# Electronic Supplementary Material (ESI) for Polymer Chemistry.
# 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
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data_mo_dm15330_0m
_database_code_depnum_ccdc_archive 'CCDC 1853301'
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_audit_creation_date 2015-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number 2014-3
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C24 H22 N2 O4 Pd'
_chemical_formula_sum 'C24 H22 N2 O4 Pd'
_chemical_formula_weight 508.83
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.3132(7)
_cell_length_b 10.8410(9)
_cell_length_c 12.8010(11)
_cell_angle_alpha 110.224(2)
_cell_angle_beta 92.769(2)
_cell_angle_gamma 105.358(2)
_cell_volume 1031.34(15)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 3723
_cell_measurement_temperature 130
_cell_measurement_theta_max 30.12
_cell_measurement_theta_min 2.57
_shelx_estimated_absorpt_T_max 0.991
_shelx_estimated_absorpt_T_min 0.767
_exptl_absorpt_coefficient_mu 0.934
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.6253
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1014 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.8381.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.639
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 516
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.01
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0277
_diffrn_reflns_av_unetI/netI 0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 10506
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 30.550
_diffrn_reflns_theta_min 1.716
_diffrn_ambient_temperature 130
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5343
_reflns_number_total 6259
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.642
_refine_diff_density_min -0.729
_refine_diff_density_rms 0.098
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.034
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 283
_refine_ls_number_reflns 6259
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0442
_refine_ls_R_factor_gt 0.0352
_refine_ls_restrained_S_all 1.034
_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^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0746
_refine_ls_wR_factor_ref 0.0787
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C13(H13), C14(H14), C15(H15),
C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
2.b Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.14443(2) 0.20947(2) 0.47921(2) 0.01803(6) Uani 1 1 d . . . . .
O1 O 0.2189(2) 0.04057(16) 0.49985(13) 0.0217(3) Uani 1 1 d . . . . .
O2 O 0.3266(2) -0.29467(17) 0.10729(14) 0.0314(4) Uani 1 1 d . . . . .
O3 O 0.4259(2) 0.23967(17) 0.23607(14) 0.0262(4) Uani 1 1 d . . . . .
O4 O -0.1448(2) 0.02601(17) 0.22273(14) 0.0265(4) Uani 1 1 d . . . . .
N1 N 0.1748(2) 0.10375(18) 0.32125(15) 0.0173(4) Uani 1 1 d . . . . .
N2 N 0.1263(2) 0.30564(19) 0.64523(16) 0.0213(4) Uani 1 1 d . . . . .
C1 C 0.2506(3) -0.0343(2) 0.41146(18) 0.0177(4) Uani 1 1 d . . . . .
C2 C 0.3122(3) -0.1503(2) 0.40715(18) 0.0191(4) Uani 1 1 d . . . . .
C3 C 0.3440(3) -0.1740(2) 0.5054(2) 0.0227(5) Uani 1 1 d . . . . .
H3 H 0.3273 -0.1142 0.5755 0.027 Uiso 1 1 calc R . . . .
C4 C 0.4002(3) -0.2852(3) 0.5004(2) 0.0288(5) Uani 1 1 d . . . . .
H4 H 0.4254 -0.3000 0.5675 0.035 Uiso 1 1 calc R . . . .
C5 C 0.4194(3) -0.3739(3) 0.3986(2) 0.0291(5) Uani 1 1 d . . . . .
H5 H 0.4554 -0.4511 0.3954 0.035 Uiso 1 1 calc R . . . .
C6 C 0.3868(3) -0.3519(2) 0.3002(2) 0.0261(5) Uani 1 1 d . . . . .
H6 H 0.3998 -0.4144 0.2301 0.031 Uiso 1 1 calc R . . . .
C7 C 0.3351(3) -0.2390(2) 0.30384(19) 0.0208(4) Uani 1 1 d . . . . .
C8 C 0.3026(3) -0.2140(2) 0.19692(19) 0.0215(4) Uani 1 1 d . . . . .
C9 C 0.2512(3) -0.0973(2) 0.20614(18) 0.0208(4) Uani 1 1 d . . . . .
H9 H 0.2335 -0.0795 0.1395 0.025 Uiso 1 1 calc R . . . .
C10 C 0.2249(3) -0.0076(2) 0.30520(18) 0.0174(4) Uani 1 1 d . . . . .
C11 C 0.1381(3) 0.1349(2) 0.22582(18) 0.0185(4) Uani 1 1 d . . . . .
C12 C -0.0304(3) 0.0997(2) 0.17689(19) 0.0208(4) Uani 1 1 d . . . . .
C13 C -0.0716(3) 0.1403(2) 0.09008(19) 0.0234(5) Uani 1 1 d . . . . .
H13 H -0.1862 0.1177 0.0584 0.028 Uiso 1 1 calc R . . . .
C14 C 0.0561(3) 0.2136(2) 0.05052(19) 0.0250(5) Uani 1 1 d . . . . .
H14 H 0.0281 0.2403 -0.0096 0.030 Uiso 1 1 calc R . . . .
C15 C 0.2239(3) 0.2495(2) 0.09609(19) 0.0236(5) Uani 1 1 d . . . . .
H15 H 0.3101 0.3007 0.0681 0.028 Uiso 1 1 calc R . . . .
C16 C 0.2644(3) 0.2092(2) 0.18385(19) 0.0209(4) Uani 1 1 d . . . . .
C17 C 0.5591(3) 0.3149(3) 0.1962(2) 0.0298(5) Uani 1 1 d . . . . .
H17A H 0.5568 0.2638 0.1160 0.045 Uiso 1 1 calc GR . . . .
H17B H 0.6675 0.3278 0.2386 0.045 Uiso 1 1 calc GR . . . .
H17C H 0.5448 0.4050 0.2064 0.045 Uiso 1 1 calc GR . . . .
C18 C -0.3180(3) -0.0112(3) 0.1788(2) 0.0300(5) Uani 1 1 d . . . . .
H18A H -0.3365 -0.0665 0.0979 0.045 Uiso 1 1 calc GR . . . .
H18B H -0.3512 0.0723 0.1905 0.045 Uiso 1 1 calc GR . . . .
H18C H -0.3861 -0.0651 0.2175 0.045 Uiso 1 1 calc GR . . . .
C19 C 0.0906(4) 0.3581(2) 0.4391(2) 0.0294(5) Uani 1 1 d . . . . .
H19A H 0.1390 0.3625 0.3717 0.044 Uiso 1 1 calc GR . . . .
H19B H 0.1385 0.4468 0.5019 0.044 Uiso 1 1 calc GR . . . .
H19C H -0.0322 0.3380 0.4242 0.044 Uiso 1 1 calc GR . . . .
C20 C 0.2102(3) 0.2736(3) 0.7197(2) 0.0275(5) Uani 1 1 d . . . . .
H20 H 0.2610 0.2022 0.6916 0.033 Uiso 1 1 calc R . . . .
C21 C 0.2261(4) 0.3391(3) 0.8343(2) 0.0338(6) Uani 1 1 d . . . . .
H21 H 0.2884 0.3144 0.8840 0.041 Uiso 1 1 calc R . . . .
C22 C 0.1497(4) 0.4418(3) 0.8766(2) 0.0336(6) Uani 1 1 d . . . . .
H22 H 0.1607 0.4904 0.9555 0.040 Uiso 1 1 calc R . . . .
C23 C 0.0580(3) 0.4710(2) 0.8012(2) 0.0303(6) Uani 1 1 d . . . . .
H23 H 0.0008 0.5384 0.8274 0.036 Uiso 1 1 calc R . . . .
C24 C 0.0492(3) 0.4025(2) 0.6875(2) 0.0252(5) Uani 1 1 d . . . . .
H24 H -0.0142 0.4247 0.6365 0.030 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 0.02147(9) 0.01659(8) 0.01825(9) 0.00747(6) 0.00557(6) 0.00750(6)
O1 0.0293(9) 0.0202(7) 0.0177(8) 0.0074(6) 0.0055(6) 0.0100(7)
O2 0.0406(11) 0.0263(9) 0.0226(9) 0.0012(7) 0.0077(8) 0.0129(8)
O3 0.0185(8) 0.0330(9) 0.0298(9) 0.0189(8) 0.0025(7) 0.0026(7)
O4 0.0195(8) 0.0322(9) 0.0292(9) 0.0163(7) 0.0025(7) 0.0037(7)
N1 0.0192(9) 0.0178(8) 0.0157(8) 0.0077(7) 0.0009(7) 0.0050(7)
N2 0.0226(10) 0.0183(9) 0.0228(9) 0.0076(8) 0.0064(8) 0.0054(8)
C1 0.0163(10) 0.0164(9) 0.0192(10) 0.0069(8) 0.0017(8) 0.0030(8)
C2 0.0179(11) 0.0178(10) 0.0215(10) 0.0082(8) 0.0015(8) 0.0043(8)
C3 0.0237(12) 0.0212(10) 0.0232(11) 0.0099(9) 0.0010(9) 0.0053(9)
C4 0.0293(13) 0.0303(13) 0.0328(13) 0.0196(11) 0.0013(10) 0.0089(11)
C5 0.0280(13) 0.0241(12) 0.0418(15) 0.0156(11) 0.0085(11) 0.0131(10)
C6 0.0245(12) 0.0224(11) 0.0310(13) 0.0081(10) 0.0075(10) 0.0083(10)
C7 0.0174(11) 0.0191(10) 0.0239(11) 0.0066(9) 0.0011(9) 0.0047(9)
C8 0.0199(11) 0.0214(11) 0.0193(11) 0.0044(9) 0.0020(8) 0.0043(9)
C9 0.0218(11) 0.0207(10) 0.0178(10) 0.0063(9) 0.0014(8) 0.0046(9)
C10 0.0146(10) 0.0190(10) 0.0174(10) 0.0076(8) 0.0000(8) 0.0025(8)
C11 0.0228(11) 0.0179(10) 0.0164(10) 0.0070(8) 0.0033(8) 0.0078(9)
C12 0.0225(11) 0.0198(10) 0.0200(10) 0.0068(9) 0.0040(9) 0.0070(9)
C13 0.0254(12) 0.0245(11) 0.0202(11) 0.0070(9) -0.0004(9) 0.0098(10)
C14 0.0358(14) 0.0237(11) 0.0188(11) 0.0098(9) 0.0025(9) 0.0119(10)
C15 0.0311(13) 0.0209(11) 0.0204(11) 0.0107(9) 0.0071(9) 0.0058(9)
C16 0.0219(11) 0.0194(10) 0.0210(11) 0.0070(9) 0.0020(9) 0.0066(9)
C17 0.0227(12) 0.0299(13) 0.0402(15) 0.0185(11) 0.0091(11) 0.0052(10)
C18 0.0201(12) 0.0314(13) 0.0363(14) 0.0115(11) 0.0029(10) 0.0058(10)
C19 0.0431(16) 0.0226(11) 0.0300(13) 0.0128(10) 0.0108(11) 0.0169(11)
C20 0.0353(14) 0.0269(12) 0.0236(12) 0.0106(10) 0.0101(10) 0.0123(11)
C21 0.0437(17) 0.0366(14) 0.0230(12) 0.0125(11) 0.0089(11) 0.0128(13)
C22 0.0420(16) 0.0240(12) 0.0233(12) 0.0014(10) 0.0126(11) 0.0000(11)
C23 0.0300(14) 0.0197(11) 0.0337(14) 0.0021(10) 0.0146(11) 0.0043(10)
C24 0.0233(12) 0.0200(11) 0.0288(12) 0.0050(9) 0.0066(10) 0.0058(9)
_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 O1 2.1737(15) . ?
Pd1 N1 2.0164(18) . ?
Pd1 N2 2.0514(19) . ?
Pd1 C19 1.998(2) . ?
O1 C1 1.231(3) . ?
O2 C8 1.241(3) . ?
O3 C16 1.373(3) . ?
O3 C17 1.420(3) . ?
O4 C12 1.365(3) . ?
O4 C18 1.418(3) . ?
N1 C10 1.333(3) . ?
N1 C11 1.416(3) . ?
N2 C20 1.344(3) . ?
N2 C24 1.343(3) . ?
C1 C2 1.464(3) . ?
C1 C10 1.502(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.397(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(3) . ?
C7 C8 1.510(3) . ?
C8 C9 1.409(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(3) . ?
C11 C12 1.402(3) . ?
C11 C16 1.394(3) . ?
C12 C13 1.388(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.378(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.395(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C21 1.374(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.372(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(3) . ?
C24 H24 0.9500 . ?
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 O1 77.98(6) . . ?
N1 Pd1 N2 174.20(7) . . ?
N2 Pd1 O1 96.39(6) . . ?
C19 Pd1 O1 171.53(8) . . ?
C19 Pd1 N1 93.99(9) . . ?
C19 Pd1 N2 91.56(9) . . ?
C1 O1 Pd1 111.93(13) . . ?
C16 O3 C17 117.33(18) . . ?
C12 O4 C18 117.59(18) . . ?
C10 N1 Pd1 117.23(14) . . ?
C10 N1 C11 117.91(18) . . ?
C11 N1 Pd1 124.78(14) . . ?
C20 N2 Pd1 115.77(16) . . ?
C24 N2 Pd1 127.11(16) . . ?
C24 N2 C20 117.0(2) . . ?
O1 C1 C2 121.33(19) . . ?
O1 C1 C10 119.80(19) . . ?
C2 C1 C10 118.87(19) . . ?
C3 C2 C1 120.1(2) . . ?
C3 C2 C7 120.2(2) . . ?
C7 C2 C1 119.72(19) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.7(2) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.7(2) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(2) . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C8 120.78(19) . . ?
C6 C7 C2 119.2(2) . . ?
C6 C7 C8 120.1(2) . . ?
O2 C8 C7 118.5(2) . . ?
O2 C8 C9 124.1(2) . . ?
C9 C8 C7 117.4(2) . . ?
C8 C9 H9 117.9 . . ?
C10 C9 C8 124.3(2) . . ?
C10 C9 H9 117.9 . . ?
N1 C10 C1 112.96(19) . . ?
N1 C10 C9 128.2(2) . . ?
C9 C10 C1 118.82(19) . . ?
C12 C11 N1 119.5(2) . . ?
C16 C11 N1 121.66(19) . . ?
C16 C11 C12 118.66(19) . . ?
O4 C12 C11 114.45(19) . . ?
O4 C12 C13 124.7(2) . . ?
C13 C12 C11 120.9(2) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.0(2) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.7(2) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 118.9(2) . . ?
C16 C15 H15 120.5 . . ?
O3 C16 C11 115.20(19) . . ?
O3 C16 C15 124.1(2) . . ?
C11 C16 C15 120.7(2) . . ?
O3 C17 H17A 109.5 . . ?
O3 C17 H17B 109.5 . . ?
O3 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Pd1 C19 H19A 109.5 . . ?
Pd1 C19 H19B 109.5 . . ?
Pd1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 H20 118.4 . . ?
N2 C20 C21 123.3(2) . . ?
C21 C20 H20 118.4 . . ?
C20 C21 H21 120.5 . . ?
C20 C21 C22 119.0(2) . . ?
C22 C21 H21 120.5 . . ?
C21 C22 H22 121.0 . . ?
C23 C22 C21 118.0(2) . . ?
C23 C22 H22 121.0 . . ?
C22 C23 H23 120.1 . . ?
C22 C23 C24 119.8(2) . . ?
C24 C23 H23 120.1 . . ?
N2 C24 C23 122.8(2) . . ?
N2 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
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 O1 C1 C2 176.67(16) . . . . ?
Pd1 O1 C1 C10 -3.8(2) . . . . ?
Pd1 N1 C10 C1 -0.1(2) . . . . ?
Pd1 N1 C10 C9 178.62(18) . . . . ?
Pd1 N1 C11 C12 -76.0(2) . . . . ?
Pd1 N1 C11 C16 99.1(2) . . . . ?
Pd1 N2 C20 C21 173.0(2) . . . . ?
Pd1 N2 C24 C23 -173.31(18) . . . . ?
O1 C1 C2 C3 -3.2(3) . . . . ?
O1 C1 C2 C7 175.4(2) . . . . ?
O1 C1 C10 N1 2.8(3) . . . . ?
O1 C1 C10 C9 -176.1(2) . . . . ?
O2 C8 C9 C10 -179.8(2) . . . . ?
O4 C12 C13 C14 -179.5(2) . . . . ?
N1 C11 C12 O4 -5.4(3) . . . . ?
N1 C11 C12 C13 173.9(2) . . . . ?
N1 C11 C16 O3 4.8(3) . . . . ?
N1 C11 C16 C15 -174.2(2) . . . . ?
N2 C20 C21 C22 1.2(4) . . . . ?
C1 C2 C3 C4 179.2(2) . . . . ?
C1 C2 C7 C6 -177.3(2) . . . . ?
C1 C2 C7 C8 2.0(3) . . . . ?
C2 C1 C10 N1 -177.64(18) . . . . ?
C2 C1 C10 C9 3.5(3) . . . . ?
C2 C3 C4 C5 -2.0(4) . . . . ?
C2 C7 C8 O2 179.2(2) . . . . ?
C2 C7 C8 C9 1.0(3) . . . . ?
C3 C2 C7 C6 1.2(3) . . . . ?
C3 C2 C7 C8 -179.5(2) . . . . ?
C3 C4 C5 C6 1.5(4) . . . . ?
C4 C5 C6 C7 0.4(4) . . . . ?
C5 C6 C7 C2 -1.7(4) . . . . ?
C5 C6 C7 C8 178.9(2) . . . . ?
C6 C7 C8 O2 -1.5(3) . . . . ?
C6 C7 C8 C9 -179.7(2) . . . . ?
C7 C2 C3 C4 0.6(3) . . . . ?
C7 C8 C9 C10 -1.7(3) . . . . ?
C8 C9 C10 N1 -179.2(2) . . . . ?
C8 C9 C10 C1 -0.6(3) . . . . ?
C10 N1 C11 C12 100.4(2) . . . . ?
C10 N1 C11 C16 -84.5(3) . . . . ?
C10 C1 C2 C3 177.3(2) . . . . ?
C10 C1 C2 C7 -4.2(3) . . . . ?
C11 N1 C10 C1 -176.77(18) . . . . ?
C11 N1 C10 C9 1.9(3) . . . . ?
C11 C12 C13 C14 1.3(3) . . . . ?
C12 C11 C16 O3 -179.99(19) . . . . ?
C12 C11 C16 C15 1.0(3) . . . . ?
C12 C13 C14 C15 -0.9(3) . . . . ?
C13 C14 C15 C16 0.5(3) . . . . ?
C14 C15 C16 O3 -179.5(2) . . . . ?
C14 C15 C16 C11 -0.5(3) . . . . ?
C16 C11 C12 O4 179.36(19) . . . . ?
C16 C11 C12 C13 -1.4(3) . . . . ?
C17 O3 C16 C11 179.9(2) . . . . ?
C17 O3 C16 C15 -1.1(3) . . . . ?
C18 O4 C12 C11 178.93(19) . . . . ?
C18 O4 C12 C13 -0.3(3) . . . . ?
C20 N2 C24 C23 2.2(3) . . . . ?
C20 C21 C22 C23 1.5(4) . . . . ?
C21 C22 C23 C24 -2.3(4) . . . . ?
C22 C23 C24 N2 0.5(4) . . . . ?
C24 N2 C20 C21 -3.0(4) . . . . ?
_shelx_res_file
;
TITL mo_dm15330_0m in P-1
CELL 0.71073 8.3132 10.841 12.801 110.224 92.769 105.358
ZERR 2 0.0007 0.0009 0.0011 0.002 0.002 0.002
LATT 1
SFAC C H N O Pd
UNIT 48 44 4 8 2
L.S. 4
PLAN -5 0 0
SIZE 0.01 0.05 0.3
TEMP -143.15
BOND $H
fmap 2
MORE -1
ACTA 52
CONF
REM
REM
REM
WGHT 0.033300
FVAR 0.13735
PD1 5 0.144429 0.209466 0.479211 11.00000 0.02147 0.01659 =
0.01825 0.00747 0.00557 0.00750
O1 4 0.218910 0.040573 0.499855 11.00000 0.02926 0.02016 =
0.01767 0.00738 0.00550 0.01002
O2 4 0.326571 -0.294674 0.107293 11.00000 0.04060 0.02635 =
0.02264 0.00116 0.00774 0.01292
O3 4 0.425938 0.239673 0.236074 11.00000 0.01848 0.03297 =
0.02978 0.01893 0.00246 0.00265
O4 4 -0.144767 0.026012 0.222733 11.00000 0.01947 0.03224 =
0.02925 0.01631 0.00249 0.00375
N1 3 0.174776 0.103754 0.321252 11.00000 0.01915 0.01776 =
0.01567 0.00766 0.00091 0.00497
N2 3 0.126329 0.305638 0.645227 11.00000 0.02255 0.01832 =
0.02279 0.00756 0.00644 0.00539
C1 1 0.250605 -0.034288 0.411460 11.00000 0.01630 0.01642 =
0.01918 0.00692 0.00174 0.00299
C2 1 0.312153 -0.150345 0.407147 11.00000 0.01792 0.01782 =
0.02148 0.00819 0.00155 0.00426
C3 1 0.343986 -0.173982 0.505403 11.00000 0.02374 0.02120 =
0.02320 0.00993 0.00102 0.00528
AFIX 43
H3 2 0.327258 -0.114154 0.575492 11.00000 -1.20000
AFIX 0
C4 1 0.400177 -0.285207 0.500393 11.00000 0.02932 0.03032 =
0.03276 0.01955 0.00126 0.00887
AFIX 43
H4 2 0.425369 -0.300003 0.567469 11.00000 -1.20000
AFIX 0
C5 1 0.419402 -0.373905 0.398571 11.00000 0.02801 0.02405 =
0.04175 0.01563 0.00855 0.01308
AFIX 43
H5 2 0.455418 -0.451113 0.395429 11.00000 -1.20000
AFIX 0
C6 1 0.386759 -0.351930 0.300183 11.00000 0.02453 0.02240 =
0.03104 0.00813 0.00753 0.00827
AFIX 43
H6 2 0.399793 -0.414353 0.230131 11.00000 -1.20000
AFIX 0
C7 1 0.335133 -0.239030 0.303842 11.00000 0.01737 0.01911 =
0.02391 0.00660 0.00111 0.00468
C8 1 0.302614 -0.214019 0.196918 11.00000 0.01985 0.02143 =
0.01926 0.00443 0.00203 0.00429
C9 1 0.251167 -0.097320 0.206141 11.00000 0.02182 0.02072 =
0.01783 0.00628 0.00140 0.00463
AFIX 43
H9 2 0.233455 -0.079541 0.139528 11.00000 -1.20000
AFIX 0
C10 1 0.224941 -0.007555 0.305196 11.00000 0.01459 0.01897 =
0.01742 0.00756 -0.00004 0.00249
C11 1 0.138097 0.134945 0.225820 11.00000 0.02277 0.01794 =
0.01637 0.00700 0.00333 0.00783
C12 1 -0.030409 0.099728 0.176894 11.00000 0.02251 0.01980 =
0.01998 0.00678 0.00397 0.00697
C13 1 -0.071604 0.140258 0.090084 11.00000 0.02544 0.02455 =
0.02025 0.00705 -0.00038 0.00979
AFIX 43
H13 2 -0.186178 0.117750 0.058386 11.00000 -1.20000
AFIX 0
C14 1 0.056071 0.213620 0.050522 11.00000 0.03577 0.02374 =
0.01881 0.00980 0.00251 0.01189
AFIX 43
H14 2 0.028146 0.240283 -0.009629 11.00000 -1.20000
AFIX 0
C15 1 0.223899 0.249486 0.096094 11.00000 0.03111 0.02086 =
0.02036 0.01069 0.00710 0.00580
AFIX 43
H15 2 0.310136 0.300721 0.068093 11.00000 -1.20000
AFIX 0
C16 1 0.264374 0.209160 0.183851 11.00000 0.02188 0.01940 =
0.02102 0.00704 0.00197 0.00658
C17 1 0.559067 0.314887 0.196161 11.00000 0.02271 0.02989 =
0.04019 0.01850 0.00913 0.00518
AFIX 137
H17A 2 0.556758 0.263760 0.115971 11.00000 -1.50000
H17B 2 0.667515 0.327794 0.238565 11.00000 -1.50000
H17C 2 0.544827 0.405029 0.206395 11.00000 -1.50000
AFIX 0
C18 1 -0.318037 -0.011209 0.178765 11.00000 0.02014 0.03140 =
0.03626 0.01145 0.00292 0.00577
AFIX 137
H18A 2 -0.336522 -0.066519 0.097946 11.00000 -1.50000
H18B 2 -0.351187 0.072299 0.190459 11.00000 -1.50000
H18C 2 -0.386136 -0.065130 0.217505 11.00000 -1.50000
AFIX 0
C19 1 0.090565 0.358115 0.439146 11.00000 0.04309 0.02257 =
0.02995 0.01279 0.01078 0.01689
AFIX 137
H19A 2 0.138969 0.362469 0.371737 11.00000 -1.50000
H19B 2 0.138518 0.446784 0.501895 11.00000 -1.50000
H19C 2 -0.032212 0.338002 0.424154 11.00000 -1.50000
AFIX 0
C20 1 0.210172 0.273622 0.719654 11.00000 0.03530 0.02695 =
0.02364 0.01062 0.01007 0.01234
AFIX 43
H20 2 0.260958 0.202194 0.691561 11.00000 -1.20000
AFIX 0
C21 1 0.226075 0.339066 0.834344 11.00000 0.04368 0.03660 =
0.02299 0.01247 0.00888 0.01276
AFIX 43
H21 2 0.288379 0.314377 0.883961 11.00000 -1.20000
AFIX 0
C22 1 0.149735 0.441812 0.876639 11.00000 0.04200 0.02400 =
0.02329 0.00145 0.01265 -0.00001
AFIX 43
H22 2 0.160659 0.490442 0.955472 11.00000 -1.20000
AFIX 0
C23 1 0.058010 0.471040 0.801165 11.00000 0.02999 0.01968 =
0.03366 0.00214 0.01462 0.00425
AFIX 43
H23 2 0.000790 0.538412 0.827440 11.00000 -1.20000
AFIX 0
C24 1 0.049191 0.402544 0.687460 11.00000 0.02332 0.02003 =
0.02875 0.00496 0.00663 0.00584
AFIX 43
H24 2 -0.014200 0.424685 0.636522 11.00000 -1.20000
AFIX 0
HKLF 4
REM mo_dm15330_0m in P-1
REM R1 = 0.0352 for 5343 Fo > 4sig(Fo) and 0.0442 for all 6259 data
REM 283 parameters refined using 0 restraints
END
WGHT 0.0335 0.0000
REM Highest difference peak 0.642, deepest hole -0.729, 1-sigma level 0.098
Q1 1 0.0868 0.1775 0.4120 11.00000 0.05 0.64
Q2 1 0.0817 0.1664 0.5127 11.00000 0.05 0.59
Q3 1 0.2378 0.2041 0.4882 11.00000 0.05 0.55
Q4 1 0.0523 0.0990 0.1848 11.00000 0.05 0.55
Q5 1 0.0381 0.2064 0.4791 11.00000 0.05 0.54
;
_shelx_res_checksum 34328
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_d8v17280_0m
_database_code_depnum_ccdc_archive 'CCDC 1853302'
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_audit_creation_date 2017-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H30 N2 O2 Pd'
_chemical_formula_sum 'C28 H30 N2 O2 Pd'
_chemical_formula_weight 532.94
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 15.0290(8)
_cell_length_b 21.2571(8)
_cell_length_c 15.4985(7)
_cell_angle_alpha 90
_cell_angle_beta 94.786(2)
_cell_angle_gamma 90
_cell_volume 4934.1(4)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 4767
_cell_measurement_temperature 303(2)
_cell_measurement_theta_max 28.488
_cell_measurement_theta_min 2.326
_shelx_estimated_absorpt_T_max 0.940
_shelx_estimated_absorpt_T_min 0.912
_exptl_absorpt_coefficient_mu 0.779
_exptl_absorpt_correction_T_max 0.7460
_exptl_absorpt_correction_T_min 0.6126
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1045 before and 0.0471 after correction. The Ratio of minimum to maximum transmission is 0.8212. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.435
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2192
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0386
_diffrn_reflns_av_unetI/netI 0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 15181
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.052
_diffrn_reflns_theta_min 2.720
_diffrn_ambient_temperature 303.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4443
_reflns_number_total 7093
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.553
_refine_diff_density_min -0.565
_refine_diff_density_rms 0.083
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 303
_refine_ls_number_reflns 7093
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0930
_refine_ls_R_factor_gt 0.0470
_refine_ls_restrained_S_all 1.053
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+5.4379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0872
_refine_ls_wR_factor_ref 0.1075
_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:
C23(H23), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13), C14(H14),
C15(H15), C16(H16), C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,
H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.61385(2) 0.61113(2) 0.43079(2) 0.04225(9) Uani 1 1 d . . . . .
O1 O 0.56805(15) 0.51488(10) 0.40953(17) 0.0539(6) Uani 1 1 d . . . . .
O2 O 0.82277(18) 0.34838(11) 0.5132(2) 0.0774(9) Uani 1 1 d . . . . .
N1 N 0.72178(17) 0.56078(11) 0.47846(17) 0.0393(6) Uani 1 1 d . . . . .
N2 N 0.49637(19) 0.65201(12) 0.38075(18) 0.0475(7) Uani 1 1 d . . . . .
C1 C 0.7146(2) 0.49836(14) 0.4724(2) 0.0391(7) Uani 1 1 d . . . . .
C2 C 0.6265(2) 0.47605(14) 0.4323(2) 0.0400(7) Uani 1 1 d . . . . .
C3 C 0.6105(2) 0.40872(15) 0.4200(2) 0.0416(7) Uani 1 1 d . . . . .
C4 C 0.5291(3) 0.38716(16) 0.3820(2) 0.0555(9) Uani 1 1 d . . . . .
H4 H 0.484018 0.415730 0.365272 0.067 Uiso 1 1 calc R . . . .
C5 C 0.5147(3) 0.32374(17) 0.3689(3) 0.0676(12) Uani 1 1 d . . . . .
H5 H 0.460237 0.309494 0.343393 0.081 Uiso 1 1 calc R . . . .
C6 C 0.5812(3) 0.28175(18) 0.3937(3) 0.0720(12) Uani 1 1 d . . . . .
H6 H 0.571489 0.238952 0.384733 0.086 Uiso 1 1 calc R . . . .
C7 C 0.6620(3) 0.30214(16) 0.4316(3) 0.0624(11) Uani 1 1 d . . . . .
H7 H 0.706432 0.273008 0.447716 0.075 Uiso 1 1 calc R . . . .
C8 C 0.6779(2) 0.36563(15) 0.4461(2) 0.0439(8) Uani 1 1 d . . . . .
C9 C 0.7648(2) 0.38781(15) 0.4886(3) 0.0512(9) Uani 1 1 d . . . . .
C10 C 0.7780(2) 0.45363(15) 0.4993(2) 0.0484(8) Uani 1 1 d . . . . .
H10 H 0.832292 0.467455 0.525923 0.058 Uiso 1 1 calc R . . . .
C11 C 0.6714(3) 0.69473(15) 0.4531(3) 0.0728(13) Uani 1 1 d . . . . .
H11A H 0.734292 0.689123 0.467131 0.109 Uiso 1 1 calc GR . . . .
H11B H 0.645674 0.714805 0.500671 0.109 Uiso 1 1 calc GR . . . .
H11C H 0.661804 0.720503 0.402341 0.109 Uiso 1 1 calc GR . . . .
C12 C 0.4355(3) 0.61520(17) 0.3412(3) 0.0698(12) Uani 1 1 d . . . . .
H12 H 0.449396 0.572827 0.335690 0.084 Uiso 1 1 calc R . . . .
C13 C 0.3530(3) 0.63513(19) 0.3075(3) 0.0717(12) Uani 1 1 d . . . . .
H13 H 0.313368 0.606908 0.279130 0.086 Uiso 1 1 calc R . . . .
C14 C 0.3302(3) 0.69517(19) 0.3158(3) 0.0783(14) Uani 1 1 d . . . . .
H14 H 0.275970 0.710413 0.290899 0.094 Uiso 1 1 calc R . . . .
C15 C 0.3885(4) 0.7330(2) 0.3614(4) 0.124(2) Uani 1 1 d . . . . .
H15 H 0.372941 0.774422 0.372556 0.148 Uiso 1 1 calc R . . . .
C16 C 0.4709(3) 0.71045(18) 0.3915(4) 0.0959(18) Uani 1 1 d . . . . .
H16 H 0.510852 0.737942 0.421046 0.115 Uiso 1 1 calc R . . . .
C17 C 0.8046(2) 0.58494(14) 0.5181(2) 0.0428(8) Uani 1 1 d . . . . .
C18 C 0.8109(3) 0.59970(16) 0.6060(2) 0.0526(9) Uani 1 1 d . . . . .
C19 C 0.8926(3) 0.61941(18) 0.6443(3) 0.0705(12) Uani 1 1 d . . . . .
H19 H 0.898600 0.628304 0.703294 0.085 Uiso 1 1 calc R . . . .
C20 C 0.9651(3) 0.62603(19) 0.5966(4) 0.0769(14) Uani 1 1 d . . . . .
H20 H 1.019830 0.638508 0.623642 0.092 Uiso 1 1 calc R . . . .
C21 C 0.9572(3) 0.61440(17) 0.5096(4) 0.0703(12) Uani 1 1 d . . . . .
H21 H 1.006138 0.620580 0.477604 0.084 Uiso 1 1 calc R . . . .
C22 C 0.8770(2) 0.59341(16) 0.4684(3) 0.0543(9) Uani 1 1 d . . . . .
C23 C 0.8715(3) 0.5805(2) 0.3730(3) 0.0716(12) Uani 1 1 d . . . . .
H23 H 0.810833 0.565462 0.356223 0.086 Uiso 1 1 calc R . . . .
C24 C 0.8854(4) 0.6398(3) 0.3202(4) 0.1127(19) Uani 1 1 d . . . . .
H24A H 0.844716 0.671908 0.335715 0.169 Uiso 1 1 calc GR . . . .
H24B H 0.874664 0.630486 0.259613 0.169 Uiso 1 1 calc GR . . . .
H24C H 0.945661 0.654405 0.332053 0.169 Uiso 1 1 calc GR . . . .
C25 C 0.9358(4) 0.5287(3) 0.3494(4) 0.122(2) Uani 1 1 d . . . . .
H25A H 0.930014 0.522187 0.287861 0.183 Uiso 1 1 calc GR . . . .
H25B H 0.921884 0.490342 0.378098 0.183 Uiso 1 1 calc GR . . . .
H25C H 0.996003 0.540970 0.367371 0.183 Uiso 1 1 calc GR . . . .
C26 C 0.7295(3) 0.59571(19) 0.6579(3) 0.0656(11) Uani 1 1 d . . . . .
H26 H 0.676788 0.597492 0.616277 0.079 Uiso 1 1 calc R . . . .
C27 C 0.7219(3) 0.6500(2) 0.7202(3) 0.0935(16) Uani 1 1 d . . . . .
H27A H 0.769703 0.647740 0.765225 0.140 Uiso 1 1 calc GR . . . .
H27B H 0.665720 0.647702 0.745203 0.140 Uiso 1 1 calc GR . . . .
H27C H 0.725613 0.689062 0.689519 0.140 Uiso 1 1 calc GR . . . .
C28 C 0.7248(4) 0.5343(2) 0.7060(4) 0.119(2) Uani 1 1 d . . . . .
H28A H 0.728110 0.499965 0.666157 0.178 Uiso 1 1 calc GR . . . .
H28B H 0.669505 0.532089 0.732710 0.178 Uiso 1 1 calc GR . . . .
H28C H 0.773800 0.531738 0.749746 0.178 Uiso 1 1 calc GR . . . .
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 0.03466(15) 0.03379(13) 0.05697(17) 0.00017(12) -0.00405(11) 0.00038(11)
O1 0.0372(14) 0.0358(11) 0.0855(18) -0.0019(12) -0.0136(13) 0.0021(10)
O2 0.0469(17) 0.0426(14) 0.138(3) 0.0095(16) -0.0192(17) 0.0075(12)
N1 0.0294(14) 0.0355(13) 0.0519(16) 0.0008(12) -0.0031(12) -0.0002(11)
N2 0.0422(17) 0.0365(14) 0.0621(18) 0.0030(13) -0.0056(14) 0.0045(12)
C1 0.0335(18) 0.0373(16) 0.0463(18) -0.0002(14) 0.0024(14) -0.0010(13)
C2 0.0343(19) 0.0378(16) 0.0476(18) -0.0024(14) 0.0016(15) -0.0027(13)
C3 0.0368(19) 0.0375(15) 0.0499(19) -0.0015(14) 0.0010(15) -0.0039(14)
C4 0.044(2) 0.0487(19) 0.072(2) -0.0001(19) -0.0105(18) -0.0056(17)
C5 0.056(3) 0.049(2) 0.093(3) -0.001(2) -0.018(2) -0.0139(19)
C6 0.073(3) 0.0416(19) 0.098(3) -0.002(2) -0.017(3) -0.011(2)
C7 0.064(3) 0.0376(18) 0.083(3) 0.0040(19) -0.010(2) 0.0008(18)
C8 0.038(2) 0.0374(15) 0.056(2) 0.0043(15) -0.0002(16) -0.0015(14)
C9 0.041(2) 0.0402(17) 0.072(2) 0.0061(18) 0.0003(18) 0.0015(16)
C10 0.0338(19) 0.0429(17) 0.067(2) -0.0007(17) -0.0076(17) -0.0002(14)
C11 0.052(3) 0.0353(17) 0.126(4) 0.006(2) -0.024(2) -0.0066(17)
C12 0.053(3) 0.0439(19) 0.107(3) -0.006(2) -0.024(2) 0.0054(18)
C13 0.056(3) 0.056(2) 0.097(3) 0.000(2) -0.026(2) 0.001(2)
C14 0.054(3) 0.061(2) 0.113(4) 0.013(3) -0.028(3) 0.008(2)
C15 0.076(4) 0.051(2) 0.233(7) -0.003(4) -0.051(4) 0.012(2)
C16 0.067(3) 0.044(2) 0.168(5) -0.004(3) -0.042(3) 0.003(2)
C17 0.0308(18) 0.0328(15) 0.064(2) 0.0054(15) -0.0045(16) -0.0027(13)
C18 0.046(2) 0.0465(19) 0.063(2) -0.0005(17) -0.0118(18) -0.0038(16)
C19 0.057(3) 0.064(3) 0.085(3) -0.008(2) -0.026(2) -0.005(2)
C20 0.041(3) 0.061(2) 0.123(4) -0.003(3) -0.026(3) -0.0098(19)
C21 0.037(2) 0.055(2) 0.119(4) 0.008(3) 0.007(2) -0.0072(18)
C22 0.035(2) 0.0445(18) 0.083(3) 0.0009(19) 0.0016(19) -0.0025(15)
C23 0.044(2) 0.088(3) 0.085(3) 0.004(3) 0.020(2) -0.004(2)
C24 0.106(5) 0.125(5) 0.107(4) 0.033(4) 0.006(4) -0.005(4)
C25 0.127(5) 0.132(5) 0.115(5) 0.001(4) 0.054(4) 0.043(4)
C26 0.065(3) 0.075(3) 0.055(2) -0.007(2) -0.009(2) -0.011(2)
C27 0.098(4) 0.095(4) 0.088(3) -0.023(3) 0.008(3) 0.004(3)
C28 0.170(6) 0.079(3) 0.115(5) 0.007(3) 0.062(4) -0.008(4)
_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 O1 2.175(2) . ?
Pd1 N1 2.030(2) . ?
Pd1 N2 2.060(3) . ?
Pd1 C11 1.994(3) . ?
O1 C2 1.235(4) . ?
O2 C9 1.245(4) . ?
N1 C1 1.334(4) . ?
N1 C17 1.436(4) . ?
N2 C12 1.315(4) . ?
N2 C16 1.314(5) . ?
C1 C2 1.493(4) . ?
C1 C10 1.386(4) . ?
C2 C3 1.461(4) . ?
C3 C4 1.391(5) . ?
C3 C8 1.400(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.370(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.374(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.386(4) . ?
C8 C9 1.490(5) . ?
C9 C10 1.421(4) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12 0.9300 . ?
C12 C13 1.372(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.330(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.346(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.374(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.394(5) . ?
C17 C22 1.396(5) . ?
C18 C19 1.385(5) . ?
C18 C26 1.521(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.374(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.365(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.390(5) . ?
C22 C23 1.501(6) . ?
C23 H23 0.9800 . ?
C23 C24 1.527(6) . ?
C23 C25 1.531(6) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26 0.9800 . ?
C26 C27 1.515(6) . ?
C26 C28 1.508(6) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
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 O1 78.02(9) . . ?
N1 Pd1 N2 173.10(10) . . ?
N2 Pd1 O1 95.12(10) . . ?
C11 Pd1 O1 172.70(13) . . ?
C11 Pd1 N1 94.88(13) . . ?
C11 Pd1 N2 92.00(13) . . ?
C2 O1 Pd1 112.1(2) . . ?
C1 N1 Pd1 116.2(2) . . ?
C1 N1 C17 116.6(3) . . ?
C17 N1 Pd1 127.21(19) . . ?
C12 N2 Pd1 117.7(2) . . ?
C16 N2 Pd1 126.9(3) . . ?
C16 N2 C12 115.0(3) . . ?
N1 C1 C2 114.1(3) . . ?
N1 C1 C10 127.7(3) . . ?
C10 C1 C2 118.1(3) . . ?
O1 C2 C1 119.4(3) . . ?
O1 C2 C3 120.8(3) . . ?
C3 C2 C1 119.8(3) . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 C8 119.8(3) . . ?
C8 C3 C2 119.7(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.8(4) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.7(4) . . ?
C8 C7 H7 119.6 . . ?
C3 C8 C9 120.5(3) . . ?
C7 C8 C3 118.6(3) . . ?
C7 C8 C9 120.9(3) . . ?
O2 C9 C8 119.2(3) . . ?
O2 C9 C10 122.7(3) . . ?
C10 C9 C8 118.2(3) . . ?
C1 C10 C9 123.7(3) . . ?
C1 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
Pd1 C11 H11A 109.5 . . ?
Pd1 C11 H11B 109.5 . . ?
Pd1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12 117.8 . . ?
N2 C12 C13 124.4(3) . . ?
C13 C12 H12 117.8 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 H14 121.2 . . ?
C13 C14 C15 117.5(4) . . ?
C15 C14 H14 121.2 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.9(4) . . ?
C16 C15 H15 120.1 . . ?
N2 C16 C15 123.4(4) . . ?
N2 C16 H16 118.3 . . ?
C15 C16 H16 118.3 . . ?
C18 C17 N1 119.0(3) . . ?
C18 C17 C22 121.2(3) . . ?
C22 C17 N1 119.9(3) . . ?
C17 C18 C26 120.8(3) . . ?
C19 C18 C17 118.2(4) . . ?
C19 C18 C26 120.9(4) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 121.0(4) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.4(4) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.8(4) . . ?
C22 C21 H21 119.6 . . ?
C17 C22 C23 122.6(3) . . ?
C21 C22 C17 118.3(4) . . ?
C21 C22 C23 119.1(4) . . ?
C22 C23 H23 107.1 . . ?
C22 C23 C24 112.2(4) . . ?
C22 C23 C25 112.5(4) . . ?
C24 C23 H23 107.1 . . ?
C24 C23 C25 110.4(4) . . ?
C25 C23 H23 107.1 . . ?
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 . . ?
C18 C26 H26 106.9 . . ?
C27 C26 C18 113.6(4) . . ?
C27 C26 H26 106.9 . . ?
C28 C26 C18 112.5(4) . . ?
C28 C26 H26 106.9 . . ?
C28 C26 C27 109.7(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
_shelx_res_file
;
TITL mo_d8v17280_0m_a.res in C2/c
mo_d8v17280_0m.res
created by SHELXL-2017/1 at 11:34:41 on 23-Aug-2017
REM Old TITL mo_d8v17280_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.146, Rweak 0.004, Alpha 0.063, Orientation as input
REM Formula found by SHELXT: C28 N O3 Pd
CELL 0.71073 15.029 21.2571 15.4985 90 94.786 90
ZERR 8 0.0008 0.0008 0.0007 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N O Pd
UNIT 224 240 16 16 8
L.S. 4
PLAN 20
SIZE 0.08 0.1 0.12
TEMP 29.87
BOND $H
list 4
fmap 2
ACTA
OMIT 1 1 0
OMIT 0 2 0
OMIT 0 2 1
OMIT 1 1 1
OMIT -1 7 2
OMIT 15 1 4
OMIT 7 3 3
REM
REM
REM
WGHT 0.029200 5.437900
FVAR 0.27942
PD1 5 0.613851 0.611128 0.430788 11.00000 0.03466 0.03379 =
0.05697 0.00017 -0.00405 0.00038
O1 4 0.568050 0.514878 0.409532 11.00000 0.03722 0.03582 =
0.08547 -0.00185 -0.01363 0.00208
O2 4 0.822773 0.348375 0.513155 11.00000 0.04686 0.04262 =
0.13809 0.00954 -0.01924 0.00748
N1 3 0.721784 0.560784 0.478459 11.00000 0.02941 0.03546 =
0.05190 0.00085 -0.00312 -0.00020
N2 3 0.496371 0.652008 0.380750 11.00000 0.04221 0.03650 =
0.06215 0.00299 -0.00560 0.00447
C1 1 0.714615 0.498364 0.472408 11.00000 0.03355 0.03733 =
0.04633 -0.00015 0.00238 -0.00102
C2 1 0.626511 0.476048 0.432262 11.00000 0.03428 0.03783 =
0.04762 -0.00242 0.00157 -0.00272
C3 1 0.610457 0.408716 0.420018 11.00000 0.03678 0.03752 =
0.04993 -0.00149 0.00098 -0.00395
C4 1 0.529058 0.387159 0.381983 11.00000 0.04353 0.04873 =
0.07161 -0.00009 -0.01055 -0.00556
AFIX 43
H4 2 0.484018 0.415730 0.365272 11.00000 -1.20000
AFIX 0
C5 1 0.514736 0.323740 0.368908 11.00000 0.05636 0.04920 =
0.09323 -0.00071 -0.01845 -0.01389
AFIX 43
H5 2 0.460237 0.309494 0.343393 11.00000 -1.20000
AFIX 0
C6 1 0.581178 0.281754 0.393681 11.00000 0.07291 0.04159 =
0.09751 -0.00239 -0.01736 -0.01064
AFIX 43
H6 2 0.571489 0.238952 0.384733 11.00000 -1.20000
AFIX 0
C7 1 0.661961 0.302145 0.431590 11.00000 0.06361 0.03764 =
0.08343 0.00399 -0.00966 0.00076
AFIX 43
H7 2 0.706432 0.273008 0.447716 11.00000 -1.20000
AFIX 0
C8 1 0.677911 0.365630 0.446063 11.00000 0.03774 0.03735 =
0.05607 0.00427 -0.00015 -0.00146
C9 1 0.764828 0.387813 0.488570 11.00000 0.04082 0.04020 =
0.07174 0.00610 0.00026 0.00149
C10 1 0.778045 0.453626 0.499329 11.00000 0.03378 0.04292 =
0.06657 -0.00069 -0.00764 -0.00016
AFIX 43
H10 2 0.832292 0.467455 0.525923 11.00000 -1.20000
AFIX 0
C11 1 0.671359 0.694726 0.453129 11.00000 0.05167 0.03528 =
0.12607 0.00639 -0.02366 -0.00658
AFIX 137
H11A 2 0.734292 0.689123 0.467131 11.00000 -1.50000
H11B 2 0.645674 0.714805 0.500671 11.00000 -1.50000
H11C 2 0.661804 0.720503 0.402341 11.00000 -1.50000
AFIX 0
C12 1 0.435538 0.615200 0.341190 11.00000 0.05349 0.04389 =
0.10685 -0.00602 -0.02417 0.00539
AFIX 43
H12 2 0.449396 0.572827 0.335690 11.00000 -1.20000
AFIX 0
C13 1 0.353025 0.635134 0.307505 11.00000 0.05639 0.05581 =
0.09734 -0.00050 -0.02609 0.00149
AFIX 43
H13 2 0.313368 0.606908 0.279130 11.00000 -1.20000
AFIX 0
C14 1 0.330186 0.695171 0.315751 11.00000 0.05443 0.06125 =
0.11328 0.01296 -0.02766 0.00848
AFIX 43
H14 2 0.275970 0.710413 0.290899 11.00000 -1.20000
AFIX 0
C15 1 0.388474 0.733039 0.361410 11.00000 0.07622 0.05071 =
0.23339 -0.00265 -0.05120 0.01183
AFIX 43
H15 2 0.372941 0.774422 0.372556 11.00000 -1.20000
AFIX 0
C16 1 0.470945 0.710451 0.391516 11.00000 0.06656 0.04421 =
0.16812 -0.00382 -0.04209 0.00321
AFIX 43
H16 2 0.510852 0.737942 0.421046 11.00000 -1.20000
AFIX 0
C17 1 0.804573 0.584935 0.518091 11.00000 0.03075 0.03279 =
0.06356 0.00539 -0.00453 -0.00270
C18 1 0.810855 0.599696 0.606014 11.00000 0.04601 0.04647 =
0.06257 -0.00046 -0.01177 -0.00384
C19 1 0.892630 0.619410 0.644342 11.00000 0.05699 0.06402 =
0.08527 -0.00766 -0.02563 -0.00473
AFIX 43
H19 2 0.898600 0.628304 0.703294 11.00000 -1.20000
AFIX 0
C20 1 0.965111 0.626032 0.596586 11.00000 0.04093 0.06079 =
0.12335 -0.00325 -0.02591 -0.00977
AFIX 43
H20 2 1.019830 0.638508 0.623642 11.00000 -1.20000
AFIX 0
C21 1 0.957237 0.614397 0.509646 11.00000 0.03678 0.05521 =
0.11881 0.00840 0.00670 -0.00720
AFIX 43
H21 2 1.006138 0.620580 0.477604 11.00000 -1.20000
AFIX 0
C22 1 0.876968 0.593413 0.468445 11.00000 0.03477 0.04454 =
0.08315 0.00090 0.00159 -0.00247
C23 1 0.871462 0.580510 0.372952 11.00000 0.04371 0.08846 =
0.08511 0.00371 0.01952 -0.00375
AFIX 13
H23 2 0.810833 0.565462 0.356223 11.00000 -1.20000
AFIX 0
C24 1 0.885422 0.639834 0.320185 11.00000 0.10642 0.12454 =
0.10678 0.03297 0.00596 -0.00455
AFIX 137
H24A 2 0.844716 0.671908 0.335715 11.00000 -1.50000
H24B 2 0.874664 0.630486 0.259613 11.00000 -1.50000
H24C 2 0.945661 0.654405 0.332053 11.00000 -1.50000
AFIX 0
C25 1 0.935842 0.528670 0.349373 11.00000 0.12697 0.13210 =
0.11500 0.00134 0.05372 0.04299
AFIX 137
H25A 2 0.930014 0.522187 0.287861 11.00000 -1.50000
H25B 2 0.921884 0.490342 0.378098 11.00000 -1.50000
H25C 2 0.996003 0.540970 0.367371 11.00000 -1.50000
AFIX 0
C26 1 0.729494 0.595705 0.657934 11.00000 0.06452 0.07528 =
0.05469 -0.00738 -0.00850 -0.01088
AFIX 13
H26 2 0.676788 0.597492 0.616277 11.00000 -1.20000
AFIX 0
C27 1 0.721941 0.650027 0.720169 11.00000 0.09783 0.09497 =
0.08760 -0.02308 0.00803 0.00420
AFIX 137
H27A 2 0.769703 0.647740 0.765225 11.00000 -1.50000
H27B 2 0.665720 0.647702 0.745203 11.00000 -1.50000
H27C 2 0.725613 0.689062 0.689519 11.00000 -1.50000
AFIX 0
C28 1 0.724801 0.534299 0.706001 11.00000 0.17026 0.07897 =
0.11548 0.00656 0.06220 -0.00805
AFIX 137
H28A 2 0.728110 0.499965 0.666157 11.00000 -1.50000
H28B 2 0.669505 0.532089 0.732710 11.00000 -1.50000
H28C 2 0.773800 0.531738 0.749746 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_d8v17280_0m_a.res in C2/c
REM R1 = 0.0470 for 4443 Fo > 4sig(Fo) and 0.0930 for all 7093 data
REM 303 parameters refined using 0 restraints
END
WGHT 0.0289 5.4958
REM Highest difference peak 0.553, deepest hole -0.565, 1-sigma level 0.083
Q1 1 0.4216 0.7356 0.2882 11.00000 0.05 0.55
Q2 1 0.5039 0.7078 0.3313 11.00000 0.05 0.47
Q3 1 0.8424 0.6111 0.7904 11.00000 0.05 0.40
Q4 1 0.5184 0.4984 0.3505 11.00000 0.05 0.31
Q5 1 0.6250 0.2935 0.4020 11.00000 0.05 0.31
Q6 1 0.6799 0.4903 0.4510 11.00000 0.05 0.30
Q7 1 0.5169 0.7398 0.4539 11.00000 0.05 0.29
Q8 1 0.4993 0.5389 0.4594 11.00000 0.05 0.29
Q9 1 1.0217 0.6097 0.4328 11.00000 0.05 0.28
Q10 1 0.5811 0.3999 0.3882 11.00000 0.05 0.28
Q11 1 0.8379 0.3103 0.5399 11.00000 0.05 0.28
Q12 1 0.7845 0.5414 0.7381 11.00000 0.05 0.28
Q13 1 0.7675 0.2972 0.5182 11.00000 0.05 0.27
Q14 1 0.6824 0.5723 0.4759 11.00000 0.05 0.27
Q15 1 1.0965 0.6058 0.6771 11.00000 0.05 0.27
Q16 1 0.9236 0.5889 0.7222 11.00000 0.05 0.27
Q17 1 0.8431 0.6173 0.4941 11.00000 0.05 0.26
Q18 1 1.0210 0.6115 0.4915 11.00000 0.05 0.26
Q19 1 0.4369 0.5583 0.4531 11.00000 0.05 0.26
Q20 1 0.6244 0.5720 0.5006 11.00000 0.05 0.26
;
_shelx_res_checksum 81019
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_d8v17018_0m
_database_code_depnum_ccdc_archive 'CCDC 1853323'
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_audit_creation_date 2017-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C49 H40 N2 O2 Pd'
_chemical_formula_sum 'C49 H40 N2 O2 Pd'
_chemical_formula_weight 795.23
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.4912(4)
_cell_length_b 13.4734(6)
_cell_length_c 14.7253(6)
_cell_angle_alpha 94.369(2)
_cell_angle_beta 109.580(2)
_cell_angle_gamma 90.382(2)
_cell_volume 1954.24(14)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9856
_cell_measurement_temperature 300(2)
_cell_measurement_theta_max 30.45
_cell_measurement_theta_min 2.517
_shelx_estimated_absorpt_T_max 0.926
_shelx_estimated_absorpt_T_min 0.895
_exptl_absorpt_coefficient_mu 0.517
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.6296
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1250 before and 0.0612 after correction. The Ratio of minimum to maximum transmission is 0.8439. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.351
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 820
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0429
_diffrn_reflns_av_unetI/netI 0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 22183
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.499
_diffrn_reflns_theta_min 2.614
_diffrn_ambient_temperature 300.11
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6233
_reflns_number_total 7103
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.502
_refine_diff_density_min -0.571
_refine_diff_density_rms 0.083
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.142
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 489
_refine_ls_number_reflns 7103
_refine_ls_number_restraints 38
_refine_ls_R_factor_all 0.0657
_refine_ls_R_factor_gt 0.0563
_refine_ls_restrained_S_all 1.169
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+5.5626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1181
_refine_ls_wR_factor_ref 0.1233
_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. Rigid bond restraints
C2, N1
with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
C20, C21
with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
C18(H18), C32(H32)
4.b Aromatic/amide H refined with riding coordinates:
C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C16(H16), C20(H20),
C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
C49(H49)
4.c Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C31(H31A,H31B,H31C)
;
_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
Pd01 Pd 0.77491(3) 0.61419(3) 0.30884(3) 0.03428(12) Uani 1 1 d . . . . .
O1 O 0.6018(3) 0.5117(2) 0.2718(3) 0.0453(8) Uani 1 1 d . . . . .
O2 O 0.1367(4) 0.7010(3) 0.1653(3) 0.0788(13) Uani 1 1 d . . . . .
N1 N 0.6200(3) 0.7075(2) 0.2748(2) 0.0299(7) Uani 1 1 d . U . . .
N2 N 0.9160(4) 0.5050(3) 0.3377(3) 0.0438(10) Uani 1 1 d . . . . .
C1 C 0.9197(4) 0.7215(4) 0.3389(4) 0.0472(12) Uani 1 1 d . . . . .
H1A H 0.967507 0.713058 0.293624 0.071 Uiso 1 1 calc GR . . . .
H1B H 0.981827 0.717340 0.403308 0.071 Uiso 1 1 calc GR . . . .
H1C H 0.879229 0.785404 0.334141 0.071 Uiso 1 1 calc GR . . . .
C2 C 0.4903(4) 0.6614(3) 0.2443(3) 0.0319(9) Uani 1 1 d . U . . .
C3 C 0.3724(4) 0.7113(4) 0.2194(3) 0.0393(11) Uani 1 1 d . . . . .
H3 H 0.375390 0.780595 0.225893 0.047 Uiso 1 1 calc R . . . .
C4 C 0.2455(5) 0.6591(4) 0.1838(4) 0.0481(12) Uani 1 1 d . . . . .
C5 C 0.2451(5) 0.5483(4) 0.1676(4) 0.0473(12) Uani 1 1 d . . . . .
C6 C 0.1249(6) 0.4941(5) 0.1197(4) 0.0672(17) Uani 1 1 d . . . . .
H6 H 0.043765 0.526823 0.097625 0.081 Uiso 1 1 calc R . . . .
C7 C 0.1261(7) 0.3919(5) 0.1051(5) 0.083(2) Uani 1 1 d . . . . .
H7 H 0.045881 0.356180 0.071324 0.100 Uiso 1 1 calc R . . . .
C8 C 0.2442(7) 0.3423(5) 0.1397(5) 0.081(2) Uani 1 1 d . . . . .
H8 H 0.243084 0.273181 0.131263 0.097 Uiso 1 1 calc R . . . .
C9 C 0.3638(6) 0.3945(4) 0.1866(5) 0.0628(16) Uani 1 1 d . . . . .
H9 H 0.443953 0.360876 0.209830 0.075 Uiso 1 1 calc R . . . .
C10 C 0.3647(5) 0.4974(4) 0.1993(4) 0.0433(11) Uani 1 1 d . . . . .
C11 C 0.4919(4) 0.5580(4) 0.2416(3) 0.0390(11) Uani 1 1 d . . . . .
C12 C 0.6290(4) 0.8126(3) 0.2756(3) 0.0275(9) Uani 1 1 d . . . . .
C13 C 0.6464(4) 0.8718(3) 0.3616(3) 0.0291(9) Uani 1 1 d . . . . .
C14 C 0.6469(4) 0.9746(3) 0.3594(3) 0.0354(10) Uani 1 1 d . . . . .
H14 H 0.655476 1.014236 0.415806 0.043 Uiso 1 1 calc R . . . .
C15 C 0.6350(4) 1.0199(3) 0.2759(3) 0.0362(10) Uani 1 1 d . . . . .
C16 C 0.6298(4) 0.9597(3) 0.1941(3) 0.0356(10) Uani 1 1 d . . . . .
H16 H 0.628232 0.989315 0.138686 0.043 Uiso 1 1 calc R . . . .
C17 C 0.6268(4) 0.8564(3) 0.1921(3) 0.0306(9) Uani 1 1 d . . . . .
C18 C 0.6261(5) 0.7895(3) 0.1033(3) 0.0364(10) Uani 1 1 d . . . . .
H18 H 0.672056 0.729125 0.128105 0.044 Uiso 1 1 calc R . . . .
C19 C 0.4852(5) 0.7548(4) 0.0358(3) 0.0490(13) Uani 1 1 d . . . . .
C20 C 0.3775(6) 0.8163(5) 0.0154(4) 0.0639(15) Uani 1 1 d . U . . .
H20 H 0.388563 0.880578 0.045341 0.077 Uiso 1 1 calc R . . . .
C21 C 0.2505(7) 0.7831(7) -0.0506(5) 0.088(2) Uani 1 1 d . U . . .
H21 H 0.176801 0.824328 -0.065299 0.106 Uiso 1 1 calc R . . . .
C22 C 0.2399(9) 0.6879(7) -0.0920(6) 0.101(2) Uani 1 1 d . U . . .
H22 H 0.156906 0.665436 -0.136666 0.121 Uiso 1 1 calc R . . . .
C23 C 0.3414(9) 0.6254(7) -0.0722(6) 0.104(3) Uani 1 1 d . U . . .
H23 H 0.328254 0.560541 -0.100847 0.125 Uiso 1 1 calc R . . . .
C24 C 0.4679(7) 0.6588(5) -0.0078(5) 0.0766(18) Uani 1 1 d . U . . .
H24 H 0.540429 0.616498 0.005716 0.092 Uiso 1 1 calc R . . . .
C25 C 0.7093(4) 0.8346(3) 0.0486(3) 0.0350(10) Uani 1 1 d . . . . .
C26 C 0.8475(5) 0.8194(4) 0.0765(3) 0.0439(11) Uani 1 1 d . . . . .
H26 H 0.887657 0.782069 0.128667 0.053 Uiso 1 1 calc R . . . .
C27 C 0.9263(5) 0.8583(4) 0.0285(4) 0.0534(14) Uani 1 1 d . . . . .
H27 H 1.018597 0.847036 0.048270 0.064 Uiso 1 1 calc R . . . .
C28 C 0.8691(6) 0.9132(4) -0.0477(4) 0.0577(15) Uani 1 1 d . . . . .
H28 H 0.922036 0.939719 -0.080160 0.069 Uiso 1 1 calc R . . . .
C29 C 0.7332(6) 0.9293(4) -0.0764(4) 0.0605(15) Uani 1 1 d . . . . .
H29 H 0.693666 0.966685 -0.128656 0.073 Uiso 1 1 calc R . . . .
C30 C 0.6544(5) 0.8903(4) -0.0282(4) 0.0481(12) Uani 1 1 d . . . . .
H30 H 0.562306 0.902147 -0.048353 0.058 Uiso 1 1 calc R . . . .
C31 C 0.6343(6) 1.1318(4) 0.2752(4) 0.0589(15) Uani 1 1 d . . . . .
H31A H 0.678671 1.152071 0.231900 0.088 Uiso 1 1 calc GR . . . .
H31B H 0.681335 1.161578 0.339296 0.088 Uiso 1 1 calc GR . . . .
H31C H 0.542593 1.153044 0.254103 0.088 Uiso 1 1 calc GR . . . .
C32 C 0.6716(4) 0.8207(3) 0.4547(3) 0.0321(9) Uani 1 1 d . . . . .
H32 H 0.726978 0.763553 0.449859 0.038 Uiso 1 1 calc R . . . .
C33 C 0.5427(5) 0.7772(3) 0.4644(3) 0.0367(10) Uani 1 1 d . . . . .
C34 C 0.5421(6) 0.6827(4) 0.4948(4) 0.0612(15) Uani 1 1 d . . . . .
H34 H 0.620136 0.646044 0.509439 0.073 Uiso 1 1 calc R . . . .
C35 C 0.4248(7) 0.6426(5) 0.5035(5) 0.081(2) Uani 1 1 d . . . . .
H35 H 0.425591 0.579789 0.525874 0.097 Uiso 1 1 calc R . . . .
C36 C 0.3079(6) 0.6947(5) 0.4794(5) 0.0718(18) Uani 1 1 d . . . . .
H36 H 0.229218 0.666921 0.484091 0.086 Uiso 1 1 calc R . . . .
C37 C 0.3079(6) 0.7869(5) 0.4486(4) 0.0614(15) Uani 1 1 d . . . . .
H37 H 0.228977 0.822601 0.432523 0.074 Uiso 1 1 calc R . . . .
C38 C 0.4242(5) 0.8284(4) 0.4408(4) 0.0479(12) Uani 1 1 d . . . . .
H38 H 0.422535 0.891692 0.419369 0.057 Uiso 1 1 calc R . . . .
C39 C 0.7578(5) 0.8868(3) 0.5446(3) 0.0374(10) Uani 1 1 d . . . . .
C40 C 0.7102(6) 0.9238(4) 0.6159(4) 0.0539(13) Uani 1 1 d . . . . .
H40 H 0.622211 0.907890 0.612340 0.065 Uiso 1 1 calc R . . . .
C41 C 0.7944(8) 0.9857(5) 0.6942(4) 0.0766(19) Uani 1 1 d . . . . .
H41 H 0.761058 1.011981 0.741718 0.092 Uiso 1 1 calc R . . . .
C42 C 0.9239(8) 1.0075(5) 0.7014(4) 0.081(2) Uani 1 1 d . . . . .
H42 H 0.979591 1.047442 0.754322 0.098 Uiso 1 1 calc R . . . .
C43 C 0.9723(6) 0.9710(5) 0.6312(5) 0.0690(18) Uani 1 1 d . . . . .
H43 H 1.060997 0.986207 0.635866 0.083 Uiso 1 1 calc R . . . .
C44 C 0.8898(5) 0.9115(4) 0.5533(4) 0.0517(13) Uani 1 1 d . . . . .
H44 H 0.923622 0.887384 0.505308 0.062 Uiso 1 1 calc R . . . .
C45 C 0.8762(6) 0.4182(4) 0.3605(5) 0.0670(17) Uani 1 1 d . . . . .
H45 H 0.791154 0.412962 0.366738 0.080 Uiso 1 1 calc R . . . .
C46 C 0.9562(6) 0.3375(5) 0.3749(5) 0.0761(19) Uani 1 1 d . . . . .
H46 H 0.926441 0.278783 0.391863 0.091 Uiso 1 1 calc R . . . .
C47 C 1.0798(6) 0.3436(5) 0.3644(5) 0.0686(17) Uani 1 1 d . . . . .
H47 H 1.135245 0.289036 0.373438 0.082 Uiso 1 1 calc R . . . .
C48 C 1.1207(6) 0.4304(5) 0.3404(5) 0.0686(17) Uani 1 1 d . . . . .
H48 H 1.204889 0.436344 0.332865 0.082 Uiso 1 1 calc R . . . .
C49 C 1.0363(5) 0.5095(4) 0.3275(4) 0.0583(15) Uani 1 1 d . . . . .
H49 H 1.065117 0.568714 0.310804 0.070 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
Pd01 0.02824(18) 0.02997(19) 0.0441(2) 0.00507(14) 0.01108(14) 0.00285(13)
O1 0.0338(17) 0.0258(16) 0.073(2) 0.0021(15) 0.0150(16) -0.0018(13)
O2 0.032(2) 0.081(3) 0.114(4) 0.012(3) 0.011(2) 0.011(2)
N1 0.0306(16) 0.0234(17) 0.035(2) 0.0023(14) 0.0097(15) 0.0028(13)
N2 0.042(2) 0.041(2) 0.050(3) 0.0111(19) 0.0147(19) 0.0125(18)
C1 0.028(2) 0.041(3) 0.068(4) 0.006(2) 0.010(2) -0.001(2)
C2 0.0298(14) 0.0396(17) 0.0271(16) 0.0006(13) 0.0110(13) 0.0106(13)
C3 0.036(2) 0.037(3) 0.043(3) 0.002(2) 0.012(2) -0.003(2)
C4 0.031(2) 0.063(3) 0.048(3) 0.011(2) 0.010(2) 0.005(2)
C5 0.036(3) 0.057(3) 0.048(3) -0.006(2) 0.015(2) -0.011(2)
C6 0.043(3) 0.087(5) 0.065(4) -0.009(3) 0.013(3) -0.015(3)
C7 0.058(4) 0.085(5) 0.100(5) -0.034(4) 0.029(4) -0.039(4)
C8 0.073(4) 0.052(4) 0.119(6) -0.036(4) 0.045(4) -0.031(3)
C9 0.053(3) 0.045(3) 0.092(5) -0.014(3) 0.032(3) -0.015(3)
C10 0.041(3) 0.042(3) 0.047(3) -0.008(2) 0.018(2) -0.012(2)
C11 0.029(2) 0.057(3) 0.030(2) -0.001(2) 0.0101(18) -0.020(2)
C12 0.0224(19) 0.027(2) 0.032(2) 0.0027(17) 0.0070(16) 0.0016(16)
C13 0.025(2) 0.029(2) 0.033(2) 0.0050(17) 0.0093(17) -0.0012(17)
C14 0.040(2) 0.032(2) 0.032(2) -0.0040(19) 0.0090(19) 0.0033(19)
C15 0.039(2) 0.029(2) 0.040(3) 0.0046(19) 0.011(2) 0.0024(19)
C16 0.043(3) 0.032(2) 0.032(2) 0.0103(19) 0.011(2) 0.0021(19)
C17 0.028(2) 0.030(2) 0.032(2) -0.0002(18) 0.0072(17) 0.0012(17)
C18 0.045(3) 0.033(2) 0.032(2) 0.0011(19) 0.014(2) 0.002(2)
C19 0.054(3) 0.062(3) 0.034(3) -0.008(2) 0.021(2) -0.017(3)
C20 0.056(3) 0.084(3) 0.052(3) -0.001(3) 0.020(2) -0.004(3)
C21 0.065(3) 0.120(4) 0.083(4) 0.006(3) 0.030(3) -0.006(3)
C22 0.086(4) 0.123(5) 0.091(4) -0.005(4) 0.031(3) -0.028(4)
C23 0.109(4) 0.105(4) 0.095(4) -0.027(3) 0.037(4) -0.024(4)
C24 0.079(3) 0.079(4) 0.073(3) -0.020(3) 0.033(3) -0.019(3)
C25 0.039(2) 0.031(2) 0.033(2) -0.0041(18) 0.0119(19) 0.0019(19)
C26 0.045(3) 0.047(3) 0.033(3) -0.001(2) 0.005(2) 0.001(2)
C27 0.037(3) 0.061(3) 0.058(3) -0.011(3) 0.015(2) -0.012(2)
C28 0.065(4) 0.052(3) 0.065(4) -0.005(3) 0.037(3) -0.019(3)
C29 0.073(4) 0.059(4) 0.057(4) 0.020(3) 0.028(3) 0.006(3)
C30 0.046(3) 0.054(3) 0.050(3) 0.016(2) 0.021(2) 0.012(2)
C31 0.091(4) 0.031(3) 0.053(3) 0.002(2) 0.022(3) 0.003(3)
C32 0.033(2) 0.027(2) 0.036(2) 0.0045(18) 0.0109(18) 0.0022(18)
C33 0.042(3) 0.037(2) 0.030(2) -0.0001(19) 0.0112(19) -0.006(2)
C34 0.052(3) 0.055(3) 0.075(4) 0.023(3) 0.015(3) -0.006(3)
C35 0.074(4) 0.070(4) 0.097(5) 0.031(4) 0.023(4) -0.022(4)
C36 0.051(4) 0.090(5) 0.077(4) 0.012(4) 0.025(3) -0.022(3)
C37 0.047(3) 0.079(4) 0.062(4) 0.000(3) 0.024(3) -0.001(3)
C38 0.045(3) 0.050(3) 0.054(3) 0.006(2) 0.023(2) 0.001(2)
C39 0.041(2) 0.032(2) 0.035(3) 0.0088(19) 0.005(2) 0.000(2)
C40 0.064(3) 0.061(3) 0.036(3) 0.002(2) 0.017(3) -0.007(3)
C41 0.104(5) 0.086(5) 0.037(3) -0.008(3) 0.023(3) -0.014(4)
C42 0.099(5) 0.086(5) 0.038(3) -0.003(3) -0.003(3) -0.030(4)
C43 0.052(3) 0.076(4) 0.062(4) 0.013(3) -0.004(3) -0.021(3)
C44 0.050(3) 0.051(3) 0.049(3) 0.007(2) 0.008(2) -0.004(2)
C45 0.047(3) 0.061(4) 0.100(5) 0.035(3) 0.027(3) 0.014(3)
C46 0.067(4) 0.050(4) 0.111(6) 0.039(4) 0.023(4) 0.018(3)
C47 0.062(4) 0.059(4) 0.081(4) 0.021(3) 0.016(3) 0.028(3)
C48 0.051(3) 0.068(4) 0.095(5) 0.024(4) 0.033(3) 0.023(3)
C49 0.044(3) 0.053(3) 0.083(4) 0.016(3) 0.027(3) 0.010(3)
_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
Pd01 O1 2.166(3) . ?
Pd01 N1 2.013(3) . ?
Pd01 N2 2.059(4) . ?
Pd01 C1 2.004(4) . ?
O1 C11 1.274(5) . ?
O2 C4 1.233(6) . ?
N1 C2 1.405(5) . ?
N1 C12 1.418(5) . ?
N2 C45 1.343(7) . ?
N2 C49 1.321(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.364(6) . ?
C2 C11 1.392(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.416(6) . ?
C4 C5 1.494(7) . ?
C5 C6 1.391(7) . ?
C5 C10 1.389(7) . ?
C6 H6 0.9300 . ?
C6 C7 1.378(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.371(10) . ?
C8 H8 0.9300 . ?
C8 C9 1.371(8) . ?
C9 H9 0.9300 . ?
C9 C10 1.385(7) . ?
C10 C11 1.478(6) . ?
C12 C13 1.400(6) . ?
C12 C17 1.397(6) . ?
C13 C14 1.388(6) . ?
C13 C32 1.526(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.383(6) . ?
C15 C16 1.385(6) . ?
C15 C31 1.509(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.390(6) . ?
C17 C18 1.529(6) . ?
C18 H18 0.9800 . ?
C18 C19 1.525(6) . ?
C18 C25 1.523(6) . ?
C19 C20 1.370(8) . ?
C19 C24 1.382(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.406(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.365(11) . ?
C22 H22 0.9300 . ?
C22 C23 1.330(11) . ?
C23 H23 0.9300 . ?
C23 C24 1.395(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.389(6) . ?
C25 C30 1.369(6) . ?
C26 H26 0.9300 . ?
C26 C27 1.379(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.359(8) . ?
C28 H28 0.9300 . ?
C28 C29 1.369(8) . ?
C29 H29 0.9300 . ?
C29 C30 1.381(7) . ?
C30 H30 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32 0.9800 . ?
C32 C33 1.524(6) . ?
C32 C39 1.539(6) . ?
C33 C34 1.382(7) . ?
C33 C38 1.379(6) . ?
C34 H34 0.9300 . ?
C34 C35 1.389(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.371(9) . ?
C36 H36 0.9300 . ?
C36 C37 1.355(9) . ?
C37 H37 0.9300 . ?
C37 C38 1.381(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.368(7) . ?
C39 C44 1.384(7) . ?
C40 H40 0.9300 . ?
C40 C41 1.403(8) . ?
C41 H41 0.9300 . ?
C41 C42 1.356(9) . ?
C42 H42 0.9300 . ?
C42 C43 1.358(9) . ?
C43 H43 0.9300 . ?
C43 C44 1.376(7) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C45 C46 1.364(7) . ?
C46 H46 0.9300 . ?
C46 C47 1.359(8) . ?
C47 H47 0.9300 . ?
C47 C48 1.355(8) . ?
C48 H48 0.9300 . ?
C48 C49 1.373(7) . ?
C49 H49 0.9300 . ?
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 Pd01 O1 78.26(12) . . ?
N1 Pd01 N2 173.10(15) . . ?
N2 Pd01 O1 94.91(14) . . ?
C1 Pd01 O1 173.40(16) . . ?
C1 Pd01 N1 95.15(17) . . ?
C1 Pd01 N2 91.67(18) . . ?
C11 O1 Pd01 110.6(3) . . ?
C2 N1 Pd01 115.3(3) . . ?
C2 N1 C12 117.9(3) . . ?
C12 N1 Pd01 126.8(3) . . ?
C45 N2 Pd01 116.2(3) . . ?
C49 N2 Pd01 126.2(4) . . ?
C49 N2 C45 117.4(4) . . ?
Pd01 C1 H1A 109.5 . . ?
Pd01 C1 H1B 109.5 . . ?
Pd01 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 N1 124.4(4) . . ?
C3 C2 C11 122.0(4) . . ?
C11 C2 N1 113.6(3) . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.9(4) . . ?
C4 C3 H3 119.6 . . ?
O2 C4 C3 123.0(5) . . ?
O2 C4 C5 119.1(5) . . ?
C3 C4 C5 117.9(4) . . ?
C6 C5 C4 120.5(5) . . ?
C10 C5 C4 120.7(4) . . ?
C10 C5 C6 118.7(5) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.9(6) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.8(5) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.1(6) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.7(6) . . ?
C10 C9 H9 120.2 . . ?
C5 C10 C11 117.2(4) . . ?
C9 C10 C5 120.7(5) . . ?
C9 C10 C11 122.0(5) . . ?
O1 C11 C2 122.0(4) . . ?
O1 C11 C10 117.4(4) . . ?
C2 C11 C10 120.5(4) . . ?
C13 C12 N1 119.7(4) . . ?
C17 C12 N1 119.9(4) . . ?
C17 C12 C13 120.3(4) . . ?
C12 C13 C32 118.6(4) . . ?
C14 C13 C12 118.7(4) . . ?
C14 C13 C32 122.7(4) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 C13 122.0(4) . . ?
C15 C14 H14 119.0 . . ?
C14 C15 C16 118.1(4) . . ?
C14 C15 C31 120.9(4) . . ?
C16 C15 C31 121.0(4) . . ?
C15 C16 H16 119.0 . . ?
C15 C16 C17 122.0(4) . . ?
C17 C16 H16 119.0 . . ?
C12 C17 C18 119.1(4) . . ?
C16 C17 C12 118.6(4) . . ?
C16 C17 C18 122.3(4) . . ?
C17 C18 H18 105.9 . . ?
C19 C18 C17 114.3(4) . . ?
C19 C18 H18 105.9 . . ?
C25 C18 C17 112.5(4) . . ?
C25 C18 H18 105.9 . . ?
C25 C18 C19 111.7(4) . . ?
C20 C19 C18 122.2(5) . . ?
C20 C19 C24 119.5(5) . . ?
C24 C19 C18 118.3(5) . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.6(6) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 121.4 . . ?
C22 C21 C20 117.2(8) . . ?
C22 C21 H21 121.4 . . ?
C21 C22 H22 118.1 . . ?
C23 C22 C21 123.8(8) . . ?
C23 C22 H22 118.1 . . ?
C22 C23 H23 120.5 . . ?
C22 C23 C24 119.0(8) . . ?
C24 C23 H23 120.5 . . ?
C19 C24 C23 119.9(7) . . ?
C19 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C26 C25 C18 119.6(4) . . ?
C30 C25 C18 123.0(4) . . ?
C30 C25 C26 117.4(4) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 C25 121.4(5) . . ?
C27 C26 H26 119.3 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(5) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.2 . . ?
C27 C28 C29 119.6(5) . . ?
C29 C28 H28 120.2 . . ?
C28 C29 H29 119.8 . . ?
C28 C29 C30 120.3(5) . . ?
C30 C29 H29 119.8 . . ?
C25 C30 C29 121.3(5) . . ?
C25 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C15 C31 H31A 109.5 . . ?
C15 C31 H31B 109.5 . . ?
C15 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C13 C32 H32 105.7 . . ?
C13 C32 C39 112.2(3) . . ?
C33 C32 C13 113.1(3) . . ?
C33 C32 H32 105.7 . . ?
C33 C32 C39 113.6(4) . . ?
C39 C32 H32 105.7 . . ?
C34 C33 C32 119.7(4) . . ?
C38 C33 C32 121.8(4) . . ?
C38 C33 C34 118.4(5) . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.0(6) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.6(6) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 120.2 . . ?
C37 C36 C35 119.5(6) . . ?
C37 C36 H36 120.2 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(6) . . ?
C38 C37 H37 119.7 . . ?
C33 C38 C37 120.9(5) . . ?
C33 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C40 C39 C32 123.5(4) . . ?
C40 C39 C44 118.1(5) . . ?
C44 C39 C32 118.4(4) . . ?
C39 C40 H40 120.0 . . ?
C39 C40 C41 119.9(6) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 119.7 . . ?
C42 C41 C40 120.6(6) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 H42 120.0 . . ?
C41 C42 C43 120.0(6) . . ?
C43 C42 H42 120.0 . . ?
C42 C43 H43 120.1 . . ?
C42 C43 C44 119.8(6) . . ?
C44 C43 H43 120.1 . . ?
C39 C44 H44 119.2 . . ?
C43 C44 C39 121.5(6) . . ?
C43 C44 H44 119.2 . . ?
N2 C45 H45 118.9 . . ?
N2 C45 C46 122.3(5) . . ?
C46 C45 H45 118.9 . . ?
C45 C46 H46 120.3 . . ?
C47 C46 C45 119.5(6) . . ?
C47 C46 H46 120.3 . . ?
C46 C47 H47 120.6 . . ?
C48 C47 C46 118.9(5) . . ?
C48 C47 H47 120.6 . . ?
C47 C48 H48 120.4 . . ?
C47 C48 C49 119.1(6) . . ?
C49 C48 H48 120.4 . . ?
N2 C49 C48 122.9(5) . . ?
N2 C49 H49 118.6 . . ?
C48 C49 H49 118.6 . . ?
_shelx_res_file
;
TITL mo_d8v17018_0m_a.res in P-1
mo_d8v17018_0m.res
created by SHELXL-2016/6 at 10:20:19 on 17-May-2017
REM Old TITL mo_d8v17018_0m in P-1
REM SHELXT solution in P-1
REM R1 0.127, Rweak 0.033, Alpha 0.070, Orientation as input
REM Formula found by SHELXT: C47 N3 O3 Pd
CELL 0.71073 10.4912 13.4734 14.7253 94.369 109.58 90.382
ZERR 2 0.0004 0.0006 0.0006 0.002 0.002 0.002
LATT 1
SFAC C H N O Pd
UNIT 98 80 4 4 2
DELU 0.002 0.002 C2 N1
DELU 0.005 0.005 C20 C21
ISOR 0.005 0.01 C24 C23 C22 C21 C20
ISOR 0.002 0.01 C2
L.S. 8
PLAN 20
SIZE 0.15 0.2 0.22
TEMP 26.96
BOND $H
list 4
fmap 2
acta
OMIT -3 51
OMIT 0 -1 1
OMIT 0 1 0
OMIT -1 2 2
OMIT -1 0 1
OMIT -1 1 0
OMIT 1 1 0
OMIT -1 -1 1
OMIT -6 10 4
OMIT 2 -4 11
OMIT -6 -14 2
OMIT 7 8 6
REM
REM
REM
WGHT 0.021500 5.562600
FVAR 0.75356
PD01 5 0.774913 0.614187 0.308836 11.00000 0.02824 0.02997 =
0.04413 0.00507 0.01108 0.00285
O1 4 0.601772 0.511695 0.271772 11.00000 0.03380 0.02585 =
0.07349 0.00213 0.01496 -0.00180
O2 4 0.136692 0.700996 0.165345 11.00000 0.03179 0.08065 =
0.11421 0.01204 0.01073 0.01089
N1 3 0.619958 0.707509 0.274773 11.00000 0.03055 0.02342 =
0.03476 0.00229 0.00969 0.00283
N2 3 0.916046 0.505037 0.337653 11.00000 0.04160 0.04074 =
0.04990 0.01105 0.01472 0.01246
C1 1 0.919730 0.721470 0.338892 11.00000 0.02783 0.04131 =
0.06809 0.00594 0.01011 -0.00125
AFIX 137
H1A 2 0.967507 0.713058 0.293624 11.00000 -1.50000
H1B 2 0.981827 0.717340 0.403308 11.00000 -1.50000
H1C 2 0.879229 0.785404 0.334141 11.00000 -1.50000
AFIX 0
C2 1 0.490259 0.661429 0.244271 11.00000 0.02985 0.03965 =
0.02710 0.00060 0.01101 0.01055
C3 1 0.372388 0.711336 0.219393 11.00000 0.03609 0.03721 =
0.04336 0.00181 0.01221 -0.00332
AFIX 43
H3 2 0.375390 0.780595 0.225893 11.00000 -1.20000
AFIX 0
C4 1 0.245547 0.659133 0.183811 11.00000 0.03125 0.06289 =
0.04844 0.01092 0.00977 0.00535
C5 1 0.245119 0.548301 0.167608 11.00000 0.03568 0.05675 =
0.04830 -0.00553 0.01483 -0.01064
C6 1 0.124857 0.494136 0.119721 11.00000 0.04288 0.08657 =
0.06528 -0.00946 0.01294 -0.01544
AFIX 43
H6 2 0.043765 0.526823 0.097625 11.00000 -1.20000
AFIX 0
C7 1 0.126087 0.391932 0.105073 11.00000 0.05842 0.08470 =
0.10038 -0.03447 0.02941 -0.03896
AFIX 43
H7 2 0.045881 0.356180 0.071324 11.00000 -1.20000
AFIX 0
C8 1 0.244166 0.342333 0.139671 11.00000 0.07291 0.05249 =
0.11853 -0.03620 0.04477 -0.03123
AFIX 43
H8 2 0.243084 0.273181 0.131263 11.00000 -1.20000
AFIX 0
C9 1 0.363797 0.394473 0.186624 11.00000 0.05343 0.04483 =
0.09226 -0.01380 0.03167 -0.01504
AFIX 43
H9 2 0.443953 0.360876 0.209830 11.00000 -1.20000
AFIX 0
C10 1 0.364714 0.497447 0.199339 11.00000 0.04118 0.04158 =
0.04748 -0.00776 0.01801 -0.01217
C11 1 0.491933 0.557983 0.241601 11.00000 0.02928 0.05729 =
0.02954 -0.00137 0.01006 -0.01956
C12 1 0.629049 0.812618 0.275648 11.00000 0.02236 0.02690 =
0.03164 0.00271 0.00702 0.00155
C13 1 0.646434 0.871780 0.361555 11.00000 0.02468 0.02941 =
0.03329 0.00495 0.00935 -0.00116
C14 1 0.646912 0.974605 0.359398 11.00000 0.03962 0.03154 =
0.03179 -0.00397 0.00896 0.00331
AFIX 43
H14 2 0.655476 1.014236 0.415806 11.00000 -1.20000
AFIX 0
C15 1 0.635033 1.019872 0.275882 11.00000 0.03851 0.02891 =
0.04009 0.00463 0.01137 0.00242
C16 1 0.629793 0.959692 0.194050 11.00000 0.04314 0.03200 =
0.03174 0.01035 0.01109 0.00213
AFIX 43
H16 2 0.628232 0.989315 0.138686 11.00000 -1.20000
AFIX 0
C17 1 0.626798 0.856392 0.192144 11.00000 0.02797 0.02962 =
0.03161 -0.00015 0.00724 0.00116
C18 1 0.626062 0.789491 0.103266 11.00000 0.04527 0.03299 =
0.03169 0.00109 0.01430 0.00210
AFIX 13
H18 2 0.672056 0.729125 0.128105 11.00000 -1.20000
AFIX 0
C19 1 0.485223 0.754769 0.035849 11.00000 0.05441 0.06165 =
0.03380 -0.00807 0.02143 -0.01749
C20 1 0.377543 0.816280 0.015365 11.00000 0.05617 0.08417 =
0.05175 -0.00057 0.01994 -0.00443
AFIX 43
H20 2 0.388563 0.880578 0.045341 11.00000 -1.20000
AFIX 0
C21 1 0.250514 0.783127 -0.050551 11.00000 0.06527 0.11989 =
0.08284 0.00580 0.03009 -0.00635
AFIX 43
H21 2 0.176801 0.824328 -0.065299 11.00000 -1.20000
AFIX 0
C22 1 0.239913 0.687911 -0.092000 11.00000 0.08620 0.12299 =
0.09085 -0.00526 0.03099 -0.02775
AFIX 43
H22 2 0.156906 0.665436 -0.136666 11.00000 -1.20000
AFIX 0
C23 1 0.341406 0.625448 -0.072203 11.00000 0.10907 0.10503 =
0.09516 -0.02725 0.03722 -0.02380
AFIX 43
H23 2 0.328254 0.560541 -0.100847 11.00000 -1.20000
AFIX 0
C24 1 0.467884 0.658778 -0.007817 11.00000 0.07875 0.07860 =
0.07327 -0.01986 0.03272 -0.01870
AFIX 43
H24 2 0.540429 0.616498 0.005716 11.00000 -1.20000
AFIX 0
C25 1 0.709317 0.834626 0.048628 11.00000 0.03949 0.03076 =
0.03348 -0.00408 0.01188 0.00194
C26 1 0.847463 0.819366 0.076504 11.00000 0.04483 0.04705 =
0.03280 -0.00135 0.00474 0.00069
AFIX 43
H26 2 0.887657 0.782069 0.128667 11.00000 -1.20000
AFIX 0
C27 1 0.926321 0.858326 0.028502 11.00000 0.03736 0.06126 =
0.05772 -0.01101 0.01478 -0.01181
AFIX 43
H27 2 1.018597 0.847036 0.048270 11.00000 -1.20000
AFIX 0
C28 1 0.869116 0.913236 -0.047716 11.00000 0.06545 0.05215 =
0.06520 -0.00454 0.03712 -0.01858
AFIX 43
H28 2 0.922036 0.939719 -0.080160 11.00000 -1.20000
AFIX 0
C29 1 0.733182 0.929318 -0.076427 11.00000 0.07292 0.05869 =
0.05717 0.02039 0.02818 0.00551
AFIX 43
H29 2 0.693666 0.966685 -0.128656 11.00000 -1.20000
AFIX 0
C30 1 0.654449 0.890328 -0.028216 11.00000 0.04585 0.05426 =
0.05022 0.01641 0.02144 0.01189
AFIX 43
H30 2 0.562306 0.902147 -0.048353 11.00000 -1.20000
AFIX 0
C31 1 0.634346 1.131827 0.275237 11.00000 0.09112 0.03058 =
0.05278 0.00232 0.02152 0.00271
AFIX 137
H31A 2 0.678671 1.152071 0.231900 11.00000 -1.50000
H31B 2 0.681335 1.161578 0.339296 11.00000 -1.50000
H31C 2 0.542593 1.153044 0.254103 11.00000 -1.50000
AFIX 0
C32 1 0.671634 0.820688 0.454744 11.00000 0.03350 0.02672 =
0.03571 0.00450 0.01087 0.00221
AFIX 13
H32 2 0.726978 0.763553 0.449859 11.00000 -1.20000
AFIX 0
C33 1 0.542742 0.777206 0.464399 11.00000 0.04184 0.03729 =
0.02968 -0.00010 0.01121 -0.00609
C34 1 0.542076 0.682740 0.494798 11.00000 0.05229 0.05457 =
0.07472 0.02280 0.01499 -0.00596
AFIX 43
H34 2 0.620136 0.646044 0.509439 11.00000 -1.20000
AFIX 0
C35 1 0.424810 0.642568 0.503492 11.00000 0.07426 0.06959 =
0.09705 0.03103 0.02316 -0.02221
AFIX 43
H35 2 0.425591 0.579789 0.525874 11.00000 -1.20000
AFIX 0
C36 1 0.307920 0.694680 0.479359 11.00000 0.05130 0.08963 =
0.07732 0.01185 0.02496 -0.02220
AFIX 43
H36 2 0.229218 0.666921 0.484091 11.00000 -1.20000
AFIX 0
C37 1 0.307947 0.786909 0.448569 11.00000 0.04667 0.07897 =
0.06186 0.00001 0.02395 -0.00099
AFIX 43
H37 2 0.228977 0.822601 0.432523 11.00000 -1.20000
AFIX 0
C38 1 0.424216 0.828388 0.440803 11.00000 0.04510 0.05017 =
0.05362 0.00559 0.02323 0.00102
AFIX 43
H38 2 0.422535 0.891692 0.419369 11.00000 -1.20000
AFIX 0
C39 1 0.757777 0.886804 0.544604 11.00000 0.04062 0.03222 =
0.03461 0.00880 0.00520 0.00012
C40 1 0.710235 0.923780 0.615865 11.00000 0.06443 0.06092 =
0.03592 0.00192 0.01695 -0.00726
AFIX 43
H40 2 0.622211 0.907890 0.612340 11.00000 -1.20000
AFIX 0
C41 1 0.794410 0.985675 0.694231 11.00000 0.10446 0.08609 =
0.03662 -0.00838 0.02333 -0.01361
AFIX 43
H41 2 0.761058 1.011981 0.741718 11.00000 -1.20000
AFIX 0
C42 1 0.923919 1.007506 0.701395 11.00000 0.09949 0.08582 =
0.03783 -0.00266 -0.00267 -0.03043
AFIX 43
H42 2 0.979591 1.047442 0.754322 11.00000 -1.20000
AFIX 0
C43 1 0.972317 0.971023 0.631238 11.00000 0.05234 0.07585 =
0.06182 0.01308 -0.00445 -0.02057
AFIX 43
H43 2 1.060997 0.986207 0.635866 11.00000 -1.20000
AFIX 0
C44 1 0.889836 0.911534 0.553282 11.00000 0.04962 0.05090 =
0.04861 0.00690 0.00809 -0.00428
AFIX 43
H44 2 0.923622 0.887384 0.505308 11.00000 -1.20000
AFIX 0
C45 1 0.876227 0.418220 0.360520 11.00000 0.04682 0.06063 =
0.09974 0.03481 0.02663 0.01407
AFIX 43
H45 2 0.791154 0.412962 0.366738 11.00000 -1.20000
AFIX 0
C46 1 0.956220 0.337516 0.374935 11.00000 0.06680 0.05041 =
0.11122 0.03903 0.02285 0.01814
AFIX 43
H46 2 0.926441 0.278783 0.391863 11.00000 -1.20000
AFIX 0
C47 1 1.079764 0.343562 0.364378 11.00000 0.06244 0.05883 =
0.08127 0.02070 0.01624 0.02846
AFIX 43
H47 2 1.135245 0.289036 0.373438 11.00000 -1.20000
AFIX 0
C48 1 1.120724 0.430378 0.340431 11.00000 0.05117 0.06833 =
0.09545 0.02385 0.03268 0.02337
AFIX 43
H48 2 1.204889 0.436344 0.332865 11.00000 -1.20000
AFIX 0
C49 1 1.036344 0.509465 0.327471 11.00000 0.04437 0.05286 =
0.08323 0.01607 0.02656 0.01002
AFIX 43
H49 2 1.065117 0.568714 0.310804 11.00000 -1.20000
AFIX 0
HKLF 4
REM mo_d8v17018_0m_a.res in P-1
REM R1 = 0.0563 for 6233 Fo > 4sig(Fo) and 0.0657 for all 7103 data
REM 489 parameters refined using 38 restraints
END
WGHT 0.0219 5.5735
REM Highest difference peak 1.502, deepest hole -0.571, 1-sigma level 0.083
Q1 1 0.4361 0.6196 0.2405 11.00000 0.05 1.50
Q2 1 0.2533 0.8389 -0.0474 11.00000 0.05 0.64
Q3 1 0.2058 0.7383 -0.1102 11.00000 0.05 0.64
Q4 1 0.8141 0.6002 0.2557 11.00000 0.05 0.60
Q5 1 0.5031 0.6948 0.2468 11.00000 0.05 0.59
Q6 1 0.2530 0.6425 -0.0800 11.00000 0.05 0.59
Q7 1 0.3142 0.6607 -0.0977 11.00000 0.05 0.51
Q8 1 0.3795 0.5849 -0.0503 11.00000 0.05 0.50
Q9 1 0.4449 0.5326 0.2213 11.00000 0.05 0.50
Q10 1 0.8606 0.6812 0.3061 11.00000 0.05 0.43
Q11 1 0.5143 0.5460 0.2779 11.00000 0.05 0.43
Q12 1 0.6998 0.6289 0.3322 11.00000 0.05 0.41
Q13 1 0.5205 0.5556 0.2333 11.00000 0.05 0.40
Q14 1 0.7969 0.6819 0.3430 11.00000 0.05 0.39
Q15 1 0.4195 0.6991 -0.0430 11.00000 0.05 0.39
Q16 1 0.7749 0.5434 0.2856 11.00000 0.05 0.38
Q17 1 0.7480 0.6361 0.3709 11.00000 0.05 0.38
Q18 1 0.3942 0.7575 0.2368 11.00000 0.05 0.37
Q19 1 0.5847 1.1588 0.2124 11.00000 0.05 0.37
Q20 1 0.3644 0.8609 0.0218 11.00000 0.05 0.36
;
_shelx_res_checksum 85763
_olex2_submission_special_instructions 'No special instructions were received'