#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:45:54 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180154 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/50/7105014.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_7105014
loop_
_publ_author_name
'Szymczak, Nathaniel K'
'Berben, Louise A'
'Peters, Jonas C'
_publ_section_title
;
 Redox rich dicobalt macrocycles as templates for multi-electron
 transformations.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6729
_journal_page_last               6731
_journal_paper_doi               10.1039/b913946j
_journal_year                    2009
_chemical_formula_sum            'C28 H46 B2 Br4 Co2 F4 N12 O8'
_chemical_formula_weight         1213.89
_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                110.2380(10)
_cell_angle_beta                 99.6700(10)
_cell_angle_gamma                102.1900(10)
_cell_formula_units_Z            1
_cell_length_a                   9.9295(7)
_cell_length_b                   11.0421(7)
_cell_length_c                   11.0924(7)
_cell_measurement_reflns_used    9024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      2.52
_cell_volume                     1076.18(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19848
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    4.561
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta. Cryst.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0377
_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)+(0.0438P)²+1.6829P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                4840
_reflns_number_total             6407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b913946j.txt
_cod_data_source_block           nks4-44p
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105014
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 0.63679(4) 0.17281(4) 0.07426(3) 0.00761(9) Uani 1 1 d . . .
Br1 Br 0.81135(3) 0.06533(3) 0.00999(3) 0.01677(8) Uani 1 1 d . . .
Br2 Br 0.46655(3) 0.28531(3) 0.13996(3) 0.01712(8) Uani 1 1 d . . .
N1 N 0.5132(3) 0.0746(2) -0.1079(2) 0.0082(4) Uani 1 1 d . . .
N2 N 0.6947(3) 0.3041(2) 0.0054(2) 0.0110(5) Uani 1 1 d . . .
N3 N 0.5802(3) 0.0481(2) 0.1604(2) 0.0086(4) Uani 1 1 d . . .
N4 N 0.7645(3) 0.2781(3) 0.2460(2) 0.0102(5) Uani 1 1 d . . .
N5 N -0.0151(3) 0.8584(3) 0.2230(3) 0.0206(6) Uani 1 1 d . . .
N6 N 0.2991(3) 0.3010(3) 0.4134(3) 0.0228(6) Uani 1 1 d . . .
C1 C 0.6349(3) 0.2799(3) -0.1160(3) 0.0106(5) Uani 1 1 d . . .
C2 C 0.5342(3) 0.1455(3) -0.1848(3) 0.0100(5) Uani 1 1 d . . .
C3 C 0.6527(3) 0.1003(3) 0.2906(3) 0.0094(5) Uani 1 1 d . . .
C4 C 0.7569(3) 0.2325(3) 0.3381(3) 0.0101(5) Uani 1 1 d . . .
C5 C 0.4626(3) 0.0937(3) -0.3204(3) 0.0110(5) Uani 1 1 d . . .
H5 H 0.4798 0.1446 -0.3729 0.013 Uiso 1 1 calc R . .
C6 C 0.6324(3) 0.0319(3) 0.3743(3) 0.0114(5) Uani 1 1 d . . .
H6 H 0.6832 0.0717 0.4657 0.014 Uiso 1 1 calc R . .
C7 C 0.8436(3) 0.3038(3) 0.4792(3) 0.0139(6) Uani 1 1 d . . .
H7A H 0.9026 0.2494 0.5006 0.021 Uiso 1 1 calc R . .
H7B H 0.7799 0.3173 0.5381 0.021 Uiso 1 1 calc R . .
H7C H 0.9053 0.3915 0.4918 0.021 Uiso 1 1 calc R . .
C8 C 0.6602(4) 0.3824(3) -0.1753(3) 0.0160(6) Uani 1 1 d . . .
H8A H 0.6072 0.4473 -0.1437 0.024 Uiso 1 1 calc R . .
H8B H 0.6276 0.3373 -0.2727 0.024 Uiso 1 1 calc R . .
H8C H 0.7624 0.4300 -0.1486 0.024 Uiso 1 1 calc R . .
C9 C -0.0256(5) 0.9780(5) 0.3246(4) 0.0428(12) Uani 1 1 d . . .
H9A H 0.0683 1.0277 0.3878 0.064 Uiso 1 1 calc R . .
H9B H -0.0940 0.9517 0.3717 0.064 Uiso 1 1 calc R . .
H9C H -0.0581 1.0355 0.2830 0.064 Uiso 1 1 calc R . .
C10 C -0.1433(4) 0.7749(4) 0.1161(4) 0.0268(8) Uani 1 1 d . . .
H10A H -0.1198 0.7043 0.0482 0.040 Uiso 1 1 calc R . .
H10B H -0.1817 0.8310 0.0759 0.040 Uiso 1 1 calc R . .
H10C H -0.2149 0.7333 0.1521 0.040 Uiso 1 1 calc R . .
C11 C 0.3336(5) 0.4246(5) 0.5315(4) 0.0426(11) Uani 1 1 d . . .
H11A H 0.4171 0.4299 0.5965 0.064 Uiso 1 1 calc R . .
H11B H 0.2521 0.4248 0.5706 0.064 Uiso 1 1 calc R . .
H11C H 0.3548 0.5024 0.5071 0.064 Uiso 1 1 calc R . .
C12 C 0.1828(5) 0.2801(6) 0.3029(4) 0.0423(12) Uani 1 1 d . . .
H12A H 0.1724 0.1958 0.2282 0.063 Uiso 1 1 calc R . .
H12B H 0.2034 0.3556 0.2751 0.063 Uiso 1 1 calc R . .
H12C H 0.0939 0.2747 0.3309 0.063 Uiso 1 1 calc R . .
C13 C 0.1057(3) 0.8243(4) 0.2292(3) 0.0181(6) Uani 1 1 d . . .
H13 H 0.1057 0.7461 0.1575 0.022 Uiso 1 1 calc R . .
C14 C 0.3828(4) 0.2204(3) 0.4016(3) 0.0170(6) Uani 1 1 d . . .
H14 H 0.3558 0.1413 0.3219 0.020 Uiso 1 1 calc R . .
B1 B 0.9014(4) 0.4515(4) 0.1854(3) 0.0190(8) Uani 1 1 d . . .
F1 F 0.9966(2) 0.3906(2) 0.1310(2) 0.0276(5) Uani 1 1 d . . .
F2 F 0.9589(2) 0.5885(2) 0.25394(19) 0.0295(5) Uani 1 1 d . . .
O1 O 0.8574(2) 0.4013(2) 0.2852(2) 0.0146(4) Uani 1 1 d . . .
O2 O 0.7772(3) 0.4326(2) 0.0799(2) 0.0178(5) Uani 1 1 d . . .
O3 O 0.2179(3) 0.8837(3) 0.3184(2) 0.0242(5) Uani 1 1 d . . .
O4 O 0.4925(2) 0.2397(2) 0.4854(2) 0.0177(5) 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
F F 0.0171 0.0103 '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'
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
N2 Co1 N4 93.81(10) . . ?
N2 Co1 N1 81.68(10) . . ?
N4 Co1 N1 175.40(10) . . ?
N2 Co1 N3 175.31(10) . . ?
N4 Co1 N3 82.14(10) . . ?
N1 Co1 N3 102.41(10) . . ?
N2 Co1 Br2 85.97(8) . . ?
N4 Co1 Br2 89.42(8) . . ?
N1 Co1 Br2 91.14(7) . . ?
N3 Co1 Br2 91.60(7) . . ?
N2 Co1 Br1 92.95(8) . . ?
N4 Co1 Br1 89.78(8) . . ?
N1 Co1 Br1 89.58(7) . . ?
N3 Co1 Br1 89.41(7) . . ?
Br2 Co1 Br1 178.61(2) . . ?
N3 N1 C2 119.9(2) 2_655 . ?
N3 N1 Co1 128.25(17) 2_655 . ?
C2 N1 Co1 111.87(19) . . ?
C1 N2 O2 115.4(2) . . ?
C1 N2 Co1 118.8(2) . . ?
O2 N2 Co1 124.72(17) . . ?
N1 N3 C3 119.2(2) 2_655 . ?
N1 N3 Co1 129.28(17) 2_655 . ?
C3 N3 Co1 111.47(19) . . ?
C4 N4 O1 115.5(2) . . ?
C4 N4 Co1 117.8(2) . . ?
O1 N4 Co1 126.62(17) . . ?
C13 N5 C9 121.3(3) . . ?
C13 N5 C10 121.4(3) . . ?
C9 N5 C10 117.3(3) . . ?
C14 N6 C12 121.7(3) . . ?
C14 N6 C11 120.7(3) . . ?
C12 N6 C11 117.0(3) . . ?
N2 C1 C2 112.3(2) . . ?
N2 C1 C8 123.1(3) . . ?
C2 C1 C8 124.5(2) . . ?
N1 C2 C5 122.4(3) . . ?
N1 C2 C1 115.1(2) . . ?
C5 C2 C1 122.4(3) . . ?
N3 C3 C6 122.9(3) . . ?
N3 C3 C4 115.5(2) . . ?
C6 C3 C4 121.6(2) . . ?
N4 C4 C3 113.0(2) . . ?
N4 C4 C7 125.1(3) . . ?
C3 C4 C7 121.8(2) . . ?
C6 C5 C2 117.8(3) 2_655 . ?
C6 C5 H5 121.1 2_655 . ?
C2 C5 H5 121.1 . . ?
C5 C6 C3 117.9(2) 2_655 . ?
C5 C6 H6 121.1 2_655 . ?
C3 C6 H6 121.1 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C1 C8 H8A 109.5 . . ?
C1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C10 H10A 109.5 . . ?
N5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C12 H12A 109.5 . . ?
N6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C13 N5 126.7(3) . . ?
O3 C13 H13 116.6 . . ?
N5 C13 H13 116.6 . . ?
O4 C14 N6 125.5(3) . . ?
O4 C14 H14 117.3 . . ?
N6 C14 H14 117.3 . . ?
F2 B1 F1 112.7(3) . . ?
F2 B1 O2 105.9(3) . . ?
F1 B1 O2 110.5(3) . . ?
F2 B1 O1 104.8(3) . . ?
F1 B1 O1 111.2(3) . . ?
O2 B1 O1 111.6(3) . . ?
N4 O1 B1 120.6(2) . . ?
N2 O2 B1 116.8(2) . . ?
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 N2 1.891(2) . ?
Co1 N4 1.903(2) . ?
Co1 N1 1.964(2) . ?
Co1 N3 1.972(2) . ?
Co1 Br2 2.3677(5) . ?
Co1 Br1 2.3706(5) . ?
N1 N3 1.333(3) 2_655 ?
N1 C2 1.354(3) . ?
N2 C1 1.286(3) . ?
N2 O2 1.355(3) . ?
N3 N1 1.333(3) 2_655 ?
N3 C3 1.355(3) . ?
N4 C4 1.292(3) . ?
N4 O1 1.348(3) . ?
N5 C13 1.330(4) . ?
N5 C9 1.446(5) . ?
N5 C10 1.455(4) . ?
N6 C14 1.330(4) . ?
N6 C12 1.451(5) . ?
N6 C11 1.454(5) . ?
C1 C2 1.455(4) . ?
C1 C8 1.493(4) . ?
C2 C5 1.403(4) . ?
C3 C6 1.398(4) . ?
C3 C4 1.458(4) . ?
C4 C7 1.490(4) . ?
C5 C6 1.362(4) 2_655 ?
C5 H5 0.9500 . ?
C6 C5 1.362(4) 2_655 ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O3 1.234(4) . ?
C13 H13 0.9500 . ?
C14 O4 1.234(4) . ?
C14 H14 0.9500 . ?
B1 F2 1.373(4) . ?
B1 F1 1.374(5) . ?
B1 O2 1.474(4) . ?
B1 O1 1.486(4) . ?
