#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:25:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180428 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/97/7209737.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_7209737
loop_
_publ_author_name
'Liu, Yong-Liang'
'Yue, Ke-Fen'
'Li, Dong-Sheng'
'Yu, Yang'
'Hou, Lei'
'Wang, Yao-Yu'
_publ_section_title
;
 The first one-fold inclined 1D → 3D polycatenation assembly
 from unique interweaving triple-stranded helices
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2791
_journal_paper_doi               10.1039/c3ce27061k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C20 H25 Co N4 O11'
_chemical_formula_weight         556.37
_chemical_name_systematic
;
?
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.8179(10)
_cell_length_b                   11.8179(10)
_cell_length_c                   37.714(5)
_cell_measurement_reflns_used    1422
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.946
_cell_measurement_theta_min      2.366
_cell_volume                     5267.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0838
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            13953
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.9257
_exptl_absorpt_correction_T_min  0.8706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2604
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0659
_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)+(0.1214P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2097
_reflns_number_gt                1498
_reflns_number_total             2604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce27061k.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      I-42d
_cod_database_code               7209737
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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 0.0000 0.5000 0.02901(3) 0.0625(4) Uani 1 2 d S
O1 O 0.0008(5) 0.3719(4) 0.07272(11) 0.0831(13) Uani 1 1 d .
O2 O -0.1550(4) 0.4364(4) 0.04889(12) 0.0712(12) Uani 1 1 d .
O3 O -0.4625(5) 0.2500 0.1250 0.117(3) Uani 1 2 d S
N1 N 0.0461(5) 0.3708(5) -0.00362(15) 0.0673(14) Uani 1 1 d .
N2 N 0.0378(5) 0.2289(5) -0.04150(16) 0.0756(17) Uani 1 1 d .
C1 C 0.1317(7) 0.2961(7) 0.0030(2) 0.085(2) Uani 1 1 d .
H1 H 0.1848 0.3035 0.0211 0.101 Uiso 1 1 calc R
C2 C 0.1281(8) 0.2115(8) -0.0200(3) 0.100(3) Uani 1 1 d .
H2 H 0.1784 0.1512 -0.0213 0.120 Uiso 1 1 calc R
C3 C -0.0062(7) 0.3257(5) -0.03180(16) 0.0647(15) Uani 1 1 d .
C4 C -0.1068(7) 0.3803(8) -0.0501(2) 0.091(2) Uani 1 1 d .
H4A H -0.1307 0.3336 -0.0696 0.136 Uiso 1 1 calc R
H4B H -0.0853 0.4535 -0.0589 0.136 Uiso 1 1 calc R
H4C H -0.1678 0.3884 -0.0335 0.136 Uiso 1 1 calc R
C7 C -0.1070(6) 0.3763(7) 0.07270(17) 0.0717(19) Uani 1 1 d .
C8 C -0.1719(6) 0.3112(7) 0.0992(2) 0.072(2) Uani 1 1 d .
C9 C -0.1144(8) 0.2500 0.1250 0.072(3) Uani 1 2 d S
H9 H -0.0357 0.2500 0.1250 0.087 Uiso 1 2 calc SR
C10 C -0.2871(7) 0.3116(9) 0.0991(2) 0.089(3) Uani 1 1 d .
H10 H -0.3284 0.3546 0.0830 0.106 Uiso 1 1 d R
C11 C -0.3451(12) 0.244(6) 0.128(2) 0.098(11) Uani 0.50 1 d P
O1W O -0.3435(6) 0.4534(6) 0.0031(2) 0.144(3) Uani 1 1 d .
O2W O 0.2171(6) 0.3319(8) 0.0993(2) 0.142(3) Uani 1 1 d .
O3W O 0.4278(7) 0.3974(8) 0.0819(3) 0.185(4) Uani 1 1 d .
C5 C 0.0005(12) 0.1605(7) -0.0722(3) 0.139(3) Uani 1 1 d DU
C6 C 0.029(2) 0.0393(11) -0.0602(6) 0.137(5) Uani 0.50 1 d PDU
C6' C 0.029(2) 0.0410(12) -0.0826(7) 0.135(5) Uani 0.50 1 d PDU
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
N1 Co1 N1 105.6(3) . 2_565
N1 Co1 O2 104.4(2) . 2_565
N1 Co1 O2 100.3(2) 2_565 2_565
N1 Co1 O2 100.3(2) . .
N1 Co1 O2 104.4(2) 2_565 .
O2 Co1 O2 138.5(2) 2_565 .
N1 Co1 O1 162.5(2) . 2_565
N1 Co1 O1 86.4(2) 2_565 2_565
O2 Co1 O1 60.18(18) 2_565 2_565
O2 Co1 O1 88.60(19) . 2_565
N1 Co1 O1 86.4(2) . .
N1 Co1 O1 162.5(2) 2_565 .
O2 Co1 O1 88.60(19) 2_565 .
O2 Co1 O1 60.18(18) . .
O1 Co1 O1 85.1(3) 2_565 .
C7 O1 Co1 88.2(4) . .
C7 O2 Co1 93.5(4) . .
C11 O3 C11 12(6) . 14_454
C3 N1 C1 103.3(7) . .
C3 N1 Co1 130.9(5) . .
C1 N1 Co1 124.9(5) . .
C3 N2 C2 106.2(7) . .
C3 N2 C5 125.3(7) . .
C2 N2 C5 128.2(7) . .
C2 C1 N1 110.0(8) . .
C2 C1 H1 125.0 . .
N1 C1 H1 125.0 . .
C1 C2 N2 107.6(8) . .
C1 C2 H2 126.2 . .
N2 C2 H2 126.2 . .
N2 C3 N1 112.7(7) . .
N2 C3 C4 123.7(6) . .
N1 C3 C4 123.6(6) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O1 C7 O2 117.8(6) . .
O1 C7 C8 119.9(6) . .
O2 C7 C8 122.3(6) . .
C10 C8 C9 119.4(7) . .
C10 C8 C7 121.2(7) . .
C9 C8 C7 119.4(6) . .
C8 C9 C8 121.5(9) . 14_454
C8 C9 H9 119.3 . .
C8 C9 H9 119.3 14_454 .
C11 C10 C8 122(2) 14_454 .
C11 C10 C11 6(3) 14_454 .
C8 C10 C11 116.6(15) . .
C11 C10 H10 115.9 14_454 .
C8 C10 H10 121.7 . .
C11 C10 H10 121.5 . .
C11 C11 C10 147(6) 14_454 14_454
C11 C11 O3 84(3) 14_454 .
C10 C11 O3 128(5) 14_454 .
C11 C11 C10 27(4) 14_454 .
C10 C11 C10 120.8(14) 14_454 .
O3 C11 C10 111(4) . .
N2 C5 C6' 130.5(14) . .
N2 C5 C6 102.2(11) . .
C6' C5 C6 32.2(11) . .
C6' C6 C6 91(3) . 2
C6' C6 C6' 55(3) . 2
C6 C6 C6' 35.8(10) 2 2
C6' C6 C5 71.5(11) . .
C6 C6 C5 128(3) 2 .
C6' C6 C5 109.3(13) 2 .
C6 C6' C6' 89(3) . 2
C6 C6' C6 53(3) . 2
C6' C6' C6 35.8(10) 2 2
C6 C6' C5 76.2(10) . .
C6' C6' C5 129(3) 2 .
C6 C6' C5 110.8(18) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.035(6) .
Co1 N1 2.035(6) 2_565
Co1 O2 2.118(4) 2_565
Co1 O2 2.118(4) .
Co1 O1 2.238(4) 2_565
Co1 O1 2.238(4) .
O1 C7 1.275(8) .
O2 C7 1.278(8) .
O3 C11 1.395(18) .
O3 C11 1.395(18) 14_454
N1 C3 1.340(8) .
N1 C1 1.366(9) .
N2 C3 1.308(8) .
N2 C2 1.355(11) .
N2 C5 1.480(11) .
C1 C2 1.326(11) .
C1 H1 0.9300 .
C2 H2 0.9300 .
C3 C4 1.519(11) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C7 C8 1.475(10) .
C8 C10 1.361(10) .
C8 C9 1.391(8) .
C9 C8 1.391(8) 14_454
C9 H9 0.9300 .
C10 C11 1.28(6) 14_454
C10 C11 1.52(7) .
C10 H10 0.9300 .
C11 C11 0.28(15) 14_454
C11 C10 1.28(6) 14_454
C5 C6' 1.505(9) .
C5 C6 1.542(10) .
C6 C6' 0.85(3) .
C6 C6 1.16(4) 2
C6 C6' 1.45(3) 2
C6' C6' 1.19(5) 2
C6' C6 1.45(3) 2
