.23(18) . . . . ?
Pd1 N2 C7 C8 -177.46(17) . . . . ?
Pd1 C12 C13 C14 -178.0(2) . . . . ?
N1 C1 C2 C3 -1.7(3) . . . . ?
N1 C1 C11 C12 -2.0(3) . . . . ?
N1 C1 C11 C16 179.5(2) . . . . ?
N1 C5 C6 N2 3.7(3) . . . . ?
N1 C5 C6 C10 -177.3(2) . . . . ?
N2 C6 C10 C9 -0.5(4) . . . . ?
N2 C7 C8 C9 -0.6(4) . . . . ?
N4 C19 C20 N3 -0.2(3) . . . . ?
C1 N1 C5 C4 0.8(4) . . . . ?
C1 N1 C5 C6 -177.9(2) . . . . ?
C1 C2 C3 C4 1.2(4) . . . . ?
C1 C11 C12 Pd1 -0.2(3) . . . . ?
C1 C11 C12 C13 -178.6(2) . . . . ?
C1 C11 C16 C15 179.1(2) . . . . ?
C2 C1 C11 C12 175.7(2) . . . . ?
C2 C1 C11 C16 -2.8(4) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C3 C4 C5 N1 -1.2(4) . . . . ?
C3 C4 C5 C6 177.3(2) . . . . ?
C4 C5 C6 N2 -175.0(2) . . . . ?
C4 C5 C6 C10 4.0(4) . . . . ?
C5 N1 C1 C2 0.7(3) . . . . ?
C5 N1 C1 C11 178.6(2) . . . . ?
C5 C6 C10 C9 -179.5(2) . . . . ?
C6 N2 C7 C8 1.4(4) . . . . ?
C7 N2 C6 C5 178.2(2) . . . . ?
C7 N2 C6 C10 -0.8(3) . . . . ?
C7 C8 C9 C10 -0.7(4) . . . . ?
C8 C9 C10 C6 1.3(4) . . . . ?
C11 C1 C2 C3 -179.2(2) . . . . ?
C11 C12 C13 C14 0.0(4) . . . . ?
C12 C11 C16 C15 0.6(4) . . . . ?
C12 C13 C14 C15 -0.4(4) . . . . ?
C13 C14 C15 C16 1.0(4) . . . . ?
C14 C15 C16 C11 -1.1(4) . . . . ?
C16 C11 C12 Pd1 178.28(18) . . . . ?
C16 C11 C12 C13 -0.1(4) . . . . ?
C18 N3 C20 C19 0.1(3) . . . . ?
C18 N4 C19 C20 0.1(3) . . . . ?
C19 N4 C18 N3 -0.1(3) . . . . ?
C19 N4 C18 C17 179.3(2) . . . . ?
C20 N3 C18 N4 -0.1(3) . . . . ?
C20 N3 C18 C17 -179.4(2) . . . . ?
C22 N3 C18 N4 -179.7(2) . . . . ?
C22 N3 C18 C17 0.9(4) . . . . ?
C22 N3 C20 C19 179.8(2) . . . . ?
C23 N4 C18 N3 175.2(2) . . . . ?
C23 N4 C18 C17 -5.4(4) . . . . ?
C23 N4 C19 C20 -175.0(2) . . . . ?
_shelx_res_file
;
mo_cxy0264_0m.res created by SHELXL-2014/7
TITL mo_cxy0264_0m_a.res in P-1
CELL 0.71073 8.2664 11.968 12.4012 73.332 73.511 74.085
ZERR 2 0.0011 0.0015 0.0016 0.004 0.004 0.004
LATT 1
SFAC C H F N P Pd
UNIT 46 38 12 8 2 2
L.S. 4
PLAN -5 0 0
SIZE 0.4 0.32 0.28
TEMP -173.15
HTAB
BOND $H
CONF
fmap 2
acta
OMIT 1 1 0
OMIT 1 1 1
REM
REM
REM
WGHT 0.010300 1.318900
EXTI 0.011295
FVAR 0.53520
PD1 6 0.230271 0.316828 0.520931 11.00000 0.01228 0.01047 =
0.01201 -0.00432 -0.00148 -0.00197
N1 4 0.059112 0.381646 0.649495 11.00000 0.01386 0.01236 =
0.01326 -0.00370 -0.00465 -0.00150
N2 4 0.275883 0.493056 0.484934 11.00000 0.01593 0.01374 =
0.01523 -0.00410 -0.00586 -0.00125
N3 4 0.628777 0.063153 0.194794 11.00000 0.01814 0.01626 =
0.01677 -0.00636 -0.00239 -0.00295
N4 4 0.730673 0.223862 0.143454 11.00000 0.01429 0.01776 =
0.01332 -0.00215 -0.00134 -0.00271
C1 1 -0.047868 0.311308 0.722374 11.00000 0.01387 0.01423 =
0.01264 -0.00254 -0.00644 -0.00091
C2 1 -0.179155 0.357340 0.807436 11.00000 0.01725 0.01852 =
0.01306 -0.00198 -0.00218 -0.00372
AFIX 43
H2 2 -0.258007 0.310490 0.858472 11.00000 -1.20000
AFIX 0
C3 1 -0.192427 0.472534 0.816113 11.00000 0.01923 0.02099 =
0.01273 -0.00668 -0.00127 -0.00024
AFIX 43
H3 2 -0.279825 0.504246 0.874622 11.00000 -1.20000
AFIX 0
C4 1 -0.079544 0.542210 0.740335 11.00000 0.02089 0.01443 =
0.01757 -0.00762 -0.00610 -0.00057
AFIX 43
H4 2 -0.088437 0.621099 0.746460 11.00000 -1.20000
AFIX 0
C5 1 0.046203 0.493960 0.655690 11.00000 0.01492 0.01386 =
0.01390 -0.00385 -0.00444 -0.00150
C6 1 0.173065 0.555650 0.564519 11.00000 0.01515 0.01415 =
0.01323 -0.00468 -0.00474 -0.00064
C7 1 0.389942 0.545558 0.398623 11.00000 0.01596 0.01836 =
0.01338 -0.00237 -0.00545 -0.00272
AFIX 43
H7 2 0.460009 0.502741 0.342083 11.00000 -1.20000
AFIX 0
C8 1 0.410022 0.659424 0.388331 11.00000 0.01953 0.01899 =
0.01614 0.00116 -0.00730 -0.00747
AFIX 43
H8 2 0.492975 0.693654 0.326400 11.00000 -1.20000
AFIX 0
C9 1 0.307186 0.722543 0.469804 11.00000 0.02461 0.01566 =
0.01998 -0.00176 -0.00956 -0.00583
AFIX 43
H9 2 0.319309 0.800545 0.465236 11.00000 -1.20000
AFIX 0
C10 1 0.186476 0.670448 0.557998 11.00000 0.02214 0.01572 =
0.01819 -0.00538 -0.00688 -0.00434
AFIX 43
H10 2 0.113109 0.713102 0.613836 11.00000 -1.20000
AFIX 0
C11 1 -0.009342 0.193289 0.695607 11.00000 0.01451 0.01393 =
0.01499 -0.00199 -0.00697 -0.00167
C12 1 0.126177 0.174251 0.598048 11.00000 0.01381 0.01302 =
0.01745 -0.00191 -0.00601 -0.00305
C13 1 0.163479 0.064687 0.568662 11.00000 0.02093 0.01691 =
0.02053 -0.00864 -0.00120 -0.00318
AFIX 43
H13 2 0.253302 0.049227 0.503866 11.00000 -1.20000
AFIX 0
C14 1 0.069967 -0.022578 0.633638 11.00000 0.02712 0.01578 =
0.02953 -0.00822 -0.00711 -0.00600
AFIX 43
H14 2 0.096636 -0.096669 0.612006 11.00000 -1.20000
AFIX 0
C15 1 -0.060576 -0.003475 0.728758 11.00000 0.01999 0.01883 =
0.02374 -0.00112 -0.00509 -0.00774
AFIX 43
H15 2 -0.121824 -0.064335 0.772856 11.00000 -1.20000
AFIX 0
C16 1 -0.101593 0.105344 0.759427 11.00000 0.01668 0.01818 =
0.01644 -0.00191 -0.00426 -0.00395
AFIX 43
H16 2 -0.192598 0.119796 0.823954 11.00000 -1.20000
AFIX 0
C17 1 0.492097 0.210369 0.314683 11.00000 0.01836 0.01550 =
0.01760 -0.00473 -0.00325 -0.00567
C18 1 0.611794 0.167677 0.221310 11.00000 0.01368 0.01559 =
0.01474 -0.00344 -0.00329 -0.00254
C19 1 0.824054 0.153278 0.066744 11.00000 0.01489 0.02823 =
0.01574 -0.00599 -0.00228 0.00433
AFIX 43
H19 2 0.916272 0.171587 0.003133 11.00000 -1.20000
AFIX 0
C20 1 0.760496 0.053856 0.098608 11.00000 0.01989 0.02265 =
0.01865 -0.01105 -0.00420 0.00518
AFIX 43
H20 2 0.799378 -0.011050 0.061512 11.00000 -1.20000
AFIX 0
C22 1 0.523807 -0.025009 0.257527 11.00000 0.02501 0.01852 =
0.03094 -0.00868 -0.00635 -0.00686
AFIX 137
H22A 2 0.581409 -0.084126 0.315404 11.00000 -1.50000
H22B 2 0.508584 -0.064959 0.203383 11.00000 -1.50000
H22C 2 0.410767 0.014712 0.296022 11.00000 -1.50000
AFIX 0
C23 1 0.746031 0.344516 0.137122 11.00000 0.02537 0.02294 =
0.02261 -0.00312 -0.00163 -0.01010
AFIX 137
H23A 2 0.653427 0.402644 0.104075 11.00000 -1.50000
H23B 2 0.858082 0.358250 0.088192 11.00000 -1.50000
H23C 2 0.736879 0.353532 0.214854 11.00000 -1.50000
AFIX 0
C24 1 0.392428 0.248984 0.394966 11.00000 0.01754 0.01138 =
0.01888 -0.00377 -0.00435 -0.00478
P1 5 0.317665 0.287448 -0.036272 11.00000 0.01436 0.02351 =
0.01810 -0.00784 -0.00037 -0.00529
F1 3 0.150791 0.373114 0.020453 11.00000 0.01739 0.07382 =
0.05746 -0.04683 0.00083 0.00071
F2 3 0.311161 0.190856 0.081016 11.00000 0.06003 0.08443 =
0.03974 0.03274 -0.01295 -0.03389
F3 3 0.199128 0.227615 -0.075765 11.00000 0.02573 0.03916 =
0.06756 -0.02536 -0.01365 -0.00939
F4 3 0.326005 0.385621 -0.154405 11.00000 0.05605 0.03117 =
0.03526 0.00294 -0.01055 -0.00936
F5 3 0.438333 0.347784 0.000713 11.00000 0.02055 0.05804 =
0.05084 -0.03863 -0.00414 -0.00641
F6 3 0.486619 0.205079 -0.096746 11.00000 0.02130 0.02908 =
0.05706 -0.02627 -0.00497 0.00140
HKLF 4
REM mo_cxy0264_0m_a.res in P-1
REM R1 = 0.0314 for 4632 Fo > 4sig(Fo) and 0.0351 for all 5010 data
REM 319 parameters refined using 0 restraints
END
WGHT 0.0103 1.3189
REM Instructions for potential hydrogen bonds
EQIV $1 x-1, y, z+1
HTAB C2 F5_$1
HTAB C2 F6_$1
EQIV $2 -x+1, -y+1, -z
HTAB C8 F4_$2
EQIV $3 x+1, y, z
HTAB C19 F3_$3
EQIV $4 -x+1, -y, -z
HTAB C20 F3_$4
HTAB C22 F6_$4
HTAB C23 F1_$3
REM Highest difference peak 0.693, deepest hole -0.525, 1-sigma level 0.102
Q1 1 0.1518 0.2988 0.0643 11.00000 0.05 0.69
Q2 1 0.2758 0.3953 -0.0820 11.00000 0.05 0.61
Q3 1 0.4087 0.2796 0.0516 11.00000 0.05 0.54
Q4 1 0.4648 0.1597 -0.0259 11.00000 0.05 0.52
Q5 1 0.3414 0.1222 0.0553 11.00000 0.05 0.42
;
_shelx_res_checksum 98308
_olex2_submission_special_instructions 'No special instructions were received'