#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:49:11 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180156 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/52/7105241.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_7105241
loop_
_publ_author_name
'Vicente, José'
'Gil-Rubio, Juan'
'Barquero, Natalia'
'Cámara, Verónica'
'Masciocchi, Norberto'
_publ_section_title
;
 Self-assembly of looped triple-stranded helicates.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1053
_journal_page_last               1055
_journal_paper_doi               10.1039/b921279e
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         C156H126Au6Fe2N12P6,4(ClO4),12(C2H3N),5(H2O)
_chemical_formula_sum            'C180 H182 Au6 Cl4 Fe2 N24 O21 P6'
_chemical_formula_weight         4638.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   19.4440(4)
_cell_length_b                   19.4440(4)
_cell_length_c                   27.9000(13)
_cell_measurement_reflns_used    6967
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.40
_cell_volume                     9134.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SCHAKAL and ORTEP'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω-scan
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            98735
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.134
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS - Bruker Nonius - V2.05'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4564
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.764
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6251
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0672P)²+24.4553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                5147
_reflns_number_total             6251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921279e.txt
_cod_data_source_block           nba372s
_cod_database_code               7105241
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-y, -x, -z+1/2'
'-x+y, -x, z'
'x, x-y, -z+1/2'
'-x+y, y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'y, x, z-1/2'
'x-y, x, -z'
'-x, -x+y, z-1/2'
'x-y, -y, z-1/2'
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
Au Au 0.773217(14) 0.114935(15) 0.707582(8) 0.04709(10) Uani 1 1 d . . .
Fe Fe 0.6667 0.3333 0.91153(5) 0.0388(3) Uani 1 3 d S . .
P P 0.86012(11) 0.10720(11) 0.65654(5) 0.0506(4) Uani 1 1 d . . .
N1 N 0.5679(3) 0.2778(3) 0.94882(18) 0.0476(11) Uani 1 1 d . . .
N2 N 0.6155(3) 0.2339(2) 0.87522(16) 0.0383(9) Uani 1 1 d . . .
C1 C 0.5478(5) 0.3068(5) 0.9863(3) 0.0687(19) Uani 1 1 d . . .
H1 H 0.5832 0.3582 0.9964 0.082 Uiso 1 1 calc R . .
C2 C 0.4778(5) 0.2646(5) 1.0104(3) 0.077(2) Uani 1 1 d . . .
H2 H 0.4665 0.2865 1.0367 0.093 Uiso 1 1 calc R . .
C3 C 0.4248(4) 0.1895(5) 0.9951(3) 0.0646(18) Uani 1 1 d . . .
H3 H 0.3769 0.1594 1.0112 0.077 Uiso 1 1 calc R . .
C4 C 0.4430(4) 0.1588(4) 0.9555(2) 0.0515(14) Uani 1 1 d . . .
H4 H 0.4071 0.1082 0.9444 0.062 Uiso 1 1 calc R . .
C5 C 0.5148(3) 0.2041(3) 0.9327(2) 0.0436(12) Uani 1 1 d . . .
C6 C 0.5431(3) 0.1785(3) 0.8915(2) 0.0408(12) Uani 1 1 d . . .
C7 C 0.5008(3) 0.1040(3) 0.8703(2) 0.0491(14) Uani 1 1 d . . .
H7 H 0.4504 0.0675 0.8814 0.059 Uiso 1 1 calc R . .
C8 C 0.5340(4) 0.0847(4) 0.8327(2) 0.0520(14) Uani 1 1 d . . .
H8 H 0.5064 0.0348 0.8186 0.062 Uiso 1 1 calc R . .
C9 C 0.6096(3) 0.1407(3) 0.81599(19) 0.0419(12) Uani 1 1 d . . .
C10 C 0.6466(3) 0.2149(3) 0.8384(2) 0.0406(11) Uani 1 1 d . . .
H10 H 0.6959 0.2534 0.8270 0.049 Uiso 1 1 calc R . .
C11 C 0.6504(3) 0.1255(3) 0.7795(2) 0.0457(13) Uani 1 1 d . . .
C12 C 0.6935(4) 0.1193(4) 0.7510(2) 0.0498(14) Uani 1 1 d . . .
C13 C 0.8109(5) 0.0522(4) 0.6027(2) 0.0588(17) Uani 1 1 d . . .
C14 C 0.7316(6) -0.0023(4) 0.6043(3) 0.075(2) Uani 1 1 d . . .
H14 H 0.7037 -0.0123 0.6329 0.090 Uiso 1 1 calc R . .
C15 C 0.6933(7) -0.0424(5) 0.5628(4) 0.095(3) Uani 1 1 d . . .
H15 H 0.6393 -0.0794 0.5637 0.114 Uiso 1 1 calc R . .
C16 C 0.7340(8) -0.0281(5) 0.5205(3) 0.098(3) Uani 1 1 d . . .
H16 H 0.7070 -0.0543 0.4928 0.118 Uiso 1 1 calc R . .
C17 C 0.8155(7) 0.0254(5) 0.5185(3) 0.094(3) Uani 1 1 d . . .
H17 H 0.8437 0.0338 0.4901 0.113 Uiso 1 1 calc R . .
C18 C 0.8528(6) 0.0655(5) 0.5598(2) 0.076(2) Uani 1 1 d . . .
H18 H 0.9069 0.1021 0.5592 0.092 Uiso 1 1 calc R . .
C19 C 0.9374(4) 0.2029(4) 0.63530(19) 0.0541(15) Uani 1 1 d . . .
C20 C 1.0158(5) 0.2236(6) 0.6299(3) 0.078(2) Uani 1 1 d . . .
H20 H 1.0324 0.1880 0.6384 0.093 Uiso 1 1 calc R . .
C21 C 1.0699(6) 0.2977(7) 0.6118(3) 0.098(3) Uani 1 1 d . . .
H21 H 1.1234 0.3129 0.6097 0.118 Uiso 1 1 calc R . .
C22 C 1.0438(7) 0.3495(6) 0.5967(3) 0.100(3) Uani 1 1 d . . .
H22 H 1.0799 0.3980 0.5831 0.120 Uiso 1 1 calc R . .
C23 C 0.9668(6) 0.3303(5) 0.6016(3) 0.075(2) Uani 1 1 d . . .
H23 H 0.9504 0.3657 0.5921 0.090 Uiso 1 1 calc R . .
C24 C 0.9128(5) 0.2574(4) 0.6211(2) 0.0617(17) Uani 1 1 d . . .
H24 H 0.8600 0.2440 0.6248 0.074 Uiso 1 1 calc R . .
C25 C 0.9096(6) 0.0573(6) 0.6813(2) 0.084(3) Uani 1 1 d . . .
H25A H 0.8707 0.0020 0.6871 0.101 Uiso 1 1 calc R . .
H25B H 0.9477 0.0590 0.6582 0.101 Uiso 1 1 calc R . .
C26 C 0.9526(5) 0.0957(7) 0.7281(2) 0.096(3) Uani 1 1 d . . .
H26A H 0.9611 0.1492 0.7302 0.115 Uiso 1 1 calc R . .
H26B H 1.0041 0.0991 0.7283 0.115 Uiso 1 1 calc R . .
Cl1 Cl 0.0000 0.0000 0.5584(2) 0.0723(16) Uani 0.50 3 d SP . .
O11 O 0.0000 0.0000 0.5000 0.217(13) Uiso 1 6 d S . .
O12 O 0.0234(6) 0.0751(6) 0.5778(4) 0.074(3) Uiso 0.50 1 d P . .
Cl2 Cl 0.0000 0.5000 0.5000 0.1109(14) Uani 1 2 d S . .
O21 O -0.0659(9) 0.4409(9) 0.5188(6) 0.107(4) Uiso 0.50 1 d P . .
O22 O -0.0161(10) 0.4213(11) 0.4780(7) 0.131(5) Uiso 0.50 1 d P . .
O23 O -0.0758(12) 0.4904(12) 0.4666(7) 0.150(6) Uiso 0.50 1 d P . .
O24 O -0.0299(12) 0.4881(12) 0.5470(7) 0.144(6) Uiso 0.50 1 d P . .
C1S C 0.5234(10) 0.3679(10) 0.1340(7) 0.188(7) Uiso 1 1 d D . .
C2S C 0.4574(10) 0.2874(11) 0.1485(7) 0.194(7) Uiso 1 1 d D . .
N1S N 0.5781(11) 0.4259(10) 0.1214(8) 0.278(10) Uiso 1 1 d D . .
C3S C 0.6588(10) 0.9042(12) 0.7500(14) 0.37(2) Uiso 1 1 d D . .
C4S C 0.7290(8) 0.9037(9) 0.7281(6) 0.166(6) Uiso 1 1 d D . .
N2S N 0.6076(7) 0.9092(7) 0.7669(4) 0.150(4) Uiso 1 1 d D . .
O1W O 0.6667 0.3333 0.0965(19) 0.45(3) Uiso 1 3 d S . .
O2W O 0.4527(9) 0.9055(17) 0.7500 0.308(13) Uiso 1 2 d S . .
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'
P P 0.1023 0.0942 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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
C12 Au P 177.99(18) . . ?
C12 Au Au 78.57(17) . 3_666 ?
P Au Au 103.44(5) . 3_666 ?
N2 Fe N2 95.65(17) . 2_655 ?
N2 Fe N2 95.65(17) . 4_665 ?
N2 Fe N2 95.65(17) 2_655 4_665 ?
N2 Fe N1 88.16(19) . 2_655 ?
N2 Fe N1 81.77(19) 2_655 2_655 ?
N2 Fe N1 175.6(2) 4_665 2_655 ?
N2 Fe N1 175.61(19) . 4_665 ?
N2 Fe N1 88.16(19) 2_655 4_665 ?
N2 Fe N1 81.77(19) 4_665 4_665 ?
N1 Fe N1 94.6(2) 2_655 4_665 ?
N2 Fe N1 81.77(19) . . ?
N2 Fe N1 175.61(19) 2_655 . ?
N2 Fe N1 88.16(19) 4_665 . ?
N1 Fe N1 94.6(2) 2_655 . ?
N1 Fe N1 94.6(2) 4_665 . ?
C19 P C25 106.6(4) . . ?
C19 P C13 104.9(3) . . ?
C25 P C13 105.4(4) . . ?
C19 P Au 113.6(2) . . ?
C25 P Au 114.1(2) . . ?
C13 P Au 111.6(3) . . ?
C1 N1 C5 118.5(5) . . ?
C1 N1 Fe 126.5(5) . . ?
C5 N1 Fe 115.0(4) . . ?
C10 N2 C6 118.2(5) . . ?
C10 N2 Fe 126.6(4) . . ?
C6 N2 Fe 115.1(4) . . ?
N1 C1 C2 123.2(7) . . ?
C1 C2 C3 118.8(7) . . ?
C2 C3 C4 119.3(6) . . ?
C5 C4 C3 119.3(6) . . ?
N1 C5 C4 120.9(5) . . ?
N1 C5 C6 113.8(5) . . ?
C4 C5 C6 125.3(6) . . ?
N2 C6 C7 121.6(5) . . ?
N2 C6 C5 114.2(5) . . ?
C7 C6 C5 124.1(5) . . ?
C8 C7 C6 119.6(5) . . ?
C7 C8 C9 119.6(5) . . ?
C10 C9 C8 116.8(5) . . ?
C10 C9 C11 119.1(5) . . ?
C8 C9 C11 124.1(5) . . ?
N2 C10 C9 124.1(5) . . ?
C12 C11 C9 172.1(6) . . ?
C11 C12 Au 174.9(5) . . ?
C14 C13 C18 119.9(7) . . ?
C14 C13 P 119.2(5) . . ?
C18 C13 P 120.9(6) . . ?
C13 C14 C15 119.3(8) . . ?
C16 C15 C14 120.8(10) . . ?
C15 C16 C17 120.8(8) . . ?
C18 C17 C16 117.8(8) . . ?
C17 C18 C13 121.3(9) . . ?
C20 C19 C24 119.2(7) . . ?
C20 C19 P 124.4(6) . . ?
C24 C19 P 116.3(5) . . ?
C19 C20 C21 119.9(8) . . ?
C20 C21 C22 119.8(9) . . ?
C23 C22 C21 121.3(9) . . ?
C22 C23 C24 119.2(9) . . ?
C23 C24 C19 120.6(7) . . ?
C26 C25 P 111.8(6) . . ?
C25 C26 C26 111.2(11) . 3_666 ?
O12 Cl1 O12 106.1(6) 4 . ?
O12 Cl1 O12 106.1(6) 4 2 ?
O12 Cl1 O12 106.1(6) . 2 ?
O12 Cl1 O11 112.7(5) 4 . ?
O12 Cl1 O11 112.7(5) . . ?
O12 Cl1 O11 112.7(5) 2 . ?
Cl1 O11 Cl1 180.000(1) 7_556 . ?
O21 Cl2 O21 180(2) 7_566 . ?
O21 Cl2 O24 130.7(9) 7_566 . ?
O21 Cl2 O24 49.3(9) . . ?
O21 Cl2 O24 49.3(9) 7_566 7_566 ?
O21 Cl2 O24 130.7(9) . 7_566 ?
O24 Cl2 O24 180.000(7) . 7_566 ?
O21 Cl2 O22 70.5(9) 7_566 7_566 ?
O21 Cl2 O22 109.5(9) . 7_566 ?
O24 Cl2 O22 69.6(10) . 7_566 ?
O24 Cl2 O22 110.4(10) 7_566 7_566 ?
O21 Cl2 O22 109.5(9) 7_566 . ?
O21 Cl2 O22 70.5(9) . . ?
O24 Cl2 O22 110.4(10) . . ?
O24 Cl2 O22 69.6(10) 7_566 . ?
O22 Cl2 O22 180.000(3) 7_566 . ?
O21 Cl2 O23 73.1(9) 7_566 7_566 ?
O21 Cl2 O23 106.9(9) . 7_566 ?
O24 Cl2 O23 76.6(10) . 7_566 ?
O24 Cl2 O23 103.4(10) 7_566 7_566 ?
O22 Cl2 O23 86.4(10) 7_566 7_566 ?
O22 Cl2 O23 93.6(9) . 7_566 ?
O21 Cl2 O23 106.9(9) 7_566 . ?
O21 Cl2 O23 73.1(9) . . ?
O24 Cl2 O23 103.4(10) . . ?
O24 Cl2 O23 76.6(10) 7_566 . ?
O22 Cl2 O23 93.6(9) 7_566 . ?
O22 Cl2 O23 86.4(10) . . ?
O23 Cl2 O23 180.000(5) 7_566 . ?
O24 O21 Cl2 68.9(13) . . ?
O24 O21 O22 117.6(16) . . ?
Cl2 O21 O22 60.4(9) . . ?
O24 O21 O23 108.2(16) . . ?
Cl2 O21 O23 62.3(9) . . ?
O22 O21 O23 78.4(11) . . ?
Cl2 O22 O21 49.1(8) . . ?
Cl2 O22 O24 51.8(9) . 7_566 ?
O21 O22 O24 96.3(13) . 7_566 ?
Cl2 O23 O21 44.6(7) . . ?
O21 O24 Cl2 61.8(13) . . ?
O21 O24 O22 110.3(18) . 7_566 ?
Cl2 O24 O22 58.7(10) . 7_566 ?
N1S C1S C2S 173.0(12) . . ?
N2S C3S C4S 176.2(19) . . ?
C3S C4S C4S 96.0(18) . 5_566 ?
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
Au C12 2.003(6) . ?
Au P 2.2715(16) . ?
Au Au 3.2144(5) 3_666 ?
Fe N2 1.958(4) . ?
Fe N2 1.958(4) 2_655 ?
Fe N2 1.958(4) 4_665 ?
Fe N1 1.965(5) 2_655 ?
Fe N1 1.965(5) 4_665 ?
Fe N1 1.965(5) . ?
P C19 1.809(7) . ?
P C25 1.810(7) . ?
P C13 1.815(7) . ?
N1 C1 1.335(8) . ?
N1 C5 1.357(8) . ?
N2 C10 1.333(7) . ?
N2 C6 1.354(7) . ?
C1 C2 1.363(10) . ?
C2 C3 1.368(11) . ?
C3 C4 1.383(9) . ?
C4 C5 1.380(8) . ?
C5 C6 1.464(8) . ?
C6 C7 1.390(8) . ?
C7 C8 1.377(8) . ?
C8 C9 1.401(8) . ?
C9 C10 1.397(8) . ?
C9 C11 1.411(8) . ?
C11 C12 1.202(8) . ?
C13 C14 1.367(11) . ?
C13 C18 1.395(10) . ?
C14 C15 1.386(11) . ?
C15 C16 1.370(14) . ?
C16 C17 1.396(15) . ?
C17 C18 1.378(11) . ?
C19 C20 1.376(10) . ?
C19 C24 1.419(9) . ?
C20 C21 1.386(13) . ?
C21 C22 1.401(15) . ?
C22 C23 1.357(14) . ?
C23 C24 1.385(11) . ?
C25 C26 1.530(13) . ?
C26 C26 1.539(15) 3_666 ?
Cl1 O12 1.403(11) 4 ?
Cl1 O12 1.403(11) . ?
Cl1 O12 1.403(11) 2 ?
Cl1 O11 1.630(6) . ?
O11 Cl1 1.630(6) 7_556 ?
Cl2 O21 1.328(15) 7_566 ?
Cl2 O21 1.328(15) . ?
Cl2 O24 1.406(19) . ?
Cl2 O24 1.406(19) 7_566 ?
Cl2 O22 1.529(18) 7_566 ?
Cl2 O22 1.529(18) . ?
Cl2 O23 1.67(2) 7_566 ?
Cl2 O23 1.67(2) . ?
O21 O24 1.14(2) . ?
O21 O22 1.66(2) . ?
O21 O23 1.81(2) . ?
O22 O24 1.68(2) 7_566 ?
O24 O22 1.68(2) 7_566 ?
C1S N1S 1.1518(10) . ?
C1S C2S 1.5015(10) . ?
C3S N2S 1.1505(10) . ?
C3S C4S 1.5004(10) . ?
C4S C4S 1.95(3) 5_566 ?
