# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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).
#
# 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_exp_3406
_database_code_depnum_ccdc_archive 'CCDC 1824536'
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_audit_creation_date 2015-07-01
_audit_creation_method
;
Olex2 1.1
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C24 H26 Br N3 Pd'
_chemical_formula_sum 'C24 H26 Br N3 Pd'
_chemical_formula_weight 542.79
_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'
Br Br -0.2901 2.4595 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.7217(3)
_cell_length_b 10.2318(3)
_cell_length_c 17.5246(4)
_cell_angle_alpha 90.00
_cell_angle_beta 102.488(2)
_cell_angle_gamma 90.00
_cell_volume 2227.13(9)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3964
_cell_measurement_temperature 101.8
_cell_measurement_theta_max 29.4575
_cell_measurement_theta_min 2.9798
_exptl_absorpt_coefficient_mu 2.642
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.73734
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.619
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1088
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.45
_exptl_crystal_size_min 0.40
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0325
_diffrn_reflns_av_unetI/netI 0.0431
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 10580
_diffrn_reflns_theta_full 26.00
_diffrn_reflns_theta_max 26.00
_diffrn_reflns_theta_min 2.99
_diffrn_ambient_temperature 101.8
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -7.00 45.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -13.4277 37.0000 0.0000 52
#__ type_ start__ end____ width___ exp.time_
2 omega -20.00 6.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -13.4277 -77.0000 -150.0000 26
#__ type_ start__ end____ width___ exp.time_
3 omega -76.00 -44.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -13.4277 -77.0000 -150.0000 32
#__ type_ start__ end____ width___ exp.time_
4 omega 4.00 88.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 18.7402 37.0000 90.0000 84
#__ type_ start__ end____ width___ exp.time_
5 omega -38.00 19.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 18.7402 -89.0000 161.0000 57
;
_diffrn_measurement_device_type 'Xcalibur, Eos, Gemini'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0130712000
_diffrn_orient_matrix_UB_12 0.0409004000
_diffrn_orient_matrix_UB_13 -0.0292838000
_diffrn_orient_matrix_UB_21 -0.0521995000
_diffrn_orient_matrix_UB_22 -0.0099819000
_diffrn_orient_matrix_UB_23 -0.0235508000
_diffrn_orient_matrix_UB_31 -0.0191546000
_diffrn_orient_matrix_UB_32 0.0550703000
_diffrn_orient_matrix_UB_33 0.0174842000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 3874
_reflns_number_total 4363
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_refine_diff_density_max 2.580
_refine_diff_density_min -0.475
_refine_diff_density_rms 0.103
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 266
_refine_ls_number_reflns 4363
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0412
_refine_ls_R_factor_gt 0.0344
_refine_ls_restrained_S_all 1.046
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+6.2328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0725
_refine_ls_wR_factor_ref 0.0752
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.90023(2) 0.73326(3) 0.131443(15) 0.01141(8) Uani 1 1 d . . .
Br1 Br 1.05235(3) 0.61892(4) 0.22233(2) 0.02135(11) Uani 1 1 d . . .
N1 N 0.8588(2) 0.5821(3) 0.05058(17) 0.0152(6) Uani 1 1 d . . .
C11 C 0.7813(3) 0.8206(4) 0.0587(2) 0.0159(8) Uani 1 1 d U . .
N2 N 1.0049(2) 0.9799(3) 0.19757(16) 0.0119(6) Uani 1 1 d . . .
C15 C 0.9080(3) 1.1075(4) 0.3590(2) 0.0182(8) Uani 1 1 d . . .
H15 H 0.8545 1.0818 0.3863 0.022 Uiso 1 1 calc R . .
C7 C 0.6452(3) 0.7891(4) -0.0639(2) 0.0188(8) Uani 1 1 d . . .
H7 H 0.6134 0.7350 -0.1067 0.023 Uiso 1 1 calc R . .
C12 C 0.9296(3) 0.8880(3) 0.2000(2) 0.0125(7) Uani 1 1 d . . .
C5 C 0.7763(3) 0.6116(4) -0.0105(2) 0.0162(8) Uani 1 1 d . . .
C10 C 0.7376(3) 0.9495(4) 0.0599(2) 0.0183(8) Uani 1 1 d . . .
H10 H 0.7686 1.0064 0.1016 0.022 Uiso 1 1 calc R . .
C14 C 0.9279(3) 1.0349(4) 0.2958(2) 0.0135(7) Uani 1 1 d . . .
C16 C 0.9698(3) 1.2181(4) 0.3798(2) 0.0206(9) Uani 1 1 d . . .
H16 H 0.9589 1.2693 0.4226 0.025 Uiso 1 1 calc R . .
N3 N 0.8818(2) 0.9207(3) 0.25929(17) 0.0133(6) Uani 1 1 d . . .
C2 C 0.8797(3) 0.3736(4) -0.0048(2) 0.0260(9) Uani 1 1 d . . .
H2 H 0.9166 0.2925 -0.0021 0.031 Uiso 1 1 calc R . .
C22 C 1.0749(3) 0.9766(4) 0.1396(2) 0.0221(9) Uani 1 1 d . . .
H22 H 1.0533 0.8982 0.1058 0.027 Uiso 1 1 calc R . .
C19 C 0.7931(3) 0.8439(4) 0.2795(2) 0.0181(8) Uani 1 1 d . . .
H19 H 0.7776 0.7699 0.2415 0.022 Uiso 1 1 calc R . .
C18 C 1.0675(3) 1.1859(4) 0.2770(2) 0.0171(8) Uani 1 1 d . . .
H18 H 1.1205 1.2128 0.2496 0.021 Uiso 1 1 calc R . .
C13 C 1.0063(3) 1.0733(4) 0.2557(2) 0.0135(7) Uani 1 1 d . . .
C20 C 0.6909(3) 0.9253(4) 0.2687(2) 0.0233(9) Uani 1 1 d . . .
H20A H 0.7033 1.0001 0.3045 0.035 Uiso 1 1 calc R . .
H20B H 0.6324 0.8714 0.2801 0.035 Uiso 1 1 calc R . .
H20C H 0.6712 0.9568 0.2147 0.035 Uiso 1 1 calc R . .
C1 C 0.9090(3) 0.4660(4) 0.0534(2) 0.0205(8) Uani 1 1 d . . .
H1 H 0.9663 0.4471 0.0965 0.025 Uiso 1 1 calc R . .
C8 C 0.6063(3) 0.9148(4) -0.0584(2) 0.0225(9) Uani 1 1 d . . .
H8 H 0.5477 0.9471 -0.0969 0.027 Uiso 1 1 calc R . .
C21 C 0.8273(3) 0.7842(4) 0.3605(2) 0.0269(10) Uani 1 1 d . . .
H21A H 0.8911 0.7295 0.3626 0.040 Uiso 1 1 calc R . .
H21B H 0.7685 0.7305 0.3715 0.040 Uiso 1 1 calc R . .
H21C H 0.8443 0.8540 0.3995 0.040 Uiso 1 1 calc R . .
C9 C 0.6552(3) 0.9931(4) 0.0050(2) 0.0221(9) Uani 1 1 d . . .
H9 H 0.6292 1.0793 0.0090 0.027 Uiso 1 1 calc R . .
C6 C 0.7310(3) 0.7418(4) -0.0066(2) 0.0151(8) Uani 1 1 d . . .
C17 C 1.0479(3) 1.2565(4) 0.3392(2) 0.0213(9) Uani 1 1 d . . .
H17 H 1.0886 1.3334 0.3551 0.026 Uiso 1 1 calc R . .
C3 C 0.7956(3) 0.4013(4) -0.0670(2) 0.0281(10) Uani 1 1 d . . .
H3 H 0.7740 0.3391 -0.1076 0.034 Uiso 1 1 calc R . .
C23 C 1.0543(4) 1.0950(5) 0.0871(3) 0.0352(11) Uani 1 1 d . . .
H23A H 0.9774 1.1002 0.0628 0.053 Uiso 1 1 calc R . .
H23B H 1.0959 1.0877 0.0463 0.053 Uiso 1 1 calc R . .
H23C H 1.0761 1.1741 0.1180 0.053 Uiso 1 1 calc R . .
C4 C 0.7432(3) 0.5195(4) -0.0697(2) 0.0247(9) Uani 1 1 d . . .
H4 H 0.6845 0.5384 -0.1119 0.030 Uiso 1 1 calc R . .
C24 C 1.1918(3) 0.9581(5) 0.1802(3) 0.0380(12) Uani 1 1 d . . .
H24A H 1.2158 1.0329 0.2144 0.057 Uiso 1 1 calc R . .
H24B H 1.2360 0.9514 0.1410 0.057 Uiso 1 1 calc R . .
H24C H 1.1992 0.8778 0.2114 0.057 Uiso 1 1 calc R . .
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 0.01178(14) 0.01262(15) 0.00967(14) -0.00190(11) 0.00193(10) -0.00008(11)
Br1 0.0205(2) 0.0240(2) 0.0171(2) -0.00050(16) -0.00140(15) 0.00609(16)
N1 0.0167(16) 0.0146(16) 0.0155(15) -0.0028(13) 0.0059(13) -0.0014(13)
C11 0.0204(15) 0.0149(14) 0.0173(14) -0.0005(12) 0.0148(12) -0.0039(12)
N2 0.0108(14) 0.0156(16) 0.0094(14) -0.0042(12) 0.0024(11) -0.0031(12)
C15 0.0168(18) 0.022(2) 0.0162(19) -0.0047(16) 0.0053(15) 0.0009(16)
C7 0.0180(19) 0.026(2) 0.0107(18) 0.0007(16) -0.0002(15) -0.0045(17)
C12 0.0116(17) 0.0133(19) 0.0111(17) -0.0002(14) -0.0011(14) 0.0012(14)
C5 0.0159(18) 0.022(2) 0.0126(17) -0.0017(16) 0.0070(15) -0.0046(16)
C10 0.0177(19) 0.025(2) 0.0152(19) -0.0114(17) 0.0110(15) -0.0113(16)
C14 0.0136(17) 0.0118(18) 0.0138(18) -0.0015(15) -0.0002(14) -0.0019(15)
C16 0.0181(19) 0.023(2) 0.019(2) -0.0105(17) 0.0005(16) 0.0002(17)
N3 0.0131(15) 0.0161(16) 0.0123(15) -0.0042(13) 0.0065(12) -0.0026(13)
C2 0.029(2) 0.019(2) 0.032(2) -0.0081(19) 0.0113(19) -0.0018(18)
C22 0.022(2) 0.031(2) 0.018(2) -0.0112(18) 0.0140(16) -0.0101(18)
C19 0.0170(19) 0.019(2) 0.021(2) -0.0057(17) 0.0106(16) -0.0075(16)
C18 0.0149(18) 0.017(2) 0.0189(19) -0.0015(16) 0.0031(15) -0.0036(16)
C13 0.0121(17) 0.0176(19) 0.0098(17) -0.0024(15) 0.0005(13) 0.0012(15)
C20 0.018(2) 0.030(2) 0.024(2) -0.0056(19) 0.0091(16) -0.0042(18)
C1 0.023(2) 0.022(2) 0.019(2) -0.0027(17) 0.0074(16) 0.0014(17)
C8 0.022(2) 0.029(2) 0.0152(19) 0.0081(17) 0.0003(16) 0.0027(18)
C21 0.034(2) 0.024(2) 0.027(2) 0.0058(18) 0.0135(19) -0.0021(19)
C9 0.036(2) 0.0103(19) 0.025(2) 0.0066(16) 0.0195(19) 0.0050(17)
C6 0.0138(17) 0.019(2) 0.0138(18) -0.0002(16) 0.0052(14) -0.0067(15)
C17 0.0182(19) 0.019(2) 0.024(2) -0.0079(17) 0.0002(16) -0.0045(17)
C3 0.027(2) 0.031(2) 0.027(2) -0.016(2) 0.0062(18) -0.0045(19)
C23 0.053(3) 0.034(3) 0.024(2) -0.003(2) 0.018(2) -0.019(2)
C4 0.023(2) 0.028(2) 0.021(2) -0.0080(18) 0.0012(17) -0.0028(18)
C24 0.020(2) 0.047(3) 0.052(3) -0.024(3) 0.019(2) -0.009(2)
_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 Br1 2.5134(5) . ?
Pd1 N1 2.087(3) . ?
Pd1 C11 1.969(4) . ?
Pd1 C12 1.973(4) . ?
N1 C5 1.360(5) . ?
N1 C1 1.345(5) . ?
C11 C10 1.433(5) . ?
C11 C6 1.433(5) . ?
N2 C12 1.350(4) . ?
N2 C22 1.489(4) . ?
N2 C13 1.394(4) . ?
C15 H15 0.9500 . ?
C15 C14 1.401(5) . ?
C15 C16 1.381(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(6) . ?
C7 C6 1.399(5) . ?
C12 N3 1.355(4) . ?
C5 C6 1.458(5) . ?
C5 C4 1.398(5) . ?
C10 H10 0.9500 . ?
C10 C9 1.337(6) . ?
C14 N3 1.398(5) . ?
C14 C13 1.395(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.397(5) . ?
N3 C19 1.480(4) . ?
C2 H2 0.9500 . ?
C2 C1 1.381(5) . ?
C2 C3 1.381(6) . ?
C22 H22 1.0000 . ?
C22 C23 1.510(6) . ?
C22 C24 1.515(6) . ?
C19 H19 1.0000 . ?
C19 C20 1.520(5) . ?
C19 C21 1.519(5) . ?
C18 H18 0.9500 . ?
C18 C13 1.395(5) . ?
C18 C17 1.375(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C1 H1 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.401(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C9 H9 0.9500 . ?
C17 H17 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.376(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C4 H4 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
N1 Pd1 Br1 97.60(9) . . ?
C11 Pd1 Br1 178.97(11) . . ?
C11 Pd1 N1 81.42(14) . . ?
C11 Pd1 C12 92.72(15) . . ?
C12 Pd1 Br1 88.25(10) . . ?
C12 Pd1 N1 174.04(13) . . ?
C5 N1 Pd1 114.1(2) . . ?
C1 N1 Pd1 125.5(3) . . ?
C1 N1 C5 120.3(3) . . ?
C10 C11 Pd1 130.9(3) . . ?
C10 C11 C6 115.0(3) . . ?
C6 C11 Pd1 114.2(3) . . ?
C12 N2 C22 122.6(3) . . ?
C12 N2 C13 110.6(3) . . ?
C13 N2 C22 126.8(3) . . ?
C14 C15 H15 121.5 . . ?
C16 C15 H15 121.5 . . ?
C16 C15 C14 117.0(3) . . ?
C8 C7 H7 119.8 . . ?
C8 C7 C6 120.4(4) . . ?
C6 C7 H7 119.8 . . ?
N2 C12 Pd1 125.6(2) . . ?
N2 C12 N3 106.9(3) . . ?
N3 C12 Pd1 127.4(3) . . ?
N1 C5 C6 114.3(3) . . ?
N1 C5 C4 119.4(4) . . ?
C4 C5 C6 126.3(3) . . ?
C11 C10 H10 118.6 . . ?
C9 C10 C11 122.9(4) . . ?
C9 C10 H10 118.6 . . ?
N3 C14 C15 132.5(3) . . ?
C13 C14 C15 121.2(3) . . ?
C13 C14 N3 106.3(3) . . ?
C15 C16 H16 119.3 . . ?
C15 C16 C17 121.5(3) . . ?
C17 C16 H16 119.3 . . ?
C12 N3 C14 110.1(3) . . ?
C12 N3 C19 123.0(3) . . ?
C14 N3 C19 126.9(3) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C3 C2 C1 118.8(4) . . ?
N2 C22 H22 107.1 . . ?
N2 C22 C23 110.3(3) . . ?
N2 C22 C24 110.8(3) . . ?
C23 C22 H22 107.1 . . ?
C23 C22 C24 114.2(4) . . ?
C24 C22 H22 107.1 . . ?
N3 C19 H19 107.0 . . ?
N3 C19 C20 110.8(3) . . ?
N3 C19 C21 110.9(3) . . ?
C20 C19 H19 107.0 . . ?
C21 C19 H19 107.0 . . ?
C21 C19 C20 113.6(3) . . ?
C13 C18 H18 121.3 . . ?
C17 C18 H18 121.3 . . ?
C17 C18 C13 117.4(3) . . ?
N2 C13 C14 106.1(3) . . ?
N2 C13 C18 132.8(3) . . ?
C18 C13 C14 121.1(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C1 C2 121.8(4) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.7(4) . . ?
C9 C8 H8 120.7 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C9 C8 121.6(4) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C11 C6 C5 116.0(3) . . ?
C7 C6 C11 121.5(4) . . ?
C7 C6 C5 122.5(3) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 C16 121.8(4) . . ?
C18 C17 H17 119.1 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 H3 120.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 H4 120.0 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
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 C5 C6 -1.5(4) . . . . ?
Pd1 N1 C5 C4 178.2(3) . . . . ?
Pd1 N1 C1 C2 -176.7(3) . . . . ?
Pd1 C11 C10 C9 -179.9(3) . . . . ?
Pd1 C11 C6 C7 -179.9(3) . . . . ?
Pd1 C11 C6 C5 -1.3(4) . . . . ?
Pd1 C12 N3 C14 177.6(3) . . . . ?
Pd1 C12 N3 C19 -3.0(5) . . . . ?
Br1 Pd1 N1 C5 -179.0(2) . . . . ?
Br1 Pd1 N1 C1 -2.0(3) . . . . ?
Br1 Pd1 C11 C10 -160(5) . . . . ?
Br1 Pd1 C11 C6 19(6) . . . . ?
Br1 Pd1 C12 N2 83.5(3) . . . . ?
Br1 Pd1 C12 N3 -94.2(3) . . . . ?
N1 Pd1 C11 C10 -178.9(3) . . . . ?
N1 Pd1 C11 C6 0.4(2) . . . . ?
N1 Pd1 C12 N2 -85.3(13) . . . . ?
N1 Pd1 C12 N3 96.9(12) . . . . ?
N1 C5 C6 C11 1.9(4) . . . . ?
N1 C5 C6 C7 -179.5(3) . . . . ?
N1 C5 C4 C3 -1.6(6) . . . . ?
C11 Pd1 N1 C5 0.7(2) . . . . ?
C11 Pd1 N1 C1 177.7(3) . . . . ?
C11 Pd1 C12 N2 -96.2(3) . . . . ?
C11 Pd1 C12 N3 86.1(3) . . . . ?
C11 C10 C9 C8 -0.5(6) . . . . ?
N2 C12 N3 C14 -0.4(4) . . . . ?
N2 C12 N3 C19 178.9(3) . . . . ?
C15 C14 N3 C12 -179.7(4) . . . . ?
C15 C14 N3 C19 1.0(6) . . . . ?
C15 C14 C13 N2 179.7(3) . . . . ?
C15 C14 C13 C18 -0.3(6) . . . . ?
C15 C16 C17 C18 -0.3(6) . . . . ?
C7 C8 C9 C10 -0.2(6) . . . . ?
C12 Pd1 N1 C5 -10.3(13) . . . . ?
C12 Pd1 N1 C1 166.7(11) . . . . ?
C12 Pd1 C11 C10 0.0(3) . . . . ?
C12 Pd1 C11 C6 179.2(3) . . . . ?
C12 N2 C22 C23 117.1(4) . . . . ?
C12 N2 C22 C24 -115.4(4) . . . . ?
C12 N2 C13 C14 0.4(4) . . . . ?
C12 N2 C13 C18 -179.6(4) . . . . ?
C12 N3 C19 C20 -117.3(4) . . . . ?
C12 N3 C19 C21 115.5(4) . . . . ?
C5 N1 C1 C2 0.2(5) . . . . ?
C10 C11 C6 C7 -0.5(5) . . . . ?
C10 C11 C6 C5 178.1(3) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C14 N3 C19 C20 61.9(5) . . . . ?
C14 N3 C19 C21 -65.3(5) . . . . ?
C16 C15 C14 N3 -179.8(4) . . . . ?
C16 C15 C14 C13 -0.2(6) . . . . ?
N3 C14 C13 N2 -0.6(4) . . . . ?
N3 C14 C13 C18 179.3(3) . . . . ?
C2 C3 C4 C5 1.1(6) . . . . ?
C22 N2 C12 Pd1 1.6(5) . . . . ?
C22 N2 C12 N3 179.7(3) . . . . ?
C22 N2 C13 C14 -179.3(3) . . . . ?
C22 N2 C13 C18 0.7(6) . . . . ?
C13 N2 C12 Pd1 -178.1(2) . . . . ?
C13 N2 C12 N3 0.0(4) . . . . ?
C13 N2 C22 C23 -63.2(5) . . . . ?
C13 N2 C22 C24 64.2(5) . . . . ?
C13 C14 N3 C12 0.7(4) . . . . ?
C13 C14 N3 C19 -178.6(3) . . . . ?
C13 C18 C17 C16 -0.3(6) . . . . ?
C1 N1 C5 C6 -178.7(3) . . . . ?
C1 N1 C5 C4 1.0(5) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
C8 C7 C6 C11 -0.2(5) . . . . ?
C8 C7 C6 C5 -178.7(3) . . . . ?
C6 C11 C10 C9 0.9(5) . . . . ?
C6 C7 C8 C9 0.6(5) . . . . ?
C6 C5 C4 C3 178.1(4) . . . . ?
C17 C18 C13 N2 -179.5(4) . . . . ?
C17 C18 C13 C14 0.6(5) . . . . ?
C3 C2 C1 N1 -0.7(6) . . . . ?
C4 C5 C6 C11 -177.8(3) . . . . ?
C4 C5 C6 C7 0.8(6) . . . . ?
#######################################################################
#
# 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_exp_3484
_database_code_depnum_ccdc_archive 'CCDC 1824538'
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_audit_creation_date 2015-09-22
_audit_creation_method
;
Olex2 1.1
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C26 H26 Br N3 Pd'
_chemical_formula_sum 'C26 H26 Br N3 Pd'
_chemical_formula_weight 566.81
_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'
Br Br -0.2901 2.4595 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.6065(6)
_cell_length_b 10.0844(4)
_cell_length_c 18.4740(9)
_cell_angle_alpha 90.00
_cell_angle_beta 98.288(5)
_cell_angle_gamma 90.00
_cell_volume 2324.05(18)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3148
_cell_measurement_temperature 113.8
_cell_measurement_theta_max 29.3599
_cell_measurement_theta_min 2.9397
_exptl_absorpt_coefficient_mu 2.536
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.62689
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.620
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1136
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.12
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0350
_diffrn_reflns_av_unetI/netI 0.0522
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 10476
_diffrn_reflns_theta_full 26.00
_diffrn_reflns_theta_max 26.00
_diffrn_reflns_theta_min 3.01
_diffrn_ambient_temperature 113.8
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -39.00 4.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- -13.4210 89.0000 -77.0000 43
#__ type_ start__ end____ width___ exp.time_
2 omega 14.00 55.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- -13.4210 37.0000 120.0000 41
#__ type_ start__ end____ width___ exp.time_
3 omega -34.00 16.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- -13.4210 89.0000 -167.0000 50
#__ type_ start__ end____ width___ exp.time_
4 omega 55.00 85.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 18.7335 37.0000 -120.0000 30
#__ type_ start__ end____ width___ exp.time_
5 omega -49.00 30.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 18.7335 -77.0000 0.0000 79
;
_diffrn_measurement_device_type 'Xcalibur, Eos, Gemini'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0313813000
_diffrn_orient_matrix_UB_12 0.0451790000
_diffrn_orient_matrix_UB_13 0.0173304000
_diffrn_orient_matrix_UB_21 -0.0436084000
_diffrn_orient_matrix_UB_22 -0.0451299000
_diffrn_orient_matrix_UB_23 -0.0050510000
_diffrn_orient_matrix_UB_31 0.0186340000
_diffrn_orient_matrix_UB_32 -0.0294037000
_diffrn_orient_matrix_UB_33 0.0343479000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 3875
_reflns_number_total 4558
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_refine_diff_density_max 1.385
_refine_diff_density_min -1.092
_refine_diff_density_rms 0.117
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 284
_refine_ls_number_reflns 4558
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0511
_refine_ls_R_factor_gt 0.0405
_refine_ls_restrained_S_all 1.026
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+6.7374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0884
_refine_ls_wR_factor_ref 0.0941
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.41153(2) 0.72389(3) 0.138929(16) 0.01304(10) Uani 1 1 d . . .
Br1 Br 0.55702(4) 0.60359(5) 0.21942(3) 0.02793(14) Uani 1 1 d . . .
N1 N 0.3767(3) 0.5696(4) 0.06370(18) 0.0154(8) Uani 1 1 d . . .
N2 N 0.3851(3) 0.9155(4) 0.25845(18) 0.0145(7) Uani 1 1 d . . .
C15 C 0.4266(3) 1.0346(4) 0.2890(2) 0.0150(9) Uani 1 1 d . . .
C18 C 0.5423(3) 1.2627(5) 0.3241(3) 0.0231(10) Uani 1 1 d . . .
H18 H 0.5815 1.3417 0.3372 0.028 Uiso 1 1 calc R . .
C14 C 0.4359(3) 0.8818(4) 0.2014(2) 0.0142(9) Uani 1 1 d . . .
C6 C 0.2567(3) 0.7352(5) 0.0110(2) 0.0151(9) Uani 1 1 d . . .
C10 C 0.3919(4) 0.3605(5) 0.0054(3) 0.0260(11) Uani 1 1 d . . .
H10 H 0.4249 0.2757 0.0064 0.031 Uiso 1 1 calc R . .
C19 C 0.4636(3) 1.2225(5) 0.3658(2) 0.0215(10) Uani 1 1 d . . .
H19 H 0.4504 1.2745 0.4065 0.026 Uiso 1 1 calc R . .
C5 C 0.1769(3) 0.7784(5) -0.0463(2) 0.0210(10) Uani 1 1 d . . .
N3 N 0.5090(2) 0.9771(4) 0.19486(17) 0.0130(7) Uani 1 1 d . . .
C16 C 0.5060(3) 1.0746(4) 0.2480(2) 0.0133(9) Uani 1 1 d . . .
C9 C 0.3162(4) 0.3950(5) -0.0518(3) 0.0281(11) Uani 1 1 d . . .
H9 H 0.2965 0.3348 -0.0910 0.034 Uiso 1 1 calc R . .
C11 C 0.4207(3) 0.4495(5) 0.0627(2) 0.0198(10) Uani 1 1 d . . .
H11 H 0.4734 0.4237 0.1022 0.024 Uiso 1 1 calc R . .
C7 C 0.2999(3) 0.6055(4) 0.0069(2) 0.0150(9) Uani 1 1 d . . .
C13 C 0.1462(4) 0.6903(6) -0.1070(2) 0.0288(12) Uani 1 1 d . . .
H13 H 0.0941 0.7190 -0.1462 0.035 Uiso 1 1 calc R . .
C20 C 0.4050(3) 1.1082(5) 0.3485(2) 0.0192(10) Uani 1 1 d . . .
H20 H 0.3514 1.0808 0.3766 0.023 Uiso 1 1 calc R . .
C17 C 0.5645(3) 1.1908(4) 0.2647(2) 0.0180(9) Uani 1 1 d . . .
H17 H 0.6174 1.2191 0.2363 0.022 Uiso 1 1 calc R . .
C8 C 0.2675(4) 0.5203(5) -0.0523(2) 0.0228(10) Uani 1 1 d . . .
C12 C 0.1888(4) 0.5690(6) -0.1098(3) 0.0313(12) Uani 1 1 d . . .
H12 H 0.1662 0.5141 -0.1509 0.038 Uiso 1 1 calc R . .
C24 C 0.5822(3) 0.9720(5) 0.1391(2) 0.0187(9) Uani 1 1 d . . .
H24 H 0.5634 0.8899 0.1096 0.022 Uiso 1 1 calc R . .
C23 C 0.3279(4) 0.7816(5) 0.3570(3) 0.0316(12) Uani 1 1 d . . .
H23A H 0.3908 0.7243 0.3579 0.047 Uiso 1 1 calc R . .
H23B H 0.2680 0.7298 0.3706 0.047 Uiso 1 1 calc R . .
H23C H 0.3446 0.8545 0.3918 0.047 Uiso 1 1 calc R . .
C21 C 0.2972(3) 0.8374(5) 0.2810(3) 0.0232(10) Uani 1 1 d . . .
H21 H 0.2850 0.7602 0.2468 0.028 Uiso 1 1 calc R . .
C1 C 0.2991(3) 0.8174(4) 0.0725(2) 0.0145(9) Uani 1 1 d U . .
C2 C 0.2536(3) 0.9422(5) 0.0721(2) 0.0200(9) Uani 1 1 d . . .
H2 H 0.2782 1.0008 0.1112 0.024 Uiso 1 1 calc R . .
C22 C 0.1941(3) 0.9176(5) 0.2718(3) 0.0285(12) Uani 1 1 d . . .
H22A H 0.2031 0.9947 0.3044 0.043 Uiso 1 1 calc R . .
H22B H 0.1354 0.8622 0.2843 0.043 Uiso 1 1 calc R . .
H22C H 0.1773 0.9474 0.2210 0.043 Uiso 1 1 calc R . .
C25 C 0.6974(3) 0.9558(5) 0.1748(3) 0.0275(11) Uani 1 1 d . . .
H25A H 0.7193 1.0340 0.2048 0.041 Uiso 1 1 calc R . .
H25B H 0.7439 0.9463 0.1369 0.041 Uiso 1 1 calc R . .
H25C H 0.7036 0.8766 0.2059 0.041 Uiso 1 1 calc R . .
C4 C 0.1355(3) 0.9069(5) -0.0414(2) 0.0241(11) Uani 1 1 d . . .
H4 H 0.0815 0.9388 -0.0785 0.029 Uiso 1 1 calc R . .
C3 C 0.1734(3) 0.9869(5) 0.0174(2) 0.0242(10) Uani 1 1 d . . .
H3 H 0.1445 1.0733 0.0206 0.029 Uiso 1 1 calc R . .
C26 C 0.5637(4) 1.0865(5) 0.0871(3) 0.0301(12) Uani 1 1 d . . .
H26A H 0.4882 1.0883 0.0649 0.045 Uiso 1 1 calc R . .
H26B H 0.6092 1.0767 0.0486 0.045 Uiso 1 1 calc R . .
H26C H 0.5816 1.1695 0.1137 0.045 Uiso 1 1 calc R . .
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 0.01203(15) 0.01497(18) 0.01189(16) -0.00144(14) 0.00097(11) 0.00054(13)
Br1 0.0258(2) 0.0290(3) 0.0264(3) -0.0008(2) -0.00493(18) 0.0050(2)
N1 0.0162(17) 0.016(2) 0.0141(17) -0.0026(16) 0.0041(13) -0.0036(15)
N2 0.0138(16) 0.0141(19) 0.0165(18) -0.0060(16) 0.0055(13) -0.0021(14)
C15 0.0125(19) 0.016(2) 0.017(2) -0.0015(19) 0.0014(15) 0.0006(17)
C18 0.020(2) 0.016(2) 0.031(3) -0.006(2) -0.0023(18) -0.0039(18)
C14 0.0114(18) 0.019(2) 0.012(2) 0.0025(18) -0.0012(15) 0.0023(17)
C6 0.0104(18) 0.021(2) 0.014(2) 0.0029(19) 0.0026(15) -0.0038(17)
C10 0.033(3) 0.018(3) 0.029(3) -0.005(2) 0.010(2) 0.003(2)
C19 0.024(2) 0.019(2) 0.022(2) -0.011(2) 0.0016(18) 0.0022(19)
C5 0.017(2) 0.026(3) 0.019(2) 0.007(2) 0.0009(17) -0.0041(19)
N3 0.0115(15) 0.0162(19) 0.0109(16) 0.0007(15) 0.0008(12) -0.0001(14)
C16 0.0102(18) 0.016(2) 0.0131(19) 0.0014(18) 0.0005(15) 0.0022(16)
C9 0.034(3) 0.028(3) 0.022(2) -0.011(2) 0.006(2) -0.008(2)
C11 0.023(2) 0.021(3) 0.016(2) 0.000(2) 0.0055(17) -0.0001(19)
C7 0.0141(19) 0.020(2) 0.0115(19) 0.0010(18) 0.0048(15) -0.0046(17)
C13 0.027(2) 0.036(3) 0.019(2) 0.003(2) -0.0085(19) -0.011(2)
C20 0.017(2) 0.020(2) 0.021(2) -0.004(2) 0.0043(17) 0.0004(18)
C17 0.017(2) 0.016(2) 0.020(2) 0.0005(19) 0.0007(17) -0.0013(17)
C8 0.029(2) 0.023(3) 0.017(2) -0.005(2) 0.0040(18) -0.008(2)
C12 0.037(3) 0.035(3) 0.019(2) -0.006(2) -0.005(2) -0.009(2)
C24 0.019(2) 0.023(3) 0.016(2) -0.003(2) 0.0088(16) -0.0052(18)
C23 0.033(3) 0.029(3) 0.036(3) 0.006(2) 0.015(2) -0.004(2)
C21 0.019(2) 0.023(3) 0.029(2) -0.005(2) 0.0102(18) -0.0081(19)
C1 0.0162(11) 0.0144(12) 0.0144(11) 0.0015(9) 0.0068(9) 0.0009(9)
C2 0.020(2) 0.021(2) 0.019(2) -0.003(2) 0.0050(17) -0.0013(19)
C22 0.018(2) 0.038(3) 0.031(3) -0.012(2) 0.0075(19) -0.005(2)
C25 0.019(2) 0.036(3) 0.030(3) -0.001(2) 0.0101(19) 0.002(2)
C4 0.018(2) 0.031(3) 0.022(2) 0.009(2) -0.0006(18) 0.000(2)
C3 0.026(2) 0.020(3) 0.030(3) 0.010(2) 0.0138(19) 0.009(2)
C26 0.029(2) 0.040(3) 0.023(2) 0.001(2) 0.0081(19) -0.008(2)
_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 Br1 2.5020(5) . ?
Pd1 N1 2.091(3) . ?
Pd1 C14 1.965(4) . ?
Pd1 C1 1.975(4) . ?
N1 C11 1.334(6) . ?
N1 C7 1.370(5) . ?
N2 C15 1.396(5) . ?
N2 C14 1.353(5) . ?
N2 C21 1.468(5) . ?
C15 C16 1.399(6) . ?
C15 C20 1.385(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.400(7) . ?
C18 C17 1.378(6) . ?
C14 N3 1.348(5) . ?
C6 C5 1.419(5) . ?
C6 C7 1.423(6) . ?
C6 C1 1.445(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.364(7) . ?
C10 C11 1.395(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(6) . ?
C5 C13 1.439(7) . ?
C5 C4 1.404(7) . ?
N3 C16 1.394(5) . ?
N3 C24 1.480(5) . ?
C16 C17 1.395(6) . ?
C9 H9 0.9500 . ?
C9 C8 1.404(7) . ?
C11 H11 0.9500 . ?
C7 C8 1.405(6) . ?
C13 H13 0.9500 . ?
C13 C12 1.340(7) . ?
C20 H20 0.9500 . ?
C17 H17 0.9500 . ?
C8 C12 1.432(6) . ?
C12 H12 0.9500 . ?
C24 H24 1.0000 . ?
C24 C25 1.515(6) . ?
C24 C26 1.499(7) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C21 1.511(7) . ?
C21 H21 1.0000 . ?
C21 C22 1.520(6) . ?
C1 C2 1.383(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.397(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C4 H4 0.9500 . ?
C4 C3 1.381(7) . ?
C3 H3 0.9500 . ?
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
N1 Pd1 Br1 95.73(10) . . ?
C14 Pd1 Br1 90.26(11) . . ?
C14 Pd1 N1 173.72(15) . . ?
C14 Pd1 C1 90.91(17) . . ?
C1 Pd1 Br1 178.04(12) . . ?
C1 Pd1 N1 83.05(16) . . ?
C11 N1 Pd1 129.6(3) . . ?
C11 N1 C7 118.6(4) . . ?
C7 N1 Pd1 111.7(3) . . ?
C15 N2 C21 126.9(4) . . ?
C14 N2 C15 109.9(3) . . ?
C14 N2 C21 123.2(4) . . ?
N2 C15 C16 106.5(4) . . ?
C20 C15 N2 132.6(4) . . ?
C20 C15 C16 120.9(4) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C17 C18 C19 121.9(4) . . ?
N2 C14 Pd1 127.6(3) . . ?
N3 C14 Pd1 125.2(3) . . ?
N3 C14 N2 107.3(4) . . ?
C5 C6 C7 118.6(4) . . ?
C5 C6 C1 123.5(4) . . ?
C7 C6 C1 117.9(3) . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.1(5) . . ?
C11 C10 H10 120.0 . . ?
C18 C19 H19 119.6 . . ?
C20 C19 C18 120.8(4) . . ?
C20 C19 H19 119.6 . . ?
C6 C5 C13 118.3(4) . . ?
C4 C5 C6 117.7(4) . . ?
C4 C5 C13 124.0(4) . . ?
C14 N3 C16 110.6(3) . . ?
C14 N3 C24 122.7(4) . . ?
C16 N3 C24 126.8(3) . . ?
N3 C16 C15 105.8(4) . . ?
N3 C16 C17 132.9(4) . . ?
C17 C16 C15 121.3(4) . . ?
C10 C9 H9 120.3 . . ?
C10 C9 C8 119.4(4) . . ?
C8 C9 H9 120.3 . . ?
N1 C11 C10 122.1(4) . . ?
N1 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
N1 C7 C6 115.9(4) . . ?
N1 C7 C8 121.9(4) . . ?
C8 C7 C6 122.2(4) . . ?
C5 C13 H13 119.0 . . ?
C12 C13 C5 122.0(4) . . ?
C12 C13 H13 119.0 . . ?
C15 C20 H20 121.0 . . ?
C19 C20 C15 118.0(4) . . ?
C19 C20 H20 121.0 . . ?
C18 C17 C16 117.1(4) . . ?
C18 C17 H17 121.4 . . ?
C16 C17 H17 121.4 . . ?
C9 C8 C7 117.9(4) . . ?
C9 C8 C12 124.7(4) . . ?
C7 C8 C12 117.4(4) . . ?
C13 C12 C8 121.5(5) . . ?
C13 C12 H12 119.2 . . ?
C8 C12 H12 119.2 . . ?
N3 C24 H24 106.6 . . ?
N3 C24 C25 110.8(3) . . ?
N3 C24 C26 111.4(4) . . ?
C25 C24 H24 106.6 . . ?
C26 C24 H24 106.6 . . ?
C26 C24 C25 114.4(4) . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
N2 C21 C23 111.2(4) . . ?
N2 C21 H21 107.0 . . ?
N2 C21 C22 110.6(4) . . ?
C23 C21 H21 107.0 . . ?
C23 C21 C22 113.6(4) . . ?
C22 C21 H21 107.0 . . ?
C6 C1 Pd1 111.5(3) . . ?
C2 C1 Pd1 134.2(3) . . ?
C2 C1 C6 114.3(4) . . ?
C1 C2 H2 118.2 . . ?
C1 C2 C3 123.6(4) . . ?
C3 C2 H2 118.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 H3 119.6 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
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 C11 C10 -176.1(3) . . . . ?
Pd1 N1 C7 C6 -2.2(4) . . . . ?
Pd1 N1 C7 C8 176.6(3) . . . . ?
Pd1 C14 N3 C16 -179.6(3) . . . . ?
Pd1 C14 N3 C24 -1.1(5) . . . . ?
Pd1 C1 C2 C3 179.7(3) . . . . ?
Br1 Pd1 N1 C11 0.2(4) . . . . ?
Br1 Pd1 N1 C7 -176.9(3) . . . . ?
Br1 Pd1 C14 N2 -93.2(3) . . . . ?
Br1 Pd1 C14 N3 86.1(3) . . . . ?
Br1 Pd1 C1 C6 51(4) . . . . ?
Br1 Pd1 C1 C2 -129(4) . . . . ?
N1 Pd1 C14 N2 104.3(14) . . . . ?
N1 Pd1 C14 N3 -76.3(14) . . . . ?
N1 Pd1 C1 C6 -0.6(3) . . . . ?
N1 Pd1 C1 C2 179.6(4) . . . . ?
N1 C7 C8 C9 0.3(6) . . . . ?
N1 C7 C8 C12 -178.3(4) . . . . ?
N2 C15 C16 N3 -0.2(4) . . . . ?
N2 C15 C16 C17 -179.6(3) . . . . ?
N2 C15 C20 C19 178.2(4) . . . . ?
N2 C14 N3 C16 -0.1(4) . . . . ?
N2 C14 N3 C24 178.4(3) . . . . ?
C15 N2 C14 Pd1 179.4(3) . . . . ?
C15 N2 C14 N3 -0.1(4) . . . . ?
C15 N2 C21 C23 -66.0(6) . . . . ?
C15 N2 C21 C22 61.2(5) . . . . ?
C15 C16 C17 C18 1.5(6) . . . . ?
C18 C19 C20 C15 0.2(6) . . . . ?
C14 Pd1 N1 C11 162.5(12) . . . . ?
C14 Pd1 N1 C7 -14.5(15) . . . . ?
C14 Pd1 C1 C6 177.6(3) . . . . ?
C14 Pd1 C1 C2 -2.2(4) . . . . ?
C14 N2 C15 C16 0.2(4) . . . . ?
C14 N2 C15 C20 -177.7(4) . . . . ?
C14 N2 C21 C23 116.4(5) . . . . ?
C14 N2 C21 C22 -116.4(4) . . . . ?
C14 N3 C16 C15 0.2(4) . . . . ?
C14 N3 C16 C17 179.4(4) . . . . ?
C14 N3 C24 C25 -113.7(4) . . . . ?
C14 N3 C24 C26 117.8(4) . . . . ?
C6 C5 C13 C12 1.4(7) . . . . ?
C6 C5 C4 C3 0.7(6) . . . . ?
C6 C7 C8 C9 179.1(4) . . . . ?
C6 C7 C8 C12 0.4(6) . . . . ?
C6 C1 C2 C3 -0.1(6) . . . . ?
C10 C9 C8 C7 0.2(7) . . . . ?
C10 C9 C8 C12 178.8(5) . . . . ?
C19 C18 C17 C16 -0.8(6) . . . . ?
C5 C6 C7 N1 179.9(4) . . . . ?
C5 C6 C7 C8 1.1(6) . . . . ?
C5 C6 C1 Pd1 -178.3(3) . . . . ?
C5 C6 C1 C2 1.5(6) . . . . ?
C5 C13 C12 C8 0.0(8) . . . . ?
C5 C4 C3 C2 0.7(7) . . . . ?
N3 C16 C17 C18 -177.7(4) . . . . ?
C16 C15 C20 C19 0.5(6) . . . . ?
C16 N3 C24 C25 64.5(6) . . . . ?
C16 N3 C24 C26 -64.0(5) . . . . ?
C9 C10 C11 N1 -0.2(7) . . . . ?
C9 C8 C12 C13 -179.5(5) . . . . ?
C11 N1 C7 C6 -179.6(4) . . . . ?
C11 N1 C7 C8 -0.8(6) . . . . ?
C11 C10 C9 C8 -0.3(7) . . . . ?
C7 N1 C11 C10 0.7(6) . . . . ?
C7 C6 C5 C13 -1.9(6) . . . . ?
C7 C6 C5 C4 -179.8(4) . . . . ?
C7 C6 C1 Pd1 -0.4(5) . . . . ?
C7 C6 C1 C2 179.5(4) . . . . ?
C7 C8 C12 C13 -1.0(7) . . . . ?
C13 C5 C4 C3 -177.0(4) . . . . ?
C20 C15 C16 N3 178.0(4) . . . . ?
C20 C15 C16 C17 -1.3(6) . . . . ?
C17 C18 C19 C20 0.0(7) . . . . ?
C24 N3 C16 C15 -178.2(4) . . . . ?
C24 N3 C16 C17 1.0(7) . . . . ?
C21 N2 C15 C16 -177.7(4) . . . . ?
C21 N2 C15 C20 4.4(7) . . . . ?
C21 N2 C14 Pd1 -2.6(6) . . . . ?
C21 N2 C14 N3 177.9(4) . . . . ?
C1 Pd1 N1 C11 178.6(4) . . . . ?
C1 Pd1 N1 C7 1.6(3) . . . . ?
C1 Pd1 C14 N2 88.3(4) . . . . ?
C1 Pd1 C14 N3 -92.3(3) . . . . ?
C1 C6 C5 C13 176.0(4) . . . . ?
C1 C6 C5 C4 -1.8(6) . . . . ?
C1 C6 C7 N1 1.8(5) . . . . ?
C1 C6 C7 C8 -177.0(4) . . . . ?
C1 C2 C3 C4 -1.0(7) . . . . ?
C4 C5 C13 C12 179.1(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_20170721a
_database_code_depnum_ccdc_archive 'CCDC 1824537'
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_audit_creation_date 2017-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C25 H28 Br N3 Pd'
_chemical_formula_sum 'C25 H28 Br N3 Pd'
_chemical_formula_weight 556.81
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1n1o1Cl1Pd1
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'
Br Br -0.2901 2.4595 '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'
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 monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 10.9330(5)
_cell_length_b 23.8367(10)
_cell_length_c 18.1370(7)
_cell_angle_alpha 90
_cell_angle_beta 98.263(4)
_cell_angle_gamma 90
_cell_volume 4677.6(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 6460
_cell_measurement_temperature 99.9(2)
_cell_measurement_theta_max 28.7810
_cell_measurement_theta_min 3.8020
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.518
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.68014
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.581
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2240
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.15
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0486
_diffrn_reflns_av_unetI/netI 0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 24217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.499
_diffrn_reflns_theta_min 3.285
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 99.9(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 4.00 83.00 1.00 5.00 -- 12.61 57.00-120.00 79
2 \w -35.00 13.00 1.00 5.00 -- 12.61 -37.00 150.00 48
3 \w -16.00 84.00 1.00 5.00 -- 12.61 57.00 -30.00 100
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0322343000
_diffrn_orient_matrix_UB_12 0.0059233000
_diffrn_orient_matrix_UB_13 0.0359442000
_diffrn_orient_matrix_UB_21 -0.0562246000
_diffrn_orient_matrix_UB_22 -0.0017903000
_diffrn_orient_matrix_UB_23 0.0151324000
_diffrn_orient_matrix_UB_31 0.0099127000
_diffrn_orient_matrix_UB_32 -0.0290989000
_diffrn_orient_matrix_UB_33 0.0064039000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6869
_reflns_number_total 8678
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.858
_refine_diff_density_min -0.852
_refine_diff_density_rms 0.117
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 551
_refine_ls_number_reflns 8678
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0594
_refine_ls_R_factor_gt 0.0414
_refine_ls_restrained_S_all 1.045
_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^)+(0.0219P)^2^+3.3701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0725
_refine_ls_wR_factor_ref 0.0796
_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 Ternary CH refined with riding coordinates:
C14(H14), C23(H23), C39(H39), C48(H48)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C18(H18), C19(H19),
C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
C35(H35), C43(H43), C44(H44), C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
H24C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C41(H41A,
H41B,H41C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_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
Br1 Br 0.99174(4) 0.38347(2) 0.62171(2) 0.02037(11) Uani 1 1 d . . . . .
C1 C 0.7138(4) 0.44766(17) 0.6560(2) 0.0188(10) Uani 1 1 d . . . . .
H1 H 0.7944 0.4435 0.6799 0.023 Uiso 1 1 calc R . . . .
C2 C 0.6312(4) 0.47892(18) 0.6903(2) 0.0247(11) Uani 1 1 d . . . . .
H2 H 0.6564 0.4962 0.7359 0.030 Uiso 1 1 calc R . . . .
C3 C 0.5115(4) 0.48387(19) 0.6557(2) 0.0290(12) Uani 1 1 d . . . . .
H3 H 0.4539 0.5038 0.6783 0.035 Uiso 1 1 calc R . . . .
C4 C 0.4769(4) 0.45897(18) 0.5868(2) 0.0274(11) Uani 1 1 d . . . . .
H4 H 0.3960 0.4619 0.5630 0.033 Uiso 1 1 calc R . . . .
C5 C 0.5645(4) 0.42957(16) 0.5537(2) 0.0183(10) Uani 1 1 d . . . . .
C6 C 0.5413(4) 0.40306(17) 0.4801(2) 0.0193(10) Uani 1 1 d . . . . .
C7 C 0.4270(4) 0.4052(2) 0.4349(2) 0.0319(12) Uani 1 1 d . . . . .
H7 H 0.3627 0.4256 0.4503 0.038 Uiso 1 1 calc R . . . .
C8 C 0.4082(4) 0.3773(2) 0.3668(2) 0.0328(12) Uani 1 1 d . . . . .
H8 H 0.3318 0.3792 0.3368 0.039 Uiso 1 1 calc R . . . .
C9 C 0.5044(4) 0.34644(18) 0.3436(2) 0.0221(10) Uani 1 1 d . . . . .
C10 C 0.6194(4) 0.34758(17) 0.3870(2) 0.0172(9) Uani 1 1 d . . . . .
H10 H 0.6846 0.3291 0.3698 0.021 Uiso 1 1 calc R . . . .
C11 C 0.6418(4) 0.37515(16) 0.4552(2) 0.0142(9) Uani 1 1 d . . . . .
C12 C 0.4783(4) 0.31132(18) 0.2739(2) 0.0223(10) Uani 1 1 d . . . . .
H12A H 0.4284 0.2797 0.2831 0.033 Uiso 1 1 calc GR . . . .
H12B H 0.5549 0.2984 0.2598 0.033 Uiso 1 1 calc GR . . . .
H12C H 0.4351 0.3336 0.2343 0.033 Uiso 1 1 calc GR . . . .
C13 C 0.8943(4) 0.34338(16) 0.4566(2) 0.0133(9) Uani 1 1 d . . . . .
C14 C 0.9520(4) 0.43288(15) 0.3999(2) 0.0154(9) Uani 1 1 d . . . . .
H14 H 0.9035 0.4471 0.4373 0.018 Uiso 1 1 calc R . . . .
C15 C 0.8890(4) 0.45362(18) 0.3249(2) 0.0260(11) Uani 1 1 d . . . . .
H15A H 0.8780 0.4935 0.3268 0.039 Uiso 1 1 calc GR . . . .
H15B H 0.8099 0.4358 0.3131 0.039 Uiso 1 1 calc GR . . . .
H15C H 0.9393 0.4447 0.2872 0.039 Uiso 1 1 calc GR . . . .
C16 C 1.0835(4) 0.45495(17) 0.4214(2) 0.0218(10) Uani 1 1 d . . . . .
H16A H 1.1336 0.4433 0.3848 0.033 Uiso 1 1 calc GR . . . .
H16B H 1.1175 0.4402 0.4693 0.033 Uiso 1 1 calc GR . . . .
H16C H 1.0819 0.4952 0.4237 0.033 Uiso 1 1 calc GR . . . .
C17 C 1.0079(4) 0.33275(16) 0.3632(2) 0.0137(9) Uani 1 1 d . . . . .
C18 C 1.0760(4) 0.33976(17) 0.3041(2) 0.0169(9) Uani 1 1 d . . . . .
H18 H 1.0908 0.3752 0.2858 0.020 Uiso 1 1 calc R . . . .
C19 C 1.1199(4) 0.29234(18) 0.2742(2) 0.0215(10) Uani 1 1 d . . . . .
H19 H 1.1653 0.2959 0.2349 0.026 Uiso 1 1 calc R . . . .
C20 C 1.0983(4) 0.23842(18) 0.3011(2) 0.0275(11) Uani 1 1 d . . . . .
H20 H 1.1290 0.2071 0.2794 0.033 Uiso 1 1 calc R . . . .
C21 C 1.0318(4) 0.23184(17) 0.3597(2) 0.0254(11) Uani 1 1 d . . . . .
H21 H 1.0174 0.1964 0.3780 0.030 Uiso 1 1 calc R . . . .
C22 C 0.9868(4) 0.27967(16) 0.3907(2) 0.0171(9) Uani 1 1 d . . . . .
C23 C 0.8756(4) 0.24472(16) 0.4980(2) 0.0175(10) Uani 1 1 d . . . . .
H23 H 0.8320 0.2643 0.5341 0.021 Uiso 1 1 calc R . . . .
C24 C 0.9866(4) 0.21578(17) 0.5421(2) 0.0225(10) Uani 1 1 d . . . . .
H24A H 0.9588 0.1886 0.5751 0.034 Uiso 1 1 calc GR . . . .
H24B H 1.0376 0.2431 0.5707 0.034 Uiso 1 1 calc GR . . . .
H24C H 1.0336 0.1973 0.5084 0.034 Uiso 1 1 calc GR . . . .
C25 C 0.7840(4) 0.20488(17) 0.4551(2) 0.0257(11) Uani 1 1 d . . . . .
H25A H 0.8232 0.1853 0.4186 0.039 Uiso 1 1 calc GR . . . .
H25B H 0.7148 0.2257 0.4305 0.039 Uiso 1 1 calc GR . . . .
H25C H 0.7560 0.1783 0.4888 0.039 Uiso 1 1 calc GR . . . .
N1 N 0.6814(3) 0.42328(13) 0.58940(17) 0.0147(8) Uani 1 1 d . . . . .
N2 N 0.9500(3) 0.37102(12) 0.40500(16) 0.0109(7) Uani 1 1 d . . . . .
N3 N 0.9168(3) 0.28783(13) 0.44868(17) 0.0142(8) Uani 1 1 d . . . . .
Pd1 Pd 0.79832(3) 0.37977(2) 0.52734(2) 0.01148(8) Uani 1 1 d . . . . .
Br2 Br 0.21083(4) 0.09621(2) 0.64175(2) 0.02464(12) Uani 1 1 d . . . . .
C26 C 0.0063(4) 0.06690(17) 0.4788(2) 0.0216(10) Uani 1 1 d . . . . .
H26 H 0.0056 0.0680 0.5300 0.026 Uiso 1 1 calc R . . . .
C27 C -0.0996(4) 0.05076(19) 0.4333(2) 0.0265(11) Uani 1 1 d . . . . .
H27 H -0.1700 0.0403 0.4533 0.032 Uiso 1 1 calc R . . . .
C28 C -0.0989(4) 0.05042(19) 0.3570(2) 0.0281(11) Uani 1 1 d . . . . .
H28 H -0.1694 0.0400 0.3251 0.034 Uiso 1 1 calc R . . . .
C29 C 0.0061(4) 0.06556(17) 0.3287(2) 0.0238(11) Uani 1 1 d . . . . .
H29 H 0.0068 0.0656 0.2775 0.029 Uiso 1 1 calc R . . . .
C30 C 0.1116(4) 0.08083(16) 0.3769(2) 0.0171(10) Uani 1 1 d . . . . .
C31 C 0.2291(4) 0.09800(16) 0.3550(2) 0.0165(9) Uani 1 1 d . . . . .
C32 C 0.2496(4) 0.09809(17) 0.2805(2) 0.0213(10) Uani 1 1 d . . . . .
H32 H 0.1869 0.0871 0.2431 0.026 Uiso 1 1 calc R . . . .
C33 C 0.3623(4) 0.11443(16) 0.2627(2) 0.0203(10) Uani 1 1 d . . . . .
H33 H 0.3750 0.1144 0.2131 0.024 Uiso 1 1 calc R . . . .
C34 C 0.4573(4) 0.13091(16) 0.3171(2) 0.0201(10) Uani 1 1 d . . . . .
C35 C 0.4366(4) 0.13121(16) 0.3913(2) 0.0186(10) Uani 1 1 d . . . . .
H35 H 0.5003 0.1421 0.4281 0.022 Uiso 1 1 calc R . . . .
C36 C 0.3241(4) 0.11572(15) 0.4117(2) 0.0154(9) Uani 1 1 d . . . . .
C37 C 0.5817(4) 0.14869(18) 0.2973(2) 0.0273(11) Uani 1 1 d . . . . .
H37A H 0.5854 0.1400 0.2460 0.041 Uiso 1 1 calc GR . . . .
H37B H 0.6462 0.1290 0.3284 0.041 Uiso 1 1 calc GR . . . .
H37C H 0.5922 0.1883 0.3051 0.041 Uiso 1 1 calc GR . . . .
C38 C 0.4250(4) 0.14843(17) 0.55976(19) 0.0148(9) Uani 1 1 d . . . . .
C39 C 0.3420(5) 0.24553(19) 0.5408(2) 0.0328(12) Uani 1 1 d . . . . .
H39 H 0.2693 0.2214 0.5290 0.039 Uiso 1 1 calc R . . . .
C40 C 0.3095(4) 0.28037(19) 0.6032(2) 0.0319(12) Uani 1 1 d . . . . .
H40A H 0.3729 0.3079 0.6168 0.048 Uiso 1 1 calc GR . . . .
H40B H 0.3026 0.2568 0.6453 0.048 Uiso 1 1 calc GR . . . .
H40C H 0.2321 0.2989 0.5879 0.048 Uiso 1 1 calc GR . . . .
C41 C 0.3542(7) 0.2695(2) 0.4706(3) 0.069(2) Uani 1 1 d . . . . .
H41A H 0.2797 0.2892 0.4517 0.104 Uiso 1 1 calc GR . . . .
H41B H 0.3686 0.2403 0.4364 0.104 Uiso 1 1 calc GR . . . .
H41C H 0.4225 0.2952 0.4762 0.104 Uiso 1 1 calc GR . . . .
C42 C 0.5601(4) 0.21648(16) 0.6028(2) 0.0148(9) Uani 1 1 d . . . . .
C43 C 0.6208(4) 0.26633(17) 0.6237(2) 0.0205(10) Uani 1 1 d . . . . .
H43 H 0.5839 0.3008 0.6106 0.025 Uiso 1 1 calc R . . . .
C44 C 0.7372(4) 0.26344(17) 0.6642(2) 0.0231(11) Uani 1 1 d . . . . .
H44 H 0.7793 0.2964 0.6790 0.028 Uiso 1 1 calc R . . . .
C45 C 0.7932(4) 0.21160(18) 0.6837(2) 0.0228(10) Uani 1 1 d . . . . .
H45 H 0.8709 0.2107 0.7123 0.027 Uiso 1 1 calc R . . . .
C46 C 0.7346(4) 0.16167(17) 0.6610(2) 0.0186(10) Uani 1 1 d . . . . .
H46 H 0.7726 0.1273 0.6726 0.022 Uiso 1 1 calc R . . . .
C47 C 0.6174(4) 0.16476(15) 0.6203(2) 0.0131(9) Uani 1 1 d . . . . .
C48 C 0.5481(4) 0.06232(16) 0.5947(2) 0.0179(10) Uani 1 1 d . . . . .
H48 H 0.4714 0.0459 0.5691 0.021 Uiso 1 1 calc R . . . .
C49 C 0.6508(4) 0.04466(17) 0.5519(2) 0.0245(11) Uani 1 1 d . . . . .
H49A H 0.7283 0.0586 0.5767 0.037 Uiso 1 1 calc GR . . . .
H49B H 0.6354 0.0597 0.5023 0.037 Uiso 1 1 calc GR . . . .
H49C H 0.6537 0.0045 0.5495 0.037 Uiso 1 1 calc GR . . . .
C50 C 0.5643(4) 0.04102(18) 0.6747(2) 0.0248(11) Uani 1 1 d . . . . .
H50A H 0.5639 0.0007 0.6748 0.037 Uiso 1 1 calc GR . . . .
H50B H 0.4977 0.0546 0.6990 0.037 Uiso 1 1 calc GR . . . .
H50C H 0.6415 0.0543 0.7008 0.037 Uiso 1 1 calc GR . . . .
N4 N 0.1101(3) 0.08107(13) 0.45235(17) 0.0145(8) Uani 1 1 d . . . . .
N5 N 0.4419(3) 0.20460(13) 0.56644(17) 0.0186(8) Uani 1 1 d . . . . .
N6 N 0.5324(3) 0.12385(13) 0.59212(17) 0.0141(8) Uani 1 1 d . . . . .
Pd2 Pd 0.27246(3) 0.11119(2) 0.51367(2) 0.01529(9) 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
Br1 0.0186(3) 0.0223(2) 0.0181(2) -0.00559(18) -0.00455(19) 0.00336(19)
C1 0.019(3) 0.022(2) 0.014(2) 0.0012(18) -0.0015(19) 0.0026(19)
C2 0.027(3) 0.031(3) 0.015(2) -0.008(2) 0.001(2) 0.007(2)
C3 0.027(3) 0.037(3) 0.025(2) -0.010(2) 0.009(2) 0.015(2)
C4 0.020(3) 0.036(3) 0.026(2) -0.010(2) 0.003(2) 0.008(2)
C5 0.020(3) 0.018(2) 0.017(2) -0.0025(18) 0.002(2) -0.0006(19)
C6 0.015(2) 0.023(2) 0.019(2) -0.0053(19) -0.0014(19) -0.0014(19)
C7 0.014(3) 0.046(3) 0.033(3) -0.021(2) -0.003(2) 0.009(2)
C8 0.014(3) 0.052(3) 0.030(3) -0.018(2) -0.006(2) 0.008(2)
C9 0.024(3) 0.029(2) 0.014(2) -0.0027(19) 0.003(2) 0.004(2)
C10 0.013(2) 0.026(2) 0.014(2) -0.0016(18) 0.0069(19) 0.0030(19)
C11 0.011(2) 0.018(2) 0.014(2) 0.0018(18) 0.0045(18) 0.0011(18)
C12 0.020(3) 0.033(3) 0.014(2) -0.0053(19) 0.003(2) 0.001(2)
C13 0.010(2) 0.016(2) 0.0120(19) 0.0020(17) -0.0052(18) -0.0007(17)
C14 0.014(2) 0.011(2) 0.022(2) -0.0011(18) 0.0043(19) -0.0006(17)
C15 0.028(3) 0.022(2) 0.027(2) 0.007(2) 0.000(2) 0.007(2)
C16 0.019(3) 0.019(2) 0.026(2) -0.0018(19) 0.002(2) -0.0007(19)
C17 0.012(2) 0.016(2) 0.013(2) -0.0027(17) 0.0029(18) 0.0033(17)
C18 0.016(2) 0.018(2) 0.017(2) 0.0006(18) 0.0041(19) 0.0015(18)
C19 0.018(3) 0.031(3) 0.017(2) 0.001(2) 0.007(2) 0.002(2)
C20 0.037(3) 0.024(2) 0.024(2) -0.004(2) 0.013(2) 0.011(2)
C21 0.039(3) 0.014(2) 0.024(2) 0.0025(19) 0.011(2) 0.006(2)
C22 0.017(3) 0.017(2) 0.018(2) 0.0013(18) 0.0051(19) 0.0042(18)
C23 0.025(3) 0.013(2) 0.016(2) 0.0016(18) 0.009(2) 0.0006(18)
C24 0.026(3) 0.019(2) 0.024(2) 0.0077(19) 0.009(2) -0.0006(19)
C25 0.034(3) 0.018(2) 0.027(2) 0.003(2) 0.009(2) -0.003(2)
N1 0.017(2) 0.0138(17) 0.0142(17) -0.0028(14) 0.0038(16) 0.0005(15)
N2 0.0122(19) 0.0089(16) 0.0117(16) 0.0010(14) 0.0018(14) -0.0003(14)
N3 0.017(2) 0.0144(17) 0.0129(17) 0.0006(14) 0.0062(15) -0.0005(15)
Pd1 0.01141(18) 0.01290(16) 0.01002(15) -0.00213(12) 0.00115(13) 0.00067(13)
Br2 0.0246(3) 0.0342(3) 0.0151(2) -0.00479(19) 0.00274(19) -0.0017(2)
C26 0.022(3) 0.024(2) 0.019(2) -0.0018(19) 0.000(2) 0.004(2)
C27 0.021(3) 0.034(3) 0.025(2) -0.003(2) 0.005(2) 0.000(2)
C28 0.021(3) 0.035(3) 0.025(2) -0.003(2) -0.010(2) 0.000(2)
C29 0.028(3) 0.026(2) 0.016(2) -0.0017(19) -0.003(2) 0.000(2)
C30 0.024(3) 0.010(2) 0.015(2) 0.0013(17) -0.004(2) 0.0046(18)
C31 0.023(3) 0.012(2) 0.013(2) 0.0010(17) -0.0042(19) 0.0047(18)
C32 0.028(3) 0.017(2) 0.018(2) 0.0005(18) -0.002(2) 0.005(2)
C33 0.032(3) 0.017(2) 0.011(2) 0.0032(18) 0.002(2) 0.004(2)
C34 0.029(3) 0.012(2) 0.020(2) 0.0055(18) 0.004(2) -0.0002(19)
C35 0.027(3) 0.016(2) 0.011(2) -0.0015(17) -0.0022(19) 0.0016(19)
C36 0.025(3) 0.0074(19) 0.013(2) 0.0009(17) 0.0020(19) 0.0041(18)
C37 0.040(3) 0.023(2) 0.021(2) 0.002(2) 0.011(2) -0.006(2)
C38 0.017(2) 0.022(2) 0.0055(18) -0.0024(17) 0.0029(18) 0.0056(19)
C39 0.039(3) 0.033(3) 0.025(2) 0.008(2) 0.004(2) 0.022(2)
C40 0.021(3) 0.038(3) 0.036(3) -0.013(2) 0.002(2) 0.003(2)
C41 0.115(6) 0.058(4) 0.031(3) 0.009(3) 0.000(4) 0.057(4)
C42 0.019(3) 0.018(2) 0.0073(19) 0.0030(17) 0.0036(18) 0.0016(18)
C43 0.032(3) 0.016(2) 0.016(2) 0.0032(18) 0.009(2) -0.001(2)
C44 0.028(3) 0.021(2) 0.023(2) -0.0058(19) 0.013(2) -0.011(2)
C45 0.018(3) 0.032(3) 0.019(2) 0.002(2) 0.004(2) -0.007(2)
C46 0.017(3) 0.020(2) 0.018(2) 0.0023(18) 0.0015(19) 0.0039(19)
C47 0.018(2) 0.015(2) 0.0070(18) 0.0038(16) 0.0053(18) -0.0007(18)
C48 0.017(3) 0.013(2) 0.022(2) -0.0004(18) -0.003(2) -0.0015(18)
C49 0.030(3) 0.016(2) 0.027(2) 0.0014(19) 0.005(2) 0.007(2)
C50 0.025(3) 0.024(2) 0.025(2) 0.010(2) 0.001(2) -0.002(2)
N4 0.017(2) 0.0127(17) 0.0131(17) -0.0013(14) -0.0017(16) 0.0029(15)
N5 0.024(2) 0.0163(18) 0.0134(17) -0.0005(15) -0.0028(16) 0.0108(16)
N6 0.020(2) 0.0118(17) 0.0109(16) -0.0021(14) 0.0022(15) 0.0016(15)
Pd2 0.01698(19) 0.01679(17) 0.01099(16) -0.00265(13) -0.00172(14) 0.00345(14)
_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
Br1 Pd1 2.5236(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.386(6) . ?
C1 N1 1.341(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.374(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(6) . ?
C5 C6 1.464(5) . ?
C5 N1 1.355(5) . ?
C6 C7 1.394(6) . ?
C6 C11 1.414(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.392(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.397(6) . ?
C9 C10 1.385(6) . ?
C9 C12 1.509(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.391(5) . ?
C11 Pd1 2.002(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N2 1.358(5) . ?
C13 N3 1.358(5) . ?
C13 Pd1 1.972(4) . ?
C14 H14 0.9800 . ?
C14 C15 1.517(5) . ?
C14 C16 1.527(6) . ?
C14 N2 1.478(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.400(5) . ?
C17 C22 1.391(5) . ?
C17 N2 1.395(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.370(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.407(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.379(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.392(6) . ?
C22 N3 1.401(5) . ?
C23 H23 0.9800 . ?
C23 C24 1.520(6) . ?
C23 C25 1.512(6) . ?
C23 N3 1.475(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
N1 Pd1 2.095(3) . ?
Br2 Pd2 2.5354(5) . ?
C26 H26 0.9300 . ?
C26 C27 1.376(6) . ?
C26 N4 1.338(5) . ?
C27 H27 0.9300 . ?
C27 C28 1.385(6) . ?
C28 H28 0.9300 . ?
C28 C29 1.372(6) . ?
C29 H29 0.9300 . ?
C29 C30 1.392(6) . ?
C30 C31 1.457(6) . ?
C30 N4 1.370(5) . ?
C31 C32 1.401(6) . ?
C31 C36 1.416(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.375(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.382(6) . ?
C34 C35 1.397(6) . ?
C34 C37 1.516(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.385(6) . ?
C36 Pd2 2.012(4) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 N5 1.355(5) . ?
C38 N6 1.367(5) . ?
C38 Pd2 1.967(4) . ?
C39 H39 0.9800 . ?
C39 C40 1.488(6) . ?
C39 C41 1.419(6) . ?
C39 N5 1.489(5) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.387(5) . ?
C42 C47 1.399(5) . ?
C42 N5 1.392(5) . ?
C43 H43 0.9300 . ?
C43 C44 1.377(6) . ?
C44 H44 0.9300 . ?
C44 C45 1.401(6) . ?
C45 H45 0.9300 . ?
C45 C46 1.386(6) . ?
C46 H46 0.9300 . ?
C46 C47 1.385(5) . ?
C47 N6 1.393(5) . ?
C48 H48 0.9800 . ?
C48 C49 1.513(6) . ?
C48 C50 1.524(5) . ?
C48 N6 1.477(5) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
N4 Pd2 2.082(3) . ?
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
C2 C1 H1 118.9 . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.2(4) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(4) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(4) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 124.8(4) . . ?
N1 C5 C4 120.6(4) . . ?
N1 C5 C6 114.6(4) . . ?
C7 C6 C5 122.9(4) . . ?
C7 C6 C11 120.1(4) . . ?
C11 C6 C5 117.0(4) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.7(4) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.8(4) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 C12 119.0(4) . . ?
C10 C9 C8 118.7(4) . . ?
C10 C9 C12 122.3(4) . . ?
C9 C10 H10 118.5 . . ?
C9 C10 C11 123.0(4) . . ?
C11 C10 H10 118.5 . . ?
C6 C11 Pd1 113.3(3) . . ?
C10 C11 C6 117.5(4) . . ?
C10 C11 Pd1 129.2(3) . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 N3 107.1(3) . . ?
N2 C13 Pd1 124.6(3) . . ?
N3 C13 Pd1 128.2(3) . . ?
C15 C14 H14 106.7 . . ?
C15 C14 C16 114.0(4) . . ?
C16 C14 H14 106.7 . . ?
N2 C14 H14 106.7 . . ?
N2 C14 C15 111.9(3) . . ?
N2 C14 C16 110.5(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 121.1(4) . . ?
C22 C17 N2 106.8(3) . . ?
N2 C17 C18 132.1(3) . . ?
C17 C18 H18 121.3 . . ?
C19 C18 C17 117.4(4) . . ?
C19 C18 H18 121.3 . . ?
C18 C19 H19 119.0 . . ?
C18 C19 C20 122.0(4) . . ?
C20 C19 H19 119.0 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.3(4) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 120.9 . . ?
C20 C21 C22 118.3(4) . . ?
C22 C21 H21 120.9 . . ?
C17 C22 C21 120.9(4) . . ?
C17 C22 N3 106.2(3) . . ?
C21 C22 N3 132.8(4) . . ?
C24 C23 H23 107.1 . . ?
C25 C23 H23 107.1 . . ?
C25 C23 C24 113.9(3) . . ?
N3 C23 H23 107.1 . . ?
N3 C23 C24 110.2(3) . . ?
N3 C23 C25 111.2(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1 N1 C5 119.5(3) . . ?
C1 N1 Pd1 126.5(3) . . ?
C5 N1 Pd1 113.8(2) . . ?
C13 N2 C14 122.7(3) . . ?
C13 N2 C17 109.9(3) . . ?
C17 N2 C14 127.3(3) . . ?
C13 N3 C22 110.0(3) . . ?
C13 N3 C23 122.6(3) . . ?
C22 N3 C23 127.4(3) . . ?
C11 Pd1 Br1 177.87(11) . . ?
C11 Pd1 N1 81.28(14) . . ?
C13 Pd1 Br1 89.10(11) . . ?
C13 Pd1 C11 92.01(15) . . ?
C13 Pd1 N1 171.99(14) . . ?
N1 Pd1 Br1 97.75(9) . . ?
C27 C26 H26 118.7 . . ?
N4 C26 H26 118.7 . . ?
N4 C26 C27 122.7(4) . . ?
C26 C27 H27 120.8 . . ?
C26 C27 C28 118.4(4) . . ?
C28 C27 H27 120.8 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 119.9(4) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.7(4) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 C31 125.8(4) . . ?
N4 C30 C29 120.1(4) . . ?
N4 C30 C31 114.1(4) . . ?
C32 C31 C30 122.2(4) . . ?
C32 C31 C36 119.9(4) . . ?
C36 C31 C30 117.9(3) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 C31 120.0(4) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 119.3 . . ?
C32 C33 C34 121.3(4) . . ?
C34 C33 H33 119.3 . . ?
C33 C34 C35 118.7(4) . . ?
C33 C34 C37 121.2(4) . . ?
C35 C34 C37 120.1(4) . . ?
C34 C35 H35 119.0 . . ?
C36 C35 C34 121.9(4) . . ?
C36 C35 H35 119.0 . . ?
C31 C36 Pd2 112.2(3) . . ?
C35 C36 C31 118.2(4) . . ?
C35 C36 Pd2 129.6(3) . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N5 C38 N6 106.7(3) . . ?
N5 C38 Pd2 125.5(3) . . ?
N6 C38 Pd2 127.8(3) . . ?
C40 C39 H39 102.6 . . ?
C40 C39 N5 111.9(4) . . ?
C41 C39 H39 102.6 . . ?
C41 C39 C40 121.4(4) . . ?
C41 C39 N5 112.6(4) . . ?
N5 C39 H39 102.6 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C47 120.8(4) . . ?
C43 C42 N5 132.7(4) . . ?
N5 C42 C47 106.5(3) . . ?
C42 C43 H43 120.9 . . ?
C44 C43 C42 118.2(4) . . ?
C44 C43 H43 120.9 . . ?
C43 C44 H44 119.5 . . ?
C43 C44 C45 121.0(4) . . ?
C45 C44 H44 119.5 . . ?
C44 C45 H45 119.5 . . ?
C46 C45 C44 121.0(4) . . ?
C46 C45 H45 119.5 . . ?
C45 C46 H46 121.1 . . ?
C47 C46 C45 117.7(4) . . ?
C47 C46 H46 121.1 . . ?
C46 C47 C42 121.2(4) . . ?
C46 C47 N6 132.5(3) . . ?
N6 C47 C42 106.3(3) . . ?
C49 C48 H48 107.0 . . ?
C49 C48 C50 113.8(3) . . ?
C50 C48 H48 107.0 . . ?
N6 C48 H48 107.0 . . ?
N6 C48 C49 110.6(3) . . ?
N6 C48 C50 111.0(3) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C26 N4 C30 119.3(4) . . ?
C26 N4 Pd2 126.7(3) . . ?
C30 N4 Pd2 113.8(3) . . ?
C38 N5 C39 122.4(4) . . ?
C38 N5 C42 110.4(3) . . ?
C42 N5 C39 127.2(4) . . ?
C38 N6 C47 110.1(3) . . ?
C38 N6 C48 121.9(3) . . ?
C47 N6 C48 128.0(3) . . ?
C36 Pd2 Br2 174.93(10) . . ?
C36 Pd2 N4 81.81(15) . . ?
C38 Pd2 Br2 89.71(11) . . ?
C38 Pd2 C36 91.94(16) . . ?
C38 Pd2 N4 171.28(14) . . ?
N4 Pd2 Br2 97.04(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
C1 C2 C3 C4 -1.7(7) . . . . ?
C2 C1 N1 C5 0.7(6) . . . . ?
C2 C1 N1 Pd1 175.4(3) . . . . ?
C2 C3 C4 C5 -0.4(7) . . . . ?
C3 C4 C5 C6 -177.7(4) . . . . ?
C3 C4 C5 N1 2.7(6) . . . . ?
C4 C5 C6 C7 0.7(7) . . . . ?
C4 C5 C6 C11 179.7(4) . . . . ?
C4 C5 N1 C1 -2.8(6) . . . . ?
C4 C5 N1 Pd1 -178.2(3) . . . . ?
C5 C6 C7 C8 -177.2(4) . . . . ?
C5 C6 C11 C10 177.0(3) . . . . ?
C5 C6 C11 Pd1 -1.2(5) . . . . ?
C6 C5 N1 C1 177.6(3) . . . . ?
C6 C5 N1 Pd1 2.2(4) . . . . ?
C6 C7 C8 C9 0.4(7) . . . . ?
C7 C6 C11 C10 -4.0(6) . . . . ?
C7 C6 C11 Pd1 177.8(3) . . . . ?
C7 C8 C9 C10 -4.3(7) . . . . ?
C7 C8 C9 C12 173.3(4) . . . . ?
C8 C9 C10 C11 4.2(6) . . . . ?
C9 C10 C11 C6 -0.1(6) . . . . ?
C9 C10 C11 Pd1 177.8(3) . . . . ?
C11 C6 C7 C8 3.8(7) . . . . ?
C12 C9 C10 C11 -173.3(4) . . . . ?
C15 C14 N2 C13 -119.5(4) . . . . ?
C15 C14 N2 C17 64.5(5) . . . . ?
C16 C14 N2 C13 112.4(4) . . . . ?
C16 C14 N2 C17 -63.6(5) . . . . ?
C17 C18 C19 C20 0.0(6) . . . . ?
C17 C22 N3 C13 0.5(4) . . . . ?
C17 C22 N3 C23 -176.9(4) . . . . ?
C18 C17 C22 C21 -0.6(6) . . . . ?
C18 C17 C22 N3 -180.0(3) . . . . ?
C18 C17 N2 C13 179.6(4) . . . . ?
C18 C17 N2 C14 -4.0(7) . . . . ?
C18 C19 C20 C21 -0.4(7) . . . . ?
C19 C20 C21 C22 0.3(7) . . . . ?
C20 C21 C22 C17 0.2(7) . . . . ?
C20 C21 C22 N3 179.4(4) . . . . ?
C21 C22 N3 C13 -178.7(5) . . . . ?
C21 C22 N3 C23 3.9(7) . . . . ?
C22 C17 C18 C19 0.5(6) . . . . ?
C22 C17 N2 C13 -0.2(4) . . . . ?
C22 C17 N2 C14 176.2(3) . . . . ?
C24 C23 N3 C13 -115.8(4) . . . . ?
C24 C23 N3 C22 61.3(5) . . . . ?
C25 C23 N3 C13 116.9(4) . . . . ?
C25 C23 N3 C22 -66.0(5) . . . . ?
N1 C1 C2 C3 1.6(6) . . . . ?
N1 C5 C6 C7 -179.7(4) . . . . ?
N1 C5 C6 C11 -0.7(5) . . . . ?
N2 C13 N3 C22 -0.6(4) . . . . ?
N2 C13 N3 C23 176.9(3) . . . . ?
N2 C17 C18 C19 -179.2(4) . . . . ?
N2 C17 C22 C21 179.1(4) . . . . ?
N2 C17 C22 N3 -0.2(4) . . . . ?
N3 C13 N2 C14 -176.1(3) . . . . ?
N3 C13 N2 C17 0.5(4) . . . . ?
Pd1 C13 N2 C14 4.5(5) . . . . ?
Pd1 C13 N2 C17 -178.9(3) . . . . ?
Pd1 C13 N3 C22 178.7(3) . . . . ?
Pd1 C13 N3 C23 -3.8(5) . . . . ?
C26 C27 C28 C29 0.5(7) . . . . ?
C27 C26 N4 C30 1.4(6) . . . . ?
C27 C26 N4 Pd2 175.7(3) . . . . ?
C27 C28 C29 C30 0.4(7) . . . . ?
C28 C29 C30 C31 -179.8(4) . . . . ?
C28 C29 C30 N4 -0.4(6) . . . . ?
C29 C30 C31 C32 -3.3(6) . . . . ?
C29 C30 C31 C36 175.8(4) . . . . ?
C29 C30 N4 C26 -0.5(6) . . . . ?
C29 C30 N4 Pd2 -175.4(3) . . . . ?
C30 C31 C32 C33 -179.7(4) . . . . ?
C30 C31 C36 C35 179.0(3) . . . . ?
C30 C31 C36 Pd2 1.2(4) . . . . ?
C31 C30 N4 C26 178.9(3) . . . . ?
C31 C30 N4 Pd2 4.0(4) . . . . ?
C31 C32 C33 C34 0.1(6) . . . . ?
C32 C31 C36 C35 -1.8(6) . . . . ?
C32 C31 C36 Pd2 -179.6(3) . . . . ?
C32 C33 C34 C35 -0.5(6) . . . . ?
C32 C33 C34 C37 179.8(4) . . . . ?
C33 C34 C35 C36 -0.2(6) . . . . ?
C34 C35 C36 C31 1.4(6) . . . . ?
C34 C35 C36 Pd2 178.7(3) . . . . ?
C36 C31 C32 C33 1.1(6) . . . . ?
C37 C34 C35 C36 179.5(4) . . . . ?
C40 C39 N5 C38 118.6(4) . . . . ?
C40 C39 N5 C42 -58.0(6) . . . . ?
C41 C39 N5 C38 -100.4(5) . . . . ?
C41 C39 N5 C42 83.0(6) . . . . ?
C42 C43 C44 C45 0.3(6) . . . . ?
C42 C47 N6 C38 -1.3(4) . . . . ?
C42 C47 N6 C48 178.9(3) . . . . ?
C43 C42 C47 C46 2.2(6) . . . . ?
C43 C42 C47 N6 179.7(3) . . . . ?
C43 C42 N5 C38 -179.0(4) . . . . ?
C43 C42 N5 C39 -2.1(7) . . . . ?
C43 C44 C45 C46 1.8(6) . . . . ?
C44 C45 C46 C47 -1.8(6) . . . . ?
C45 C46 C47 C42 -0.1(6) . . . . ?
C45 C46 C47 N6 -176.9(4) . . . . ?
C46 C47 N6 C38 175.8(4) . . . . ?
C46 C47 N6 C48 -4.0(7) . . . . ?
C47 C42 C43 C44 -2.2(6) . . . . ?
C47 C42 N5 C38 -1.0(4) . . . . ?
C47 C42 N5 C39 175.9(4) . . . . ?
C49 C48 N6 C38 117.6(4) . . . . ?
C49 C48 N6 C47 -62.7(5) . . . . ?
C50 C48 N6 C38 -115.2(4) . . . . ?
C50 C48 N6 C47 64.6(5) . . . . ?
N4 C26 C27 C28 -1.4(7) . . . . ?
N4 C30 C31 C32 177.3(4) . . . . ?
N4 C30 C31 C36 -3.5(5) . . . . ?
N5 C38 N6 C47 0.7(4) . . . . ?
N5 C38 N6 C48 -179.5(3) . . . . ?
N5 C42 C43 C44 175.6(4) . . . . ?
N5 C42 C47 C46 -176.1(3) . . . . ?
N5 C42 C47 N6 1.4(4) . . . . ?
N6 C38 N5 C39 -176.9(3) . . . . ?
N6 C38 N5 C42 0.2(4) . . . . ?
Pd2 C38 N5 C39 2.0(5) . . . . ?
Pd2 C38 N5 C42 179.1(3) . . . . ?
Pd2 C38 N6 C47 -178.2(3) . . . . ?
Pd2 C38 N6 C48 1.6(5) . . . . ?
_shelx_res_file
;
20170721a.res created by SHELXL-2014/7
TITL 20170721a_a.res in P2(1)/c
REM Old TITL 20170721a in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.127, Rweak 0.008, Alpha 0.052, Orientation as input
REM Formula found by SHELXT: C44 N7 Br2
CELL 0.71073 10.933 23.8367 18.137 90 98.263 90
ZERR 8 0.0005 0.001 0.0007 0 0.004 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N Pd
UNIT 200 224 8 24 8
L.S. 8
PLAN 17
BOND $H
MORE -1
CONF
fmap 2
acta
OMIT -3 51
OMIT -14 3 11
REM
REM
REM
WGHT 0.021900 3.370100
FVAR 1.37284
BR1 3 0.991739 0.383470 0.621713 11.00000 0.01856 0.02232 =
0.01812 -0.00559 -0.00455 0.00336
C1 1 0.713813 0.447665 0.655961 11.00000 0.01904 0.02203 =
0.01434 0.00119 -0.00147 0.00261
AFIX 43
H1 2 0.794421 0.443463 0.679870 11.00000 -1.20000
AFIX 0
C2 1 0.631202 0.478922 0.690318 11.00000 0.02709 0.03117 =
0.01537 -0.00751 0.00094 0.00652
AFIX 43
H2 2 0.656356 0.496207 0.735949 11.00000 -1.20000
AFIX 0
C3 1 0.511454 0.483870 0.655653 11.00000 0.02661 0.03697 =
0.02503 -0.01035 0.00896 0.01496
AFIX 43
H3 2 0.453899 0.503832 0.678275 11.00000 -1.20000
AFIX 0
C4 1 0.476918 0.458971 0.586847 11.00000 0.02045 0.03620 =
0.02569 -0.00992 0.00339 0.00764
AFIX 43
H4 2 0.395955 0.461866 0.563037 11.00000 -1.20000
AFIX 0
C5 1 0.564528 0.429568 0.553655 11.00000 0.01974 0.01757 =
0.01716 -0.00248 0.00167 -0.00065
C6 1 0.541322 0.403062 0.480131 11.00000 0.01475 0.02325 =
0.01890 -0.00535 -0.00137 -0.00138
C7 1 0.427008 0.405235 0.434872 11.00000 0.01438 0.04594 =
0.03340 -0.02123 -0.00313 0.00912
AFIX 43
H7 2 0.362654 0.425553 0.450330 11.00000 -1.20000
AFIX 0
C8 1 0.408203 0.377299 0.366769 11.00000 0.01413 0.05174 =
0.02966 -0.01786 -0.00630 0.00768
AFIX 43
H8 2 0.331787 0.379179 0.336800 11.00000 -1.20000
AFIX 0
C9 1 0.504394 0.346437 0.343556 11.00000 0.02377 0.02867 =
0.01402 -0.00273 0.00339 0.00372
C10 1 0.619397 0.347575 0.386979 11.00000 0.01350 0.02584 =
0.01371 -0.00156 0.00688 0.00301
AFIX 43
H10 2 0.684617 0.329052 0.369762 11.00000 -1.20000
AFIX 0
C11 1 0.641850 0.375154 0.455174 11.00000 0.01144 0.01776 =
0.01429 0.00178 0.00449 0.00108
C12 1 0.478319 0.311324 0.273852 11.00000 0.01960 0.03320 =
0.01425 -0.00531 0.00329 0.00075
AFIX 137
H12A 2 0.428352 0.279684 0.283089 11.00000 -1.50000
H12B 2 0.554874 0.298378 0.259832 11.00000 -1.50000
H12C 2 0.435139 0.333569 0.234287 11.00000 -1.50000
AFIX 0
C13 1 0.894331 0.343380 0.456571 11.00000 0.01021 0.01582 =
0.01202 0.00199 -0.00518 -0.00065
C14 1 0.952024 0.432877 0.399874 11.00000 0.01410 0.01100 =
0.02158 -0.00112 0.00434 -0.00062
AFIX 13
H14 2 0.903477 0.447095 0.437282 11.00000 -1.20000
AFIX 0
C15 1 0.889024 0.453621 0.324857 11.00000 0.02784 0.02160 =
0.02721 0.00705 -0.00027 0.00670
AFIX 137
H15A 2 0.877954 0.493519 0.326805 11.00000 -1.50000
H15B 2 0.809932 0.435757 0.313082 11.00000 -1.50000
H15C 2 0.939314 0.444717 0.287205 11.00000 -1.50000
AFIX 0
C16 1 1.083465 0.454950 0.421420 11.00000 0.01947 0.01898 =
0.02644 -0.00181 0.00180 -0.00070
AFIX 137
H16A 2 1.133593 0.443326 0.384848 11.00000 -1.50000
H16B 2 1.117489 0.440220 0.469256 11.00000 -1.50000
H16C 2 1.081920 0.495176 0.423698 11.00000 -1.50000
AFIX 0
C17 1 1.007917 0.332750 0.363198 11.00000 0.01243 0.01572 =
0.01314 -0.00274 0.00295 0.00333
C18 1 1.075953 0.339762 0.304087 11.00000 0.01635 0.01836 =
0.01663 0.00062 0.00406 0.00154
AFIX 43
H18 2 1.090756 0.375205 0.285838 11.00000 -1.20000
AFIX 0
C19 1 1.119862 0.292345 0.274187 11.00000 0.01783 0.03127 =
0.01674 0.00107 0.00713 0.00185
AFIX 43
H19 2 1.165349 0.295908 0.234872 11.00000 -1.20000
AFIX 0
C20 1 1.098263 0.238420 0.301124 11.00000 0.03745 0.02357 =
0.02394 -0.00429 0.01260 0.01089
AFIX 43
H20 2 1.128958 0.207073 0.279355 11.00000 -1.20000
AFIX 0
C21 1 1.031768 0.231841 0.359674 11.00000 0.03922 0.01428 =
0.02449 0.00248 0.01077 0.00552
AFIX 43
H21 2 1.017359 0.196366 0.377963 11.00000 -1.20000
AFIX 0
C22 1 0.986800 0.279670 0.390666 11.00000 0.01732 0.01696 =
0.01766 0.00130 0.00507 0.00419
C23 1 0.875556 0.244724 0.498041 11.00000 0.02530 0.01304 =
0.01591 0.00163 0.00913 0.00064
AFIX 13
H23 2 0.831983 0.264280 0.534058 11.00000 -1.20000
AFIX 0
C24 1 0.986607 0.215779 0.542115 11.00000 0.02647 0.01863 =
0.02414 0.00767 0.00918 -0.00062
AFIX 137
H24A 2 0.958806 0.188604 0.575076 11.00000 -1.50000
H24B 2 1.037570 0.243143 0.570697 11.00000 -1.50000
H24C 2 1.033587 0.197309 0.508410 11.00000 -1.50000
AFIX 0
C25 1 0.784048 0.204880 0.455054 11.00000 0.03419 0.01799 =
0.02651 0.00274 0.00945 -0.00319
AFIX 137
H25A 2 0.823248 0.185278 0.418562 11.00000 -1.50000
H25B 2 0.714758 0.225723 0.430539 11.00000 -1.50000
H25C 2 0.756043 0.178345 0.488771 11.00000 -1.50000
AFIX 0
N1 4 0.681387 0.423282 0.589398 11.00000 0.01670 0.01380 =
0.01419 -0.00283 0.00382 0.00052
N2 4 0.949995 0.371017 0.404999 11.00000 0.01216 0.00887 =
0.01170 0.00101 0.00178 -0.00029
N3 4 0.916803 0.287831 0.448680 11.00000 0.01661 0.01440 =
0.01287 0.00063 0.00623 -0.00051
PD1 5 0.798321 0.379766 0.527344 11.00000 0.01141 0.01290 =
0.01002 -0.00213 0.00115 0.00067
BR2 3 0.210826 0.096214 0.641751 11.00000 0.02458 0.03425 =
0.01507 -0.00479 0.00274 -0.00175
C26 1 0.006268 0.066902 0.478795 11.00000 0.02204 0.02361 =
0.01851 -0.00180 0.00033 0.00357
AFIX 43
H26 2 0.005597 0.068010 0.529991 11.00000 -1.20000
AFIX 0
C27 1 -0.099634 0.050756 0.433310 11.00000 0.02077 0.03362 =
0.02550 -0.00334 0.00453 0.00041
AFIX 43
H27 2 -0.169968 0.040329 0.453313 11.00000 -1.20000
AFIX 0
C28 1 -0.098855 0.050425 0.357039 11.00000 0.02134 0.03473 =
0.02450 -0.00286 -0.00978 -0.00041
AFIX 43
H28 2 -0.169418 0.039955 0.325079 11.00000 -1.20000
AFIX 0
C29 1 0.006136 0.065558 0.328668 11.00000 0.02753 0.02573 =
0.01649 -0.00170 -0.00259 0.00046
AFIX 43
H29 2 0.006841 0.065614 0.277454 11.00000 -1.20000
AFIX 0
C30 1 0.111614 0.080830 0.376922 11.00000 0.02384 0.01028 =
0.01516 0.00125 -0.00373 0.00462
C31 1 0.229124 0.097996 0.355018 11.00000 0.02256 0.01207 =
0.01294 0.00104 -0.00418 0.00474
C32 1 0.249576 0.098094 0.280514 11.00000 0.02826 0.01664 =
0.01759 0.00050 -0.00157 0.00541
AFIX 43
H32 2 0.186887 0.087111 0.243109 11.00000 -1.20000
AFIX 0
C33 1 0.362325 0.114428 0.262711 11.00000 0.03213 0.01729 =
0.01126 0.00321 0.00217 0.00414
AFIX 43
H33 2 0.374974 0.114387 0.213089 11.00000 -1.20000
AFIX 0
C34 1 0.457256 0.130911 0.317094 11.00000 0.02883 0.01187 =
0.01990 0.00550 0.00437 -0.00018
C35 1 0.436601 0.131214 0.391322 11.00000 0.02739 0.01581 =
0.01125 -0.00151 -0.00218 0.00161
AFIX 43
H35 2 0.500295 0.142143 0.428133 11.00000 -1.20000
AFIX 0
C36 1 0.324051 0.115717 0.411717 11.00000 0.02543 0.00742 =
0.01319 0.00088 0.00198 0.00414
C37 1 0.581672 0.148689 0.297345 11.00000 0.03960 0.02327 =
0.02096 0.00241 0.01099 -0.00628
AFIX 137
H37A 2 0.585414 0.139987 0.246037 11.00000 -1.50000
H37B 2 0.646210 0.128995 0.328421 11.00000 -1.50000
H37C 2 0.592177 0.188342 0.305071 11.00000 -1.50000
AFIX 0
C38 1 0.425022 0.148435 0.559761 11.00000 0.01701 0.02220 =
0.00551 -0.00242 0.00290 0.00560
C39 1 0.341998 0.245534 0.540804 11.00000 0.03911 0.03350 =
0.02546 0.00768 0.00378 0.02196
AFIX 13
H39 2 0.269287 0.221373 0.529033 11.00000 -1.20000
AFIX 0
C40 1 0.309516 0.280374 0.603246 11.00000 0.02066 0.03833 =
0.03603 -0.01331 0.00219 0.00344
AFIX 137
H40A 2 0.372911 0.307879 0.616784 11.00000 -1.50000
H40B 2 0.302562 0.256787 0.645346 11.00000 -1.50000
H40C 2 0.232117 0.298936 0.587895 11.00000 -1.50000
AFIX 0
C41 1 0.354170 0.269505 0.470616 11.00000 0.11549 0.05783 =
0.03064 0.00929 -0.00020 0.05652
AFIX 137
H41A 2 0.279651 0.289204 0.451703 11.00000 -1.50000
H41B 2 0.368605 0.240329 0.436411 11.00000 -1.50000
H41C 2 0.422491 0.295202 0.476248 11.00000 -1.50000
AFIX 0
C42 1 0.560080 0.216478 0.602776 11.00000 0.01947 0.01808 =
0.00732 0.00303 0.00363 0.00161
C43 1 0.620791 0.266332 0.623657 11.00000 0.03178 0.01569 =
0.01576 0.00320 0.00889 -0.00119
AFIX 43
H43 2 0.583912 0.300767 0.610608 11.00000 -1.20000
AFIX 0
C44 1 0.737193 0.263438 0.664247 11.00000 0.02834 0.02073 =
0.02288 -0.00583 0.01302 -0.01108
AFIX 43
H44 2 0.779277 0.296395 0.678983 11.00000 -1.20000
AFIX 0
C45 1 0.793198 0.211598 0.683684 11.00000 0.01799 0.03175 =
0.01903 0.00246 0.00426 -0.00725
AFIX 43
H45 2 0.870925 0.210685 0.712279 11.00000 -1.20000
AFIX 0
C46 1 0.734583 0.161672 0.660967 11.00000 0.01717 0.02004 =
0.01823 0.00230 0.00155 0.00394
AFIX 43
H46 2 0.772605 0.127268 0.672650 11.00000 -1.20000
AFIX 0
C47 1 0.617428 0.164758 0.620264 11.00000 0.01805 0.01518 =
0.00701 0.00376 0.00532 -0.00068
C48 1 0.548140 0.062316 0.594705 11.00000 0.01730 0.01292 =
0.02179 -0.00042 -0.00295 -0.00148
AFIX 13
H48 2 0.471413 0.045918 0.569080 11.00000 -1.20000
AFIX 0
C49 1 0.650765 0.044655 0.551911 11.00000 0.02994 0.01632 =
0.02744 0.00142 0.00511 0.00722
AFIX 137
H49A 2 0.728294 0.058601 0.576703 11.00000 -1.50000
H49B 2 0.635376 0.059705 0.502347 11.00000 -1.50000
H49C 2 0.653745 0.004454 0.549527 11.00000 -1.50000
AFIX 0
C50 1 0.564313 0.041018 0.674743 11.00000 0.02495 0.02386 =
0.02488 0.01027 0.00071 -0.00165
AFIX 137
H50A 2 0.563937 0.000745 0.674750 11.00000 -1.50000
H50B 2 0.497702 0.054589 0.699049 11.00000 -1.50000
H50C 2 0.641489 0.054306 0.700849 11.00000 -1.50000
AFIX 0
N4 4 0.110139 0.081068 0.452346 11.00000 0.01664 0.01272 =
0.01306 -0.00132 -0.00174 0.00288
N5 4 0.441944 0.204605 0.566438 11.00000 0.02435 0.01634 =
0.01344 -0.00054 -0.00280 0.01077
N6 4 0.532383 0.123847 0.592123 11.00000 0.01970 0.01179 =
0.01093 -0.00212 0.00220 0.00158
PD2 5 0.272464 0.111191 0.513665 11.00000 0.01698 0.01679 =
0.01099 -0.00265 -0.00172 0.00345
HKLF 4
REM 20170721a_a.res in P2(1)/c
REM R1 = 0.0414 for 6869 Fo > 4sig(Fo) and 0.0594 for all 8678 data
REM 551 parameters refined using 0 restraints
END
WGHT 0.0219 3.3678
REM Highest difference peak 0.858, deepest hole -0.852, 1-sigma level 0.117
Q1 1 0.2688 0.2472 0.4694 11.00000 0.05 0.86
Q2 1 0.2877 0.1379 0.4897 11.00000 0.05 0.79
Q3 1 0.2240 0.1261 0.6198 11.00000 0.05 0.78
Q4 1 1.0206 0.3505 0.5998 11.00000 0.05 0.74
Q5 1 1.0099 0.4205 0.5972 11.00000 0.05 0.70
Q6 1 0.7637 0.3419 0.5471 11.00000 0.05 0.66
Q7 1 0.8196 0.3449 0.5033 11.00000 0.05 0.64
Q8 1 0.7986 0.4110 0.5589 11.00000 0.05 0.64
Q9 1 0.8707 0.3410 0.5158 11.00000 0.05 0.60
Q10 1 0.2116 0.0647 0.6038 11.00000 0.05 0.57
Q11 1 0.3944 0.2784 0.5416 11.00000 0.05 0.57
Q12 1 0.9054 0.3908 0.5811 11.00000 0.05 0.56
Q13 1 0.2871 0.0808 0.4875 11.00000 0.05 0.55
Q14 1 0.7979 0.4053 0.4838 11.00000 0.05 0.51
Q15 1 0.9914 0.4198 0.6578 11.00000 0.05 0.50
Q16 1 1.1018 0.3793 0.3968 11.00000 0.05 0.47
Q17 1 0.9650 0.4233 0.6415 11.00000 0.05 0.46
;
_shelx_res_checksum 91265
_olex2_date_sample_data_collection 2017-07-21
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.727
#######################################################################
#
# 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_20170613-yxc-20
_database_code_depnum_ccdc_archive 'CCDC 1824539'
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_audit_creation_date 2017-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C32 H39 Br2 N5 Pd'
_chemical_formula_sum 'C32 H39 Br2 N5 Pd'
_chemical_formula_weight 759.90
_chemical_melting_point ?
_chemical_oxdiff_formula 'Pd C H N Br'
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'
Br Br -0.6763 1.2805 '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'
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 monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 32.3500(3)
_cell_length_b 8.65960(10)
_cell_length_c 25.0145(2)
_cell_angle_alpha 90
_cell_angle_beta 94.5210(10)
_cell_angle_gamma 90
_cell_volume 6985.71(12)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 22369
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 73.7080
_cell_measurement_theta_min 3.9060
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 7.165
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.55011
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.22a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light yellow'
_exptl_crystal_density_diffrn 1.445
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 3056
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0693
_diffrn_reflns_av_unetI/netI 0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max 40
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 41137
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.908
_diffrn_reflns_theta_min 3.545
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -22.00 89.00 0.50 1.00 -- 0.00 57.00 -30.00 222
2 \w -89.00 22.00 0.50 1.00 -- 0.00 -57.00 -60.00 222
3 \w -89.00 18.00 0.50 1.00 -- 0.00 -19.00-150.00 214
4 \w 32.00 107.00 0.50 6.00 -- 94.60 -30.00-120.00 150
5 \w 37.00 63.00 0.50 6.00 -- 94.60 -77.00-180.00 52
6 \w 47.00 80.00 0.50 6.00 -- 94.60 -30.00 150.00 66
7 \w 5.00 115.00 0.50 6.00 -- 94.60 -15.00 -30.00 220
8 \w 74.00 123.00 0.50 6.00 -- 94.60 -77.00-180.00 98
9 \w 83.00 109.00 0.50 6.00 -- 94.60 15.00 -90.00 52
10 \w 146.00 177.00 0.50 6.00 -- 94.60 15.00 -90.00 62
11 \w 28.00 117.00 0.50 6.00 -- 94.60 -61.00-180.00 178
12 \w 10.00 36.00 0.50 6.00 -- 94.60 -30.00 150.00 52
13 \w 8.00 118.00 0.50 6.00 -- 94.60 -15.00-150.00 220
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0352614000
_diffrn_orient_matrix_UB_12 -0.0393903000
_diffrn_orient_matrix_UB_13 0.0428674000
_diffrn_orient_matrix_UB_21 0.0280047000
_diffrn_orient_matrix_UB_22 -0.0455909000
_diffrn_orient_matrix_UB_23 -0.0444545000
_diffrn_orient_matrix_UB_31 0.0159271000
_diffrn_orient_matrix_UB_32 0.1673860000
_diffrn_orient_matrix_UB_33 -0.0020531000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 12112
_reflns_number_total 13750
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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 'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 2.375
_refine_diff_density_min -2.293
_refine_diff_density_rms 0.158
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 749
_refine_ls_number_reflns 13750
_refine_ls_number_restraints 169
_refine_ls_R_factor_all 0.0714
_refine_ls_R_factor_gt 0.0656
_refine_ls_restrained_S_all 1.076
_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^)+(0.0981P)^2^+28.8836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1747
_refine_ls_wR_factor_ref 0.1791
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C46') \\sim Ueq, Uanis(C47') \\sim Ueq, Uanis(C48') \\sim Ueq,
Uanis(C49') \\sim Ueq, Uanis(C50') \\sim Ueq, Uanis(C51') \\sim Ueq, Uanis(C52)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Same fragment restrains
{C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as
{C34, C35, C36, C37, C38}
4. Others
Fixed Sof: H45A(0.5) H45B(0.5) H45C(0.5) H45D(0.5) C46(0.5) C47(0.5) H47(0.5)
C48(0.5) H48(0.5) C49(0.5) H49(0.5) C50(0.5) H50(0.5) C51(0.5) H51(0.5)
C46'(0.5) C47'(0.5) H47'(0.5) C48'(0.5) H48'(0.5) C49'(0.5) H49'(0.5)
C50'(0.5) H50'(0.5) C51'(0.5) H51'(0.5)
5.a Ternary CH refined with riding coordinates:
C21(H21), C30(H30), C53(H53), C62(H62)
5.b Secondary CH2 refined with riding coordinates:
C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C13(H13A,H13B), C35(H35A,H35B),
C36(H36A,H36B), C37(H37A,H37B), C45(H45A,H45B), C45(H45C,H45D)
5.c Aromatic/amide H refined with riding coordinates:
C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
C18(H18), C19(H19), C25(H25), C26(H26), C27(H27), C28(H28), C40(H40), C41(H41),
C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50),
C51(H51), C47'(H47'), C48'(H48'), C49'(H49'), C50'(H50'), C51'(H51'), C57(H57),
C58(H58), C59(H59), C60(H60)
5.d Fitted hexagon refined as free rotating group:
C39(C40,C41,C42,C43,C44), C46(C47,C48,C49,C50,C51), C46'(C47',C48',C49',C50',
C51')
5.e Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,
H31C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C54(H54A,H54B,H54C), C55(H55A,
H55B,H55C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C)
;
_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
Br1 Br 0.36853(2) -0.10596(7) 0.55032(2) 0.02646(14) Uani 1 1 d . . . . .
Br2 Br 0.42113(2) 0.19983(8) 0.70543(2) 0.03007(15) Uani 1 1 d . . . . .
C1 C 0.42681(15) 0.1948(6) 0.57866(18) 0.0219(10) Uani 1 1 d . . . . .
C2 C 0.40693(15) 0.3171(7) 0.55209(18) 0.0248(11) Uani 1 1 d D . . . .
C3 C 0.36139(15) 0.3552(8) 0.54653(19) 0.0287(12) Uani 1 1 d D . . . .
H3A H 0.3559 0.4192 0.5149 0.034 Uiso 1 1 calc R . . . .
H3B H 0.3460 0.2599 0.5405 0.034 Uiso 1 1 calc R . . . .
C4 C 0.34523(15) 0.4363(7) 0.5932(2) 0.0250(11) Uani 1 1 d D . . . .
H4A H 0.3562 0.5406 0.5953 0.030 Uiso 1 1 calc R . . . .
H4B H 0.3546 0.3829 0.6260 0.030 Uiso 1 1 calc R . . . .
C5 C 0.29718(16) 0.4423(8) 0.5880(2) 0.0314(12) Uani 1 1 d D . . . .
H5A H 0.2880 0.4869 0.5535 0.038 Uiso 1 1 calc R . . . .
H5B H 0.2865 0.3377 0.5887 0.038 Uiso 1 1 calc R . . . .
C6 C 0.2791(2) 0.5334(9) 0.6311(2) 0.0443(16) Uani 1 1 d D . . . .
H6A H 0.2494 0.5301 0.6259 0.066 Uiso 1 1 calc GR . . . .
H6B H 0.2883 0.6386 0.6295 0.066 Uiso 1 1 calc GR . . . .
H6C H 0.2880 0.4902 0.6654 0.066 Uiso 1 1 calc GR . . . .
C7 C 0.50313(16) 0.1213(6) 0.58290(19) 0.0235(10) Uani 1 1 d . . . . .
C8 C 0.50882(17) 0.0636(7) 0.63468(19) 0.0293(12) Uani 1 1 d . . . . .
H8 H 0.4892 0.0821 0.6592 0.035 Uiso 1 1 calc R . . . .
C9 C 0.54379(18) -0.0211(8) 0.6493(2) 0.0333(13) Uani 1 1 d . . . . .
H9 H 0.5482 -0.0578 0.6842 0.040 Uiso 1 1 calc R . . . .
C10 C 0.57271(18) -0.0530(8) 0.6125(2) 0.0334(13) Uani 1 1 d . . . . .
H10 H 0.5961 -0.1119 0.6226 0.040 Uiso 1 1 calc R . . . .
C11 C 0.56639(17) 0.0036(7) 0.5612(2) 0.0297(12) Uani 1 1 d . . . . .
H11 H 0.5859 -0.0154 0.5367 0.036 Uiso 1 1 calc R . . . .
C12 C 0.53105(17) 0.0891(7) 0.5457(2) 0.0267(11) Uani 1 1 d . . . . .
H12 H 0.5264 0.1240 0.5105 0.032 Uiso 1 1 calc R . . . .
C13 C 0.43287(16) 0.5470(6) 0.50032(19) 0.0232(10) Uani 1 1 d . . . . .
H13A H 0.4595 0.5992 0.5045 0.028 Uiso 1 1 calc R . . . .
H13B H 0.4129 0.6112 0.5169 0.028 Uiso 1 1 calc R . . . .
C14 C 0.41979(15) 0.5336(6) 0.44102(18) 0.0218(10) Uani 1 1 d . . . . .
C15 C 0.44042(17) 0.4376(7) 0.4085(2) 0.0296(12) Uani 1 1 d . . . . .
H15 H 0.4616 0.3744 0.4231 0.036 Uiso 1 1 calc R . . . .
C16 C 0.42936(18) 0.4353(7) 0.3534(2) 0.0308(12) Uani 1 1 d . . . . .
H16 H 0.4433 0.3704 0.3313 0.037 Uiso 1 1 calc R . . . .
C17 C 0.39802(18) 0.5280(7) 0.3316(2) 0.0295(12) Uani 1 1 d . . . . .
H17 H 0.3907 0.5255 0.2949 0.035 Uiso 1 1 calc R . . . .
C18 C 0.37736(18) 0.6248(7) 0.3641(2) 0.0312(12) Uani 1 1 d . . . . .
H18 H 0.3561 0.6873 0.3493 0.037 Uiso 1 1 calc R . . . .
C19 C 0.38825(17) 0.6295(7) 0.4191(2) 0.0293(12) Uani 1 1 d . . . . .
H19 H 0.3746 0.6960 0.4410 0.035 Uiso 1 1 calc R . . . .
C20 C 0.37378(15) -0.1131(6) 0.67603(17) 0.0198(10) Uani 1 1 d . . . . .
C21 C 0.4312(2) -0.3100(11) 0.6954(3) 0.055(2) Uani 1 1 d . . . . .
H21 H 0.4280 -0.4162 0.7080 0.066 Uiso 1 1 calc R . . . .
C22 C 0.46089(17) -0.2411(8) 0.7380(2) 0.0333(13) Uani 1 1 d . . . . .
H22A H 0.4873 -0.2919 0.7378 0.050 Uiso 1 1 calc GR . . . .
H22B H 0.4502 -0.2543 0.7725 0.050 Uiso 1 1 calc GR . . . .
H22C H 0.4642 -0.1330 0.7311 0.050 Uiso 1 1 calc GR . . . .
C23 C 0.44460(19) -0.3309(13) 0.6430(3) 0.063(3) Uani 1 1 d . . . . .
H23A H 0.4514 -0.2324 0.6284 0.095 Uiso 1 1 calc GR . . . .
H23B H 0.4228 -0.3779 0.6203 0.095 Uiso 1 1 calc GR . . . .
H23C H 0.4686 -0.3964 0.6449 0.095 Uiso 1 1 calc GR . . . .
C24 C 0.36023(18) -0.3094(7) 0.73027(19) 0.0272(11) Uani 1 1 d . . . . .
C25 C 0.3597(2) -0.4434(7) 0.7612(2) 0.0371(14) Uani 1 1 d . . . . .
H25 H 0.3818 -0.5124 0.7631 0.045 Uiso 1 1 calc R . . . .
C26 C 0.3246(2) -0.4698(8) 0.7892(2) 0.0424(17) Uani 1 1 d . . . . .
H26 H 0.3233 -0.5588 0.8098 0.051 Uiso 1 1 calc R . . . .
C27 C 0.2919(2) -0.3677(8) 0.7870(2) 0.0381(15) Uani 1 1 d . . . . .
H27 H 0.2693 -0.3878 0.8069 0.046 Uiso 1 1 calc R . . . .
C28 C 0.29182(19) -0.2381(8) 0.7564(2) 0.0323(13) Uani 1 1 d . . . . .
H28 H 0.2694 -0.1706 0.7546 0.039 Uiso 1 1 calc R . . . .
C29 C 0.32637(16) -0.2083(6) 0.72740(18) 0.0236(10) Uani 1 1 d . . . . .
C30 C 0.30997(17) 0.0449(7) 0.6776(2) 0.0280(11) Uani 1 1 d . . . . .
H30 H 0.3252 0.1069 0.6529 0.034 Uiso 1 1 calc R . . . .
C31 C 0.26985(18) -0.0038(8) 0.6474(3) 0.0389(14) Uani 1 1 d . . . . .
H31A H 0.2534 -0.0608 0.6709 0.058 Uiso 1 1 calc GR . . . .
H31B H 0.2758 -0.0676 0.6176 0.058 Uiso 1 1 calc GR . . . .
H31C H 0.2548 0.0862 0.6346 0.058 Uiso 1 1 calc GR . . . .
C32 C 0.3039(2) 0.1448(9) 0.7259(3) 0.0431(15) Uani 1 1 d . . . . .
H32A H 0.2881 0.2346 0.7148 0.065 Uiso 1 1 calc GR . . . .
H32B H 0.3304 0.1759 0.7423 0.065 Uiso 1 1 calc GR . . . .
H32C H 0.2893 0.0872 0.7513 0.065 Uiso 1 1 calc GR . . . .
N1 N 0.46735(13) 0.2151(6) 0.56772(15) 0.0233(9) Uani 1 1 d . . . . .
N2 N 0.47380(13) 0.3392(6) 0.53793(15) 0.0235(9) Uani 1 1 d . . . . .
N3 N 0.43644(12) 0.4001(6) 0.52913(15) 0.0224(9) Uani 1 1 d . . . . .
N4 N 0.38899(14) -0.2447(6) 0.69774(16) 0.0265(10) Uani 1 1 d . . . . .
N5 N 0.33614(12) -0.0899(5) 0.69328(15) 0.0210(8) Uani 1 1 d . . . . .
Pd1 Pd 0.40106(2) 0.03698(5) 0.62693(2) 0.02293(12) Uani 1 1 d . . . . .
Br3 Br 0.18641(2) 0.85891(10) 0.79880(3) 0.04635(19) Uani 1 1 d . . . . .
Br4 Br 0.12438(2) 0.58518(10) 0.94315(4) 0.0539(2) Uani 1 1 d . . . . .
C33 C 0.11035(19) 0.8890(9) 0.8711(3) 0.0442(16) Uani 1 1 d . . . . .
C34 C 0.1082(2) 1.0240(9) 0.8986(3) 0.0493(17) Uani 1 1 d D U . . .
C35 C 0.1445(5) 1.1089(17) 0.9293(6) 0.121(5) Uani 1 1 d D U . . .
H35A H 0.1689 1.1033 0.9092 0.145 Uiso 1 1 calc R . . . .
H35B H 0.1374 1.2168 0.9334 0.145 Uiso 1 1 calc R . . . .
C36 C 0.1530(5) 1.041(2) 0.9803(6) 0.137(6) Uani 1 1 d D U . . .
H36A H 0.1533 0.9288 0.9777 0.165 Uiso 1 1 calc R . . . .
H36B H 0.1326 1.0713 1.0047 0.165 Uiso 1 1 calc R . . . .
C37 C 0.1998(3) 1.1096(14) 0.9999(5) 0.091(3) Uani 1 1 d D U . . .
H37A H 0.2161 1.0336 1.0208 0.109 Uiso 1 1 calc R . . . .
H37B H 0.2147 1.1395 0.9694 0.109 Uiso 1 1 calc R . . . .
C38 C 0.1913(4) 1.2408(15) 1.0319(6) 0.120(5) Uani 1 1 d D U . . .
H38A H 0.1866 1.3295 1.0092 0.180 Uiso 1 1 calc GR . . . .
H38B H 0.2146 1.2600 1.0573 0.180 Uiso 1 1 calc GR . . . .
H38C H 0.1671 1.2211 1.0507 0.180 Uiso 1 1 calc GR . . . .
C39 C 0.0540(3) 0.7512(12) 0.8177(4) 0.119(5) Uani 1 1 d . U . . .
C40 C 0.0731(3) 0.7032(13) 0.7726(5) 0.122(5) Uani 1 1 d G U . . .
H40 H 0.0964 0.7549 0.7624 0.146 Uiso 1 1 calc R . . . .
C41 C 0.0572(4) 0.5780(14) 0.7429(4) 0.124(5) Uani 1 1 d G U . . .
H41 H 0.0699 0.5458 0.7127 0.149 Uiso 1 1 calc R . . . .
C42 C 0.0224(4) 0.5007(12) 0.7582(5) 0.160(7) Uani 1 1 d G U . . .
H42 H 0.0118 0.4169 0.7383 0.191 Uiso 1 1 calc R . . . .
C43 C 0.0034(4) 0.5488(15) 0.8033(6) 0.174(8) Uani 1 1 d G U . . .
H43 H -0.0199 0.4971 0.8136 0.208 Uiso 1 1 calc R . . . .
C44 C 0.0192(4) 0.6740(16) 0.8331(4) 0.156(7) Uani 1 1 d G U . . .
H44 H 0.0065 0.7061 0.8632 0.187 Uiso 1 1 calc R . . . .
C45 C 0.0559(3) 1.2455(10) 0.8965(4) 0.062(2) Uani 1 1 d . U . . .
H45A H 0.0382 1.2821 0.8660 0.075 Uiso 0.5 1 calc R . P A 1
H45B H 0.0787 1.3178 0.9023 0.075 Uiso 0.5 1 calc R . P A 1
H45C H 0.0774 1.3059 0.9159 0.075 Uiso 0.5 1 calc R . P B 2
H45D H 0.0471 1.3004 0.8638 0.075 Uiso 0.5 1 calc R . P B 2
C46 C 0.0299(4) 1.2478(19) 0.9479(7) 0.062(6) Uani 0.5 1 d . U P C 1
C47 C -0.0121(4) 1.2146(18) 0.9384(5) 0.075(5) Uani 0.5 1 d G U P C 1
H47 H -0.0229 1.1880 0.9041 0.090 Uiso 0.5 1 calc R . P C 1
C48 C -0.0379(4) 1.221(2) 0.9802(7) 0.086(7) Uani 0.5 1 d G U P C 1
H48 H -0.0660 1.1991 0.9739 0.104 Uiso 0.5 1 calc R . P C 1
C49 C -0.0218(6) 1.261(3) 1.0315(6) 0.128(11) Uani 0.5 1 d G U P C 1
H49 H -0.0390 1.2656 1.0595 0.153 Uiso 0.5 1 calc R . P C 1
C50 C 0.0202(7) 1.294(3) 1.0410(6) 0.163(15) Uani 0.5 1 d G U P C 1
H50 H 0.0310 1.3210 1.0753 0.196 Uiso 0.5 1 calc R . P C 1
C51 C 0.0460(4) 1.288(2) 0.9992(8) 0.123(10) Uani 0.5 1 d G U P C 1
H51 H 0.0741 1.3099 1.0056 0.148 Uiso 0.5 1 calc R . P C 1
C46' C 0.0212(4) 1.230(2) 0.9289(6) 0.053(4) Uani 0.5 1 d . U P C 2
C47' C -0.0025(6) 1.0964(18) 0.9307(7) 0.119(9) Uani 0.5 1 d G U P C 2
H47' H 0.0015 1.0157 0.9071 0.142 Uiso 0.5 1 calc R . P C 2
C48' C -0.0322(6) 1.0834(19) 0.9678(8) 0.124(10) Uani 0.5 1 d G U P C 2
H48' H -0.0480 0.9941 0.9690 0.149 Uiso 0.5 1 calc R . P C 2
C49' C -0.0381(5) 1.204(2) 1.0030(6) 0.075(6) Uani 0.5 1 d G U P C 2
H49' H -0.0580 1.1954 1.0278 0.090 Uiso 0.5 1 calc R . P C 2
C50' C -0.0145(6) 1.338(2) 1.0012(7) 0.148(13) Uani 0.5 1 d G U P C 2
H50' H -0.0185 1.4184 1.0247 0.178 Uiso 0.5 1 calc R . P C 2
C51' C 0.0152(5) 1.3506(17) 0.9641(8) 0.112(9) Uani 0.5 1 d G U P C 2
H51' H 0.0310 1.4400 0.9629 0.134 Uiso 0.5 1 calc R . P C 2
C52 C 0.20025(17) 0.5663(8) 0.8747(2) 0.0334(13) Uani 1 1 d . U . . .
C53 C 0.1731(2) 0.4082(13) 0.7970(3) 0.067(3) Uani 1 1 d . . . . .
H53 H 0.1571 0.5040 0.7931 0.081 Uiso 1 1 calc R . . . .
C54 C 0.1953(2) 0.4011(11) 0.7462(3) 0.0535(19) Uani 1 1 d . . . . .
H54A H 0.2159 0.3213 0.7494 0.080 Uiso 1 1 calc GR . . . .
H54B H 0.2083 0.4986 0.7405 0.080 Uiso 1 1 calc GR . . . .
H54C H 0.1756 0.3788 0.7164 0.080 Uiso 1 1 calc GR . . . .
C55 C 0.1423(3) 0.2930(18) 0.8049(4) 0.099(5) Uani 1 1 d . . . . .
H55A H 0.1236 0.2855 0.7732 0.149 Uiso 1 1 calc GR . . . .
H55B H 0.1270 0.3214 0.8348 0.149 Uiso 1 1 calc GR . . . .
H55C H 0.1555 0.1951 0.8119 0.149 Uiso 1 1 calc GR . . . .
C56 C 0.23780(19) 0.3540(8) 0.8624(2) 0.0360(13) Uani 1 1 d . . . . .
C57 C 0.2527(2) 0.2121(8) 0.8456(3) 0.0477(18) Uani 1 1 d . . . . .
H57 H 0.2380 0.1546 0.8190 0.057 Uiso 1 1 calc R . . . .
C58 C 0.2892(3) 0.1611(9) 0.8693(3) 0.056(2) Uani 1 1 d . . . . .
H58 H 0.3001 0.0678 0.8585 0.067 Uiso 1 1 calc R . . . .
C59 C 0.3110(3) 0.2465(10) 0.9100(3) 0.057(2) Uani 1 1 d . . . . .
H59 H 0.3362 0.2091 0.9251 0.069 Uiso 1 1 calc R . . . .
C60 C 0.2958(2) 0.3875(9) 0.9288(2) 0.0457(17) Uani 1 1 d . . . . .
H60 H 0.3100 0.4435 0.9561 0.055 Uiso 1 1 calc R . . . .
C61 C 0.25810(18) 0.4378(7) 0.9040(2) 0.0335(13) Uani 1 1 d . . . . .
C62 C 0.24230(19) 0.6960(8) 0.9485(2) 0.0339(13) Uani 1 1 d . . . . .
H62 H 0.2194 0.7697 0.9425 0.041 Uiso 1 1 calc R . . . .
C63 C 0.2817(2) 0.7799(9) 0.9363(3) 0.0460(16) Uani 1 1 d . . . . .
H63A H 0.2856 0.8683 0.9592 0.069 Uiso 1 1 calc GR . . . .
H63B H 0.2794 0.8128 0.8995 0.069 Uiso 1 1 calc GR . . . .
H63C H 0.3049 0.7116 0.9423 0.069 Uiso 1 1 calc GR . . . .
C64 C 0.2425(2) 0.6416(10) 1.0068(2) 0.0462(17) Uani 1 1 d . . . . .
H64A H 0.2651 0.5711 1.0145 0.069 Uiso 1 1 calc GR . . . .
H64B H 0.2168 0.5906 1.0120 0.069 Uiso 1 1 calc GR . . . .
H64C H 0.2458 0.7290 1.0303 0.069 Uiso 1 1 calc GR . . . .
N6 N 0.0742(2) 0.8906(10) 0.8416(3) 0.076(2) Uani 1 1 d . U . . .
N7 N 0.0508(3) 1.0124(12) 0.8482(4) 0.095(3) Uani 1 1 d . U . . .
N8 N 0.07263(17) 1.0959(8) 0.8830(3) 0.0505(15) Uani 1 1 d . . . . .
N9 N 0.20247(15) 0.4381(7) 0.8446(2) 0.0369(12) Uani 1 1 d . . . . .
N10 N 0.23396(14) 0.5681(6) 0.91064(17) 0.0276(10) Uani 1 1 d . . . . .
Pd2 Pd 0.15499(2) 0.72534(6) 0.87151(2) 0.03512(13) 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
Br1 0.0343(3) 0.0318(3) 0.0139(2) -0.0008(2) 0.00651(19) -0.0018(2)
Br2 0.0286(3) 0.0483(4) 0.0136(2) -0.0015(2) 0.00381(19) -0.0070(2)
C1 0.021(2) 0.032(3) 0.0127(19) -0.0008(19) 0.0021(16) -0.007(2)
C2 0.024(2) 0.039(3) 0.0118(19) 0.003(2) 0.0046(17) -0.005(2)
C3 0.020(2) 0.048(4) 0.019(2) 0.002(2) 0.0059(18) -0.006(2)
C4 0.024(2) 0.030(3) 0.021(2) 0.000(2) 0.0038(18) -0.004(2)
C5 0.024(2) 0.042(4) 0.028(3) -0.003(2) 0.001(2) -0.001(2)
C6 0.037(3) 0.062(5) 0.034(3) -0.010(3) 0.003(2) 0.016(3)
C7 0.025(2) 0.029(3) 0.017(2) 0.001(2) 0.0033(18) -0.004(2)
C8 0.029(3) 0.046(4) 0.014(2) 0.004(2) 0.0075(19) 0.003(2)
C9 0.035(3) 0.042(4) 0.023(2) 0.005(2) 0.004(2) 0.006(3)
C10 0.032(3) 0.038(3) 0.030(3) 0.000(2) 0.003(2) 0.003(2)
C11 0.031(3) 0.030(3) 0.029(3) -0.002(2) 0.016(2) -0.002(2)
C12 0.032(3) 0.032(3) 0.018(2) 0.004(2) 0.0105(19) -0.004(2)
C13 0.024(2) 0.029(3) 0.017(2) 0.000(2) 0.0078(18) -0.002(2)
C14 0.024(2) 0.027(3) 0.015(2) 0.0018(19) 0.0062(17) -0.002(2)
C15 0.031(3) 0.042(3) 0.016(2) 0.001(2) 0.0022(19) 0.009(2)
C16 0.039(3) 0.040(3) 0.014(2) -0.002(2) 0.005(2) 0.003(3)
C17 0.037(3) 0.037(3) 0.014(2) 0.004(2) 0.003(2) -0.001(2)
C18 0.034(3) 0.037(3) 0.022(2) 0.004(2) 0.001(2) 0.008(2)
C19 0.030(3) 0.041(3) 0.017(2) -0.001(2) 0.0044(19) 0.005(2)
C20 0.023(2) 0.026(3) 0.0110(19) 0.0031(18) 0.0050(16) 0.0014(19)
C21 0.031(3) 0.096(7) 0.036(3) -0.023(4) -0.005(3) 0.032(4)
C22 0.027(3) 0.049(4) 0.024(2) 0.004(2) -0.001(2) 0.004(2)
C23 0.022(3) 0.123(8) 0.044(4) -0.042(4) 0.001(3) 0.011(4)
C24 0.038(3) 0.030(3) 0.013(2) -0.001(2) 0.0030(19) -0.004(2)
C25 0.060(4) 0.030(3) 0.019(2) -0.001(2) -0.011(2) 0.004(3)
C26 0.071(4) 0.039(4) 0.017(2) 0.004(2) 0.002(3) -0.030(3)
C27 0.045(3) 0.048(4) 0.022(2) 0.002(3) 0.005(2) -0.021(3)
C28 0.038(3) 0.043(4) 0.017(2) 0.000(2) 0.009(2) -0.017(3)
C29 0.027(2) 0.030(3) 0.014(2) -0.0029(19) 0.0041(18) -0.007(2)
C30 0.028(3) 0.028(3) 0.029(3) 0.003(2) 0.010(2) 0.005(2)
C31 0.030(3) 0.043(4) 0.043(3) 0.007(3) 0.000(2) 0.004(3)
C32 0.041(3) 0.043(4) 0.047(4) -0.010(3) 0.012(3) 0.009(3)
N1 0.022(2) 0.035(3) 0.0132(17) 0.0009(17) 0.0066(15) -0.0005(18)
N2 0.0219(19) 0.035(3) 0.0142(17) 0.0002(17) 0.0048(15) -0.0020(18)
N3 0.0196(18) 0.035(3) 0.0133(17) -0.0018(17) 0.0065(14) -0.0032(18)
N4 0.028(2) 0.038(3) 0.0139(18) -0.0042(18) 0.0073(16) 0.006(2)
N5 0.0205(19) 0.028(2) 0.0157(17) 0.0005(16) 0.0090(14) 0.0002(17)
Pd1 0.02123(18) 0.0381(2) 0.01020(17) 0.00310(14) 0.00560(12) -0.00512(15)
Br3 0.0413(3) 0.0629(5) 0.0359(3) -0.0022(3) 0.0102(3) 0.0102(3)
Br4 0.0393(4) 0.0535(5) 0.0725(5) 0.0039(4) 0.0269(3) 0.0047(3)
C33 0.026(3) 0.064(5) 0.043(3) -0.007(3) 0.008(2) 0.000(3)
C34 0.032(3) 0.051(4) 0.065(4) -0.018(3) 0.006(3) 0.009(3)
C35 0.139(9) 0.106(8) 0.117(8) -0.017(7) 0.004(7) 0.040(7)
C36 0.162(10) 0.124(9) 0.131(9) 0.004(7) 0.045(8) -0.013(8)
C37 0.078(6) 0.102(7) 0.086(6) -0.024(5) -0.025(5) 0.018(5)
C38 0.105(9) 0.098(9) 0.144(10) -0.041(8) -0.066(8) 0.028(7)
C39 0.091(7) 0.131(9) 0.125(8) -0.002(7) -0.042(6) -0.001(7)
C40 0.091(7) 0.144(9) 0.125(8) -0.024(7) -0.032(6) -0.002(7)
C41 0.107(8) 0.118(8) 0.146(9) -0.036(7) 0.003(7) -0.005(7)
C42 0.170(11) 0.153(10) 0.153(10) -0.006(8) -0.003(8) 0.002(9)
C43 0.172(11) 0.163(11) 0.182(11) -0.003(9) -0.009(9) -0.013(9)
C44 0.146(10) 0.144(10) 0.174(10) -0.007(8) -0.015(8) -0.017(8)
C45 0.045(4) 0.055(5) 0.090(5) -0.005(4) 0.025(4) 0.006(3)
C46 0.054(8) 0.064(9) 0.071(9) -0.002(7) 0.025(7) 0.011(7)
C47 0.061(8) 0.069(9) 0.099(9) -0.014(7) 0.032(7) -0.009(7)
C48 0.079(9) 0.088(11) 0.097(10) -0.002(8) 0.042(8) 0.001(8)
C49 0.121(13) 0.137(14) 0.127(13) 0.001(9) 0.026(9) 0.002(9)
C50 0.164(17) 0.172(17) 0.154(17) 0.002(10) 0.018(10) 0.011(10)
C51 0.111(12) 0.134(13) 0.126(13) 0.006(9) 0.024(9) 0.016(9)
C46' 0.040(7) 0.057(8) 0.064(8) -0.012(7) 0.011(6) 0.008(6)
C47' 0.114(12) 0.117(12) 0.127(12) -0.004(9) 0.026(9) -0.004(9)
C48' 0.121(12) 0.128(13) 0.125(13) -0.003(9) 0.027(9) -0.001(9)
C49' 0.073(9) 0.079(10) 0.076(9) -0.014(8) 0.021(7) 0.009(7)
C50' 0.142(15) 0.150(16) 0.154(15) -0.006(10) 0.025(10) 0.004(10)
C51' 0.107(11) 0.118(12) 0.112(11) -0.011(9) 0.017(9) -0.002(9)
C52 0.028(3) 0.046(4) 0.028(3) -0.010(2) 0.010(2) -0.005(2)
C53 0.040(4) 0.114(8) 0.050(4) -0.042(5) 0.015(3) -0.033(4)
C54 0.042(4) 0.075(6) 0.044(4) -0.016(4) 0.007(3) -0.006(4)
C55 0.053(5) 0.184(14) 0.059(5) 0.013(7) -0.003(4) -0.047(7)
C56 0.037(3) 0.034(3) 0.041(3) -0.001(3) 0.025(3) -0.006(3)
C57 0.062(4) 0.032(4) 0.055(4) 0.006(3) 0.041(4) -0.002(3)
C58 0.086(6) 0.041(4) 0.045(4) 0.011(3) 0.037(4) 0.010(4)
C59 0.060(4) 0.066(5) 0.051(4) 0.042(4) 0.034(4) 0.031(4)
C60 0.044(3) 0.066(5) 0.029(3) 0.024(3) 0.014(3) 0.013(3)
C61 0.035(3) 0.038(3) 0.031(3) 0.014(2) 0.019(2) 0.005(3)
C62 0.036(3) 0.041(4) 0.026(3) -0.005(2) 0.004(2) -0.005(3)
C63 0.052(4) 0.049(4) 0.038(3) -0.007(3) 0.009(3) -0.019(3)
C64 0.051(4) 0.065(5) 0.024(3) 0.000(3) 0.010(3) -0.009(3)
N6 0.049(3) 0.073(5) 0.099(5) -0.029(4) -0.039(3) 0.024(3)
N7 0.072(5) 0.091(6) 0.115(6) -0.026(5) -0.044(4) 0.033(4)
N8 0.027(2) 0.056(4) 0.070(4) -0.003(3) 0.013(3) 0.002(3)
N9 0.027(2) 0.046(3) 0.039(3) -0.010(2) 0.012(2) -0.003(2)
N10 0.028(2) 0.034(3) 0.022(2) -0.0007(19) 0.0065(17) -0.0018(19)
Pd2 0.0240(2) 0.0479(3) 0.0339(2) -0.01157(19) 0.00479(16) 0.00310(18)
_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
Br1 Pd1 2.4483(6) . ?
Br2 Pd1 2.4627(6) . ?
C1 C2 1.382(8) . ?
C1 N1 1.372(6) . ?
C1 Pd1 2.044(5) . ?
C2 C3 1.505(7) . ?
C2 N3 1.358(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.492(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.550(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.490(8) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.387(7) . ?
C7 C12 1.376(7) . ?
C7 N1 1.440(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.373(8) . ?
C9 H9 0.9300 . ?
C9 C10 1.389(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.374(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.392(8) . ?
C12 H12 0.9300 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.515(6) . ?
C13 N3 1.462(7) . ?
C14 C15 1.372(7) . ?
C14 C19 1.393(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.397(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.372(8) . ?
C17 H17 0.9300 . ?
C17 C18 1.377(8) . ?
C18 H18 0.9300 . ?
C18 C19 1.394(7) . ?
C19 H19 0.9300 . ?
C20 N4 1.339(7) . ?
C20 N5 1.339(6) . ?
C20 Pd1 2.037(5) . ?
C21 H21 0.9800 . ?
C21 C22 1.502(9) . ?
C21 C23 1.425(9) . ?
C21 N4 1.483(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.395(8) . ?
C24 C29 1.400(8) . ?
C24 N4 1.400(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.399(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.377(11) . ?
C27 H27 0.9300 . ?
C27 C28 1.359(9) . ?
C28 H28 0.9300 . ?
C28 C29 1.403(7) . ?
C29 N5 1.387(7) . ?
C30 H30 0.9800 . ?
C30 C31 1.509(8) . ?
C30 C32 1.512(8) . ?
C30 N5 1.476(7) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
N1 N2 1.333(6) . ?
N2 N3 1.321(6) . ?
Br3 Pd2 2.4434(8) . ?
Br4 Pd2 2.4382(9) . ?
C33 C34 1.360(10) . ?
C33 N6 1.333(8) . ?
C33 Pd2 2.023(7) . ?
C34 C35 1.537(13) . ?
C34 N8 1.340(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.413(15) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.667(15) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.429(13) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C39 N6 1.475(11) . ?
C40 H40 0.9300 . ?
C40 C41 1.3900 . ?
C41 H41 0.9300 . ?
C41 C42 1.3900 . ?
C42 H42 0.9300 . ?
C42 C43 1.3900 . ?
C43 H43 0.9300 . ?
C43 C44 1.3900 . ?
C44 H44 0.9300 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 H45C 0.9700 . ?
C45 H45D 0.9700 . ?
C45 C46 1.591(15) . ?
C45 C46' 1.441(14) . ?
C45 N8 1.454(10) . ?
C46 C47 1.3900 . ?
C46 C51 1.3900 . ?
C47 H47 0.9300 . ?
C47 C48 1.3900 . ?
C48 H48 0.9300 . ?
C48 C49 1.3900 . ?
C49 H49 0.9300 . ?
C49 C50 1.3900 . ?
C50 H50 0.9300 . ?
C50 C51 1.3900 . ?
C51 H51 0.9300 . ?
C46' C47' 1.3900 . ?
C46' C51' 1.3900 . ?
C47' H47' 0.9300 . ?
C47' C48' 1.3900 . ?
C48' H48' 0.9300 . ?
C48' C49' 1.3900 . ?
C49' H49' 0.9300 . ?
C49' C50' 1.3900 . ?
C50' H50' 0.9300 . ?
C50' C51' 1.3900 . ?
C51' H51' 0.9300 . ?
C52 N9 1.348(8) . ?
C52 N10 1.357(7) . ?
C52 Pd2 2.007(6) . ?
C53 H53 0.9800 . ?
C53 C54 1.509(10) . ?
C53 C55 1.435(13) . ?
C53 N9 1.484(9) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 C57 1.396(9) . ?
C56 C61 1.391(9) . ?
C56 N9 1.398(8) . ?
C57 H57 0.9300 . ?
C57 C58 1.355(12) . ?
C58 H58 0.9300 . ?
C58 C59 1.403(13) . ?
C59 H59 0.9300 . ?
C59 C60 1.411(11) . ?
C60 H60 0.9300 . ?
C60 C61 1.393(9) . ?
C61 N10 1.390(8) . ?
C62 H62 0.9800 . ?
C62 C63 1.518(9) . ?
C62 C64 1.530(8) . ?
C62 N10 1.469(7) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
N6 N7 1.315(11) . ?
N7 N8 1.297(11) . ?
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
C2 C1 Pd1 126.9(4) . . ?
N1 C1 C2 102.8(4) . . ?
N1 C1 Pd1 130.1(4) . . ?
C1 C2 C3 128.8(5) . . ?
N3 C2 C1 107.0(4) . . ?
N3 C2 C3 124.1(5) . . ?
C2 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.4 . . ?
C4 C3 C2 115.6(4) . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
C3 C4 C5 111.2(4) . . ?
H4A C4 H4B 108.0 . . ?
C5 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 C4 113.9(5) . . ?
C6 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N1 119.6(4) . . ?
C12 C7 C8 120.9(5) . . ?
C12 C7 N1 119.5(4) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 119.1(5) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 120.9(5) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.2(6) . . ?
C11 C10 H10 120.4 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.6(5) . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C11 119.1(5) . . ?
C7 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
N3 C13 H13A 108.5 . . ?
N3 C13 H13B 108.5 . . ?
N3 C13 C14 114.9(4) . . ?
C15 C14 C13 121.0(5) . . ?
C15 C14 C19 120.2(5) . . ?
C19 C14 C13 118.6(5) . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.7(5) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(5) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(5) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.3(5) . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 119.4(5) . . ?
C14 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
N4 C20 Pd1 128.7(4) . . ?
N5 C20 N4 108.2(4) . . ?
N5 C20 Pd1 123.1(4) . . ?
C22 C21 H21 102.9 . . ?
C23 C21 H21 102.9 . . ?
C23 C21 C22 118.7(6) . . ?
C23 C21 N4 115.6(5) . . ?
N4 C21 H21 102.9 . . ?
N4 C21 C22 111.1(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 120.3(5) . . ?
C25 C24 N4 133.9(6) . . ?
C29 C24 N4 105.8(5) . . ?
C24 C25 H25 121.3 . . ?
C24 C25 C26 117.3(6) . . ?
C26 C25 H25 121.3 . . ?
C25 C26 H26 119.1 . . ?
C27 C26 C25 121.8(6) . . ?
C27 C26 H26 119.1 . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.3(6) . . ?
C28 C27 H27 119.4 . . ?
C27 C28 H28 120.7 . . ?
C27 C28 C29 118.5(6) . . ?
C29 C28 H28 120.7 . . ?
C24 C29 C28 120.7(5) . . ?
N5 C29 C24 106.2(4) . . ?
N5 C29 C28 133.1(5) . . ?
C31 C30 H30 107.1 . . ?
C31 C30 C32 113.5(5) . . ?
C32 C30 H30 107.1 . . ?
N5 C30 H30 107.1 . . ?
N5 C30 C31 111.4(5) . . ?
N5 C30 C32 110.4(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1 N1 C7 129.5(5) . . ?
N2 N1 C1 114.1(4) . . ?
N2 N1 C7 116.4(4) . . ?
N3 N2 N1 103.5(4) . . ?
C2 N3 C13 129.6(4) . . ?
N2 N3 C2 112.5(4) . . ?
N2 N3 C13 117.7(4) . . ?
C20 N4 C21 128.2(6) . . ?
C20 N4 C24 109.7(4) . . ?
C24 N4 C21 121.7(6) . . ?
C20 N5 C29 110.1(4) . . ?
C20 N5 C30 123.4(4) . . ?
C29 N5 C30 126.5(4) . . ?
Br1 Pd1 Br2 169.62(2) . . ?
C1 Pd1 Br1 92.62(13) . . ?
C1 Pd1 Br2 89.65(13) . . ?
C20 Pd1 Br1 88.24(13) . . ?
C20 Pd1 Br2 89.10(14) . . ?
C20 Pd1 C1 177.6(2) . . ?
C34 C33 Pd2 131.6(5) . . ?
N6 C33 C34 101.2(7) . . ?
N6 C33 Pd2 127.2(6) . . ?
C33 C34 C35 126.6(8) . . ?
N8 C34 C33 109.2(6) . . ?
N8 C34 C35 121.8(8) . . ?
C34 C35 H35A 109.7 . . ?
C34 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
C36 C35 C34 109.7(12) . . ?
C36 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
C35 C36 H36A 111.2 . . ?
C35 C36 H36B 111.2 . . ?
C35 C36 C37 102.9(11) . . ?
H36A C36 H36B 109.1 . . ?
C37 C36 H36A 111.2 . . ?
C37 C36 H36B 111.2 . . ?
C36 C37 H37A 111.0 . . ?
C36 C37 H37B 111.0 . . ?
H37A C37 H37B 109.0 . . ?
C38 C37 C36 103.9(10) . . ?
C38 C37 H37A 111.0 . . ?
C38 C37 H37B 111.0 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C44 120.0 . . ?
C40 C39 N6 111.3(9) . . ?
C44 C39 N6 128.6(9) . . ?
C39 C40 H40 120.0 . . ?
C41 C40 C39 120.0 . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 120.0 . . ?
C40 C41 C42 120.0 . . ?
C42 C41 H41 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C44 C43 H43 120.0 . . ?
C39 C44 H44 120.0 . . ?
C43 C44 C39 120.0 . . ?
C43 C44 H44 120.0 . . ?
H45A C45 H45B 107.5 . . ?
H45C C45 H45D 108.0 . . ?
C46 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
C46' C45 H45C 109.3 . . ?
C46' C45 H45D 109.3 . . ?
C46' C45 N8 111.6(9) . . ?
N8 C45 H45A 108.4 . . ?
N8 C45 H45B 108.4 . . ?
N8 C45 H45C 109.3 . . ?
N8 C45 H45D 109.3 . . ?
N8 C45 C46 115.4(9) . . ?
C47 C46 C45 115.5(11) . . ?
C47 C46 C51 120.0 . . ?
C51 C46 C45 124.4(11) . . ?
C46 C47 H47 120.0 . . ?
C46 C47 C48 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 H48 120.0 . . ?
C47 C48 C49 120.0 . . ?
C49 C48 H48 120.0 . . ?
C48 C49 H49 120.0 . . ?
C48 C49 C50 120.0 . . ?
C50 C49 H49 120.0 . . ?
C49 C50 H50 120.0 . . ?
C49 C50 C51 120.0 . . ?
C51 C50 H50 120.0 . . ?
C46 C51 H51 120.0 . . ?
C50 C51 C46 120.0 . . ?
C50 C51 H51 120.0 . . ?
C47' C46' C45 123.5(12) . . ?
C47' C46' C51' 120.0 . . ?
C51' C46' C45 116.1(12) . . ?
C46' C47' H47' 120.0 . . ?
C48' C47' C46' 120.0 . . ?
C48' C47' H47' 120.0 . . ?
C47' C48' H48' 120.0 . . ?
C49' C48' C47' 120.0 . . ?
C49' C48' H48' 120.0 . . ?
C48' C49' H49' 120.0 . . ?
C50' C49' C48' 120.0 . . ?
C50' C49' H49' 120.0 . . ?
C49' C50' H50' 120.0 . . ?
C51' C50' C49' 120.0 . . ?
C51' C50' H50' 120.0 . . ?
C46' C51' H51' 120.0 . . ?
C50' C51' C46' 120.0 . . ?
C50' C51' H51' 120.0 . . ?
N9 C52 N10 107.7(5) . . ?
N9 C52 Pd2 127.9(4) . . ?
N10 C52 Pd2 124.4(4) . . ?
C54 C53 H53 103.5 . . ?
C55 C53 H53 103.5 . . ?
C55 C53 C54 117.9(8) . . ?
C55 C53 N9 114.8(8) . . ?
N9 C53 H53 103.5 . . ?
N9 C53 C54 111.4(6) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C57 C56 N9 130.9(7) . . ?
C61 C56 C57 122.1(7) . . ?
C61 C56 N9 107.0(5) . . ?
C56 C57 H57 121.2 . . ?
C58 C57 C56 117.6(8) . . ?
C58 C57 H57 121.2 . . ?
C57 C58 H58 119.4 . . ?
C57 C58 C59 121.2(7) . . ?
C59 C58 H58 119.4 . . ?
C58 C59 H59 119.0 . . ?
C58 C59 C60 122.0(7) . . ?
C60 C59 H59 119.0 . . ?
C59 C60 H60 122.0 . . ?
C61 C60 C59 116.0(7) . . ?
C61 C60 H60 122.0 . . ?
C56 C61 C60 121.0(6) . . ?
N10 C61 C56 106.1(5) . . ?
N10 C61 C60 132.9(7) . . ?
C63 C62 H62 107.1 . . ?
C63 C62 C64 113.5(5) . . ?
C64 C62 H62 107.1 . . ?
N10 C62 H62 107.1 . . ?
N10 C62 C63 110.1(5) . . ?
N10 C62 C64 111.6(5) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C33 N6 C39 123.8(8) . . ?
N7 N6 C33 115.2(7) . . ?
N7 N6 C39 117.8(8) . . ?
N8 N7 N6 104.1(7) . . ?
C34 N8 C45 132.4(7) . . ?
N7 N8 C34 110.2(7) . . ?
N7 N8 C45 117.4(7) . . ?
C52 N9 C53 122.2(6) . . ?
C52 N9 C56 109.2(5) . . ?
C56 N9 C53 128.3(6) . . ?
C52 N10 C61 109.9(5) . . ?
C52 N10 C62 122.2(5) . . ?
C61 N10 C62 127.8(5) . . ?
Br4 Pd2 Br3 178.38(3) . . ?
C33 Pd2 Br3 90.2(2) . . ?
C33 Pd2 Br4 91.2(2) . . ?
C52 Pd2 Br3 90.57(17) . . ?
C52 Pd2 Br4 88.05(17) . . ?
C52 Pd2 C33 177.7(3) . . ?
_shelx_res_file
;
20170613-yxc-20.res created by SHELXL-2014/7
TITL 20170613-yxc-20_a.res in P2(1)/c
REM Old TITL 20170613-YXC-20 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.162, Rweak 0.007, Alpha 0.051, Orientation as input
REM Formula found by SHELXT: C56 N7 Br4 N9
CELL 1.54184 32.35 8.6596 25.0145 90 94.521 90
ZERR 8 0.0003 0.0001 0.0002 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N Pd
UNIT 256 312 16 40 8
ISOR 0.01 0.02 C34 > C52
ISOR 0.01 0.02 N6 N7
L.S. 10
PLAN 5
BOND $H
ABIN
fmap 2
acta
OMIT -5 1 4
OMIT -3 0 4
OMIT 4 1 3
OMIT 4 1 1
OMIT -4 0 6
OMIT -1 1 1
OMIT 8 0 8
OMIT -5 1 1
OMIT -8 1 4
OMIT 0 0 8
OMIT 7 3 2
OMIT -6 0 6
OMIT -1 0 10
OMIT -2 1 5
OMIT -7 0 4
OMIT 5 1 3
OMIT 6 0 6
OMIT -14 1 6
OMIT 3 0 0
OMIT 1 1 11
OMIT -15 2 1
OMIT -6 1 2
OMIT 0 1 12
OMIT 5 0 4
OMIT -3 0 2
OMIT 4 1 0
OMIT -2 1 6
OMIT 1 0 10
OMIT -7 2 11
OMIT -1 0 4
OMIT -14 3 3
OMIT -1 1 5
OMIT -1 0 2
OMIT 7 3 7
OMIT 9 2 10
OMIT 6 1 11
OMIT -10 2 5
OMIT -4 0 4
OMIT 3 0 8
OMIT 8 1 0
OMIT 4 2 4
OMIT 4 0 4
OMIT -9 1 2
OMIT 2 2 2
OMIT -5 2 15
OMIT 2 0 4
OMIT 9 4 11
OMIT -17 1 1
OMIT 8 3 14
OMIT -3 0 6
REM
REM
REM
WGHT 0.098100 28.883600
FVAR 0.12761
BR1 3 0.368529 -0.105960 0.550315 11.00000 0.03434 0.03183 =
0.01394 -0.00076 0.00651 -0.00176
BR2 3 0.421128 0.199833 0.705425 11.00000 0.02860 0.04832 =
0.01363 -0.00152 0.00381 -0.00700
C1 1 0.426807 0.194824 0.578661 11.00000 0.02088 0.03209 =
0.01271 -0.00080 0.00212 -0.00749
C2 1 0.406931 0.317101 0.552087 11.00000 0.02440 0.03884 =
0.01176 0.00341 0.00457 -0.00540
C3 1 0.361391 0.355197 0.546529 11.00000 0.01975 0.04784 =
0.01907 0.00174 0.00594 -0.00642
AFIX 23
H3A 2 0.355903 0.419210 0.514945 11.00000 -1.20000
H3B 2 0.345973 0.259900 0.540461 11.00000 -1.20000
AFIX 0
C4 1 0.345231 0.436323 0.593212 11.00000 0.02426 0.02971 =
0.02133 -0.00027 0.00384 -0.00402
AFIX 23
H4A 2 0.356162 0.540638 0.595317 11.00000 -1.20000
H4B 2 0.354631 0.382937 0.626034 11.00000 -1.20000
AFIX 0
C5 1 0.297181 0.442313 0.588019 11.00000 0.02440 0.04154 =
0.02823 -0.00268 0.00142 -0.00137
AFIX 23
H5A 2 0.288015 0.486883 0.553529 11.00000 -1.20000
H5B 2 0.286543 0.337663 0.588706 11.00000 -1.20000
AFIX 0
C6 1 0.279128 0.533423 0.631051 11.00000 0.03699 0.06180 =
0.03424 -0.00959 0.00347 0.01602
AFIX 137
H6A 2 0.249417 0.530129 0.625942 11.00000 -1.50000
H6B 2 0.288332 0.638612 0.629534 11.00000 -1.50000
H6C 2 0.288007 0.490214 0.665394 11.00000 -1.50000
AFIX 0
C7 1 0.503128 0.121295 0.582898 11.00000 0.02512 0.02899 =
0.01672 0.00075 0.00330 -0.00364
C8 1 0.508823 0.063635 0.634682 11.00000 0.02880 0.04563 =
0.01431 0.00385 0.00748 0.00257
AFIX 43
H8 2 0.489231 0.082123 0.659205 11.00000 -1.20000
AFIX 0
C9 1 0.543789 -0.021140 0.649252 11.00000 0.03527 0.04158 =
0.02318 0.00501 0.00358 0.00580
AFIX 43
H9 2 0.548168 -0.057754 0.684190 11.00000 -1.20000
AFIX 0
C10 1 0.572712 -0.052979 0.612537 11.00000 0.03220 0.03829 =
0.02996 0.00020 0.00332 0.00272
AFIX 43
H10 2 0.596078 -0.111907 0.622575 11.00000 -1.20000
AFIX 0
C11 1 0.566393 0.003602 0.561233 11.00000 0.03141 0.03049 =
0.02940 -0.00225 0.01555 -0.00178
AFIX 43
H11 2 0.585923 -0.015410 0.536672 11.00000 -1.20000
AFIX 0
C12 1 0.531054 0.089081 0.545664 11.00000 0.03164 0.03163 =
0.01811 0.00417 0.01048 -0.00359
AFIX 43
H12 2 0.526367 0.123992 0.510550 11.00000 -1.20000
AFIX 0
C13 1 0.432874 0.546969 0.500325 11.00000 0.02388 0.02935 =
0.01737 -0.00044 0.00776 -0.00154
AFIX 23
H13A 2 0.459456 0.599217 0.504493 11.00000 -1.20000
H13B 2 0.412901 0.611221 0.516887 11.00000 -1.20000
AFIX 0
C14 1 0.419786 0.533588 0.441023 11.00000 0.02394 0.02744 =
0.01485 0.00178 0.00618 -0.00166
C15 1 0.440415 0.437594 0.408510 11.00000 0.03089 0.04209 =
0.01588 0.00072 0.00221 0.00931
AFIX 43
H15 2 0.461648 0.374407 0.423101 11.00000 -1.20000
AFIX 0
C16 1 0.429362 0.435255 0.353370 11.00000 0.03911 0.03992 =
0.01401 -0.00236 0.00532 0.00316
AFIX 43
H16 2 0.443344 0.370388 0.331279 11.00000 -1.20000
AFIX 0
C17 1 0.398017 0.528025 0.331602 11.00000 0.03704 0.03713 =
0.01446 0.00439 0.00296 -0.00083
AFIX 43
H17 2 0.390726 0.525525 0.294899 11.00000 -1.20000
AFIX 0
C18 1 0.377363 0.624803 0.364107 11.00000 0.03423 0.03671 =
0.02242 0.00353 0.00138 0.00790
AFIX 43
H18 2 0.356061 0.687315 0.349298 11.00000 -1.20000
AFIX 0
C19 1 0.388253 0.629476 0.419139 11.00000 0.03046 0.04056 =
0.01723 -0.00086 0.00438 0.00525
AFIX 43
H19 2 0.374597 0.695975 0.441035 11.00000 -1.20000
AFIX 0
C20 1 0.373777 -0.113143 0.676026 11.00000 0.02271 0.02638 =
0.01096 0.00313 0.00498 0.00138
C21 1 0.431182 -0.309965 0.695405 11.00000 0.03135 0.09606 =
0.03612 -0.02251 -0.00530 0.03152
AFIX 13
H21 2 0.427955 -0.416165 0.707957 11.00000 -1.20000
AFIX 0
C22 1 0.460892 -0.241091 0.738038 11.00000 0.02712 0.04879 =
0.02355 0.00363 -0.00051 0.00439
AFIX 137
H22A 2 0.487250 -0.291941 0.737849 11.00000 -1.50000
H22B 2 0.450176 -0.254320 0.772456 11.00000 -1.50000
H22C 2 0.464244 -0.132984 0.731061 11.00000 -1.50000
AFIX 0
C23 1 0.444597 -0.330862 0.642966 11.00000 0.02242 0.12251 =
0.04412 -0.04152 0.00122 0.01056
AFIX 137
H23A 2 0.451445 -0.232432 0.628373 11.00000 -1.50000
H23B 2 0.422772 -0.377869 0.620338 11.00000 -1.50000
H23C 2 0.468610 -0.396361 0.644866 11.00000 -1.50000
AFIX 0
C24 1 0.360231 -0.309427 0.730265 11.00000 0.03830 0.03011 =
0.01325 -0.00076 0.00300 -0.00434
C25 1 0.359696 -0.443396 0.761189 11.00000 0.06023 0.02973 =
0.01921 -0.00060 -0.01057 0.00354
AFIX 43
H25 2 0.381798 -0.512373 0.763137 11.00000 -1.20000
AFIX 0
C26 1 0.324571 -0.469819 0.789157 11.00000 0.07122 0.03889 =
0.01684 0.00402 0.00241 -0.02998
AFIX 43
H26 2 0.323288 -0.558801 0.809777 11.00000 -1.20000
AFIX 0
C27 1 0.291857 -0.367691 0.786986 11.00000 0.04547 0.04751 =
0.02168 0.00234 0.00464 -0.02091
AFIX 43
H27 2 0.269349 -0.387807 0.806866 11.00000 -1.20000
AFIX 0
C28 1 0.291822 -0.238112 0.756363 11.00000 0.03766 0.04332 =
0.01713 0.00006 0.00933 -0.01696
AFIX 43
H28 2 0.269388 -0.170648 0.754638 11.00000 -1.20000
AFIX 0
C29 1 0.326372 -0.208308 0.727400 11.00000 0.02737 0.02954 =
0.01441 -0.00295 0.00414 -0.00731
C30 1 0.309971 0.044888 0.677586 11.00000 0.02809 0.02822 =
0.02898 0.00288 0.00973 0.00497
AFIX 13
H30 2 0.325217 0.106889 0.652915 11.00000 -1.20000
AFIX 0
C31 1 0.269851 -0.003762 0.647432 11.00000 0.02991 0.04316 =
0.04330 0.00749 0.00050 0.00443
AFIX 137
H31A 2 0.253422 -0.060800 0.670943 11.00000 -1.50000
H31B 2 0.275758 -0.067644 0.617607 11.00000 -1.50000
H31C 2 0.254847 0.086205 0.634560 11.00000 -1.50000
AFIX 0
C32 1 0.303870 0.144768 0.725906 11.00000 0.04134 0.04275 =
0.04658 -0.01034 0.01217 0.00871
AFIX 137
H32A 2 0.288054 0.234626 0.714837 11.00000 -1.50000
H32B 2 0.330396 0.175936 0.742280 11.00000 -1.50000
H32C 2 0.289285 0.087166 0.751282 11.00000 -1.50000
AFIX 0
N1 4 0.467353 0.215135 0.567721 11.00000 0.02240 0.03513 =
0.01318 0.00088 0.00656 -0.00047
N2 4 0.473797 0.339179 0.537933 11.00000 0.02192 0.03478 =
0.01424 0.00019 0.00475 -0.00199
N3 4 0.436442 0.400076 0.529126 11.00000 0.01956 0.03509 =
0.01333 -0.00177 0.00649 -0.00317
N4 4 0.388986 -0.244674 0.697738 11.00000 0.02812 0.03840 =
0.01392 -0.00418 0.00734 0.00598
N5 4 0.336135 -0.089857 0.693275 11.00000 0.02047 0.02819 =
0.01567 0.00047 0.00904 0.00020
PD1 5 0.401059 0.036980 0.626928 11.00000 0.02123 0.03806 =
0.01020 0.00310 0.00560 -0.00512
BR3 3 0.186405 0.858911 0.798801 11.00000 0.04133 0.06293 =
0.03592 -0.00218 0.01016 0.01015
BR4 3 0.124381 0.585178 0.943150 11.00000 0.03928 0.05351 =
0.07252 0.00394 0.02691 0.00466
C33 1 0.110346 0.888987 0.871105 11.00000 0.02565 0.06431 =
0.04344 -0.00737 0.00761 -0.00029
SAME 0.02 0.04 C2 > C6
C34 1 0.108233 1.023957 0.898586 11.00000 0.03208 0.05085 =
0.06530 -0.01775 0.00621 0.00858
C35 1 0.144468 1.108886 0.929287 11.00000 0.13854 0.10611 =
0.11690 -0.01724 0.00360 0.04015
AFIX 23
H35A 2 0.168887 1.103276 0.909219 11.00000 -1.20000
H35B 2 0.137392 1.216842 0.933443 11.00000 -1.20000
AFIX 0
C36 1 0.152971 1.040577 0.980265 11.00000 0.16232 0.12425 =
0.13055 0.00372 0.04480 -0.01319
AFIX 23
H36A 2 0.153346 0.928818 0.977728 11.00000 -1.20000
H36B 2 0.132647 1.071283 1.004729 11.00000 -1.20000
AFIX 0
C37 1 0.199827 1.109594 0.999937 11.00000 0.07812 0.10235 =
0.08642 -0.02378 -0.02474 0.01820
AFIX 23
H37A 2 0.216104 1.033560 1.020845 11.00000 -1.20000
H37B 2 0.214668 1.139540 0.969354 11.00000 -1.20000
AFIX 0
C38 1 0.191329 1.240808 1.031924 11.00000 0.10507 0.09753 =
0.14447 -0.04054 -0.06585 0.02756
AFIX 137
H38A 2 0.186600 1.329458 1.009219 11.00000 -1.50000
H38B 2 0.214567 1.259999 1.057340 11.00000 -1.50000
H38C 2 0.167110 1.221128 1.050704 11.00000 -1.50000
AFIX 66
C39 1 0.054049 0.751236 0.817723 11.00000 0.09149 0.13098 =
0.12527 -0.00204 -0.04171 -0.00070
C40 1 0.073052 0.703210 0.772637 11.00000 0.09088 0.14365 =
0.12507 -0.02434 -0.03164 -0.00239
AFIX 43
H40 2 0.096354 0.754880 0.762372 11.00000 -1.20000
AFIX 65
C41 1 0.057226 0.577958 0.742892 11.00000 0.10681 0.11766 =
0.14613 -0.03567 0.00298 -0.00519
AFIX 43
H41 2 0.069939 0.545826 0.712727 11.00000 -1.20000
AFIX 65
C42 1 0.022398 0.500731 0.758234 11.00000 0.17010 0.15328 =
0.15271 -0.00601 -0.00251 0.00158
AFIX 43
H42 2 0.011809 0.416929 0.738333 11.00000 -1.20000
AFIX 65
C43 1 0.003395 0.548755 0.803320 11.00000 0.17208 0.16294 =
0.18227 -0.00349 -0.00927 -0.01308
AFIX 43
H43 2 -0.019907 0.497085 0.813584 11.00000 -1.20000
AFIX 65
C44 1 0.019221 0.674007 0.833065 11.00000 0.14639 0.14369 =
0.17416 -0.00685 -0.01490 -0.01722
AFIX 43
H44 2 0.006507 0.706139 0.863230 11.00000 -1.20000
AFIX 0
C45 1 0.055875 1.245483 0.896514 11.00000 0.04453 0.05531 =
0.08987 -0.00470 0.02455 0.00610
PART 1
AFIX 23
H45A 2 0.038206 1.282120 0.866009 10.50000 -1.20000
H45B 2 0.078698 1.317766 0.902270 10.50000 -1.20000
AFIX 23
PART 0
PART 2
H45C 2 0.077414 1.305925 0.915880 10.50000 -1.20000
H45D 2 0.047089 1.300405 0.863777 10.50000 -1.20000
AFIX 66
PART 0
PART 1
C46 1 0.029912 1.247844 0.947934 10.50000 0.05391 0.06392 =
0.07130 -0.00210 0.02545 0.01108
C47 1 -0.012063 1.214645 0.938429 10.50000 0.06120 0.06934 =
0.09873 -0.01430 0.03190 -0.00905
AFIX 43
H47 2 -0.022860 1.187978 0.904113 10.50000 -1.20000
AFIX 65
C48 1 -0.037899 1.221302 0.980213 10.50000 0.07910 0.08847 =
0.09718 -0.00173 0.04162 0.00137
AFIX 43
H48 2 -0.065983 1.199090 0.973854 10.50000 -1.20000
AFIX 65
C49 1 -0.021762 1.261159 1.031502 10.50000 0.12074 0.13737 =
0.12702 0.00063 0.02605 0.00249
AFIX 43
H49 2 -0.039048 1.265614 1.059458 10.50000 -1.20000
AFIX 65
C50 1 0.020213 1.294359 1.041007 10.50000 0.16390 0.17231 =
0.15424 0.00178 0.01799 0.01109
AFIX 43
H50 2 0.031009 1.321026 1.075323 10.50000 -1.20000
AFIX 65
C51 1 0.046049 1.287701 0.999224 10.50000 0.11128 0.13444 =
0.12647 0.00587 0.02368 0.01584
AFIX 43
H51 2 0.074133 1.309914 1.005584 10.50000 -1.20000
AFIX 66
PART 0
PART 2
C46' 1 0.021166 1.230001 0.928879 10.50000 0.04014 0.05709 =
0.06428 -0.01198 0.01119 0.00768
C47' 1 -0.002499 1.096403 0.930705 10.50000 0.11426 0.11690 =
0.12746 -0.00370 0.02590 -0.00372
AFIX 43
H47' 2 0.001511 1.015690 0.907139 10.50000 -1.20000
AFIX 65
C48' 1 -0.032156 1.083438 0.967753 10.50000 0.12144 0.12836 =
0.12499 -0.00311 0.02716 -0.00062
AFIX 43
H48' 2 -0.047989 0.994051 0.968974 10.50000 -1.20000
AFIX 65
C49' 1 -0.038149 1.204071 1.002975 10.50000 0.07341 0.07869 =
0.07606 -0.01353 0.02056 0.00883
AFIX 43
H49' 2 -0.057992 1.195396 1.027763 10.50000 -1.20000
AFIX 65
C50' 1 -0.014485 1.337671 1.001151 10.50000 0.14205 0.15000 =
0.15447 -0.00644 0.02490 0.00383
AFIX 43
H50' 2 -0.018495 1.418382 1.024717 10.50000 -1.20000
AFIX 65
C51' 1 0.015172 1.350638 0.964103 10.50000 0.10694 0.11830 =
0.11168 -0.01098 0.01695 -0.00217
AFIX 43
H51' 2 0.031005 1.440025 0.962882 10.50000 -1.20000
AFIX 0
PART 0
C52 1 0.200248 0.566281 0.874744 11.00000 0.02775 0.04609 =
0.02760 -0.00976 0.00957 -0.00484
C53 1 0.173116 0.408183 0.797049 11.00000 0.04016 0.11377 =
0.04967 -0.04188 0.01454 -0.03254
AFIX 13
H53 2 0.157057 0.504031 0.793123 11.00000 -1.20000
AFIX 0
C54 1 0.195261 0.401077 0.746230 11.00000 0.04213 0.07457 =
0.04441 -0.01566 0.00718 -0.00602
AFIX 137
H54A 2 0.215928 0.321348 0.749410 11.00000 -1.50000
H54B 2 0.208317 0.498603 0.740512 11.00000 -1.50000
H54C 2 0.175629 0.378759 0.716434 11.00000 -1.50000
AFIX 0
C55 1 0.142255 0.292998 0.804860 11.00000 0.05340 0.18426 =
0.05880 0.01260 -0.00339 -0.04694
AFIX 137
H55A 2 0.123596 0.285506 0.773168 11.00000 -1.50000
H55B 2 0.127027 0.321389 0.834785 11.00000 -1.50000
H55C 2 0.155502 0.195068 0.811851 11.00000 -1.50000
AFIX 0
C56 1 0.237800 0.353998 0.862353 11.00000 0.03724 0.03373 =
0.04058 -0.00099 0.02513 -0.00565
C57 1 0.252656 0.212091 0.845572 11.00000 0.06182 0.03237 =
0.05461 0.00629 0.04053 -0.00211
AFIX 43
H57 2 0.237978 0.154574 0.819021 11.00000 -1.20000
AFIX 0
C58 1 0.289214 0.161123 0.869334 11.00000 0.08613 0.04135 =
0.04537 0.01092 0.03661 0.00979
AFIX 43
H58 2 0.300058 0.067823 0.858458 11.00000 -1.20000
AFIX 0
C59 1 0.310996 0.246530 0.910038 11.00000 0.06029 0.06595 =
0.05061 0.04182 0.03351 0.03145
AFIX 43
H59 2 0.336229 0.209109 0.925106 11.00000 -1.20000
AFIX 0
C60 1 0.295764 0.387516 0.928800 11.00000 0.04397 0.06628 =
0.02860 0.02350 0.01369 0.01264
AFIX 43
H60 2 0.310009 0.443528 0.956116 11.00000 -1.20000
AFIX 0
C61 1 0.258102 0.437814 0.903958 11.00000 0.03498 0.03764 =
0.03051 0.01356 0.01925 0.00492
C62 1 0.242298 0.696045 0.948542 11.00000 0.03552 0.04057 =
0.02602 -0.00467 0.00434 -0.00485
AFIX 13
H62 2 0.219403 0.769694 0.942520 11.00000 -1.20000
AFIX 0
C63 1 0.281658 0.779880 0.936253 11.00000 0.05206 0.04861 =
0.03819 -0.00667 0.00875 -0.01851
AFIX 137
H63A 2 0.285564 0.868344 0.959226 11.00000 -1.50000
H63B 2 0.279373 0.812761 0.899488 11.00000 -1.50000
H63C 2 0.304928 0.711552 0.942275 11.00000 -1.50000
AFIX 0
C64 1 0.242510 0.641597 1.006753 11.00000 0.05149 0.06453 =
0.02363 -0.00042 0.01036 -0.00856
AFIX 137
H64A 2 0.265088 0.571055 1.014455 11.00000 -1.50000
H64B 2 0.216799 0.590572 1.012013 11.00000 -1.50000
H64C 2 0.245775 0.729003 1.030315 11.00000 -1.50000
AFIX 0
N6 4 0.074212 0.890626 0.841573 11.00000 0.04861 0.07260 =
0.09894 -0.02922 -0.03862 0.02406
N7 4 0.050842 1.012376 0.848203 11.00000 0.07157 0.09124 =
0.11491 -0.02591 -0.04358 0.03320
N8 4 0.072633 1.095913 0.883007 11.00000 0.02717 0.05602 =
0.06965 -0.00250 0.01259 0.00220
N9 4 0.202470 0.438055 0.844558 11.00000 0.02709 0.04613 =
0.03894 -0.00967 0.01188 -0.00300
N10 4 0.233955 0.568084 0.910643 11.00000 0.02807 0.03358 =
0.02186 -0.00066 0.00649 -0.00176
PD2 5 0.154988 0.725339 0.871507 11.00000 0.02400 0.04788 =
0.03389 -0.01157 0.00479 0.00310
HKLF 4
REM 20170613-yxc-20_a.res in P2(1)/c
REM R1 = 0.0656 for 12112 Fo > 4sig(Fo) and 0.0714 for all 13750 data
REM 749 parameters refined using 169 restraints
END
WGHT 0.0981 28.8778
REM Highest difference peak 2.375, deepest hole -2.293, 1-sigma level 0.158
Q1 1 0.1754 1.1281 0.9455 11.00000 0.05 2.38
Q2 1 0.1292 1.0510 0.9546 11.00000 0.05 2.18
Q3 1 0.0693 0.8067 0.7882 11.00000 0.05 1.63
Q4 1 0.1645 0.7972 0.8474 11.00000 0.05 1.43
Q5 1 0.3812 0.0841 0.6365 11.00000 0.05 1.37
;
_shelx_res_checksum 9922
_shelx_fab_file
;
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-40 1 2 0.2500 0.3270
-40 1 3 -0.7153 -1.0582
-40 1 4 -0.6105 -0.2048
-39 0 2 -1.3646 0.2067
-39 0 4 -0.9327 -1.0884
-39 0 6 1.4827 -1.3016
-39 0 8 -1.3237 0.1011
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-39 1 2 -0.0118 0.2308
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-39 2 7 1.8270 0.0627
-38 0 2 -1.7498 -2.4108
-38 0 4 0.6629 -1.5266
-38 0 6 0.5239 -0.5288
-38 0 8 0.5913 0.2853
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-38 0 12 -1.7647 0.7649
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-38 1 9 0.0638 0.2181
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-38 2 5 2.9489 -0.0146
-38 2 6 1.9681 0.2640
-38 2 7 -0.8757 0.0759
-38 2 8 -0.6118 -0.3787
-38 2 9 -1.9313 -0.0893
-38 2 10 -1.4517 0.4212
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-38 3 2 -0.4928 0.2426
-38 3 3 0.4886 -0.0992
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-38 3 5 0.4584 -0.2004
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-37 0 8 1.2618 0.2811
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-37 1 1 0.3330 0.4795
-37 1 2 -0.3395 0.2610
-37 1 3 0.2879 0.4700
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-37 1 5 -1.1740 0.4512
-37 1 6 0.2036 -0.2721
-37 1 7 0.3045 -0.3040
-37 1 8 1.8237 -0.1825
-37 1 9 0.8904 0.2346
-37 1 10 -0.3186 0.2688
-37 1 11 0.0836 0.1558
-37 1 12 -0.7518 0.4538
-37 1 13 -0.3577 0.9823
-37 1 14 -0.5870 -0.8426
-37 2 1 -0.6142 0.1191
-37 2 2 -0.1586 -1.3886
-37 2 3 1.5297 -0.3269
-37 2 4 1.2627 -0.3476
-37 2 5 2.0669 0.1437
-37 2 6 0.6830 0.4922
-37 2 7 -3.3420 -0.0884
-37 2 8 -2.0758 -0.0985
-37 2 9 -0.0616 -0.0164
-37 2 10 -0.4999 0.9029
-37 2 11 -0.5622 0.2498
-37 2 12 1.3193 0.1277
-37 2 13 0.3676 0.0290
-37 3 1 0.1242 0.6228
-37 3 2 -1.0340 -0.2836
-37 3 3 0.4754 -0.4403
-37 3 4 -0.1280 -0.8618
-37 3 5 0.6840 0.3158
-37 3 6 1.1881 0.2507
-37 3 7 -0.2965 0.6558
-37 3 8 1.6020 0.4953
-37 3 9 -0.3739 -0.3526
-37 3 10 -0.6239 0.0859
-37 4 1 0.0949 -0.9152
-37 4 2 0.1843 -0.0144
-37 4 4 -0.9943 -0.8423
-37 4 5 -0.6133 0.5279
-37 4 6 0.1313 -0.1818
-36 0 2 -0.1043 -1.6807
-36 0 4 0.9262 1.7598
-36 0 6 0.4036 0.4897
-36 0 8 -0.1515 0.3629
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-36 0 12 0.2410 -0.3942
-36 0 14 -2.1874 -0.0999
-36 1 1 0.0962 0.6959
-36 1 2 -0.8589 -0.1479
-36 1 3 -0.4263 0.0960
-36 1 4 -0.6612 -0.7352
-36 1 5 -0.9418 0.0048
-36 1 6 1.2548 -0.2821
-36 1 7 1.7787 -0.1055
-36 1 8 1.3187 -0.1302
-36 1 9 0.6528 -0.1574
-36 1 10 -1.4857 0.3865
-36 1 11 -0.5722 0.3523
-36 1 12 -0.6742 -0.2377
-36 1 13 0.5967 -0.1928
-36 1 14 -0.8252 -0.6457
-36 1 15 1.0625 -1.6286
-36 2 1 0.4983 -0.2228
-36 2 2 1.2685 -0.7164
-36 2 3 2.5379 -0.0330
-36 2 4 0.7575 0.3636
-36 2 5 -0.8562 0.0172
-36 2 6 -1.6407 0.3543
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-36 2 8 -1.5477 0.3050
-36 2 9 1.7608 0.2401
-36 2 10 0.7867 0.7348
-36 2 11 -1.0403 0.2612
-36 2 12 1.1503 -0.0020
-36 2 13 1.9962 -0.3079
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-36 3 4 1.3303 -0.1601
-36 3 5 0.2839 0.5590
-36 3 6 1.1543 0.6170
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38 2 4 0.7943 0.1547
38 2 5 0.3922 0.1357
38 2 6 -1.3853 0.2317
38 3 0 -0.5960 -0.3922
38 3 1 0.0058 -0.0106
38 3 2 -0.6795 0.0730
39 0 0 0.5747 -3.0188
39 0 2 0.9234 0.5907
39 0 4 0.5839 -0.1064
39 1 0 -0.4410 -0.3771
39 1 1 -0.5426 -0.0924
39 1 2 0.1885 -0.0729
39 1 3 -0.9253 0.2104
39 1 4 -0.0429 -0.4694
39 2 0 0.7053 1.5231
39 2 1 0.6955 -0.1123
39 2 2 0.4241 -0.5436
39 2 3 -1.1379 0.3230
40 1 0 -0.4609 -0.8661
0 0 0 0.0 0.0
;
_shelx_fab_checksum 39441
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.138
_oxdiff_exptl_absorpt_empirical_full_min 0.354
#===END