#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/24/7012492.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_7012492
loop_
_publ_author_name
'Walker, Glen W.'
'Geue, Rodney J.'
'Haller, Kenneth J.'
'David Rae, A.'
'Sargeson, Alan M.'
_publ_section_title
;
 New synthetic routes to hexa-aza cages using cobalt(iii)
 tris(1,2-diamine) templates
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              279
_journal_paper_doi               10.1039/b211343k
_journal_year                    2003
_chemical_formula_moiety         '(C28 H54 N6 Co 3+), (Cl -)2, (Cl O4 -)'
_chemical_formula_sum            'C28 H54 Cl3 Co N6 O4'
_chemical_formula_weight         704.07
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      92
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_audit_creation_date             2002-03-14
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;

structure also known as glen

2002-03-15  run through checkcif
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.315(2)
_cell_length_b                   15.315(2)
_cell_length_c                   13.764(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      48.7
_cell_measurement_theta_min      40.3
_cell_volume                     3228.3(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'RAELS96 (Rae, 1996)'
_computing_structure_solution
;
Shelxs86 (Sheldrick, 1986)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and  evacuated collimator
and beam tunnel. Data cannot be collected beyond ψ 60 deg
in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10049
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        -2.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.8
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_density_meas      ?
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.5
_refine_diff_density_min         -0.9
_refine_ls_abs_structure_details
;
Absolute structure by comparative refinement.  Opposite hand in P4₃2₁2
gives R=0.126, wR=0.178, S=4.66.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.300
_refine_ls_goodness_of_fit_ref   1.376
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     184
_refine_ls_number_reflns         1752
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.0009|Fo|²]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0582
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                1752
_reflns_number_total             2414
_reflns_threshold_expression     I>3.00σ(I)
_cod_data_source_file            b211343k.txt
_cod_data_source_block           kjh3
_cod_original_cell_volume        3228(1)
_cod_original_formula_sum        'C28 H54 Cl3 Co N6 O4 '
_cod_database_code               7012492
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y, 1/2+z'
'   1/2-x,  1/2+y, 1/4-z'
'   1/2+x,  1/2-y, 3/4-z'
'   +y,   x, -z'
'   -y, -x, 1/2-z'
'   1/2-y,  1/2+x, 1/4+z'
'   1/2+y,  1/2-x, 3/4+z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_refinement_flags
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Co1 0.82504(5) 0.17496(5) 0.25000(0) 1.0 0.0305(3) . Uani d ?
C1 0.6866(4) 0.0346(4) 0.5045(4) 1.0 0.069(2) . Uani d ?
C2 0.7349(4) 0.0795(4) 0.4201(4) 1.0 0.056(2) . Uani d ?
C11 0.8302(4) 0.0660(4) 0.4300(4) 1.0 0.052(1) . Uani d ?
N12 0.8841(2) 0.0981(2) 0.3467(3) 1.0 0.036(1) . Uani d ?
C13 0.9311(3) 0.0261(3) 0.2942(3) 1.0 0.040(1) . Uani d ?
C14 0.9973(4) -0.0218(4) 0.3554(4) 1.0 0.055(1) . Uani d ?
C15 1.0455(4) -0.0873(4) 0.2946(5) 1.0 0.068(2) . Uani d ?
C21 0.7127(4) 0.1777(4) 0.4274(4) 1.0 0.060(2) . Uani d ?
N22 0.7565(3) 0.2348(3) 0.3527(3) 1.0 0.037(1) . Uani d ?
C23 0.8128(3) 0.3036(3) 0.3987(3) 1.0 0.041(1) . Uani d ?
C24 0.7604(4) 0.3738(4) 0.4515(4) 1.0 0.057(2) . Uani d ?
C25 0.8213(4) 0.4438(4) 0.4917(5) 1.0 0.068(2) . Uani d ?
C26 0.8788(4) 0.4820(4) 0.4129(5) 1.0 0.065(2) . Uani d ?
C27 0.9308(4) 0.4121(4) 0.3602(4) 1.0 0.056(2) . Uani d ?
C28 0.8674(3) 0.3448(3) 0.3190(4) 1.0 0.038(1) . Uani d ?
N29 0.9117(3) 0.2703(2) 0.2660(3) 1.0 0.037(1) . Uani d ?
C30 0.9559(4) 0.3001(4) 0.1737(4) 1.0 0.058(1) . Uani d ?
Cl1 1.0446(1) 0.2052(1) 0.4307(1) 1.0 0.056(1) . Uani d ?
Cl2 0.7358(6) 0.2733(7) 0.7400(8) 0.5 0.112(6) . Uani d ?
O1 0.8007(10) 0.2656(16) 0.6733(14) 0.5 0.243(10) . Uani d ?
O2 0.7677(11) 0.3115(13) 0.8218(14) 0.5 0.249(11) . Uani d ?
O3 0.6705(9) 0.3234(10) 0.7029(9) 0.5 0.177(8) . Uani d ?
O4 0.7041(14) 0.1928(9) 0.7621(18) 0.5 0.220(8) . Uani d ?
H1C1 0.6223 0.0440 0.4973 1.0 0.069 . Uani d ?
H2C1 0.6995 -0.0294 0.5035 1.0 0.069 . Uani d ?
H3C1 0.7068 0.0600 0.5676 1.0 0.069 . Uani d ?
H1C11 0.8410 0.0020 0.4373 1.0 0.052 . Uani d ?
H2C11 0.8501 0.0971 0.4899 1.0 0.052 . Uani d ?
H1N12 0.9310 0.1348 0.3765 1.0 0.036 . Uani d ?
H1C13 0.8868 -0.0169 0.2706 1.0 0.040 . Uani d ?
H1C14 0.9665 -0.0528 0.4095 1.0 0.055 . Uani d ?
H2C14 1.0398 0.0210 0.3832 1.0 0.055 . Uani d ?
H1C15 1.0036 -0.1333 0.2727 1.0 0.068 . Uani d ?
H2C15 1.0923 -0.1147 0.3350 1.0 0.068 . Uani d ?
H1C21 0.7307 0.1987 0.4933 1.0 0.060 . Uani d ?
H2C21 0.6481 0.1844 0.4199 1.0 0.060 . Uani d ?
H1N22 0.7085 0.2666 0.3185 1.0 0.037 . Uani d ?
H1C23 0.8528 0.2748 0.4464 1.0 0.041 . Uani d ?
H1C24 0.7274 0.3464 0.5063 1.0 0.057 . Uani d ?
H2C24 0.7184 0.4012 0.4050 1.0 0.057 . Uani d ?
H1C25 0.8591 0.4173 0.5430 1.0 0.068 . Uani d ?
H2C25 0.7853 0.4916 0.5209 1.0 0.068 . Uani d ?
H1C26 0.9204 0.5244 0.4432 1.0 0.065 . Uani d ?
H2C26 0.8412 0.5132 0.3648 1.0 0.065 . Uani d ?
H1C27 0.9717 0.3831 0.4066 1.0 0.056 . Uani d ?
H2C27 0.9649 0.4392 0.3061 1.0 0.056 . Uani d ?
H1C28 0.8273 0.3750 0.2726 1.0 0.038 . Uani d ?
H1N29 0.9586 0.2476 0.3099 1.0 0.037 . Uani d ?
H1C30 0.9516 0.3652 0.1711 1.0 0.058 . Uani d ?
H2C30 1.0187 0.2825 0.1778 1.0 0.058 . Uani d ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 112 0.0181 0.0091
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0 216 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Cl 0 12 0.3639 0.7018
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Co 0 4 -2.3653 3.6143
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N 0 24 0.00311 0.0180
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O 0 16 0.0492 0.0322
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 0 4
2 2 0
1 0 3
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
N22 Co1 N29 86.3(2) . . . yes
N12 Co1 N12 84.8(2) . . 6_665 yes
N12 Co1 N22 92.1(1) . . . yes
N12 Co1 N29 93.2(2) . . . yes
N12 Co1 N29 90.8(2) . . 6_665 yes
N22 Co1 N22 91.1(2) . . 6_665 yes
N22 Co1 N29 89.9(2) . . 6_665 yes
N12 Co1 N22 175.6(2) . . 6_665 yes
N29 Co1 N29 174.6(2) . . 6_665 yes
C1 C2 C11 110.0(4) . . . yes
C1 C2 C21 106.3(5) . . . yes
C11 C2 C21 110.3(5) . . . yes
C1 C2 C30 108.4(5) . . 6_665 yes
C11 C2 C30 112.4(5) . . 6_665 yes
C21 C2 C30 109.3(5) . . 6_665 yes
C2 C11 N12 115.4(4) . . . yes
Co1 N12 C11 117.0(3) . . . yes
Co1 N12 C13 109.2(3) . . . yes
C11 N12 C13 113.1(4) . . . yes
N12 C13 C14 114.2(4) . . . yes
N12 C13 C13 105.9(3) . . 6_665 yes
C14 C13 C13 111.4(3) . . 6_665 yes
C13 C14 C15 110.1(4) . . . yes
C14 C15 C15 112.1(4) . . 6_665 yes
C2 C21 N22 115.0(4) . . . yes
Co1 N22 C21 117.0(3) . . . yes
Co1 N22 C23 108.7(3) . . . yes
C21 N22 C23 112.0(4) . . . yes
N22 C23 C24 113.2(4) . . . yes
N22 C23 C28 107.7(4) . . . yes
C24 C23 C28 109.9(4) . . . yes
C23 C24 C25 110.4(4) . . . yes
C24 C25 C26 111.5(5) . . . yes
C25 C26 C27 112.0(5) . . . yes
C26 C27 C28 108.7(4) . . . yes
C23 C28 C27 111.3(4) . . . yes
C23 C28 N29 106.4(3) . . . yes
C27 C28 N29 113.8(4) . . . yes
Co1 N29 C28 107.9(3) . . . yes
Co1 N29 C30 115.3(3) . . . yes
C28 N29 C30 112.2(4) . . . yes
N29 C30 C2 117.0(4) . . 6_665 yes
Co1 N12 Cl1 106.8(1) . . . yes
C11 N12 Cl1 108.6(3) . . . yes
C13 N12 Cl1 100.6(2) . . . yes
Co1 N22 Cl1 122.2(2) . . 4_455 yes
C21 N22 Cl1 79.9(3) . . 4_455 yes
C23 N22 Cl1 114.5(2) . . 4_455 yes
Co1 N29 Cl1 105.9(1) . . . yes
C28 N29 Cl1 100.2(2) . . . yes
C30 N29 Cl1 113.9(3) . . . yes
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 N12 1.995(4) . . yes
Co1 N22 1.985(4) . . yes
Co1 N29 1.986(4) . . yes
C1 C2 1.540(7) . . yes
C2 C30 1.499(7) . 6_665 yes
C2 C11 1.481(8) . . yes
C11 N12 1.495(6) . . yes
N12 C13 1.502(6) . . yes
C13 C13 1.528(9) . 6_665 yes
C13 C14 1.509(7) . . yes
C14 C15 1.501(8) . . yes
C15 C15 1.525(13) . 6_665 yes
C2 C21 1.545(8) . . yes
C21 N22 1.506(7) . . yes
N22 C23 1.501(6) . . yes
C23 C24 1.525(7) . . yes
C24 C25 1.525(8) . . yes
C25 C26 1.516(9) . . yes
C26 C27 1.519(7) . . yes
C23 C28 1.517(7) . . yes
C27 C28 1.524(7) . . yes
C28 N29 1.515(6) . . yes
N29 C30 1.510(6) . . yes
C30 C2 1.499(7) . *6_665 yes
N12 Cl1 3.173(4) . . yes
N29 Cl1 3.205(4) . . yes
N22 Cl1 3.404(4) . 4_455 yes
Cl2 O1 1.359(7) . . yes
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
C11 N12 Co1 N22 37.8(4) . . . . no
C13 N12 Co1 N22 167.9(3) . . . . no
C11 N12 Co1 N29 124.2(3) . . . . no
C13 N12 Co1 N29 -105.6(3) . . . . no
C11 N12 Co1 N12 -145.3(4) . . . 6_665 no
C13 N12 Co1 N12 -15.2(2) . . . 6_665 no
C11 N12 Co1 N29 -52.2(4) . . . 6_665 no
C13 N12 Co1 N29 78.0(3) . . . 6_665 no
C21 N22 Co1 N12 -46.5(4) . . . . no
C23 N22 Co1 N12 81.5(3) . . . . no
C21 N22 Co1 N29 -139.6(4) . . . . no
C23 N22 Co1 N29 -11.6(3) . . . . no
C21 N22 Co1 N22 130.5(4) . . . 6_665 no
C23 N22 Co1 N22 -101.4(3) . . . 6_665 no
C21 N22 Co1 N29 44.2(4) . . . 6_665 no
C23 N22 Co1 N29 172.3(3) . . . 6_665 no
C28 N29 Co1 N12 -109.0(3) . . . . no
C30 N29 Co1 N12 124.6(4) . . . . no
C28 N29 Co1 N22 -17.1(3) . . . . no
C30 N29 Co1 N22 -143.5(4) . . . . no
C28 N29 Co1 N12 166.2(3) . . . 6_665 no
C30 N29 Co1 N12 39.8(4) . . . 6_665 no
C28 N29 Co1 N22 74.1(3) . . . 6_665 no
C30 N29 Co1 N22 -52.4(4) . . . 6_665 no
N12 C11 C2 C1 173.6(5) . . . . no
N12 C11 C2 C21 -69.5(6) . . . . no
N12 C11 C2 C30 52.7(7) . . . 6_665 no
N22 C21 C2 C1 177.9(5) . . . . no
N22 C21 C2 C11 58.7(6) . . . . no
N22 C21 C2 C30 -65.3(6) . . . 6_665 no
Co1 N12 C11 C2 12.5(6) . . . . no
C13 N12 C11 C2 -115.8(5) . . . . no
C14 C13 N12 Co1 164.6(3) . . . . no
C13 C13 N12 Co1 41.6(4) 6_665 . . . no
C14 C13 N12 C11 -63.2(5) . . . . no
C13 C13 N12 C11 173.8(4) 6_665 . . . no
C15 C14 C13 N12 -175.5(4) . . . . no
C15 C14 C13 C13 -55.6(6) . . . 6_665 no
C15 C15 C14 C13 54.8(7) 6_665 . . . no
Co1 N22 C21 C2 5.9(6) . . . . no
C23 N22 C21 C2 -120.5(5) . . . . no
C24 C23 N22 Co1 159.6(3) . . . . no
C28 C23 N22 Co1 37.9(4) . . . . no
C24 C23 N22 C21 -69.6(5) . . . . no
C28 C23 N22 C21 168.7(4) . . . . no
C25 C24 C23 N22 -177.1(5) . . . . no
C25 C24 C23 C28 -56.6(6) . . . . no
C27 C28 C23 N22 -176.7(4) . . . . no
N29 C28 C23 N22 -52.2(4) . . . . no
C27 C28 C23 C24 59.6(5) . . . . no
N29 C28 C23 C24 -175.9(4) . . . . no
C26 C25 C24 C23 54.8(6) . . . . no
C27 C26 C25 C24 -55.6(6) . . . . no
C28 C27 C26 C25 56.4(6) . . . . no
C23 C28 C27 C26 -58.7(5) . . . . no
N29 C28 C27 C26 181.1(4) . . . . no
Co1 N29 C28 C23 41.7(4) . . . . no
C30 N29 C28 C23 169.9(4) . . . . no
Cl1 N29 C28 C23 -68.9(3) . . . . no
Co1 N29 C28 C27 164.7(3) . . . . no
C30 N29 C28 C27 -67.1(5) . . . . no
C2 C30 N29 Co1 9.1(6) 6_665 . . . no
C2 C30 N29 C28 -115.1(5) 6_665 . . . no
