Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_B201459A    

_database_code_CSD	179470


_journal_coden_Cambridge      182

loop_
_publ_author_name
_publ_author_address

'Guo Dong'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;

'Han Gang'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;

'Duan Chun-ying'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;

'Pang Ke-liang'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;

'Meng Qing-jin'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;

_publ_contact_author_name             'Dr. Duan Chun-ying'
_publ_contact_author_address          
;
Coordination Chemistry Institute
The State Key Laboratory of Coordinaiton Chemistry
Nanjing University , Nanjing 210093
P. R. China
; 
_publ_contact_author_email           duancy@nju.edu.cn
_publ_contact_author_fax             '00 86 25 331 7761'
_publ_contact_author_phone           '00 86 25 359 7006'


_publ_requested_journal              'Chemical Communication'
_publ_requested_category             'No. B201459A '  

#========================================================================

# TITLE AND AUTHOR LIST

_publ_section_title
; 
Novel ferrocene-containing helical triangular macrocycle achieved 
via an exchange reaction
;



#=====================================================================




_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
'(C42 H42 N6 Fe3) (CH3 CN)'
_chemical_formula_sum 
'C44 H45 Fe3 N7' 
_chemical_formula_weight          839.42 

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' 
'Fe'  'Fe'   0.3463   0.8444 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting           'Rhombohedral'
_symmetry_space_group_name_H-M   'R-3c  '

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-y, x-y, z' 
'-x+y, -x, z' 
'y, x, -z+1/2' 
'x-y, -y, -z+1/2' 
'-x, -x+y, -z+1/2' 
'x+2/3, y+1/3, z+1/3' 
'-y+2/3, x-y+1/3, z+1/3' 
'-x+y+2/3, -x+1/3, z+1/3' 
'y+2/3, x+1/3, -z+5/6' 
'x-y+2/3, -y+1/3, -z+5/6' 
'-x+2/3, -x+y+1/3, -z+5/6' 
'x+1/3, y+2/3, z+2/3' 
'-y+1/3, x-y+2/3, z+2/3' 
'-x+y+1/3, -x+2/3, z+2/3' 
'y+1/3, x+2/3, -z+7/6' 
'x-y+1/3, -y+2/3, -z+7/6' 
'-x+1/3, -x+y+2/3, -z+7/6' 
'-x, -y, -z' 
'y, -x+y, -z' 
'x-y, x, -z' 
'-y, -x, z-1/2' 
'-x+y, y, z-1/2' 
'x, x-y, z-1/2' 
'-x+2/3, -y+1/3, -z+1/3' 
'y+2/3, -x+y+1/3, -z+1/3' 
'x-y+2/3, x+1/3, -z+1/3' 
'-y+2/3, -x+1/3, z-1/6' 
'-x+y+2/3, y+1/3, z-1/6' 
'x+2/3, x-y+1/3, z-1/6' 
'-x+1/3, -y+2/3, -z+2/3' 
'y+1/3, -x+y+2/3, -z+2/3' 
'x-y+1/3, x+2/3, -z+2/3' 
'-y+1/3, -x+2/3, z+1/6' 
'-x+y+1/3, y+2/3, z+1/6' 
'x+1/3, x-y+2/3, z+1/6' 

_cell_length_a                    13.5900(19) 
_cell_length_b                    13.5900(19) 
_cell_length_c                    37.595(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      6013.1(17) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        plate
_exptl_crystal_colour             red  
_exptl_crystal_size_max           0.35 
_exptl_crystal_size_mid           0.35 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.391 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2616 
_exptl_absorpt_coefficient_mu     1.112 

_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.202 
_exptl_absorpt_correction_T_max   1.070 
_exptl_absorpt_process_details    '(Blessing, 1995, 1997)' 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(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   'NONIUS KappaCCD' 
_diffrn_measurement_method        'CCD' 
_diffrn_detector_area_resol_mean  0.76 
_diffrn_reflns_number             22051 
_diffrn_reflns_av_R_equivalents   0.1208 
_diffrn_reflns_av_sigmaI/netI     0.0481 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -44 
_diffrn_reflns_limit_l_max        44 
_diffrn_reflns_theta_min          3.41 
_diffrn_reflns_theta_max          24.99 
_reflns_number_total              1177 
_reflns_number_gt                 842 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'KappaCCD (Nonius B. V., 1998)' 
_computing_cell_refinement        'HKL Scalepack (Otwinowski & Minor, 1997)' 
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL V5.1 (Sheldrick, 1998)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 

_publ_section_references
;
collect:
Collect data collection software, Nonius B.V., Delft, The Netherlands, 1998.

HKL Scalepack & HKL Denzo:
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet,
Eds., Academic Press.

absorption correction:
R.H. Blessing (1995) Acta Cryst. A51, 33-37.
R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426.

maXus: 
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland
maXus: a computer program for the solution and refinement of crystal
structures from diffraction data, University of Glasgow, Scotland, UK,
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama,
Japan (1998).

Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen,
Germany.
; 

_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^)+(0.0983P)^2^+14.4742P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1177 
_refine_ls_number_parameters      89 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0836 
_refine_ls_R_factor_gt            0.0539 
_refine_ls_wR_factor_ref          0.1612 
_refine_ls_wR_factor_gt           0.1512 
_refine_ls_goodness_of_fit_ref    1.035 
_refine_ls_restrained_S_all       1.035 
_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 
Fe1 Fe 0.94556(6) 0.6667 0.9167 0.0319(4) Uani 1 2 d S . . 
N1 N 1.0747(3) 0.4584(3) 0.90678(11) 0.0415(10) Uani 1 1 d . . . 
C1 C 0.8269(4) 0.4987(4) 0.90903(14) 0.0407(12) Uani 1 1 d . . . 
H1A H 0.7732 0.4476 0.9269 0.049 Uiso 1 1 calc R . . 
C2 C 0.8070(4) 0.5665(4) 0.88498(14) 0.0442(13) Uani 1 1 d . . . 
H2A H 0.7373 0.5710 0.8835 0.053 Uiso 1 1 calc R . . 
C3 C 0.9044(4) 0.6277(4) 0.86388(14) 0.0419(12) Uani 1 1 d . . . 
H3A H 0.9140 0.6820 0.8451 0.050 Uiso 1 1 calc R . . 
C4 C 0.9875(4) 0.5988(4) 0.87453(13) 0.0358(11) Uani 1 1 d . . . 
H4A H 1.0635 0.6286 0.8642 0.043 Uiso 1 1 calc R . . 
C5 C 0.9397(4) 0.5178(4) 0.90306(13) 0.0359(11) Uani 1 1 d . . . 
C6 C 0.9930(4) 0.4630(4) 0.92226(12) 0.0355(11) Uani 1 1 d . . . 
C7 C 0.9443(4) 0.4098(4) 0.95753(13) 0.0450(13) Uani 1 1 d . . . 
H7A H 1.0043 0.4182 0.9729 0.068 Uiso 1 1 calc R . . 
H7B H 0.8907 0.3305 0.9543 0.068 Uiso 1 1 calc R . . 
H7C H 0.9067 0.4465 0.9680 0.068 Uiso 1 1 calc R . . 
C8 C 1.3333 0.6667 0.8486(5) 0.078(9) Uani 0.50 3 d SP . . 
N2 N 1.3333 0.6667 0.8229(8) 0.097(8) Uani 0.50 3 d SP . . 
C9 C 1.3333 0.6667 0.8793(10) 0.117(12) Uani 0.50 3 d SP . . 
H9A H 1.2834 0.5897 0.8873 0.176 Uiso 0.50 1 d PR . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Fe1 0.0225(5) 0.0244(6) 0.0494(7) 0.0030(4) 0.0015(2) 0.0122(3) 
N1 0.038(2) 0.039(2) 0.055(3) 0.0028(19) -0.005(2) 0.025(2) 
C1 0.024(2) 0.026(2) 0.067(3) 0.002(2) -0.001(2) 0.009(2) 
C2 0.026(3) 0.036(3) 0.072(4) 0.001(2) -0.009(2) 0.017(2) 
C3 0.042(3) 0.038(3) 0.050(3) 0.000(2) -0.010(2) 0.023(2) 
C4 0.035(3) 0.034(3) 0.043(3) -0.003(2) -0.003(2) 0.021(2) 
C5 0.034(3) 0.024(2) 0.050(3) -0.004(2) -0.007(2) 0.015(2) 
C6 0.033(3) 0.026(2) 0.050(3) -0.008(2) -0.011(2) 0.017(2) 
C7 0.055(3) 0.044(3) 0.047(3) 0.003(2) -0.001(2) 0.033(3) 
C8 0.104(15) 0.104(15) 0.025(10) 0.000 0.000 0.052(8) 
N2 0.036(6) 0.036(6) 0.22(3) 0.000 0.000 0.018(3) 
C9 0.031(7) 0.031(7) 0.29(4) 0.000 0.000 0.015(4) 

_geom_special_details 
; 
All esds (except the esd in the dihedral angle between two l.s. planes) 
are estimated using the full covariance matrix.  The cell esds are taken 
into account individually in the estimation of esds in distances, angles 
and torsion angles; correlations between esds in cell parameters are only 
used when they are defined by crystal symmetry.  An approximate (isotropic) 
treatment of cell esds is used for estimating esds involving l.s. planes. 
; 

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
Fe1 C5 2.050(5) 11_566 ? 
Fe1 C5 2.050(4) . ? 
Fe1 C4 2.052(5) 11_566 ? 
Fe1 C4 2.052(5) . ? 
Fe1 C1 2.053(5) 11_566 ? 
Fe1 C1 2.053(5) . ? 
Fe1 C3 2.058(5) 11_566 ? 
Fe1 C3 2.058(5) . ? 
Fe1 C2 2.063(5) 11_566 ? 
Fe1 C2 2.063(5) . ? 
N1 C6 1.283(6) . ? 
N1 N1 1.400(7) 10_546 ? 
C1 C2 1.411(7) . ? 
C1 C5 1.439(6) . ? 
C1 H1A 0.9800 . ? 
C2 C3 1.404(7) . ? 
C2 H2A 0.9800 . ? 
C3 C4 1.427(6) . ? 
C3 H3A 0.9800 . ? 
C4 C5 1.438(6) . ? 
C4 H4A 0.9800 . ? 
C5 C6 1.462(6) . ? 
C6 C7 1.497(6) . ? 
C7 H7A 0.9600 . ? 
C7 H7B 0.9600 . ? 
C7 H7C 0.9600 . ? 
C8 N2 0.97(3) . ? 
C8 C9 1.15(4) . ? 
C9 H9A 0.9669 . ? 

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 
C5 Fe1 C5 125.9(2) 11_566 . ? 
C5 Fe1 C4 41.04(18) 11_566 11_566 ? 
C5 Fe1 C4 107.27(18) . 11_566 ? 
C5 Fe1 C4 107.27(18) 11_566 . ? 
C5 Fe1 C4 41.04(18) . . ? 
C4 Fe1 C4 119.6(3) 11_566 . ? 
C5 Fe1 C1 41.06(18) 11_566 11_566 ? 
C5 Fe1 C1 164.30(19) . 11_566 ? 
C4 Fe1 C1 68.43(19) 11_566 11_566 ? 
C4 Fe1 C1 126.75(19) . 11_566 ? 
C5 Fe1 C1 164.30(19) 11_566 . ? 
C5 Fe1 C1 41.06(18) . . ? 
C4 Fe1 C1 126.75(19) 11_566 . ? 
C4 Fe1 C1 68.43(19) . . ? 
C1 Fe1 C1 153.5(3) 11_566 . ? 
C5 Fe1 C3 68.54(18) 11_566 11_566 ? 
C5 Fe1 C3 119.8(2) . 11_566 ? 
C4 Fe1 C3 40.64(17) 11_566 11_566 ? 
C4 Fe1 C3 154.6(2) . 11_566 ? 
C1 Fe1 C3 67.5(2) 11_566 11_566 ? 
C1 Fe1 C3 108.4(2) . 11_566 ? 
C5 Fe1 C3 119.8(2) 11_566 . ? 
C5 Fe1 C3 68.54(18) . . ? 
C4 Fe1 C3 154.6(2) 11_566 . ? 
C4 Fe1 C3 40.64(17) . . ? 
C1 Fe1 C3 108.5(2) 11_566 . ? 
C1 Fe1 C3 67.5(2) . . ? 
C3 Fe1 C3 163.5(3) 11_566 . ? 
C5 Fe1 C2 68.45(19) 11_566 11_566 ? 
C5 Fe1 C2 153.9(2) . 11_566 ? 
C4 Fe1 C2 67.97(19) 11_566 11_566 ? 
C4 Fe1 C2 164.02(19) . 11_566 ? 
C1 Fe1 C2 40.11(18) 11_566 11_566 ? 
C1 Fe1 C2 119.8(2) . 11_566 ? 
C3 Fe1 C2 39.8(2) 11_566 11_566 ? 
C3 Fe1 C2 126.91(19) . 11_566 ? 
C5 Fe1 C2 153.87(19) 11_566 . ? 
C5 Fe1 C2 68.45(19) . . ? 
C4 Fe1 C2 164.02(19) 11_566 . ? 
C4 Fe1 C2 67.98(19) . . ? 
C1 Fe1 C2 119.82(19) 11_566 . ? 
C1 Fe1 C2 40.11(18) . . ? 
C3 Fe1 C2 126.9(2) 11_566 . ? 
C3 Fe1 C2 39.8(2) . . ? 
C2 Fe1 C2 108.7(3) 11_566 . ? 
C6 N1 N1 115.5(5) . 10_546 ? 
C2 C1 C5 108.5(4) . . ? 
C2 C1 Fe1 70.3(3) . . ? 
C5 C1 Fe1 69.4(2) . . ? 
C2 C1 H1A 125.8 . . ? 
C5 C1 H1A 125.8 . . ? 
Fe1 C1 H1A 125.8 . . ? 
C3 C2 C1 108.5(4) . . ? 
C3 C2 Fe1 69.9(3) . . ? 
C1 C2 Fe1 69.6(3) . . ? 
C3 C2 H2A 125.8 . . ? 
C1 C2 H2A 125.8 . . ? 
Fe1 C2 H2A 125.8 . . ? 
C2 C3 C4 108.7(4) . . ? 
C2 C3 Fe1 70.3(3) . . ? 
C4 C3 Fe1 69.5(3) . . ? 
C2 C3 H3A 125.7 . . ? 
C4 C3 H3A 125.7 . . ? 
Fe1 C3 H3A 125.7 . . ? 
C3 C4 C5 107.6(4) . . ? 
C3 C4 Fe1 69.9(3) . . ? 
C5 C4 Fe1 69.4(3) . . ? 
C3 C4 H4A 126.2 . . ? 
C5 C4 H4A 126.2 . . ? 
Fe1 C4 H4A 126.2 . . ? 
C4 C5 C1 106.7(4) . . ? 
C4 C5 C6 127.5(4) . . ? 
C1 C5 C6 125.8(4) . . ? 
C4 C5 Fe1 69.6(2) . . ? 
C1 C5 Fe1 69.6(3) . . ? 
C6 C5 Fe1 126.5(3) . . ? 
N1 C6 C5 117.5(4) . . ? 
N1 C6 C7 124.2(4) . . ? 
C5 C6 C7 118.2(4) . . ? 
C6 C7 H7A 109.5 . . ? 
C6 C7 H7B 109.5 . . ? 
H7A C7 H7B 109.5 . . ? 
C6 C7 H7C 109.5 . . ? 
H7A C7 H7C 109.5 . . ? 
H7B C7 H7C 109.5 . . ? 
N2 C8 C9 180.00(3) . . ? 
C8 C9 H9A 108.1 . . ? 

_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              24.99 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.911 
_refine_diff_density_min   -0.315 
_refine_diff_density_rms    0.094