# CIF-file generated for KUNB 4320-133
# Compound 1
#===================================================================
data_global
#===================================================================
# 0. AUDIT DETAILS
_audit_creation_date 5-Nov-03
_audit_creation_method 'PLATON
option'
_audit_update_record
;
5-Nov-03 Updated by the Author E.H.
Textwriting by E.H.
Checkcif OK
8-Dez-04 Updated by the Author E.H.
4-Mar-05 Updated by the Author E.H.
;
#===================================================================
# 1. SUBMISSION DETAILS
#===================================================================
# Name and address of author for X-ray correspondence
_publ_contact_author
;
Dr. Eberhardt Herdtweck,
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
_publ_contact_author_email 'eberhardt.herdtweck@ch.tum.de'
_publ_contact_author_fax ' +49(0)89 289 13473'
_publ_contact_author_phone '+49(0)89 289 13143'
_publ_requested_journal 'Organometallics'
# Publication choise FI FM FO CI CM CO
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter # Include date of submission
;
Date of submission: March 2005
;
#===================================================================
# 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY)
#===================================================================
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_coeditor_notes
; ?
;
_journal_techeditor_code ?
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#===================================================================
# 3. TITLE AND AUTHOR LIST
#===================================================================
_publ_section_title
;
Cycloheptatrienyl-Cyclopentadienlyl-Zirconium Sandwich Complexes:
Structure and Bonding
;
# The loop structure below should contain the names and adresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
'Tamm, M.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Kunst, A.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Bannenberg, T.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Herdtweck, E.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Schmid, R.'
;
Lehrstuhl f\"ur Anorganische Chemie II,
Ruhr-Universit\"at Bochum,
Organometallics & Materials Chemistry,
Universit\"atsstrasse 150
D-44780 Bochum,
Germany.
;
#=====================================================================
# 4. TEXT
#=====================================================================
_publ_section_synopsis
;
;
_publ_section_abstract
;
...
;
# Insert blank lines between paragraphs
_publ_section_comment
;
;
_publ_section_experimental
;
;
# Insert blank lines between references
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436.
Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices.
Nonius BV, Delft, The Netherlands.
Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices,
Nonius BV, Delft, The Netherlands.
Sheldrick, G. M. (1998). SHELXL97, University of G\"ottingen, G\"ottingen,
Germany.
Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht
University, Utrecht, The Netherlands.
;
_publ_section_figure_captions
;
;
_publ_section_acknowledgements
;
;
_publ_section_table_legends
;
;
#===================================================================
data_KUNB-4320-133
#===================================================================
#===================================================================
# 5. CHEMICAL DATA
#===================================================================
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_formula_moiety
'C12 H12 Zr'
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum
'C12 H12 Zr'
_chemical_formula_weight 247.44
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zr Zr -2.9673 0.5597
'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'
C C 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===================================================================
# 6. CRYSTAL DATA
#===================================================================
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2n'
_symmetry_space_group_name_H-M 'P n m a'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
1/2+x,1/2-y,1/2-z
-x,1/2+y,-z
-x,-y,-z
1/2+x,y,1/2-z
1/2-x,1/2+y,1/2+z
x,1/2-y,z
_cell_length_a 11.1033(2)
_cell_length_b 10.5715(2)
_cell_length_c 8.2212(1)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 964.99(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 133(1)
_cell_measurement_reflns_used 1059
_cell_measurement_theta_min 3.08
_cell_measurement_theta_max 25.39
_exptl_crystal_description 'fragment'
_exptl_crystal_colour 'purple'
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas none
_exptl_crystal_density_diffrn 1.703
_exptl_crystal_density_method none
_exptl_crystal_F_000 496
_exptl_absorpt_coefficient_mu 1.084
_exptl_absorpt_correction_type 'multi-scan'
_exptl_absorpt_correction_T_min 0.723
_exptl_absorpt_correction_T_max 0.918
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_special_details
;
Diffractometer operator E. Herdtweck
scanspeed 2 x 40 s per film
repetition 1
dx 40
566 films measured in 9 data sets
set 1: phi-scan with delta_phi = 2.0
set 2 to 9 omega-scans with delta_omega = 2.0
;
_publ_section_exptl_prep
;
The crystal was fixed in a capillary with perfluorinated ether and
transferred to the diffractometer.
;
_publ_section_exptl_refinement
;
Straight forward after integration with the program NPROCESS,
source: Nonius (2001b).
Hydrogen atoms could be located in the difference Fourier maps
and were allowed to refine freely.
;
#===================================================================
# 7. EXPERIMENTAL DATA
#===================================================================
_diffrn_ambient_temperature 133(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'NONIUS FR 591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device ' \k-geometry diffractometer '
_diffrn_measurement_device_type ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method ' phi- and omega-rotation '
_diffrn_detector ' CCD plate '
_diffrn_detector_area_resol_mean 18 # 9 for binned mode
_diffrn_standards_decay_% 0
# number of measured reflections (redundant set)
_diffrn_reflns_number 23575
_diffrn_reflns_av_R_equivalents 0.036
_diffrn_reflns_av_sigmaI/netI 0.0146
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_theta_min 3.08
_diffrn_reflns_theta_max 25.39
_reflns_number_total 935
_reflns_number_gt 897
# number of observed reflections (> n sig(I))
_reflns_threshold_expression 'I>2\s(I)'
_computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_cell_refinement 'DENZO (Nonius, 2001b)'
_computing_data_reduction 'DENZO (Nonius, 2001b)'
_computing_structure_solution 'SIR92 (Altomare, 1994)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)'
_computing_molecular_graphics 'PLATON (Spek, 2001)'
_computing_publication_material 'PLATON (Spek, 2001)'
#===================================================================
# 8. REFINEMENT DATA
#===================================================================
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0099P)^2^+0.6089P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment refall
_refine_ls_number_reflns 935
_refine_ls_number_parameters 90
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0155
_refine_ls_R_factor_gt 0.0143
_refine_ls_wR_factor_ref 0.0338
_refine_ls_wR_factor_gt 0.0334
_refine_ls_goodness_of_fit_ref 1.101
_refine_ls_restrained_S_all 1.101
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.39
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.276
_refine_diff_density_min -0.223
_refine_diff_density_rms 0.044
#===================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
#===================================================================
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Zr Zr Uani 0.13759(2) 0.25000 0.94639(2) 1.000 0.0164(1) . .
C1 C Uani 0.3468(2) 0.25000 0.9525(3) 1.000 0.0297(8) . .
C2 C Uani 0.30899(14) 0.12893(17) 0.8967(2) 1.000 0.0272(5) . .
C3 C Uani 0.22363(14) 0.09904(15) 0.77399(19) 1.000 0.0237(5) . .
C4 C Uani 0.15492(13) 0.18264(15) 0.67607(18) 1.000 0.0229(4) . .
C5 C Uani 0.0870(2) 0.25000 1.2419(3) 1.000 0.0248(7) . .
C6 C Uani 0.03087(14) 0.14208(15) 1.17553(18) 1.000 0.0232(5) . .
C7 C Uani -0.05931(13) 0.18341(15) 1.06761(18) 1.000 0.0215(4) . .
H11 H Uiso 0.397(2) 0.25000 1.042(3) 1.000 0.038(7) . .
H21 H Uiso 0.3353(16) 0.0631(19) 0.955(2) 1.000 0.035(5) . .
H31 H Uiso 0.2050(15) 0.0138(17) 0.761(2) 1.000 0.029(4) . .
H41 H Uiso 0.0951(15) 0.1426(17) 0.611(2) 1.000 0.031(4) . .
H51 H Uiso 0.149(2) 0.25000 1.309(3) 1.000 0.037(8) . .
H61 H Uiso 0.0523(15) 0.0590(16) 1.1969(19) 1.000 0.028(5) . .
H71 H Uiso -0.1078(15) 0.1347(18) 1.007(2) 1.000 0.028(5) . .
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
Zr 0.0152(1) 0.0203(1) 0.0137(1) 0.0000 0.0039(1) 0.0000
C1 0.0158(11) 0.0544(17) 0.0190(12) 0.0000 -0.0018(9) 0.0000
C2 0.0246(8) 0.0326(9) 0.0245(8) 0.0101(7) 0.0071(7) 0.0127(7)
C3 0.0286(8) 0.0180(8) 0.0246(8) -0.0018(7) 0.0110(7) 0.0007(6)
C4 0.0231(8) 0.0296(8) 0.0161(7) -0.0055(7) 0.0014(6) -0.0048(7)
C5 0.0193(11) 0.0433(14) 0.0117(10) 0.0000 0.0024(9) 0.0000
C6 0.0254(8) 0.0226(8) 0.0216(8) 0.0070(7) 0.0101(6) 0.0029(6)
C7 0.0168(7) 0.0260(8) 0.0216(8) -0.0034(7) 0.0049(6) -0.0060(6)
#==================================================================
# 10. MOLECULAR GEOMETRY
#===================================================================
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr C1 2.323(2) . . yes
Zr C2 2.3295(16) . . yes
Zr C3 2.3384(16) . . yes
Zr C4 2.3416(15) . . yes
Zr C5 2.494(2) . . yes
Zr C6 2.5009(15) . . yes
Zr C7 2.5037(15) . . yes
C1 C2 1.423(2) . . no
C2 C3 1.420(2) . . no
C3 C4 1.418(2) . . no
C4 C4 1.424(2) . 8_555 no
C5 C6 1.410(2) . . no
C6 C7 1.407(2) . . no
C7 C7 1.408(2) . 8_555 no
C1 H11 0.92(2) . . no
C2 H21 0.894(19) . . no
C3 H31 0.931(18) . . no
C4 H41 0.952(17) . . no
C5 H51 0.88(2) . . no
C6 H61 0.927(17) . . no
C7 H71 0.896(17) . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Zr C2 35.61(5) . . . yes
C1 Zr C3 66.71(6) . . . yes
C1 Zr C4 86.47(7) . . . yes
C1 Zr C5 101.78(8) . . . yes
C1 Zr C6 117.22(6) . . . yes
C1 Zr C7 149.82(6) . . . yes
C1 Zr C2 35.61(5) . . 8_555 yes
C1 Zr C3 66.71(6) . . 8_555 yes
C1 Zr C4 86.47(7) . . 8_555 yes
C1 Zr C6 117.22(6) . . 8_555 yes
C1 Zr C7 149.82(6) . . 8_555 yes
C2 Zr C3 35.41(6) . . . yes
C2 Zr C4 66.38(5) . . . yes
C2 Zr C5 110.79(6) . . . yes
C2 Zr C6 105.58(6) . . . yes
C2 Zr C7 128.95(6) . . . yes
C2 Zr C2 66.65(6) . . 8_555 yes
C2 Zr C3 86.27(6) . . 8_555 yes
C2 Zr C4 86.19(6) . . 8_555 yes
C2 Zr C6 140.34(5) . . 8_555 yes
C2 Zr C7 159.66(6) . . 8_555 yes
C3 Zr C4 35.28(5) . . . yes
C3 Zr C5 133.04(4) . . . yes
C3 Zr C6 109.80(5) . . . yes
C3 Zr C7 113.96(5) . . . yes
C2 Zr C3 86.27(6) 8_555 . . yes
C3 Zr C3 86.07(5) . . 8_555 yes
C3 Zr C4 66.34(5) . . 8_555 yes
C3 Zr C6 164.04(5) . . 8_555 yes
C3 Zr C7 142.17(5) . . 8_555 yes
C4 Zr C5 160.60(4) . . . yes
C4 Zr C6 127.96(5) . . . yes
C4 Zr C7 111.35(5) . . . yes
C2 Zr C4 86.19(6) 8_555 . . yes
C3 Zr C4 66.34(5) 8_555 . . yes
C4 Zr C4 35.41(5) . . 8_555 yes
C4 Zr C6 153.20(5) . . 8_555 yes
C4 Zr C7 122.35(5) . . 8_555 yes
C5 Zr C6 32.79(4) . . . yes
C5 Zr C7 54.23(6) . . . yes
C2 Zr C5 110.79(6) 8_555 . . yes
C3 Zr C5 133.04(4) 8_555 . . yes
C4 Zr C5 160.60(4) 8_555 . . yes
C5 Zr C6 32.79(4) . . 8_555 yes
C5 Zr C7 54.23(6) . . 8_555 yes
C6 Zr C7 32.67(5) . . . yes
C2 Zr C6 140.34(5) 8_555 . . yes
C3 Zr C6 164.04(5) 8_555 . . yes
C4 Zr C6 153.20(5) 8_555 . . yes
C6 Zr C6 54.28(5) . . 8_555 yes
C6 Zr C7 54.17(5) . . 8_555 yes
C2 Zr C7 159.66(6) 8_555 . . yes
C3 Zr C7 142.17(5) 8_555 . . yes
C4 Zr C7 122.35(5) 8_555 . . yes
C6 Zr C7 54.17(5) 8_555 . . yes
C7 Zr C7 32.66(5) . . 8_555 yes
C2 Zr C3 35.41(6) 8_555 . 8_555 yes
C2 Zr C4 66.38(5) 8_555 . 8_555 yes
C2 Zr C6 105.58(6) 8_555 . 8_555 yes
C2 Zr C7 128.95(6) 8_555 . 8_555 yes
C3 Zr C4 35.28(5) 8_555 . 8_555 yes
C3 Zr C6 109.80(5) 8_555 . 8_555 yes
C3 Zr C7 113.96(5) 8_555 . 8_555 yes
C4 Zr C6 127.96(5) 8_555 . 8_555 yes
C4 Zr C7 111.35(5) 8_555 . 8_555 yes
C6 Zr C7 32.67(5) 8_555 . 8_555 yes
Zr C1 C2 72.43(11) . . . yes
Zr C1 C2 72.43(11) . . 8_555 yes
C2 C1 C2 128.17(19) . . 8_555 no
Zr C2 C1 71.96(11) . . . yes
Zr C2 C3 72.63(9) . . . yes
C1 C2 C3 128.77(16) . . . no
Zr C3 C2 71.95(9) . . . yes
Zr C3 C4 72.48(9) . . . yes
C2 C3 C4 128.59(15) . . . no
Zr C4 C3 72.24(9) . . . yes
Zr C4 C4 72.30(9) . . 8_555 yes
C3 C4 C4 128.55(14) . . 8_555 no
Zr C5 C6 73.89(11) . . . yes
Zr C5 C6 73.89(11) . . 8_555 yes
C6 C5 C6 108.04(18) . . 8_555 no
Zr C6 C5 73.32(11) . . . yes
Zr C6 C7 73.78(9) . . . yes
C5 C6 C7 107.89(14) . . . no
Zr C7 C6 73.56(9) . . . yes
Zr C7 C7 73.67(8) . . 8_555 yes
C6 C7 C7 108.09(13) . . 8_555 no
Zr C1 H11 128.4(14) . . . no
C2 C1 H11 115.79(13) . . . no
C2 C1 H11 115.79(13) 8_555 . . no
Zr C2 H21 126.9(11) . . . no
C1 C2 H21 115.5(12) . . . no
C3 C2 H21 115.2(12) . . . no
Zr C3 H31 129.8(10) . . . no
C2 C3 H31 116.4(10) . . . no
C4 C3 H31 114.8(10) . . . no
Zr C4 H41 127.7(10) . . . no
C3 C4 H41 114.7(11) . . . no
C4 C4 H41 116.4(11) 8_555 . . no
Zr C5 H51 115.7(15) . . . no
C6 C5 H51 125.94(11) . . . no
C6 C5 H51 125.94(11) 8_555 . . no
Zr C6 H61 117.0(10) . . . no
C5 C6 H61 125.5(10) . . . no
C7 C6 H61 126.6(10) . . . no
Zr C7 H71 117.7(11) . . . no
C6 C7 H71 126.8(12) . . . no
C7 C7 H71 125.1(12) 8_555 . . no
### End
# CIF-file generated for KUNA 4319-133
# Compound 2a
#===================================================================
data_global
#===================================================================
# 0. AUDIT DETAILS
_audit_creation_date 6-Nov-03
_audit_creation_method 'PLATON option'
_audit_update_record
;
6-Nov-03 Updated by the Author E.H.
Textwriting by E.H.
Checkcif OK
8-Dez-04 Updated by the Author E.H.
4-Mar-05 Updated by the Author E.H.
;
#===================================================================
# 1. SUBMISSION DETAILS
#===================================================================
# Name and address of author for X-ray correspondence
_publ_contact_author
;
Dr. Eberhardt Herdtweck,
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
_publ_contact_author_email 'eberhardt.herdtweck@ch.tum.de'
_publ_contact_author_fax ' +49(0)89 289 13473'
_publ_contact_author_phone '+49(0)89 289 13143'
_publ_requested_journal 'Organometallics'
# Publication choise FI FM FO CI CM CO
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter # Include date of submission
;
Date of submission: March 2005
;
#===================================================================
# 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY)
#===================================================================
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_coeditor_notes
; ?
;
_journal_techeditor_code ?
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#===================================================================
# 3. TITLE AND AUTHOR LIST
#===================================================================
_publ_section_title
;
Cycloheptatrienyl-Cyclopentadienlyl-Zirconium Sandwich Complexes:
Structure and Bonding
;
# The loop structure below should contain the names and adresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
'Tamm, M.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Kunst, A.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Bannenberg, T.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Herdtweck, E.'
;
Department Chemie,
Lehrstuhl f\"ur Anorganische Chemie,
Technische Universit\"at M\"unchen,
Lichtenbergstrasse 4,
D-85747 Garching bei M\"unchen,
Germany.
;
'Schmid, R.'
;
Lehrstuhl f\"ur Anorganische Chemie II,
Ruhr-Universit\"at Bochum,
Organometallics & Materials Chemistry,
Universit\"atsstrasse 150
D-44780 Bochum,
Germany.
;
#=====================================================================
# 4. TEXT
#=====================================================================
_publ_section_synopsis
;
;
_publ_section_abstract
;
...
;
# Insert blank lines between paragraphs
_publ_section_comment
;
;
_publ_section_experimental
;
;
# Insert blank lines between references
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436.
Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices.
Nonius BV, Delft, The Netherlands.
Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices,
Nonius BV, Delft, The Netherlands.
Sheldrick, G. M. (1998). SHELXL97, University of G\"ottingen, G\"ottingen,
Germany.
Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht
University, Utrecht, The Netherlands.
;
_publ_section_figure_captions
;
;
_publ_section_acknowledgements
;
;
_publ_section_table_legends
;
;
#===================================================================
data_KUNA-4319-133
#===================================================================
#===================================================================
# 5. CHEMICAL DATA
#===================================================================
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_formula_moiety
'C17 H21 N Zr'
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum
'C17 H21 N Zr'
_chemical_formula_weight 330.57
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zr Zr -2.9673 0.5597
'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'
H H 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===================================================================
# 6. CRYSTAL DATA
#===================================================================
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_Hall '-P 2c 2b'
_symmetry_space_group_name_H-M 'P b c m'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,1/2+z
x,1/2-y,-z
-x,1/2+y,1/2-z
-x,-y,-z
x,y,1/2-z
-x,1/2+y,z
x,1/2-y,1/2+z
_cell_length_a 8.3304(1)
_cell_length_b 18.5959(2)
_cell_length_c 10.1241(1)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1568.34(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 133(1)
_cell_measurement_reflns_used 1694
_cell_measurement_theta_min 2.19
_cell_measurement_theta_max 25.37
_exptl_crystal_description 'fragment'
_exptl_crystal_colour 'orange'
_exptl_crystal_size_max 0.56
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas none
_exptl_crystal_density_diffrn 1.400
_exptl_crystal_density_method none
_exptl_crystal_F_000 680
_exptl_absorpt_coefficient_mu 0.688
_exptl_absorpt_correction_type 'multi-scan'
_exptl_absorpt_correction_T_min 0.667
_exptl_absorpt_correction_T_max 0.870
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_special_details
;
Diffractometer operator E. Herdtweck
scanspeed 2 x 15 s per film
repetition 1
dx 40
1076 films measured in 9 data sets
set 1: phi-scan with delta_phi = 1.0
set 2 to 9 omega-scans with delta_omega = 1.0
;
_publ_section_exptl_prep
;
The crystal was fixed in a capillary with perfluorinated ether and
transferred to the diffractometer.
;
_publ_section_exptl_refinement
;
Straight forward after integration with the program NPROCESS,
source: Nonius (2001b).
Hydrogen atoms could not be located in the difference Fourier maps
and were calculated in ideal positions (riding model).
;
#===================================================================
# 7. EXPERIMENTAL DATA
#===================================================================
_diffrn_ambient_temperature 133(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'NONIUS FR 591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device ' \k-geometry diffractometer '
_diffrn_measurement_device_type ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method ' phi- and omega-rotation '
_diffrn_detector ' CCD plate '
_diffrn_detector_area_resol_mean 18 # 9 for binned mode
_diffrn_standards_decay_% 0
# number of measured reflections (redundant set)
_diffrn_reflns_number 35406
_diffrn_reflns_av_R_equivalents 0.035
_diffrn_reflns_av_sigmaI/netI 0.0112
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 2.19
_diffrn_reflns_theta_max 25.37
_reflns_number_total 1532
_reflns_number_gt 1456
# number of observed reflections (> n sig(I))
_reflns_threshold_expression 'I>2\s(I)'
_computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_cell_refinement 'DENZO (Nonius, 2001b)'
_computing_data_reduction 'DENZO (Nonius, 2001b)'
_computing_structure_solution 'SIR92 (Altomare, 1994)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)'
_computing_molecular_graphics 'PLATON (Spek, 2001)'
_computing_publication_material 'PLATON (Spek, 2001)'
#===================================================================
# 8. REFINEMENT DATA
#===================================================================
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0207P)^2^+2.0911P] 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_number_reflns 1532
_refine_ls_number_parameters 98
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0255
_refine_ls_R_factor_gt 0.0242
_refine_ls_wR_factor_ref 0.0580
_refine_ls_wR_factor_gt 0.0571
_refine_ls_goodness_of_fit_ref 1.089
_refine_ls_restrained_S_all 1.089
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.524
_refine_diff_density_min -0.428
_refine_diff_density_rms 0.058
#===================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
#===================================================================
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Zr Zr Uani 0.84401(3) 0.09908(1) 0.25000 1.000 0.0184(1) . .
N N Uani 0.5941(3) 0.25197(13) 0.25000 1.000 0.0286(7) . .
C1 C Uani 0.5712(4) 0.05300(19) 0.25000 1.000 0.084(3) . .
C2 C Uani 0.6406(5) 0.04179(15) 0.1237(4) 1.000 0.0747(15) . .
C3 C Uani 0.7867(5) 0.00976(16) 0.0957(3) 1.000 0.0664(12) . .
C4 C Uani 0.8898(3) -0.02228(12) 0.1835(4) 1.000 0.0613(12) . .
C5 C Uani 1.1455(4) 0.1057(2) 0.25000 1.000 0.081(2) . .
C6 C Uani 1.0957(3) 0.14389(14) 0.1375(4) 1.000 0.0616(10) . .
C7 C Uani 1.0154(3) 0.20510(11) 0.1810(2) 1.000 0.0362(7) . .
C8 C Uani 0.6697(3) 0.20021(15) 0.25000 1.000 0.0279(9) . .
C9 C Uani 0.5134(4) 0.32200(14) 0.25000 1.000 0.0260(8) . .
C10 C Uani 0.6461(4) 0.37850(16) 0.25000 1.000 0.0391(10) . .
C11 C Uani 0.4114(3) 0.32638(12) 0.1259(2) 1.000 0.0383(7) . .
H11 H Uiso 0.46400 0.07030 0.25000 1.000 0.1000 calc R
H21 H Uiso 0.58000 0.05810 0.05010 1.000 0.0900 calc R
H31 H Uiso 0.81920 0.01000 0.00580 1.000 0.0800 calc R
H41 H Uiso 0.97480 -0.04870 0.14410 1.000 0.0740 calc R
H51 H Uiso 1.20300 0.06160 0.25000 1.000 0.0980 calc R
H61 H Uiso 1.11350 0.13040 0.04820 1.000 0.0740 calc R
H71 H Uiso 0.96860 0.24080 0.12610 1.000 0.0430 calc R
H101 H Uiso 0.59810 0.42660 0.25000 1.000 0.0590 calc R
H102 H Uiso 0.71270 0.37260 0.17100 0.500 0.0590 calc R
H103 H Uiso 0.71270 0.37260 0.32900 0.500 0.0590 calc R
H111 H Uiso 0.48000 0.32080 0.04800 1.000 0.0580 calc R
H112 H Uiso 0.35740 0.37320 0.12250 1.000 0.0580 calc R
H113 H Uiso 0.33080 0.28800 0.12720 1.000 0.0580 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
Zr 0.0180(2) 0.0139(2) 0.0235(2) 0.0000 0.0000 -0.0005(1)
N 0.0257(12) 0.0179(11) 0.0423(15) 0.0000 0.0000 0.0033(11)
C1 0.0115(16) 0.0155(17) 0.224(8) 0.0000 0.0000 -0.0026(13)
C2 0.095(3) 0.0321(14) 0.097(3) 0.0295(16) -0.078(2) -0.0332(16)
C3 0.120(3) 0.0484(17) 0.0309(14) -0.0151(13) 0.0199(18) -0.051(2)
C4 0.0429(14) 0.0241(11) 0.117(3) -0.0298(14) 0.0352(16) -0.0078(10)
C5 0.0171(18) 0.027(2) 0.200(7) 0.0000 0.0000 -0.0022(14)
C6 0.0447(15) 0.0480(16) 0.092(2) -0.0281(16) 0.0425(17) -0.0249(13)
C7 0.0363(12) 0.0283(11) 0.0440(12) 0.0047(10) 0.0066(11) -0.0137(9)
C8 0.0252(15) 0.0190(14) 0.0395(17) 0.0000 0.0000 -0.0029(12)
C9 0.0286(15) 0.0138(12) 0.0356(16) 0.0000 0.0000 0.0053(11)
C10 0.0364(18) 0.0189(14) 0.062(2) 0.0000 0.0000 -0.0005(13)
C11 0.0455(13) 0.0292(11) 0.0403(13) -0.0033(10) -0.0080(11) 0.0097(10)
#==================================================================
# 10. MOLECULAR GEOMETRY
#===================================================================
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr C1 2.429(3) . . yes
Zr C2 2.375(4) . . yes
Zr C3 2.330(3) . . yes
Zr C4 2.386(2) . . yes
Zr C5 2.515(3) . . yes
Zr C6 2.527(3) . . yes
Zr C7 2.532(2) . . yes
Zr C8 2.376(3) . . yes
N C8 1.150(4) . . yes
N C9 1.466(4) . . yes
C1 C2 1.419(4) . . no
C2 C3 1.384(6) . . no
C3 C4 1.372(5) . . no
C4 C4 1.347(6) . 6_555 no
C5 C6 1.405(4) . . no
C6 C7 1.392(4) . . no
C7 C7 1.397(3) . 6_555 no
C9 C10 1.525(4) . . no
C9 C11 1.519(3) . . no
C1 H11 0.9492 . . no
C2 H21 0.9498 . . no
C3 H31 0.9496 . . no
C4 H41 0.9497 . . no
C5 H51 0.9497 . . no
C6 H61 0.9499 . . no
C7 H71 0.9496 . . no
C10 H101 0.9798 . . no
C10 H102 0.9796 . . no
C10 H103 0.9796 . . no
C11 H111 0.9795 . . no
C11 H112 0.9806 . . no
C11 H113 0.9800 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Zr C2 34.33(10) . . . yes
C1 Zr C3 63.68(11) . . . yes
C1 Zr C4 79.39(10) . . . yes
C1 Zr C5 162.14(12) . . . yes
C1 Zr C6 153.20(9) . . . yes
C1 Zr C7 143.34(9) . . . yes
C1 Zr C8 72.99(10) . . . yes
C1 Zr C2 34.33(10) . . 6_555 yes
C1 Zr C3 63.68(11) . . 6_555 yes
C1 Zr C4 79.39(10) . . 6_555 yes
C1 Zr C6 153.20(9) . . 6_555 yes
C1 Zr C7 143.34(9) . . 6_555 yes
C2 Zr C3 34.21(13) . . . yes
C2 Zr C4 62.47(11) . . . yes
C2 Zr C5 137.27(11) . . . yes
C2 Zr C6 119.81(13) . . . yes
C2 Zr C7 127.08(10) . . . yes
C2 Zr C8 85.36(10) . . . yes
C2 Zr C2 65.14(14) . . 6_555 yes
C2 Zr C3 83.97(12) . . 6_555 yes
C2 Zr C4 80.89(11) . . 6_555 yes
C2 Zr C6 169.22(11) . . 6_555 yes
C2 Zr C7 154.15(9) . . 6_555 yes
C3 Zr C4 33.81(12) . . . yes
C3 Zr C5 103.86(12) . . . yes
C3 Zr C6 95.91(12) . . . yes
C3 Zr C7 119.05(10) . . . yes
C3 Zr C8 116.05(10) . . . yes
C2 Zr C3 83.97(12) 6_555 . . yes
C3 Zr C3 84.22(11) . . 6_555 yes
C3 Zr C4 63.10(12) . . 6_555 yes
C3 Zr C6 135.01(12) . . 6_555 yes
C3 Zr C7 148.82(10) . . 6_555 yes
C4 Zr C5 83.49(10) . . . yes
C4 Zr C6 92.98(9) . . . yes
C4 Zr C7 124.64(9) . . . yes
C4 Zr C8 147.83(9) . . . yes
C2 Zr C4 80.89(11) 6_555 . . yes
C3 Zr C4 63.10(12) 6_555 . . yes
C4 Zr C4 32.78(13) . . 6_555 yes
C4 Zr C6 107.84(9) . . 6_555 yes
C4 Zr C7 136.39(8) . . 6_555 yes
C5 Zr C6 32.36(9) . . . yes
C5 Zr C7 53.04(10) . . . yes
C5 Zr C8 124.87(11) . . . yes
C2 Zr C5 137.27(11) 6_555 . . yes
C3 Zr C5 103.86(12) 6_555 . . yes
C4 Zr C5 83.49(10) 6_555 . . yes
C5 Zr C6 32.36(9) . . 6_555 yes
C5 Zr C7 53.04(10) . . 6_555 yes
C6 Zr C7 31.93(8) . . . yes
C6 Zr C8 104.25(8) . . . yes
C2 Zr C6 169.22(11) 6_555 . . yes
C3 Zr C6 135.01(12) 6_555 . . yes
C4 Zr C6 107.84(9) 6_555 . . yes
C6 Zr C6 53.57(12) . . 6_555 yes
C6 Zr C7 53.13(9) . . 6_555 yes
C7 Zr C8 74.24(8) . . . yes
C2 Zr C7 154.15(9) 6_555 . . yes
C3 Zr C7 148.82(10) 6_555 . . yes
C4 Zr C7 136.39(8) 6_555 . . yes
C6 Zr C7 53.13(9) 6_555 . . yes
C7 Zr C7 32.03(7) . . 6_555 yes
C2 Zr C8 85.36(10) 6_555 . . yes
C3 Zr C8 116.05(10) 6_555 . . yes
C4 Zr C8 147.83(9) 6_555 . . yes
C6 Zr C8 104.25(8) 6_555 . . yes
C7 Zr C8 74.24(8) 6_555 . . yes
C2 Zr C3 34.21(13) 6_555 . 6_555 yes
C2 Zr C4 62.47(11) 6_555 . 6_555 yes
C2 Zr C6 119.81(13) 6_555 . 6_555 yes
C2 Zr C7 127.08(10) 6_555 . 6_555 yes
C3 Zr C4 33.81(12) 6_555 . 6_555 yes
C3 Zr C6 95.91(12) 6_555 . 6_555 yes
C3 Zr C7 119.05(10) 6_555 . 6_555 yes
C4 Zr C6 92.98(9) 6_555 . 6_555 yes
C4 Zr C7 124.64(9) 6_555 . 6_555 yes
C6 Zr C7 31.93(8) 6_555 . 6_555 yes
C8 N C9 174.1(3) . . . yes
Zr C1 C2 70.8(2) . . . yes
Zr C1 C2 70.8(2) . . 6_555 yes
C2 C1 C2 128.7(3) . . 6_555 no
Zr C2 C1 74.9(2) . . . yes
Zr C2 C3 71.1(2) . . . yes
C1 C2 C3 127.3(3) . . . no
Zr C3 C2 74.7(2) . . . yes
Zr C3 C4 75.34(18) . . . yes
C2 C3 C4 127.2(3) . . . no
Zr C4 C3 70.85(16) . . . yes
Zr C4 C4 73.61(16) . . 6_555 yes
C3 C4 C4 130.4(3) . . 6_555 no
Zr C5 C6 74.32(17) . . . yes
Zr C5 C6 74.32(17) . . 6_555 yes
C6 C5 C6 108.3(3) . . 6_555 no
Zr C6 C5 73.32(19) . . . yes
Zr C6 C7 74.23(15) . . . yes
C5 C6 C7 107.4(3) . . . no
Zr C7 C6 73.83(14) . . . yes
Zr C7 C7 73.99(13) . . 6_555 yes
C6 C7 C7 108.4(2) . . 6_555 no
Zr C8 N 175.5(2) . . . yes
N C9 C10 106.2(3) . . . yes
N C9 C11 107.71(15) . . . yes
N C9 C11 107.71(15) . . 6_555 yes
C10 C9 C11 111.63(15) . . . no
C10 C9 C11 111.63(15) . . 6_555 no
C11 C9 C11 111.6(2) . . 6_555 no
Zr C1 H11 139.53 . . . no
C2 C1 H11 115.67 . . . no
C2 C1 H11 115.67 6_555 . . no
Zr C2 H21 131.17 . . . no
C1 C2 H21 116.33 . . . no
C3 C2 H21 116.36 . . . no
Zr C3 H31 125.52 . . . no
C2 C3 H31 116.42 . . . no
C4 C3 H31 116.39 . . . no
Zr C4 H41 136.64 . . . no
C3 C4 H41 114.79 . . . no
C4 C4 H41 114.84 6_555 . . no
Zr C5 H51 117.48 . . . no
C6 C5 H51 125.83 . . . no
C6 C5 H51 125.83 6_555 . . no
Zr C6 H61 118.12 . . . no
C5 C6 H61 126.30 . . . no
C7 C6 H61 126.31 . . . no
Zr C7 H71 118.31 . . . no
C6 C7 H71 125.73 . . . no
C7 C7 H71 125.83 6_555 . . no
C9 C10 H101 109.46 . . . no
C9 C10 H102 109.47 . . . no
C9 C10 H103 109.47 . . . no
H101 C10 H102 109.48 . . . no
H101 C10 H103 109.48 . . . no
H102 C10 H103 109.47 . . . no
C9 C11 H111 109.51 . . . no
C9 C11 H112 109.47 . . . no
C9 C11 H113 109.46 . . . no
H111 C11 H112 109.48 . . . no
H111 C11 H113 109.48 . . . no
H112 C11 H113 109.44 . . . no
### End of Crystallographic Information Files