#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:14:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179959 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/53/7025377.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7025377
loop_
_publ_author_name
'Dimiza, Filitsa'
'Papadopoulos, Athanasios N.'
'Tangoulis, Vassilis'
'Psycharis, Vassilis'
'Raptopoulou, Catherine P.'
'Kessissoglou, Dimitris P.'
'Psomas, George'
_publ_section_title
;
 Biological evaluation of non-steroidal anti-inflammatory drugs-cobalt(II)
 complexes.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4517
_journal_page_last               4528
_journal_paper_doi               10.1039/b927472c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C36 H52 Co N2 O10'
_chemical_formula_weight         731.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.2790(10)
_cell_angle_beta                 99.2940(10)
_cell_angle_gamma                92.7690(10)
_cell_formula_units_Z            1
_cell_length_a                   7.66020(10)
_cell_length_b                   7.88870(10)
_cell_length_c                   15.7633(3)
_cell_measurement_reflns_used    12175
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      71.75
_cell_measurement_theta_min      6.92
_cell_volume                     938.88(2)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Rigaku, R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11946
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.92
_exptl_absorpt_coefficient_mu    4.053
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             389
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.67
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0133(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0686P)²+0.8212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                2743
_reflns_number_total             2968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b927472c.txt
_cod_data_source_block           psfd27
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025377
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Co Co 0.0000 0.5000 0.0000 0.0272(3) Uani 1 2 d S
O1 O 0.0386(3) 0.4615(3) 0.13075(12) 0.0317(5) Uani 1 1 d .
O21 O 0.2365(5) 0.6469(7) 0.01182(19) 0.1052(18) Uani 1 1 d .
H21O H 0.283(10) 0.667(10) -0.025(5) 0.137 Uiso 1 1 d .
O22 O 0.1420(7) 0.2901(6) -0.01671(19) 0.123(2) Uani 1 1 d .
H22O H 0.206(11) 0.300(11) 0.022(5) 0.160 Uiso 1 1 d .
O2 O 0.2637(3) 0.2914(3) 0.14652(13) 0.0464(7) Uani 1 1 d .
N N -0.0553(4) 0.6063(3) 0.26637(16) 0.0289(6) Uani 1 1 d .
C1 C 0.1615(4) 0.3860(4) 0.17685(18) 0.0264(7) Uani 1 1 d .
C2 C 0.1851(4) 0.4120(3) 0.27242(17) 0.0216(6) Uani 1 1 d .
C3 C 0.3182(4) 0.3255(3) 0.32319(18) 0.0240(6) Uani 1 1 d .
C4 C 0.3505(4) 0.3425(4) 0.41150(19) 0.0267(7) Uani 1 1 d .
C5 C 0.2466(4) 0.4475(4) 0.45106(18) 0.0272(7) Uani 1 1 d .
C6 C 0.1138(4) 0.5340(4) 0.40304(18) 0.0243(6) Uani 1 1 d .
C7 C 0.0786(4) 0.5191(3) 0.31295(17) 0.0218(6) Uani 1 1 d .
C8 C -0.1695(4) 0.7106(4) 0.30350(17) 0.0243(6) Uani 1 1 d .
C9 C -0.3435(4) 0.6550(4) 0.30238(19) 0.0279(7) Uani 1 1 d .
C10 C -0.4574(5) 0.7532(4) 0.3386(2) 0.0313(7) Uani 1 1 d .
C11 C -0.3961(5) 0.9072(4) 0.3770(2) 0.0320(7) Uani 1 1 d .
C12 C -0.2217(4) 0.9667(4) 0.3781(2) 0.0329(7) Uani 1 1 d .
C13 C -0.1073(4) 0.8693(4) 0.3394(2) 0.0309(7) Uani 1 1 d .
C14 C 0.0793(5) 0.9359(5) 0.3345(3) 0.0515(10) Uani 1 1 d .
H14A H 0.1530 0.9280 0.3912 0.067 Uiso 1 1 calc R
H14B H 0.0774 1.0547 0.3166 0.067 Uiso 1 1 calc R
H14C H 0.1285 0.8681 0.2926 0.067 Uiso 1 1 calc R
C15 C -0.1581(6) 1.1367(5) 0.4196(3) 0.0599(12) Uani 1 1 d .
H15A H -0.1258 1.2147 0.3759 0.078 Uiso 1 1 calc R
H15B H -0.0544 1.1219 0.4638 0.078 Uiso 1 1 calc R
H15C H -0.2528 1.1836 0.4461 0.078 Uiso 1 1 calc R
C21 C 0.3480(8) 0.7196(8) 0.0811(3) 0.091(2) Uani 1 1 d .
H21A H 0.2859 0.7228 0.1308 0.118 Uiso 1 1 calc R
H21B H 0.3845 0.8354 0.0670 0.118 Uiso 1 1 calc R
H21C H 0.4528 0.6522 0.0950 0.118 Uiso 1 1 calc R
C22 C 0.1371(8) 0.1593(6) -0.0682(3) 0.0752(15) Uani 1 1 d .
H22A H 0.1647 0.0575 -0.0343 0.098 Uiso 1 1 calc R
H22B H 0.2243 0.1786 -0.1068 0.098 Uiso 1 1 calc R
H22C H 0.0184 0.1438 -0.1023 0.098 Uiso 1 1 calc R
CM C 0.3082(7) 0.8137(6) -0.1857(3) 0.0673(13) Uani 1 1 d .
HCMA H 0.1906 0.8366 -0.1727 0.088 Uiso 1 1 calc R
HCMB H 0.2962 0.7640 -0.2436 0.088 Uiso 1 1 calc R
HCMC H 0.3806 0.9200 -0.1828 0.088 Uiso 1 1 calc R
OM O 0.3875(6) 0.7029(7) -0.1272(3) 0.1041(17) Uani 1 1 d .
H1N H -0.084(5) 0.577(4) 0.217(2) 0.036(10) Uiso 1 1 d .
HOM H 0.4613 0.676(6) -0.130(3) 0.056(16) Uiso 1 1 d .
H3 H 0.387(4) 0.253(4) 0.296(2) 0.029(8) Uiso 1 1 d .
H4 H 0.444(5) 0.281(4) 0.445(2) 0.038(9) Uiso 1 1 d .
H5 H 0.266(4) 0.461(4) 0.513(2) 0.028(8) Uiso 1 1 d .
H6 H 0.045(4) 0.598(4) 0.4276(19) 0.019(7) Uiso 1 1 d .
H9 H -0.384(4) 0.545(4) 0.2765(19) 0.024(8) Uiso 1 1 d .
H10 H -0.575(5) 0.714(4) 0.336(2) 0.034(9) Uiso 1 1 d .
H11 H -0.475(5) 0.981(5) 0.402(2) 0.042(10) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Co O1 180.00(12) 2_565 .
O1 Co O22 90.16(11) 2_565 2_565
O1 Co O22 89.84(11) . 2_565
O1 Co O22 89.84(11) 2_565 .
O1 Co O22 90.16(11) . .
O22 Co O22 180.00(16) 2_565 .
O1 Co O21 89.41(10) 2_565 .
O1 Co O21 90.59(10) . .
O22 Co O21 91.8(2) 2_565 .
O22 Co O21 88.2(2) . .
O1 Co O21 90.59(10) 2_565 2_565
O1 Co O21 89.41(10) . 2_565
O22 Co O21 88.2(2) 2_565 2_565
O22 Co O21 91.8(2) . 2_565
O21 Co O21 180.0 . 2_565
C1 O1 Co 128.86(17) . .
C21 O21 Co 133.2(3) . .
C21 O21 H21O 104(6) . .
Co O21 H21O 123(6) . .
C22 O22 Co 140.1(3) . .
C22 O22 H22O 122(7) . .
Co O22 H22O 98(7) . .
C7 N C8 124.2(2) . .
C7 N H1N 116(3) . .
C8 N H1N 118(3) . .
O2 C1 O1 123.3(3) . .
O2 C1 C2 118.7(3) . .
O1 C1 C2 118.0(2) . .
C3 C2 C7 119.1(2) . .
C3 C2 C1 117.8(2) . .
C7 C2 C1 123.1(3) . .
C4 C3 C2 121.9(3) . .
C4 C3 H3 119(2) . .
C2 C3 H3 119(2) . .
C3 C4 C5 118.9(3) . .
C3 C4 H4 120(2) . .
C5 C4 H4 121(2) . .
C6 C5 C4 120.7(3) . .
C6 C5 H5 118.6(19) . .
C4 C5 H5 120.7(19) . .
C5 C6 C7 121.4(3) . .
C5 C6 H6 121(2) . .
C7 C6 H6 117(2) . .
N C7 C6 120.4(3) . .
N C7 C2 121.7(2) . .
C6 C7 C2 117.9(3) . .
C9 C8 C13 120.4(3) . .
C9 C8 N 119.1(3) . .
C13 C8 N 120.5(3) . .
C8 C9 C10 120.5(3) . .
C8 C9 H9 119.0(19) . .
C10 C9 H9 120.6(19) . .
C9 C10 C11 119.7(3) . .
C9 C10 H10 119(2) . .
C11 C10 H10 121(2) . .
C10 C11 C12 120.8(3) . .
C10 C11 H11 122(2) . .
C12 C11 H11 117(2) . .
C11 C12 C13 119.5(3) . .
C11 C12 C15 119.9(3) . .
C13 C12 C15 120.6(3) . .
C8 C13 C12 119.0(3) . .
C8 C13 C14 120.3(3) . .
C12 C13 C14 120.6(3) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
O21 C21 H21A 109.5 . .
O21 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
O21 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
O22 C22 H22A 109.5 . .
O22 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
O22 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
OM CM HCMA 109.5 . .
OM CM HCMB 109.5 . .
HCMA CM HCMB 109.5 . .
OM CM HCMC 109.5 . .
HCMA CM HCMC 109.5 . .
HCMB CM HCMC 109.5 . .
CM OM HOM 122(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co O1 2.0604(18) 2_565
Co O1 2.0604(18) .
Co O22 2.063(3) 2_565
Co O22 2.063(3) .
Co O21 2.084(3) .
Co O21 2.084(3) 2_565
O1 C1 1.267(4) .
O21 C21 1.377(6) .
O21 H21O 0.74(7) .
O22 C22 1.305(5) .
O22 H22O 0.73(8) .
O2 C1 1.254(4) .
N C7 1.376(4) .
N C8 1.420(4) .
N H1N 0.81(4) .
C1 C2 1.500(4) .
C2 C3 1.398(4) .
C2 C7 1.420(4) .
C3 C4 1.379(4) .
C3 H3 0.94(3) .
C4 C5 1.388(4) .
C4 H4 0.97(4) .
C5 C6 1.377(4) .
C5 H5 0.97(3) .
C6 C7 1.405(4) .
C6 H6 0.88(3) .
C8 C9 1.381(4) .
C8 C13 1.401(4) .
C9 C10 1.381(4) .
C9 H9 0.97(3) .
C10 C11 1.382(5) .
C10 H10 0.94(4) .
C11 C12 1.392(5) .
C11 H11 0.99(4) .
C12 C13 1.401(4) .
C12 C15 1.513(5) .
C13 C14 1.513(5) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
CM OM 1.364(6) .
CM HCMA 0.9800 .
CM HCMB 0.9800 .
CM HCMC 0.9800 .
OM HOM 0.62(2) .
