#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:16:38 +0100 (vie 25 de mar de 2016) $
#$Revision: 179807 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/03/7010382.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_7010382
loop_
_publ_author_name
'Clarkson, Andrea J.'
'Blackman, Allan G.'
'Clark, Charles R.'
_publ_section_title
;
 Preparation, structures and reactions of isomeric
 [Co(cyclen)(O2C2O2)]+ and [Co(cyclen)(O2CCH2CO2)]+ complexes
 (cyclen = 1,4,7,10-tetraazacyclododecane) †
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              758
_journal_paper_doi               10.1039/b008350j
_journal_year                    2001
_chemical_formula_sum            'C10 H20 Cl Co N4 O8'
_chemical_formula_weight         418.68
_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                77.850(18)
_cell_angle_beta                 86.805(18)
_cell_angle_gamma                68.773(11)
_cell_formula_units_Z            2
_cell_length_a                   7.406(4)
_cell_length_b                   8.610(5)
_cell_length_c                   14.305(10)
_cell_measurement_reflns_used    8909
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.59
_cell_volume                     831.0(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'WINGX (Farrugia, 1999)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8909
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.480126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          1.01
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0801P)²+1.5461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                2785
_reflns_number_total             2986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008350j.txt
_cod_data_source_block           cycox
_cod_original_cell_volume        831.1(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010382
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.30186(6) 0.33210(6) 0.19869(3) 0.01781(19) Uani 1 1 d . . .
Cl2 Cl 0.18354(14) -0.19944(12) 0.40701(7) 0.0302(3) Uani 1 1 d . . .
O1 O 0.1914(4) 0.5548(3) 0.11237(18) 0.0231(5) Uani 1 1 d . . .
O4 O 0.5463(3) 0.3747(3) 0.18413(18) 0.0213(5) Uani 1 1 d . . .
N1 N 0.0404(4) 0.3244(4) 0.2026(2) 0.0208(6) Uani 1 1 d . . .
H1C H -0.0339 0.4242 0.1617 0.025 Uiso 1 1 calc R . .
N3 N 0.4361(4) 0.1125(4) 0.2853(2) 0.0219(6) Uani 1 1 d . . .
H3C H 0.3473 0.0600 0.3065 0.026 Uiso 1 1 calc R . .
O3 O 0.6661(4) 0.5750(4) 0.1038(2) 0.0291(6) Uani 1 1 d . . .
N4 N 0.2375(4) 0.4249(4) 0.3184(2) 0.0225(6) Uani 1 1 d . . .
H4C H 0.2723 0.5201 0.3118 0.027 Uiso 1 1 calc R . .
O2 O 0.2865(4) 0.7653(3) 0.02340(19) 0.0291(6) Uani 1 1 d . . .
N2 N 0.3517(4) 0.1944(4) 0.0957(2) 0.0191(6) Uani 1 1 d . . .
H2C H 0.4066 0.2443 0.0435 0.023 Uiso 1 1 calc R . .
C10 C 0.5311(5) 0.5192(5) 0.1256(2) 0.0215(7) Uani 1 1 d . . .
C2 C 0.1552(5) 0.1952(5) 0.0654(3) 0.0231(7) Uani 1 1 d . . .
H2A H 0.1745 0.0974 0.0350 0.028 Uiso 1 1 calc R . .
H2B H 0.0870 0.3015 0.0189 0.028 Uiso 1 1 calc R . .
C9 C 0.3184(5) 0.6286(4) 0.0815(2) 0.0202(7) Uani 1 1 d . . .
C1 C 0.0343(5) 0.1827(5) 0.1573(3) 0.0233(7) Uani 1 1 d . . .
H1A H -0.1006 0.1995 0.1411 0.028 Uiso 1 1 calc R . .
H1B H 0.0927 0.0706 0.2007 0.028 Uiso 1 1 calc R . .
C3 C 0.4901(5) 0.0109(5) 0.1345(3) 0.0261(8) Uani 1 1 d . . .
H3A H 0.5894 -0.0262 0.0866 0.031 Uiso 1 1 calc R . .
H3B H 0.4164 -0.0667 0.1464 0.031 Uiso 1 1 calc R . .
C8 C -0.0460(5) 0.3405(5) 0.3007(3) 0.0254(8) Uani 1 1 d . . .
H8A H 0.0062 0.2310 0.3471 0.030 Uiso 1 1 calc R . .
H8B H -0.1889 0.3770 0.2974 0.030 Uiso 1 1 calc R . .
C4 C 0.5898(5) 0.0022(5) 0.2286(3) 0.0269(8) Uani 1 1 d . . .
H4A H 0.6423 -0.1167 0.2650 0.032 Uiso 1 1 calc R . .
H4B H 0.6976 0.0452 0.2148 0.032 Uiso 1 1 calc R . .
C7 C 0.0169(5) 0.4787(5) 0.3292(3) 0.0254(8) Uani 1 1 d . . .
H7A H -0.0492 0.5908 0.2870 0.030 Uiso 1 1 calc R . .
H7B H -0.0182 0.4880 0.3961 0.030 Uiso 1 1 calc R . .
C5 C 0.5156(5) 0.1486(5) 0.3705(3) 0.0266(8) Uani 1 1 d . . .
H5A H 0.6259 0.1866 0.3515 0.032 Uiso 1 1 calc R . .
H5B H 0.5607 0.0450 0.4217 0.032 Uiso 1 1 calc R . .
C6 C 0.3479(6) 0.2903(5) 0.4058(3) 0.0284(8) Uani 1 1 d . . .
H6A H 0.3997 0.3443 0.4470 0.034 Uiso 1 1 calc R . .
H6B H 0.2586 0.2411 0.4440 0.034 Uiso 1 1 calc R . .
O5 O 0.2285(5) -0.0626(4) 0.4352(2) 0.0427(8) Uani 1 1 d . . .
O6 O 0.2311(6) -0.3488(5) 0.4851(3) 0.0567(10) Uani 1 1 d . . .
O7 O 0.3030(6) -0.2450(5) 0.3241(3) 0.0566(10) Uani 1 1 d . . .
O8 O -0.0212(6) -0.1404(6) 0.3801(4) 0.0755(13) Uani 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 0.0033 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
N1 Co1 O1 86.51(12) . . ?
N1 Co1 O4 171.49(11) . . ?
O1 Co1 O4 85.05(10) . . ?
N1 Co1 N3 98.91(13) . . ?
O1 Co1 N3 174.54(11) . . ?
O4 Co1 N3 89.51(12) . . ?
N1 Co1 N4 86.83(12) . . ?
O1 Co1 N4 94.71(13) . . ?
O4 Co1 N4 92.77(11) . . ?
N3 Co1 N4 85.05(13) . . ?
N1 Co1 N2 86.08(12) . . ?
O1 Co1 N2 95.69(12) . . ?
O4 Co1 N2 95.83(11) . . ?
N3 Co1 N2 85.33(13) . . ?
N4 Co1 N2 167.03(12) . . ?
O8 Cl2 O6 109.9(3) . . ?
O8 Cl2 O5 110.2(2) . . ?
O6 Cl2 O5 110.6(2) . . ?
O8 Cl2 O7 109.5(3) . . ?
O6 Cl2 O7 109.2(2) . . ?
O5 Cl2 O7 107.4(2) . . ?
C9 O1 Co1 114.3(2) . . ?
C10 O4 Co1 113.3(2) . . ?
C1 N1 C8 119.4(3) . . ?
C1 N1 Co1 110.8(2) . . ?
C8 N1 Co1 110.8(2) . . ?
C4 N3 C5 114.0(3) . . ?
C4 N3 Co1 107.7(2) . . ?
C5 N3 Co1 107.9(2) . . ?
C7 N4 C6 111.7(3) . . ?
C7 N4 Co1 106.9(2) . . ?
C6 N4 Co1 110.8(2) . . ?
C2 N2 C3 110.6(3) . . ?
C2 N2 Co1 107.5(2) . . ?
C3 N2 Co1 109.9(2) . . ?
O3 C10 O4 125.8(3) . . ?
O3 C10 C9 119.6(3) . . ?
O4 C10 C9 114.6(3) . . ?
N2 C2 C1 107.3(3) . . ?
O2 C9 O1 126.7(3) . . ?
O2 C9 C10 120.7(3) . . ?
O1 C9 C10 112.6(3) . . ?
N1 C1 C2 104.2(3) . . ?
N2 C3 C4 110.0(3) . . ?
N1 C8 C7 103.9(3) . . ?
N3 C4 C3 106.6(3) . . ?
N4 C7 C8 107.7(3) . . ?
N3 C5 C6 106.4(3) . . ?
C5 C6 N4 109.1(3) . . ?
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 N1 1.959(3) . ?
Co1 O1 1.962(3) . ?
Co1 O4 1.965(3) . ?
Co1 N3 1.972(3) . ?
Co1 N4 2.002(3) . ?
Co1 N2 2.017(3) . ?
Cl2 O8 1.460(4) . ?
Cl2 O6 1.462(4) . ?
Cl2 O5 1.470(3) . ?
Cl2 O7 1.474(3) . ?
O1 C9 1.323(4) . ?
O4 C10 1.316(4) . ?
N1 C1 1.512(5) . ?
N1 C8 1.521(5) . ?
N3 C4 1.515(5) . ?
N3 C5 1.517(5) . ?
O3 C10 1.256(4) . ?
N4 C7 1.537(4) . ?
N4 C6 1.547(5) . ?
O2 C9 1.242(5) . ?
N2 C2 1.539(4) . ?
N2 C3 1.542(4) . ?
C10 C9 1.598(5) . ?
C2 C1 1.556(5) . ?
C3 C4 1.546(5) . ?
C8 C7 1.558(5) . ?
C5 C6 1.542(6) . ?
