# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_coden_Cambridge 222
_journal_volume ?
_journal_page_first ?
_journal_year ?
loop_
_publ_author_name
_publ_author_address
'Dastgir, Sarim'
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario M3J 1P3
Canada
;
'Lavoie, Gino'
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario M3J 1P3
Canada
;
_publ_contact_author_name 'Lavoie, Gino '
_publ_contact_author_email glavoie@yorku.ca
_publ_section_title
;
Coordination Study of a New Class
of Imine Imidazol-2-imine Ligands to Titanium(IV)
and Palladium(II)
;
_publ_contact_author_address
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario M3J 1P3
Canada
;
_publ_contact_author_fax '+1 416 736 5936'
_publ_contact_author_phone '+1 416 736 2100'
#TrackingRef '- CombinedCIF.cif'
_publ_requested_journal 'Dalton Trans.'
# Attachment '- CombinedCIF.cif'
data_k09163a
_database_code_depnum_ccdc_archive 'CCDC 778192'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C31 H37 N4, 2(C H2 Cl2), Cl'
_chemical_formula_sum 'C33 H41 Cl5 N4'
_chemical_formula_weight 670.95
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.8893(8)
_cell_length_b 15.8157(5)
_cell_length_c 13.8555(9)
_cell_angle_alpha 90.00
_cell_angle_beta 90.3420(18)
_cell_angle_gamma 90.00
_cell_volume 3481.8(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 19493
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 25.0
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.280
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1408
_exptl_absorpt_coefficient_mu 0.445
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.780
_exptl_absorpt_correction_T_max 0.989
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_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 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 19493
_diffrn_reflns_av_R_equivalents 0.0743
_diffrn_reflns_av_sigmaI/netI 0.0864
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.56
_diffrn_reflns_theta_max 25.00
_reflns_number_total 6120
_reflns_number_gt 3435
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
;
_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^)+(0.0896P)^2^] 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 mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6120
_refine_ls_number_parameters 392
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1251
_refine_ls_R_factor_gt 0.0590
_refine_ls_wR_factor_ref 0.1736
_refine_ls_wR_factor_gt 0.1379
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_restrained_S_all 1.018
_refine_ls_shift/su_max 0.000
_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
N1 N 0.37568(18) 0.56102(16) 0.1745(2) 0.0301(7) Uani 1 1 d . . .
N2 N 0.45871(17) 0.49478(15) 0.2740(2) 0.0264(7) Uani 1 1 d . . .
N3 N 0.31977(17) 0.43545(15) 0.2417(2) 0.0273(7) Uani 1 1 d . . .
N4 N 0.26812(18) 0.30241(18) 0.2603(2) 0.0307(7) Uani 1 1 d . . .
H4N H 0.274(2) 0.249(2) 0.248(2) 0.033(10) Uiso 1 1 d . . .
C1 C 0.3828(2) 0.49035(19) 0.2290(2) 0.0268(8) Uani 1 1 d . . .
C2 C 0.4486(2) 0.6094(2) 0.1852(3) 0.0315(9) Uani 1 1 d . . .
H2A H 0.4598 0.6619 0.1546 0.038 Uiso 1 1 calc R . .
C3 C 0.5001(2) 0.56863(19) 0.2460(3) 0.0300(9) Uani 1 1 d . . .
H3A H 0.5545 0.5865 0.2664 0.036 Uiso 1 1 calc R . .
C4 C 0.3290(2) 0.35366(19) 0.2305(3) 0.0267(8) Uani 1 1 d . . .
C5 C 0.4031(2) 0.3111(2) 0.1840(3) 0.0341(9) Uani 1 1 d . . .
H5A H 0.4369 0.3533 0.1499 0.051 Uiso 1 1 calc R . .
H5B H 0.3830 0.2684 0.1380 0.051 Uiso 1 1 calc R . .
H5C H 0.4377 0.2838 0.2338 0.051 Uiso 1 1 calc R . .
C6 C 0.1954(2) 0.32809(19) 0.3142(3) 0.0301(9) Uani 1 1 d . . .
C7 C 0.1928(2) 0.3022(2) 0.4109(3) 0.0345(9) Uani 1 1 d . . .
C8 C 0.1210(3) 0.3234(2) 0.4634(3) 0.0462(11) Uani 1 1 d . . .
H8A H 0.1175 0.3075 0.5294 0.055 Uiso 1 1 calc R . .
C9 C 0.0554(3) 0.3668(2) 0.4211(3) 0.0510(11) Uani 1 1 d . . .
H9A H 0.0069 0.3800 0.4578 0.061 Uiso 1 1 calc R . .
C10 C 0.0598(3) 0.3917(2) 0.3248(3) 0.0478(11) Uani 1 1 d . . .
H10A H 0.0143 0.4218 0.2963 0.057 Uiso 1 1 calc R . .
C11 C 0.1311(2) 0.37244(19) 0.2697(3) 0.0332(9) Uani 1 1 d . . .
C12 C 0.2629(3) 0.2525(2) 0.4570(3) 0.0450(11) Uani 1 1 d . . .
H12A H 0.3167 0.2805 0.4444 0.068 Uiso 1 1 calc R . .
H12B H 0.2638 0.1953 0.4300 0.068 Uiso 1 1 calc R . .
H12C H 0.2538 0.2494 0.5269 0.068 Uiso 1 1 calc R . .
C13 C 0.1338(3) 0.3982(2) 0.1646(3) 0.0453(11) Uani 1 1 d . . .
H13A H 0.1590 0.3525 0.1266 0.068 Uiso 1 1 calc R . .
H13B H 0.1677 0.4496 0.1579 0.068 Uiso 1 1 calc R . .
H13C H 0.0765 0.4091 0.1412 0.068 Uiso 1 1 calc R . .
C14 C 0.3037(2) 0.58342(19) 0.1152(3) 0.0307(9) Uani 1 1 d . . .
C15 C 0.2959(2) 0.5473(2) 0.0237(3) 0.0322(9) Uani 1 1 d . . .
C16 C 0.2287(2) 0.5738(2) -0.0338(3) 0.0357(9) Uani 1 1 d . . .
H16A H 0.2217 0.5499 -0.0962 0.043 Uiso 1 1 calc R . .
C17 C 0.1717(2) 0.6343(2) -0.0024(3) 0.0366(9) Uani 1 1 d . . .
C18 C 0.1810(2) 0.6660(2) 0.0903(3) 0.0382(10) Uani 1 1 d . . .
H18A H 0.1413 0.7060 0.1132 0.046 Uiso 1 1 calc R . .
C19 C 0.2464(2) 0.6412(2) 0.1511(3) 0.0338(9) Uani 1 1 d . . .
C20 C 0.2532(3) 0.6742(2) 0.2526(3) 0.0444(11) Uani 1 1 d . . .
H20A H 0.2576 0.6265 0.2976 0.067 Uiso 1 1 calc R . .
H20B H 0.2032 0.7077 0.2678 0.067 Uiso 1 1 calc R . .
H20C H 0.3035 0.7097 0.2587 0.067 Uiso 1 1 calc R . .
C21 C 0.1010(3) 0.6643(3) -0.0668(3) 0.0502(11) Uani 1 1 d . . .
H21A H 0.0514 0.6767 -0.0275 0.075 Uiso 1 1 calc R . .
H21B H 0.0872 0.6201 -0.1138 0.075 Uiso 1 1 calc R . .
H21C H 0.1185 0.7156 -0.1009 0.075 Uiso 1 1 calc R . .
C22 C 0.3560(3) 0.4797(2) -0.0107(3) 0.0413(10) Uani 1 1 d . . .
H22A H 0.4137 0.5014 -0.0079 0.062 Uiso 1 1 calc R . .
H22B H 0.3419 0.4641 -0.0772 0.062 Uiso 1 1 calc R . .
H22C H 0.3513 0.4299 0.0310 0.062 Uiso 1 1 calc R . .
C23 C 0.4915(2) 0.43420(18) 0.3433(3) 0.0272(8) Uani 1 1 d . . .
C24 C 0.4483(2) 0.42187(19) 0.4297(3) 0.0284(8) Uani 1 1 d . . .
C25 C 0.4819(2) 0.3623(2) 0.4939(3) 0.0322(9) Uani 1 1 d . . .
H25A H 0.4534 0.3517 0.5527 0.039 Uiso 1 1 calc R . .
C26 C 0.5556(2) 0.31809(19) 0.4746(3) 0.0290(9) Uani 1 1 d . . .
C27 C 0.5976(2) 0.33500(19) 0.3892(3) 0.0298(9) Uani 1 1 d . . .
H27A H 0.6492 0.3068 0.3768 0.036 Uiso 1 1 calc R . .
C28 C 0.5664(2) 0.39212(19) 0.3211(2) 0.0276(8) Uani 1 1 d . . .
C29 C 0.3709(2) 0.4700(2) 0.4572(3) 0.0336(9) Uani 1 1 d . . .
H29A H 0.3642 0.4682 0.5275 0.050 Uiso 1 1 calc R . .
H29B H 0.3216 0.4443 0.4261 0.050 Uiso 1 1 calc R . .
H29C H 0.3763 0.5288 0.4362 0.050 Uiso 1 1 calc R . .
C30 C 0.5914(3) 0.2554(2) 0.5460(3) 0.0432(10) Uani 1 1 d . . .
H30A H 0.5769 0.2730 0.6117 0.065 Uiso 1 1 calc R . .
H30B H 0.6528 0.2534 0.5396 0.065 Uiso 1 1 calc R . .
H30C H 0.5678 0.1993 0.5332 0.065 Uiso 1 1 calc R . .
C31 C 0.6135(2) 0.4076(2) 0.2294(3) 0.0325(9) Uani 1 1 d . . .
H31A H 0.5734 0.4157 0.1762 0.049 Uiso 1 1 calc R . .
H31B H 0.6496 0.3589 0.2155 0.049 Uiso 1 1 calc R . .
H31C H 0.6484 0.4583 0.2365 0.049 Uiso 1 1 calc R . .
Cl1 Cl 0.28891(6) 0.11324(5) 0.20973(7) 0.0406(3) Uani 1 1 d . . .
Cl2 Cl 0.16841(8) 0.59939(7) 0.68321(9) 0.0625(4) Uani 1 1 d . . .
Cl3 Cl 0.17340(9) 0.58459(9) 0.47468(10) 0.0848(5) Uani 1 1 d . . .
C32 C 0.1655(3) 0.5301(3) 0.5847(3) 0.0575(12) Uani 1 1 d . . .
H32A H 0.1121 0.4978 0.5856 0.069 Uiso 1 1 calc R . .
H32B H 0.2125 0.4892 0.5903 0.069 Uiso 1 1 calc R . .
Cl4 Cl -0.00423(8) 0.37388(8) 0.70134(9) 0.0700(4) Uani 1 1 d . . .
Cl5 Cl 0.05938(9) 0.42578(8) 0.88912(10) 0.0800(4) Uani 1 1 d . . .
C33 C 0.0711(3) 0.3557(3) 0.7920(3) 0.0549(12) Uani 1 1 d . . .
H33A H 0.1281 0.3622 0.7646 0.066 Uiso 1 1 calc R . .
H33B H 0.0656 0.2969 0.8156 0.066 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
N1 0.0272(18) 0.0282(15) 0.0349(19) 0.0039(13) -0.0064(14) -0.0031(13)
N2 0.0238(17) 0.0233(14) 0.0321(18) 0.0020(12) -0.0009(14) -0.0026(12)
N3 0.0255(18) 0.0216(15) 0.0348(18) 0.0013(12) -0.0037(14) -0.0033(12)
N4 0.0276(19) 0.0224(16) 0.042(2) -0.0016(13) 0.0029(15) 0.0003(13)
C1 0.030(2) 0.0236(17) 0.027(2) -0.0005(15) -0.0008(17) 0.0005(15)
C2 0.029(2) 0.0266(18) 0.038(2) 0.0020(16) -0.0012(18) -0.0062(16)
C3 0.027(2) 0.0282(18) 0.035(2) 0.0015(16) -0.0008(18) -0.0035(15)
C4 0.023(2) 0.0246(18) 0.033(2) 0.0004(15) -0.0049(17) -0.0006(15)
C5 0.028(2) 0.0309(19) 0.044(2) -0.0035(16) 0.0023(18) -0.0028(15)
C6 0.024(2) 0.0226(17) 0.043(3) -0.0013(16) 0.0027(18) -0.0036(15)
C7 0.029(2) 0.0255(18) 0.049(3) -0.0005(17) 0.0008(19) -0.0028(15)
C8 0.049(3) 0.049(2) 0.040(3) 0.0011(19) 0.008(2) -0.003(2)
C9 0.034(3) 0.055(3) 0.064(3) 0.002(2) 0.011(2) 0.013(2)
C10 0.029(3) 0.043(2) 0.071(3) 0.007(2) 0.003(2) 0.0023(18)
C11 0.026(2) 0.0267(18) 0.047(3) -0.0001(17) -0.0046(19) -0.0001(16)
C12 0.045(3) 0.042(2) 0.047(3) 0.0074(19) -0.004(2) 0.0002(19)
C13 0.036(3) 0.051(2) 0.049(3) 0.0047(19) -0.008(2) 0.0034(18)
C14 0.029(2) 0.0250(17) 0.038(2) 0.0086(16) -0.0057(18) -0.0047(15)
C15 0.032(2) 0.0285(18) 0.036(2) 0.0054(16) -0.0009(19) -0.0040(16)
C16 0.039(3) 0.036(2) 0.032(2) 0.0021(16) -0.005(2) -0.0091(17)
C17 0.030(2) 0.039(2) 0.040(3) 0.0115(18) -0.0068(19) -0.0032(17)
C18 0.030(2) 0.039(2) 0.046(3) 0.0067(18) 0.000(2) 0.0045(17)
C19 0.035(2) 0.0301(19) 0.036(2) 0.0045(16) -0.0025(19) -0.0043(17)
C20 0.049(3) 0.042(2) 0.042(3) 0.0017(18) -0.004(2) 0.0071(18)
C21 0.043(3) 0.060(3) 0.048(3) 0.005(2) -0.011(2) 0.007(2)
C22 0.048(3) 0.037(2) 0.039(2) 0.0034(17) -0.001(2) -0.0009(18)
C23 0.026(2) 0.0205(17) 0.035(2) 0.0011(15) -0.0031(17) -0.0016(15)
C24 0.028(2) 0.0244(17) 0.033(2) -0.0030(15) -0.0056(18) -0.0038(15)
C25 0.037(2) 0.0299(18) 0.030(2) -0.0034(15) 0.0015(18) -0.0022(16)
C26 0.033(2) 0.0253(17) 0.029(2) 0.0001(15) -0.0055(18) -0.0036(15)
C27 0.028(2) 0.0273(18) 0.034(2) -0.0007(16) -0.0041(18) 0.0007(15)
C28 0.028(2) 0.0239(17) 0.031(2) -0.0048(15) -0.0041(17) -0.0042(15)
C29 0.031(2) 0.0331(19) 0.037(2) -0.0060(16) 0.0019(18) -0.0007(16)
C30 0.048(3) 0.036(2) 0.046(3) 0.0087(18) -0.004(2) 0.0040(18)
C31 0.032(2) 0.0314(19) 0.035(2) -0.0017(16) 0.0007(18) -0.0001(16)
Cl1 0.0333(6) 0.0275(5) 0.0609(7) -0.0065(4) -0.0058(5) 0.0023(4)
Cl2 0.0466(8) 0.0711(7) 0.0696(9) -0.0060(6) -0.0102(6) 0.0049(5)
Cl3 0.0682(10) 0.1235(11) 0.0628(9) 0.0399(8) 0.0180(7) 0.0392(8)
C32 0.060(3) 0.061(3) 0.052(3) 0.008(2) 0.003(2) 0.015(2)
Cl4 0.0555(8) 0.0879(8) 0.0667(9) 0.0061(7) -0.0077(7) -0.0006(6)
Cl5 0.0890(11) 0.0780(8) 0.0729(10) -0.0125(7) -0.0008(8) -0.0150(7)
C33 0.042(3) 0.050(2) 0.073(3) 0.006(2) -0.003(2) 0.009(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.354(4) . ?
N1 C2 1.396(4) . ?
N1 C14 1.448(4) . ?
N2 C1 1.356(4) . ?
N2 C3 1.397(4) . ?
N2 C23 1.450(4) . ?
N3 C4 1.311(4) . ?
N3 C1 1.338(4) . ?
N4 C4 1.330(4) . ?
N4 C6 1.438(4) . ?
N4 H4N 0.86(3) . ?
C2 C3 1.336(5) . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9500 . ?
C4 C5 1.504(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.382(5) . ?
C6 C7 1.401(5) . ?
C7 C8 1.397(5) . ?
C7 C12 1.503(5) . ?
C8 C9 1.377(6) . ?
C8 H8A 0.9500 . ?
C9 C10 1.394(6) . ?
C9 H9A 0.9500 . ?
C10 C11 1.403(5) . ?
C10 H10A 0.9500 . ?
C11 C13 1.512(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.385(5) . ?
C14 C15 1.396(5) . ?
C15 C16 1.392(5) . ?
C15 C22 1.512(5) . ?
C16 C17 1.389(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.386(5) . ?
C17 C21 1.507(5) . ?
C18 C19 1.389(5) . ?
C18 H18A 0.9500 . ?
C19 C20 1.503(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.397(5) . ?
C23 C28 1.400(5) . ?
C24 C25 1.399(5) . ?
C24 C29 1.498(5) . ?
C25 C26 1.391(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.388(5) . ?
C26 C30 1.509(5) . ?
C27 C28 1.395(5) . ?
C27 H27A 0.9500 . ?
C28 C31 1.498(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Cl2 C32 1.752(4) . ?
Cl3 C32 1.756(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
Cl4 C33 1.754(4) . ?
Cl5 C33 1.755(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
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 N1 C2 109.0(3) . . ?
C1 N1 C14 125.6(3) . . ?
C2 N1 C14 125.4(3) . . ?
C1 N2 C3 109.5(3) . . ?
C1 N2 C23 125.8(3) . . ?
C3 N2 C23 124.6(3) . . ?
C4 N3 C1 122.7(3) . . ?
C4 N4 C6 125.3(3) . . ?
C4 N4 H4N 116(2) . . ?
C6 N4 H4N 118(2) . . ?
N3 C1 N1 123.3(3) . . ?
N3 C1 N2 129.6(3) . . ?
N1 C1 N2 106.6(3) . . ?
C3 C2 N1 107.9(3) . . ?
C3 C2 H2A 126.0 . . ?
N1 C2 H2A 126.0 . . ?
C2 C3 N2 106.9(3) . . ?
C2 C3 H3A 126.5 . . ?
N2 C3 H3A 126.5 . . ?
N3 C4 N4 118.8(3) . . ?
N3 C4 C5 125.5(3) . . ?
N4 C4 C5 115.7(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 123.3(3) . . ?
C11 C6 N4 120.4(3) . . ?
C7 C6 N4 116.2(3) . . ?
C8 C7 C6 117.2(3) . . ?
C8 C7 C12 120.5(4) . . ?
C6 C7 C12 122.3(3) . . ?
C9 C8 C7 121.0(4) . . ?
C9 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C9 C10 C11 120.4(4) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C6 C11 C10 117.7(4) . . ?
C6 C11 C13 122.7(3) . . ?
C10 C11 C13 119.6(3) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 122.7(3) . . ?
C19 C14 N1 118.5(3) . . ?
C15 C14 N1 118.7(3) . . ?
C16 C15 C14 117.4(3) . . ?
C16 C15 C22 121.1(3) . . ?
C14 C15 C22 121.5(3) . . ?
C17 C16 C15 121.8(3) . . ?
C17 C16 H16A 119.1 . . ?
C15 C16 H16A 119.1 . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 C21 120.7(4) . . ?
C16 C17 C21 121.1(4) . . ?
C17 C18 C19 122.4(4) . . ?
C17 C18 H18A 118.8 . . ?
C19 C18 H18A 118.8 . . ?
C14 C19 C18 117.4(3) . . ?
C14 C19 C20 121.3(3) . . ?
C18 C19 C20 121.3(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 123.0(3) . . ?
C24 C23 N2 118.9(3) . . ?
C28 C23 N2 118.1(3) . . ?
C23 C24 C25 116.8(3) . . ?
C23 C24 C29 123.8(3) . . ?
C25 C24 C29 119.4(3) . . ?
C26 C25 C24 122.3(3) . . ?
C26 C25 H25A 118.8 . . ?
C24 C25 H25A 118.8 . . ?
C27 C26 C25 118.5(3) . . ?
C27 C26 C30 120.2(3) . . ?
C25 C26 C30 121.3(3) . . ?
C26 C27 C28 122.0(3) . . ?
C26 C27 H27A 119.0 . . ?
C28 C27 H27A 119.0 . . ?
C27 C28 C23 117.3(3) . . ?
C27 C28 C31 120.2(3) . . ?
C23 C28 C31 122.5(3) . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Cl2 C32 Cl3 111.6(2) . . ?
Cl2 C32 H32A 109.3 . . ?
Cl3 C32 H32A 109.3 . . ?
Cl2 C32 H32B 109.3 . . ?
Cl3 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
Cl4 C33 Cl5 111.7(2) . . ?
Cl4 C33 H33A 109.3 . . ?
Cl5 C33 H33A 109.3 . . ?
Cl4 C33 H33B 109.3 . . ?
Cl5 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
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
N4 H4N Cl1 0.86(3) 2.23(3) 3.091(3) 178(3) .
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.493
_refine_diff_density_min -0.362
_refine_diff_density_rms 0.071
#
data_k09161
_database_code_depnum_ccdc_archive 'CCDC 778193'
#TrackingRef '- CombinedCIF.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C37 H49 N4, 2(C H2 Cl2), Cl'
_chemical_formula_sum 'C39 H53 Cl5 N4'
_chemical_formula_weight 755.10
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 10.9207(3)
_cell_length_b 23.5718(6)
_cell_length_c 16.7583(4)
_cell_angle_alpha 90.00
_cell_angle_beta 108.0720(12)
_cell_angle_gamma 90.00
_cell_volume 4101.11(18)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 17529
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 25.0
_exptl_crystal_description plate
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.223
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1600
_exptl_absorpt_coefficient_mu 0.385
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.522
_exptl_absorpt_correction_T_max 0.935
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_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 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 17529
_diffrn_reflns_av_R_equivalents 0.0516
_diffrn_reflns_av_sigmaI/netI 0.0553
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.56
_diffrn_reflns_theta_max 25.00
_reflns_number_total 7134
_reflns_number_gt 5139
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
;
_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^)+(0.0730P)^2^+7.5468P] 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 mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7134
_refine_ls_number_parameters 473
_refine_ls_number_restraints 18
_refine_ls_R_factor_all 0.1010
_refine_ls_R_factor_gt 0.0720
_refine_ls_wR_factor_ref 0.2027
_refine_ls_wR_factor_gt 0.1850
_refine_ls_goodness_of_fit_ref 1.094
_refine_ls_restrained_S_all 1.093
_refine_ls_shift/su_max 0.000
_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
N1 N 0.4623(3) 0.66150(12) 0.17532(18) 0.0291(7) Uani 1 1 d . . .
N2 N 0.5171(3) 0.67585(12) 0.31009(18) 0.0301(7) Uani 1 1 d . . .
N3 N 0.4129(3) 0.58820(12) 0.26255(18) 0.0297(7) Uani 1 1 d . . .
N4 N 0.3807(3) 0.49247(14) 0.2517(2) 0.0340(7) Uani 1 1 d . . .
H4N H 0.406(4) 0.4596(19) 0.242(3) 0.037(11) Uiso 1 1 d . . .
C1 C 0.4667(3) 0.63703(15) 0.2492(2) 0.0279(8) Uani 1 1 d . . .
C2 C 0.5096(4) 0.71685(16) 0.1903(2) 0.0334(9) Uani 1 1 d . . .
H2A H 0.5163 0.7433 0.1491 0.040 Uiso 1 1 calc R . .
C3 C 0.5438(4) 0.72602(16) 0.2736(2) 0.0347(9) Uani 1 1 d . . .
H3A H 0.5791 0.7599 0.3021 0.042 Uiso 1 1 calc R . .
C4 C 0.4499(3) 0.53786(15) 0.2467(2) 0.0299(8) Uani 1 1 d . . .
C5 C 0.5708(4) 0.52616(17) 0.2233(3) 0.0434(10) Uani 1 1 d . . .
H5A H 0.6334 0.5566 0.2452 0.065 Uiso 1 1 calc R . .
H5B H 0.5493 0.5245 0.1620 0.065 Uiso 1 1 calc R . .
H5C H 0.6078 0.4898 0.2475 0.065 Uiso 1 1 calc R . .
C6 C 0.2554(4) 0.49549(16) 0.2632(2) 0.0330(8) Uani 1 1 d . . .
C7 C 0.1488(4) 0.48530(17) 0.1931(3) 0.0389(9) Uani 1 1 d . . .
C8 C 0.0279(4) 0.48823(19) 0.2044(3) 0.0490(11) Uani 1 1 d . . .
H8A H -0.0468 0.4821 0.1577 0.059 Uiso 1 1 calc R . .
C9 C 0.0143(5) 0.4999(2) 0.2819(3) 0.0543(12) Uani 1 1 d . . .
H9A H -0.0693 0.5012 0.2881 0.065 Uiso 1 1 calc R . .
C10 C 0.1201(4) 0.50951(19) 0.3497(3) 0.0480(11) Uani 1 1 d . . .
H10A H 0.1094 0.5181 0.4025 0.058 Uiso 1 1 calc R . .
C11 C 0.2446(4) 0.50684(16) 0.3423(2) 0.0365(9) Uani 1 1 d . . .
C12 C 0.1646(4) 0.47188(19) 0.1093(3) 0.0477(11) Uani 1 1 d . . .
H12A H 0.0797 0.4697 0.0669 0.072 Uiso 1 1 calc R . .
H12B H 0.2089 0.4354 0.1125 0.072 Uiso 1 1 calc R . .
H12C H 0.2156 0.5018 0.0940 0.072 Uiso 1 1 calc R . .
C13 C 0.3613(4) 0.51577(19) 0.4172(3) 0.0447(10) Uani 1 1 d . . .
H13A H 0.4265 0.4872 0.4173 0.067 Uiso 1 1 calc R . .
H13B H 0.3372 0.5123 0.4687 0.067 Uiso 1 1 calc R . .
H13C H 0.3965 0.5537 0.4145 0.067 Uiso 1 1 calc R . .
C14 C 0.4024(3) 0.63708(15) 0.0930(2) 0.0304(8) Uani 1 1 d . . .
C15 C 0.2675(4) 0.63109(16) 0.0656(2) 0.0325(8) Uani 1 1 d . . .
C16 C 0.2129(4) 0.60660(17) -0.0130(2) 0.0386(9) Uani 1 1 d . . .
H16A H 0.1224 0.6008 -0.0332 0.046 Uiso 1 1 calc R . .
C17 C 0.2882(4) 0.59050(18) -0.0623(2) 0.0431(10) Uani 1 1 d . . .
H17A H 0.2488 0.5735 -0.1155 0.052 Uiso 1 1 calc R . .
C18 C 0.4190(4) 0.59890(17) -0.0349(2) 0.0385(9) Uani 1 1 d . . .
H18A H 0.4687 0.5888 -0.0703 0.046 Uiso 1 1 calc R . .
C19 C 0.4799(4) 0.62194(16) 0.0437(2) 0.0338(9) Uani 1 1 d . . .
C20 C 0.1841(4) 0.65469(19) 0.1160(3) 0.0421(10) Uani 1 1 d . . .
H20A H 0.2306 0.6473 0.1767 0.051 Uiso 1 1 calc R . .
C21 C 0.0526(4) 0.6273(2) 0.0961(3) 0.0509(11) Uani 1 1 d . . .
H21A H 0.0623 0.5859 0.0996 0.076 Uiso 1 1 calc R . .
H21B H 0.0001 0.6380 0.0393 0.076 Uiso 1 1 calc R . .
H21C H 0.0103 0.6402 0.1366 0.076 Uiso 1 1 calc R . .
C22 C 0.1691(5) 0.7189(2) 0.1050(4) 0.0671(15) Uani 1 1 d . . .
H22A H 0.1236 0.7338 0.1426 0.101 Uiso 1 1 calc R . .
H22B H 0.1196 0.7276 0.0467 0.101 Uiso 1 1 calc R . .
H22C H 0.2543 0.7365 0.1186 0.101 Uiso 1 1 calc R . .
C23 C 0.6246(4) 0.63217(17) 0.0705(2) 0.0375(9) Uani 1 1 d . . .
H23A H 0.6542 0.6417 0.1317 0.045 Uiso 1 1 calc R . .
C24 C 0.6552(4) 0.68275(19) 0.0222(3) 0.0445(10) Uani 1 1 d . . .
H24A H 0.6088 0.7164 0.0317 0.067 Uiso 1 1 calc R . .
H24B H 0.6282 0.6740 -0.0380 0.067 Uiso 1 1 calc R . .
H24C H 0.7480 0.6902 0.0418 0.067 Uiso 1 1 calc R . .
C25 C 0.6986(4) 0.5799(2) 0.0571(3) 0.0513(11) Uani 1 1 d . . .
H25A H 0.6743 0.5471 0.0848 0.077 Uiso 1 1 calc R . .
H25B H 0.7913 0.5867 0.0811 0.077 Uiso 1 1 calc R . .
H25C H 0.6777 0.5723 -0.0031 0.077 Uiso 1 1 calc R . .
C26 C 0.5310(4) 0.66711(15) 0.3974(2) 0.0312(8) Uani 1 1 d . A .
C27 C 0.4236(4) 0.67777(17) 0.4244(2) 0.0360(9) Uani 1 1 d . . .
C28 C 0.4381(4) 0.66713(18) 0.5081(3) 0.0449(10) Uani 1 1 d . . .
H28A H 0.3679 0.6742 0.5290 0.054 Uiso 1 1 calc R . .
C29 C 0.5531(4) 0.64634(19) 0.5623(3) 0.0459(11) Uani 1 1 d . . .
H29A H 0.5599 0.6382 0.6190 0.055 Uiso 1 1 calc R . .
C30 C 0.6574(4) 0.63754(18) 0.5338(2) 0.0436(10) Uani 1 1 d . A .
H30A H 0.7360 0.6240 0.5716 0.052 Uiso 1 1 calc R . .
C31 C 0.6494(4) 0.64814(16) 0.4510(2) 0.0355(9) Uani 1 1 d . . .
C32 C 0.7675(4) 0.64066(15) 0.4214(3) 0.0459(10) Uani 1 1 d D A 1
H32 H 0.7378 0.6442 0.3588 0.055 Uiso 0.87(4) 1 calc PR B 1
C33 C 0.8310(15) 0.5833(4) 0.4427(9) 0.074(3) Uani 0.87(4) 1 d PD A 1
H33A H 0.8741 0.5810 0.5034 0.111 Uiso 0.87(4) 1 calc PR B 1
H33B H 0.8947 0.5783 0.4130 0.111 Uiso 0.87(4) 1 calc PR B 1
H33C H 0.7656 0.5535 0.4257 0.111 Uiso 0.87(4) 1 calc PR B 1
C34 C 0.8634(10) 0.6879(6) 0.4559(11) 0.082(4) Uani 0.87(4) 1 d PD A 1
H34A H 0.8832 0.6898 0.5170 0.123 Uiso 0.87(4) 1 calc PR B 1
H34B H 0.8264 0.7241 0.4311 0.123 Uiso 0.87(4) 1 calc PR B 1
H34C H 0.9426 0.6805 0.4418 0.123 Uiso 0.87(4) 1 calc PR B 1
H32A H 0.7524 0.6576 0.3644 0.055 Uiso 0.13(4) 1 calc PR B 2
C33A C 0.791(5) 0.5774(5) 0.420(3) 0.035(13) Uiso 0.13(4) 1 d PD A 2
H33D H 0.8132 0.5624 0.4775 0.052 Uiso 0.13(4) 1 calc PR B 2
H33E H 0.8625 0.5703 0.3976 0.052 Uiso 0.13(4) 1 calc PR B 2
H33F H 0.7133 0.5586 0.3848 0.052 Uiso 0.13(4) 1 calc PR B 2
C34A C 0.882(3) 0.668(3) 0.485(3) 0.054(15) Uiso 0.13(4) 1 d PD A 2
H34D H 0.8540 0.7032 0.5060 0.082 Uiso 0.13(4) 1 calc PR B 2
H34E H 0.9478 0.6771 0.4586 0.082 Uiso 0.13(4) 1 calc PR B 2
H34F H 0.9175 0.6420 0.5321 0.082 Uiso 0.13(4) 1 calc PR B 2
C35 C 0.2989(4) 0.70130(18) 0.3660(3) 0.0431(10) Uani 1 1 d . . .
H35A H 0.3026 0.6975 0.3073 0.052 Uiso 1 1 calc R . .
C36 C 0.2882(6) 0.7638(2) 0.3828(4) 0.0773(17) Uani 1 1 d . . .
H36A H 0.3676 0.7831 0.3828 0.116 Uiso 1 1 calc R . .
H36B H 0.2748 0.7688 0.4376 0.116 Uiso 1 1 calc R . .
H36C H 0.2151 0.7801 0.3389 0.116 Uiso 1 1 calc R . .
C37 C 0.1821(5) 0.6687(3) 0.3707(5) 0.088(2) Uani 1 1 d . . .
H37A H 0.1868 0.6296 0.3522 0.132 Uiso 1 1 calc R . .
H37B H 0.1038 0.6868 0.3343 0.132 Uiso 1 1 calc R . .
H37C H 0.1799 0.6687 0.4287 0.132 Uiso 1 1 calc R . .
Cl1 Cl 0.45722(10) 0.37094(4) 0.21530(6) 0.0416(3) Uani 1 1 d . . .
Cl2 Cl 0.84644(18) 0.76292(15) 0.20209(17) 0.0689(8) Uani 0.836(8) 1 d PD C 1
Cl3 Cl 0.9382(3) 0.82391(11) 0.35776(13) 0.0838(11) Uani 0.836(8) 1 d PD C 1
C38 C 0.8366(6) 0.8246(4) 0.2557(3) 0.0537(17) Uani 0.836(8) 1 d PD C 1
H38A H 0.8588 0.8573 0.2257 0.064 Uiso 0.836(8) 1 calc PR C 1
H38B H 0.7469 0.8298 0.2561 0.064 Uiso 0.836(8) 1 calc PR C 1
Cl2A Cl 0.8898(14) 0.8001(8) 0.3748(8) 0.092(4) Uiso 0.164(8) 1 d PD C 2
Cl3A Cl 0.8529(11) 0.7387(6) 0.2249(8) 0.069(4) Uiso 0.164(8) 1 d PD C 2
C38A C 0.843(6) 0.8050(10) 0.2665(9) 0.08(2) Uiso 0.164(8) 1 d PD C 2
H38C H 0.7532 0.8192 0.2452 0.100 Uiso 0.164(8) 1 calc PR C 2
H38D H 0.8994 0.8320 0.2493 0.100 Uiso 0.164(8) 1 calc PR C 2
Cl4 Cl 0.78956(18) 0.43152(7) 0.40755(10) 0.0854(5) Uani 1 1 d D D 1
Cl5 Cl 0.8793(3) 0.36441(11) 0.2934(2) 0.0799(11) Uani 0.890(11) 1 d PD D 1
C39 C 0.7763(5) 0.3687(2) 0.3527(3) 0.0688(15) Uani 1 1 d D D 1
H39A H 0.7941 0.3368 0.3930 0.083 Uiso 0.890(11) 1 calc PR D 1
H39B H 0.6866 0.3647 0.3153 0.083 Uiso 0.890(11) 1 calc PR D 1
Cl5A Cl 0.9199(15) 0.3499(10) 0.338(2) 0.099(8) Uiso 0.110(11) 1 d PD D 2
H39C H 0.7487 0.3382 0.3840 0.083 Uiso 0.110(11) 1 calc PR D 2
H39D H 0.7094 0.3728 0.2975 0.083 Uiso 0.110(11) 1 calc PR D 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
N1 0.0297(16) 0.0289(16) 0.0286(16) -0.0012(13) 0.0086(13) -0.0023(12)
N2 0.0332(17) 0.0286(16) 0.0293(16) -0.0039(13) 0.0110(13) -0.0049(13)
N3 0.0308(16) 0.0270(16) 0.0341(16) 0.0003(13) 0.0140(13) -0.0039(13)
N4 0.0327(18) 0.0252(17) 0.047(2) -0.0052(15) 0.0158(15) -0.0028(14)
C1 0.0257(18) 0.0282(19) 0.0313(19) -0.0037(16) 0.0109(15) 0.0002(14)
C2 0.038(2) 0.029(2) 0.035(2) 0.0026(17) 0.0148(17) -0.0050(16)
C3 0.038(2) 0.0257(19) 0.040(2) 0.0011(17) 0.0116(17) -0.0056(16)
C4 0.0273(19) 0.032(2) 0.0296(19) -0.0003(16) 0.0076(15) -0.0004(15)
C5 0.034(2) 0.036(2) 0.068(3) 0.000(2) 0.027(2) 0.0016(17)
C6 0.032(2) 0.0289(19) 0.039(2) 0.0004(17) 0.0126(17) -0.0054(15)
C7 0.038(2) 0.036(2) 0.041(2) -0.0007(18) 0.0105(18) -0.0070(17)
C8 0.035(2) 0.051(3) 0.058(3) -0.003(2) 0.010(2) -0.0112(19)
C9 0.043(3) 0.058(3) 0.069(3) 0.003(2) 0.027(2) -0.009(2)
C10 0.050(3) 0.050(3) 0.053(3) -0.002(2) 0.029(2) -0.007(2)
C11 0.044(2) 0.029(2) 0.039(2) 0.0029(17) 0.0179(18) -0.0009(17)
C12 0.049(3) 0.048(3) 0.042(2) -0.005(2) 0.009(2) -0.010(2)
C13 0.052(3) 0.045(2) 0.035(2) 0.0001(19) 0.0110(19) -0.003(2)
C14 0.031(2) 0.0283(19) 0.0308(19) -0.0014(16) 0.0077(15) -0.0030(15)
C15 0.031(2) 0.032(2) 0.034(2) 0.0030(17) 0.0090(16) -0.0040(16)
C16 0.033(2) 0.042(2) 0.037(2) 0.0026(18) 0.0049(17) -0.0082(17)
C17 0.048(3) 0.047(2) 0.030(2) -0.0040(19) 0.0070(18) -0.011(2)
C18 0.040(2) 0.042(2) 0.036(2) -0.0022(18) 0.0154(18) -0.0040(18)
C19 0.037(2) 0.033(2) 0.032(2) -0.0017(17) 0.0119(16) -0.0023(16)
C20 0.033(2) 0.051(3) 0.042(2) -0.002(2) 0.0114(18) -0.0002(18)
C21 0.034(2) 0.063(3) 0.058(3) 0.001(2) 0.017(2) -0.002(2)
C22 0.051(3) 0.053(3) 0.104(4) -0.009(3) 0.033(3) -0.002(2)
C23 0.032(2) 0.046(2) 0.035(2) -0.0029(18) 0.0129(17) -0.0016(17)
C24 0.043(2) 0.050(3) 0.042(2) -0.004(2) 0.0157(19) -0.013(2)
C25 0.044(3) 0.053(3) 0.064(3) -0.004(2) 0.028(2) 0.000(2)
C26 0.039(2) 0.0307(19) 0.0271(19) -0.0047(16) 0.0140(16) -0.0048(16)
C27 0.040(2) 0.035(2) 0.036(2) -0.0073(17) 0.0153(17) -0.0056(17)
C28 0.051(3) 0.048(3) 0.044(2) -0.008(2) 0.026(2) -0.010(2)
C29 0.061(3) 0.047(3) 0.030(2) -0.0007(19) 0.016(2) -0.010(2)
C30 0.048(3) 0.045(2) 0.032(2) 0.0008(19) 0.0050(19) 0.0008(19)
C31 0.037(2) 0.034(2) 0.034(2) -0.0042(17) 0.0099(17) -0.0024(17)
C32 0.038(2) 0.056(3) 0.044(2) -0.002(2) 0.0137(19) 0.005(2)
C33 0.065(7) 0.073(5) 0.082(6) 0.004(4) 0.022(5) 0.022(4)
C34 0.061(5) 0.086(7) 0.115(8) -0.025(7) 0.049(5) -0.023(4)
C32A 0.038(2) 0.056(3) 0.044(2) -0.002(2) 0.0137(19) 0.005(2)
C35 0.041(2) 0.044(2) 0.047(2) -0.008(2) 0.0171(19) 0.0001(19)
C36 0.081(4) 0.057(3) 0.083(4) -0.002(3) 0.008(3) 0.017(3)
C37 0.031(3) 0.082(4) 0.139(6) 0.036(4) 0.009(3) -0.001(3)
Cl1 0.0524(6) 0.0316(5) 0.0464(6) -0.0016(4) 0.0237(5) 0.0005(4)
Cl2 0.0623(11) 0.0801(18) 0.0621(12) -0.0166(13) 0.0163(8) -0.0105(10)
Cl3 0.0936(18) 0.0742(15) 0.0568(12) -0.0122(10) -0.0155(10) 0.0112(13)
C38 0.032(3) 0.070(5) 0.055(4) 0.006(3) 0.009(3) 0.011(3)
Cl4 0.1180(13) 0.0656(9) 0.0808(10) -0.0077(8) 0.0425(9) 0.0084(8)
Cl5 0.0880(16) 0.0856(14) 0.083(2) -0.0089(12) 0.0515(15) -0.0071(11)
C39 0.057(3) 0.060(3) 0.096(4) -0.003(3) 0.032(3) 0.000(3)
Cl4A 0.1180(13) 0.0656(9) 0.0808(10) -0.0077(8) 0.0425(9) 0.0084(8)
C39A 0.057(3) 0.060(3) 0.096(4) -0.003(3) 0.032(3) 0.000(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.353(5) . ?
N1 C2 1.397(5) . ?
N1 C14 1.450(5) . ?
N2 C1 1.354(5) . ?
N2 C3 1.403(5) . ?
N2 C26 1.438(5) . ?
N3 C4 1.307(5) . ?
N3 C1 1.343(5) . ?
N4 C4 1.328(5) . ?
N4 C6 1.441(5) . ?
C2 C3 1.345(5) . ?
C4 C5 1.515(5) . ?
C6 C11 1.394(5) . ?
C6 C7 1.394(5) . ?
C7 C8 1.392(6) . ?
C7 C12 1.501(6) . ?
C8 C9 1.381(7) . ?
C9 C10 1.365(7) . ?
C10 C11 1.404(6) . ?
C11 C13 1.501(6) . ?
C14 C19 1.399(5) . ?
C14 C15 1.407(5) . ?
C15 C16 1.392(5) . ?
C15 C20 1.527(6) . ?
C16 C17 1.388(6) . ?
C17 C18 1.372(6) . ?
C18 C19 1.389(5) . ?
C19 C23 1.522(5) . ?
C20 C21 1.515(6) . ?
C20 C22 1.527(7) . ?
C23 C25 1.528(6) . ?
C23 C24 1.536(6) . ?
C26 C31 1.399(5) . ?
C26 C27 1.404(5) . ?
C27 C28 1.386(6) . ?
C27 C35 1.515(6) . ?
C28 C29 1.391(6) . ?
C29 C30 1.380(6) . ?
C30 C31 1.387(6) . ?
C31 C32 1.528(6) . ?
C32 C33 1.511(5) . ?
C32 C34 1.516(5) . ?
C35 C36 1.512(7) . ?
C35 C37 1.512(7) . ?
Cl2 C38 1.730(6) . ?
Cl3 C38 1.727(5) . ?
Cl2A C38A 1.729(7) . ?
Cl3A C38A 1.729(7) . ?
Cl4 C39 1.724(4) . ?
Cl5 C39 1.721(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 109.1(3) . . ?
C1 N1 C14 125.3(3) . . ?
C2 N1 C14 125.1(3) . . ?
C1 N2 C3 109.4(3) . . ?
C1 N2 C26 124.1(3) . . ?
C3 N2 C26 126.4(3) . . ?
C4 N3 C1 124.4(3) . . ?
C4 N4 C6 123.5(3) . . ?
N3 C1 N1 128.7(3) . . ?
N3 C1 N2 123.4(3) . . ?
N1 C1 N2 107.0(3) . . ?
C3 C2 N1 107.7(3) . . ?
C2 C3 N2 106.8(3) . . ?
N3 C4 N4 120.0(3) . . ?
N3 C4 C5 124.6(3) . . ?
N4 C4 C5 115.4(3) . . ?
C11 C6 C7 122.6(4) . . ?
C11 C6 N4 120.1(3) . . ?
C7 C6 N4 117.3(3) . . ?
C8 C7 C6 117.2(4) . . ?
C8 C7 C12 121.7(4) . . ?
C6 C7 C12 121.1(4) . . ?
C9 C8 C7 121.4(4) . . ?
C10 C9 C8 120.4(4) . . ?
C9 C10 C11 120.8(4) . . ?
C6 C11 C10 117.6(4) . . ?
C6 C11 C13 121.5(4) . . ?
C10 C11 C13 121.0(4) . . ?
C19 C14 C15 123.0(3) . . ?
C19 C14 N1 119.0(3) . . ?
C15 C14 N1 117.9(3) . . ?
C16 C15 C14 116.7(3) . . ?
C16 C15 C20 121.4(3) . . ?
C14 C15 C20 121.8(3) . . ?
C17 C16 C15 121.2(4) . . ?
C18 C17 C16 120.6(4) . . ?
C17 C18 C19 121.1(4) . . ?
C18 C19 C14 117.4(4) . . ?
C18 C19 C23 119.3(3) . . ?
C14 C19 C23 123.2(3) . . ?
C21 C20 C15 114.2(4) . . ?
C21 C20 C22 109.7(4) . . ?
C15 C20 C22 110.8(4) . . ?
C19 C23 C25 112.1(3) . . ?
C19 C23 C24 110.1(3) . . ?
C25 C23 C24 109.7(3) . . ?
C31 C26 C27 123.2(3) . . ?
C31 C26 N2 118.9(3) . . ?
C27 C26 N2 117.8(3) . . ?
C28 C27 C26 116.7(4) . . ?
C28 C27 C35 121.2(4) . . ?
C26 C27 C35 122.1(3) . . ?
C27 C28 C29 121.3(4) . . ?
C30 C29 C28 120.2(4) . . ?
C29 C30 C31 121.1(4) . . ?
C30 C31 C26 117.3(4) . . ?
C30 C31 C32 120.4(4) . . ?
C26 C31 C32 122.2(3) . . ?
C33 C32 C34 110.8(6) . . ?
C33 C32 C31 113.5(5) . . ?
C34 C32 C31 110.1(4) . . ?
C36 C35 C37 111.7(4) . . ?
C36 C35 C27 110.0(4) . . ?
C37 C35 C27 112.6(4) . . ?
Cl3 C38 Cl2 112.4(5) . . ?
Cl3A C38A Cl2A 109.0(11) . . ?
Cl5 C39 Cl4 113.4(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
N4 H4N Cl1 0.86(4) 2.24(5) 3.098(4) 175(4) .
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 0.955
_refine_diff_density_min -0.438
_refine_diff_density_rms 0.065
_vrf_ABSTM02_k09161
;
PROBLEM: The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
RESPONSE: Multi-scan absorption correction using redundant data.
;
# end Validation Reply Form
#
data_k09228
_database_code_depnum_ccdc_archive 'CCDC 778194'
#TrackingRef '- CombinedCIF.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C31 H36 Cl4 N4 Ti, C H Cl3'
_chemical_formula_sum 'C32 H37 Cl7 N4 Ti'
_chemical_formula_weight 773.71
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'
Cl Cl 0.1484 0.1585 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
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'
'-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 31.2113(7)
_cell_length_b 9.2685(4)
_cell_length_c 25.6275(8)
_cell_angle_alpha 90.00
_cell_angle_beta 105.3630(18)
_cell_angle_gamma 90.00
_cell_volume 7148.7(4)
_cell_formula_units_Z 8
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 22260
_cell_measurement_theta_min 2.7
_cell_measurement_theta_max 27.5
_exptl_crystal_description plate
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.438
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3184
_exptl_absorpt_coefficient_mu 0.792
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.751
_exptl_absorpt_correction_T_max 0.886
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_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 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 22260
_diffrn_reflns_av_R_equivalents 0.0735
_diffrn_reflns_av_sigmaI/netI 0.1132
_diffrn_reflns_limit_h_min -40
_diffrn_reflns_limit_h_max 38
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_theta_min 2.72
_diffrn_reflns_theta_max 27.48
_reflns_number_total 8106
_reflns_number_gt 4189
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_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^)+(0.0950P)^2^] 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_number_reflns 8106
_refine_ls_number_parameters 406
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1526
_refine_ls_R_factor_gt 0.0631
_refine_ls_wR_factor_ref 0.1909
_refine_ls_wR_factor_gt 0.1441
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_restrained_S_all 1.019
_refine_ls_shift/su_max 0.002
_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
Ti1 Ti 0.62551(2) 0.20294(8) 0.65375(3) 0.0240(2) Uani 1 1 d . . .
Cl1 Cl 0.68448(3) 0.14820(12) 0.61805(4) 0.0315(3) Uani 1 1 d . . .
Cl2 Cl 0.56914(3) 0.26026(12) 0.69216(4) 0.0320(3) Uani 1 1 d . . .
Cl3 Cl 0.67472(4) 0.19266(14) 0.73775(4) 0.0382(3) Uani 1 1 d . . .
Cl4 Cl 0.59577(3) -0.01670(12) 0.63134(5) 0.0322(3) Uani 1 1 d . . .
N1 N 0.67631(11) 0.6549(4) 0.63538(13) 0.0252(8) Uani 1 1 d . . .
N2 N 0.65122(10) 0.6298(4) 0.70636(13) 0.0235(8) Uani 1 1 d . . .
N3 N 0.63210(10) 0.4409(4) 0.63959(13) 0.0226(8) Uani 1 1 d . . .
N4 N 0.59255(10) 0.2930(4) 0.57836(13) 0.0225(8) Uani 1 1 d . . .
C1 C 0.65139(13) 0.5678(5) 0.65880(16) 0.0239(9) Uani 1 1 d . . .
C2 C 0.69116(13) 0.7718(5) 0.66909(18) 0.0290(10) Uani 1 1 d . . .
H2A H 0.7091 0.8485 0.6622 0.035 Uiso 1 1 calc R . .
C3 C 0.67583(13) 0.7579(5) 0.71301(18) 0.0281(10) Uani 1 1 d . . .
H3A H 0.6807 0.8225 0.7428 0.034 Uiso 1 1 calc R . .
C4 C 0.69439(13) 0.6144(5) 0.59064(16) 0.0246(9) Uani 1 1 d . . .
C5 C 0.68017(13) 0.6869(5) 0.54111(17) 0.0276(10) Uani 1 1 d . . .
C6 C 0.69853(14) 0.6394(5) 0.49981(17) 0.0307(11) Uani 1 1 d . . .
H6A H 0.6897 0.6857 0.4655 0.037 Uiso 1 1 calc R . .
C7 C 0.72865(13) 0.5290(5) 0.50691(17) 0.0299(11) Uani 1 1 d . . .
C8 C 0.74403(14) 0.4669(5) 0.55819(18) 0.0319(11) Uani 1 1 d . . .
H8A H 0.7661 0.3937 0.5638 0.038 Uiso 1 1 calc R . .
C9 C 0.72770(13) 0.5101(5) 0.60110(17) 0.0279(10) Uani 1 1 d . . .
C10 C 0.64859(14) 0.8145(5) 0.53123(18) 0.0330(11) Uani 1 1 d . . .
H10A H 0.6356 0.8251 0.5619 0.050 Uiso 1 1 calc R . .
H10B H 0.6249 0.7982 0.4980 0.050 Uiso 1 1 calc R . .
H10C H 0.6649 0.9024 0.5274 0.050 Uiso 1 1 calc R . .
C11 C 0.74548(15) 0.4752(6) 0.46048(19) 0.0411(13) Uani 1 1 d . . .
H11A H 0.7713 0.4128 0.4744 0.062 Uiso 1 1 calc R . .
H11B H 0.7541 0.5575 0.4415 0.062 Uiso 1 1 calc R . .
H11C H 0.7220 0.4203 0.4354 0.062 Uiso 1 1 calc R . .
C12 C 0.74721(13) 0.4516(5) 0.65690(17) 0.0317(11) Uani 1 1 d . . .
H12A H 0.7571 0.5317 0.6822 0.048 Uiso 1 1 calc R . .
H12B H 0.7726 0.3897 0.6568 0.048 Uiso 1 1 calc R . .
H12C H 0.7247 0.3951 0.6682 0.048 Uiso 1 1 calc R . .
C13 C 0.63011(13) 0.5790(5) 0.74691(16) 0.0250(10) Uani 1 1 d . . .
C14 C 0.65744(13) 0.5265(5) 0.79532(17) 0.0286(10) Uani 1 1 d . . .
C15 C 0.63802(15) 0.4883(5) 0.83573(18) 0.0322(11) Uani 1 1 d . . .
H15A H 0.6564 0.4528 0.8689 0.039 Uiso 1 1 calc R . .
C16 C 0.59256(14) 0.4998(5) 0.82969(17) 0.0300(11) Uani 1 1 d . . .
C17 C 0.56685(14) 0.5515(5) 0.78067(18) 0.0304(10) Uani 1 1 d . . .
H17A H 0.5357 0.5595 0.7758 0.037 Uiso 1 1 calc R . .
C18 C 0.58430(13) 0.5924(5) 0.73816(17) 0.0270(10) Uani 1 1 d . . .
C19 C 0.70767(14) 0.5126(5) 0.80459(19) 0.0399(12) Uani 1 1 d . . .
H19A H 0.7142 0.4757 0.7717 0.060 Uiso 1 1 calc R . .
H19B H 0.7195 0.4458 0.8346 0.060 Uiso 1 1 calc R . .
H19C H 0.7216 0.6075 0.8135 0.060 Uiso 1 1 calc R . .
C20 C 0.57175(16) 0.4608(6) 0.87464(18) 0.0414(12) Uani 1 1 d . . .
H20A H 0.5433 0.4125 0.8594 0.062 Uiso 1 1 calc R . .
H20B H 0.5669 0.5487 0.8935 0.062 Uiso 1 1 calc R . .
H20C H 0.5916 0.3959 0.9002 0.062 Uiso 1 1 calc R . .
C21 C 0.55477(14) 0.6484(5) 0.68578(18) 0.0357(12) Uani 1 1 d . . .
H21A H 0.5270 0.6846 0.6919 0.054 Uiso 1 1 calc R . .
H21B H 0.5481 0.5702 0.6591 0.054 Uiso 1 1 calc R . .
H21C H 0.5699 0.7268 0.6722 0.054 Uiso 1 1 calc R . .
C22 C 0.60379(13) 0.4282(5) 0.58929(16) 0.0242(9) Uani 1 1 d . . .
C23 C 0.58347(13) 0.5492(5) 0.55300(17) 0.0299(10) Uani 1 1 d . . .
H23A H 0.5986 0.5596 0.5242 0.045 Uiso 1 1 calc R . .
H23B H 0.5865 0.6389 0.5739 0.045 Uiso 1 1 calc R . .
H23C H 0.5519 0.5290 0.5369 0.045 Uiso 1 1 calc R . .
C24 C 0.56715(13) 0.2470(4) 0.52589(16) 0.0221(9) Uani 1 1 d . . .
C25 C 0.58702(13) 0.2318(5) 0.48379(17) 0.0277(10) Uani 1 1 d . . .
C26 C 0.56174(14) 0.1806(5) 0.43395(17) 0.0308(11) Uani 1 1 d . . .
H26A H 0.5750 0.1709 0.4048 0.037 Uiso 1 1 calc R . .
C27 C 0.51790(14) 0.1439(5) 0.42660(19) 0.0340(11) Uani 1 1 d . . .
H27A H 0.5014 0.1057 0.3929 0.041 Uiso 1 1 calc R . .
C28 C 0.49787(14) 0.1623(5) 0.46781(18) 0.0288(10) Uani 1 1 d . . .
H28A H 0.4673 0.1395 0.4618 0.035 Uiso 1 1 calc R . .
C29 C 0.52167(13) 0.2139(4) 0.51844(16) 0.0240(9) Uani 1 1 d . . .
C30 C 0.63509(14) 0.2747(6) 0.48931(18) 0.0382(12) Uani 1 1 d . . .
H30A H 0.6508 0.2837 0.5277 0.057 Uiso 1 1 calc R . .
H30B H 0.6359 0.3673 0.4712 0.057 Uiso 1 1 calc R . .
H30C H 0.6496 0.2006 0.4726 0.057 Uiso 1 1 calc R . .
C31 C 0.49936(13) 0.2375(5) 0.56305(18) 0.0341(11) Uani 1 1 d . . .
H31A H 0.4678 0.2127 0.5500 0.051 Uiso 1 1 calc R . .
H31B H 0.5023 0.3390 0.5742 0.051 Uiso 1 1 calc R . .
H31C H 0.5134 0.1762 0.5940 0.051 Uiso 1 1 calc R . .
Cl5 Cl 0.54540(5) 0.10833(16) 0.81911(6) 0.0567(4) Uani 1 1 d . . .
Cl6 Cl 0.60566(6) -0.09763(16) 0.79458(6) 0.0653(4) Uani 1 1 d . . .
Cl7 Cl 0.63762(5) 0.10418(16) 0.88106(6) 0.0639(4) Uani 1 1 d . . .
C32 C 0.60032(16) 0.0783(5) 0.81671(19) 0.0402(12) Uani 1 1 d . . .
H32B H 0.6078 0.1479 0.7906 0.048 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
Ti1 0.0261(4) 0.0222(4) 0.0240(4) 0.0008(3) 0.0073(3) 0.0005(3)
Cl1 0.0296(6) 0.0317(7) 0.0359(6) -0.0008(5) 0.0134(5) 0.0023(5)
Cl2 0.0345(6) 0.0345(7) 0.0306(6) -0.0004(5) 0.0149(5) -0.0003(5)
Cl3 0.0378(6) 0.0454(8) 0.0276(6) 0.0008(5) 0.0019(5) 0.0020(6)
Cl4 0.0342(6) 0.0227(6) 0.0393(7) -0.0022(5) 0.0093(5) -0.0030(5)
N1 0.0297(19) 0.023(2) 0.0220(19) -0.0035(16) 0.0061(15) -0.0034(16)
N2 0.0229(17) 0.023(2) 0.025(2) -0.0024(16) 0.0076(15) -0.0011(16)
N3 0.0220(17) 0.023(2) 0.0223(19) -0.0009(16) 0.0044(14) -0.0026(15)
N4 0.0267(19) 0.021(2) 0.0208(18) -0.0014(15) 0.0087(15) -0.0038(16)
C1 0.026(2) 0.023(2) 0.024(2) -0.0013(19) 0.0101(18) -0.0003(19)
C2 0.027(2) 0.027(3) 0.033(3) -0.002(2) 0.0083(19) -0.007(2)
C3 0.028(2) 0.024(2) 0.032(2) -0.009(2) 0.0080(19) -0.007(2)
C4 0.027(2) 0.024(2) 0.026(2) 0.0006(19) 0.0121(18) 0.000(2)
C5 0.029(2) 0.029(3) 0.026(2) 0.003(2) 0.0080(19) -0.004(2)
C6 0.035(2) 0.037(3) 0.021(2) -0.002(2) 0.0085(19) -0.006(2)
C7 0.028(2) 0.034(3) 0.030(3) -0.007(2) 0.0123(19) -0.007(2)
C8 0.026(2) 0.036(3) 0.036(3) -0.003(2) 0.012(2) 0.004(2)
C9 0.025(2) 0.029(3) 0.031(3) 0.001(2) 0.0094(19) -0.0056(19)
C10 0.039(3) 0.027(3) 0.035(3) 0.004(2) 0.013(2) 0.004(2)
C11 0.035(3) 0.057(4) 0.035(3) -0.005(3) 0.016(2) 0.007(2)
C12 0.026(2) 0.040(3) 0.030(2) 0.001(2) 0.0085(19) 0.003(2)
C13 0.031(2) 0.026(2) 0.022(2) -0.0034(19) 0.0137(18) -0.005(2)
C14 0.030(2) 0.030(3) 0.027(2) -0.005(2) 0.0100(19) -0.002(2)
C15 0.038(3) 0.033(3) 0.023(2) -0.003(2) 0.0044(19) -0.002(2)
C16 0.039(3) 0.027(3) 0.030(3) -0.002(2) 0.021(2) 0.000(2)
C17 0.028(2) 0.029(3) 0.039(3) 0.000(2) 0.017(2) 0.001(2)
C18 0.030(2) 0.023(2) 0.029(2) -0.002(2) 0.0112(19) -0.004(2)
C19 0.039(3) 0.044(3) 0.037(3) -0.002(2) 0.009(2) -0.003(2)
C20 0.056(3) 0.040(3) 0.035(3) -0.001(2) 0.025(2) -0.001(3)
C21 0.029(2) 0.042(3) 0.038(3) 0.009(2) 0.012(2) 0.002(2)
C22 0.023(2) 0.029(3) 0.024(2) -0.002(2) 0.0122(17) 0.0003(19)
C23 0.033(2) 0.020(2) 0.035(3) 0.001(2) 0.007(2) 0.002(2)
C24 0.027(2) 0.017(2) 0.020(2) 0.0014(18) 0.0023(17) -0.0011(18)
C25 0.026(2) 0.028(3) 0.029(2) 0.000(2) 0.0088(19) -0.001(2)
C26 0.038(3) 0.035(3) 0.018(2) -0.001(2) 0.0065(19) 0.005(2)
C27 0.039(3) 0.025(3) 0.032(3) -0.004(2) 0.000(2) 0.002(2)
C28 0.026(2) 0.021(2) 0.036(3) -0.003(2) 0.0032(19) -0.0020(19)
C29 0.027(2) 0.019(2) 0.025(2) 0.0013(19) 0.0054(18) 0.0002(19)
C30 0.035(3) 0.054(3) 0.028(3) 0.000(2) 0.012(2) -0.002(2)
C31 0.025(2) 0.042(3) 0.036(3) -0.004(2) 0.010(2) -0.008(2)
Cl5 0.0615(8) 0.0566(9) 0.0598(9) 0.0028(7) 0.0296(7) 0.0029(7)
Cl6 0.0968(11) 0.0412(9) 0.0699(10) -0.0189(7) 0.0433(9) -0.0043(8)
Cl7 0.0829(10) 0.0511(10) 0.0467(9) 0.0001(7) -0.0023(7) -0.0019(8)
C32 0.058(3) 0.031(3) 0.036(3) -0.005(2) 0.020(2) -0.002(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N4 2.106(3) . ?
Ti1 Cl4 2.2480(13) . ?
Ti1 N3 2.253(3) . ?
Ti1 Cl3 2.2913(13) . ?
Ti1 Cl2 2.2944(12) . ?
Ti1 Cl1 2.3182(12) . ?
Ti1 C22 2.637(4) . ?
N1 C1 1.365(5) . ?
N1 C2 1.386(5) . ?
N1 C4 1.455(5) . ?
N2 C1 1.349(5) . ?
N2 C3 1.400(5) . ?
N2 C13 1.449(5) . ?
N3 C1 1.354(5) . ?
N3 C22 1.361(5) . ?
N4 C22 1.312(5) . ?
N4 C24 1.433(5) . ?
C2 C3 1.341(6) . ?
C4 C9 1.393(6) . ?
C4 C5 1.400(6) . ?
C5 C6 1.401(6) . ?
C5 C10 1.517(6) . ?
C6 C7 1.369(6) . ?
C7 C8 1.398(6) . ?
C7 C11 1.507(6) . ?
C8 C9 1.388(6) . ?
C9 C12 1.500(6) . ?
C13 C18 1.393(5) . ?
C13 C14 1.394(6) . ?
C14 C15 1.378(6) . ?
C14 C19 1.528(6) . ?
C15 C16 1.390(6) . ?
C16 C17 1.385(6) . ?
C16 C20 1.509(6) . ?
C17 C18 1.394(6) . ?
C18 C21 1.505(6) . ?
C22 C23 1.487(6) . ?
C24 C25 1.387(6) . ?
C24 C29 1.415(5) . ?
C25 C26 1.395(6) . ?
C25 C30 1.522(6) . ?
C26 C27 1.374(6) . ?
C27 C28 1.373(6) . ?
C28 C29 1.398(6) . ?
C29 C31 1.504(6) . ?
Cl5 C32 1.754(5) . ?
Cl6 C32 1.749(5) . ?
Cl7 C32 1.765(5) . ?
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
N4 Ti1 Cl4 93.22(10) . . ?
N4 Ti1 N3 60.50(12) . . ?
Cl4 Ti1 N3 153.42(9) . . ?
N4 Ti1 Cl3 157.13(10) . . ?
Cl4 Ti1 Cl3 109.33(5) . . ?
N3 Ti1 Cl3 97.18(9) . . ?
N4 Ti1 Cl2 93.33(9) . . ?
Cl4 Ti1 Cl2 90.43(5) . . ?
N3 Ti1 Cl2 87.45(9) . . ?
Cl3 Ti1 Cl2 90.33(5) . . ?
N4 Ti1 Cl1 88.31(9) . . ?
Cl4 Ti1 Cl1 91.05(5) . . ?
N3 Ti1 Cl1 91.99(9) . . ?
Cl3 Ti1 Cl1 87.54(5) . . ?
Cl2 Ti1 Cl1 177.72(5) . . ?
N4 Ti1 C22 29.49(12) . . ?
Cl4 Ti1 C22 122.46(10) . . ?
N3 Ti1 C22 31.07(12) . . ?
Cl3 Ti1 C22 128.21(10) . . ?
Cl2 Ti1 C22 89.21(9) . . ?
Cl1 Ti1 C22 91.45(9) . . ?
C1 N1 C2 108.9(3) . . ?
C1 N1 C4 125.4(3) . . ?
C2 N1 C4 123.8(3) . . ?
C1 N2 C3 109.8(3) . . ?
C1 N2 C13 128.4(3) . . ?
C3 N2 C13 121.9(3) . . ?
C1 N3 C22 122.3(4) . . ?
C1 N3 Ti1 147.5(3) . . ?
C22 N3 Ti1 90.3(3) . . ?
C22 N4 C24 122.3(3) . . ?
C22 N4 Ti1 98.3(2) . . ?
C24 N4 Ti1 139.3(3) . . ?
N2 C1 N3 126.2(4) . . ?
N2 C1 N1 106.5(3) . . ?
N3 C1 N1 127.2(4) . . ?
C3 C2 N1 108.3(4) . . ?
C2 C3 N2 106.6(4) . . ?
C9 C4 C5 123.3(4) . . ?
C9 C4 N1 116.9(4) . . ?
C5 C4 N1 119.7(4) . . ?
C4 C5 C6 116.0(4) . . ?
C4 C5 C10 124.1(4) . . ?
C6 C5 C10 119.8(4) . . ?
C7 C6 C5 122.6(4) . . ?
C6 C7 C8 119.0(4) . . ?
C6 C7 C11 120.9(4) . . ?
C8 C7 C11 120.1(4) . . ?
C9 C8 C7 121.3(4) . . ?
C8 C9 C4 117.4(4) . . ?
C8 C9 C12 120.6(4) . . ?
C4 C9 C12 121.9(4) . . ?
C18 C13 C14 122.3(4) . . ?
C18 C13 N2 119.9(4) . . ?
C14 C13 N2 117.7(3) . . ?
C15 C14 C13 118.1(4) . . ?
C15 C14 C19 120.0(4) . . ?
C13 C14 C19 121.9(4) . . ?
C14 C15 C16 122.4(4) . . ?
C17 C16 C15 117.2(4) . . ?
C17 C16 C20 120.8(4) . . ?
C15 C16 C20 122.0(4) . . ?
C16 C17 C18 123.4(4) . . ?
C13 C18 C17 116.5(4) . . ?
C13 C18 C21 122.3(4) . . ?
C17 C18 C21 121.1(4) . . ?
N4 C22 N3 110.7(4) . . ?
N4 C22 C23 122.8(4) . . ?
N3 C22 C23 126.1(4) . . ?
N4 C22 Ti1 52.2(2) . . ?
N3 C22 Ti1 58.7(2) . . ?
C23 C22 Ti1 170.0(3) . . ?
C25 C24 C29 120.8(4) . . ?
C25 C24 N4 120.7(4) . . ?
C29 C24 N4 118.5(3) . . ?
C24 C25 C26 119.1(4) . . ?
C24 C25 C30 122.3(4) . . ?
C26 C25 C30 118.6(4) . . ?
C27 C26 C25 120.7(4) . . ?
C28 C27 C26 120.3(4) . . ?
C27 C28 C29 121.2(4) . . ?
C28 C29 C24 117.8(4) . . ?
C28 C29 C31 121.1(4) . . ?
C24 C29 C31 121.1(4) . . ?
Cl6 C32 Cl5 109.7(3) . . ?
Cl6 C32 Cl7 109.5(3) . . ?
Cl5 C32 Cl7 110.8(3) . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 0.787
_refine_diff_density_min -0.660
_refine_diff_density_rms 0.116
#
data_k09220
_database_code_depnum_ccdc_archive 'CCDC 778195'
#TrackingRef '- CombinedCIF.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C74 H96 Cl4 N8 Pd2, 2(C H2 Cl2)'
_chemical_formula_sum 'C76 H100 Cl8 N8 Pd2'
_chemical_formula_weight 1622.04
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'
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 Monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.0092(3)
_cell_length_b 21.2077(6)
_cell_length_c 14.3841(4)
_cell_angle_alpha 90.00
_cell_angle_beta 94.8230(16)
_cell_angle_gamma 90.00
_cell_volume 4258.43(19)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 28275
_cell_measurement_theta_min 2.7
_cell_measurement_theta_max 27.5
_exptl_crystal_description needle
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.265
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1680
_exptl_absorpt_coefficient_mu 0.716
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.662
_exptl_absorpt_correction_T_max 0.921
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_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 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 28275
_diffrn_reflns_av_R_equivalents 0.0629
_diffrn_reflns_av_sigmaI/netI 0.0636
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.74
_diffrn_reflns_theta_max 27.49
_reflns_number_total 9700
_reflns_number_gt 6444
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_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^)+(0.1582P)^2^+9.0389P] 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_number_reflns 9700
_refine_ls_number_parameters 469
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.1276
_refine_ls_R_factor_gt 0.0863
_refine_ls_wR_factor_ref 0.2769
_refine_ls_wR_factor_gt 0.2379
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_restrained_S_all 1.033
_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 0.59912(3) 0.01851(2) 0.07324(3) 0.0392(2) Uani 0.8304(16) 1 d P . 1
Cl1 Cl 0.48735(12) -0.06315(8) 0.05680(13) 0.0528(4) Uani 0.8304(16) 1 d P . 1
Cl2 Cl 0.67081(14) -0.03185(8) 0.20173(13) 0.0532(4) Uani 0.8304(16) 1 d P . 1
N1 N 0.8051(3) 0.2722(2) 0.2175(3) 0.0443(10) Uani 1 1 d . . .
N2 N 0.8659(4) 0.1918(2) 0.2967(4) 0.0554(13) Uani 1 1 d . . .
N3 N 0.7809(3) 0.1725(2) 0.1452(3) 0.0443(11) Uani 1 1 d . . .
N4 N 0.6943(3) 0.0901(2) 0.0764(4) 0.0513(12) Uani 1 1 d . . .
C1 C 0.8107(4) 0.2082(2) 0.2163(4) 0.0420(12) Uani 1 1 d . . .
C2 C 0.8579(4) 0.2959(3) 0.2965(4) 0.0506(14) Uani 1 1 d . . .
H2A H 0.8659 0.3391 0.3128 0.061 Uiso 1 1 calc R . .
C3 C 0.8948(5) 0.2470(3) 0.3445(5) 0.0579(16) Uani 1 1 d . . .
H3B H 0.9340 0.2491 0.4016 0.069 Uiso 1 1 calc R . .
C4 C 0.9084(5) 0.1303(3) 0.3148(5) 0.0636(18) Uani 1 1 d . . .
C5 C 0.8685(7) 0.0892(3) 0.3797(5) 0.076(2) Uani 1 1 d . . .
C6 C 0.9136(8) 0.0313(4) 0.3946(7) 0.090(3) Uani 1 1 d . . .
H6A H 0.8923 0.0025 0.4389 0.107 Uiso 1 1 calc R . .
C7 C 0.9906(9) 0.0161(4) 0.3437(7) 0.094(3) Uani 1 1 d . . .
H7A H 1.0174 -0.0249 0.3518 0.113 Uiso 1 1 calc R . .
C8 C 1.0304(7) 0.0557(4) 0.2828(6) 0.087(3) Uani 1 1 d . . .
H8 H 1.0853 0.0437 0.2526 0.105 Uiso 1 1 calc R . .
C9 C 0.9863(7) 0.1156(3) 0.2664(5) 0.074(2) Uani 1 1 d . . .
C10 C 1.0326(6) 0.1606(4) 0.2029(6) 0.081(2) Uani 1 1 d . . .
H10A H 0.9937 0.2002 0.2012 0.097 Uiso 1 1 calc R . .
C11 C 1.1364(8) 0.1794(6) 0.2369(8) 0.114(4) Uani 1 1 d . . .
H11A H 1.1370 0.1993 0.2985 0.171 Uiso 1 1 calc R . .
H11B H 1.1611 0.2092 0.1927 0.171 Uiso 1 1 calc R . .
H11C H 1.1769 0.1417 0.2412 0.171 Uiso 1 1 calc R . .
C12 C 1.0315(8) 0.1369(5) 0.1009(6) 0.103(3) Uani 1 1 d . . .
H12A H 0.9655 0.1275 0.0769 0.155 Uiso 1 1 calc R . .
H12B H 1.0705 0.0986 0.0990 0.155 Uiso 1 1 calc R . .
H12C H 1.0578 0.1696 0.0622 0.155 Uiso 1 1 calc R . .
C13 C 0.7876(6) 0.1075(4) 0.4366(6) 0.079(2) Uani 1 1 d . . .
H13A H 0.7511 0.1422 0.4027 0.095 Uiso 1 1 calc R . .
C14 C 0.8250(7) 0.1328(5) 0.5328(6) 0.091(3) Uani 1 1 d . . .
H14A H 0.8657 0.1697 0.5250 0.136 Uiso 1 1 calc R . .
H14B H 0.8624 0.1000 0.5672 0.136 Uiso 1 1 calc R . .
H14C H 0.7707 0.1450 0.5677 0.136 Uiso 1 1 calc R . .
C15 C 0.7168(8) 0.0528(5) 0.4490(8) 0.111(4) Uani 1 1 d . . .
H15A H 0.7022 0.0315 0.3891 0.166 Uiso 1 1 calc R . .
H15B H 0.6577 0.0696 0.4712 0.166 Uiso 1 1 calc R . .
H15C H 0.7458 0.0226 0.4947 0.166 Uiso 1 1 calc R . .
C16 C 0.7530(5) 0.3082(3) 0.1453(4) 0.0502(14) Uani 1 1 d . . .
C17 C 0.6588(5) 0.3228(3) 0.1551(4) 0.0572(16) Uani 1 1 d . . .
C18 C 0.6088(6) 0.3555(3) 0.0827(5) 0.069(2) Uani 1 1 d . . .
H18A H 0.5428 0.3647 0.0864 0.083 Uiso 1 1 calc R . .
C19 C 0.6528(7) 0.3749(3) 0.0058(5) 0.079(2) Uani 1 1 d . . .
H19A H 0.6180 0.3983 -0.0422 0.094 Uiso 1 1 calc R . .
C20 C 0.7475(8) 0.3603(3) -0.0013(5) 0.085(3) Uani 1 1 d . . .
H20A H 0.7774 0.3734 -0.0550 0.102 Uiso 1 1 calc R . .
C21 C 0.8011(6) 0.3265(3) 0.0687(5) 0.0649(18) Uani 1 1 d . . .
C22 C 0.6083(5) 0.3062(3) 0.2430(4) 0.0576(16) Uani 1 1 d . . .
H22A H 0.6485 0.2737 0.2783 0.069 Uiso 1 1 calc R . .
C23 C 0.6038(6) 0.3629(4) 0.3055(5) 0.073(2) Uani 1 1 d . . .
H23A H 0.6687 0.3792 0.3211 0.110 Uiso 1 1 calc R . .
H23B H 0.5755 0.3508 0.3629 0.110 Uiso 1 1 calc R . .
H23C H 0.5644 0.3957 0.2732 0.110 Uiso 1 1 calc R . .
C24 C 0.5080(6) 0.2771(4) 0.2203(7) 0.087(2) Uani 1 1 d . . .
H24A H 0.4862 0.2577 0.2765 0.130 Uiso 1 1 calc R . .
H24B H 0.5112 0.2450 0.1716 0.130 Uiso 1 1 calc R . .
H24C H 0.4629 0.3103 0.1981 0.130 Uiso 1 1 calc R . .
C25 C 0.9041(7) 0.3108(4) 0.0603(7) 0.088(3) Uani 1 1 d . . .
H25A H 0.9233 0.2777 0.1079 0.105 Uiso 1 1 calc R . .
C26 C 0.9661(10) 0.3708(7) 0.0845(12) 0.167(6) Uani 1 1 d . . .
H26A H 0.9240 0.4074 0.0896 0.250 Uiso 1 1 calc R . .
H26B H 1.0089 0.3784 0.0351 0.250 Uiso 1 1 calc R . .
H26C H 1.0044 0.3644 0.1440 0.250 Uiso 1 1 calc R . .
C27 C 0.9259(10) 0.2862(6) -0.0332(9) 0.125(4) Uani 1 1 d . . .
H27A H 0.8836 0.2505 -0.0506 0.188 Uiso 1 1 calc R . .
H27B H 0.9928 0.2722 -0.0303 0.188 Uiso 1 1 calc R . .
H27C H 0.9156 0.3197 -0.0799 0.188 Uiso 1 1 calc R . .
C28 C 0.7116(4) 0.1303(3) 0.1470(4) 0.0477(13) Uani 1 1 d . . .
C29 C 0.6461(5) 0.1270(3) 0.2241(5) 0.0607(17) Uani 1 1 d . . .
H29A H 0.6529 0.1654 0.2619 0.091 Uiso 1 1 calc R . .
H29B H 0.6628 0.0902 0.2635 0.091 Uiso 1 1 calc R . .
H29C H 0.5797 0.1231 0.1973 0.091 Uiso 1 1 calc R . .
C30 C 0.7465(4) 0.0971(2) -0.0049(4) 0.0434(12) Uani 1 1 d . . .
C31 C 0.8205(4) 0.0542(3) -0.0180(4) 0.0491(13) Uani 1 1 d . . .
C32 C 0.8669(5) 0.0582(4) -0.1001(5) 0.0654(19) Uani 1 1 d . . .
H32A H 0.9168 0.0295 -0.1111 0.079 Uiso 1 1 calc R . .
C33 C 0.8394(6) 0.1043(4) -0.1658(5) 0.074(2) Uani 1 1 d . . .
H33A H 0.8696 0.1070 -0.2224 0.088 Uiso 1 1 calc R . .
C34 C 0.7681(6) 0.1459(4) -0.1479(5) 0.072(2) Uani 1 1 d . . .
H34A H 0.7504 0.1775 -0.1929 0.087 Uiso 1 1 calc R . .
C35 C 0.7215(4) 0.1439(3) -0.0681(5) 0.0565(15) Uani 1 1 d . . .
C36 C 0.6468(5) 0.1936(3) -0.0475(6) 0.0680(19) Uani 1 1 d . . .
H36A H 0.6158 0.2097 -0.1064 0.102 Uiso 1 1 calc R . .
H36B H 0.6783 0.2284 -0.0123 0.102 Uiso 1 1 calc R . .
H36C H 0.5986 0.1745 -0.0108 0.102 Uiso 1 1 calc R . .
C37 C 0.8503(5) 0.0041(4) 0.0542(6) 0.0711(19) Uani 1 1 d . . .
H37A H 0.8510 0.0223 0.1169 0.107 Uiso 1 1 calc R . .
H37B H 0.9145 -0.0113 0.0440 0.107 Uiso 1 1 calc R . .
H37C H 0.8047 -0.0310 0.0484 0.107 Uiso 1 1 calc R . .
Pd1A Pd 0.45669(17) -0.07424(12) -0.02010(17) 0.0412(9) Uiso 0.1696(16) 1 d P .
2
Cl1A Cl 0.6053(7) -0.0277(5) 0.0157(7) 0.060(2) Uiso 0.1696(16) 1 d P . 2
Cl2A Cl 0.5342(7) -0.1694(5) -0.0257(7) 0.063(2) Uiso 0.1696(16) 1 d P . 2
Cl3 Cl 0.6243(8) -0.1935(6) -0.0759(8) 0.207(3) Uani 0.50 1 d PD . .
Cl4 Cl 0.7955(8) -0.2307(6) 0.0152(8) 0.207(3) Uani 0.50 1 d PD . .
C1S C 0.7264(9) -0.1682(9) -0.0183(12) 0.110(7) Uani 0.50 1 d PDU . .
H1S1 H 0.7116 -0.1436 0.0372 0.132 Uiso 0.50 1 calc PR . .
H1S2 H 0.7612 -0.1404 -0.0592 0.132 Uiso 0.50 1 calc PR . .
Cl5 Cl 0.6354(4) -0.0711(4) -0.1723(7) 0.149(3) Uani 0.50 1 d PD . .
Cl6 Cl 0.6796(7) -0.0039(4) -0.3303(5) 0.162(3) Uani 0.50 1 d PD . .
C2S C 0.6250(15) -0.0021(7) -0.2304(8) 0.100(6) Uani 0.50 1 d PD . .
H2S1 H 0.5562 0.0077 -0.2449 0.120 Uiso 0.50 1 calc PR . .
H2S2 H 0.6534 0.0320 -0.1899 0.120 Uiso 0.50 1 calc PR . .
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 0.0386(3) 0.0281(3) 0.0505(3) -0.0029(2) 0.0025(2) -0.00565(19)
Cl1 0.0482(9) 0.0410(9) 0.0673(11) 0.0109(8) -0.0060(8) -0.0148(7)
Cl2 0.0646(11) 0.0328(8) 0.0602(10) 0.0020(7) -0.0070(8) -0.0065(7)
N1 0.056(3) 0.029(2) 0.047(2) -0.0048(19) -0.001(2) 0.000(2)
N2 0.068(3) 0.031(2) 0.064(3) -0.005(2) -0.020(3) 0.002(2)
N3 0.051(3) 0.032(2) 0.048(2) -0.0020(19) -0.008(2) -0.012(2)
N4 0.046(3) 0.048(3) 0.061(3) -0.021(2) 0.012(2) -0.014(2)
C1 0.047(3) 0.031(3) 0.047(3) 0.001(2) -0.003(2) -0.005(2)
C2 0.055(3) 0.035(3) 0.060(3) -0.009(3) -0.005(3) -0.003(3)
C3 0.067(4) 0.040(3) 0.062(4) -0.013(3) -0.022(3) 0.002(3)
C4 0.081(5) 0.041(3) 0.064(4) -0.016(3) -0.021(4) 0.008(3)
C5 0.113(6) 0.038(3) 0.069(4) 0.008(3) -0.037(4) -0.008(4)
C6 0.118(7) 0.050(4) 0.092(6) 0.002(4) -0.039(6) 0.001(5)
C7 0.150(10) 0.047(4) 0.077(5) -0.006(4) -0.044(6) 0.021(5)
C8 0.111(7) 0.068(5) 0.074(5) -0.031(4) -0.040(5) 0.028(5)
C9 0.108(6) 0.050(4) 0.058(4) -0.008(3) -0.024(4) 0.010(4)
C10 0.076(5) 0.083(6) 0.081(5) -0.032(5) -0.006(4) 0.024(4)
C11 0.109(7) 0.123(9) 0.104(7) -0.039(7) -0.031(6) 0.019(7)
C12 0.104(7) 0.125(8) 0.079(6) -0.040(6) -0.008(5) -0.007(6)
C13 0.088(5) 0.055(4) 0.090(5) 0.016(4) -0.012(5) 0.000(4)
C14 0.099(6) 0.100(7) 0.070(5) 0.011(5) -0.017(4) -0.006(5)
C15 0.113(8) 0.086(7) 0.129(8) 0.036(6) -0.018(7) -0.029(6)
C16 0.073(4) 0.030(3) 0.047(3) -0.005(2) -0.001(3) 0.003(3)
C17 0.081(4) 0.036(3) 0.052(3) -0.002(3) -0.010(3) 0.012(3)
C18 0.089(5) 0.051(4) 0.065(4) -0.002(3) -0.008(4) 0.025(4)
C19 0.129(7) 0.049(4) 0.055(4) 0.004(3) -0.008(4) 0.028(4)
C20 0.160(9) 0.045(4) 0.051(4) 0.007(3) 0.016(5) 0.010(5)
C21 0.095(5) 0.041(3) 0.059(4) 0.004(3) 0.008(4) -0.002(3)
C22 0.065(4) 0.052(4) 0.055(3) 0.001(3) 0.001(3) 0.015(3)
C23 0.086(5) 0.064(4) 0.071(4) -0.014(4) 0.015(4) 0.016(4)
C24 0.090(6) 0.071(5) 0.098(6) 0.007(5) -0.002(5) 0.003(5)
C25 0.095(6) 0.077(5) 0.097(6) 0.018(5) 0.039(5) 0.000(5)
C26 0.119(10) 0.164(13) 0.225(17) -0.068(13) 0.057(10) -0.050(10)
C27 0.153(10) 0.105(8) 0.125(9) -0.016(7) 0.051(8) 0.011(8)
C28 0.042(3) 0.037(3) 0.064(3) -0.012(3) 0.003(3) 0.000(2)
C29 0.056(4) 0.059(4) 0.068(4) -0.022(3) 0.014(3) -0.010(3)
C30 0.046(3) 0.031(3) 0.054(3) -0.012(2) 0.007(2) -0.011(2)
C31 0.048(3) 0.042(3) 0.056(3) -0.014(3) 0.000(3) -0.009(3)
C32 0.054(3) 0.068(4) 0.077(4) -0.032(4) 0.017(3) -0.013(3)
C33 0.084(5) 0.084(5) 0.056(4) -0.008(4) 0.021(4) -0.029(4)
C34 0.076(5) 0.067(5) 0.072(5) 0.014(4) -0.004(4) -0.015(4)
C35 0.052(3) 0.040(3) 0.077(4) 0.003(3) 0.003(3) -0.017(3)
C36 0.062(4) 0.051(4) 0.089(5) 0.009(4) -0.004(4) -0.005(3)
C37 0.057(4) 0.069(5) 0.086(5) 0.002(4) -0.001(4) 0.005(4)
Cl3 0.187(6) 0.225(8) 0.213(7) -0.042(6) 0.040(5) -0.050(6)
Cl4 0.187(6) 0.225(8) 0.213(7) -0.042(6) 0.040(5) -0.050(6)
C1S 0.100(11) 0.149(15) 0.085(10) 0.003(11) 0.036(9) -0.036(11)
Cl5 0.089(4) 0.143(6) 0.225(8) -0.036(6) 0.060(4) -0.003(4)
Cl6 0.186(7) 0.202(7) 0.107(4) -0.079(5) 0.063(5) -0.015(6)
C2S 0.098(13) 0.085(12) 0.117(16) -0.049(12) 0.014(12) -0.007(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 N4 2.019(5) . ?
Pd1 Cl2 2.2920(18) . ?
Pd1 Cl1 2.3335(16) . ?
Pd1 Cl1 2.3413(18) 3_655 ?
Cl1 Pd1 2.3413(18) 3_655 ?
N1 C1 1.360(7) . ?
N1 C2 1.395(7) . ?
N1 C16 1.438(7) . ?
N2 C1 1.381(7) . ?
N2 C3 1.401(7) . ?
N2 C4 1.447(8) . ?
N3 C1 1.313(7) . ?
N3 C28 1.321(7) . ?
N4 C28 1.332(7) . ?
N4 C30 1.439(7) . ?
N4 Pd1A 2.226(5) 3_655 ?
C2 C3 1.327(9) . ?
C4 C9 1.378(12) . ?
C4 C5 1.425(11) . ?
C5 C6 1.390(11) . ?
C5 C13 1.502(13) . ?
C6 C7 1.391(15) . ?
C7 C8 1.365(15) . ?
C8 C9 1.423(11) . ?
C9 C10 1.506(13) . ?
C10 C11 1.547(13) . ?
C10 C12 1.550(11) . ?
C13 C14 1.536(11) . ?
C13 C15 1.546(12) . ?
C16 C17 1.375(10) . ?
C16 C21 1.395(9) . ?
C17 C18 1.391(9) . ?
C17 C22 1.540(10) . ?
C18 C19 1.374(11) . ?
C19 C20 1.375(13) . ?
C20 C21 1.402(11) . ?
C21 C25 1.495(12) . ?
C22 C23 1.507(9) . ?
C22 C24 1.544(11) . ?
C25 C27 1.498(14) . ?
C25 C26 1.564(15) . ?
C28 C29 1.499(9) . ?
C30 C35 1.370(9) . ?
C30 C31 1.404(8) . ?
C31 C32 1.398(9) . ?
C31 C37 1.520(10) . ?
C32 C33 1.392(11) . ?
C33 C34 1.373(12) . ?
C34 C35 1.368(11) . ?
C35 C36 1.532(10) . ?
Pd1A N4 2.226(5) 3_655 ?
Pd1A Cl2A 2.296(11) . ?
Pd1A Cl1A 2.322(10) . ?
Pd1A Cl1A 2.332(10) 3_655 ?
Cl1A Pd1A 2.332(10) 3_655 ?
Cl2A Cl3 1.590(15) . ?
Cl3 C1S 1.681(10) . ?
Cl4 C1S 1.687(10) . ?
Cl5 C2S 1.686(10) . ?
Cl6 C2S 1.684(10) . ?
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
N4 Pd1 Cl2 95.07(16) . . ?
N4 Pd1 Cl1 175.48(16) . . ?
Cl2 Pd1 Cl1 88.89(6) . . ?
N4 Pd1 Cl1 90.60(16) . 3_655 ?
Cl2 Pd1 Cl1 174.20(6) . 3_655 ?
Cl1 Pd1 Cl1 85.50(6) . 3_655 ?
Pd1 Cl1 Pd1 94.50(6) . 3_655 ?
C1 N1 C2 110.0(5) . . ?
C1 N1 C16 123.2(5) . . ?
C2 N1 C16 126.8(5) . . ?
C1 N2 C3 108.5(5) . . ?
C1 N2 C4 124.8(5) . . ?
C3 N2 C4 124.6(5) . . ?
C1 N3 C28 124.2(5) . . ?
C28 N4 C30 118.8(5) . . ?
C28 N4 Pd1 125.2(4) . . ?
C30 N4 Pd1 116.0(3) . . ?
C28 N4 Pd1A 118.7(4) . 3_655 ?
C30 N4 Pd1A 104.6(3) . 3_655 ?
Pd1 N4 Pd1A 43.31(11) . 3_655 ?
N3 C1 N1 124.8(5) . . ?
N3 C1 N2 128.7(5) . . ?
N1 C1 N2 105.7(4) . . ?
C3 C2 N1 107.4(5) . . ?
C2 C3 N2 108.4(5) . . ?
C9 C4 C5 124.3(7) . . ?
C9 C4 N2 116.4(7) . . ?
C5 C4 N2 119.3(7) . . ?
C6 C5 C4 116.2(10) . . ?
C6 C5 C13 119.9(8) . . ?
C4 C5 C13 123.7(7) . . ?
C5 C6 C7 119.1(10) . . ?
C8 C7 C6 124.8(8) . . ?
C7 C8 C9 117.4(10) . . ?
C4 C9 C8 118.0(8) . . ?
C4 C9 C10 124.2(7) . . ?
C8 C9 C10 117.6(9) . . ?
C9 C10 C11 114.4(8) . . ?
C9 C10 C12 113.5(8) . . ?
C11 C10 C12 108.5(8) . . ?
C5 C13 C14 111.4(7) . . ?
C5 C13 C15 113.0(8) . . ?
C14 C13 C15 109.3(8) . . ?
C17 C16 C21 123.4(6) . . ?
C17 C16 N1 118.6(6) . . ?
C21 C16 N1 118.0(6) . . ?
C16 C17 C18 117.6(7) . . ?
C16 C17 C22 122.9(5) . . ?
C18 C17 C22 119.5(6) . . ?
C19 C18 C17 121.4(8) . . ?
C18 C19 C20 119.6(7) . . ?
C19 C20 C21 121.6(8) . . ?
C16 C21 C20 116.4(8) . . ?
C16 C21 C25 122.4(7) . . ?
C20 C21 C25 121.2(7) . . ?
C23 C22 C17 110.5(6) . . ?
C23 C22 C24 111.2(6) . . ?
C17 C22 C24 112.9(6) . . ?
C21 C25 C27 114.9(9) . . ?
C21 C25 C26 108.8(8) . . ?
C27 C25 C26 109.4(9) . . ?
N3 C28 N4 120.3(5) . . ?
N3 C28 C29 122.9(5) . . ?
N4 C28 C29 116.7(5) . . ?
C35 C30 C31 122.1(6) . . ?
C35 C30 N4 119.7(5) . . ?
C31 C30 N4 118.2(5) . . ?
C32 C31 C30 118.3(6) . . ?
C32 C31 C37 120.0(6) . . ?
C30 C31 C37 121.7(6) . . ?
C33 C32 C31 119.6(7) . . ?
C34 C33 C32 119.2(7) . . ?
C35 C34 C33 122.9(7) . . ?
C34 C35 C30 117.8(6) . . ?
C34 C35 C36 121.4(6) . . ?
C30 C35 C36 120.7(6) . . ?
N4 Pd1A Cl2A 107.0(3) 3_655 . ?
N4 Pd1A Cl1A 162.1(3) 3_655 . ?
Cl2A Pd1A Cl1A 87.9(4) . . ?
N4 Pd1A Cl1A 78.8(3) 3_655 3_655 ?
Cl2A Pd1A Cl1A 173.6(4) . 3_655 ?
Cl1A Pd1A Cl1A 85.9(4) . 3_655 ?
Pd1A Cl1A Pd1A 94.1(4) . 3_655 ?
Cl3 Cl2A Pd1A 134.0(8) . . ?
Cl2A Cl3 C1S 110.4(10) . . ?
Cl3 C1S Cl4 109.5(12) . . ?
Cl6 C2S Cl5 112.1(10) . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 27.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 1.514
_refine_diff_density_min -1.118
_refine_diff_density_rms 0.131
_vrf_PLAT431_k09220
;
PROBLEM: Short Inter HL..A Contact Cl3 .. Cl2A .. 1.59 Ang.
RESPONSE: These atoms are 0.5 and 0.17 occupancy and do not
necessarily occupy these sites simoultaneously
;
_vrf_PLAT432_k09220
;
PROBLEM: Short Inter X...Y Contact C1S .. Cl2A .. 2.69 Ang.
RESPONSE: These atoms are 0.5 and 0.17 occupancy and do not
necessarily occupy these sites simoultaneously
;
_vrf_PLAT780_k09220
;
PROBLEM: Coordinates do not Form a Properly Connected Set ?
RESPONSE: Must be referring to disordered central Pd~2~Cl~4~ unit
which is disordered over two sites 0.83:0.17 occupancy
;