#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/56/7005690.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_7005690
loop_
_publ_author_name
'Broge, Louise'
'Søtofte, Inger'
'Jensen, Kristian'
'Jensen, Nicolai'
'Pretzmann, Ulla'
'Springborg, Johan'
_publ_section_title
;
 Bowl adamanzanes--bicyclic tetraamines: syntheses and crystal
 structures of complexes with cobalt(III) and chelating coordinated
 oxo-anions.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3826
_journal_page_last               3839
_journal_paper_doi               10.1039/b704451h
_journal_year                    2007
_chemical_formula_moiety         '[Co(C11H24N4)(H2O)(OH)](ClO4)2,1.75H2O'
_chemical_formula_sum            'C11 H30.5 Cl2 Co N4 O11.75'
_chemical_formula_weight         536.72
_chemical_name_systematic
;
?
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.9090(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.2694(9)
_cell_length_b                   12.2362(6)
_cell_length_c                   19.6977(9)
_cell_measurement_reflns_used    27972
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      1.23
_cell_volume                     3993.8(3)
_computing_cell_refinement       'SAINT (Bruker AXS,1998)'
_computing_data_collection       'SMART (Bruker AXS,1998)'
_computing_data_reduction        'SAINT (Bruker AXS,1998)'
_computing_molecular_graphics    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_structure_refinement  'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_structure_solution    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens SMART CCD Platform'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27972
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,ver2.03 (Sheldrick,2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.754
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         9614
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0667
_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)+(0.0927P)²+10.8502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                7300
_reflns_number_total             9614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704451h.txt
_cod_data_source_block           315ak
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C11 H30.50 Cl2 Co N4 O11.75'
_cod_database_code               7005690
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_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
Co1 Co 0.03392(3) 0.15962(4) 0.07756(3) 0.01210(13) Uani 1 1 d . . .
O1 O 0.08659(18) 0.1136(2) 0.01524(17) 0.0226(6) Uani 1 1 d D . .
H1O1 H 0.089(3) 0.042(2) 0.032(3) 0.027 Uiso 1 1 d D . .
H2O1 H 0.076(3) 0.151(3) -0.0269(17) 0.027 Uiso 1 1 d D . .
O2 O -0.05830(17) 0.0868(2) 0.00192(16) 0.0224(6) Uani 1 1 d . . .
H2 H -0.0846 0.1315 -0.0320 0.027 Uiso 1 1 calc R . .
N1 N 0.0016(2) 0.3002(3) 0.0287(2) 0.0233(7) Uani 1 1 d . . .
H1 H -0.0181 0.2884 -0.0226 0.028 Uiso 1 1 calc R . .
C1 C -0.0655(3) 0.3472(3) 0.0437(3) 0.0283(10) Uani 1 1 d . . .
H11 H -0.1098 0.3708 -0.0040 0.034 Uiso 1 1 calc R . .
H12 H -0.0460 0.4119 0.0765 0.034 Uiso 1 1 calc R . .
C2 C -0.0977(3) 0.2600(4) 0.0821(3) 0.0284(9) Uani 1 1 d . . .
H21 H -0.1247 0.2968 0.1101 0.034 Uiso 1 1 calc R . .
H22 H -0.1377 0.2126 0.0436 0.034 Uiso 1 1 calc R . .
N2 N -0.0299(2) 0.1927(3) 0.1340(2) 0.0236(7) Uani 1 1 d . . .
C3 C -0.0593(3) 0.0826(3) 0.1450(3) 0.0280(10) Uani 1 1 d . . .
H31 H -0.1007 0.0547 0.0970 0.034 Uiso 1 1 calc R . .
H32 H -0.0834 0.0874 0.1815 0.034 Uiso 1 1 calc R . .
C4 C 0.0159(3) 0.0047(3) 0.1752(2) 0.0280(10) Uani 1 1 d . . .
H41 H 0.0476 0.0168 0.2295 0.034 Uiso 1 1 calc R . .
H42 H -0.0023 -0.0724 0.1675 0.034 Uiso 1 1 calc R . .
N3 N 0.0670(2) 0.0270(3) 0.13465(19) 0.0216(7) Uani 1 1 d . . .
H3 H 0.0608 -0.0305 0.1018 0.026 Uiso 1 1 calc R . .
C5 C 0.1541(3) 0.0349(3) 0.1872(2) 0.0283(10) Uani 1 1 d . . .
H51 H 0.1820 -0.0339 0.1859 0.034 Uiso 1 1 calc R . .
H52 H 0.1594 0.0459 0.2389 0.034 Uiso 1 1 calc R . .
C6 C 0.1943(3) 0.1335(4) 0.1642(2) 0.0266(9) Uani 1 1 d . . .
H61 H 0.2459 0.1539 0.2063 0.032 Uiso 1 1 calc R . .
H62 H 0.2054 0.1133 0.1208 0.032 Uiso 1 1 calc R . .
N4 N 0.1364(2) 0.2261(3) 0.1446(2) 0.0229(7) Uani 1 1 d . . .
C7 C 0.1515(3) 0.3063(4) 0.0942(3) 0.0279(9) Uani 1 1 d . . .
H71 H 0.1673 0.2667 0.0585 0.033 Uiso 1 1 calc R . .
H72 H 0.1961 0.3560 0.1243 0.033 Uiso 1 1 calc R . .
C8 C 0.0739(3) 0.3726(3) 0.0510(2) 0.0215(8) Uani 1 1 d . . .
H81 H 0.0701 0.4329 0.0829 0.026 Uiso 1 1 calc R . .
H82 H 0.0758 0.4051 0.0057 0.026 Uiso 1 1 calc R . .
C9 C 0.0089(3) 0.2467(4) 0.2092(3) 0.0308(10) Uani 1 1 d . . .
H91 H 0.0337 0.1894 0.2476 0.037 Uiso 1 1 calc R . .
H92 H -0.0338 0.2825 0.2198 0.037 Uiso 1 1 calc R . .
C10 C 0.0735(3) 0.3319(3) 0.2173(2) 0.0265(9) Uani 1 1 d . . .
H101 H 0.0512 0.3849 0.1755 0.032 Uiso 1 1 calc R . .
H102 H 0.0881 0.3725 0.2647 0.032 Uiso 1 1 calc R . .
C11 C 0.1466(3) 0.2808(4) 0.2170(3) 0.0293(10) Uani 1 1 d . . .
H111 H 0.1666 0.2256 0.2575 0.035 Uiso 1 1 calc R . .
H112 H 0.1888 0.3377 0.2292 0.035 Uiso 1 1 calc R . .
Co2 Co 0.46243(3) 0.84501(4) 0.41623(3) 0.01341(13) Uani 1 1 d . . .
O1A O 0.41268(19) 0.9597(2) 0.44890(17) 0.0239(6) Uani 1 1 d D . .
H1A1 H 0.413(3) 0.898(3) 0.476(2) 0.029 Uiso 1 1 d D . .
H2A1 H 0.3595(13) 0.956(4) 0.437(3) 0.029 Uiso 1 1 d D . .
O2A O 0.5404(2) 0.8490(2) 0.52018(17) 0.0347(8) Uani 1 1 d . . .
H2A H 0.5612 0.9116 0.5304 0.042 Uiso 1 1 calc R . .
N1A N 0.5244(2) 0.9504(3) 0.3889(2) 0.0228(7) Uani 1 1 d . . .
H1A H 0.5439 1.0029 0.4265 0.027 Uiso 1 1 calc R . .
C1A C 0.4709(3) 1.0062(3) 0.3174(2) 0.0232(8) Uani 1 1 d . . .
H11A H 0.4867 0.9841 0.2771 0.028 Uiso 1 1 calc R . .
H12A H 0.4776 1.0863 0.3238 0.028 Uiso 1 1 calc R . .
C2A C 0.3822(2) 0.9755(3) 0.2954(2) 0.0202(8) Uani 1 1 d . . .
H21A H 0.3595 1.0211 0.3234 0.024 Uiso 1 1 calc R . .
H22A H 0.3499 0.9878 0.2412 0.024 Uiso 1 1 calc R . .
N2A N 0.3794(2) 0.8574(3) 0.31393(19) 0.0191(7) Uani 1 1 d . . .
C3A C 0.3022(2) 0.8298(3) 0.3194(3) 0.0265(9) Uani 1 1 d . . .
H31A H 0.2599 0.8126 0.2691 0.032 Uiso 1 1 calc R . .
H32A H 0.2838 0.8935 0.3392 0.032 Uiso 1 1 calc R . .
C4A C 0.3147(3) 0.7315(4) 0.3714(3) 0.0338(11) Uani 1 1 d . . .
H41A H 0.2747 0.7340 0.3931 0.041 Uiso 1 1 calc R . .
H42A H 0.3061 0.6631 0.3422 0.041 Uiso 1 1 calc R . .
N3A N 0.3982(2) 0.7319(3) 0.4332(2) 0.0270(8) Uani 1 1 d . . .
H3A H 0.3936 0.7492 0.4772 0.032 Uiso 1 1 calc R . .
C5A C 0.4419(3) 0.6243(3) 0.4456(3) 0.0279(10) Uani 1 1 d . . .
H51A H 0.4132 0.5752 0.4025 0.033 Uiso 1 1 calc R . .
H52A H 0.4430 0.5888 0.4912 0.033 Uiso 1 1 calc R . .
C6A C 0.5285(3) 0.6430(3) 0.4544(2) 0.0245(9) Uani 1 1 d . . .
H61A H 0.5630 0.6664 0.5063 0.029 Uiso 1 1 calc R . .
H62A H 0.5507 0.5740 0.4447 0.029 Uiso 1 1 calc R . .
N4A N 0.5286(2) 0.7290(3) 0.40041(19) 0.0195(7) Uani 1 1 d . . .
C7A C 0.6092(2) 0.7830(3) 0.4244(3) 0.0274(9) Uani 1 1 d . . .
H71A H 0.6453 0.7373 0.4103 0.033 Uiso 1 1 calc R . .
H72A H 0.6346 0.7932 0.4794 0.033 Uiso 1 1 calc R . .
C8A C 0.5950(3) 0.8938(4) 0.3847(3) 0.0324(11) Uani 1 1 d . . .
H81A H 0.6438 0.9398 0.4086 0.039 Uiso 1 1 calc R . .
H82A H 0.5847 0.8830 0.3317 0.039 Uiso 1 1 calc R . .
C9A C 0.3864(3) 0.7913(4) 0.2523(2) 0.0296(10) Uani 1 1 d . . .
H91A H 0.3323 0.7861 0.2102 0.036 Uiso 1 1 calc R . .
H92A H 0.4217 0.8314 0.2340 0.036 Uiso 1 1 calc R . .
C10A C 0.4192(3) 0.6779(4) 0.2735(3) 0.0307(10) Uani 1 1 d . . .
H11B H 0.3891 0.6402 0.2983 0.037 Uiso 1 1 calc R . .
H12B H 0.4108 0.6366 0.2276 0.037 Uiso 1 1 calc R . .
C11A C 0.5065(3) 0.6782(3) 0.3246(2) 0.0249(9) Uani 1 1 d . . .
H21B H 0.5357 0.7178 0.2997 0.030 Uiso 1 1 calc R . .
H22B H 0.5260 0.6017 0.3320 0.030 Uiso 1 1 calc R . .
Cl1 Cl 0.12569(6) -0.34235(9) 0.17426(6) 0.0277(2) Uani 1 1 d . . .
O3 O 0.0484(2) -0.3962(3) 0.1402(2) 0.0402(9) Uani 1 1 d . . .
O4 O 0.1204(3) -0.2436(4) 0.1329(2) 0.0647(13) Uani 1 1 d . . .
O5 O 0.1429(3) -0.3140(5) 0.2478(2) 0.087(2) Uani 1 1 d . . .
O6 O 0.1847(3) -0.4079(5) 0.1669(4) 0.100(2) Uani 1 1 d . . .
Cl2 Cl 0.79413(6) 0.95609(8) 0.58233(6) 0.0212(2) Uani 1 1 d . . .
O7 O 0.7618(2) 1.0648(3) 0.5610(2) 0.0390(8) Uani 1 1 d . . .
O8 O 0.87764(19) 0.9630(3) 0.63267(19) 0.0382(8) Uani 1 1 d . . .
O9 O 0.7850(2) 0.8971(3) 0.51687(19) 0.0387(8) Uani 1 1 d . . .
O10 O 0.7502(2) 0.9034(3) 0.6188(2) 0.0378(8) Uani 1 1 d . . .
Cl3 Cl 0.29204(6) 0.94325(9) 0.05744(6) 0.0250(2) Uani 1 1 d . . .
O11 O 0.23983(19) 0.8948(3) 0.0870(2) 0.0403(9) Uani 1 1 d . . .
O12 O 0.2727(5) 1.0609(4) 0.0432(4) 0.0506(18) Uani 0.712(10) 1 d P . .
O12' O 0.3092(12) 1.0444(12) 0.0888(11) 0.0506(18) Uani 0.288(10) 1 d P . .
O13 O 0.3739(3) 0.9345(6) 0.1089(4) 0.057(2) Uani 0.784(11) 1 d P . .
O13' O 0.3678(11) 0.874(2) 0.0759(13) 0.057(2) Uani 0.216(11) 1 d P . .
O14 O 0.2783(4) 0.8896(7) -0.0096(4) 0.0376(15) Uani 0.624(10) 1 d P . .
O14' O 0.2613(8) 0.9420(11) -0.0229(7) 0.0376(15) Uani 0.376(10) 1 d P . .
Cl4 Cl 0.38891(10) 0.34466(10) 0.31239(8) 0.0480(4) Uani 1 1 d . . .
O15 O 0.3673(4) 0.2668(5) 0.2583(4) 0.062(2) Uani 0.848(13) 1 d P . .
O15' O 0.376(2) 0.238(3) 0.302(2) 0.062(2) Uani 0.152(13) 1 d P . .
O16 O 0.3516(4) 0.3674(9) 0.3574(3) 0.058(2) Uani 0.794(17) 1 d P . .
O16' O 0.3488(16) 0.304(3) 0.3555(15) 0.058(2) Uani 0.206(17) 1 d P . .
O17 O 0.4470(4) 0.4166(6) 0.3114(6) 0.069(2) Uani 0.750(15) 1 d P . .
O17' O 0.4557(15) 0.395(2) 0.3543(18) 0.069(2) Uani 0.250(15) 1 d P . .
O18 O 0.4677(5) 0.2697(7) 0.3732(5) 0.0572(17) Uani 0.50 1 d P . .
O18' O 0.3253(5) 0.4224(7) 0.2479(5) 0.0572(17) Uani 0.50 1 d P . .
O20 O 0.0754(2) 0.2750(3) 0.39629(19) 0.0338(8) Uani 1 1 d D . .
H201 H 0.1240(19) 0.308(4) 0.414(3) 0.041 Uiso 1 1 d D . .
H202 H 0.058(3) 0.209(2) 0.379(3) 0.041 Uiso 1 1 d D . .
O30 O 0.2122(3) 0.3564(4) 0.3961(3) 0.0602(12) Uani 1 1 d D . .
H301 H 0.237(4) 0.404(5) 0.434(3) 0.072 Uiso 1 1 d D . .
H302 H 0.257(3) 0.344(6) 0.388(4) 0.072 Uiso 1 1 d D . .
O40 O 0.5682(4) 0.2222(6) 0.4118(4) 0.0378(9) Uani 0.50 1 d P . .
O40' O 0.6246(4) 0.1666(6) 0.4318(4) 0.0378(9) Uani 0.50 1 d P . .
O50 O 0.7043(4) 0.1286(6) 0.4115(4) 0.0378(9) Uani 0.50 1 d P . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Co1 O2 91.09(13) . . ?
N3 Co1 O1 90.45(14) . . ?
O2 Co1 O1 83.21(12) . . ?
N3 Co1 N1 174.51(15) . . ?
O2 Co1 N1 92.41(13) . . ?
O1 Co1 N1 94.17(14) . . ?
N3 Co1 N4 88.88(15) . . ?
O2 Co1 N4 170.86(13) . . ?
O1 Co1 N4 87.65(14) . . ?
N1 Co1 N4 88.34(15) . . ?
N3 Co1 N2 87.58(15) . . ?
O2 Co1 N2 89.93(13) . . ?
O1 Co1 N2 172.82(13) . . ?
N1 Co1 N2 88.19(15) . . ?
N4 Co1 N2 99.20(15) . . ?
Co1 O1 H1O1 91(3) . . ?
Co1 O1 H2O1 118(3) . . ?
H1O1 O1 H2O1 140(4) . . ?
Co1 O2 H2 109.5 . . ?
C1 N1 C8 114.4(3) . . ?
C1 N1 Co1 110.4(3) . . ?
C8 N1 Co1 109.5(3) . . ?
C1 N1 H1 107.4 . . ?
C8 N1 H1 107.4 . . ?
Co1 N1 H1 107.4 . . ?
N1 C1 C2 109.9(3) . . ?
N1 C1 H11 109.7 . . ?
C2 C1 H11 109.7 . . ?
N1 C1 H12 109.7 . . ?
C2 C1 H12 109.7 . . ?
H11 C1 H12 108.2 . . ?
N2 C2 C1 109.9(3) . . ?
N2 C2 H21 109.7 . . ?
C1 C2 H21 109.7 . . ?
N2 C2 H22 109.7 . . ?
C1 C2 H22 109.7 . . ?
H21 C2 H22 108.2 . . ?
C2 N2 C9 110.3(3) . . ?
C2 N2 C3 110.7(3) . . ?
C9 N2 C3 107.6(3) . . ?
C2 N2 Co1 104.3(3) . . ?
C9 N2 Co1 120.2(3) . . ?
C3 N2 Co1 103.4(2) . . ?
N2 C3 C4 106.9(3) . . ?
N2 C3 H31 110.3 . . ?
C4 C3 H31 110.3 . . ?
N2 C3 H32 110.3 . . ?
C4 C3 H32 110.3 . . ?
H31 C3 H32 108.6 . . ?
N3 C4 C3 109.4(3) . . ?
N3 C4 H41 109.8 . . ?
C3 C4 H41 109.8 . . ?
N3 C4 H42 109.8 . . ?
C3 C4 H42 109.8 . . ?
H41 C4 H42 108.2 . . ?
C4 N3 C5 111.5(3) . . ?
C4 N3 Co1 110.8(3) . . ?
C5 N3 Co1 109.4(3) . . ?
C4 N3 H3 108.3 . . ?
C5 N3 H3 108.3 . . ?
Co1 N3 H3 108.3 . . ?
N3 C5 C6 109.9(3) . . ?
N3 C5 H51 109.7 . . ?
C6 C5 H51 109.7 . . ?
N3 C5 H52 109.7 . . ?
C6 C5 H52 109.7 . . ?
H51 C5 H52 108.2 . . ?
N4 C6 C5 106.9(3) . . ?
N4 C6 H61 110.3 . . ?
C5 C6 H61 110.3 . . ?
N4 C6 H62 110.3 . . ?
C5 C6 H62 110.3 . . ?
H61 C6 H62 108.6 . . ?
C6 N4 C7 111.1(3) . . ?
C6 N4 C11 107.5(3) . . ?
C7 N4 C11 110.5(3) . . ?
C6 N4 Co1 103.5(3) . . ?
C7 N4 Co1 102.4(3) . . ?
C11 N4 Co1 121.5(3) . . ?
N4 C7 C8 109.1(3) . . ?
N4 C7 H71 109.9 . . ?
C8 C7 H71 109.9 . . ?
N4 C7 H72 109.9 . . ?
C8 C7 H72 109.9 . . ?
H71 C7 H72 108.3 . . ?
N1 C8 C7 110.1(3) . . ?
N1 C8 H81 109.6 . . ?
C7 C8 H81 109.6 . . ?
N1 C8 H82 109.6 . . ?
C7 C8 H82 109.6 . . ?
H81 C8 H82 108.2 . . ?
N2 C9 C10 115.2(3) . . ?
N2 C9 H91 108.5 . . ?
C10 C9 H91 108.5 . . ?
N2 C9 H92 108.5 . . ?
C10 C9 H92 108.5 . . ?
H91 C9 H92 107.5 . . ?
C11 C10 C9 111.7(4) . . ?
C11 C10 H101 109.3 . . ?
C9 C10 H101 109.3 . . ?
C11 C10 H102 109.3 . . ?
C9 C10 H102 109.3 . . ?
H101 C10 H102 108.0 . . ?
C10 C11 N4 116.0(4) . . ?
C10 C11 H111 108.3 . . ?
N4 C11 H111 108.3 . . ?
C10 C11 H112 108.3 . . ?
N4 C11 H112 108.3 . . ?
H111 C11 H112 107.4 . . ?
O1A Co2 N3A 93.32(14) . . ?
O1A Co2 N1A 91.23(14) . . ?
N3A Co2 N1A 173.68(16) . . ?
O1A Co2 O2A 82.48(13) . . ?
N3A Co2 O2A 93.77(16) . . ?
N1A Co2 O2A 91.18(16) . . ?
O1A Co2 N2A 91.02(13) . . ?
N3A Co2 N2A 88.25(15) . . ?
N1A Co2 N2A 87.28(14) . . ?
O2A Co2 N2A 173.28(13) . . ?
O1A Co2 N4A 170.05(14) . . ?
N3A Co2 N4A 88.21(14) . . ?
N1A Co2 N4A 88.07(14) . . ?
O2A Co2 N4A 87.62(13) . . ?
N2A Co2 N4A 98.86(14) . . ?
O1A Co2 H1A1 27.9(6) . . ?
N3A Co2 H1A1 69.8(10) . . ?
N1A Co2 H1A1 115.7(10) . . ?
O2A Co2 H1A1 70.3(14) . . ?
N2A Co2 H1A1 104.5(14) . . ?
N4A Co2 H1A1 147.0(8) . . ?
Co2 O1A H1A1 73(3) . . ?
Co2 O1A H2A1 120(3) . . ?
H1A1 O1A H2A1 82(4) . . ?
Co2 O2A H2A 109.5 . . ?
C8A N1A C1A 113.2(4) . . ?
C8A N1A Co2 109.0(2) . . ?
C1A N1A Co2 109.8(2) . . ?
C8A N1A H1A 108.2 . . ?
C1A N1A H1A 108.2 . . ?
Co2 N1A H1A 108.2 . . ?
N1A C1A C2A 110.2(3) . . ?
N1A C1A H11A 109.6 . . ?
C2A C1A H11A 109.6 . . ?
N1A C1A H12A 109.6 . . ?
C2A C1A H12A 109.6 . . ?
H11A C1A H12A 108.1 . . ?
N2A C2A C1A 107.9(3) . . ?
N2A C2A H21A 110.1 . . ?
C1A C2A H21A 110.1 . . ?
N2A C2A H22A 110.1 . . ?
C1A C2A H22A 110.1 . . ?
H21A C2A H22A 108.4 . . ?
C2A N2A C3A 111.3(3) . . ?
C2A N2A C9A 107.4(3) . . ?
C3A N2A C9A 109.9(3) . . ?
C2A N2A Co2 103.6(2) . . ?
C3A N2A Co2 104.7(3) . . ?
C9A N2A Co2 119.8(3) . . ?
N2A C3A C4A 110.1(3) . . ?
N2A C3A H31A 109.6 . . ?
C4A C3A H31A 109.6 . . ?
N2A C3A H32A 109.6 . . ?
C4A C3A H32A 109.6 . . ?
H31A C3A H32A 108.2 . . ?
N3A C4A C3A 110.8(3) . . ?
N3A C4A H41A 109.5 . . ?
C3A C4A H41A 109.5 . . ?
N3A C4A H42A 109.5 . . ?
C3A C4A H42A 109.5 . . ?
H41A C4A H42A 108.1 . . ?
C4A N3A C5A 114.7(4) . . ?
C4A N3A Co2 110.3(3) . . ?
C5A N3A Co2 109.6(3) . . ?
C4A N3A H3A 107.3 . . ?
C5A N3A H3A 107.3 . . ?
Co2 N3A H3A 107.3 . . ?
N3A C5A C6A 109.8(3) . . ?
N3A C5A H51A 109.7 . . ?
C6A C5A H51A 109.7 . . ?
N3A C5A H52A 109.7 . . ?
C6A C5A H52A 109.7 . . ?
H51A C5A H52A 108.2 . . ?
N4A C6A C5A 109.5(3) . . ?
N4A C6A H61A 109.8 . . ?
C5A C6A H61A 109.8 . . ?
N4A C6A H62A 109.8 . . ?
C5A C6A H62A 109.8 . . ?
H61A C6A H62A 108.2 . . ?
C7A N4A C6A 112.4(3) . . ?
C7A N4A C11A 108.1(3) . . ?
C6A N4A C11A 109.5(3) . . ?
C7A N4A Co2 102.7(2) . . ?
C6A N4A Co2 102.1(2) . . ?
C11A N4A Co2 121.9(2) . . ?
N4A C7A C8A 107.3(3) . . ?
N4A C7A H71A 110.3 . . ?
C8A C7A H71A 110.3 . . ?
N4A C7A H72A 110.3 . . ?
C8A C7A H72A 110.3 . . ?
H71A C7A H72A 108.5 . . ?
N1A C8A C7A 110.2(4) . . ?
N1A C8A H81A 109.6 . . ?
C7A C8A H81A 109.6 . . ?
N1A C8A H82A 109.6 . . ?
C7A C8A H82A 109.6 . . ?
H81A C8A H82A 108.1 . . ?
C10A C9A N2A 115.6(4) . . ?
C10A C9A H91A 108.4 . . ?
N2A C9A H91A 108.4 . . ?
C10A C9A H92A 108.4 . . ?
N2A C9A H92A 108.4 . . ?
H91A C9A H92A 107.5 . . ?
C11A C10A C9A 112.1(4) . . ?
C11A C10A H11B 109.2 . . ?
C9A C10A H11B 109.2 . . ?
C11A C10A H12B 109.2 . . ?
C9A C10A H12B 109.2 . . ?
H11B C10A H12B 107.9 . . ?
C10A C11A N4A 115.7(3) . . ?
C10A C11A H21B 108.3 . . ?
N4A C11A H21B 108.3 . . ?
C10A C11A H22B 108.3 . . ?
N4A C11A H22B 108.3 . . ?
H21B C11A H22B 107.4 . . ?
O5 Cl1 O6 113.9(4) . . ?
O5 Cl1 O4 108.2(3) . . ?
O6 Cl1 O4 107.0(4) . . ?
O5 Cl1 O3 110.2(3) . . ?
O6 Cl1 O3 109.7(3) . . ?
O4 Cl1 O3 107.6(2) . . ?
O9 Cl2 O8 110.0(2) . . ?
O9 Cl2 O10 110.4(2) . . ?
O8 Cl2 O10 109.7(2) . . ?
O9 Cl2 O7 109.0(2) . . ?
O8 Cl2 O7 109.5(2) . . ?
O10 Cl2 O7 108.3(2) . . ?
O12' Cl3 O14 140.4(8) . . ?
O12' Cl3 O13 76.8(9) . . ?
O14 Cl3 O13 110.8(5) . . ?
O12' Cl3 O11 104.9(7) . . ?
O14 Cl3 O11 107.7(3) . . ?
O13 Cl3 O11 111.1(3) . . ?
O12' Cl3 O14' 114.6(10) . . ?
O14 Cl3 O14' 29.1(4) . . ?
O13 Cl3 O14' 126.4(6) . . ?
O11 Cl3 O14' 115.0(5) . . ?
O12' Cl3 O12 36.1(7) . . ?
O14 Cl3 O12 110.1(5) . . ?
O13 Cl3 O12 107.8(4) . . ?
O11 Cl3 O12 109.4(3) . . ?
O14' Cl3 O12 81.3(6) . . ?
O12' Cl3 O13' 112.5(13) . . ?
O14 Cl3 O13' 75.5(11) . . ?
O13 Cl3 O13' 37.8(9) . . ?
O11 Cl3 O13' 111.4(8) . . ?
O14' Cl3 O13' 98.7(11) . . ?
O12 Cl3 O13' 134.6(9) . . ?
O12' O12 Cl3 64.5(11) . . ?
O12 O12' Cl3 79.4(14) . . ?
O12 O12' O13 124.1(15) . . ?
Cl3 O12' O13 53.0(6) . . ?
O13' O13 Cl3 77.7(13) . . ?
O13' O13 O12' 125.0(15) . . ?
Cl3 O13 O12' 50.2(7) . . ?
O13 O13' Cl3 64.5(16) . . ?
O13 O13' O14 111(2) . . ?
Cl3 O13' O14 49.0(6) . . ?
O14' O14 Cl3 78.5(13) . . ?
O14' O14 O13' 121.5(17) . . ?
Cl3 O14 O13' 55.5(10) . . ?
O14 O14' Cl3 72.5(13) . . ?
O17' Cl4 O15' 128(2) . . ?
O17' Cl4 O16 94.8(12) . . ?
O15' Cl4 O16 101.6(16) . . ?
O17' Cl4 O15 135.4(11) . . ?
O15' Cl4 O15 38.3(17) . . ?
O16 Cl4 O15 126.6(5) . . ?
O17' Cl4 O17 36.1(12) . . ?
O15' Cl4 O17 135.0(15) . . ?
O16 Cl4 O17 118.6(5) . . ?
O15 Cl4 O17 114.0(4) . . ?
O17' Cl4 O16' 111.4(18) . . ?
O15' Cl4 O16' 69(2) . . ?
O16 Cl4 O16' 32.4(12) . . ?
O15 Cl4 O16' 99.8(14) . . ?
O17 Cl4 O16' 145.0(14) . . ?
O17' Cl4 O18' 113.1(14) . . ?
O15' Cl4 O18' 116.0(19) . . ?
O16 Cl4 O18' 90.0(5) . . ?
O15 Cl4 O18' 85.5(5) . . ?
O17 Cl4 O18' 85.3(5) . . ?
O16' Cl4 O18' 107.1(13) . . ?
O17' Cl4 O18 61.2(14) . . ?
O15' Cl4 O18 67.5(18) . . ?
O16 Cl4 O18 99.2(5) . . ?
O15 Cl4 O18 93.1(5) . . ?
O17 Cl4 O18 85.7(5) . . ?
O16' Cl4 O18 83.5(13) . . ?
O18' Cl4 O18 169.4(4) . . ?
O15' O15 Cl4 69(2) . . ?
O15 O15' Cl4 73(3) . . ?
O15 O15' O16' 118(4) . . ?
Cl4 O15' O16' 58.4(18) . . ?
O15 O15' O18 116(3) . . ?
Cl4 O15' O18 66.9(13) . . ?
O16' O15' O18 79.3(18) . . ?
O16' O16 Cl4 79(2) . . ?
O16 O16' Cl4 69(2) . . ?
O16 O16' O15' 121(3) . . ?
Cl4 O16' O15' 52.2(16) . . ?
O17' O17 Cl4 66.5(15) . . ?
O17 O17' Cl4 77(2) . . ?
O17 O17' O18 120(2) . . ?
Cl4 O17' O18 72.1(11) . . ?
O17' O18 Cl4 46.7(10) . . ?
O17' O18 O15' 91.9(17) . . ?
Cl4 O18 O15' 45.6(13) . . ?
O17' O18 O40 116.2(10) . . ?
Cl4 O18 O40 154.2(6) . . ?
O15' O18 O40 139.4(13) . . ?
H201 O20 H202 134(5) . . ?
H301 O30 H302 94(6) . . ?
O40' O40 O18 163.1(7) . . ?
O40 O40' O50 142.8(7) . . ?
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
Co1 N3 1.921(3) . ?
Co1 O2 1.933(3) . ?
Co1 O1 1.935(3) . ?
Co1 N1 1.938(3) . ?
Co1 N4 1.956(3) . ?
Co1 N2 1.963(3) . ?
O1 H1O1 0.931(19) . ?
O1 H2O1 0.893(19) . ?
O2 H2 0.8400 . ?
N1 C1 1.491(5) . ?
N1 C8 1.496(5) . ?
N1 H1 0.9300 . ?
C1 C2 1.559(6) . ?
C1 H11 0.9900 . ?
C1 H12 0.9900 . ?
C2 N2 1.480(6) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
N2 C9 1.499(6) . ?
N2 C3 1.499(5) . ?
C3 C4 1.569(7) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
C4 N3 1.488(5) . ?
C4 H41 0.9900 . ?
C4 H42 0.9900 . ?
N3 C5 1.492(5) . ?
N3 H3 0.9300 . ?
C5 C6 1.574(6) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N4 1.486(5) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N4 C7 1.503(5) . ?
N4 C11 1.514(5) . ?
C7 C8 1.542(6) . ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 C10 1.532(6) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 C11 1.477(6) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
Co2 O1A 1.924(3) . ?
Co2 N3A 1.933(4) . ?
Co2 N1A 1.935(3) . ?
Co2 O2A 1.941(3) . ?
Co2 N2A 1.952(3) . ?
Co2 N4A 1.972(3) . ?
Co2 H1A1 1.87(5) . ?
O1A H1A1 0.916(19) . ?
O1A H2A1 0.900(19) . ?
O2A H2A 0.8400 . ?
N1A C8A 1.496(5) . ?
N1A C1A 1.498(5) . ?
N1A H1A 0.9300 . ?
C1A C2A 1.539(6) . ?
C1A H11A 0.9900 . ?
C1A H12A 0.9900 . ?
C2A N2A 1.496(5) . ?
C2A H21A 0.9900 . ?
C2A H22A 0.9900 . ?
N2A C3A 1.499(5) . ?
N2A C9A 1.508(5) . ?
C3A C4A 1.533(6) . ?
C3A H31A 0.9900 . ?
C3A H32A 0.9900 . ?
C4A N3A 1.498(6) . ?
C4A H41A 0.9900 . ?
C4A H42A 0.9900 . ?
N3A C5A 1.506(5) . ?
N3A H3A 0.9300 . ?
C5A C6A 1.533(6) . ?
C5A H51A 0.9900 . ?
C5A H52A 0.9900 . ?
C6A N4A 1.498(5) . ?
C6A H61A 0.9900 . ?
C6A H62A 0.9900 . ?
N4A C7A 1.497(5) . ?
N4A C11A 1.507(5) . ?
C7A C8A 1.532(6) . ?
C7A H71A 0.9900 . ?
C7A H72A 0.9900 . ?
C8A H81A 0.9900 . ?
C8A H82A 0.9900 . ?
C9A C10A 1.499(6) . ?
C9A H91A 0.9900 . ?
C9A H92A 0.9900 . ?
C10A C11A 1.485(6) . ?
C10A H11B 0.9900 . ?
C10A H12B 0.9900 . ?
C11A H21B 0.9900 . ?
C11A H22B 0.9900 . ?
Cl1 O5 1.391(5) . ?
Cl1 O6 1.400(5) . ?
Cl1 O4 1.437(4) . ?
Cl1 O3 1.442(3) . ?
Cl2 O9 1.425(3) . ?
Cl2 O8 1.430(3) . ?
Cl2 O10 1.436(3) . ?
Cl2 O7 1.444(3) . ?
Cl3 O12' 1.359(15) . ?
Cl3 O14 1.401(6) . ?
Cl3 O13 1.413(5) . ?
Cl3 O11 1.438(3) . ?
Cl3 O14' 1.439(12) . ?
Cl3 O12 1.480(6) . ?
Cl3 O13' 1.53(2) . ?
O12 O12' 0.888(18) . ?
O12' O13 1.722(18) . ?
O13 O13' 0.96(3) . ?
O13' O14 1.80(2) . ?
O14 O14' 0.714(11) . ?
Cl4 O17' 1.30(2) . ?
Cl4 O15' 1.32(3) . ?
Cl4 O16 1.355(6) . ?
Cl4 O15 1.358(5) . ?
Cl4 O17 1.385(6) . ?
Cl4 O16' 1.42(3) . ?
Cl4 O18' 1.621(7) . ?
Cl4 O18 1.702(7) . ?
O15 O15' 0.88(4) . ?
O15' O16' 1.57(4) . ?
O15' O18 1.71(4) . ?
O16 O16' 0.78(3) . ?
O17 O17' 0.84(3) . ?
O17' O18 1.57(3) . ?
O18 O40 1.764(11) . ?
O20 H201 0.90(2) . ?
O20 H202 0.89(2) . ?
O30 H301 0.90(2) . ?
O30 H302 0.91(2) . ?
O40 O40' 1.156(10) . ?
O40' O50 1.728(10) . ?
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
O1 H1O1 O2 0.931(19) 1.71(3) 2.500(4) 141(4) 3
O1 H2O1 O20 0.893(19) 1.76(2) 2.643(4) 169(5) 4_565
O2A H2A O1A 0.84 1.65 2.479(4) 170.2 3_676
O20 H201 O30 0.90(2) 1.88(3) 2.692(6) 148(5) .
N1 H1 O4 0.93 2.26 3.100(6) 150.3 3
N3 H3 O2 0.93 2.14 2.973(4) 148.9 3
N1A H1A O1A 0.93 2.29 3.105(5) 146.7 3_676
N3A H3A O40 0.93 2.03 2.905(8) 157.0 3_666
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
Co1 N1 C1 C2 -9.5(4) . . . . ?
N1 C1 C2 N2 36.3(5) . . . . ?
C1 C2 N2 Co1 -44.2(4) . . . . ?
C2 N2 Co1 N1 32.1(3) . . . . ?
N2 Co1 N1 C1 -12.6(3) . . . . ?
Co1 N2 C3 C4 48.9(4) . . . . ?
N2 C3 C4 N3 -40.7(4) . . . . ?
C3 C4 N3 Co1 11.8(4) . . . . ?
C4 N3 Co1 N2 13.4(3) . . . . ?
N3 Co1 N2 C3 -35.6(3) . . . . ?
Co1 N3 C5 C6 -14.5(4) . . . . ?
N3 C5 C6 N4 42.4(5) . . . . ?
C5 C6 N4 Co1 -48.1(3) . . . . ?
C6 N4 Co1 N3 34.0(3) . . . . ?
N4 Co1 N3 C5 -10.7(3) . . . . ?
Co1 N4 C7 C8 47.8(4) . . . . ?
N4 C7 C8 N1 -38.8(5) . . . . ?
C7 C8 N1 Co1 9.4(4) . . . . ?
C8 N1 Co1 N4 14.9(3) . . . . ?
N1 Co1 N4 C7 -35.1(3) . . . . ?
Co1 N2 C9 C10 36.2(5) . . . . ?
N2 C9 C10 C11 -69.4(5) . . . . ?
C9 C10 C11 N4 65.6(5) . . . . ?
C10 C11 N4 Co1 -30.5(5) . . . . ?
C11 N4 Co1 N2 0.8(3) . . . . ?
N4 Co1 N2 C9 -4.2(3) . . . . ?
Co1 N2 C9 C10 36.2(5) . . . . ?
Co2 N1A C1A C2A 8.9(4) . . . . ?
N1A C1A C2A N2A -38.4(4) . . . . ?
C1A C2A N2A Co2 48.5(3) . . . . ?
C2A N2A Co2 N1A -36.2(2) . . . . ?
N2A Co2 N1A C1A 15.6(3) . . . . ?
Co2 N2A C3A C4A -42.5(4) . . . . ?
N2A C3A C4A N3A 33.6(5) . . . . ?
C3A C4A N3A Co2 -7.5(5) . . . . ?
C4A N3A Co2 N2A -13.8(3) . . . . ?
N3A Co2 N2A C3A 31.5(2) . . . . ?
Co2 N3A C5A C6A 9.9(4) . . . . ?
N3A C5A C6A N4A -39.5(5) . . . . ?
C5A C6A N4A Co2 48.1(3) . . . . ?
C6A N4A Co2 N3A -34.8(3) . . . . ?
N4A Co2 N3A C5A 14.5(3) . . . . ?
Co2 N4A C7A C8A -49.5(4) . . . . ?
N4A C7A C8A N1A 44.6(5) . . . . ?
C7A C8A N1A Co2 -16.4(5) . . . . ?
C8A N1A Co2 N4A -10.0(3) . . . . ?
N1A Co2 N4A C7A 33.7(3) . . . . ?
Co2 N2A C9A C10A 37.7(5) . . . . ?
N2A C9A C10A C11A -70.6(5) . . . . ?
C9A C10A C11A N4A 64.4(5) . . . . ?
C10A C11A N4A Co2 -28.0(5) . . . . ?
C11A N4A Co2 N2A -0.4(3) . . . . ?
N4A Co2 N2A C9A -4.3(3) . . . . ?
Co2 N2A C9A C10A 37.7(5) . . . . ?
