#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006454.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006454
loop_
_publ_author_name
'Dickman, M. H.'
_publ_section_title
;
Bis(1,1,1,5,5,5-hexafluoroacetylacetonato-O,O')bis(2,2,6,6-tetramethylpiperidinyl-1-oxy-O)cobalt(II)
;
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 1192
_journal_page_last 1195
_journal_volume 53
_journal_year 1997
_chemical_formula_moiety '[Co (C5 H1 F6 O2)2 (C9 H18 N1 O)2]'
_chemical_formula_sum 'C28 H38 Co F12 N2 O6'
_chemical_formula_weight 785.53
_chemical_name_systematic
;
bis(2,2,6,6-tetramethyl-piperidinyl-1-oxy-O)bis(1,1,1,5,5,5-
hexafluoroacetylacetonato-O,O")cobalt(II)
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_audit_creation_method SHELXL
_cell_angle_alpha 90.00
_cell_angle_beta 112.530(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 10.3960(10)
_cell_length_b 14.468(2)
_cell_length_c 12.155(2)
_cell_measurement_reflns_used 40
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 12.494
_cell_measurement_theta_min 4.831
_cell_volume 1688.7(4)
_computing_cell_refinement XSCANS
_computing_data_collection 'XSCANS (Siemens, 1990a)'
_computing_data_reduction XSCANS
_computing_molecular_graphics 'SHELXTL (Siemens, 1990b)'
_computing_publication_material SHELXTL
_computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_measurement_device 'Siemens P4/RA'
_diffrn_measurement_method '2\q/\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.049
_diffrn_reflns_av_sigmaI/netI 0.0544
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 9488
_diffrn_reflns_theta_max 28.51
_diffrn_reflns_theta_min 2.12
_diffrn_standards_decay_% 5.6
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.617
_exptl_absorpt_correction_type none
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.545
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Block
_exptl_crystal_F_000 806
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_refine_diff_density_max 0.43
_refine_diff_density_min -0.47
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.03
_refine_ls_goodness_of_fit_obs 1.089
_refine_ls_hydrogen_treatment 'H atoms refined isotropically'
_refine_ls_matrix_type full
_refine_ls_number_parameters 303
_refine_ls_number_reflns 3886
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.034
_refine_ls_restrained_S_obs 1.089
_refine_ls_R_factor_all 0.0711
_refine_ls_R_factor_obs 0.044
_refine_ls_shift/esd_max 0.017
_refine_ls_shift/esd_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.5850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.112
_refine_ls_wR_factor_obs 0.0989
_reflns_number_observed 2821
_reflns_number_total 3886
_reflns_observed_criterion >2sigma(I)
_[local]_cod_data_source_file bk1320.cif
_[local]_cod_data_source_block cot1
_cod_database_code 2006454
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co 0.0244(2) 0.0206(2) 0.0186(2) 0.0043(2) 0.0072(2) 0.0008(2)
N 0.0285(10) 0.0249(10) 0.0255(10) -0.0034(8) 0.0142(8) -0.0025(8)
O1 0.0356(12) 0.0320(10) 0.0251(10) -0.0046(9) 0.0172(9) -0.0008(8)
O2 0.0303(9) 0.0322(9) 0.0241(8) 0.0078(8) 0.0050(7) -0.0033(7)
O3 0.0283(9) 0.0238(8) 0.0253(8) 0.0025(7) 0.0100(7) -0.0005(7)
C1 0.0280(12) 0.0213(11) 0.0378(13) -0.0005(10) 0.0150(11) 0.0006(10)
C2 0.051(2) 0.0318(14) 0.048(2) 0.0024(13) 0.025(2) 0.0122(13)
C3 0.052(2) 0.043(2) 0.044(2) -0.0001(14) 0.032(2) 0.0116(13)
C4 0.0361(15) 0.045(2) 0.0263(12) 0.0053(12) 0.0165(12) 0.0051(11)
C5 0.0316(12) 0.0276(12) 0.0244(11) -0.0006(10) 0.0141(10) -0.0041(9)
C6 0.036(2) 0.0298(14) 0.053(2) 0.0022(12) 0.0192(14) -0.0059(13)
C7 0.0352(15) 0.0334(15) 0.045(2) -0.0033(12) 0.0146(13) -0.0108(13)
C8 0.046(2) 0.0293(13) 0.0370(15) 0.0087(13) 0.0162(13) 0.0011(12)
C9 0.045(2) 0.044(2) 0.039(2) -0.0158(14) 0.0236(14) -0.0191(13)
C10 0.0242(11) 0.0319(12) 0.0217(11) 0.0009(10) 0.0092(9) 0.0021(10)
C11 0.0232(12) 0.0288(12) 0.0301(12) 0.0071(10) 0.0076(10) 0.0054(10)
C12 0.0239(11) 0.0232(11) 0.0279(12) 0.0023(9) 0.0136(10) 0.0056(9)
C13 0.0268(12) 0.048(2) 0.0273(12) 0.0050(11) 0.0036(10) -0.0041(11)
C14 0.0328(13) 0.0237(11) 0.0375(13) 0.0028(10) 0.0157(11) 0.0018(10)
F1 0.0442(11) 0.153(2) 0.0357(9) 0.0253(13) 0.0018(8) -0.0413(12)
F2 0.0559(11) 0.0592(11) 0.0372(9) 0.0178(10) -0.0102(9) 0.0000(8)
F3 0.0678(14) 0.0719(14) 0.0554(12) -0.0338(12) -0.0043(11) -0.0030(10)
F4 0.124(2) 0.0353(9) 0.0819(14) 0.0160(11) 0.0830(14) 0.0049(9)
F5 0.0709(13) 0.0446(10) 0.0670(12) 0.0340(10) -0.0012(11) -0.0053(9)
F6 0.0516(11) 0.0294(8) 0.0914(15) -0.0069(8) 0.0319(11) -0.0149(9)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Co 0.0000 0.0000 0.0000 0.02149(13) Uani d S 1 Co
N 0.1751(2) 0.08668(13) -0.1517(2) 0.0251(4) Uani d . 1 N
O1 0.1533(2) 0.05383(14) -0.0607(2) 0.0293(4) Uani d P 0.90 O
O1A 0.084(2) 0.0768(14) -0.1034(19) 0.036(5) Uiso d P 0.10 O
O2 0.1543(2) 0.01076(12) 0.16462(14) 0.0305(4) Uani d . 1 O
O3 0.0730(2) -0.12909(11) -0.01484(14) 0.0259(4) Uani d . 1 O
C1 0.2281(3) 0.1845(2) -0.1349(2) 0.0284(5) Uani d . 1 C
C2 0.2425(4) 0.2182(2) -0.2494(3) 0.0418(7) Uani d . 1 C
C3 0.3131(4) 0.1484(2) -0.3005(3) 0.0422(7) Uani d . 1 C
C4 0.2235(3) 0.0623(2) -0.3345(2) 0.0344(6) Uani d . 1 C
C5 0.2042(3) 0.0156(2) -0.2291(2) 0.0269(5) Uani d . 1 C
C6 0.1227(3) 0.2435(2) -0.1087(3) 0.0389(6) Uani d . 1 C
C7 0.3681(3) 0.1865(2) -0.0300(3) 0.0382(6) Uani d . 1 C
C8 0.3364(3) -0.0370(2) -0.1523(3) 0.0372(6) Uani d . 1 C
C9 0.0809(3) -0.0498(2) -0.2746(3) 0.0405(7) Uani d . 1 C
C10 0.2473(2) -0.0472(2) 0.2128(2) 0.0258(5) Uani d . 1 C
C11 0.2683(3) -0.1329(2) 0.1695(2) 0.0281(5) Uani d . 1 C
C12 0.1805(2) -0.1657(2) 0.0586(2) 0.0239(5) Uani d . 1 C
C13 0.3530(3) -0.0160(2) 0.3352(2) 0.0359(6) Uani d . 1 C
C14 0.2175(3) -0.2582(2) 0.0161(2) 0.0307(5) Uani d . 1 C
F1 0.2909(2) 0.0181(2) 0.4010(2) 0.0816(8) Uani d . 1 F
F2 0.4368(2) -0.08258(13) 0.39626(15) 0.0592(5) Uani d . 1 F
F3 0.4343(2) 0.0499(2) 0.3220(2) 0.0734(7) Uani d . 1 F
F4 0.2489(3) -0.24676(12) -0.0782(2) 0.0673(6) Uani d . 1 F
F5 0.3239(2) -0.30157(13) 0.0971(2) 0.0691(6) Uani d . 1 F
F6 0.1119(2) -0.31680(11) -0.0146(2) 0.0561(5) Uani d . 1 F
H1C2 0.153(4) 0.231(2) -0.305(3) 0.053(10) Uiso d . 1 H
H2C2 0.290(4) 0.274(2) -0.232(3) 0.050(9) Uiso d . 1 H
H1C3 0.407(3) 0.1342(19) -0.244(3) 0.031(7) Uiso d . 1 H
H2C3 0.328(4) 0.174(2) -0.366(3) 0.055(10) Uiso d . 1 H
H1C4 0.135(3) 0.0805(18) -0.389(2) 0.025(7) Uiso d . 1 H
H2C4 0.258(3) 0.018(2) -0.371(3) 0.046(9) Uiso d . 1 H
H1C6 0.116(3) 0.2273(19) -0.037(3) 0.033(8) Uiso d . 1 H
H2C6 0.153(3) 0.307(2) -0.104(3) 0.037(8) Uiso d . 1 H
H3C6 0.030(3) 0.236(2) -0.174(3) 0.040(8) Uiso d . 1 H
H1C7 0.355(3) 0.163(2) 0.033(3) 0.037(8) Uiso d . 1 H
H2C7 0.403(3) 0.252(2) -0.017(3) 0.043(8) Uiso d . 1 H
H3C7 0.434(3) 0.153(2) -0.049(3) 0.046(9) Uiso d . 1 H
H1C8 0.348(3) -0.091(2) -0.195(3) 0.040(8) Uiso d . 1 H
H2C8 0.331(3) -0.058(2) -0.079(3) 0.043(8) Uiso d . 1 H
H3C8 0.421(4) -0.002(3) -0.138(3) 0.064(11) Uiso d . 1 H
H1C9 0.066(3) -0.082(2) -0.212(3) 0.041(8) Uiso d . 1 H
H2C9 0.104(3) -0.096(2) -0.329(3) 0.047(9) Uiso d . 1 H
H3C9 -0.006(4) -0.013(2) -0.323(3) 0.053(10) Uiso d . 1 H
H11C 0.338(3) -0.1674(19) 0.214(2) 0.030(7) Uiso d . 1 H
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Co O2 3 . 180.0 ?
O2 Co O3 3 3 88.70(6) ?
O2 Co O3 . 3 91.30(6) yes
O2 Co O3 3 . 91.30(6) ?
O2 Co O3 . . 88.70(6) yes
O3 Co O3 3 . 180.0 ?
O2 Co O1A 3 . 78.7(6) yes
O2 Co O1A . . 101.3(6) yes
O3 Co O1A 3 . 79.8(6) yes
O3 Co O1A . . 100.2(6) yes
O2 Co O1A 3 3 101.3(6) ?
O2 Co O1A . 3 78.7(6) ?
O3 Co O1A 3 3 100.2(6) ?
O3 Co O1A . 3 79.8(6) yes
O1A Co O1A . 3 180.0 ?
O2 Co O1 3 . 95.70(8) yes
O2 Co O1 . . 84.30(8) yes
O3 Co O1 3 . 92.79(7) yes
O3 Co O1 . . 87.21(7) yes
O1A Co O1 . . 21.3(6) yes
O1A Co O1 3 . 158.7(6) yes
O2 Co O1 3 3 84.30(8) ?
O2 Co O1 . 3 95.70(8) ?
O3 Co O1 3 3 87.21(7) ?
O3 Co O1 . 3 92.79(7) ?
O1A Co O1 . 3 158.7(6) ?
O1A Co O1 3 3 21.3(6) ?
O1 Co O1 . 3 180.0 ?
O1 N O1A . . 35.1(9) yes
O1 N C5 . . 115.1(2) yes
O1A N C5 . . 124.4(9) yes
O1 N C1 . . 113.8(2) yes
O1A N C1 . . 109.5(9) yes
C5 N C1 . . 125.3(2) yes
O1A O1 N . . 72.5(15) ?
O1A O1 Co . . 76.3(15) ?
N O1 Co . . 145.1(2) yes
O1 O1A N . . 72.4(16) ?
O1 O1A Co . . 82.5(15) ?
N O1A Co . . 150.4(15) yes
C10 O2 Co . . 126.1(2) yes
C12 O3 Co . . 125.7(2) yes
N C1 C6 . . 107.5(2) ?
N C1 C7 . . 108.3(2) ?
C6 C1 C7 . . 110.4(2) ?
N C1 C2 . . 109.5(2) ?
C6 C1 C2 . . 110.0(2) ?
C7 C1 C2 . . 111.0(2) ?
C3 C2 C1 . . 113.1(2) ?
C3 C2 H1C2 . . 110.(2) ?
C1 C2 H1C2 . . 108.(2) ?
C3 C2 H2C2 . . 112.(2) ?
C1 C2 H2C2 . . 107.(2) ?
H1C2 C2 H2C2 . . 106.(3) ?
C2 C3 C4 . . 108.4(3) ?
C2 C3 H1C3 . . 111.3(16) ?
C4 C3 H1C3 . . 111.3(16) ?
C2 C3 H2C3 . . 111.(2) ?
C4 C3 H2C3 . . 112.(2) ?
H1C3 C3 H2C3 . . 104.(3) ?
C3 C4 C5 . . 113.5(2) ?
C3 C4 H1C4 . . 107.2(16) ?
C5 C4 H1C4 . . 107.7(16) ?
C3 C4 H2C4 . . 113.(2) ?
C5 C4 H2C4 . . 107.4(19) ?
H1C4 C4 H2C4 . . 108.(3) ?
N C5 C9 . . 108.1(2) ?
N C5 C4 . . 110.2(2) ?
C9 C5 C4 . . 109.5(2) ?
N C5 C8 . . 107.9(2) ?
C9 C5 C8 . . 110.4(2) ?
C4 C5 C8 . . 110.8(2) ?
C1 C6 H1C6 . . 112.0(18) ?
C1 C6 H2C6 . . 107.5(17) ?
H1C6 C6 H2C6 . . 109.(2) ?
C1 C6 H3C6 . . 109.6(17) ?
H1C6 C6 H3C6 . . 109.(2) ?
H2C6 C6 H3C6 . . 110.(2) ?
C1 C7 H1C7 . . 107.3(19) ?
C1 C7 H2C7 . . 108.7(17) ?
H1C7 C7 H2C7 . . 113.(3) ?
C1 C7 H3C7 . . 109.7(19) ?
H1C7 C7 H3C7 . . 113.(3) ?
H2C7 C7 H3C7 . . 106.(3) ?
C5 C8 H1C8 . . 109.6(18) ?
C5 C8 H2C8 . . 111.0(19) ?
H1C8 C8 H2C8 . . 108.(3) ?
C5 C8 H3C8 . . 113.(2) ?
H1C8 C8 H3C8 . . 103.(3) ?
H2C8 C8 H3C8 . . 112.(3) ?
C5 C9 H1C9 . . 112.7(18) ?
C5 C9 H2C9 . . 105.3(18) ?
H1C9 C9 H2C9 . . 111.(2) ?
C5 C9 H3C9 . . 109.1(18) ?
H1C9 C9 H3C9 . . 109.(3) ?
H2C9 C9 H3C9 . . 110.(3) ?
O2 C10 C11 . . 128.8(2) yes
O2 C10 C13 . . 113.3(2) yes
C11 C10 C13 . . 117.8(2) yes
C12 C11 C10 . . 121.9(2) yes
C12 C11 H11C . . 119.1(18) ?
C10 C11 H11C . . 119.0(18) ?
O3 C12 C11 . . 128.5(2) yes
O3 C12 C14 . . 113.6(2) yes
C11 C12 C14 . . 117.9(2) yes
F1 C13 F2 . . 107.8(2) ?
F1 C13 F3 . . 106.9(3) ?
F2 C13 F3 . . 106.2(2) ?
F1 C13 C10 . . 111.5(2) ?
F2 C13 C10 . . 113.8(2) ?
F3 C13 C10 . . 110.3(2) ?
F4 C14 F6 . . 106.8(2) ?
F4 C14 F5 . . 107.0(2) ?
F6 C14 F5 . . 105.9(2) ?
F4 C14 C12 . . 111.1(2) ?
F6 C14 C12 . . 111.5(2) ?
F5 C14 C12 . . 114.2(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co O2 3 2.035(2) ?
Co O2 . 2.035(2) yes
Co O3 3 2.050(2) ?
Co O3 . 2.050(2) yes
Co O1A . 2.10(2) yes
Co O1A 3 2.10(2) ?
Co O1 . 2.143(2) yes
Co O1 3 2.143(2) ?
N O1 . 1.300(3) yes
N O1A . 1.30(2) yes
N C5 . 1.501(3) yes
N C1 . 1.504(3) yes
O1 O1A . 0.78(2) ?
O2 C10 . 1.244(3) yes
O3 C12 . 1.250(3) yes
C1 C6 . 1.517(4) ?
C1 C7 . 1.524(4) ?
C1 C2 . 1.535(4) ?
C2 C3 . 1.514(4) ?
C2 H1C2 . 0.94(3) ?
C2 H2C2 . 0.93(3) ?
C3 C4 . 1.515(4) ?
C3 H1C3 . 0.98(3) ?
C3 H2C3 . 0.94(4) ?
C4 C5 . 1.529(3) ?
C4 H1C4 . 0.94(3) ?
C4 H2C4 . 0.93(3) ?
C5 C9 . 1.517(4) ?
C5 C8 . 1.534(4) ?
C6 H1C6 . 0.93(3) ?
C6 H2C6 . 0.97(3) ?
C6 H3C6 . 0.99(3) ?
C7 H1C7 . 0.89(3) ?
C7 H2C7 . 1.01(3) ?
C7 H3C7 . 0.93(3) ?
C8 H1C8 . 0.96(3) ?
C8 H2C8 . 0.97(3) ?
C8 H3C8 . 0.97(4) ?
C9 H1C9 . 0.95(3) ?
C9 H2C9 . 1.03(3) ?
C9 H3C9 . 1.01(4) ?
C10 C11 . 1.396(3) yes
C10 C13 . 1.540(3) yes
C11 C12 . 1.391(3) yes
C11 H11C . 0.87(3) yes
C12 C14 . 1.536(3) yes
C13 F1 . 1.303(3) ?
C13 F2 . 1.320(3) ?
C13 F3 . 1.324(3) ?
C14 F4 . 1.317(3) ?
C14 F6 . 1.322(3) ?
C14 F5 . 1.323(3) ?
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
N O1 Co O2 -170.2(3)
N O1 Co O3 100.8(3)
N C1 C2 C3 -45.9(3)
C1 C2 C3 C4 62.7(3)
C2 C3 C4 C5 -61.5(3)
C3 C4 C5 N 43.8(3)
C4 C5 N C1 -30.3(3)
C5 N C1 C2 31.3(3)