# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

# OTBALB

_nottingham_internal_coll_name   OTBALB
_nottingham_internal_coll_number 11841
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time 20
_nottingham_internal_coll_frame_width '0.3 and 0.5'
_nottingham_internal_coll_frame_method '\w and \f'
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   10/09/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 13/09/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 21/12/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 21/12/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?

_audit_creation_method           SHELXL97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H21 I'
_chemical_formula_sum            'C22 H21 I'
_chemical_formula_weight         412.29

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.2219(8)
_cell_length_b                   8.8418(8)
_cell_length_c                   16.0675(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.897(7)
_cell_angle_gamma                90.00
_cell_volume                     1861.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    3408
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      25.76

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.078
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_max          0.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    1.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8903
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         27.26
_reflns_number_total             2084
_reflns_number_gt                1841
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.039P)²+1.277P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2084
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.10
_refine_ls_restrained_S_all      1.10
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
I1 I 0.5000 0.93978(3) 0.2500 0.03471(12) Uani 1 2 d S . .
C1 C 0.5000 0.7016(4) 0.2500 0.0230(8) Uani 1 2 d S . .
C2 C 0.4695(2) 0.6254(3) 0.31217(19) 0.0244(6) Uani 1 1 d . . .
C3 C 0.4714(2) 0.4680(3) 0.3114(2) 0.0329(7) Uani 1 1 d . . .
H3 H 0.4529 0.4133 0.3536 0.039 Uiso 1 1 calc R . .
C4 C 0.5000 0.3893(5) 0.2500 0.0404(11) Uani 1 2 d S . .
H4 H 0.5000 0.2819 0.2500 0.048 Uiso 1 2 calc SR . .
C5 C 0.4349(2) 0.7063(3) 0.37639(19) 0.0263(6) Uani 1 1 d . . .
C6 C 0.3308(2) 0.7409(3) 0.3499(2) 0.0313(7) Uani 1 1 d . . .
C7 C 0.2987(2) 0.8171(4) 0.4099(2) 0.0354(7) Uani 1 1 d . . .
H7 H 0.2285 0.8407 0.3926 0.042 Uiso 1 1 calc R . .
C8 C 0.3683(3) 0.8590(4) 0.4947(2) 0.0369(7) Uani 1 1 d . . .
H8 H 0.3456 0.9110 0.5352 0.044 Uiso 1 1 calc R . .
C9 C 0.4704(3) 0.8253(4) 0.5203(2) 0.0359(7) Uani 1 1 d . . .
H9 H 0.5177 0.8558 0.5782 0.043 Uiso 1 1 calc R . .
C10 C 0.5053(2) 0.7469(3) 0.46236(19) 0.0303(6) Uani 1 1 d . . .
C11 C 0.2553(2) 0.6970(4) 0.2569(2) 0.0383(8) Uani 1 1 d . . .
H11A H 0.2697 0.7544 0.2111 0.057 Uiso 1 1 calc R . .
H11B H 0.1858 0.7196 0.2521 0.057 Uiso 1 1 calc R . .
H11C H 0.2613 0.5885 0.2475 0.057 Uiso 1 1 calc R . .
C12 C 0.6170(2) 0.7103(4) 0.4916(2) 0.0411(8) Uani 1 1 d . . .
H12A H 0.6272 0.6011 0.5018 0.062 Uiso 1 1 calc R . .
H12B H 0.6560 0.7644 0.5478 0.062 Uiso 1 1 calc R . .
H12C H 0.6405 0.7415 0.4444 0.062 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
I1 C1 2.106(4) . ?
C1 C2 1.406(3) 2_655 ?
C1 C2 1.406(3) . ?
C2 C3 1.393(4) . ?
C2 C5 1.488(4) . ?
C3 C4 1.391(4) . ?
C3 H3 0.9500 . ?
C4 C3 1.391(4) 2_655 ?
C4 H4 0.9500 . ?
C5 C10 1.401(4) . ?
C5 C6 1.405(4) . ?
C6 C7 1.390(4) . ?
C6 C11 1.512(4) . ?
C7 C8 1.387(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.398(4) . ?
C9 H9 0.9500 . ?
C10 C12 1.507(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
C2 C1 C2 122.8(3) 2_655 . ?
C2 C1 I1 118.60(17) 2_655 . ?
C2 C1 I1 118.60(17) . . ?
C3 C2 C1 117.3(3) . . ?
C3 C2 C5 120.0(3) . . ?
C1 C2 C5 122.7(3) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C3 119.9(4) . 2_655 ?
C3 C4 H4 120.0 . . ?
C3 C4 H4 120.0 2_655 . ?
C10 C5 C6 120.5(3) . . ?
C10 C5 C2 120.3(2) . . ?
C6 C5 C2 119.2(2) . . ?
C7 C6 C5 119.1(3) . . ?
C7 C6 C11 120.7(3) . . ?
C5 C6 C11 120.2(3) . . ?
C8 C7 C6 120.7(3) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.9(3) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C5 118.8(3) . . ?
C9 C10 C12 120.2(3) . . ?
C5 C10 C12 121.0(3) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C3 0.8(2) 2_655 . . . ?
I1 C1 C2 C3 -179.2(2) . . . . ?
C2 C1 C2 C5 -178.5(3) 2_655 . . . ?
I1 C1 C2 C5 1.5(3) . . . . ?
C1 C2 C3 C4 -1.6(4) . . . . ?
C5 C2 C3 C4 177.7(2) . . . . ?
C2 C3 C4 C3 0.8(2) . . . 2_655 ?
C3 C2 C5 C10 90.3(4) . . . . ?
C1 C2 C5 C10 -90.4(3) . . . . ?
C3 C2 C5 C6 -89.5(4) . . . . ?
C1 C2 C5 C6 89.8(3) . . . . ?
C10 C5 C6 C7 0.6(4) . . . . ?
C2 C5 C6 C7 -179.7(3) . . . . ?
C10 C5 C6 C11 179.9(3) . . . . ?
C2 C5 C6 C11 -0.4(4) . . . . ?
C5 C6 C7 C8 0.2(5) . . . . ?
C11 C6 C7 C8 -179.2(3) . . . . ?
C6 C7 C8 C9 0.1(5) . . . . ?
C7 C8 C9 C10 -1.0(5) . . . . ?
C8 C9 C10 C5 1.7(4) . . . . ?
C8 C9 C10 C12 -179.7(3) . . . . ?
C6 C5 C10 C9 -1.5(4) . . . . ?
C2 C5 C10 C9 178.8(3) . . . . ?
C6 C5 C10 C12 179.9(3) . . . . ?
C2 C5 C10 C12 0.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.26
_diffrn_measured_fraction_theta_full 0.993

_refine_diff_density_max         0.71
_refine_diff_density_min         -0.70
_refine_diff_density_rms         0.10
_database_code_depnum_ccdc_archive 'CCDC 989599'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

#OTBALA

_nottingham_internal_coll_name   OTBALA
_nottingham_internal_coll_number 11746
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time 5
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   09/08/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 09/08/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 21/12/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 21/12/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?


_audit_creation_method           SHELXL97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H21 I'
_chemical_formula_sum            'C22 H21 I'
_chemical_formula_weight         412.29

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   7.759(2)
_cell_length_b                   27.311(8)
_cell_length_c                   8.450(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1790.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    8288
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      27.57

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_T_max  0.397
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7411
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.022
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         25.03
_reflns_number_total             1610
_reflns_number_gt                1590
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+11.68P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1610
_refine_ls_number_parameters     111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.102
_refine_ls_wR_factor_gt          0.102
_refine_ls_goodness_of_fit_ref   1.50
_refine_ls_restrained_S_all      1.50
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
I1 I 0.22507(6) 0.2500 0.61203(7) 0.02072(19) Uani 1 2 d S . .
C1 C -0.0263(9) 0.2500 0.5211(8) 0.0124(15) Uani 1 2 d S . .
C2 C -0.1064(7) 0.29464(18) 0.4857(6) 0.0128(10) Uani 1 1 d . . .
C3 C -0.2666(7) 0.29361(19) 0.4121(6) 0.0180(11) Uani 1 1 d . . .
H3 H -0.3218 0.3237 0.3872 0.022 Uiso 1 1 calc R . .
C4 C -0.3483(10) 0.2500 0.3740(10) 0.0225(18) Uani 1 2 d S . .
H4 H -0.4575 0.2500 0.3230 0.027 Uiso 1 2 calc SR . .
C5 C -0.0284(6) 0.34321(18) 0.5235(6) 0.0129(11) Uani 1 1 d . . .
C6 C -0.0056(7) 0.35869(19) 0.6785(6) 0.0152(11) Uani 1 1 d . . .
H6 H -0.0357 0.3372 0.7626 0.018 Uiso 1 1 calc R . .
C7 C 0.0596(6) 0.40433(18) 0.7139(6) 0.0133(11) Uani 1 1 d . . .
C8 C 0.1066(7) 0.43526(19) 0.5897(7) 0.0182(12) Uani 1 1 d . . .
H8 H 0.1535 0.4666 0.6127 0.022 Uiso 1 1 calc R . .
C9 C 0.0860(6) 0.42105(19) 0.4336(6) 0.0147(11) Uani 1 1 d . . .
C10 C 0.0153(7) 0.37498(19) 0.4027(6) 0.0158(11) Uani 1 1 d . . .
H10 H -0.0032 0.3653 0.2961 0.019 Uiso 1 1 calc R . .
C11 C 0.0795(7) 0.42075(19) 0.8838(6) 0.0183(11) Uani 1 1 d . . .
H11A H 0.2013 0.4192 0.9141 0.027 Uiso 1 1 calc R . .
H11B H 0.0120 0.3992 0.9529 0.027 Uiso 1 1 calc R . .
H11C H 0.0382 0.4545 0.8946 0.027 Uiso 1 1 calc R . .
C12 C 0.1405(8) 0.4540(2) 0.3001(7) 0.0223(12) Uani 1 1 d . . .
H12A H 0.2390 0.4394 0.2449 0.033 Uiso 1 1 calc R . .
H12B H 0.1735 0.4861 0.3426 0.033 Uiso 1 1 calc R . .
H12C H 0.0445 0.4580 0.2258 0.033 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
I1 C1 2.097(7) . ?
C1 C2 1.401(6) 8_565 ?
C1 C2 1.401(6) . ?
C2 C3 1.390(7) . ?
C2 C5 1.493(7) . ?
C3 C4 1.387(7) . ?
C3 H3 0.9500 . ?
C4 C3 1.387(7) 8_565 ?
C4 H4 0.9500 . ?
C5 C10 1.382(7) . ?
C5 C6 1.388(8) . ?
C6 C7 1.378(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(7) . ?
C7 C11 1.512(7) . ?
C8 C9 1.385(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.397(7) . ?
C9 C12 1.503(7) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
C2 C1 C2 121.0(7) 8_565 . ?
C2 C1 I1 119.4(3) 8_565 . ?
C2 C1 I1 119.4(3) . . ?
C3 C2 C1 118.3(5) . . ?
C3 C2 C5 118.5(5) . . ?
C1 C2 C5 123.2(5) . . ?
C4 C3 C2 122.0(5) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C3 118.3(7) . 8_565 ?
C3 C4 H4 120.8 . . ?
C3 C4 H4 120.8 8_565 . ?
C10 C5 C6 118.3(5) . . ?
C10 C5 C2 120.0(5) . . ?
C6 C5 C2 121.6(5) . . ?
C7 C6 C5 121.8(5) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C8 118.7(5) . . ?
C6 C7 C11 120.8(5) . . ?
C8 C7 C11 120.5(5) . . ?
C9 C8 C7 121.1(5) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 118.4(5) . . ?
C8 C9 C12 121.0(5) . . ?
C10 C9 C12 120.6(5) . . ?
C5 C10 C9 121.6(5) . . ?
C5 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C3 -1.0(10) 8_565 . . . ?
I1 C1 C2 C3 174.2(4) . . . . ?
C2 C1 C2 C5 178.9(4) 8_565 . . . ?
I1 C1 C2 C5 -6.0(8) . . . . ?
C1 C2 C3 C4 0.2(9) . . . . ?
C5 C2 C3 C4 -179.6(6) . . . . ?
C2 C3 C4 C3 0.5(11) . . . 8_565 ?
C3 C2 C5 C10 -63.8(7) . . . . ?
C1 C2 C5 C10 116.4(6) . . . . ?
C3 C2 C5 C6 113.0(6) . . . . ?
C1 C2 C5 C6 -66.8(7) . . . . ?
C10 C5 C6 C7 -0.3(8) . . . . ?
C2 C5 C6 C7 -177.2(5) . . . . ?
C5 C6 C7 C8 -1.2(8) . . . . ?
C5 C6 C7 C11 178.6(5) . . . . ?
C6 C7 C8 C9 1.1(8) . . . . ?
C11 C7 C8 C9 -178.8(5) . . . . ?
C7 C8 C9 C10 0.6(8) . . . . ?
C7 C8 C9 C12 -178.6(5) . . . . ?
C6 C5 C10 C9 2.0(8) . . . . ?
C2 C5 C10 C9 178.9(5) . . . . ?
C8 C9 C10 C5 -2.2(8) . . . . ?
C12 C9 C10 C5 177.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         1.61
_refine_diff_density_min         -2.63
_refine_diff_density_rms         0.12
_database_code_depnum_ccdc_archive 'CCDC 989600'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

#ARDLKB

_nottingham_internal_coll_name   ARDLKB
_nottingham_internal_coll_number 11164
_nottingham_internal_coll_client AR/DLK
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time 30
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   11/2/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user WL
_nottingham_internal_process_date 13/02/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 07/08/2013
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 07/08/2013
_nottingham_internal_validation_user WL
_nottingham_internal_validation_date 27/9/2013
_nottingham_internal_archive_date 27/9/2013


_audit_creation_date             2013-08-07
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H33 I'
_chemical_formula_sum            'C28 H33 I'
_chemical_formula_weight         496.44
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.708(2)
_cell_length_b                   9.292(3)
_cell_length_c                   15.373(4)
_cell_angle_alpha                73.294(4)
_cell_angle_beta                 77.896(4)
_cell_angle_gamma                77.855(4)
_cell_volume                     1149.9(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8952
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.32
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.0760 before and 0.0319 after correction.
The Ratio of minimum to maximum transmission is 0.7242.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.23
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9719
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.379
_diffrn_reflns_theta_min         2.318
_diffrn_ambient_temperature      90.15
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4872
_reflns_number_total             5041
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5041
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0616P)²+0.8218P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0900
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.96185(2) 0.93997(2) 0.62751(2) 0.02219(8) Uani 1 1 d . . . . .
C1 C 0.7907(3) 1.0084(3) 0.73259(16) 0.0201(4) Uani 1 1 d . . . . .
C2 C 0.8123(3) 0.9365(3) 0.82401(16) 0.0209(4) Uani 1 1 d . . . . .
C3 C 0.7031(3) 0.9868(3) 0.89371(16) 0.0230(4) Uani 1 1 d . . . . .
H3 H 0.7157 0.9404 0.9560 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5768(3) 1.1026(3) 0.87422(18) 0.0252(5) Uani 1 1 d . . . . .
H4 H 0.5044 1.1363 0.9226 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5569(3) 1.1691(3) 0.78334(17) 0.0234(5) Uani 1 1 d . . . . .
H5 H 0.4689 1.2473 0.7702 0.028 Uiso 1 1 calc R U . . .
C6 C 0.6627(3) 1.1241(3) 0.71068(16) 0.0208(4) Uani 1 1 d . . . . .
C7 C 0.9474(3) 0.8147(3) 0.84871(16) 0.0205(4) Uani 1 1 d . . . . .
C8 C 0.9426(3) 0.6635(3) 0.84873(16) 0.0219(4) Uani 1 1 d . . . . .
C9 C 1.0699(3) 0.5500(3) 0.87390(16) 0.0243(5) Uani 1 1 d . . . . .
C10 C 1.2001(3) 0.5854(3) 0.89909(17) 0.0248(5) Uani 1 1 d . . . . .
C11 C 1.2056(3) 0.7357(3) 0.89762(16) 0.0231(5) Uani 1 1 d . . . . .
C12 C 1.0793(3) 0.8508(3) 0.87179(16) 0.0209(4) Uani 1 1 d . . . . .
C13 C 0.8025(3) 0.6260(3) 0.8203(2) 0.0293(5) Uani 1 1 d . . . . .
H13A H 0.8379 0.5925 0.7634 0.044 Uiso 1 1 calc R U . . .
H13B H 0.7208 0.7167 0.8101 0.044 Uiso 1 1 calc R U . . .
H13C H 0.7581 0.5444 0.8690 0.044 Uiso 1 1 calc R U . . .
C14 C 1.0678(4) 0.3875(3) 0.8747(2) 0.0319(6) Uani 1 1 d . . . . .
H14A H 1.0470 0.3269 0.9384 0.048 Uiso 1 1 calc R U . . .
H14B H 1.1711 0.3450 0.8445 0.048 Uiso 1 1 calc R U . . .
H14C H 0.9840 0.3851 0.8416 0.048 Uiso 1 1 calc R U . . .
C15 C 1.3362(4) 0.4608(3) 0.9270(2) 0.0329(6) Uani 1 1 d . . . . .
H15A H 1.4003 0.4323 0.8722 0.049 Uiso 1 1 calc R U . . .
H15B H 1.2939 0.3719 0.9694 0.049 Uiso 1 1 calc R U . . .
H15C H 1.4027 0.4974 0.9575 0.049 Uiso 1 1 calc R U . . .
C16 C 1.3467(3) 0.7740(3) 0.9245(2) 0.0334(6) Uani 1 1 d . . . . .
H16A H 1.3341 0.8843 0.9157 0.050 Uiso 1 1 calc R U . . .
H16B H 1.4446 0.7399 0.8860 0.050 Uiso 1 1 calc R U . . .
H16C H 1.3529 0.7226 0.9893 0.050 Uiso 1 1 calc R U . . .
C17 C 1.0846(3) 1.0139(3) 0.86735(18) 0.0261(5) Uani 1 1 d . . . . .
H17A H 1.0643 1.0276 0.9299 0.039 Uiso 1 1 calc R U . . .
H17B H 1.0032 1.0812 0.8326 0.039 Uiso 1 1 calc R U . . .
H17C H 1.1898 1.0388 0.8367 0.039 Uiso 1 1 calc R U . . .
C18 C 0.6307(3) 1.1972(3) 0.61450(17) 0.0202(4) Uani 1 1 d . . . . .
C19 C 0.5030(3) 1.1618(3) 0.58644(16) 0.0211(4) Uani 1 1 d . . . . .
C20 C 0.4710(3) 1.2298(3) 0.49683(17) 0.0221(4) Uani 1 1 d . . . . .
C21 C 0.5714(3) 1.3259(3) 0.43425(17) 0.0236(5) Uani 1 1 d . . . . .
C22 C 0.6964(3) 1.3645(3) 0.46345(17) 0.0236(5) Uani 1 1 d . . . . .
C23 C 0.7248(3) 1.3024(3) 0.55416(17) 0.0223(4) Uani 1 1 d . . . . .
C24 C 0.3988(3) 1.0515(3) 0.65052(18) 0.0259(5) Uani 1 1 d . . . . .
H24A H 0.4525 0.9914 0.7026 0.039 Uiso 1 1 calc R U . . .
H24B H 0.3790 0.9834 0.6173 0.039 Uiso 1 1 calc R U . . .
H24C H 0.2975 1.1082 0.6733 0.039 Uiso 1 1 calc R U . . .
C25 C 0.3268(3) 1.1982(3) 0.46996(19) 0.0289(5) Uani 1 1 d . . . . .
H25A H 0.3478 1.0951 0.4612 0.043 Uiso 1 1 calc R U . . .
H25B H 0.3035 1.2721 0.4125 0.043 Uiso 1 1 calc R U . . .
H25C H 0.2353 1.2071 0.5187 0.043 Uiso 1 1 calc R U . . .
C26 C 0.5462(4) 1.3898(3) 0.33500(19) 0.0300(6) Uani 1 1 d . . . . .
H26A H 0.4891 1.3237 0.3185 0.045 Uiso 1 1 calc R U . . .
H26B H 0.6495 1.3950 0.2949 0.045 Uiso 1 1 calc R U . . .
H26C H 0.4835 1.4922 0.3274 0.045 Uiso 1 1 calc R U . . .
C27 C 0.7982(3) 1.4743(3) 0.39686(19) 0.0304(6) Uani 1 1 d . . . . .
H27A H 0.8861 1.4807 0.4256 0.046 Uiso 1 1 calc R U . . .
H27B H 0.7335 1.5751 0.3805 0.046 Uiso 1 1 calc R U . . .
H27C H 0.8411 1.4383 0.3412 0.046 Uiso 1 1 calc R U . . .
C28 C 0.8530(3) 1.3509(3) 0.58712(19) 0.0284(5) Uani 1 1 d . . . . .
H28A H 0.8486 1.3064 0.6535 0.043 Uiso 1 1 calc R U . . .
H28B H 0.8360 1.4621 0.5744 0.043 Uiso 1 1 calc R U . . .
H28C H 0.9575 1.3155 0.5549 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
I1 C1 2.102(2) . ?
C1 C2 1.405(3) . ?
C1 C6 1.398(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.480(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.395(3) . ?
C6 C18 1.497(3) . ?
C7 C8 1.414(3) . ?
C7 C12 1.400(3) . ?
C8 C9 1.395(3) . ?
C8 C13 1.514(3) . ?
C9 C10 1.399(4) . ?
C9 C14 1.510(3) . ?
C10 C11 1.402(3) . ?
C10 C15 1.510(3) . ?
C11 C12 1.398(3) . ?
C11 C16 1.513(4) . ?
C12 C17 1.507(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.402(3) . ?
C18 C23 1.409(3) . ?
C19 C20 1.401(3) . ?
C19 C24 1.510(3) . ?
C20 C21 1.403(3) . ?
C20 C25 1.509(3) . ?
C21 C22 1.405(3) . ?
C21 C26 1.515(3) . ?
C22 C23 1.400(3) . ?
C22 C27 1.508(3) . ?
C23 C28 1.512(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

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
C2 C1 I1 117.66(17) . . ?
C6 C1 I1 120.22(17) . . ?
C6 C1 C2 122.1(2) . . ?
C1 C2 C7 123.0(2) . . ?
C3 C2 C1 117.7(2) . . ?
C3 C2 C7 119.2(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.5(2) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.3(2) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.7(2) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C18 123.6(2) . . ?
C5 C6 C1 117.5(2) . . ?
C5 C6 C18 118.8(2) . . ?
C8 C7 C2 120.0(2) . . ?
C12 C7 C2 119.4(2) . . ?
C12 C7 C8 120.6(2) . . ?
C7 C8 C13 120.5(2) . . ?
C9 C8 C7 119.0(2) . . ?
C9 C8 C13 120.5(2) . . ?
C8 C9 C10 120.3(2) . . ?
C8 C9 C14 120.2(2) . . ?
C10 C9 C14 119.5(2) . . ?
C9 C10 C11 120.5(2) . . ?
C9 C10 C15 119.6(2) . . ?
C11 C10 C15 119.9(2) . . ?
C10 C11 C16 120.4(2) . . ?
C12 C11 C10 119.7(2) . . ?
C12 C11 C16 119.9(2) . . ?
C7 C12 C17 119.6(2) . . ?
C11 C12 C7 119.8(2) . . ?
C11 C12 C17 120.6(2) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C6 118.8(2) . . ?
C19 C18 C23 120.7(2) . . ?
C23 C18 C6 120.5(2) . . ?
C18 C19 C24 121.6(2) . . ?
C20 C19 C18 119.5(2) . . ?
C20 C19 C24 118.9(2) . . ?
C19 C20 C21 120.1(2) . . ?
C19 C20 C25 118.6(2) . . ?
C21 C20 C25 121.3(2) . . ?
C20 C21 C22 120.1(2) . . ?
C20 C21 C26 120.6(2) . . ?
C22 C21 C26 119.3(2) . . ?
C21 C22 C27 119.6(2) . . ?
C23 C22 C21 120.1(2) . . ?
C23 C22 C27 120.3(2) . . ?
C18 C23 C28 120.6(2) . . ?
C22 C23 C18 119.3(2) . . ?
C22 C23 C28 120.0(2) . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I1 C1 C2 C3 176.97(17) . . . . ?
I1 C1 C2 C7 -1.0(3) . . . . ?
I1 C1 C6 C5 -177.23(17) . . . . ?
I1 C1 C6 C18 5.1(3) . . . . ?
C1 C2 C3 C4 0.5(4) . . . . ?
C1 C2 C7 C8 -80.4(3) . . . . ?
C1 C2 C7 C12 99.5(3) . . . . ?
C1 C6 C18 C19 106.7(3) . . . . ?
C1 C6 C18 C23 -74.9(3) . . . . ?
C2 C1 C6 C5 1.2(3) . . . . ?
C2 C1 C6 C18 -176.4(2) . . . . ?
C2 C3 C4 C5 0.9(4) . . . . ?
C2 C7 C8 C9 -178.8(2) . . . . ?
C2 C7 C8 C13 2.2(4) . . . . ?
C2 C7 C12 C11 178.3(2) . . . . ?
C2 C7 C12 C17 -2.5(3) . . . . ?
C3 C2 C7 C8 101.6(3) . . . . ?
C3 C2 C7 C12 -78.5(3) . . . . ?
C3 C4 C5 C6 -1.2(4) . . . . ?
C4 C5 C6 C1 0.1(4) . . . . ?
C4 C5 C6 C18 177.9(2) . . . . ?
C5 C6 C18 C19 -70.9(3) . . . . ?
C5 C6 C18 C23 107.5(3) . . . . ?
C6 C1 C2 C3 -1.5(3) . . . . ?
C6 C1 C2 C7 -179.5(2) . . . . ?
C6 C18 C19 C20 179.7(2) . . . . ?
C6 C18 C19 C24 -0.5(3) . . . . ?
C6 C18 C23 C22 177.5(2) . . . . ?
C6 C18 C23 C28 -3.8(3) . . . . ?
C7 C2 C3 C4 178.5(2) . . . . ?
C7 C8 C9 C10 0.3(3) . . . . ?
C7 C8 C9 C14 179.9(2) . . . . ?
C8 C7 C12 C11 -1.8(4) . . . . ?
C8 C7 C12 C17 177.4(2) . . . . ?
C8 C9 C10 C11 -1.3(4) . . . . ?
C8 C9 C10 C15 179.4(2) . . . . ?
C9 C10 C11 C12 0.7(4) . . . . ?
C9 C10 C11 C16 -179.8(2) . . . . ?
C10 C11 C12 C7 0.8(3) . . . . ?
C10 C11 C12 C17 -178.4(2) . . . . ?
C12 C7 C8 C9 1.3(4) . . . . ?
C12 C7 C8 C13 -177.7(2) . . . . ?
C13 C8 C9 C10 179.2(2) . . . . ?
C13 C8 C9 C14 -1.1(4) . . . . ?
C14 C9 C10 C11 179.1(2) . . . . ?
C14 C9 C10 C15 -0.2(4) . . . . ?
C15 C10 C11 C12 -180.0(2) . . . . ?
C15 C10 C11 C16 -0.4(4) . . . . ?
C16 C11 C12 C7 -178.7(2) . . . . ?
C16 C11 C12 C17 2.1(3) . . . . ?
C18 C19 C20 C21 3.5(3) . . . . ?
C18 C19 C20 C25 -176.1(2) . . . . ?
C19 C18 C23 C22 -4.2(4) . . . . ?
C19 C18 C23 C28 174.5(2) . . . . ?
C19 C20 C21 C22 -5.5(4) . . . . ?
C19 C20 C21 C26 175.0(2) . . . . ?
C20 C21 C22 C23 2.5(4) . . . . ?
C20 C21 C22 C27 -176.8(2) . . . . ?
C21 C22 C23 C18 2.2(3) . . . . ?
C21 C22 C23 C28 -176.5(2) . . . . ?
C23 C18 C19 C20 1.3(4) . . . . ?
C23 C18 C19 C24 -178.9(2) . . . . ?
C24 C19 C20 C21 -176.3(2) . . . . ?
C24 C19 C20 C25 4.1(3) . . . . ?
C25 C20 C21 C22 174.1(2) . . . . ?
C25 C20 C21 C26 -5.4(4) . . . . ?
C26 C21 C22 C23 -177.9(2) . . . . ?
C26 C21 C22 C27 2.8(4) . . . . ?
C27 C22 C23 C18 -178.4(2) . . . . ?
C27 C22 C23 C28 2.9(4) . . . . ?

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 989601'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

#LITBLA

_nottingham_internal_coll_name   LITBLA
_nottingham_internal_coll_number 12726
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time 10,20,80
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   14/08/2013
_nottingham_internal_coll_location NOTT
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 07/03/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 20/08/2013
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 20/08/2013
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 11/2/2014
_nottingham_internal_archive_date 11/2/2014

_refine_special_details          
;
The flanking aryl group C81-C88 is disordered over two positions. 
The occupancies of the two components were refined competitively, 
converging at a ratio of 0.51:0.49. The central aryl ring C23-C28 
was also disordered over two positions. The occupancies of the 
two components were refined competitively, converging at a ratio 
of 0.54:0.46. Chemically equivalent 1,2-distances of the disordered 
rings were restrained to be approximately equal. Global enhanced 
rigid bond restraints were applied to the structure.
;


_audit_creation_date             2013-10-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C44 H42 Li2'
_chemical_formula_sum            'C44 H42 Li2'
_chemical_formula_weight         584.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H42 Li2'
_chemical_oxdiff_usercomment     
'LITBALA1 #12726 mounted in fomblin film on micromount for TB/DLK'
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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.6871(3)
_cell_length_b                   42.4827(9)
_cell_length_c                   15.9595(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.596(3)
_cell_angle_gamma                90
_cell_volume                     6944.0(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    12547
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      69.2540
_cell_measurement_theta_min      4.2440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  1.212
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.3398
_exptl_crystal_size_mid          0.2307
_exptl_crystal_size_min          0.1218
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30836
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.071
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.0750
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9838
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -80.00  -36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 44

#__ type_ start__ end____ width___ exp.time_
  2 omega -116.00  -81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000   60.0000 35

#__ type_ start__ end____ width___ exp.time_
  3 omega  -71.00  -45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega  -49.00   36.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   38.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
  5 omega    2.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 51

#__ type_ start__ end____ width___ exp.time_
  6 omega   68.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 52

#__ type_ start__ end____ width___ exp.time_
  7 omega    4.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000 -120.0000 61

#__ type_ start__ end____ width___ exp.time_
  8 omega   32.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -30.0000 90

#__ type_ start__ end____ width___ exp.time_
  9 omega   57.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 34

#__ type_ start__ end____ width___ exp.time_
 10 omega   37.00   87.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 50

#__ type_ start__ end____ width___ exp.time_
 11 omega   35.00   82.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 47

#__ type_ start__ end____ width___ exp.time_
 12 omega   32.00  112.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000 -150.0000 80

#__ type_ start__ end____ width___ exp.time_
 13 omega   42.00  149.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000   90.0000 107

#__ type_ start__ end____ width___ exp.time_
 14 omega  124.00  150.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 15 omega   36.00  103.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -60.0000 67

#__ type_ start__ end____ width___ exp.time_
 16 omega   49.00   75.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   47.00   73.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 18 omega   49.00   75.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega   88.00  113.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 20 omega  149.00  175.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 21 omega   49.00  116.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 67

#__ type_ start__ end____ width___ exp.time_
 22 omega   83.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 23 omega   33.00   74.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 41

#__ type_ start__ end____ width___ exp.time_
 24 omega  133.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000  -90.0000 44

#__ type_ start__ end____ width___ exp.time_
 25 omega   50.00  128.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000  -90.0000 78
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0763598000
_diffrn_orient_matrix_UB_12      -0.0287786000
_diffrn_orient_matrix_UB_13      -0.0469949000
_diffrn_orient_matrix_UB_21      -0.1130345000
_diffrn_orient_matrix_UB_22      0.0217060000
_diffrn_orient_matrix_UB_23      -0.0483998000
_diffrn_orient_matrix_UB_31      0.0632976000
_diffrn_orient_matrix_UB_32      0.0040491000
_diffrn_orient_matrix_UB_33      -0.0747904000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10029
_reflns_number_total             12192
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         12192
_refine_ls_number_restraints     1167
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0745
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+11.7159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.1870
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C26 \\sim C26-C27 \\sim C25A-C26A \\sim C26A-C27A
 with sigma of 0.02
 C23-C24 \\sim C23-C28 \\sim C23A-C24A \\sim C23A-C28A
 with sigma of 0.02
 C24-C25 \\sim C27-C28 \\sim C24A-C25A \\sim C27A-C28A
 with sigma of 0.02
 C25-C26 \\sim C26-C27 \\sim C25A-C26A \\sim C26A-C27A
 with sigma of 0.02
 C24-C29 \\sim C24A-C29 \\sim C28-C37 \\sim C28A-C37
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=1-FVAR(1)
 Sof(C28)=Sof(C26)=Sof(H26)=Sof(C25)=Sof(H25)=Sof(C23)=Sof(C27)=Sof(H27)=
 Sof(C24)=FVAR(1)
 Sof(C81A)=Sof(C82A)=Sof(H82A)=Sof(C86A)=Sof(H86A)=Sof(C85A)=Sof(C84A)=
 Sof(H84A)=Sof(C83A)=Sof(C87A)=Sof(H87D)=Sof(H87E)=Sof(H87F)=Sof(C88A)=
 Sof(H88D)=Sof(H88E)=Sof(H88F)=1-FVAR(2)
 Sof(C81)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(C84)=Sof(H84)=Sof(C85)=Sof(C86)=
 Sof(H86)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C88)=Sof(H88A)=Sof(H88B)=
 Sof(H88C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12), C16(H16), C18(H18),
 C20(H20), C30(H30), C32(H32), C34(H34), C38(H38), C40(H40), C42(H42), C47(H47),
  C48(H48), C49(H49), C52(H52), C54(H54), C56(H56), C60(H60), C62(H62),
 C64(H64), C69(H69), C70(H70), C71(H71), C74(H74), C76(H76), C78(H78), C82(H82),
  C84(H84), C86(H86), C26(H26), C25(H25), C27(H27), C25A(H25A), C26A(H26A),
 C27A(H27A), C82A(H82A), C86A(H86A), C84A(H84A)
5.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,
 H87C), C88(H88A,H88B,H88C), C87A(H87D,H87E,H87F), C88A(H88D,H88E,H88F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0160(3) 0.63373(7) 0.7848(2) 0.0309(6) Uani 1 1 d . U . . .
C2 C -0.1328(3) 0.62906(7) 0.7166(2) 0.0312(6) Uani 1 1 d . U . . .
C3 C -0.2293(3) 0.65219(8) 0.6898(2) 0.0346(7) Uani 1 1 d . U . . .
H3 H -0.3076 0.6478 0.6452 0.041 Uiso 1 1 calc R U . . .
C4 C -0.2096(3) 0.68164(8) 0.7289(2) 0.0376(7) Uani 1 1 d . U . . .
H4 H -0.2733 0.6977 0.7098 0.045 Uiso 1 1 calc R U . . .
C5 C -0.0982(3) 0.68758(8) 0.7954(2) 0.0343(7) Uani 1 1 d . U . . .
H5 H -0.0848 0.7077 0.8222 0.041 Uiso 1 1 calc R U . . .
C6 C -0.0039(3) 0.66386(7) 0.8238(2) 0.0303(6) Uani 1 1 d . U . . .
C7 C -0.1557(3) 0.59773(7) 0.6718(2) 0.0344(7) Uani 1 1 d . U . . .
C8 C -0.2756(3) 0.58212(8) 0.6538(2) 0.0413(8) Uani 1 1 d . U . . .
H8 H -0.3461 0.5918 0.6691 0.050 Uiso 1 1 calc R U . . .
C9 C -0.2940(4) 0.55283(9) 0.6141(3) 0.0492(9) Uani 1 1 d . U . . .
C10 C -0.1893(4) 0.53850(8) 0.5932(3) 0.0505(9) Uani 1 1 d . U . . .
H10 H -0.2008 0.5182 0.5668 0.061 Uiso 1 1 calc R U . . .
C11 C -0.0687(4) 0.55321(8) 0.6100(2) 0.0436(8) Uani 1 1 d . U . . .
C12 C -0.0535(3) 0.58270(8) 0.6486(2) 0.0361(7) Uani 1 1 d . U . . .
H12 H 0.0285 0.5930 0.6597 0.043 Uiso 1 1 calc R U . . .
C13 C -0.4253(4) 0.53668(10) 0.5931(3) 0.0652(12) Uani 1 1 d . U . . .
H13A H -0.4625 0.5393 0.6421 0.098 Uiso 1 1 calc R U . . .
H13B H -0.4145 0.5142 0.5831 0.098 Uiso 1 1 calc R U . . .
H13C H -0.4841 0.5461 0.5403 0.098 Uiso 1 1 calc R U . . .
C14 C 0.0436(4) 0.53840(9) 0.5840(3) 0.0583(11) Uani 1 1 d . U . . .
H14A H 0.0498 0.5479 0.5293 0.088 Uiso 1 1 calc R U . . .
H14B H 0.0284 0.5157 0.5756 0.088 Uiso 1 1 calc R U . . .
H14C H 0.1252 0.5420 0.6302 0.088 Uiso 1 1 calc R U . . .
C15 C 0.1123(3) 0.67039(7) 0.8990(2) 0.0316(6) Uani 1 1 d . U . . .
C16 C 0.1755(3) 0.69967(8) 0.9127(2) 0.0345(7) Uani 1 1 d . U . . .
H16 H 0.1438 0.7162 0.8720 0.041 Uiso 1 1 calc R U . . .
C17 C 0.2828(3) 0.70526(8) 0.9839(2) 0.0374(7) Uani 1 1 d . U . . .
C18 C 0.3332(3) 0.68062(8) 1.0420(2) 0.0394(7) Uani 1 1 d . U . . .
H18 H 0.4085 0.6841 1.0899 0.047 Uiso 1 1 calc R U . . .
C19 C 0.2741(3) 0.65122(8) 1.0303(2) 0.0357(7) Uani 1 1 d . U . . .
C20 C 0.1638(3) 0.64665(8) 0.9603(2) 0.0319(6) Uani 1 1 d . U . . .
H20 H 0.1216 0.6267 0.9537 0.038 Uiso 1 1 calc R U . . .
C21 C 0.3458(3) 0.73743(9) 0.9999(3) 0.0480(9) Uani 1 1 d . U . . .
H21A H 0.4287 0.7370 0.9851 0.072 Uiso 1 1 calc R U . . .
H21B H 0.3621 0.7431 1.0616 0.072 Uiso 1 1 calc R U . . .
H21C H 0.2875 0.7530 0.9633 0.072 Uiso 1 1 calc R U . . .
C22 C 0.3259(3) 0.62460(9) 1.0930(2) 0.0431(8) Uani 1 1 d . U . . .
H22A H 0.2556 0.6163 1.1148 0.065 Uiso 1 1 calc R U . . .
H22B H 0.3969 0.6323 1.1422 0.065 Uiso 1 1 calc R U . . .
H22C H 0.3590 0.6079 1.0627 0.065 Uiso 1 1 calc R U . . .
C28 C 0.2233(17) 0.5453(5) 0.8815(19) 0.032(4) Uani 0.54(5) 1 d D U P A 1
C29 C 0.3804(3) 0.60377(7) 0.7695(2) 0.0297(6) Uani 1 1 d D U . . .
C30 C 0.4191(3) 0.63164(7) 0.8162(2) 0.0323(6) Uani 1 1 d . U . . .
H30 H 0.4261 0.6322 0.8768 0.039 Uiso 1 1 calc R U . . .
C31 C 0.4478(3) 0.65862(8) 0.7755(2) 0.0392(7) Uani 1 1 d . U . . .
C32 C 0.4347(3) 0.65730(9) 0.6865(3) 0.0454(8) Uani 1 1 d . U . . .
H32 H 0.4552 0.6754 0.6582 0.054 Uiso 1 1 calc R U . . .
C33 C 0.3926(3) 0.63039(9) 0.6378(2) 0.0449(8) Uani 1 1 d . U . . .
C34 C 0.3672(3) 0.60354(8) 0.6800(2) 0.0383(7) Uani 1 1 d . U . . .
H34 H 0.3404 0.5848 0.6475 0.046 Uiso 1 1 calc R U . . .
C35 C 0.4992(4) 0.68758(9) 0.8283(3) 0.0551(10) Uani 1 1 d . U . . .
H35A H 0.4524 0.6907 0.8722 0.083 Uiso 1 1 calc R U . . .
H35B H 0.4860 0.7059 0.7895 0.083 Uiso 1 1 calc R U . . .
H35C H 0.5926 0.6850 0.8575 0.083 Uiso 1 1 calc R U . . .
C36 C 0.3751(5) 0.62986(13) 0.5406(3) 0.0730(14) Uani 1 1 d . U . . .
H36A H 0.4219 0.6118 0.5260 0.110 Uiso 1 1 calc R U . . .
H36B H 0.4099 0.6493 0.5232 0.110 Uiso 1 1 calc R U . . .
H36C H 0.2819 0.6281 0.5094 0.110 Uiso 1 1 calc R U . . .
C37 C 0.1073(3) 0.54155(7) 0.9170(2) 0.0313(6) Uani 1 1 d D U . . .
C38 C -0.0016(3) 0.52733(8) 0.8621(2) 0.0346(7) Uani 1 1 d . U . . .
H38 H 0.0012 0.5202 0.8063 0.041 Uiso 1 1 calc R U . . .
C39 C -0.1160(3) 0.52321(8) 0.8868(2) 0.0354(7) Uani 1 1 d . U . . .
C40 C -0.1178(3) 0.53427(7) 0.9680(2) 0.0354(7) Uani 1 1 d . U . . .
H40 H -0.1946 0.5315 0.9859 0.043 Uiso 1 1 calc R U . . .
C41 C -0.0119(3) 0.54915(8) 1.0237(2) 0.0390(7) Uani 1 1 d . U . . .
C42 C 0.1012(3) 0.55267(8) 0.9978(2) 0.0383(7) Uani 1 1 d . U . . .
H42 H 0.1752 0.5628 1.0358 0.046 Uiso 1 1 calc R U . . .
C43 C -0.2318(3) 0.50680(10) 0.8270(3) 0.0541(10) Uani 1 1 d . U . . .
H43A H -0.2881 0.5223 0.7885 0.081 Uiso 1 1 calc R U . . .
H43B H -0.2811 0.4961 0.8619 0.081 Uiso 1 1 calc R U . . .
H43C H -0.2019 0.4913 0.7916 0.081 Uiso 1 1 calc R U . . .
C44 C -0.0151(4) 0.56146(11) 1.1122(3) 0.0592(11) Uani 1 1 d . U . . .
H44A H -0.0447 0.5834 1.1065 0.089 Uiso 1 1 calc R U . . .
H44B H 0.0727 0.5603 1.1533 0.089 Uiso 1 1 calc R U . . .
H44C H -0.0752 0.5487 1.1342 0.089 Uiso 1 1 calc R U . . .
C45 C 0.8436(3) 0.67545(8) 0.2541(2) 0.0342(7) Uani 1 1 d . U . . .
C46 C 0.7512(3) 0.67630(8) 0.1707(2) 0.0381(7) Uani 1 1 d . U . . .
C47 C 0.6869(3) 0.70371(9) 0.1339(3) 0.0457(8) Uani 1 1 d . U . . .
H47 H 0.6258 0.7030 0.0774 0.055 Uiso 1 1 calc R U . . .
C48 C 0.7119(3) 0.73185(9) 0.1790(3) 0.0460(9) Uani 1 1 d . U . . .
H48 H 0.6653 0.7504 0.1551 0.055 Uiso 1 1 calc R U . . .
C49 C 0.8055(3) 0.73277(8) 0.2594(2) 0.0415(8) Uani 1 1 d . U . . .
H49 H 0.8259 0.7521 0.2901 0.050 Uiso 1 1 calc R U . . .
C50 C 0.8700(3) 0.70514(8) 0.2954(2) 0.0360(7) Uani 1 1 d . U . . .
C51 C 0.7226(3) 0.64678(8) 0.1180(2) 0.0388(7) Uani 1 1 d . U . . .
C52 C 0.6720(3) 0.62022(8) 0.1490(2) 0.0398(7) Uani 1 1 d . U . . .
H52 H 0.6592 0.6207 0.2055 0.048 Uiso 1 1 calc R U . . .
C53 C 0.6400(3) 0.59301(8) 0.0985(2) 0.0417(8) Uani 1 1 d . U . . .
C54 C 0.6642(3) 0.59229(9) 0.0173(3) 0.0434(8) Uani 1 1 d . U . . .
H54 H 0.6424 0.5739 -0.0178 0.052 Uiso 1 1 calc R U . . .
C55 C 0.7197(3) 0.61781(9) -0.0137(2) 0.0426(8) Uani 1 1 d . U . . .
C56 C 0.7466(3) 0.64479(9) 0.0364(2) 0.0411(8) Uani 1 1 d . U . . .
H56 H 0.7823 0.6625 0.0149 0.049 Uiso 1 1 calc R U . . .
C57 C 0.5807(4) 0.56477(9) 0.1301(3) 0.0527(10) Uani 1 1 d . U . . .
H57A H 0.6475 0.5485 0.1501 0.079 Uiso 1 1 calc R U . . .
H57B H 0.5092 0.5565 0.0821 0.079 Uiso 1 1 calc R U . . .
H57C H 0.5467 0.5710 0.1785 0.079 Uiso 1 1 calc R U . . .
C58 C 0.7516(4) 0.61552(10) -0.1001(3) 0.0515(9) Uani 1 1 d . U . . .
H58A H 0.7495 0.6366 -0.1255 0.077 Uiso 1 1 calc R U . . .
H58B H 0.6870 0.6021 -0.1402 0.077 Uiso 1 1 calc R U . . .
H58C H 0.8388 0.6064 -0.0904 0.077 Uiso 1 1 calc R U . . .
C59 C 0.9770(3) 0.70719(7) 0.3793(2) 0.0322(7) Uani 1 1 d . U . . .
C60 C 1.0862(3) 0.72645(7) 0.3862(2) 0.0339(7) Uani 1 1 d . U . . .
H60 H 1.0885 0.7396 0.3384 0.041 Uiso 1 1 calc R U . . .
C61 C 1.1903(3) 0.72671(8) 0.4610(2) 0.0361(7) Uani 1 1 d . U . . .
C62 C 1.1858(3) 0.70754(8) 0.5307(2) 0.0373(7) Uani 1 1 d . U . . .
H62 H 1.2575 0.7075 0.5822 0.045 Uiso 1 1 calc R U . . .
C63 C 1.0780(3) 0.68837(8) 0.5268(2) 0.0362(7) Uani 1 1 d . U . . .
C64 C 0.9759(3) 0.68824(8) 0.4506(2) 0.0352(7) Uani 1 1 d . U . . .
H64 H 0.9030 0.6749 0.4467 0.042 Uiso 1 1 calc R U . . .
C65 C 1.3074(4) 0.74749(9) 0.4671(3) 0.0501(9) Uani 1 1 d . U . . .
H65A H 1.3065 0.7545 0.4084 0.075 Uiso 1 1 calc R U . . .
H65B H 1.3876 0.7356 0.4933 0.075 Uiso 1 1 calc R U . . .
H65C H 1.3040 0.7659 0.5035 0.075 Uiso 1 1 calc R U . . .
C66 C 1.0727(4) 0.66871(10) 0.6046(2) 0.0497(9) Uani 1 1 d . U . . .
H66A H 1.0054 0.6771 0.6292 0.075 Uiso 1 1 calc R U . . .
H66B H 1.1577 0.6694 0.6490 0.075 Uiso 1 1 calc R U . . .
H66C H 1.0517 0.6469 0.5860 0.075 Uiso 1 1 calc R U . . .
C67 C 1.0892(3) 0.61275(7) 0.3159(2) 0.0319(6) Uani 1 1 d . U . . .
C68 C 1.2140(3) 0.61722(7) 0.30263(19) 0.0306(6) Uani 1 1 d . U . . .
C69 C 1.3060(3) 0.59309(8) 0.3155(2) 0.0351(7) Uani 1 1 d . U . . .
H69 H 1.3888 0.5971 0.3068 0.042 Uiso 1 1 calc R U . . .
C70 C 1.2780(3) 0.56350(8) 0.3409(2) 0.0391(7) Uani 1 1 d . U . . .
H70 H 1.3406 0.5471 0.3486 0.047 Uiso 1 1 calc R U . . .
C71 C 1.1575(3) 0.55788(8) 0.3549(2) 0.0399(8) Uani 1 1 d . U . . .
H71 H 1.1374 0.5376 0.3727 0.048 Uiso 1 1 calc R U . . .
C72 C 1.0659(3) 0.58225(8) 0.3428(2) 0.0348(7) Uani 1 1 d . U . . .
C73 C 1.2480(3) 0.64937(7) 0.2787(2) 0.0305(6) Uani 1 1 d . U . . .
C74 C 1.3691(3) 0.66301(8) 0.3189(2) 0.0334(7) Uani 1 1 d . U . . .
H74 H 1.4329 0.6510 0.3602 0.040 Uiso 1 1 calc R U . . .
C75 C 1.3991(3) 0.69350(8) 0.3003(2) 0.0364(7) Uani 1 1 d . U . . .
C76 C 1.3048(3) 0.71102(8) 0.2403(2) 0.0372(7) Uani 1 1 d . U . . .
H76 H 1.3237 0.7321 0.2279 0.045 Uiso 1 1 calc R U . . .
C77 C 1.1837(3) 0.69829(8) 0.1982(2) 0.0356(7) Uani 1 1 d . U . . .
C78 C 1.1572(3) 0.66747(8) 0.2162(2) 0.0334(7) Uani 1 1 d . U . . .
H78 H 1.0757 0.6584 0.1856 0.040 Uiso 1 1 calc R U . . .
C79 C 1.5315(3) 0.70735(9) 0.3442(3) 0.0487(9) Uani 1 1 d . U . . .
H79A H 1.5592 0.7010 0.4058 0.073 Uiso 1 1 calc R U . . .
H79B H 1.5266 0.7304 0.3402 0.073 Uiso 1 1 calc R U . . .
H79C H 1.5948 0.6997 0.3150 0.073 Uiso 1 1 calc R U . . .
C80 C 1.0823(3) 0.71702(9) 0.1316(2) 0.0471(9) Uani 1 1 d . U . . .
H80A H 1.0689 0.7076 0.0736 0.071 Uiso 1 1 calc R U . . .
H80B H 1.1123 0.7388 0.1309 0.071 Uiso 1 1 calc R U . . .
H80C H 0.9999 0.7168 0.1470 0.071 Uiso 1 1 calc R U . . .
C81 C 0.934(2) 0.5740(6) 0.3509(18) 0.036(3) Uani 0.49(5) 1 d . U P B 1
C82 C 0.8696(18) 0.5456(5) 0.3258(15) 0.034(3) Uani 0.49(5) 1 d . U P B 1
H82 H 0.9091 0.5297 0.3001 0.041 Uiso 0.49(5) 1 calc R U P B 1
C83 C 0.7498(14) 0.5403(5) 0.3379(13) 0.039(3) Uani 0.49(5) 1 d . U P B 1
C84 C 0.6905(15) 0.5636(6) 0.3735(13) 0.041(3) Uani 0.49(5) 1 d . U P B 1
H84 H 0.6055 0.5600 0.3790 0.049 Uiso 0.49(5) 1 calc R U P B 1
C85 C 0.7512(18) 0.5919(6) 0.4014(13) 0.039(3) Uani 0.49(5) 1 d . U P B 1
C86 C 0.877(2) 0.5964(6) 0.3900(16) 0.035(3) Uani 0.49(5) 1 d . U P B 1
H86 H 0.9228 0.6154 0.4100 0.043 Uiso 0.49(5) 1 calc R U P B 1
C87 C 0.6781(13) 0.5094(5) 0.3105(16) 0.051(4) Uani 0.49(5) 1 d . U P B 1
H87A H 0.7157 0.4984 0.2693 0.077 Uiso 0.49(5) 1 calc R U P B 1
H87B H 0.5855 0.5136 0.2824 0.077 Uiso 0.49(5) 1 calc R U P B 1
H87C H 0.6870 0.4962 0.3622 0.077 Uiso 0.49(5) 1 calc R U P B 1
C88 C 0.6910(17) 0.6177(6) 0.4401(12) 0.043(3) Uani 0.49(5) 1 d . U P B 1
H88A H 0.6734 0.6358 0.4003 0.065 Uiso 0.49(5) 1 calc R U P B 1
H88B H 0.7511 0.6240 0.4963 0.065 Uiso 0.49(5) 1 calc R U P B 1
H88C H 0.6090 0.6103 0.4490 0.065 Uiso 0.49(5) 1 calc R U P B 1
Li1 Li 0.1912(5) 0.62318(13) 0.8283(4) 0.0369(11) Uani 1 1 d . U . . .
Li2 Li 0.0332(5) 0.58413(13) 0.8074(4) 0.0381(12) Uani 1 1 d . U . . .
Li3 Li 1.0439(5) 0.66182(13) 0.3238(4) 0.0364(11) Uani 1 1 d . U . . .
Li4 Li 0.8833(5) 0.62537(14) 0.2610(4) 0.0414(13) Uani 1 1 d . U . . .
C26 C 0.420(2) 0.5234(3) 0.861(2) 0.058(5) Uani 0.54(5) 1 d D U P A 1
H26 H 0.4817 0.5067 0.8690 0.069 Uiso 0.54(5) 1 calc R U P A 1
C25 C 0.4388(16) 0.5506(3) 0.8193(16) 0.034(3) Uani 0.54(5) 1 d D U P A 1
H25 H 0.5102 0.5527 0.7954 0.041 Uiso 0.54(5) 1 calc R U P A 1
C23 C 0.238(2) 0.5745(5) 0.8442(19) 0.033(4) Uani 0.54(5) 1 d D U P A 1
C27 C 0.311(2) 0.5206(4) 0.891(2) 0.051(4) Uani 0.54(5) 1 d D U P A 1
H27 H 0.2958 0.5017 0.9187 0.061 Uiso 0.54(5) 1 calc R U P A 1
C24 C 0.3499(16) 0.5749(4) 0.8132(16) 0.027(2) Uani 0.54(5) 1 d D U P A 1
C23A C 0.246(2) 0.5726(5) 0.8437(18) 0.024(3) Uani 0.46(5) 1 d D U P A 2
C24A C 0.365(2) 0.5749(4) 0.8204(19) 0.030(3) Uani 0.46(5) 1 d D U P A 2
C25A C 0.4596(19) 0.5521(3) 0.8480(17) 0.033(3) Uani 0.46(5) 1 d D U P A 2
H25A H 0.5381 0.5539 0.8317 0.040 Uiso 0.46(5) 1 calc R U P A 2
C26A C 0.4449(13) 0.5268(4) 0.8981(18) 0.045(4) Uani 0.46(5) 1 d D U P A 2
H26A H 0.5117 0.5114 0.9151 0.054 Uiso 0.46(5) 1 calc R U P A 2
C27A C 0.3322(12) 0.5239(4) 0.9234(16) 0.037(3) Uani 0.46(5) 1 d D U P A 2
H27A H 0.3216 0.5069 0.9593 0.044 Uiso 0.46(5) 1 calc R U P A 2
C28A C 0.2346(18) 0.5464(6) 0.896(2) 0.025(3) Uani 0.46(5) 1 d D U P A 2
C81A C 0.939(2) 0.5779(5) 0.3673(17) 0.032(3) Uani 0.51(5) 1 d . U P B 2
C82A C 0.8670(19) 0.5505(5) 0.3470(17) 0.043(4) Uani 0.51(5) 1 d . U P B 2
H82A H 0.9009 0.5336 0.3211 0.051 Uiso 0.51(5) 1 calc R U P B 2
C86A C 0.8845(17) 0.6028(5) 0.4050(15) 0.030(3) Uani 0.51(5) 1 d . U P B 2
H86A H 0.9324 0.6218 0.4209 0.036 Uiso 0.51(5) 1 calc R U P B 2
C85A C 0.7626(14) 0.5999(5) 0.4189(13) 0.036(3) Uani 0.51(5) 1 d . U P B 2
C84A C 0.6940(13) 0.5722(5) 0.3976(15) 0.042(3) Uani 0.51(5) 1 d . U P B 2
H84A H 0.6102 0.5705 0.4068 0.050 Uiso 0.51(5) 1 calc R U P B 2
C83A C 0.7435(15) 0.5467(4) 0.3634(17) 0.046(3) Uani 0.51(5) 1 d . U P B 2
C87A C 0.6702(15) 0.5164(4) 0.344(2) 0.063(4) Uani 0.51(5) 1 d . U P B 2
H87D H 0.7099 0.5030 0.3084 0.095 Uiso 0.51(5) 1 calc R U P B 2
H87E H 0.5791 0.5206 0.3117 0.095 Uiso 0.51(5) 1 calc R U P B 2
H87F H 0.6737 0.5056 0.3988 0.095 Uiso 0.51(5) 1 calc R U P B 2
C88A C 0.7068(15) 0.6275(5) 0.4584(14) 0.041(3) Uani 0.51(5) 1 d . U P B 2
H88D H 0.7724 0.6350 0.5109 0.062 Uiso 0.51(5) 1 calc R U P B 2
H88E H 0.6289 0.6205 0.4740 0.062 Uiso 0.51(5) 1 calc R U P B 2
H88F H 0.6832 0.6446 0.4156 0.062 Uiso 0.51(5) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C2 1.416(4) . ?
C1 C6 1.413(4) . ?
C1 Li1 2.170(6) . ?
C1 Li2 2.177(6) . ?
C2 C3 1.400(4) . ?
C2 C7 1.497(4) . ?
C2 Li2 2.724(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.406(4) . ?
C6 C15 1.486(4) . ?
C6 Li1 2.693(6) . ?
C7 C8 1.398(4) . ?
C7 C12 1.404(4) . ?
C7 Li2 2.568(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.384(5) . ?
C9 C10 1.396(6) . ?
C9 C13 1.511(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.388(5) . ?
C11 C12 1.385(5) . ?
C11 C14 1.514(5) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.403(4) . ?
C15 C20 1.404(4) . ?
C15 Li1 2.559(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(5) . ?
C17 C18 1.400(5) . ?
C17 C21 1.513(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.388(5) . ?
C19 C20 1.386(4) . ?
C19 C22 1.506(5) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C28 C37 1.510(10) . ?
C28 Li2 2.623(17) . ?
C28 C23 1.407(11) . ?
C28 C27 1.382(11) . ?
C29 C30 1.397(4) . ?
C29 C34 1.393(4) . ?
C29 Li1 2.596(6) . ?
C29 C24 1.493(10) . ?
C29 C24A 1.506(11) . ?
C30 H30 0.9500 . ?
C30 C31 1.394(4) . ?
C31 C32 1.387(5) . ?
C31 C35 1.504(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.384(6) . ?
C33 C34 1.391(5) . ?
C33 C36 1.509(5) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.380(4) . ?
C37 C42 1.393(4) . ?
C37 Li2 2.483(6) . ?
C37 C28A 1.507(11) . ?
C38 H38 0.9500 . ?
C38 C39 1.398(4) . ?
C39 C40 1.385(5) . ?
C39 C43 1.501(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.377(5) . ?
C41 C42 1.392(4) . ?
C41 C44 1.516(5) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.413(5) . ?
C45 C50 1.414(5) . ?
C45 Li3 2.190(6) . ?
C45 Li4 2.166(7) . ?
C46 C47 1.394(5) . ?
C46 C51 1.492(5) . ?
C46 Li4 2.755(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.385(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.398(4) . ?
C50 C59 1.494(5) . ?
C50 Li3 2.563(6) . ?
C51 C52 1.401(5) . ?
C51 C56 1.401(5) . ?
C51 Li4 2.598(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.395(5) . ?
C53 C54 1.392(5) . ?
C53 C57 1.510(5) . ?
C54 H54 0.9500 . ?
C54 C55 1.392(5) . ?
C55 C56 1.380(5) . ?
C55 C58 1.515(5) . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.404(4) . ?
C59 C64 1.397(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.380(5) . ?
C61 C62 1.392(5) . ?
C61 C65 1.511(4) . ?
C62 H62 0.9500 . ?
C62 C63 1.397(5) . ?
C63 C64 1.382(5) . ?
C63 C66 1.512(5) . ?
C64 H64 0.9500 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C68 1.422(4) . ?
C67 C72 1.409(4) . ?
C67 Li3 2.152(6) . ?
C67 Li4 2.190(6) . ?
C68 C69 1.394(4) . ?
C68 C73 1.491(4) . ?
C68 Li3 2.713(6) . ?
C69 H69 0.9500 . ?
C69 C70 1.379(5) . ?
C70 H70 0.9500 . ?
C70 C71 1.390(5) . ?
C71 H71 0.9500 . ?
C71 C72 1.400(4) . ?
C72 C81 1.49(2) . ?
C72 Li4 2.722(6) . ?
C72 C81A 1.53(2) . ?
C73 C74 1.395(4) . ?
C73 C78 1.405(4) . ?
C73 Li3 2.539(6) . ?
C74 H74 0.9500 . ?
C74 C75 1.387(4) . ?
C75 C76 1.392(5) . ?
C75 C79 1.508(4) . ?
C76 H76 0.9500 . ?
C76 C77 1.386(5) . ?
C77 C78 1.387(5) . ?
C77 C80 1.510(4) . ?
C78 H78 0.9500 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 C82 1.39(2) . ?
C81 C86 1.38(2) . ?
C82 H82 0.9500 . ?
C82 C83 1.367(17) . ?
C83 C84 1.381(15) . ?
C83 C87 1.521(15) . ?
C84 H84 0.9500 . ?
C84 C85 1.380(15) . ?
C85 C86 1.42(2) . ?
C85 C88 1.491(16) . ?
C86 H86 0.9500 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
Li1 Li2 2.322(8) . ?
Li1 C23 2.12(2) . ?
Li1 C24 2.717(16) . ?
Li1 C23A 2.22(2) . ?
Li2 C23 2.14(2) . ?
Li2 C23A 2.24(2) . ?
Li2 C28A 2.731(17) . ?
Li3 Li4 2.316(8) . ?
C26 H26 0.9500 . ?
C26 C25 1.374(10) . ?
C26 C27 1.396(10) . ?
C25 H25 0.9500 . ?
C25 C24 1.387(11) . ?
C23 C24 1.421(11) . ?
C27 H27 0.9500 . ?
C23A C24A 1.424(12) . ?
C23A C28A 1.415(12) . ?
C24A C25A 1.382(12) . ?
C25A H25A 0.9500 . ?
C25A C26A 1.375(11) . ?
C26A H26A 0.9500 . ?
C26A C27A 1.381(10) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.389(11) . ?
C81A C82A 1.38(2) . ?
C81A C86A 1.421(18) . ?
C82A H82A 0.9500 . ?
C82A C83A 1.426(19) . ?
C86A H86A 0.9500 . ?
C86A C85A 1.388(18) . ?
C85A C84A 1.380(14) . ?
C85A C88A 1.529(14) . ?
C84A H84A 0.9500 . ?
C84A C83A 1.382(15) . ?
C83A C87A 1.494(15) . ?
C87A H87D 0.9800 . ?
C87A H87E 0.9800 . ?
C87A H87F 0.9800 . ?
C88A H88D 0.9800 . ?
C88A H88E 0.9800 . ?
C88A H88F 0.9800 . ?

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
C2 C1 Li1 144.3(3) . . ?
C2 C1 Li2 96.3(3) . . ?
C6 C1 C2 114.6(3) . . ?
C6 C1 Li1 95.1(2) . . ?
C6 C1 Li2 144.7(3) . . ?
Li1 C1 Li2 64.6(2) . . ?
C1 C2 C7 118.7(3) . . ?
C1 C2 Li2 52.6(2) . . ?
C3 C2 C1 123.1(3) . . ?
C3 C2 C7 118.2(3) . . ?
C3 C2 Li2 164.8(3) . . ?
C7 C2 Li2 67.9(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.1(3) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C15 118.4(3) . . ?
C1 C6 Li1 53.4(2) . . ?
C5 C6 C1 122.7(3) . . ?
C5 C6 C15 118.9(3) . . ?
C5 C6 Li1 161.3(3) . . ?
C15 C6 Li1 68.7(2) . . ?
C2 C7 Li2 79.4(2) . . ?
C8 C7 C2 122.4(3) . . ?
C8 C7 C12 117.8(3) . . ?
C8 C7 Li2 121.4(3) . . ?
C12 C7 C2 119.8(3) . . ?
C12 C7 Li2 68.6(2) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 C7 121.5(3) . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C10 118.9(3) . . ?
C8 C9 C13 120.8(4) . . ?
C10 C9 C13 120.4(4) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 C9 121.4(3) . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C14 121.6(3) . . ?
C12 C11 C10 118.5(3) . . ?
C12 C11 C14 119.8(3) . . ?
C7 C12 H12 119.1 . . ?
C11 C12 C7 121.8(3) . . ?
C11 C12 H12 119.1 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 Li1 78.6(2) . . ?
C16 C15 C6 123.1(3) . . ?
C16 C15 C20 116.9(3) . . ?
C16 C15 Li1 124.0(2) . . ?
C20 C15 C6 120.0(3) . . ?
C20 C15 Li1 68.4(2) . . ?
C15 C16 H16 119.0 . . ?
C17 C16 C15 122.0(3) . . ?
C17 C16 H16 119.0 . . ?
C16 C17 C18 119.1(3) . . ?
C16 C17 C21 121.2(3) . . ?
C18 C17 C21 119.7(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(3) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C22 121.3(3) . . ?
C20 C19 C18 118.9(3) . . ?
C20 C19 C22 119.8(3) . . ?
C15 C20 H20 118.8 . . ?
C19 C20 C15 122.3(3) . . ?
C19 C20 H20 118.8 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C37 C28 Li2 67.8(6) . . ?
C23 C28 C37 117.0(11) . . ?
C23 C28 Li2 54.4(9) . . ?
C27 C28 C37 118.6(11) . . ?
C27 C28 Li2 160(2) . . ?
C27 C28 C23 124.4(12) . . ?
C30 C29 Li1 71.4(2) . . ?
C30 C29 C24 121.2(11) . . ?
C30 C29 C24A 117.5(13) . . ?
C34 C29 C30 118.7(3) . . ?
C34 C29 Li1 120.8(2) . . ?
C34 C29 C24 120.1(11) . . ?
C34 C29 C24A 123.6(12) . . ?
C24 C29 Li1 78.2(6) . . ?
C24A C29 Li1 81.1(7) . . ?
C29 C30 H30 119.4 . . ?
C31 C30 C29 121.3(3) . . ?
C31 C30 H30 119.4 . . ?
C30 C31 C35 120.3(3) . . ?
C32 C31 C30 118.2(3) . . ?
C32 C31 C35 121.4(3) . . ?
C31 C32 H32 119.0 . . ?
C33 C32 C31 122.0(3) . . ?
C33 C32 H32 119.0 . . ?
C32 C33 C34 118.8(3) . . ?
C32 C33 C36 121.0(4) . . ?
C34 C33 C36 120.2(4) . . ?
C29 C34 H34 119.5 . . ?
C33 C34 C29 120.9(3) . . ?
C33 C34 H34 119.5 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C28 C37 Li2 77.9(7) . . ?
C38 C37 C28 116.3(13) . . ?
C38 C37 C42 118.8(3) . . ?
C38 C37 Li2 80.2(2) . . ?
C38 C37 C28A 124.7(14) . . ?
C42 C37 C28 124.9(13) . . ?
C42 C37 Li2 108.4(3) . . ?
C42 C37 C28A 116.5(14) . . ?
C28A C37 Li2 82.5(7) . . ?
C37 C38 H38 119.2 . . ?
C37 C38 C39 121.6(3) . . ?
C39 C38 H38 119.2 . . ?
C38 C39 C43 120.6(3) . . ?
C40 C39 C38 117.9(3) . . ?
C40 C39 C43 121.5(3) . . ?
C39 C40 H40 119.0 . . ?
C41 C40 C39 122.1(3) . . ?
C41 C40 H40 119.0 . . ?
C40 C41 C42 118.8(3) . . ?
C40 C41 C44 121.8(3) . . ?
C42 C41 C44 119.5(3) . . ?
C37 C42 H42 119.6 . . ?
C41 C42 C37 120.8(3) . . ?
C41 C42 H42 119.6 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C50 114.2(3) . . ?
C46 C45 Li3 143.5(3) . . ?
C46 C45 Li4 98.5(3) . . ?
C50 C45 Li3 87.9(2) . . ?
C50 C45 Li4 147.4(3) . . ?
Li4 C45 Li3 64.2(2) . . ?
C45 C46 C51 119.0(3) . . ?
C45 C46 Li4 51.1(2) . . ?
C47 C46 C45 123.1(4) . . ?
C47 C46 C51 117.9(3) . . ?
C47 C46 Li4 173.7(3) . . ?
C51 C46 Li4 68.1(2) . . ?
C46 C47 H47 119.9 . . ?
C48 C47 C46 120.3(4) . . ?
C48 C47 H47 119.9 . . ?
C47 C48 H48 120.4 . . ?
C47 C48 C49 119.2(3) . . ?
C49 C48 H48 120.4 . . ?
C48 C49 H49 120.1 . . ?
C48 C49 C50 119.9(4) . . ?
C50 C49 H49 120.1 . . ?
C45 C50 C59 118.0(3) . . ?
C45 C50 Li3 58.6(2) . . ?
C49 C50 C45 123.2(3) . . ?
C49 C50 C59 118.7(3) . . ?
C49 C50 Li3 157.3(3) . . ?
C59 C50 Li3 63.4(2) . . ?
C46 C51 Li4 79.7(2) . . ?
C52 C51 C46 121.0(3) . . ?
C52 C51 Li4 68.5(2) . . ?
C56 C51 C46 120.8(3) . . ?
C56 C51 C52 118.1(3) . . ?
C56 C51 Li4 123.0(3) . . ?
C51 C52 H52 119.4 . . ?
C53 C52 C51 121.2(3) . . ?
C53 C52 H52 119.4 . . ?
C52 C53 C57 121.5(3) . . ?
C54 C53 C52 118.5(3) . . ?
C54 C53 C57 120.1(4) . . ?
C53 C54 H54 119.2 . . ?
C53 C54 C55 121.7(4) . . ?
C55 C54 H54 119.2 . . ?
C54 C55 C58 120.2(4) . . ?
C56 C55 C54 118.7(3) . . ?
C56 C55 C58 121.1(3) . . ?
C51 C56 H56 119.1 . . ?
C55 C56 C51 121.7(3) . . ?
C55 C56 H56 119.1 . . ?
C53 C57 H57A 109.5 . . ?
C53 C57 H57B 109.5 . . ?
C53 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 C50 120.7(3) . . ?
C64 C59 C50 120.9(3) . . ?
C64 C59 C60 118.2(3) . . ?
C59 C60 H60 119.4 . . ?
C61 C60 C59 121.3(3) . . ?
C61 C60 H60 119.4 . . ?
C60 C61 C62 118.9(3) . . ?
C60 C61 C65 120.6(3) . . ?
C62 C61 C65 120.5(3) . . ?
C61 C62 H62 119.3 . . ?
C61 C62 C63 121.4(3) . . ?
C63 C62 H62 119.3 . . ?
C62 C63 C66 120.6(3) . . ?
C64 C63 C62 118.4(3) . . ?
C64 C63 C66 121.0(3) . . ?
C59 C64 H64 119.1 . . ?
C63 C64 C59 121.7(3) . . ?
C63 C64 H64 119.1 . . ?
C61 C65 H65A 109.5 . . ?
C61 C65 H65B 109.5 . . ?
C61 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C68 C67 Li3 96.6(2) . . ?
C68 C67 Li4 141.8(3) . . ?
C72 C67 C68 115.1(3) . . ?
C72 C67 Li3 144.1(3) . . ?
C72 C67 Li4 95.8(2) . . ?
Li3 C67 Li4 64.5(2) . . ?
C67 C68 C73 117.9(3) . . ?
C67 C68 Li3 52.0(2) . . ?
C69 C68 C67 122.1(3) . . ?
C69 C68 C73 119.9(3) . . ?
C69 C68 Li3 164.7(3) . . ?
C73 C68 Li3 67.22(19) . . ?
C68 C69 H69 119.6 . . ?
C70 C69 C68 120.7(3) . . ?
C70 C69 H69 119.6 . . ?
C69 C70 H70 120.3 . . ?
C69 C70 C71 119.5(3) . . ?
C71 C70 H70 120.3 . . ?
C70 C71 H71 120.2 . . ?
C70 C71 C72 119.6(3) . . ?
C72 C71 H71 120.2 . . ?
C67 C72 C81 119.7(11) . . ?
C67 C72 Li4 53.15(19) . . ?
C67 C72 C81A 115.9(9) . . ?
C71 C72 C67 123.0(3) . . ?
C71 C72 C81 117.0(11) . . ?
C71 C72 Li4 160.2(3) . . ?
C71 C72 C81A 120.9(9) . . ?
C81 C72 Li4 68.6(11) . . ?
C81A C72 Li4 68.7(9) . . ?
C68 C73 Li3 80.0(2) . . ?
C74 C73 C68 121.7(3) . . ?
C74 C73 C78 117.4(3) . . ?
C74 C73 Li3 122.8(3) . . ?
C78 C73 C68 120.9(3) . . ?
C78 C73 Li3 67.2(2) . . ?
C73 C74 H74 119.0 . . ?
C75 C74 C73 122.0(3) . . ?
C75 C74 H74 119.0 . . ?
C74 C75 C76 118.7(3) . . ?
C74 C75 C79 120.6(3) . . ?
C76 C75 C79 120.7(3) . . ?
C75 C76 H76 119.4 . . ?
C77 C76 C75 121.2(3) . . ?
C77 C76 H76 119.4 . . ?
C76 C77 C78 119.0(3) . . ?
C76 C77 C80 121.2(3) . . ?
C78 C77 C80 119.7(3) . . ?
C73 C78 H78 119.2 . . ?
C77 C78 C73 121.5(3) . . ?
C77 C78 H78 119.2 . . ?
C75 C79 H79A 109.5 . . ?
C75 C79 H79B 109.5 . . ?
C75 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C77 C80 H80A 109.5 . . ?
C77 C80 H80B 109.5 . . ?
C77 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C82 C81 C72 125.6(16) . . ?
C86 C81 C72 115.5(16) . . ?
C86 C81 C82 118.8(16) . . ?
C81 C82 H82 119.7 . . ?
C83 C82 C81 120.6(14) . . ?
C83 C82 H82 119.7 . . ?
C82 C83 C84 120.0(11) . . ?
C82 C83 C87 121.1(11) . . ?
C84 C83 C87 118.9(10) . . ?
C83 C84 H84 119.1 . . ?
C85 C84 C83 121.9(11) . . ?
C85 C84 H84 119.1 . . ?
C84 C85 C86 116.8(12) . . ?
C84 C85 C88 123.8(13) . . ?
C86 C85 C88 119.4(12) . . ?
C81 C86 C85 121.7(14) . . ?
C81 C86 H86 119.1 . . ?
C85 C86 H86 119.1 . . ?
C83 C87 H87A 109.5 . . ?
C83 C87 H87B 109.5 . . ?
C83 C87 H87C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C85 C88 H88A 109.5 . . ?
C85 C88 H88B 109.5 . . ?
C85 C88 H88C 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C1 Li1 C6 31.52(13) . . ?
C1 Li1 C15 62.93(17) . . ?
C1 Li1 C29 141.1(3) . . ?
C1 Li1 Li2 57.9(2) . . ?
C1 Li1 C24 137.2(6) . . ?
C1 Li1 C23A 116.6(7) . . ?
C6 Li1 C24 168.7(6) . . ?
C15 Li1 C6 32.75(12) . . ?
C15 Li1 C29 142.9(2) . . ?
C15 Li1 C24 157.5(6) . . ?
C29 Li1 C6 150.6(2) . . ?
C29 Li1 C24 32.5(2) . . ?
Li2 Li1 C6 86.0(2) . . ?
Li2 Li1 C15 107.8(2) . . ?
Li2 Li1 C29 109.3(3) . . ?
Li2 Li1 C24 83.9(4) . . ?
C23 Li1 C1 115.0(7) . . ?
C23 Li1 C6 141.4(5) . . ?
C23 Li1 C15 143.7(7) . . ?
C23 Li1 C29 63.5(4) . . ?
C23 Li1 Li2 57.2(6) . . ?
C23 Li1 C24 31.2(3) . . ?
C23A Li1 C6 143.3(6) . . ?
C23A Li1 C15 145.0(6) . . ?
C23A Li1 C29 61.6(5) . . ?
C23A Li1 Li2 58.9(7) . . ?
C1 Li2 C2 31.11(13) . . ?
C1 Li2 C7 63.12(18) . . ?
C1 Li2 C28 143.5(6) . . ?
C1 Li2 C37 146.6(3) . . ?
C1 Li2 Li1 57.6(2) . . ?
C1 Li2 C23A 115.8(6) . . ?
C1 Li2 C28A 140.5(7) . . ?
C2 Li2 C28A 169.6(5) . . ?
C7 Li2 C2 32.69(12) . . ?
C7 Li2 C28 147.5(7) . . ?
C7 Li2 C28A 151.8(8) . . ?
C28 Li2 C2 169.7(3) . . ?
C37 Li2 C2 156.0(2) . . ?
C37 Li2 C7 140.6(3) . . ?
C37 Li2 C28 34.3(3) . . ?
C37 Li2 C28A 33.2(3) . . ?
Li1 Li2 C2 85.0(2) . . ?
Li1 Li2 C7 109.0(3) . . ?
Li1 Li2 C28 87.0(5) . . ?
Li1 Li2 C37 110.3(3) . . ?
Li1 Li2 C28A 84.9(6) . . ?
C23 Li2 C1 114.2(6) . . ?
C23 Li2 C2 137.7(5) . . ?
C23 Li2 C7 140.5(7) . . ?
C23 Li2 C28 32.4(4) . . ?
C23 Li2 C37 64.7(5) . . ?
C23 Li2 Li1 56.7(6) . . ?
C23A Li2 C2 138.7(5) . . ?
C23A Li2 C7 139.9(7) . . ?
C23A Li2 C37 64.0(5) . . ?
C23A Li2 Li1 58.3(6) . . ?
C23A Li2 C28A 31.1(3) . . ?
C45 Li3 C50 33.47(14) . . ?
C45 Li3 C68 135.6(3) . . ?
C45 Li3 C73 134.9(3) . . ?
C45 Li3 Li4 57.4(2) . . ?
C50 Li3 C68 163.3(3) . . ?
C67 Li3 C45 115.5(3) . . ?
C67 Li3 C50 148.2(3) . . ?
C67 Li3 C68 31.37(12) . . ?
C67 Li3 C73 63.65(17) . . ?
C67 Li3 Li4 58.6(2) . . ?
C73 Li3 C50 137.6(2) . . ?
C73 Li3 C68 32.77(11) . . ?
Li4 Li3 C50 89.6(2) . . ?
Li4 Li3 C68 85.4(2) . . ?
Li4 Li3 C73 109.2(3) . . ?
C45 Li4 C46 30.48(14) . . ?
C45 Li4 C51 62.63(18) . . ?
C45 Li4 C67 114.9(3) . . ?
C45 Li4 C72 142.0(3) . . ?
C45 Li4 Li3 58.4(2) . . ?
C51 Li4 C46 32.20(13) . . ?
C51 Li4 C72 149.4(3) . . ?
C67 Li4 C46 135.1(3) . . ?
C67 Li4 C51 140.7(3) . . ?
C67 Li4 C72 31.00(13) . . ?
C67 Li4 Li3 57.0(2) . . ?
C72 Li4 C46 165.8(2) . . ?
Li3 Li4 C46 84.7(2) . . ?
Li3 Li4 C51 111.6(3) . . ?
Li3 Li4 C72 84.3(2) . . ?
C25 C26 H26 120.4 . . ?
C25 C26 C27 119.3(11) . . ?
C27 C26 H26 120.4 . . ?
C26 C25 H25 121.0 . . ?
C26 C25 C24 118.0(11) . . ?
C24 C25 H25 121.0 . . ?
C28 C23 Li1 149.3(14) . . ?
C28 C23 Li2 93.3(11) . . ?
C28 C23 C24 111.3(13) . . ?
Li1 C23 Li2 66.1(6) . . ?
C24 C23 Li1 98.1(10) . . ?
C24 C23 Li2 143.3(18) . . ?
C28 C27 C26 120.3(11) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C29 C24 Li1 69.3(5) . . ?
C25 C24 C29 114.1(10) . . ?
C25 C24 Li1 171.1(18) . . ?
C25 C24 C23 126.6(12) . . ?
C23 C24 C29 119.3(11) . . ?
C23 C24 Li1 50.7(9) . . ?
Li1 C23A Li2 62.8(6) . . ?
C24A C23A Li1 97.5(11) . . ?
C24A C23A Li2 146.5(16) . . ?
C28A C23A Li1 139.6(17) . . ?
C28A C23A Li2 94.2(11) . . ?
C28A C23A C24A 116.1(14) . . ?
C23A C24A C29 116.3(12) . . ?
C25A C24A C29 124.0(14) . . ?
C25A C24A C23A 119.7(14) . . ?
C24A C25A H25A 118.7 . . ?
C26A C25A C24A 122.6(13) . . ?
C26A C25A H25A 118.7 . . ?
C25A C26A H26A 120.2 . . ?
C25A C26A C27A 119.6(13) . . ?
C27A C26A H26A 120.2 . . ?
C26A C27A H27A 120.5 . . ?
C26A C27A C28A 119.0(12) . . ?
C28A C27A H27A 120.5 . . ?
C37 C28A Li2 64.3(6) . . ?
C23A C28A C37 118.3(12) . . ?
C23A C28A Li2 54.7(10) . . ?
C27A C28A C37 118.6(12) . . ?
C27A C28A Li2 168(2) . . ?
C27A C28A C23A 123.0(13) . . ?
C82A C81A C72 121.2(14) . . ?
C82A C81A C86A 117.2(15) . . ?
C86A C81A C72 121.4(14) . . ?
C81A C82A H82A 118.8 . . ?
C81A C82A C83A 122.3(13) . . ?
C83A C82A H82A 118.8 . . ?
C81A C86A H86A 119.3 . . ?
C85A C86A C81A 121.3(13) . . ?
C85A C86A H86A 119.3 . . ?
C86A C85A C88A 119.6(10) . . ?
C84A C85A C86A 119.5(12) . . ?
C84A C85A C88A 120.9(10) . . ?
C85A C84A H84A 119.0 . . ?
C85A C84A C83A 122.0(11) . . ?
C83A C84A H84A 119.0 . . ?
C82A C83A C87A 121.1(12) . . ?
C84A C83A C82A 117.6(11) . . ?
C84A C83A C87A 121.3(12) . . ?
C83A C87A H87D 109.5 . . ?
C83A C87A H87E 109.5 . . ?
C83A C87A H87F 109.5 . . ?
H87D C87A H87E 109.5 . . ?
H87D C87A H87F 109.5 . . ?
H87E C87A H87F 109.5 . . ?
C85A C88A H88D 109.5 . . ?
C85A C88A H88E 109.5 . . ?
C85A C88A H88F 109.5 . . ?
H88D C88A H88E 109.5 . . ?
H88D C88A H88F 109.5 . . ?
H88E C88A H88F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 2.4(5) . . . . ?
C1 C2 C7 C8 134.9(3) . . . . ?
C1 C2 C7 C12 -43.5(4) . . . . ?
C1 C2 C7 Li2 14.3(3) . . . . ?
C1 C6 C15 C16 143.5(3) . . . . ?
C1 C6 C15 C20 -36.4(4) . . . . ?
C1 C6 C15 Li1 20.1(3) . . . . ?
C2 C1 C6 C5 -1.8(4) . . . . ?
C2 C1 C6 C15 176.9(3) . . . . ?
C2 C1 C6 Li1 -159.6(3) . . . . ?
C2 C3 C4 C5 -2.2(5) . . . . ?
C2 C7 C8 C9 -178.5(3) . . . . ?
C2 C7 C12 C11 177.7(3) . . . . ?
C3 C2 C7 C8 -44.0(4) . . . . ?
C3 C2 C7 C12 137.7(3) . . . . ?
C3 C2 C7 Li2 -164.6(3) . . . . ?
C3 C4 C5 C6 0.1(5) . . . . ?
C4 C5 C6 C1 2.1(5) . . . . ?
C4 C5 C6 C15 -176.7(3) . . . . ?
C4 C5 C6 Li1 73.7(9) . . . . ?
C5 C6 C15 C16 -37.7(4) . . . . ?
C5 C6 C15 C20 142.4(3) . . . . ?
C5 C6 C15 Li1 -161.1(3) . . . . ?
C6 C1 C2 C3 -0.4(4) . . . . ?
C6 C1 C2 C7 -179.2(3) . . . . ?
C6 C1 C2 Li2 -162.5(3) . . . . ?
C6 C15 C16 C17 179.3(3) . . . . ?
C6 C15 C20 C19 178.2(3) . . . . ?
C7 C2 C3 C4 -178.8(3) . . . . ?
C7 C8 C9 C10 1.0(6) . . . . ?
C7 C8 C9 C13 -178.5(4) . . . . ?
C8 C7 C12 C11 -0.7(5) . . . . ?
C8 C9 C10 C11 -1.0(6) . . . . ?
C9 C10 C11 C12 0.2(6) . . . . ?
C9 C10 C11 C14 -177.4(4) . . . . ?
C10 C11 C12 C7 0.7(5) . . . . ?
C12 C7 C8 C9 -0.2(5) . . . . ?
C13 C9 C10 C11 178.4(4) . . . . ?
C14 C11 C12 C7 178.3(3) . . . . ?
C15 C16 C17 C18 2.6(5) . . . . ?
C15 C16 C17 C21 -177.1(3) . . . . ?
C16 C15 C20 C19 -1.7(4) . . . . ?
C16 C17 C18 C19 -2.0(5) . . . . ?
C17 C18 C19 C20 -0.4(5) . . . . ?
C17 C18 C19 C22 -179.2(3) . . . . ?
C18 C19 C20 C15 2.3(5) . . . . ?
C20 C15 C16 C17 -0.8(4) . . . . ?
C21 C17 C18 C19 177.7(3) . . . . ?
C22 C19 C20 C15 -178.9(3) . . . . ?
C28 C37 C38 C39 -178.5(7) . . . . ?
C28 C37 C42 C41 177.6(8) . . . . ?
C28 C37 C28A Li2 58(9) . . . . ?
C28 C37 C28A C23A 67(8) . . . . ?
C28 C37 C28A C27A -109(11) . . . . ?
C28 C23 C24 C29 179(2) . . . . ?
C28 C23 C24 Li1 -171(3) . . . . ?
C28 C23 C24 C25 -2(4) . . . . ?
C29 C30 C31 C32 1.1(4) . . . . ?
C29 C30 C31 C35 -175.3(3) . . . . ?
C29 C24A C25A C26A 176.8(18) . . . . ?
C30 C29 C34 C33 0.4(4) . . . . ?
C30 C29 C24 Li1 59.4(5) . . . . ?
C30 C29 C24 C25 -111.7(19) . . . . ?
C30 C29 C24 C23 68(2) . . . . ?
C30 C29 C24A C23A 80(3) . . . . ?
C30 C29 C24A C25A -97(2) . . . . ?
C30 C31 C32 C33 0.9(5) . . . . ?
C31 C32 C33 C34 -2.3(5) . . . . ?
C31 C32 C33 C36 178.1(3) . . . . ?
C32 C33 C34 C29 1.6(5) . . . . ?
C34 C29 C30 C31 -1.8(4) . . . . ?
C34 C29 C24 Li1 -118.9(4) . . . . ?
C34 C29 C24 C25 70(2) . . . . ?
C34 C29 C24 C23 -110(2) . . . . ?
C34 C29 C24A C23A -104(2) . . . . ?
C34 C29 C24A C25A 78(3) . . . . ?
C35 C31 C32 C33 177.3(3) . . . . ?
C36 C33 C34 C29 -178.8(3) . . . . ?
C37 C28 C23 Li1 18(6) . . . . ?
C37 C28 C23 Li2 -28(3) . . . . ?
C37 C28 C23 C24 -180(2) . . . . ?
C37 C28 C27 C26 -178.7(16) . . . . ?
C37 C38 C39 C40 0.9(5) . . . . ?
C37 C38 C39 C43 -178.1(3) . . . . ?
C38 C37 C42 C41 0.9(5) . . . . ?
C38 C37 C28A Li2 72.6(6) . . . . ?
C38 C37 C28A C23A 82(3) . . . . ?
C38 C37 C28A C27A -94(2) . . . . ?
C38 C39 C40 C41 0.5(5) . . . . ?
C39 C40 C41 C42 -1.1(5) . . . . ?
C39 C40 C41 C44 179.4(3) . . . . ?
C40 C41 C42 C37 0.4(5) . . . . ?
C42 C37 C38 C39 -1.6(5) . . . . ?
C42 C37 C28A Li2 -106.9(4) . . . . ?
C42 C37 C28A C23A -97(3) . . . . ?
C42 C37 C28A C27A 87(3) . . . . ?
C43 C39 C40 C41 179.5(3) . . . . ?
C44 C41 C42 C37 179.9(3) . . . . ?
C45 C46 C47 C48 -0.2(5) . . . . ?
C45 C46 C51 C52 60.8(4) . . . . ?
C45 C46 C51 C56 -118.7(3) . . . . ?
C45 C46 C51 Li4 3.7(3) . . . . ?
C45 C50 C59 C60 118.9(3) . . . . ?
C45 C50 C59 C64 -56.2(4) . . . . ?
C46 C45 C50 C49 3.2(4) . . . . ?
C46 C45 C50 C59 -173.4(3) . . . . ?
C46 C45 C50 Li3 -150.0(3) . . . . ?
C46 C47 C48 C49 2.9(5) . . . . ?
C46 C51 C52 C53 177.3(3) . . . . ?
C46 C51 C56 C55 -179.4(3) . . . . ?
C47 C46 C51 C52 -120.8(3) . . . . ?
C47 C46 C51 C56 59.7(4) . . . . ?
C47 C46 C51 Li4 -177.8(3) . . . . ?
C47 C48 C49 C50 -2.4(5) . . . . ?
C48 C49 C50 C45 -0.8(5) . . . . ?
C48 C49 C50 C59 175.8(3) . . . . ?
C48 C49 C50 Li3 86.5(8) . . . . ?
C49 C50 C59 C60 -57.9(4) . . . . ?
C49 C50 C59 C64 127.1(3) . . . . ?
C50 C45 C46 C47 -2.7(4) . . . . ?
C50 C45 C46 C51 175.6(3) . . . . ?
C50 C45 C46 Li4 -179.9(3) . . . . ?
C50 C59 C60 C61 -174.9(3) . . . . ?
C50 C59 C64 C63 175.8(3) . . . . ?
C51 C46 C47 C48 -178.6(3) . . . . ?
C51 C52 C53 C54 2.4(5) . . . . ?
C51 C52 C53 C57 -177.6(3) . . . . ?
C52 C51 C56 C55 1.1(5) . . . . ?
C52 C53 C54 C55 0.4(5) . . . . ?
C53 C54 C55 C56 -2.4(5) . . . . ?
C53 C54 C55 C58 176.6(3) . . . . ?
C54 C55 C56 C51 1.6(5) . . . . ?
C56 C51 C52 C53 -3.2(5) . . . . ?
C57 C53 C54 C55 -179.6(3) . . . . ?
C58 C55 C56 C51 -177.3(3) . . . . ?
C59 C60 C61 C62 -0.3(5) . . . . ?
C59 C60 C61 C65 179.7(3) . . . . ?
C60 C59 C64 C63 0.6(5) . . . . ?
C60 C61 C62 C63 -0.6(5) . . . . ?
C61 C62 C63 C64 1.4(5) . . . . ?
C61 C62 C63 C66 -177.5(3) . . . . ?
C62 C63 C64 C59 -1.5(5) . . . . ?
C64 C59 C60 C61 0.3(5) . . . . ?
C65 C61 C62 C63 179.4(3) . . . . ?
C66 C63 C64 C59 177.5(3) . . . . ?
C67 C68 C69 C70 0.9(5) . . . . ?
C67 C68 C73 C74 134.5(3) . . . . ?
C67 C68 C73 C78 -43.7(4) . . . . ?
C67 C68 C73 Li3 12.0(3) . . . . ?
C67 C72 C81 C82 139.6(19) . . . . ?
C67 C72 C81 C86 -43(2) . . . . ?
C67 C72 C81A C82A 142.6(16) . . . . ?
C67 C72 C81A C86A -32(2) . . . . ?
C68 C67 C72 C71 -0.6(5) . . . . ?
C68 C67 C72 C81 -174.4(12) . . . . ?
C68 C67 C72 Li4 -156.9(4) . . . . ?
C68 C67 C72 C81A 173.4(11) . . . . ?
C68 C69 C70 C71 -1.0(5) . . . . ?
C68 C73 C74 C75 -176.6(3) . . . . ?
C68 C73 C78 C77 175.0(3) . . . . ?
C69 C68 C73 C74 -42.2(4) . . . . ?
C69 C68 C73 C78 139.5(3) . . . . ?
C69 C68 C73 Li3 -164.8(3) . . . . ?
C69 C70 C71 C72 0.3(5) . . . . ?
C70 C71 C72 C67 0.5(5) . . . . ?
C70 C71 C72 C81 174.5(12) . . . . ?
C70 C71 C72 Li4 72.6(9) . . . . ?
C70 C71 C72 C81A -173.2(11) . . . . ?
C71 C72 C81 C82 -35(3) . . . . ?
C71 C72 C81 C86 142.6(16) . . . . ?
C71 C72 C81A C82A -43(2) . . . . ?
C71 C72 C81A C86A 142.4(14) . . . . ?
C72 C67 C68 C69 -0.1(5) . . . . ?
C72 C67 C68 C73 -176.8(3) . . . . ?
C72 C67 C68 Li3 -162.7(4) . . . . ?
C72 C81 C82 C83 179(2) . . . . ?
C72 C81 C86 C85 179(2) . . . . ?
C72 C81A C82A C83A -175.4(18) . . . . ?
C72 C81A C86A C85A 173.3(19) . . . . ?
C73 C68 C69 C70 177.5(3) . . . . ?
C73 C74 C75 C76 0.5(5) . . . . ?
C73 C74 C75 C79 -179.3(3) . . . . ?
C74 C73 C78 C77 -3.3(5) . . . . ?
C74 C75 C76 C77 -1.2(5) . . . . ?
C75 C76 C77 C78 -0.4(5) . . . . ?
C75 C76 C77 C80 -178.7(3) . . . . ?
C76 C77 C78 C73 2.8(5) . . . . ?
C78 C73 C74 C75 1.7(5) . . . . ?
C79 C75 C76 C77 178.6(3) . . . . ?
C80 C77 C78 C73 -179.0(3) . . . . ?
C81 C72 C81A C82A 30(9) . . . . ?
C81 C72 C81A C86A -144(11) . . . . ?
C81 C82 C83 C84 1(3) . . . . ?
C81 C82 C83 C87 179.9(18) . . . . ?
C82 C81 C86 C85 -3(3) . . . . ?
C82 C83 C84 C85 -3(2) . . . . ?
C83 C84 C85 C86 1(2) . . . . ?
C83 C84 C85 C88 179.9(13) . . . . ?
C84 C85 C86 C81 2(3) . . . . ?
C86 C81 C82 C83 2(3) . . . . ?
C87 C83 C84 C85 178.6(13) . . . . ?
C88 C85 C86 C81 -176.9(18) . . . . ?
Li1 C1 C2 C3 -143.8(4) . . . . ?
Li1 C1 C2 C7 37.4(6) . . . . ?
Li1 C1 C2 Li2 54.1(4) . . . . ?
Li1 C1 C6 C5 157.7(3) . . . . ?
Li1 C1 C6 C15 -23.5(3) . . . . ?
Li1 C6 C15 C16 123.4(3) . . . . ?
Li1 C6 C15 C20 -56.6(3) . . . . ?
Li1 C15 C16 C17 -81.8(4) . . . . ?
Li1 C15 C20 C19 116.5(3) . . . . ?
Li1 C29 C30 C31 -117.3(3) . . . . ?
Li1 C29 C34 C33 84.7(4) . . . . ?
Li1 C29 C24 C25 -171(2) . . . . ?
Li1 C29 C24 C23 9(2) . . . . ?
Li1 C29 C24A C23A 17(2) . . . . ?
Li1 C29 C24A C25A -160(3) . . . . ?
Li1 C23 C24 C29 -10(3) . . . . ?
Li1 C23 C24 C25 169(2) . . . . ?
Li1 C23A C24A C29 -20(3) . . . . ?
Li1 C23A C24A C25A 158(2) . . . . ?
Li1 C23A C28A C37 41(5) . . . . ?
Li1 C23A C28A Li2 52(2) . . . . ?
Li1 C23A C28A C27A -143(2) . . . . ?
Li2 C1 C2 C3 162.1(3) . . . . ?
Li2 C1 C2 C7 -16.7(3) . . . . ?
Li2 C1 C6 C5 -150.6(4) . . . . ?
Li2 C1 C6 C15 28.1(6) . . . . ?
Li2 C1 C6 Li1 51.7(4) . . . . ?
Li2 C2 C3 C4 71.0(11) . . . . ?
Li2 C2 C7 C8 120.6(3) . . . . ?
Li2 C2 C7 C12 -57.7(3) . . . . ?
Li2 C7 C8 C9 -80.9(4) . . . . ?
Li2 C7 C12 C11 114.5(4) . . . . ?
Li2 C28 C37 C38 72.6(5) . . . . ?
Li2 C28 C37 C42 -104.2(6) . . . . ?
Li2 C28 C37 C28A -121(9) . . . . ?
Li2 C28 C23 Li1 46(4) . . . . ?
Li2 C28 C23 C24 -152(3) . . . . ?
Li2 C28 C27 C26 78(4) . . . . ?
Li2 C37 C38 C39 -107.3(3) . . . . ?
Li2 C37 C42 C41 89.7(4) . . . . ?
Li2 C37 C28A C23A 10(3) . . . . ?
Li2 C37 C28A C27A -166(3) . . . . ?
Li2 C23 C24 C29 50(4) . . . . ?
Li2 C23 C24 Li1 60(2) . . . . ?
Li2 C23 C24 C25 -130(3) . . . . ?
Li2 C23A C24A C29 31(5) . . . . ?
Li2 C23A C24A C25A -152(3) . . . . ?
Li2 C23A C28A C37 -11(3) . . . . ?
Li2 C23A C28A C27A 165(3) . . . . ?
Li3 C45 C46 C47 -125.4(5) . . . . ?
Li3 C45 C46 C51 53.0(6) . . . . ?
Li3 C45 C46 Li4 57.5(4) . . . . ?
Li3 C45 C50 C49 153.2(3) . . . . ?
Li3 C45 C50 C59 -23.4(3) . . . . ?
Li3 C50 C59 C60 96.6(3) . . . . ?
Li3 C50 C59 C64 -78.5(3) . . . . ?
Li3 C67 C68 C69 162.7(3) . . . . ?
Li3 C67 C68 C73 -14.0(3) . . . . ?
Li3 C67 C72 C71 -150.4(4) . . . . ?
Li3 C67 C72 C81 35.8(13) . . . . ?
Li3 C67 C72 Li4 53.3(4) . . . . ?
Li3 C67 C72 C81A 23.6(12) . . . . ?
Li3 C68 C69 C70 63.4(11) . . . . ?
Li3 C68 C73 C74 122.6(3) . . . . ?
Li3 C68 C73 C78 -55.6(3) . . . . ?
Li3 C73 C74 C75 -77.7(4) . . . . ?
Li3 C73 C78 C77 113.1(3) . . . . ?
Li4 C45 C46 C47 177.2(3) . . . . ?
Li4 C45 C46 C51 -4.5(3) . . . . ?
Li4 C45 C50 C49 -176.6(4) . . . . ?
Li4 C45 C50 C59 6.8(6) . . . . ?
Li4 C45 C50 Li3 30.2(4) . . . . ?
Li4 C46 C51 C52 57.0(3) . . . . ?
Li4 C46 C51 C56 -122.5(3) . . . . ?
Li4 C51 C52 C53 -120.1(3) . . . . ?
Li4 C51 C56 C55 82.5(4) . . . . ?
Li4 C67 C68 C69 -140.9(4) . . . . ?
Li4 C67 C68 C73 42.3(6) . . . . ?
Li4 C67 C68 Li3 56.4(4) . . . . ?
Li4 C67 C72 C71 156.3(3) . . . . ?
Li4 C67 C72 C81 -17.5(12) . . . . ?
Li4 C67 C72 C81A -29.7(11) . . . . ?
Li4 C72 C81 C82 125(2) . . . . ?
Li4 C72 C81 C86 -58.3(17) . . . . ?
Li4 C72 C81A C82A 117(2) . . . . ?
Li4 C72 C81A C86A -57.0(16) . . . . ?
C26 C25 C24 C29 178.1(14) . . . . ?
C26 C25 C24 C23 -1(3) . . . . ?
C25 C26 C27 C28 -2(2) . . . . ?
C23 C28 C37 C38 97(3) . . . . ?
C23 C28 C37 C42 -80(3) . . . . ?
C23 C28 C37 Li2 24(2) . . . . ?
C23 C28 C37 C28A -97(10) . . . . ?
C23 C28 C27 C26 -2(4) . . . . ?
C27 C28 C37 C38 -86(2) . . . . ?
C27 C28 C37 C42 97(2) . . . . ?
C27 C28 C37 Li2 -159(2) . . . . ?
C27 C28 C37 C28A 80(8) . . . . ?
C27 C28 C23 Li1 -159(3) . . . . ?
C27 C28 C23 Li2 155(2) . . . . ?
C27 C28 C23 C24 3(4) . . . . ?
C27 C26 C25 C24 3(2) . . . . ?
C24 C29 C30 C31 179.9(7) . . . . ?
C24 C29 C34 C33 178.7(7) . . . . ?
C24 C29 C24A C23A -46(14) . . . . ?
C24 C29 C24A C25A 137(18) . . . . ?
C23A C24A C25A C26A 0(4) . . . . ?
C24A C29 C30 C31 173.9(9) . . . . ?
C24A C29 C34 C33 -175.0(10) . . . . ?
C24A C29 C24 Li1 116(16) . . . . ?
C24A C29 C24 C25 -55(14) . . . . ?
C24A C29 C24 C23 124(17) . . . . ?
C24A C23A C28A C37 -176(2) . . . . ?
C24A C23A C28A Li2 -165(3) . . . . ?
C24A C23A C28A C27A 0(5) . . . . ?
C24A C25A C26A C27A -1(2) . . . . ?
C25A C26A C27A C28A 2(2) . . . . ?
C26A C27A C28A C37 174.6(18) . . . . ?
C26A C27A C28A Li2 74(6) . . . . ?
C26A C27A C28A C23A -1(4) . . . . ?
C28A C37 C38 C39 179.0(8) . . . . ?
C28A C37 C42 C41 -179.6(7) . . . . ?
C28A C23A C24A C29 -177(2) . . . . ?
C28A C23A C24A C25A 1(4) . . . . ?
C81A C72 C81 C82 -147(12) . . . . ?
C81A C72 C81 C86 30(9) . . . . ?
C81A C82A C83A C84A 3(3) . . . . ?
C81A C82A C83A C87A -177.6(18) . . . . ?
C81A C86A C85A C84A 1(3) . . . . ?
C81A C86A C85A C88A -179.1(15) . . . . ?
C82A C81A C86A C85A -1(3) . . . . ?
C86A C81A C82A C83A -1(3) . . . . ?
C86A C85A C84A C83A 1(2) . . . . ?
C85A C84A C83A C82A -3(2) . . . . ?
C85A C84A C83A C87A 177.6(13) . . . . ?
C88A C85A C84A C83A -178.7(12) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6 9 0 0.0928 -6.0052 9.0052 0.0034 0.1992 0.8741 -0.3439
7 -7 -3 0.1051 7.0060 -6.9906 -2.9984 -0.1929 -0.7985 0.6394
6 0 -8 0.1060 6.0049 0.0361 -7.9885 -0.0842 -0.2913 0.9777
4 5 -10 0.1342 4.0031 5.0482 -9.9837 0.0182 0.1403 1.0205
1 27 2 0.0596 0.9984 26.9794 2.0023 -0.9468 0.3758 0.0227
-2 -27 1 0.0426 -1.9993 -26.9946 0.9931 0.8829 -0.4080 -0.3101
1 -23 -6 0.0777 1.0029 -22.9613 -5.9955 0.8660 -0.3216 0.4189
-5 -3 9 0.1967 -5.0040 -3.0420 8.9860 0.0473 0.0647 -1.0011
1 -10 9 0.1103 1.0011 -10.0479 8.9830 -0.2094 -0.7660 -0.6492
-1 20 7 0.1209 -1.0027 19.9567 6.9932 -0.8264 0.2081 -0.5057
5 14 -7 0.1159 5.0030 14.0276 -6.9869 -0.4574 0.0771 0.8960
5 2 -9 0.1025 5.0040 2.0423 -8.9862 -0.0186 -0.0864 0.9971
-5 -14 -2 0.0836 -5.0025 -13.9781 -1.9985 0.8782 0.3588 -0.2238
_database_code_depnum_ccdc_archive 'CCDC 989602'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

#FHDLKA

_refine_special_details          
; 
A second twin component was detected with a twinning matrix of 
(-1 0 0, 0 1 0, 0 0 -1). The batch scale factor was refined to 0.664(14) 
and 0.336(14) for the major and minor twin components, respectively.  
;

_nottingham_internal_coll_name   FHDLKA
_nottingham_internal_coll_number 11925
_nottingham_internal_coll_client FH/DLK
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time 60
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   22/10/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 23/10/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 09/01/2013
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 09/01/2013
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H42 Zn'
_chemical_formula_sum            'C44 H42 Zn'
_chemical_formula_weight         636.15

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41'
_symmetry_space_group_name_Hall  'P 4w'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z+1/4'
'-x, -y, z+1/2'
'y, -x, z+3/4'

_cell_length_a                   10.4016(7)
_cell_length_b                   10.4016(7)
_cell_length_c                   31.197(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3375.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    4113
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      26.01

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.09
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21418
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.071
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.49
_reflns_number_total             7624
_reflns_number_gt                7111
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.035P)²+0.056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         7624
_refine_ls_number_parameters     415
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.109
_refine_ls_wR_factor_gt          0.105
_refine_ls_goodness_of_fit_ref   1.18
_refine_ls_restrained_S_all      1.18
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.49453(7) 0.97086(4) 0.55326(2) 0.02385(11) Uani 1 1 d . . .
C1 C 0.5844(4) 1.1352(4) 0.55168(16) 0.0224(9) Uani 1 1 d . . .
C2 C 0.6106(4) 1.1869(4) 0.51105(14) 0.0221(9) Uani 1 1 d . . .
C3 C 0.6799(5) 1.3018(5) 0.50738(16) 0.0286(11) Uani 1 1 d . . .
H3 H 0.6972 1.3366 0.4798 0.034 Uiso 1 1 calc R . .
C4 C 0.7230(5) 1.3649(4) 0.54358(15) 0.0287(12) Uani 1 1 d . . .
H4 H 0.7715 1.4419 0.5409 0.034 Uiso 1 1 calc R . .
C5 C 0.6952(5) 1.3153(5) 0.58393(15) 0.0283(11) Uani 1 1 d . . .
H5 H 0.7226 1.3602 0.6088 0.034 Uiso 1 1 calc R . .
C6 C 0.6278(5) 1.2007(5) 0.58828(14) 0.0261(10) Uani 1 1 d . . .
C7 C 0.5658(5) 1.1163(4) 0.47160(13) 0.0220(9) Uani 1 1 d . . .
C8 C 0.4420(5) 1.1413(5) 0.45567(16) 0.0299(12) Uani 1 1 d . . .
C9 C 0.3993(5) 1.0681(5) 0.42091(15) 0.0354(11) Uani 1 1 d . . .
H9 H 0.3147 1.0803 0.4102 0.043 Uiso 1 1 calc R . .
C10 C 0.4784(5) 0.9788(5) 0.40217(14) 0.0392(12) Uani 1 1 d . . .
H10 H 0.4487 0.9315 0.3781 0.047 Uiso 1 1 calc R . .
C11 C 0.6008(5) 0.9567(5) 0.41791(16) 0.0356(12) Uani 1 1 d . . .
H11 H 0.6545 0.8946 0.4046 0.043 Uiso 1 1 calc R . .
C12 C 0.6451(5) 1.0251(5) 0.45315(15) 0.0288(11) Uani 1 1 d . . .
C13 C 0.3562(5) 1.2416(6) 0.47515(17) 0.0379(13) Uani 1 1 d . . .
H13A H 0.3401 1.2204 0.5053 0.057 Uiso 1 1 calc R . .
H13B H 0.2744 1.2441 0.4596 0.057 Uiso 1 1 calc R . .
H13C H 0.3981 1.3258 0.4733 0.057 Uiso 1 1 calc R . .
C14 C 0.7786(5) 1.0016(6) 0.47032(17) 0.0346(12) Uani 1 1 d . . .
H14A H 0.8254 1.0832 0.4717 0.052 Uiso 1 1 calc R . .
H14B H 0.8242 0.9421 0.4513 0.052 Uiso 1 1 calc R . .
H14C H 0.7728 0.9641 0.4991 0.052 Uiso 1 1 calc R . .
C15 C 0.6005(5) 1.1495(5) 0.63254(14) 0.0262(10) Uani 1 1 d . . .
C16 C 0.6801(5) 1.0530(5) 0.64959(16) 0.0302(11) Uani 1 1 d . . .
C17 C 0.6526(5) 1.0072(5) 0.69090(16) 0.0393(13) Uani 1 1 d . . .
H17 H 0.7027 0.9397 0.7028 0.047 Uiso 1 1 calc R . .
C18 C 0.5537(6) 1.0597(5) 0.71420(16) 0.0432(15) Uani 1 1 d . . .
H18 H 0.5374 1.0293 0.7424 0.052 Uiso 1 1 calc R . .
C19 C 0.4786(6) 1.1543(5) 0.69759(17) 0.0435(14) Uani 1 1 d . . .
H19 H 0.4105 1.1889 0.7143 0.052 Uiso 1 1 calc R . .
C20 C 0.5001(5) 1.2007(5) 0.65676(14) 0.0325(11) Uani 1 1 d . . .
C21 C 0.7948(5) 1.0032(6) 0.62494(16) 0.0356(12) Uani 1 1 d . . .
H21A H 0.7673 0.9753 0.5964 0.053 Uiso 1 1 calc R . .
H21B H 0.8327 0.9303 0.6403 0.053 Uiso 1 1 calc R . .
H21C H 0.8589 1.0718 0.6221 0.053 Uiso 1 1 calc R . .
C22 C 0.4140(6) 1.3066(6) 0.63791(19) 0.0429(15) Uani 1 1 d . . .
H22A H 0.3822 1.2794 0.6098 0.064 Uiso 1 1 calc R . .
H22B H 0.4639 1.3859 0.6348 0.064 Uiso 1 1 calc R . .
H22C H 0.3411 1.3219 0.6571 0.064 Uiso 1 1 calc R . .
C23 C 0.4015(4) 0.8089(4) 0.55537(15) 0.0235(9) Uani 1 1 d . . .
C24 C 0.4632(4) 0.6883(4) 0.55175(16) 0.0244(9) Uani 1 1 d . . .
C25 C 0.3934(5) 0.5736(4) 0.55497(17) 0.0306(10) Uani 1 1 d . . .
H25 H 0.4357 0.4931 0.5521 0.037 Uiso 1 1 calc R . .
C26 C 0.2624(5) 0.5785(5) 0.56241(15) 0.0302(12) Uani 1 1 d . . .
H26 H 0.2149 0.5009 0.5650 0.036 Uiso 1 1 calc R . .
C27 C 0.2003(5) 0.6946(5) 0.56613(13) 0.0303(12) Uani 1 1 d . . .
H27 H 0.1104 0.6965 0.5715 0.036 Uiso 1 1 calc R . .
C28 C 0.2689(5) 0.8115(5) 0.56208(12) 0.0258(10) Uani 1 1 d . . .
C29 C 0.6038(5) 0.6829(4) 0.54309(15) 0.0258(11) Uani 1 1 d . . .
C30 C 0.6923(5) 0.6934(5) 0.57686(16) 0.0273(10) Uani 1 1 d . . .
C31 C 0.8238(5) 0.6940(5) 0.56784(16) 0.0315(11) Uani 1 1 d . . .
H31 H 0.8841 0.7033 0.5905 0.038 Uiso 1 1 calc R . .
C32 C 0.8668(5) 0.6812(5) 0.52605(16) 0.0306(10) Uani 1 1 d . . .
H32 H 0.9563 0.6827 0.5202 0.037 Uiso 1 1 calc R . .
C33 C 0.7808(5) 0.6663(5) 0.49312(14) 0.0309(11) Uani 1 1 d . . .
H33 H 0.8114 0.6552 0.4647 0.037 Uiso 1 1 calc R . .
C34 C 0.6495(5) 0.6674(5) 0.50091(16) 0.0309(12) Uani 1 1 d . . .
C35 C 0.6471(5) 0.6956(6) 0.62258(16) 0.0355(13) Uani 1 1 d . . .
H35A H 0.5863 0.6251 0.6273 0.053 Uiso 1 1 calc R . .
H35B H 0.6046 0.7778 0.6285 0.053 Uiso 1 1 calc R . .
H35C H 0.7210 0.6854 0.6418 0.053 Uiso 1 1 calc R . .
C36 C 0.5552(5) 0.6483(5) 0.46461(15) 0.0352(13) Uani 1 1 d . . .
H36A H 0.4942 0.7201 0.4640 0.053 Uiso 1 1 calc R . .
H36B H 0.5084 0.5676 0.4689 0.053 Uiso 1 1 calc R . .
H36C H 0.6020 0.6448 0.4374 0.053 Uiso 1 1 calc R . .
C37 C 0.1999(4) 0.9377(5) 0.56573(14) 0.0245(10) Uani 1 1 d . . .
C38 C 0.1412(4) 0.9918(5) 0.52928(15) 0.0300(10) Uani 1 1 d . . .
C39 C 0.0813(5) 1.1108(6) 0.53338(18) 0.0387(13) Uani 1 1 d . . .
H39 H 0.0424 1.1489 0.5089 0.046 Uiso 1 1 calc R . .
C40 C 0.0771(5) 1.1748(6) 0.57216(19) 0.0395(13) Uani 1 1 d . . .
H40 H 0.0331 1.2545 0.5745 0.047 Uiso 1 1 calc R . .
C41 C 0.1373(5) 1.1222(5) 0.60740(17) 0.0353(12) Uani 1 1 d . . .
H41 H 0.1367 1.1675 0.6338 0.042 Uiso 1 1 calc R . .
C42 C 0.1987(4) 1.0042(5) 0.60479(14) 0.0274(10) Uani 1 1 d . . .
C43 C 0.1448(6) 0.9230(6) 0.48651(15) 0.0391(14) Uani 1 1 d . . .
H43A H 0.2338 0.9001 0.4795 0.059 Uiso 1 1 calc R . .
H43B H 0.1105 0.9796 0.4642 0.059 Uiso 1 1 calc R . .
H43C H 0.0926 0.8447 0.4881 0.059 Uiso 1 1 calc R . .
C44 C 0.2643(5) 0.9467(5) 0.64367(14) 0.0324(12) Uani 1 1 d . . .
H44A H 0.2435 0.8550 0.6456 0.049 Uiso 1 1 calc R . .
H44B H 0.2342 0.9906 0.6696 0.049 Uiso 1 1 calc R . .
H44C H 0.3575 0.9573 0.6410 0.049 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Zn1 C23 1.944(4) . ?
Zn1 C1 1.949(4) . ?
C1 C2 1.403(6) . ?
C1 C6 1.404(6) . ?
C2 C3 1.400(7) . ?
C2 C7 1.507(6) . ?
C3 C4 1.381(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(7) . ?
C5 H5 0.9500 . ?
C6 C15 1.507(6) . ?
C7 C12 1.382(6) . ?
C7 C8 1.405(7) . ?
C8 C9 1.397(7) . ?
C8 C13 1.501(7) . ?
C9 C10 1.372(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(7) . ?
C11 H11 0.9500 . ?
C12 C14 1.508(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.395(7) . ?
C15 C16 1.405(7) . ?
C16 C17 1.403(7) . ?
C16 C21 1.511(7) . ?
C17 C18 1.373(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.359(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(7) . ?
C19 H19 0.9500 . ?
C20 C22 1.536(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C28 1.395(6) . ?
C23 C24 1.413(6) . ?
C24 C25 1.401(6) . ?
C24 C29 1.488(7) . ?
C25 C26 1.384(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.375(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.416(6) . ?
C27 H27 0.9500 . ?
C28 C37 1.501(7) . ?
C29 C30 1.404(6) . ?
C29 C34 1.408(7) . ?
C30 C31 1.396(6) . ?
C30 C35 1.502(7) . ?
C31 C32 1.385(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.371(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.387(7) . ?
C33 H33 0.9500 . ?
C34 C36 1.511(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C42 1.401(6) . ?
C37 C38 1.408(6) . ?
C38 C39 1.392(7) . ?
C38 C43 1.515(7) . ?
C39 C40 1.382(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.378(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.386(7) . ?
C41 H41 0.9500 . ?
C42 C44 1.515(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

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
C23 Zn1 C1 178.7(2) . . ?
C2 C1 C6 119.1(4) . . ?
C2 C1 Zn1 116.9(3) . . ?
C6 C1 Zn1 124.0(3) . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 C7 120.5(4) . . ?
C1 C2 C7 119.4(4) . . ?
C4 C3 C2 120.4(5) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.8(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 119.9(4) . . ?
C5 C6 C15 119.2(4) . . ?
C1 C6 C15 120.9(4) . . ?
C12 C7 C8 121.8(4) . . ?
C12 C7 C2 119.3(4) . . ?
C8 C7 C2 118.8(4) . . ?
C9 C8 C7 117.7(5) . . ?
C9 C8 C13 120.3(5) . . ?
C7 C8 C13 122.0(5) . . ?
C10 C9 C8 120.6(5) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.9(5) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C12 120.1(5) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C7 C12 C11 118.9(4) . . ?
C7 C12 C14 120.8(4) . . ?
C11 C12 C14 120.2(5) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 120.6(4) . . ?
C20 C15 C6 120.2(5) . . ?
C16 C15 C6 119.2(5) . . ?
C17 C16 C15 118.0(5) . . ?
C17 C16 C21 120.8(5) . . ?
C15 C16 C21 121.2(4) . . ?
C18 C17 C16 120.3(5) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 121.1(5) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 120.8(6) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C15 119.2(5) . . ?
C19 C20 C22 120.6(5) . . ?
C15 C20 C22 120.2(4) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C28 C23 C24 118.6(4) . . ?
C28 C23 Zn1 118.7(3) . . ?
C24 C23 Zn1 122.7(3) . . ?
C25 C24 C23 121.0(4) . . ?
C25 C24 C29 119.3(4) . . ?
C23 C24 C29 119.6(4) . . ?
C26 C25 C24 119.4(5) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C27 C26 C25 120.7(4) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 120.7(5) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C23 C28 C27 119.7(5) . . ?
C23 C28 C37 120.1(4) . . ?
C27 C28 C37 120.2(4) . . ?
C30 C29 C34 119.3(5) . . ?
C30 C29 C24 120.4(4) . . ?
C34 C29 C24 120.4(4) . . ?
C31 C30 C29 119.5(5) . . ?
C31 C30 C35 119.9(5) . . ?
C29 C30 C35 120.6(5) . . ?
C32 C31 C30 120.4(5) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 120.4(5) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 120.7(4) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C33 C34 C29 119.8(5) . . ?
C33 C34 C36 120.4(5) . . ?
C29 C34 C36 119.8(5) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C42 C37 C38 120.1(5) . . ?
C42 C37 C28 120.2(4) . . ?
C38 C37 C28 119.7(4) . . ?
C39 C38 C37 118.4(5) . . ?
C39 C38 C43 120.8(4) . . ?
C37 C38 C43 120.8(4) . . ?
C40 C39 C38 121.5(5) . . ?
C40 C39 H39 119.2 . . ?
C38 C39 H39 119.2 . . ?
C41 C40 C39 119.5(5) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
C40 C41 C42 120.9(5) . . ?
C40 C41 H41 119.5 . . ?
C42 C41 H41 119.5 . . ?
C41 C42 C37 119.5(4) . . ?
C41 C42 C44 120.7(4) . . ?
C37 C42 C44 119.8(5) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C23 Zn1 C1 C2 -111(10) . . . . ?
C23 Zn1 C1 C6 71(10) . . . . ?
C6 C1 C2 C3 0.4(7) . . . . ?
Zn1 C1 C2 C3 -177.2(4) . . . . ?
C6 C1 C2 C7 179.2(4) . . . . ?
Zn1 C1 C2 C7 1.7(6) . . . . ?
C1 C2 C3 C4 0.1(7) . . . . ?
C7 C2 C3 C4 -178.7(4) . . . . ?
C2 C3 C4 C5 -1.3(8) . . . . ?
C3 C4 C5 C6 2.0(8) . . . . ?
C4 C5 C6 C1 -1.5(8) . . . . ?
C4 C5 C6 C15 179.5(5) . . . . ?
C2 C1 C6 C5 0.3(7) . . . . ?
Zn1 C1 C6 C5 177.7(4) . . . . ?
C2 C1 C6 C15 179.3(5) . . . . ?
Zn1 C1 C6 C15 -3.3(7) . . . . ?
C3 C2 C7 C12 89.7(6) . . . . ?
C1 C2 C7 C12 -89.1(5) . . . . ?
C3 C2 C7 C8 -93.0(5) . . . . ?
C1 C2 C7 C8 88.1(5) . . . . ?
C12 C7 C8 C9 1.7(7) . . . . ?
C2 C7 C8 C9 -175.5(4) . . . . ?
C12 C7 C8 C13 -179.0(5) . . . . ?
C2 C7 C8 C13 3.8(7) . . . . ?
C7 C8 C9 C10 -2.5(7) . . . . ?
C13 C8 C9 C10 178.1(5) . . . . ?
C8 C9 C10 C11 1.7(8) . . . . ?
C9 C10 C11 C12 0.1(8) . . . . ?
C8 C7 C12 C11 0.1(7) . . . . ?
C2 C7 C12 C11 177.3(4) . . . . ?
C8 C7 C12 C14 178.9(4) . . . . ?
C2 C7 C12 C14 -3.9(7) . . . . ?
C10 C11 C12 C7 -1.0(8) . . . . ?
C10 C11 C12 C14 -179.8(5) . . . . ?
C5 C6 C15 C20 79.1(6) . . . . ?
C1 C6 C15 C20 -99.9(6) . . . . ?
C5 C6 C15 C16 -98.6(6) . . . . ?
C1 C6 C15 C16 82.4(6) . . . . ?
C20 C15 C16 C17 2.1(7) . . . . ?
C6 C15 C16 C17 179.9(4) . . . . ?
C20 C15 C16 C21 -175.7(5) . . . . ?
C6 C15 C16 C21 2.1(7) . . . . ?
C15 C16 C17 C18 -2.5(7) . . . . ?
C21 C16 C17 C18 175.3(5) . . . . ?
C16 C17 C18 C19 1.6(8) . . . . ?
C17 C18 C19 C20 -0.2(8) . . . . ?
C18 C19 C20 C15 -0.2(8) . . . . ?
C18 C19 C20 C22 179.3(5) . . . . ?
C16 C15 C20 C19 -0.9(7) . . . . ?
C6 C15 C20 C19 -178.6(4) . . . . ?
C16 C15 C20 C22 179.7(5) . . . . ?
C6 C15 C20 C22 2.0(7) . . . . ?
C1 Zn1 C23 C28 13(10) . . . . ?
C1 Zn1 C23 C24 -165(32) . . . . ?
C28 C23 C24 C25 -0.3(7) . . . . ?
Zn1 C23 C24 C25 177.7(4) . . . . ?
C28 C23 C24 C29 177.9(4) . . . . ?
Zn1 C23 C24 C29 -4.2(6) . . . . ?
C23 C24 C25 C26 -0.9(8) . . . . ?
C29 C24 C25 C26 -179.1(4) . . . . ?
C24 C25 C26 C27 0.8(7) . . . . ?
C25 C26 C27 C28 0.5(7) . . . . ?
C24 C23 C28 C27 1.5(6) . . . . ?
Zn1 C23 C28 C27 -176.5(3) . . . . ?
C24 C23 C28 C37 -179.5(4) . . . . ?
Zn1 C23 C28 C37 2.5(5) . . . . ?
C26 C27 C28 C23 -1.7(6) . . . . ?
C26 C27 C28 C37 179.4(4) . . . . ?
C25 C24 C29 C30 -98.0(6) . . . . ?
C23 C24 C29 C30 83.8(6) . . . . ?
C25 C24 C29 C34 82.1(6) . . . . ?
C23 C24 C29 C34 -96.1(6) . . . . ?
C34 C29 C30 C31 2.8(7) . . . . ?
C24 C29 C30 C31 -177.1(4) . . . . ?
C34 C29 C30 C35 -173.3(5) . . . . ?
C24 C29 C30 C35 6.8(8) . . . . ?
C29 C30 C31 C32 -1.6(8) . . . . ?
C35 C30 C31 C32 174.6(5) . . . . ?
C30 C31 C32 C33 -0.7(8) . . . . ?
C31 C32 C33 C34 1.8(8) . . . . ?
C32 C33 C34 C29 -0.5(8) . . . . ?
C32 C33 C34 C36 -178.8(5) . . . . ?
C30 C29 C34 C33 -1.8(7) . . . . ?
C24 C29 C34 C33 178.1(5) . . . . ?
C30 C29 C34 C36 176.5(5) . . . . ?
C24 C29 C34 C36 -3.6(7) . . . . ?
C23 C28 C37 C42 -82.1(5) . . . . ?
C27 C28 C37 C42 96.8(5) . . . . ?
C23 C28 C37 C38 95.1(5) . . . . ?
C27 C28 C37 C38 -85.9(5) . . . . ?
C42 C37 C38 C39 -0.8(7) . . . . ?
C28 C37 C38 C39 -178.1(4) . . . . ?
C42 C37 C38 C43 178.3(4) . . . . ?
C28 C37 C38 C43 1.1(7) . . . . ?
C37 C38 C39 C40 -0.9(7) . . . . ?
C43 C38 C39 C40 180.0(5) . . . . ?
C38 C39 C40 C41 2.2(8) . . . . ?
C39 C40 C41 C42 -1.9(8) . . . . ?
C40 C41 C42 C37 0.3(7) . . . . ?
C40 C41 C42 C44 -179.8(5) . . . . ?
C38 C37 C42 C41 1.1(7) . . . . ?
C28 C37 C42 C41 178.4(4) . . . . ?
C38 C37 C42 C44 -178.8(4) . . . . ?
C28 C37 C42 C44 -1.6(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         0.60
_refine_diff_density_min         -0.37
_refine_diff_density_rms         0.06
_database_code_depnum_ccdc_archive 'CCDC 989603'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

#FHDLKC 

_refine_special_details          
; 
Merohedral crystal twinning was detected. A twin matrix (0 1 0/1 0 0/0 0 -1) was
identified and the twin fraction refined to 0.6166(13) and 0.3834(13)
for the major and minor twin components, respectively.

A rigid bond restraint (DELU) was applied to atoms C24, C25, C23, C29, 
C26, C28, C30 and C34.  
;

_nottingham_internal_coll_name   FHDLKC
_nottingham_internal_coll_number 11985
_nottingham_internal_coll_client FH/TB/DLK
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time 60
_nottingham_internal_coll_frame_width '0.3 and 0.5'
_nottingham_internal_coll_frame_method '\w and \f'
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   01/11/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 05/11/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 26/01/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 26/01/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?


_audit_creation_method           SHELXL97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H42 Cd'
_chemical_formula_sum            'C44 H42 Cd'
_chemical_formula_weight         683.18

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 43'
_symmetry_space_group_name_Hall  'P 4cw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z+3/4'
'-x, -y, z+1/2'
'y, -x, z+1/4'

_cell_length_a                   10.5072(3)
_cell_length_b                   10.5072(3)
_cell_length_c                   31.0528(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3428.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    4628
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      26.85

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.11
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_max          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            42410
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         27.51
_reflns_number_total             7863
_reflns_number_gt                7333
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.022P)²+0.660P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_number_reflns         7863
_refine_ls_number_parameters     415
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.0906
_refine_ls_wR_factor_gt          0.0884
_refine_ls_goodness_of_fit_ref   1.15
_refine_ls_restrained_S_all      1.15
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cd1 Cd 0.50901(6) 0.02817(3) 0.47139(2) 0.02377(8) Uani 1 1 d . . .
C1 C 0.4113(5) -0.1477(5) 0.4730(2) 0.0266(12) Uani 1 1 d . . .
C2 C 0.3683(6) -0.2112(6) 0.43614(18) 0.0284(14) Uani 1 1 d . . .
C3 C 0.3018(6) -0.3256(6) 0.43995(19) 0.0286(15) Uani 1 1 d . . .
H3 H 0.2766 -0.3703 0.4148 0.034 Uiso 1 1 calc R . .
C4 C 0.2720(6) -0.3749(5) 0.4804(2) 0.0285(15) Uani 1 1 d . . .
H4 H 0.2228 -0.4504 0.4829 0.034 Uiso 1 1 calc R . .
C5 C 0.3151(6) -0.3124(6) 0.5169(2) 0.0289(15) Uani 1 1 d . . .
H5 H 0.2975 -0.3471 0.5446 0.035 Uiso 1 1 calc R . .
C6 C 0.3837(5) -0.1996(6) 0.51363(18) 0.0251(13) Uani 1 1 d . . .
C7 C 0.3992(6) -0.1574(7) 0.39143(18) 0.0253(13) Uani 1 1 d . . .
C8 C 0.5036(7) -0.2056(6) 0.36840(19) 0.0343(15) Uani 1 1 d . . .
C9 C 0.5283(7) -0.1552(6) 0.32771(19) 0.0391(17) Uani 1 1 d . . .
H9 H 0.5978 -0.1867 0.3113 0.047 Uiso 1 1 calc R . .
C10 C 0.4528(6) -0.0603(6) 0.31130(17) 0.0345(15) Uani 1 1 d . . .
H10 H 0.4715 -0.0270 0.2836 0.041 Uiso 1 1 calc R . .
C11 C 0.3521(6) -0.0126(7) 0.3336(2) 0.0371(15) Uani 1 1 d . . .
H11 H 0.3023 0.0540 0.3217 0.045 Uiso 1 1 calc R . .
C12 C 0.3220(6) -0.0626(6) 0.37455(19) 0.0266(15) Uani 1 1 d . . .
C13 C 0.5899(7) -0.3066(7) 0.3877(2) 0.0402(18) Uani 1 1 d . . .
H13A H 0.6116 -0.2831 0.4174 0.060 Uiso 1 1 calc R . .
H13B H 0.6680 -0.3130 0.3706 0.060 Uiso 1 1 calc R . .
H13C H 0.5459 -0.3888 0.3877 0.060 Uiso 1 1 calc R . .
C14 C 0.2064(6) -0.0132(7) 0.3984(2) 0.0367(16) Uani 1 1 d . . .
H14A H 0.1419 -0.0804 0.4001 0.055 Uiso 1 1 calc R . .
H14B H 0.1712 0.0602 0.3830 0.055 Uiso 1 1 calc R . .
H14C H 0.2312 0.0125 0.4276 0.055 Uiso 1 1 calc R . .
C15 C 0.4322(6) -0.1288(6) 0.55252(17) 0.0215(12) Uani 1 1 d . . .
C16 C 0.3550(6) -0.0380(6) 0.57195(18) 0.0248(14) Uani 1 1 d . . .
C17 C 0.4028(6) 0.0321(6) 0.60578(18) 0.0318(14) Uani 1 1 d . . .
H17 H 0.3509 0.0949 0.6191 0.038 Uiso 1 1 calc R . .
C18 C 0.5252(7) 0.0124(5) 0.62060(17) 0.0400(15) Uani 1 1 d . . .
H18 H 0.5562 0.0606 0.6443 0.048 Uiso 1 1 calc R . .
C19 C 0.6026(6) -0.0767(7) 0.60134(18) 0.0362(15) Uani 1 1 d . . .
H19 H 0.6876 -0.0874 0.6112 0.043 Uiso 1 1 calc R . .
C20 C 0.5570(7) -0.1518(6) 0.56732(19) 0.0280(15) Uani 1 1 d . . .
C21 C 0.2217(6) -0.0144(7) 0.5560(2) 0.0329(16) Uani 1 1 d . . .
H21A H 0.2245 0.0100 0.5255 0.049 Uiso 1 1 calc R . .
H21B H 0.1829 0.0543 0.5728 0.049 Uiso 1 1 calc R . .
H21C H 0.1711 -0.0921 0.5592 0.049 Uiso 1 1 calc R . .
C22 C 0.6401(6) -0.2494(7) 0.5472(2) 0.0354(16) Uani 1 1 d . . .
H22A H 0.6034 -0.3340 0.5518 0.053 Uiso 1 1 calc R . .
H22B H 0.7250 -0.2457 0.5603 0.053 Uiso 1 1 calc R . .
H22C H 0.6469 -0.2329 0.5162 0.053 Uiso 1 1 calc R . .
C23 C 0.6067(6) 0.2044(5) 0.4696(2) 0.0263(11) Uani 1 1 d U . .
C24 C 0.5423(5) 0.3209(5) 0.47258(19) 0.0242(11) Uani 1 1 d U . .
C25 C 0.6085(5) 0.4362(5) 0.4692(2) 0.0284(11) Uani 1 1 d U . .
H25 H 0.5647 0.5149 0.4719 0.034 Uiso 1 1 calc R . .
C26 C 0.7383(6) 0.4341(6) 0.46195(17) 0.0286(14) Uani 1 1 d U . .
H26 H 0.7832 0.5120 0.4589 0.034 Uiso 1 1 calc R . .
C27 C 0.8034(6) 0.3209(7) 0.45908(16) 0.0333(16) Uani 1 1 d . . .
H27 H 0.8928 0.3212 0.4545 0.040 Uiso 1 1 calc R . .
C28 C 0.7376(5) 0.2035(5) 0.46299(14) 0.0242(11) Uani 1 1 d U . .
C29 C 0.4023(6) 0.3201(6) 0.48070(19) 0.0281(13) Uani 1 1 d U . .
C30 C 0.3562(6) 0.3300(6) 0.52279(19) 0.0274(14) Uani 1 1 d U . .
C31 C 0.2265(6) 0.3239(6) 0.53042(18) 0.0331(14) Uani 1 1 d . . .
H31 H 0.1956 0.3323 0.5590 0.040 Uiso 1 1 calc R . .
C32 C 0.1423(6) 0.3061(6) 0.4974(2) 0.0302(15) Uani 1 1 d . . .
H32 H 0.0538 0.2990 0.5032 0.036 Uiso 1 1 calc R . .
C33 C 0.1869(6) 0.2983(6) 0.45545(19) 0.0297(14) Uani 1 1 d . . .
H33 H 0.1278 0.2877 0.4326 0.036 Uiso 1 1 calc R . .
C34 C 0.3160(6) 0.3057(6) 0.44608(19) 0.0276(13) Uani 1 1 d U . .
C35 C 0.4480(7) 0.3510(6) 0.56020(18) 0.0352(17) Uani 1 1 d . . .
H35A H 0.5052 0.2776 0.5627 0.053 Uiso 1 1 calc R . .
H35B H 0.3997 0.3607 0.5870 0.053 Uiso 1 1 calc R . .
H35C H 0.4982 0.4280 0.5550 0.053 Uiso 1 1 calc R . .
C36 C 0.3614(7) 0.3039(7) 0.40087(19) 0.0327(16) Uani 1 1 d . . .
H36A H 0.4157 0.3782 0.3957 0.049 Uiso 1 1 calc R . .
H36B H 0.2882 0.3064 0.3813 0.049 Uiso 1 1 calc R . .
H36C H 0.4103 0.2260 0.3957 0.049 Uiso 1 1 calc R . .
C37 C 0.8055(6) 0.0778(6) 0.46009(17) 0.0252(14) Uani 1 1 d . . .
C38 C 0.8069(5) 0.0093(7) 0.42113(19) 0.0319(14) Uani 1 1 d . . .
C39 C 0.8626(6) -0.1097(7) 0.4191(2) 0.0353(16) Uani 1 1 d . . .
H39 H 0.8628 -0.1562 0.3929 0.042 Uiso 1 1 calc R . .
C40 C 0.9182(6) -0.1605(7) 0.4557(2) 0.0404(18) Uani 1 1 d . . .
H40 H 0.9589 -0.2411 0.4543 0.048 Uiso 1 1 calc R . .
C41 C 0.9151(6) -0.0957(7) 0.4943(2) 0.0395(17) Uani 1 1 d . . .
H41 H 0.9521 -0.1330 0.5192 0.047 Uiso 1 1 calc R . .
C42 C 0.8592(5) 0.0222(7) 0.49720(18) 0.0305(13) Uani 1 1 d . . .
C43 C 0.7421(7) 0.0647(7) 0.38145(18) 0.0360(17) Uani 1 1 d . . .
H43A H 0.6509 0.0455 0.3824 0.054 Uiso 1 1 calc R . .
H43B H 0.7794 0.0272 0.3555 0.054 Uiso 1 1 calc R . .
H43C H 0.7543 0.1572 0.3809 0.054 Uiso 1 1 calc R . .
C44 C 0.8541(7) 0.0910(7) 0.53997(19) 0.0386(18) Uani 1 1 d . . .
H44A H 0.8977 0.1731 0.5374 0.058 Uiso 1 1 calc R . .
H44B H 0.8963 0.0393 0.5620 0.058 Uiso 1 1 calc R . .
H44C H 0.7652 0.1051 0.5482 0.058 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Cd1 C1 2.115(5) . ?
Cd1 C23 2.118(5) . ?
C1 C2 1.400(8) . ?
C1 C6 1.405(8) . ?
C2 C3 1.395(9) . ?
C2 C7 1.534(8) . ?
C3 C4 1.395(8) . ?
C4 C5 1.386(8) . ?
C5 C6 1.391(9) . ?
C6 C15 1.508(8) . ?
C7 C12 1.388(9) . ?
C7 C8 1.404(9) . ?
C8 C9 1.395(8) . ?
C8 C13 1.519(10) . ?
C9 C10 1.372(9) . ?
C10 C11 1.360(9) . ?
C11 C12 1.412(9) . ?
C12 C14 1.515(9) . ?
C15 C16 1.389(8) . ?
C15 C20 1.410(9) . ?
C16 C17 1.378(8) . ?
C16 C21 1.506(8) . ?
C17 C18 1.382(9) . ?
C18 C19 1.376(8) . ?
C19 C20 1.403(9) . ?
C20 C22 1.485(9) . ?
C23 C28 1.391(8) . ?
C23 C24 1.401(8) . ?
C24 C25 1.401(7) . ?
C24 C29 1.493(9) . ?
C25 C26 1.382(8) . ?
C26 C27 1.375(10) . ?
C27 C28 1.419(7) . ?
C28 C37 1.504(8) . ?
C29 C30 1.398(8) . ?
C29 C34 1.414(8) . ?
C30 C31 1.384(9) . ?
C30 C35 1.526(8) . ?
C31 C32 1.367(8) . ?
C32 C33 1.387(8) . ?
C33 C34 1.390(8) . ?
C34 C36 1.483(8) . ?
C37 C38 1.408(8) . ?
C37 C42 1.409(8) . ?
C38 C39 1.382(9) . ?
C38 C43 1.524(8) . ?
C39 C40 1.385(9) . ?
C40 C41 1.377(9) . ?
C41 C42 1.374(9) . ?
C42 C44 1.513(8) . ?

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
C1 Cd1 C23 179.9(3) . . ?
C2 C1 C6 118.9(5) . . ?
C2 C1 Cd1 123.6(5) . . ?
C6 C1 Cd1 117.5(5) . . ?
C3 C2 C1 120.2(5) . . ?
C3 C2 C7 120.0(5) . . ?
C1 C2 C7 119.8(6) . . ?
C4 C3 C2 120.6(6) . . ?
C5 C4 C3 119.2(5) . . ?
C4 C5 C6 120.9(6) . . ?
C5 C6 C1 120.3(6) . . ?
C5 C6 C15 122.5(5) . . ?
C1 C6 C15 117.2(5) . . ?
C12 C7 C8 121.6(6) . . ?
C12 C7 C2 118.9(6) . . ?
C8 C7 C2 119.6(6) . . ?
C9 C8 C7 118.0(6) . . ?
C9 C8 C13 120.8(6) . . ?
C7 C8 C13 121.2(6) . . ?
C10 C9 C8 120.3(6) . . ?
C11 C10 C9 121.9(6) . . ?
C10 C11 C12 119.7(7) . . ?
C7 C12 C11 118.4(6) . . ?
C7 C12 C14 122.0(6) . . ?
C11 C12 C14 119.6(6) . . ?
C16 C15 C20 121.3(6) . . ?
C16 C15 C6 119.3(5) . . ?
C20 C15 C6 119.4(6) . . ?
C17 C16 C15 119.0(6) . . ?
C17 C16 C21 120.1(6) . . ?
C15 C16 C21 120.8(6) . . ?
C16 C17 C18 120.9(6) . . ?
C19 C18 C17 120.5(6) . . ?
C18 C19 C20 120.5(6) . . ?
C19 C20 C15 117.8(6) . . ?
C19 C20 C22 120.3(6) . . ?
C15 C20 C22 121.9(6) . . ?
C28 C23 C24 119.6(5) . . ?
C28 C23 Cd1 118.5(4) . . ?
C24 C23 Cd1 121.9(4) . . ?
C25 C24 C23 120.7(5) . . ?
C25 C24 C29 120.4(6) . . ?
C23 C24 C29 118.8(5) . . ?
C26 C25 C24 119.2(6) . . ?
C27 C26 C25 121.0(5) . . ?
C26 C27 C28 120.2(6) . . ?
C23 C28 C27 119.3(6) . . ?
C23 C28 C37 119.0(5) . . ?
C27 C28 C37 121.8(5) . . ?
C30 C29 C34 119.8(6) . . ?
C30 C29 C24 119.9(5) . . ?
C34 C29 C24 120.2(6) . . ?
C31 C30 C29 119.8(6) . . ?
C31 C30 C35 119.9(6) . . ?
C29 C30 C35 120.2(6) . . ?
C32 C31 C30 121.0(6) . . ?
C31 C32 C33 119.6(6) . . ?
C32 C33 C34 121.5(6) . . ?
C33 C34 C29 118.2(6) . . ?
C33 C34 C36 120.8(6) . . ?
C29 C34 C36 121.0(6) . . ?
C38 C37 C42 119.1(6) . . ?
C38 C37 C28 120.4(5) . . ?
C42 C37 C28 120.3(5) . . ?
C39 C38 C37 120.4(6) . . ?
C39 C38 C43 119.9(6) . . ?
C37 C38 C43 119.7(6) . . ?
C38 C39 C40 119.3(6) . . ?
C41 C40 C39 120.9(6) . . ?
C42 C41 C40 120.9(6) . . ?
C41 C42 C37 119.4(6) . . ?
C41 C42 C44 120.2(6) . . ?
C37 C42 C44 120.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         0.81
_refine_diff_density_min         -0.50
_refine_diff_density_rms         0.08
_database_code_depnum_ccdc_archive 'CCDC 989604'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_7

#FHDLKB

_nottingham_internal_coll_name   FHDLKB
_nottingham_internal_coll_number 11925
_nottingham_internal_coll_client FH/TB/DLK
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time 30
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   30/10/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 31/10/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 21/12/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 21/12/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H42 Hg'
_chemical_formula_sum            'C44 H42 Hg'
_chemical_formula_weight         771.37

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'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41/a
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   20.903(9)
_cell_length_b                   20.903(9)
_cell_length_c                   31.72(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     13861(14)
_cell_formula_units_Z            16
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    4530
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      24.28

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.11
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_max          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             6176
_exptl_absorpt_coefficient_mu    4.471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            60540
_diffrn_reflns_av_R_equivalents  0.107
_diffrn_reflns_av_sigmaI/netI    0.063
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         27.53
_reflns_number_total             7895
_reflns_number_gt                5594
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.030P)²+9.94P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7895
_refine_ls_number_parameters     414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.0865
_refine_ls_wR_factor_gt          0.0775
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_restrained_S_all      1.06
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
Hg1 Hg 0.735881(9) 0.738086(9) 0.486179(6) 0.02650(7) Uani 1 1 d . . .
C23 C 0.8153(2) 0.6765(2) 0.48474(17) 0.0299(12) Uani 1 1 d . . .
C1 C 0.6543(2) 0.7955(2) 0.48902(18) 0.0280(11) Uani 1 1 d . . .
C4 C 0.5380(3) 0.8623(3) 0.4925(2) 0.0434(16) Uani 1 1 d . . .
H4 H 0.4981 0.8841 0.4938 0.052 Uiso 1 1 calc R . .
C29 C 0.7392(3) 0.5827(2) 0.48572(19) 0.0343(13) Uani 1 1 d . . .
C24 C 0.8062(2) 0.6109(3) 0.48655(17) 0.0312(12) Uani 1 1 d . . .
C22 C 0.7316(3) 0.8944(3) 0.5582(2) 0.0427(15) Uani 1 1 d . . .
H22A H 0.7529 0.8837 0.5316 0.064 Uiso 1 1 calc R . .
H22B H 0.7605 0.9200 0.5757 0.064 Uiso 1 1 calc R . .
H22C H 0.6927 0.9190 0.5523 0.064 Uiso 1 1 calc R . .
C21 C 0.5951(3) 0.6933(3) 0.5746(2) 0.0502(17) Uani 1 1 d . . .
H21A H 0.5544 0.7164 0.5761 0.075 Uiso 1 1 calc R . .
H21B H 0.5933 0.6556 0.5929 0.075 Uiso 1 1 calc R . .
H21C H 0.6028 0.6796 0.5454 0.075 Uiso 1 1 calc R . .
C27 C 0.9306(3) 0.6607(3) 0.48352(19) 0.0404(15) Uani 1 1 d . . .
H27 H 0.9727 0.6776 0.4824 0.049 Uiso 1 1 calc R . .
C14 C 0.7220(3) 0.8981(3) 0.4173(2) 0.0502(17) Uani 1 1 d . . .
H14A H 0.6840 0.9223 0.4258 0.075 Uiso 1 1 calc R . .
H14B H 0.7482 0.9244 0.3984 0.075 Uiso 1 1 calc R . .
H14C H 0.7470 0.8867 0.4423 0.075 Uiso 1 1 calc R . .
C13 C 0.5826(3) 0.6990(3) 0.4055(2) 0.0512(17) Uani 1 1 d . . .
H13A H 0.5424 0.7230 0.4072 0.077 Uiso 1 1 calc R . .
H13B H 0.5946 0.6838 0.4336 0.077 Uiso 1 1 calc R . .
H13C H 0.5771 0.6623 0.3866 0.077 Uiso 1 1 calc R . .
C15 C 0.6634(2) 0.7939(3) 0.56756(18) 0.0338(13) Uani 1 1 d . . .
C43 C 0.8958(3) 0.7854(4) 0.5560(2) 0.065(2) Uani 1 1 d . . .
H43A H 0.9056 0.8191 0.5765 0.098 Uiso 1 1 calc R . .
H43B H 0.9291 0.7524 0.5572 0.098 Uiso 1 1 calc R . .
H43C H 0.8543 0.7663 0.5627 0.098 Uiso 1 1 calc R . .
C20 C 0.6490(3) 0.7369(3) 0.58884(19) 0.0382(14) Uani 1 1 d . . .
C9 C 0.6666(3) 0.7274(3) 0.3510(2) 0.0475(16) Uani 1 1 d . . .
H9 H 0.6545 0.6903 0.3356 0.057 Uiso 1 1 calc R . .
C16 C 0.7142(3) 0.8339(3) 0.58115(18) 0.0343(13) Uani 1 1 d . . .
C35 C 0.7404(3) 0.5922(3) 0.40649(18) 0.0425(15) Uani 1 1 d . . .
H35A H 0.7492 0.6383 0.4064 0.064 Uiso 1 1 calc R . .
H35B H 0.7123 0.5816 0.3828 0.064 Uiso 1 1 calc R . .
H35C H 0.7807 0.5686 0.4038 0.064 Uiso 1 1 calc R . .
C12 C 0.7017(3) 0.8381(3) 0.3947(2) 0.0396(14) Uani 1 1 d . . .
C3 C 0.5648(3) 0.8486(3) 0.4538(2) 0.0381(14) Uani 1 1 d . . .
H3 H 0.5443 0.8619 0.4286 0.046 Uiso 1 1 calc R . .
C8 C 0.6350(3) 0.7422(3) 0.3884(2) 0.0417(15) Uani 1 1 d . . .
C26 C 0.9215(3) 0.5949(3) 0.4862(2) 0.0439(15) Uani 1 1 d . . .
H26 H 0.9575 0.5672 0.4874 0.053 Uiso 1 1 calc R . .
C2 C 0.6230(2) 0.8145(2) 0.45207(18) 0.0319(13) Uani 1 1 d . . .
C44 C 0.8793(3) 0.7581(3) 0.3991(2) 0.0569(18) Uani 1 1 d . . .
H44A H 0.9172 0.7307 0.3971 0.085 Uiso 1 1 calc R . .
H44B H 0.8757 0.7843 0.3736 0.085 Uiso 1 1 calc R . .
H44C H 0.8411 0.7314 0.4021 0.085 Uiso 1 1 calc R . .
C5 C 0.5690(3) 0.8446(3) 0.5296(2) 0.0377(14) Uani 1 1 d . . .
H5 H 0.5504 0.8549 0.5561 0.045 Uiso 1 1 calc R . .
C7 C 0.6522(3) 0.7980(3) 0.41053(18) 0.0360(14) Uani 1 1 d . . .
C42 C 0.8855(3) 0.8010(3) 0.4369(2) 0.0446(16) Uani 1 1 d . . .
C33 C 0.6459(3) 0.5390(3) 0.5208(2) 0.0518(18) Uani 1 1 d . . .
H33 H 0.6245 0.5266 0.5459 0.062 Uiso 1 1 calc R . .
C30 C 0.7081(3) 0.5743(2) 0.44715(19) 0.0360(14) Uani 1 1 d . . .
C25 C 0.8597(3) 0.5692(3) 0.48710(18) 0.0399(14) Uani 1 1 d . . .
H25 H 0.8536 0.5242 0.4881 0.048 Uiso 1 1 calc R . .
C39 C 0.8982(3) 0.8804(3) 0.5060(3) 0.058(2) Uani 1 1 d . . .
H39 H 0.9028 0.9082 0.5295 0.070 Uiso 1 1 calc R . .
C6 C 0.6274(2) 0.8118(2) 0.52827(18) 0.0310(13) Uani 1 1 d . . .
C38 C 0.8936(3) 0.8137(3) 0.5125(2) 0.0475(16) Uani 1 1 d . . .
C28 C 0.8777(2) 0.7024(3) 0.48247(18) 0.0334(13) Uani 1 1 d . . .
C10 C 0.7151(3) 0.7657(3) 0.3362(2) 0.0524(17) Uani 1 1 d . . .
H10 H 0.7368 0.7541 0.3110 0.063 Uiso 1 1 calc R . .
C31 C 0.6462(3) 0.5479(3) 0.4461(2) 0.0453(16) Uani 1 1 d . . .
H31 H 0.6251 0.5417 0.4199 0.054 Uiso 1 1 calc R . .
C11 C 0.7329(3) 0.8212(3) 0.3574(2) 0.0494(17) Uani 1 1 d . . .
H11 H 0.7662 0.8474 0.3466 0.059 Uiso 1 1 calc R . .
C37 C 0.8870(2) 0.7737(3) 0.4774(2) 0.0399(15) Uani 1 1 d . . .
C19 C 0.6862(3) 0.7196(3) 0.6239(2) 0.0462(16) Uani 1 1 d . . .
H19 H 0.6780 0.6805 0.6381 0.055 Uiso 1 1 calc R . .
C17 C 0.7487(3) 0.8158(3) 0.61699(19) 0.0420(15) Uani 1 1 d . . .
H17 H 0.7820 0.8426 0.6271 0.050 Uiso 1 1 calc R . .
C18 C 0.7349(3) 0.7594(3) 0.6378(2) 0.0484(17) Uani 1 1 d . . .
H18 H 0.7591 0.7478 0.6620 0.058 Uiso 1 1 calc R . .
C34 C 0.7083(3) 0.5657(3) 0.52335(19) 0.0420(15) Uani 1 1 d . . .
C36 C 0.7410(3) 0.5749(3) 0.56521(19) 0.0552(18) Uani 1 1 d . . .
H36A H 0.7790 0.5476 0.5666 0.083 Uiso 1 1 calc R . .
H36B H 0.7115 0.5634 0.5880 0.083 Uiso 1 1 calc R . .
H36C H 0.7537 0.6198 0.5683 0.083 Uiso 1 1 calc R . .
C32 C 0.6163(3) 0.5309(3) 0.4832(3) 0.0525(18) Uani 1 1 d . . .
H32 H 0.5744 0.5134 0.4823 0.063 Uiso 1 1 calc R . .
C40 C 0.8963(3) 0.9055(4) 0.4659(3) 0.064(2) Uani 1 1 d . . .
H40 H 0.8987 0.9505 0.4619 0.076 Uiso 1 1 calc R . .
C41 C 0.8908(3) 0.8665(3) 0.4321(3) 0.0565(19) Uani 1 1 d . . .
H41 H 0.8906 0.8844 0.4046 0.068 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Hg1 C1 2.087(5) . ?
Hg1 C23 2.101(5) . ?
C23 C24 1.387(7) . ?
C23 C28 1.414(7) . ?
C1 C2 1.400(7) . ?
C1 C6 1.408(7) . ?
C4 C3 1.380(8) . ?
C4 C5 1.395(8) . ?
C4 H4 0.9500 . ?
C29 C30 1.396(8) . ?
C29 C34 1.403(8) . ?
C29 C24 1.520(7) . ?
C24 C25 1.417(7) . ?
C22 C16 1.504(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21 C20 1.519(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C27 C26 1.392(8) . ?
C27 C28 1.408(7) . ?
C27 H27 0.9500 . ?
C14 C12 1.507(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 C8 1.519(8) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 C20 1.402(8) . ?
C15 C16 1.419(7) . ?
C15 C6 1.504(8) . ?
C43 C38 1.503(10) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C20 C19 1.403(8) . ?
C9 C10 1.375(8) . ?
C9 C8 1.391(8) . ?
C9 H9 0.9500 . ?
C16 C17 1.399(8) . ?
C35 C30 1.504(8) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C12 C11 1.396(8) . ?
C12 C7 1.423(8) . ?
C3 C2 1.410(7) . ?
C3 H3 0.9500 . ?
C8 C7 1.408(8) . ?
C26 C25 1.399(8) . ?
C26 H26 0.9500 . ?
C2 C7 1.492(8) . ?
C44 C42 1.501(9) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C5 C6 1.400(7) . ?
C5 H5 0.9500 . ?
C42 C41 1.382(8) . ?
C42 C37 1.406(9) . ?
C33 C32 1.354(9) . ?
C33 C34 1.421(9) . ?
C33 H33 0.9500 . ?
C30 C31 1.407(8) . ?
C25 H25 0.9500 . ?
C39 C40 1.377(10) . ?
C39 C38 1.412(9) . ?
C39 H39 0.9500 . ?
C38 C37 1.400(8) . ?
C28 C37 1.512(8) . ?
C10 C11 1.391(9) . ?
C10 H10 0.9500 . ?
C31 C32 1.378(9) . ?
C31 H31 0.9500 . ?
C11 H11 0.9500 . ?
C19 C18 1.387(9) . ?
C19 H19 0.9500 . ?
C17 C18 1.381(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C34 C36 1.506(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C32 H32 0.9500 . ?
C40 C41 1.352(10) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?

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
C1 Hg1 C23 177.1(2) . . ?
C24 C23 C28 120.5(5) . . ?
C24 C23 Hg1 119.8(4) . . ?
C28 C23 Hg1 119.7(4) . . ?
C2 C1 C6 119.0(5) . . ?
C2 C1 Hg1 120.6(4) . . ?
C6 C1 Hg1 120.2(4) . . ?
C3 C4 C5 120.5(5) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C30 C29 C34 119.9(5) . . ?
C30 C29 C24 119.5(5) . . ?
C34 C29 C24 120.5(5) . . ?
C23 C24 C25 120.0(5) . . ?
C23 C24 C29 120.7(5) . . ?
C25 C24 C29 119.3(5) . . ?
C16 C22 H22A 109.5 . . ?
C16 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C16 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C26 C27 C28 120.4(5) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C20 C15 C16 121.1(5) . . ?
C20 C15 C6 120.2(5) . . ?
C16 C15 C6 118.7(5) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C15 C20 C19 118.7(5) . . ?
C15 C20 C21 121.7(6) . . ?
C19 C20 C21 119.6(5) . . ?
C10 C9 C8 120.7(6) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C17 C16 C15 118.2(5) . . ?
C17 C16 C22 119.8(5) . . ?
C15 C16 C22 122.0(5) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C11 C12 C7 119.4(6) . . ?
C11 C12 C14 118.8(5) . . ?
C7 C12 C14 121.7(6) . . ?
C4 C3 C2 119.4(6) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C9 C8 C7 119.3(6) . . ?
C9 C8 C13 120.8(6) . . ?
C7 C8 C13 119.9(5) . . ?
C27 C26 C25 120.4(5) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C1 C2 C3 120.9(5) . . ?
C1 C2 C7 118.9(5) . . ?
C3 C2 C7 120.2(5) . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C4 C5 C6 120.6(5) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C8 C7 C12 119.7(6) . . ?
C8 C7 C2 121.9(5) . . ?
C12 C7 C2 118.3(5) . . ?
C41 C42 C37 120.0(6) . . ?
C41 C42 C44 120.7(7) . . ?
C37 C42 C44 119.2(5) . . ?
C32 C33 C34 121.3(6) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C29 C30 C31 119.9(6) . . ?
C29 C30 C35 120.8(5) . . ?
C31 C30 C35 119.4(5) . . ?
C26 C25 C24 119.6(5) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C40 C39 C38 120.6(7) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C5 C6 C1 119.6(5) . . ?
C5 C6 C15 122.2(5) . . ?
C1 C6 C15 118.2(5) . . ?
C37 C38 C39 118.7(7) . . ?
C37 C38 C43 119.9(6) . . ?
C39 C38 C43 121.3(6) . . ?
C27 C28 C23 119.1(5) . . ?
C27 C28 C37 120.8(5) . . ?
C23 C28 C37 120.1(5) . . ?
C9 C10 C11 121.2(6) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C32 C31 C30 119.9(6) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C10 C11 C12 119.6(6) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C38 C37 C42 119.1(6) . . ?
C38 C37 C28 121.1(6) . . ?
C42 C37 C28 119.7(5) . . ?
C18 C19 C20 120.4(6) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C18 C17 C16 120.9(6) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 120.8(6) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C29 C34 C33 118.2(6) . . ?
C29 C34 C36 120.6(6) . . ?
C33 C34 C36 121.2(6) . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C32 C31 120.8(6) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C41 C40 C39 120.4(7) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 C42 121.2(8) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 H41 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C28 C23 C24 C25 1.4(8) . . . . ?
Hg1 C23 C24 C25 -177.8(4) . . . . ?
C28 C23 C24 C29 -175.4(5) . . . . ?
Hg1 C23 C24 C29 5.3(7) . . . . ?
C30 C29 C24 C23 82.4(7) . . . . ?
C34 C29 C24 C23 -97.0(6) . . . . ?
C30 C29 C24 C25 -94.5(6) . . . . ?
C34 C29 C24 C25 86.1(7) . . . . ?
C16 C15 C20 C19 -0.6(8) . . . . ?
C6 C15 C20 C19 176.1(5) . . . . ?
C16 C15 C20 C21 -179.6(5) . . . . ?
C6 C15 C20 C21 -3.0(8) . . . . ?
C20 C15 C16 C17 -1.4(8) . . . . ?
C6 C15 C16 C17 -178.1(5) . . . . ?
C20 C15 C16 C22 178.5(5) . . . . ?
C6 C15 C16 C22 1.8(8) . . . . ?
C5 C4 C3 C2 2.0(8) . . . . ?
C10 C9 C8 C7 1.4(9) . . . . ?
C10 C9 C8 C13 -178.3(6) . . . . ?
C28 C27 C26 C25 1.2(9) . . . . ?
C6 C1 C2 C3 -1.1(7) . . . . ?
Hg1 C1 C2 C3 174.4(4) . . . . ?
C6 C1 C2 C7 179.2(5) . . . . ?
Hg1 C1 C2 C7 -5.4(6) . . . . ?
C4 C3 C2 C1 -1.0(8) . . . . ?
C4 C3 C2 C7 178.8(5) . . . . ?
C3 C4 C5 C6 -0.9(8) . . . . ?
C9 C8 C7 C12 -0.4(8) . . . . ?
C13 C8 C7 C12 179.4(5) . . . . ?
C9 C8 C7 C2 -176.1(5) . . . . ?
C13 C8 C7 C2 3.6(8) . . . . ?
C11 C12 C7 C8 -0.5(8) . . . . ?
C14 C12 C7 C8 -179.8(5) . . . . ?
C11 C12 C7 C2 175.4(5) . . . . ?
C14 C12 C7 C2 -3.9(8) . . . . ?
C1 C2 C7 C8 93.6(6) . . . . ?
C3 C2 C7 C8 -86.2(7) . . . . ?
C1 C2 C7 C12 -82.2(6) . . . . ?
C3 C2 C7 C12 98.0(6) . . . . ?
C34 C29 C30 C31 -0.9(8) . . . . ?
C24 C29 C30 C31 179.7(5) . . . . ?
C34 C29 C30 C35 179.9(5) . . . . ?
C24 C29 C30 C35 0.5(8) . . . . ?
C27 C26 C25 C24 -1.9(9) . . . . ?
C23 C24 C25 C26 0.6(8) . . . . ?
C29 C24 C25 C26 177.5(5) . . . . ?
C4 C5 C6 C1 -1.2(8) . . . . ?
C4 C5 C6 C15 177.8(5) . . . . ?
C2 C1 C6 C5 2.1(7) . . . . ?
Hg1 C1 C6 C5 -173.3(4) . . . . ?
C2 C1 C6 C15 -176.9(5) . . . . ?
Hg1 C1 C6 C15 7.7(6) . . . . ?
C20 C15 C6 C5 85.8(7) . . . . ?
C16 C15 C6 C5 -97.5(6) . . . . ?
C20 C15 C6 C1 -95.3(6) . . . . ?
C16 C15 C6 C1 81.5(6) . . . . ?
C40 C39 C38 C37 0.0(9) . . . . ?
C40 C39 C38 C43 179.9(6) . . . . ?
C26 C27 C28 C23 0.8(9) . . . . ?
C26 C27 C28 C37 -176.9(6) . . . . ?
C24 C23 C28 C27 -2.1(8) . . . . ?
Hg1 C23 C28 C27 177.1(4) . . . . ?
C24 C23 C28 C37 175.6(5) . . . . ?
Hg1 C23 C28 C37 -5.2(7) . . . . ?
C8 C9 C10 C11 -1.6(10) . . . . ?
C29 C30 C31 C32 0.6(8) . . . . ?
C35 C30 C31 C32 179.7(5) . . . . ?
C9 C10 C11 C12 0.7(10) . . . . ?
C7 C12 C11 C10 0.3(9) . . . . ?
C14 C12 C11 C10 179.6(6) . . . . ?
C39 C38 C37 C42 0.3(8) . . . . ?
C43 C38 C37 C42 -179.6(5) . . . . ?
C39 C38 C37 C28 -176.1(5) . . . . ?
C43 C38 C37 C28 4.0(8) . . . . ?
C41 C42 C37 C38 0.4(9) . . . . ?
C44 C42 C37 C38 179.2(5) . . . . ?
C41 C42 C37 C28 176.8(5) . . . . ?
C44 C42 C37 C28 -4.4(8) . . . . ?
C27 C28 C37 C38 -90.7(7) . . . . ?
C23 C28 C37 C38 91.5(7) . . . . ?
C27 C28 C37 C42 92.9(7) . . . . ?
C23 C28 C37 C42 -84.8(7) . . . . ?
C15 C20 C19 C18 2.1(9) . . . . ?
C21 C20 C19 C18 -178.9(5) . . . . ?
C15 C16 C17 C18 1.9(8) . . . . ?
C22 C16 C17 C18 -178.0(5) . . . . ?
C16 C17 C18 C19 -0.5(9) . . . . ?
C20 C19 C18 C17 -1.6(9) . . . . ?
C30 C29 C34 C33 1.1(8) . . . . ?
C24 C29 C34 C33 -179.5(5) . . . . ?
C30 C29 C34 C36 -179.5(5) . . . . ?
C24 C29 C34 C36 -0.1(8) . . . . ?
C32 C33 C34 C29 -1.0(9) . . . . ?
C32 C33 C34 C36 179.7(6) . . . . ?
C34 C33 C32 C31 0.7(9) . . . . ?
C30 C31 C32 C33 -0.4(9) . . . . ?
C38 C39 C40 C41 -1.0(10) . . . . ?
C39 C40 C41 C42 1.6(10) . . . . ?
C37 C42 C41 C40 -1.3(9) . . . . ?
C44 C42 C41 C40 179.9(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.989

_refine_diff_density_max         1.41
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.14
_database_code_depnum_ccdc_archive 'CCDC 989605'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8

#FHDLKK

_nottingham_internal_coll_name   FHDLKK
_nottingham_internal_coll_number ?
_nottingham_internal_coll_client FH/TB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '10 and 40'
_nottingham_internal_coll_frame_width 1.0
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   27/01/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 28/01/2013
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 28/01/2013
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 28/01/2013
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H42 Zn'
_chemical_formula_sum            'C44 H42 Zn'
_chemical_formula_weight         636.15

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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6431(7)
_cell_length_b                   11.2772(6)
_cell_length_c                   15.6417(7)
_cell_angle_alpha                81.846(4)
_cell_angle_beta                 87.869(4)
_cell_angle_gamma                65.639(6)
_cell_volume                     1692.47(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    13611
_cell_measurement_theta_min      4.31
_cell_measurement_theta_max      74.44


_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.069
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_max          0.152
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_T_max  1.007
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24405
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_sigmaI/netI    0.017
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.35
_diffrn_reflns_theta_max         74.65
_reflns_number_total             6784
_reflns_number_gt                6299
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.036P)²+0.825P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6784
_refine_ls_number_parameters     414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0716
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_restrained_S_all      1.03
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.243918(17) 0.607179(16) 0.230464(11) 0.01811(6) Uani 1 1 d . . .
C1 C 0.29553(13) 0.74591(12) 0.17720(8) 0.0179(2) Uani 1 1 d . . .
C2 C 0.21230(13) 0.83480(13) 0.10827(8) 0.0193(3) Uani 1 1 d . . .
C3 C 0.23321(14) 0.94638(13) 0.07433(9) 0.0234(3) Uani 1 1 d . . .
H3 H 0.1779 1.0045 0.0269 0.028 Uiso 1 1 calc R . .
C4 C 0.33519(15) 0.97220(14) 0.11014(10) 0.0267(3) Uani 1 1 d . . .
H4 H 0.3481 1.0492 0.0880 0.032 Uiso 1 1 calc R . .
C5 C 0.41856(15) 0.88591(14) 0.17827(9) 0.0248(3) Uani 1 1 d . . .
H5 H 0.4879 0.9043 0.2026 0.030 Uiso 1 1 calc R . .
C6 C 0.40061(13) 0.77205(13) 0.21112(8) 0.0203(3) Uani 1 1 d . . .
C7 C 0.10447(13) 0.80185(12) 0.07244(8) 0.0200(3) Uani 1 1 d . . .
C8 C 0.00972(13) 0.77461(13) 0.12742(9) 0.0209(3) Uani 1 1 d . . .
H8 H 0.0059 0.7901 0.1858 0.025 Uiso 1 1 calc R . .
C9 C -0.07913(14) 0.72518(13) 0.09826(9) 0.0236(3) Uani 1 1 d . . .
C10 C -0.07408(15) 0.70624(14) 0.01202(10) 0.0270(3) Uani 1 1 d . . .
H10 H -0.1329 0.6714 -0.0085 0.032 Uiso 1 1 calc R . .
C11 C 0.01520(15) 0.73720(15) -0.04503(9) 0.0279(3) Uani 1 1 d . . .
C12 C 0.10399(14) 0.78478(14) -0.01403(9) 0.0244(3) Uani 1 1 d . . .
H12 H 0.1652 0.8059 -0.0525 0.029 Uiso 1 1 calc R . .
C13 C -0.17620(16) 0.69152(16) 0.15960(11) 0.0311(3) Uani 1 1 d . . .
H13A H -0.1386 0.5962 0.1769 0.047 Uiso 1 1 calc R . .
H13B H -0.2664 0.7213 0.1308 0.047 Uiso 1 1 calc R . .
H13C H -0.1866 0.7353 0.2109 0.047 Uiso 1 1 calc R . .
C14 C 0.0153(2) 0.7207(2) -0.13911(11) 0.0420(4) Uani 1 1 d . . .
H14A H -0.0372 0.8063 -0.1733 0.063 Uiso 1 1 calc R . .
H14B H -0.0273 0.6604 -0.1462 0.063 Uiso 1 1 calc R . .
H14C H 0.1105 0.6848 -0.1590 0.063 Uiso 1 1 calc R . .
C15 C 0.49059(13) 0.67686(13) 0.28288(9) 0.0212(3) Uani 1 1 d . . .
C16 C 0.55203(14) 0.54262(14) 0.27609(9) 0.0233(3) Uani 1 1 d . . .
H16 H 0.5391 0.5132 0.2245 0.028 Uiso 1 1 calc R . .
C17 C 0.63213(14) 0.45122(14) 0.34398(10) 0.0269(3) Uani 1 1 d . . .
C18 C 0.64622(15) 0.49534(15) 0.41992(10) 0.0285(3) Uani 1 1 d . . .
H18 H 0.6988 0.4332 0.4668 0.034 Uiso 1 1 calc R . .
C19 C 0.58558(14) 0.62808(15) 0.42950(9) 0.0264(3) Uani 1 1 d . . .
C20 C 0.51047(14) 0.71794(14) 0.35950(9) 0.0234(3) Uani 1 1 d . . .
H20 H 0.4719 0.8092 0.3640 0.028 Uiso 1 1 calc R . .
C21 C 0.70246(18) 0.30720(16) 0.33460(12) 0.0381(4) Uani 1 1 d . . .
H21A H 0.6538 0.2881 0.2901 0.057 Uiso 1 1 calc R . .
H21B H 0.7010 0.2544 0.3898 0.057 Uiso 1 1 calc R . .
H21C H 0.7982 0.2855 0.3178 0.057 Uiso 1 1 calc R . .
C22 C 0.59930(17) 0.67227(18) 0.51378(10) 0.0335(3) Uani 1 1 d . . .
H22A H 0.6923 0.6685 0.5196 0.050 Uiso 1 1 calc R . .
H22B H 0.5835 0.6143 0.5618 0.050 Uiso 1 1 calc R . .
H22C H 0.5311 0.7627 0.5148 0.050 Uiso 1 1 calc R . .
C23 C 0.17315(13) 0.48814(12) 0.29431(8) 0.0172(2) Uani 1 1 d . . .
C24 C 0.22149(13) 0.35793(12) 0.27716(8) 0.0182(2) Uani 1 1 d . . .
C25 C 0.17254(14) 0.27014(13) 0.32301(8) 0.0207(3) Uani 1 1 d . . .
H25 H 0.2095 0.1810 0.3131 0.025 Uiso 1 1 calc R . .
C26 C 0.06974(14) 0.31375(13) 0.38298(8) 0.0220(3) Uani 1 1 d . . .
H26 H 0.0351 0.2547 0.4132 0.026 Uiso 1 1 calc R . .
C27 C 0.01735(14) 0.44345(13) 0.39888(8) 0.0207(3) Uani 1 1 d . . .
H27 H -0.0548 0.4734 0.4387 0.025 Uiso 1 1 calc R . .
C28 C 0.07050(13) 0.53023(12) 0.35637(8) 0.0181(2) Uani 1 1 d . . .
C29 C 0.32392(14) 0.31652(13) 0.20782(9) 0.0197(3) Uani 1 1 d . . .
C30 C 0.44567(14) 0.20279(13) 0.22184(9) 0.0230(3) Uani 1 1 d . . .
H30 H 0.4622 0.1482 0.2760 0.028 Uiso 1 1 calc R . .
C31 C 0.54358(15) 0.16775(14) 0.15769(10) 0.0267(3) Uani 1 1 d . . .
C32 C 0.51649(15) 0.24759(14) 0.07789(10) 0.0265(3) Uani 1 1 d . . .
H32 H 0.5823 0.2236 0.0337 0.032 Uiso 1 1 calc R . .
C33 C 0.39590(15) 0.36119(14) 0.06140(9) 0.0231(3) Uani 1 1 d . . .
C34 C 0.30006(14) 0.39473(13) 0.12713(9) 0.0205(3) Uani 1 1 d . . .
H34 H 0.2171 0.4721 0.1168 0.025 Uiso 1 1 calc R . .
C35 C 0.67744(17) 0.04759(16) 0.17454(12) 0.0388(4) Uani 1 1 d . . .
H35A H 0.7514 0.0742 0.1856 0.058 Uiso 1 1 calc R . .
H35B H 0.6995 0.0009 0.1240 0.058 Uiso 1 1 calc R . .
H35C H 0.6684 -0.0105 0.2250 0.058 Uiso 1 1 calc R . .
C36 C 0.36797(16) 0.44561(16) -0.02557(9) 0.0308(3) Uani 1 1 d . . .
H36A H 0.2742 0.4661 -0.0457 0.046 Uiso 1 1 calc R . .
H36B H 0.4346 0.3982 -0.0670 0.046 Uiso 1 1 calc R . .
H36C H 0.3769 0.5274 -0.0205 0.046 Uiso 1 1 calc R . .
C37 C 0.01834(14) 0.66779(13) 0.37610(8) 0.0190(3) Uani 1 1 d . . .
C38 C -0.12230(14) 0.74117(13) 0.38751(8) 0.0216(3) Uani 1 1 d . . .
H38 H -0.1852 0.7017 0.3847 0.026 Uiso 1 1 calc R . .
C39 C -0.17172(15) 0.87159(14) 0.40297(9) 0.0249(3) Uani 1 1 d . . .
C40 C -0.07922(16) 0.92993(14) 0.40360(9) 0.0271(3) Uani 1 1 d . . .
H40 H -0.1130 1.0198 0.4115 0.033 Uiso 1 1 calc R . .
C41 C 0.06090(15) 0.86014(14) 0.39302(9) 0.0249(3) Uani 1 1 d . . .
C42 C 0.10866(14) 0.72832(13) 0.38140(8) 0.0208(3) Uani 1 1 d . . .
H42 H 0.2050 0.6784 0.3770 0.025 Uiso 1 1 calc R . .
C43 C -0.32177(16) 0.94774(15) 0.42047(11) 0.0337(3) Uani 1 1 d . . .
H43A H -0.3781 0.9167 0.3894 0.050 Uiso 1 1 calc R . .
H43B H -0.3479 1.0414 0.4008 0.050 Uiso 1 1 calc R . .
H43C H -0.3370 0.9347 0.4826 0.050 Uiso 1 1 calc R . .
C44 C 0.15988(18) 0.92511(16) 0.39294(12) 0.0357(4) Uani 1 1 d . . .
H44A H 0.2353 0.8729 0.4348 0.054 Uiso 1 1 calc R . .
H44B H 0.1109 1.0136 0.4088 0.054 Uiso 1 1 calc R . .
H44C H 0.1976 0.9310 0.3352 0.054 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Zn1 C1 1.9362(13) . ?
Zn1 C23 1.9402(13) . ?
C1 C6 1.4071(18) . ?
C1 C2 1.4085(18) . ?
C2 C3 1.3954(19) . ?
C2 C7 1.4927(18) . ?
C3 C4 1.389(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3990(19) . ?
C5 H5 0.9500 . ?
C6 C15 1.4897(18) . ?
C7 C12 1.3934(19) . ?
C7 C8 1.4025(19) . ?
C8 C9 1.3972(19) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(2) . ?
C9 C13 1.509(2) . ?
C10 C11 1.394(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(2) . ?
C11 C14 1.509(2) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.397(2) . ?
C15 C16 1.398(2) . ?
C16 C17 1.396(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(2) . ?
C17 C21 1.509(2) . ?
C18 C19 1.393(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.395(2) . ?
C19 C22 1.506(2) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.4039(18) . ?
C23 C28 1.4090(18) . ?
C24 C25 1.4008(18) . ?
C24 C29 1.4895(18) . ?
C25 C26 1.3890(19) . ?
C25 H25 0.9500 . ?
C26 C27 1.3900(19) . ?
C26 H26 0.9500 . ?
C27 C28 1.4013(18) . ?
C27 H27 0.9500 . ?
C28 C37 1.4909(18) . ?
C29 C30 1.3937(19) . ?
C29 C34 1.3996(19) . ?
C30 C31 1.394(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.395(2) . ?
C31 C35 1.506(2) . ?
C32 C33 1.389(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.3981(19) . ?
C33 C36 1.508(2) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.3991(19) . ?
C37 C42 1.4000(19) . ?
C38 C39 1.397(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.392(2) . ?
C39 C43 1.505(2) . ?
C40 C41 1.386(2) . ?
C40 H40 0.9500 . ?
C41 C42 1.3955(19) . ?
C41 C44 1.511(2) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

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
C1 Zn1 C23 171.18(5) . . ?
C6 C1 C2 118.46(12) . . ?
C6 C1 Zn1 122.93(10) . . ?
C2 C1 Zn1 118.07(9) . . ?
C3 C2 C1 120.90(12) . . ?
C3 C2 C7 122.18(12) . . ?
C1 C2 C7 116.90(11) . . ?
C4 C3 C2 119.76(12) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.34(13) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.21(13) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 120.28(12) . . ?
C5 C6 C15 121.12(12) . . ?
C1 C6 C15 118.59(12) . . ?
C12 C7 C8 118.49(12) . . ?
C12 C7 C2 121.01(12) . . ?
C8 C7 C2 120.20(12) . . ?
C9 C8 C7 121.48(13) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 118.30(13) . . ?
C10 C9 C13 121.24(13) . . ?
C8 C9 C13 120.46(13) . . ?
C9 C10 C11 121.57(13) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C12 C11 C10 118.97(13) . . ?
C12 C11 C14 120.28(14) . . ?
C10 C11 C14 120.75(14) . . ?
C7 C12 C11 121.12(13) . . ?
C7 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 118.54(13) . . ?
C20 C15 C6 121.34(12) . . ?
C16 C15 C6 120.06(12) . . ?
C17 C16 C15 120.99(13) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C16 118.79(14) . . ?
C18 C17 C21 120.71(14) . . ?
C16 C17 C21 120.50(14) . . ?
C17 C18 C19 121.92(13) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
C18 C19 C20 118.14(13) . . ?
C18 C19 C22 120.56(13) . . ?
C20 C19 C22 121.29(14) . . ?
C19 C20 C15 121.55(13) . . ?
C19 C20 H20 119.2 . . ?
C15 C20 H20 119.2 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 118.63(11) . . ?
C24 C23 Zn1 119.87(9) . . ?
C28 C23 Zn1 121.47(9) . . ?
C25 C24 C23 120.77(12) . . ?
C25 C24 C29 120.96(12) . . ?
C23 C24 C29 118.26(11) . . ?
C26 C25 C24 119.83(12) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 120.22(12) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 120.29(12) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C27 C28 C23 120.16(12) . . ?
C27 C28 C37 120.28(11) . . ?
C23 C28 C37 119.56(11) . . ?
C30 C29 C34 118.71(12) . . ?
C30 C29 C24 121.57(12) . . ?
C34 C29 C24 119.70(12) . . ?
C29 C30 C31 121.14(13) . . ?
C29 C30 H30 119.4 . . ?
C31 C30 H30 119.4 . . ?
C30 C31 C32 118.72(13) . . ?
C30 C31 C35 120.82(14) . . ?
C32 C31 C35 120.45(13) . . ?
C33 C32 C31 121.73(13) . . ?
C33 C32 H32 119.1 . . ?
C31 C32 H32 119.1 . . ?
C32 C33 C34 118.38(13) . . ?
C32 C33 C36 120.93(13) . . ?
C34 C33 C36 120.69(13) . . ?
C33 C34 C29 121.31(13) . . ?
C33 C34 H34 119.3 . . ?
C29 C34 H34 119.3 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C42 118.14(12) . . ?
C38 C37 C28 121.08(12) . . ?
C42 C37 C28 120.75(12) . . ?
C39 C38 C37 121.06(13) . . ?
C39 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C40 C39 C38 118.90(13) . . ?
C40 C39 C43 120.16(13) . . ?
C38 C39 C43 120.93(13) . . ?
C41 C40 C39 121.62(13) . . ?
C41 C40 H40 119.2 . . ?
C39 C40 H40 119.2 . . ?
C40 C41 C42 118.42(13) . . ?
C40 C41 C44 121.03(13) . . ?
C42 C41 C44 120.54(13) . . ?
C41 C42 C37 121.72(13) . . ?
C41 C42 H42 119.1 . . ?
C37 C42 H42 119.1 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.07(19) . . . . ?
Zn1 C1 C2 C3 171.79(10) . . . . ?
C6 C1 C2 C7 178.38(11) . . . . ?
Zn1 C1 C2 C7 -9.75(16) . . . . ?
C1 C2 C3 C4 -1.5(2) . . . . ?
C7 C2 C3 C4 -179.92(13) . . . . ?
C2 C3 C4 C5 1.5(2) . . . . ?
C3 C4 C5 C6 0.2(2) . . . . ?
C4 C5 C6 C1 -1.9(2) . . . . ?
C4 C5 C6 C15 178.75(13) . . . . ?
C2 C1 C6 C5 1.77(19) . . . . ?
Zn1 C1 C6 C5 -169.68(10) . . . . ?
C2 C1 C6 C15 -178.82(12) . . . . ?
Zn1 C1 C6 C15 9.74(17) . . . . ?
C3 C2 C7 C12 57.89(18) . . . . ?
C1 C2 C7 C12 -120.55(14) . . . . ?
C3 C2 C7 C8 -128.50(14) . . . . ?
C1 C2 C7 C8 53.07(17) . . . . ?
C12 C7 C8 C9 3.16(19) . . . . ?
C2 C7 C8 C9 -170.61(12) . . . . ?
C7 C8 C9 C10 -1.5(2) . . . . ?
C7 C8 C9 C13 177.53(13) . . . . ?
C8 C9 C10 C11 -1.0(2) . . . . ?
C13 C9 C10 C11 179.94(14) . . . . ?
C9 C10 C11 C12 1.8(2) . . . . ?
C9 C10 C11 C14 -177.67(15) . . . . ?
C8 C7 C12 C11 -2.3(2) . . . . ?
C2 C7 C12 C11 171.41(13) . . . . ?
C10 C11 C12 C7 -0.1(2) . . . . ?
C14 C11 C12 C7 179.37(14) . . . . ?
C5 C6 C15 C20 51.89(19) . . . . ?
C1 C6 C15 C20 -127.52(14) . . . . ?
C5 C6 C15 C16 -131.13(14) . . . . ?
C1 C6 C15 C16 49.46(18) . . . . ?
C20 C15 C16 C17 -0.3(2) . . . . ?
C6 C15 C16 C17 -177.37(12) . . . . ?
C15 C16 C17 C18 2.1(2) . . . . ?
C15 C16 C17 C21 -177.60(13) . . . . ?
C16 C17 C18 C19 -1.5(2) . . . . ?
C21 C17 C18 C19 178.21(14) . . . . ?
C17 C18 C19 C20 -0.9(2) . . . . ?
C17 C18 C19 C22 178.12(13) . . . . ?
C18 C19 C20 C15 2.8(2) . . . . ?
C22 C19 C20 C15 -176.19(13) . . . . ?
C16 C15 C20 C19 -2.2(2) . . . . ?
C6 C15 C20 C19 174.79(12) . . . . ?
C28 C23 C24 C25 -2.34(18) . . . . ?
Zn1 C23 C24 C25 179.49(10) . . . . ?
C28 C23 C24 C29 176.45(11) . . . . ?
Zn1 C23 C24 C29 -1.72(16) . . . . ?
C23 C24 C25 C26 3.41(19) . . . . ?
C29 C24 C25 C26 -175.35(12) . . . . ?
C24 C25 C26 C27 -1.3(2) . . . . ?
C25 C26 C27 C28 -1.8(2) . . . . ?
C26 C27 C28 C23 2.86(19) . . . . ?
C26 C27 C28 C37 -177.47(12) . . . . ?
C24 C23 C28 C27 -0.78(18) . . . . ?
Zn1 C23 C28 C27 177.36(9) . . . . ?
C24 C23 C28 C37 179.55(11) . . . . ?
Zn1 C23 C28 C37 -2.31(16) . . . . ?
C25 C24 C29 C30 -51.23(18) . . . . ?
C23 C24 C29 C30 129.98(13) . . . . ?
C25 C24 C29 C34 130.46(13) . . . . ?
C23 C24 C29 C34 -48.33(17) . . . . ?
C34 C29 C30 C31 1.0(2) . . . . ?
C24 C29 C30 C31 -177.29(13) . . . . ?
C29 C30 C31 C32 -1.2(2) . . . . ?
C29 C30 C31 C35 177.53(14) . . . . ?
C30 C31 C32 C33 0.8(2) . . . . ?
C35 C31 C32 C33 -177.96(14) . . . . ?
C31 C32 C33 C34 -0.2(2) . . . . ?
C31 C32 C33 C36 -179.48(14) . . . . ?
C32 C33 C34 C29 0.0(2) . . . . ?
C36 C33 C34 C29 179.28(13) . . . . ?
C30 C29 C34 C33 -0.4(2) . . . . ?
C24 C29 C34 C33 177.95(12) . . . . ?
C27 C28 C37 C38 -41.27(18) . . . . ?
C23 C28 C37 C38 138.39(13) . . . . ?
C27 C28 C37 C42 140.47(13) . . . . ?
C23 C28 C37 C42 -39.86(17) . . . . ?
C42 C37 C38 C39 0.58(19) . . . . ?
C28 C37 C38 C39 -177.72(12) . . . . ?
C37 C38 C39 C40 2.5(2) . . . . ?
C37 C38 C39 C43 -176.33(13) . . . . ?
C38 C39 C40 C41 -2.8(2) . . . . ?
C43 C39 C40 C41 175.98(14) . . . . ?
C39 C40 C41 C42 0.1(2) . . . . ?
C39 C40 C41 C44 179.38(14) . . . . ?
C40 C41 C42 C37 3.1(2) . . . . ?
C44 C41 C42 C37 -176.17(13) . . . . ?
C38 C37 C42 C41 -3.44(19) . . . . ?
C28 C37 C42 C41 174.87(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        67.50
_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         0.30
_refine_diff_density_min         -0.26
_refine_diff_density_rms         0.04
_database_code_depnum_ccdc_archive 'CCDC 989606'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_9

#FHDLKJ

_nottingham_internal_coll_name   FHDLKJ
_nottingham_internal_coll_number 12112
_nottingham_internal_coll_client FH/TB/DLK
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time 1
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   08/12/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 08/12/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 26/01/2013
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 26/01/2013
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?


_audit_creation_method           SHELXL97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H42 Cd'
_chemical_formula_sum            'C44 H42 Cd'
_chemical_formula_weight         683.18

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.748(3)
_cell_length_b                   12.914(4)
_cell_length_c                   13.331(4)
_cell_angle_alpha                76.688(4)
_cell_angle_beta                 83.692(4)
_cell_angle_gamma                78.257(4)
_cell_volume                     1759.1(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    8922
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.79

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.46
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_max          0.85
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             708
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11908
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.03
_reflns_number_total             6047
_reflns_number_gt                5309
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ' ? '
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.033P)²+1.079P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6047
_refine_ls_number_parameters     414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0702
_refine_ls_wR_factor_gt          0.0678
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_restrained_S_all      1.06
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Cd1 Cd 0.741385(17) 0.183432(15) 0.236679(14) 0.01988(7) Uani 1 1 d . . .
C1 C 0.6247(2) 0.0790(2) 0.21178(19) 0.0209(5) Uani 1 1 d . . .
C2 C 0.5456(2) 0.1083(2) 0.12883(19) 0.0215(5) Uani 1 1 d . . .
C3 C 0.4632(2) 0.0408(2) 0.1191(2) 0.0251(6) Uani 1 1 d . . .
H3 H 0.4088 0.0615 0.0635 0.030 Uiso 1 1 calc R . .
C4 C 0.4601(2) -0.0559(2) 0.1894(2) 0.0288(6) Uani 1 1 d . . .
H4 H 0.4049 -0.1019 0.1814 0.035 Uiso 1 1 calc R . .
C5 C 0.5375(2) -0.0855(2) 0.2715(2) 0.0266(6) Uani 1 1 d . . .
H5 H 0.5349 -0.1518 0.3201 0.032 Uiso 1 1 calc R . .
C6 C 0.6193(2) -0.0188(2) 0.28349(19) 0.0212(5) Uani 1 1 d . . .
C7 C 0.5479(2) 0.2113(2) 0.05136(19) 0.0208(5) Uani 1 1 d . . .
C8 C 0.6618(2) 0.2375(2) 0.00066(19) 0.0240(6) Uani 1 1 d . . .
H8 H 0.7395 0.1885 0.0163 0.029 Uiso 1 1 calc R . .
C9 C 0.6643(3) 0.3335(2) -0.0721(2) 0.0273(6) Uani 1 1 d . . .
C10 C 0.5503(3) 0.4051(2) -0.0929(2) 0.0272(6) Uani 1 1 d . . .
H10 H 0.5513 0.4712 -0.1419 0.033 Uiso 1 1 calc R . .
C11 C 0.4347(3) 0.3826(2) -0.0439(2) 0.0267(6) Uani 1 1 d . . .
C12 C 0.4348(2) 0.2849(2) 0.02777(19) 0.0238(6) Uani 1 1 d . . .
H12 H 0.3564 0.2681 0.0612 0.029 Uiso 1 1 calc R . .
C13 C 0.7881(3) 0.3604(2) -0.1283(2) 0.0387(7) Uani 1 1 d . . .
H13A H 0.8070 0.3269 -0.1885 0.058 Uiso 1 1 calc R . .
H13B H 0.8574 0.3325 -0.0816 0.058 Uiso 1 1 calc R . .
H13C H 0.7799 0.4391 -0.1511 0.058 Uiso 1 1 calc R . .
C14 C 0.3127(3) 0.4621(2) -0.0676(2) 0.0351(7) Uani 1 1 d . . .
H14A H 0.2806 0.4523 -0.1301 0.053 Uiso 1 1 calc R . .
H14B H 0.3288 0.5361 -0.0785 0.053 Uiso 1 1 calc R . .
H14C H 0.2493 0.4497 -0.0095 0.053 Uiso 1 1 calc R . .
C15 C 0.7049(2) -0.0516(2) 0.37062(19) 0.0221(5) Uani 1 1 d . . .
C16 C 0.7053(2) 0.0170(2) 0.4377(2) 0.0248(6) Uani 1 1 d . . .
H16 H 0.6456 0.0831 0.4309 0.030 Uiso 1 1 calc R . .
C17 C 0.7918(3) -0.0098(2) 0.5143(2) 0.0287(6) Uani 1 1 d . . .
C18 C 0.8782(3) -0.1071(2) 0.5231(2) 0.0315(6) Uani 1 1 d . . .
H18 H 0.9383 -0.1256 0.5745 0.038 Uiso 1 1 calc R . .
C19 C 0.8789(2) -0.1778(2) 0.4591(2) 0.0293(6) Uani 1 1 d . . .
C20 C 0.7908(2) -0.1494(2) 0.3833(2) 0.0258(6) Uani 1 1 d . . .
H20 H 0.7896 -0.1977 0.3395 0.031 Uiso 1 1 calc R . .
C21 C 0.7906(3) 0.0643(3) 0.5870(2) 0.0384(7) Uani 1 1 d . . .
H21A H 0.7633 0.0293 0.6570 0.058 Uiso 1 1 calc R . .
H21B H 0.7314 0.1323 0.5644 0.058 Uiso 1 1 calc R . .
H21C H 0.8764 0.0793 0.5869 0.058 Uiso 1 1 calc R . .
C22 C 0.9732(3) -0.2838(3) 0.4690(3) 0.0422(8) Uani 1 1 d . . .
H22A H 0.9269 -0.3441 0.4827 0.063 Uiso 1 1 calc R . .
H22B H 1.0269 -0.2918 0.5262 0.063 Uiso 1 1 calc R . .
H22C H 1.0268 -0.2840 0.4046 0.063 Uiso 1 1 calc R . .
C23 C 0.8427(2) 0.30177(19) 0.25743(19) 0.0204(5) Uani 1 1 d . . .
C24 C 0.9619(2) 0.3101(2) 0.20567(19) 0.0216(5) Uani 1 1 d . . .
C25 C 1.0222(2) 0.3949(2) 0.2105(2) 0.0262(6) Uani 1 1 d . . .
H25 H 1.1025 0.4007 0.1740 0.031 Uiso 1 1 calc R . .
C26 C 0.9655(2) 0.4704(2) 0.2682(2) 0.0270(6) Uani 1 1 d . . .
H26 H 1.0065 0.5283 0.2708 0.032 Uiso 1 1 calc R . .
C27 C 0.8485(2) 0.4617(2) 0.3223(2) 0.0238(6) Uani 1 1 d . . .
H27 H 0.8103 0.5130 0.3627 0.029 Uiso 1 1 calc R . .
C28 C 0.7871(2) 0.37810(19) 0.31741(19) 0.0200(5) Uani 1 1 d . . .
C29 C 1.0241(2) 0.2281(2) 0.1442(2) 0.0232(6) Uani 1 1 d . . .
C30 C 1.0789(2) 0.2588(2) 0.0448(2) 0.0264(6) Uani 1 1 d . . .
H30 H 1.0785 0.3334 0.0162 0.032 Uiso 1 1 calc R . .
C31 C 1.1342(2) 0.1828(2) -0.0134(2) 0.0286(6) Uani 1 1 d . . .
C32 C 1.1337(2) 0.0740(2) 0.0288(2) 0.0292(6) Uani 1 1 d . . .
H32 H 1.1708 0.0218 -0.0109 0.035 Uiso 1 1 calc R . .
C33 C 1.0805(2) 0.0395(2) 0.1277(2) 0.0267(6) Uani 1 1 d . . .
C34 C 1.0273(2) 0.1172(2) 0.1846(2) 0.0246(6) Uani 1 1 d . . .
H34 H 0.9920 0.0947 0.2528 0.029 Uiso 1 1 calc R . .
C35 C 1.1936(3) 0.2172(3) -0.1204(2) 0.0402(7) Uani 1 1 d . . .
H35A H 1.1334 0.2749 -0.1609 0.060 Uiso 1 1 calc R . .
H35B H 1.2146 0.1552 -0.1538 0.060 Uiso 1 1 calc R . .
H35C H 1.2714 0.2441 -0.1160 0.060 Uiso 1 1 calc R . .
C36 C 1.0814(3) -0.0789(2) 0.1723(2) 0.0326(7) Uani 1 1 d . . .
H36A H 1.1661 -0.1141 0.1957 0.049 Uiso 1 1 calc R . .
H36B H 1.0607 -0.1130 0.1192 0.049 Uiso 1 1 calc R . .
H36C H 1.0180 -0.0868 0.2309 0.049 Uiso 1 1 calc R . .
C37 C 0.6633(2) 0.36767(19) 0.3771(2) 0.0209(5) Uani 1 1 d . . .
C38 C 0.6480(2) 0.37231(19) 0.4813(2) 0.0228(6) Uani 1 1 d . . .
H38 H 0.7163 0.3858 0.5129 0.027 Uiso 1 1 calc R . .
C39 C 0.5348(3) 0.35759(19) 0.5402(2) 0.0260(6) Uani 1 1 d . . .
C40 C 0.4358(3) 0.3380(2) 0.4925(2) 0.0283(6) Uani 1 1 d . . .
H40 H 0.3587 0.3268 0.5321 0.034 Uiso 1 1 calc R . .
C41 C 0.4464(2) 0.3343(2) 0.3882(2) 0.0271(6) Uani 1 1 d . . .
C42 C 0.5599(2) 0.35049(19) 0.3315(2) 0.0237(6) Uani 1 1 d . . .
H42 H 0.5677 0.3499 0.2599 0.028 Uiso 1 1 calc R . .
C43 C 0.5231(3) 0.3627(2) 0.6528(2) 0.0331(7) Uani 1 1 d . . .
H43A H 0.5845 0.3036 0.6904 0.050 Uiso 1 1 calc R . .
H43B H 0.4366 0.3556 0.6816 0.050 Uiso 1 1 calc R . .
H43C H 0.5406 0.4323 0.6596 0.050 Uiso 1 1 calc R . .
C44 C 0.3376(3) 0.3139(3) 0.3368(3) 0.0426(8) Uani 1 1 d . . .
H44A H 0.3227 0.2402 0.3661 0.064 Uiso 1 1 calc R . .
H44B H 0.3592 0.3222 0.2624 0.064 Uiso 1 1 calc R . .
H44C H 0.2604 0.3661 0.3487 0.064 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Cd1 C1 2.119(2) . ?
Cd1 C23 2.130(2) . ?
C1 C2 1.404(3) . ?
C1 C6 1.405(3) . ?
C2 C3 1.398(3) . ?
C2 C7 1.487(3) . ?
C3 C4 1.382(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(4) . ?
C5 H5 0.9500 . ?
C6 C15 1.491(3) . ?
C7 C8 1.397(4) . ?
C7 C12 1.399(4) . ?
C8 C9 1.390(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(4) . ?
C9 C13 1.517(4) . ?
C10 C11 1.391(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.397(4) . ?
C11 C14 1.506(4) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.393(4) . ?
C15 C16 1.397(4) . ?
C16 C17 1.394(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(4) . ?
C17 C21 1.507(4) . ?
C18 C19 1.385(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(4) . ?
C19 C22 1.517(4) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.398(3) . ?
C23 C28 1.409(3) . ?
C24 C25 1.398(4) . ?
C24 C29 1.494(4) . ?
C25 C26 1.384(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.391(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(3) . ?
C27 H27 0.9500 . ?
C28 C37 1.487(3) . ?
C29 C30 1.393(4) . ?
C29 C34 1.403(4) . ?
C30 C31 1.390(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(4) . ?
C31 C35 1.503(4) . ?
C32 C33 1.390(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.390(4) . ?
C33 C36 1.506(4) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.394(4) . ?
C37 C42 1.401(4) . ?
C38 C39 1.396(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.391(4) . ?
C39 C43 1.508(4) . ?
C40 C41 1.394(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.390(4) . ?
C41 C44 1.513(4) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

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
C1 Cd1 C23 174.10(9) . . ?
C2 C1 C6 118.8(2) . . ?
C2 C1 Cd1 121.54(18) . . ?
C6 C1 Cd1 119.51(18) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 C7 119.5(2) . . ?
C1 C2 C7 120.6(2) . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.8(2) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 120.4(2) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 120.3(2) . . ?
C5 C6 C15 120.6(2) . . ?
C1 C6 C15 119.1(2) . . ?
C8 C7 C12 118.3(2) . . ?
C8 C7 C2 121.4(2) . . ?
C12 C7 C2 120.3(2) . . ?
C9 C8 C7 121.6(2) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C10 C9 C8 118.6(2) . . ?
C10 C9 C13 120.2(2) . . ?
C8 C9 C13 121.3(2) . . ?
C9 C10 C11 121.8(2) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C12 118.4(2) . . ?
C10 C11 C14 120.7(2) . . ?
C12 C11 C14 120.9(2) . . ?
C11 C12 C7 121.3(2) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 118.7(2) . . ?
C20 C15 C6 120.2(2) . . ?
C16 C15 C6 121.0(2) . . ?
C17 C16 C15 121.2(2) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C18 C17 C16 118.5(3) . . ?
C18 C17 C21 120.7(2) . . ?
C16 C17 C21 120.7(3) . . ?
C19 C18 C17 121.8(3) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 118.6(3) . . ?
C18 C19 C22 121.6(3) . . ?
C20 C19 C22 119.8(3) . . ?
C15 C20 C19 121.2(3) . . ?
C15 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 118.7(2) . . ?
C24 C23 Cd1 120.47(18) . . ?
C28 C23 Cd1 120.64(17) . . ?
C23 C24 C25 120.5(2) . . ?
C23 C24 C29 119.5(2) . . ?
C25 C24 C29 120.0(2) . . ?
C26 C25 C24 120.2(2) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C27 120.0(2) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 120.2(2) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C27 C28 C23 120.3(2) . . ?
C27 C28 C37 120.1(2) . . ?
C23 C28 C37 119.6(2) . . ?
C30 C29 C34 117.9(2) . . ?
C30 C29 C24 121.4(2) . . ?
C34 C29 C24 120.7(2) . . ?
C31 C30 C29 121.5(2) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C32 C31 C30 118.8(3) . . ?
C32 C31 C35 120.4(3) . . ?
C30 C31 C35 120.8(3) . . ?
C31 C32 C33 121.8(3) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C32 C33 C34 118.1(2) . . ?
C32 C33 C36 120.9(2) . . ?
C34 C33 C36 121.0(2) . . ?
C33 C34 C29 121.9(2) . . ?
C33 C34 H34 119.0 . . ?
C29 C34 H34 119.0 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C42 118.0(2) . . ?
C38 C37 C28 120.6(2) . . ?
C42 C37 C28 121.4(2) . . ?
C37 C38 C39 121.7(2) . . ?
C37 C38 H38 119.2 . . ?
C39 C38 H38 119.2 . . ?
C40 C39 C38 118.3(2) . . ?
C40 C39 C43 121.9(2) . . ?
C38 C39 C43 119.7(2) . . ?
C39 C40 C41 121.8(2) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 H40 119.1 . . ?
C42 C41 C40 118.3(2) . . ?
C42 C41 C44 120.3(3) . . ?
C40 C41 C44 121.4(2) . . ?
C41 C42 C37 121.8(3) . . ?
C41 C42 H42 119.1 . . ?
C37 C42 H42 119.1 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.2(4) . . . . ?
Cd1 C1 C2 C3 -175.44(19) . . . . ?
C6 C1 C2 C7 179.8(2) . . . . ?
Cd1 C1 C2 C7 4.1(3) . . . . ?
C1 C2 C3 C4 -1.1(4) . . . . ?
C7 C2 C3 C4 179.3(2) . . . . ?
C2 C3 C4 C5 1.2(4) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C4 C5 C6 C1 -0.5(4) . . . . ?
C4 C5 C6 C15 -178.7(2) . . . . ?
C2 C1 C6 C5 0.5(4) . . . . ?
Cd1 C1 C6 C5 176.30(19) . . . . ?
C2 C1 C6 C15 178.8(2) . . . . ?
Cd1 C1 C6 C15 -5.5(3) . . . . ?
C3 C2 C7 C8 -128.1(3) . . . . ?
C1 C2 C7 C8 52.3(3) . . . . ?
C3 C2 C7 C12 52.2(3) . . . . ?
C1 C2 C7 C12 -127.4(3) . . . . ?
C12 C7 C8 C9 -0.5(4) . . . . ?
C2 C7 C8 C9 179.8(2) . . . . ?
C7 C8 C9 C10 1.0(4) . . . . ?
C7 C8 C9 C13 -178.8(3) . . . . ?
C8 C9 C10 C11 -0.7(4) . . . . ?
C13 C9 C10 C11 179.1(3) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C9 C10 C11 C14 179.6(2) . . . . ?
C10 C11 C12 C7 0.8(4) . . . . ?
C14 C11 C12 C7 -179.1(2) . . . . ?
C8 C7 C12 C11 -0.4(4) . . . . ?
C2 C7 C12 C11 179.3(2) . . . . ?
C5 C6 C15 C20 56.8(3) . . . . ?
C1 C6 C15 C20 -121.4(3) . . . . ?
C5 C6 C15 C16 -126.5(3) . . . . ?
C1 C6 C15 C16 55.2(3) . . . . ?
C20 C15 C16 C17 1.6(4) . . . . ?
C6 C15 C16 C17 -175.1(2) . . . . ?
C15 C16 C17 C18 -0.2(4) . . . . ?
C15 C16 C17 C21 -179.3(2) . . . . ?
C16 C17 C18 C19 -0.9(4) . . . . ?
C21 C17 C18 C19 178.2(3) . . . . ?
C17 C18 C19 C20 0.6(4) . . . . ?
C17 C18 C19 C22 -180.0(3) . . . . ?
C16 C15 C20 C19 -2.0(4) . . . . ?
C6 C15 C20 C19 174.8(2) . . . . ?
C18 C19 C20 C15 0.9(4) . . . . ?
C22 C19 C20 C15 -178.6(2) . . . . ?
C28 C23 C24 C25 -2.3(4) . . . . ?
Cd1 C23 C24 C25 173.12(18) . . . . ?
C28 C23 C24 C29 178.3(2) . . . . ?
Cd1 C23 C24 C29 -6.3(3) . . . . ?
C23 C24 C25 C26 1.2(4) . . . . ?
C29 C24 C25 C26 -179.4(2) . . . . ?
C24 C25 C26 C27 0.5(4) . . . . ?
C25 C26 C27 C28 -1.0(4) . . . . ?
C26 C27 C28 C23 -0.2(4) . . . . ?
C26 C27 C28 C37 178.7(2) . . . . ?
C24 C23 C28 C27 1.8(4) . . . . ?
Cd1 C23 C28 C27 -173.60(18) . . . . ?
C24 C23 C28 C37 -177.1(2) . . . . ?
Cd1 C23 C28 C37 7.5(3) . . . . ?
C23 C24 C29 C30 133.8(3) . . . . ?
C25 C24 C29 C30 -45.7(3) . . . . ?
C23 C24 C29 C34 -45.3(3) . . . . ?
C25 C24 C29 C34 135.3(2) . . . . ?
C34 C29 C30 C31 0.6(4) . . . . ?
C24 C29 C30 C31 -178.5(2) . . . . ?
C29 C30 C31 C32 0.3(4) . . . . ?
C29 C30 C31 C35 -179.7(2) . . . . ?
C30 C31 C32 C33 -0.5(4) . . . . ?
C35 C31 C32 C33 179.5(2) . . . . ?
C31 C32 C33 C34 -0.2(4) . . . . ?
C31 C32 C33 C36 -179.8(2) . . . . ?
C32 C33 C34 C29 1.2(4) . . . . ?
C36 C33 C34 C29 -179.3(2) . . . . ?
C30 C29 C34 C33 -1.4(4) . . . . ?
C24 C29 C34 C33 177.7(2) . . . . ?
C27 C28 C37 C38 -48.4(3) . . . . ?
C23 C28 C37 C38 130.5(2) . . . . ?
C27 C28 C37 C42 133.0(3) . . . . ?
C23 C28 C37 C42 -48.1(3) . . . . ?
C42 C37 C38 C39 1.7(4) . . . . ?
C28 C37 C38 C39 -176.9(2) . . . . ?
C37 C38 C39 C40 -0.1(4) . . . . ?
C37 C38 C39 C43 179.6(2) . . . . ?
C38 C39 C40 C41 -0.9(4) . . . . ?
C43 C39 C40 C41 179.4(2) . . . . ?
C39 C40 C41 C42 0.2(4) . . . . ?
C39 C40 C41 C44 -179.5(3) . . . . ?
C40 C41 C42 C37 1.5(4) . . . . ?
C44 C41 C42 C37 -178.9(2) . . . . ?
C38 C37 C42 C41 -2.4(4) . . . . ?
C28 C37 C42 C41 176.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.973

_refine_diff_density_max         0.50
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.06
_database_code_depnum_ccdc_archive 'CCDC 989607'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_10

#FHDLKI

_nottingham_internal_coll_name   FHDLKI
_nottingham_internal_coll_number 12090
_nottingham_internal_coll_client FH/DLK
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time 30
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   08/12/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 13/12/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 21/12/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 21/12/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 13/2/2013
_nottingham_internal_archive_date ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H42 Hg'
_chemical_formula_sum            'C44 H42 Hg'
_chemical_formula_weight         771.37

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'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.688(2)
_cell_length_b                   12.974(3)
_cell_length_c                   13.401(3)
_cell_angle_alpha                76.323(3)
_cell_angle_beta                 83.448(3)
_cell_angle_gamma                78.253(3)
_cell_volume                     1763.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2336
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      26.83

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.07
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_max          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    4.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.311
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15701
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.097
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         27.55
_reflns_number_total             7950
_reflns_number_gt                5875
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0442P)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7950
_refine_ls_number_parameters     414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.106
_refine_ls_wR_factor_gt          0.097
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_restrained_S_all      0.98
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Hg1 Hg 0.26391(2) 0.81291(2) 0.26477(2) 0.03317(9) Uani 1 1 d . . .
C1 C 0.3749(6) 0.9194(5) 0.2887(5) 0.0341(15) Uani 1 1 d . . .
C2 C 0.4534(6) 0.8913(5) 0.3712(5) 0.0370(16) Uani 1 1 d . . .
C3 C 0.5344(6) 0.9595(5) 0.3808(5) 0.0381(16) Uani 1 1 d . . .
H3 H 0.5900 0.9391 0.4354 0.046 Uiso 1 1 calc R . .
C4 C 0.5338(6) 1.0562(6) 0.3112(5) 0.0413(17) Uani 1 1 d . . .
H4 H 0.5864 1.1038 0.3199 0.050 Uiso 1 1 calc R . .
C5 C 0.4580(6) 1.0847(5) 0.2292(5) 0.0406(17) Uani 1 1 d . . .
H5 H 0.4608 1.1508 0.1807 0.049 Uiso 1 1 calc R . .
C6 C 0.3773(6) 1.0179(5) 0.2164(5) 0.0335(15) Uani 1 1 d . . .
C7 C 0.4537(6) 0.7872(5) 0.4484(5) 0.0331(15) Uani 1 1 d . . .
C8 C 0.5664(6) 0.7135(5) 0.4693(5) 0.0338(15) Uani 1 1 d . . .
H8 H 0.6447 0.7296 0.4340 0.041 Uiso 1 1 calc R . .
C9 C 0.5669(7) 0.6166(5) 0.5408(5) 0.0370(16) Uani 1 1 d . . .
C10 C 0.4515(7) 0.5952(5) 0.5938(5) 0.0399(17) Uani 1 1 d . . .
H10 H 0.4517 0.5297 0.6439 0.048 Uiso 1 1 calc R . .
C11 C 0.3381(7) 0.6658(5) 0.5760(5) 0.0383(16) Uani 1 1 d . . .
C12 C 0.3395(6) 0.7628(5) 0.5011(5) 0.0356(16) Uani 1 1 d . . .
H12 H 0.2615 0.8121 0.4866 0.043 Uiso 1 1 calc R . .
C13 C 0.6911(7) 0.5354(6) 0.5629(6) 0.049(2) Uani 1 1 d . . .
H13A H 0.7555 0.5503 0.5059 0.074 Uiso 1 1 calc R . .
H13B H 0.6749 0.4622 0.5704 0.074 Uiso 1 1 calc R . .
H13C H 0.7226 0.5416 0.6268 0.074 Uiso 1 1 calc R . .
C14 C 0.2152(7) 0.6395(6) 0.6343(6) 0.0496(19) Uani 1 1 d . . .
H14A H 0.2021 0.6675 0.6972 0.074 Uiso 1 1 calc R . .
H14B H 0.2204 0.5611 0.6523 0.074 Uiso 1 1 calc R . .
H14C H 0.1433 0.6729 0.5911 0.074 Uiso 1 1 calc R . .
C15 C 0.2912(6) 1.0503(5) 0.1304(5) 0.0375(16) Uani 1 1 d . . .
C16 C 0.2028(6) 1.1466(6) 0.1183(5) 0.0411(17) Uani 1 1 d . . .
H16 H 0.2021 1.1938 0.1629 0.049 Uiso 1 1 calc R . .
C17 C 0.1166(7) 1.1749(6) 0.0439(6) 0.0427(18) Uani 1 1 d . . .
C18 C 0.1204(7) 1.1079(6) -0.0226(6) 0.0478(19) Uani 1 1 d . . .
H18 H 0.0601 1.1274 -0.0738 0.057 Uiso 1 1 calc R . .
C19 C 0.2099(7) 1.0122(6) -0.0174(5) 0.0420(17) Uani 1 1 d . . .
C20 C 0.2963(6) 0.9849(6) 0.0595(5) 0.0408(17) Uani 1 1 d . . .
H20 H 0.3594 0.9211 0.0640 0.049 Uiso 1 1 calc R . .
C21 C 0.0186(8) 1.2777(7) 0.0356(7) 0.066(2) Uani 1 1 d . . .
H21A H -0.0280 1.2795 0.1027 0.099 Uiso 1 1 calc R . .
H21B H -0.0418 1.2806 -0.0152 0.099 Uiso 1 1 calc R . .
H21C H 0.0619 1.3399 0.0138 0.099 Uiso 1 1 calc R . .
C22 C 0.2132(8) 0.9408(6) -0.0908(6) 0.055(2) Uani 1 1 d . . .
H22A H 0.1264 0.9292 -0.0951 0.083 Uiso 1 1 calc R . .
H22B H 0.2688 0.8713 -0.0664 0.083 Uiso 1 1 calc R . .
H22C H 0.2466 0.9752 -0.1591 0.083 Uiso 1 1 calc R . .
C23 C 0.1628(6) 0.6983(5) 0.2420(5) 0.0332(15) Uani 1 1 d . . .
C24 C 0.2181(6) 0.6249(5) 0.1828(5) 0.0299(14) Uani 1 1 d . . .
C25 C 0.1532(6) 0.5418(5) 0.1774(5) 0.0353(15) Uani 1 1 d . . .
H25 H 0.1907 0.4912 0.1366 0.042 Uiso 1 1 calc R . .
C26 C 0.0371(6) 0.5333(6) 0.2301(6) 0.0424(18) Uani 1 1 d . . .
H26 H -0.0050 0.4766 0.2266 0.051 Uiso 1 1 calc R . .
C27 C -0.0191(6) 0.6075(6) 0.2886(5) 0.0392(17) Uani 1 1 d . . .
H27 H -0.1005 0.6022 0.3241 0.047 Uiso 1 1 calc R . .
C28 C 0.0434(6) 0.6903(5) 0.2958(5) 0.0344(15) Uani 1 1 d . . .
C29 C 0.3429(6) 0.6344(5) 0.1213(5) 0.0352(16) Uani 1 1 d . . .
C30 C 0.4495(6) 0.6465(5) 0.1652(6) 0.0386(17) Uani 1 1 d . . .
H30 H 0.4432 0.6462 0.2366 0.046 Uiso 1 1 calc R . .
C31 C 0.5640(6) 0.6591(5) 0.1086(6) 0.0392(17) Uani 1 1 d . . .
C32 C 0.5712(7) 0.6580(5) 0.0050(6) 0.0407(17) Uani 1 1 d . . .
H32 H 0.6488 0.6675 -0.0353 0.049 Uiso 1 1 calc R . .
C33 C 0.4687(7) 0.6434(5) -0.0419(6) 0.0389(17) Uani 1 1 d . . .
C34 C 0.3551(6) 0.6319(5) 0.0174(5) 0.0375(16) Uani 1 1 d . . .
H34 H 0.2841 0.6222 -0.0136 0.045 Uiso 1 1 calc R . .
C35 C 0.6760(7) 0.6758(7) 0.1591(6) 0.058(2) Uani 1 1 d . . .
H35A H 0.6931 0.7488 0.1304 0.087 Uiso 1 1 calc R . .
H35B H 0.7521 0.6228 0.1461 0.087 Uiso 1 1 calc R . .
H35C H 0.6553 0.6665 0.2335 0.087 Uiso 1 1 calc R . .
C36 C 0.4773(8) 0.6397(6) -0.1540(6) 0.054(2) Uani 1 1 d . . .
H36A H 0.5609 0.6542 -0.1860 0.081 Uiso 1 1 calc R . .
H36B H 0.4093 0.6943 -0.1888 0.081 Uiso 1 1 calc R . .
H36C H 0.4675 0.5680 -0.1602 0.081 Uiso 1 1 calc R . .
C37 C -0.0203(6) 0.7708(6) 0.3572(6) 0.0380(16) Uani 1 1 d . . .
C38 C -0.0282(6) 0.8812(5) 0.3174(5) 0.0358(16) Uani 1 1 d . . .
H38 H 0.0053 0.9052 0.2489 0.043 Uiso 1 1 calc R . .
C39 C -0.0836(7) 0.9574(6) 0.3749(6) 0.0423(18) Uani 1 1 d . . .
C40 C -0.1332(6) 0.9208(6) 0.4722(6) 0.0452(18) Uani 1 1 d . . .
H40 H -0.1709 0.9723 0.5121 0.054 Uiso 1 1 calc R . .
C41 C -0.1317(7) 0.8123(6) 0.5161(6) 0.0432(18) Uani 1 1 d . . .
C42 C -0.0730(6) 0.7384(6) 0.4566(6) 0.0400(17) Uani 1 1 d . . .
H42 H -0.0690 0.6635 0.4851 0.048 Uiso 1 1 calc R . .
C43 C -0.0864(7) 1.0761(6) 0.3297(6) 0.0485(19) Uani 1 1 d . . .
H43A H -0.0187 1.0847 0.2741 0.073 Uiso 1 1 calc R . .
H43B H -0.0723 1.1115 0.3834 0.073 Uiso 1 1 calc R . .
H43C H -0.1699 1.1090 0.3022 0.073 Uiso 1 1 calc R . .
C44 C -0.1885(8) 0.7738(7) 0.6237(6) 0.057(2) Uani 1 1 d . . .
H44A H -0.2604 0.7386 0.6205 0.086 Uiso 1 1 calc R . .
H44B H -0.2190 0.8356 0.6559 0.086 Uiso 1 1 calc R . .
H44C H -0.1229 0.7223 0.6645 0.086 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Hg1 C1 2.093(6) . ?
Hg1 C23 2.102(6) . ?
C1 C2 1.398(9) . ?
C1 C6 1.413(8) . ?
C2 C3 1.392(9) . ?
C2 C7 1.495(9) . ?
C3 C4 1.374(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(9) . ?
C5 H5 0.9500 . ?
C6 C15 1.486(9) . ?
C7 C8 1.388(9) . ?
C7 C12 1.394(9) . ?
C8 C9 1.388(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.396(9) . ?
C9 C13 1.527(9) . ?
C10 C11 1.370(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.413(9) . ?
C11 C14 1.508(9) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.392(9) . ?
C15 C20 1.405(10) . ?
C16 C17 1.370(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(10) . ?
C17 C21 1.508(10) . ?
C18 C19 1.398(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(9) . ?
C19 C22 1.496(10) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.381(9) . ?
C23 C28 1.402(9) . ?
C24 C25 1.415(8) . ?
C24 C29 1.497(9) . ?
C25 C26 1.368(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.383(10) . ?
C26 H26 0.9500 . ?
C27 C28 1.403(9) . ?
C27 H27 0.9500 . ?
C28 C37 1.490(9) . ?
C29 C34 1.390(9) . ?
C29 C30 1.393(9) . ?
C30 C31 1.383(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(10) . ?
C31 C35 1.516(9) . ?
C32 C33 1.389(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(9) . ?
C33 C36 1.507(10) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C42 1.389(9) . ?
C37 C38 1.394(9) . ?
C38 C39 1.394(9) . ?
C38 H38 0.9500 . ?
C39 C40 1.363(10) . ?
C39 C43 1.510(10) . ?
C40 C41 1.390(10) . ?
C40 H40 0.9500 . ?
C41 C42 1.396(9) . ?
C41 C44 1.510(10) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

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
C1 Hg1 C23 176.4(2) . . ?
C2 C1 C6 119.5(6) . . ?
C2 C1 Hg1 121.0(5) . . ?
C6 C1 Hg1 119.4(5) . . ?
C3 C2 C1 120.0(6) . . ?
C3 C2 C7 119.3(6) . . ?
C1 C2 C7 120.6(6) . . ?
C4 C3 C2 120.0(6) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.7(6) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 120.8(6) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 118.9(6) . . ?
C5 C6 C15 121.1(6) . . ?
C1 C6 C15 120.0(6) . . ?
C8 C7 C12 118.9(6) . . ?
C8 C7 C2 121.1(6) . . ?
C12 C7 C2 120.0(6) . . ?
C7 C8 C9 121.2(6) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C10 118.7(6) . . ?
C8 C9 C13 121.0(6) . . ?
C10 C9 C13 120.3(6) . . ?
C11 C10 C9 122.0(6) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 118.3(6) . . ?
C10 C11 C14 120.5(6) . . ?
C12 C11 C14 121.2(6) . . ?
C7 C12 C11 120.9(6) . . ?
C7 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 118.3(6) . . ?
C16 C15 C6 120.6(6) . . ?
C20 C15 C6 121.2(6) . . ?
C17 C16 C15 121.7(7) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 119.0(7) . . ?
C16 C17 C21 120.4(7) . . ?
C18 C17 C21 120.6(7) . . ?
C17 C18 C19 122.2(7) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C20 C19 C18 117.6(7) . . ?
C20 C19 C22 120.9(7) . . ?
C18 C19 C22 121.5(6) . . ?
C19 C20 C15 121.1(7) . . ?
C19 C20 H20 119.5 . . ?
C15 C20 H20 119.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 120.1(6) . . ?
C24 C23 Hg1 120.5(5) . . ?
C28 C23 Hg1 119.0(5) . . ?
C23 C24 C25 119.3(6) . . ?
C23 C24 C29 121.1(5) . . ?
C25 C24 C29 119.6(6) . . ?
C26 C25 C24 120.9(6) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 120.0(6) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 120.4(6) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C23 C28 C27 119.4(6) . . ?
C23 C28 C37 121.1(6) . . ?
C27 C28 C37 119.4(6) . . ?
C34 C29 C30 118.0(6) . . ?
C34 C29 C24 120.4(6) . . ?
C30 C29 C24 121.6(6) . . ?
C31 C30 C29 122.3(7) . . ?
C31 C30 H30 118.9 . . ?
C29 C30 H30 118.9 . . ?
C30 C31 C32 117.8(7) . . ?
C30 C31 C35 120.4(7) . . ?
C32 C31 C35 121.8(7) . . ?
C31 C32 C33 122.1(7) . . ?
C31 C32 H32 118.9 . . ?
C33 C32 H32 118.9 . . ?
C34 C33 C32 118.3(7) . . ?
C34 C33 C36 119.5(7) . . ?
C32 C33 C36 122.2(6) . . ?
C33 C34 C29 121.5(6) . . ?
C33 C34 H34 119.2 . . ?
C29 C34 H34 119.2 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C42 C37 C38 117.6(7) . . ?
C42 C37 C28 121.1(6) . . ?
C38 C37 C28 121.3(6) . . ?
C39 C38 C37 122.1(7) . . ?
C39 C38 H38 119.0 . . ?
C37 C38 H38 119.0 . . ?
C40 C39 C38 117.7(7) . . ?
C40 C39 C43 122.1(7) . . ?
C38 C39 C43 120.2(7) . . ?
C39 C40 C41 123.4(7) . . ?
C39 C40 H40 118.3 . . ?
C41 C40 H40 118.3 . . ?
C40 C41 C42 117.0(7) . . ?
C40 C41 C44 122.4(7) . . ?
C42 C41 C44 120.5(7) . . ?
C37 C42 C41 122.1(7) . . ?
C37 C42 H42 118.9 . . ?
C41 C42 H42 118.9 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.9(10) . . . . ?
Hg1 C1 C2 C3 174.7(5) . . . . ?
C6 C1 C2 C7 -179.5(6) . . . . ?
Hg1 C1 C2 C7 -3.9(9) . . . . ?
C1 C2 C3 C4 2.3(10) . . . . ?
C7 C2 C3 C4 -179.1(6) . . . . ?
C2 C3 C4 C5 -2.8(11) . . . . ?
C3 C4 C5 C6 1.9(11) . . . . ?
C4 C5 C6 C1 -0.5(10) . . . . ?
C4 C5 C6 C15 177.5(7) . . . . ?
C2 C1 C6 C5 0.0(10) . . . . ?
Hg1 C1 C6 C5 -175.7(5) . . . . ?
C2 C1 C6 C15 -178.0(6) . . . . ?
Hg1 C1 C6 C15 6.4(9) . . . . ?
C3 C2 C7 C8 -54.1(9) . . . . ?
C1 C2 C7 C8 124.5(7) . . . . ?
C3 C2 C7 C12 125.7(7) . . . . ?
C1 C2 C7 C12 -55.7(9) . . . . ?
C12 C7 C8 C9 0.3(10) . . . . ?
C2 C7 C8 C9 -179.8(6) . . . . ?
C7 C8 C9 C10 -1.5(10) . . . . ?
C7 C8 C9 C13 179.6(6) . . . . ?
C8 C9 C10 C11 1.3(10) . . . . ?
C13 C9 C10 C11 -179.8(7) . . . . ?
C9 C10 C11 C12 0.1(10) . . . . ?
C9 C10 C11 C14 179.5(6) . . . . ?
C8 C7 C12 C11 1.1(10) . . . . ?
C2 C7 C12 C11 -178.7(6) . . . . ?
C10 C11 C12 C7 -1.4(10) . . . . ?
C14 C11 C12 C7 179.2(6) . . . . ?
C5 C6 C15 C16 -56.8(9) . . . . ?
C1 C6 C15 C16 121.1(7) . . . . ?
C5 C6 C15 C20 123.5(7) . . . . ?
C1 C6 C15 C20 -58.5(9) . . . . ?
C20 C15 C16 C17 4.1(10) . . . . ?
C6 C15 C16 C17 -175.6(6) . . . . ?
C15 C16 C17 C18 -2.0(11) . . . . ?
C15 C16 C17 C21 177.6(7) . . . . ?
C16 C17 C18 C19 -0.5(11) . . . . ?
C21 C17 C18 C19 179.9(7) . . . . ?
C17 C18 C19 C20 0.8(10) . . . . ?
C17 C18 C19 C22 -179.5(7) . . . . ?
C18 C19 C20 C15 1.4(10) . . . . ?
C22 C19 C20 C15 -178.3(6) . . . . ?
C16 C15 C20 C19 -3.7(10) . . . . ?
C6 C15 C20 C19 175.9(6) . . . . ?
C28 C23 C24 C25 -0.2(9) . . . . ?
Hg1 C23 C24 C25 173.6(5) . . . . ?
C28 C23 C24 C29 177.5(6) . . . . ?
Hg1 C23 C24 C29 -8.8(8) . . . . ?
C23 C24 C25 C26 -0.2(10) . . . . ?
C29 C24 C25 C26 -177.9(6) . . . . ?
C24 C25 C26 C27 0.9(10) . . . . ?
C25 C26 C27 C28 -1.2(10) . . . . ?
C24 C23 C28 C27 -0.2(9) . . . . ?
Hg1 C23 C28 C27 -174.0(5) . . . . ?
C24 C23 C28 C37 -177.8(6) . . . . ?
Hg1 C23 C28 C37 8.3(8) . . . . ?
C26 C27 C28 C23 0.9(10) . . . . ?
C26 C27 C28 C37 178.5(6) . . . . ?
C23 C24 C29 C34 -129.1(7) . . . . ?
C25 C24 C29 C34 48.5(8) . . . . ?
C23 C24 C29 C30 50.5(8) . . . . ?
C25 C24 C29 C30 -131.9(7) . . . . ?
C34 C29 C30 C31 1.8(9) . . . . ?
C24 C29 C30 C31 -177.8(6) . . . . ?
C29 C30 C31 C32 -0.8(9) . . . . ?
C29 C30 C31 C35 178.0(6) . . . . ?
C30 C31 C32 C33 -0.9(10) . . . . ?
C35 C31 C32 C33 -179.6(6) . . . . ?
C31 C32 C33 C34 1.4(10) . . . . ?
C31 C32 C33 C36 -178.6(6) . . . . ?
C32 C33 C34 C29 -0.2(9) . . . . ?
C36 C33 C34 C29 179.7(6) . . . . ?
C30 C29 C34 C33 -1.3(9) . . . . ?
C24 C29 C34 C33 178.3(6) . . . . ?
C23 C28 C37 C42 -133.3(6) . . . . ?
C27 C28 C37 C42 49.1(9) . . . . ?
C23 C28 C37 C38 46.1(9) . . . . ?
C27 C28 C37 C38 -131.5(7) . . . . ?
C42 C37 C38 C39 1.6(9) . . . . ?
C28 C37 C38 C39 -177.8(6) . . . . ?
C37 C38 C39 C40 -1.4(9) . . . . ?
C37 C38 C39 C43 178.2(6) . . . . ?
C38 C39 C40 C41 -0.3(10) . . . . ?
C43 C39 C40 C41 -179.8(6) . . . . ?
C39 C40 C41 C42 1.5(10) . . . . ?
C39 C40 C41 C44 -179.4(7) . . . . ?
C38 C37 C42 C41 -0.3(9) . . . . ?
C28 C37 C42 C41 179.1(6) . . . . ?
C40 C41 C42 C37 -1.2(10) . . . . ?
C44 C41 C42 C37 179.7(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995

_refine_diff_density_max         1.75
_refine_diff_density_min         -0.87
_refine_diff_density_rms         0.15
_database_code_depnum_ccdc_archive 'CCDC 989608'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_11.0.5(C6H14)

#ZNTBLD

_nottingham_internal_coll_name   ZNTBLD
_nottingham_internal_coll_number 11160
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   hemisphare
_nottingham_internal_coll_frame_time 50
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   14/2/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user WL
_nottingham_internal_process_date 15/02/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 20/02/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 20/02/2012
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 23/2/2012
_nottingham_internal_archive_date 23/2/2012

_refine_special_details          
; 
Several large peaks appeared in the difference electron density map that could 
not be modelled as any sensible chemical species. PLATON SQUEEZE was used to 
generate a set of intensities for which the contribution from the disordered 
region had been removed; the final structure was refined against this set of 
intensities. The solvent voids are positioned across a centre of symmetry, and 
each equate to a hexane molecule (the solvent used for crystallisation) in terms 
of electron density. Hence a half molecule of hexane was included in the formula, 
and consequentially the calculation of Mr, density and other derived parameters. 
See below for PLATON SQUEEZE output.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;

# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.015 0.000 0.000 445 59 'C6 H14'
2 -0.012 0.500 0.500 445 59 'C6 H14'
3 0.000 0.000 0.500 16 1 ' '
4 0.500 0.500 0.000 16 1 ' '
_platon_squeeze_details          
;
;


_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H66 Zn, 0.5(C6 H14)'
_chemical_formula_sum            'C59 H73 Zn'
_chemical_formula_weight         847.54

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.178(3)
_cell_length_b                   22.671(5)
_cell_length_c                   18.854(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.559(4)
_cell_angle_gamma                90.00
_cell_volume                     5189(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    8940
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.67

_exptl_crystal_description       LATH
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.04
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_max          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1828
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27280
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         25.50
_reflns_number_total             9593
_reflns_number_gt                7417
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0569P)²+3.5393P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9593
_refine_ls_number_parameters     534
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1402
_refine_ls_wR_factor_gt          0.1335
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.41490(3) 0.311275(15) 0.152540(17) 0.02102(11) Uani 1 1 d . . .
C1 C 0.4610(2) 0.29798(11) 0.05778(15) 0.0189(6) Uani 1 1 d . . .
C2 C 0.3848(2) 0.29051(12) -0.00187(15) 0.0211(6) Uani 1 1 d . . .
C3 C 0.4199(2) 0.27398(13) -0.06709(16) 0.0242(7) Uani 1 1 d . . .
H3 H 0.3674 0.2683 -0.1065 0.029 Uiso 1 1 calc R . .
C4 C 0.5316(2) 0.26562(13) -0.07553(16) 0.0240(6) Uani 1 1 d . . .
H4 H 0.5549 0.2534 -0.1201 0.029 Uiso 1 1 calc R . .
C5 C 0.6084(3) 0.27532(12) -0.01830(16) 0.0234(6) Uani 1 1 d . . .
H5 H 0.6847 0.2708 -0.0242 0.028 Uiso 1 1 calc R . .
C6 C 0.5744(2) 0.29158(12) 0.04770(15) 0.0199(6) Uani 1 1 d . . .
C7 C 0.2635(2) 0.30135(14) 0.00307(15) 0.0263(7) Uani 1 1 d . . .
C8 C 0.2228(3) 0.35913(15) -0.00649(16) 0.0290(7) Uani 1 1 d . . .
C9 C 0.1084(3) 0.36919(16) -0.00446(17) 0.0343(8) Uani 1 1 d . . .
C10 C 0.0376(3) 0.32280(18) 0.00889(17) 0.0382(9) Uani 1 1 d . . .
C11 C 0.0792(3) 0.26566(18) 0.01876(17) 0.0372(9) Uani 1 1 d . . .
C12 C 0.1926(3) 0.25432(15) 0.01455(16) 0.0311(7) Uani 1 1 d . . .
C13 C 0.3001(3) 0.40958(14) -0.01983(19) 0.0356(8) Uani 1 1 d . . .
H13A H 0.2979 0.4387 0.0184 0.053 Uiso 1 1 calc R . .
H13B H 0.2771 0.4282 -0.0655 0.053 Uiso 1 1 calc R . .
H13C H 0.3753 0.3944 -0.0210 0.053 Uiso 1 1 calc R . .
C14 C 0.0611(3) 0.43015(18) -0.0185(2) 0.0490(10) Uani 1 1 d . . .
H14A H 0.0077 0.4289 -0.0602 0.073 Uiso 1 1 calc R . .
H14B H 0.1207 0.4576 -0.0274 0.073 Uiso 1 1 calc R . .
H14C H 0.0243 0.4434 0.0230 0.073 Uiso 1 1 calc R . .
C15 C -0.0846(3) 0.3349(2) 0.0110(2) 0.0530(11) Uani 1 1 d . . .
H15A H -0.0951 0.3720 0.0363 0.079 Uiso 1 1 calc R . .
H15B H -0.1189 0.3025 0.0357 0.079 Uiso 1 1 calc R . .
H15C H -0.1188 0.3379 -0.0377 0.079 Uiso 1 1 calc R . .
C16 C 0.0011(3) 0.2146(2) 0.0315(2) 0.0605(13) Uani 1 1 d . . .
H16A H -0.0457 0.2253 0.0695 0.091 Uiso 1 1 calc R . .
H16B H 0.0442 0.1794 0.0456 0.091 Uiso 1 1 calc R . .
H16C H -0.0451 0.2064 -0.0123 0.091 Uiso 1 1 calc R . .
C17 C 0.2378(3) 0.19271(16) 0.0197(2) 0.0419(9) Uani 1 1 d . . .
H17A H 0.1981 0.1678 -0.0162 0.063 Uiso 1 1 calc R . .
H17B H 0.2287 0.1768 0.0672 0.063 Uiso 1 1 calc R . .
H17C H 0.3163 0.1933 0.0115 0.063 Uiso 1 1 calc R . .
C18 C 0.6620(2) 0.30266(12) 0.10691(15) 0.0203(6) Uani 1 1 d . . .
C19 C 0.7165(2) 0.25447(13) 0.14092(15) 0.0227(6) Uani 1 1 d . . .
C20 C 0.8055(2) 0.26452(14) 0.19119(16) 0.0249(7) Uani 1 1 d . . .
C21 C 0.8408(3) 0.32202(14) 0.20727(16) 0.0277(7) Uani 1 1 d . . .
C22 C 0.7862(3) 0.37018(13) 0.17372(16) 0.0262(7) Uani 1 1 d . . .
C23 C 0.6960(2) 0.36059(13) 0.12317(15) 0.0234(6) Uani 1 1 d . . .
C24 C 0.6787(3) 0.19220(13) 0.12303(17) 0.0302(7) Uani 1 1 d . . .
H24A H 0.6078 0.1935 0.0946 0.045 Uiso 1 1 calc R . .
H24B H 0.6705 0.1703 0.1671 0.045 Uiso 1 1 calc R . .
H24C H 0.7335 0.1726 0.0958 0.045 Uiso 1 1 calc R . .
C25 C 0.8640(3) 0.21151(15) 0.22644(18) 0.0329(8) Uani 1 1 d . . .
H25A H 0.8130 0.1902 0.2549 0.049 Uiso 1 1 calc R . .
H25B H 0.9276 0.2250 0.2574 0.049 Uiso 1 1 calc R . .
H25C H 0.8892 0.1852 0.1898 0.049 Uiso 1 1 calc R . .
C26 C 0.9406(3) 0.33231(16) 0.26033(19) 0.0394(9) Uani 1 1 d . . .
H26A H 0.9563 0.3747 0.2638 0.059 Uiso 1 1 calc R . .
H26B H 1.0047 0.3117 0.2440 0.059 Uiso 1 1 calc R . .
H26C H 0.9248 0.3172 0.3071 0.059 Uiso 1 1 calc R . .
C27 C 0.8274(3) 0.43239(14) 0.1891(2) 0.0381(9) Uani 1 1 d . . .
H27A H 0.8996 0.4375 0.1704 0.057 Uiso 1 1 calc R . .
H27B H 0.8340 0.4391 0.2406 0.057 Uiso 1 1 calc R . .
H27C H 0.7752 0.4608 0.1663 0.057 Uiso 1 1 calc R . .
C28 C 0.6392(3) 0.41254(13) 0.08443(17) 0.0290(7) Uani 1 1 d . . .
H28A H 0.5844 0.3979 0.0478 0.044 Uiso 1 1 calc R . .
H28B H 0.6941 0.4363 0.0620 0.044 Uiso 1 1 calc R . .
H28C H 0.6027 0.4369 0.1185 0.044 Uiso 1 1 calc R . .
C29 C 0.3645(2) 0.31869(13) 0.24713(15) 0.0218(6) Uani 1 1 d . . .
C30 C 0.3441(3) 0.26868(13) 0.28804(16) 0.0248(7) Uani 1 1 d . . .
C31 C 0.3001(3) 0.27459(15) 0.35362(17) 0.0338(8) Uani 1 1 d . . .
H31 H 0.2869 0.2404 0.3807 0.041 Uiso 1 1 calc R . .
C32 C 0.2756(3) 0.32930(15) 0.37971(18) 0.0366(8) Uani 1 1 d . . .
H32 H 0.2438 0.3327 0.4239 0.044 Uiso 1 1 calc R . .
C33 C 0.2975(3) 0.37939(14) 0.34125(17) 0.0316(7) Uani 1 1 d . . .
H33 H 0.2823 0.4173 0.3597 0.038 Uiso 1 1 calc R . .
C34 C 0.3416(3) 0.37432(14) 0.27563(15) 0.0245(7) Uani 1 1 d . . .
C35 C 0.3707(3) 0.20738(13) 0.26349(16) 0.0241(7) Uani 1 1 d . . .
C36 C 0.4769(3) 0.18386(14) 0.28034(16) 0.0272(7) Uani 1 1 d . . .
C37 C 0.4985(3) 0.12552(14) 0.26019(17) 0.0306(7) Uani 1 1 d . . .
C38 C 0.4166(3) 0.09262(14) 0.22257(17) 0.0314(8) Uani 1 1 d . . .
C39 C 0.3110(3) 0.11615(14) 0.20499(17) 0.0295(7) Uani 1 1 d . . .
C40 C 0.2877(3) 0.17371(13) 0.22642(16) 0.0275(7) Uani 1 1 d . . .
C41 C 0.5657(3) 0.22109(15) 0.31970(18) 0.0328(8) Uani 1 1 d . . .
H41A H 0.6253 0.2282 0.2888 0.049 Uiso 1 1 calc R . .
H41B H 0.5949 0.2002 0.3626 0.049 Uiso 1 1 calc R . .
H41C H 0.5342 0.2589 0.3331 0.049 Uiso 1 1 calc R . .
C42 C 0.6109(3) 0.09817(15) 0.2807(2) 0.0398(9) Uani 1 1 d . . .
H42A H 0.6028 0.0661 0.3148 0.060 Uiso 1 1 calc R . .
H42B H 0.6605 0.1283 0.3024 0.060 Uiso 1 1 calc R . .
H42C H 0.6416 0.0825 0.2381 0.060 Uiso 1 1 calc R . .
C43 C 0.4423(4) 0.02997(15) 0.1998(2) 0.0477(10) Uani 1 1 d . . .
H43A H 0.3747 0.0064 0.1969 0.072 Uiso 1 1 calc R . .
H43B H 0.4965 0.0123 0.2348 0.072 Uiso 1 1 calc R . .
H43C H 0.4724 0.0309 0.1532 0.072 Uiso 1 1 calc R . .
C44 C 0.2244(3) 0.07888(15) 0.1635(2) 0.0416(9) Uani 1 1 d . . .
H44A H 0.2541 0.0641 0.1201 0.062 Uiso 1 1 calc R . .
H44B H 0.1590 0.1030 0.1508 0.062 Uiso 1 1 calc R . .
H44C H 0.2043 0.0455 0.1929 0.062 Uiso 1 1 calc R . .
C45 C 0.1737(3) 0.20037(15) 0.21165(19) 0.0347(8) Uani 1 1 d . . .
H45A H 0.1634 0.2321 0.2459 0.052 Uiso 1 1 calc R . .
H45B H 0.1178 0.1698 0.2163 0.052 Uiso 1 1 calc R . .
H45C H 0.1663 0.2164 0.1632 0.052 Uiso 1 1 calc R . .
C46 C 0.3680(3) 0.42995(13) 0.23741(16) 0.0243(6) Uani 1 1 d . . .
C47 C 0.2856(3) 0.45650(14) 0.19091(16) 0.0273(7) Uani 1 1 d . . .
C48 C 0.3083(3) 0.51098(14) 0.15990(17) 0.0313(7) Uani 1 1 d . . .
C49 C 0.4111(3) 0.53859(14) 0.17536(18) 0.0317(7) Uani 1 1 d . . .
C50 C 0.4937(3) 0.51066(14) 0.21969(18) 0.0326(8) Uani 1 1 d . . .
C51 C 0.4717(3) 0.45605(14) 0.25055(17) 0.0285(7) Uani 1 1 d . . .
C52 C 0.1757(3) 0.42652(16) 0.17596(19) 0.0359(8) Uani 1 1 d . . .
H52A H 0.1735 0.4069 0.1295 0.054 Uiso 1 1 calc R . .
H52B H 0.1168 0.4560 0.1755 0.054 Uiso 1 1 calc R . .
H52C H 0.1656 0.3972 0.2131 0.054 Uiso 1 1 calc R . .
C53 C 0.2208(3) 0.54206(16) 0.1115(2) 0.0439(9) Uani 1 1 d . . .
H53A H 0.1656 0.5133 0.0930 0.066 Uiso 1 1 calc R . .
H53B H 0.2553 0.5604 0.0717 0.066 Uiso 1 1 calc R . .
H53C H 0.1851 0.5725 0.1385 0.066 Uiso 1 1 calc R . .
C54 C 0.4311(4) 0.59881(16) 0.1437(2) 0.0481(10) Uani 1 1 d . . .
H54A H 0.4956 0.6170 0.1693 0.072 Uiso 1 1 calc R . .
H54B H 0.3664 0.6239 0.1480 0.072 Uiso 1 1 calc R . .
H54C H 0.4443 0.5944 0.0934 0.072 Uiso 1 1 calc R . .
C55 C 0.6051(3) 0.54074(17) 0.2343(2) 0.0505(10) Uani 1 1 d . . .
H55A H 0.5966 0.5758 0.2638 0.076 Uiso 1 1 calc R . .
H55B H 0.6334 0.5524 0.1892 0.076 Uiso 1 1 calc R . .
H55C H 0.6569 0.5133 0.2595 0.076 Uiso 1 1 calc R . .
C56 C 0.5607(3) 0.42510(16) 0.2984(2) 0.0405(9) Uani 1 1 d . . .
H56A H 0.5273 0.3932 0.3245 0.061 Uiso 1 1 calc R . .
H56B H 0.5956 0.4535 0.3322 0.061 Uiso 1 1 calc R . .
H56C H 0.6162 0.4086 0.2692 0.061 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Zn1 C1 1.939(3) . ?
Zn1 C29 1.939(3) . ?
C1 C2 1.411(4) . ?
C1 C6 1.416(4) . ?
C2 C3 1.385(4) . ?
C2 C7 1.508(4) . ?
C3 C4 1.395(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
C6 C18 1.502(4) . ?
C7 C12 1.399(4) . ?
C7 C8 1.407(4) . ?
C8 C9 1.414(4) . ?
C8 C13 1.515(5) . ?
C9 C10 1.396(5) . ?
C9 C14 1.513(5) . ?
C10 C11 1.398(5) . ?
C10 C15 1.516(5) . ?
C11 C12 1.413(5) . ?
C11 C16 1.529(5) . ?
C12 C17 1.502(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.404(4) . ?
C18 C19 1.406(4) . ?
C19 C20 1.401(4) . ?
C19 C24 1.514(4) . ?
C20 C21 1.399(4) . ?
C20 C25 1.523(4) . ?
C21 C22 1.403(4) . ?
C21 C26 1.529(4) . ?
C22 C23 1.413(4) . ?
C22 C27 1.517(4) . ?
C23 C28 1.523(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.405(4) . ?
C29 C34 1.408(4) . ?
C30 C31 1.392(4) . ?
C30 C35 1.508(4) . ?
C31 C32 1.376(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.385(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.392(4) . ?
C33 H33 0.9500 . ?
C34 C46 1.500(4) . ?
C35 C40 1.408(4) . ?
C35 C36 1.411(4) . ?
C36 C37 1.407(4) . ?
C36 C41 1.518(4) . ?
C37 C38 1.394(5) . ?
C37 C42 1.523(4) . ?
C38 C39 1.408(5) . ?
C38 C43 1.523(5) . ?
C39 C40 1.402(4) . ?
C39 C44 1.518(5) . ?
C40 C45 1.519(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C51 1.399(4) . ?
C46 C47 1.414(4) . ?
C47 C48 1.403(4) . ?
C47 C52 1.507(4) . ?
C48 C49 1.409(5) . ?
C48 C53 1.520(4) . ?
C49 C50 1.406(5) . ?
C49 C54 1.518(5) . ?
C50 C51 1.403(5) . ?
C50 C55 1.524(5) . ?
C51 C56 1.524(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?

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
C1 Zn1 C29 175.78(12) . . ?
C2 C1 C6 117.9(3) . . ?
C2 C1 Zn1 122.2(2) . . ?
C6 C1 Zn1 119.8(2) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 C7 118.2(2) . . ?
C1 C2 C7 121.2(3) . . ?
C2 C3 C4 120.7(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 120.6(3) . . ?
C5 C6 C18 117.7(3) . . ?
C1 C6 C18 121.7(3) . . ?
C12 C7 C8 120.9(3) . . ?
C12 C7 C2 120.3(3) . . ?
C8 C7 C2 118.7(3) . . ?
C7 C8 C9 118.9(3) . . ?
C7 C8 C13 120.5(3) . . ?
C9 C8 C13 120.6(3) . . ?
C10 C9 C8 120.5(3) . . ?
C10 C9 C14 119.2(3) . . ?
C8 C9 C14 120.3(3) . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 C15 119.4(4) . . ?
C11 C10 C15 120.6(4) . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 C16 120.0(3) . . ?
C12 C11 C16 119.6(4) . . ?
C7 C12 C11 119.2(3) . . ?
C7 C12 C17 119.4(3) . . ?
C11 C12 C17 121.4(3) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.4(3) . . ?
C23 C18 C6 119.9(2) . . ?
C19 C18 C6 119.3(2) . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 C24 120.5(3) . . ?
C18 C19 C24 119.9(3) . . ?
C21 C20 C19 120.4(3) . . ?
C21 C20 C25 121.1(3) . . ?
C19 C20 C25 118.5(3) . . ?
C20 C21 C22 120.1(3) . . ?
C20 C21 C26 119.9(3) . . ?
C22 C21 C26 120.0(3) . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 C27 119.9(3) . . ?
C23 C22 C27 120.0(3) . . ?
C18 C23 C22 119.5(3) . . ?
C18 C23 C28 120.3(3) . . ?
C22 C23 C28 120.2(3) . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 117.7(3) . . ?
C30 C29 Zn1 121.2(2) . . ?
C34 C29 Zn1 121.1(2) . . ?
C31 C30 C29 120.5(3) . . ?
C31 C30 C35 117.9(3) . . ?
C29 C30 C35 121.6(3) . . ?
C32 C31 C30 120.9(3) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C31 C32 C33 119.7(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C34 120.1(3) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C33 C34 C29 121.0(3) . . ?
C33 C34 C46 118.0(3) . . ?
C29 C34 C46 120.9(3) . . ?
C40 C35 C36 121.1(3) . . ?
C40 C35 C30 119.2(3) . . ?
C36 C35 C30 119.6(3) . . ?
C37 C36 C35 118.8(3) . . ?
C37 C36 C41 120.9(3) . . ?
C35 C36 C41 120.3(3) . . ?
C38 C37 C36 119.9(3) . . ?
C38 C37 C42 120.2(3) . . ?
C36 C37 C42 119.8(3) . . ?
C37 C38 C39 121.4(3) . . ?
C37 C38 C43 119.2(3) . . ?
C39 C38 C43 119.4(3) . . ?
C40 C39 C38 119.1(3) . . ?
C40 C39 C44 121.2(3) . . ?
C38 C39 C44 119.6(3) . . ?
C39 C40 C35 119.6(3) . . ?
C39 C40 C45 121.4(3) . . ?
C35 C40 C45 119.0(3) . . ?
C36 C41 H41A 109.5 . . ?
C36 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C36 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C40 C45 H45A 109.5 . . ?
C40 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C40 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C51 C46 C47 121.1(3) . . ?
C51 C46 C34 119.7(3) . . ?
C47 C46 C34 119.2(3) . . ?
C48 C47 C46 118.6(3) . . ?
C48 C47 C52 121.4(3) . . ?
C46 C47 C52 120.0(3) . . ?
C47 C48 C49 120.4(3) . . ?
C47 C48 C53 120.4(3) . . ?
C49 C48 C53 119.1(3) . . ?
C50 C49 C48 120.3(3) . . ?
C50 C49 C54 120.6(3) . . ?
C48 C49 C54 119.1(3) . . ?
C51 C50 C49 119.5(3) . . ?
C51 C50 C55 121.1(3) . . ?
C49 C50 C55 119.4(3) . . ?
C46 C51 C50 119.9(3) . . ?
C46 C51 C56 119.9(3) . . ?
C50 C51 C56 120.1(3) . . ?
C47 C52 H52A 109.5 . . ?
C47 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C47 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C48 C53 H53A 109.5 . . ?
C48 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C48 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C49 C54 H54A 109.5 . . ?
C49 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C49 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C50 C55 H55A 109.5 . . ?
C50 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C50 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C51 C56 H56A 109.5 . . ?
C51 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C51 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 3.8(4) . . . . ?
Zn1 C1 C2 C3 -172.1(2) . . . . ?
C6 C1 C2 C7 -175.1(3) . . . . ?
Zn1 C1 C2 C7 9.1(4) . . . . ?
C1 C2 C3 C4 -1.4(4) . . . . ?
C7 C2 C3 C4 177.5(3) . . . . ?
C2 C3 C4 C5 -1.5(4) . . . . ?
C3 C4 C5 C6 1.9(4) . . . . ?
C4 C5 C6 C1 0.6(4) . . . . ?
C4 C5 C6 C18 -178.7(3) . . . . ?
C2 C1 C6 C5 -3.4(4) . . . . ?
Zn1 C1 C6 C5 172.6(2) . . . . ?
C2 C1 C6 C18 175.9(2) . . . . ?
Zn1 C1 C6 C18 -8.2(4) . . . . ?
C3 C2 C7 C12 84.8(4) . . . . ?
C1 C2 C7 C12 -96.4(3) . . . . ?
C3 C2 C7 C8 -93.1(3) . . . . ?
C1 C2 C7 C8 85.8(4) . . . . ?
C12 C7 C8 C9 -0.1(4) . . . . ?
C2 C7 C8 C9 177.7(3) . . . . ?
C12 C7 C8 C13 -179.2(3) . . . . ?
C2 C7 C8 C13 -1.4(4) . . . . ?
C7 C8 C9 C10 1.9(5) . . . . ?
C13 C8 C9 C10 -179.0(3) . . . . ?
C7 C8 C9 C14 -176.6(3) . . . . ?
C13 C8 C9 C14 2.5(5) . . . . ?
C8 C9 C10 C11 -1.5(5) . . . . ?
C14 C9 C10 C11 177.1(3) . . . . ?
C8 C9 C10 C15 179.8(3) . . . . ?
C14 C9 C10 C15 -1.6(5) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
C15 C10 C11 C12 178.0(3) . . . . ?
C9 C10 C11 C16 -178.5(3) . . . . ?
C15 C10 C11 C16 0.2(5) . . . . ?
C8 C7 C12 C11 -2.0(5) . . . . ?
C2 C7 C12 C11 -179.8(3) . . . . ?
C8 C7 C12 C17 176.0(3) . . . . ?
C2 C7 C12 C17 -1.8(4) . . . . ?
C10 C11 C12 C7 2.4(5) . . . . ?
C16 C11 C12 C7 -179.8(3) . . . . ?
C10 C11 C12 C17 -175.5(3) . . . . ?
C16 C11 C12 C17 2.3(5) . . . . ?
C5 C6 C18 C23 98.1(3) . . . . ?
C1 C6 C18 C23 -81.2(4) . . . . ?
C5 C6 C18 C19 -75.8(4) . . . . ?
C1 C6 C18 C19 104.9(3) . . . . ?
C23 C18 C19 C20 -0.2(4) . . . . ?
C6 C18 C19 C20 173.7(3) . . . . ?
C23 C18 C19 C24 179.9(3) . . . . ?
C6 C18 C19 C24 -6.3(4) . . . . ?
C18 C19 C20 C21 -0.5(5) . . . . ?
C24 C19 C20 C21 179.5(3) . . . . ?
C18 C19 C20 C25 -179.1(3) . . . . ?
C24 C19 C20 C25 0.8(5) . . . . ?
C19 C20 C21 C22 0.8(5) . . . . ?
C25 C20 C21 C22 179.5(3) . . . . ?
C19 C20 C21 C26 -177.9(3) . . . . ?
C25 C20 C21 C26 0.8(5) . . . . ?
C20 C21 C22 C23 -0.6(5) . . . . ?
C26 C21 C22 C23 178.2(3) . . . . ?
C20 C21 C22 C27 -177.6(3) . . . . ?
C26 C21 C22 C27 1.1(5) . . . . ?
C19 C18 C23 C22 0.5(5) . . . . ?
C6 C18 C23 C22 -173.4(3) . . . . ?
C19 C18 C23 C28 178.0(3) . . . . ?
C6 C18 C23 C28 4.1(4) . . . . ?
C21 C22 C23 C18 -0.1(5) . . . . ?
C27 C22 C23 C18 177.0(3) . . . . ?
C21 C22 C23 C28 -177.6(3) . . . . ?
C27 C22 C23 C28 -0.5(5) . . . . ?
C34 C29 C30 C31 1.5(4) . . . . ?
Zn1 C29 C30 C31 -175.2(2) . . . . ?
C34 C29 C30 C35 -177.3(3) . . . . ?
Zn1 C29 C30 C35 6.0(4) . . . . ?
C29 C30 C31 C32 0.1(5) . . . . ?
C35 C30 C31 C32 179.0(3) . . . . ?
C30 C31 C32 C33 -1.7(6) . . . . ?
C31 C32 C33 C34 1.6(5) . . . . ?
C32 C33 C34 C29 0.1(5) . . . . ?
C32 C33 C34 C46 -177.6(3) . . . . ?
C30 C29 C34 C33 -1.6(4) . . . . ?
Zn1 C29 C34 C33 175.1(2) . . . . ?
C30 C29 C34 C46 176.0(3) . . . . ?
Zn1 C29 C34 C46 -7.3(4) . . . . ?
C31 C30 C35 C40 86.4(4) . . . . ?
C29 C30 C35 C40 -94.7(4) . . . . ?
C31 C30 C35 C36 -91.1(4) . . . . ?
C29 C30 C35 C36 87.7(4) . . . . ?
C40 C35 C36 C37 -0.8(5) . . . . ?
C30 C35 C36 C37 176.8(3) . . . . ?
C40 C35 C36 C41 179.4(3) . . . . ?
C30 C35 C36 C41 -3.1(4) . . . . ?
C35 C36 C37 C38 1.7(5) . . . . ?
C41 C36 C37 C38 -178.4(3) . . . . ?
C35 C36 C37 C42 -177.2(3) . . . . ?
C41 C36 C37 C42 2.6(5) . . . . ?
C36 C37 C38 C39 -1.1(5) . . . . ?
C42 C37 C38 C39 177.9(3) . . . . ?
C36 C37 C38 C43 178.7(3) . . . . ?
C42 C37 C38 C43 -2.3(5) . . . . ?
C37 C38 C39 C40 -0.6(5) . . . . ?
C43 C38 C39 C40 179.6(3) . . . . ?
C37 C38 C39 C44 179.6(3) . . . . ?
C43 C38 C39 C44 -0.2(5) . . . . ?
C38 C39 C40 C35 1.5(5) . . . . ?
C44 C39 C40 C35 -178.7(3) . . . . ?
C38 C39 C40 C45 -177.4(3) . . . . ?
C44 C39 C40 C45 2.4(5) . . . . ?
C36 C35 C40 C39 -0.9(5) . . . . ?
C30 C35 C40 C39 -178.4(3) . . . . ?
C36 C35 C40 C45 178.1(3) . . . . ?
C30 C35 C40 C45 0.5(4) . . . . ?
C33 C34 C46 C51 88.6(4) . . . . ?
C29 C34 C46 C51 -89.1(4) . . . . ?
C33 C34 C46 C47 -88.7(4) . . . . ?
C29 C34 C46 C47 93.6(4) . . . . ?
C51 C46 C47 C48 -2.3(5) . . . . ?
C34 C46 C47 C48 174.9(3) . . . . ?
C51 C46 C47 C52 178.1(3) . . . . ?
C34 C46 C47 C52 -4.6(4) . . . . ?
C46 C47 C48 C49 -0.4(5) . . . . ?
C52 C47 C48 C49 179.2(3) . . . . ?
C46 C47 C48 C53 -178.0(3) . . . . ?
C52 C47 C48 C53 1.5(5) . . . . ?
C47 C48 C49 C50 2.7(5) . . . . ?
C53 C48 C49 C50 -179.7(3) . . . . ?
C47 C48 C49 C54 -177.2(3) . . . . ?
C53 C48 C49 C54 0.5(5) . . . . ?
C48 C49 C50 C51 -2.3(5) . . . . ?
C54 C49 C50 C51 177.5(3) . . . . ?
C48 C49 C50 C55 178.6(3) . . . . ?
C54 C49 C50 C55 -1.5(5) . . . . ?
C47 C46 C51 C50 2.7(5) . . . . ?
C34 C46 C51 C50 -174.5(3) . . . . ?
C47 C46 C51 C56 -177.3(3) . . . . ?
C34 C46 C51 C56 5.5(5) . . . . ?
C49 C50 C51 C46 -0.4(5) . . . . ?
C55 C50 C51 C46 178.7(3) . . . . ?
C49 C50 C51 C56 179.6(3) . . . . ?
C55 C50 C51 C56 -1.3(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 989609'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_12

#CDTBLB

_nottingham_internal_coll_name   CDTBLB
_nottingham_internal_coll_number 10959
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   hemishpere
_nottingham_internal_coll_frame_time 10
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   12/12/2011
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user TB
_nottingham_internal_process_date 16/01/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 16/01/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 16/01/2012
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 1/2/2012
_nottingham_internal_archive_date 1/2/2012


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H66 Cd'
_chemical_formula_sum            'C56 H66 Cd'
_chemical_formula_weight         851.49

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.978(5)
_cell_length_b                   18.737(7)
_cell_length_c                   34.854(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9129(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    7339
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.44

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_max          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3600
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13736
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2628
_reflns_number_gt                2483
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0396P)²+17.6214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2628
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cd1 Cd 0.1250 0.1250 0.1250 0.01667(9) Uani 1 4 d S . .
C1 C 0.1250 0.23773(12) 0.1250 0.0164(4) Uani 1 2 d S . .
C2 C 0.05899(11) 0.27652(8) 0.10275(4) 0.0175(3) Uani 1 1 d . . .
C3 C 0.05748(11) 0.35101(9) 0.10363(4) 0.0200(3) Uani 1 1 d . . .
H3 H 0.0101 0.3763 0.0896 0.024 Uiso 1 1 calc R . .
C4 C 0.1250 0.38837(13) 0.1250 0.0200(4) Uani 1 2 d S . .
H4 H 0.1250 0.4391 0.1250 0.024 Uiso 1 2 calc SR . .
C5 C -0.01124(11) 0.23882(8) 0.07730(4) 0.0182(3) Uani 1 1 d . . .
C6 C -0.10460(12) 0.22573(9) 0.09060(5) 0.0208(3) Uani 1 1 d . . .
C7 C -0.17197(12) 0.19647(9) 0.06538(5) 0.0232(3) Uani 1 1 d . . .
C8 C -0.14639(12) 0.18005(9) 0.02735(5) 0.0242(3) Uani 1 1 d . . .
C9 C -0.05230(12) 0.19094(9) 0.01459(5) 0.0231(3) Uani 1 1 d . . .
C10 C 0.01603(11) 0.22015(8) 0.03979(4) 0.0198(3) Uani 1 1 d . . .
C11 C -0.13050(12) 0.24264(10) 0.13193(5) 0.0252(4) Uani 1 1 d . . .
H11A H -0.0751 0.2638 0.1449 0.038 Uiso 1 1 calc R . .
H11B H -0.1491 0.1986 0.1452 0.038 Uiso 1 1 calc R . .
H11C H -0.1840 0.2764 0.1324 0.038 Uiso 1 1 calc R . .
C12 C -0.27348(13) 0.18311(10) 0.07836(6) 0.0321(4) Uani 1 1 d . . .
H12A H -0.2801 0.1967 0.1054 0.048 Uiso 1 1 calc R . .
H12B H -0.2887 0.1324 0.0754 0.048 Uiso 1 1 calc R . .
H12C H -0.3175 0.2116 0.0627 0.048 Uiso 1 1 calc R . .
C13 C -0.22350(14) 0.15107(11) 0.00087(6) 0.0346(4) Uani 1 1 d . . .
H13A H -0.2746 0.1865 -0.0019 0.052 Uiso 1 1 calc R . .
H13B H -0.2499 0.1071 0.0117 0.052 Uiso 1 1 calc R . .
H13C H -0.1957 0.1409 -0.0244 0.052 Uiso 1 1 calc R . .
C14 C -0.02249(14) 0.17431(10) -0.02638(5) 0.0296(4) Uani 1 1 d . . .
H14A H -0.0121 0.2190 -0.0404 0.044 Uiso 1 1 calc R . .
H14B H -0.0730 0.1467 -0.0390 0.044 Uiso 1 1 calc R . .
H14C H 0.0369 0.1465 -0.0261 0.044 Uiso 1 1 calc R . .
C15 C 0.11826(12) 0.23138(10) 0.02653(5) 0.0235(3) Uani 1 1 d . . .
H15A H 0.1539 0.2574 0.0463 0.035 Uiso 1 1 calc R . .
H15B H 0.1184 0.2590 0.0027 0.035 Uiso 1 1 calc R . .
H15C H 0.1486 0.1850 0.0221 0.035 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Cd1 C1 2.112(2) 2 ?
Cd1 C1 2.112(2) . ?
C1 C2 1.4075(19) 4 ?
C1 C2 1.4075(19) . ?
C2 C3 1.396(2) . ?
C2 C5 1.500(2) . ?
C3 C4 1.391(2) . ?
C3 H3 0.9500 . ?
C4 C3 1.391(2) 4 ?
C4 H4 0.9500 . ?
C5 C10 1.406(2) . ?
C5 C6 1.406(2) . ?
C6 C7 1.400(2) . ?
C6 C11 1.519(2) . ?
C7 C8 1.407(2) . ?
C7 C12 1.510(2) . ?
C8 C9 1.403(3) . ?
C8 C13 1.519(2) . ?
C9 C10 1.408(2) . ?
C9 C14 1.520(2) . ?
C10 C15 1.517(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

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
C1 Cd1 C1 180.0 2 . ?
C2 C1 C2 117.8(2) 4 . ?
C2 C1 Cd1 121.09(10) 4 . ?
C2 C1 Cd1 121.09(10) . . ?
C3 C2 C1 120.93(15) . . ?
C3 C2 C5 118.29(14) . . ?
C1 C2 C5 120.79(15) . . ?
C4 C3 C2 120.30(16) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C3 119.6(2) 4 . ?
C3 C4 H4 120.2 4 . ?
C3 C4 H4 120.2 . . ?
C10 C5 C6 120.97(14) . . ?
C10 C5 C2 119.31(14) . . ?
C6 C5 C2 119.65(14) . . ?
C7 C6 C5 119.05(15) . . ?
C7 C6 C11 121.12(15) . . ?
C5 C6 C11 119.83(14) . . ?
C6 C7 C8 120.41(15) . . ?
C6 C7 C12 120.59(16) . . ?
C8 C7 C12 119.00(15) . . ?
C9 C8 C7 120.33(15) . . ?
C9 C8 C13 121.62(16) . . ?
C7 C8 C13 118.04(16) . . ?
C8 C9 C10 119.64(15) . . ?
C8 C9 C14 121.67(15) . . ?
C10 C9 C14 118.66(15) . . ?
C5 C10 C9 119.52(15) . . ?
C5 C10 C15 120.28(14) . . ?
C9 C10 C15 120.20(14) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C3 -1.78(10) 4 . . . ?
Cd1 C1 C2 C3 178.22(10) . . . . ?
C2 C1 C2 C5 177.90(15) 4 . . . ?
Cd1 C1 C2 C5 -2.10(15) . . . . ?
C1 C2 C3 C4 3.6(2) . . . . ?
C5 C2 C3 C4 -176.11(12) . . . . ?
C2 C3 C4 C3 -1.77(10) . . . 4 ?
C3 C2 C5 C10 93.09(18) . . . . ?
C1 C2 C5 C10 -86.60(17) . . . . ?
C3 C2 C5 C6 -83.90(19) . . . . ?
C1 C2 C5 C6 96.41(16) . . . . ?
C10 C5 C6 C7 -2.8(2) . . . . ?
C2 C5 C6 C7 174.17(14) . . . . ?
C10 C5 C6 C11 176.59(15) . . . . ?
C2 C5 C6 C11 -6.5(2) . . . . ?
C5 C6 C7 C8 0.4(2) . . . . ?
C11 C6 C7 C8 -178.98(16) . . . . ?
C5 C6 C7 C12 -178.69(15) . . . . ?
C11 C6 C7 C12 2.0(2) . . . . ?
C6 C7 C8 C9 1.8(2) . . . . ?
C12 C7 C8 C9 -179.11(15) . . . . ?
C6 C7 C8 C13 -177.70(16) . . . . ?
C12 C7 C8 C13 1.4(2) . . . . ?
C7 C8 C9 C10 -1.6(2) . . . . ?
C13 C8 C9 C10 177.89(16) . . . . ?
C7 C8 C9 C14 -179.52(16) . . . . ?
C13 C8 C9 C14 0.0(3) . . . . ?
C6 C5 C10 C9 3.0(2) . . . . ?
C2 C5 C10 C9 -173.98(14) . . . . ?
C6 C5 C10 C15 -177.06(15) . . . . ?
C2 C5 C10 C15 6.0(2) . . . . ?
C8 C9 C10 C5 -0.8(2) . . . . ?
C14 C9 C10 C5 177.22(15) . . . . ?
C8 C9 C10 C15 179.27(15) . . . . ?
C14 C9 C10 C15 -2.8(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.071
_database_code_depnum_ccdc_archive 'CCDC 989610'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_13

#HGTBLA

_nottingham_internal_coll_name   HGTBLA
_nottingham_internal_coll_number 10928
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time 7
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   25/11/11
_nottingham_internal_process_user TB/WL
_nottingham_internal_process_date 25/11/2011
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 16/01/2012
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 16/01/2012
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 25/1/2012
_nottingham_internal_archive_date 25/1/2012

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H66 Hg'
_chemical_formula_sum            'C56 H66 Hg'
_chemical_formula_weight         939.68

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'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.998(3)
_cell_length_b                   18.670(4)
_cell_length_c                   34.919(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9126(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5168
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      27.19

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_min          0.05
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_max          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3856
_exptl_absorpt_coefficient_mu    3.409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_process_details   'SADABS 2007/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13405
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         27.57
_reflns_number_total             2653
_reflns_number_gt                2337
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ' ? '
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2653
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0648
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Hg1 Hg 0.1250 0.1250 0.1250 0.01805(8) Uani 1 4 d S . .
C1 C 0.1250 0.0126(2) 0.1250 0.0182(7) Uani 1 2 d S . .
C2 C 0.19092(19) -0.02557(15) 0.10273(7) 0.0193(5) Uani 1 1 d . . .
C3 C 0.1923(2) -0.10039(15) 0.10367(8) 0.0219(5) Uani 1 1 d . . .
H3 H 0.2396 -0.1257 0.0896 0.026 Uiso 1 1 calc R . .
C4 C 0.1250 -0.1383(2) 0.1250 0.0233(8) Uani 1 2 d S . .
H4 H 0.1250 -0.1892 0.1250 0.028 Uiso 1 2 calc SR . .
C5 C 0.26084(19) 0.01233(14) 0.07716(7) 0.0193(5) Uani 1 1 d . . .
C6 C 0.3542(2) 0.02515(16) 0.09037(8) 0.0233(6) Uani 1 1 d . . .
C7 C 0.4216(2) 0.05400(15) 0.06496(9) 0.0255(6) Uani 1 1 d . . .
C8 C 0.3962(2) 0.07013(16) 0.02705(9) 0.0269(6) Uani 1 1 d . . .
C9 C 0.3022(2) 0.05912(15) 0.01437(8) 0.0256(6) Uani 1 1 d . . .
C10 C 0.2335(2) 0.03023(15) 0.03979(7) 0.0224(6) Uani 1 1 d . . .
C11 C 0.3804(2) 0.00847(18) 0.13148(9) 0.0273(6) Uani 1 1 d . . .
H11A H 0.3235 -0.0078 0.1453 0.041 Uiso 1 1 calc R . .
H11B H 0.4057 0.0517 0.1438 0.041 Uiso 1 1 calc R . .
H11C H 0.4291 -0.0293 0.1320 0.041 Uiso 1 1 calc R . .
C12 C 0.5235(2) 0.06761(18) 0.07762(10) 0.0354(7) Uani 1 1 d . . .
H12A H 0.5376 0.1189 0.0757 0.053 Uiso 1 1 calc R . .
H12B H 0.5674 0.0408 0.0611 0.053 Uiso 1 1 calc R . .
H12C H 0.5314 0.0519 0.1042 0.053 Uiso 1 1 calc R . .
C13 C 0.4729(2) 0.09883(19) 0.00040(10) 0.0379(8) Uani 1 1 d . . .
H13A H 0.5007 0.1424 0.0114 0.057 Uiso 1 1 calc R . .
H13B H 0.4445 0.1100 -0.0246 0.057 Uiso 1 1 calc R . .
H13C H 0.5230 0.0627 -0.0028 0.057 Uiso 1 1 calc R . .
C14 C 0.2723(2) 0.07537(17) -0.02644(8) 0.0324(7) Uani 1 1 d . . .
H14A H 0.2546 0.0307 -0.0394 0.049 Uiso 1 1 calc R . .
H14B H 0.3256 0.0979 -0.0401 0.049 Uiso 1 1 calc R . .
H14C H 0.2174 0.1080 -0.0262 0.049 Uiso 1 1 calc R . .
C15 C 0.13110(19) 0.01914(17) 0.02674(8) 0.0256(6) Uani 1 1 d . . .
H15A H 0.0962 -0.0081 0.0462 0.038 Uiso 1 1 calc R . .
H15B H 0.1307 -0.0075 0.0025 0.038 Uiso 1 1 calc R . .
H15C H 0.1003 0.0658 0.0230 0.038 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Hg1 C1 2.099(4) . ?
Hg1 C1 2.099(4) 2 ?
C1 C2 1.401(3) . ?
C1 C2 1.401(3) 4 ?
C2 C3 1.397(4) . ?
C2 C5 1.502(4) . ?
C3 C4 1.394(4) . ?
C3 H3 0.9500 . ?
C4 C3 1.394(4) 4 ?
C4 H4 0.9500 . ?
C5 C10 1.401(4) . ?
C5 C6 1.406(4) . ?
C6 C7 1.403(4) . ?
C6 C11 1.514(4) . ?
C7 C8 1.403(4) . ?
C7 C12 1.515(4) . ?
C8 C9 1.404(4) . ?
C8 C13 1.519(4) . ?
C9 C10 1.415(4) . ?
C9 C14 1.516(4) . ?
C10 C15 1.518(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

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
C1 Hg1 C1 180.0 . 2 ?
C2 C1 C2 118.9(3) . 4 ?
C2 C1 Hg1 120.56(17) . . ?
C2 C1 Hg1 120.56(17) 4 . ?
C3 C2 C1 120.3(3) . . ?
C3 C2 C5 118.4(2) . . ?
C1 C2 C5 121.3(2) . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C3 119.0(4) . 4 ?
C3 C4 H4 120.5 . . ?
C3 C4 H4 120.5 4 . ?
C10 C5 C6 121.3(2) . . ?
C10 C5 C2 119.2(2) . . ?
C6 C5 C2 119.4(2) . . ?
C7 C6 C5 118.9(3) . . ?
C7 C6 C11 121.0(3) . . ?
C5 C6 C11 120.1(2) . . ?
C6 C7 C8 120.5(3) . . ?
C6 C7 C12 120.9(3) . . ?
C8 C7 C12 118.6(3) . . ?
C7 C8 C9 120.3(3) . . ?
C7 C8 C13 118.3(3) . . ?
C9 C8 C13 121.4(3) . . ?
C8 C9 C10 119.7(3) . . ?
C8 C9 C14 121.7(3) . . ?
C10 C9 C14 118.6(3) . . ?
C5 C10 C9 119.3(3) . . ?
C5 C10 C15 120.4(2) . . ?
C9 C10 C15 120.3(2) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C3 -1.77(18) 4 . . . ?
Hg1 C1 C2 C3 178.23(18) . . . . ?
C2 C1 C2 C5 177.7(3) 4 . . . ?
Hg1 C1 C2 C5 -2.3(3) . . . . ?
C1 C2 C3 C4 3.6(4) . . . . ?
C5 C2 C3 C4 -175.9(2) . . . . ?
C2 C3 C4 C3 -1.79(18) . . . 4 ?
C3 C2 C5 C10 92.4(3) . . . . ?
C1 C2 C5 C10 -87.1(3) . . . . ?
C3 C2 C5 C6 -83.7(3) . . . . ?
C1 C2 C5 C6 96.8(3) . . . . ?
C10 C5 C6 C7 -2.4(4) . . . . ?
C2 C5 C6 C7 173.6(3) . . . . ?
C10 C5 C6 C11 177.1(3) . . . . ?
C2 C5 C6 C11 -6.9(4) . . . . ?
C5 C6 C7 C8 0.3(4) . . . . ?
C11 C6 C7 C8 -179.2(3) . . . . ?
C5 C6 C7 C12 -179.0(3) . . . . ?
C11 C6 C7 C12 1.5(4) . . . . ?
C6 C7 C8 C9 1.5(4) . . . . ?
C12 C7 C8 C9 -179.2(3) . . . . ?
C6 C7 C8 C13 -177.9(3) . . . . ?
C12 C7 C8 C13 1.4(4) . . . . ?
C7 C8 C9 C10 -1.3(4) . . . . ?
C13 C8 C9 C10 178.1(3) . . . . ?
C7 C8 C9 C14 -179.5(3) . . . . ?
C13 C8 C9 C14 -0.1(4) . . . . ?
C6 C5 C10 C9 2.6(4) . . . . ?
C2 C5 C10 C9 -173.5(3) . . . . ?
C6 C5 C10 C15 -177.1(3) . . . . ?
C2 C5 C10 C15 6.9(4) . . . . ?
C8 C9 C10 C5 -0.7(4) . . . . ?
C14 C9 C10 C5 177.6(3) . . . . ?
C8 C9 C10 C15 179.0(3) . . . . ?
C14 C9 C10 C15 -2.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.105

#=== END of CIF

_database_code_depnum_ccdc_archive 'CCDC 989611'
