#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:23:13 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180180 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/76/7107617.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_7107617
loop_
_publ_author_name
'Wei-Quan Lin'
'Ji-Dong Leng'
'Ming-Liang Tong'
_publ_section_title
;
 A novel nanosized {Co16} metallamacrocycle incorporating four linear
 {Co4} subunits bridged by polytriazolate ligands
;
_journal_issue                   37
_journal_name_full               Chem.Commun.
_journal_page_first              4477
_journal_page_last               4479
_journal_paper_doi               10.1039/c2cc31141k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C42 H36 Co4 N20 O10'
_chemical_formula_weight         1216.63
_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                104.525(5)
_cell_angle_beta                 90.905(5)
_cell_angle_gamma                100.770(6)
_cell_formula_units_Z            1
_cell_length_a                   7.452(2)
_cell_length_b                   10.774(3)
_cell_length_c                   15.446(4)
_cell_measurement_temperature    298(2)
_cell_volume                     1176.8(5)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω 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  0.0861
_diffrn_reflns_av_sigmaI/netI    0.1747
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8234
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.8793
_exptl_absorpt_correction_T_min  0.7886
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.0024(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.2025
_refine_ls_R_factor_gt           0.0544
_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)+(0.0728P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1788
_reflns_number_gt                1675
_reflns_number_total             4516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31141k.txt
_cod_data_source_block           1
_cod_original_cell_volume        1176.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107617
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
Co1 Co 0.12357(17) 0.13551(10) 0.70134(6) 0.0501(4) Uani 1 1 d .
Co2 Co 0.03427(16) 0.40044(10) 0.91493(6) 0.0485(4) Uani 1 1 d .
N1 N 0.2848(9) 0.1760(6) 0.5904(3) 0.0516(18) Uani 1 1 d .
N2 N 0.2293(9) 0.3346(6) 0.7478(4) 0.0504(18) Uani 1 1 d .
N3 N 0.2060(9) 0.4371(6) 0.8179(3) 0.0460(17) Uani 1 1 d .
N4 N 0.3677(9) 0.5197(6) 0.7151(4) 0.0519(18) Uani 1 1 d .
N5 N 0.3134(9) 0.9032(6) 0.8402(4) 0.0544(19) Uani 1 1 d .
N6 N 0.0530(9) 0.7976(6) 1.1066(3) 0.0457(17) Uani 1 1 d .
N7 N 0.0191(9) 0.8786(6) 1.1865(3) 0.0475(17) Uani 1 1 d .
N8 N 0.1826(9) 1.0060(6) 1.1091(4) 0.0501(17) Uani 1 1 d .
N9 N -0.0099(9) 1.0779(6) 1.3285(4) 0.0532(18) Uani 1 1 d .
N10 N -0.1355(10) 0.2881(7) 0.6529(5) 0.065(2) Uani 1 1 d .
O1 O 0.3529(9) 0.0828(5) 0.7473(3) 0.0624(16) Uani 1 1 d .
H1O H 0.3206 0.0317 0.7806 0.075 Uiso 1 1 d R
O2 O -0.1347(7) 0.5180(5) 0.9590(3) 0.0488(14) Uani 1 1 d .
O3 O -0.1076(8) 0.1703(5) 0.6370(3) 0.0680(17) Uani 1 1 d .
O4 O -0.1168(12) 0.3413(7) 0.5919(5) 0.115(3) Uani 1 1 d .
O5 O -0.1668(10) 0.3473(6) 0.7263(4) 0.095(2) Uani 1 1 d .
C1 C 0.3127(12) 0.0953(8) 0.5125(5) 0.060(2) Uani 1 1 d .
H1 H 0.2593 0.0071 0.5010 0.072 Uiso 1 1 calc R
C2 C 0.4170(13) 0.1376(8) 0.4487(5) 0.061(3) Uani 1 1 d .
H2 H 0.4318 0.0782 0.3954 0.073 Uiso 1 1 calc R
C3 C 0.4989(13) 0.2665(9) 0.4635(5) 0.072(3) Uani 1 1 d .
H3 H 0.5712 0.2962 0.4214 0.086 Uiso 1 1 calc R
C4 C 0.4695(12) 0.3527(8) 0.5449(5) 0.063(3) Uani 1 1 d .
H4 H 0.5223 0.4412 0.5577 0.076 Uiso 1 1 calc R
C5 C 0.3617(12) 0.3044(8) 0.6051(5) 0.051(2) Uani 1 1 d .
C6 C 0.3228(11) 0.3887(7) 0.6886(5) 0.049(2) Uani 1 1 d .
C7 C 0.2908(11) 0.5454(7) 0.7956(4) 0.047(2) Uani 1 1 d .
C8 C 0.2890(11) 0.6792(7) 0.8454(4) 0.045(2) Uani 1 1 d .
C9 C 0.3275(11) 0.7800(7) 0.8028(5) 0.053(2) Uani 1 1 d .
H9 H 0.3652 0.7600 0.7446 0.063 Uiso 1 1 calc R
C10 C 0.2600(11) 0.9315(7) 0.9236(4) 0.052(2) Uani 1 1 d .
H10 H 0.2501 1.0173 0.9503 0.062 Uiso 1 1 calc R
C11 C 0.2180(11) 0.8389(7) 0.9731(4) 0.046(2) Uani 1 1 d .
C12 C 0.2375(11) 0.7126(7) 0.9340(4) 0.047(2) Uani 1 1 d .
H12 H 0.2164 0.6496 0.9662 0.056 Uiso 1 1 calc R
C13 C 0.1519(11) 0.8799(7) 1.0640(4) 0.045(2) Uani 1 1 d .
C14 C 0.0997(12) 0.9985(8) 1.1853(4) 0.048(2) Uani 1 1 d .
C15 C 0.0845(12) 1.1098(7) 1.2589(4) 0.052(2) Uani 1 1 d .
C16 C 0.1576(13) 1.2370(8) 1.2591(5) 0.065(3) Uani 1 1 d .
H16 H 0.2261 1.2555 1.2124 0.078 Uiso 1 1 calc R
C17 C 0.1270(13) 1.3378(9) 1.3306(5) 0.071(3) Uani 1 1 d .
H17 H 0.1706 1.4247 1.3312 0.085 Uiso 1 1 calc R
C18 C 0.0309(13) 1.3064(8) 1.4005(5) 0.071(3) Uani 1 1 d .
H18 H 0.0092 1.3721 1.4488 0.085 Uiso 1 1 calc R
C19 C -0.0322(12) 1.1775(8) 1.3981(5) 0.060(2) Uani 1 1 d .
H19 H -0.0929 1.1577 1.4466 0.072 Uiso 1 1 calc R
C20 C 0.5137(16) 0.1678(12) 0.7865(8) 0.126(5) Uani 1 1 d .
H20A H 0.6060 0.1185 0.7924 0.189 Uiso 1 1 calc R
H20B H 0.4915 0.2179 0.8447 0.189 Uiso 1 1 calc R
H20C H 0.5547 0.2258 0.7496 0.189 Uiso 1 1 calc R
C21 C -0.2777(13) 0.5529(10) 0.9140(5) 0.083(3) Uani 1 1 d .
H21A H -0.2762 0.6446 0.9369 0.125 Uiso 1 1 calc R
H21B H -0.3934 0.5036 0.9238 0.125 Uiso 1 1 calc R
H21C H -0.2603 0.5342 0.8510 0.125 Uiso 1 1 calc R
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'
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
O1 Co1 N7 94.4(2) . 2_567
O1 Co1 N2 93.6(2) . .
N7 Co1 N2 95.2(2) 2_567 .
O1 Co1 O3 171.9(2) . .
N7 Co1 O3 91.2(2) 2_567 .
N2 Co1 O3 91.7(2) . .
O1 Co1 N1 86.4(2) . .
N7 Co1 N1 173.0(2) 2_567 .
N2 Co1 N1 77.8(2) . .
O3 Co1 N1 88.8(2) . .
O1 Co1 N9 83.2(2) . 2_567
N7 Co1 N9 77.9(2) 2_567 2_567
N2 Co1 N9 172.1(2) . 2_567
O3 Co1 N9 92.2(2) . 2_567
N1 Co1 N9 109.1(2) . 2_567
O2 Co2 O2 78.4(2) . 2_567
O2 Co2 N6 119.6(2) . 2_567
O2 Co2 N6 111.0(2) 2_567 2_567
O2 Co2 N3 119.4(2) . .
O2 Co2 N3 115.6(2) 2_567 .
N6 Co2 N3 109.4(2) 2_567 .
C1 N1 C5 117.6(6) . .
C1 N1 Co1 130.1(5) . .
C5 N1 Co1 112.3(4) . .
C6 N2 N3 106.1(6) . .
C6 N2 Co1 114.8(4) . .
N3 N2 Co1 137.8(5) . .
C7 N3 N2 104.9(5) . .
C7 N3 Co2 135.1(5) . .
N2 N3 Co2 119.2(5) . .
C6 N4 C7 101.6(6) . .
C9 N5 C10 117.8(6) . .
C13 N6 N7 104.0(6) . .
C13 N6 Co2 137.2(5) . 2_567
N7 N6 Co2 118.7(4) . 2_567
C14 N7 N6 106.1(6) . .
C14 N7 Co1 115.3(4) . 2_567
N6 N7 Co1 138.5(5) . 2_567
C13 N8 C14 101.0(6) . .
C19 N9 C15 117.3(6) . .
C19 N9 Co1 130.8(5) . 2_567
C15 N9 Co1 111.6(4) . 2_567
O5 N10 O4 120.6(9) . .
O5 N10 O3 122.0(8) . .
O4 N10 O3 117.3(7) . .
C20 O1 Co1 125.9(6) . .
C20 O1 H1O 107.7 . .
Co1 O1 H1O 109.2 . .
C21 O2 Co2 131.4(4) . .
C21 O2 Co2 126.6(5) . 2_567
Co2 O2 Co2 101.6(2) . 2_567
N10 O3 Co1 118.8(5) . .
N1 C1 C2 122.8(8) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C3 C2 C1 120.3(7) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C2 C3 C4 117.5(8) . .
C2 C3 H3 121.3 . .
C4 C3 H3 121.3 . .
C5 C4 C3 119.2(8) . .
C5 C4 H4 120.4 . .
C3 C4 H4 120.4 . .
N1 C5 C4 122.6(6) . .
N1 C5 C6 115.7(7) . .
C4 C5 C6 121.7(7) . .
N2 C6 N4 113.8(6) . .
N2 C6 C5 118.9(7) . .
N4 C6 C5 127.3(7) . .
N3 C7 N4 113.5(6) . .
N3 C7 C8 125.3(6) . .
N4 C7 C8 121.0(7) . .
C9 C8 C12 116.9(7) . .
C9 C8 C7 119.6(6) . .
C12 C8 C7 123.3(7) . .
N5 C9 C8 124.0(7) . .
N5 C9 H9 118.0 . .
C8 C9 H9 118.0 . .
N5 C10 C11 123.4(7) . .
N5 C10 H10 118.3 . .
C11 C10 H10 118.3 . .
C12 C11 C10 117.9(6) . .
C12 C11 C13 123.2(7) . .
C10 C11 C13 118.8(7) . .
C11 C12 C8 119.9(7) . .
C11 C12 H12 120.0 . .
C8 C12 H12 120.0 . .
N8 C13 N6 114.6(6) . .
N8 C13 C11 120.9(6) . .
N6 C13 C11 124.5(6) . .
N7 C14 N8 114.2(6) . .
N7 C14 C15 120.6(7) . .
N8 C14 C15 125.1(7) . .
N9 C15 C16 122.5(6) . .
N9 C15 C14 114.5(7) . .
C16 C15 C14 123.0(7) . .
C15 C16 C17 118.7(8) . .
C15 C16 H16 120.7 . .
C17 C16 H16 120.7 . .
C18 C17 C16 119.0(8) . .
C18 C17 H17 120.5 . .
C16 C17 H17 120.5 . .
C19 C18 C17 119.5(7) . .
C19 C18 H18 120.3 . .
C17 C18 H18 120.3 . .
N9 C19 C18 122.9(7) . .
N9 C19 H19 118.5 . .
C18 C19 H19 118.5 . .
O1 C20 H20A 109.5 . .
O1 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
O1 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
O2 C21 H21A 109.5 . .
O2 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
O2 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.067(6) .
Co1 N7 2.070(6) 2_567
Co1 N2 2.078(6) .
Co1 O3 2.114(6) .
Co1 N1 2.194(6) .
Co1 N9 2.224(6) 2_567
Co2 O2 1.961(5) .
Co2 O2 1.994(5) 2_567
Co2 N6 2.051(6) 2_567
Co2 N3 2.051(6) .
N1 C1 1.341(8) .
N1 C5 1.355(9) .
N2 C6 1.340(9) .
N2 N3 1.378(7) .
N3 C7 1.347(9) .
N4 C6 1.342(9) .
N4 C7 1.364(8) .
N5 C9 1.333(9) .
N5 C10 1.334(8) .
N6 C13 1.352(8) .
N6 N7 1.379(7) .
N6 Co2 2.051(6) 2_567
N7 C14 1.324(9) .
N7 Co1 2.070(6) 2_567
N8 C13 1.337(8) .
N8 C14 1.351(8) .
N9 C19 1.352(8) .
N9 C15 1.374(9) .
N9 Co1 2.224(6) 2_567
N10 O5 1.203(7) .
N10 O4 1.217(8) .
N10 O3 1.288(8) .
O1 C20 1.390(11) .
O1 H1O 0.8499 .
O2 C21 1.421(9) .
O2 Co2 1.994(5) 2_567
C1 C2 1.378(10) .
C1 H1 0.9300 .
C2 C3 1.369(11) .
C2 H2 0.9300 .
C3 C4 1.411(10) .
C3 H3 0.9300 .
C4 C5 1.376(10) .
C4 H4 0.9300 .
C5 C6 1.447(9) .
C7 C8 1.456(9) .
C8 C9 1.395(10) .
C8 C12 1.403(9) .
C9 H9 0.9300 .
C10 C11 1.396(10) .
C10 H10 0.9300 .
C11 C12 1.380(9) .
C11 C13 1.483(9) .
C12 H12 0.9300 .
C14 C15 1.455(9) .
C15 C16 1.377(11) .
C16 C17 1.397(10) .
C16 H16 0.9300 .
C17 C18 1.382(11) .
C17 H17 0.9300 .
C18 C19 1.372(11) .
C18 H18 0.9300 .
C19 H19 0.9300 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
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 H1O N5 0.85 1.84 2.661(8) 162.6 1_545
