# 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_compound_2

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H56 Ce K N4 Si8'
_chemical_formula_weight         708.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c      '
_symmetry_Int_Tables_number      15

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                   19.6084(7)
_cell_length_b                   11.0986(4)
_cell_length_c                   18.1627(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.2270(10)
_cell_angle_gamma                90.00
_cell_volume                     3795.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(1)
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22

_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1476
_exptl_absorpt_coefficient_mu    1.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.6888
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      143(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            35784
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4365
_reflns_number_gt                4164
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0194P)²+2.8789P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4365
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0158
_refine_ls_wR_factor_ref         0.0419
_refine_ls_wR_factor_gt          0.0404
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_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
Ce1 Ce 0.5000 0.426921(9) 0.2500 0.02141(4) Uani 1 2 d S . .
K1 K 0.5000 0.5000 0.0000 0.04105(11) Uani 1 2 d S . .
Si1 Si 0.55899(2) 0.22656(4) 0.15072(2) 0.03063(9) Uani 1 1 d . . .
Si2 Si 0.40226(2) 0.26356(4) 0.07153(2) 0.03109(9) Uani 1 1 d . . .
Si3 Si 0.38865(2) 0.63820(4) 0.14093(3) 0.03692(10) Uani 1 1 d . . .
Si4 Si 0.36333(2) 0.58208(4) 0.29581(2) 0.03055(9) Uani 1 1 d . . .
N1 N 0.48015(6) 0.29805(11) 0.13728(7) 0.0292(2) Uani 1 1 d . . .
N2 N 0.40210(7) 0.56273(11) 0.22445(8) 0.0315(3) Uani 1 1 d . . .
C1 C 0.60125(12) 0.2448(2) 0.07078(12) 0.0570(5) Uani 1 1 d . . .
H1a H 0.5676 0.2200 0.0223 0.085 Uiso 1 1 calc R . .
H1b H 0.6439 0.1944 0.0809 0.085 Uiso 1 1 calc R . .
H1c H 0.6143 0.3294 0.0673 0.085 Uiso 1 1 calc R . .
C2 C 0.56199(12) 0.06326(15) 0.17537(14) 0.0530(5) Uani 1 1 d . . .
H2a H 0.5434 0.0514 0.2196 0.079 Uiso 1 1 calc R . .
H2b H 0.6112 0.0347 0.1880 0.079 Uiso 1 1 calc R . .
H2c H 0.5330 0.0178 0.1315 0.079 Uiso 1 1 calc R . .
C3 C 0.40070(13) 0.11469(17) 0.02322(12) 0.0596(6) Uani 1 1 d . . .
H3a H 0.4402 0.1104 0.0001 0.089 Uiso 1 1 calc R . .
H3b H 0.3557 0.1056 -0.0169 0.089 Uiso 1 1 calc R . .
H3c H 0.4054 0.0500 0.0610 0.089 Uiso 1 1 calc R . .
C4 C 0.32445(10) 0.2688(2) 0.11155(11) 0.0593(6) Uani 1 1 d . . .
H4a H 0.3275 0.2019 0.1476 0.089 Uiso 1 1 calc R . .
H4b H 0.2805 0.2617 0.0697 0.089 Uiso 1 1 calc R . .
H4c H 0.3245 0.3454 0.1384 0.089 Uiso 1 1 calc R . .
C5 C 0.30104(12) 0.6105(3) 0.06967(14) 0.0775(8) Uani 1 1 d . . .
H5a H 0.2936 0.5235 0.0619 0.116 Uiso 1 1 calc R . .
H5b H 0.3004 0.6488 0.0208 0.116 Uiso 1 1 calc R . .
H5c H 0.2631 0.6445 0.0888 0.116 Uiso 1 1 calc R . .
C6 C 0.40439(19) 0.80320(18) 0.14924(15) 0.0848(9) Uani 1 1 d . . .
H6a H 0.3671 0.8416 0.1675 0.127 Uiso 1 1 calc R . .
H6b H 0.4036 0.8362 0.0989 0.127 Uiso 1 1 calc R . .
H6c H 0.4508 0.8190 0.1857 0.127 Uiso 1 1 calc R . .
C7 C 0.35898(14) 0.74048(18) 0.32695(12) 0.0626(6) Uani 1 1 d . . .
H7a H 0.4063 0.7768 0.3384 0.094 Uiso 1 1 calc R . .
H7b H 0.3423 0.7422 0.3730 0.094 Uiso 1 1 calc R . .
H7c H 0.3260 0.7860 0.2859 0.094 Uiso 1 1 calc R . .
C8 C 0.27477(11) 0.5117(3) 0.27899(15) 0.0716(7) Uani 1 1 d . . .
H8a H 0.2403 0.5552 0.2381 0.107 Uiso 1 1 calc R . .
H8b H 0.2599 0.5151 0.3262 0.107 Uiso 1 1 calc R . .
H8c H 0.2771 0.4274 0.2638 0.107 Uiso 1 1 calc R . .
H9 H 0.6056(10) 0.2851(17) 0.2150(11) 0.045(5) Uiso 1 1 d . . .
H10 H 0.3888(9) 0.3503(16) 0.0128(10) 0.039(5) Uiso 1 1 d . . .
H11 H 0.4408(11) 0.5919(17) 0.1069(12) 0.050(6) Uiso 1 1 d . . .
H12 H 0.4096(9) 0.5200(16) 0.3616(10) 0.036(4) Uiso 1 1 d . . .


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
Ce1 N2 2.3820(12) 2_655 ?
Ce1 N2 2.3821(12) . ?
Ce1 N1 2.4379(12) 2_655 ?
Ce1 N1 2.4379(12) . ?
K1 N1 3.4546(12) . ?
K1 N1 3.4546(12) 5_665 ?
Si1 N1 1.6935(12) . ?
Si1 C2 1.8639(17) . ?
Si1 C1 1.8730(18) . ?
Si2 N1 1.6988(13) . ?
Si2 C4 1.865(2) . ?
Si2 C3 1.8670(19) . ?
Si3 N2 1.6878(13) . ?
Si3 C6 1.856(2) . ?
Si3 C5 1.865(2) . ?
Si4 N2 1.6897(13) . ?
Si4 C8 1.850(2) . ?
Si4 C7 1.8560(19) . ?

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
N2 Ce1 N2 101.49(6) 2_655 . ?
N2 Ce1 N1 106.07(4) 2_655 2_655 ?
N2 Ce1 N1 117.75(4) . 2_655 ?
N2 Ce1 N1 117.75(4) 2_655 . ?
N2 Ce1 N1 106.07(4) . . ?
N1 Ce1 N1 108.16(6) 2_655 . ?
N1 K1 N1 180.0 . 5_665 ?
N1 Si1 C2 117.16(8) . . ?
N1 Si1 C1 114.93(8) . . ?
C2 Si1 C1 107.45(10) . . ?
N1 Si2 C4 113.06(7) . . ?
N1 Si2 C3 115.04(8) . . ?
C4 Si2 C3 107.62(11) . . ?
N2 Si3 C6 115.84(9) . . ?
N2 Si3 C5 115.10(9) . . ?
C6 Si3 C5 108.61(14) . . ?
N2 Si4 C8 114.98(9) . . ?
N2 Si4 C7 115.03(8) . . ?
C8 Si4 C7 109.24(12) . . ?
Si1 N1 Si2 126.94(7) . . ?
Si1 N1 Ce1 103.22(6) . . ?
Si2 N1 Ce1 128.59(6) . . ?
Si1 N1 K1 97.22(5) . . ?
Si2 N1 K1 84.22(5) . . ?
Ce1 N1 K1 101.64(4) . . ?
Si3 N2 Si4 129.46(8) . . ?
Si3 N2 Ce1 113.84(6) . . ?
Si4 N2 Ce1 116.22(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.049
_database_code_depnum_ccdc_archive 'CCDC 1000019'
#######################################################################
#
#                 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_compound_4

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H46 Ce N2 O4'
_chemical_formula_weight         590.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c      '
_symmetry_Int_Tables_number      15

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                   12.4757(7)
_cell_length_b                   14.8427(9)
_cell_length_c                   16.6276(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.250(2)
_cell_angle_gamma                90.00
_cell_volume                     3060.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(1)
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05

_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      143(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            33179
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0085
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.65
_reflns_number_total             3552
_reflns_number_gt                3422
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0202P)²+3.2571P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3552
_refine_ls_number_parameters     187
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0450
_refine_ls_wR_factor_gt          0.0432
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.131
_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
Ce1 Ce 0.5000 0.301243(7) 0.7500 0.02531(4) Uani 1 2 d S . .
N1 N 0.47050(12) 0.44366(10) 0.65166(8) 0.0364(3) Uani 1 1 d . . .
O1 O 0.66457(9) 0.32844(9) 0.73885(8) 0.0400(3) Uani 1 1 d . . .
O2 O 0.52583(12) 0.21399(9) 0.84885(8) 0.0435(3) Uani 1 1 d . A .
C1 C 0.37751(17) 0.45169(16) 0.60501(13) 0.0522(5) Uani 1 1 d . . .
H1 H 0.3267 0.4060 0.6059 0.069 Uiso 1 1 calc R . .
C2 C 0.3532(2) 0.5251(2) 0.55528(15) 0.0685(7) Uani 1 1 d . . .
H2 H 0.2869 0.5286 0.5239 0.091 Uiso 1 1 calc R . .
C3 C 0.4270(2) 0.59193(17) 0.55261(15) 0.0704(7) Uani 1 1 d . . .
H3 H 0.4127 0.6415 0.5189 0.094 Uiso 1 1 calc R . .
C4 C 0.5225(2) 0.58463(16) 0.60052(15) 0.0690(7) Uani 1 1 d . . .
H4 H 0.5743 0.6296 0.6005 0.092 Uiso 1 1 calc R . .
C5 C 0.54114(18) 0.50959(14) 0.64896(12) 0.0497(5) Uani 1 1 d . . .
H5 H 0.6066 0.5052 0.6813 0.066 Uiso 1 1 calc R . .
C6 C 0.77193(15) 0.31504(19) 0.72447(14) 0.0571(6) Uani 1 1 d . . .
C7 C 0.7836(2) 0.3315(2) 0.63673(16) 0.0763(8) Uani 1 1 d . . .
H7a H 0.7395 0.2894 0.6041 0.114 Uiso 1 1 calc R . .
H7b H 0.8576 0.3237 0.6274 0.114 Uiso 1 1 calc R . .
H7c H 0.7610 0.3918 0.6226 0.114 Uiso 1 1 calc R . .
C8 C 0.8403(2) 0.3837(4) 0.7755(2) 0.150(2) Uani 1 1 d . . .
H8a H 0.8055 0.4415 0.7710 0.225 Uiso 1 1 calc R . .
H8b H 0.9100 0.3880 0.7565 0.225 Uiso 1 1 calc R . .
H8c H 0.8483 0.3649 0.8310 0.225 Uiso 1 1 calc R . .
C9 C 0.8026(3) 0.2193(3) 0.7456(3) 0.148(2) Uani 1 1 d . . .
H9a H 0.8042 0.2108 0.8029 0.221 Uiso 1 1 calc R . .
H9b H 0.8726 0.2067 0.7293 0.221 Uiso 1 1 calc R . .
H9c H 0.7506 0.1791 0.7180 0.221 Uiso 1 1 calc R . .
C10 C 0.54107(16) 0.14758(12) 0.90812(11) 0.0421(4) Uani 1 1 d DU . .
C11 C 0.5914(5) 0.0670(3) 0.8731(3) 0.0678(12) Uani 0.55 1 d PDU A 1
H11a H 0.5441 0.0443 0.8283 0.102 Uiso 0.55 1 calc PR A 1
H11b H 0.6034 0.0210 0.9138 0.102 Uiso 0.55 1 calc PR A 1
H11c H 0.6590 0.0839 0.8549 0.102 Uiso 0.55 1 calc PR A 1
C12 C 0.4348(5) 0.1257(5) 0.9391(5) 0.108(3) Uani 0.55 1 d PDU A 1
H12a H 0.4076 0.1784 0.9635 0.162 Uiso 0.55 1 calc PR A 1
H12b H 0.4451 0.0785 0.9787 0.162 Uiso 0.55 1 calc PR A 1
H12c H 0.3841 0.1063 0.8949 0.162 Uiso 0.55 1 calc PR A 1
C13 C 0.6225(7) 0.1861(4) 0.9751(4) 0.107(3) Uani 0.55 1 d PDU A 1
H13a H 0.6895 0.1980 0.9536 0.161 Uiso 0.55 1 calc PR A 1
H13b H 0.6342 0.1433 1.0184 0.161 Uiso 0.55 1 calc PR A 1
H13c H 0.5948 0.2411 0.9951 0.161 Uiso 0.55 1 calc PR A 1
C11' C 0.6565(5) 0.1183(6) 0.9227(6) 0.097(2) Uani 0.45 1 d PDU A 2
H11a' H 0.6803 0.0981 0.8727 0.146 Uiso 0.45 1 calc PR A 2
H11b' H 0.6630 0.0701 0.9613 0.146 Uiso 0.45 1 calc PR A 2
H11c' H 0.7003 0.1682 0.9433 0.146 Uiso 0.45 1 calc PR A 2
C12' C 0.4735(7) 0.0660(4) 0.8760(5) 0.096(2) Uani 0.45 1 d PDU A 2
H12a' H 0.3999 0.0841 0.8628 0.144 Uiso 0.45 1 calc PR A 2
H12b' H 0.4772 0.0199 0.9168 0.144 Uiso 0.45 1 calc PR A 2
H12c' H 0.5013 0.0429 0.8285 0.144 Uiso 0.45 1 calc PR A 2
C13' C 0.5003(10) 0.1808(6) 0.9837(4) 0.105(3) Uani 0.45 1 d PDU A 2
H13a' H 0.5412 0.2326 1.0033 0.158 Uiso 0.45 1 calc PR A 2
H13b' H 0.5076 0.1342 1.0239 0.158 Uiso 0.45 1 calc PR A 2
H13c' H 0.4256 0.1971 0.9725 0.158 Uiso 0.45 1 calc PR A 2


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
Ce1 O2 2.0897(13) 2_656 ?
Ce1 O2 2.0897(12) . ?
Ce1 O1 2.1203(12) . ?
Ce1 O1 2.1203(12) 2_656 ?
Ce1 N1 2.6733(14) 2_656 ?
Ce1 N1 2.6733(14) . ?
N1 C5 1.321(2) . ?
N1 C1 1.329(2) . ?
O1 C6 1.400(2) . ?
O2 C10 1.392(2) . ?
C1 C2 1.381(3) . ?
C2 C3 1.358(4) . ?
C3 C4 1.363(4) . ?
C4 C5 1.379(3) . ?
C6 C7 1.502(3) . ?
C6 C9 1.504(4) . ?
C6 C8 1.526(4) . ?
C10 C13' 1.490(6) . ?
C10 C11 1.498(4) . ?
C10 C11' 1.498(6) . ?
C10 C12 1.509(5) . ?
C10 C12' 1.537(6) . ?
C10 C13 1.533(5) . ?

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
O2 Ce1 O2 103.41(8) 2_656 . ?
O2 Ce1 O1 96.72(5) 2_656 . ?
O2 Ce1 O1 96.83(5) . . ?
O2 Ce1 O1 96.83(5) 2_656 2_656 ?
O2 Ce1 O1 96.72(6) . 2_656 ?
O1 Ce1 O1 158.05(8) . 2_656 ?
O2 Ce1 N1 165.99(5) 2_656 2_656 ?
O2 Ce1 N1 90.56(5) . 2_656 ?
O1 Ce1 N1 80.38(5) . 2_656 ?
O1 Ce1 N1 82.31(5) 2_656 2_656 ?
O2 Ce1 N1 90.56(5) 2_656 . ?
O2 Ce1 N1 165.99(5) . . ?
O1 Ce1 N1 82.31(5) . . ?
O1 Ce1 N1 80.38(5) 2_656 . ?
N1 Ce1 N1 75.49(6) 2_656 . ?
C5 N1 C1 117.20(17) . . ?
C5 N1 Ce1 123.96(12) . . ?
C1 N1 Ce1 118.76(13) . . ?
C6 O1 Ce1 160.27(15) . . ?
C10 O2 Ce1 173.22(13) . . ?
N1 C1 C2 122.8(2) . . ?
C3 C2 C1 119.4(2) . . ?
C2 C3 C4 118.4(2) . . ?
C3 C4 C5 119.1(2) . . ?
N1 C5 C4 123.2(2) . . ?
O1 C6 C7 109.77(19) . . ?
O1 C6 C9 108.5(2) . . ?
C7 C6 C9 109.4(3) . . ?
O1 C6 C8 107.3(2) . . ?
C7 C6 C8 108.9(3) . . ?
C9 C6 C8 112.9(4) . . ?
O2 C10 C13' 109.2(3) . . ?
O2 C10 C11 108.7(2) . . ?
C13' C10 C11 142.0(4) . . ?
O2 C10 C11' 112.0(3) . . ?
C13' C10 C11' 111.8(6) . . ?
C11 C10 C11' 52.8(4) . . ?
O2 C10 C12 109.7(3) . . ?
C13' C10 C12 52.4(5) . . ?
C11 C10 C12 112.5(4) . . ?
C11' C10 C12 138.4(4) . . ?
O2 C10 C12' 106.5(3) . . ?
C13' C10 C12' 109.2(6) . . ?
C11 C10 C12' 58.2(4) . . ?
C11' C10 C12' 108.0(5) . . ?
C12 C10 C12' 58.7(5) . . ?
O2 C10 C13 106.2(3) . . ?
C13' C10 C13 61.6(6) . . ?
C11 C10 C13 107.9(4) . . ?
C11' C10 C13 56.1(4) . . ?
C12 C10 C13 111.7(5) . . ?
C12' C10 C13 147.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.65
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.051

_shelxl_version_number           1997-3

_shelx_ins_file                  
;
TITL  mo_4286a_0m
CELL  0.71073 12.4757 14.8427 16.6276 90.000 96.250 90.000
ZERR  4 0.0007 0.0009 0.0009 0.000 0.002 0.000
LATT 7
SYMM    -X,    +Y, .50-Z
SFAC C H N O CE
UNIT 104 184 8 16 4
L.S. 8
ACTA
DFIX 1.54 0.010 C10 C11 C10 C12 C10 C13 C10 C11' C10 C12' C10 C13'
DELU C10 > C13'
SIMU C10 > C13'
WGHT    0.020200    3.257100
FVAR       0.08857   0.00000
CE1   5    0.500000    0.301239    0.750000    10.50000    0.02072    0.02710 =
         0.02789    0.00000    0.00241    0.00000
N1    3    0.470536    0.443763    0.651680    11.00000    0.03722    0.03963 =
         0.03164    0.00584   -0.00067   -0.00033
O1    4    0.664608    0.328479    0.738858    11.00000    0.02316    0.05128 =
         0.04629    0.00400    0.00514   -0.00142
O2    4    0.525835    0.213955    0.848846    11.00000    0.04941    0.03828 =
         0.04272    0.01365    0.00125   -0.00093
C1    1    0.377440    0.451709    0.605047    11.00000    0.04347    0.06463 =
         0.04580    0.01375   -0.00718   -0.00583
AFIX  43
H1    2    0.326597    0.406003    0.605967    11.00000   -1.33000
AFIX   0
C2    1    0.353179    0.525098    0.555290    11.00000    0.06011    0.08644 =
         0.05521    0.02480   -0.01405    0.01126
AFIX  43
H2    2    0.286871    0.528677    0.523946    11.00000   -1.33000
AFIX   0
C3    1    0.426956    0.591965    0.552532    11.00000    0.09786    0.04910 =
         0.05964    0.01918   -0.01133    0.00787
AFIX  43
H3    2    0.412696    0.641501    0.518812    11.00000   -1.33000
AFIX   0
C4    1    0.522542    0.584683    0.600460    11.00000    0.09457    0.04672 =
         0.06145    0.01534   -0.01246   -0.02022
AFIX  43
H4    2    0.574412    0.629683    0.600453    11.00000   -1.33000
AFIX   0
C5    1    0.541194    0.509564    0.648979    11.00000    0.05387    0.04833 =
         0.04397    0.01072   -0.00866   -0.01107
AFIX  43
H5    2    0.606679    0.505137    0.681294    11.00000   -1.33000
AFIX   0
C6    1    0.771829    0.314932    0.724469    11.00000    0.02266    0.10478 =
         0.04560    0.01288    0.00826    0.00261
C7    1    0.783669    0.331440    0.636759    11.00000    0.06522    0.10930 =
         0.05857    0.01225    0.02844    0.00105
AFIX 137
H7A   2    0.739115    0.289781    0.604028    11.00000   -1.50000
H7B   2    0.857631    0.323136    0.627459    11.00000   -1.50000
H7C   2    0.761828    0.391954    0.622726    11.00000   -1.50000
AFIX   0
C8    1    0.840268    0.383897    0.775455    11.00000    0.04364    0.31452 =
         0.09163   -0.06233    0.01758   -0.06812
AFIX 137
H8A   2    0.804648    0.441316    0.771896    11.00000   -1.50000
H8B   2    0.909449    0.389211    0.755639    11.00000   -1.50000
H8C   2    0.849678    0.364462    0.830842    11.00000   -1.50000
AFIX   0
C9    1    0.802549    0.219095    0.745802    11.00000    0.09903    0.19035 =
         0.16796    0.11250    0.07700    0.10334
AFIX 137
H9A   2    0.806102    0.211182    0.803332    11.00000   -1.50000
H9B   2    0.871660    0.206014    0.728208    11.00000   -1.50000
H9C   2    0.749474    0.178978    0.719468    11.00000   -1.50000
AFIX   0
C10   1    0.541013    0.147525    0.908120    11.00000    0.05526    0.03712 =
         0.03389    0.00967    0.00473    0.00693
PART 1
C11   1    0.591495    0.066974    0.872962    10.55000    0.09848    0.04476 =
         0.06165    0.00040    0.01270    0.01816
AFIX 137
H11A  2    0.544796    0.045002    0.827487    10.55000   -1.50000
H11B  2    0.602353    0.020576    0.913249    10.55000   -1.50000
H11C  2    0.659658    0.083769    0.855639    10.55000   -1.50000
AFIX   0
C12   1    0.434461    0.125384    0.938882    10.55000    0.10617    0.09280 =
         0.13639    0.06836    0.07140    0.02794
AFIX 137
H12A  2    0.409936    0.176462    0.967208    10.55000   -1.50000
H12B  2    0.443529    0.074795    0.974955    10.55000   -1.50000
H12C  2    0.382247    0.110832    0.894022    10.55000   -1.50000
AFIX   0
C13   1    0.622176    0.186091    0.975219    10.55000    0.16216    0.08087 =
         0.06487   -0.01829   -0.06143    0.03973
AFIX 137
H13A  2    0.689901    0.196342    0.954328    10.55000   -1.50000
H13B  2    0.632136    0.144081    1.019298    10.55000   -1.50000
H13C  2    0.595300    0.241992    0.994036    10.55000   -1.50000
AFIX   0
PART 2
C11'  1    0.656758    0.118311    0.922716    10.45000    0.06857    0.09752 =
         0.12334    0.03869   -0.00216    0.02733
AFIX 137
H11D  2    0.681258    0.099862    0.872484    10.45000   -1.50000
H11E  2    0.662900    0.068758    0.960039    10.45000   -1.50000
H11F  2    0.700098    0.167638    0.944954    10.45000   -1.50000
AFIX   0
C12'  1    0.473579    0.066193    0.876136    10.45000    0.13452    0.06192 =
         0.09096    0.02675   -0.01887   -0.03996
AFIX 137
H12D  2    0.399704    0.084163    0.863762    10.45000   -1.50000
H12E  2    0.478259    0.019750    0.916549    10.45000   -1.50000
H12F  2    0.500548    0.043739    0.828070    10.45000   -1.50000
AFIX   0
C13'  1    0.499858    0.180805    0.983724    10.45000    0.16675    0.10299 =
         0.05022    0.01304    0.04017    0.04813
AFIX 137
H13D  2    0.540782    0.232554    1.003433    10.45000   -1.50000
H13E  2    0.507051    0.134157    1.023943    10.45000   -1.50000
H13F  2    0.425274    0.197106    0.972414    10.45000   -1.50000
HKLF 4
END  
;
_database_code_depnum_ccdc_archive 'CCDC 1000020'
#######################################################################
#
#                 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_compound_5

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C172 H136 Ce2 O8'
_chemical_formula_weight         2611.05

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c a '
_symmetry_Int_Tables_number      54

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

_cell_length_a                   22.8092(9)
_cell_length_b                   22.1996(9)
_cell_length_c                   24.9446(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12630.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07

_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5392
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.7119
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            310384
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         27.58
_reflns_number_total             14581
_reflns_number_gt                9934
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0306P)²+117.1498P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14581
_refine_ls_number_parameters     840
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1309
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.059
_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
Ce1 Ce 0.2500 0.0000 0.603818(13) 0.01790(9) Uani 1 2 d S . .
O1 O 0.27735(16) -0.06800(15) 0.65681(12) 0.0233(7) Uani 1 1 d . . .
O2 O 0.32503(15) 0.03881(15) 0.56695(13) 0.0235(7) Uani 1 1 d . . .
C1 C 0.2882(2) -0.1017(2) 0.70107(18) 0.0245(10) Uani 1 1 d . . .
C2 C 0.2732(2) -0.1636(2) 0.70047(19) 0.0271(11) Uani 1 1 d . . .
C3 C 0.2826(3) -0.1970(2) 0.7467(2) 0.0324(12) Uani 1 1 d . . .
H3 H 0.2725 -0.2376 0.7471 0.043 Uiso 1 1 calc R . .
C4 C 0.3064(3) -0.1715(3) 0.7922(2) 0.0393(14) Uani 1 1 d . . .
H4 H 0.3117 -0.1946 0.8230 0.052 Uiso 1 1 calc R . .
C5 C 0.3222(3) -0.1114(3) 0.7918(2) 0.0355(13) Uani 1 1 d . . .
H5 H 0.3388 -0.0946 0.8224 0.047 Uiso 1 1 calc R . .
C6 C 0.3139(2) -0.0753(2) 0.74688(19) 0.0244(10) Uani 1 1 d . . .
C7 C 0.2499(3) -0.1940(2) 0.65142(17) 0.0232(9) Uani 1 1 d . . .
C8 C 0.1953(3) -0.1799(2) 0.6299(2) 0.0314(12) Uani 1 1 d . . .
H8 H 0.1726 -0.1501 0.6458 0.042 Uiso 1 1 calc R . .
C9 C 0.1743(3) -0.2098(2) 0.5850(2) 0.0337(12) Uani 1 1 d . . .
H9 H 0.1377 -0.1998 0.5710 0.045 Uiso 1 1 calc R . .
C10 C 0.2074(3) -0.2542(3) 0.5611(2) 0.0396(14) Uani 1 1 d . . .
H10 H 0.1932 -0.2746 0.5312 0.053 Uiso 1 1 calc R . .
C11 C 0.2620(3) -0.2683(3) 0.5818(2) 0.0425(16) Uani 1 1 d . . .
H11 H 0.2848 -0.2976 0.5652 0.057 Uiso 1 1 calc R . .
C12 C 0.2828(3) -0.2390(2) 0.6271(2) 0.0368(13) Uani 1 1 d . . .
H12 H 0.3190 -0.2497 0.6413 0.049 Uiso 1 1 calc R . .
C13 C 0.3322(2) -0.0108(2) 0.74785(18) 0.0234(10) Uani 1 1 d . . .
C14 C 0.3193(2) 0.0249(2) 0.79210(19) 0.0285(11) Uani 1 1 d . . .
H14 H 0.2987 0.0086 0.8208 0.038 Uiso 1 1 calc R . .
C15 C 0.3369(2) 0.0849(2) 0.7937(2) 0.0306(12) Uani 1 1 d . . .
H15 H 0.3276 0.1088 0.8232 0.041 Uiso 1 1 calc R . .
C16 C 0.3681(2) 0.1088(2) 0.7515(2) 0.0304(11) Uani 1 1 d . . .
H16 H 0.3789 0.1492 0.7519 0.040 Uiso 1 1 calc R . .
C17 C 0.3835(2) 0.0727(2) 0.7082(2) 0.0303(11) Uani 1 1 d . . .
H17 H 0.4064 0.0883 0.6807 0.040 Uiso 1 1 calc R . .
C18 C 0.3647(2) 0.0134(2) 0.70616(19) 0.0270(11) Uani 1 1 d . . .
H18 H 0.3739 -0.0103 0.6766 0.036 Uiso 1 1 calc R . .
C19 C 0.3505(2) 0.0683(2) 0.52534(18) 0.0234(10) Uani 1 1 d . . .
C20 C 0.4115(2) 0.0775(2) 0.52441(19) 0.0274(11) Uani 1 1 d . . .
C21 C 0.4359(3) 0.1068(3) 0.4798(2) 0.0333(12) Uani 1 1 d . . .
H21 H 0.4762 0.1133 0.4786 0.044 Uiso 1 1 calc R . .
C22 C 0.4015(3) 0.1261(3) 0.4377(2) 0.0360(13) Uani 1 1 d . . .
H22 H 0.4187 0.1442 0.4079 0.048 Uiso 1 1 calc R . .
C23 C 0.3424(3) 0.1186(2) 0.4399(2) 0.0295(11) Uani 1 1 d . . .
H23 H 0.3193 0.1325 0.4118 0.039 Uiso 1 1 calc R . .
C24 C 0.3155(2) 0.0904(2) 0.48366(18) 0.0242(10) Uani 1 1 d . . .
C25 C 0.4508(2) 0.0586(3) 0.5689(2) 0.0290(11) Uani 1 1 d . . .
C26 C 0.4509(2) 0.0002(3) 0.58861(19) 0.0297(10) Uani 1 1 d . . .
H26 H 0.4248 -0.0280 0.5748 0.039 Uiso 1 1 calc R . .
C27 C 0.4897(3) -0.0164(3) 0.6287(2) 0.0383(14) Uani 1 1 d . . .
H27 H 0.4896 -0.0559 0.6410 0.051 Uiso 1 1 calc R . .
C28 C 0.5278(3) 0.0237(3) 0.6506(2) 0.0411(14) Uani 1 1 d . . .
H28 H 0.5529 0.0120 0.6781 0.055 Uiso 1 1 calc R . .
C29 C 0.5286(3) 0.0820(3) 0.6314(2) 0.0424(15) Uani 1 1 d . . .
H29 H 0.5546 0.1099 0.6457 0.056 Uiso 1 1 calc R . .
C30 C 0.4904(2) 0.0991(3) 0.5907(2) 0.0362(13) Uani 1 1 d . . .
H30 H 0.4915 0.1384 0.5778 0.048 Uiso 1 1 calc R . .
C31 C 0.2509(2) 0.08582(19) 0.48554(17) 0.0207(9) Uani 1 1 d . . .
C32 C 0.2192(3) 0.0652(2) 0.44100(19) 0.0286(11) Uani 1 1 d . . .
H32 H 0.2392 0.0529 0.4104 0.038 Uiso 1 1 calc R . .
C33 C 0.1588(3) 0.0629(2) 0.4417(2) 0.0327(12) Uani 1 1 d . . .
H33 H 0.1385 0.0486 0.4119 0.043 Uiso 1 1 calc R . .
C34 C 0.1281(3) 0.0816(2) 0.4865(2) 0.0324(12) Uani 1 1 d . . .
H34 H 0.0874 0.0794 0.4872 0.043 Uiso 1 1 calc R . .
C35 C 0.1585(3) 0.1038(2) 0.5306(2) 0.0314(12) Uani 1 1 d . . .
H35 H 0.1381 0.1179 0.5603 0.042 Uiso 1 1 calc R . .
C36 C 0.2191(2) 0.1051(2) 0.53035(19) 0.0270(11) Uani 1 1 d . . .
H36 H 0.2391 0.1189 0.5604 0.036 Uiso 1 1 calc R . .
Ce2 Ce 0.2500 0.5000 0.370015(14) 0.01929(9) Uani 1 2 d S . .
O3 O 0.18181(16) 0.53302(16) 0.41890(13) 0.0258(7) Uani 1 1 d . . .
O4 O 0.29136(15) 0.57203(15) 0.32969(13) 0.0229(7) Uani 1 1 d . . .
C37 C 0.1511(2) 0.5499(2) 0.46249(19) 0.0253(10) Uani 1 1 d . . .
C38 C 0.0896(2) 0.5447(2) 0.46202(19) 0.0277(11) Uani 1 1 d . . .
C39 C 0.0587(3) 0.5612(2) 0.5082(2) 0.0339(12) Uani 1 1 d . . .
H39 H 0.0180 0.5576 0.5088 0.045 Uiso 1 1 calc R . .
C40 C 0.0874(3) 0.5826(3) 0.5526(2) 0.0379(13) Uani 1 1 d . . .
H40 H 0.0661 0.5926 0.5831 0.050 Uiso 1 1 calc R . .
C41 C 0.1475(3) 0.5895(2) 0.5524(2) 0.0330(13) Uani 1 1 d . . .
H41 H 0.1663 0.6048 0.5825 0.044 Uiso 1 1 calc R . .
C42 C 0.1806(2) 0.5736(2) 0.50712(18) 0.0253(10) Uani 1 1 d . . .
C43 C 0.0565(3) 0.5231(3) 0.4141(2) 0.0348(13) Uani 1 1 d . . .
C44 C 0.0120(3) 0.5581(3) 0.3928(3) 0.0466(16) Uani 1 1 d . . .
H44 H 0.0028 0.5950 0.4082 0.062 Uiso 1 1 calc R . .
C45 C -0.0194(3) 0.5375(4) 0.3477(3) 0.058(2) Uani 1 1 d . . .
H45 H -0.0486 0.5614 0.3328 0.077 Uiso 1 1 calc R . .
C46 C -0.0070(3) 0.4825(4) 0.3259(3) 0.060(2) Uani 1 1 d . . .
H46 H -0.0284 0.4690 0.2964 0.079 Uiso 1 1 calc R . .
C47 C 0.0368(3) 0.4466(4) 0.3469(3) 0.0525(19) Uani 1 1 d . . .
H47 H 0.0451 0.4093 0.3318 0.070 Uiso 1 1 calc R . .
C48 C 0.0682(3) 0.4670(3) 0.3909(2) 0.0420(15) Uani 1 1 d . . .
H48 H 0.0976 0.4429 0.4053 0.056 Uiso 1 1 calc R . .
C49 C 0.2451(3) 0.5834(2) 0.50830(18) 0.0246(10) Uani 1 1 d . . .
C50 C 0.2781(3) 0.5696(2) 0.5536(2) 0.0317(12) Uani 1 1 d . . .
H50 H 0.2597 0.5523 0.5831 0.042 Uiso 1 1 calc R . .
C51 C 0.3376(3) 0.5809(3) 0.5556(2) 0.0352(13) Uani 1 1 d . . .
H51 H 0.3591 0.5703 0.5858 0.047 Uiso 1 1 calc R . .
C52 C 0.3652(3) 0.6079(3) 0.5129(2) 0.0357(13) Uani 1 1 d . . .
H52 H 0.4052 0.6156 0.5141 0.047 Uiso 1 1 calc R . .
C53 C 0.3328(3) 0.6236(3) 0.4682(2) 0.0361(13) Uani 1 1 d . . .
H53 H 0.3509 0.6431 0.4396 0.048 Uiso 1 1 calc R . .
C54 C 0.2740(3) 0.6106(2) 0.4655(2) 0.0295(11) Uani 1 1 d . . .
H54 H 0.2531 0.6202 0.4346 0.039 Uiso 1 1 calc R . .
C55 C 0.3136(2) 0.5965(2) 0.28448(18) 0.0227(10) Uani 1 1 d . . .
C56 C 0.3207(2) 0.6597(2) 0.28037(19) 0.0266(11) Uani 1 1 d . . .
C57 C 0.3380(3) 0.6838(2) 0.2313(2) 0.0346(13) Uani 1 1 d . . .
H57 H 0.3418 0.7253 0.2279 0.046 Uiso 1 1 calc R . .
C58 C 0.3495(3) 0.6476(3) 0.1875(2) 0.0376(14) Uani 1 1 d . . .
H58 H 0.3591 0.6647 0.1546 0.050 Uiso 1 1 calc R . .
C59 C 0.3467(3) 0.5858(3) 0.1930(2) 0.0329(12) Uani 1 1 d . . .
H59 H 0.3563 0.5613 0.1640 0.044 Uiso 1 1 calc R . .
C60 C 0.3297(2) 0.5595(2) 0.24114(18) 0.0240(10) Uani 1 1 d . . .
C61 C 0.3131(2) 0.7006(2) 0.32718(19) 0.0264(11) Uani 1 1 d . . .
C62 C 0.2623(3) 0.7019(2) 0.3567(2) 0.0332(13) Uani 1 1 d . . .
H62 H 0.2310 0.6769 0.3477 0.044 Uiso 1 1 calc R . .
C63 C 0.2579(3) 0.7418(2) 0.4010(2) 0.0367(14) Uani 1 1 d . . .
H63 H 0.2239 0.7423 0.4216 0.049 Uiso 1 1 calc R . .
C64 C 0.3037(3) 0.7796(2) 0.4135(2) 0.0403(15) Uani 1 1 d . . .
H64 H 0.3009 0.8055 0.4427 0.054 Uiso 1 1 calc R . .
C65 C 0.3537(3) 0.7790(3) 0.3828(2) 0.0409(15) Uani 1 1 d . . .
H65 H 0.3844 0.8049 0.3910 0.054 Uiso 1 1 calc R . .
C66 C 0.3585(3) 0.7403(2) 0.3399(2) 0.0333(12) Uani 1 1 d . . .
H66 H 0.3924 0.7406 0.3192 0.044 Uiso 1 1 calc R . .
C67 C 0.3293(2) 0.4927(2) 0.24580(18) 0.0228(10) Uani 1 1 d . . .
C68 C 0.3117(2) 0.4565(3) 0.2028(2) 0.0310(12) Uani 1 1 d . . .
H68 H 0.2979 0.4746 0.1716 0.041 Uiso 1 1 calc R . .
C69 C 0.3142(3) 0.3940(3) 0.2056(2) 0.0372(13) Uani 1 1 d . . .
H69 H 0.3022 0.3710 0.1764 0.049 Uiso 1 1 calc R . .
C70 C 0.3343(3) 0.3662(3) 0.2510(2) 0.0379(13) Uani 1 1 d . . .
H70 H 0.3354 0.3244 0.2529 0.050 Uiso 1 1 calc R . .
C71 C 0.3532(3) 0.4007(3) 0.2946(2) 0.0345(12) Uani 1 1 d . . .
H71 H 0.3670 0.3821 0.3255 0.046 Uiso 1 1 calc R . .
C72 C 0.3509(2) 0.4633(2) 0.2911(2) 0.0277(11) Uani 1 1 d . . .
H72 H 0.3642 0.4862 0.3198 0.037 Uiso 1 1 calc R . .
C73 C -0.0562(4) 0.2338(4) 0.9254(4) 0.073(2) Uani 1 1 d . . .
H73 H -0.0823 0.2173 0.9008 0.097 Uiso 1 1 calc R . .
C74 C -0.0739(4) 0.2409(4) 0.9779(5) 0.078(3) Uani 1 1 d . . .
H74 H -0.1119 0.2308 0.9880 0.104 Uiso 1 1 calc R . .
C75 C -0.0350(4) 0.2633(4) 1.0153(4) 0.071(2) Uani 1 1 d . . .
H75 H -0.0457 0.2673 1.0511 0.094 Uiso 1 1 calc R . .
C76 C 0.0199(4) 0.2793(3) 0.9982(4) 0.071(2) Uani 1 1 d . . .
H76 H 0.0462 0.2949 1.0231 0.094 Uiso 1 1 calc R . .
C77 C 0.0381(4) 0.2732(3) 0.9455(4) 0.063(2) Uani 1 1 d . . .
C78 C -0.0025(4) 0.2500(3) 0.9088(4) 0.063(2) Uani 1 1 d . . .
H78 H 0.0077 0.2458 0.8729 0.084 Uiso 1 1 calc R . .
C79 C 0.0973(4) 0.2901(4) 0.9286(5) 0.091(3) Uani 1 1 d . . .
H79a H 0.1053 0.3308 0.9395 0.137 Uiso 1 1 calc R . .
H79b H 0.1003 0.2872 0.8903 0.137 Uiso 1 1 calc R . .
H79c H 0.1253 0.2635 0.9449 0.137 Uiso 1 1 calc R . .
C80 C 0.0000 0.3231(7) 0.7500 0.132(8) Uani 1 2 d S . .
H80a H 0.0284 0.3375 0.7753 0.197 Uiso 0.50 1 calc PR . .
H80b H -0.0382 0.3375 0.7599 0.197 Uiso 0.50 1 calc PR . .
H80c H 0.0098 0.3375 0.7148 0.197 Uiso 0.50 1 calc PR . .
C81 C 0.0000 0.2562(6) 0.7500 0.073(4) Uani 1 2 d S . .
C82 C 0.0469(4) 0.2247(5) 0.7334(4) 0.080(3) Uani 1 1 d . . .
H82 H 0.0801 0.2458 0.7225 0.106 Uiso 1 1 calc R . .
C83 C 0.0481(5) 0.1630(5) 0.7319(4) 0.093(3) Uani 1 1 d . . .
H83 H 0.0810 0.1431 0.7188 0.124 Uiso 1 1 calc R . .
C84 C 0.0000 0.1302(7) 0.7500 0.099(6) Uani 1 2 d S . .
H84 H 0.0000 0.0883 0.7500 0.132 Uiso 1 2 calc SR . .
C85 C 0.5116(5) 0.7339(4) 0.2860(4) 0.070(4) Uani 0.50 1 d PGU A -1
C86 C 0.5010(10) 0.6891(3) 0.2480(5) 0.056(3) Uani 0.50 1 d PGU A -1
H86 H 0.5043 0.6488 0.2575 0.074 Uiso 0.50 1 calc PR A -1
C87 C 0.4855(9) 0.7049(5) 0.1957(5) 0.087(5) Uani 0.50 1 d PGU A -1
H87 H 0.4784 0.6750 0.1704 0.115 Uiso 0.50 1 calc PR A -1
C88 C 0.4806(7) 0.7655(6) 0.1815(4) 0.095(6) Uani 0.50 1 d PGU A -1
H88 H 0.4703 0.7760 0.1466 0.127 Uiso 0.50 1 calc PR A -1
C89 C 0.4912(12) 0.8102(4) 0.2195(6) 0.135(8) Uani 0.50 1 d PGU A -1
H89 H 0.4880 0.8506 0.2100 0.179 Uiso 0.50 1 calc PR A -1
C90 C 0.5067(10) 0.7945(4) 0.2717(6) 0.096(6) Uani 0.50 1 d PGU A -1
H90 H 0.5138 0.8243 0.2971 0.128 Uiso 0.50 1 calc PR A -1
C91 C 0.5287(7) 0.7165(8) 0.3437(4) 0.122(8) Uani 0.50 1 d PGU A -1
H91a H 0.5344 0.7524 0.3646 0.183 Uiso 0.50 1 calc PR A -1
H91b H 0.5644 0.6936 0.3431 0.183 Uiso 0.50 1 calc PR A -1
H91c H 0.4980 0.6927 0.3593 0.183 Uiso 0.50 1 calc PR A -1


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
Ce1 O1 2.101(3) 4 ?
Ce1 O1 2.101(3) . ?
Ce1 O2 2.125(3) . ?
Ce1 O2 2.125(3) 4 ?
Ce1 C36 3.049(5) 4 ?
Ce1 C36 3.049(5) . ?
O1 C1 1.357(6) . ?
O2 C19 1.358(6) . ?
C1 C6 1.413(7) . ?
C1 C2 1.416(7) . ?
C2 C3 1.387(7) . ?
C2 C7 1.495(7) . ?
C3 C4 1.380(8) . ?
C4 C5 1.382(8) . ?
C5 C6 1.391(7) . ?
C6 C13 1.490(7) . ?
C7 C12 1.389(7) . ?
C7 C8 1.392(8) . ?
C8 C9 1.387(7) . ?
C9 C10 1.378(8) . ?
C10 C11 1.382(9) . ?
C11 C12 1.388(8) . ?
C13 C18 1.385(7) . ?
C13 C14 1.391(7) . ?
C14 C15 1.392(8) . ?
C15 C16 1.378(8) . ?
C16 C17 1.389(7) . ?
C17 C18 1.386(7) . ?
C19 C24 1.399(7) . ?
C19 C20 1.407(7) . ?
C20 C21 1.404(7) . ?
C20 C25 1.489(7) . ?
C21 C22 1.379(8) . ?
C22 C23 1.361(8) . ?
C23 C24 1.398(7) . ?
C24 C31 1.478(8) . ?
C25 C26 1.385(8) . ?
C25 C30 1.386(8) . ?
C26 C27 1.386(7) . ?
C27 C28 1.358(9) . ?
C28 C29 1.380(9) . ?
C29 C30 1.389(8) . ?
C31 C36 1.399(7) . ?
C31 C32 1.403(7) . ?
C32 C33 1.379(8) . ?
C33 C34 1.381(8) . ?
C34 C35 1.390(8) . ?
C35 C36 1.383(8) . ?
Ce2 O3 2.108(3) 4_565 ?
Ce2 O3 2.108(3) . ?
Ce2 O4 2.112(3) . ?
Ce2 O4 2.112(3) 4_565 ?
O3 C37 1.347(6) . ?
O4 C55 1.351(5) . ?
C37 C42 1.403(7) . ?
C37 C38 1.408(8) . ?
C38 C39 1.399(7) . ?
C38 C43 1.492(7) . ?
C39 C40 1.370(8) . ?
C40 C41 1.380(9) . ?
C41 C42 1.403(7) . ?
C42 C49 1.489(8) . ?
C43 C44 1.384(9) . ?
C43 C48 1.399(9) . ?
C44 C45 1.410(10) . ?
C45 C46 1.366(11) . ?
C46 C47 1.382(11) . ?
C47 C48 1.386(8) . ?
C49 C50 1.392(7) . ?
C49 C54 1.392(7) . ?
C50 C51 1.382(8) . ?
C51 C52 1.372(8) . ?
C52 C53 1.384(8) . ?
C53 C54 1.373(8) . ?
C55 C60 1.408(7) . ?
C55 C56 1.415(7) . ?
C56 C57 1.394(7) . ?
C56 C61 1.489(7) . ?
C57 C58 1.381(8) . ?
C58 C59 1.380(8) . ?
C59 C60 1.391(7) . ?
C60 C67 1.487(7) . ?
C61 C62 1.374(8) . ?
C61 C66 1.397(8) . ?
C62 C63 1.419(7) . ?
C63 C64 1.377(9) . ?
C64 C65 1.374(9) . ?
C65 C66 1.376(8) . ?
C67 C72 1.393(7) . ?
C67 C68 1.399(7) . ?
C68 C69 1.390(8) . ?
C69 C70 1.370(9) . ?
C70 C71 1.397(8) . ?
C71 C72 1.395(7) . ?
C73 C78 1.342(12) . ?
C73 C74 1.378(13) . ?
C74 C75 1.381(13) . ?
C75 C76 1.370(12) . ?
C76 C77 1.384(12) . ?
C77 C78 1.401(12) . ?
C77 C79 1.464(12) . ?
C80 C81 1.485(19) . ?
C81 C82 1.342(11) . ?
C81 C82 1.342(11) 7_557 ?
C82 C83 1.372(14) . ?
C83 C84 1.392(14) . ?
C84 C83 1.392(14) 7_557 ?
C85 C86 1.3950 . ?
C85 C90 1.3950 . ?
C85 C91 1.5402 . ?
C86 C87 1.3949 . ?
C87 C88 1.3950 . ?
C88 C89 1.3950 . ?
C89 C90 1.3949 . ?

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
O1 Ce1 O1 102.04(17) 4 . ?
O1 Ce1 O2 102.71(13) 4 . ?
O1 Ce1 O2 108.93(13) . . ?
O1 Ce1 O2 108.93(13) 4 4 ?
O1 Ce1 O2 102.71(13) . 4 ?
O2 Ce1 O2 128.72(17) . 4 ?
O1 Ce1 C36 175.10(14) 4 4 ?
O1 Ce1 C36 76.11(13) . 4 ?
O2 Ce1 C36 82.19(13) . 4 ?
O2 Ce1 C36 67.39(14) 4 4 ?
O1 Ce1 C36 76.11(13) 4 . ?
O1 Ce1 C36 175.10(14) . . ?
O2 Ce1 C36 67.39(14) . . ?
O2 Ce1 C36 82.19(14) 4 . ?
C36 Ce1 C36 106.09(19) 4 . ?
C1 O1 Ce1 164.3(3) . . ?
C19 O2 Ce1 150.5(3) . . ?
O1 C1 C6 120.3(4) . . ?
O1 C1 C2 118.9(4) . . ?
C6 C1 C2 120.8(4) . . ?
C3 C2 C1 118.1(5) . . ?
C3 C2 C7 119.7(5) . . ?
C1 C2 C7 122.2(4) . . ?
C4 C3 C2 121.8(5) . . ?
C3 C4 C5 119.5(5) . . ?
C4 C5 C6 121.8(5) . . ?
C5 C6 C1 117.9(5) . . ?
C5 C6 C13 120.1(5) . . ?
C1 C6 C13 121.9(4) . . ?
C12 C7 C8 118.4(5) . . ?
C12 C7 C2 119.3(5) . . ?
C8 C7 C2 122.2(5) . . ?
C9 C8 C7 120.9(5) . . ?
C10 C9 C8 120.1(6) . . ?
C9 C10 C11 119.6(5) . . ?
C10 C11 C12 120.4(6) . . ?
C7 C12 C11 120.5(6) . . ?
C18 C13 C14 119.2(5) . . ?
C18 C13 C6 120.6(4) . . ?
C14 C13 C6 120.1(4) . . ?
C15 C14 C13 120.6(5) . . ?
C16 C15 C14 119.6(5) . . ?
C15 C16 C17 120.2(5) . . ?
C18 C17 C16 119.9(5) . . ?
C13 C18 C17 120.4(5) . . ?
O2 C19 C24 119.6(5) . . ?
O2 C19 C20 120.3(4) . . ?
C24 C19 C20 120.0(5) . . ?
C21 C20 C19 118.2(5) . . ?
C21 C20 C25 118.9(5) . . ?
C19 C20 C25 122.9(5) . . ?
C22 C21 C20 121.5(5) . . ?
C23 C22 C21 119.6(5) . . ?
C22 C23 C24 121.4(5) . . ?
C23 C24 C19 119.2(5) . . ?
C23 C24 C31 119.5(5) . . ?
C19 C24 C31 121.3(4) . . ?
C26 C25 C30 117.9(5) . . ?
C26 C25 C20 122.0(5) . . ?
C30 C25 C20 120.1(5) . . ?
C25 C26 C27 120.3(6) . . ?
C28 C27 C26 121.7(6) . . ?
C27 C28 C29 118.9(6) . . ?
C28 C29 C30 120.1(6) . . ?
C25 C30 C29 121.1(6) . . ?
C36 C31 C32 117.7(5) . . ?
C36 C31 C24 121.4(4) . . ?
C32 C31 C24 120.8(4) . . ?
C33 C32 C31 121.2(5) . . ?
C32 C33 C34 120.3(5) . . ?
C33 C34 C35 119.6(5) . . ?
C36 C35 C34 120.2(5) . . ?
C35 C36 C31 121.0(5) . . ?
C35 C36 Ce1 102.3(3) . . ?
C31 C36 Ce1 97.3(3) . . ?
O3 Ce2 O3 109.31(19) 4_565 . ?
O3 Ce2 O4 102.08(13) 4_565 . ?
O3 Ce2 O4 109.99(13) . . ?
O3 Ce2 O4 109.99(13) 4_565 4_565 ?
O3 Ce2 O4 102.08(13) . 4_565 ?
O4 Ce2 O4 123.10(17) . 4_565 ?
C37 O3 Ce2 161.4(3) . . ?
C55 O4 Ce2 150.5(3) . . ?
O3 C37 C42 119.7(5) . . ?
O3 C37 C38 119.3(4) . . ?
C42 C37 C38 121.0(5) . . ?
C39 C38 C37 118.3(5) . . ?
C39 C38 C43 119.3(5) . . ?
C37 C38 C43 122.5(5) . . ?
C40 C39 C38 121.0(6) . . ?
C39 C40 C41 120.7(5) . . ?
C40 C41 C42 120.7(5) . . ?
C41 C42 C37 118.3(5) . . ?
C41 C42 C49 118.6(5) . . ?
C37 C42 C49 123.0(4) . . ?
C44 C43 C48 118.7(6) . . ?
C44 C43 C38 119.8(6) . . ?
C48 C43 C38 121.4(6) . . ?
C43 C44 C45 119.8(7) . . ?
C46 C45 C44 120.2(7) . . ?
C45 C46 C47 120.8(7) . . ?
C46 C47 C48 119.2(7) . . ?
C47 C48 C43 121.3(7) . . ?
C50 C49 C54 117.6(5) . . ?
C50 C49 C42 121.2(5) . . ?
C54 C49 C42 121.0(5) . . ?
C51 C50 C49 121.3(5) . . ?
C52 C51 C50 120.1(5) . . ?
C51 C52 C53 119.4(6) . . ?
C54 C53 C52 120.5(5) . . ?
C53 C54 C49 121.0(5) . . ?
O4 C55 C60 120.3(4) . . ?
O4 C55 C56 120.2(4) . . ?
C60 C55 C56 119.6(4) . . ?
C57 C56 C55 118.4(5) . . ?
C57 C56 C61 119.2(5) . . ?
C55 C56 C61 122.3(4) . . ?
C58 C57 C56 121.7(5) . . ?
C59 C58 C57 119.5(5) . . ?
C58 C59 C60 121.0(5) . . ?
C59 C60 C55 119.4(5) . . ?
C59 C60 C67 119.2(4) . . ?
C55 C60 C67 121.4(4) . . ?
C62 C61 C66 119.4(5) . . ?
C62 C61 C56 122.0(5) . . ?
C66 C61 C56 118.5(5) . . ?
C61 C62 C63 119.3(6) . . ?
C64 C63 C62 120.3(6) . . ?
C65 C64 C63 119.8(5) . . ?
C64 C65 C66 120.4(6) . . ?
C65 C66 C61 120.8(6) . . ?
C72 C67 C68 117.0(5) . . ?
C72 C67 C60 121.8(4) . . ?
C68 C67 C60 121.0(4) . . ?
C69 C68 C67 121.5(5) . . ?
C70 C69 C68 120.3(5) . . ?
C69 C70 C71 120.0(5) . . ?
C72 C71 C70 119.1(5) . . ?
C67 C72 C71 122.0(5) . . ?
C78 C73 C74 122.0(10) . . ?
C73 C74 C75 119.6(9) . . ?
C76 C75 C74 118.1(9) . . ?
C75 C76 C77 122.9(9) . . ?
C76 C77 C78 117.3(8) . . ?
C76 C77 C79 121.6(9) . . ?
C78 C77 C79 121.1(9) . . ?
C73 C78 C77 120.0(9) . . ?
C82 C81 C82 117.4(13) . 7_557 ?
C82 C81 C80 121.3(7) . . ?
C82 C81 C80 121.3(7) 7_557 . ?
C81 C82 C83 123.0(11) . . ?
C82 C83 C84 119.8(12) . . ?
C83 C84 C83 117.0(14) 7_557 . ?
C86 C85 C90 120.0 . . ?
C86 C85 C91 120.0 . . ?
C90 C85 C91 120.0 . . ?
C87 C86 C85 120.0 . . ?
C86 C87 C88 120.0 . . ?
C89 C88 C87 120.0 . . ?
C90 C89 C88 120.0 . . ?
C89 C90 C85 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         7.797
_refine_diff_density_min         -3.055
_refine_diff_density_rms         0.144
_database_code_depnum_ccdc_archive 'CCDC 1000021'
#######################################################################
#
#                 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_compound_7

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H32 Ce2 F40 O10'
_chemical_formula_weight         2001.13

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7924(6)
_cell_length_b                   12.1912(7)
_cell_length_c                   14.0728(7)
_cell_angle_alpha                82.987(2)
_cell_angle_beta                 81.252(2)
_cell_angle_gamma                66.025(2)
_cell_volume                     1668.43(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3.7828
_cell_measurement_theta_min      23.5775
_cell_measurement_theta_max      100.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   0.8016
_exptl_transmission_factor_max   0.9491
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.039
_exptl_absorpt_coefficient_mu    1.519
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30711
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.467
_diffrn_reflns_theta_max         28.340
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8223
_reflns_number_gt                5654
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'APEX2 v2013.4-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0090P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8223
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0594
_refine_ls_goodness_of_fit_ref   0.810
_refine_ls_restrained_S_all      0.810
_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_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
Ce1 Ce 0.07152(2) 0.92658(2) 0.37693(2) 0.01638(6) Uani 1 1 d . . . . .
F10 F 0.3227(2) 0.57794(19) 0.22766(16) 0.0353(6) Uani 1 1 d . . . . .
F11 F 0.5435(2) 0.57158(19) 0.10700(16) 0.0344(6) Uani 1 1 d . . . . .
F12 F 0.7366(2) 0.62682(19) 0.16854(15) 0.0307(6) Uani 1 1 d . . . . .
F13 F 0.7146(2) 0.67583(18) 0.35473(16) 0.0298(6) Uani 1 1 d . . . . .
F14 F 0.4987(2) 0.67312(18) 0.47865(15) 0.0290(5) Uani 1 1 d . . . . .
F20 F 0.0087(2) 0.62619(18) 0.32027(14) 0.0260(5) Uani 1 1 d . . . . .
F21 F 0.1464(2) 0.43075(18) 0.21951(16) 0.0303(6) Uani 1 1 d . . . . .
F22 F 0.1641(2) 0.4522(2) 0.02413(17) 0.0449(7) Uani 1 1 d . . . . .
F23 F 0.0450(3) 0.6700(2) -0.06905(16) 0.0533(8) Uani 1 1 d . . . . .
F24 F -0.0896(2) 0.8664(2) 0.03059(17) 0.0412(6) Uani 1 1 d . . . . .
F30 F 0.1480(2) 0.9079(2) 0.08629(17) 0.0383(6) Uani 1 1 d . . . . .
F31 F 0.2858(3) 0.7668(2) -0.05975(18) 0.0523(7) Uani 1 1 d . . . . .
F32 F 0.5559(2) 0.7167(2) -0.10936(17) 0.0513(7) Uani 1 1 d . . . . .
F33 F 0.6874(2) 0.8056(2) -0.00911(16) 0.0387(6) Uani 1 1 d . . . . .
F34 F 0.5522(2) 0.94014(19) 0.13957(15) 0.0307(6) Uani 1 1 d . . . . .
F40 F 0.49472(19) 0.92328(17) 0.37380(15) 0.0249(5) Uani 1 1 d . . . . .
F41 F 0.57935(19) 1.08812(19) 0.27485(15) 0.0283(5) Uani 1 1 d . . . . .
F42 F 0.4435(2) 1.32448(18) 0.30761(15) 0.0291(6) Uani 1 1 d . . . . .
F43 F 0.2159(2) 1.39577(18) 0.43716(15) 0.0292(5) Uani 1 1 d . . . . .
F44 F 0.13041(19) 1.23327(17) 0.53615(14) 0.0235(5) Uani 1 1 d . . . . .
O01 O -0.0488(2) 1.1413(2) 0.31652(18) 0.0238(6) Uani 1 1 d . . . . .
O40 O 0.1176(2) 1.0111(2) 0.50089(17) 0.0179(6) Uani 1 1 d . . . . .
O10 O 0.1860(2) 0.7533(2) 0.43082(18) 0.0229(6) Uani 1 1 d . . . . .
O20 O -0.0421(2) 0.8936(2) 0.28626(17) 0.0222(6) Uani 1 1 d . . . . .
O30 O 0.2285(2) 0.9520(2) 0.27966(17) 0.0227(6) Uani 1 1 d . . . . .
C10 C 0.2786(3) 0.6331(3) 0.4252(3) 0.0255(10) Uani 1 1 d . . . . .
H10A H 0.2354 0.5866 0.4029 0.031 Uiso 1 1 calc R U . . .
H10B H 0.3053 0.5995 0.4886 0.031 Uiso 1 1 calc R U . . .
C11 C 0.4033(3) 0.6254(3) 0.3568(3) 0.0205(9) Uani 1 1 d . . . . .
C12 C 0.4191(4) 0.6010(3) 0.2623(3) 0.0240(9) Uani 1 1 d . . . . .
C13 C 0.5294(4) 0.6001(3) 0.1985(3) 0.0236(9) Uani 1 1 d . . . . .
C14 C 0.6285(4) 0.6267(3) 0.2298(3) 0.0222(9) Uani 1 1 d . . . . .
C15 C 0.6168(4) 0.6513(3) 0.3237(3) 0.0205(9) Uani 1 1 d . . . . .
C16 C 0.5063(4) 0.6495(3) 0.3859(3) 0.0207(9) Uani 1 1 d . . . . .
C01 C -0.1587(4) 1.1872(3) 0.2581(3) 0.0338(11) Uani 1 1 d . . . . .
H01A H -0.2146 1.1405 0.2714 0.041 Uiso 1 1 calc R U . . .
H01B H -0.1245 1.1854 0.1902 0.041 Uiso 1 1 calc R U . . .
C02 C -0.2377(4) 1.3123(4) 0.2853(4) 0.0495(14) Uani 1 1 d . . . . .
H02A H -0.2989 1.3150 0.3439 0.059 Uiso 1 1 calc R U . . .
H02B H -0.2904 1.3613 0.2342 0.059 Uiso 1 1 calc R U . . .
C03 C -0.1270(4) 1.3539(3) 0.3005(3) 0.0279(10) Uani 1 1 d . . . . .
H03A H -0.0939 1.3868 0.2406 0.033 Uiso 1 1 calc R U . . .
H03B H -0.1605 1.4141 0.3477 0.033 Uiso 1 1 calc R U . . .
C20 C -0.1259(4) 0.8622(3) 0.2361(3) 0.0247(10) Uani 1 1 d . . . . .
H20A H -0.1728 0.9296 0.1925 0.030 Uiso 1 1 calc R U . . .
H20B H -0.1945 0.8465 0.2820 0.030 Uiso 1 1 calc R U . . .
C21 C -0.0461(3) 0.7536(3) 0.1798(3) 0.0176(8) Uani 1 1 d . . . . .
C22 C 0.0174(3) 0.6402(3) 0.2233(3) 0.0175(8) Uani 1 1 d . . . . .
C23 C 0.0877(4) 0.5389(3) 0.1737(3) 0.0208(9) Uani 1 1 d . . . . .
C24 C 0.0972(4) 0.5492(4) 0.0741(3) 0.0298(10) Uani 1 1 d . . . . .
C25 C 0.0367(4) 0.6596(4) 0.0280(3) 0.0301(10) Uani 1 1 d . . . . .
C26 C -0.0322(4) 0.7595(4) 0.0801(3) 0.0273(10) Uani 1 1 d . . . . .
C30 C 0.2634(4) 1.0128(3) 0.1962(3) 0.0242(9) Uani 1 1 d . . . . .
H30A H 0.3170 1.0542 0.2119 0.029 Uiso 1 1 calc R U . . .
H30B H 0.1808 1.0730 0.1729 0.029 Uiso 1 1 calc R U . . .
C31 C 0.3437(4) 0.9298(3) 0.1175(3) 0.0189(8) Uani 1 1 d . . . . .
C32 C 0.2824(4) 0.8822(3) 0.0643(3) 0.0232(9) Uani 1 1 d . . . . .
C33 C 0.3514(4) 0.8113(4) -0.0110(3) 0.0298(10) Uani 1 1 d . . . . .
C34 C 0.4876(4) 0.7858(4) -0.0365(3) 0.0303(10) Uani 1 1 d . . . . .
C35 C 0.5535(4) 0.8302(3) 0.0156(3) 0.0257(9) Uani 1 1 d . . . . .
C36 C 0.4824(4) 0.8989(3) 0.0911(3) 0.0194(9) Uani 1 1 d . . . . .
C40 C 0.2541(3) 0.9848(3) 0.5151(3) 0.0192(9) Uani 1 1 d . . . . .
H40A H 0.3115 0.9041 0.4961 0.023 Uiso 1 1 calc R U . . .
H40B H 0.2592 0.9867 0.5831 0.023 Uiso 1 1 calc R U . . .
C41 C 0.3080(3) 1.0730(3) 0.4579(2) 0.0155(8) Uani 1 1 d . . . . .
C42 C 0.4222(3) 1.0400(3) 0.3911(3) 0.0161(8) Uani 1 1 d . . . . .
C43 C 0.4667(3) 1.1233(3) 0.3401(3) 0.0180(8) Uani 1 1 d . . . . .
C44 C 0.3987(4) 1.2435(3) 0.3553(3) 0.0199(9) Uani 1 1 d . . . . .
C45 C 0.2842(4) 1.2788(3) 0.4211(3) 0.0181(8) Uani 1 1 d . . . . .
C46 C 0.2416(3) 1.1944(3) 0.4708(2) 0.0154(8) Uani 1 1 d . . . . .
C04 C -0.0178(4) 1.2410(3) 0.3364(3) 0.0267(10) Uani 1 1 d . . . . .
H04A H 0.0708 1.2336 0.3037 0.032 Uiso 1 1 calc R U . . .
H04B H -0.0163 1.2417 0.4051 0.032 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
Ce1 O20 2.073(2) . ?
Ce1 O10 2.082(2) . ?
Ce1 O30 2.111(2) . ?
Ce1 O40 2.339(2) . ?
Ce1 O40 2.385(2) 2_576 ?
Ce1 O01 2.508(2) . ?
Ce1 Ce1 3.9023(5) 2_576 ?
F10 C12 1.351(4) . ?
F11 C13 1.345(4) . ?
F12 C14 1.342(4) . ?
F13 C15 1.349(4) . ?
F14 C16 1.354(4) . ?
F20 C22 1.347(4) . ?
F21 C23 1.339(4) . ?
F22 C24 1.330(4) . ?
F23 C25 1.349(4) . ?
F24 C26 1.350(4) . ?
F30 C32 1.347(4) . ?
F31 C33 1.348(4) . ?
F32 C34 1.335(4) . ?
F33 C35 1.350(4) . ?
F34 C36 1.354(4) . ?
F40 C42 1.348(4) . ?
F41 C43 1.355(4) . ?
F42 C44 1.336(4) . ?
F43 C45 1.342(4) . ?
F44 C46 1.348(4) . ?
O01 C01 1.428(4) . ?
O01 C04 1.453(4) . ?
O40 C40 1.416(4) . ?
O40 Ce1 2.385(2) 2_576 ?
O10 C10 1.402(4) . ?
O20 C20 1.415(4) . ?
O30 C30 1.397(4) . ?
C10 C11 1.507(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.368(5) . ?
C11 C16 1.387(5) . ?
C12 C13 1.374(5) . ?
C13 C14 1.379(5) . ?
C14 C15 1.368(5) . ?
C15 C16 1.374(5) . ?
C01 C02 1.478(5) . ?
C01 H01A 0.9700 . ?
C01 H01B 0.9700 . ?
C02 C03 1.527(5) . ?
C02 H02A 0.9700 . ?
C02 H02B 0.9700 . ?
C03 C04 1.494(5) . ?
C03 H03A 0.9700 . ?
C03 H03B 0.9700 . ?
C20 C21 1.499(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.381(5) . ?
C21 C26 1.384(5) . ?
C22 C23 1.370(5) . ?
C23 C24 1.383(5) . ?
C24 C25 1.364(5) . ?
C25 C26 1.375(5) . ?
C30 C31 1.508(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.380(5) . ?
C31 C36 1.389(5) . ?
C32 C33 1.372(5) . ?
C33 C34 1.371(5) . ?
C34 C35 1.380(5) . ?
C35 C36 1.365(5) . ?
C40 C41 1.516(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.379(5) . ?
C41 C46 1.379(5) . ?
C42 C43 1.376(5) . ?
C43 C44 1.374(5) . ?
C44 C45 1.374(5) . ?
C45 C46 1.367(5) . ?
C04 H04A 0.9700 . ?
C04 H04B 0.9700 . ?

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
O20 Ce1 O10 101.67(9) . . ?
O20 Ce1 O30 102.42(9) . . ?
O10 Ce1 O30 97.56(9) . . ?
O20 Ce1 O40 158.55(8) . . ?
O10 Ce1 O40 91.40(9) . . ?
O30 Ce1 O40 92.50(8) . . ?
O20 Ce1 O40 91.96(8) . 2_576 ?
O10 Ce1 O40 101.31(9) . 2_576 ?
O30 Ce1 O40 153.42(8) . 2_576 ?
O40 Ce1 O40 68.62(8) . 2_576 ?
O20 Ce1 O01 83.62(8) . . ?
O10 Ce1 O01 174.34(8) . . ?
O30 Ce1 O01 79.17(9) . . ?
O40 Ce1 O01 84.17(8) . . ?
O40 Ce1 O01 80.38(8) 2_576 . ?
O20 Ce1 Ce1 125.36(7) . 2_576 ?
O10 Ce1 Ce1 97.73(7) . 2_576 ?
O30 Ce1 Ce1 124.95(7) . 2_576 ?
O40 Ce1 Ce1 34.69(5) . 2_576 ?
O40 Ce1 Ce1 33.93(5) 2_576 2_576 ?
O01 Ce1 Ce1 80.62(6) . 2_576 ?
C01 O01 C04 108.3(3) . . ?
C01 O01 Ce1 126.7(2) . . ?
C04 O01 Ce1 125.0(2) . . ?
C40 O40 Ce1 120.2(2) . . ?
C40 O40 Ce1 124.5(2) . 2_576 ?
Ce1 O40 Ce1 111.38(8) . 2_576 ?
C10 O10 Ce1 155.7(2) . . ?
C20 O20 Ce1 171.7(2) . . ?
C30 O30 Ce1 147.4(2) . . ?
O10 C10 C11 110.2(3) . . ?
O10 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
O10 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C16 116.0(4) . . ?
C12 C11 C10 123.0(3) . . ?
C16 C11 C10 120.9(4) . . ?
F10 C12 C11 119.9(3) . . ?
F10 C12 C13 117.1(4) . . ?
C11 C12 C13 123.1(4) . . ?
F11 C13 C12 121.2(3) . . ?
F11 C13 C14 119.6(4) . . ?
C12 C13 C14 119.1(4) . . ?
F12 C14 C15 120.2(3) . . ?
F12 C14 C13 120.1(4) . . ?
C15 C14 C13 119.7(4) . . ?
F13 C15 C14 119.8(3) . . ?
F13 C15 C16 120.7(3) . . ?
C14 C15 C16 119.5(3) . . ?
F14 C16 C15 118.0(3) . . ?
F14 C16 C11 119.5(3) . . ?
C15 C16 C11 122.5(4) . . ?
O01 C01 C02 104.6(3) . . ?
O01 C01 H01A 110.8 . . ?
C02 C01 H01A 110.8 . . ?
O01 C01 H01B 110.8 . . ?
C02 C01 H01B 110.8 . . ?
H01A C01 H01B 108.9 . . ?
C01 C02 C03 103.0(3) . . ?
C01 C02 H02A 111.2 . . ?
C03 C02 H02A 111.2 . . ?
C01 C02 H02B 111.2 . . ?
C03 C02 H02B 111.2 . . ?
H02A C02 H02B 109.1 . . ?
C04 C03 C02 103.1(3) . . ?
C04 C03 H03A 111.1 . . ?
C02 C03 H03A 111.1 . . ?
C04 C03 H03B 111.1 . . ?
C02 C03 H03B 111.1 . . ?
H03A C03 H03B 109.1 . . ?
O20 C20 C21 112.4(3) . . ?
O20 C20 H20A 109.1 . . ?
C21 C20 H20A 109.1 . . ?
O20 C20 H20B 109.1 . . ?
C21 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
C22 C21 C26 115.1(4) . . ?
C22 C21 C20 122.6(3) . . ?
C26 C21 C20 122.3(4) . . ?
F20 C22 C23 117.2(3) . . ?
F20 C22 C21 119.0(3) . . ?
C23 C22 C21 123.8(4) . . ?
F21 C23 C22 121.4(3) . . ?
F21 C23 C24 119.7(3) . . ?
C22 C23 C24 118.9(4) . . ?
F22 C24 C25 120.5(4) . . ?
F22 C24 C23 120.2(4) . . ?
C25 C24 C23 119.3(4) . . ?
F23 C25 C24 119.5(4) . . ?
F23 C25 C26 120.3(4) . . ?
C24 C25 C26 120.2(4) . . ?
F24 C26 C25 117.6(4) . . ?
F24 C26 C21 119.8(4) . . ?
C25 C26 C21 122.6(4) . . ?
O30 C30 C31 112.6(3) . . ?
O30 C30 H30A 109.1 . . ?
C31 C30 H30A 109.1 . . ?
O30 C30 H30B 109.1 . . ?
C31 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C32 C31 C36 115.3(3) . . ?
C32 C31 C30 121.8(3) . . ?
C36 C31 C30 122.9(3) . . ?
F30 C32 C33 118.4(3) . . ?
F30 C32 C31 118.5(3) . . ?
C33 C32 C31 123.1(4) . . ?
F31 C33 C34 120.0(4) . . ?
F31 C33 C32 120.2(4) . . ?
C34 C33 C32 119.8(3) . . ?
F32 C34 C33 120.3(4) . . ?
F32 C34 C35 120.6(4) . . ?
C33 C34 C35 119.1(4) . . ?
F33 C35 C36 120.8(3) . . ?
F33 C35 C34 119.5(4) . . ?
C36 C35 C34 119.7(4) . . ?
F34 C36 C35 117.2(3) . . ?
F34 C36 C31 119.8(3) . . ?
C35 C36 C31 123.0(3) . . ?
O40 C40 C41 112.3(3) . . ?
O40 C40 H40A 109.2 . . ?
C41 C40 H40A 109.2 . . ?
O40 C40 H40B 109.2 . . ?
C41 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
C42 C41 C46 116.0(3) . . ?
C42 C41 C40 123.9(3) . . ?
C46 C41 C40 120.1(3) . . ?
F40 C42 C43 117.6(3) . . ?
F40 C42 C41 120.5(3) . . ?
C43 C42 C41 121.9(3) . . ?
F41 C43 C44 118.9(3) . . ?
F41 C43 C42 120.6(3) . . ?
C44 C43 C42 120.5(3) . . ?
F42 C44 C45 120.6(3) . . ?
F42 C44 C43 120.7(3) . . ?
C45 C44 C43 118.6(3) . . ?
F43 C45 C46 120.4(3) . . ?
F43 C45 C44 119.7(3) . . ?
C46 C45 C44 119.9(3) . . ?
F44 C46 C45 117.6(3) . . ?
F44 C46 C41 119.4(3) . . ?
C45 C46 C41 123.0(3) . . ?
O01 C04 C03 107.1(3) . . ?
O01 C04 H04A 110.3 . . ?
C03 C04 H04A 110.3 . . ?
O01 C04 H04B 110.3 . . ?
C03 C04 H04B 110.3 . . ?
H04A C04 H04B 108.5 . . ?

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
Ce1 O10 C10 C11 45.7(6) . . . . ?
O10 C10 C11 C12 -96.3(4) . . . . ?
O10 C10 C11 C16 80.2(4) . . . . ?
C16 C11 C12 F10 -179.3(3) . . . . ?
C10 C11 C12 F10 -2.6(5) . . . . ?
C16 C11 C12 C13 -0.1(6) . . . . ?
C10 C11 C12 C13 176.5(3) . . . . ?
F10 C12 C13 F11 -3.1(5) . . . . ?
C11 C12 C13 F11 177.7(3) . . . . ?
F10 C12 C13 C14 178.1(3) . . . . ?
C11 C12 C13 C14 -1.1(6) . . . . ?
F11 C13 C14 F12 1.5(5) . . . . ?
C12 C13 C14 F12 -179.7(3) . . . . ?
F11 C13 C14 C15 -177.6(3) . . . . ?
C12 C13 C14 C15 1.2(6) . . . . ?
F12 C14 C15 F13 0.0(5) . . . . ?
C13 C14 C15 F13 179.1(3) . . . . ?
F12 C14 C15 C16 -179.2(3) . . . . ?
C13 C14 C15 C16 -0.1(6) . . . . ?
F13 C15 C16 F14 0.2(5) . . . . ?
C14 C15 C16 F14 179.4(3) . . . . ?
F13 C15 C16 C11 179.6(3) . . . . ?
C14 C15 C16 C11 -1.2(6) . . . . ?
C12 C11 C16 F14 -179.3(3) . . . . ?
C10 C11 C16 F14 4.0(5) . . . . ?
C12 C11 C16 C15 1.3(5) . . . . ?
C10 C11 C16 C15 -175.4(3) . . . . ?
C04 O01 C01 C02 -29.1(4) . . . . ?
Ce1 O01 C01 C02 150.5(3) . . . . ?
O01 C01 C02 C03 37.5(4) . . . . ?
C01 C02 C03 C04 -31.6(5) . . . . ?
O20 C20 C21 C22 67.2(4) . . . . ?
O20 C20 C21 C26 -113.6(4) . . . . ?
C26 C21 C22 F20 -179.8(3) . . . . ?
C20 C21 C22 F20 -0.5(5) . . . . ?
C26 C21 C22 C23 -1.2(5) . . . . ?
C20 C21 C22 C23 178.1(3) . . . . ?
F20 C22 C23 F21 -0.7(5) . . . . ?
C21 C22 C23 F21 -179.4(3) . . . . ?
F20 C22 C23 C24 179.1(3) . . . . ?
C21 C22 C23 C24 0.4(6) . . . . ?
F21 C23 C24 F22 0.2(5) . . . . ?
C22 C23 C24 F22 -179.6(3) . . . . ?
F21 C23 C24 C25 179.8(3) . . . . ?
C22 C23 C24 C25 0.0(6) . . . . ?
F22 C24 C25 F23 0.0(6) . . . . ?
C23 C24 C25 F23 -179.6(3) . . . . ?
F22 C24 C25 C26 -179.9(3) . . . . ?
C23 C24 C25 C26 0.4(6) . . . . ?
F23 C25 C26 F24 -0.2(5) . . . . ?
C24 C25 C26 F24 179.8(3) . . . . ?
F23 C25 C26 C21 178.7(3) . . . . ?
C24 C25 C26 C21 -1.4(6) . . . . ?
C22 C21 C26 F24 -179.5(3) . . . . ?
C20 C21 C26 F24 1.2(5) . . . . ?
C22 C21 C26 C25 1.7(5) . . . . ?
C20 C21 C26 C25 -177.6(3) . . . . ?
Ce1 O30 C30 C31 -116.8(4) . . . . ?
O30 C30 C31 C32 75.1(4) . . . . ?
O30 C30 C31 C36 -107.1(4) . . . . ?
C36 C31 C32 F30 179.6(3) . . . . ?
C30 C31 C32 F30 -2.3(5) . . . . ?
C36 C31 C32 C33 -1.4(5) . . . . ?
C30 C31 C32 C33 176.6(4) . . . . ?
F30 C32 C33 F31 -1.5(5) . . . . ?
C31 C32 C33 F31 179.6(3) . . . . ?
F30 C32 C33 C34 178.5(3) . . . . ?
C31 C32 C33 C34 -0.5(6) . . . . ?
F31 C33 C34 F32 -0.2(6) . . . . ?
C32 C33 C34 F32 179.8(3) . . . . ?
F31 C33 C34 C35 -178.7(3) . . . . ?
C32 C33 C34 C35 1.3(6) . . . . ?
F32 C34 C35 F33 1.5(6) . . . . ?
C33 C34 C35 F33 -180.0(3) . . . . ?
F32 C34 C35 C36 -178.8(3) . . . . ?
C33 C34 C35 C36 -0.3(6) . . . . ?
F33 C35 C36 F34 -0.2(5) . . . . ?
C34 C35 C36 F34 -179.9(3) . . . . ?
F33 C35 C36 C31 178.0(3) . . . . ?
C34 C35 C36 C31 -1.7(6) . . . . ?
C32 C31 C36 F34 -179.3(3) . . . . ?
C30 C31 C36 F34 2.7(5) . . . . ?
C32 C31 C36 C35 2.5(5) . . . . ?
C30 C31 C36 C35 -175.5(3) . . . . ?
Ce1 O40 C40 C41 90.0(3) . . . . ?
Ce1 O40 C40 C41 -114.4(3) 2_576 . . . ?
O40 C40 C41 C42 -122.1(4) . . . . ?
O40 C40 C41 C46 57.6(4) . . . . ?
C46 C41 C42 F40 179.5(3) . . . . ?
C40 C41 C42 F40 -0.8(5) . . . . ?
C46 C41 C42 C43 -0.3(5) . . . . ?
C40 C41 C42 C43 179.4(3) . . . . ?
F40 C42 C43 F41 0.2(5) . . . . ?
C41 C42 C43 F41 -180.0(3) . . . . ?
F40 C42 C43 C44 -179.0(3) . . . . ?
C41 C42 C43 C44 0.8(5) . . . . ?
F41 C43 C44 F42 -0.9(5) . . . . ?
C42 C43 C44 F42 178.3(3) . . . . ?
F41 C43 C44 C45 179.7(3) . . . . ?
C42 C43 C44 C45 -1.1(5) . . . . ?
F42 C44 C45 F43 0.6(5) . . . . ?
C43 C44 C45 F43 -180.0(3) . . . . ?
F42 C44 C45 C46 -178.5(3) . . . . ?
C43 C44 C45 C46 0.9(5) . . . . ?
F43 C45 C46 F44 -0.5(5) . . . . ?
C44 C45 C46 F44 178.6(3) . . . . ?
F43 C45 C46 C41 -179.6(3) . . . . ?
C44 C45 C46 C41 -0.5(5) . . . . ?
C42 C41 C46 F44 -178.9(3) . . . . ?
C40 C41 C46 F44 1.4(5) . . . . ?
C42 C41 C46 C45 0.2(5) . . . . ?
C40 C41 C46 C45 -179.6(3) . . . . ?
C01 O01 C04 C03 8.5(4) . . . . ?
Ce1 O01 C04 C03 -171.1(2) . . . . ?
C02 C03 C04 O01 14.7(4) . . . . ?

_refine_diff_density_max         1.464
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.127

_shelxl_version_number           2013-3



_database_code_depnum_ccdc_archive 'CCDC 1000022'
#######################################################################
#
#                 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_compound_6

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C118 H168 Ce2 D6 O12'
_chemical_formula_weight         2070.85

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1       '
_symmetry_Int_Tables_number      2

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

_cell_length_a                   13.6271(2)
_cell_length_b                   14.2125(2)
_cell_length_c                   15.8924(2)
_cell_angle_alpha                68.7980(10)
_cell_angle_beta                 69.1490(10)
_cell_angle_gamma                72.8070(10)
_cell_volume                     2632.04(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(1)
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.067

_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1094
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.6090
_exptl_absorpt_correction_T_max  0.8053
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         Imus
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Apex II Duo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            34295
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         28.28
_reflns_number_total             12996
_reflns_number_gt                10901
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0516P)²+1.3761P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12996
_refine_ls_number_parameters     644
_refine_ls_number_restraints     1157
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0957
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.002
_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
C01 C 0.1524(2) 0.5597(2) 0.5335(2) 0.0272(6) Uani 1 1 d U . .
H01A H 0.1529 0.5114 0.5966 0.033 Uiso 1 1 calc R . .
H01B H 0.1263 0.6300 0.5406 0.033 Uiso 1 1 calc R . .
O1 O 0.07832(14) 0.53801(14) 0.50192(12) 0.0180(4) Uani 1 1 d U . .
Ce1 Ce 0.063045(12) 0.523649(11) 0.364447(10) 0.01634(5) Uani 1 1 d U . .
C02 C 0.2662(2) 0.5528(2) 0.4710(2) 0.0238(6) Uani 1 1 d U . .
O2 O 0.21473(15) 0.54850(15) 0.28065(13) 0.0233(4) Uani 1 1 d U . .
C03 C 0.3387(2) 0.4583(2) 0.4852(2) 0.0255(6) Uani 1 1 d U . .
O3 O 0.03659(16) 0.45386(15) 0.28021(14) 0.0250(4) Uani 1 1 d U . .
O4 O -0.02486(16) 0.67303(14) 0.32100(13) 0.0220(4) Uani 1 1 d U . .
C04 C 0.3010(3) 0.3620(2) 0.5560(2) 0.0341(7) Uani 1 1 d U . .
H04A H 0.3414 0.3023 0.5330 0.051 Uiso 1 1 calc R . .
H04B H 0.2246 0.3686 0.5647 0.051 Uiso 1 1 calc R . .
H04C H 0.3126 0.3526 0.6162 0.051 Uiso 1 1 calc R . .
C05 C 0.4467(2) 0.4542(2) 0.4334(2) 0.0260(6) Uani 1 1 d U . .
O5 O 0.16166(16) 0.34262(14) 0.42559(15) 0.0269(5) Uani 1 1 d U . .
C06 C 0.5276(3) 0.3550(2) 0.4481(2) 0.0338(7) Uani 1 1 d U . .
H06A H 0.4960 0.3043 0.5052 0.051 Uiso 1 1 calc R . .
H06B H 0.5910 0.3678 0.4547 0.051 Uiso 1 1 calc R . .
H06C H 0.5484 0.3285 0.3940 0.051 Uiso 1 1 calc R . .
C101 C 0.427(2) 0.0370(12) -0.0510(16) 0.128(4) Uani 0.50 1 d PGU A -1
H101 D 0.380(2) 0.0478(12) -0.0868(16) 0.153 Uiso 0.50 1 calc PRU A -1
C102 C 0.387(2) 0.0274(12) 0.0447(16) 0.128(4) Uani 0.50 1 d PGU A -1
H102 D 0.312(2) 0.0315(15) 0.0743(17) 0.153 Uiso 0.50 1 calc PRU A -1
C103 C 0.456(2) 0.0116(12) 0.0970(16) 0.128(4) Uani 0.50 1 d PGU A -1
H103 D 0.429(2) 0.0050(14) 0.1624(16) 0.153 Uiso 0.50 1 calc PRU A -1
C104 C 0.565(2) 0.0056(12) 0.0536(16) 0.128(4) Uani 0.50 1 d PGU A -1
H104 D 0.613(2) -0.0052(15) 0.0894(17) 0.153 Uiso 0.50 1 calc PRU A -1
C105 C 0.605(2) 0.0152(12) -0.0421(16) 0.128(4) Uani 0.50 1 d PGU A -1
H105 D 0.680(2) 0.0111(14) -0.0717(17) 0.153 Uiso 0.50 1 calc PRU A -1
C106 C 0.536(2) 0.0310(11) -0.0944(16) 0.128(4) Uani 0.50 1 d PGU A -1
H106 D 0.563(2) 0.0376(14) -0.1598(16) 0.153 Uiso 0.50 1 calc PRU A -1
C07 C 0.4812(2) 0.5441(2) 0.3682(2) 0.0252(6) Uani 1 1 d U . .
C08 C 0.5983(2) 0.5360(3) 0.3126(2) 0.0332(7) Uani 1 1 d U . .
H08A H 0.6098 0.6022 0.2659 0.050 Uiso 1 1 calc R . .
H08B H 0.6183 0.4829 0.2806 0.050 Uiso 1 1 calc R . .
H08C H 0.6423 0.5176 0.3554 0.050 Uiso 1 1 calc R . .
C09 C 0.4090(2) 0.6382(2) 0.3541(2) 0.0252(6) Uani 1 1 d U . .
C10 C 0.4448(3) 0.7369(2) 0.2879(2) 0.0374(8) Uani 1 1 d U . .
H10A H 0.5206 0.7312 0.2807 0.056 Uiso 1 1 calc R . .
H10B H 0.4023 0.7943 0.3135 0.056 Uiso 1 1 calc R . .
H10C H 0.4348 0.7491 0.2264 0.056 Uiso 1 1 calc R . .
C11 C 0.3003(2) 0.6409(2) 0.4042(2) 0.0246(6) Uani 1 1 d U . .
C12 C 0.2199(3) 0.7393(2) 0.3853(2) 0.0336(7) Uani 1 1 d U . .
H12A H 0.1493 0.7231 0.4005 0.050 Uiso 1 1 calc R . .
H12B H 0.2416 0.7780 0.3188 0.050 Uiso 1 1 calc R . .
H12C H 0.2164 0.7807 0.4243 0.050 Uiso 1 1 calc R . .
C13 C 0.3107(2) 0.5669(2) 0.2097(2) 0.0294(7) Uani 1 1 d U . .
H13A H 0.3691 0.5491 0.2392 0.035 Uiso 1 1 calc R . .
H13B H 0.3026 0.6411 0.1752 0.035 Uiso 1 1 calc R . .
C14 C 0.3416(2) 0.5053(2) 0.1400(2) 0.0235(6) Uani 1 1 d U . .
C15 C 0.2805(2) 0.5322(2) 0.0770(2) 0.0250(6) Uani 1 1 d U . .
C16 C 0.1864(3) 0.6203(2) 0.0784(2) 0.0366(8) Uani 1 1 d U . .
H16A H 0.1997 0.6740 0.0182 0.055 Uiso 1 1 calc R . .
H16B H 0.1762 0.6484 0.1295 0.055 Uiso 1 1 calc R . .
H16C H 0.1219 0.5958 0.0882 0.055 Uiso 1 1 calc R . .
C17 C 0.3072(2) 0.4776(2) 0.0118(2) 0.0261(6) Uani 1 1 d U . .
C18 C 0.2389(3) 0.5075(3) -0.0540(2) 0.0399(8) Uani 1 1 d U . .
H18A H 0.1759 0.4752 -0.0221 0.060 Uiso 1 1 calc R . .
H18B H 0.2806 0.4844 -0.1099 0.060 Uiso 1 1 calc R . .
H18C H 0.2159 0.5825 -0.0729 0.060 Uiso 1 1 calc R . .
C19 C 0.3957(2) 0.3961(2) 0.0086(2) 0.0256(6) Uani 1 1 d U . .
C20 C 0.4233(3) 0.3348(3) -0.0598(2) 0.0377(8) Uani 1 1 d U . .
H20A H 0.3575 0.3319 -0.0700 0.057 Uiso 1 1 calc R . .
H20B H 0.4597 0.2649 -0.0340 0.057 Uiso 1 1 calc R . .
H20C H 0.4704 0.3679 -0.1197 0.057 Uiso 1 1 calc R . .
C21 C 0.4580(2) 0.3705(2) 0.0700(2) 0.0240(6) Uani 1 1 d U . .
C22 C 0.5548(3) 0.2836(2) 0.0657(2) 0.0339(8) Uani 1 1 d U . .
H22A H 0.5324 0.2183 0.1056 0.051 Uiso 1 1 calc R . .
H22B H 0.6071 0.2957 0.0880 0.051 Uiso 1 1 calc R . .
H22C H 0.5873 0.2807 0.0007 0.051 Uiso 1 1 calc R . .
C23 C 0.4305(2) 0.4234(2) 0.1372(2) 0.0237(6) Uani 1 1 d U . .
C24 C 0.4970(3) 0.3892(3) 0.2051(2) 0.0340(7) Uani 1 1 d U . .
H24A H 0.5687 0.4046 0.1709 0.051 Uiso 1 1 calc R . .
H24B H 0.5025 0.3150 0.2352 0.051 Uiso 1 1 calc R . .
H24C H 0.4629 0.4258 0.2531 0.051 Uiso 1 1 calc R . .
C25 C 0.0453(3) 0.4092(2) 0.2113(2) 0.0260(6) Uani 1 1 d U . .
H25A H 0.1148 0.4155 0.1629 0.031 Uiso 1 1 calc R . .
H25B H -0.0122 0.4466 0.1803 0.031 Uiso 1 1 calc R . .
C26 C 0.0369(2) 0.2961(2) 0.25427(19) 0.0223(6) Uani 1 1 d U . .
C27 C -0.0640(2) 0.2697(2) 0.30065(19) 0.0223(6) Uani 1 1 d U . .
C28 C -0.1653(3) 0.3505(2) 0.3015(2) 0.0310(7) Uani 1 1 d U . .
H28A H -0.1474 0.4189 0.2792 0.046 Uiso 1 1 calc R . .
H28B H -0.2130 0.3396 0.3657 0.046 Uiso 1 1 calc R . .
H28C H -0.2011 0.3454 0.2601 0.046 Uiso 1 1 calc R . .
C29 C -0.0727(2) 0.1659(2) 0.3453(2) 0.0238(6) Uani 1 1 d U . .
C30 C -0.1818(3) 0.1363(3) 0.3926(2) 0.0350(8) Uani 1 1 d U . .
H30A H -0.1804 0.0725 0.3812 0.052 Uiso 1 1 calc R . .
H30B H -0.2356 0.1913 0.3667 0.052 Uiso 1 1 calc R . .
H30C H -0.2000 0.1259 0.4603 0.052 Uiso 1 1 calc R . .
C31 C 0.0192(2) 0.0896(2) 0.3427(2) 0.0235(6) Uani 1 1 d U . .
C32 C 0.0093(3) -0.0213(2) 0.3919(2) 0.0334(7) Uani 1 1 d U . .
H32A H -0.0437 -0.0265 0.4535 0.050 Uiso 1 1 calc R . .
H32B H 0.0787 -0.0622 0.4004 0.050 Uiso 1 1 calc R . .
H32C H -0.0136 -0.0472 0.3540 0.050 Uiso 1 1 calc R . .
C33 C 0.1205(2) 0.1152(2) 0.2925(2) 0.0243(6) Uani 1 1 d U . .
C34 C 0.2190(3) 0.0309(2) 0.2837(3) 0.0340(7) Uani 1 1 d U . .
H34A H 0.2793 0.0599 0.2351 0.051 Uiso 1 1 calc R . .
H34B H 0.2051 -0.0224 0.2663 0.051 Uiso 1 1 calc R . .
H34C H 0.2363 0.0008 0.3439 0.051 Uiso 1 1 calc R . .
C35 C 0.1299(2) 0.2188(2) 0.2489(2) 0.0232(6) Uani 1 1 d U . .
C36 C 0.2387(3) 0.2456(3) 0.1923(3) 0.0374(8) Uani 1 1 d U . .
H36A H 0.2912 0.2044 0.2272 0.056 Uiso 1 1 calc R . .
H36B H 0.2353 0.3188 0.1813 0.056 Uiso 1 1 calc R . .
H36C H 0.2602 0.2308 0.1319 0.056 Uiso 1 1 calc R . .
C37 C -0.0759(2) 0.7704(2) 0.27530(19) 0.0227(6) Uani 1 1 d U . .
H37A H -0.0653 0.8235 0.2962 0.027 Uiso 1 1 calc R . .
H37B H -0.1538 0.7718 0.2943 0.027 Uiso 1 1 calc R . .
C38 C -0.0344(2) 0.79702(19) 0.16869(19) 0.0205(6) Uani 1 1 d U . .
C39 C -0.0825(2) 0.7682(2) 0.1196(2) 0.0243(6) Uani 1 1 d U . .
C40 C -0.1665(3) 0.7016(3) 0.1722(2) 0.0359(8) Uani 1 1 d U . .
H40A H -0.1579 0.6629 0.2351 0.054 Uiso 1 1 calc R . .
H40B H -0.1579 0.6535 0.1377 0.054 Uiso 1 1 calc R . .
H40C H -0.2379 0.7452 0.1779 0.054 Uiso 1 1 calc R . .
C41 C -0.0498(3) 0.7982(2) 0.0205(2) 0.0289(7) Uani 1 1 d U . .
C42 C -0.1056(3) 0.7715(3) -0.0322(3) 0.0489(10) Uani 1 1 d U . .
H42A H -0.1035 0.8239 -0.0929 0.073 Uiso 1 1 calc R . .
H42B H -0.1802 0.7690 0.0047 0.073 Uiso 1 1 calc R . .
H42C H -0.0694 0.7043 -0.0425 0.073 Uiso 1 1 calc R . .
C43 C 0.0349(3) 0.8523(2) -0.0278(2) 0.0284(7) Uani 1 1 d U . .
C44 C 0.0787(3) 0.8766(3) -0.1336(2) 0.0432(9) Uani 1 1 d U . .
H44A H 0.0735 0.9511 -0.1614 0.065 Uiso 1 1 calc R . .
H44B H 0.0371 0.8522 -0.1580 0.065 Uiso 1 1 calc R . .
H44C H 0.1537 0.8422 -0.1500 0.065 Uiso 1 1 calc R . .
C45 C 0.0838(2) 0.8790(2) 0.0219(2) 0.0241(6) Uani 1 1 d U . .
C46 C 0.1760(3) 0.9358(2) -0.0311(2) 0.0337(7) Uani 1 1 d U . .
H46A H 0.2413 0.8874 -0.0510 0.051 Uiso 1 1 calc R . .
H46B H 0.1865 0.9673 0.0099 0.051 Uiso 1 1 calc R . .
H46C H 0.1598 0.9895 -0.0866 0.051 Uiso 1 1 calc R . .
C47 C 0.0510(2) 0.8499(2) 0.1205(2) 0.0212(6) Uani 1 1 d U . .
C48 C 0.1126(3) 0.8687(2) 0.1731(2) 0.0326(7) Uani 1 1 d U . .
H48A H 0.1894 0.8468 0.1462 0.049 Uiso 1 1 calc R . .
H48B H 0.0914 0.8294 0.2395 0.049 Uiso 1 1 calc R . .
H48C H 0.0970 0.9421 0.1678 0.049 Uiso 1 1 calc R . .
C49 C 0.2720(2) 0.3125(2) 0.3746(2) 0.0337(8) Uani 1 1 d U . .
H49A H 0.3188 0.3494 0.3813 0.040 Uiso 1 1 calc R . .
H49B H 0.2789 0.3285 0.3069 0.040 Uiso 1 1 calc R . .
C50 C 0.3029(3) 0.1975(3) 0.4172(3) 0.0510(11) Uani 1 1 d U . .
H50A H 0.3238 0.1608 0.3692 0.061 Uiso 1 1 calc R . .
H50B H 0.3636 0.1818 0.4437 0.061 Uiso 1 1 calc R . .
C51 C 0.2069(3) 0.1669(2) 0.4919(3) 0.0465(10) Uani 1 1 d U . .
H51A H 0.2147 0.1569 0.5543 0.056 Uiso 1 1 calc R . .
H51B H 0.1955 0.1019 0.4906 0.056 Uiso 1 1 calc R . .
C52 C 0.1140(2) 0.2531(2) 0.4728(2) 0.0234(6) Uani 1 1 d U . .
H52A H 0.0806 0.2413 0.4323 0.028 Uiso 1 1 calc R . .
H52B H 0.0590 0.2599 0.5321 0.028 Uiso 1 1 calc R . .
O1T O 0.5149(5) 0.0830(5) 0.2660(5) 0.067(2) Uani 0.492(5) 1 d PU B 1
C1T C 0.6204(8) -0.0753(8) 0.2892(11) 0.074(3) Uani 0.492(5) 1 d PU B 1
H1TA H 0.6240 -0.1466 0.3314 0.089 Uiso 0.492(5) 1 calc PR B 1
H1TB H 0.6557 -0.0769 0.2233 0.089 Uiso 0.492(5) 1 calc PR B 1
C2T C 0.6667(9) -0.0139(10) 0.3156(11) 0.057(3) Uani 0.492(5) 1 d PU B 1
H2TA H 0.7429 -0.0147 0.2795 0.068 Uiso 0.492(5) 1 calc PR B 1
H2TB H 0.6614 -0.0400 0.3836 0.068 Uiso 0.492(5) 1 calc PR B 1
C3T C 0.6027(7) 0.0900(7) 0.2924(7) 0.056(2) Uani 0.492(5) 1 d PU B 1
H3TA H 0.5753 0.1171 0.3475 0.067 Uiso 0.492(5) 1 calc PR B 1
H3TB H 0.6468 0.1369 0.2398 0.067 Uiso 0.492(5) 1 calc PR B 1
C4T C 0.5048(8) -0.0154(7) 0.3020(9) 0.055(2) Uani 0.492(5) 1 d PU B 1
H4TA H 0.4679 -0.0328 0.2676 0.066 Uiso 0.492(5) 1 calc PR B 1
H4TB H 0.4641 -0.0303 0.3693 0.066 Uiso 0.492(5) 1 calc PR B 1
O2T O 0.5056(6) -0.0108(6) 0.4485(5) 0.089(2) Uani 0.508(5) 1 d PU . 2
C5T C 0.5862(7) 0.0411(7) 0.3937(9) 0.075(3) Uani 0.508(5) 1 d PU B 2
H5T1 H 0.6425 0.0214 0.4260 0.090 Uiso 0.508(5) 1 calc PR B 2
H5T2 H 0.5586 0.1160 0.3825 0.090 Uiso 0.508(5) 1 calc PR B 2
C6T C 0.6324(15) 0.0161(14) 0.3018(15) 0.117(6) Uani 0.508(5) 1 d PU B 2
H6T1 H 0.7072 -0.0219 0.2936 0.141 Uiso 0.508(5) 1 calc PR B 2
H6T2 H 0.6281 0.0783 0.2477 0.141 Uiso 0.508(5) 1 calc PR B 2
C7T C 0.5530(18) -0.0538(16) 0.3184(17) 0.142(6) Uani 0.508(5) 1 d PU B 2
H7T1 H 0.5185 -0.0265 0.2668 0.171 Uiso 0.508(5) 1 calc PR B 2
H7T2 H 0.5930 -0.1244 0.3184 0.171 Uiso 0.508(5) 1 calc PR B 2
C8T C 0.4810(10) -0.0561(8) 0.3976(10) 0.087(3) Uani 0.508(5) 1 d PU B 2
H8T1 H 0.4755 -0.1283 0.4340 0.104 Uiso 0.508(5) 1 calc PR B 2
H8T2 H 0.4108 -0.0195 0.3861 0.104 Uiso 0.508(5) 1 calc PR B 2


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
C01 O1 1.423(4) . ?
C01 C02 1.511(4) . ?
O1 Ce1 2.3514(19) . ?
O1 Ce1 2.3934(18) 2_566 ?
Ce1 O2 2.0743(19) . ?
Ce1 O3 2.103(2) . ?
Ce1 O4 2.1081(18) . ?
Ce1 O1 2.3935(18) 2_566 ?
Ce1 O5 2.5390(19) . ?
Ce1 Ce1 3.9097(3) 2_566 ?
C02 C11 1.394(4) . ?
C02 C03 1.409(4) . ?
O2 C13 1.411(3) . ?
C03 C05 1.403(4) . ?
C03 C04 1.515(4) . ?
O3 C25 1.408(3) . ?
O4 C37 1.411(3) . ?
C05 C07 1.407(4) . ?
C05 C06 1.512(4) . ?
O5 C52 1.433(3) . ?
O5 C49 1.451(3) . ?
C101 C102 1.3900 . ?
C101 C106 1.3900 . ?
C102 C103 1.3900 . ?
C103 C104 1.3900 . ?
C104 C105 1.3900 . ?
C105 C106 1.3900 . ?
C07 C09 1.404(4) . ?
C07 C08 1.516(4) . ?
C09 C11 1.407(4) . ?
C09 C10 1.511(4) . ?
C11 C12 1.507(4) . ?
C13 C14 1.523(4) . ?
C14 C15 1.403(4) . ?
C14 C23 1.411(4) . ?
C15 C17 1.398(4) . ?
C15 C16 1.505(4) . ?
C17 C19 1.404(4) . ?
C17 C18 1.509(5) . ?
C19 C21 1.399(4) . ?
C19 C20 1.511(4) . ?
C21 C23 1.404(4) . ?
C21 C22 1.517(4) . ?
C23 C24 1.509(4) . ?
C25 C26 1.523(4) . ?
C26 C27 1.399(4) . ?
C26 C35 1.410(4) . ?
C27 C29 1.407(4) . ?
C27 C28 1.512(4) . ?
C29 C31 1.393(4) . ?
C29 C30 1.516(4) . ?
C31 C33 1.407(4) . ?
C31 C32 1.507(4) . ?
C33 C35 1.405(4) . ?
C33 C34 1.514(4) . ?
C35 C36 1.513(4) . ?
C37 C38 1.521(4) . ?
C38 C39 1.399(4) . ?
C38 C47 1.404(4) . ?
C39 C41 1.411(4) . ?
C39 C40 1.514(4) . ?
C41 C43 1.407(5) . ?
C41 C42 1.509(5) . ?
C43 C45 1.397(5) . ?
C43 C44 1.514(4) . ?
C45 C47 1.402(4) . ?
C45 C46 1.515(4) . ?
C47 C48 1.505(4) . ?
C49 C50 1.517(4) . ?
C50 C51 1.472(5) . ?
C51 C52 1.511(4) . ?
O1T C4T 1.334(12) . ?
O1T C3T 1.440(11) . ?
C1T C2T 1.454(19) . ?
C1T C4T 1.534(13) . ?
C2T C3T 1.468(13) . ?
O2T C5T 1.357(12) . ?
O2T C8T 1.370(14) . ?
O2T O2T 1.721(17) 2_656 ?
C5T C6T 1.50(2) . ?
C6T C7T 1.57(3) . ?
C7T C8T 1.29(2) . ?

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
O1 C01 C02 115.9(2) . . ?
C01 O1 Ce1 139.74(16) . . ?
C01 O1 Ce1 108.67(15) . 2_566 ?
Ce1 O1 Ce1 110.97(8) . 2_566 ?
O2 Ce1 O3 96.11(8) . . ?
O2 Ce1 O4 99.02(8) . . ?
O3 Ce1 O4 99.68(8) . . ?
O2 Ce1 O1 96.72(7) . . ?
O3 Ce1 O1 156.87(7) . . ?
O4 Ce1 O1 97.21(7) . . ?
O2 Ce1 O1 160.75(7) . 2_566 ?
O3 Ce1 O1 93.57(7) . 2_566 ?
O4 Ce1 O1 95.69(7) . 2_566 ?
O1 Ce1 O1 69.03(8) . 2_566 ?
O2 Ce1 O5 83.63(7) . . ?
O3 Ce1 O5 81.61(7) . . ?
O4 Ce1 O5 176.88(7) . . ?
O1 Ce1 O5 80.79(7) . . ?
O1 Ce1 O5 81.37(6) 2_566 . ?
O2 Ce1 Ce1 130.42(6) . 2_566 ?
O3 Ce1 Ce1 126.24(5) . 2_566 ?
O4 Ce1 Ce1 97.83(5) . 2_566 ?
O1 Ce1 Ce1 34.87(4) . 2_566 ?
O1 Ce1 Ce1 34.17(5) 2_566 2_566 ?
O5 Ce1 Ce1 79.15(5) . 2_566 ?
C11 C02 C03 120.6(3) . . ?
C11 C02 C01 119.9(3) . . ?
C03 C02 C01 119.4(3) . . ?
C13 O2 Ce1 169.2(2) . . ?
C05 C03 C02 119.4(3) . . ?
C05 C03 C04 120.1(3) . . ?
C02 C03 C04 120.6(3) . . ?
C25 O3 Ce1 165.82(19) . . ?
C37 O4 Ce1 169.46(17) . . ?
C03 C05 C07 119.8(3) . . ?
C03 C05 C06 121.1(3) . . ?
C07 C05 C06 119.1(3) . . ?
C52 O5 C49 109.0(2) . . ?
C52 O5 Ce1 125.37(16) . . ?
C49 O5 Ce1 118.51(16) . . ?
C102 C101 C106 120.0 . . ?
C101 C102 C103 120.0 . . ?
C104 C103 C102 120.0 . . ?
C103 C104 C105 120.0 . . ?
C104 C105 C106 120.0 . . ?
C105 C106 C101 120.0 . . ?
C09 C07 C05 120.9(3) . . ?
C09 C07 C08 121.1(3) . . ?
C05 C07 C08 118.1(3) . . ?
C07 C09 C11 118.9(3) . . ?
C07 C09 C10 122.0(3) . . ?
C11 C09 C10 119.1(3) . . ?
C02 C11 C09 120.4(3) . . ?
C02 C11 C12 119.6(3) . . ?
C09 C11 C12 119.9(3) . . ?
O2 C13 C14 112.8(2) . . ?
C15 C14 C23 119.9(3) . . ?
C15 C14 C13 118.7(3) . . ?
C23 C14 C13 121.3(3) . . ?
C17 C15 C14 120.1(3) . . ?
C17 C15 C16 119.3(3) . . ?
C14 C15 C16 120.5(3) . . ?
C15 C17 C19 120.1(3) . . ?
C15 C17 C18 118.8(3) . . ?
C19 C17 C18 121.1(3) . . ?
C21 C19 C17 119.9(3) . . ?
C21 C19 C20 119.7(3) . . ?
C17 C19 C20 120.5(3) . . ?
C19 C21 C23 120.4(3) . . ?
C19 C21 C22 120.0(3) . . ?
C23 C21 C22 119.6(3) . . ?
C21 C23 C14 119.5(3) . . ?
C21 C23 C24 118.4(3) . . ?
C14 C23 C24 122.1(3) . . ?
O3 C25 C26 111.3(2) . . ?
C27 C26 C35 120.2(3) . . ?
C27 C26 C25 119.3(3) . . ?
C35 C26 C25 120.4(3) . . ?
C26 C27 C29 120.0(3) . . ?
C26 C27 C28 121.3(3) . . ?
C29 C27 C28 118.7(3) . . ?
C31 C29 C27 119.9(3) . . ?
C31 C29 C30 119.7(3) . . ?
C27 C29 C30 120.3(3) . . ?
C29 C31 C33 120.4(3) . . ?
C29 C31 C32 119.5(3) . . ?
C33 C31 C32 120.1(3) . . ?
C35 C33 C31 120.0(3) . . ?
C35 C33 C34 120.2(3) . . ?
C31 C33 C34 119.9(3) . . ?
C33 C35 C26 119.5(3) . . ?
C33 C35 C36 119.6(3) . . ?
C26 C35 C36 120.9(3) . . ?
O4 C37 C38 113.0(2) . . ?
C39 C38 C47 120.7(3) . . ?
C39 C38 C37 119.1(3) . . ?
C47 C38 C37 120.2(3) . . ?
C38 C39 C41 119.9(3) . . ?
C38 C39 C40 120.5(3) . . ?
C41 C39 C40 119.6(3) . . ?
C43 C41 C39 119.3(3) . . ?
C43 C41 C42 121.0(3) . . ?
C39 C41 C42 119.7(3) . . ?
C45 C43 C41 120.3(3) . . ?
C45 C43 C44 119.1(3) . . ?
C41 C43 C44 120.4(3) . . ?
C43 C45 C47 120.5(3) . . ?
C43 C45 C46 119.6(3) . . ?
C47 C45 C46 119.8(3) . . ?
C45 C47 C38 119.2(3) . . ?
C45 C47 C48 119.8(3) . . ?
C38 C47 C48 120.9(3) . . ?
O5 C49 C50 106.4(3) . . ?
C51 C50 C49 105.4(3) . . ?
C50 C51 C52 106.5(3) . . ?
O5 C52 C51 103.8(2) . . ?
C4T O1T C3T 106.1(7) . . ?
C2T C1T C4T 100.6(9) . . ?
C1T C2T C3T 104.3(9) . . ?
O1T C3T C2T 107.4(9) . . ?
O1T C4T C1T 104.1(9) . . ?
C5T O2T C8T 110.3(10) . . ?
C5T O2T O2T 96.7(9) . 2_656 ?
C8T O2T O2T 152.8(10) . 2_656 ?
O2T C5T C6T 109.5(12) . . ?
C5T C6T C7T 98.0(14) . . ?
C8T C7T C6T 109.9(17) . . ?
C7T C8T O2T 110.9(14) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.379
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 1000023'
