#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:20:38 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180473 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/42/7214268.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_7214268
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 Br12 F30 N18 Zn6'
_chemical_formula_sum            'C162 H84 Br12 F30 N18 Zn6'
_chemical_formula_weight         4203.61
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   38.394(4)
_cell_length_b                   38.394(4)
_cell_length_c                   11.5576(15)
_cell_measurement_reflns_used    6781
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      67.46
_cell_measurement_theta_min      4.05
_cell_volume                     14755(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1096
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29568
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.988
_diffrn_reflns_theta_min         4.049
_exptl_absorpt_coefficient_mu    4.311
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       Block
_exptl_crystal_F_000             6156
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
;
_refine_diff_density_max         1.403
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5754
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[σ²(Fo²)+(0.0865P)²+109.6151P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1903
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4031
_reflns_number_total             5754
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42012d.txt
_cod_data_source_block           squeeze
_cod_database_code               7214268
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.277
_shelx_estimated_absorpt_t_max   0.564
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Zn1 Zn 0.67666(2) 0.73935(2) 0.25725(6) 0.04206(16) Uani 1 1 d . .
Br1 Br 0.70693(2) 0.79248(2) 0.39013(5) 0.05374(15) Uani 1 1 d . .
Br2 Br 0.70942(2) 0.71150(2) 0.15231(5) 0.05297(14) Uani 1 1 d . .
N1 N 0.42614(10) 0.43946(10) 0.2040(3) 0.0397(10) Uani 1 1 d . .
N2 N 0.50957(11) 0.56293(11) 0.4321(3) 0.0428(10) Uani 1 1 d . .
N3 N 0.62936(12) 0.69400(11) 0.3433(3) 0.0436(10) Uani 1 1 d . .
C1 C 0.40929(13) 0.43186(13) 0.3092(4) 0.0427(12) Uani 1 1 d . .
H1A H 0.3863 0.4064 0.3238 0.051 Uiso 1 1 calc R U
C2 C 0.42449(13) 0.46026(14) 0.3978(4) 0.0435(12) Uani 1 1 d . .
H2A H 0.4115 0.4541 0.4711 0.052 Uiso 1 1 calc R U
C3 C 0.45829(13) 0.49737(13) 0.3798(4) 0.0403(12) Uani 1 1 d . .
C4 C 0.47498(14) 0.50446(13) 0.2699(4) 0.0431(12) Uani 1 1 d . U
H4A H 0.4979 0.5297 0.2526 0.052 Uiso 1 1 calc R U
C5 C 0.45863(14) 0.47536(15) 0.1859(5) 0.0475(13) Uani 1 1 d . U
H5A H 0.4710 0.4810 0.1118 0.057 Uiso 1 1 calc R U
C6 C 0.47618(14) 0.52929(13) 0.4674(4) 0.0442(12) Uani 1 1 d . .
C7 C 0.46175(14) 0.52658(13) 0.5785(4) 0.0430(12) Uani 1 1 d . .
H7A H 0.4383 0.5026 0.6019 0.052 Uiso 1 1 calc R U
C8 C 0.48080(14) 0.55833(14) 0.6575(4) 0.0464(13) Uani 1 1 d . .
C9 C 0.51481(14) 0.59209(13) 0.6181(4) 0.0434(12) Uani 1 1 d . .
H9A H 0.5290 0.6145 0.6680 0.052 Uiso 1 1 calc R U
C10 C 0.52841(14) 0.59362(13) 0.5063(4) 0.0437(13) Uani 1 1 d . .
C11 C 0.60331(19) 0.66197(16) 0.2857(5) 0.0633(18) Uani 1 1 d . .
H11A H 0.6072 0.6612 0.2048 0.076 Uiso 1 1 calc R U
C12 C 0.57063(19) 0.62929(16) 0.3358(5) 0.0618(18) Uani 1 1 d . .
H12A H 0.5529 0.6069 0.2896 0.074 Uiso 1 1 calc R U
C13 C 0.56396(14) 0.62929(13) 0.4524(4) 0.0448(13) Uani 1 1 d . .
C14 C 0.59100(14) 0.66275(14) 0.5130(5) 0.0463(13) Uani 1 1 d . .
H14A H 0.5878 0.6643 0.5940 0.056 Uiso 1 1 calc R U
C15 C 0.62284(14) 0.69409(14) 0.4564(5) 0.0478(13) Uani 1 1 d . .
H15A H 0.6411 0.7169 0.5003 0.057 Uiso 1 1 calc R U
C16 C 0.46528(14) 0.55539(15) 0.7761(5) 0.0502(14) Uani 1 1 d . .
C17 C 0.44756(14) 0.51878(15) 0.8359(5) 0.0513(14) Uani 1 1 d . .
H17A H 0.4456 0.4957 0.7992 0.062 Uiso 1 1 calc R U
C18 C 0.43293(15) 0.51538(16) 0.9471(5) 0.0517(14) Uani 1 1 d . .
H18A H 0.4216 0.4904 0.9869 0.062 Uiso 1 1 calc R U
C19 C 0.43492(15) 0.54897(17) 1.0003(5) 0.0542(15) Uani 1 1 d . .
C20 C 0.45293(16) 0.58582(16) 0.9396(5) 0.0568(15) Uani 1 1 d . .
H20A H 0.4554 0.6093 0.9752 0.068 Uiso 1 1 calc R U
C21 C 0.46649(15) 0.58767(15) 0.8321(5) 0.0521(13) Uani 1 1 d . .
H21A H 0.4776 0.6126 0.7920 0.063 Uiso 1 1 calc R U
C22 C 0.42077(16) 0.54567(18) 1.1234(5) 0.0603(16) Uani 1 1 d . .
C23 C 0.38682(18) 0.5123(2) 1.1635(5) 0.0687(19) Uani 1 1 d . .
C24 C 0.3730(2) 0.5068(3) 1.2774(6) 0.087(2) Uani 1 1 d . .
C25 C 0.3946(2) 0.5363(2) 1.3564(6) 0.086(2) Uani 1 1 d . .
C26 C 0.4290(2) 0.5708(2) 1.3208(6) 0.0797(18) Uani 1 1 d . .
C27 C 0.44083(17) 0.57392(18) 1.2071(6) 0.0665(16) Uani 1 1 d . .
F1 F 0.36304(10) 0.48208(12) 1.0879(3) 0.0806(12) Uani 1 1 d . .
F2 F 0.33974(12) 0.47305(17) 1.3083(4) 0.1107(18) Uani 1 1 d . .
F3 F 0.38322(13) 0.53182(17) 1.4661(4) 0.1151(16) Uani 1 1 d . .
F4 F 0.45034(13) 0.59999(13) 1.3967(4) 0.0997(13) Uani 1 1 d . .
F5 F 0.47563(11) 0.60857(11) 1.1777(3) 0.0745(11) 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 0.0181 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'
Br Br -0.6763 1.2805 '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'
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
N3 Zn1 N1 107.51(17) . 15
N3 Zn1 Br1 105.42(11) . .
N1 Zn1 Br1 105.19(10) 15 .
N3 Zn1 Br2 108.27(13) . .
N1 Zn1 Br2 103.34(11) 15 .
Br1 Zn1 Br2 125.98(3) . .
C5 N1 C1 117.9(4) . .
C5 N1 Zn1 120.0(3) . 14_455
C1 N1 Zn1 121.9(3) . 14_455
C10 N2 C6 119.0(4) . .
C11 N3 C15 116.3(4) . .
C11 N3 Zn1 119.3(4) . .
C15 N3 Zn1 124.4(3) . .
N1 C1 C2 121.9(4) . .
N1 C1 H1A 119.0 . .
C2 C1 H1A 119.0 . .
C3 C2 C1 120.4(4) . .
C3 C2 H2A 119.8 . .
C1 C2 H2A 119.8 . .
C2 C3 C4 116.4(4) . .
C2 C3 C6 124.2(4) . .
C4 C3 C6 119.4(4) . .
C5 C4 C3 120.6(4) . .
C5 C4 H4A 119.7 . .
C3 C4 H4A 119.7 . .
N1 C5 C4 122.7(5) . .
N1 C5 H5A 118.6 . .
C4 C5 H5A 118.6 . .
N2 C6 C7 120.4(4) . .
N2 C6 C3 114.4(4) . .
C7 C6 C3 125.1(4) . .
C6 C7 C8 121.7(4) . .
C6 C7 H7A 119.2 . .
C8 C7 H7A 119.2 . .
C9 C8 C7 116.1(5) . .
C9 C8 C16 122.4(4) . .
C7 C8 C16 121.6(4) . .
C8 C9 C10 120.6(4) . .
C8 C9 H9A 119.7 . .
C10 C9 H9A 119.7 . .
N2 C10 C9 122.3(4) . .
N2 C10 C13 112.4(4) . .
C9 C10 C13 125.3(4) . .
N3 C11 C12 124.0(5) . .
N3 C11 H11A 118.0 . .
C12 C11 H11A 118.0 . .
C13 C12 C11 119.7(5) . .
C13 C12 H12A 120.1 . .
C11 C12 H12A 120.1 . .
C12 C13 C14 116.6(4) . .
C12 C13 C10 119.5(4) . .
C14 C13 C10 123.9(5) . .
C13 C14 C15 120.0(5) . .
C13 C14 H14A 120.0 . .
C15 C14 H14A 120.0 . .
N3 C15 C14 123.3(4) . .
N3 C15 H15A 118.3 . .
C14 C15 H15A 118.3 . .
C21 C16 C17 116.9(5) . .
C21 C16 C8 122.4(5) . .
C17 C16 C8 120.7(5) . .
C18 C17 C16 121.6(5) . .
C18 C17 H17A 119.2 . .
C16 C17 H17A 119.2 . .
C17 C18 C19 119.4(5) . .
C17 C18 H18A 120.3 . .
C19 C18 H18A 120.3 . .
C18 C19 C20 118.7(5) . .
C18 C19 C22 119.2(5) . .
C20 C19 C22 122.0(5) . .
C21 C20 C19 119.9(5) . .
C21 C20 H20A 120.1 . .
C19 C20 H20A 120.1 . .
C20 C21 C16 123.5(5) . .
C20 C21 H21A 118.2 . .
C16 C21 H21A 118.2 . .
C27 C22 C23 113.3(5) . .
C27 C22 C19 124.4(5) . .
C23 C22 C19 122.2(5) . .
C22 C23 F1 119.5(5) . .
C22 C23 C24 124.9(6) . .
F1 C23 C24 115.5(5) . .
F2 C24 C25 121.1(6) . .
F2 C24 C23 120.4(6) . .
C25 C24 C23 118.5(6) . .
F3 C25 C24 120.4(6) . .
F3 C25 C26 120.3(6) . .
C24 C25 C26 119.3(6) . .
F4 C26 C27 121.2(6) . .
F4 C26 C25 120.0(6) . .
C27 C26 C25 118.8(6) . .
C22 C27 F5 118.8(5) . .
C22 C27 C26 125.2(5) . .
F5 C27 C26 116.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N3 2.039(4) .
Zn1 N1 2.068(4) 15
Zn1 Br1 2.3454(8) .
Zn1 Br2 2.3541(9) .
N1 C5 1.334(5) .
N1 C1 1.338(6) .
N1 Zn1 2.068(4) 14_455
N2 C10 1.340(6) .
N2 C6 1.350(5) .
N3 C11 1.314(6) .
N3 C15 1.331(7) .
C1 C2 1.394(7) .
C1 H1A 0.9500 .
C2 C3 1.381(6) .
C2 H2A 0.9500 .
C3 C4 1.386(7) .
C3 C6 1.469(6) .
C4 C5 1.372(7) .
C4 H4A 0.9500 .
C5 H5A 0.9500 .
C6 C7 1.381(7) .
C7 C8 1.401(7) .
C7 H7A 0.9500 .
C8 C9 1.379(6) .
C8 C16 1.476(8) .
C9 C10 1.383(7) .
C9 H9A 0.9500 .
C10 C13 1.503(6) .
C11 C12 1.381(7) .
C11 H11A 0.9500 .
C12 C13 1.372(8) .
C12 H12A 0.9500 .
C13 C14 1.373(6) .
C14 C15 1.378(6) .
C14 H14A 0.9500 .
C15 H15A 0.9500 .
C16 C21 1.378(8) .
C16 C17 1.400(8) .
C17 C18 1.382(8) .
C17 H17A 0.9500 .
C18 C19 1.396(9) .
C18 H18A 0.9500 .
C19 C20 1.412(8) .
C19 C22 1.505(8) .
C20 C21 1.336(8) .
C20 H20A 0.9500 .
C21 H21A 0.9500 .
C22 C27 1.368(8) .
C22 C23 1.373(8) .
C23 F1 1.373(7) .
C23 C24 1.395(9) .
C24 F2 1.334(8) .
C24 C25 1.367(10) .
C25 F3 1.324(8) .
C25 C26 1.384(9) .
C26 F4 1.333(8) .
C26 C27 1.376(9) .
C27 F5 1.376(6) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.006 1378 369 ' '
2 0.333 0.667 0.707 1372 369 ' '
3 0.667 0.333 0.374 1372 369 ' '
