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# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
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data_l15812
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C19 H33 N3 Pd'
_chemical_formula_sum 'C19 H33 N3 Pd'
_chemical_formula_weight 409.88
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M Cc
loop_
_symmetry_equiv_pos_as_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'
_cell_length_a 12.010(5)
_cell_length_b 14.065(5)
_cell_length_c 12.461(5)
_cell_angle_alpha 90.00
_cell_angle_beta 113.96(2)
_cell_angle_gamma 90.00
_cell_volume 1923.6(13)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 8229
_cell_measurement_theta_min 2.35
_cell_measurement_theta_max 26.85
_exptl_crystal_description rectangular
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas no
_exptl_crystal_density_diffrn 1.415
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 856
_exptl_absorpt_coefficient_mu 0.969
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8130
_exptl_absorpt_correction_T_max 0.9523
_exptl_absorpt_process_details 'sadabs v2008/1'
_exptl_special_details
;
All H atoms were added in their calculated positions
and were treated using appropriate riding models.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 16565
_diffrn_reflns_av_R_equivalents 0.0592
_diffrn_reflns_av_sigmaI/netI 0.0520
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.35
_diffrn_reflns_theta_max 26.85
_reflns_number_total 4071
_reflns_number_gt 3779
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00(2)
_refine_ls_number_reflns 4071
_refine_ls_number_parameters 213
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0299
_refine_ls_R_factor_gt 0.0260
_refine_ls_wR_factor_ref 0.0542
_refine_ls_wR_factor_gt 0.0525
_refine_ls_goodness_of_fit_ref 1.010
_refine_ls_restrained_S_all 1.010
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 0.32038(2) 0.199581(12) 0.52269(2) 0.01749(6) Uani 1 1 d . . .
N1 N 0.3486(4) 0.2127(2) 0.7091(4) 0.0196(8) Uani 1 1 d . . .
N2 N 0.1187(2) 0.06690(17) 0.5985(2) 0.0262(6) Uani 1 1 d . . .
N3 N 0.3551(2) 0.04636(18) 0.5746(2) 0.0221(6) Uani 1 1 d . . .
C1 C 0.2804(3) 0.3339(2) 0.4630(3) 0.0186(6) Uani 1 1 d . . .
C2 C 0.2271(3) 0.4044(2) 0.5066(3) 0.0215(6) Uani 1 1 d . . .
H2 H 0.2078 0.3902 0.5716 0.026 Uiso 1 1 calc R . .
C3 C 0.2019(3) 0.4948(2) 0.4565(3) 0.0265(7) Uani 1 1 d . . .
H3 H 0.1655 0.5412 0.4876 0.032 Uiso 1 1 calc R . .
C4 C 0.2290(3) 0.5174(2) 0.3632(3) 0.0279(7) Uani 1 1 d . . .
H4 H 0.2145 0.5798 0.3313 0.033 Uiso 1 1 calc R . .
C5 C 0.2782(3) 0.4480(2) 0.3150(3) 0.0244(7) Uani 1 1 d . . .
H5 H 0.2953 0.4626 0.2487 0.029 Uiso 1 1 calc R . .
C6 C 0.3024(3) 0.3568(2) 0.3643(3) 0.0196(6) Uani 1 1 d . . .
C7 C 0.3520(3) 0.2743(2) 0.3167(3) 0.0219(7) Uani 1 1 d . . .
C8 C 0.3053(5) 0.1848(3) 0.3569(5) 0.0260(11) Uani 1 1 d . . .
H8A H 0.3530 0.1288 0.3520 0.031 Uiso 1 1 calc R . .
H8B H 0.2189 0.1737 0.3040 0.031 Uiso 1 1 calc R . .
C9 C 0.3072(3) 0.2778(2) 0.1837(3) 0.0319(8) Uani 1 1 d . . .
H9A H 0.2179 0.2791 0.1479 0.048 Uiso 1 1 calc R . .
H9B H 0.3360 0.2214 0.1564 0.048 Uiso 1 1 calc R . .
H9C H 0.3388 0.3351 0.1610 0.048 Uiso 1 1 calc R . .
C10 C 0.4915(3) 0.2755(2) 0.3728(3) 0.0277(7) Uani 1 1 d . . .
H10A H 0.5209 0.3340 0.3502 0.042 Uiso 1 1 calc R . .
H10B H 0.5226 0.2203 0.3455 0.042 Uiso 1 1 calc R . .
H10C H 0.5203 0.2730 0.4584 0.042 Uiso 1 1 calc R . .
C11 C 0.2335(3) 0.2051(2) 0.7285(3) 0.0246(7) Uani 1 1 d . . .
H11A H 0.2147 0.2687 0.7510 0.030 Uiso 1 1 calc R . .
H11B H 0.2490 0.1621 0.7960 0.030 Uiso 1 1 calc R . .
C12 C 0.1201(3) 0.1689(2) 0.6243(3) 0.0238(7) Uani 1 1 d . . .
H12A H 0.0474 0.1837 0.6398 0.029 Uiso 1 1 calc R . .
H12B H 0.1126 0.2048 0.5534 0.029 Uiso 1 1 calc R . .
C13 C 0.1254(3) 0.0399(2) 0.4895(3) 0.0232(7) Uani 1 1 d . . .
H13A H 0.1167 0.0977 0.4413 0.028 Uiso 1 1 calc R . .
H13B H 0.0561 -0.0026 0.4457 0.028 Uiso 1 1 calc R . .
C14 C 0.2449(3) -0.0108(2) 0.5054(3) 0.0242(7) Uani 1 1 d . . .
H14A H 0.2494 -0.0723 0.5456 0.029 Uiso 1 1 calc R . .
H14B H 0.2441 -0.0244 0.4271 0.029 Uiso 1 1 calc R . .
C15 C 0.4346(3) 0.1318(2) 0.7631(3) 0.0269(7) Uani 1 1 d . . .
H15A H 0.4500 0.1264 0.8471 0.032 Uiso 1 1 calc R . .
H15B H 0.5134 0.1451 0.7581 0.032 Uiso 1 1 calc R . .
C16 C 0.3841(3) 0.0389(2) 0.7020(3) 0.0248(7) Uani 1 1 d . . .
H16A H 0.4446 -0.0124 0.7370 0.030 Uiso 1 1 calc R . .
H16B H 0.3094 0.0223 0.7132 0.030 Uiso 1 1 calc R . .
C17 C 0.4155(3) 0.3009(2) 0.7677(3) 0.0304(8) Uani 1 1 d . . .
H17A H 0.4950 0.3026 0.7630 0.046 Uiso 1 1 calc R . .
H17B H 0.4273 0.3011 0.8502 0.046 Uiso 1 1 calc R . .
H17C H 0.3680 0.3569 0.7280 0.046 Uiso 1 1 calc R . .
C18 C 0.0424(3) 0.0084(2) 0.6352(3) 0.0338(8) Uani 1 1 d . . .
H18A H 0.0601 0.0213 0.7178 0.051 Uiso 1 1 calc R . .
H18B H 0.0584 -0.0588 0.6260 0.051 Uiso 1 1 calc R . .
H18C H -0.0434 0.0227 0.5868 0.051 Uiso 1 1 calc R . .
C19 C 0.4600(3) 0.0093(3) 0.5545(3) 0.0298(8) Uani 1 1 d . . .
H19A H 0.4462 0.0193 0.4723 0.045 Uiso 1 1 calc R . .
H19B H 0.4693 -0.0588 0.5724 0.045 Uiso 1 1 calc R . .
H19C H 0.5342 0.0429 0.6056 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 0.01922(10) 0.01538(9) 0.01903(10) 0.00002(15) 0.00896(8) -0.00176(15)
N1 0.0197(17) 0.0214(16) 0.0166(18) -0.0017(14) 0.0063(14) -0.0067(14)
N2 0.0250(15) 0.0218(14) 0.0354(16) -0.0064(12) 0.0159(13) -0.0088(11)
N3 0.0176(14) 0.0216(13) 0.0292(15) 0.0026(11) 0.0118(12) 0.0040(10)
C1 0.0148(15) 0.0171(14) 0.0206(16) -0.0037(13) 0.0039(13) -0.0058(12)
C2 0.0145(15) 0.0219(16) 0.0293(17) -0.0035(14) 0.0100(13) -0.0061(13)
C3 0.0213(18) 0.0198(16) 0.036(2) -0.0028(14) 0.0086(16) -0.0003(13)
C4 0.0273(18) 0.0190(16) 0.036(2) 0.0051(14) 0.0119(16) 0.0006(13)
C5 0.0246(17) 0.0251(16) 0.0242(17) 0.0032(14) 0.0106(15) -0.0040(13)
C6 0.0135(15) 0.0159(15) 0.0267(17) -0.0018(13) 0.0053(13) -0.0019(12)
C7 0.0262(17) 0.0221(15) 0.0200(17) -0.0014(13) 0.0123(14) -0.0031(13)
C8 0.030(3) 0.0191(18) 0.029(3) -0.0030(19) 0.012(2) -0.0027(17)
C9 0.044(2) 0.0331(18) 0.0198(18) -0.0040(15) 0.0139(17) -0.0091(16)
C10 0.0263(19) 0.0291(17) 0.0289(19) -0.0016(15) 0.0125(16) 0.0005(14)
C11 0.0294(18) 0.0246(17) 0.0250(18) -0.0033(13) 0.0163(16) -0.0056(13)
C12 0.0182(16) 0.0233(15) 0.0315(19) -0.0033(14) 0.0118(15) -0.0041(13)
C13 0.0199(18) 0.0170(16) 0.0305(19) -0.0024(14) 0.0079(16) -0.0039(13)
C14 0.029(2) 0.0151(16) 0.0279(18) -0.0014(13) 0.0110(18) 0.0021(15)
C15 0.0242(18) 0.0290(17) 0.0265(18) 0.0060(14) 0.0092(15) 0.0035(14)
C16 0.0215(16) 0.0256(16) 0.0257(18) 0.0087(14) 0.0078(14) 0.0050(13)
C17 0.034(2) 0.0303(19) 0.0234(19) -0.0084(14) 0.0085(16) -0.0126(15)
C18 0.031(2) 0.0324(19) 0.037(2) 0.0003(16) 0.0131(18) -0.0097(15)
C19 0.025(2) 0.030(2) 0.034(2) -0.0018(17) 0.012(2) 0.0043(17)
_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 C8 2.010(6) . ?
Pd1 C1 2.015(3) . ?
Pd1 N1 2.215(4) . ?
Pd1 N3 2.240(3) . ?
N1 C17 1.498(4) . ?
N1 C15 1.500(5) . ?
N1 C11 1.501(5) . ?
N2 C18 1.438(4) . ?
N2 C13 1.444(4) . ?
N2 C12 1.469(4) . ?
N3 C19 1.476(4) . ?
N3 C16 1.484(4) . ?
N3 C14 1.488(4) . ?
C1 C6 1.396(4) . ?
C1 C2 1.405(4) . ?
C2 C3 1.394(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.367(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.530(4) . ?
C7 C9 1.522(4) . ?
C7 C10 1.531(5) . ?
C7 C8 1.542(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.537(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.542(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.510(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
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 . ?
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
C8 Pd1 C1 78.99(14) . . ?
C8 Pd1 N1 176.5(2) . . ?
C1 Pd1 N1 102.80(12) . . ?
C8 Pd1 N3 97.22(12) . . ?
C1 Pd1 N3 175.42(11) . . ?
N1 Pd1 N3 81.12(10) . . ?
C17 N1 C15 106.0(3) . . ?
C17 N1 C11 109.1(3) . . ?
C15 N1 C11 112.7(3) . . ?
C17 N1 Pd1 113.8(3) . . ?
C15 N1 Pd1 101.0(2) . . ?
C11 N1 Pd1 113.9(3) . . ?
C18 N2 C13 115.8(3) . . ?
C18 N2 C12 116.2(3) . . ?
C13 N2 C12 117.5(3) . . ?
C19 N3 C16 108.1(3) . . ?
C19 N3 C14 109.3(3) . . ?
C16 N3 C14 110.4(2) . . ?
C19 N3 Pd1 111.2(2) . . ?
C16 N3 Pd1 108.21(18) . . ?
C14 N3 Pd1 109.58(19) . . ?
C6 C1 C2 117.1(3) . . ?
C6 C1 Pd1 116.1(2) . . ?
C2 C1 Pd1 126.6(2) . . ?
C3 C2 C1 121.4(3) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 121.3(3) . . ?
C1 C6 C7 114.1(3) . . ?
C5 C6 C7 124.6(3) . . ?
C9 C7 C6 112.1(3) . . ?
C9 C7 C10 109.5(3) . . ?
C6 C7 C10 109.9(3) . . ?
C9 C7 C8 111.5(3) . . ?
C6 C7 C8 104.1(3) . . ?
C10 C7 C8 109.6(3) . . ?
C7 C8 Pd1 110.9(3) . . ?
C7 C8 H8A 109.5 . . ?
Pd1 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
Pd1 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 116.4(3) . . ?
N1 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N1 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.3 . . ?
N2 C12 C11 115.8(3) . . ?
N2 C12 H12A 108.3 . . ?
C11 C12 H12A 108.3 . . ?
N2 C12 H12B 108.3 . . ?
C11 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
N2 C13 C14 113.9(3) . . ?
N2 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
N2 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
N3 C14 C13 112.7(3) . . ?
N3 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
N3 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
N1 C15 C16 111.6(3) . . ?
N1 C15 H15A 109.3 . . ?
C16 C15 H15A 109.3 . . ?
N1 C15 H15B 109.3 . . ?
C16 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
N3 C16 C15 110.5(2) . . ?
N3 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
N3 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
C1 Pd1 N1 C17 -39.7(3) . . . . ?
N3 Pd1 N1 C17 142.7(3) . . . . ?
C1 Pd1 N1 C15 -152.8(2) . . . . ?
N3 Pd1 N1 C15 29.6(2) . . . . ?
C1 Pd1 N1 C11 86.1(2) . . . . ?
N3 Pd1 N1 C11 -91.5(2) . . . . ?
C8 Pd1 N3 C19 55.1(3) . . . . ?
N1 Pd1 N3 C19 -121.8(2) . . . . ?
C8 Pd1 N3 C16 173.6(2) . . . . ?
N1 Pd1 N3 C16 -3.2(2) . . . . ?
C8 Pd1 N3 C14 -65.9(3) . . . . ?
N1 Pd1 N3 C14 117.2(2) . . . . ?
C8 Pd1 C1 C6 -20.3(3) . . . . ?
N1 Pd1 C1 C6 156.6(2) . . . . ?
C8 Pd1 C1 C2 156.1(3) . . . . ?
N1 Pd1 C1 C2 -27.0(3) . . . . ?
C6 C1 C2 C3 -2.6(4) . . . . ?
Pd1 C1 C2 C3 -178.9(2) . . . . ?
C1 C2 C3 C4 -0.2(5) . . . . ?
C2 C3 C4 C5 2.4(5) . . . . ?
C3 C4 C5 C6 -1.7(5) . . . . ?
C2 C1 C6 C5 3.3(4) . . . . ?
Pd1 C1 C6 C5 -180.0(2) . . . . ?
C2 C1 C6 C7 -175.8(3) . . . . ?
Pd1 C1 C6 C7 0.9(3) . . . . ?
C4 C5 C6 C1 -1.2(5) . . . . ?
C4 C5 C6 C7 177.8(3) . . . . ?
C1 C6 C7 C9 146.3(3) . . . . ?
C5 C6 C7 C9 -32.8(4) . . . . ?
C1 C6 C7 C10 -91.7(3) . . . . ?
C5 C6 C7 C10 89.2(4) . . . . ?
C1 C6 C7 C8 25.7(4) . . . . ?
C5 C6 C7 C8 -153.4(3) . . . . ?
C9 C7 C8 Pd1 -162.7(3) . . . . ?
C6 C7 C8 Pd1 -41.7(4) . . . . ?
C10 C7 C8 Pd1 75.9(4) . . . . ?
C1 Pd1 C8 C7 34.7(3) . . . . ?
N3 Pd1 C8 C7 -147.9(3) . . . . ?
C17 N1 C11 C12 140.8(3) . . . . ?
C15 N1 C11 C12 -101.7(4) . . . . ?
Pd1 N1 C11 C12 12.6(3) . . . . ?
C18 N2 C12 C11 103.5(3) . . . . ?
C13 N2 C12 C11 -113.0(3) . . . . ?
N1 C11 C12 N2 73.4(4) . . . . ?
C18 N2 C13 C14 -103.9(3) . . . . ?
C12 N2 C13 C14 112.4(3) . . . . ?
C19 N3 C14 C13 -162.1(3) . . . . ?
C16 N3 C14 C13 79.2(3) . . . . ?
Pd1 N3 C14 C13 -39.9(3) . . . . ?
N2 C13 C14 N3 -56.3(4) . . . . ?
C17 N1 C15 C16 -173.4(3) . . . . ?
C11 N1 C15 C16 67.4(4) . . . . ?
Pd1 N1 C15 C16 -54.5(3) . . . . ?
C19 N3 C16 C15 95.6(3) . . . . ?
C14 N3 C16 C15 -144.9(3) . . . . ?
Pd1 N3 C16 C15 -25.0(3) . . . . ?
N1 C15 C16 N3 56.5(4) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C16 H16B N2 0.99 2.24 2.939(4) 126.4 .
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 26.85
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 0.321
_refine_diff_density_min -0.341
_refine_diff_density_rms 0.060
_iucr_refine_instructions_details
;
TITL lm15812/lt/smart/Fengrui/Me3tacnPdII in Cc
CELL 0.71073 12.0104 14.0647 12.4613 90.000 113.961 90.000
ZERR 4.00 0.0047 0.0052 0.0050 0.000 0.020 0.000
LATT -7
SYMM X, -Y, 0.5+Z
SFAC C H N PD
UNIT 76 132 12 4
TEMP -173.0
SIZE 0.051 0.132 0.223
OMIT -3.0
L.S. 10
PLAN 5
wpdb -2
list 4
bond $h
htab
HTAB C16 N2
conf
more 2
fmap 2
acta
WGHT 0.013000
FVAR 0.09756
PD1 4 0.320379 0.199581 0.522691 11.00000 0.01922 0.01538 =
0.01903 0.00002 0.00896 -0.00176
N1 3 0.348613 0.212660 0.709146 11.00000 0.01969 0.02139 =
0.01655 -0.00173 0.00627 -0.00675
N2 3 0.118699 0.066905 0.598544 11.00000 0.02501 0.02185 =
0.03541 -0.00640 0.01594 -0.00879
N3 3 0.355090 0.046363 0.574621 11.00000 0.01763 0.02164 =
0.02922 0.00258 0.01176 0.00396
C1 1 0.280450 0.333856 0.462974 11.00000 0.01477 0.01712 =
0.02062 -0.00375 0.00391 -0.00580
C2 1 0.227087 0.404424 0.506600 11.00000 0.01455 0.02191 =
0.02928 -0.00349 0.01004 -0.00610
AFIX 43
H2 2 0.207772 0.390228 0.571606 11.00000 -1.20000
AFIX 0
C3 1 0.201865 0.494843 0.456549 11.00000 0.02131 0.01983 =
0.03563 -0.00284 0.00864 -0.00034
AFIX 43
H3 2 0.165496 0.541177 0.487601 11.00000 -1.20000
AFIX 0
C4 1 0.229016 0.517375 0.363202 11.00000 0.02728 0.01897 =
0.03642 0.00508 0.01191 0.00059
AFIX 43
H4 2 0.214528 0.579792 0.331337 11.00000 -1.20000
AFIX 0
C5 1 0.278242 0.447952 0.314959 11.00000 0.02456 0.02512 =
0.02417 0.00322 0.01058 -0.00403
AFIX 43
H5 2 0.295286 0.462576 0.248733 11.00000 -1.20000
AFIX 0
C6 1 0.302417 0.356821 0.364326 11.00000 0.01351 0.01592 =
0.02668 -0.00180 0.00534 -0.00194
C7 1 0.351990 0.274287 0.316731 11.00000 0.02621 0.02215 =
0.02003 -0.00138 0.01229 -0.00313
C8 1 0.305315 0.184764 0.356917 11.00000 0.03009 0.01913 =
0.02912 -0.00298 0.01226 -0.00273
AFIX 23
H8A 2 0.353011 0.128796 0.351996 11.00000 -1.20000
H8B 2 0.218916 0.173677 0.304010 11.00000 -1.20000
AFIX 0
C9 1 0.307203 0.277761 0.183669 11.00000 0.04368 0.03307 =
0.01978 -0.00404 0.01388 -0.00913
AFIX 137
H9A 2 0.217933 0.279097 0.147909 11.00000 -1.50000
H9B 2 0.336043 0.221351 0.156409 11.00000 -1.50000
H9C 2 0.338795 0.335072 0.161015 11.00000 -1.50000
AFIX 0
C10 1 0.491496 0.275491 0.372759 11.00000 0.02626 0.02909 =
0.02893 -0.00160 0.01246 0.00045
AFIX 137
H10A 2 0.520883 0.333958 0.350200 11.00000 -1.50000
H10B 2 0.522563 0.220280 0.345511 11.00000 -1.50000
H10C 2 0.520321 0.273004 0.458422 11.00000 -1.50000
AFIX 0
C11 1 0.233492 0.205093 0.728550 11.00000 0.02937 0.02457 =
0.02503 -0.00334 0.01632 -0.00556
AFIX 23
H11A 2 0.214678 0.268679 0.750957 11.00000 -1.20000
H11B 2 0.249014 0.162097 0.796024 11.00000 -1.20000
AFIX 0
C12 1 0.120139 0.168913 0.624326 11.00000 0.01816 0.02334 =
0.03155 -0.00327 0.01182 -0.00405
AFIX 23
H12A 2 0.047436 0.183656 0.639850 11.00000 -1.20000
H12B 2 0.112565 0.204827 0.553361 11.00000 -1.20000
AFIX 0
C13 1 0.125407 0.039903 0.489499 11.00000 0.01985 0.01697 =
0.03054 -0.00236 0.00789 -0.00391
AFIX 23
H13A 2 0.116652 0.097670 0.441336 11.00000 -1.20000
H13B 2 0.056082 -0.002642 0.445703 11.00000 -1.20000
AFIX 0
C14 1 0.244904 -0.010817 0.505400 11.00000 0.02910 0.01508 =
0.02788 -0.00136 0.01096 0.00209
AFIX 23
H14A 2 0.249400 -0.072341 0.545553 11.00000 -1.20000
H14B 2 0.244065 -0.024408 0.427124 11.00000 -1.20000
AFIX 0
C15 1 0.434639 0.131776 0.763061 11.00000 0.02416 0.02895 =
0.02649 0.00602 0.00916 0.00346
AFIX 23
H15A 2 0.449967 0.126355 0.847112 11.00000 -1.20000
H15B 2 0.513371 0.145061 0.758124 11.00000 -1.20000
AFIX 0
C16 1 0.384094 0.038880 0.701980 11.00000 0.02151 0.02564 =
0.02566 0.00867 0.00782 0.00501
AFIX 23
H16A 2 0.444579 -0.012359 0.737019 11.00000 -1.20000
H16B 2 0.309411 0.022285 0.713173 11.00000 -1.20000
AFIX 0
C17 1 0.415513 0.300945 0.767659 11.00000 0.03425 0.03034 =
0.02341 -0.00843 0.00847 -0.01257
AFIX 137
H17A 2 0.495010 0.302557 0.763014 11.00000 -1.50000
H17B 2 0.427285 0.301120 0.850224 11.00000 -1.50000
H17C 2 0.368017 0.356925 0.728026 11.00000 -1.50000
AFIX 0
C18 1 0.042380 0.008365 0.635214 11.00000 0.03145 0.03235 =
0.03676 0.00029 0.01306 -0.00968
AFIX 137
H18A 2 0.060061 0.021309 0.717824 11.00000 -1.50000
H18B 2 0.058435 -0.058785 0.625980 11.00000 -1.50000
H18C 2 -0.043375 0.022667 0.586833 11.00000 -1.50000
AFIX 0
C19 1 0.460001 0.009322 0.554540 11.00000 0.02530 0.03045 =
0.03376 -0.00179 0.01213 0.00427
AFIX 137
H19A 2 0.446198 0.019338 0.472266 11.00000 -1.50000
H19B 2 0.469315 -0.058822 0.572397 11.00000 -1.50000
H19C 2 0.534160 0.042854 0.605622 11.00000 -1.50000
HKLF 4
REM lm15812/lt/smart/Fengrui/Me3tacnPdII in Cc
REM R1 = 0.0260 for 3779 Fo > 4sig(Fo) and 0.0299 for all 4071 data
REM 213 parameters refined using 2 restraints
END
WGHT 0.0130 0.0000
REM Highest difference peak 0.321, deepest hole -0.341, 1-sigma level 0.060
Q1 1 0.3237 0.0854 0.5242 11.00000 0.05 0.32
Q2 1 0.3231 0.2991 0.5220 11.00000 0.05 0.32
Q3 1 0.3417 0.3166 0.3417 11.00000 0.05 0.27
Q4 1 0.3220 0.1670 0.4326 11.00000 0.05 0.23
Q5 1 0.1222 0.1203 0.6024 11.00000 0.05 0.23
;
_database_code_depnum_ccdc_archive 'CCDC 972256'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_l15612
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C19 H34 N3 O Pd, Cl O4'
_chemical_formula_sum 'C19 H34 Cl N3 O5 Pd'
_chemical_formula_weight 526.34
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M Pca2(1)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
_cell_length_a 16.768(5)
_cell_length_b 8.477(2)
_cell_length_c 14.704(4)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2090.1(10)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9351
_cell_measurement_theta_min 2.69
_cell_measurement_theta_max 27.15
_exptl_crystal_description rectangular
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas no
_exptl_crystal_density_diffrn 1.673
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1088
_exptl_absorpt_coefficient_mu 1.052
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8324
_exptl_absorpt_correction_T_max 0.8675
_exptl_absorpt_process_details 'sadabs v2008/1'
_exptl_special_details
;
All H atoms were added in their calculated positions
and were treated using appropriate riding models.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 54583
_diffrn_reflns_av_R_equivalents 0.0682
_diffrn_reflns_av_sigmaI/netI 0.0301
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.40
_diffrn_reflns_theta_max 27.58
_reflns_number_total 4780
_reflns_number_gt 4446
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.3130P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.005(18)
_refine_ls_number_reflns 4780
_refine_ls_number_parameters 268
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0247
_refine_ls_R_factor_gt 0.0215
_refine_ls_wR_factor_ref 0.0498
_refine_ls_wR_factor_gt 0.0482
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_restrained_S_all 1.035
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 0.517330(9) 0.396461(16) 0.499806(16) 0.01264(5) Uani 1 1 d . . .
Cl1 Cl 0.33919(4) 0.95254(7) 0.72949(4) 0.02201(13) Uani 1 1 d . . .
O1 O 0.56908(11) 0.38323(19) 0.37610(11) 0.0161(4) Uani 1 1 d . . .
H1 H 0.5917 0.2954 0.3704 0.024 Uiso 1 1 calc R . .
O2 O 0.28164(13) 1.0729(2) 0.70961(15) 0.0392(5) Uani 1 1 d . . .
O3 O 0.30666(13) 0.8013(2) 0.70352(16) 0.0452(6) Uani 1 1 d . . .
O4 O 0.41129(13) 0.9802(2) 0.67986(14) 0.0344(5) Uani 1 1 d . . .
O5 O 0.35673(16) 0.9487(3) 0.82505(15) 0.0536(6) Uani 1 1 d . . .
N1 N 0.58447(13) 0.6234(2) 0.52638(13) 0.0171(5) Uani 1 1 d . . .
N2 N 0.47313(12) 0.4400(2) 0.63228(14) 0.0171(4) Uani 1 1 d . . .
N3 N 0.62087(12) 0.3000(2) 0.57663(13) 0.0160(4) Uani 1 1 d . . .
C1 C 0.41611(14) 0.4625(3) 0.43516(16) 0.0159(5) Uani 1 1 d . . .
C2 C 0.39053(16) 0.6184(3) 0.42412(17) 0.0193(5) Uani 1 1 d . . .
H2 H 0.4200 0.7019 0.4511 0.023 Uiso 1 1 calc R . .
C3 C 0.32242(16) 0.6520(3) 0.37412(16) 0.0192(5) Uani 1 1 d . . .
H3 H 0.3057 0.7584 0.3672 0.023 Uiso 1 1 calc R . .
C4 C 0.27843(15) 0.5321(3) 0.33404(16) 0.0194(5) Uani 1 1 d . . .
H4 H 0.2322 0.5561 0.2993 0.023 Uiso 1 1 calc R . .
C5 C 0.30275(15) 0.3755(3) 0.34531(16) 0.0187(5) Uani 1 1 d . . .
H5 H 0.2728 0.2929 0.3180 0.022 Uiso 1 1 calc R . .
C6 C 0.37089(15) 0.3390(3) 0.39644(16) 0.0156(5) Uani 1 1 d . . .
C7 C 0.39729(15) 0.1714(3) 0.41471(16) 0.0168(5) Uani 1 1 d . . .
C8 C 0.46794(14) 0.1763(3) 0.48081(15) 0.0180(6) Uani 1 1 d . . .
H8A H 0.5099 0.1044 0.4580 0.022 Uiso 1 1 calc R . .
H8B H 0.4500 0.1356 0.5405 0.022 Uiso 1 1 calc R . .
C9 C 0.32785(16) 0.0785(3) 0.45864(18) 0.0227(6) Uani 1 1 d . . .
H9A H 0.2838 0.0695 0.4151 0.034 Uiso 1 1 calc R . .
H9B H 0.3094 0.1342 0.5131 0.034 Uiso 1 1 calc R . .
H9C H 0.3463 -0.0272 0.4756 0.034 Uiso 1 1 calc R . .
C10 C 0.42157(17) 0.0880(3) 0.32607(17) 0.0220(6) Uani 1 1 d . . .
H10A H 0.4664 0.1442 0.2982 0.033 Uiso 1 1 calc R . .
H10B H 0.3763 0.0873 0.2839 0.033 Uiso 1 1 calc R . .
H10C H 0.4375 -0.0208 0.3395 0.033 Uiso 1 1 calc R . .
C11 C 0.55475(17) 0.6896(3) 0.61346(17) 0.0245(6) Uani 1 1 d . . .
H11A H 0.5483 0.8051 0.6071 0.029 Uiso 1 1 calc R . .
H11B H 0.5947 0.6700 0.6618 0.029 Uiso 1 1 calc R . .
C12 C 0.47501(17) 0.6167(3) 0.6416(2) 0.0250(6) Uani 1 1 d . . .
H12A H 0.4639 0.6450 0.7057 0.030 Uiso 1 1 calc R . .
H12B H 0.4321 0.6626 0.6037 0.030 Uiso 1 1 calc R . .
C13 C 0.52748(17) 0.3637(3) 0.70150(18) 0.0249(6) Uani 1 1 d . . .
H13A H 0.5603 0.4464 0.7308 0.030 Uiso 1 1 calc R . .
H13B H 0.4945 0.3136 0.7493 0.030 Uiso 1 1 calc R . .
C14 C 0.58189(15) 0.2412(3) 0.66098(16) 0.0211(5) Uani 1 1 d . . .
H14A H 0.6233 0.2124 0.7060 0.025 Uiso 1 1 calc R . .
H14B H 0.5507 0.1451 0.6468 0.025 Uiso 1 1 calc R . .
C15 C 0.67819(16) 0.4310(3) 0.59759(18) 0.0225(6) Uani 1 1 d . . .
H15A H 0.6693 0.4681 0.6606 0.027 Uiso 1 1 calc R . .
H15B H 0.7335 0.3906 0.5934 0.027 Uiso 1 1 calc R . .
C16 C 0.66827(15) 0.5661(3) 0.53352(19) 0.0215(5) Uani 1 1 d . . .
H16A H 0.7026 0.6543 0.5539 0.026 Uiso 1 1 calc R . .
H16B H 0.6868 0.5334 0.4724 0.026 Uiso 1 1 calc R . .
C17 C 0.58354(17) 0.7411(3) 0.45193(17) 0.0242(6) Uani 1 1 d . . .
H17A H 0.5321 0.7960 0.4515 0.036 Uiso 1 1 calc R . .
H17B H 0.5914 0.6874 0.3936 0.036 Uiso 1 1 calc R . .
H17C H 0.6265 0.8177 0.4614 0.036 Uiso 1 1 calc R . .
C18 C 0.38943(17) 0.3900(3) 0.6495(2) 0.0248(6) Uani 1 1 d . . .
H18A H 0.3858 0.2748 0.6458 0.037 Uiso 1 1 calc R . .
H18B H 0.3543 0.4375 0.6038 0.037 Uiso 1 1 calc R . .
H18C H 0.3731 0.4248 0.7103 0.037 Uiso 1 1 calc R . .
C19 C 0.66450(16) 0.1701(3) 0.53176(18) 0.0235(6) Uani 1 1 d . . .
H19A H 0.6885 0.2086 0.4752 0.035 Uiso 1 1 calc R . .
H19B H 0.6274 0.0840 0.5179 0.035 Uiso 1 1 calc R . .
H19C H 0.7065 0.1314 0.5724 0.035 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 0.01418(8) 0.01038(7) 0.01335(7) -0.00072(9) -0.00016(10) 0.00005(6)
Cl1 0.0252(3) 0.0196(3) 0.0213(3) 0.0015(2) 0.0031(3) -0.0019(3)
O1 0.0206(10) 0.0136(8) 0.0143(8) 0.0019(6) 0.0006(7) -0.0011(7)
O2 0.0353(13) 0.0293(11) 0.0531(15) 0.0053(10) 0.0109(11) 0.0117(9)
O3 0.0428(13) 0.0231(11) 0.0696(16) -0.0059(11) -0.0086(12) -0.0103(10)
O4 0.0285(11) 0.0326(12) 0.0421(12) 0.0139(9) 0.0126(9) 0.0026(9)
O5 0.0672(18) 0.0690(16) 0.0244(11) -0.0008(12) -0.0016(12) 0.0044(14)
N1 0.0164(10) 0.0148(10) 0.0201(11) -0.0032(7) -0.0008(8) -0.0006(8)
N2 0.0186(11) 0.0157(10) 0.0171(10) -0.0011(8) 0.0018(8) 0.0015(8)
N3 0.0161(10) 0.0164(10) 0.0153(10) -0.0014(8) 0.0007(8) 0.0010(8)
C1 0.0167(12) 0.0161(11) 0.0149(11) 0.0009(9) -0.0009(9) -0.0001(10)
C2 0.0244(14) 0.0133(12) 0.0203(13) -0.0001(9) -0.0001(11) -0.0006(10)
C3 0.0217(13) 0.0171(12) 0.0187(12) 0.0028(10) 0.0034(10) 0.0054(10)
C4 0.0185(13) 0.0225(13) 0.0172(12) 0.0018(10) -0.0011(10) 0.0029(10)
C5 0.0197(13) 0.0182(12) 0.0183(12) 0.0008(9) -0.0009(10) -0.0030(10)
C6 0.0156(13) 0.0146(12) 0.0167(12) 0.0000(9) 0.0010(9) -0.0006(10)
C7 0.0214(13) 0.0108(11) 0.0182(12) -0.0003(9) -0.0015(10) -0.0024(10)
C8 0.0205(12) 0.0108(10) 0.0228(17) 0.0005(9) -0.0024(9) -0.0016(9)
C9 0.0226(14) 0.0178(13) 0.0278(13) 0.0029(10) 0.0003(11) -0.0047(11)
C10 0.0267(15) 0.0179(13) 0.0215(13) -0.0006(10) -0.0017(11) 0.0025(11)
C11 0.0306(15) 0.0165(13) 0.0264(14) -0.0092(10) 0.0005(12) -0.0014(12)
C12 0.0315(17) 0.0186(14) 0.0249(14) -0.0072(11) 0.0046(11) 0.0029(11)
C13 0.0284(16) 0.0322(15) 0.0142(12) 0.0041(10) 0.0015(10) 0.0055(12)
C14 0.0237(14) 0.0228(13) 0.0166(12) 0.0034(10) -0.0005(10) -0.0009(11)
C15 0.0184(13) 0.0237(13) 0.0253(13) -0.0036(11) -0.0049(11) -0.0023(11)
C16 0.0161(13) 0.0180(12) 0.0303(13) -0.0005(10) 0.0004(10) -0.0024(10)
C17 0.0291(15) 0.0174(12) 0.0262(14) 0.0049(10) -0.0017(11) -0.0046(12)
C18 0.0224(15) 0.0250(14) 0.0270(15) 0.0020(11) 0.0076(12) 0.0003(11)
C19 0.0204(13) 0.0235(13) 0.0267(12) -0.0036(10) -0.0036(10) 0.0072(11)
_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 2.0185(17) . ?
Pd1 C1 2.024(2) . ?
Pd1 C8 2.061(2) . ?
Pd1 N2 2.117(2) . ?
Pd1 N3 2.227(2) . ?
Pd1 N1 2.263(2) . ?
Cl1 O4 1.432(2) . ?
Cl1 O2 1.435(2) . ?
Cl1 O5 1.436(2) . ?
Cl1 O3 1.444(2) . ?
O1 H1 0.8400 . ?
N1 C17 1.481(3) . ?
N1 C11 1.484(3) . ?
N1 C16 1.490(3) . ?
N2 C18 1.488(3) . ?
N2 C12 1.505(3) . ?
N2 C13 1.512(3) . ?
N3 C19 1.478(3) . ?
N3 C14 1.488(3) . ?
N3 C15 1.501(3) . ?
C1 C2 1.399(3) . ?
C1 C6 1.413(3) . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.512(3) . ?
C7 C8 1.533(3) . ?
C7 C10 1.538(3) . ?
C7 C9 1.547(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.530(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.505(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.492(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
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 . ?
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
O1 Pd1 C1 87.29(9) . . ?
O1 Pd1 C8 90.02(8) . . ?
C1 Pd1 C8 81.36(9) . . ?
O1 Pd1 N2 171.73(8) . . ?
C1 Pd1 N2 95.18(9) . . ?
C8 Pd1 N2 98.15(9) . . ?
O1 Pd1 N3 95.83(7) . . ?
C1 Pd1 N3 173.45(8) . . ?
C8 Pd1 N3 92.85(8) . . ?
N2 Pd1 N3 82.54(8) . . ?
O1 Pd1 N1 89.37(7) . . ?
C1 Pd1 N1 105.25(9) . . ?
C8 Pd1 N1 173.32(8) . . ?
N2 Pd1 N1 82.37(8) . . ?
N3 Pd1 N1 80.60(7) . . ?
O4 Cl1 O2 110.34(12) . . ?
O4 Cl1 O5 109.24(15) . . ?
O2 Cl1 O5 110.70(14) . . ?
O4 Cl1 O3 109.25(14) . . ?
O2 Cl1 O3 108.86(14) . . ?
O5 Cl1 O3 108.41(15) . . ?
Pd1 O1 H1 109.5 . . ?
C17 N1 C11 112.32(19) . . ?
C17 N1 C16 106.3(2) . . ?
C11 N1 C16 112.3(2) . . ?
C17 N1 Pd1 116.08(15) . . ?
C11 N1 Pd1 107.64(15) . . ?
C16 N1 Pd1 101.78(14) . . ?
C18 N2 C12 106.7(2) . . ?
C18 N2 C13 109.4(2) . . ?
C12 N2 C13 110.6(2) . . ?
C18 N2 Pd1 115.94(16) . . ?
C12 N2 Pd1 104.49(16) . . ?
C13 N2 Pd1 109.51(15) . . ?
C19 N3 C14 109.86(19) . . ?
C19 N3 C15 109.04(19) . . ?
C14 N3 C15 110.99(19) . . ?
C19 N3 Pd1 115.67(15) . . ?
C14 N3 Pd1 101.74(14) . . ?
C15 N3 Pd1 109.39(15) . . ?
C2 C1 C6 119.3(2) . . ?
C2 C1 Pd1 124.96(18) . . ?
C6 C1 Pd1 115.74(17) . . ?
C3 C2 C1 120.5(2) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 120.8(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.4(2) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 120.7(2) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 119.4(2) . . ?
C5 C6 C7 122.7(2) . . ?
C1 C6 C7 117.9(2) . . ?
C6 C7 C8 108.26(19) . . ?
C6 C7 C10 111.0(2) . . ?
C8 C7 C10 110.2(2) . . ?
C6 C7 C9 109.4(2) . . ?
C8 C7 C9 109.32(19) . . ?
C10 C7 C9 108.6(2) . . ?
C7 C8 Pd1 114.92(16) . . ?
C7 C8 H8A 108.5 . . ?
Pd1 C8 H8A 108.5 . . ?
C7 C8 H8B 108.5 . . ?
Pd1 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 112.0(2) . . ?
N1 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
N1 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N2 C12 C11 113.3(2) . . ?
N2 C12 H12A 108.9 . . ?
C11 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C11 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C14 C13 N2 113.2(2) . . ?
C14 C13 H13A 108.9 . . ?
N2 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
N2 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
N3 C14 C13 111.4(2) . . ?
N3 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
N3 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 N3 111.5(2) . . ?
C16 C15 H15A 109.3 . . ?
N3 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
N3 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
N1 C16 C15 113.6(2) . . ?
N1 C16 H16A 108.9 . . ?
C15 C16 H16A 108.9 . . ?
N1 C16 H16B 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
O1 Pd1 N1 C17 46.41(18) . . . . ?
C1 Pd1 N1 C17 -40.61(19) . . . . ?
N2 Pd1 N1 C17 -133.93(19) . . . . ?
N3 Pd1 N1 C17 142.42(19) . . . . ?
O1 Pd1 N1 C11 173.23(16) . . . . ?
C1 Pd1 N1 C11 86.21(17) . . . . ?
N2 Pd1 N1 C11 -7.11(16) . . . . ?
N3 Pd1 N1 C11 -90.75(16) . . . . ?
O1 Pd1 N1 C16 -68.56(15) . . . . ?
C1 Pd1 N1 C16 -155.58(15) . . . . ?
N2 Pd1 N1 C16 111.10(16) . . . . ?
N3 Pd1 N1 C16 27.45(15) . . . . ?
C1 Pd1 N2 C18 41.39(18) . . . . ?
C8 Pd1 N2 C18 -40.61(18) . . . . ?
N3 Pd1 N2 C18 -132.43(18) . . . . ?
N1 Pd1 N2 C18 146.12(18) . . . . ?
C1 Pd1 N2 C12 -75.75(17) . . . . ?
C8 Pd1 N2 C12 -157.74(16) . . . . ?
N3 Pd1 N2 C12 110.44(16) . . . . ?
N1 Pd1 N2 C12 28.99(16) . . . . ?
C1 Pd1 N2 C13 165.76(17) . . . . ?
C8 Pd1 N2 C13 83.77(17) . . . . ?
N3 Pd1 N2 C13 -8.05(16) . . . . ?
N1 Pd1 N2 C13 -89.50(17) . . . . ?
O1 Pd1 N3 C19 -38.62(17) . . . . ?
C8 Pd1 N3 C19 51.68(18) . . . . ?
N2 Pd1 N3 C19 149.54(18) . . . . ?
N1 Pd1 N3 C19 -127.01(17) . . . . ?
O1 Pd1 N3 C14 -157.62(14) . . . . ?
C8 Pd1 N3 C14 -67.31(15) . . . . ?
N2 Pd1 N3 C14 30.54(14) . . . . ?
N1 Pd1 N3 C14 113.99(15) . . . . ?
O1 Pd1 N3 C15 84.93(15) . . . . ?
C8 Pd1 N3 C15 175.24(16) . . . . ?
N2 Pd1 N3 C15 -86.91(16) . . . . ?
N1 Pd1 N3 C15 -3.46(15) . . . . ?
O1 Pd1 C1 C2 -97.5(2) . . . . ?
C8 Pd1 C1 C2 172.1(2) . . . . ?
N2 Pd1 C1 C2 74.6(2) . . . . ?
N1 Pd1 C1 C2 -8.9(2) . . . . ?
O1 Pd1 C1 C6 80.20(18) . . . . ?
C8 Pd1 C1 C6 -10.23(18) . . . . ?
N2 Pd1 C1 C6 -107.71(18) . . . . ?
N1 Pd1 C1 C6 168.81(17) . . . . ?
C6 C1 C2 C3 -1.3(4) . . . . ?
Pd1 C1 C2 C3 176.29(19) . . . . ?
C1 C2 C3 C4 -0.1(4) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 C6 -0.1(4) . . . . ?
C4 C5 C6 C1 -1.3(4) . . . . ?
C4 C5 C6 C7 176.8(2) . . . . ?
C2 C1 C6 C5 2.0(4) . . . . ?
Pd1 C1 C6 C5 -175.82(18) . . . . ?
C2 C1 C6 C7 -176.2(2) . . . . ?
Pd1 C1 C6 C7 6.0(3) . . . . ?
C5 C6 C7 C8 -173.9(2) . . . . ?
C1 C6 C7 C8 4.3(3) . . . . ?
C5 C6 C7 C10 65.0(3) . . . . ?
C1 C6 C7 C10 -116.8(2) . . . . ?
C5 C6 C7 C9 -54.8(3) . . . . ?
C1 C6 C7 C9 123.3(2) . . . . ?
C6 C7 C8 Pd1 -12.4(2) . . . . ?
C10 C7 C8 Pd1 109.17(19) . . . . ?
C9 C7 C8 Pd1 -131.54(17) . . . . ?
O1 Pd1 C8 C7 -74.61(17) . . . . ?
C1 Pd1 C8 C7 12.65(17) . . . . ?
N2 Pd1 C8 C7 106.70(17) . . . . ?
N3 Pd1 C8 C7 -170.44(17) . . . . ?
C17 N1 C11 C12 111.9(2) . . . . ?
C16 N1 C11 C12 -128.3(2) . . . . ?
Pd1 N1 C11 C12 -17.1(2) . . . . ?
C18 N2 C12 C11 -172.3(2) . . . . ?
C13 N2 C12 C11 68.8(3) . . . . ?
Pd1 N2 C12 C11 -49.0(2) . . . . ?
N1 C11 C12 N2 45.6(3) . . . . ?
C18 N2 C13 C14 111.1(2) . . . . ?
C12 N2 C13 C14 -131.6(2) . . . . ?
Pd1 N2 C13 C14 -17.0(3) . . . . ?
C19 N3 C14 C13 -171.9(2) . . . . ?
C15 N3 C14 C13 67.4(3) . . . . ?
Pd1 N3 C14 C13 -48.9(2) . . . . ?
N2 C13 C14 N3 47.0(3) . . . . ?
C19 N3 C15 C16 104.9(3) . . . . ?
C14 N3 C15 C16 -134.0(2) . . . . ?
Pd1 N3 C15 C16 -22.5(2) . . . . ?
C17 N1 C16 C15 -172.6(2) . . . . ?
C11 N1 C16 C15 64.2(3) . . . . ?
Pd1 N1 C16 C15 -50.6(2) . . . . ?
N3 C15 C16 N1 52.1(3) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C12 H12A O1 0.99 2.58 3.526(3) 160.6 2_665
C15 H15B O3 0.99 2.60 3.309(3) 128.3 3_565
C17 H17B O1 0.98 2.62 3.241(3) 121.6 .
C18 H18A O2 0.98 2.62 3.358(3) 132.3 1_545
C18 H18A O4 0.98 2.58 3.522(3) 160.4 1_545
C19 H19C O3 0.98 2.62 3.481(3) 146.8 3_565
O1 H1 O5 0.84 2.34 3.167(3) 168.4 2_664
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 27.58
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max 0.273
_refine_diff_density_min -0.516
_refine_diff_density_rms 0.060
_iucr_refine_instructions_details
;
TITL lm15612/lt/smart/Fengrui/Me3tacnPdIVOH in Pca2(1)
CELL 0.71073 16.7685 8.4769 14.7041 90.000 90.000 90.000
ZERR 4.00 0.0045 0.0024 0.0043 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 0.5+Z
SYMM 0.5+X, -Y, Z
SYMM 0.5-X, Y, 0.5+Z
SFAC C H N O CL PD
UNIT 76 136 12 20 4 4
TEMP -173.140
SIZE 0.139 0.148 0.181
OMIT -3.0
L.S. 10
PLAN 5
EQIV $1 -x+1, -y+1, z+1/2
HTAB C12 O1_$1
EQIV $2 x+1/2, -y+1, z
HTAB C15 O3_$2
HTAB C17 O1
EQIV $3 x, y-1, z
HTAB C18 O2_$3
HTAB C18 O4_$3
HTAB C19 O3_$2
EQIV $4 -x+1, -y+1, z-1/2
HTAB O1 O5_$4
acta
wpdb -2
list 4
bond $h
htab
conf
more 2
fmap 2
WGHT 0.023900 0.313000
FVAR 0.12600
PD1 6 0.517330 0.396461 0.499806 11.00000 0.01418 0.01038 =
0.01335 -0.00072 -0.00016 0.00005
CL1 5 0.339192 0.952540 0.729491 11.00000 0.02516 0.01957 =
0.02129 0.00155 0.00308 -0.00187
O1 4 0.569084 0.383226 0.376104 11.00000 0.02062 0.01356 =
0.01426 0.00190 0.00057 -0.00109
AFIX 147
H1 2 0.591693 0.295355 0.370398 11.00000 -1.50000
AFIX 0
rem located H1 2 0.589574 0.292207 0.379915 11.00000 0.04634
O2 4 0.281644 1.072925 0.709606 11.00000 0.03532 0.02929 =
0.05313 0.00533 0.01087 0.01167
O3 4 0.306656 0.801346 0.703521 11.00000 0.04284 0.02307 =
0.06958 -0.00587 -0.00856 -0.01025
O4 4 0.411291 0.980216 0.679858 11.00000 0.02846 0.03256 =
0.04209 0.01388 0.01264 0.00257
O5 4 0.356735 0.948680 0.825050 11.00000 0.06724 0.06903 =
0.02438 -0.00076 -0.00162 0.00444
N1 3 0.584469 0.623408 0.526381 11.00000 0.01643 0.01476 =
0.02010 -0.00322 -0.00081 -0.00058
N2 3 0.473128 0.439956 0.632282 11.00000 0.01862 0.01574 =
0.01709 -0.00107 0.00176 0.00149
N3 3 0.620868 0.300025 0.576629 11.00000 0.01612 0.01639 =
0.01534 -0.00139 0.00070 0.00096
C1 1 0.416108 0.462516 0.435162 11.00000 0.01670 0.01610 =
0.01495 0.00090 -0.00085 -0.00006
C2 1 0.390528 0.618382 0.424122 11.00000 0.02438 0.01332 =
0.02033 -0.00015 -0.00007 -0.00058
AFIX 43
H2 2 0.420006 0.701896 0.451067 11.00000 -1.20000
AFIX 0
C3 1 0.322424 0.652021 0.374117 11.00000 0.02169 0.01710 =
0.01867 0.00283 0.00336 0.00538
AFIX 43
H3 2 0.305725 0.758446 0.367245 11.00000 -1.20000
AFIX 0
C4 1 0.278433 0.532078 0.334039 11.00000 0.01847 0.02253 =
0.01722 0.00180 -0.00108 0.00292
AFIX 43
H4 2 0.232248 0.556099 0.299279 11.00000 -1.20000
AFIX 0
C5 1 0.302745 0.375466 0.345311 11.00000 0.01970 0.01816 =
0.01826 0.00084 -0.00091 -0.00298
AFIX 43
H5 2 0.272785 0.292939 0.318050 11.00000 -1.20000
AFIX 0
C6 1 0.370887 0.339008 0.396437 11.00000 0.01557 0.01461 =
0.01666 0.00004 0.00099 -0.00062
C7 1 0.397293 0.171387 0.414715 11.00000 0.02142 0.01076 =
0.01818 -0.00029 -0.00151 -0.00241
C8 1 0.467941 0.176326 0.480811 11.00000 0.02047 0.01081 =
0.02283 0.00046 -0.00237 -0.00164
AFIX 23
H8A 2 0.509927 0.104384 0.457998 11.00000 -1.20000
H8B 2 0.450018 0.135558 0.540501 11.00000 -1.20000
AFIX 0
C9 1 0.327846 0.078456 0.458643 11.00000 0.02265 0.01778 =
0.02776 0.00292 0.00035 -0.00471
AFIX 137
H9A 2 0.283849 0.069464 0.415081 11.00000 -1.50000
H9B 2 0.309364 0.134241 0.513081 11.00000 -1.50000
H9C 2 0.346338 -0.027199 0.475592 11.00000 -1.50000
AFIX 0
C10 1 0.421566 0.087959 0.326067 11.00000 0.02667 0.01789 =
0.02152 -0.00060 -0.00174 0.00252
AFIX 137
H10A 2 0.466424 0.144189 0.298243 11.00000 -1.50000
H10B 2 0.376288 0.087337 0.283928 11.00000 -1.50000
H10C 2 0.437454 -0.020814 0.339536 11.00000 -1.50000
AFIX 0
C11 1 0.554747 0.689556 0.613463 11.00000 0.03057 0.01646 =
0.02637 -0.00918 0.00053 -0.00135
AFIX 23
H11A 2 0.548273 0.805113 0.607091 11.00000 -1.20000
H11B 2 0.594660 0.670037 0.661781 11.00000 -1.20000
AFIX 0
C12 1 0.475014 0.616747 0.641647 11.00000 0.03151 0.01862 =
0.02486 -0.00720 0.00462 0.00286
AFIX 23
H12A 2 0.463932 0.645028 0.705737 11.00000 -1.20000
H12B 2 0.432098 0.662617 0.603718 11.00000 -1.20000
AFIX 0
C13 1 0.527480 0.363658 0.701503 11.00000 0.02844 0.03216 =
0.01416 0.00408 0.00147 0.00546
AFIX 23
H13A 2 0.560263 0.446436 0.730796 11.00000 -1.20000
H13B 2 0.494488 0.313644 0.749316 11.00000 -1.20000
AFIX 0
C14 1 0.581895 0.241187 0.660985 11.00000 0.02374 0.02282 =
0.01663 0.00342 -0.00047 -0.00087
AFIX 23
H14A 2 0.623340 0.212378 0.705967 11.00000 -1.20000
H14B 2 0.550741 0.145104 0.646751 11.00000 -1.20000
AFIX 0
C15 1 0.678195 0.431025 0.597587 11.00000 0.01842 0.02372 =
0.02527 -0.00364 -0.00488 -0.00231
AFIX 23
H15A 2 0.669325 0.468090 0.660628 11.00000 -1.20000
H15B 2 0.733466 0.390612 0.593415 11.00000 -1.20000
AFIX 0
C16 1 0.668266 0.566104 0.533515 11.00000 0.01614 0.01797 =
0.03031 -0.00054 0.00036 -0.00236
AFIX 23
H16A 2 0.702579 0.654297 0.553935 11.00000 -1.20000
H16B 2 0.686792 0.533427 0.472426 11.00000 -1.20000
AFIX 0
C17 1 0.583540 0.741080 0.451934 11.00000 0.02910 0.01739 =
0.02622 0.00494 -0.00171 -0.00463
AFIX 137
H17A 2 0.532101 0.795952 0.451536 11.00000 -1.50000
H17B 2 0.591400 0.687450 0.393576 11.00000 -1.50000
H17C 2 0.626505 0.817701 0.461430 11.00000 -1.50000
AFIX 0
C18 1 0.389429 0.390015 0.649495 11.00000 0.02242 0.02495 =
0.02704 0.00203 0.00762 0.00029
AFIX 137
H18A 2 0.385757 0.274816 0.645773 11.00000 -1.50000
H18B 2 0.354311 0.437510 0.603796 11.00000 -1.50000
H18C 2 0.373081 0.424821 0.710255 11.00000 -1.50000
AFIX 0
C19 1 0.664498 0.170058 0.531756 11.00000 0.02042 0.02352 =
0.02666 -0.00362 -0.00364 0.00721
AFIX 137
H19A 2 0.688508 0.208644 0.475211 11.00000 -1.50000
H19B 2 0.627406 0.083991 0.517940 11.00000 -1.50000
H19C 2 0.706509 0.131362 0.572365 11.00000 -1.50000
HKLF 4
REM lm15612/lt/smart/Fengrui/Me3tacnPdIVOH in Pca2(1)
REM R1 = 0.0215 for 4446 Fo > 4sig(Fo) and 0.0247 for all 4780 data
REM 268 parameters refined using 1 restraints
END
WGHT 0.0239 0.3129
REM Highest difference peak 0.273, deepest hole -0.516, 1-sigma level 0.060
Q1 1 0.5828 0.3578 0.3507 11.00000 0.05 0.27
Q2 1 0.4737 0.3982 0.5764 11.00000 0.05 0.27
Q3 1 0.5299 0.3863 0.3805 11.00000 0.05 0.26
Q4 1 0.5776 0.3379 0.5415 11.00000 0.05 0.26
Q5 1 0.4754 0.4016 0.4253 11.00000 0.05 0.24
;
_database_code_depnum_ccdc_archive 'CCDC 972257'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_l23312
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C19 H33 I N3 Pd, I'
_chemical_formula_sum 'C19 H33 I2 N3 Pd'
_chemical_formula_weight 663.68
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M Pca2(1)
_symmetry_space_group_name_Hall 'P 2c -2ac'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
_cell_length_a 16.110(2)
_cell_length_b 8.7912(14)
_cell_length_c 15.537(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2200.3(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9050
_cell_measurement_theta_min 2.32
_cell_measurement_theta_max 39.01
_exptl_crystal_description rectangular
_exptl_crystal_colour red
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas no
_exptl_crystal_density_diffrn 2.003
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1280
_exptl_absorpt_coefficient_mu 3.657
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.3363
_exptl_absorpt_correction_T_max 0.6304
_exptl_absorpt_process_details 'sadabs v2008/1'
_exptl_special_details
;
All H atoms were added in their calculated positions
and were treated using appropriate riding models.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 159143
_diffrn_reflns_av_R_equivalents 0.0409
_diffrn_reflns_av_sigmaI/netI 0.0223
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 2.32
_diffrn_reflns_theta_max 39.06
_reflns_number_total 12564
_reflns_number_gt 12029
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.7295P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.010(8)
_refine_ls_number_reflns 12564
_refine_ls_number_parameters 238
_refine_ls_number_restraints 10
_refine_ls_R_factor_all 0.0218
_refine_ls_R_factor_gt 0.0196
_refine_ls_wR_factor_ref 0.0391
_refine_ls_wR_factor_gt 0.0385
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_restrained_S_all 1.080
_refine_ls_shift/su_max 0.008
_refine_ls_shift/su_mean 0.001
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 0.76466(2) 0.65269(3) 0.978732(10) 0.00786(3) Uani 0.967(2) 1 d PDU A 1
I1 I 0.858396(13) 0.50876(5) 1.086958(9) 0.01060(4) Uani 0.967(2) 1 d PDU A 1
Pd1' Pd 0.7490(5) 0.6673(7) 0.9774(4) 0.00786(3) Uani 0.033(2) 1 d PDU A 2
I1' I 0.8504(3) 0.5433(11) 1.0837(4) 0.01060(4) Uani 0.033(2) 1 d PDU A 2
I2 I 0.523695(6) 0.272226(13) 0.746431(9) 0.01809(2) Uani 1 1 d . . .
N1 N 0.78306(8) 0.49998(15) 0.86583(9) 0.0120(2) Uani 1 1 d D . .
N2 N 0.67651(8) 0.76007(16) 0.88983(9) 0.0142(2) Uani 1 1 d D . .
C3 C 0.80955(9) 0.93278(17) 1.06821(10) 0.0128(3) Uani 1 1 d . A .
N3 N 0.65420(8) 0.49029(15) 0.99667(10) 0.0128(2) Uani 1 1 d D . .
C4 C 0.74935(9) 0.81765(16) 1.06791(10) 0.0106(2) Uani 1 1 d D . .
C17 C 0.62694(9) 0.45056(18) 1.08472(13) 0.0167(3) Uani 1 1 d . A .
H17A H 0.6005 0.5391 1.1114 0.025 Uiso 1 1 calc R . .
H17B H 0.6751 0.4198 1.1190 0.025 Uiso 1 1 calc R . .
H17C H 0.5871 0.3664 1.0820 0.025 Uiso 1 1 calc R . .
C5 C 0.67981(9) 0.82989(17) 1.12080(11) 0.0129(2) Uani 1 1 d . A .
H5 H 0.6396 0.7508 1.1216 0.016 Uiso 1 1 calc R . .
C1 C 0.86537(9) 0.78608(18) 0.94718(12) 0.0141(3) Uani 1 1 d D . .
H1A H 0.9151 0.7202 0.9437 0.017 Uiso 1 1 calc R A 1
H1B H 0.8560 0.8298 0.8892 0.017 Uiso 1 1 calc R A 1
C14 C 0.72133(9) 0.37421(18) 0.86760(11) 0.0152(3) Uani 1 1 d . A .
H14A H 0.7482 0.2795 0.8474 0.018 Uiso 1 1 calc R . .
H14B H 0.6755 0.3984 0.8274 0.018 Uiso 1 1 calc R . .
C13 C 0.68583(10) 0.34798(18) 0.95627(12) 0.0156(3) Uani 1 1 d . A .
H13A H 0.6399 0.2735 0.9522 0.019 Uiso 1 1 calc R . .
H13B H 0.7294 0.3036 0.9936 0.019 Uiso 1 1 calc R . .
C15 C 0.86781(9) 0.43649(18) 0.85649(11) 0.0136(2) Uani 1 1 d . A .
H15A H 0.8707 0.3748 0.8040 0.020 Uiso 1 1 calc R . .
H15B H 0.8808 0.3729 0.9065 0.020 Uiso 1 1 calc R . .
H15C H 0.9080 0.5199 0.8527 0.020 Uiso 1 1 calc R . .
C2 C 0.88346(9) 0.91625(18) 1.00985(12) 0.0144(3) Uani 1 1 d . A .
C11 C 0.59388(9) 0.7223(2) 0.92771(12) 0.0164(3) Uani 1 1 d D A .
H11A H 0.5499 0.7553 0.8873 0.020 Uiso 1 1 calc R . .
H11B H 0.5868 0.7803 0.9818 0.020 Uiso 1 1 calc R . .
C9 C 0.76735(10) 0.6042(2) 0.79239(11) 0.0163(3) Uani 1 1 d . A .
H9A H 0.7663 0.5447 0.7383 0.020 Uiso 1 1 calc R . .
H9B H 0.8133 0.6786 0.7883 0.020 Uiso 1 1 calc R . .
C8 C 0.79861(10) 1.05919(18) 1.12166(12) 0.0160(3) Uani 1 1 d . . .
H8 H 0.8395 1.1370 1.1228 0.019 Uiso 1 1 calc R A .
C18 C 0.96261(10) 0.8879(2) 1.06316(14) 0.0224(4) Uani 1 1 d . . .
H18A H 0.9716 0.9734 1.1025 0.034 Uiso 1 1 calc R A .
H18B H 1.0103 0.8782 1.0244 0.034 Uiso 1 1 calc R . .
H18C H 0.9562 0.7939 1.0964 0.034 Uiso 1 1 calc R . .
C6 C 0.66909(10) 0.95785(19) 1.17255(11) 0.0159(3) Uani 1 1 d . . .
H6 H 0.6210 0.9668 1.2075 0.019 Uiso 1 1 calc R A .
C12 C 0.58291(9) 0.5543(2) 0.94655(12) 0.0169(3) Uani 1 1 d . A .
H12A H 0.5310 0.5393 0.9796 0.020 Uiso 1 1 calc R . .
H12B H 0.5776 0.4983 0.8916 0.020 Uiso 1 1 calc R . .
C10 C 0.68602(11) 0.6886(2) 0.80219(11) 0.0181(3) Uani 1 1 d . A .
H10A H 0.6827 0.7691 0.7577 0.022 Uiso 1 1 calc R . .
H10B H 0.6396 0.6170 0.7924 0.022 Uiso 1 1 calc R . .
C7 C 0.72825(11) 1.07191(19) 1.17322(12) 0.0172(3) Uani 1 1 d . A .
H7 H 0.7209 1.1588 1.2088 0.021 Uiso 1 1 calc R . .
C19 C 0.89794(12) 1.0619(2) 0.95696(15) 0.0232(4) Uani 1 1 d . . .
H19A H 0.8467 1.0894 0.9268 0.035 Uiso 1 1 calc R A .
H19B H 0.9422 1.0440 0.9149 0.035 Uiso 1 1 calc R . .
H19C H 0.9142 1.1449 0.9955 0.035 Uiso 1 1 calc R . .
C16 C 0.68254(12) 0.9272(2) 0.88220(12) 0.0200(3) Uani 1 1 d . A .
H16A H 0.6354 0.9656 0.8488 0.030 Uiso 1 1 calc R . .
H16B H 0.7344 0.9541 0.8530 0.030 Uiso 1 1 calc R . .
H16C H 0.6818 0.9729 0.9397 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 0.00644(7) 0.00846(5) 0.00869(4) -0.00132(4) 0.00013(5) -0.00007(5)
I1 0.01056(4) 0.01021(9) 0.01103(4) -0.00028(5) -0.00018(4) 0.00066(5)
Pd1' 0.00644(7) 0.00846(5) 0.00869(4) -0.00132(4) 0.00013(5) -0.00007(5)
I1' 0.01056(4) 0.01021(9) 0.01103(4) -0.00028(5) -0.00018(4) 0.00066(5)
I2 0.01093(3) 0.02389(5) 0.01945(5) -0.00863(4) 0.00000(4) -0.00067(3)
N1 0.0100(5) 0.0150(5) 0.0112(6) -0.0031(4) 0.0002(4) 0.0010(4)
N2 0.0128(5) 0.0178(6) 0.0121(6) -0.0017(5) -0.0009(4) 0.0039(4)
C3 0.0113(5) 0.0102(5) 0.0170(7) -0.0009(5) -0.0013(5) -0.0011(4)
N3 0.0101(4) 0.0137(5) 0.0145(6) -0.0043(4) 0.0010(4) -0.0025(4)
C4 0.0107(5) 0.0095(5) 0.0118(6) -0.0009(4) 0.0001(4) -0.0003(4)
C17 0.0159(6) 0.0179(6) 0.0165(7) -0.0041(6) 0.0037(6) -0.0072(5)
C5 0.0123(5) 0.0139(6) 0.0126(7) -0.0025(5) 0.0012(5) -0.0012(4)
C1 0.0123(6) 0.0137(6) 0.0164(7) 0.0001(5) 0.0042(5) -0.0021(4)
C14 0.0120(6) 0.0167(6) 0.0169(7) -0.0084(6) -0.0002(5) -0.0021(5)
C13 0.0131(6) 0.0139(6) 0.0198(8) -0.0070(5) 0.0028(5) -0.0040(5)
C15 0.0105(5) 0.0157(6) 0.0146(7) -0.0023(5) 0.0012(5) 0.0024(4)
C2 0.0105(5) 0.0110(6) 0.0216(8) 0.0004(5) 0.0022(5) -0.0027(4)
C11 0.0103(5) 0.0223(7) 0.0164(7) -0.0042(6) -0.0014(5) 0.0050(5)
C9 0.0157(6) 0.0229(7) 0.0103(6) -0.0022(5) -0.0012(5) 0.0039(5)
C8 0.0174(6) 0.0121(6) 0.0183(8) -0.0045(5) -0.0026(5) -0.0009(5)
C18 0.0120(6) 0.0179(7) 0.0373(11) -0.0041(7) -0.0044(6) -0.0011(5)
C6 0.0173(6) 0.0168(7) 0.0137(7) -0.0046(5) 0.0022(5) 0.0013(5)
C12 0.0095(5) 0.0228(7) 0.0183(7) -0.0054(6) -0.0005(5) -0.0009(5)
C10 0.0180(7) 0.0255(8) 0.0108(7) -0.0020(6) -0.0025(5) 0.0069(6)
C7 0.0212(7) 0.0133(6) 0.0170(8) -0.0068(5) 0.0003(5) 0.0004(5)
C19 0.0224(8) 0.0140(7) 0.0332(11) 0.0042(6) 0.0085(7) -0.0050(6)
C16 0.0234(7) 0.0182(7) 0.0185(8) 0.0029(6) -0.0012(6) 0.0062(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C4 2.0207(15) . ?
Pd1 C1 2.0610(15) . ?
Pd1 N2 2.1944(14) . ?
Pd1 N1 2.2287(14) . ?
Pd1 N3 2.2983(13) . ?
Pd1 I1 2.5902(3) . ?
Pd1' C4 1.930(6) . ?
Pd1' N2 1.970(8) . ?
Pd1' C1 2.197(6) . ?
Pd1' N3 2.200(6) . ?
Pd1' N1 2.339(7) . ?
Pd1' I1' 2.565(4) . ?
N1 C15 1.4821(19) . ?
N1 C9 1.485(2) . ?
N1 C14 1.487(2) . ?
N2 C16 1.478(2) . ?
N2 C11 1.493(2) . ?
N2 C10 1.507(2) . ?
C3 C8 1.398(2) . ?
C3 C4 1.402(2) . ?
C3 C2 1.504(2) . ?
N3 C17 1.479(2) . ?
N3 C13 1.490(2) . ?
N3 C12 1.497(2) . ?
C4 C5 1.393(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C5 C6 1.393(2) . ?
C5 H5 0.9500 . ?
C1 C2 1.531(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C14 C13 1.509(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C2 C19 1.539(2) . ?
C2 C18 1.541(2) . ?
C11 C12 1.516(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C9 C10 1.514(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8 C7 1.392(2) . ?
C8 H8 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C6 C7 1.383(2) . ?
C6 H6 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C7 H7 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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
C4 Pd1 C1 81.42(6) . . ?
C4 Pd1 N2 92.52(6) . . ?
C1 Pd1 N2 96.60(6) . . ?
C4 Pd1 N1 171.17(6) . . ?
C1 Pd1 N1 92.91(6) . . ?
N2 Pd1 N1 81.36(5) . . ?
C4 Pd1 N3 105.56(6) . . ?
C1 Pd1 N3 172.63(6) . . ?
N2 Pd1 N3 80.94(6) . . ?
N1 Pd1 N3 79.88(5) . . ?
C4 Pd1 I1 88.66(4) . . ?
C1 Pd1 I1 88.48(5) . . ?
N2 Pd1 I1 174.90(4) . . ?
N1 Pd1 I1 97.99(4) . . ?
N3 Pd1 I1 93.97(4) . . ?
C4 Pd1' N2 102.8(4) . . ?
C4 Pd1' C1 80.1(2) . . ?
N2 Pd1' C1 99.3(3) . . ?
C4 Pd1' N3 112.8(3) . . ?
N2 Pd1' N3 88.6(3) . . ?
C1 Pd1' N3 163.2(4) . . ?
C4 Pd1' N1 165.9(4) . . ?
N2 Pd1' N1 83.5(2) . . ?
C1 Pd1' N1 86.6(3) . . ?
N3 Pd1' N1 79.58(19) . . ?
C4 Pd1' I1' 79.6(3) . . ?
N2 Pd1' I1' 176.2(3) . . ?
C1 Pd1' I1' 78.2(3) . . ?
N3 Pd1' I1' 93.1(2) . . ?
N1 Pd1' I1' 93.5(2) . . ?
C15 N1 C9 108.30(13) . . ?
C15 N1 C14 109.74(12) . . ?
C9 N1 C14 111.03(13) . . ?
C15 N1 Pd1 115.25(10) . . ?
C9 N1 Pd1 102.15(9) . . ?
C14 N1 Pd1 110.14(10) . . ?
C15 N1 Pd1' 121.7(2) . . ?
C9 N1 Pd1' 98.14(19) . . ?
C14 N1 Pd1' 107.26(17) . . ?
C16 N2 C11 108.14(13) . . ?
C16 N2 C10 109.59(14) . . ?
C11 N2 C10 110.75(13) . . ?
C16 N2 Pd1' 115.36(19) . . ?
C11 N2 Pd1' 99.4(2) . . ?
C10 N2 Pd1' 113.0(2) . . ?
C16 N2 Pd1 115.83(11) . . ?
C11 N2 Pd1 103.49(10) . . ?
C10 N2 Pd1 108.88(9) . . ?
C8 C3 C4 119.25(15) . . ?
C8 C3 C2 122.32(14) . . ?
C4 C3 C2 118.42(13) . . ?
C17 N3 C13 107.04(13) . . ?
C17 N3 C12 110.00(12) . . ?
C13 N3 C12 111.04(13) . . ?
C17 N3 Pd1' 119.93(19) . . ?
C13 N3 Pd1' 107.4(2) . . ?
C12 N3 Pd1' 101.3(2) . . ?
C17 N3 Pd1 119.27(10) . . ?
C13 N3 Pd1 101.88(9) . . ?
C12 N3 Pd1 107.30(10) . . ?
C5 C4 C3 119.90(14) . . ?
C5 C4 Pd1' 118.7(2) . . ?
C3 C4 Pd1' 120.0(2) . . ?
C5 C4 Pd1 123.91(11) . . ?
C3 C4 Pd1 115.85(11) . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C4 C5 C6 120.15(14) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C2 C1 Pd1 115.08(11) . . ?
C2 C1 Pd1' 112.4(2) . . ?
C2 C1 H1A 108.5 . . ?
Pd1 C1 H1A 108.5 . . ?
Pd1' C1 H1A 115.1 . . ?
C2 C1 H1B 108.5 . . ?
Pd1 C1 H1B 108.5 . . ?
Pd1' C1 H1B 104.4 . . ?
H1A C1 H1B 107.5 . . ?
N1 C14 C13 112.57(13) . . ?
N1 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
N1 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N3 C13 C14 112.70(14) . . ?
N3 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
N3 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C3 C2 C1 107.77(12) . . ?
C3 C2 C19 111.20(13) . . ?
C1 C2 C19 108.12(16) . . ?
C3 C2 C18 110.30(15) . . ?
C1 C2 C18 112.23(13) . . ?
C19 C2 C18 107.24(14) . . ?
N2 C11 C12 113.36(13) . . ?
N2 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N1 C9 C10 111.89(14) . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C7 C8 C3 120.53(15) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
C2 C18 H18A 109.5 . . ?
C2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C7 C6 C5 120.27(15) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
N3 C12 C11 112.16(13) . . ?
N3 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
N3 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N2 C10 C9 112.54(13) . . ?
N2 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
N2 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C6 C7 C8 119.88(15) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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
C1 Pd1 N1 C15 52.02(12) . . . . ?
N2 Pd1 N1 C15 148.26(12) . . . . ?
N3 Pd1 N1 C15 -129.48(12) . . . . ?
I1 Pd1 N1 C15 -36.85(11) . . . . ?
C1 Pd1 N1 C9 -65.15(10) . . . . ?
N2 Pd1 N1 C9 31.09(9) . . . . ?
N3 Pd1 N1 C9 113.35(10) . . . . ?
I1 Pd1 N1 C9 -154.02(9) . . . . ?
C1 Pd1 N1 C14 176.82(11) . . . . ?
N2 Pd1 N1 C14 -86.94(11) . . . . ?
N3 Pd1 N1 C14 -4.68(10) . . . . ?
I1 Pd1 N1 C14 87.95(10) . . . . ?
C1 Pd1 N1 Pd1' -118.1(12) . . . . ?
N2 Pd1 N1 Pd1' -21.9(12) . . . . ?
N3 Pd1 N1 Pd1' 60.4(12) . . . . ?
I1 Pd1 N1 Pd1' 153.0(12) . . . . ?
C4 Pd1' N1 C15 27.4(16) . . . . ?
N2 Pd1' N1 C15 145.11(17) . . . . ?
C1 Pd1' N1 C15 45.4(3) . . . . ?
N3 Pd1' N1 C15 -125.12(18) . . . . ?
I1' Pd1' N1 C15 -32.6(3) . . . . ?
C4 Pd1' N1 C9 -90.1(15) . . . . ?
N2 Pd1' N1 C9 27.6(2) . . . . ?
C1 Pd1' N1 C9 -72.1(2) . . . . ?
N3 Pd1' N1 C9 117.40(18) . . . . ?
I1' Pd1' N1 C9 -150.1(2) . . . . ?
C4 Pd1' N1 C14 154.8(14) . . . . ?
N2 Pd1' N1 C14 -87.45(19) . . . . ?
C1 Pd1' N1 C14 172.80(17) . . . . ?
N3 Pd1' N1 C14 2.3(2) . . . . ?
I1' Pd1' N1 C14 94.8(3) . . . . ?
C4 Pd1' N1 Pd1 37.9(11) . . . . ?
N2 Pd1' N1 Pd1 155.6(13) . . . . ?
C1 Pd1' N1 Pd1 55.9(11) . . . . ?
N3 Pd1' N1 Pd1 -114.6(13) . . . . ?
I1' Pd1' N1 Pd1 -22.1(11) . . . . ?
C4 Pd1' N2 C16 35.4(3) . . . . ?
C1 Pd1' N2 C16 -46.4(3) . . . . ?
N3 Pd1' N2 C16 148.51(15) . . . . ?
N1 Pd1' N2 C16 -131.82(15) . . . . ?
C4 Pd1' N2 C11 -79.9(3) . . . . ?
C1 Pd1' N2 C11 -161.7(2) . . . . ?
N3 Pd1' N2 C11 33.2(2) . . . . ?
N1 Pd1' N2 C11 112.83(16) . . . . ?
C4 Pd1' N2 C10 162.6(2) . . . . ?
C1 Pd1' N2 C10 80.8(2) . . . . ?
N3 Pd1' N2 C10 -84.3(2) . . . . ?
N1 Pd1' N2 C10 -4.6(2) . . . . ?
C4 Pd1' N2 Pd1 132(2) . . . . ?
C1 Pd1' N2 Pd1 50.4(18) . . . . ?
N3 Pd1' N2 Pd1 -114.7(19) . . . . ?
N1 Pd1' N2 Pd1 -35.1(18) . . . . ?
C4 Pd1 N2 C16 41.84(12) . . . . ?
C1 Pd1 N2 C16 -39.81(13) . . . . ?
N1 Pd1 N2 C16 -131.76(12) . . . . ?
N3 Pd1 N2 C16 147.20(12) . . . . ?
C4 Pd1 N2 C11 -76.31(10) . . . . ?
C1 Pd1 N2 C11 -157.96(10) . . . . ?
N1 Pd1 N2 C11 110.08(10) . . . . ?
N3 Pd1 N2 C11 29.05(10) . . . . ?
C4 Pd1 N2 C10 165.85(11) . . . . ?
C1 Pd1 N2 C10 84.19(12) . . . . ?
N1 Pd1 N2 C10 -7.76(11) . . . . ?
N3 Pd1 N2 C10 -88.80(11) . . . . ?
C4 Pd1 N2 Pd1' -43.7(19) . . . . ?
C1 Pd1 N2 Pd1' -125.3(19) . . . . ?
N1 Pd1 N2 Pd1' 142.7(19) . . . . ?
N3 Pd1 N2 Pd1' 61.7(19) . . . . ?
C4 Pd1' N3 C17 -28.1(5) . . . . ?
N2 Pd1' N3 C17 -131.41(18) . . . . ?
C1 Pd1' N3 C17 110.1(11) . . . . ?
N1 Pd1' N3 C17 144.89(14) . . . . ?
I1' Pd1' N3 C17 51.9(2) . . . . ?
C4 Pd1' N3 C13 -150.5(3) . . . . ?
N2 Pd1' N3 C13 106.2(2) . . . . ?
C1 Pd1' N3 C13 -12.3(13) . . . . ?
N1 Pd1' N3 C13 22.6(2) . . . . ?
I1' Pd1' N3 C13 -70.4(2) . . . . ?
C4 Pd1' N3 C12 93.0(3) . . . . ?
N2 Pd1' N3 C12 -10.3(3) . . . . ?
C1 Pd1' N3 C12 -128.8(12) . . . . ?
N1 Pd1' N3 C12 -93.95(19) . . . . ?
I1' Pd1' N3 C12 173.10(18) . . . . ?
C4 Pd1' N3 Pd1 -114.5(16) . . . . ?
N2 Pd1' N3 Pd1 142.2(16) . . . . ?
C1 Pd1' N3 Pd1 23.7(7) . . . . ?
N1 Pd1' N3 Pd1 58.6(14) . . . . ?
I1' Pd1' N3 Pd1 -34.4(13) . . . . ?
C4 Pd1 N3 C17 -41.21(12) . . . . ?
N2 Pd1 N3 C17 -131.31(12) . . . . ?
N1 Pd1 N3 C17 145.93(12) . . . . ?
I1 Pd1 N3 C17 48.50(11) . . . . ?
C4 Pd1 N3 C13 -158.67(10) . . . . ?
N2 Pd1 N3 C13 111.23(11) . . . . ?
N1 Pd1 N3 C13 28.46(10) . . . . ?
I1 Pd1 N3 C13 -68.96(10) . . . . ?
C4 Pd1 N3 C12 84.60(11) . . . . ?
N2 Pd1 N3 C12 -5.50(10) . . . . ?
N1 Pd1 N3 C12 -88.26(10) . . . . ?
I1 Pd1 N3 C12 174.32(10) . . . . ?
C4 Pd1 N3 Pd1' 56.3(14) . . . . ?
N2 Pd1 N3 Pd1' -33.8(14) . . . . ?
N1 Pd1 N3 Pd1' -116.6(14) . . . . ?
I1 Pd1 N3 Pd1' 146.0(14) . . . . ?
C8 C3 C4 C5 -0.3(2) . . . . ?
C2 C3 C4 C5 -179.58(15) . . . . ?
C8 C3 C4 Pd1' 165.7(3) . . . . ?
C2 C3 C4 Pd1' -13.6(3) . . . . ?
C8 C3 C4 Pd1 173.26(12) . . . . ?
C2 C3 C4 Pd1 -6.06(18) . . . . ?
N2 Pd1' C4 C5 76.0(3) . . . . ?
C1 Pd1' C4 C5 173.33(14) . . . . ?
N3 Pd1' C4 C5 -17.9(5) . . . . ?
N1 Pd1' C4 C5 -168.4(14) . . . . ?
I1' Pd1' C4 C5 -107.0(3) . . . . ?
N2 Pd1' C4 C3 -90.2(3) . . . . ?
C1 Pd1' C4 C3 7.2(3) . . . . ?
N3 Pd1' C4 C3 175.9(2) . . . . ?
N1 Pd1' C4 C3 25.4(16) . . . . ?
I1' Pd1' C4 C3 86.9(2) . . . . ?
N2 Pd1' C4 Pd1 -150.4(14) . . . . ?
C1 Pd1' C4 Pd1 -53.0(12) . . . . ?
N3 Pd1' C4 Pd1 115.7(14) . . . . ?
N1 Pd1' C4 Pd1 -34.8(11) . . . . ?
I1' Pd1' C4 Pd1 26.7(12) . . . . ?
C1 Pd1 C4 C5 171.86(14) . . . . ?
N2 Pd1 C4 C5 75.56(14) . . . . ?
N3 Pd1 C4 C5 -5.74(14) . . . . ?
I1 Pd1 C4 C5 -99.48(13) . . . . ?
C1 Pd1 C4 C3 -1.37(12) . . . . ?
N2 Pd1 C4 C3 -97.67(12) . . . . ?
N3 Pd1 C4 C3 -178.97(11) . . . . ?
I1 Pd1 C4 C3 87.29(11) . . . . ?
C1 Pd1 C4 Pd1' 122.0(13) . . . . ?
N2 Pd1 C4 Pd1' 25.7(13) . . . . ?
N3 Pd1 C4 Pd1' -55.6(13) . . . . ?
I1 Pd1 C4 Pd1' -149.4(13) . . . . ?
C3 C4 C5 C6 1.4(2) . . . . ?
Pd1' C4 C5 C6 -164.7(3) . . . . ?
Pd1 C4 C5 C6 -171.56(12) . . . . ?
C4 Pd1 C1 C2 8.25(12) . . . . ?
N2 Pd1 C1 C2 99.81(12) . . . . ?
N1 Pd1 C1 C2 -178.55(12) . . . . ?
I1 Pd1 C1 C2 -80.63(11) . . . . ?
C4 Pd1 C1 Pd1' -60.1(14) . . . . ?
N2 Pd1 C1 Pd1' 31.5(14) . . . . ?
N1 Pd1 C1 Pd1' 113.1(14) . . . . ?
I1 Pd1 C1 Pd1' -148.9(14) . . . . ?
C4 Pd1' C1 C2 0.0(3) . . . . ?
N2 Pd1' C1 C2 101.5(2) . . . . ?
N3 Pd1' C1 C2 -141.4(11) . . . . ?
N1 Pd1' C1 C2 -175.67(15) . . . . ?
I1' Pd1' C1 C2 -81.41(19) . . . . ?
C4 Pd1' C1 Pd1 114.4(15) . . . . ?
N2 Pd1' C1 Pd1 -144.1(16) . . . . ?
N3 Pd1' C1 Pd1 -27.0(8) . . . . ?
N1 Pd1' C1 Pd1 -61.3(14) . . . . ?
I1' Pd1' C1 Pd1 33.0(13) . . . . ?
C15 N1 C14 C13 106.80(15) . . . . ?
C9 N1 C14 C13 -133.50(14) . . . . ?
Pd1 N1 C14 C13 -21.10(16) . . . . ?
Pd1' N1 C14 C13 -27.3(2) . . . . ?
C17 N3 C13 C14 -176.11(13) . . . . ?
C12 N3 C13 C14 63.81(16) . . . . ?
Pd1' N3 C13 C14 -46.1(2) . . . . ?
Pd1 N3 C13 C14 -50.17(14) . . . . ?
N1 C14 C13 N3 51.02(18) . . . . ?
C8 C3 C2 C1 -167.21(15) . . . . ?
C4 C3 C2 C1 12.1(2) . . . . ?
C8 C3 C2 C19 -48.9(2) . . . . ?
C4 C3 C2 C19 130.41(16) . . . . ?
C8 C3 C2 C18 69.96(19) . . . . ?
C4 C3 C2 C18 -110.75(16) . . . . ?
Pd1 C1 C2 C3 -12.77(16) . . . . ?
Pd1' C1 C2 C3 -6.0(3) . . . . ?
Pd1 C1 C2 C19 -133.06(12) . . . . ?
Pd1' C1 C2 C19 -126.3(2) . . . . ?
Pd1 C1 C2 C18 108.86(14) . . . . ?
Pd1' C1 C2 C18 115.6(2) . . . . ?
C16 N2 C11 C12 -174.71(14) . . . . ?
C10 N2 C11 C12 65.19(18) . . . . ?
Pd1' N2 C11 C12 -54.0(2) . . . . ?
Pd1 N2 C11 C12 -51.34(15) . . . . ?
C15 N1 C9 C10 -173.27(14) . . . . ?
C14 N1 C9 C10 66.18(17) . . . . ?
Pd1 N1 C9 C10 -51.21(15) . . . . ?
Pd1' N1 C9 C10 -45.9(2) . . . . ?
C4 C3 C8 C7 -0.9(2) . . . . ?
C2 C3 C8 C7 178.42(16) . . . . ?
C4 C5 C6 C7 -1.4(3) . . . . ?
C17 N3 C12 C11 111.17(15) . . . . ?
C13 N3 C12 C11 -130.52(15) . . . . ?
Pd1' N3 C12 C11 -16.7(2) . . . . ?
Pd1 N3 C12 C11 -19.99(16) . . . . ?
N2 C11 C12 N3 50.14(19) . . . . ?
C16 N2 C10 C9 109.77(17) . . . . ?
C11 N2 C10 C9 -131.01(16) . . . . ?
Pd1' N2 C10 C9 -20.4(3) . . . . ?
Pd1 N2 C10 C9 -17.85(18) . . . . ?
N1 C9 C10 N2 49.0(2) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C3 C8 C7 C6 0.8(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 39.06
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 1.407
_refine_diff_density_min -0.690
_refine_diff_density_rms 0.106
_iucr_refine_instructions_details
;
TITL lm23312/lt/x8/Fengrui/Me3tacnPd(IV) in Pca2(1)
CELL 0.71073 16.1097 8.7912 15.5366 90.000 90.000 90.000
ZERR 4.00 0.0024 0.0014 0.0023 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 0.5+Z
SYMM 0.5+X, -Y, Z
SYMM 0.5-X, Y, 0.5+Z
SFAC C H N PD I
UNIT 76 132 12 4 8
TEMP -173.0
SIZE 0.139 0.157 0.381
omit -3.0
L.S. 20
acta
wpdb -2
list 4
bond $h
HTAB
conf
more 2
FMAP 2
PLAN 10
delu $pd $i
eadp pd1 pd1'
eadp i1 i1'
sadi 0.005 pd1 i1 pd1' i1'
sadi pd1 n1 pd1' n1
sadi pd1 n2 pd1' n2
sadi pd1 n3 pd1' n3
sadi pd1 c4 pd1' c4
sadi pd1 c1 pd1' c1
sadi pd1 c11 pd1' c11
WGHT 0.016700 0.729500
FVAR 0.08067 0.96745
part 1
PD1 4 0.764656 0.652695 0.978732 21.00000 0.00644 0.00846 =
0.00869 -0.00132 0.00013 -0.00007
I1 5 0.858396 0.508756 1.086958 21.00000 0.01056 0.01021 =
0.01103 -0.00028 -0.00018 0.00066
part 2
PD1' 4 0.748967 0.667266 0.977412 -21.00000 0.00644 0.00846 =
0.00869 -0.00132 0.00013 -0.00007
I1' 5 0.850372 0.543349 1.083661 -21.00000 0.01056 0.01021 =
0.01103 -0.00028 -0.00018 0.00066
part 0
I2 5 0.523695 0.272226 0.746431 11.00000 0.01093 0.02389 =
0.01945 -0.00863 0.00000 -0.00067
N1 3 0.783064 0.499983 0.865833 11.00000 0.00997 0.01497 =
0.01118 -0.00311 0.00019 0.00098
N2 3 0.676507 0.760066 0.889829 11.00000 0.01278 0.01781 =
0.01207 -0.00175 -0.00093 0.00394
C3 1 0.809547 0.932782 1.068214 11.00000 0.01127 0.01017 =
0.01699 -0.00094 -0.00133 -0.00108
N3 3 0.654202 0.490286 0.996668 11.00000 0.01011 0.01369 =
0.01451 -0.00431 0.00103 -0.00253
C4 1 0.749350 0.817650 1.067910 11.00000 0.01067 0.00951 =
0.01177 -0.00088 0.00009 -0.00034
C17 1 0.626940 0.450559 1.084720 11.00000 0.01588 0.01785 =
0.01649 -0.00406 0.00371 -0.00720
AFIX 137
H17A 2 0.600483 0.539143 1.111435 11.00000 -1.50000
H17B 2 0.675137 0.419802 1.119046 11.00000 -1.50000
H17C 2 0.587130 0.366401 1.082036 11.00000 -1.50000
AFIX 0
C5 1 0.679810 0.829892 1.120796 11.00000 0.01230 0.01387 =
0.01263 -0.00249 0.00117 -0.00117
AFIX 43
H5 2 0.639621 0.750823 1.121573 11.00000 -1.20000
AFIX 0
C1 1 0.865369 0.786076 0.947176 11.00000 0.01226 0.01365 =
0.01645 0.00007 0.00417 -0.00214
AFIX 23
H1A 2 0.915112 0.720227 0.943749 11.00000 -1.20000
H1B 2 0.856032 0.829754 0.889247 11.00000 -1.20000
AFIX 0
C14 1 0.721328 0.374210 0.867604 11.00000 0.01199 0.01672 =
0.01687 -0.00838 -0.00018 -0.00211
AFIX 23
H14A 2 0.748220 0.279469 0.847381 11.00000 -1.20000
H14B 2 0.675541 0.398384 0.827365 11.00000 -1.20000
AFIX 0
C13 1 0.685834 0.347979 0.956272 11.00000 0.01314 0.01386 =
0.01984 -0.00704 0.00284 -0.00396
AFIX 23
H13A 2 0.639903 0.273503 0.952239 11.00000 -1.20000
H13B 2 0.729365 0.303615 0.993593 11.00000 -1.20000
AFIX 0
C15 1 0.867813 0.436494 0.856487 11.00000 0.01054 0.01572 =
0.01456 -0.00230 0.00123 0.00239
AFIX 137
H15A 2 0.870678 0.374781 0.804041 11.00000 -1.50000
H15B 2 0.880760 0.372863 0.906508 11.00000 -1.50000
H15C 2 0.908038 0.519856 0.852731 11.00000 -1.50000
AFIX 0
C2 1 0.883456 0.916251 1.009854 11.00000 0.01046 0.01104 =
0.02163 0.00040 0.00222 -0.00268
C11 1 0.593879 0.722332 0.927711 11.00000 0.01032 0.02234 =
0.01643 -0.00419 -0.00139 0.00503
AFIX 23
H11A 2 0.549862 0.755290 0.887346 11.00000 -1.20000
H11B 2 0.586758 0.780288 0.981844 11.00000 -1.20000
AFIX 0
C9 1 0.767352 0.604173 0.792394 11.00000 0.01566 0.02294 =
0.01027 -0.00216 -0.00124 0.00387
AFIX 23
H9A 2 0.766287 0.544691 0.738299 11.00000 -1.20000
H9B 2 0.813302 0.678602 0.788312 11.00000 -1.20000
AFIX 0
C8 1 0.798613 1.059188 1.121663 11.00000 0.01739 0.01212 =
0.01835 -0.00450 -0.00258 -0.00085
AFIX 43
H8 2 0.839517 1.137003 1.122809 11.00000 -1.20000
AFIX 0
C18 1 0.962613 0.887852 1.063159 11.00000 0.01202 0.01792 =
0.03728 -0.00412 -0.00444 -0.00109
AFIX 137
H18A 2 0.971601 0.973389 1.102519 11.00000 -1.50000
H18B 2 1.010344 0.878239 1.024433 11.00000 -1.50000
H18C 2 0.956237 0.793864 1.096425 11.00000 -1.50000
AFIX 0
C6 1 0.669088 0.957854 1.172546 11.00000 0.01728 0.01680 =
0.01371 -0.00457 0.00218 0.00132
AFIX 43
H6 2 0.620954 0.966807 1.207506 11.00000 -1.20000
AFIX 0
C12 1 0.582908 0.554301 0.946548 11.00000 0.00950 0.02285 =
0.01827 -0.00538 -0.00051 -0.00087
AFIX 23
H12A 2 0.530988 0.539274 0.979559 11.00000 -1.20000
H12B 2 0.577559 0.498252 0.891559 11.00000 -1.20000
AFIX 0
C10 1 0.686024 0.688628 0.802191 11.00000 0.01800 0.02547 =
0.01082 -0.00203 -0.00254 0.00690
AFIX 23
H10A 2 0.682705 0.769081 0.757737 11.00000 -1.20000
H10B 2 0.639556 0.616998 0.792391 11.00000 -1.20000
AFIX 0
C7 1 0.728252 1.071913 1.173220 11.00000 0.02118 0.01334 =
0.01696 -0.00677 0.00031 0.00043
AFIX 43
H7 2 0.720889 1.158763 1.208794 11.00000 -1.20000
AFIX 0
C19 1 0.897936 1.061867 0.956962 11.00000 0.02245 0.01400 =
0.03320 0.00421 0.00849 -0.00504
AFIX 137
H19A 2 0.846679 1.089413 0.926779 11.00000 -1.50000
H19B 2 0.942193 1.044020 0.914881 11.00000 -1.50000
H19C 2 0.914157 1.144894 0.995545 11.00000 -1.50000
AFIX 0
C16 1 0.682543 0.927231 0.882205 11.00000 0.02335 0.01823 =
0.01854 0.00289 -0.00115 0.00619
AFIX 137
H16A 2 0.635370 0.965552 0.848799 11.00000 -1.50000
H16B 2 0.734431 0.954141 0.853012 11.00000 -1.50000
H16C 2 0.681833 0.972874 0.939747 11.00000 -1.50000
HKLF 4
REM lm23312/lt/x8/Fengrui/Me3tacnPd(IV) in Pca2(1)
REM R1 = 0.0196 for 12029 Fo > 4sig(Fo) and 0.0218 for all 12564 data
REM 238 parameters refined using 10 restraints
END
WGHT 0.0167 0.7307
REM Highest difference peak 1.407, deepest hole -0.690, 1-sigma level 0.106
Q1 1 0.7532 0.6016 1.0022 11.00000 0.05 1.41
Q2 1 0.7299 0.6584 0.9961 11.00000 0.05 1.05
Q3 1 0.5272 0.3322 0.7165 11.00000 0.05 0.94
Q4 1 0.8225 0.5178 1.0693 11.00000 0.05 0.93
Q5 1 0.4920 0.2284 0.7504 11.00000 0.05 0.91
Q6 1 0.7434 0.6209 0.9561 11.00000 0.05 0.85
Q7 1 0.8580 0.4370 1.0656 11.00000 0.05 0.84
Q8 1 0.5209 0.2076 0.7740 11.00000 0.05 0.81
Q9 1 0.5280 0.2149 0.7168 11.00000 0.05 0.75
Q10 1 0.8284 0.5093 1.1225 11.00000 0.05 0.71
;
_database_code_depnum_ccdc_archive 'CCDC 972258'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_l5513
_audit_creation_method SHELXL-2012
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C19 H33 Cl N3 Pd, Cl O4'
_chemical_formula_sum 'C19 H33 Cl2 N3 O4 Pd'
_chemical_formula_weight 544.78
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'
Cl Cl 0.1484 0.1585 '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 orthorhombic
_space_group_IT_number 29
_space_group_name_H-M_alt 'P c a 21'
_space_group_name_Hall 'P 2c -2ac'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
_cell_length_a 16.5967(7)
_cell_length_b 8.3780(4)
_cell_length_c 15.0330(6)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2090.30(16)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9729
_cell_measurement_theta_min 2.43
_cell_measurement_theta_max 39.99
_exptl_crystal_description cubic
_exptl_crystal_colour yellow
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.731
_exptl_crystal_F_000 1120
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.258
_exptl_crystal_size_mid 0.257
_exptl_crystal_size_min 0.251
_exptl_absorpt_coefficient_mu 1.176
_shelx_estimated_absorpt_T_min 0.751
_shelx_estimated_absorpt_T_max 0.757
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7252
_exptl_absorpt_correction_T_max 0.8032
_exptl_absorpt_process_details 'sadabs v2012/1'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 79064
_diffrn_reflns_av_unetI/netI 0.0335
_diffrn_reflns_av_R_equivalents 0.0439
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.431
_diffrn_reflns_theta_max 38.999
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total 11727
_reflns_number_gt 10814
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.876
_reflns_Friedel_fraction_max 0.927
_reflns_Friedel_fraction_full 0.994
_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.
;
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
All H atoms were positioned geometrically and refined using a
riding model with C---H = 0.95--0.99 \%A and with U~iso~(H)
= 1.2 (1.5 for methyl groups) times U~eq~(C).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.6938P]
where P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_abs_structure_details
;
Flack x determined using 4730 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack -0.002(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns 11727
_refine_ls_number_parameters 295
_refine_ls_number_restraints 24
_refine_ls_R_factor_all 0.0307
_refine_ls_R_factor_gt 0.0264
_refine_ls_wR_factor_ref 0.0613
_refine_ls_wR_factor_gt 0.0597
_refine_ls_goodness_of_fit_ref 1.043
_refine_ls_restrained_S_all 1.044
_refine_ls_shift/su_max 0.008
_refine_ls_shift/su_mean 0.000
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 0.01852(2) 0.39994(2) 0.98576(2) 0.00771(3) Uani 1 1 d D . . . .
Cl1 Cl 0.07828(4) 0.37596(8) 0.85215(5) 0.01958(12) Uani 0.9602(17) 1 d D . P A
1
Cl1' Cl 0.0972(8) 0.4638(18) 0.8693(7) 0.01958(12) Uani 0.0398(17) 1 d D . P A
2
N1 N 0.12098(10) 0.3049(2) 1.06383(12) 0.0107(3) Uani 1 1 d . . . . .
N2 N 0.08600(11) 0.6296(2) 1.01358(13) 0.0125(3) Uani 1 1 d . . . . .
N3 N -0.02916(10) 0.4447(2) 1.11298(13) 0.0121(3) Uani 1 1 d . . . . .
C1 C -0.08206(11) 0.4642(2) 0.91953(14) 0.0100(3) Uani 1 1 d . . . . .
C2 C -0.10705(13) 0.6215(2) 0.90647(15) 0.0129(3) Uani 1 1 d . . . . .
H2 H -0.0771 0.7066 0.9320 0.016 Uiso 1 1 calc R U . . .
C3 C -0.17554(12) 0.6545(2) 0.85623(15) 0.0131(3) Uani 1 1 d . . . . .
H3 H -0.1926 0.7617 0.8483 0.016 Uiso 1 1 calc R U . . .
C4 C -0.21878(12) 0.5309(3) 0.81779(15) 0.0131(3) Uani 1 1 d . . . . .
H4 H -0.2647 0.5536 0.7823 0.016 Uiso 1 1 calc R U . . .
C5 C -0.19496(12) 0.3741(2) 0.83112(14) 0.0124(3) Uani 1 1 d . . . . .
H5 H -0.2252 0.2896 0.8053 0.015 Uiso 1 1 calc R U . . .
C6 C -0.12680(11) 0.3392(2) 0.88222(14) 0.0098(3) Uani 1 1 d . . . . .
C7 C -0.10077(11) 0.1703(2) 0.90137(14) 0.0114(3) Uani 1 1 d . . . . .
C8 C -0.03061(11) 0.1766(2) 0.96766(14) 0.0114(4) Uani 1 1 d . . . . .
H8A H 0.0123 0.1035 0.9468 0.014 Uiso 1 1 calc R U . . .
H8B H -0.0498 0.1365 1.0259 0.014 Uiso 1 1 calc R U . . .
C9 C -0.07554(13) 0.0854(2) 0.81512(16) 0.0147(4) Uani 1 1 d . . . . .
H9A H -0.1209 0.0845 0.7734 0.022 Uiso 1 1 calc R U . . .
H9B H -0.0596 -0.0246 0.8287 0.022 Uiso 1 1 calc R U . . .
H9C H -0.0300 0.1421 0.7883 0.022 Uiso 1 1 calc R U . . .
C10 C -0.17038(13) 0.0760(2) 0.94445(17) 0.0152(4) Uani 1 1 d . . . . .
H10A H -0.1895 0.1331 0.9973 0.023 Uiso 1 1 calc R U . . .
H10B H -0.1512 -0.0302 0.9617 0.023 Uiso 1 1 calc R U . . .
H10C H -0.2146 0.0652 0.9017 0.023 Uiso 1 1 calc R U . . .
C11 C 0.08002(13) 0.2440(3) 1.14518(15) 0.0143(3) Uani 1 1 d . . . . .
H11A H 0.1209 0.2155 1.1904 0.017 Uiso 1 1 calc R U . . .
H11B H 0.0492 0.1464 1.1303 0.017 Uiso 1 1 calc R U . . .
C12 C 0.02341(13) 0.3685(3) 1.18309(16) 0.0158(4) Uani 1 1 d . . . . .
H12A H -0.0114 0.3179 1.2286 0.019 Uiso 1 1 calc R U . . .
H12B H 0.0555 0.4526 1.2129 0.019 Uiso 1 1 calc R U . . .
C13 C -0.02786(14) 0.6233(3) 1.12104(18) 0.0165(4) Uani 1 1 d . . . . .
H13A H -0.0423 0.6534 1.1827 0.020 Uiso 1 1 calc R U . . .
H13B H -0.0692 0.6689 1.0809 0.020 Uiso 1 1 calc R U . . .
C14 C 0.05344(14) 0.6953(3) 1.09828(17) 0.0174(4) Uani 1 1 d . . . . .
H14A H 0.0479 0.8126 1.0929 0.021 Uiso 1 1 calc R U . . .
H14B H 0.0919 0.6730 1.1471 0.021 Uiso 1 1 calc R U . . .
C15 C 0.17052(13) 0.5735(3) 1.02331(17) 0.0152(4) Uani 1 1 d . . . . .
H15A H 0.2044 0.6631 1.0445 0.018 Uiso 1 1 calc R U . . .
H15B H 0.1911 0.5399 0.9644 0.018 Uiso 1 1 calc R U . . .
C16 C 0.17765(13) 0.4363(3) 1.08746(16) 0.0151(4) Uani 1 1 d . . . . .
H16A H 0.2336 0.3952 1.0867 0.018 Uiso 1 1 calc R U . . .
H16B H 0.1658 0.4742 1.1484 0.018 Uiso 1 1 calc R U . . .
C17 C 0.16622(13) 0.1750(3) 1.01981(17) 0.0159(4) Uani 1 1 d . . . . .
H17A H 0.1290 0.0890 1.0034 0.024 Uiso 1 1 calc R U . . .
H17B H 0.2072 0.1334 1.0607 0.024 Uiso 1 1 calc R U . . .
H17C H 0.1924 0.2164 0.9662 0.024 Uiso 1 1 calc R U . . .
C18 C 0.08682(15) 0.7504(3) 0.94147(18) 0.0197(4) Uani 1 1 d . . . . .
H18A H 0.1001 0.6985 0.8849 0.030 Uiso 1 1 calc R U . . .
H18B H 0.1273 0.8321 0.9548 0.030 Uiso 1 1 calc R U . . .
H18C H 0.0336 0.8004 0.9370 0.030 Uiso 1 1 calc R U . . .
C19 C -0.11395(13) 0.3925(3) 1.12685(18) 0.0167(4) Uani 1 1 d . . . . .
H19A H -0.1482 0.4385 1.0803 0.025 Uiso 1 1 calc R U . . .
H19B H -0.1326 0.4290 1.1853 0.025 Uiso 1 1 calc R U . . .
H19C H -0.1168 0.2758 1.1241 0.025 Uiso 1 1 calc R U . . .
Cl2 Cl 0.1708(2) 1.0277(5) 0.71116(10) 0.0173(3) Uani 0.89(3) 1 d D U P B 1
Cl2' Cl 0.1595(14) 1.051(3) 0.7111(11) 0.0173(3) Uani 0.11(3) 1 d . . P B 2
O1 O 0.09405(12) 1.0121(3) 0.66497(16) 0.0285(4) Uani 1 1 d . U . . .
O2 O 0.19962(13) 1.1881(2) 0.69684(16) 0.0304(5) Uani 1 1 d . U . . .
O3 O 0.2281(5) 0.9137(16) 0.6794(18) 0.036(2) Uani 0.70(12) 1 d D U P B 1
O4 O 0.1540(11) 1.022(4) 0.8052(3) 0.062(4) Uani 0.58(6) 1 d D U P B 1
O3' O 0.2275(10) 0.924(2) 0.6675(18) 0.021(4) Uani 0.30(12) 1 d D . P B 2
O4' O 0.1625(9) 0.9818(15) 0.8025(5) 0.034(2) Uani 0.42(6) 1 d D U P B 2
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 0.00800(4) 0.00664(4) 0.00850(5) -0.00033(6) -0.00006(6) 0.00004(3)
Cl1 0.0190(2) 0.0229(3) 0.0169(3) 0.0018(2) 0.0002(2) -0.00261(19)
Cl1' 0.0190(2) 0.0229(3) 0.0169(3) 0.0018(2) 0.0002(2) -0.00261(19)
N1 0.0108(6) 0.0107(6) 0.0107(7) -0.0008(5) -0.0007(5) 0.0005(5)
N2 0.0133(7) 0.0090(6) 0.0150(8) -0.0006(5) 0.0004(6) -0.0008(5)
N3 0.0123(6) 0.0128(6) 0.0113(8) -0.0024(6) 0.0022(6) -0.0006(5)
C1 0.0102(7) 0.0097(7) 0.0101(8) -0.0002(6) -0.0008(6) 0.0001(5)
C2 0.0146(8) 0.0099(7) 0.0142(9) 0.0001(6) -0.0015(7) 0.0015(6)
C3 0.0138(7) 0.0119(7) 0.0136(9) 0.0012(7) -0.0001(7) 0.0034(6)
C4 0.0108(7) 0.0156(8) 0.0128(9) 0.0009(7) -0.0006(6) 0.0026(6)
C5 0.0109(7) 0.0147(7) 0.0116(9) -0.0003(6) -0.0018(6) -0.0002(6)
C6 0.0099(7) 0.0083(6) 0.0113(8) -0.0006(6) -0.0005(6) 0.0001(5)
C7 0.0111(7) 0.0093(7) 0.0136(9) -0.0013(6) -0.0009(6) -0.0006(5)
C8 0.0129(7) 0.0075(6) 0.0136(10) 0.0004(5) -0.0020(6) -0.0008(5)
C9 0.0177(8) 0.0129(8) 0.0136(9) -0.0033(7) -0.0016(7) 0.0014(6)
C10 0.0137(8) 0.0124(7) 0.0196(11) 0.0004(7) 0.0003(7) -0.0030(6)
C11 0.0168(8) 0.0147(8) 0.0114(9) 0.0025(7) -0.0010(7) 0.0008(6)
C12 0.0179(9) 0.0206(9) 0.0088(9) 0.0001(7) 0.0015(7) 0.0012(7)
C13 0.0180(9) 0.0122(8) 0.0194(11) -0.0053(7) 0.0029(8) 0.0008(6)
C14 0.0195(9) 0.0123(8) 0.0204(11) -0.0064(7) 0.0027(8) -0.0018(7)
C15 0.0126(8) 0.0141(8) 0.0189(10) 0.0009(7) 0.0003(7) -0.0024(6)
C16 0.0127(7) 0.0160(8) 0.0167(10) -0.0004(7) -0.0036(7) -0.0009(6)
C17 0.0144(8) 0.0152(8) 0.0181(10) -0.0041(7) -0.0019(7) 0.0062(6)
C18 0.0203(9) 0.0132(8) 0.0256(12) 0.0063(8) -0.0009(8) -0.0037(7)
C19 0.0125(8) 0.0191(9) 0.0186(11) -0.0020(8) 0.0050(7) -0.0013(7)
Cl2 0.0193(6) 0.0166(6) 0.0158(2) 0.0050(3) -0.0067(3) -0.0063(5)
Cl2' 0.0193(6) 0.0166(6) 0.0158(2) 0.0050(3) -0.0067(3) -0.0063(5)
O1 0.0206(8) 0.0270(9) 0.0380(12) -0.0111(8) -0.0123(8) 0.0018(7)
O2 0.0340(10) 0.0174(8) 0.0398(13) -0.0058(8) 0.0120(9) -0.0114(7)
O3 0.029(3) 0.018(2) 0.062(6) 0.009(3) -0.024(4) -0.0023(19)
O4 0.067(6) 0.103(11) 0.017(3) 0.024(3) -0.013(3) -0.034(6)
O3' 0.017(5) 0.026(6) 0.021(9) 0.009(4) 0.004(6) 0.010(4)
O4' 0.042(4) 0.035(4) 0.026(4) 0.021(2) 0.011(3) 0.020(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 C1 2.0170(19) . ?
Pd1 C8 2.0592(19) . ?
Pd1 N3 2.1035(19) . ?
Pd1 N1 2.2144(17) . ?
Pd1 Cl1 2.2490(7) . ?
Pd1 Cl1' 2.249(6) . ?
Pd1 N2 2.2651(17) . ?
N1 C17 1.479(3) . ?
N1 C11 1.489(3) . ?
N1 C16 1.491(3) . ?
N2 C18 1.483(3) . ?
N2 C15 1.486(3) . ?
N2 C14 1.489(3) . ?
N3 C19 1.488(3) . ?
N3 C13 1.502(3) . ?
N3 C12 1.510(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.401(3) . ?
C2 C3 1.392(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.507(3) . ?
C7 C8 1.534(3) . ?
C7 C9 1.537(3) . ?
C7 C10 1.542(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.515(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.517(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.506(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
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 . ?
Cl2 O3 1.430(6) . ?
Cl2 O4 1.442(5) . ?
Cl2 O2 1.442(3) . ?
Cl2 O1 1.457(4) . ?
Cl2' O1 1.329(17) . ?
Cl2' O2 1.347(15) . ?
Cl2' O4' 1.490(18) . ?
Cl2' O3' 1.68(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
C1 Pd1 C8 81.36(7) . . ?
C1 Pd1 N3 95.16(8) . . ?
C8 Pd1 N3 97.65(8) . . ?
C1 Pd1 N1 173.35(7) . . ?
C8 Pd1 N1 92.71(7) . . ?
N3 Pd1 N1 82.59(7) . . ?
C1 Pd1 Cl1 87.02(6) . . ?
C8 Pd1 Cl1 88.60(6) . . ?
N3 Pd1 Cl1 173.62(5) . . ?
N1 Pd1 Cl1 95.89(5) . . ?
C1 Pd1 Cl1' 91.9(4) . . ?
C8 Pd1 Cl1' 110.1(4) . . ?
N3 Pd1 Cl1' 152.1(4) . . ?
N1 Pd1 Cl1' 93.0(4) . . ?
C1 Pd1 N2 105.87(7) . . ?
C8 Pd1 N2 172.75(7) . . ?
N3 Pd1 N2 82.34(7) . . ?
N1 Pd1 N2 80.09(6) . . ?
Cl1 Pd1 N2 91.31(5) . . ?
Cl1' Pd1 N2 69.8(4) . . ?
C17 N1 C11 110.33(17) . . ?
C17 N1 C16 109.25(16) . . ?
C11 N1 C16 110.18(17) . . ?
C17 N1 Pd1 114.68(13) . . ?
C11 N1 Pd1 102.00(12) . . ?
C16 N1 Pd1 110.19(12) . . ?
C18 N2 C15 106.19(18) . . ?
C18 N2 C14 112.09(18) . . ?
C15 N2 C14 112.04(19) . . ?
C18 N2 Pd1 116.68(15) . . ?
C15 N2 Pd1 102.50(12) . . ?
C14 N2 Pd1 107.02(13) . . ?
C19 N3 C13 107.15(17) . . ?
C19 N3 C12 108.94(18) . . ?
C13 N3 C12 110.90(18) . . ?
C19 N3 Pd1 115.51(15) . . ?
C13 N3 Pd1 104.22(14) . . ?
C12 N3 Pd1 110.00(13) . . ?
C2 C1 C6 119.49(18) . . ?
C2 C1 Pd1 124.59(15) . . ?
C6 C1 Pd1 115.87(13) . . ?
C3 C2 C1 120.42(19) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 120.04(18) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 119.99(19) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.55(19) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 119.48(18) . . ?
C5 C6 C7 122.22(17) . . ?
C1 C6 C7 118.27(17) . . ?
C6 C7 C8 108.03(16) . . ?
C6 C7 C9 110.57(18) . . ?
C8 C7 C9 110.93(16) . . ?
C6 C7 C10 110.27(16) . . ?
C8 C7 C10 108.27(17) . . ?
C9 C7 C10 108.75(17) . . ?
C7 C8 Pd1 114.70(13) . . ?
C7 C8 H8A 108.6 . . ?
Pd1 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
Pd1 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 110.88(17) . . ?
N1 C11 H11A 109.5 . . ?
C12 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N3 C12 C11 112.75(19) . . ?
N3 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
N3 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
N3 C13 C14 112.99(18) . . ?
N3 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N3 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N2 C14 C13 111.64(18) . . ?
N2 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
N2 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
N2 C15 C16 112.24(18) . . ?
N2 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
N2 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
N1 C16 C15 111.21(18) . . ?
N1 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
N1 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 Cl2 O4 115.6(19) . . ?
O3 Cl2 O2 110.6(7) . . ?
O4 Cl2 O2 104.1(11) . . ?
O3 Cl2 O1 111.2(7) . . ?
O4 Cl2 O1 107.1(6) . . ?
O2 Cl2 O1 107.6(3) . . ?
O1 Cl2' O2 121.9(16) . . ?
O1 Cl2' O4' 114.4(12) . . ?
O2 Cl2' O4' 117.4(12) . . ?
O1 Cl2' O3' 101.1(15) . . ?
O2 Cl2' O3' 98.5(15) . . ?
O4' Cl2' O3' 95.3(18) . . ?
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
C6 C1 C2 C3 -0.5(3) . . . . ?
Pd1 C1 C2 C3 177.01(17) . . . . ?
C1 C2 C3 C4 -0.9(3) . . . . ?
C2 C3 C4 C5 1.6(3) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C4 C5 C6 C1 -0.5(3) . . . . ?
C4 C5 C6 C7 177.5(2) . . . . ?
C2 C1 C6 C5 1.2(3) . . . . ?
Pd1 C1 C6 C5 -176.54(16) . . . . ?
C2 C1 C6 C7 -176.9(2) . . . . ?
Pd1 C1 C6 C7 5.4(2) . . . . ?
C5 C6 C7 C8 -173.35(19) . . . . ?
C1 C6 C7 C8 4.7(3) . . . . ?
C5 C6 C7 C9 65.1(2) . . . . ?
C1 C6 C7 C9 -116.9(2) . . . . ?
C5 C6 C7 C10 -55.2(3) . . . . ?
C1 C6 C7 C10 122.8(2) . . . . ?
C6 C7 C8 Pd1 -12.4(2) . . . . ?
C9 C7 C8 Pd1 108.89(16) . . . . ?
C10 C7 C8 Pd1 -131.86(14) . . . . ?
C17 N1 C11 C12 -171.36(18) . . . . ?
C16 N1 C11 C12 67.9(2) . . . . ?
Pd1 N1 C11 C12 -49.09(18) . . . . ?
C19 N3 C12 C11 110.9(2) . . . . ?
C13 N3 C12 C11 -131.4(2) . . . . ?
Pd1 N3 C12 C11 -16.6(2) . . . . ?
N1 C11 C12 N3 46.6(2) . . . . ?
C19 N3 C13 C14 -173.6(2) . . . . ?
C12 N3 C13 C14 67.6(3) . . . . ?
Pd1 N3 C13 C14 -50.7(2) . . . . ?
C18 N2 C14 C13 110.8(2) . . . . ?
C15 N2 C14 C13 -130.0(2) . . . . ?
Pd1 N2 C14 C13 -18.4(2) . . . . ?
N3 C13 C14 N2 47.6(3) . . . . ?
C18 N2 C15 C16 -173.5(2) . . . . ?
C14 N2 C15 C16 63.8(2) . . . . ?
Pd1 N2 C15 C16 -50.6(2) . . . . ?
C17 N1 C16 C15 102.9(2) . . . . ?
C11 N1 C16 C15 -135.75(19) . . . . ?
Pd1 N1 C16 C15 -24.0(2) . . . . ?
N2 C15 C16 N1 52.7(3) . . . . ?
O2 Cl2' O1 Cl2 128(6) . . . . ?
O4' Cl2' O1 Cl2 -80(4) . . . . ?
O3' Cl2' O1 Cl2 21(4) . . . . ?
O3 Cl2 O1 Cl2' -162(5) . . . . ?
O4 Cl2 O1 Cl2' 70(4) . . . . ?
O2 Cl2 O1 Cl2' -41(4) . . . . ?
O1 Cl2' O2 Cl2 -132(6) . . . . ?
O4' Cl2' O2 Cl2 78(4) . . . . ?
O3' Cl2' O2 Cl2 -23(4) . . . . ?
O3 Cl2 O2 Cl2' 159(4) . . . . ?
O4 Cl2 O2 Cl2' -76(4) . . . . ?
O1 Cl2 O2 Cl2' 37(4) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
# C16 H16A O2 0.99 2.64 3.343(3) 127.9 4_545
# C17 H17B O2 0.98 2.61 3.472(3) 147.3 4_545
# C17 H17B O3' 0.98 2.62 3.53(3) 155.6 4_545
# C17 H17C Cl1 0.98 2.88 3.364(2) 111.2 .
# C19 H19B Cl1' 0.98 2.97 3.848(10) 150.1 2_565
C13 H13A Cl1 0.99 2.63 3.574(3) 159.9 2_565
C15 H15B Cl1' 0.99 2.21 2.773(15) 114.7 .
C18 H18A Cl1 0.98 2.77 3.415(3) 123.9 .
C18 H18A Cl1' 0.98 1.98 2.641(16) 122.6 .
C19 H19C O1 0.98 2.52 3.454(3) 159.8 2_565
C19 H19C O3 0.98 2.57 3.285(10) 129.6 2_565
C19 H19C O3' 0.98 2.57 3.31(2) 132.4 2_565
_refine_diff_density_max 1.843
_refine_diff_density_min -1.100
_refine_diff_density_rms 0.097
_shelxl_version_number 2012-9
_shelx_res_file
;
TITL lm5513/lt/Fengrui in Pca2(1)
CELL 0.71073 16.5967 8.3780 15.0330 90.000 90.000 90.000
ZERR 4.00 0.0007 0.0004 0.0006 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 0.5+Z
SYMM 0.5+X, -Y, Z
SYMM 0.5-X, Y, 0.5+Z
SFAC C H N O CL PD
UNIT 76 132 12 16 8 4
TEMP -173.0
SIZE 0.251 0.257 0.258
OMIT -3.0 78.0
sadi 0.005 cl2 o3 cl2 o4 cl2 o3' cl2 o4'
sadi 0.005 pd1 cl1 pd1 cl1'
delu cl2 $O
rem eadp o4' o4
eadp cl1 cl1'
eadp cl2 cl2'
isor 0.003 o4'
L.S. 20
PLAN 5
wpdb -2
list 4
bond $h
conf
more 2
fmap 2
acta
EQIV $1 -x, -y+1, z+1/2
HTAB C13 Cl1_$1
HTAB C15 Cl1'
EQIV $2 -x+1/2, y-1, z+1/2
HTAB C16 O2_$2
HTAB C17 O2_$2
HTAB C17 O3'_$2
HTAB C17 Cl1
HTAB C18 Cl1
HTAB C18 Cl1'
HTAB C19 Cl1'_$1
HTAB C19 O1_$1
HTAB C19 O3_$1
HTAB C19 O3'_$1
WGHT 0.027800 0.693800
FVAR 0.12342 0.96024 0.89402 0.70216 0.57972
PD1 6 0.018520 0.399943 0.985755 11.00000 0.00800 0.00664 =
0.00850 -0.00033 -0.00006 0.00004
PART 1
CL1 5 0.078281 0.375957 0.852151 21.00000 0.01902 0.02287 =
0.01686 0.00180 0.00017 -0.00261
PART 2
CL1' 5 0.097207 0.463768 0.869255 -21.00000 0.01902 0.02287 =
0.01686 0.00180 0.00017 -0.00261
PART 0
N1 3 0.120976 0.304870 1.063833 11.00000 0.01084 0.01066 =
0.01069 -0.00079 -0.00068 0.00051
N2 3 0.086002 0.629584 1.013584 11.00000 0.01334 0.00904 =
0.01498 -0.00061 0.00044 -0.00080
N3 3 -0.029155 0.444696 1.112982 11.00000 0.01225 0.01277 =
0.01135 -0.00240 0.00216 -0.00058
C1 1 -0.082065 0.464244 0.919527 11.00000 0.01025 0.00974 =
0.01013 -0.00020 -0.00080 0.00006
C2 1 -0.107047 0.621468 0.906470 11.00000 0.01463 0.00992 =
0.01422 0.00011 -0.00147 0.00147
AFIX 43
H2 2 -0.077141 0.706597 0.932016 11.00000 -1.20000
AFIX 0
C3 1 -0.175542 0.654451 0.856233 11.00000 0.01382 0.01187 =
0.01356 0.00117 -0.00014 0.00342
AFIX 43
H3 2 -0.192643 0.761726 0.848305 11.00000 -1.20000
AFIX 0
C4 1 -0.218783 0.530879 0.817790 11.00000 0.01084 0.01558 =
0.01275 0.00088 -0.00065 0.00259
AFIX 43
H4 2 -0.264741 0.553611 0.782312 11.00000 -1.20000
AFIX 0
C5 1 -0.194956 0.374076 0.831120 11.00000 0.01086 0.01466 =
0.01159 -0.00026 -0.00176 -0.00021
AFIX 43
H5 2 -0.225187 0.289648 0.805320 11.00000 -1.20000
AFIX 0
C6 1 -0.126800 0.339170 0.882221 11.00000 0.00987 0.00826 =
0.01131 -0.00055 -0.00047 0.00012
C7 1 -0.100770 0.170293 0.901372 11.00000 0.01113 0.00933 =
0.01364 -0.00127 -0.00088 -0.00061
C8 1 -0.030613 0.176600 0.967665 11.00000 0.01293 0.00749 =
0.01364 0.00039 -0.00205 -0.00083
AFIX 23
H8A 2 0.012291 0.103549 0.946789 11.00000 -1.20000
H8B 2 -0.049785 0.136512 1.025886 11.00000 -1.20000
AFIX 0
C9 1 -0.075538 0.085409 0.815120 11.00000 0.01769 0.01290 =
0.01360 -0.00330 -0.00162 0.00144
AFIX 137
H9A 2 -0.120936 0.084550 0.773437 11.00000 -1.50000
H9B 2 -0.059607 -0.024575 0.828661 11.00000 -1.50000
H9C 2 -0.029982 0.142128 0.788268 11.00000 -1.50000
AFIX 0
C10 1 -0.170375 0.076010 0.944449 11.00000 0.01375 0.01237 =
0.01963 0.00037 0.00032 -0.00300
AFIX 137
H10A 2 -0.189516 0.133072 0.997287 11.00000 -1.50000
H10B 2 -0.151215 -0.030203 0.961725 11.00000 -1.50000
H10C 2 -0.214631 0.065240 0.901711 11.00000 -1.50000
AFIX 0
C11 1 0.080020 0.244042 1.145184 11.00000 0.01684 0.01474 =
0.01139 0.00246 -0.00101 0.00079
AFIX 23
H11A 2 0.120938 0.215539 1.190393 11.00000 -1.20000
H11B 2 0.049213 0.146428 1.130330 11.00000 -1.20000
AFIX 0
C12 1 0.023409 0.368525 1.183094 11.00000 0.01795 0.02062 =
0.00884 0.00006 0.00154 0.00124
AFIX 23
H12A 2 -0.011363 0.317891 1.228557 11.00000 -1.20000
H12B 2 0.055497 0.452561 1.212902 11.00000 -1.20000
AFIX 0
C13 1 -0.027859 0.623347 1.121038 11.00000 0.01795 0.01222 =
0.01944 -0.00526 0.00289 0.00077
AFIX 23
H13A 2 -0.042282 0.653374 1.182709 11.00000 -1.20000
H13B 2 -0.069174 0.668922 1.080898 11.00000 -1.20000
AFIX 0
C14 1 0.053444 0.695308 1.098276 11.00000 0.01954 0.01226 =
0.02036 -0.00640 0.00274 -0.00179
AFIX 23
H14A 2 0.047912 0.812564 1.092864 11.00000 -1.20000
H14B 2 0.091854 0.672971 1.147100 11.00000 -1.20000
AFIX 0
C15 1 0.170516 0.573533 1.023307 11.00000 0.01260 0.01414 =
0.01894 0.00089 0.00026 -0.00244
AFIX 23
H15A 2 0.204392 0.663069 1.044479 11.00000 -1.20000
H15B 2 0.191131 0.539890 0.964422 11.00000 -1.20000
AFIX 0
C16 1 0.177651 0.436270 1.087462 11.00000 0.01269 0.01596 =
0.01668 -0.00038 -0.00357 -0.00087
AFIX 23
H16A 2 0.233575 0.395182 1.086709 11.00000 -1.20000
H16B 2 0.165761 0.474229 1.148430 11.00000 -1.20000
AFIX 0
C17 1 0.166222 0.174968 1.019813 11.00000 0.01436 0.01517 =
0.01806 -0.00407 -0.00194 0.00619
AFIX 137
H17A 2 0.129022 0.089006 1.003445 11.00000 -1.50000
H17B 2 0.207184 0.133421 1.060660 11.00000 -1.50000
H17C 2 0.192448 0.216381 0.966159 11.00000 -1.50000
AFIX 0
C18 1 0.086818 0.750372 0.941468 11.00000 0.02034 0.01318 =
0.02557 0.00631 -0.00088 -0.00368
AFIX 137
H18A 2 0.100106 0.698462 0.884921 11.00000 -1.50000
H18B 2 0.127298 0.832095 0.954813 11.00000 -1.50000
H18C 2 0.033589 0.800372 0.937018 11.00000 -1.50000
AFIX 0
C19 1 -0.113951 0.392533 1.126849 11.00000 0.01251 0.01906 =
0.01863 -0.00204 0.00496 -0.00127
AFIX 137
H19A 2 -0.148207 0.438457 1.080326 11.00000 -1.50000
H19B 2 -0.132644 0.428990 1.185253 11.00000 -1.50000
H19C 2 -0.116836 0.275804 1.124100 11.00000 -1.50000
AFIX 0
part 1
CL2 5 0.170835 1.027690 0.711160 31.00000 0.01933 0.01661 =
0.01583 0.00495 -0.00675 -0.00633
part 2
CL2' 5 0.159526 1.050573 0.711068 -31.00000 0.01933 0.01661 =
0.01583 0.00495 -0.00675 -0.00633
part 0
O1 4 0.094050 1.012130 0.664968 11.00000 0.02060 0.02697 =
0.03801 -0.01109 -0.01228 0.00181
O2 4 0.199621 1.188072 0.696840 11.00000 0.03404 0.01736 =
0.03978 -0.00577 0.01201 -0.01145
PART 1
O3 4 0.228087 0.913664 0.679391 41.00000 0.02920 0.01771 =
0.06241 0.00901 -0.02427 -0.00232
O4 4 0.153992 1.021566 0.805207 51.00000 0.06684 0.10328 =
0.01668 0.02357 -0.01325 -0.03358
PART 2
O3' 4 0.227453 0.923644 0.667539 -41.00000 0.01687 0.02564 =
0.02115 0.00863 0.00441 0.00951
O4' 4 0.162463 0.981805 0.802451 -51.00000 0.04224 0.03499 =
0.02583 0.02122 0.01072 0.02020
PART 0
HKLF 4
REM lm5513/lt/Fengrui in Pca2(1)
REM R1 = 0.0264 for 10814 Fo > 4sig(Fo) and 0.0307 for all 11727 data
REM 295 parameters refined using 24 restraints
END
WGHT 0.0278 0.6939
REM Highest difference peak 1.843, deepest hole -1.100, 1-sigma level 0.097
Q1 1 0.0189 0.4443 0.9546 11.00000 0.05 1.84
Q2 1 0.0190 0.4458 1.0163 11.00000 0.05 1.71
Q3 1 0.0227 0.3356 0.9870 11.00000 0.05 0.94
Q4 1 0.1696 1.1009 0.6992 11.00000 0.05 0.65
Q5 1 -0.0185 0.3861 0.9807 11.00000 0.05 0.63
;
_shelx_res_checksum 79105
_shelx_hkl_file
;
0 1 0 611.90 22.91
0 1 0 641.36 21.96
0 -1 0 594.62 24.02
0 1 0 618.57 22.81
0 1 0 596.56 24.04
0 2 0 242.79 8.77
0 2 0 249.98 9.10
0 2 0 241.08 9.21
0 -2 0 242.97 8.83
0 -2 0 241.76 9.61
0 -2 0 244.81 9.04
0 3 0 422.78 15.36
0 3 0 408.93 16.11
0 -3 0 424.05 16.82
0 -3 0 446.82 15.84
0 3 0 433.11 15.93
0 3 0 447.45 19.20
0 -3 0 422.88 15.46
0 4 0 443.80 19.11
0 -4 0 429.96 15.83
0 4 0 428.05 15.92
0 -4 0 412.86 16.80
0 -4 0 423.96 15.46
0 4 0 419.20 15.35
0 -5 0 618.14 24.45
0 5 0 616.63 22.33
0 5 0 638.56 27.82
0 5 0 614.92 23.14
0 -5 0 593.23 22.45
0 -5 0 649.53 23.04
0 -6 0 52.20 2.62
0 6 0 53.44 2.52
0 6 0 54.13 2.62
0 6 0 51.99 2.41
0 -6 0 54.81 2.51
0 -6 0 50.41 2.38
0 -7 0 1.05 0.42
0 7 0 0.78 0.26
0 -7 0 0.82 0.38
0 7 0 0.50 0.36
0 -7 0 1.60 0.47
0 7 0 1.17 0.43
0 8 0 14.65 1.18
0 8 0 14.71 1.22
0 -8 0 15.06 1.17
0 -8 0 15.96 1.32
0 -8 0 16.59 1.26
0 -9 0 90.77 4.35
0 9 0 95.20 4.28
0 -9 0 96.37 4.50
0 -9 0 95.56 4.64
0 9 0 93.74 4.42
0 -9 0 96.56 4.26
0 10 0 44.20 2.70
0 10 0 50.46 2.73
0 -10 0 50.02 2.84
0 -10 0 46.20 2.71
0 -10 0 46.33 2.63
0 11 0 1.21 0.61
0 11 0 0.75 0.59
0 -11 0 1.21 0.67
0 -11 0 0.34 0.56
0 -11 0 0.56 0.55
0 -12 0 0.95 0.71
0 -12 0 0.74 0.61
0 -12 0 1.52 0.70
0 12 0 0.69 0.67
0 12 0 0.87 0.65
0 13 0 18.65 2.06
0 -13 0 16.21 1.96
0 13 0 15.41 1.94
0 -13 0 21.29 2.37
0 -13 0 18.05 2.03
0 14 0 42.13 3.08
0 14 0 43.46 2.97
0 -14 0 38.41 2.90
0 -14 0 39.13 2.84
0 -15 0 3.59 1.20
0 1 -1 0.02 0.08
0 1 -1 0.15 0.09
0 1 1 0.61 0.13
0 -1 1 0.01 0.08
0 1 -1 -0.07 0.08
0 -1 -1 -0.01 0.08
0 1 1 -0.06 0.06
0 -2 -1 -0.49 0.16
0 2 -1 -0.49 0.15
0 -2 1 -0.29 0.16
0 2 1 -0.32 0.15
0 2 1 -0.48 0.13
0 -2 -1 -0.50 0.14
0 2 1 0.34 0.20
0 -2 -1 -0.30 0.15
0 -2 1 -0.47 0.12
0 -2 1 -0.44 0.15
0 2 -1 -0.38 0.16
0 2 -1 -0.46 0.15
0 2 1 0.21 0.19
0 3 1 0.47 0.23
0 3 1 -0.12 0.14
0 -3 1 -0.18 0.17
0 -3 -1 -0.30 0.15
0 3 1 0.06 0.19
0 3 -1 -0.16 0.18
0 -3 1 -0.20 0.16
0 3 -1 0.02 0.19
0 3 -1 0.02 0.21
0 -3 1 -0.20 0.18
0 -3 -1 -0.26 0.19
0 -3 -1 -0.10 0.18
0 -4 1 0.10 0.22
0 4 1 0.14 0.20
0 -4 1 -0.10 0.19
0 4 1 0.03 0.19
0 -4 -1 -0.06 0.18
0 4 -1 0.03 0.20
0 4 -1 0.01 0.12
0 -4 -1 -0.10 0.21
0 4 -1 0.14 0.21
0 4 -1 0.25 0.21
0 -4 -1 0.30 0.23
0 4 1 0.05 0.15
0 -4 1 0.03 0.19
0 5 1 0.69 0.30
0 -5 1 0.26 0.26
0 5 1 0.24 0.25
0 -5 1 -0.02 0.21
0 5 1 0.09 0.17
0 -5 -1 0.02 0.24
0 -5 -1 -0.25 0.20
0 5 -1 0.10 0.13
0 5 -1 0.09 0.21
0 5 -1 0.30 0.27
0 -5 -1 -0.11 0.20
0 -5 1 -0.20 0.23
0 6 1 0.24 0.27
0 -6 -1 -0.03 0.25
0 -6 1 0.11 0.24
0 6 -1 0.15 0.26
0 -6 1 0.06 0.26
0 -6 -1 -0.12 0.24
0 -6 1 -0.07 0.26
0 6 1 0.12 0.17
0 6 -1 0.11 0.15
0 6 -1 -0.04 0.26
0 -6 -1 -0.44 0.19
0 6 1 0.03 0.24
0 7 1 0.24 0.29
0 -7 -1 0.04 0.31
0 -7 -1 -0.03 0.28
0 7 1 0.38 0.35
0 -7 1 -0.54 0.24
0 -7 -1 0.12 0.29
0 7 -1 -0.10 0.28
0 -7 1 0.25 0.31
0 -7 1 -0.08 0.29
0 7 1 0.15 0.19
0 7 -1 0.30 0.31
0 -8 1 -0.03 0.32
0 8 1 0.46 0.42
0 -8 1 0.39 0.40
0 8 -1 -0.17 0.34
0 -8 -1 -0.38 0.29
0 -8 -1 -0.23 0.32
0 -8 -1 -0.46 0.27
0 -8 1 -0.28 0.30
0 8 1 -0.14 0.30
0 8 -1 -0.08 0.34
0 -9 1 -0.05 0.39
0 -9 1 -0.05 0.40
0 -9 -1 0.36 0.47
0 -9 -1 0.33 0.42
0 -9 1 0.51 0.44
0 9 -1 -0.35 0.34
0 -9 1 0.45 0.42
0 -9 -1 -0.04 0.38
0 9 1 0.30 0.41
0 9 1 -0.20 0.33
0 -9 -1 0.49 0.45
0 9 -1 0.13 0.40
0 -10 -1 -0.53 0.30
0 -10 1 0.15 0.42
0 10 1 0.11 0.48
0 10 -1 -0.09 0.39
0 -10 -1 -0.09 0.45
0 10 1 -0.36 0.36
0 -10 -1 -0.06 0.49
0 10 -1 -0.06 0.40
0 -10 1 0.07 0.47
0 -10 1 -0.62 0.29
0 -10 1 -0.38 0.37
0 -11 -1 0.00 0.44
0 -11 1 0.70 0.56
0 -11 1 0.61 0.53
0 11 -1 0.21 0.58
0 11 -1 0.17 0.50
0 -11 1 0.21 0.54
0 11 1 0.67 0.61
0 11 1 -0.05 0.45
0 -11 -1 0.11 0.51
0 -11 -1 0.61 0.60
0 -12 1 -0.55 0.47
0 12 -1 -0.05 0.55
0 -12 1 0.46 0.65
0 -12 -1 0.32 0.60
0 -12 -1 0.27 0.64
0 12 1 0.01 0.52
0 -12 1 0.42 0.65
0 12 1 0.45 0.56
0 -12 -1 -0.34 0.56
0 12 -1 -0.38 0.53
0 -13 1 0.70 0.66
0 13 -1 0.57 0.75
0 -13 -1 0.42 0.71
0 -13 -1 0.41 0.67
0 -13 -1 0.05 0.73
0 13 -1 -0.42 0.55
0 13 1 0.39 0.60
0 13 1 -0.12 0.54
0 -13 1 0.24 0.63
0 -13 1 -0.03 0.65
0 -14 1 -0.27 0.63
0 14 1 -0.69 0.50
0 -14 1 -0.26 0.68
0 14 -1 0.47 0.73
0 14 -1 -0.01 0.81
0 -14 -1 0.33 0.75
0 -14 -1 0.00 0.68
0 -15 1 0.16 0.77
0 -15 -1 -0.39 0.73
0 1 -2 973.43 36.20
0 -1 2 950.26 35.52
0 1 2 983.71 43.81
0 1 -2 971.13 35.89
0 1 -2 970.51 34.61
0 -1 -2 1000.00 37.76
0 -1 2 940.03 37.81
0 1 2 953.12 37.67
0 -2 -2 53.03 1.98
0 -2 2 46.01 2.15
0 2 -2 46.71 1.97
0 2 2 52.76 2.06
0 2 -2 48.19 2.06
0 -2 2 48.02 1.98
0 2 2 59.96 2.18
0 2 2 52.27 1.99
0 2 2 54.65 2.46
0 2 -2 45.75 2.04
0 -2 -2 54.02 2.03
0 -2 2 47.83 2.03
0 3 2 14.06 0.80
0 -3 -2 13.69 0.74
0 3 -2 15.45 0.79
0 3 2 13.81 0.76
0 -3 2 13.44 0.83
0 -3 2 13.11 0.75
0 3 -2 14.86 0.81
0 -3 -2 13.69 0.78
0 3 2 13.39 0.85
0 -3 -2 13.46 0.81
0 -3 2 13.76 0.79
0 3 -2 15.43 0.82
0 -4 2 377.14 14.67
0 4 2 412.72 17.80
0 4 -2 385.73 14.93
0 4 2 387.84 14.25
0 4 -2 390.43 14.77
0 -4 2 379.92 14.33
0 -4 -2 411.89 15.60
0 4 2 400.52 14.78
0 -4 -2 409.59 14.67
0 4 -2 391.22 14.25
0 -4 -2 400.67 14.33
0 -4 2 389.06 15.61
0 -5 2 128.02 5.41
0 -5 -2 122.36 4.91
0 5 2 131.84 5.95
0 -5 2 131.41 4.96
0 5 2 124.14 4.93
0 5 -2 125.27 5.11
0 5 -2 125.14 5.14
0 -5 2 128.22 5.09
0 -5 -2 120.72 5.04
0 -5 -2 124.18 5.36
0 5 2 127.65 5.12
0 5 -2 126.97 4.94
0 6 -2 131.26 5.51
0 -6 -2 129.94 5.30
0 -6 2 131.39 5.47
0 6 -2 138.91 6.19
0 6 2 138.69 5.34
0 -6 2 140.47 5.84
0 6 -2 130.23 5.31
0 6 2 134.78 5.52
0 -6 -2 132.89 5.78
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9 -5 20 0.26 0.33
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9 -6 20 18.80 1.39
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9 -4 22 7.82 1.55
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9 -7 23 2.64 1.25
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10 -1 0 74.05 3.27
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10 -8 0 18.49 1.60
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10 -8 0 19.08 1.48
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10 -9 0 10.29 1.31
10 -9 0 10.25 1.33
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-10 -9 0 10.49 1.35
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10 -10 0 11.24 1.43
10 -10 0 10.18 1.43
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10 -12 0 -0.29 0.54
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10 -13 0 3.66 1.08
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10 -13 0 3.12 1.06
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-10 -1 -1 27.76 1.49
-10 -1 -1 25.41 1.43
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-10 1 1 24.71 1.37
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10 -1 1 24.21 1.48
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-10 -1 1 22.53 1.33
-10 -1 1 25.19 1.33
-10 1 -1 27.48 1.40
10 -1 -1 29.87 1.54
10 -1 -1 26.98 1.41
-10 1 -1 28.13 1.50
-10 -1 1 22.75 1.39
-10 -1 1 24.13 1.45
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-10 1 -1 28.02 1.43
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-10 -2 -1 25.82 1.41
-10 -2 -1 25.68 1.37
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10 2 -1 23.75 1.37
-10 2 1 24.24 1.34
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10 -2 1 21.47 1.40
10 2 1 26.28 1.40
-10 -2 1 21.92 1.39
10 -2 -1 24.77 1.36
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-10 -2 1 21.00 1.34
-10 2 -1 22.19 1.34
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-10 2 -1 20.80 1.24
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-10 -2 1 21.59 1.31
10 -2 -1 27.56 1.50
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-10 -3 -1 52.02 2.68
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-10 -3 -1 48.60 2.56
10 -3 1 57.38 2.60
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10 -3 1 58.83 2.77
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-10 -3 -1 55.07 2.56
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-10 3 -1 54.66 2.41
-10 -3 1 63.45 2.64
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-10 3 -1 54.60 2.62
-10 -3 1 57.00 2.64
10 -3 -1 55.34 2.72
10 -3 -1 51.05 2.53
-10 3 -1 55.58 2.51
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10 -4 1 37.58 2.08
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-10 -4 -1 39.96 1.98
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10 -4 1 35.26 1.94
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-10 -4 1 38.17 2.09
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10 -4 -1 40.64 2.00
-10 -4 1 36.59 1.96
10 -4 -1 37.70 2.07
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-10 -5 -1 38.52 2.06
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10 -5 1 39.68 2.10
10 -5 1 39.84 2.23
-10 -5 -1 38.57 2.20
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10 -5 -1 39.14 2.22
10 -5 -1 38.59 2.08
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-10 5 -1 36.05 1.93
-10 -5 1 40.42 2.24
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-10 -6 -1 71.59 3.46
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10 -6 1 68.61 3.30
-10 -6 -1 65.83 3.21
-10 -6 -1 67.10 3.31
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10 -6 -1 73.36 3.52
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-10 6 -1 75.00 3.43
-10 -6 1 65.19 3.28
10 -6 -1 68.90 3.29
-10 6 -1 71.76 3.24
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10 -7 1 9.10 1.12
-10 -7 -1 8.52 1.05
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-10 -7 -1 10.31 1.19
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-10 -7 -1 9.12 1.14
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10 -7 1 8.80 1.15
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-10 -7 1 9.16 1.11
10 -7 -1 9.06 1.12
10 -7 -1 10.23 1.17
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10 -8 1 7.83 1.12
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10 -8 1 8.70 1.16
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-10 -8 -1 5.92 0.99
10 -8 1 8.97 1.14
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10 -8 -1 7.48 1.05
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-10 -8 1 9.15 1.18
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10 -8 -1 6.34 1.01
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10 -9 1 23.79 1.75
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10 -9 1 20.64 1.72
-10 -9 -1 23.41 1.86
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10 -9 1 22.93 1.90
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-10 -9 -1 24.48 1.81
10 -9 -1 23.79 1.74
-10 -9 1 20.90 1.83
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-10 -9 1 22.96 1.87
-10 9 -1 21.91 1.85
10 -9 -1 22.25 1.79
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-10 -10 -1 57.59 3.42
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-10 -10 -1 57.74 3.32
10 -10 1 53.67 3.25
10 -10 1 59.16 3.22
10 -10 -1 59.88 3.22
-10 10 -1 59.32 3.44
-10 -10 1 56.93 3.35
-10 10 -1 59.76 3.21
-10 10 -1 59.67 3.33
-10 -10 1 60.12 3.47
10 -10 -1 55.53 3.24
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10 -11 1 39.79 2.64
-10 -11 -1 43.08 2.77
10 -11 1 36.24 2.64
-10 11 1 41.85 2.57
-10 -11 -1 44.93 2.89
10 -11 -1 43.14 2.69
-10 11 -1 35.85 2.58
-10 11 -1 36.35 2.51
10 -11 -1 40.64 2.71
-10 -11 1 40.25 2.81
-10 -11 1 36.72 2.62
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-10 -12 -1 6.00 1.32
-10 12 1 4.36 1.10
-10 -12 -1 5.84 1.28
10 -12 1 5.12 1.16
-10 -12 1 8.81 1.53
10 -12 -1 6.92 1.26
10 -12 -1 7.50 1.42
-10 12 -1 10.83 1.49
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-10 12 -1 8.91 1.45
10 -13 1 4.27 1.18
-10 -13 -1 3.56 1.10
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10 -13 1 3.63 1.11
-10 13 1 2.25 0.87
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10 -13 -1 2.70 1.04
-10 -13 1 3.84 1.11
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10 -13 -1 2.51 0.96
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10 -14 1 10.49 1.73
-10 -14 -1 10.11 1.73
10 -14 -1 12.88 1.89
10 -14 -1 9.89 1.74
-10 -14 1 9.96 1.73
10 0 2 45.40 2.16
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-10 0 -2 46.84 2.15
10 0 -2 46.83 2.28
-10 0 2 45.51 2.21
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-10 -1 -2 41.14 1.99
10 -1 2 44.42 2.22
10 1 -2 44.41 2.08
-10 1 2 42.19 1.82
-10 -1 -2 42.98 2.07
-10 1 2 38.86 2.02
10 -1 2 44.57 2.09
10 1 -2 47.22 2.23
-10 -1 -2 45.36 2.15
-10 1 2 42.25 1.96
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-10 1 -2 41.39 2.06
10 1 2 42.04 2.07
-10 -1 2 40.15 2.04
-10 -1 2 41.70 2.11
-10 -1 2 41.63 2.00
10 -1 -2 43.82 2.06
-10 -1 2 40.19 1.91
10 -1 -2 44.13 2.19
-10 1 -2 46.25 2.16
-10 1 -2 46.06 2.03
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-10 -2 -2 10.62 0.85
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-10 -2 -2 10.59 0.88
-10 -2 -2 10.75 0.83
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10 -2 2 12.72 0.97
10 -2 2 11.09 0.87
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10 -2 -2 11.78 0.92
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10 -2 -2 11.96 0.86
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10 -3 2 12.46 1.02
10 -3 2 16.03 1.05
10 -3 -2 13.56 0.98
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10 -3 -2 14.54 1.06
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10 -4 2 20.59 1.34
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10 -4 2 17.61 1.20
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10 -4 -2 17.41 1.24
10 -4 -2 15.94 1.14
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10 -5 2 11.91 1.09
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10 -5 2 12.17 1.02
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10 -5 -2 10.19 0.95
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10 -5 -2 13.24 1.09
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-10 6 2 17.09 1.22
-10 -6 -2 18.30 1.39
-10 -6 -2 19.38 1.38
10 -6 2 17.10 1.40
10 -6 2 18.71 1.36
-10 6 2 16.29 1.14
-10 -6 -2 17.19 1.28
-10 6 -2 20.24 1.45
10 -6 -2 17.86 1.38
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10 -6 -2 17.33 1.32
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10 -7 2 1.38 0.57
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10 -7 -2 0.71 0.48
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10 -7 -2 0.56 0.45
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10 -8 2 2.14 0.68
10 -8 2 3.32 0.75
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10 -8 2 3.66 0.79
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10 -8 -2 3.21 0.75
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10 -9 2 10.47 1.35
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10 -9 2 10.73 1.47
-10 -9 -2 9.21 1.28
10 -9 2 11.64 1.41
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10 -9 -2 9.57 1.28
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10 -9 -2 9.99 1.27
10 -10 2 1.58 0.69
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10 -10 2 2.72 0.91
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10 -10 -2 3.50 0.90
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10 -10 -2 3.21 0.87
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10 -11 2 8.05 1.40
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-10 -11 -2 5.81 1.18
10 -11 2 9.61 1.42
10 -11 -2 7.48 1.30
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-10 -11 2 8.25 1.41
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-10 11 -2 9.21 1.50
10 -11 -2 8.31 1.30
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10 -12 2 1.06 0.71
10 -12 2 0.98 0.78
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-10 -12 -2 0.28 0.74
10 -12 -2 0.83 0.68
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10 -12 -2 0.30 0.74
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10 -13 2 2.69 1.00
10 -13 2 1.77 0.87
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-10 -13 -2 1.79 0.95
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10 -13 -2 2.40 1.01
10 -13 -2 0.12 0.77
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10 -14 2 4.75 1.34
-10 -14 -2 5.23 1.28
10 -14 -2 6.64 1.45
10 -14 -2 3.90 1.18
-10 -14 2 2.08 0.95
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-10 0 -3 261.14 9.70
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10 0 3 264.18 10.85
10 0 -3 264.08 9.95
10 0 -3 265.22 10.57
-10 0 -3 255.91 9.93
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10 -1 3 216.09 9.04
-10 -1 -3 230.73 8.87
-10 -1 -3 221.85 8.33
-10 -1 -3 215.71 8.52
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10 -1 -3 225.30 8.50
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-10 1 -3 213.57 8.31
-10 -1 3 210.24 8.30
-10 -1 3 213.53 8.31
-10 1 -3 219.02 8.85
-10 1 -3 207.83 8.50
10 1 3 221.40 8.52
-10 -1 3 207.14 8.49
10 1 3 226.49 9.06
10 -1 -3 219.50 9.01
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-10 2 3 73.08 2.98
-10 2 3 76.77 2.89
10 -2 3 69.82 3.22
-10 2 3 75.25 3.19
-10 2 3 72.02 3.15
10 2 -3 77.28 3.25
-10 -2 -3 77.43 3.40
-10 -2 -3 78.47 3.22
10 -2 3 75.32 3.46
-10 -2 -3 78.85 3.31
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-10 2 -3 70.66 3.27
-10 2 -3 73.95 3.22
-10 2 -3 74.36 3.40
-10 2 -3 74.15 3.32
-10 -2 3 68.92 3.17
10 -2 -3 75.47 3.41
-10 -2 3 72.36 3.38
10 -2 -3 77.02 3.23
-10 -2 3 68.05 3.24
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-10 -4 -3 108.45 4.74
10 -4 3 109.34 4.98
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10 -4 -3 111.79 4.66
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10 -5 -3 76.57 3.44
-10 -5 3 77.57 3.72
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-10 -6 -3 109.22 4.81
10 -6 3 98.56 4.78
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-10 -6 3 97.80 4.49
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10 -6 -3 107.00 4.52
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10 -7 -3 6.98 0.95
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10 -8 3 13.21 1.23
-10 -8 -3 13.51 1.48
10 -8 3 14.33 1.40
-10 -8 3 12.85 1.25
-10 -8 3 13.99 1.40
10 -8 -3 12.02 1.35
-10 -8 3 14.27 1.32
10 -8 -3 10.68 1.26
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-10 8 -3 13.45 1.22
-10 8 -3 13.95 1.29
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10 -9 3 35.21 2.32
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-10 9 3 36.06 2.14
10 -9 3 36.56 2.27
-10 -9 -3 32.43 2.23
-10 -9 -3 38.93 2.43
-10 -9 3 36.89 2.38
-10 -9 3 39.41 2.47
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-10 9 -3 32.76 2.19
-10 9 -3 34.04 2.34
10 -9 -3 32.42 2.20
10 -9 -3 34.68 2.19
-10 -9 3 36.15 2.51
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-10 -10 -3 42.33 2.69
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10 -10 3 41.07 2.74
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-10 10 -3 39.62 2.77
10 -10 -3 44.88 2.69
10 -10 -3 43.19 2.75
-10 -10 3 44.85 2.86
-10 10 -3 41.54 2.73
-10 -10 3 40.73 2.89
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