#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/42/7214266.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_7214266
loop_
_publ_author_name
'Constable, Edwin C.'
'Housecroft, Catherine E.'
'Vujovic, Srboljub'
'Zampese, Jennifer A.'
_publ_section_title
;
 Metallohexacycles containing
 4′-aryl-4,2′:6′,4′′-terpyridines:
 conformational preferences and fullerene capture
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              328
_journal_paper_doi               10.1039/c3ce42012d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'C162 H84 Cl12 F30 N18 Zn6, 3(C H Cl3), 3(C H4 O), 6(H2 O)'
_chemical_formula_sum            'C168 H111 Cl21 F30 N18 O9 Zn6'
_chemical_formula_weight         4232.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            3
_cell_length_a                   37.998(4)
_cell_length_b                   37.998(4)
_cell_length_c                   11.3178(11)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      67.90
_cell_measurement_theta_min      4.03
_cell_volume                     14152(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32865
_diffrn_reflns_theta_full        67.63
_diffrn_reflns_theta_max         67.63
_diffrn_reflns_theta_min         4.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.340
_exptl_absorpt_correction_T_max  0.5621
_exptl_absorpt_correction_T_min  0.2893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5662
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1099P)²+88.3671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                5423
_reflns_number_total             5662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42012d.txt
_cod_data_source_block           sv65
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        14152(2)
_cod_original_sg_symbol_Hall     -R3
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7214266
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Zn1 Zn 0.680089(8) 0.741424(9) 0.26698(3) 0.02691(8) Uani 1 1 d . . .
Cl1 Cl 0.70632(2) 0.791653(19) 0.39688(5) 0.04081(17) Uani 1 1 d . . .
Cl2 Cl 0.712320(17) 0.71572(2) 0.16688(5) 0.04039(14) Uani 1 1 d . . .
N1 N 0.42700(5) 0.43774(6) 0.19703(16) 0.0269(4) Uani 1 1 d . . .
N2 N 0.50930(5) 0.56215(6) 0.43366(16) 0.0273(5) Uani 1 1 d . . .
N3 N 0.63170(6) 0.69468(6) 0.35274(17) 0.0274(4) Uani 1 1 d . . .
C1 C 0.40946(6) 0.43003(7) 0.3043(2) 0.0278(5) Uani 1 1 d . . .
H1A H 0.3863 0.4041 0.3185 0.033 Uiso 1 1 calc R . .
C2 C 0.42372(6) 0.45824(7) 0.3947(2) 0.0273(5) Uani 1 1 d . . .
H2A H 0.4103 0.4517 0.4691 0.033 Uiso 1 1 calc R . .
C3 C 0.45747(6) 0.49591(7) 0.3765(2) 0.0274(5) Uani 1 1 d . . .
C4 C 0.47566(7) 0.50367(8) 0.2653(2) 0.0357(7) Uani 1 1 d . . .
H4A H 0.4990 0.5292 0.2490 0.043 Uiso 1 1 calc R . .
C5 C 0.45974(7) 0.47420(8) 0.1796(2) 0.0336(6) Uani 1 1 d . . .
H5A H 0.4726 0.4800 0.1044 0.040 Uiso 1 1 calc R . .
C6 C 0.47585(7) 0.52844(7) 0.4685(2) 0.0285(5) Uani 1 1 d . . .
C7 C 0.45945(7) 0.52472(7) 0.5809(2) 0.0309(6) Uani 1 1 d . . .
H7A H 0.4354 0.5006 0.6030 0.037 Uiso 1 1 calc R . .
C8 C 0.47879(7) 0.55684(7) 0.6605(2) 0.0310(6) Uani 1 1 d . . .
C9 C 0.51377(7) 0.59164(7) 0.6236(2) 0.0291(5) Uani 1 1 d . . .
H9A H 0.5279 0.6140 0.6757 0.035 Uiso 1 1 calc R . .
C10 C 0.52786(7) 0.59321(7) 0.5083(2) 0.0271(5) Uani 1 1 d . . .
C11 C 0.60487(8) 0.66265(8) 0.2897(2) 0.0389(7) Uani 1 1 d . . .
H11A H 0.6094 0.6625 0.2072 0.047 Uiso 1 1 calc R . .
C12 C 0.57137(8) 0.63020(8) 0.3372(2) 0.0398(7) Uani 1 1 d . . .
H12A H 0.5530 0.6084 0.2881 0.048 Uiso 1 1 calc R . .
C13 C 0.56431(7) 0.62923(7) 0.4587(2) 0.0270(5) Uani 1 1 d . . .
C14 C 0.59207(7) 0.66212(7) 0.5245(2) 0.0314(6) Uani 1 1 d . . .
H14A H 0.5885 0.6627 0.6074 0.038 Uiso 1 1 calc R . .
C15 C 0.62498(7) 0.69411(7) 0.4694(2) 0.0311(6) Uani 1 1 d . . .
H15A H 0.6436 0.7166 0.5159 0.037 Uiso 1 1 calc R . .
C16 C 0.46232(7) 0.55354(7) 0.7820(2) 0.0333(6) Uani 1 1 d . . .
C17 C 0.44505(7) 0.51665(8) 0.8414(2) 0.0357(6) Uani 1 1 d . . .
H17A H 0.4435 0.4935 0.8039 0.043 Uiso 1 1 calc R . .
C18 C 0.43009(7) 0.51335(8) 0.9550(2) 0.0359(6) Uani 1 1 d . . .
H18A H 0.4184 0.4880 0.9950 0.043 Uiso 1 1 calc R . .
C19 C 0.43217(8) 0.54724(8) 1.0114(2) 0.0367(6) Uani 1 1 d . . .
C20 C 0.45030(8) 0.58352(8) 0.9528(2) 0.0401(7) Uani 1 1 d . . .
H20A H 0.4525 0.6069 0.9906 0.048 Uiso 1 1 calc R . .
C21 C 0.46554(8) 0.58701(8) 0.8396(2) 0.0401(7) Uani 1 1 d . . .
H21A H 0.4783 0.6127 0.8013 0.048 Uiso 1 1 calc R . .
C22 C 0.41767(8) 0.54360(8) 1.1361(2) 0.0406(7) Uani 1 1 d . . .
C23 C 0.38182(8) 0.50932(9) 1.1741(3) 0.0437(7) Uani 1 1 d . . .
C24 C 0.36867(9) 0.50451(11) 1.2906(3) 0.0552(8) Uani 1 1 d . . .
C25 C 0.39087(10) 0.53434(11) 1.3716(3) 0.0601(8) Uani 1 1 d . . .
C26 C 0.42631(10) 0.56900(11) 1.3374(3) 0.0564(8) Uani 1 1 d . . .
C27 C 0.43918(9) 0.57275(9) 1.2205(3) 0.0463(7) Uani 1 1 d . . .
F1 F 0.35928(5) 0.47944(6) 1.09967(17) 0.0570(5) Uani 1 1 d . . .
F2 F 0.33551(6) 0.47095(8) 1.32501(19) 0.0763(7) Uani 1 1 d . . .
F3 F 0.37866(7) 0.52985(8) 1.48408(18) 0.0873(7) Uani 1 1 d . . .
F4 F 0.44871(7) 0.59850(7) 1.41526(17) 0.0760(6) Uani 1 1 d . . .
F5 F 0.47452(6) 0.60664(6) 1.19328(16) 0.0567(5) Uani 1 1 d . . .
C100 C 0.3506(4) 0.5539(5) 0.7533(12) 0.136(6) Uani 0.50 1 d P A 1
H10A H 0.3782 0.5715 0.7189 0.163 Uiso 0.50 1 calc PR A 1
Cl10 Cl 0.34817(7) 0.50944(9) 0.7636(3) 0.0983(8) Uani 0.50 1 d P A 1
Cl11 Cl 0.35308(12) 0.57641(14) 0.8761(6) 0.208(2) Uani 0.50 1 d P A 1
Cl12 Cl 0.32040(15) 0.55462(16) 0.6491(6) 0.232(2) Uani 0.50 1 d P A 1
C200 C 0.3167(3) 0.56766(19) 1.1734(8) 0.083(3) Uani 0.50 1 d PD B 1
H20B H 0.3320 0.5781 1.2472 0.124 Uiso 0.50 1 calc PR B 1
H20C H 0.2962 0.5389 1.1832 0.124 Uiso 0.50 1 calc PR B 1
H20D H 0.3032 0.5831 1.1537 0.124 Uiso 0.50 1 calc PR B 1
O200 O 0.34235(18) 0.57154(19) 1.0857(10) 0.149(4) Uani 0.50 1 d PD B 1
H200 H 0.3621 0.5954 1.0847 0.223 Uiso 0.50 1 calc PR B 1
O300 O 0.3448(3) 0.5945(4) 1.3225(18) 0.233(6) Uani 0.50 1 d PU C 2
O400 O 0.3406(6) 0.5903(6) 1.460(3) 0.188(8) Uani 0.25 1 d PU D 3
O500 O 0.2641(5) 0.5445(6) 0.6479(19) 0.170(7) Uani 0.25 1 d P E 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 Zn1 N3 106.26(8) 15 .
N1 Zn1 Cl1 105.33(5) 15 .
N3 Zn1 Cl1 104.74(6) . .
N1 Zn1 Cl2 103.19(6) 15 .
N3 Zn1 Cl2 108.24(6) . .
Cl1 Zn1 Cl2 127.49(3) . .
C5 N1 C1 117.58(19) . .
C5 N1 Zn1 119.62(16) . 14_455
C1 N1 Zn1 122.64(14) . 14_455
C10 N2 C6 119.4(2) . .
C11 N3 C15 117.21(19) . .
C11 N3 Zn1 118.74(16) . .
C15 N3 Zn1 124.05(14) . .
N1 C1 C2 122.69(19) . .
N1 C1 H1A 118.7 . .
C2 C1 H1A 118.7 . .
C3 C2 C1 119.7(2) . .
C3 C2 H2A 120.2 . .
C1 C2 H2A 120.2 . .
C2 C3 C4 117.4(2) . .
C2 C3 C6 124.2(2) . .
C4 C3 C6 118.45(19) . .
C5 C4 C3 119.7(2) . .
C5 C4 H4A 120.1 . .
C3 C4 H4A 120.1 . .
N1 C5 C4 122.9(2) . .
N1 C5 H5A 118.5 . .
C4 C5 H5A 118.5 . .
N2 C6 C7 122.0(2) . .
N2 C6 C3 114.50(19) . .
C7 C6 C3 123.49(19) . .
C6 C7 C8 119.2(2) . .
C6 C7 H7A 120.4 . .
C8 C7 H7A 120.4 . .
C9 C8 C7 118.2(2) . .
C9 C8 C16 121.3(2) . .
C7 C8 C16 120.52(19) . .
C8 C9 C10 119.0(2) . .
C8 C9 H9A 120.5 . .
C10 C9 H9A 120.5 . .
N2 C10 C9 122.12(19) . .
N2 C10 C13 114.4(2) . .
C9 C10 C13 123.4(2) . .
N3 C11 C12 123.7(2) . .
N3 C11 H11A 118.1 . .
C12 C11 H11A 118.1 . .
C11 C12 C13 119.4(2) . .
C11 C12 H12A 120.3 . .
C13 C12 H12A 120.3 . .
C14 C13 C12 117.2(2) . .
C14 C13 C10 124.6(2) . .
C12 C13 C10 118.26(19) . .
C15 C14 C13 119.9(2) . .
C15 C14 H14A 120.1 . .
C13 C14 H14A 120.1 . .
N3 C15 C14 122.6(2) . .
N3 C15 H15A 118.7 . .
C14 C15 H15A 118.7 . .
C21 C16 C17 118.8(2) . .
C21 C16 C8 121.2(2) . .
C17 C16 C8 119.9(2) . .
C18 C17 C16 120.4(3) . .
C18 C17 H17A 119.8 . .
C16 C17 H17A 119.8 . .
C17 C18 C19 120.4(2) . .
C17 C18 H18A 119.8 . .
C19 C18 H18A 119.8 . .
C20 C19 C18 118.3(2) . .
C20 C19 C22 121.8(3) . .
C18 C19 C22 119.6(2) . .
C19 C20 C21 121.4(3) . .
C19 C20 H20A 119.3 . .
C21 C20 H20A 119.3 . .
C16 C21 C20 120.6(3) . .
C16 C21 H21A 119.7 . .
C20 C21 H21A 119.7 . .
C27 C22 C23 116.4(3) . .
C27 C22 C19 122.4(2) . .
C23 C22 C19 121.1(2) . .
F1 C23 C24 117.0(2) . .
F1 C23 C22 120.9(2) . .
C24 C23 C22 122.1(3) . .
F2 C24 C25 119.6(3) . .
F2 C24 C23 120.8(3) . .
C25 C24 C23 119.6(3) . .
F3 C25 C24 120.0(3) . .
F3 C25 C26 119.8(3) . .
C24 C25 C26 120.1(3) . .
F4 C26 C25 121.2(3) . .
F4 C26 C27 119.6(3) . .
C25 C26 C27 119.1(3) . .
F5 C27 C22 121.0(3) . .
F5 C27 C26 116.4(3) . .
C22 C27 C26 122.6(3) . .
Cl11 C100 Cl10 116.2(9) . .
Cl11 C100 Cl12 117.7(12) . .
Cl10 C100 Cl12 112.6(8) . .
Cl11 C100 H10A 102.5 . .
Cl10 C100 H10A 102.5 . .
Cl12 C100 H10A 102.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.0510(19) 15
Zn1 N3 2.0522(18) .
Zn1 Cl1 2.2126(7) .
Zn1 Cl2 2.2212(8) .
N1 C5 1.335(3) .
N1 C1 1.345(3) .
N1 Zn1 2.0508(19) 14_455
N2 C10 1.331(3) .
N2 C6 1.335(3) .
N3 C11 1.338(3) .
N3 C15 1.343(3) .
C1 C2 1.381(3) .
C1 H1A 0.9500 .
C2 C3 1.379(3) .
C2 H2A 0.9500 .
C3 C4 1.394(3) .
C3 C6 1.495(3) .
C4 C5 1.373(3) .
C4 H4A 0.9500 .
C5 H5A 0.9500 .
C6 C7 1.392(3) .
C7 C8 1.395(3) .
C7 H7A 0.9500 .
C8 C9 1.390(3) .
C8 C16 1.490(3) .
C9 C10 1.400(3) .
C9 H9A 0.9500 .
C10 C13 1.487(3) .
C11 C12 1.364(3) .
C11 H11A 0.9500 .
C12 C13 1.399(3) .
C12 H12A 0.9500 .
C13 C14 1.382(3) .
C14 C15 1.382(3) .
C14 H14A 0.9500 .
C15 H15A 0.9500 .
C16 C21 1.379(4) .
C16 C17 1.388(4) .
C17 C18 1.386(4) .
C17 H17A 0.9500 .
C18 C19 1.403(4) .
C18 H18A 0.9500 .
C19 C20 1.365(4) .
C19 C22 1.497(4) .
C20 C21 1.385(4) .
C20 H20A 0.9500 .
C21 H21A 0.9500 .
C22 C27 1.379(4) .
C22 C23 1.401(4) .
C23 F1 1.326(3) .
C23 C24 1.389(4) .
C24 F2 1.326(4) .
C24 C25 1.371(5) .
C25 F3 1.337(4) .
C25 C26 1.387(5) .
C26 F4 1.343(4) .
C26 C27 1.393(4) .
C27 F5 1.352(3) .
C100 Cl11 1.610(15) .
C100 Cl10 1.650(19) .
C100 Cl12 1.654(17) .
C100 H10A 1.0000 .
C200 O200 1.347(11) .
C200 H20B 0.9800 .
C200 H20C 0.9800 .
C200 H20D 0.9800 .
O200 H200 0.8400 .
