# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
loop_
_publ_author_name
_publ_author_address
T.G.Larocque
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
M3J 1P3, Canada
;
A.C.Badaj
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
M3J 1P3, Canada
;
S.Dastgir
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
M3J 1P3, Canada
;
G.G.Lavoie
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
M3J 1P3, Canada
;
_publ_contact_author_address
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
M3J 1P3, Canada
;
_publ_contact_author_email glavoie@yorku.ca
_publ_contact_author_fax '+1 416-736-5936'
_publ_contact_author_phone '+1 416-736-2100'
_publ_contact_author_name 'Prof. Gino G. Lavoie'
data_k09214
_database_code_depnum_ccdc_archive 'CCDC 808924'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C25 H31 N3'
_chemical_formula_sum 'C25 H31 N3'
_chemical_formula_weight 373.53
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'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.5723(3)
_cell_length_b 11.8829(7)
_cell_length_c 12.3644(8)
_cell_angle_alpha 70.656(2)
_cell_angle_beta 88.378(3)
_cell_angle_gamma 69.372(3)
_cell_volume 1106.61(10)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 10345
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.121
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 404
_exptl_absorpt_coefficient_mu 0.066
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.768
_exptl_absorpt_correction_T_max 0.985
_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 10345
_diffrn_reflns_av_R_equivalents 0.0480
_diffrn_reflns_av_sigmaI/netI 0.0701
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.59
_diffrn_reflns_theta_max 27.50
_reflns_number_total 4990
_reflns_number_gt 2899
_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^)+(0.1206P)^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 4990
_refine_ls_number_parameters 261
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1269
_refine_ls_R_factor_gt 0.0699
_refine_ls_wR_factor_ref 0.2146
_refine_ls_wR_factor_gt 0.1747
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_restrained_S_all 1.049
_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
C1 C 0.7112(2) 0.2549(2) 0.79425(19) 0.0362(5) Uani 1 1 d . . .
C2 C 0.7055(3) 0.3033(2) 0.5977(2) 0.0414(6) Uani 1 1 d . . .
H2 H 0.7107 0.2929 0.5246 0.050 Uiso 1 1 calc R . .
C3 C 0.6784(3) 0.4120(2) 0.6183(2) 0.0413(6) Uani 1 1 d . . .
H3 H 0.6608 0.4941 0.5629 0.050 Uiso 1 1 calc R . .
C4 C 0.7487(2) 0.0776(2) 0.71982(18) 0.0317(5) Uani 1 1 d . . .
C5 C 0.8993(2) -0.0265(2) 0.8010(2) 0.0385(5) Uani 1 1 d . . .
C6 C 0.5014(2) 0.1388(2) 0.59849(19) 0.0333(5) Uani 1 1 d . . .
C7 C 0.4952(3) 0.1623(2) 0.47937(19) 0.0382(5) Uani 1 1 d . . .
C8 C 0.3450(3) 0.2388(2) 0.4130(2) 0.0451(6) Uani 1 1 d . . .
H8 H 0.3391 0.2558 0.3323 0.054 Uiso 1 1 calc R . .
C9 C 0.2029(3) 0.2912(2) 0.4618(2) 0.0490(6) Uani 1 1 d . . .
H9 H 0.1006 0.3443 0.4147 0.059 Uiso 1 1 calc R . .
C10 C 0.2100(3) 0.2662(2) 0.5796(2) 0.0439(6) Uani 1 1 d . . .
H10 H 0.1116 0.3019 0.6127 0.053 Uiso 1 1 calc R . .
C11 C 0.3591(2) 0.1894(2) 0.65042(19) 0.0348(5) Uani 1 1 d . . .
C12 C 0.6499(3) 0.1020(2) 0.4265(2) 0.0477(6) Uani 1 1 d . . .
H12A H 0.6185 0.1129 0.3471 0.072 Uiso 1 1 calc R . .
H12B H 0.7009 0.0105 0.4715 0.072 Uiso 1 1 calc R . .
H12C H 0.7303 0.1435 0.4268 0.072 Uiso 1 1 calc R . .
C13 C 0.3643(3) 0.1581(2) 0.7785(2) 0.0406(6) Uani 1 1 d . . .
H13A H 0.2519 0.1978 0.7990 0.061 Uiso 1 1 calc R . .
H13B H 0.4416 0.1909 0.8035 0.061 Uiso 1 1 calc R . .
H13C H 0.4028 0.0650 0.8167 0.061 Uiso 1 1 calc R . .
C14 C 0.6493(2) 0.47202(19) 0.79622(18) 0.0309(5) Uani 1 1 d . . .
C15 C 0.4832(2) 0.5442(2) 0.80397(19) 0.0348(5) Uani 1 1 d . . .
C16 C 0.4559(2) 0.6313(2) 0.86117(19) 0.0362(5) Uani 1 1 d . . .
H16 H 0.3439 0.6804 0.8680 0.043 Uiso 1 1 calc R . .
C17 C 0.5862(2) 0.6491(2) 0.90865(18) 0.0358(5) Uani 1 1 d . . .
C18 C 0.7497(2) 0.5739(2) 0.90033(18) 0.0342(5) Uani 1 1 d . . .
H18 H 0.8403 0.5835 0.9340 0.041 Uiso 1 1 calc R . .
C19 C 0.7839(2) 0.48528(19) 0.84441(18) 0.0326(5) Uani 1 1 d . . .
C20 C 0.3381(3) 0.5272(2) 0.7534(2) 0.0483(6) Uani 1 1 d . . .
H20A H 0.3414 0.5490 0.6699 0.073 Uiso 1 1 calc R . .
H20B H 0.2325 0.5836 0.7696 0.073 Uiso 1 1 calc R . .
H20C H 0.3463 0.4380 0.7880 0.073 Uiso 1 1 calc R . .
C21 C 0.5511(3) 0.7498(2) 0.9640(2) 0.0478(6) Uani 1 1 d . . .
H21A H 0.6514 0.7329 1.0120 0.072 Uiso 1 1 calc R . .
H21B H 0.4585 0.7476 1.0120 0.072 Uiso 1 1 calc R . .
H21C H 0.5205 0.8343 0.9040 0.072 Uiso 1 1 calc R . .
C22 C 0.9612(2) 0.4078(2) 0.8340(2) 0.0413(6) Uani 1 1 d . . .
H22A H 0.9803 0.3165 0.8691 0.062 Uiso 1 1 calc R . .
H22B H 1.0384 0.4290 0.8737 0.062 Uiso 1 1 calc R . .
H22C H 0.9804 0.4275 0.7525 0.062 Uiso 1 1 calc R . .
C23 C 0.8561(3) -0.0484(2) 0.9257(2) 0.0498(6) Uani 1 1 d . . .
H23A H 0.8228 0.0325 0.9406 0.075 Uiso 1 1 calc R . .
H23B H 0.9544 -0.1116 0.9785 0.075 Uiso 1 1 calc R . .
H23C H 0.7635 -0.0801 0.9377 0.075 Uiso 1 1 calc R . .
C24 C 1.0518(3) 0.0143(2) 0.7831(3) 0.0523(7) Uani 1 1 d . . .
H24A H 1.0697 0.0385 0.7012 0.078 Uiso 1 1 calc R . .
H24B H 1.1512 -0.0572 0.8281 0.078 Uiso 1 1 calc R . .
H24C H 1.0319 0.0875 0.8086 0.078 Uiso 1 1 calc R . .
C25 C 0.9374(3) -0.1512(2) 0.7758(3) 0.0562(7) Uani 1 1 d . . .
H25A H 0.8386 -0.1756 0.7857 0.084 Uiso 1 1 calc R . .
H25B H 1.0318 -0.2193 0.8292 0.084 Uiso 1 1 calc R . .
H25C H 0.9663 -0.1382 0.6965 0.084 Uiso 1 1 calc R . .
N1 N 0.72460(19) 0.20879(16) 0.70419(15) 0.0327(4) Uani 1 1 d . . .
N2 N 0.68126(19) 0.38048(16) 0.73744(15) 0.0336(4) Uani 1 1 d . . .
N3 N 0.6513(2) 0.04824(16) 0.66850(15) 0.0348(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0347(11) 0.0352(12) 0.0384(13) -0.0149(11) 0.0027(9) -0.0101(9)
C2 0.0556(14) 0.0403(14) 0.0319(13) -0.0127(11) 0.0049(10) -0.0215(11)
C3 0.0565(13) 0.0368(13) 0.0306(13) -0.0069(11) -0.0002(10) -0.0211(10)
C4 0.0344(11) 0.0306(12) 0.0336(12) -0.0154(10) 0.0109(8) -0.0125(9)
C5 0.0335(11) 0.0307(12) 0.0473(15) -0.0116(11) -0.0024(9) -0.0083(9)
C6 0.0403(11) 0.0287(11) 0.0341(13) -0.0127(10) 0.0006(9) -0.0141(9)
C7 0.0511(13) 0.0338(12) 0.0333(13) -0.0099(10) 0.0021(10) -0.0212(10)
C8 0.0593(15) 0.0424(14) 0.0364(14) -0.0084(12) -0.0027(11) -0.0258(11)
C9 0.0490(14) 0.0418(15) 0.0494(17) -0.0053(12) -0.0130(11) -0.0168(11)
C10 0.0387(12) 0.0375(13) 0.0514(16) -0.0128(12) -0.0001(10) -0.0112(10)
C11 0.0345(11) 0.0330(12) 0.0386(13) -0.0135(11) 0.0028(9) -0.0128(9)
C12 0.0662(15) 0.0473(15) 0.0391(15) -0.0219(13) 0.0135(11) -0.0257(12)
C13 0.0384(12) 0.0464(14) 0.0396(14) -0.0194(12) 0.0073(9) -0.0142(10)
C14 0.0346(11) 0.0253(11) 0.0301(12) -0.0082(9) 0.0029(8) -0.0091(8)
C15 0.0335(11) 0.0302(12) 0.0372(13) -0.0078(10) 0.0015(9) -0.0108(9)
C16 0.0333(11) 0.0310(12) 0.0393(13) -0.0100(10) 0.0074(9) -0.0081(9)
C17 0.0445(12) 0.0324(12) 0.0305(12) -0.0112(10) 0.0077(9) -0.0140(9)
C18 0.0395(11) 0.0339(12) 0.0297(12) -0.0091(10) 0.0018(8) -0.0154(9)
C19 0.0335(11) 0.0279(11) 0.0324(12) -0.0066(10) 0.0012(8) -0.0097(8)
C20 0.0347(12) 0.0436(15) 0.0655(18) -0.0183(13) 0.0003(11) -0.0129(10)
C21 0.0565(14) 0.0432(14) 0.0497(16) -0.0250(13) 0.0114(11) -0.0172(11)
C22 0.0360(12) 0.0406(14) 0.0463(15) -0.0169(12) 0.0000(9) -0.0106(9)
C23 0.0588(15) 0.0401(14) 0.0425(16) -0.0028(12) -0.0109(11) -0.0180(11)
C24 0.0334(12) 0.0428(15) 0.078(2) -0.0209(14) -0.0017(11) -0.0104(10)
C25 0.0420(13) 0.0388(15) 0.083(2) -0.0254(15) -0.0061(12) -0.0048(10)
N1 0.0345(9) 0.0318(10) 0.0345(11) -0.0141(9) 0.0033(7) -0.0126(7)
N2 0.0364(9) 0.0298(10) 0.0339(11) -0.0115(8) 0.0014(7) -0.0106(7)
N3 0.0359(9) 0.0335(10) 0.0365(11) -0.0147(9) 0.0049(7) -0.0119(8)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 N2 1.354(3) . ?
C1 N1 1.380(3) . ?
C2 C3 1.338(3) . ?
C2 N1 1.388(3) . ?
C3 N2 1.393(3) . ?
C4 N3 1.266(3) . ?
C4 N1 1.444(3) . ?
C4 C5 1.526(3) . ?
C5 C24 1.533(3) . ?
C5 C23 1.534(3) . ?
C5 C25 1.535(3) . ?
C6 C11 1.399(3) . ?
C6 C7 1.404(3) . ?
C6 N3 1.425(3) . ?
C7 C8 1.377(3) . ?
C7 C12 1.513(3) . ?
C8 C9 1.382(3) . ?
C9 C10 1.385(3) . ?
C10 C11 1.395(3) . ?
C11 C13 1.500(3) . ?
C14 C19 1.393(3) . ?
C14 C15 1.400(3) . ?
C14 N2 1.445(2) . ?
C15 C16 1.390(3) . ?
C15 C20 1.511(3) . ?
C16 C17 1.387(3) . ?
C17 C18 1.394(3) . ?
C17 C21 1.505(3) . ?
C18 C19 1.388(3) . ?
C19 C22 1.502(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
N2 C1 N1 101.48(19) . . ?
C3 C2 N1 106.5(2) . . ?
C2 C3 N2 106.1(2) . . ?
N3 C4 N1 122.38(18) . . ?
N3 C4 C5 120.47(18) . . ?
N1 C4 C5 117.15(17) . . ?
C4 C5 C24 109.91(19) . . ?
C4 C5 C23 109.01(16) . . ?
C24 C5 C23 110.11(19) . . ?
C4 C5 C25 108.90(17) . . ?
C24 C5 C25 109.93(18) . . ?
C23 C5 C25 109.0(2) . . ?
C11 C6 C7 121.56(18) . . ?
C11 C6 N3 119.69(19) . . ?
C7 C6 N3 118.26(17) . . ?
C8 C7 C6 118.5(2) . . ?
C8 C7 C12 121.3(2) . . ?
C6 C7 C12 120.24(19) . . ?
C7 C8 C9 121.2(2) . . ?
C8 C9 C10 119.9(2) . . ?
C9 C10 C11 121.1(2) . . ?
C10 C11 C6 117.8(2) . . ?
C10 C11 C13 120.84(18) . . ?
C6 C11 C13 121.32(18) . . ?
C19 C14 C15 121.82(18) . . ?
C19 C14 N2 119.37(16) . . ?
C15 C14 N2 118.80(17) . . ?
C16 C15 C14 117.67(18) . . ?
C16 C15 C20 120.91(18) . . ?
C14 C15 C20 121.41(19) . . ?
C17 C16 C15 122.38(18) . . ?
C16 C17 C18 117.98(19) . . ?
C16 C17 C21 120.65(18) . . ?
C18 C17 C21 121.34(19) . . ?
C19 C18 C17 121.95(19) . . ?
C18 C19 C14 118.18(17) . . ?
C18 C19 C22 120.88(18) . . ?
C14 C19 C22 120.93(18) . . ?
C1 N1 C2 112.55(18) . . ?
C1 N1 C4 123.25(18) . . ?
C2 N1 C4 124.15(17) . . ?
C1 N2 C3 113.41(17) . . ?
C1 N2 C14 122.37(18) . . ?
C3 N2 C14 124.18(18) . . ?
C4 N3 C6 123.86(18) . . ?
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full 27.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max 0.423
_refine_diff_density_min -0.270
_refine_diff_density_rms 0.060
#
data_k1010
_database_code_depnum_ccdc_archive 'CCDC 808925'
#TrackingRef 'Combined_CIF.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C25 H31 Cl4 N3 Ti, C H2 Cl2'
_chemical_formula_sum 'C26 H33 Cl6 N3 Ti'
_chemical_formula_weight 648.15
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 '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 9.7534(5)
_cell_length_b 18.8425(11)
_cell_length_c 16.5548(7)
_cell_angle_alpha 90.00
_cell_angle_beta 93.221(3)
_cell_angle_gamma 90.00
_cell_volume 3037.6(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 20804
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 25.1
_exptl_crystal_description needle
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.417
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1336
_exptl_absorpt_coefficient_mu 0.830
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.774
_exptl_absorpt_correction_T_max 0.977
_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 20804
_diffrn_reflns_av_R_equivalents 0.0855
_diffrn_reflns_av_sigmaI/netI 0.0765
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.60
_diffrn_reflns_theta_max 25.07
_reflns_number_total 5388
_reflns_number_gt 3386
_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^)+(0.0717P)^2^+7.0837P] 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 5388
_refine_ls_number_parameters 337
_refine_ls_number_restraints 18
_refine_ls_R_factor_all 0.1173
_refine_ls_R_factor_gt 0.0675
_refine_ls_wR_factor_ref 0.1895
_refine_ls_wR_factor_gt 0.1643
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.045
_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
Ti1 Ti 0.73626(10) 0.28688(5) 0.27616(5) 0.0364(3) Uani 1 1 d . . .
Cl3 Cl 0.96837(15) 0.30114(8) 0.28837(8) 0.0482(4) Uani 1 1 d . . .
Cl2 Cl 0.50298(15) 0.30342(8) 0.26966(9) 0.0508(4) Uani 1 1 d . . .
Cl4 Cl 0.73612(18) 0.19681(7) 0.18410(8) 0.0535(4) Uani 1 1 d . . .
Cl1 Cl 0.73217(15) 0.23159(7) 0.39558(8) 0.0451(4) Uani 1 1 d . . .
N1 N 0.7457(4) 0.4496(2) 0.2683(2) 0.0377(11) Uani 1 1 d . . .
N2 N 0.7375(4) 0.4260(2) 0.3951(3) 0.0388(11) Uani 1 1 d . . .
N3 N 0.7444(4) 0.3675(2) 0.1676(2) 0.0337(10) Uani 1 1 d . . .
C1 C 0.7395(5) 0.3945(3) 0.3223(3) 0.0358(12) Uani 1 1 d . . .
C2 C 0.7502(6) 0.5142(3) 0.3092(4) 0.0483(15) Uani 1 1 d . . .
H2A H 0.7556 0.5601 0.2860 0.058 Uiso 1 1 calc R . .
C3 C 0.7453(6) 0.4987(3) 0.3873(4) 0.0495(15) Uani 1 1 d . . .
H3A H 0.7469 0.5320 0.4304 0.059 Uiso 1 1 calc R . .
C4 C 0.7493(5) 0.4345(3) 0.1827(3) 0.0359(12) Uani 1 1 d . . .
C5 C 0.7563(6) 0.5000(3) 0.1280(3) 0.0414(13) Uani 1 1 d . . .
C24 C 0.6262(6) 0.5461(3) 0.1379(4) 0.0543(16) Uani 1 1 d . . .
H24A H 0.5444 0.5193 0.1193 0.081 Uiso 1 1 calc R . .
H24B H 0.6323 0.5895 0.1056 0.081 Uiso 1 1 calc R . .
H24C H 0.6198 0.5587 0.1950 0.081 Uiso 1 1 calc R . .
C23 C 0.8918(6) 0.5406(3) 0.1503(4) 0.0536(16) Uani 1 1 d . . .
H23A H 0.9692 0.5147 0.1290 0.080 Uiso 1 1 calc R . .
H23B H 0.9048 0.5443 0.2092 0.080 Uiso 1 1 calc R . .
H23C H 0.8868 0.5882 0.1266 0.080 Uiso 1 1 calc R . .
C25 C 0.7580(7) 0.4841(3) 0.0367(3) 0.0586(17) Uani 1 1 d . . .
H25A H 0.8424 0.4585 0.0256 0.088 Uiso 1 1 calc R . .
H25B H 0.7543 0.5288 0.0063 0.088 Uiso 1 1 calc R . .
H25C H 0.6782 0.4549 0.0200 0.088 Uiso 1 1 calc R . .
C14 C 0.7312(6) 0.3931(3) 0.4742(3) 0.0387(13) Uani 1 1 d . . .
C19 C 0.6029(6) 0.3838(3) 0.5053(3) 0.0432(14) Uani 1 1 d . . .
C18 C 0.5997(6) 0.3578(3) 0.5846(3) 0.0480(15) Uani 1 1 d . . .
H18A H 0.5136 0.3510 0.6075 0.058 Uiso 1 1 calc R . .
C17 C 0.7201(7) 0.3415(3) 0.6306(3) 0.0497(15) Uani 1 1 d . . .
C16 C 0.8441(6) 0.3509(3) 0.5960(3) 0.0430(14) Uani 1 1 d . . .
H16A H 0.9262 0.3389 0.6265 0.052 Uiso 1 1 calc R . .
C15 C 0.8537(6) 0.3773(3) 0.5182(3) 0.0409(13) Uani 1 1 d . . .
C22 C 0.4719(6) 0.4012(3) 0.4573(4) 0.0558(16) Uani 1 1 d . . .
H22A H 0.4725 0.3786 0.4040 0.084 Uiso 1 1 calc R . .
H22B H 0.4641 0.4527 0.4507 0.084 Uiso 1 1 calc R . .
H22C H 0.3936 0.3835 0.4860 0.084 Uiso 1 1 calc R . .
C21 C 0.7139(8) 0.3159(4) 0.7168(3) 0.0645(19) Uani 1 1 d . . .
H21A H 0.7865 0.3389 0.7507 0.097 Uiso 1 1 calc R . .
H21B H 0.7270 0.2643 0.7186 0.097 Uiso 1 1 calc R . .
H21C H 0.6242 0.3278 0.7370 0.097 Uiso 1 1 calc R . .
C20 C 0.9916(6) 0.3900(3) 0.4845(4) 0.0520(15) Uani 1 1 d . . .
H20A H 1.0642 0.3746 0.5239 0.078 Uiso 1 1 calc R . .
H20B H 1.0024 0.4407 0.4733 0.078 Uiso 1 1 calc R . .
H20C H 0.9980 0.3630 0.4342 0.078 Uiso 1 1 calc R . .
C6 C 0.7461(6) 0.3394(3) 0.0853(3) 0.0371(13) Uani 1 1 d . . .
C11 C 0.6202(6) 0.3257(3) 0.0430(3) 0.0417(14) Uani 1 1 d . . .
C10 C 0.6229(7) 0.2928(3) -0.0323(3) 0.0499(15) Uani 1 1 d . . .
H10A H 0.5388 0.2832 -0.0621 0.060 Uiso 1 1 calc R . .
C9 C 0.7448(7) 0.2741(3) -0.0644(3) 0.0535(16) Uani 1 1 d . . .
H9A H 0.7446 0.2507 -0.1152 0.064 Uiso 1 1 calc R . .
C8 C 0.8660(7) 0.2893(3) -0.0226(3) 0.0501(15) Uani 1 1 d . . .
H8A H 0.9498 0.2768 -0.0456 0.060 Uiso 1 1 calc R . .
C7 C 0.8709(6) 0.3229(3) 0.0533(3) 0.0408(13) Uani 1 1 d . . .
C13 C 0.4833(6) 0.3474(4) 0.0733(3) 0.0533(16) Uani 1 1 d . . .
H13A H 0.4192 0.3579 0.0271 0.080 Uiso 1 1 calc R . .
H13B H 0.4952 0.3898 0.1073 0.080 Uiso 1 1 calc R . .
H13C H 0.4467 0.3086 0.1051 0.080 Uiso 1 1 calc R . .
C12 C 1.0080(6) 0.3409(4) 0.0928(3) 0.0516(16) Uani 1 1 d . . .
H12A H 0.9989 0.3822 0.1282 0.077 Uiso 1 1 calc R . .
H12B H 1.0723 0.3521 0.0512 0.077 Uiso 1 1 calc R . .
H12C H 1.0427 0.3004 0.1249 0.077 Uiso 1 1 calc R . .
Cl5 Cl 0.1708(3) 0.47315(19) 0.33092(16) 0.1337(11) Uani 1 1 d D . .
Cl6 Cl 0.2686(2) 0.49583(17) 0.17301(14) 0.1140(9) Uani 1 1 d D . .
C1S C 0.2491(14) 0.4371(6) 0.2511(4) 0.085(4) Uani 0.522(11) 1 d PDU A 1
H1SA H 0.1944 0.3960 0.2304 0.102 Uiso 0.522(11) 1 calc PR A 1
H1SB H 0.3407 0.4192 0.2702 0.102 Uiso 0.522(11) 1 calc PR A 1
C2S C 0.3110(10) 0.4816(9) 0.2735(3) 0.085(4) Uani 0.478(11) 1 d PDU A 2
H2SA H 0.3680 0.5217 0.2946 0.102 Uiso 0.478(11) 1 calc PR A 2
H2SB H 0.3671 0.4379 0.2791 0.102 Uiso 0.478(11) 1 calc PR A 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
Ti1 0.0497(6) 0.0256(5) 0.0340(5) 0.0000(4) 0.0036(4) 0.0002(4)
Cl3 0.0498(9) 0.0516(9) 0.0437(8) 0.0067(6) 0.0064(7) 0.0075(7)
Cl2 0.0483(9) 0.0506(9) 0.0532(9) 0.0020(7) 0.0009(7) -0.0060(7)
Cl4 0.0924(12) 0.0282(7) 0.0402(8) -0.0024(6) 0.0065(8) 0.0000(7)
Cl1 0.0619(9) 0.0361(8) 0.0376(7) 0.0047(6) 0.0061(6) 0.0002(7)
N1 0.051(3) 0.025(2) 0.037(2) 0.0013(19) 0.002(2) 0.001(2)
N2 0.045(3) 0.034(3) 0.038(2) -0.005(2) 0.006(2) -0.001(2)
N3 0.036(2) 0.033(2) 0.032(2) 0.0010(19) 0.0019(19) 0.002(2)
C1 0.043(3) 0.028(3) 0.036(3) -0.002(2) 0.001(2) 0.002(2)
C2 0.071(4) 0.024(3) 0.050(4) -0.008(3) 0.005(3) -0.004(3)
C3 0.068(4) 0.030(3) 0.051(4) -0.010(3) 0.007(3) -0.002(3)
C4 0.040(3) 0.034(3) 0.035(3) 0.003(2) 0.004(2) 0.002(2)
C5 0.051(3) 0.030(3) 0.044(3) 0.009(2) 0.005(3) -0.001(3)
C24 0.064(4) 0.032(3) 0.067(4) 0.008(3) 0.004(3) 0.003(3)
C23 0.056(4) 0.034(3) 0.072(4) 0.006(3) 0.011(3) 0.002(3)
C25 0.085(5) 0.042(4) 0.049(4) 0.018(3) 0.006(3) 0.000(3)
C14 0.052(4) 0.030(3) 0.035(3) -0.008(2) 0.010(3) 0.000(3)
C19 0.052(4) 0.037(3) 0.041(3) -0.008(2) 0.006(3) 0.002(3)
C18 0.050(4) 0.046(4) 0.050(4) -0.005(3) 0.016(3) -0.006(3)
C17 0.069(4) 0.038(3) 0.042(3) -0.001(3) 0.007(3) -0.003(3)
C16 0.047(4) 0.041(3) 0.041(3) -0.004(3) 0.000(3) 0.000(3)
C15 0.045(3) 0.036(3) 0.042(3) -0.009(2) 0.007(3) -0.003(3)
C22 0.052(4) 0.060(4) 0.056(4) -0.007(3) 0.004(3) 0.008(3)
C21 0.083(5) 0.068(5) 0.043(4) 0.005(3) 0.010(3) -0.010(4)
C20 0.053(4) 0.052(4) 0.051(4) -0.004(3) 0.005(3) -0.006(3)
C6 0.052(4) 0.026(3) 0.034(3) 0.006(2) 0.006(3) 0.003(2)
C11 0.054(4) 0.034(3) 0.037(3) 0.002(2) 0.000(3) -0.002(3)
C10 0.065(4) 0.050(4) 0.034(3) 0.002(3) -0.005(3) -0.003(3)
C9 0.074(5) 0.054(4) 0.032(3) 0.001(3) 0.001(3) 0.000(3)
C8 0.066(4) 0.050(4) 0.035(3) 0.004(3) 0.012(3) 0.011(3)
C7 0.053(4) 0.037(3) 0.033(3) 0.006(2) 0.005(3) 0.005(3)
C13 0.048(4) 0.064(4) 0.046(3) 0.005(3) -0.004(3) 0.001(3)
C12 0.049(4) 0.066(4) 0.041(3) 0.007(3) 0.006(3) 0.001(3)
Cl5 0.117(2) 0.186(3) 0.1004(18) 0.0355(19) 0.0307(16) -0.029(2)
Cl6 0.0709(14) 0.197(3) 0.0758(14) 0.0037(15) 0.0174(11) 0.0001(16)
C1S 0.101(8) 0.062(7) 0.087(7) -0.021(6) -0.044(6) 0.027(6)
C2S 0.101(8) 0.062(7) 0.087(7) -0.021(6) -0.044(6) 0.027(6)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 2.167(5) . ?
Ti1 Cl1 2.2370(16) . ?
Ti1 Cl3 2.2775(18) . ?
Ti1 Cl4 2.2808(16) . ?
Ti1 Cl2 2.2930(18) . ?
Ti1 N3 2.358(4) . ?
N1 C1 1.373(6) . ?
N1 C2 1.392(7) . ?
N1 C4 1.448(6) . ?
N2 C1 1.344(6) . ?
N2 C3 1.379(7) . ?
N2 C14 1.453(7) . ?
N3 C4 1.288(6) . ?
N3 C6 1.463(6) . ?
C2 C3 1.329(8) . ?
C4 C5 1.535(7) . ?
C5 C25 1.542(8) . ?
C5 C23 1.552(8) . ?
C5 C24 1.554(8) . ?
C14 C19 1.390(8) . ?
C14 C15 1.396(8) . ?
C19 C18 1.403(8) . ?
C19 C22 1.502(8) . ?
C18 C17 1.397(8) . ?
C17 C16 1.379(8) . ?
C17 C21 1.512(8) . ?
C16 C15 1.388(7) . ?
C15 C20 1.504(8) . ?
C6 C7 1.390(8) . ?
C6 C11 1.403(7) . ?
C11 C10 1.394(8) . ?
C11 C13 1.508(8) . ?
C10 C9 1.375(9) . ?
C9 C8 1.367(8) . ?
C8 C7 1.405(8) . ?
C7 C12 1.494(8) . ?
Cl5 C1S 1.704(6) . ?
Cl5 C2S 1.717(6) . ?
Cl6 C2S 1.712(6) . ?
Cl6 C1S 1.721(6) . ?
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 Ti1 Cl1 97.19(14) . . ?
C1 Ti1 Cl3 82.16(15) . . ?
Cl1 Ti1 Cl3 92.49(6) . . ?
C1 Ti1 Cl4 158.65(15) . . ?
Cl1 Ti1 Cl4 104.16(6) . . ?
Cl3 Ti1 Cl4 96.34(7) . . ?
C1 Ti1 Cl2 83.34(15) . . ?
Cl1 Ti1 Cl2 92.17(6) . . ?
Cl3 Ti1 Cl2 165.21(7) . . ?
Cl4 Ti1 Cl2 96.11(7) . . ?
C1 Ti1 N3 70.42(16) . . ?
Cl1 Ti1 N3 167.58(11) . . ?
Cl3 Ti1 N3 85.17(11) . . ?
Cl4 Ti1 N3 88.23(11) . . ?
Cl2 Ti1 N3 87.27(11) . . ?
C1 N1 C2 110.2(4) . . ?
C1 N1 C4 119.6(4) . . ?
C2 N1 C4 130.2(4) . . ?
C1 N2 C3 110.5(4) . . ?
C1 N2 C14 128.6(4) . . ?
C3 N2 C14 120.8(4) . . ?
C4 N3 C6 122.3(4) . . ?
C4 N3 Ti1 119.1(3) . . ?
C6 N3 Ti1 118.6(3) . . ?
N2 C1 N1 104.7(4) . . ?
N2 C1 Ti1 136.7(4) . . ?
N1 C1 Ti1 118.6(3) . . ?
C3 C2 N1 106.2(5) . . ?
C2 C3 N2 108.3(5) . . ?
N3 C4 N1 112.3(4) . . ?
N3 C4 C5 132.6(5) . . ?
N1 C4 C5 115.1(4) . . ?
C4 C5 C25 115.2(4) . . ?
C4 C5 C23 108.7(4) . . ?
C25 C5 C23 105.9(5) . . ?
C4 C5 C24 108.9(5) . . ?
C25 C5 C24 105.4(5) . . ?
C23 C5 C24 112.9(5) . . ?
C19 C14 C15 122.8(5) . . ?
C19 C14 N2 118.1(5) . . ?
C15 C14 N2 118.9(5) . . ?
C14 C19 C18 117.2(5) . . ?
C14 C19 C22 122.2(5) . . ?
C18 C19 C22 120.5(5) . . ?
C17 C18 C19 121.6(5) . . ?
C16 C17 C18 118.4(5) . . ?
C16 C17 C21 121.1(6) . . ?
C18 C17 C21 120.5(6) . . ?
C17 C16 C15 122.5(5) . . ?
C16 C15 C14 117.4(5) . . ?
C16 C15 C20 120.6(5) . . ?
C14 C15 C20 121.9(5) . . ?
C7 C6 C11 121.9(5) . . ?
C7 C6 N3 119.5(5) . . ?
C11 C6 N3 118.4(5) . . ?
C10 C11 C6 117.9(5) . . ?
C10 C11 C13 118.7(5) . . ?
C6 C11 C13 123.4(5) . . ?
C9 C10 C11 121.3(6) . . ?
C8 C9 C10 119.5(6) . . ?
C9 C8 C7 122.1(6) . . ?
C6 C7 C8 117.1(5) . . ?
C6 C7 C12 124.3(5) . . ?
C8 C7 C12 118.6(5) . . ?
C1S Cl5 C2S 37.0(6) . . ?
C2S Cl6 C1S 36.9(6) . . ?
Cl5 C1S Cl6 113.5(6) . . ?
Cl6 C2S Cl5 113.3(6) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.07
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 1.290
_refine_diff_density_min -1.080
_refine_diff_density_rms 0.083
#
data_k1024a
_database_code_depnum_ccdc_archive 'CCDC 808926'
#TrackingRef 'Combined_CIF.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C25 H31 Cl4 N3 Zr'
_chemical_formula_sum 'C25 H31 Cl4 N3 Zr'
_chemical_formula_weight 606.55
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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P n m a'
_symmetry_space_group_name_Hall '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
_cell_length_a 25.3593(6)
_cell_length_b 10.6747(9)
_cell_length_c 16.5496(12)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 4480.0(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 18378
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 25.0
_exptl_crystal_description plate
_exptl_crystal_colour white
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 0.899
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1240
_exptl_absorpt_coefficient_mu 0.495
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.676
_exptl_absorpt_correction_T_max 0.929
_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 4139
_diffrn_reflns_av_R_equivalents 0.089
_diffrn_reflns_av_sigmaI/netI 0.071
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.59
_diffrn_reflns_theta_max 25.08
_reflns_number_total 4139
_reflns_number_gt 2628
_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^)+(0.1419P)^2^+1.5093P] 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 4139
_refine_ls_number_parameters 180
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1080
_refine_ls_R_factor_gt 0.0800
_refine_ls_wR_factor_ref 0.2569
_refine_ls_wR_factor_gt 0.2419
_refine_ls_goodness_of_fit_ref 1.126
_refine_ls_restrained_S_all 1.126
_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
Zr1 Zr 0.26692(7) 0.2500 0.31074(11) 0.0462(9) Uani 1 2 d S . .
Cl3 Cl 0.1954(2) 0.2500 0.4058(3) 0.083(2) Uani 1 2 d S . .
Cl2 Cl 0.2783(2) 0.0251(4) 0.3058(3) 0.0697(14) Uani 1 1 d . . .
Cl1 Cl 0.2256(2) 0.2500 0.1813(3) 0.072(2) Uani 1 2 d S . .
N2 N 0.3811(6) 0.2500 0.2004(10) 0.066(6) Uani 1 2 d S . .
N3 N 0.3283(6) 0.2500 0.4274(8) 0.041(4) Uani 1 2 d S . .
C1 C 0.3540(7) 0.2500 0.2727(10) 0.035(4) Uani 1 2 d S . .
C3 C 0.4362(8) 0.2500 0.2192(14) 0.085(10) Uani 1 2 d S . .
H3 H 0.4640 0.2500 0.1808 0.102 Uiso 1 2 calc SR . .
C4 C 0.3818(7) 0.2500 0.4129(11) 0.041(4) Uani 1 2 d S . .
C5 C 0.4261(7) 0.2500 0.4708(13) 0.045(5) Uani 1 2 d S . .
C6 C 0.3587(8) 0.2500 0.1212(11) 0.057(6) Uani 1 2 d S . .
C7 C 0.3507(5) 0.1335(15) 0.0862(9) 0.051(4) Uani 1 1 d . . .
C8 C 0.3278(6) 0.1406(19) 0.0061(9) 0.062(5) Uani 1 1 d . . .
H8 H 0.3208 0.0655 -0.0226 0.075 Uiso 1 1 calc R . .
C9 C 0.3163(8) 0.2500 -0.0279(12) 0.047(5) Uani 1 2 d S . .
C10 C 0.3621(7) 0.006(2) 0.1216(11) 0.088(6) Uani 1 1 d . . .
H10A H 0.3886 0.0142 0.1643 0.132 Uiso 1 1 calc R . .
H10B H 0.3754 -0.0494 0.0792 0.132 Uiso 1 1 calc R . .
H10C H 0.3296 -0.0288 0.1444 0.132 Uiso 1 1 calc R . .
C11 C 0.2908(9) 0.2500 -0.1146(16) 0.064(7) Uani 1 2 d S . .
H11A H 0.3174 0.2741 -0.1547 0.096 Uiso 0.50 1 calc PR . .
H11B H 0.2615 0.3099 -0.1161 0.096 Uiso 0.50 1 calc PR . .
H11C H 0.2775 0.1660 -0.1271 0.096 Uiso 0.50 1 calc PR . .
C12 C 0.3067(7) 0.2500 0.5066(12) 0.043(5) Uani 1 2 d S . .
C13 C 0.2942(6) 0.1335(16) 0.5440(9) 0.058(4) Uani 1 1 d . . .
C14 C 0.2679(6) 0.1357(17) 0.6143(10) 0.058(5) Uani 1 1 d . . .
H14 H 0.2594 0.0592 0.6406 0.070 Uiso 1 1 calc R . .
C15 C 0.2529(10) 0.2500 0.6493(16) 0.076(8) Uani 1 2 d S . .
H15 H 0.2323 0.2500 0.6973 0.091 Uiso 1 2 calc SR . .
C16 C 0.3112(7) 0.0141(15) 0.5081(9) 0.062(4) Uani 1 1 d . . .
H16A H 0.3146 -0.0493 0.5506 0.094 Uiso 1 1 calc R . .
H16B H 0.3454 0.0256 0.4813 0.094 Uiso 1 1 calc R . .
H16C H 0.2851 -0.0137 0.4683 0.094 Uiso 1 1 calc R . .
C17 C 0.4086(8) 0.2500 0.5647(11) 0.048(5) Uani 1 2 d S . .
H17A H 0.4368 0.2130 0.5975 0.073 Uiso 0.50 1 calc PR . .
H17B H 0.3763 0.2007 0.5711 0.073 Uiso 0.50 1 calc PR . .
H17C H 0.4022 0.3363 0.5824 0.073 Uiso 0.50 1 calc PR . .
C18 C 0.4608(7) 0.1263(17) 0.4666(12) 0.074(5) Uani 1 1 d . . .
H18A H 0.4920 0.1360 0.5010 0.111 Uiso 1 1 calc R . .
H18B H 0.4719 0.1115 0.4107 0.111 Uiso 1 1 calc R . .
H18C H 0.4399 0.0548 0.4856 0.111 Uiso 1 1 calc R . .
N1 N 0.3936(5) 0.2500 0.3332(9) 0.041(4) Uani 1 2 d S . .
C2 C 0.4417(9) 0.2500 0.2907(14) 0.095(11) Uani 1 2 d S . .
H2 H 0.4751 0.2500 0.3165 0.114 Uiso 1 2 calc SR . .
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
Zr1 0.0312(12) 0.0718(17) 0.0355(13) 0.000 -0.0011(7) 0.000
Cl3 0.036(3) 0.171(7) 0.043(3) 0.000 0.004(2) 0.000
Cl2 0.092(3) 0.065(3) 0.052(2) -0.001(2) -0.0075(19) -0.015(2)
Cl1 0.050(3) 0.130(6) 0.038(3) 0.000 -0.011(2) 0.000
N2 0.027(9) 0.127(18) 0.042(10) 0.000 -0.013(7) 0.000
N3 0.038(8) 0.058(10) 0.026(8) 0.000 -0.002(6) 0.000
C1 0.040(10) 0.040(11) 0.026(9) 0.000 -0.002(7) 0.000
C3 0.028(11) 0.19(3) 0.039(13) 0.000 0.014(9) 0.000
C4 0.040(10) 0.043(11) 0.040(10) 0.000 -0.006(8) 0.000
C5 0.044(10) 0.040(11) 0.052(12) 0.000 0.005(9) 0.000
C6 0.057(13) 0.10(2) 0.015(9) 0.000 -0.011(8) 0.000
C7 0.030(7) 0.080(12) 0.042(8) 0.012(8) 0.003(6) -0.004(6)
C8 0.045(8) 0.104(14) 0.038(8) 0.002(9) -0.001(6) -0.012(8)
C9 0.046(11) 0.058(14) 0.037(10) 0.000 -0.001(8) 0.000
C10 0.078(12) 0.135(18) 0.051(9) 0.020(12) -0.001(9) 0.043(12)
C11 0.047(12) 0.059(14) 0.086(17) 0.000 -0.041(12) 0.000
C12 0.026(8) 0.057(12) 0.046(11) 0.000 -0.013(8) 0.000
C13 0.044(8) 0.081(12) 0.048(9) 0.021(8) -0.004(7) -0.012(7)
C14 0.056(9) 0.078(13) 0.041(9) 0.009(8) -0.013(7) -0.018(8)
C15 0.055(13) 0.13(3) 0.048(14) 0.000 0.013(12) 0.000
C16 0.084(12) 0.064(11) 0.039(8) -0.001(8) -0.011(8) -0.002(9)
C17 0.046(11) 0.066(14) 0.032(10) 0.000 -0.007(8) 0.000
C18 0.062(10) 0.076(13) 0.083(13) -0.016(10) -0.004(9) 0.010(8)
N1 0.023(7) 0.064(11) 0.036(8) 0.000 0.001(6) 0.000
C2 0.030(11) 0.22(4) 0.038(14) 0.000 0.017(9) 0.000
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Zr1 C1 2.297(17) . ?
Zr1 Cl1 2.385(5) . ?
Zr1 Cl3 2.401(5) . ?
Zr1 Cl2 2.419(5) . ?
Zr1 Cl2 2.419(5) 8_565 ?
Zr1 N3 2.479(14) . ?
N2 C1 1.38(2) . ?
N2 C3 1.43(3) . ?
N2 C6 1.43(2) . ?
N3 C4 1.38(2) . ?
N3 C12 1.42(3) . ?
C1 N1 1.42(2) . ?
C3 C2 1.19(3) . ?
C4 N1 1.35(2) . ?
C4 C5 1.48(3) . ?
C5 C18 1.589(19) . ?
C5 C18 1.589(19) 8_565 ?
C5 C17 1.62(3) . ?
C6 C7 1.386(18) . ?
C6 C7 1.386(18) 8_565 ?
C7 C8 1.45(2) . ?
C7 C10 1.51(2) . ?
C8 C9 1.33(2) . ?
C9 C8 1.33(2) 8_565 ?
C9 C11 1.57(3) . ?
C12 C13 1.425(18) . ?
C12 C13 1.425(18) 8_565 ?
C13 C14 1.34(2) . ?
C13 C16 1.47(2) . ?
C14 C15 1.40(2) . ?
C15 C14 1.40(2) 8_565 ?
N1 C2 1.41(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 Zr1 Cl1 100.1(4) . . ?
C1 Zr1 Cl3 155.0(4) . . ?
Cl1 Zr1 Cl3 104.9(2) . . ?
C1 Zr1 Cl2 82.85(13) . . ?
Cl1 Zr1 Cl2 91.25(11) . . ?
Cl3 Zr1 Cl2 96.48(12) . . ?
C1 Zr1 Cl2 82.85(13) . 8_565 ?
Cl1 Zr1 Cl2 91.25(11) . 8_565 ?
Cl3 Zr1 Cl2 96.48(12) . 8_565 ?
Cl2 Zr1 Cl2 165.7(3) . 8_565 ?
C1 Zr1 N3 67.0(5) . . ?
Cl1 Zr1 N3 167.2(4) . . ?
Cl3 Zr1 N3 87.9(4) . . ?
Cl2 Zr1 N3 87.22(11) . . ?
Cl2 Zr1 N3 87.22(11) 8_565 . ?
C1 N2 C3 107.3(16) . . ?
C1 N2 C6 126.8(16) . . ?
C3 N2 C6 126.0(18) . . ?
C4 N3 C12 122.6(14) . . ?
C4 N3 Zr1 118.8(11) . . ?
C12 N3 Zr1 118.5(10) . . ?
N2 C1 N1 105.1(14) . . ?
N2 C1 Zr1 135.7(12) . . ?
N1 C1 Zr1 119.2(11) . . ?
C2 C3 N2 109.3(19) . . ?
N1 C4 N3 112.8(15) . . ?
N1 C4 C5 117.7(16) . . ?
N3 C4 C5 129.5(16) . . ?
C4 C5 C18 113.1(11) . . ?
C4 C5 C18 113.1(11) . 8_565 ?
C18 C5 C18 112.5(18) . 8_565 ?
C4 C5 C17 114.6(15) . . ?
C18 C5 C17 101.2(12) . . ?
C18 C5 C17 101.2(12) 8_565 . ?
C7 C6 C7 127.6(17) . 8_565 ?
C7 C6 N2 116.1(9) . . ?
C7 C6 N2 116.1(9) 8_565 . ?
C6 C7 C8 113.1(14) . . ?
C6 C7 C10 128.2(14) . . ?
C8 C7 C10 118.7(16) . . ?
C9 C8 C7 121.5(17) . . ?
C8 C9 C8 123(2) . 8_565 ?
C8 C9 C11 118.5(11) . . ?
C8 C9 C11 118.5(11) 8_565 . ?
C13 C12 C13 122(2) . 8_565 ?
C13 C12 N3 119.1(10) . . ?
C13 C12 N3 119.1(10) 8_565 . ?
C14 C13 C12 118.2(16) . . ?
C14 C13 C16 120.8(15) . . ?
C12 C13 C16 121.0(14) . . ?
C13 C14 C15 120.5(17) . . ?
C14 C15 C14 121(2) . 8_565 ?
C4 N1 C2 132.7(17) . . ?
C4 N1 C1 122.1(14) . . ?
C2 N1 C1 105.1(16) . . ?
C3 C2 N1 113(2) . . ?
_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full 25.08
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max 2.713
_refine_diff_density_min -1.076
_refine_diff_density_rms 0.270
_vrf_PLAT049_k1024a
;
PROBLEM: Calculated Density less than 1.0 gcm-3 ......... 0.90
RESPONSE: The calculated density is lower as the contribution form
the highly disordered solvent molecules has not been included in
the emprical formula.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.028 -0.005 1061 280 ' '
2 0.000 -0.034 0.204 1061 279 ' '
_platon_squeeze_details
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure !
RESPONSE: During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly THF). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
large solvent cavity. In the final cycles of refinement,
this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
Staehler, R., Naether, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
_vrf_PLAT602_k1024a
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure !
RESPONSE: During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly THF). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
large solvent cavity. In the final cycles of refinement,
this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
#
data_k10226
_database_code_depnum_ccdc_archive 'CCDC 840138'
#TrackingRef 'Combined_CIF.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C29 H39 Cl3 N3 O Ti'
_chemical_formula_sum 'C29 H39 Cl3 N3 O Ti'
_chemical_formula_weight 599.88
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'
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'
O O 0.0106 0.0060 '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 Tetragonal
_symmetry_space_group_name_H-M 'I 41/a'
_symmetry_space_group_name_Hall '-I 4ad'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
_cell_length_a 34.9199(4)
_cell_length_b 34.9199(4)
_cell_length_c 11.2791(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 13753.7(3)
_cell_formula_units_Z 16
_cell_measurement_temperature 150
_cell_measurement_reflns_used 34391
_cell_measurement_theta_min 2.55
_cell_measurement_theta_max 27.48
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.159
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5040
_exptl_absorpt_coefficient_mu 0.505
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.781
_exptl_absorpt_correction_T_max 0.908
_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 51252
_diffrn_reflns_av_R_equivalents 0.067
_diffrn_reflns_av_sigmaI/netI 0.056
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_k_min -45
_diffrn_reflns_limit_k_max 45
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 2.61
_diffrn_reflns_theta_max 27.50
_reflns_number_total 7841
_reflns_number_gt 5365
_reflns_threshold_expression >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 Cameron
_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^ > 2\s(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^)+(0.0734P)^2^+21.1824P] 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 7841
_refine_ls_number_parameters 343
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0899
_refine_ls_R_factor_gt 0.0615
_refine_ls_wR_factor_ref 0.1788
_refine_ls_wR_factor_gt 0.1605
_refine_ls_goodness_of_fit_ref 1.115
_refine_ls_restrained_S_all 1.115
_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
Ti1 Ti 0.407096(14) 0.910009(14) 0.10946(5) 0.03443(17) Uani 1 1 d . . .
Cl2 Cl 0.42137(2) 0.86030(2) 0.25231(8) 0.0500(2) Uani 1 1 d . . .
Cl1 Cl 0.37271(2) 0.87077(2) -0.01702(8) 0.0527(2) Uani 1 1 d . . .
Cl3 Cl 0.39693(2) 0.96471(2) -0.00923(7) 0.0455(2) Uani 1 1 d . . .
N2 N 0.48021(6) 0.87047(6) -0.02917(19) 0.0327(5) Uani 1 1 d . . .
N1 N 0.49334(6) 0.90550(6) 0.12209(19) 0.0311(5) Uani 1 1 d . . .
N3 N 0.45098(6) 0.94451(6) 0.2147(2) 0.0324(5) Uani 1 1 d . . .
C14 C 0.46140(8) 0.85199(8) -0.1283(2) 0.0348(6) Uani 1 1 d . . .
O1 O 0.35797(6) 0.92382(6) 0.2146(2) 0.0475(5) Uani 1 1 d . . .
C6 C 0.43740(8) 0.97871(8) 0.2737(3) 0.0374(6) Uani 1 1 d . . .
C3 C 0.51866(8) 0.86467(8) -0.0040(3) 0.0365(6) Uani 1 1 d . . .
H2 H 0.5354 0.8489 -0.0455 0.044 Uiso 1 1 calc R . .
C5 C 0.52015(8) 0.94429(9) 0.2913(3) 0.0405(7) Uani 1 1 d . . .
C4 C 0.48602(8) 0.93380(7) 0.2110(2) 0.0321(6) Uani 1 1 d . . .
C11 C 0.41690(9) 0.97596(10) 0.3797(3) 0.0454(7) Uani 1 1 d . . .
C12 C 0.46779(10) 1.01745(9) 0.1080(3) 0.0496(8) Uani 1 1 d . . .
H25A H 0.4943 1.0169 0.1306 0.074 Uiso 1 1 calc R . .
H25B H 0.4622 1.0412 0.0686 0.074 Uiso 1 1 calc R . .
H25C H 0.4626 0.9965 0.0553 0.074 Uiso 1 1 calc R . .
C2 C 0.52726(8) 0.88608(8) 0.0917(2) 0.0359(6) Uani 1 1 d . . .
H3 H 0.5508 0.8877 0.1299 0.043 Uiso 1 1 calc R . .
C19 C 0.45349(9) 0.81314(9) -0.1188(3) 0.0398(7) Uani 1 1 d . . .
C24 C 0.52925(9) 0.90762(10) 0.3624(3) 0.0446(7) Uani 1 1 d . . .
H6A H 0.5498 0.9127 0.4167 0.067 Uiso 1 1 calc R . .
H6B H 0.5367 0.8876 0.3088 0.067 Uiso 1 1 calc R . .
H6C H 0.5069 0.8998 0.4058 0.067 Uiso 1 1 calc R . .
C18 C 0.43763(10) 0.79540(9) -0.2188(3) 0.0495(8) Uani 1 1 d . . .
H11 H 0.4326 0.7693 -0.2161 0.059 Uiso 1 1 calc R . .
C17 C 0.42913(10) 0.81532(10) -0.3211(3) 0.0516(8) Uani 1 1 d . . .
C15 C 0.45355(9) 0.87331(9) -0.2283(3) 0.0403(6) Uani 1 1 d . . .
C7 C 0.44317(9) 1.01389(9) 0.2167(3) 0.0449(7) Uani 1 1 d . . .
C25 C 0.51068(10) 0.97507(10) 0.3838(3) 0.0511(9) Uani 1 1 d . . .
H8A H 0.4905 0.9661 0.4345 0.077 Uiso 1 1 calc R . .
H8B H 0.5026 0.9980 0.3443 0.077 Uiso 1 1 calc R . .
H8C H 0.5330 0.9804 0.4305 0.077 Uiso 1 1 calc R . .
C8 C 0.42675(10) 1.04650(10) 0.2661(4) 0.0551(9) Uani 1 1 d . . .
H22 H 0.4300 1.0701 0.2292 0.066 Uiso 1 1 calc R . .
C23 C 0.55509(8) 0.95956(9) 0.2213(3) 0.0443(7) Uani 1 1 d . . .
H7A H 0.5500 0.9852 0.1948 0.066 Uiso 1 1 calc R . .
H7B H 0.5597 0.9434 0.1540 0.066 Uiso 1 1 calc R . .
H7C H 0.5772 0.9596 0.2717 0.066 Uiso 1 1 calc R . .
C1 C 0.46419(8) 0.89497(8) 0.0471(2) 0.0329(6) Uani 1 1 d . . .
C10 C 0.40114(10) 1.00940(12) 0.4257(3) 0.0608(10) Uani 1 1 d . . .
H20 H 0.3872 1.0083 0.4959 0.073 Uiso 1 1 calc R . .
C13 C 0.41324(11) 0.93871(12) 0.4458(3) 0.0604(9) Uani 1 1 d . . .
H24A H 0.4139 0.9436 0.5296 0.091 Uiso 1 1 calc R . .
H24B H 0.4341 0.9221 0.4246 0.091 Uiso 1 1 calc R . .
H24C H 0.3894 0.9267 0.4254 0.091 Uiso 1 1 calc R . .
C9 C 0.40570(11) 1.04403(12) 0.3696(4) 0.0661(12) Uani 1 1 d . . .
H21 H 0.3946 1.0659 0.4015 0.079 Uiso 1 1 calc R . .
C22 C 0.46035(11) 0.79097(9) -0.0069(3) 0.0508(8) Uani 1 1 d . . .
H15A H 0.4491 0.7660 -0.0141 0.076 Uiso 1 1 calc R . .
H15B H 0.4489 0.8042 0.0587 0.076 Uiso 1 1 calc R . .
H15C H 0.4874 0.7885 0.0062 0.076 Uiso 1 1 calc R . .
C20 C 0.46275(11) 0.91530(10) -0.2377(3) 0.0529(8) Uani 1 1 d . . .
H17A H 0.4462 0.9295 -0.1859 0.079 Uiso 1 1 calc R . .
H17B H 0.4590 0.9237 -0.3179 0.079 Uiso 1 1 calc R . .
H17C H 0.4889 0.9195 -0.2153 0.079 Uiso 1 1 calc R . .
C26 C 0.33267(12) 0.89439(12) 0.2617(5) 0.0767(14) Uani 1 1 d . . .
H26A H 0.3466 0.8777 0.3154 0.092 Uiso 1 1 calc R . .
H26B H 0.3223 0.8790 0.1977 0.092 Uiso 1 1 calc R . .
C16 C 0.43698(10) 0.85434(10) -0.3246(3) 0.0471(7) Uani 1 1 d . . .
H13 H 0.4311 0.8682 -0.3927 0.057 Uiso 1 1 calc R . .
C29 C 0.33710(9) 0.95972(10) 0.2143(3) 0.0519(8) Uani 1 1 d . . .
H29A H 0.3241 0.9635 0.1392 0.062 Uiso 1 1 calc R . .
H29B H 0.3543 0.9811 0.2279 0.062 Uiso 1 1 calc R . .
C21 C 0.41180(15) 0.79566(14) -0.4282(4) 0.0826(14) Uani 1 1 d . . .
H16A H 0.4045 0.8146 -0.4857 0.124 Uiso 1 1 calc R . .
H16B H 0.3896 0.7814 -0.4042 0.124 Uiso 1 1 calc R . .
H16C H 0.4303 0.7786 -0.4624 0.124 Uiso 1 1 calc R . .
C28 C 0.30866(14) 0.95628(14) 0.3136(5) 0.0896(16) Uani 1 1 d . . .
H28A H 0.3190 0.9667 0.3866 0.108 Uiso 1 1 calc R . .
H28B H 0.2851 0.9697 0.2945 0.108 Uiso 1 1 calc R . .
C27 C 0.30166(13) 0.91431(14) 0.3250(5) 0.0913(16) Uani 1 1 d . . .
H27A H 0.3015 0.9069 0.4079 0.110 Uiso 1 1 calc R . .
H27B H 0.2771 0.9077 0.2908 0.110 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 0.0303(3) 0.0282(3) 0.0448(3) 0.0005(2) 0.0001(2) -0.00059(18)
Cl2 0.0556(5) 0.0348(4) 0.0597(5) 0.0111(3) 0.0053(4) 0.0043(3)
Cl1 0.0470(5) 0.0417(4) 0.0695(6) -0.0095(4) -0.0072(4) -0.0094(3)
Cl3 0.0475(4) 0.0376(4) 0.0515(4) 0.0078(3) -0.0080(3) -0.0027(3)
N2 0.0345(12) 0.0329(12) 0.0307(11) -0.0071(9) -0.0017(9) 0.0045(9)
N1 0.0286(11) 0.0342(11) 0.0305(11) -0.0087(9) -0.0022(9) 0.0046(9)
N3 0.0324(11) 0.0304(11) 0.0343(12) -0.0013(9) -0.0009(9) 0.0029(9)
C14 0.0368(14) 0.0314(13) 0.0361(14) -0.0098(11) -0.0040(11) 0.0017(11)
O1 0.0352(11) 0.0378(11) 0.0694(15) 0.0068(10) 0.0136(10) 0.0014(8)
C6 0.0337(14) 0.0356(14) 0.0429(15) -0.0087(12) -0.0044(12) 0.0082(11)
C3 0.0372(14) 0.0367(14) 0.0355(14) -0.0063(11) -0.0019(11) 0.0050(11)
C5 0.0391(15) 0.0480(17) 0.0344(14) -0.0095(12) -0.0056(12) 0.0052(12)
C4 0.0348(14) 0.0314(13) 0.0300(13) -0.0033(10) -0.0015(10) -0.0016(10)
C11 0.0416(16) 0.0552(19) 0.0393(16) -0.0123(14) -0.0002(13) 0.0109(14)
C12 0.059(2) 0.0381(16) 0.0513(19) 0.0014(14) -0.0101(15) -0.0094(14)
C2 0.0276(13) 0.0441(15) 0.0358(14) -0.0060(12) -0.0018(11) 0.0050(11)
C19 0.0403(15) 0.0374(15) 0.0417(16) -0.0108(12) -0.0023(12) 0.0062(12)
C24 0.0429(16) 0.0553(19) 0.0355(15) -0.0052(13) -0.0023(12) 0.0110(14)
C18 0.058(2) 0.0336(15) 0.057(2) -0.0091(14) -0.0043(16) -0.0042(13)
C17 0.060(2) 0.0543(19) 0.0405(17) -0.0132(15) -0.0100(15) -0.0049(16)
C15 0.0432(16) 0.0381(15) 0.0396(15) -0.0035(12) -0.0064(13) -0.0014(12)
C7 0.0489(17) 0.0332(14) 0.0527(18) -0.0109(13) -0.0150(14) 0.0078(12)
C25 0.0440(17) 0.064(2) 0.0458(18) -0.0278(16) -0.0141(14) 0.0121(15)
C8 0.057(2) 0.0361(16) 0.072(2) -0.0111(16) -0.0194(18) 0.0114(14)
C23 0.0350(15) 0.0483(17) 0.0494(17) -0.0115(14) -0.0071(13) -0.0047(12)
C1 0.0341(14) 0.0325(13) 0.0321(13) -0.0008(10) -0.0016(11) -0.0014(11)
C10 0.0469(19) 0.085(3) 0.050(2) -0.023(2) -0.0012(16) 0.0237(18)
C13 0.056(2) 0.080(3) 0.0454(19) 0.0053(18) 0.0094(16) 0.0109(19)
C9 0.057(2) 0.060(2) 0.082(3) -0.032(2) -0.017(2) 0.0273(18)
C22 0.070(2) 0.0346(16) 0.0476(18) 0.0007(13) -0.0031(16) 0.0034(15)
C20 0.074(2) 0.0440(18) 0.0405(17) 0.0009(14) -0.0088(16) -0.0160(16)
C26 0.063(2) 0.052(2) 0.115(4) 0.015(2) 0.045(2) -0.0109(18)
C16 0.0564(19) 0.0482(18) 0.0368(15) -0.0013(13) -0.0097(14) 0.0007(14)
C29 0.0403(17) 0.0450(18) 0.070(2) 0.0018(16) 0.0066(16) 0.0092(13)
C21 0.107(4) 0.076(3) 0.065(3) -0.022(2) -0.030(3) -0.016(3)
C28 0.077(3) 0.082(3) 0.110(4) 0.007(3) 0.033(3) 0.024(3)
C27 0.057(3) 0.089(3) 0.127(4) 0.005(3) 0.034(3) -0.013(2)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 2.141(2) . ?
Ti1 C1 2.178(3) . ?
Ti1 N3 2.282(2) . ?
Ti1 Cl1 2.3139(9) . ?
Ti1 Cl3 2.3595(9) . ?
Ti1 Cl2 2.4202(9) . ?
N2 C1 1.336(3) . ?
N2 C3 1.388(4) . ?
N2 C14 1.448(3) . ?
N1 C1 1.374(3) . ?
N1 C2 1.407(3) . ?
N1 C4 1.431(3) . ?
N3 C4 1.280(3) . ?
N3 C6 1.447(3) . ?
C14 C15 1.379(4) . ?
C14 C19 1.389(4) . ?
O1 C29 1.450(4) . ?
O1 C26 1.455(4) . ?
C6 C11 1.397(4) . ?
C6 C7 1.401(5) . ?
C3 C2 1.347(4) . ?
C5 C25 1.534(4) . ?
C5 C4 1.541(4) . ?
C5 C24 1.544(4) . ?
C5 C23 1.548(4) . ?
C11 C10 1.391(5) . ?
C11 C13 1.505(5) . ?
C12 C7 1.503(5) . ?
C19 C18 1.401(4) . ?
C19 C22 1.499(4) . ?
C18 C17 1.380(5) . ?
C17 C16 1.391(5) . ?
C17 C21 1.515(5) . ?
C15 C16 1.398(4) . ?
C15 C20 1.505(4) . ?
C7 C8 1.391(4) . ?
C8 C9 1.383(6) . ?
C10 C9 1.374(6) . ?
C26 C27 1.472(6) . ?
C29 C28 1.501(6) . ?
C28 C27 1.491(7) . ?
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 Ti1 C1 165.15(10) . . ?
O1 Ti1 N3 97.52(9) . . ?
C1 Ti1 N3 71.37(9) . . ?
O1 Ti1 Cl1 93.40(7) . . ?
C1 Ti1 Cl1 97.65(8) . . ?
N3 Ti1 Cl1 169.00(7) . . ?
O1 Ti1 Cl3 90.65(6) . . ?
C1 Ti1 Cl3 98.61(8) . . ?
N3 Ti1 Cl3 88.21(6) . . ?
Cl1 Ti1 Cl3 92.96(3) . . ?
O1 Ti1 Cl2 87.58(7) . . ?
C1 Ti1 Cl2 81.58(7) . . ?
N3 Ti1 Cl2 83.92(6) . . ?
Cl1 Ti1 Cl2 95.31(4) . . ?
Cl3 Ti1 Cl2 171.63(4) . . ?
C1 N2 C3 111.5(2) . . ?
C1 N2 C14 126.3(2) . . ?
C3 N2 C14 122.1(2) . . ?
C1 N1 C2 110.2(2) . . ?
C1 N1 C4 118.9(2) . . ?
C2 N1 C4 130.8(2) . . ?
C4 N3 C6 124.7(2) . . ?
C4 N3 Ti1 118.07(18) . . ?
C6 N3 Ti1 117.04(17) . . ?
C15 C14 C19 123.4(3) . . ?
C15 C14 N2 118.8(2) . . ?
C19 C14 N2 117.8(3) . . ?
C29 O1 C26 107.8(3) . . ?
C29 O1 Ti1 126.60(19) . . ?
C26 O1 Ti1 122.0(2) . . ?
C11 C6 C7 121.8(3) . . ?
C11 C6 N3 120.3(3) . . ?
C7 C6 N3 117.7(3) . . ?
C2 C3 N2 107.4(2) . . ?
C25 C5 C4 113.6(2) . . ?
C25 C5 C24 105.8(3) . . ?
C4 C5 C24 105.5(2) . . ?
C25 C5 C23 106.0(3) . . ?
C4 C5 C23 113.0(2) . . ?
C24 C5 C23 112.8(3) . . ?
N3 C4 N1 113.3(2) . . ?
N3 C4 C5 130.6(2) . . ?
N1 C4 C5 116.0(2) . . ?
C10 C11 C6 117.6(3) . . ?
C10 C11 C13 120.5(3) . . ?
C6 C11 C13 121.8(3) . . ?
C3 C2 N1 106.0(2) . . ?
C14 C19 C18 116.6(3) . . ?
C14 C19 C22 122.5(3) . . ?
C18 C19 C22 120.8(3) . . ?
C17 C18 C19 122.4(3) . . ?
C18 C17 C16 118.4(3) . . ?
C18 C17 C21 121.6(3) . . ?
C16 C17 C21 120.0(3) . . ?
C14 C15 C16 117.5(3) . . ?
C14 C15 C20 122.8(3) . . ?
C16 C15 C20 119.7(3) . . ?
C8 C7 C6 118.4(3) . . ?
C8 C7 C12 119.6(3) . . ?
C6 C7 C12 122.0(3) . . ?
C9 C8 C7 120.4(4) . . ?
N2 C1 N1 104.9(2) . . ?
N2 C1 Ti1 138.2(2) . . ?
N1 C1 Ti1 114.52(18) . . ?
C9 C10 C11 121.5(4) . . ?
C10 C9 C8 120.3(3) . . ?
O1 C26 C27 106.8(3) . . ?
C17 C16 C15 121.6(3) . . ?
O1 C29 C28 105.2(3) . . ?
C27 C28 C29 104.6(4) . . ?
C26 C27 C28 107.6(3) . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 0.475
_refine_diff_density_min -0.425
_refine_diff_density_rms 0.075
_vrf_PLAT601_k10226
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of 522.00 A**3
RESPONSE:
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly dichloromethane). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 522 \%A^3^ containing approximately 100
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by Staehler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
Staehler, R., Naether, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.125 22 2 ' '
2 0.000 0.750 0.875 22 2 ' '
3 0.250 0.000 0.192 535 105 ' '
4 0.250 0.500 0.802 535 105 ' '
5 0.500 0.250 0.375 22 2 ' '
6 0.500 0.750 0.625 22 2 ' '
7 0.750 0.000 0.302 535 105 ' '
8 0.750 0.500 0.692 535 105 ' '
_platon_squeeze_details
;
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly dichloromethane). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 522 \%A^3^ containing approximately 100
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by Staehler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
Staehler, R., Naether, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
#
data_edwin_0m
_database_code_depnum_ccdc_archive 'CCDC 840139'
#TrackingRef 'Combined_CIF.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C29 H39 Cl3 Cr N3 O, C H2 Cl2'
_chemical_formula_sum 'C30 H41 Cl5 Cr N3 O'
_chemical_formula_weight 688.91
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'
Cr Cr 0.3209 0.6236 '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'
_symmetry_cell_setting Tetragonal
_symmetry_space_group_name_H-M I4(1)/a
_symmetry_space_group_name_Hall '-I 4ad'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
_cell_length_a 34.553(6)
_cell_length_b 34.553
_cell_length_c 11.316(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 13510(3)
_cell_formula_units_Z 16
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9080
_cell_measurement_theta_min 2.36
_cell_measurement_theta_max 26.25
_exptl_crystal_description block
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.349
_exptl_crystal_size_mid 0.101
_exptl_crystal_size_min 0.083
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.355
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5744
_exptl_absorpt_coefficient_mu 0.762
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.8123
_exptl_absorpt_correction_T_max 0.9759
_exptl_absorpt_process_details SADABS
_exptl_special_details
;
?
;
_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 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 62831
_diffrn_reflns_av_R_equivalents 0.1289
_diffrn_reflns_av_sigmaI/netI 0.0635
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_h_max 41
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_k_max 33
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 1.89
_diffrn_reflns_theta_max 24.99
_reflns_number_total 5953
_reflns_number_gt 4225
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX 2 v2010.3'
_computing_cell_refinement 'SAINT V7.46A (Bruker AXS, 2007)'
_computing_data_reduction 'SAINT V7.46A (Bruker AXS, 2007)'
_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^)+(0.0405P)^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 refall
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5953
_refine_ls_number_parameters 378
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.0942
_refine_ls_R_factor_gt 0.0595
_refine_ls_wR_factor_ref 0.1291
_refine_ls_wR_factor_gt 0.1178
_refine_ls_goodness_of_fit_ref 1.372
_refine_ls_restrained_S_all 1.372
_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
Cr1 Cr 0.089095(18) 0.089948(18) 0.11743(6) 0.01943(18) Uani 1 1 d . . .
Cl2 Cl 0.07575(3) 0.14043(3) 0.25181(10) 0.0286(3) Uani 1 1 d . . .
Cl1 Cl 0.12629(3) 0.12950(3) 0.00053(11) 0.0287(3) Uani 1 1 d . . .
Cl3 Cl 0.09789(3) 0.03866(3) -0.00912(10) 0.0248(3) Uani 1 1 d . . .
O1 O 0.13777(8) 0.07471(8) 0.2184(3) 0.0299(8) Uani 1 1 d . . .
N1 N 0.00583(9) 0.09424(9) 0.1212(3) 0.0174(7) Uani 1 1 d . . .
N2 N 0.02124(9) 0.13038(9) -0.0275(3) 0.0168(7) Uani 1 1 d . . .
N3 N 0.04818(10) 0.05552(9) 0.2156(3) 0.0195(8) Uani 1 1 d . . .
C1 C 0.03643(11) 0.10518(11) 0.0503(4) 0.0163(9) Uani 1 1 d . . .
C2 C -0.02798(11) 0.11401(11) 0.0868(4) 0.0200(9) Uani 1 1 d . . .
H2 H -0.0528 0.1122 0.1224 0.024 Uiso 1 1 calc R . .
C3 C -0.01815(11) 0.13596(11) -0.0060(4) 0.0191(9) Uani 1 1 d . . .
H3 H -0.0350 0.1524 -0.0495 0.023 Uiso 1 1 calc R . .
C4 C 0.01242(11) 0.06578(11) 0.2100(4) 0.0171(9) Uani 1 1 d . . .
C5 C -0.02194(12) 0.05476(12) 0.2888(4) 0.0227(10) Uani 1 1 d . . .
C24 C -0.03136(13) 0.09205(12) 0.3602(4) 0.0264(10) Uani 1 1 d . . .
H6A H -0.0085 0.0999 0.4055 0.040 Uiso 1 1 calc R . .
H6B H -0.0529 0.0869 0.4144 0.040 Uiso 1 1 calc R . .
H6C H -0.0386 0.1128 0.3056 0.040 Uiso 1 1 calc R . .
C23 C -0.05707(12) 0.03948(12) 0.2181(4) 0.0271(11) Uani 1 1 d . . .
H7A H -0.0625 0.0570 0.1521 0.041 Uiso 1 1 calc R . .
H7B H -0.0797 0.0381 0.2700 0.041 Uiso 1 1 calc R . .
H7C H -0.0512 0.0136 0.1874 0.041 Uiso 1 1 calc R . .
C25 C -0.01243(13) 0.02375(13) 0.3817(4) 0.0328(11) Uani 1 1 d . . .
H8A H -0.0048 -0.0003 0.3419 0.049 Uiso 1 1 calc R . .
H8B H -0.0353 0.0189 0.4307 0.049 Uiso 1 1 calc R . .
H8C H 0.0089 0.0328 0.4317 0.049 Uiso 1 1 calc R . .
C14 C 0.04079(11) 0.14911(11) -0.1258(4) 0.0176(9) Uani 1 1 d . . .
C19 C 0.04883(11) 0.18872(11) -0.1162(4) 0.0210(9) Uani 1 1 d . . .
C18 C 0.06460(12) 0.20675(12) -0.2147(4) 0.0277(11) Uani 1 1 d . . .
H11 H 0.0699 0.2337 -0.2114 0.033 Uiso 1 1 calc R . .
C17 C 0.07296(13) 0.18653(12) -0.3184(4) 0.0271(10) Uani 1 1 d . . .
C16 C 0.06485(12) 0.14723(13) -0.3227(4) 0.0280(10) Uani 1 1 d . . .
H13 H 0.0707 0.1331 -0.3925 0.034 Uiso 1 1 calc R . .
C15 C 0.04826(12) 0.12782(11) -0.2265(4) 0.0216(9) Uani 1 1 d . . .
C22 C 0.04117(13) 0.21062(12) -0.0029(4) 0.0273(10) Uani 1 1 d . . .
H15A H 0.0531 0.2363 -0.0077 0.041 Uiso 1 1 calc R . .
H15B H 0.0523 0.1963 0.0638 0.041 Uiso 1 1 calc R . .
H15C H 0.0132 0.2134 0.0085 0.041 Uiso 1 1 calc R . .
C21 C 0.09004(16) 0.20687(15) -0.4242(5) 0.0435(14) Uani 1 1 d . . .
H16A H 0.1162 0.2159 -0.4051 0.065 Uiso 1 1 calc R . .
H16B H 0.0738 0.2291 -0.4453 0.065 Uiso 1 1 calc R . .
H16C H 0.0913 0.1889 -0.4910 0.065 Uiso 1 1 calc R . .
C20 C 0.03811(14) 0.08557(12) -0.2372(4) 0.0303(11) Uani 1 1 d . . .
H17A H 0.0548 0.0704 -0.1848 0.045 Uiso 1 1 calc R . .
H17B H 0.0419 0.0771 -0.3190 0.045 Uiso 1 1 calc R . .
H17C H 0.0110 0.0817 -0.2146 0.045 Uiso 1 1 calc R . .
C6 C 0.06244(12) 0.02092(12) 0.2744(4) 0.0245(10) Uani 1 1 d . . .
C11 C 0.08337(12) 0.02377(13) 0.3793(4) 0.0303(11) Uani 1 1 d . . .
C10 C 0.09992(14) -0.00996(16) 0.4251(5) 0.0417(13) Uani 1 1 d . . .
H20 H 0.1144 -0.0087 0.4962 0.050 Uiso 1 1 calc R . .
C9 C 0.09548(14) -0.04508(15) 0.3683(5) 0.0458(15) Uani 1 1 d . . .
H21 H 0.1072 -0.0677 0.4000 0.055 Uiso 1 1 calc R . .
C8 C 0.07413(14) -0.04741(13) 0.2659(5) 0.0380(13) Uani 1 1 d . . .
H22 H 0.0712 -0.0718 0.2281 0.046 Uiso 1 1 calc R . .
C7 C 0.05667(12) -0.01474(12) 0.2164(4) 0.0275(11) Uani 1 1 d . . .
C13 C 0.08621(15) 0.06096(15) 0.4474(5) 0.0433(13) Uani 1 1 d . . .
H24A H 0.1120 0.0632 0.4824 0.065 Uiso 1 1 calc R . .
H24B H 0.0667 0.0612 0.5102 0.065 Uiso 1 1 calc R . .
H24C H 0.0817 0.0828 0.3939 0.065 Uiso 1 1 calc R . .
C12 C 0.03147(13) -0.01857(12) 0.1094(4) 0.0314(11) Uani 1 1 d . . .
H25A H 0.0364 -0.0436 0.0713 0.047 Uiso 1 1 calc R . .
H25B H 0.0373 0.0024 0.0539 0.047 Uiso 1 1 calc R . .
H25C H 0.0042 -0.0170 0.1330 0.047 Uiso 1 1 calc R . .
C26 C 0.16059(13) 0.03969(13) 0.2009(5) 0.0354(12) Uani 1 1 d . . .
H26A H 0.1735 0.0400 0.1228 0.043 Uiso 1 1 calc R . .
H26B H 0.1441 0.0163 0.2064 0.043 Uiso 1 1 calc R . .
C27 C 0.19014(16) 0.04056(16) 0.3003(6) 0.0578(17) Uani 1 1 d . . .
H27A H 0.1793 0.0297 0.3742 0.069 Uiso 1 1 calc R . .
H27B H 0.2139 0.0262 0.2787 0.069 Uiso 1 1 calc R . .
C28 C 0.19813(16) 0.08372(17) 0.3124(7) 0.068(2) Uani 1 1 d . . .
H28A H 0.2031 0.0904 0.3961 0.082 Uiso 1 1 calc R . .
H28B H 0.2211 0.0910 0.2652 0.082 Uiso 1 1 calc R . .
C29 C 0.16361(16) 0.10416(14) 0.2688(6) 0.0588(19) Uani 1 1 d . . .
H29A H 0.1506 0.1179 0.3345 0.071 Uiso 1 1 calc R . .
H29B H 0.1709 0.1233 0.2078 0.071 Uiso 1 1 calc R . .
C30 C 0.1995(3) 0.9208(3) 0.5520(11) 0.077(3) Uani 0.731(4) 1 d PU A 1
H30A H 0.1782 0.9062 0.5902 0.093 Uiso 0.731(4) 1 calc PR A 1
H30B H 0.2241 0.9072 0.5682 0.093 Uiso 0.731(4) 1 calc PR A 1
Cl4 Cl 0.19154(9) 0.92333(12) 0.3991(3) 0.0865(10) Uani 0.731(4) 1 d P A 1
Cl5 Cl 0.20129(14) 0.96697(10) 0.6083(3) 0.1087(12) Uani 0.731(4) 1 d P A 1
C30A C 0.1819(10) 0.9270(11) 0.571(3) 0.077(3) Uani 0.269(4) 1 d PU A 2
H30C H 0.1759 0.9085 0.6347 0.093 Uiso 0.269(4) 1 calc PR A 2
H30D H 0.1594 0.9445 0.5609 0.093 Uiso 0.269(4) 1 calc PR A 2
Cl4A Cl 0.1900(3) 0.9017(3) 0.4385(9) 0.0865(10) Uani 0.269(4) 1 d P A 2
Cl5A Cl 0.2274(4) 0.9570(3) 0.6126(10) 0.1087(12) Uani 0.269(4) 1 d P A 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
Cr1 0.0189(3) 0.0152(3) 0.0242(4) -0.0025(3) -0.0026(3) 0.0010(3)
Cl2 0.0363(6) 0.0185(5) 0.0309(7) -0.0066(5) -0.0052(5) 0.0037(4)
Cl1 0.0236(5) 0.0210(5) 0.0414(7) -0.0003(5) 0.0039(5) -0.0045(4)
Cl3 0.0253(5) 0.0206(5) 0.0284(6) -0.0056(5) 0.0027(5) -0.0013(4)
O1 0.0279(16) 0.0209(15) 0.041(2) -0.0057(14) -0.0118(15) 0.0014(13)
N1 0.0207(17) 0.0173(17) 0.0142(19) 0.0063(15) 0.0006(15) -0.0002(14)
N2 0.0180(17) 0.0166(17) 0.0158(19) 0.0036(14) -0.0006(14) 0.0013(13)
N3 0.0261(19) 0.0180(17) 0.0145(19) 0.0000(14) -0.0009(15) 0.0043(15)
C1 0.021(2) 0.016(2) 0.012(2) -0.0036(17) 0.0046(17) -0.0040(16)
C2 0.017(2) 0.024(2) 0.020(2) 0.0018(18) 0.0010(17) 0.0025(17)
C3 0.0159(19) 0.024(2) 0.018(2) 0.0024(18) 0.0024(18) 0.0025(16)
C4 0.025(2) 0.0121(19) 0.014(2) 0.0000(16) -0.0010(17) 0.0021(17)
C5 0.028(2) 0.028(2) 0.013(2) 0.0069(18) 0.0052(18) 0.0051(18)
C24 0.032(2) 0.032(2) 0.015(2) 0.005(2) 0.0028(19) 0.0108(19)
C23 0.027(2) 0.022(2) 0.033(3) 0.005(2) 0.009(2) -0.0019(18)
C25 0.036(3) 0.036(3) 0.027(3) 0.014(2) 0.011(2) 0.011(2)
C14 0.0148(19) 0.020(2) 0.019(2) 0.0067(18) 0.0030(17) 0.0002(16)
C19 0.017(2) 0.024(2) 0.022(2) 0.0062(19) 0.0021(18) 0.0041(17)
C18 0.029(2) 0.018(2) 0.036(3) 0.006(2) 0.005(2) -0.0004(18)
C17 0.029(2) 0.027(2) 0.026(3) 0.008(2) 0.008(2) 0.0005(19)
C16 0.031(2) 0.031(3) 0.022(3) -0.001(2) 0.005(2) 0.001(2)
C15 0.024(2) 0.020(2) 0.021(2) -0.0012(18) 0.0033(19) -0.0005(17)
C22 0.034(2) 0.023(2) 0.026(3) -0.001(2) 0.002(2) 0.0034(19)
C21 0.057(3) 0.039(3) 0.034(3) 0.013(2) 0.020(3) -0.002(3)
C20 0.046(3) 0.024(2) 0.021(3) -0.002(2) 0.004(2) -0.009(2)
C6 0.026(2) 0.025(2) 0.022(3) 0.0100(19) 0.0033(19) 0.0072(18)
C11 0.025(2) 0.041(3) 0.025(3) 0.008(2) 0.004(2) 0.010(2)
C10 0.038(3) 0.056(4) 0.031(3) 0.023(3) 0.001(2) 0.017(3)
C9 0.039(3) 0.043(3) 0.056(4) 0.030(3) 0.021(3) 0.021(2)
C8 0.040(3) 0.025(2) 0.049(4) 0.013(2) 0.021(3) 0.013(2)
C7 0.028(2) 0.023(2) 0.032(3) 0.008(2) 0.013(2) 0.0022(18)
C13 0.048(3) 0.058(3) 0.024(3) -0.004(3) -0.007(2) 0.009(3)
C12 0.040(3) 0.021(2) 0.034(3) 0.000(2) 0.008(2) -0.008(2)
C26 0.026(2) 0.032(3) 0.048(3) -0.001(2) -0.005(2) 0.012(2)
C27 0.046(3) 0.053(4) 0.074(5) -0.006(3) -0.029(3) 0.018(3)
C28 0.032(3) 0.064(4) 0.109(6) -0.030(4) -0.024(3) 0.002(3)
C29 0.049(3) 0.030(3) 0.097(5) -0.012(3) -0.046(3) -0.007(2)
C30 0.092(7) 0.073(5) 0.067(5) 0.013(4) -0.006(5) -0.001(5)
Cl4 0.0766(15) 0.121(3) 0.062(2) -0.0131(18) 0.0031(15) -0.009(2)
Cl5 0.145(4) 0.075(2) 0.107(2) -0.0268(17) 0.001(3) 0.007(2)
C30A 0.092(7) 0.073(5) 0.067(5) 0.013(4) -0.006(5) -0.001(5)
Cl4A 0.0766(15) 0.121(3) 0.062(2) -0.0131(18) 0.0031(15) -0.009(2)
Cl5A 0.145(4) 0.075(2) 0.107(2) -0.0268(17) 0.001(3) 0.007(2)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Cr1 C1 2.041(4) . ?
Cr1 O1 2.100(3) . ?
Cr1 N3 2.156(3) . ?
Cr1 Cl1 2.2954(13) . ?
Cr1 Cl3 2.2985(12) . ?
Cr1 Cl2 2.3596(12) . ?
O1 C26 1.458(5) . ?
O1 C29 1.469(5) . ?
N1 C1 1.380(5) . ?
N1 C2 1.408(5) . ?
N1 C4 1.424(5) . ?
N2 C1 1.345(5) . ?
N2 C3 1.396(5) . ?
N2 C14 1.453(5) . ?
N3 C4 1.287(5) . ?
N3 C6 1.454(5) . ?
C2 C3 1.340(6) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.533(6) . ?
C5 C25 1.537(6) . ?
C5 C23 1.546(6) . ?
C5 C24 1.555(6) . ?
C24 H6A 0.9800 . ?
C24 H6B 0.9800 . ?
C24 H6C 0.9800 . ?
C23 H7A 0.9800 . ?
C23 H7B 0.9800 . ?
C23 H7C 0.9800 . ?
C25 H8A 0.9800 . ?
C25 H8B 0.9800 . ?
C25 H8C 0.9800 . ?
C14 C15 1.381(6) . ?
C14 C19 1.401(5) . ?
C19 C18 1.388(6) . ?
C19 C22 1.512(6) . ?
C18 C17 1.396(6) . ?
C18 H11 0.9500 . ?
C17 C16 1.387(6) . ?
C17 C21 1.508(6) . ?
C16 C15 1.401(6) . ?
C16 H13 0.9500 . ?
C15 C20 1.506(5) . ?
C22 H15A 0.9800 . ?
C22 H15B 0.9800 . ?
C22 H15C 0.9800 . ?
C21 H16A 0.9800 . ?
C21 H16B 0.9800 . ?
C21 H16C 0.9800 . ?
C20 H17A 0.9800 . ?
C20 H17B 0.9800 . ?
C20 H17C 0.9800 . ?
C6 C11 1.394(6) . ?
C6 C7 1.410(6) . ?
C11 C10 1.397(6) . ?
C11 C13 1.501(7) . ?
C10 C9 1.382(8) . ?
C10 H20 0.9500 . ?
C9 C8 1.375(8) . ?
C9 H21 0.9500 . ?
C8 C7 1.397(6) . ?
C8 H22 0.9500 . ?
C7 C12 1.497(7) . ?
C13 H24A 0.9800 . ?
C13 H24B 0.9800 . ?
C13 H24C 0.9800 . ?
C12 H25A 0.9800 . ?
C12 H25B 0.9800 . ?
C12 H25C 0.9800 . ?
C26 C27 1.520(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.523(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.471(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 Cl5 1.718(13) . ?
C30 Cl4 1.754(13) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30A Cl4A 1.75(4) . ?
C30A Cl5A 1.94(4) . ?
C30A H30C 0.9900 . ?
C30A H30D 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 Cr1 O1 168.84(15) . . ?
C1 Cr1 N3 75.50(14) . . ?
O1 Cr1 N3 96.10(13) . . ?
C1 Cr1 Cl1 97.53(11) . . ?
O1 Cr1 Cl1 90.83(9) . . ?
N3 Cr1 Cl1 173.03(10) . . ?
C1 Cr1 Cl3 94.86(11) . . ?
O1 Cr1 Cl3 92.28(9) . . ?
N3 Cr1 Cl3 89.00(9) . . ?
Cl1 Cr1 Cl3 91.48(5) . . ?
C1 Cr1 Cl2 82.82(11) . . ?
O1 Cr1 Cl2 89.50(9) . . ?
N3 Cr1 Cl2 86.99(9) . . ?
Cl1 Cr1 Cl2 92.33(5) . . ?
Cl3 Cr1 Cl2 175.77(5) . . ?
C26 O1 C29 107.4(3) . . ?
C26 O1 Cr1 124.6(3) . . ?
C29 O1 Cr1 121.6(3) . . ?
C1 N1 C2 110.0(3) . . ?
C1 N1 C4 118.5(3) . . ?
C2 N1 C4 131.5(3) . . ?
C1 N2 C3 110.9(3) . . ?
C1 N2 C14 127.4(3) . . ?
C3 N2 C14 121.6(3) . . ?
C4 N3 C6 125.1(3) . . ?
C4 N3 Cr1 116.9(3) . . ?
C6 N3 Cr1 117.8(2) . . ?
N2 C1 N1 105.0(3) . . ?
N2 C1 Cr1 139.3(3) . . ?
N1 C1 Cr1 113.3(3) . . ?
C3 C2 N1 106.3(3) . . ?
C3 C2 H2 126.8 . . ?
N1 C2 H2 126.8 . . ?
C2 C3 N2 107.8(3) . . ?
C2 C3 H3 126.1 . . ?
N2 C3 H3 126.1 . . ?
N3 C4 N1 112.3(3) . . ?
N3 C4 C5 130.3(4) . . ?
N1 C4 C5 117.3(3) . . ?
C4 C5 C25 113.9(3) . . ?
C4 C5 C23 113.1(3) . . ?
C25 C5 C23 106.5(4) . . ?
C4 C5 C24 105.0(3) . . ?
C25 C5 C24 105.5(3) . . ?
C23 C5 C24 112.8(3) . . ?
C5 C24 H6A 109.5 . . ?
C5 C24 H6B 109.5 . . ?
H6A C24 H6B 109.5 . . ?
C5 C24 H6C 109.5 . . ?
H6A C24 H6C 109.5 . . ?
H6B C24 H6C 109.5 . . ?
C5 C23 H7A 109.5 . . ?
C5 C23 H7B 109.5 . . ?
H7A C23 H7B 109.5 . . ?
C5 C23 H7C 109.5 . . ?
H7A C23 H7C 109.5 . . ?
H7B C23 H7C 109.5 . . ?
C5 C25 H8A 109.5 . . ?
C5 C25 H8B 109.5 . . ?
H8A C25 H8B 109.5 . . ?
C5 C25 H8C 109.5 . . ?
H8A C25 H8C 109.5 . . ?
H8B C25 H8C 109.5 . . ?
C15 C14 C19 123.2(4) . . ?
C15 C14 N2 118.8(3) . . ?
C19 C14 N2 117.9(4) . . ?
C18 C19 C14 117.0(4) . . ?
C18 C19 C22 121.6(4) . . ?
C14 C19 C22 121.3(4) . . ?
C19 C18 C17 122.1(4) . . ?
C19 C18 H11 118.9 . . ?
C17 C18 H11 118.9 . . ?
C16 C17 C18 118.5(4) . . ?
C16 C17 C21 120.5(4) . . ?
C18 C17 C21 121.0(4) . . ?
C17 C16 C15 121.6(4) . . ?
C17 C16 H13 119.2 . . ?
C15 C16 H13 119.2 . . ?
C14 C15 C16 117.6(4) . . ?
C14 C15 C20 122.6(4) . . ?
C16 C15 C20 119.8(4) . . ?
C19 C22 H15A 109.5 . . ?
C19 C22 H15B 109.5 . . ?
H15A C22 H15B 109.5 . . ?
C19 C22 H15C 109.5 . . ?
H15A C22 H15C 109.5 . . ?
H15B C22 H15C 109.5 . . ?
C17 C21 H16A 109.5 . . ?
C17 C21 H16B 109.5 . . ?
H16A C21 H16B 109.5 . . ?
C17 C21 H16C 109.5 . . ?
H16A C21 H16C 109.5 . . ?
H16B C21 H16C 109.5 . . ?
C15 C20 H17A 109.5 . . ?
C15 C20 H17B 109.5 . . ?
H17A C20 H17B 109.5 . . ?
C15 C20 H17C 109.5 . . ?
H17A C20 H17C 109.5 . . ?
H17B C20 H17C 109.5 . . ?
C11 C6 C7 122.1(4) . . ?
C11 C6 N3 120.5(4) . . ?
C7 C6 N3 117.3(4) . . ?
C6 C11 C10 118.0(5) . . ?
C6 C11 C13 122.1(4) . . ?
C10 C11 C13 119.8(5) . . ?
C9 C10 C11 121.0(5) . . ?
C9 C10 H20 119.5 . . ?
C11 C10 H20 119.5 . . ?
C8 C9 C10 120.2(5) . . ?
C8 C9 H21 119.9 . . ?
C10 C9 H21 119.9 . . ?
C9 C8 C7 121.5(5) . . ?
C9 C8 H22 119.3 . . ?
C7 C8 H22 119.3 . . ?
C8 C7 C6 117.3(5) . . ?
C8 C7 C12 120.3(4) . . ?
C6 C7 C12 122.4(4) . . ?
C11 C13 H24A 109.5 . . ?
C11 C13 H24B 109.5 . . ?
H24A C13 H24B 109.5 . . ?
C11 C13 H24C 109.5 . . ?
H24A C13 H24C 109.5 . . ?
H24B C13 H24C 109.5 . . ?
C7 C12 H25A 109.5 . . ?
C7 C12 H25B 109.5 . . ?
H25A C12 H25B 109.5 . . ?
C7 C12 H25C 109.5 . . ?
H25A C12 H25C 109.5 . . ?
H25B C12 H25C 109.5 . . ?
O1 C26 C27 104.3(4) . . ?
O1 C26 H26A 110.9 . . ?
C27 C26 H26A 110.9 . . ?
O1 C26 H26B 110.9 . . ?
C27 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
C28 C27 C26 102.0(4) . . ?
C28 C27 H27A 111.4 . . ?
C26 C27 H27A 111.4 . . ?
C28 C27 H27B 111.4 . . ?
C26 C27 H27B 111.4 . . ?
H27A C27 H27B 109.2 . . ?
C29 C28 C27 107.0(4) . . ?
C29 C28 H28A 110.3 . . ?
C27 C28 H28A 110.3 . . ?
C29 C28 H28B 110.3 . . ?
C27 C28 H28B 110.3 . . ?
H28A C28 H28B 108.6 . . ?
O1 C29 C28 106.9(4) . . ?
O1 C29 H29A 110.3 . . ?
C28 C29 H29A 110.3 . . ?
O1 C29 H29B 110.3 . . ?
C28 C29 H29B 110.3 . . ?
H29A C29 H29B 108.6 . . ?
Cl5 C30 Cl4 109.0(7) . . ?
Cl5 C30 H30A 109.9 . . ?
Cl4 C30 H30A 109.9 . . ?
Cl5 C30 H30B 109.9 . . ?
Cl4 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
Cl4A C30A Cl5A 110.3(18) . . ?
Cl4A C30A H30C 109.6 . . ?
Cl5A C30A H30C 109.6 . . ?
Cl4A C30A H30D 109.6 . . ?
Cl5A C30A H30D 109.6 . . ?
H30C C30A H30D 108.1 . . ?
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 Cr1 O1 C26 124.0(7) . . . . ?
N3 Cr1 O1 C26 83.4(3) . . . . ?
Cl1 Cr1 O1 C26 -97.3(3) . . . . ?
Cl3 Cr1 O1 C26 -5.8(3) . . . . ?
Cl2 Cr1 O1 C26 170.4(3) . . . . ?
C1 Cr1 O1 C29 -87.7(8) . . . . ?
N3 Cr1 O1 C29 -128.3(4) . . . . ?
Cl1 Cr1 O1 C29 51.0(4) . . . . ?
Cl3 Cr1 O1 C29 142.5(4) . . . . ?
Cl2 Cr1 O1 C29 -41.4(4) . . . . ?
C1 Cr1 N3 C4 -15.5(3) . . . . ?
O1 Cr1 N3 C4 157.0(3) . . . . ?
Cl1 Cr1 N3 C4 -16.8(10) . . . . ?
Cl3 Cr1 N3 C4 -110.8(3) . . . . ?
Cl2 Cr1 N3 C4 67.9(3) . . . . ?
C1 Cr1 N3 C6 159.4(3) . . . . ?
O1 Cr1 N3 C6 -28.0(3) . . . . ?
Cl1 Cr1 N3 C6 158.2(7) . . . . ?
Cl3 Cr1 N3 C6 64.1(3) . . . . ?
Cl2 Cr1 N3 C6 -117.2(3) . . . . ?
C3 N2 C1 N1 0.9(4) . . . . ?
C14 N2 C1 N1 -176.6(3) . . . . ?
C3 N2 C1 Cr1 -159.4(4) . . . . ?
C14 N2 C1 Cr1 23.1(7) . . . . ?
C2 N1 C1 N2 -1.5(4) . . . . ?
C4 N1 C1 N2 176.9(3) . . . . ?
C2 N1 C1 Cr1 164.7(3) . . . . ?
C4 N1 C1 Cr1 -17.0(4) . . . . ?
O1 Cr1 C1 N2 133.4(6) . . . . ?
N3 Cr1 C1 N2 175.4(5) . . . . ?
Cl1 Cr1 C1 N2 -4.8(4) . . . . ?
Cl3 Cr1 C1 N2 -96.9(4) . . . . ?
Cl2 Cr1 C1 N2 86.6(4) . . . . ?
O1 Cr1 C1 N1 -25.8(9) . . . . ?
N3 Cr1 C1 N1 16.1(3) . . . . ?
Cl1 Cr1 C1 N1 -164.0(2) . . . . ?
Cl3 Cr1 C1 N1 103.8(3) . . . . ?
Cl2 Cr1 C1 N1 -72.6(3) . . . . ?
C1 N1 C2 C3 1.6(4) . . . . ?
C4 N1 C2 C3 -176.5(4) . . . . ?
N1 C2 C3 N2 -1.0(4) . . . . ?
C1 N2 C3 C2 0.1(5) . . . . ?
C14 N2 C3 C2 177.7(3) . . . . ?
C6 N3 C4 N1 -163.7(4) . . . . ?
Cr1 N3 C4 N1 10.8(4) . . . . ?
C6 N3 C4 C5 22.0(7) . . . . ?
Cr1 N3 C4 C5 -163.5(3) . . . . ?
C1 N1 C4 N3 3.8(5) . . . . ?
C2 N1 C4 N3 -178.3(4) . . . . ?
C1 N1 C4 C5 178.9(3) . . . . ?
C2 N1 C4 C5 -3.1(6) . . . . ?
N3 C4 C5 C25 -6.2(6) . . . . ?
N1 C4 C5 C25 179.7(4) . . . . ?
N3 C4 C5 C23 -127.9(4) . . . . ?
N1 C4 C5 C23 57.9(5) . . . . ?
N3 C4 C5 C24 108.7(5) . . . . ?
N1 C4 C5 C24 -65.4(4) . . . . ?
C1 N2 C14 C15 75.8(5) . . . . ?
C3 N2 C14 C15 -101.4(4) . . . . ?
C1 N2 C14 C19 -108.3(4) . . . . ?
C3 N2 C14 C19 74.5(5) . . . . ?
C15 C14 C19 C18 0.8(6) . . . . ?
N2 C14 C19 C18 -174.9(3) . . . . ?
C15 C14 C19 C22 -178.3(4) . . . . ?
N2 C14 C19 C22 6.0(6) . . . . ?
C14 C19 C18 C17 -1.2(6) . . . . ?
C22 C19 C18 C17 177.9(4) . . . . ?
C19 C18 C17 C16 0.5(7) . . . . ?
C19 C18 C17 C21 179.9(4) . . . . ?
C18 C17 C16 C15 0.7(7) . . . . ?
C21 C17 C16 C15 -178.7(4) . . . . ?
C19 C14 C15 C16 0.3(6) . . . . ?
N2 C14 C15 C16 176.0(4) . . . . ?
C19 C14 C15 C20 -177.7(4) . . . . ?
N2 C14 C15 C20 -2.0(6) . . . . ?
C17 C16 C15 C14 -1.1(6) . . . . ?
C17 C16 C15 C20 176.9(4) . . . . ?
C4 N3 C6 C11 -109.0(5) . . . . ?
Cr1 N3 C6 C11 76.6(4) . . . . ?
C4 N3 C6 C7 75.6(5) . . . . ?
Cr1 N3 C6 C7 -98.9(4) . . . . ?
C7 C6 C11 C10 2.0(6) . . . . ?
N3 C6 C11 C10 -173.2(4) . . . . ?
C7 C6 C11 C13 -173.8(4) . . . . ?
N3 C6 C11 C13 11.0(6) . . . . ?
C6 C11 C10 C9 -0.4(7) . . . . ?
C13 C11 C10 C9 175.6(5) . . . . ?
C11 C10 C9 C8 -0.8(7) . . . . ?
C10 C9 C8 C7 0.4(7) . . . . ?
C9 C8 C7 C6 1.2(7) . . . . ?
C9 C8 C7 C12 -176.0(4) . . . . ?
C11 C6 C7 C8 -2.4(6) . . . . ?
N3 C6 C7 C8 172.9(4) . . . . ?
C11 C6 C7 C12 174.7(4) . . . . ?
N3 C6 C7 C12 -9.9(6) . . . . ?
C29 O1 C26 C27 32.1(6) . . . . ?
Cr1 O1 C26 C27 -175.9(3) . . . . ?
O1 C26 C27 C28 -34.8(6) . . . . ?
C26 C27 C28 C29 25.5(7) . . . . ?
C26 O1 C29 C28 -15.9(7) . . . . ?
Cr1 O1 C29 C28 -168.9(4) . . . . ?
C27 C28 C29 O1 -6.8(8) . . . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 0.583
_refine_diff_density_min -0.619
_refine_diff_density_rms 0.078
# start Validation Reply Form
_vrf_PLAT220_edwin_0m
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PROBLEM: Large Non-Solvent C Ueq(max)Ueq(min) ... 4.3 Ratio
RESPONSE: The thermal parameters of the THF ligand bonded to the central metal
atom are larger than expected due to intermolecular interactions with the
disordered solvent molecule. Attempts to model disorder for THF did not result
in a satisfactory model.
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# end Validation Reply Form