# Supplementary Material (ESI) for Perkin Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 207/403
# CIF Belonging to paper B000196L - R. Blaauw et al
# CIF-file generated for s1537a
data_global
#=======================================================================
# 0. AUDIT DETAILS
_audit_creation_date 'Nov 8 15:44:56 1999'
_audit_creation_method 'PLATON
option'
#=======================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name # Name of author for correspondence
; Dr. A.L. Spek
;
_publ_contact_author_address # Address of author for correspondence
;
Bijvoet Center for Biomolecular Research
Department of Crystal and Structural Chemistry
Utrecht University
Padualaan 8
3584 CH Utrecht
The Netherlands
;
_publ_contact_author_email 'spea@chem.uu.nl'
_publ_contact_author_fax '+31 30 2533940'
_publ_contact_author_phone '+31 30 2532538'
#=======================================================================
data_s1537a
#=======================================================================
# 5. CHEMICAL DATA
_chemical_name_common 'Bridged (beta-alkoxyalkyl)Co(III)salen'
_chemical_formula_moiety 'C22 H25 Co N2 O4, C H2 Cl2'
_chemical_formula_sum 'C23 H27 Cl2 Co N2 O4'
_chemical_formula_weight 525.30
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060
'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'
Co Co 0.3494 0.9721
'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'
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 Monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 21/c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
_cell_length_a 12.4467(14)
_cell_length_b 11.4978(7)
_cell_length_c 19.0943(18)
_cell_angle_alpha 90
_cell_angle_beta 125.340(7)
_cell_angle_gamma 90
_cell_volume 2229.1(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 150
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 10.11
_cell_measurement_theta_max 13.84
_cell_special_details
; SET4
;
_exptl_crystal_description needle
_exptl_crystal_colour red
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_exptl_crystal_density_diffrn 1.565
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 1088
_exptl_absorpt_coefficient_mu 1.04
_exptl_absorpt_correction_type none
#=======================================================================
# 7. EXPERIMENTAL DATA
_diffrn_ambient_temperature 150
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device_type 'CAD4T'
_diffrn_measurement_method 'omega-scan'
_diffrn_standards_number 3
_diffrn_standards_decay_% 2
# number of measured reflections (redundant set)
_diffrn_reflns_number 4578
_diffrn_reflns_av_R_equivalents 0.0701
_diffrn_reflns_av_sigmaI/netI 0.1340
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 0
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.01
_diffrn_reflns_theta_max 25.00
# number of unique reflections
_reflns_number_total 3932
# number of observed reflections (> n sig(I))
_reflns_number_gt 2223
_reflns_threshold_expression 'I>2sigma(I)'
_computing_data_collection 'Locally modified CAD4-Version 5 Software'
_computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_reduction 'HELENA (Spek, 1997)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1986)'
_computing_structure_refinement 'SHELXL96 (Sheldrick, 1996)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#=======================================================================
# 8. REFINEMENT DATA
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme 'calc '
_refine_ls_weighting_details
'w-1 = sigma**2(Fo**2) + (0.0374P)**2 + 2.16P'
_refine_ls_hydrogen_treatment 'H-atom refinement: see text '
_refine_ls_extinction_method none
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack none
_refine_ls_number_reflns 3932
_refine_ls_number_parameters 309
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.1424
_refine_ls_R_factor_gt 0.0655
_refine_ls_wR_factor_ref 0.1327
_refine_ls_wR_factor_gt 0.1062
_refine_ls_goodness_of_fit_ref 1.017
_refine_ls_restrained_S_all 1.019
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.604
_refine_diff_density_min -0.437
_refine_diff_density_rms 0.102
#=======================================================================
# 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
Co1 Co Uani 0.56606(7) 0.40018(7) 0.07168(5) 1.000
0.0150(2)
O1 O Uani 0.4050(3) 0.4083(4) -0.0409(2) 1.000
0.0166(12)
O2 O Uani 0.6447(3) 0.3413(3) 0.0191(2) 1.000
0.0153(12)
O3 O Uani 0.5733(4) 0.0678(4) 0.1752(3) 1.000
0.0312(17)
O4 O Uani 0.4632(5) -0.1547(5) 0.0983(4) 1.000
0.067(3)
N1 N Uani 0.4873(5) 0.4635(4) 0.1217(3) 1.000
0.0159(17)
N2 N Uani 0.7240(4) 0.4119(4) 0.1804(3) 1.000
0.0166(16)
C1 C Uani 0.2872(5) 0.3943(5) -0.0553(4) 1.000
0.0175(17)
C2 C Uani 0.1800(5) 0.3575(5) -0.1371(4) 1.000
0.0196(17)
C3 C Uani 0.0539(6) 0.3523(5) -0.1580(4) 1.000
0.024(2)
C4 C Uani 0.0292(6) 0.3814(5) -0.0973(4) 1.000
0.023(2)
C5 C Uani 0.1328(5) 0.4160(5) -0.0169(4) 1.000
0.0221(19)
C6 C Uani 0.2623(5) 0.4216(5) 0.0058(4) 1.000
0.0180(19)
C7 C Uani 0.3651(6) 0.4646(5) 0.0907(4) 1.000
0.0184(17)
C8 C Uani 0.5832(5) 0.5178(5) 0.2054(4) 1.000
0.019(2)
C9 C Uani 0.7097(6) 0.4472(5) 0.2495(4) 1.000
0.0186(19)
C10 C Uani 0.8406(5) 0.3897(5) 0.2006(4) 1.000
0.0187(17)
C11 C Uani 0.8707(5) 0.3465(5) 0.1438(3) 1.000
0.0135(17)
C12 C Uani 1.0038(6) 0.3292(5) 0.1758(4) 1.000
0.022(2)
C13 C Uani 1.0408(6) 0.2882(6) 0.1255(4) 1.000
0.028(2)
C14 C Uani 0.9431(6) 0.2638(6) 0.0399(4) 1.000
0.026(2)
C15 C Uani 0.8117(6) 0.2819(5) 0.0051(4) 1.000
0.0193(17)
C16 C Uani 0.7717(5) 0.3227(5) 0.0556(4) 1.000
0.0172(17)
C17 C Uani 0.7139(6) 0.3430(5) 0.2995(4) 1.000
0.0221(19)
C18 C Uani 0.6112(6) 0.2472(6) 0.2483(4) 1.000
0.025(2)
C19 C Uani 0.6161(6) 0.1872(5) 0.1796(4) 1.000
0.0214(19)
C20 C Uani 0.5291(5) 0.2421(5) 0.0914(4) 1.000
0.0193(17)
C21 C Uani 0.6297(7) -0.0113(7) 0.1507(6) 1.000
0.053(3)
C22 C Uani 0.5961(7) -0.1334(6) 0.1522(5) 1.000
0.037(2)
Cl1 Cl Uiso 0.1173(11) 0.5101(14) 0.3990(6) 0.580
0.067(3)
Cl2 Cl Uiso 0.2118(8) 0.3899(8) 0.5631(5) 0.580
0.0597(18)
C50 C Uani 0.2439(7) 0.4437(8) 0.4922(4) 1.000
0.061(3)
Cl11 Cl Uiso 0.1397(18) 0.506(2) 0.3914(9) 0.420
0.093(7)
Cl21 Cl Uiso 0.1608(14) 0.4287(13) 0.5398(9) 0.420
0.138(7)
H4 H Uiso 0.44960 -0.21280 0.06750 1.000
0.0800
H21 H Uiso 0.19490 0.33580 -0.17890 1.000
0.0230
H31 H Uiso -0.01680 0.32880 -0.21400 1.000
0.0290
H41 H Uiso -0.05750 0.37730 -0.11150 1.000
0.0280
H51 H Uiso 0.11660 0.43660 0.02440 1.000
0.0270
H71 H Uiso 0.33960 0.49540 0.12530 1.000
0.0220
H81 H Uiso 0.54860 0.51830 0.24090 1.000
0.0270
H82 H Uiso 0.60020 0.59910 0.19740 1.000
0.0270
H91 H Uiso 0.78490 0.49960 0.29010 1.000
0.0220
H101 H Uiso 0.91260 0.40340 0.25850 1.000
0.0220
H121 H Uiso 1.07010 0.34660 0.23430 1.000
0.0270
H131 H Uiso 1.13110 0.27680 0.14860 1.000
0.0340
H141 H Uiso 0.96730 0.23390 0.00450 1.000
0.0310
H151 H Uiso 0.74740 0.26640 -0.05400 1.000
0.0230
H171 H Uiso 0.70360 0.37120 0.34430 1.000
0.0300
H172 H Uiso 0.80240 0.30740 0.32920 1.000
0.0300
H181 H Uiso 0.62200 0.18740 0.28920 1.000
0.0340
H182 H Uiso 0.52250 0.28170 0.22070 1.000
0.0340
H191 H Uiso 0.70920 0.18660 0.19760 1.000
0.0250
H201 H Uiso 0.43790 0.24180 0.07530 1.000
0.0260
H202 H Uiso 0.53020 0.19000 0.05050 1.000
0.0260
H211 H Uiso 0.72660 -0.00270 0.18930 1.000
0.0710
H212 H Uiso 0.60150 0.00810 0.09180 1.000
0.0710
H221 H Uiso 0.64220 -0.18360 0.13530 1.000
0.0510
H222 H Uiso 0.62810 -0.15450 0.21150 1.000
0.0510
H501 H Uiso 0.31680 0.50040 0.52370 0.580
0.0830
H502 H Uiso 0.27650 0.37840 0.47550 0.580
0.0830
H503 H Uiso 0.32240 0.49350 0.52830 0.420
0.0830
H504 H Uiso 0.27370 0.36650 0.48670 0.420
0.0830
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
Co1 0.0148(4) 0.0144(4) 0.0140(4) 0.0000(4) 0.0073(3) 0.0000(4)
O1 0.013(2) 0.019(2) 0.014(2) 0.000(2) 0.0057(17) -0.002(2)
O2 0.014(2) 0.018(2) 0.010(2) -0.0008(19) 0.0047(17) 0.0004(18)
O3 0.038(3) 0.012(3) 0.051(3) 0.001(2) 0.030(3) -0.001(2)
O4 0.042(3) 0.067(5) 0.088(5) -0.054(4) 0.036(3) -0.021(3)
N1 0.021(3) 0.011(3) 0.015(3) -0.002(2) 0.010(2) -0.002(2)
N2 0.020(3) 0.014(3) 0.012(2) -0.003(2) 0.007(2) -0.001(2)
C1 0.020(3) 0.006(3) 0.019(3) -0.001(3) 0.007(3) -0.002(3)
C2 0.020(3) 0.013(3) 0.022(3) 0.000(3) 0.010(3) 0.005(3)
C3 0.016(3) 0.022(4) 0.026(4) -0.002(3) 0.007(3) -0.004(3)
C4 0.017(3) 0.021(4) 0.035(4) 0.000(3) 0.017(3) -0.006(3)
C5 0.025(3) 0.019(4) 0.025(3) 0.001(3) 0.016(3) 0.002(3)
C6 0.014(3) 0.014(4) 0.023(3) 0.002(3) 0.009(3) 0.000(3)
C7 0.024(3) 0.014(3) 0.023(3) 0.007(3) 0.017(3) 0.001(3)
C8 0.027(4) 0.017(4) 0.014(3) -0.003(3) 0.012(3) -0.004(3)
C9 0.021(3) 0.021(4) 0.009(3) -0.003(3) 0.006(3) -0.004(3)
C10 0.017(3) 0.015(3) 0.015(3) 0.005(3) 0.004(3) 0.001(3)
C11 0.017(3) 0.011(3) 0.013(3) 0.004(3) 0.009(3) 0.004(3)
C12 0.019(3) 0.020(4) 0.023(4) 0.009(3) 0.009(3) 0.003(3)
C13 0.021(3) 0.034(4) 0.034(4) 0.007(4) 0.018(3) 0.004(3)
C14 0.026(4) 0.024(4) 0.029(4) 0.000(3) 0.017(3) 0.002(3)
C15 0.025(3) 0.015(3) 0.014(3) 0.001(3) 0.009(3) 0.001(3)
C16 0.017(3) 0.013(3) 0.019(3) 0.000(3) 0.009(3) 0.002(3)
C17 0.028(3) 0.026(4) 0.015(3) 0.000(3) 0.014(3) 0.003(3)
C18 0.035(4) 0.023(4) 0.019(3) 0.003(3) 0.016(3) -0.001(3)
C19 0.025(3) 0.017(3) 0.026(4) 0.006(3) 0.017(3) 0.003(3)
C20 0.022(3) 0.013(3) 0.024(3) -0.003(3) 0.014(3) -0.004(3)
C21 0.041(5) 0.029(5) 0.085(7) -0.011(5) 0.034(5) -0.001(4)
C22 0.039(4) 0.026(4) 0.034(4) -0.007(3) 0.014(4) -0.010(3)
C50 0.052(5) 0.078(7) 0.052(6) 0.018(5) 0.029(5) 0.021(5)
#=======================================================================
# 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
Co1 O1 1.914(3) . .
yes
Co1 O2 1.887(4) . .
yes
Co1 N1 1.867(6) . .
yes
Co1 N2 1.863(5) . .
yes
Co1 C20 1.964(6) . .
yes
Cl1 C50 1.729(14) . .
yes
Cl2 C50 1.732(13) . .
yes
Cl11 C50 1.735(17) . .
yes
Cl21 C50 1.74(2) . .
yes
O1 C1 1.336(9) . .
yes
O2 C16 1.325(8) . .
yes
O3 C19 1.457(8) . .
yes
O3 C21 1.385(11) . .
yes
O4 C22 1.373(12) . .
yes
O4 H4 0.8400 . .
no
N1 C8 1.470(8) . .
yes
N1 C7 1.274(11) . .
yes
N2 C10 1.293(10) . .
yes
N2 C9 1.486(9) . .
yes
C1 C6 1.405(10) . .
no
C1 C2 1.410(9) . .
no
C2 C3 1.379(11) . .
no
C3 C4 1.401(11) . .
no
C4 C5 1.374(9) . .
no
C5 C6 1.408(11) . .
no
C6 C7 1.453(9) . .
no
C8 C9 1.521(10) . .
no
C9 C17 1.514(9) . .
no
C10 C11 1.426(9) . .
no
C11 C16 1.424(8) . .
no
C11 C12 1.409(11) . .
no
C12 C13 1.367(11) . .
no
C13 C14 1.389(9) . .
no
C14 C15 1.379(12) . .
no
C15 C16 1.398(10) . .
no
C17 C18 1.535(10) . .
no
C18 C19 1.514(10) . .
no
C19 C20 1.516(9) . .
no
C21 C22 1.470(11) . .
no
C2 H21 0.9513 . .
no
C3 H31 0.9498 . .
no
C4 H41 0.9496 . .
no
C5 H51 0.9500 . .
no
C7 H71 0.9514 . .
no
C8 H82 0.9896 . .
no
C8 H81 0.9913 . .
no
C9 H91 1.0003 . .
no
C10 H101 0.9508 . .
no
C12 H121 0.9499 . .
no
C13 H131 0.9495 . .
no
C14 H141 0.9494 . .
no
C15 H151 0.9492 . .
no
C17 H172 0.9899 . .
no
C17 H171 0.9900 . .
no
C18 H181 0.9896 . .
no
C18 H182 0.9904 . .
no
C19 H191 1.0001 . .
no
C20 H201 0.9896 . .
no
C20 H202 0.9906 . .
no
C21 H212 0.9905 . .
no
C21 H211 0.9896 . .
no
C22 H221 0.9903 . .
no
C22 H222 0.9889 . .
no
C50 H501 0.9893 . .
no
C50 H502 0.9898 . .
no
C50 H503 0.9892 . .
no
C50 H504 0.9907 . .
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
O1 Co1 O2 87.05(17) . . .
yes
O1 Co1 N1 92.1(2) . . .
yes
O1 Co1 N2 173.0(2) . . .
yes
O1 Co1 C20 92.9(2) . . .
yes
O2 Co1 N1 177.95(19) . . .
yes
O2 Co1 N2 94.6(2) . . .
yes
O2 Co1 C20 91.2(2) . . .
yes
N1 Co1 N2 86.0(2) . . .
yes
N1 Co1 C20 90.7(3) . . .
yes
N2 Co1 C20 93.8(2) . . .
yes
Co1 O1 C1 122.5(4) . . .
yes
Co1 O2 C16 127.3(3) . . .
yes
C19 O3 C21 113.5(6) . . .
yes
C22 O4 H4 109.52 . . .
no
Co1 N1 C7 127.2(4) . . .
yes
Co1 N1 C8 112.7(5) . . .
yes
C7 N1 C8 120.1(6) . . .
yes
Co1 N2 C10 126.6(4) . . .
yes
C9 N2 C10 118.6(5) . . .
yes
Co1 N2 C9 114.7(5) . . .
yes
O1 C1 C6 123.0(6) . . .
yes
C2 C1 C6 117.7(7) . . .
no
O1 C1 C2 119.1(6) . . .
yes
C1 C2 C3 121.5(6) . . .
no
C2 C3 C4 120.5(6) . . .
no
C3 C4 C5 118.7(8) . . .
no
C4 C5 C6 121.6(7) . . .
no
C1 C6 C5 119.8(6) . . .
no
C1 C6 C7 121.9(7) . . .
no
C5 C6 C7 118.1(6) . . .
no
N1 C7 C6 124.0(7) . . .
yes
N1 C8 C9 107.7(5) . . .
yes
N2 C9 C17 111.4(5) . . .
yes
C8 C9 C17 114.7(7) . . .
no
N2 C9 C8 105.8(5) . . .
yes
N2 C10 C11 125.8(6) . . .
yes
C10 C11 C16 122.5(6) . . .
no
C12 C11 C16 118.8(6) . . .
no
C10 C11 C12 118.7(5) . . .
no
C11 C12 C13 122.2(6) . . .
no
C12 C13 C14 118.4(8) . . .
no
C13 C14 C15 121.6(7) . . .
no
C14 C15 C16 121.0(6) . . .
no
O2 C16 C11 122.9(6) . . .
yes
C11 C16 C15 118.1(7) . . .
no
O2 C16 C15 118.9(6) . . .
yes
C9 C17 C18 117.0(5) . . .
no
C17 C18 C19 116.3(7) . . .
no
O3 C19 C20 109.0(5) . . .
yes
C18 C19 C20 114.3(6) . . .
no
O3 C19 C18 106.4(6) . . .
yes
Co1 C20 C19 120.2(4) . . .
yes
O3 C21 C22 114.5(8) . . .
yes
O4 C22 C21 112.9(7) . . .
yes
C1 C2 H21 119.30 . . .
no
C3 C2 H21 119.17 . . .
no
C2 C3 H31 119.76 . . .
no
C4 C3 H31 119.71 . . .
no
C3 C4 H41 120.59 . . .
no
C5 C4 H41 120.70 . . .
no
C4 C5 H51 119.15 . . .
no
C6 C5 H51 119.21 . . .
no
N1 C7 H71 117.99 . . .
no
C6 C7 H71 117.99 . . .
no
N1 C8 H81 110.19 . . .
no
N1 C8 H82 110.18 . . .
no
C9 C8 H81 110.16 . . .
no
C9 C8 H82 110.14 . . .
no
H81 C8 H82 108.44 . . .
no
N2 C9 H91 108.28 . . .
no
C8 C9 H91 108.21 . . .
no
C17 C9 H91 108.20 . . .
no
N2 C10 H101 117.03 . . .
no
C11 C10 H101 117.16 . . .
no
C11 C12 H121 118.94 . . .
no
C13 C12 H121 118.83 . . .
no
C12 C13 H131 120.70 . . .
no
C14 C13 H131 120.94 . . .
no
C13 C14 H141 119.24 . . .
no
C15 C14 H141 119.19 . . .
no
C14 C15 H151 119.59 . . .
no
C16 C15 H151 119.43 . . .
no
C9 C17 H171 108.13 . . .
no
C9 C17 H172 108.03 . . .
no
C18 C17 H171 107.99 . . .
no
C18 C17 H172 107.99 . . .
no
H171 C17 H172 107.32 . . .
no
C17 C18 H181 108.24 . . .
no
C17 C18 H182 108.22 . . .
no
C19 C18 H181 108.18 . . .
no
C19 C18 H182 108.22 . . .
no
H181 C18 H182 107.40 . . .
no
O3 C19 H191 109.00 . . .
no
C18 C19 H191 108.95 . . .
no
C20 C19 H191 109.01 . . .
no
Co1 C20 H201 107.30 . . .
no
Co1 C20 H202 107.27 . . .
no
C19 C20 H201 107.31 . . .
no
C19 C20 H202 107.30 . . .
no
H201 C20 H202 106.82 . . .
no
O3 C21 H211 108.68 . . .
no
O3 C21 H212 108.64 . . .
no
C22 C21 H211 108.59 . . .
no
C22 C21 H212 108.62 . . .
no
H211 C21 H212 107.57 . . .
no
O4 C22 H221 109.00 . . .
no
O4 C22 H222 109.10 . . .
no
C21 C22 H221 108.98 . . .
no
C21 C22 H222 109.02 . . .
no
H221 C22 H222 107.73 . . .
no
Cl1 C50 Cl2 118.5(8) . . .
yes
Cl11 C50 Cl21 109.4(11) . . .
yes
Cl1 C50 H501 107.71 . . .
no
Cl1 C50 H502 107.62 . . .
no
Cl2 C50 H501 107.77 . . .
no
Cl2 C50 H502 107.68 . . .
no
Cl11 C50 H503 109.71 . . .
no
Cl11 C50 H504 109.74 . . .
no
Cl21 C50 H503 109.89 . . .
no
Cl21 C50 H504 109.85 . . .
no
H501 C50 H502 107.04 . . .
no
H503 C50 H504 108.24 . . .
no
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
O2 Co1 O1 C1 148.7(5) . . .
. no
N1 Co1 O1 C1 -33.1(5) . . .
. no
C20 Co1 O1 C1 57.7(5) . . .
. no
O1 Co1 O2 C16 171.5(4) . . .
. no
N2 Co1 O2 C16 -1.7(5) . . .
. no
C20 Co1 O2 C16 -95.6(5) . . .
. no
O1 Co1 N1 C7 21.9(5) . . .
. no
O1 Co1 N1 C8 -157.2(4) . . .
. no
N2 Co1 N1 C7 -164.8(5) . . .
. no
N2 Co1 N1 C8 16.0(4) . . .
. no
C20 Co1 N1 C7 -71.1(5) . . .
. no
C20 Co1 N1 C8 109.8(4) . . .
. no
O2 Co1 N2 C9 -174.8(4) . . .
. no
O2 Co1 N2 C10 3.3(5) . . .
. no
N1 Co1 N2 C9 7.2(4) . . .
. no
N1 Co1 N2 C10 -174.7(5) . . .
. no
C20 Co1 N2 C9 -83.2(4) . . .
. no
C20 Co1 N2 C10 94.8(5) . . .
. no
O1 Co1 C20 C19 -171.3(6) . . .
. no
O2 Co1 C20 C19 101.6(6) . . .
. no
N1 Co1 C20 C19 -79.1(6) . . .
. no
N2 Co1 C20 C19 6.9(6) . . .
. no
Co1 O1 C1 C6 28.1(8) . . .
. no
Co1 O1 C1 C2 -156.0(4) . . .
. no
Co1 O2 C16 C11 -0.3(8) . . .
. no
Co1 O2 C16 C15 -177.9(4) . . .
. no
C21 O3 C19 C20 86.3(8) . . .
. no
C19 O3 C21 C22 175.5(6) . . .
. no
C21 O3 C19 C18 -149.9(6) . . .
. no
Co1 N1 C8 C9 -34.5(6) . . .
. no
Co1 N1 C7 C6 -4.2(9) . . .
. no
C8 N1 C7 C6 174.9(5) . . .
. no
C7 N1 C8 C9 146.3(6) . . .
. no
C10 N2 C9 C8 154.8(5) . . .
. no
Co1 N2 C9 C8 -27.0(6) . . .
. no
Co1 N2 C9 C17 98.3(6) . . .
. no
C9 N2 C10 C11 174.9(5) . . .
. no
C10 N2 C9 C17 -79.9(7) . . .
. no
Co1 N2 C10 C11 -3.0(9) . . .
. no
C6 C1 C2 C3 2.3(9) . . .
. no
O1 C1 C2 C3 -173.7(5) . . .
. no
C2 C1 C6 C5 -2.5(8) . . .
. no
O1 C1 C6 C5 173.4(5) . . .
. no
O1 C1 C6 C7 -1.7(9) . . .
. no
C2 C1 C6 C7 -177.6(5) . . .
. no
C1 C2 C3 C4 -1.4(9) . . .
. no
C2 C3 C4 C5 0.5(9) . . .
. no
C3 C4 C5 C6 -0.7(9) . . .
. no
C4 C5 C6 C1 1.7(9) . . .
. no
C4 C5 C6 C7 177.0(5) . . .
. no
C1 C6 C7 N1 -11.8(9) . . .
. no
C5 C6 C7 N1 173.1(6) . . .
. no
N1 C8 C9 C17 -85.5(7) . . .
. no
N1 C8 C9 N2 37.7(7) . . .
. no
N2 C9 C17 C18 -57.6(9) . . .
. no
C8 C9 C17 C18 62.5(8) . . .
. no
N2 C10 C11 C16 0.1(10) . . .
. no
N2 C10 C11 C12 178.7(6) . . .
. no
C10 C11 C12 C13 -179.9(6) . . .
. no
C16 C11 C12 C13 -1.3(9) . . .
. no
C10 C11 C16 O2 1.6(9) . . .
. no
C10 C11 C16 C15 179.2(6) . . .
. no
C12 C11 C16 O2 -176.9(5) . . .
. no
C12 C11 C16 C15 0.7(8) . . .
. no
C11 C12 C13 C14 0.4(10) . . .
. no
C12 C13 C14 C15 1.1(10) . . .
. no
C13 C14 C15 C16 -1.8(10) . . .
. no
C14 C15 C16 O2 178.5(6) . . .
. no
C14 C15 C16 C11 0.8(9) . . .
. no
C9 C17 C18 C19 61.4(9) . . .
. no
C17 C18 C19 C20 -91.6(8) . . .
. no
C17 C18 C19 O3 148.0(6) . . .
. no
O3 C19 C20 Co1 -175.9(5) . . .
. no
C18 C19 C20 Co1 65.1(8) . . .
. no
O3 C21 C22 O4 60.2(10) . . .
. no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Co1 Co1 3.2029(12) . 3_665
no
Co1 O1 2.360(5) . 3_665
no
Co1 O2 3.669(4) . 3_665
no
Co1 N1 3.701(5) . 3_665
no
Co1 C1 3.111(7) . 3_665
no
Co1 C2 3.840(7) . 3_665
no
Co1 C6 3.822(7) . 3_665
no
Co1 H4 3.3381 . 3_655
no
Cl1 C14 3.384(17) . 2_655
no
Cl1 C15 3.468(16) . 2_655
no
Cl1 C10 3.610(13) . 1_455
no
Cl1 C13 3.640(17) . 2_655
no
Cl2 C14 3.576(14) . 4_455
no
Cl2 C9 3.636(11) . 3_666
no
Cl2 C13 3.616(13) . 4_455
no
Cl11 C10 3.637(19) . 1_455
no
Cl11 C21 3.40(3) . 2_655
no
Cl11 C15 3.60(2) . 2_655
no
Cl11 C14 3.62(2) . 2_655
no
Cl21 C17 3.633(16) . 3_666
no
Cl21 C14 3.50(2) . 4_455
no
Cl21 C9 3.649(16) . 3_666
no
Cl1 H101 2.6993 . 1_455
no
Cl2 H201 3.0836 . 4_555
no
Cl2 H171 3.1026 . 3_666
no
Cl2 H91 3.0561 . 3_666
no
Cl2 H141 2.9326 . 4_455
no
Cl2 H131 3.0405 . 4_455
no
Cl11 H101 2.7428 . 1_455
no
Cl11 H212 3.0470 . 2_655
no
Cl11 H211 2.8496 . 2_655
no
Cl21 H91 3.0242 . 3_666
no
Cl21 H141 2.8057 . 4_455
no
Cl21 H171 2.9527 . 3_666
no
O1 Co1 2.360(5) . 3_665
no
O1 O1 2.865(6) . 3_665
no
O1 N1 2.957(7) . 3_665
no
O1 O2 3.024(6) . 3_665
no
O1 C8 3.338(8) . 3_665
no
O1 N2 3.000(6) . 3_665
no
O2 C6 3.104(7) . 3_665
no
O2 C1 3.124(7) . 3_665
no
O2 N1 3.139(6) . 3_665
no
O2 O4 2.819(7) . 3_655
no
O2 Co1 3.669(4) . 3_665
no
O2 O1 3.024(6) . 3_665
no
O2 C7 3.016(7) . 3_665
no
O3 O4 2.872(8) . .
no
O4 C16 3.313(9) . 3_655
no
O4 O3 2.872(8) . .
no
O4 O2 2.819(7) . 3_655
no
O4 C50 3.323(11) . 4_554
no
O4 C15 3.151(10) . 3_655
no
O2 H4 2.0124 . 3_655
no
O3 H503 2.8255 . 4_554
no
O3 H501 2.9140 . 4_554
no
O3 H81 2.8292 . 2_645
no
O4 H202 2.9179 . 3_655
no
O4 H501 2.3440 . 4_554
no
O4 H171 2.8692 . 2_645
no
O4 H503 2.3629 . 4_554
no
O4 H151 2.5828 . 3_655
no
N1 O1 2.957(7) . 3_665
no
N1 Co1 3.701(5) . 3_665
no
N1 O2 3.139(6) . 3_665
no
N1 C18 3.177(8) . .
no
N2 C2 3.207(8) . 3_665
no
N2 O1 3.000(6) . 3_665
no
N2 C1 3.210(8) . 3_665
no
N1 H182 2.6789 . .
no
N2 H191 2.6310 . .
no
C1 C11 3.429(8) . 3_665
no
C1 C16 3.335(8) . 3_665
no
C1 N2 3.210(8) . 3_665
no
C1 C10 3.360(8) . 3_665
no
C1 O2 3.124(7) . 3_665
no
C1 Co1 3.111(7) . 3_665
no
C2 C11 3.450(8) . 3_665
no
C2 N2 3.207(8) . 3_665
no
C2 C10 3.102(8) . 3_665
no
C2 Co1 3.840(7) . 3_665
no
C3 C12 3.539(9) . 4_454
no
C3 C10 3.524(9) . 3_665
no
C3 C11 3.557(8) . 3_665
no
C4 C12 3.574(8) . 3_665
no
C5 C15 3.523(8) . 3_665
no
C5 C14 3.574(11) . 1_455
no
C5 C16 3.464(9) . 3_665
no
C6 C15 3.506(8) . 3_665
no
C6 Co1 3.822(7) . 3_665
no
C6 C16 3.102(8) . 3_665
no
C6 O2 3.104(7) . 3_665
no
C6 C11 3.541(8) . 3_665
no
C6 C20 3.418(10) . .
no
C7 C16 3.344(8) . 3_665
no
C7 C15 3.468(9) . 3_665
no
C7 O2 3.016(7) . 3_665
no
C8 O1 3.338(8) . 3_665
no
C9 Cl2 3.636(11) . 3_666
no
C9 Cl21 3.649(16) . 3_666
no
C10 Cl1 3.610(13) . 1_655
no
C10 C1 3.360(8) . 3_665
no
C10 Cl11 3.637(19) . 1_655
no
C10 C19 3.478(10) . .
no
C10 C3 3.524(9) . 3_665
no
C10 C2 3.102(8) . 3_665
no
C11 C3 3.557(8) . 3_665
no
C11 C2 3.450(8) . 3_665
no
C11 C6 3.541(8) . 3_665
no
C11 C1 3.429(8) . 3_665
no
C12 C4 3.574(8) . 3_665
no
C12 C3 3.539(9) . 4_655
no
C13 Cl2 3.616(13) . 4_654
no
C13 Cl1 3.640(17) . 2_645
no
C14 Cl21 3.50(2) . 4_654
no
C14 C5 3.574(11) . 1_655
no
C14 Cl2 3.576(14) . 4_654
no
C14 Cl1 3.384(17) . 2_645
no
C14 Cl11 3.62(2) . 2_645
no
C15 O4 3.151(10) . 3_655
no
C15 C7 3.468(9) . 3_665
no
C15 Cl11 3.60(2) . 2_645
no
C15 C6 3.506(8) . 3_665
no
C15 Cl1 3.468(16) . 2_645
no
C15 C5 3.523(8) . 3_665
no
C16 C7 3.344(8) . 3_665
no
C16 C1 3.335(8) . 3_665
no
C16 C6 3.102(8) . 3_665
no
C16 O4 3.313(9) . 3_655
no
C16 C5 3.464(9) . 3_665
no
C17 Cl21 3.633(16) . 3_666
no
C18 N1 3.177(8) . .
no
C19 C10 3.478(10) . .
no
C20 C6 3.418(10) . .
no
C21 Cl11 3.40(3) . 2_645
no
C50 O4 3.323(11) . 4_555
no
C1 H201 2.7203 . .
no
C2 H221 2.9679 . 3_655
no
C2 H121 3.0858 . 4_454
no
C4 H141 2.9968 . 1_455
no
C6 H201 2.7306 . .
no
C7 H182 2.9659 . .
no
C7 H201 2.7889 . .
no
C8 H182 2.8776 . .
no
C10 H191 2.8325 . .
no
C10 H172 2.9158 . .
no
C10 H31 2.9619 . 4_655
no
C11 H31 2.9995 . 4_655
no
C12 H21 3.0528 . 4_655
no
C12 H31 2.9013 . 4_655
no
C14 H51 3.0721 . 1_655
no
C15 H171 3.0914 . 4_554
no
C15 H4 2.8133 . 3_655
no
C16 H4 2.6868 . 3_655
no
C17 H101 3.0743 . .
no
C17 H151 2.8691 . 4_555
no
C20 H502 2.9416 . 4_554
no
C20 H212 2.8360 . .
no
C20 H504 2.8826 . 4_554
no
C21 H202 2.7947 . .
no
C50 H201 2.9095 . 4_555
no
H4 H151 2.3932 . 3_655
no
H4 C15 2.8133 . 3_655
no
H4 C16 2.6868 . 3_655
no
H4 Co1 3.3381 . 3_655
no
H4 O2 2.0124 . 3_655
no
H4 H202 2.4215 . 3_655
no
H21 H221 2.4318 . 3_655
no
H21 C12 3.0528 . 4_454
no
H21 H121 2.5651 . 4_454
no
H31 C11 2.9995 . 4_454
no
H31 C12 2.9013 . 4_454
no
H31 C10 2.9619 . 4_454
no
H41 H172 2.5590 . 4_454
no
H51 C14 3.0721 . 1_455
no
H51 H71 2.3847 . .
no
H71 H81 2.2508 . .
no
H71 H51 2.3847 . .
no
H81 H71 2.2508 . .
no
H81 H171 2.4646 . .
no
H81 O3 2.8292 . 2_655
no
H91 H101 2.2855 . .
no
H91 Cl2 3.0561 . 3_666
no
H91 Cl21 3.0242 . 3_666
no
H101 Cl11 2.7428 . 1_655
no
H101 Cl1 2.6993 . 1_655
no
H101 H91 2.2855 . .
no
H101 H121 2.3518 . .
no
H101 C17 3.0743 . .
no
H121 H101 2.3518 . .
no
H121 C2 3.0858 . 4_655
no
H121 H21 2.5651 . 4_655
no
H131 Cl2 3.0405 . 4_654
no
H141 C4 2.9968 . 1_655
no
H141 Cl2 2.9326 . 4_654
no
H141 Cl21 2.8057 . 4_654
no
H151 O4 2.5828 . 3_655
no
H151 H181 2.5052 . 4_554
no
H151 H4 2.3932 . 3_655
no
H151 C17 2.8691 . 4_554
no
H151 H171 2.3122 . 4_554
no
H171 Cl21 2.9527 . 3_666
no
H171 C15 3.0914 . 4_555
no
H171 H151 2.3122 . 4_555
no
H171 Cl2 3.1026 . 3_666
no
H171 H81 2.4646 . .
no
H171 O4 2.8692 . 2_655
no
H172 C10 2.9158 . .
no
H172 H191 2.4934 . .
no
H172 H41 2.5590 . 4_655
no
H181 H151 2.5052 . 4_555
no
H182 C7 2.9659 . .
no
H182 C8 2.8776 . .
no
H182 N1 2.6789 . .
no
H182 H201 2.3760 . .
no
H191 N2 2.6310 . .
no
H191 C10 2.8325 . .
no
H191 H211 2.2021 . .
no
H191 H172 2.4934 . .
no
H201 C6 2.7306 . .
no
H201 C7 2.7889 . .
no
H201 C1 2.7203 . .
no
H201 H504 2.1423 . 4_554
no
H201 Cl2 3.0836 . 4_554
no
H201 C50 2.9095 . 4_554
no
H201 H182 2.3760 . .
no
H201 H502 2.2690 . 4_554
no
H202 C21 2.7947 . .
no
H202 H212 2.2302 . .
no
H202 O4 2.9179 . 3_655
no
H202 H4 2.4215 . 3_655
no
H211 H191 2.2021 . .
no
H211 Cl11 2.8496 . 2_645
no
H212 H202 2.2302 . .
no
H212 Cl11 3.0470 . 2_645
no
H212 C20 2.8360 . .
no
H221 H21 2.4318 . 3_655
no
H221 C2 2.9679 . 3_655
no
H501 O3 2.9140 . 4_555
no
H501 O4 2.3440 . 4_555
no
H502 C20 2.9416 . 4_555
no
H502 H201 2.2690 . 4_555
no
H503 O3 2.8255 . 4_555
no
H503 O4 2.3629 . 4_555
no
H504 C20 2.8826 . 4_555
no
H504 H201 2.1423 . 4_555
no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D H A D - H H...A D...A D - H...A symm(A)
#
O4 H4 O2 0.8400 2.0124 2.819(7) 160.86
3_655 yes
C10 H101 Cl1 0.9508 2.6993 3.610(13) 160.72
1_655 yes
C15 H151 O4 0.9492 2.5828 3.151(10) 118.74
3_655 yes
C50 H501 O4 0.9893 2.3440 3.323(11) 170.22
4_555 yes