# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_HfCp2Cl2
_database_code_depnum_ccdc_archive 'CCDC 2195632'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   odpm149
_manchester_internal_coll_client BR
_manchester_internal_coll_user   BR
_manchester_internal_coll_date   19/02/2020
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 25s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_process_date 19/02/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 19/02/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 23/02/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 29/05/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 29/05/2020
_manchester_internal_archive_user AW
_audit_author_email              
;
benjamin.reant@postgrad.manchester.ac.uk, david.mills@manchester.ac.uk    
;
# start Validation Reply Form
_vrf_PLAT971_HfCp2Cl2            
;
PROBLEM: Check Calcd Resid. Dens.  1.76A   From C11             3.58 eA-3  
RESPONSE: Residual density is an artefact of twinning due to
pseudosyummetric C-centering. No reliable twin law could be found
so this was left as is in the final refinement.
;
# end Validation Reply Form
_refine_special_details          -
_audit_creation_date             2020-02-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        "[Hf(Cp'')2Cl2]"
_chemical_formula_moiety         'C22 H42 Cl2 Hf Si4'
_chemical_formula_sum            'C22 H42 Cl2 Hf Si4'
_chemical_formula_weight         668.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Hf1 Si4 Cl2 C22'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   17.8746(12)
_cell_length_b                   9.0854(5)
_cell_length_c                   18.3865(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2985.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3480
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9390
_cell_measurement_theta_min      3.3100
_shelx_estimated_absorpt_T_max   0.734
_shelx_estimated_absorpt_T_min   0.335
_exptl_absorpt_coefficient_mu    3.841
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 1 22 0.0763
-14 -1 -22 0.0383
-3 -13 2 0.1879
3 13 -2 0.1609
-21 1 14 0.0509
21 -1 -14 0.0349

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 'Recrystallised from hexane at -25 oC'
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.086
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
13.9975 1.0002 21.9992 -0.2229 -0.9728 -0.1966
-13.9975 -1.0002 -21.9992 0.2229 0.9728 0.1966
-3.0012 -12.9999 1.9996 -0.0099 -0.1209 1.0178
3.0012 12.9999 -1.9996 0.0099 0.1209 -1.0178
-20.9987 1.0000 13.9986 0.9678 -0.2315 0.0422
20.9987 -1.0000 -13.9986 -0.9678 0.2315 -0.0422

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13683
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.813
_diffrn_reflns_theta_min         2.748
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00  85.00   1.00   25.00    --   10.64  37.00   0.00   83
  2  ω    -13.00  74.00   1.00   25.00    --   10.64  57.00  90.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0369662000
_diffrn_orient_matrix_UB_12      0.0112801000
_diffrn_orient_matrix_UB_13      0.0128775000
_diffrn_orient_matrix_UB_21      -0.0128760000
_diffrn_orient_matrix_UB_22      0.0066853000
_diffrn_orient_matrix_UB_23      -0.0363328000
_diffrn_orient_matrix_UB_31      -0.0065284000
_diffrn_orient_matrix_UB_32      -0.0769848000
_diffrn_orient_matrix_UB_33      -0.0012812000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2308
_reflns_number_total             3652
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.405
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0533
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0497P)²+2.1246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1303
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C6(H6), C5(H5)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.500000 0.70442(4) 0.250000 0.02099(14) Uani 1 2 d S T P . .
Cl1 Cl 0.40554(12) 0.5298(2) 0.28624(11) 0.0416(5) Uani 1 1 d . . . . .
Si2 Si 0.38715(11) 0.9665(2) 0.37980(11) 0.0303(5) Uani 1 1 d . . . . .
Si1 Si 0.62937(12) 0.5319(2) 0.40178(12) 0.0333(5) Uani 1 1 d . . . . .
C4 C 0.5729(4) 0.6923(7) 0.3684(4) 0.0243(15) Uani 1 1 d . . . . .
C11 C 0.4985(4) 0.7265(7) 0.3867(4) 0.0224(14) Uani 1 1 d . . . . .
H11 H 0.466929 0.664750 0.414931 0.027 Uiso 1 1 calc R . . . .
C6 C 0.5417(4) 0.9204(7) 0.3223(4) 0.0262(16) Uani 1 1 d . . . . .
H6 H 0.545301 1.013374 0.298941 0.031 Uiso 1 1 calc R . . . .
C7 C 0.4763(4) 0.8644(7) 0.3578(4) 0.0250(16) Uani 1 1 d . . . . .
C5 C 0.5991(4) 0.8180(7) 0.3272(4) 0.0283(16) Uani 1 1 d . . . . .
H5 H 0.647699 0.828590 0.306906 0.034 Uiso 1 1 calc R . . . .
C1 C 0.5788(5) 0.3544(8) 0.3867(5) 0.051(2) Uani 1 1 d . . . . .
H1A H 0.530183 0.357801 0.411332 0.077 Uiso 1 1 calc GR . . . .
H1B H 0.608524 0.273089 0.406532 0.077 Uiso 1 1 calc GR . . . .
H1C H 0.571176 0.339244 0.334499 0.077 Uiso 1 1 calc GR . . . .
C9 C 0.3774(5) 1.1337(9) 0.3221(5) 0.048(2) Uani 1 1 d . . . . .
H9A H 0.425379 1.185824 0.320173 0.073 Uiso 1 1 calc GR . . . .
H9B H 0.339197 1.198540 0.342902 0.073 Uiso 1 1 calc GR . . . .
H9C H 0.362570 1.104750 0.272819 0.073 Uiso 1 1 calc GR . . . .
C2 C 0.7239(4) 0.5347(10) 0.3605(5) 0.058(3) Uani 1 1 d . . . . .
H2A H 0.719658 0.523929 0.307639 0.087 Uiso 1 1 calc GR . . . .
H2B H 0.753698 0.453358 0.380197 0.087 Uiso 1 1 calc GR . . . .
H2C H 0.748507 0.628394 0.371862 0.087 Uiso 1 1 calc GR . . . .
C8 C 0.3930(5) 1.0214(9) 0.4757(4) 0.048(2) Uani 1 1 d . . . . .
H8A H 0.401147 0.934009 0.505926 0.071 Uiso 1 1 calc GR . . . .
H8B H 0.346201 1.069369 0.490159 0.071 Uiso 1 1 calc GR . . . .
H8C H 0.434732 1.090054 0.482175 0.071 Uiso 1 1 calc GR . . . .
C10 C 0.3056(4) 0.8434(10) 0.3676(5) 0.055(2) Uani 1 1 d . . . . .
H10A H 0.304657 0.806718 0.317453 0.082 Uiso 1 1 calc GR . . . .
H10B H 0.259469 0.898224 0.377464 0.082 Uiso 1 1 calc GR . . . .
H10C H 0.309447 0.760253 0.401279 0.082 Uiso 1 1 calc GR . . . .
C3 C 0.6383(5) 0.5581(10) 0.5023(4) 0.056(3) Uani 1 1 d . . . . .
H3A H 0.657439 0.657134 0.512413 0.085 Uiso 1 1 calc GR . . . .
H3B H 0.673094 0.484803 0.522043 0.085 Uiso 1 1 calc GR . . . .
H3C H 0.589215 0.546060 0.525231 0.085 Uiso 1 1 calc GR . . . .


_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
Hf1 Cl1 2.4109(18) 3_655 ?
Hf1 Cl1 2.4110(18) . ?
Hf1 C4 2.540(7) . ?
Hf1 C4 2.540(7) 3_655 ?
Hf1 C11 2.521(7) . ?
Hf1 C11 2.521(7) 3_655 ?
Hf1 C6 2.484(7) . ?
Hf1 C6 2.484(6) 3_655 ?
Hf1 C7 2.494(7) 3_655 ?
Hf1 C7 2.494(7) . ?
Hf1 C5 2.494(7) 3_655 ?
Hf1 C5 2.494(7) . ?
Si2 C7 1.887(7) . ?
Si2 C9 1.861(8) . ?
Si2 C8 1.835(8) . ?
Si2 C10 1.851(9) . ?
Si1 C4 1.876(7) . ?
Si1 C1 1.869(8) . ?
Si1 C2 1.853(8) . ?
Si1 C3 1.871(8) . ?
C4 C11 1.408(9) . ?
C4 C5 1.447(9) . ?
C11 H11 0.9500 . ?
C11 C7 1.417(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.433(10) . ?
C6 C5 1.388(10) . ?
C5 H5 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Hf1 Cl1 97.68(10) 3_655 . ?
Cl1 Hf1 C4 95.41(16) . . ?
Cl1 Hf1 C4 81.31(16) . 3_655 ?
Cl1 Hf1 C4 81.31(16) 3_655 . ?
Cl1 Hf1 C4 95.41(16) 3_655 3_655 ?
Cl1 Hf1 C11 76.66(16) 3_655 3_655 ?
Cl1 Hf1 C11 109.61(16) . 3_655 ?
Cl1 Hf1 C11 76.66(16) . . ?
Cl1 Hf1 C11 109.61(16) 3_655 . ?
Cl1 Hf1 C6 125.60(17) 3_655 3_655 ?
Cl1 Hf1 C6 125.60(17) . . ?
Cl1 Hf1 C6 117.21(17) 3_655 . ?
Cl1 Hf1 C6 117.21(17) . 3_655 ?
Cl1 Hf1 C7 136.24(17) 3_655 . ?
Cl1 Hf1 C7 92.58(17) . . ?
Cl1 Hf1 C7 92.58(17) 3_655 3_655 ?
Cl1 Hf1 C7 136.24(17) . 3_655 ?
Cl1 Hf1 C5 127.77(17) . . ?
Cl1 Hf1 C5 86.10(17) 3_655 . ?
Cl1 Hf1 C5 86.10(17) . 3_655 ?
Cl1 Hf1 C5 127.76(17) 3_655 3_655 ?
C4 Hf1 C4 175.0(3) 3_655 . ?
C11 Hf1 C4 148.4(2) . 3_655 ?
C11 Hf1 C4 32.3(2) . . ?
C11 Hf1 C4 32.3(2) 3_655 3_655 ?
C11 Hf1 C4 148.4(2) 3_655 . ?
C11 Hf1 C11 170.9(3) . 3_655 ?
C6 Hf1 C4 130.3(2) 3_655 . ?
C6 Hf1 C4 54.7(2) . . ?
C6 Hf1 C4 54.7(2) 3_655 3_655 ?
C6 Hf1 C4 130.3(2) . 3_655 ?
C6 Hf1 C11 117.8(2) 3_655 . ?
C6 Hf1 C11 117.8(2) . 3_655 ?
C6 Hf1 C11 53.6(2) . . ?
C6 Hf1 C11 53.6(2) 3_655 3_655 ?
C6 Hf1 C6 75.7(3) 3_655 . ?
C6 Hf1 C7 33.5(2) 3_655 3_655 ?
C6 Hf1 C7 85.1(2) . 3_655 ?
C6 Hf1 C7 33.5(2) . . ?
C6 Hf1 C7 85.1(2) 3_655 . ?
C6 Hf1 C5 32.4(2) 3_655 3_655 ?
C6 Hf1 C5 32.4(2) . . ?
C6 Hf1 C5 101.0(2) . 3_655 ?
C6 Hf1 C5 101.0(2) 3_655 . ?
C7 Hf1 C4 55.4(2) 3_655 3_655 ?
C7 Hf1 C4 55.4(2) . . ?
C7 Hf1 C4 128.2(2) . 3_655 ?
C7 Hf1 C4 128.2(2) 3_655 . ?
C7 Hf1 C11 138.4(2) . 3_655 ?
C7 Hf1 C11 32.8(2) 3_655 3_655 ?
C7 Hf1 C11 138.4(2) 3_655 . ?
C7 Hf1 C11 32.8(2) . . ?
C7 Hf1 C7 108.7(3) . 3_655 ?
C7 Hf1 C5 55.1(2) . . ?
C7 Hf1 C5 95.2(2) . 3_655 ?
C7 Hf1 C5 55.1(2) 3_655 3_655 ?
C7 Hf1 C5 95.2(2) 3_655 . ?
C5 Hf1 C4 33.4(2) 3_655 3_655 ?
C5 Hf1 C4 150.5(2) . 3_655 ?
C5 Hf1 C4 33.4(2) . . ?
C5 Hf1 C4 150.5(2) 3_655 . ?
C5 Hf1 C11 121.8(2) 3_655 . ?
C5 Hf1 C11 53.6(2) 3_655 3_655 ?
C5 Hf1 C11 121.8(2) . 3_655 ?
C5 Hf1 C11 53.7(2) . . ?
C5 Hf1 C5 131.1(3) 3_655 . ?
C9 Si2 C7 111.0(3) . . ?
C8 Si2 C7 107.0(4) . . ?
C8 Si2 C9 109.3(4) . . ?
C8 Si2 C10 109.0(4) . . ?
C10 Si2 C7 110.0(3) . . ?
C10 Si2 C9 110.5(4) . . ?
C1 Si1 C4 111.2(4) . . ?
C1 Si1 C3 107.3(4) . . ?
C2 Si1 C4 110.2(4) . . ?
C2 Si1 C1 113.1(4) . . ?
C2 Si1 C3 108.9(4) . . ?
C3 Si1 C4 105.7(4) . . ?
Si1 C4 Hf1 126.2(3) . . ?
C11 C4 Hf1 73.1(4) . . ?
C11 C4 Si1 127.0(5) . . ?
C11 C4 C5 104.9(6) . . ?
C5 C4 Hf1 71.6(4) . . ?
C5 C4 Si1 127.6(6) . . ?
Hf1 C11 H11 120.3 . . ?
C4 C11 Hf1 74.6(4) . . ?
C4 C11 H11 124.1 . . ?
C4 C11 C7 111.7(6) . . ?
C7 C11 Hf1 72.5(4) . . ?
C7 C11 H11 124.1 . . ?
Hf1 C6 H6 118.7 . . ?
C7 C6 Hf1 73.6(4) . . ?
C7 C6 H6 125.2 . . ?
C5 C6 Hf1 74.2(4) . . ?
C5 C6 H6 125.2 . . ?
C5 C6 C7 109.6(6) . . ?
Si2 C7 Hf1 126.9(3) . . ?
C11 C7 Hf1 74.6(4) . . ?
C11 C7 Si2 126.2(5) . . ?
C11 C7 C6 104.8(6) . . ?
C6 C7 Hf1 72.9(4) . . ?
C6 C7 Si2 127.8(5) . . ?
Hf1 C5 H5 117.9 . . ?
C4 C5 Hf1 75.0(4) . . ?
C4 C5 H5 125.6 . . ?
C6 C5 Hf1 73.4(4) . . ?
C6 C5 C4 108.9(6) . . ?
C6 C5 H5 125.6 . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hf1 C4 C11 C7 -63.6(5) . . . . ?
Hf1 C4 C5 C6 66.2(5) . . . . ?
Hf1 C11 C7 Si2 124.8(5) . . . . ?
Hf1 C11 C7 C6 -67.2(4) . . . . ?
Hf1 C6 C7 Si2 -123.8(5) . . . . ?
Hf1 C6 C7 C11 68.4(5) . . . . ?
Hf1 C6 C5 C4 -67.3(5) . . . . ?
Si1 C4 C11 Hf1 -122.9(5) . . . . ?
Si1 C4 C11 C7 173.5(5) . . . . ?
Si1 C4 C5 Hf1 121.9(5) . . . . ?
Si1 C4 C5 C6 -171.9(5) . . . . ?
C4 C11 C7 Hf1 64.8(5) . . . . ?
C4 C11 C7 Si2 -170.4(5) . . . . ?
C4 C11 C7 C6 -2.4(8) . . . . ?
C11 C4 C5 Hf1 -66.1(4) . . . . ?
C11 C4 C5 C6 0.1(8) . . . . ?
C7 C6 C5 Hf1 65.7(5) . . . . ?
C7 C6 C5 C4 -1.6(8) . . . . ?
C5 C4 C11 Hf1 65.0(4) . . . . ?
C5 C4 C11 C7 1.4(8) . . . . ?
C5 C6 C7 Hf1 -66.0(5) . . . . ?
C5 C6 C7 Si2 170.2(5) . . . . ?
C5 C6 C7 C11 2.4(7) . . . . ?
C1 Si1 C4 Hf1 -42.9(5) . . . . ?
C1 Si1 C4 C11 52.9(7) . . . . ?
C1 Si1 C4 C5 -136.8(6) . . . . ?
C9 Si2 C7 Hf1 -76.4(5) . . . . ?
C9 Si2 C7 C11 -174.3(6) . . . . ?
C9 Si2 C7 C6 20.4(7) . . . . ?
C2 Si1 C4 Hf1 83.4(5) . . . . ?
C2 Si1 C4 C11 179.2(6) . . . . ?
C2 Si1 C4 C5 -10.5(7) . . . . ?
C8 Si2 C7 Hf1 164.5(4) . . . . ?
C8 Si2 C7 C11 66.5(7) . . . . ?
C8 Si2 C7 C6 -98.8(6) . . . . ?
C10 Si2 C7 Hf1 46.2(5) . . . . ?
C10 Si2 C7 C11 -51.8(7) . . . . ?
C10 Si2 C7 C6 142.9(6) . . . . ?
C3 Si1 C4 Hf1 -159.0(4) . . . . ?
C3 Si1 C4 C11 -63.3(7) . . . . ?
C3 Si1 C4 C5 107.0(7) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR3.273
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.752
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-Nd
_database_code_depnum_ccdc_archive 'CCDC 2195633'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   ldpm177
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   27/11/2020
_manchester_internal_process_date 27/11/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 11/12/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 11/12/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 15/12/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 15/12/2020
_manchester_internal_archive_user AW
_refine_special_details          -
_vrf_PLAT971_2-Nd                
;
PROBLEM: Check Calcd Resid. Dens.  1.35A   From C7              3.36 eA-3  
RESPONSE: Residual density is located near heavy atoms
and present despite applying face-indexed absorption correction.
They are not chemically significant.
;
_audit_creation_date             2020-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        "[{Nd(Cp'')2(uI)}2]"
_chemical_formula_moiety         'C44 H84 I2 Nd2 Si8'
_chemical_formula_sum            'C44 H84 I2 Nd2 Si8'
_chemical_formula_weight         1380.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nd2 I2 Si8 C44'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7367(3)
_cell_length_b                   11.5169(3)
_cell_length_c                   13.3589(4)
_cell_angle_alpha                73.257(3)
_cell_angle_beta                 83.329(2)
_cell_angle_gamma                78.423(2)
_cell_volume                     1546.66(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      75.9850
_cell_measurement_theta_min      3.4320
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.860
_exptl_absorpt_coefficient_mu    22.162
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             686
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 7 0 0.0210
-7 -2 -2 0.0303
7 2 2 0.0163
1 2 9 0.0723
-1 -2 -9 0.0683
0 -7 0 0.0270

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 
'Crystallised from concentrated toluene at -25oC'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.047
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 7.0000 -0.0000 0.9176 -0.3802 -0.0010
-7.0000 -2.0000 -2.0000 0.3361 0.9100 -0.2869
7.0000 2.0000 2.0000 -0.3361 -0.9100 0.2869
1.0000 2.0000 9.0000 -0.0197 0.0478 1.0375
-1.0000 -2.0000 -9.0000 0.0197 -0.0478 -1.0375
0.0000 -7.0000 0.0000 -0.9176 0.3802 0.0010

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18441
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.219
_diffrn_reflns_theta_min         3.462
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    119.00 163.00   1.00    1.00    --  108.20  19.00  35.00   44
  2  ω     35.00 108.00   1.00    1.00    --  108.20  19.00  35.00   73
  3  ω    -44.00  17.00   1.00    1.00    --   44.60  60.00-150.00   61
  4  ω     18.00  45.00   1.00    1.00    --   44.60  19.00  35.00   27
  5  ω    -44.00  39.00   1.00    1.00    --   44.60  60.00  90.00   83
  6  ω     71.00 106.00   1.00    1.00    --   44.60  60.00-150.00   35
  7  ω    -45.00  68.00   1.00    1.00    --   44.60  60.00 -30.00  113
  8  ω     77.00 113.00   1.00    1.00    --   44.60  60.00 -30.00   36
  9  ω     99.00 133.00   1.00    1.00    --   44.60  60.00  90.00   34
 10  ω     44.00  78.00   1.00    1.00    --   44.60  60.00  90.00   34
 11  ω    -45.00  57.00   1.00    1.00    --   44.60  60.00 -90.00  102
 12  ω     65.00 133.00   1.00    1.00    --   44.60  60.00 -90.00   68
 13  ω     20.00 137.00   1.00    1.00    --  108.20  50.00-180.00  117
 14  ω    126.00 188.00   1.00    1.00    --  108.20  50.00  90.00   62
 15  ω     21.00  73.00   1.00    1.00    --  108.20  50.00  90.00   52
 16  ω    149.00 198.00   1.00    1.00    --  108.20  50.00-180.00   49
 17  ω     22.00 198.00   1.00    1.00    --  108.20  50.00 120.00  176
 18  ω    152.00 179.00   1.00    1.00    --  108.20  50.00-150.00   27
 19  ω    147.00 194.00   1.00    1.00    --  108.20  50.00 150.00   47
 20  ω     75.00 161.00   1.00    1.00    --  108.20  50.00   0.00   86
 21  ω     37.00  71.00   1.00    1.00    --  108.20  50.00   0.00   34
 22  ω     50.00  75.00   1.00    1.00    --  108.20  50.00 150.00   25
 23  ω    120.00 196.00   1.00    1.00    --  108.20  50.00  30.00   76
 24  ω     19.00 198.00   1.00    1.00    --  108.20  50.00 -30.00  179
 25  ω    114.00 198.00   1.00    1.00    --  108.20  50.00 -90.00   84
 26  ω     23.00  91.00   1.00    1.00    --  108.20  50.00 -90.00   68
 27  ω     61.00  87.00   1.00    1.00    --  108.20  50.00  30.00   26
 28  ω     40.00  65.00   1.00    1.00    --  108.20  50.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0790340000
_diffrn_orient_matrix_UB_12      0.1310908000
_diffrn_orient_matrix_UB_13      -0.0225343000
_diffrn_orient_matrix_UB_21      -0.1233670000
_diffrn_orient_matrix_UB_22      -0.0543151000
_diffrn_orient_matrix_UB_23      0.0310940000
_diffrn_orient_matrix_UB_31      0.0083375000
_diffrn_orient_matrix_UB_32      -0.0001383000
_diffrn_orient_matrix_UB_33      0.1143858000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5784
_reflns_number_total             6153
_reflns_odcompleteness_completeness 98.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.273
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0374
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0680P)²+0.6420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.0993
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C12(H12), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.47951(2) 0.50346(2) 0.67512(2) 0.03284(8) Uani 1 1 d . . . . .
I1 I 0.52682(3) 0.68577(2) 0.45337(2) 0.04297(9) Uani 1 1 d . . . . .
Si1 Si 0.79333(11) 0.67627(10) 0.66478(10) 0.0440(3) Uani 1 1 d . . . . .
Si2 Si 0.72940(11) 0.16621(10) 0.78622(10) 0.0440(3) Uani 1 1 d . . . . .
Si3 Si 0.20597(12) 0.31669(10) 0.86878(10) 0.0469(3) Uani 1 1 d . . . . .
Si4 Si 0.28115(11) 0.82413(9) 0.74916(10) 0.0408(2) Uani 1 1 d . . . . .
C1 C 0.7389(4) 0.4288(4) 0.6953(3) 0.0389(8) Uani 1 1 d . . . . .
H1 H 0.788850 0.417006 0.634293 0.047 Uiso 1 1 calc R . . . .
C2 C 0.6832(4) 0.3351(4) 0.7717(3) 0.0405(8) Uani 1 1 d . . . . .
C3 C 0.8193(6) 0.1415(5) 0.6643(4) 0.0634(13) Uani 1 1 d . . . . .
H3A H 0.764951 0.178188 0.605090 0.095 Uiso 1 1 calc GR . . . .
H3B H 0.845300 0.052917 0.671988 0.095 Uiso 1 1 calc GR . . . .
H3C H 0.895106 0.180252 0.651509 0.095 Uiso 1 1 calc GR . . . .
C4 C 0.5909(5) 0.0827(4) 0.8181(5) 0.0651(14) Uani 1 1 d . . . . .
H4A H 0.551895 0.086418 0.887441 0.098 Uiso 1 1 calc GR . . . .
H4B H 0.620453 -0.003526 0.818109 0.098 Uiso 1 1 calc GR . . . .
H4C H 0.527849 0.121513 0.765477 0.098 Uiso 1 1 calc GR . . . .
C5 C 0.8356(5) 0.1011(5) 0.8973(4) 0.0609(13) Uani 1 1 d . . . . .
H5A H 0.911121 0.140481 0.881697 0.091 Uiso 1 1 calc GR . . . .
H5B H 0.861827 0.012193 0.907197 0.091 Uiso 1 1 calc GR . . . .
H5C H 0.789687 0.116441 0.961324 0.091 Uiso 1 1 calc GR . . . .
C6 C 0.6153(4) 0.3946(4) 0.8471(3) 0.0412(9) Uani 1 1 d . . . . .
H6 H 0.567250 0.356554 0.907598 0.049 Uiso 1 1 calc R . . . .
C7 C 0.6312(4) 0.5195(4) 0.8171(4) 0.0427(9) Uani 1 1 d . . . . .
H7 H 0.595200 0.578687 0.854067 0.051 Uiso 1 1 calc R . . . .
C8 C 0.7095(4) 0.5418(4) 0.7229(3) 0.0383(8) Uani 1 1 d . . . . .
C9 C 0.9027(5) 0.6760(6) 0.7628(5) 0.0699(15) Uani 1 1 d . . . . .
H9A H 0.855206 0.672217 0.830592 0.105 Uiso 1 1 calc GR . . . .
H9B H 0.939382 0.751449 0.739718 0.105 Uiso 1 1 calc GR . . . .
H9C H 0.971133 0.604189 0.769878 0.105 Uiso 1 1 calc GR . . . .
C10 C 0.6829(6) 0.8273(4) 0.6385(5) 0.0645(14) Uani 1 1 d . . . . .
H10A H 0.622377 0.830168 0.587945 0.097 Uiso 1 1 calc GR . . . .
H10B H 0.732002 0.893971 0.609796 0.097 Uiso 1 1 calc GR . . . .
H10C H 0.636330 0.837138 0.703954 0.097 Uiso 1 1 calc GR . . . .
C11 C 0.8876(5) 0.6582(6) 0.5427(5) 0.0651(14) Uani 1 1 d . . . . .
H11A H 0.947710 0.580026 0.558179 0.098 Uiso 1 1 calc GR . . . .
H11B H 0.934670 0.726478 0.514847 0.098 Uiso 1 1 calc GR . . . .
H11C H 0.830002 0.658489 0.490808 0.098 Uiso 1 1 calc GR . . . .
C12 C 0.2870(4) 0.5571(3) 0.8165(3) 0.0377(8) Uani 1 1 d . . . . .
H12 H 0.310961 0.547160 0.885150 0.045 Uiso 1 1 calc R . . . .
C13 C 0.2511(4) 0.4633(3) 0.7825(3) 0.0382(8) Uani 1 1 d . . . . .
C14 C 0.3113(6) 0.2545(5) 0.9813(4) 0.0683(15) Uani 1 1 d . . . . .
H14A H 0.397634 0.224412 0.955933 0.102 Uiso 1 1 calc GR . . . .
H14B H 0.277851 0.186649 1.032956 0.102 Uiso 1 1 calc GR . . . .
H14C H 0.313589 0.320020 1.014073 0.102 Uiso 1 1 calc GR . . . .
C15 C 0.0373(6) 0.3503(6) 0.9233(5) 0.0708(15) Uani 1 1 d . . . . .
H15A H 0.030012 0.413284 0.960786 0.106 Uiso 1 1 calc GR . . . .
H15B H 0.014119 0.274884 0.971636 0.106 Uiso 1 1 calc GR . . . .
H15C H -0.020102 0.380344 0.865810 0.106 Uiso 1 1 calc GR . . . .
C16 C 0.2145(6) 0.2016(5) 0.7943(5) 0.0657(14) Uani 1 1 d . . . . .
H16A H 0.155941 0.234781 0.737666 0.099 Uiso 1 1 calc GR . . . .
H16B H 0.190382 0.125826 0.841345 0.099 Uiso 1 1 calc GR . . . .
H16C H 0.301610 0.183396 0.764466 0.099 Uiso 1 1 calc GR . . . .
C17 C 0.2220(4) 0.5183(4) 0.6762(3) 0.0410(9) Uani 1 1 d . . . . .
H17 H 0.195006 0.478246 0.631662 0.049 Uiso 1 1 calc R . . . .
C18 C 0.2396(4) 0.6412(4) 0.6477(3) 0.0403(8) Uani 1 1 d . . . . .
H18 H 0.225353 0.698163 0.580991 0.048 Uiso 1 1 calc R . . . .
C19 C 0.2824(4) 0.6672(3) 0.7346(3) 0.0362(8) Uani 1 1 d . . . . .
C20 C 0.3927(5) 0.8153(4) 0.8488(4) 0.0544(11) Uani 1 1 d . . . . .
H20A H 0.366117 0.762753 0.916511 0.082 Uiso 1 1 calc GR . . . .
H20B H 0.391655 0.898152 0.855221 0.082 Uiso 1 1 calc GR . . . .
H20C H 0.479045 0.780425 0.827086 0.082 Uiso 1 1 calc GR . . . .
C21 C 0.1165(5) 0.8811(5) 0.7996(5) 0.0679(15) Uani 1 1 d . . . . .
H21A H 0.055456 0.889346 0.747723 0.102 Uiso 1 1 calc GR . . . .
H21B H 0.113728 0.961397 0.812001 0.102 Uiso 1 1 calc GR . . . .
H21C H 0.094259 0.822254 0.865295 0.102 Uiso 1 1 calc GR . . . .
C22 C 0.3179(6) 0.9326(4) 0.6216(4) 0.0654(14) Uani 1 1 d . . . . .
H22A H 0.401777 0.901462 0.592536 0.098 Uiso 1 1 calc GR . . . .
H22B H 0.318139 1.013528 0.631721 0.098 Uiso 1 1 calc GR . . . .
H22C H 0.253047 0.940275 0.572993 0.098 Uiso 1 1 calc GR . . . .


_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
Nd1 I1 3.1531(3) 2_666 ?
Nd1 I1 3.1522(3) . ?
Nd1 C1 2.766(4) . ?
Nd1 C2 2.779(4) . ?
Nd1 C6 2.713(4) . ?
Nd1 C7 2.706(4) . ?
Nd1 C8 2.769(4) . ?
Nd1 C12 2.734(4) . ?
Nd1 C13 2.746(4) . ?
Nd1 C17 2.734(4) . ?
Nd1 C18 2.744(4) . ?
Nd1 C19 2.745(4) . ?
Si1 C8 1.875(4) . ?
Si1 C9 1.856(5) . ?
Si1 C10 1.863(5) . ?
Si1 C11 1.858(5) . ?
Si2 C2 1.866(4) . ?
Si2 C3 1.860(6) . ?
Si2 C4 1.873(5) . ?
Si2 C5 1.863(5) . ?
Si3 C13 1.868(4) . ?
Si3 C14 1.871(6) . ?
Si3 C15 1.880(6) . ?
Si3 C16 1.857(5) . ?
Si4 C19 1.870(4) . ?
Si4 C20 1.860(5) . ?
Si4 C21 1.877(5) . ?
Si4 C22 1.854(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.431(6) . ?
C1 C8 1.419(5) . ?
C2 C6 1.429(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6 0.9500 . ?
C6 C7 1.417(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.418(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 0.9500 . ?
C12 C13 1.419(5) . ?
C12 C19 1.412(5) . ?
C13 C17 1.421(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 0.9500 . ?
C17 C18 1.402(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.424(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Nd1 I1 84.417(8) . 2_666 ?
C1 Nd1 I1 90.97(9) . . ?
C1 Nd1 I1 91.88(8) . 2_666 ?
C1 Nd1 C2 29.91(12) . . ?
C1 Nd1 C8 29.71(11) . . ?
C2 Nd1 I1 119.40(9) . . ?
C2 Nd1 I1 85.84(9) . 2_666 ?
C6 Nd1 I1 110.97(9) . 2_666 ?
C6 Nd1 I1 135.66(9) . . ?
C6 Nd1 C1 48.94(13) . . ?
C6 Nd1 C2 30.13(13) . . ?
C6 Nd1 C8 49.78(12) . . ?
C6 Nd1 C12 84.23(13) . . ?
C6 Nd1 C13 93.51(13) . . ?
C6 Nd1 C17 123.51(13) . . ?
C6 Nd1 C18 132.63(13) . . ?
C6 Nd1 C19 105.65(13) . . ?
C7 Nd1 I1 111.72(9) . . ?
C7 Nd1 I1 135.68(9) . 2_666 ?
C7 Nd1 C1 48.90(12) . . ?
C7 Nd1 C2 50.00(12) . . ?
C7 Nd1 C6 30.32(12) . . ?
C7 Nd1 C8 29.99(13) . . ?
C7 Nd1 C12 83.83(13) . . ?
C7 Nd1 C13 105.99(13) . . ?
C7 Nd1 C17 132.55(13) . . ?
C7 Nd1 C18 122.25(13) . . ?
C7 Nd1 C19 92.29(12) . . ?
C8 Nd1 I1 86.23(9) . . ?
C8 Nd1 I1 120.48(8) . 2_666 ?
C8 Nd1 C2 50.04(11) . . ?
C12 Nd1 I1 122.61(8) . 2_666 ?
C12 Nd1 I1 123.20(8) . . ?
C12 Nd1 C1 130.90(12) . . ?
C12 Nd1 C2 112.13(12) . . ?
C12 Nd1 C8 111.39(12) . . ?
C12 Nd1 C13 30.01(11) . . ?
C12 Nd1 C17 48.85(12) . . ?
C12 Nd1 C18 48.66(12) . . ?
C12 Nd1 C19 29.87(11) . . ?
C13 Nd1 I1 128.22(8) . . ?
C13 Nd1 I1 92.67(8) . 2_666 ?
C13 Nd1 C1 140.80(12) . . ?
C13 Nd1 C2 111.86(12) . . ?
C13 Nd1 C8 135.94(12) . . ?
C17 Nd1 I1 80.28(9) . 2_666 ?
C17 Nd1 I1 99.49(9) . . ?
C17 Nd1 C1 166.19(12) . . ?
C17 Nd1 C2 137.09(12) . . ?
C17 Nd1 C8 159.06(12) . . ?
C17 Nd1 C13 30.06(12) . . ?
C17 Nd1 C18 29.65(12) . . ?
C17 Nd1 C19 49.70(12) . . ?
C18 Nd1 I1 80.19(9) . . ?
C18 Nd1 I1 100.57(9) . 2_666 ?
C18 Nd1 C1 163.87(12) . . ?
C18 Nd1 C2 160.09(13) . . ?
C18 Nd1 C8 135.15(12) . . ?
C18 Nd1 C13 49.49(12) . . ?
C18 Nd1 C19 30.07(12) . . ?
C19 Nd1 I1 128.98(8) . 2_666 ?
C19 Nd1 I1 93.47(8) . . ?
C19 Nd1 C1 139.14(12) . . ?
C19 Nd1 C2 135.78(12) . . ?
C19 Nd1 C8 110.17(12) . . ?
C19 Nd1 C13 50.24(11) . . ?
Nd1 I1 Nd1 95.583(8) . 2_666 ?
C9 Si1 C8 107.0(2) . . ?
C9 Si1 C10 107.1(3) . . ?
C9 Si1 C11 109.3(3) . . ?
C10 Si1 C8 113.1(2) . . ?
C11 Si1 C8 109.9(2) . . ?
C11 Si1 C10 110.3(3) . . ?
C2 Si2 C4 113.6(2) . . ?
C3 Si2 C2 109.1(2) . . ?
C3 Si2 C4 110.4(3) . . ?
C3 Si2 C5 109.1(3) . . ?
C5 Si2 C2 107.2(2) . . ?
C5 Si2 C4 107.4(3) . . ?
C13 Si3 C14 109.7(2) . . ?
C13 Si3 C15 108.7(2) . . ?
C14 Si3 C15 108.0(3) . . ?
C16 Si3 C13 111.2(2) . . ?
C16 Si3 C14 111.0(3) . . ?
C16 Si3 C15 108.1(3) . . ?
C19 Si4 C21 107.3(2) . . ?
C20 Si4 C19 110.3(2) . . ?
C20 Si4 C21 107.4(3) . . ?
C22 Si4 C19 111.2(2) . . ?
C22 Si4 C20 111.8(3) . . ?
C22 Si4 C21 108.7(3) . . ?
Nd1 C1 H1 116.4 . . ?
C2 C1 Nd1 75.5(2) . . ?
C2 C1 H1 124.6 . . ?
C8 C1 Nd1 75.3(2) . . ?
C8 C1 H1 124.6 . . ?
C8 C1 C2 110.8(4) . . ?
Si2 C2 Nd1 130.3(2) . . ?
C1 C2 Nd1 74.5(2) . . ?
C1 C2 Si2 125.2(3) . . ?
C6 C2 Nd1 72.4(2) . . ?
C6 C2 Si2 127.7(3) . . ?
C6 C2 C1 105.1(3) . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Nd1 C6 H6 114.6 . . ?
C2 C6 Nd1 77.5(2) . . ?
C2 C6 H6 125.4 . . ?
C7 C6 Nd1 74.6(2) . . ?
C7 C6 C2 109.1(4) . . ?
C7 C6 H6 125.4 . . ?
Nd1 C7 H7 114.1 . . ?
C6 C7 Nd1 75.1(2) . . ?
C6 C7 H7 125.5 . . ?
C6 C7 C8 109.0(4) . . ?
C8 C7 Nd1 77.5(2) . . ?
C8 C7 H7 125.5 . . ?
Si1 C8 Nd1 129.30(19) . . ?
C1 C8 Nd1 75.0(2) . . ?
C1 C8 Si1 124.9(3) . . ?
C7 C8 Nd1 72.6(2) . . ?
C7 C8 Si1 127.3(3) . . ?
C7 C8 C1 106.0(3) . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Nd1 C12 H12 116.2 . . ?
C13 C12 Nd1 75.5(2) . . ?
C13 C12 H12 124.6 . . ?
C19 C12 Nd1 75.5(2) . . ?
C19 C12 H12 124.6 . . ?
C19 C12 C13 110.9(4) . . ?
Si3 C13 Nd1 129.12(19) . . ?
C12 C13 Nd1 74.5(2) . . ?
C12 C13 Si3 126.0(3) . . ?
C12 C13 C17 105.5(3) . . ?
C17 C13 Nd1 74.5(2) . . ?
C17 C13 Si3 126.3(3) . . ?
Si3 C14 H14A 109.5 . . ?
Si3 C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si3 C15 H15A 109.5 . . ?
Si3 C15 H15B 109.5 . . ?
Si3 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si3 C16 H16A 109.5 . . ?
Si3 C16 H16B 109.5 . . ?
Si3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Nd1 C17 H17 115.5 . . ?
C13 C17 Nd1 75.4(2) . . ?
C13 C17 H17 125.5 . . ?
C18 C17 Nd1 75.6(2) . . ?
C18 C17 C13 109.0(4) . . ?
C18 C17 H17 125.5 . . ?
Nd1 C18 H18 116.7 . . ?
C17 C18 Nd1 74.8(2) . . ?
C17 C18 H18 125.4 . . ?
C17 C18 C19 109.2(4) . . ?
C19 C18 Nd1 75.0(2) . . ?
C19 C18 H18 125.4 . . ?
Si4 C19 Nd1 129.83(18) . . ?
C12 C19 Nd1 74.6(2) . . ?
C12 C19 Si4 126.2(3) . . ?
C12 C19 C18 105.5(3) . . ?
C18 C19 Nd1 74.9(2) . . ?
C18 C19 Si4 125.7(3) . . ?
Si4 C20 H20A 109.5 . . ?
Si4 C20 H20B 109.5 . . ?
Si4 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si4 C21 H21A 109.5 . . ?
Si4 C21 H21B 109.5 . . ?
Si4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si4 C22 H22A 109.5 . . ?
Si4 C22 H22B 109.5 . . ?
Si4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 C1 C2 Si2 128.7(3) . . . . ?
Nd1 C1 C2 C6 -66.5(3) . . . . ?
Nd1 C1 C8 Si1 -127.8(3) . . . . ?
Nd1 C1 C8 C7 66.4(3) . . . . ?
Nd1 C2 C6 C7 -68.6(3) . . . . ?
Nd1 C6 C7 C8 -70.8(3) . . . . ?
Nd1 C7 C8 Si1 126.5(3) . . . . ?
Nd1 C7 C8 C1 -68.2(3) . . . . ?
Nd1 C12 C13 Si3 127.4(3) . . . . ?
Nd1 C12 C13 C17 -68.6(3) . . . . ?
Nd1 C12 C19 Si4 -128.5(3) . . . . ?
Nd1 C12 C19 C18 69.1(3) . . . . ?
Nd1 C13 C17 C18 -68.8(3) . . . . ?
Nd1 C17 C18 C19 -67.8(3) . . . . ?
Nd1 C18 C19 Si4 128.5(3) . . . . ?
Nd1 C18 C19 C12 -68.9(3) . . . . ?
Si2 C2 C6 Nd1 -127.7(3) . . . . ?
Si2 C2 C6 C7 163.7(3) . . . . ?
Si3 C13 C17 Nd1 -127.5(3) . . . . ?
Si3 C13 C17 C18 163.7(3) . . . . ?
C1 C2 C6 Nd1 68.0(3) . . . . ?
C1 C2 C6 C7 -0.6(4) . . . . ?
C2 C1 C8 Nd1 -67.9(3) . . . . ?
C2 C1 C8 Si1 164.3(3) . . . . ?
C2 C1 C8 C7 -1.5(5) . . . . ?
C2 C6 C7 Nd1 70.5(3) . . . . ?
C2 C6 C7 C8 -0.3(5) . . . . ?
C3 Si2 C2 Nd1 82.3(3) . . . . ?
C3 Si2 C2 C1 -17.5(4) . . . . ?
C3 Si2 C2 C6 -178.8(4) . . . . ?
C4 Si2 C2 Nd1 -41.2(4) . . . . ?
C4 Si2 C2 C1 -141.0(4) . . . . ?
C4 Si2 C2 C6 57.6(5) . . . . ?
C5 Si2 C2 Nd1 -159.7(3) . . . . ?
C5 Si2 C2 C1 100.5(4) . . . . ?
C5 Si2 C2 C6 -60.8(4) . . . . ?
C6 C7 C8 Nd1 69.2(3) . . . . ?
C6 C7 C8 Si1 -164.3(3) . . . . ?
C6 C7 C8 C1 1.0(4) . . . . ?
C8 C1 C2 Nd1 67.7(3) . . . . ?
C8 C1 C2 Si2 -163.5(3) . . . . ?
C8 C1 C2 C6 1.3(5) . . . . ?
C9 Si1 C8 Nd1 157.5(3) . . . . ?
C9 Si1 C8 C1 -103.1(4) . . . . ?
C9 Si1 C8 C7 59.6(4) . . . . ?
C10 Si1 C8 Nd1 39.8(3) . . . . ?
C10 Si1 C8 C1 139.2(4) . . . . ?
C10 Si1 C8 C7 -58.1(4) . . . . ?
C11 Si1 C8 Nd1 -83.9(3) . . . . ?
C11 Si1 C8 C1 15.5(4) . . . . ?
C11 Si1 C8 C7 178.2(4) . . . . ?
C12 C13 C17 Nd1 68.6(3) . . . . ?
C12 C13 C17 C18 -0.2(4) . . . . ?
C13 C12 C19 Nd1 -67.9(3) . . . . ?
C13 C12 C19 Si4 163.6(3) . . . . ?
C13 C12 C19 C18 1.2(5) . . . . ?
C13 C17 C18 Nd1 68.7(3) . . . . ?
C13 C17 C18 C19 0.9(5) . . . . ?
C14 Si3 C13 Nd1 60.2(3) . . . . ?
C14 Si3 C13 C12 -39.3(4) . . . . ?
C14 Si3 C13 C17 159.9(4) . . . . ?
C15 Si3 C13 Nd1 178.0(3) . . . . ?
C15 Si3 C13 C12 78.5(4) . . . . ?
C15 Si3 C13 C17 -82.2(4) . . . . ?
C16 Si3 C13 Nd1 -63.0(3) . . . . ?
C16 Si3 C13 C12 -162.5(4) . . . . ?
C16 Si3 C13 C17 36.8(4) . . . . ?
C17 C18 C19 Nd1 67.6(3) . . . . ?
C17 C18 C19 Si4 -163.8(3) . . . . ?
C17 C18 C19 C12 -1.3(4) . . . . ?
C19 C12 C13 Nd1 68.0(3) . . . . ?
C19 C12 C13 Si3 -164.6(3) . . . . ?
C19 C12 C13 C17 -0.6(5) . . . . ?
C20 Si4 C19 Nd1 -60.3(3) . . . . ?
C20 Si4 C19 C12 40.2(4) . . . . ?
C20 Si4 C19 C18 -160.8(4) . . . . ?
C21 Si4 C19 Nd1 -176.9(3) . . . . ?
C21 Si4 C19 C12 -76.4(4) . . . . ?
C21 Si4 C19 C18 82.6(4) . . . . ?
C22 Si4 C19 Nd1 64.3(3) . . . . ?
C22 Si4 C19 C12 164.8(4) . . . . ?
C22 Si4 C19 C18 -36.2(4) . . . . ?

_audit_author_email              
;
benjamin.reant@postgrad.manchester.ac.uk, david.mills@manchester.ac.uk    
;
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 1s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_type   custom
_olex2_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR4.347
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.085
_oxdiff_exptl_absorpt_empirical_full_min 0.461
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-Ti
_database_code_depnum_ccdc_archive 'CCDC 2195635'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   rdpm242
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   15/10/2020
_manchester_internal_process_date 15/10/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 16/10/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 16/10/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 16/10/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 16/10/2020
_manchester_internal_archive_user AW
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_audit_creation_date             2020-10-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        "[Ti(Cp'')2{Si(SiMe3)3}]"
_chemical_formula_moiety         'C31 H69 Si8 Ti'
_chemical_formula_sum            'C31 H69 Si8 Ti'
_chemical_formula_weight         714.48
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ti1 Si8 C31 H69'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_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'

_cell_length_a                   10.2297(2)
_cell_length_b                   23.3116(4)
_cell_length_c                   18.6778(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.213(2)
_cell_angle_gamma                90
_cell_volume                     4369.09(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9980
_cell_measurement_theta_min      1.7390
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.846
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blackish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 -9 -9 0.0882
-14 9 9 0.0502
-3 -7 -24 0.1944
3 7 24 0.1944
-3 -31 9 0.0720
3 31 -9 0.0720

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method -
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.138
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
14.0000 -8.9999 -9.0000 -0.3535 -0.9578 0.0133
-14.0000 8.9999 9.0000 0.3535 0.9578 -0.0133
-3.0000 -6.9999 -24.0000 0.0018 -0.0219 -1.0147
3.0000 6.9999 24.0000 -0.0018 0.0219 1.0147
-3.0000 -30.9999 9.0001 -0.9522 0.3435 0.0443
3.0000 30.9999 -9.0001 0.9522 -0.3435 -0.0443

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26334
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         1.747
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  33.00   1.00    5.00    --   -7.30  38.00 -60.00   71
  2  ω    -80.00  20.00   1.00    5.00    --   -7.30 -57.00  90.00  100
  3  ω    -66.00  -7.00   1.00    5.00    --   -7.30 -57.00 -30.00   59
  4  ω    -54.00  72.00   1.00    5.00    --   -7.50  19.00-120.00  126
  5  ω    -84.00 -12.00   1.00    5.00    --   -7.50   0.00  60.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0109236000
_diffrn_orient_matrix_UB_12      0.0296374000
_diffrn_orient_matrix_UB_13      -0.0073557000
_diffrn_orient_matrix_UB_21      -0.0636935000
_diffrn_orient_matrix_UB_22      -0.0021583000
_diffrn_orient_matrix_UB_23      0.0095053000
_diffrn_orient_matrix_UB_31      0.0287613000
_diffrn_orient_matrix_UB_32      0.0064703000
_diffrn_orient_matrix_UB_33      0.0367963000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                7530
_reflns_number_total             8020
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8020
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0279
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0465P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0708
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.90(2)
 0.10(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C16(H16), C21(H21), C26(H26), C27(H27)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.51849(5) 0.66528(2) 0.50825(3) 0.01290(11) Uani 1 1 d . . . . .
Si1 Si 0.52145(9) 0.78419(3) 0.50780(5) 0.01551(15) Uani 1 1 d . . . . .
Si2 Si 0.36716(8) 0.83623(3) 0.42025(5) 0.02372(19) Uani 1 1 d . . . . .
Si3 Si 0.72249(8) 0.83694(3) 0.51229(5) 0.02273(19) Uani 1 1 d . . . . .
Si4 Si 0.47163(8) 0.81302(4) 0.62069(5) 0.02451(19) Uani 1 1 d . . . . .
Si5 Si 0.33301(8) 0.55185(3) 0.35733(4) 0.01923(18) Uani 1 1 d . . . . .
Si6 Si 0.24262(8) 0.63104(3) 0.63072(4) 0.02124(18) Uani 1 1 d . . . . .
Si7 Si 0.68878(7) 0.54455(3) 0.64936(4) 0.01701(17) Uani 1 1 d . . . . .
Si8 Si 0.75523(8) 0.64620(3) 0.37352(4) 0.01981(18) Uani 1 1 d . . . . .
C1 C 0.1904(3) 0.80951(14) 0.40124(19) 0.0311(8) Uani 1 1 d . . . . .
H1A H 0.187286 0.771167 0.379448 0.047 Uiso 1 1 calc GR . . . .
H1B H 0.134594 0.835754 0.367364 0.047 Uiso 1 1 calc GR . . . .
H1C H 0.157238 0.807660 0.447002 0.047 Uiso 1 1 calc GR . . . .
C2 C 0.4244(5) 0.8352(2) 0.3301(2) 0.0657(15) Uani 1 1 d . . . . .
H2A H 0.509141 0.855834 0.334964 0.099 Uiso 1 1 calc GR . . . .
H2B H 0.357283 0.853757 0.292741 0.099 Uiso 1 1 calc GR . . . .
H2C H 0.436642 0.795376 0.315827 0.099 Uiso 1 1 calc GR . . . .
C3 C 0.3458(4) 0.91356(14) 0.4457(3) 0.0506(11) Uani 1 1 d . . . . .
H3A H 0.313767 0.915193 0.491836 0.076 Uiso 1 1 calc GR . . . .
H3B H 0.280923 0.932192 0.407222 0.076 Uiso 1 1 calc GR . . . .
H3C H 0.431589 0.933446 0.451322 0.076 Uiso 1 1 calc GR . . . .
C4 C 0.7016(4) 0.91740(13) 0.5087(2) 0.0405(9) Uani 1 1 d . . . . .
H4A H 0.655722 0.928824 0.459773 0.061 Uiso 1 1 calc GR . . . .
H4B H 0.789379 0.935748 0.519948 0.061 Uiso 1 1 calc GR . . . .
H4C H 0.648777 0.929398 0.544630 0.061 Uiso 1 1 calc GR . . . .
C5 C 0.8084(4) 0.82233(14) 0.4337(2) 0.0330(8) Uani 1 1 d . . . . .
H5A H 0.828615 0.781313 0.432067 0.049 Uiso 1 1 calc GR . . . .
H5B H 0.891393 0.844411 0.440125 0.049 Uiso 1 1 calc GR . . . .
H5C H 0.749894 0.833670 0.387871 0.049 Uiso 1 1 calc GR . . . .
C6 C 0.8493(3) 0.82242(15) 0.59825(19) 0.0326(8) Uani 1 1 d . . . . .
H6A H 0.816129 0.837182 0.640491 0.049 Uiso 1 1 calc GR . . . .
H6B H 0.933333 0.841540 0.595120 0.049 Uiso 1 1 calc GR . . . .
H6C H 0.864290 0.780994 0.603740 0.049 Uiso 1 1 calc GR . . . .
C7 C 0.5123(4) 0.88988(15) 0.6480(2) 0.0399(9) Uani 1 1 d . . . . .
H7A H 0.608508 0.896056 0.653856 0.060 Uiso 1 1 calc GR . . . .
H7B H 0.484256 0.897917 0.694288 0.060 Uiso 1 1 calc GR . . . .
H7C H 0.465097 0.915574 0.610092 0.060 Uiso 1 1 calc GR . . . .
C8 C 0.5711(4) 0.76846(17) 0.69639(18) 0.0390(9) Uani 1 1 d . . . . .
H8A H 0.552606 0.727710 0.686254 0.058 Uiso 1 1 calc GR . . . .
H8B H 0.546120 0.778714 0.742806 0.058 Uiso 1 1 calc GR . . . .
H8C H 0.666388 0.775806 0.699461 0.058 Uiso 1 1 calc GR . . . .
C9 C 0.2881(4) 0.80778(15) 0.62167(18) 0.0322(8) Uani 1 1 d . . . . .
H9A H 0.238651 0.834028 0.585194 0.048 Uiso 1 1 calc GR . . . .
H9B H 0.272607 0.818197 0.670162 0.048 Uiso 1 1 calc GR . . . .
H9C H 0.257655 0.768391 0.610153 0.048 Uiso 1 1 calc GR . . . .
C10 C 0.3553(3) 0.59218(11) 0.50740(15) 0.0164(6) Uani 1 1 d . . . . .
H10 H 0.380554 0.555812 0.528584 0.020 Uiso 1 1 calc R . . . .
C11 C 0.3165(3) 0.63970(12) 0.54631(15) 0.0166(6) Uani 1 1 d . . . . .
C12 C 0.0694(3) 0.65996(16) 0.6062(2) 0.0358(8) Uani 1 1 d . . . . .
H12A H 0.072616 0.700590 0.593192 0.054 Uiso 1 1 calc GR . . . .
H12B H 0.025114 0.655924 0.647985 0.054 Uiso 1 1 calc GR . . . .
H12C H 0.019504 0.638533 0.564556 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.2317(3) 0.55211(14) 0.64652(18) 0.0301(7) Uani 1 1 d . . . . .
H13A H 0.178703 0.534005 0.603047 0.045 Uiso 1 1 calc GR . . . .
H13B H 0.189198 0.545369 0.688476 0.045 Uiso 1 1 calc GR . . . .
H13C H 0.321532 0.535601 0.656329 0.045 Uiso 1 1 calc GR . . . .
C14 C 0.3248(4) 0.66619(14) 0.71743(18) 0.0334(8) Uani 1 1 d . . . . .
H14A H 0.418241 0.654151 0.729788 0.050 Uiso 1 1 calc GR . . . .
H14B H 0.279010 0.654965 0.756735 0.050 Uiso 1 1 calc GR . . . .
H14C H 0.320289 0.707947 0.711365 0.050 Uiso 1 1 calc GR . . . .
C15 C 0.2896(3) 0.68477(12) 0.49298(15) 0.0160(6) Uani 1 1 d . . . . .
H15 H 0.261807 0.722547 0.501928 0.019 Uiso 1 1 calc R . . . .
C16 C 0.3109(3) 0.66404(11) 0.42527(16) 0.0162(6) Uani 1 1 d . . . . .
H16 H 0.299843 0.685719 0.381432 0.019 Uiso 1 1 calc R . . . .
C17 C 0.3514(3) 0.60596(11) 0.43269(15) 0.0161(6) Uani 1 1 d . . . . .
C18 C 0.3643(4) 0.58508(13) 0.27126(17) 0.0290(7) Uani 1 1 d . . . . .
H18A H 0.311423 0.620222 0.261060 0.044 Uiso 1 1 calc GR . . . .
H18B H 0.338836 0.558052 0.230760 0.044 Uiso 1 1 calc GR . . . .
H18C H 0.459191 0.594395 0.276790 0.044 Uiso 1 1 calc GR . . . .
C19 C 0.1541(3) 0.53049(14) 0.34257(18) 0.0277(7) Uani 1 1 d . . . . .
H19A H 0.133324 0.516406 0.388525 0.042 Uiso 1 1 calc GR . . . .
H19B H 0.136914 0.500085 0.305706 0.042 Uiso 1 1 calc GR . . . .
H19C H 0.097908 0.563770 0.325722 0.042 Uiso 1 1 calc GR . . . .
C20 C 0.4377(3) 0.48668(13) 0.38389(17) 0.0252(7) Uani 1 1 d . . . . .
H20A H 0.531396 0.495920 0.384609 0.038 Uiso 1 1 calc GR . . . .
H20B H 0.409016 0.455987 0.348454 0.038 Uiso 1 1 calc GR . . . .
H20C H 0.427546 0.473960 0.432518 0.038 Uiso 1 1 calc GR . . . .
C21 C 0.6749(3) 0.59119(11) 0.50170(15) 0.0170(6) Uani 1 1 d . . . . .
H21 H 0.646530 0.556243 0.477421 0.020 Uiso 1 1 calc R . . . .
C22 C 0.6814(3) 0.60121(11) 0.57765(15) 0.0162(6) Uani 1 1 d . . . . .
C23 C 0.6080(3) 0.47697(12) 0.60967(17) 0.0270(7) Uani 1 1 d . . . . .
H23A H 0.511364 0.482691 0.596343 0.041 Uiso 1 1 calc GR . . . .
H23B H 0.627290 0.446061 0.645736 0.041 Uiso 1 1 calc GR . . . .
H23C H 0.642729 0.466650 0.566065 0.041 Uiso 1 1 calc GR . . . .
C24 C 0.6150(3) 0.56924(15) 0.72746(17) 0.0293(7) Uani 1 1 d . . . . .
H24A H 0.639441 0.609397 0.738381 0.044 Uiso 1 1 calc GR . . . .
H24B H 0.649009 0.545518 0.770359 0.044 Uiso 1 1 calc GR . . . .
H24C H 0.517789 0.565828 0.714803 0.044 Uiso 1 1 calc GR . . . .
C25 C 0.8710(3) 0.53199(14) 0.68271(18) 0.0271(7) Uani 1 1 d . . . . .
H25A H 0.911562 0.519328 0.641980 0.041 Uiso 1 1 calc GR . . . .
H25B H 0.883602 0.502356 0.720653 0.041 Uiso 1 1 calc GR . . . .
H25C H 0.913431 0.567692 0.702978 0.041 Uiso 1 1 calc GR . . . .
C26 C 0.7265(3) 0.65844(12) 0.58987(16) 0.0167(6) Uani 1 1 d . . . . .
H26 H 0.739824 0.677829 0.635447 0.020 Uiso 1 1 calc R . . . .
C27 C 0.7485(3) 0.68210(12) 0.52390(15) 0.0157(6) Uani 1 1 d . . . . .
H27 H 0.779738 0.719845 0.517946 0.019 Uiso 1 1 calc R . . . .
C28 C 0.7164(3) 0.64022(12) 0.46727(16) 0.0167(6) Uani 1 1 d . . . . .
C29 C 0.6399(4) 0.69808(14) 0.31614(17) 0.0308(7) Uani 1 1 d . . . . .
H29A H 0.547387 0.686174 0.314323 0.046 Uiso 1 1 calc GR . . . .
H29B H 0.658332 0.698667 0.266595 0.046 Uiso 1 1 calc GR . . . .
H29C H 0.653506 0.736529 0.337505 0.046 Uiso 1 1 calc GR . . . .
C30 C 0.9323(4) 0.66995(15) 0.3836(2) 0.0326(8) Uani 1 1 d . . . . .
H30A H 0.943564 0.707261 0.408181 0.049 Uiso 1 1 calc GR . . . .
H30B H 0.955323 0.673345 0.335207 0.049 Uiso 1 1 calc GR . . . .
H30C H 0.990915 0.641709 0.412595 0.049 Uiso 1 1 calc GR . . . .
C31 C 0.7444(3) 0.57333(14) 0.33154(17) 0.0284(7) Uani 1 1 d . . . . .
H31A H 0.809194 0.547861 0.361522 0.043 Uiso 1 1 calc GR . . . .
H31B H 0.764085 0.575855 0.282332 0.043 Uiso 1 1 calc GR . . . .
H31C H 0.654404 0.557976 0.328713 0.043 Uiso 1 1 calc GR . . . .


_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
Ti1 Si1 2.7722(8) . ?
Ti1 C10 2.384(3) . ?
Ti1 C11 2.388(3) . ?
Ti1 C15 2.348(3) . ?
Ti1 C16 2.373(3) . ?
Ti1 C17 2.426(3) . ?
Ti1 C21 2.374(3) . ?
Ti1 C22 2.418(3) . ?
Ti1 C26 2.370(3) . ?
Ti1 C27 2.347(3) . ?
Ti1 C28 2.373(3) . ?
Si1 Si2 2.3734(11) . ?
Si1 Si3 2.3836(12) . ?
Si1 Si4 2.3613(12) . ?
Si2 C1 1.880(3) . ?
Si2 C2 1.887(4) . ?
Si2 C3 1.888(4) . ?
Si3 C4 1.887(3) . ?
Si3 C5 1.883(3) . ?
Si3 C6 1.888(3) . ?
Si4 C7 1.887(3) . ?
Si4 C8 1.885(4) . ?
Si4 C9 1.885(4) . ?
Si5 C17 1.872(3) . ?
Si5 C18 1.868(3) . ?
Si5 C19 1.865(3) . ?
Si5 C20 1.869(3) . ?
Si6 C11 1.887(3) . ?
Si6 C12 1.868(3) . ?
Si6 C13 1.870(3) . ?
Si6 C14 1.863(3) . ?
Si7 C22 1.872(3) . ?
Si7 C23 1.864(3) . ?
Si7 C24 1.859(3) . ?
Si7 C25 1.870(3) . ?
Si8 C28 1.874(3) . ?
Si8 C29 1.874(3) . ?
Si8 C30 1.868(4) . ?
Si8 C31 1.865(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.423(4) . ?
C10 C17 1.425(4) . ?
C11 C15 1.437(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 0.9500 . ?
C15 C16 1.410(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.415(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 0.9500 . ?
C21 C22 1.426(4) . ?
C21 C28 1.417(4) . ?
C22 C26 1.416(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.408(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.430(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 Ti1 Si1 136.29(7) . . ?
C10 Ti1 C11 34.70(9) . . ?
C10 Ti1 C17 34.45(10) . . ?
C10 Ti1 C22 88.33(9) . . ?
C11 Ti1 Si1 105.14(7) . . ?
C11 Ti1 C17 58.56(10) . . ?
C11 Ti1 C22 103.43(10) . . ?
C15 Ti1 Si1 79.47(7) . . ?
C15 Ti1 C10 57.09(9) . . ?
C15 Ti1 C11 35.32(9) . . ?
C15 Ti1 C16 34.75(10) . . ?
C15 Ti1 C17 57.75(10) . . ?
C15 Ti1 C21 143.23(10) . . ?
C15 Ti1 C22 138.75(10) . . ?
C15 Ti1 C26 147.23(10) . . ?
C15 Ti1 C28 154.43(10) . . ?
C16 Ti1 Si1 91.10(7) . . ?
C16 Ti1 C10 56.65(10) . . ?
C16 Ti1 C11 58.35(10) . . ?
C16 Ti1 C17 34.26(9) . . ?
C16 Ti1 C21 118.95(10) . . ?
C16 Ti1 C22 141.11(10) . . ?
C17 Ti1 Si1 125.10(7) . . ?
C21 Ti1 Si1 136.01(7) . . ?
C21 Ti1 C10 87.59(9) . . ?
C21 Ti1 C11 117.69(10) . . ?
C21 Ti1 C17 87.77(10) . . ?
C21 Ti1 C22 34.62(10) . . ?
C22 Ti1 Si1 127.76(7) . . ?
C22 Ti1 C17 107.09(8) . . ?
C26 Ti1 Si1 93.46(7) . . ?
C26 Ti1 C10 119.76(10) . . ?
C26 Ti1 C11 120.82(10) . . ?
C26 Ti1 C16 175.40(8) . . ?
C26 Ti1 C17 141.14(9) . . ?
C26 Ti1 C21 56.92(10) . . ?
C26 Ti1 C22 34.37(9) . . ?
C26 Ti1 C28 58.34(10) . . ?
C27 Ti1 Si1 79.75(7) . . ?
C27 Ti1 C10 143.54(10) . . ?
C27 Ti1 C11 155.41(10) . . ?
C27 Ti1 C15 159.22(8) . . ?
C27 Ti1 C16 146.24(10) . . ?
C27 Ti1 C17 138.03(10) . . ?
C27 Ti1 C21 57.20(10) . . ?
C27 Ti1 C22 57.77(10) . . ?
C27 Ti1 C26 34.72(10) . . ?
C27 Ti1 C28 35.26(10) . . ?
C28 Ti1 Si1 103.57(7) . . ?
C28 Ti1 C10 117.55(10) . . ?
C28 Ti1 C11 151.25(9) . . ?
C28 Ti1 C16 119.84(10) . . ?
C28 Ti1 C17 102.77(10) . . ?
C28 Ti1 C21 34.73(10) . . ?
C28 Ti1 C22 58.57(10) . . ?
Si2 Si1 Ti1 120.47(4) . . ?
Si2 Si1 Si3 102.36(4) . . ?
Si3 Si1 Ti1 121.71(4) . . ?
Si4 Si1 Ti1 106.11(4) . . ?
Si4 Si1 Si2 103.86(4) . . ?
Si4 Si1 Si3 98.99(4) . . ?
C1 Si2 Si1 116.55(10) . . ?
C1 Si2 C2 106.3(2) . . ?
C1 Si2 C3 102.11(17) . . ?
C2 Si2 Si1 109.13(13) . . ?
C2 Si2 C3 108.0(2) . . ?
C3 Si2 Si1 114.12(13) . . ?
C4 Si3 Si1 114.86(12) . . ?
C4 Si3 C6 105.22(17) . . ?
C5 Si3 Si1 114.17(12) . . ?
C5 Si3 C4 102.66(17) . . ?
C5 Si3 C6 106.44(17) . . ?
C6 Si3 Si1 112.51(12) . . ?
C7 Si4 Si1 115.94(13) . . ?
C8 Si4 Si1 109.51(11) . . ?
C8 Si4 C7 105.18(17) . . ?
C9 Si4 Si1 112.24(11) . . ?
C9 Si4 C7 103.08(16) . . ?
C9 Si4 C8 110.52(17) . . ?
C18 Si5 C17 111.02(13) . . ?
C18 Si5 C20 112.34(15) . . ?
C19 Si5 C17 104.08(14) . . ?
C19 Si5 C18 108.14(16) . . ?
C19 Si5 C20 108.51(15) . . ?
C20 Si5 C17 112.30(13) . . ?
C12 Si6 C11 105.76(14) . . ?
C12 Si6 C13 108.11(16) . . ?
C13 Si6 C11 106.44(14) . . ?
C14 Si6 C11 119.54(15) . . ?
C14 Si6 C12 107.49(17) . . ?
C14 Si6 C13 109.04(15) . . ?
C23 Si7 C22 111.01(13) . . ?
C23 Si7 C25 109.66(15) . . ?
C24 Si7 C22 112.14(14) . . ?
C24 Si7 C23 110.94(16) . . ?
C24 Si7 C25 108.50(16) . . ?
C25 Si7 C22 104.34(14) . . ?
C29 Si8 C28 110.97(14) . . ?
C30 Si8 C28 107.79(15) . . ?
C30 Si8 C29 110.89(16) . . ?
C31 Si8 C28 108.61(13) . . ?
C31 Si8 C29 111.60(15) . . ?
C31 Si8 C30 106.80(15) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Ti1 C10 H10 120.1 . . ?
C11 C10 Ti1 72.81(15) . . ?
C11 C10 H10 124.2 . . ?
C11 C10 C17 111.5(2) . . ?
C17 C10 Ti1 74.41(16) . . ?
C17 C10 H10 124.2 . . ?
Si6 C11 Ti1 141.79(14) . . ?
C10 C11 Ti1 72.49(16) . . ?
C10 C11 Si6 122.7(2) . . ?
C10 C11 C15 104.5(2) . . ?
C15 C11 Ti1 70.81(16) . . ?
C15 C11 Si6 127.1(2) . . ?
Si6 C12 H12A 109.5 . . ?
Si6 C12 H12B 109.5 . . ?
Si6 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si6 C13 H13A 109.5 . . ?
Si6 C13 H13B 109.5 . . ?
Si6 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si6 C14 H14A 109.5 . . ?
Si6 C14 H14B 109.5 . . ?
Si6 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Ti1 C15 H15 118.9 . . ?
C11 C15 Ti1 73.87(16) . . ?
C11 C15 H15 125.4 . . ?
C16 C15 Ti1 73.61(16) . . ?
C16 C15 C11 109.2(2) . . ?
C16 C15 H15 125.4 . . ?
Ti1 C16 H16 119.9 . . ?
C15 C16 Ti1 71.64(16) . . ?
C15 C16 H16 125.3 . . ?
C15 C16 C17 109.5(2) . . ?
C17 C16 Ti1 74.93(16) . . ?
C17 C16 H16 125.3 . . ?
Si5 C17 Ti1 141.05(15) . . ?
C10 C17 Ti1 71.14(15) . . ?
C10 C17 Si5 124.3(2) . . ?
C16 C17 Ti1 70.81(15) . . ?
C16 C17 Si5 125.9(2) . . ?
C16 C17 C10 105.3(2) . . ?
Si5 C18 H18A 109.5 . . ?
Si5 C18 H18B 109.5 . . ?
Si5 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si5 C19 H19A 109.5 . . ?
Si5 C19 H19B 109.5 . . ?
Si5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si5 C20 H20A 109.5 . . ?
Si5 C20 H20B 109.5 . . ?
Si5 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Ti1 C21 H21 120.1 . . ?
C22 C21 Ti1 74.40(16) . . ?
C22 C21 H21 124.5 . . ?
C28 C21 Ti1 72.59(16) . . ?
C28 C21 H21 124.5 . . ?
C28 C21 C22 111.1(2) . . ?
Si7 C22 Ti1 138.33(15) . . ?
C21 C22 Ti1 70.99(15) . . ?
C21 C22 Si7 125.7(2) . . ?
C26 C22 Ti1 70.94(15) . . ?
C26 C22 Si7 125.7(2) . . ?
C26 C22 C21 105.4(2) . . ?
Si7 C23 H23A 109.5 . . ?
Si7 C23 H23B 109.5 . . ?
Si7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si7 C24 H24A 109.5 . . ?
Si7 C24 H24B 109.5 . . ?
Si7 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si7 C25 H25A 109.5 . . ?
Si7 C25 H25B 109.5 . . ?
Si7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Ti1 C26 H26 119.9 . . ?
C22 C26 Ti1 74.69(16) . . ?
C22 C26 H26 125.3 . . ?
C27 C26 Ti1 71.76(16) . . ?
C27 C26 C22 109.3(3) . . ?
C27 C26 H26 125.3 . . ?
Ti1 C27 H27 119.5 . . ?
C26 C27 Ti1 73.52(16) . . ?
C26 C27 H27 125.4 . . ?
C26 C27 C28 109.1(2) . . ?
C28 C27 Ti1 73.34(16) . . ?
C28 C27 H27 125.4 . . ?
Si8 C28 Ti1 129.21(14) . . ?
C21 C28 Ti1 72.68(16) . . ?
C21 C28 Si8 128.4(2) . . ?
C21 C28 C27 105.1(2) . . ?
C27 C28 Ti1 71.40(16) . . ?
C27 C28 Si8 125.5(2) . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si8 C31 H31A 109.5 . . ?
Si8 C31 H31B 109.5 . . ?
Si8 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 C10 C11 Si6 -140.9(2) . . . . ?
Ti1 C10 C11 C15 64.06(18) . . . . ?
Ti1 C10 C17 Si5 139.6(2) . . . . ?
Ti1 C10 C17 C16 -63.03(19) . . . . ?
Ti1 C11 C15 C16 65.7(2) . . . . ?
Ti1 C15 C16 C17 65.9(2) . . . . ?
Ti1 C16 C17 Si5 -139.9(2) . . . . ?
Ti1 C16 C17 C10 63.25(19) . . . . ?
Ti1 C21 C22 Si7 136.5(2) . . . . ?
Ti1 C21 C22 C26 -63.06(19) . . . . ?
Ti1 C21 C28 Si8 -126.7(2) . . . . ?
Ti1 C21 C28 C27 64.51(19) . . . . ?
Ti1 C22 C26 C27 -63.9(2) . . . . ?
Ti1 C26 C27 C28 -65.2(2) . . . . ?
Ti1 C27 C28 Si8 125.4(2) . . . . ?
Ti1 C27 C28 C21 -65.40(19) . . . . ?
Si6 C11 C15 Ti1 141.3(2) . . . . ?
Si6 C11 C15 C16 -153.1(2) . . . . ?
Si7 C22 C26 Ti1 -136.4(2) . . . . ?
Si7 C22 C26 C27 159.6(2) . . . . ?
C10 C11 C15 Ti1 -65.23(18) . . . . ?
C10 C11 C15 C16 0.5(3) . . . . ?
C11 C10 C17 Ti1 63.9(2) . . . . ?
C11 C10 C17 Si5 -156.5(2) . . . . ?
C11 C10 C17 C16 0.9(3) . . . . ?
C11 C15 C16 Ti1 -65.85(19) . . . . ?
C11 C15 C16 C17 0.1(3) . . . . ?
C12 Si6 C11 Ti1 140.3(2) . . . . ?
C12 Si6 C11 C10 -115.9(3) . . . . ?
C12 Si6 C11 C15 33.2(3) . . . . ?
C13 Si6 C11 Ti1 -104.8(2) . . . . ?
C13 Si6 C11 C10 -1.1(3) . . . . ?
C13 Si6 C11 C15 148.0(3) . . . . ?
C14 Si6 C11 Ti1 19.1(3) . . . . ?
C14 Si6 C11 C10 122.8(2) . . . . ?
C14 Si6 C11 C15 -88.1(3) . . . . ?
C15 C16 C17 Ti1 -63.8(2) . . . . ?
C15 C16 C17 Si5 156.3(2) . . . . ?
C15 C16 C17 C10 -0.6(3) . . . . ?
C17 C10 C11 Ti1 -64.9(2) . . . . ?
C17 C10 C11 Si6 154.2(2) . . . . ?
C17 C10 C11 C15 -0.8(3) . . . . ?
C18 Si5 C17 Ti1 -66.5(3) . . . . ?
C18 Si5 C17 C10 -169.3(2) . . . . ?
C18 Si5 C17 C16 38.0(3) . . . . ?
C19 Si5 C17 Ti1 177.4(2) . . . . ?
C19 Si5 C17 C10 74.6(3) . . . . ?
C19 Si5 C17 C16 -78.1(3) . . . . ?
C20 Si5 C17 Ti1 60.2(3) . . . . ?
C20 Si5 C17 C10 -42.6(3) . . . . ?
C20 Si5 C17 C16 164.7(3) . . . . ?
C21 C22 C26 Ti1 63.09(19) . . . . ?
C21 C22 C26 C27 -0.8(3) . . . . ?
C22 C21 C28 Ti1 -65.0(2) . . . . ?
C22 C21 C28 Si8 168.3(2) . . . . ?
C22 C21 C28 C27 -0.5(3) . . . . ?
C22 C26 C27 Ti1 65.8(2) . . . . ?
C22 C26 C27 C28 0.6(3) . . . . ?
C23 Si7 C22 Ti1 74.6(2) . . . . ?
C23 Si7 C22 C21 -27.2(3) . . . . ?
C23 Si7 C22 C26 176.2(3) . . . . ?
C24 Si7 C22 Ti1 -50.2(3) . . . . ?
C24 Si7 C22 C21 -151.9(3) . . . . ?
C24 Si7 C22 C26 51.5(3) . . . . ?
C25 Si7 C22 Ti1 -167.4(2) . . . . ?
C25 Si7 C22 C21 90.8(3) . . . . ?
C25 Si7 C22 C26 -65.8(3) . . . . ?
C26 C27 C28 Ti1 65.4(2) . . . . ?
C26 C27 C28 Si8 -169.3(2) . . . . ?
C26 C27 C28 C21 0.0(3) . . . . ?
C28 C21 C22 Ti1 63.9(2) . . . . ?
C28 C21 C22 Si7 -159.6(2) . . . . ?
C28 C21 C22 C26 0.8(3) . . . . ?
C29 Si8 C28 Ti1 19.3(2) . . . . ?
C29 Si8 C28 C21 118.3(3) . . . . ?
C29 Si8 C28 C27 -75.0(3) . . . . ?
C30 Si8 C28 Ti1 140.95(18) . . . . ?
C30 Si8 C28 C21 -120.1(3) . . . . ?
C30 Si8 C28 C27 46.6(3) . . . . ?
C31 Si8 C28 Ti1 -103.68(19) . . . . ?
C31 Si8 C28 C21 -4.7(3) . . . . ?
C31 Si8 C28 C27 162.0(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.789
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.90(2)
2 0.10(2)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-La
_database_code_depnum_ccdc_archive 'CCDC 2195637'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   adpm650
_manchester_internal_coll_client AW
_manchester_internal_coll_user   AW
_manchester_internal_coll_date   08/09/2020
_manchester_internal_process_date 08/09/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 10/09/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 10/09/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 25/09/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 25/09/2020
_manchester_internal_archive_user AW
_refine_special_details          
'The Si(SiMe3)3 group is disordered over two orientations. The occupanices were allowed to freely refine converging at 0.53:0.47. Selected chemically equivalent Si-C and C-C distances were restrained to be approximately equal.Enhanced rigid bond and similarity thermla restraints were applied to disordered groups.'
_vrf_PLAT201_3-La                
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report
RESPONSE: Selected atoms in disordered components were refined
isotropically.
;
_audit_creation_date             2020-09-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[La(C5H3(1,3-SiMe))2{Si(SiMe3)3}]'
_chemical_formula_moiety         'C31 H69 La Si8'
_chemical_formula_sum            'C31 H69 La Si8'
_chemical_formula_weight         805.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         C31H69LaSi8
_chemical_oxdiff_usercomment     BR4.309
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'
La La -0.2871 2.4523 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.9162(10)
_cell_length_b                   13.3218(7)
_cell_length_c                   20.3331(16)
_cell_angle_alpha                90
_cell_angle_beta                 111.465(8)
_cell_angle_gamma                90
_cell_volume                     4516.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5693
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.1530
_cell_measurement_theta_min      2.4190
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.703
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-24 2 1 0.0371
-13 2 28 0.1437
13 -2 -28 0.1437
-3 -18 -3 0.0010
3 18 3 0.0271
24 -2 -1 0.0371

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 'Crystallised from pentane at -25oC'
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.028
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-24.0003 2.0000 1.0013 0.1827 0.6953 -0.7145
-13.0009 2.0002 27.9995 0.3001 0.7840 0.5378
13.0009 -2.0002 -27.9995 -0.3001 -0.7840 -0.5378
-2.9998 -17.9997 -2.9998 -0.9462 0.2199 -0.1181
2.9998 17.9997 2.9998 0.9462 -0.2199 0.1181
24.0003 -2.0000 -1.0013 -0.1827 -0.6953 0.7145

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8258
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.869
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  26.00   1.00   15.00    --   19.02  77.00 -30.00   35
  2  ω     -4.00  34.00   1.00   15.00    --   19.02  77.00 120.00   38
  3  ω     41.00  90.00   1.00   15.00    --   19.02  37.00 -90.00   49
  4  ω    -50.00  29.00   1.00   15.00    --   19.02 -57.00 -30.00   79
  5  ω      7.00  46.00   1.00   15.00    --   19.02  37.00-180.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0030328000
_diffrn_orient_matrix_UB_12      0.0521398000
_diffrn_orient_matrix_UB_13      0.0055843000
_diffrn_orient_matrix_UB_21      -0.0291596000
_diffrn_orient_matrix_UB_22      -0.0098850000
_diffrn_orient_matrix_UB_23      0.0151688000
_diffrn_orient_matrix_UB_31      0.0308304000
_diffrn_orient_matrix_UB_32      -0.0042129000
_diffrn_orient_matrix_UB_33      0.0338230000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6553
_reflns_number_total             8258
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.796
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8258
_refine_ls_number_restraints     948
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0604
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+11.1771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1479
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.823(2)
 0.177(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Si4A-C7A \\sim Si4A-C9A \\sim Si4A-C8A \\sim Si3-C5 \\sim Si3-C6 \\sim Si3-C4
\\sim Si3A-C5A \\sim Si3A-
 C6A \\sim Si3A-C4A \\sim Si2-C1 \\sim Si2-C3 \\sim Si2-C2 \\sim Si2A-C3A \\sim
Si2A-C2A \\sim Si4-C9 \\sim Si4-
 C7 \\sim Si4-C8
 with sigma of 0.02
 C2A-C1A \\sim C3A-C2A \\sim C3A-C1A \\sim C9-C8 \\sim C9-C7 \\sim C8-C7 \\sim
C9A-C8A \\sim C9A-C7A \\sim C8A-
 C7A \\sim C6-C5 \\sim C5-C4 \\sim C6-C4 \\sim C6A-C5A \\sim C5A-C4A \\sim
C6A-C4A \\sim C3-C1 \\sim C2-C1 \\sim C3-
 C2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Si2 \\sim Si2A \\sim Si4A \\sim C1 \\sim C2 \\sim C3 \\sim C1A \\sim C2A \\sim
C3A \\sim C7A \\sim C8A \\sim C9A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Si1 \\sim Si2 \\sim Si3 \\sim Si4 \\sim Si2A \\sim Si3A \\sim Si4A \\sim C1
\\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Si2A)=Sof(Si3A)=Sof(Si4A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(Si2)=Sof(Si3)=Sof(Si4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C20(H20), C21(H21), C26(H26), C27(H27)
7.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,
 H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC),
  C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,
 H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.44320(2) 0.62122(3) 0.73449(2) 0.02442(12) Uani 1 1 d . U . . .
Si1 Si 0.57632(9) 0.45049(13) 0.77719(9) 0.0228(4) Uani 1 1 d . U . . .
Si5 Si 0.47221(13) 0.86044(16) 0.88450(12) 0.0396(5) Uani 1 1 d . U . . .
Si6 Si 0.46923(14) 0.85503(18) 0.60078(12) 0.0476(6) Uani 1 1 d . U . . .
Si7 Si 0.32188(11) 0.4957(2) 0.55041(11) 0.0472(6) Uani 1 1 d . U . . .
Si8 Si 0.32197(10) 0.51083(15) 0.83929(11) 0.0333(5) Uani 1 1 d . U . . .
Si2 Si 0.63706(19) 0.4221(3) 0.90023(18) 0.0274(8) Uani 0.527(3) 1 d D U P A 1
Si3 Si 0.68695(19) 0.4977(3) 0.75098(17) 0.0258(8) Uani 0.527(3) 1 d D U P A 1
Si4 Si 0.5502(2) 0.2845(3) 0.7336(2) 0.0363(10) Uani 0.527(3) 1 d D U P A 1
Si2A Si 0.5583(2) 0.2890(3) 0.8114(2) 0.0344(10) Uani 0.473(3) 1 d D U P A 2
Si3A Si 0.6876(2) 0.5095(3) 0.87393(19) 0.0253(9) Uani 0.473(3) 1 d D U P A 2
Si4A Si 0.6411(2) 0.4253(3) 0.6950(2) 0.0277(10) Uani 0.473(3) 1 d D U P A 2
C10 C 0.3672(4) 0.8439(7) 0.8793(5) 0.058(2) Uani 1 1 d . U . . .
H10A H 0.330215 0.867247 0.833145 0.086 Uiso 1 1 calc GR . . . .
H10B H 0.358793 0.883062 0.916778 0.086 Uiso 1 1 calc GR . . . .
H10C H 0.357235 0.772763 0.885120 0.086 Uiso 1 1 calc GR . . . .
C11 C 0.5440(4) 0.8030(6) 0.9673(4) 0.0459(19) Uani 1 1 d . U . . .
H11A H 0.532194 0.731292 0.968120 0.069 Uiso 1 1 calc GR . . . .
H11B H 0.538544 0.836044 1.008342 0.069 Uiso 1 1 calc GR . . . .
H11C H 0.598932 0.811544 0.968781 0.069 Uiso 1 1 calc GR . . . .
C12 C 0.4943(7) 0.9976(6) 0.8839(5) 0.080(3) Uani 1 1 d . U . . .
H12A H 0.545337 1.006813 0.877300 0.119 Uiso 1 1 calc GR . . . .
H12B H 0.497746 1.027582 0.928936 0.119 Uiso 1 1 calc GR . . . .
H12C H 0.451231 1.030268 0.845115 0.119 Uiso 1 1 calc GR . . . .
C13 C 0.4880(4) 0.8051(5) 0.8061(3) 0.0270(13) Uani 1 1 d . U . . .
C14 C 0.5610(4) 0.7629(5) 0.8059(4) 0.0286(14) Uani 1 1 d . U . . .
H14 H 0.603598 0.739352 0.846573 0.034 Uiso 1 1 calc R . . . .
C15 C 0.5605(4) 0.7613(5) 0.7372(4) 0.0288(14) Uani 1 1 d . U . . .
H15 H 0.602264 0.735830 0.723668 0.035 Uiso 1 1 calc R . . . .
C16 C 0.4871(4) 0.8040(5) 0.6904(4) 0.0304(14) Uani 1 1 d . U . . .
C17 C 0.5363(5) 0.7925(7) 0.5611(4) 0.054(2) Uani 1 1 d . U . . .
H17A H 0.591869 0.795223 0.594570 0.080 Uiso 1 1 calc GR . . . .
H17B H 0.532157 0.827293 0.517390 0.080 Uiso 1 1 calc GR . . . .
H17C H 0.519988 0.722333 0.550427 0.080 Uiso 1 1 calc GR . . . .
C18 C 0.4945(7) 0.9920(7) 0.6117(6) 0.087(3) Uani 1 1 d . U . . .
H18A H 0.462382 1.024785 0.635551 0.131 Uiso 1 1 calc GR . . . .
H18B H 0.482700 1.022591 0.565193 0.131 Uiso 1 1 calc GR . . . .
H18C H 0.551599 1.000156 0.640195 0.131 Uiso 1 1 calc GR . . . .
C19 C 0.3625(5) 0.8401(8) 0.5432(4) 0.073(3) Uani 1 1 d . U . . .
H19A H 0.350928 0.768954 0.531856 0.110 Uiso 1 1 calc GR . . . .
H19B H 0.351743 0.878239 0.499447 0.110 Uiso 1 1 calc GR . . . .
H19C H 0.328384 0.865327 0.567784 0.110 Uiso 1 1 calc GR . . . .
C20 C 0.4447(4) 0.8307(5) 0.7342(4) 0.0301(14) Uani 1 1 d . U . . .
H20 H 0.393468 0.862024 0.717778 0.036 Uiso 1 1 calc R . . . .
C21 C 0.3214(4) 0.4809(5) 0.6952(4) 0.0342(15) Uani 1 1 d . U . . .
H21 H 0.339816 0.413389 0.702252 0.041 Uiso 1 1 calc R . . . .
C22 C 0.3062(4) 0.5365(6) 0.6321(4) 0.0345(15) Uani 1 1 d . U . . .
C23 C 0.3152(6) 0.3580(8) 0.5394(6) 0.090(4) Uani 1 1 d . U . . .
H23A H 0.353826 0.325971 0.581531 0.135 Uiso 1 1 calc GR . . . .
H23B H 0.327360 0.339207 0.497842 0.135 Uiso 1 1 calc GR . . . .
H23C H 0.260852 0.335799 0.533101 0.135 Uiso 1 1 calc GR . . . .
C24 C 0.4242(4) 0.5387(6) 0.5610(4) 0.049(2) Uani 1 1 d . U . . .
H24A H 0.428031 0.611491 0.568611 0.073 Uiso 1 1 calc GR . . . .
H24B H 0.434881 0.522422 0.518306 0.073 Uiso 1 1 calc GR . . . .
H24C H 0.463689 0.504986 0.601798 0.073 Uiso 1 1 calc GR . . . .
C25 C 0.2455(5) 0.5585(10) 0.4732(5) 0.100(4) Uani 1 1 d . U . . .
H25A H 0.191700 0.540697 0.471222 0.150 Uiso 1 1 calc GR . . . .
H25B H 0.252119 0.536457 0.429612 0.150 Uiso 1 1 calc GR . . . .
H25C H 0.252599 0.631435 0.477955 0.150 Uiso 1 1 calc GR . . . .
C26 C 0.2821(4) 0.6339(6) 0.6449(4) 0.0365(15) Uani 1 1 d . U . . .
H26 H 0.268917 0.688309 0.612519 0.044 Uiso 1 1 calc R . . . .
C27 C 0.2811(3) 0.6361(6) 0.7136(4) 0.0338(15) Uani 1 1 d . U . . .
H27 H 0.266675 0.692368 0.735042 0.041 Uiso 1 1 calc R . . . .
C28 C 0.3052(4) 0.5405(6) 0.7461(4) 0.0327(15) Uani 1 1 d . U . . .
C29 C 0.2455(4) 0.5770(6) 0.8655(4) 0.050(2) Uani 1 1 d . U . . .
H29A H 0.245702 0.648612 0.854636 0.075 Uiso 1 1 calc GR . . . .
H29B H 0.258323 0.568290 0.916309 0.075 Uiso 1 1 calc GR . . . .
H29C H 0.192389 0.548760 0.839304 0.075 Uiso 1 1 calc GR . . . .
C30 C 0.3172(4) 0.3735(5) 0.8517(4) 0.0460(19) Uani 1 1 d . U . . .
H30A H 0.261581 0.350639 0.829324 0.069 Uiso 1 1 calc GR . . . .
H30B H 0.336687 0.358070 0.902303 0.069 Uiso 1 1 calc GR . . . .
H30C H 0.350764 0.339134 0.829982 0.069 Uiso 1 1 calc GR . . . .
C31 C 0.4258(4) 0.5555(5) 0.8903(4) 0.0358(16) Uani 1 1 d . U . . .
H31A H 0.463890 0.519600 0.874419 0.054 Uiso 1 1 calc GR . . . .
H31B H 0.438813 0.542802 0.940769 0.054 Uiso 1 1 calc GR . . . .
H31C H 0.429323 0.627721 0.882587 0.054 Uiso 1 1 calc GR . . . .
C1 C 0.7406(7) 0.3672(12) 0.9307(9) 0.040(4) Uani 0.527(3) 1 d D U P A 1
H1A H 0.742165 0.312872 0.898687 0.060 Uiso 0.527(3) 1 calc GR . P A 1
H1B H 0.754787 0.340618 0.978632 0.060 Uiso 0.527(3) 1 calc GR . P A 1
H1C H 0.779072 0.419500 0.930542 0.060 Uiso 0.527(3) 1 calc GR . P A 1
C2 C 0.5743(7) 0.3406(10) 0.9355(8) 0.044(4) Uiso 0.527(3) 1 d D U P A 1
H2A H 0.534979 0.382292 0.946025 0.067 Uiso 0.527(3) 1 calc GR . P A 1
H2B H 0.608982 0.306994 0.978735 0.067 Uiso 0.527(3) 1 calc GR . P A 1
H2C H 0.546156 0.290090 0.900016 0.067 Uiso 0.527(3) 1 calc GR . P A 1
C3 C 0.6485(14) 0.5445(10) 0.9511(12) 0.029(4) Uani 0.527(3) 1 d D U P A 1
H3A H 0.678155 0.592904 0.933772 0.044 Uiso 0.527(3) 1 calc GR . P A 1
H3B H 0.677873 0.532000 1.001522 0.044 Uiso 0.527(3) 1 calc GR . P A 1
H3C H 0.595311 0.571588 0.944270 0.044 Uiso 0.527(3) 1 calc GR . P A 1
C4 C 0.7473(7) 0.5965(8) 0.8144(6) 0.027(3) Uani 0.527(3) 1 d D U P A 1
H4A H 0.711453 0.650007 0.818098 0.041 Uiso 0.527(3) 1 calc GR . P A 1
H4B H 0.787184 0.624686 0.797097 0.041 Uiso 0.527(3) 1 calc GR . P A 1
H4C H 0.774537 0.566280 0.861010 0.041 Uiso 0.527(3) 1 calc GR . P A 1
C5 C 0.6560(17) 0.5527(13) 0.6596(7) 0.036(6) Uani 0.527(3) 1 d D U P A 1
H5A H 0.634983 0.499356 0.624469 0.054 Uiso 0.527(3) 1 calc GR . P A 1
H5B H 0.702488 0.584029 0.653501 0.054 Uiso 0.527(3) 1 calc GR . P A 1
H5C H 0.614236 0.603387 0.653270 0.054 Uiso 0.527(3) 1 calc GR . P A 1
C6 C 0.7600(10) 0.3946(13) 0.7527(10) 0.031(4) Uani 0.527(3) 1 d D U P A 1
H6A H 0.788245 0.372706 0.801597 0.046 Uiso 0.527(3) 1 calc GR . P A 1
H6B H 0.798859 0.419847 0.733151 0.046 Uiso 0.527(3) 1 calc GR . P A 1
H6C H 0.730679 0.337732 0.724373 0.046 Uiso 0.527(3) 1 calc GR . P A 1
C7 C 0.5465(9) 0.2790(12) 0.6396(5) 0.060(4) Uani 0.527(3) 1 d D U P A 1
H7A H 0.502136 0.320719 0.609357 0.089 Uiso 0.527(3) 1 calc GR . P A 1
H7B H 0.538191 0.209425 0.622841 0.089 Uiso 0.527(3) 1 calc GR . P A 1
H7C H 0.597148 0.304021 0.637841 0.089 Uiso 0.527(3) 1 calc GR . P A 1
C8 C 0.6277(10) 0.1895(14) 0.7842(8) 0.051(5) Uani 0.527(3) 1 d D U P A 1
H8A H 0.681079 0.212924 0.788344 0.077 Uiso 0.527(3) 1 calc GR . P A 1
H8B H 0.616384 0.125089 0.759204 0.077 Uiso 0.527(3) 1 calc GR . P A 1
H8C H 0.626019 0.180915 0.831552 0.077 Uiso 0.527(3) 1 calc GR . P A 1
C9 C 0.4517(8) 0.2344(19) 0.7318(10) 0.054(6) Uani 0.527(3) 1 d D U P A 1
H9A H 0.455344 0.219953 0.780121 0.081 Uiso 0.527(3) 1 calc GR . P A 1
H9B H 0.438645 0.172585 0.703716 0.081 Uiso 0.527(3) 1 calc GR . P A 1
H9C H 0.409632 0.284397 0.710548 0.081 Uiso 0.527(3) 1 calc GR . P A 1
C1A C 0.6411(10) 0.1950(18) 0.8169(9) 0.045(5) Uani 0.473(3) 1 d D U P A 2
H1AA H 0.646852 0.190621 0.770891 0.068 Uiso 0.473(3) 1 calc GR . P A 2
H1AB H 0.626931 0.128846 0.829963 0.068 Uiso 0.473(3) 1 calc GR . P A 2
H1AC H 0.691813 0.217328 0.852687 0.068 Uiso 0.473(3) 1 calc GR . P A 2
C2A C 0.4635(8) 0.229(2) 0.7520(9) 0.035(5) Uani 0.473(3) 1 d D U P A 2
H2AA H 0.418021 0.256943 0.761852 0.053 Uiso 0.473(3) 1 calc GR . P A 2
H2AB H 0.466303 0.156436 0.760367 0.053 Uiso 0.473(3) 1 calc GR . P A 2
H2AC H 0.456254 0.242201 0.702637 0.053 Uiso 0.473(3) 1 calc GR . P A 2
C3A C 0.5557(9) 0.2899(12) 0.9036(6) 0.043(3) Uani 0.473(3) 1 d D U P A 2
H3AA H 0.606684 0.315784 0.936971 0.064 Uiso 0.473(3) 1 calc GR . P A 2
H3AB H 0.547319 0.221397 0.917075 0.064 Uiso 0.473(3) 1 calc GR . P A 2
H3AC H 0.511716 0.332942 0.904479 0.064 Uiso 0.473(3) 1 calc GR . P A 2
C4A C 0.6486(14) 0.5606(14) 0.9413(12) 0.034(6) Uani 0.473(3) 1 d D U P A 2
H4AA H 0.609979 0.614315 0.919943 0.051 Uiso 0.473(3) 1 calc GR . P A 2
H4AB H 0.693360 0.587352 0.981578 0.051 Uiso 0.473(3) 1 calc GR . P A 2
H4AC H 0.622226 0.506723 0.957427 0.051 Uiso 0.473(3) 1 calc GR . P A 2
C5A C 0.7445(8) 0.6126(10) 0.8505(7) 0.033(3) Uani 0.473(3) 1 d D U P A 2
H5AA H 0.778435 0.583972 0.826835 0.049 Uiso 0.473(3) 1 calc GR . P A 2
H5AB H 0.778150 0.647360 0.893600 0.049 Uiso 0.473(3) 1 calc GR . P A 2
H5AC H 0.706617 0.660277 0.818745 0.049 Uiso 0.473(3) 1 calc GR . P A 2
C6A C 0.7634(8) 0.4102(10) 0.9211(10) 0.037(4) Uani 0.473(3) 1 d D U P A 2
H6AA H 0.739619 0.363963 0.945439 0.056 Uiso 0.473(3) 1 calc GR . P A 2
H6AB H 0.810783 0.442183 0.955621 0.056 Uiso 0.473(3) 1 calc GR . P A 2
H6AC H 0.778999 0.372893 0.886599 0.056 Uiso 0.473(3) 1 calc GR . P A 2
C7A C 0.6463(17) 0.5467(12) 0.6491(10) 0.030(5) Uani 0.473(3) 1 d D U P A 2
H7AA H 0.591901 0.568499 0.620133 0.045 Uiso 0.473(3) 1 calc GR . P A 2
H7AB H 0.677469 0.536449 0.618910 0.045 Uiso 0.473(3) 1 calc GR . P A 2
H7AC H 0.672143 0.598260 0.684539 0.045 Uiso 0.473(3) 1 calc GR . P A 2
C8A C 0.7461(8) 0.3756(16) 0.7315(12) 0.037(5) Uani 0.473(3) 1 d D U P A 2
H8AA H 0.780936 0.424257 0.764895 0.055 Uiso 0.473(3) 1 calc GR . P A 2
H8AB H 0.765415 0.364693 0.692736 0.055 Uiso 0.473(3) 1 calc GR . P A 2
H8AC H 0.746966 0.311942 0.755862 0.055 Uiso 0.473(3) 1 calc GR . P A 2
C9A C 0.5808(8) 0.3376(11) 0.6222(7) 0.047(4) Uiso 0.473(3) 1 d D U P A 2
H9AA H 0.564371 0.279002 0.642767 0.071 Uiso 0.473(3) 1 calc GR . P A 2
H9AB H 0.613653 0.315534 0.595502 0.071 Uiso 0.473(3) 1 calc GR . P A 2
H9AC H 0.533097 0.372507 0.590447 0.071 Uiso 0.473(3) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 Si1 3.1779(16) . ?
La1 C13 2.812(6) . ?
La1 C14 2.807(6) . ?
La1 C15 2.795(6) . ?
La1 C16 2.805(7) . ?
La1 C20 2.791(6) . ?
La1 C21 2.760(6) . ?
La1 C22 2.809(6) . ?
La1 C26 2.798(6) . ?
La1 C27 2.784(6) . ?
La1 C28 2.785(6) . ?
Si1 Si2 2.365(4) . ?
Si1 Si3 2.320(4) . ?
Si1 Si4 2.364(4) . ?
Si1 Si2A 2.319(5) . ?
Si1 Si3A 2.365(4) . ?
Si1 Si4A 2.381(4) . ?
Si5 C10 1.858(7) . ?
Si5 C11 1.868(8) . ?
Si5 C12 1.870(9) . ?
Si5 C13 1.870(7) . ?
Si6 C16 1.859(7) . ?
Si6 C17 1.871(8) . ?
Si6 C18 1.873(10) . ?
Si6 C19 1.851(9) . ?
Si7 C22 1.863(7) . ?
Si7 C23 1.846(10) . ?
Si7 C24 1.856(7) . ?
Si7 C25 1.862(9) . ?
Si8 C28 1.849(7) . ?
Si8 C29 1.862(7) . ?
Si8 C30 1.853(7) . ?
Si8 C31 1.866(6) . ?
Si2 C1 1.876(10) . ?
Si2 C2 1.884(10) . ?
Si2 C3 1.901(11) . ?
Si3 C4 1.882(9) . ?
Si3 C5 1.882(11) . ?
Si3 C6 1.888(10) . ?
Si4 C7 1.890(10) . ?
Si4 C8 1.883(10) . ?
Si4 C9 1.875(11) . ?
Si2A C1A 1.913(17) . ?
Si2A C2A 1.866(11) . ?
Si2A C3A 1.893(10) . ?
Si3A C4A 1.878(11) . ?
Si3A C5A 1.872(10) . ?
Si3A C6A 1.886(10) . ?
Si4A C7A 1.886(11) . ?
Si4A C8A 1.873(11) . ?
Si4A C9A 1.885(10) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.423(8) . ?
C13 C20 1.422(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.394(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.429(9) . ?
C16 C20 1.413(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.419(10) . ?
C21 C28 1.417(9) . ?
C22 C26 1.422(10) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.402(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.427(10) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 La1 Si1 116.00(13) . . ?
C14 La1 Si1 89.60(14) . . ?
C14 La1 C13 29.34(17) . . ?
C14 La1 C22 160.2(2) . . ?
C15 La1 Si1 89.36(14) . . ?
C15 La1 C13 48.54(18) . . ?
C15 La1 C14 28.82(19) . . ?
C15 La1 C16 29.57(19) . . ?
C15 La1 C22 136.8(2) . . ?
C15 La1 C26 124.2(2) . . ?
C16 La1 Si1 116.00(14) . . ?
C16 La1 C13 49.38(19) . . ?
C16 La1 C14 48.4(2) . . ?
C16 La1 C22 112.5(2) . . ?
C20 La1 Si1 135.20(13) . . ?
C20 La1 C13 29.40(19) . . ?
C20 La1 C14 47.38(19) . . ?
C20 La1 C15 47.55(18) . . ?
C20 La1 C16 29.26(18) . . ?
C20 La1 C22 114.0(2) . . ?
C20 La1 C26 86.9(2) . . ?
C21 La1 Si1 91.66(15) . . ?
C21 La1 C13 141.80(19) . . ?
C21 La1 C14 165.9(2) . . ?
C21 La1 C15 165.2(2) . . ?
C21 La1 C16 141.2(2) . . ?
C21 La1 C20 133.1(2) . . ?
C21 La1 C22 29.5(2) . . ?
C21 La1 C26 48.3(2) . . ?
C21 La1 C27 48.2(2) . . ?
C21 La1 C28 29.6(2) . . ?
C22 La1 Si1 106.23(15) . . ?
C22 La1 C13 137.8(2) . . ?
C26 La1 Si1 135.50(16) . . ?
C26 La1 C13 108.4(2) . . ?
C26 La1 C14 134.2(2) . . ?
C26 La1 C16 94.7(2) . . ?
C26 La1 C22 29.4(2) . . ?
C27 La1 Si1 136.82(16) . . ?
C27 La1 C13 95.8(2) . . ?
C27 La1 C14 125.2(2) . . ?
C27 La1 C15 133.6(2) . . ?
C27 La1 C16 106.8(2) . . ?
C27 La1 C20 86.5(2) . . ?
C27 La1 C22 48.4(2) . . ?
C27 La1 C26 29.10(19) . . ?
C27 La1 C28 29.7(2) . . ?
C28 La1 Si1 107.54(15) . . ?
C28 La1 C13 112.76(19) . . ?
C28 La1 C14 137.59(19) . . ?
C28 La1 C15 160.1(2) . . ?
C28 La1 C16 136.4(2) . . ?
C28 La1 C20 113.3(2) . . ?
C28 La1 C22 49.1(2) . . ?
C28 La1 C26 48.8(2) . . ?
Si2 Si1 La1 114.35(10) . . ?
Si3 Si1 La1 111.22(10) . . ?
Si3 Si1 Si2 100.68(13) . . ?
Si3 Si1 Si4 103.65(14) . . ?
Si4 Si1 La1 122.77(10) . . ?
Si4 Si1 Si2 101.43(15) . . ?
Si2A Si1 La1 124.96(11) . . ?
Si2A Si1 Si3A 103.09(15) . . ?
Si2A Si1 Si4A 103.68(16) . . ?
Si3A Si1 La1 108.02(11) . . ?
Si3A Si1 Si4A 98.72(14) . . ?
Si4A Si1 La1 114.76(11) . . ?
C10 Si5 C11 110.6(4) . . ?
C10 Si5 C12 109.1(5) . . ?
C10 Si5 C13 111.8(3) . . ?
C11 Si5 C12 109.2(4) . . ?
C11 Si5 C13 109.7(3) . . ?
C13 Si5 C12 106.3(4) . . ?
C16 Si6 C17 110.6(3) . . ?
C16 Si6 C18 107.0(4) . . ?
C17 Si6 C18 108.6(5) . . ?
C19 Si6 C16 110.4(4) . . ?
C19 Si6 C17 110.9(4) . . ?
C19 Si6 C18 109.2(5) . . ?
C23 Si7 C22 111.9(5) . . ?
C23 Si7 C24 109.8(4) . . ?
C23 Si7 C25 110.5(6) . . ?
C24 Si7 C22 105.7(3) . . ?
C24 Si7 C25 110.4(5) . . ?
C25 Si7 C22 108.5(4) . . ?
C28 Si8 C29 109.3(3) . . ?
C28 Si8 C30 110.6(4) . . ?
C28 Si8 C31 104.9(3) . . ?
C29 Si8 C31 112.2(4) . . ?
C30 Si8 C29 110.7(4) . . ?
C30 Si8 C31 109.0(3) . . ?
C1 Si2 Si1 115.3(6) . . ?
C1 Si2 C2 107.8(6) . . ?
C1 Si2 C3 105.0(7) . . ?
C2 Si2 Si1 112.8(5) . . ?
C2 Si2 C3 104.3(6) . . ?
C3 Si2 Si1 110.8(8) . . ?
C4 Si3 Si1 110.9(4) . . ?
C4 Si3 C6 106.0(6) . . ?
C5 Si3 Si1 111.3(9) . . ?
C5 Si3 C4 107.0(6) . . ?
C5 Si3 C6 104.7(7) . . ?
C6 Si3 Si1 116.3(8) . . ?
C7 Si4 Si1 110.1(5) . . ?
C8 Si4 Si1 114.8(7) . . ?
C8 Si4 C7 105.9(6) . . ?
C9 Si4 Si1 113.3(8) . . ?
C9 Si4 C7 106.3(6) . . ?
C9 Si4 C8 105.8(7) . . ?
C1A Si2A Si1 115.8(8) . . ?
C2A Si2A Si1 113.4(8) . . ?
C2A Si2A C1A 105.1(8) . . ?
C2A Si2A C3A 107.2(7) . . ?
C3A Si2A Si1 110.4(5) . . ?
C3A Si2A C1A 104.2(7) . . ?
C4A Si3A Si1 107.5(8) . . ?
C4A Si3A C6A 105.9(7) . . ?
C5A Si3A Si1 113.8(5) . . ?
C5A Si3A C4A 107.6(7) . . ?
C5A Si3A C6A 106.6(6) . . ?
C6A Si3A Si1 114.9(6) . . ?
C7A Si4A Si1 110.6(9) . . ?
C8A Si4A Si1 116.7(9) . . ?
C8A Si4A C7A 105.9(8) . . ?
C8A Si4A C9A 107.2(7) . . ?
C9A Si4A Si1 110.7(5) . . ?
C9A Si4A C7A 105.1(7) . . ?
Si5 C10 H10A 109.5 . . ?
Si5 C10 H10B 109.5 . . ?
Si5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si5 C11 H11A 109.5 . . ?
Si5 C11 H11B 109.5 . . ?
Si5 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si5 C12 H12A 109.5 . . ?
Si5 C12 H12B 109.5 . . ?
Si5 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si5 C13 La1 132.9(3) . . ?
C14 C13 La1 75.1(4) . . ?
C14 C13 Si5 125.7(5) . . ?
C20 C13 La1 74.5(4) . . ?
C20 C13 Si5 125.8(5) . . ?
C20 C13 C14 104.5(5) . . ?
La1 C14 H14 116.2 . . ?
C13 C14 La1 75.5(4) . . ?
C13 C14 H14 125.1 . . ?
C15 C14 La1 75.1(4) . . ?
C15 C14 C13 109.8(6) . . ?
C15 C14 H14 125.1 . . ?
La1 C15 H15 115.0 . . ?
C14 C15 La1 76.1(4) . . ?
C14 C15 H15 125.4 . . ?
C14 C15 C16 109.2(6) . . ?
C16 C15 La1 75.6(4) . . ?
C16 C15 H15 125.4 . . ?
Si6 C16 La1 131.5(3) . . ?
C15 C16 La1 74.8(4) . . ?
C15 C16 Si6 125.8(5) . . ?
C20 C16 La1 74.9(4) . . ?
C20 C16 Si6 125.9(5) . . ?
C20 C16 C15 104.8(6) . . ?
Si6 C17 H17A 109.5 . . ?
Si6 C17 H17B 109.5 . . ?
Si6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si6 C18 H18A 109.5 . . ?
Si6 C18 H18B 109.5 . . ?
Si6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si6 C19 H19A 109.5 . . ?
Si6 C19 H19B 109.5 . . ?
Si6 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
La1 C20 H20 115.5 . . ?
C13 C20 La1 76.1(4) . . ?
C13 C20 H20 124.2 . . ?
C16 C20 La1 75.9(4) . . ?
C16 C20 C13 111.7(5) . . ?
C16 C20 H20 124.2 . . ?
La1 C21 H21 113.8 . . ?
C22 C21 La1 77.2(4) . . ?
C22 C21 H21 124.9 . . ?
C28 C21 La1 76.1(4) . . ?
C28 C21 H21 124.9 . . ?
C28 C21 C22 110.2(6) . . ?
Si7 C22 La1 113.7(3) . . ?
C21 C22 La1 73.3(4) . . ?
C21 C22 Si7 127.7(6) . . ?
C21 C22 C26 106.3(6) . . ?
C26 C22 La1 74.8(4) . . ?
C26 C22 Si7 125.8(6) . . ?
Si7 C23 H23A 109.5 . . ?
Si7 C23 H23B 109.5 . . ?
Si7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si7 C24 H24A 109.5 . . ?
Si7 C24 H24B 109.5 . . ?
Si7 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si7 C25 H25A 109.5 . . ?
Si7 C25 H25B 109.5 . . ?
Si7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
La1 C26 H26 115.7 . . ?
C22 C26 La1 75.8(4) . . ?
C22 C26 H26 125.7 . . ?
C27 C26 La1 74.9(4) . . ?
C27 C26 C22 108.5(7) . . ?
C27 C26 H26 125.7 . . ?
La1 C27 H27 115.5 . . ?
C26 C27 La1 76.0(4) . . ?
C26 C27 H27 125.3 . . ?
C26 C27 C28 109.3(7) . . ?
C28 C27 La1 75.2(3) . . ?
C28 C27 H27 125.3 . . ?
Si8 C28 La1 110.7(3) . . ?
C21 C28 La1 74.2(4) . . ?
C21 C28 Si8 129.0(6) . . ?
C21 C28 C27 105.6(6) . . ?
C27 C28 La1 75.1(4) . . ?
C27 C28 Si8 125.0(5) . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si8 C31 H31A 109.5 . . ?
Si8 C31 H31B 109.5 . . ?
Si8 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2A C1A H1AA 109.5 . . ?
Si2A C1A H1AB 109.5 . . ?
Si2A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
Si2A C2A H2AA 109.5 . . ?
Si2A C2A H2AB 109.5 . . ?
Si2A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
Si2A C3A H3AA 109.5 . . ?
Si2A C3A H3AB 109.5 . . ?
Si2A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
Si3A C4A H4AA 109.5 . . ?
Si3A C4A H4AB 109.5 . . ?
Si3A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
Si3A C5A H5AA 109.5 . . ?
Si3A C5A H5AB 109.5 . . ?
Si3A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
Si3A C6A H6AA 109.5 . . ?
Si3A C6A H6AB 109.5 . . ?
Si3A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
Si4A C7A H7AA 109.5 . . ?
Si4A C7A H7AB 109.5 . . ?
Si4A C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
Si4A C8A H8AA 109.5 . . ?
Si4A C8A H8AB 109.5 . . ?
Si4A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
Si4A C9A H9AA 109.5 . . ?
Si4A C9A H9AB 109.5 . . ?
Si4A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 C13 C14 C15 68.0(5) . . . . ?
La1 C13 C20 C16 -68.4(5) . . . . ?
La1 C14 C15 C16 69.0(5) . . . . ?
La1 C15 C16 Si6 -130.7(5) . . . . ?
La1 C15 C16 C20 69.4(4) . . . . ?
La1 C16 C20 C13 68.5(5) . . . . ?
La1 C21 C22 Si7 107.4(5) . . . . ?
La1 C21 C22 C26 -68.2(4) . . . . ?
La1 C21 C28 Si8 -104.1(5) . . . . ?
La1 C21 C28 C27 69.1(4) . . . . ?
La1 C22 C26 C27 -68.4(5) . . . . ?
La1 C26 C27 C28 -68.5(4) . . . . ?
La1 C27 C28 Si8 105.0(5) . . . . ?
La1 C27 C28 C21 -68.5(4) . . . . ?
Si5 C13 C14 La1 132.5(5) . . . . ?
Si5 C13 C14 C15 -159.5(5) . . . . ?
Si5 C13 C20 La1 -132.1(5) . . . . ?
Si5 C13 C20 C16 159.5(5) . . . . ?
Si6 C16 C20 La1 130.7(5) . . . . ?
Si6 C16 C20 C13 -160.8(5) . . . . ?
Si7 C22 C26 La1 -108.6(5) . . . . ?
Si7 C22 C26 C27 -177.0(5) . . . . ?
C10 Si5 C13 La1 -45.5(5) . . . . ?
C10 Si5 C13 C14 -149.1(6) . . . . ?
C10 Si5 C13 C20 57.1(7) . . . . ?
C11 Si5 C13 La1 77.6(5) . . . . ?
C11 Si5 C13 C14 -26.0(7) . . . . ?
C11 Si5 C13 C20 -179.7(6) . . . . ?
C12 Si5 C13 La1 -164.5(5) . . . . ?
C12 Si5 C13 C14 91.9(7) . . . . ?
C12 Si5 C13 C20 -61.8(7) . . . . ?
C13 C14 C15 La1 -68.2(5) . . . . ?
C13 C14 C15 C16 0.8(8) . . . . ?
C14 C13 C20 La1 69.7(4) . . . . ?
C14 C13 C20 C16 1.3(7) . . . . ?
C14 C15 C16 La1 -69.4(5) . . . . ?
C14 C15 C16 Si6 160.0(5) . . . . ?
C14 C15 C16 C20 0.1(8) . . . . ?
C15 C16 C20 La1 -69.4(4) . . . . ?
C15 C16 C20 C13 -0.9(7) . . . . ?
C17 Si6 C16 La1 -74.9(5) . . . . ?
C17 Si6 C16 C15 27.2(7) . . . . ?
C17 Si6 C16 C20 -177.1(6) . . . . ?
C18 Si6 C16 La1 166.9(5) . . . . ?
C18 Si6 C16 C15 -91.0(7) . . . . ?
C18 Si6 C16 C20 64.8(7) . . . . ?
C19 Si6 C16 La1 48.3(6) . . . . ?
C19 Si6 C16 C15 150.3(6) . . . . ?
C19 Si6 C16 C20 -53.9(7) . . . . ?
C20 C13 C14 La1 -69.2(4) . . . . ?
C20 C13 C14 C15 -1.3(8) . . . . ?
C21 C22 C26 La1 67.1(4) . . . . ?
C21 C22 C26 C27 -1.3(7) . . . . ?
C22 C21 C28 La1 -70.5(4) . . . . ?
C22 C21 C28 Si8 -174.5(5) . . . . ?
C22 C21 C28 C27 -1.3(7) . . . . ?
C22 C26 C27 La1 69.0(4) . . . . ?
C22 C26 C27 C28 0.5(7) . . . . ?
C23 Si7 C22 La1 113.5(4) . . . . ?
C23 Si7 C22 C21 26.8(7) . . . . ?
C23 Si7 C22 C26 -158.5(6) . . . . ?
C24 Si7 C22 La1 -5.9(5) . . . . ?
C24 Si7 C22 C21 -92.7(6) . . . . ?
C24 Si7 C22 C26 82.0(6) . . . . ?
C25 Si7 C22 La1 -124.3(5) . . . . ?
C25 Si7 C22 C21 148.9(7) . . . . ?
C25 Si7 C22 C26 -36.4(8) . . . . ?
C26 C27 C28 La1 69.0(5) . . . . ?
C26 C27 C28 Si8 174.1(5) . . . . ?
C26 C27 C28 C21 0.5(7) . . . . ?
C28 C21 C22 La1 69.8(4) . . . . ?
C28 C21 C22 Si7 177.2(5) . . . . ?
C28 C21 C22 C26 1.6(7) . . . . ?
C29 Si8 C28 La1 124.0(4) . . . . ?
C29 Si8 C28 C21 -149.9(6) . . . . ?
C29 Si8 C28 C27 38.0(6) . . . . ?
C30 Si8 C28 La1 -113.9(3) . . . . ?
C30 Si8 C28 C21 -27.8(7) . . . . ?
C30 Si8 C28 C27 160.1(5) . . . . ?
C31 Si8 C28 La1 3.5(4) . . . . ?
C31 Si8 C28 C21 89.6(6) . . . . ?
C31 Si8 C28 C27 -82.5(6) . . . . ?

_audit_author_email              
;
benjamin.reant@postgrad.manchester.ac.uk, david.mills@manchester.ac.uk    
;
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 15s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_type   custom
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.586
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.823(2)
2 0.177(2)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-U
_database_code_depnum_ccdc_archive 'CCDC 2195634'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   rdpm227
_manchester_internal_coll_client AW
_manchester_internal_coll_user   AW
_manchester_internal_coll_date   06/08/2020
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 1s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_process_date 08/09/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 10/09/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 25/09/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 25/09/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 25/09/2020
_manchester_internal_archive_user AW
# start Validation Reply Form
_vrf_PLAT971_2-U                 
;
PROBLEM: Check Calcd Resid. Dens.  1.41A   From C21             7.14 eA-3  
RESPONSE: Residual density is located near heavy atoms
and present despite applying face-indexed absorption 
correction. They are not chemically significant.
;
_vrf_PLAT972_2-U                 
;
PROBLEM: Check Calcd Resid. Dens.  0.82A   From U1             -2.76 eA-3  
RESPONSE: Residual density is located near heavy atoms
and present despite applying face-indexed absorption 
correction. They are not chemically significant.
;
_audit_author_email              
;
benjamin.reant@postgrad.manchester.ac.uk, david.mills@manchester.ac.uk    
;
_refine_special_details          -
_audit_creation_date             2020-09-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[U(C5H3(1,3-SiMe3))2(I)]2'
_chemical_formula_moiety         'C44 H84 I2 Si8 U2'
_chemical_formula_sum            'C44 H84 I2 Si8 U2'
_chemical_formula_weight         1567.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         C44H84I2Si8U2
_chemical_oxdiff_usercomment     ' 	BR4.302'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6833(4)
_cell_length_b                   11.4914(4)
_cell_length_c                   13.2297(5)
_cell_angle_alpha                73.117(4)
_cell_angle_beta                 83.273(3)
_cell_angle_gamma                78.875(4)
_cell_volume                     1521.72(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9175
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1000
_cell_measurement_theta_min      3.4850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.523
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.072
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             750
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 5 7 0.0714
-3 -5 -7 0.0274
-3 3 -5 0.0050
3 -3 5 0.0590
-5 -6 -1 0.0256
5 6 1 0.0256

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 
'Crystallised from concentrated toluene solution at -25oC'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.051
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0000 5.0000 7.0000 0.1380 0.5146 0.8108
-3.0000 -5.0000 -7.0000 -0.1380 -0.5146 -0.8108
-3.0000 3.0000 -5.0000 -0.2565 -0.9005 0.2073
3.0000 -3.0000 5.0000 0.2565 0.9005 -0.2073
-5.0000 -6.0000 -1.0000 0.6442 -0.2035 -0.7408
5.0000 6.0000 1.0000 -0.6442 0.2035 0.7408

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15458
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.499
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -100.00  -9.00   1.00    1.00    --  -45.40 -38.00  60.00   91
  2  ω    -86.00 -22.00   1.00    1.00    --  -45.40  76.00   0.00   64
  3  ω    -85.00 -55.00   1.00    1.00    --  -45.40  38.00  30.00   30
  4  ω    -75.00 -50.00   1.00    1.00    --  -45.40  57.00 -60.00   25
  5  ω   -135.00-109.00   1.00    1.00    --  -45.40 -38.00  60.00   26
  6  ω    -42.00  44.00   1.00    1.00    --  -45.40  57.00 -60.00   86
  7  ω   -113.00 -15.00   1.00    1.00    --  -45.40 -57.00-180.00   98
  8  ω    -24.00  41.00   1.00    1.00    --  -45.40  38.00  30.00   65
  9  ω   -147.00 -19.00   1.00    1.00    -- -107.20  76.00 -90.00  128
 10  ω   -148.00 -39.00   1.00    1.00    -- -107.20   0.00 150.00  109
 11  ω   -109.00 -83.00   1.00    1.00    -- -107.20 -57.00  30.00   26
 12  ω   -197.00 -80.00   1.00    1.00    -- -107.20 -38.00 -60.00  117
 13  ω   -109.00 -24.00   1.00    1.00    -- -107.20  57.00 -90.00   85
 14  ω    -55.00 -28.00   1.00    1.00    -- -107.20  76.00-150.00   27
 15  ω   -163.00-131.00   1.00    1.00    -- -107.20 -57.00  30.00   32
 16  ω   -134.00 -84.00   1.00    1.00    -- -107.20  76.00-150.00   50
 17  ω   -196.00 -68.00   1.00    1.00    -- -107.20 -38.00 -30.00  128
 18  ω   -121.00 -89.00   1.00    1.00    -- -107.20  76.00 120.00   32
 19  ω   -117.00 -82.00   1.00    1.00    -- -107.20  76.00-180.00   35
 20  ω    -96.00 -59.00   1.00    1.00    -- -107.20  76.00 -60.00   37
 21  ω   -131.00 -18.00   1.00    1.00    -- -107.20  76.00  30.00  113
 22  ω   -119.00 -94.00   1.00    1.00    -- -107.20  76.00 -30.00   25
 23  ω   -131.00 -99.00   1.00    1.00    -- -107.20  76.00  90.00   32
 24  ω   -140.00 -19.00   1.00    1.00    -- -107.20  76.00 150.00  121
 25  ω   -121.00 -96.00   1.00    1.00    -- -107.20  76.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1020590000
_diffrn_orient_matrix_UB_12      -0.0373442000
_diffrn_orient_matrix_UB_13      0.0901217000
_diffrn_orient_matrix_UB_21      0.1061712000
_diffrn_orient_matrix_UB_22      -0.0672402000
_diffrn_orient_matrix_UB_23      0.0760451000
_diffrn_orient_matrix_UB_31      -0.0014440000
_diffrn_orient_matrix_UB_32      0.1194871000
_diffrn_orient_matrix_UB_33      0.0311007000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5285
_reflns_number_total             5530
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.777
_refine_diff_density_min         -2.703
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5530
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0830P)²+4.0484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1151
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C11(H11), C5(H5), C16(H16), C6(H6)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C3(H3A,H3B,
 H3C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C2(H2A,H2B,H2C), C9(H9A,H9B,
 H9C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C1(H1A,H1B,
 H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.47788(2) 0.50285(2) 0.17560(2) 0.02576(11) Uani 1 1 d . . . . .
I1 I 0.46976(4) 0.31129(4) 0.04784(3) 0.03036(13) Uani 1 1 d . . . . .
Si3 Si 0.72624(18) 0.16427(17) 0.29135(15) 0.0312(4) Uani 1 1 d . . . . .
Si2 Si 0.27943(18) 0.82687(16) 0.24289(15) 0.0303(4) Uani 1 1 d . . . . .
Si1 Si 0.20094(19) 0.31659(17) 0.37247(16) 0.0326(4) Uani 1 1 d . . . . .
Si4 Si 0.79650(18) 0.67411(17) 0.16977(15) 0.0316(4) Uani 1 1 d . . . . .
C7 C 0.2776(6) 0.6683(6) 0.2316(5) 0.0249(12) Uani 1 1 d . . . . .
C21 C 0.6282(6) 0.5180(6) 0.3227(5) 0.0301(14) Uani 1 1 d . . . . .
H21 H 0.593305 0.576138 0.359049 0.036 Uiso 1 1 calc R . . . .
C22 C 0.6115(7) 0.3925(6) 0.3531(6) 0.0318(14) Uani 1 1 d . . . . .
H22 H 0.563236 0.355076 0.412642 0.038 Uiso 1 1 calc R . . . .
C11 C 0.2823(6) 0.5590(6) 0.3160(5) 0.0287(13) Uani 1 1 d . . . . .
H11 H 0.306510 0.550751 0.383323 0.034 Uiso 1 1 calc R . . . .
C17 C 0.7081(6) 0.5395(6) 0.2265(6) 0.0310(14) Uani 1 1 d . . . . .
C5 C 0.2166(6) 0.5174(7) 0.1751(6) 0.0307(14) Uani 1 1 d . . . . .
H5 H 0.189721 0.477071 0.132024 0.037 Uiso 1 1 calc R . . . .
C4 C 0.2452(6) 0.4634(6) 0.2842(6) 0.0302(14) Uani 1 1 d . . . . .
C16 C 0.7387(7) 0.4274(6) 0.2003(6) 0.0316(14) Uani 1 1 d . . . . .
H16 H 0.789737 0.415610 0.140988 0.038 Uiso 1 1 calc R . . . .
C6 C 0.2359(6) 0.6408(6) 0.1442(6) 0.0305(14) Uani 1 1 d . . . . .
H6 H 0.223368 0.695494 0.077506 0.037 Uiso 1 1 calc R . . . .
C15 C 0.6809(6) 0.3327(6) 0.2771(5) 0.0289(13) Uani 1 1 d . . . . .
C14 C 0.8134(8) 0.1410(7) 0.1652(6) 0.0416(17) Uani 1 1 d . . . . .
H14A H 0.757553 0.175264 0.108223 0.062 Uiso 1 1 calc GR . . . .
H14B H 0.840471 0.054419 0.172874 0.062 Uiso 1 1 calc GR . . . .
H14C H 0.886834 0.181530 0.149952 0.062 Uiso 1 1 calc GR . . . .
C19 C 0.6894(8) 0.8268(7) 0.1456(7) 0.0411(17) Uani 1 1 d . . . . .
H19A H 0.634403 0.835325 0.090547 0.062 Uiso 1 1 calc GR . . . .
H19B H 0.740092 0.891337 0.124471 0.062 Uiso 1 1 calc GR . . . .
H19C H 0.638465 0.832232 0.209378 0.062 Uiso 1 1 calc GR . . . .
C18 C 0.8886(7) 0.6585(8) 0.0436(6) 0.0419(17) Uani 1 1 d . . . . .
H18A H 0.938755 0.577476 0.055134 0.063 Uiso 1 1 calc GR . . . .
H18B H 0.944042 0.719082 0.020824 0.063 Uiso 1 1 calc GR . . . .
H18C H 0.830180 0.670985 -0.009977 0.063 Uiso 1 1 calc GR . . . .
C3 C 0.0320(8) 0.3465(8) 0.4277(6) 0.0421(17) Uani 1 1 d . . . . .
H3A H 0.022525 0.411492 0.461545 0.063 Uiso 1 1 calc GR . . . .
H3B H 0.011647 0.272902 0.478559 0.063 Uiso 1 1 calc GR . . . .
H3C H -0.024850 0.370584 0.371419 0.063 Uiso 1 1 calc GR . . . .
C12 C 0.8362(8) 0.0973(7) 0.4012(7) 0.0414(17) Uani 1 1 d . . . . .
H12A H 0.908853 0.138901 0.386058 0.062 Uiso 1 1 calc GR . . . .
H12B H 0.864453 0.011079 0.407636 0.062 Uiso 1 1 calc GR . . . .
H12C H 0.791945 0.107513 0.466291 0.062 Uiso 1 1 calc GR . . . .
C10 C 0.1139(8) 0.8916(8) 0.2844(8) 0.050(2) Uani 1 1 d . . . . .
H10A H 0.058075 0.902889 0.229306 0.075 Uiso 1 1 calc GR . . . .
H10B H 0.114059 0.969610 0.297277 0.075 Uiso 1 1 calc GR . . . .
H10C H 0.084580 0.835622 0.347985 0.075 Uiso 1 1 calc GR . . . .
C2 C 0.2113(8) 0.1997(7) 0.2985(7) 0.0436(18) Uani 1 1 d . . . . .
H2A H 0.155252 0.231339 0.241539 0.065 Uiso 1 1 calc GR . . . .
H2B H 0.186500 0.125628 0.345436 0.065 Uiso 1 1 calc GR . . . .
H2C H 0.297587 0.181693 0.270340 0.065 Uiso 1 1 calc GR . . . .
C9 C 0.3845(7) 0.8177(7) 0.3499(6) 0.0377(16) Uani 1 1 d . . . . .
H9A H 0.350929 0.770664 0.416549 0.057 Uiso 1 1 calc GR . . . .
H9B H 0.386953 0.899387 0.353727 0.057 Uiso 1 1 calc GR . . . .
H9C H 0.469372 0.778359 0.334304 0.057 Uiso 1 1 calc GR . . . .
C20 C 0.9097(8) 0.6682(8) 0.2696(7) 0.0468(19) Uani 1 1 d . . . . .
H20A H 0.863291 0.666788 0.336537 0.070 Uiso 1 1 calc GR . . . .
H20B H 0.950794 0.739565 0.246355 0.070 Uiso 1 1 calc GR . . . .
H20C H 0.973074 0.595050 0.277237 0.070 Uiso 1 1 calc GR . . . .
C8 C 0.3263(9) 0.9328(7) 0.1142(7) 0.0460(19) Uani 1 1 d . . . . .
H8A H 0.411639 0.902184 0.091098 0.069 Uiso 1 1 calc GR . . . .
H8B H 0.323135 1.013480 0.122799 0.069 Uiso 1 1 calc GR . . . .
H8C H 0.268392 0.937379 0.062415 0.069 Uiso 1 1 calc GR . . . .
C13 C 0.5876(8) 0.0798(7) 0.3267(7) 0.0448(19) Uani 1 1 d . . . . .
H13A H 0.547031 0.088586 0.393356 0.067 Uiso 1 1 calc GR . . . .
H13B H 0.617106 -0.005987 0.331959 0.067 Uiso 1 1 calc GR . . . .
H13C H 0.527378 0.113411 0.272866 0.067 Uiso 1 1 calc GR . . . .
C1 C 0.3071(8) 0.2572(8) 0.4862(6) 0.0444(18) Uani 1 1 d . . . . .
H1A H 0.393222 0.233208 0.460393 0.067 Uiso 1 1 calc GR . . . .
H1B H 0.277784 0.187086 0.535997 0.067 Uiso 1 1 calc GR . . . .
H1C H 0.304698 0.320772 0.520384 0.067 Uiso 1 1 calc GR . . . .


_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
U1 I1 3.1653(5) 2_665 ?
U1 I1 3.1589(5) . ?
U1 C7 2.761(6) . ?
U1 C21 2.727(6) . ?
U1 C22 2.741(7) . ?
U1 C11 2.738(7) . ?
U1 C17 2.763(7) . ?
U1 C5 2.764(7) . ?
U1 C4 2.769(7) . ?
U1 C16 2.782(7) . ?
U1 C6 2.767(7) . ?
U1 C15 2.802(7) . ?
Si3 C15 1.861(7) . ?
Si3 C14 1.877(8) . ?
Si3 C12 1.867(8) . ?
Si3 C13 1.866(8) . ?
Si2 C7 1.875(6) . ?
Si2 C10 1.866(8) . ?
Si2 C9 1.875(8) . ?
Si2 C8 1.861(8) . ?
Si1 C4 1.863(7) . ?
Si1 C3 1.873(8) . ?
Si1 C2 1.859(8) . ?
Si1 C1 1.876(8) . ?
Si4 C17 1.889(7) . ?
Si4 C19 1.864(8) . ?
Si4 C18 1.873(8) . ?
Si4 C20 1.872(8) . ?
C7 C11 1.414(9) . ?
C7 C6 1.423(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.421(9) . ?
C21 C17 1.433(10) . ?
C22 H22 0.9300 . ?
C22 C15 1.437(10) . ?
C11 H11 0.9300 . ?
C11 C4 1.419(9) . ?
C17 C16 1.400(10) . ?
C5 H5 0.9300 . ?
C5 C4 1.438(10) . ?
C5 C6 1.406(10) . ?
C16 H16 0.9300 . ?
C16 C15 1.438(9) . ?
C6 H6 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?

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
I1 U1 I1 85.794(12) . 2_665 ?
C7 U1 I1 92.54(13) . 2_665 ?
C7 U1 I1 127.98(13) . . ?
C7 U1 C17 110.9(2) . . ?
C7 U1 C5 49.22(19) . . ?
C7 U1 C4 49.95(19) . . ?
C7 U1 C16 139.45(19) . . ?
C7 U1 C6 29.82(19) . . ?
C7 U1 C15 136.26(19) . . ?
C21 U1 I1 135.70(15) . . ?
C21 U1 I1 111.58(14) . 2_665 ?
C21 U1 C7 92.9(2) . . ?
C21 U1 C22 30.1(2) . . ?
C21 U1 C11 83.6(2) . . ?
C21 U1 C17 30.3(2) . . ?
C21 U1 C5 132.1(2) . . ?
C21 U1 C4 105.2(2) . . ?
C21 U1 C16 48.7(2) . . ?
C21 U1 C6 122.7(2) . . ?
C21 U1 C15 49.8(2) . . ?
C22 U1 I1 135.55(14) . 2_665 ?
C22 U1 I1 110.77(15) . . ?
C22 U1 C7 106.3(2) . . ?
C22 U1 C17 49.7(2) . . ?
C22 U1 C5 123.1(2) . . ?
C22 U1 C4 93.0(2) . . ?
C22 U1 C16 48.7(2) . . ?
C22 U1 C6 132.8(2) . . ?
C22 U1 C15 30.0(2) . . ?
C11 U1 I1 122.21(14) . . ?
C11 U1 I1 122.29(14) . 2_665 ?
C11 U1 C7 29.81(19) . . ?
C11 U1 C22 84.3(2) . . ?
C11 U1 C17 111.4(2) . . ?
C11 U1 C5 48.7(2) . . ?
C11 U1 C4 29.9(2) . . ?
C11 U1 C16 130.6(2) . . ?
C11 U1 C6 48.6(2) . . ?
C11 U1 C15 112.2(2) . . ?
C17 U1 I1 86.12(14) . 2_665 ?
C17 U1 I1 120.75(15) . . ?
C17 U1 C5 159.1(2) . . ?
C17 U1 C4 135.4(2) . . ?
C17 U1 C16 29.2(2) . . ?
C17 U1 C6 135.9(2) . . ?
C17 U1 C15 49.75(19) . . ?
C5 U1 I1 99.87(14) . 2_665 ?
C5 U1 I1 79.82(15) . . ?
C5 U1 C4 30.1(2) . . ?
C5 U1 C16 165.9(2) . . ?
C5 U1 C6 29.5(2) . . ?
C5 U1 C15 136.7(2) . . ?
C4 U1 I1 92.42(14) . . ?
C4 U1 I1 128.39(14) . 2_665 ?
C4 U1 C16 140.2(2) . . ?
C4 U1 C15 111.5(2) . . ?
C16 U1 I1 91.32(14) . 2_665 ?
C16 U1 I1 92.56(15) . . ?
C16 U1 C15 29.84(19) . . ?
C6 U1 I1 80.00(14) . 2_665 ?
C6 U1 I1 99.80(15) . . ?
C6 U1 C4 49.5(2) . . ?
C6 U1 C16 164.3(2) . . ?
C6 U1 C15 160.0(2) . . ?
C15 U1 I1 119.75(14) . 2_665 ?
C15 U1 I1 86.00(14) . . ?
U1 I1 U1 94.208(12) . 2_665 ?
C15 Si3 C14 108.9(3) . . ?
C15 Si3 C12 108.0(3) . . ?
C15 Si3 C13 113.6(3) . . ?
C12 Si3 C14 108.9(4) . . ?
C13 Si3 C14 110.4(4) . . ?
C13 Si3 C12 107.0(4) . . ?
C7 Si2 C9 110.0(3) . . ?
C10 Si2 C7 107.9(3) . . ?
C10 Si2 C9 106.9(4) . . ?
C8 Si2 C7 112.1(3) . . ?
C8 Si2 C10 107.6(4) . . ?
C8 Si2 C9 112.1(4) . . ?
C4 Si1 C3 109.3(3) . . ?
C4 Si1 C1 109.5(3) . . ?
C3 Si1 C1 108.0(4) . . ?
C2 Si1 C4 111.2(3) . . ?
C2 Si1 C3 107.9(4) . . ?
C2 Si1 C1 110.8(4) . . ?
C19 Si4 C17 113.2(3) . . ?
C19 Si4 C18 109.8(4) . . ?
C19 Si4 C20 107.4(4) . . ?
C18 Si4 C17 109.6(3) . . ?
C20 Si4 C17 107.1(4) . . ?
C20 Si4 C18 109.6(4) . . ?
Si2 C7 U1 128.5(3) . . ?
C11 C7 U1 74.2(4) . . ?
C11 C7 Si2 126.3(5) . . ?
C11 C7 C6 106.1(6) . . ?
C6 C7 U1 75.3(4) . . ?
C6 C7 Si2 125.6(5) . . ?
U1 C21 H21 114.6 . . ?
C22 C21 U1 75.5(4) . . ?
C22 C21 H21 125.9 . . ?
C22 C21 C17 108.3(6) . . ?
C17 C21 U1 76.3(4) . . ?
C17 C21 H21 125.9 . . ?
U1 C22 H22 114.9 . . ?
C21 C22 U1 74.4(4) . . ?
C21 C22 H22 125.4 . . ?
C21 C22 C15 109.1(6) . . ?
C15 C22 U1 77.3(4) . . ?
C15 C22 H22 125.4 . . ?
U1 C11 H11 115.0 . . ?
C7 C11 U1 76.0(4) . . ?
C7 C11 H11 124.5 . . ?
C7 C11 C4 110.9(6) . . ?
C4 C11 U1 76.3(4) . . ?
C4 C11 H11 124.5 . . ?
Si4 C17 U1 129.9(3) . . ?
C21 C17 U1 73.5(4) . . ?
C21 C17 Si4 126.3(5) . . ?
C16 C17 U1 76.1(4) . . ?
C16 C17 Si4 124.7(5) . . ?
C16 C17 C21 106.6(6) . . ?
U1 C5 H5 116.0 . . ?
C4 C5 U1 75.1(4) . . ?
C4 C5 H5 125.5 . . ?
C6 C5 U1 75.4(4) . . ?
C6 C5 H5 125.5 . . ?
C6 C5 C4 109.0(6) . . ?
Si1 C4 U1 128.2(3) . . ?
C11 C4 U1 73.9(4) . . ?
C11 C4 Si1 126.7(5) . . ?
C11 C4 C5 105.1(6) . . ?
C5 C4 U1 74.8(4) . . ?
C5 C4 Si1 126.3(5) . . ?
U1 C16 H16 116.8 . . ?
C17 C16 U1 74.7(4) . . ?
C17 C16 H16 124.4 . . ?
C17 C16 C15 111.2(6) . . ?
C15 C16 U1 75.9(4) . . ?
C15 C16 H16 124.4 . . ?
U1 C6 H6 116.4 . . ?
C7 C6 U1 74.8(4) . . ?
C7 C6 H6 125.6 . . ?
C5 C6 U1 75.2(4) . . ?
C5 C6 C7 108.9(6) . . ?
C5 C6 H6 125.6 . . ?
Si3 C15 U1 130.1(3) . . ?
C22 C15 U1 72.7(4) . . ?
C22 C15 Si3 128.0(5) . . ?
C22 C15 C16 104.8(6) . . ?
C16 C15 U1 74.3(4) . . ?
C16 C15 Si3 125.2(5) . . ?
Si3 C14 H14A 109.5 . . ?
Si3 C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C19 H19A 109.5 . . ?
Si4 C19 H19B 109.5 . . ?
Si4 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si4 C18 H18A 109.5 . . ?
Si4 C18 H18B 109.5 . . ?
Si4 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si4 C20 H20A 109.5 . . ?
Si4 C20 H20B 109.5 . . ?
Si4 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 C7 C11 C4 -69.0(5) . . . . ?
U1 C7 C6 C5 68.1(5) . . . . ?
U1 C21 C22 C15 70.2(5) . . . . ?
U1 C21 C17 Si4 127.7(5) . . . . ?
U1 C21 C17 C16 -69.5(5) . . . . ?
U1 C22 C15 Si3 -127.8(5) . . . . ?
U1 C22 C15 C16 67.9(4) . . . . ?
U1 C11 C4 Si1 126.0(5) . . . . ?
U1 C11 C4 C5 -68.8(5) . . . . ?
U1 C17 C16 C15 -67.8(5) . . . . ?
U1 C5 C4 Si1 -126.6(5) . . . . ?
U1 C5 C4 C11 68.2(4) . . . . ?
U1 C5 C6 C7 -67.9(5) . . . . ?
U1 C16 C15 Si3 128.4(5) . . . . ?
U1 C16 C15 C22 -66.8(4) . . . . ?
Si2 C7 C11 U1 -126.6(5) . . . . ?
Si2 C7 C11 C4 164.4(5) . . . . ?
Si2 C7 C6 U1 127.2(5) . . . . ?
Si2 C7 C6 C5 -164.7(5) . . . . ?
Si4 C17 C16 U1 -129.2(5) . . . . ?
Si4 C17 C16 C15 163.0(5) . . . . ?
C7 C11 C4 U1 68.9(5) . . . . ?
C7 C11 C4 Si1 -165.1(5) . . . . ?
C7 C11 C4 C5 0.0(8) . . . . ?
C21 C22 C15 U1 -68.3(5) . . . . ?
C21 C22 C15 Si3 164.0(5) . . . . ?
C21 C22 C15 C16 -0.3(8) . . . . ?
C21 C17 C16 U1 67.7(5) . . . . ?
C21 C17 C16 C15 -0.1(8) . . . . ?
C22 C21 C17 U1 69.4(5) . . . . ?
C22 C21 C17 Si4 -162.9(5) . . . . ?
C22 C21 C17 C16 -0.1(8) . . . . ?
C11 C7 C6 U1 -68.4(4) . . . . ?
C11 C7 C6 C5 -0.3(7) . . . . ?
C17 C21 C22 U1 -69.9(5) . . . . ?
C17 C21 C22 C15 0.3(8) . . . . ?
C17 C16 C15 U1 67.0(5) . . . . ?
C17 C16 C15 Si3 -164.6(5) . . . . ?
C17 C16 C15 C22 0.3(8) . . . . ?
C4 C5 C6 U1 68.2(5) . . . . ?
C4 C5 C6 C7 0.3(8) . . . . ?
C6 C7 C11 U1 69.2(4) . . . . ?
C6 C7 C11 C4 0.2(8) . . . . ?
C6 C5 C4 U1 -68.4(5) . . . . ?
C6 C5 C4 Si1 165.0(5) . . . . ?
C6 C5 C4 C11 -0.2(8) . . . . ?
C14 Si3 C15 U1 79.5(5) . . . . ?
C14 Si3 C15 C22 178.9(6) . . . . ?
C14 Si3 C15 C16 -19.7(7) . . . . ?
C19 Si4 C17 U1 41.2(6) . . . . ?
C19 Si4 C17 C21 -57.6(7) . . . . ?
C19 Si4 C17 C16 142.6(6) . . . . ?
C18 Si4 C17 U1 -81.7(5) . . . . ?
C18 Si4 C17 C21 179.5(6) . . . . ?
C18 Si4 C17 C16 19.7(7) . . . . ?
C3 Si1 C4 U1 178.1(4) . . . . ?
C3 Si1 C4 C11 79.7(7) . . . . ?
C3 Si1 C4 C5 -82.4(7) . . . . ?
C12 Si3 C15 U1 -162.4(4) . . . . ?
C12 Si3 C15 C22 -63.0(7) . . . . ?
C12 Si3 C15 C16 98.4(6) . . . . ?
C10 Si2 C7 U1 -179.8(4) . . . . ?
C10 Si2 C7 C11 -81.0(7) . . . . ?
C10 Si2 C7 C6 80.3(7) . . . . ?
C2 Si1 C4 U1 -62.9(5) . . . . ?
C2 Si1 C4 C11 -161.3(6) . . . . ?
C2 Si1 C4 C5 36.6(7) . . . . ?
C9 Si2 C7 U1 -63.5(5) . . . . ?
C9 Si2 C7 C11 35.4(7) . . . . ?
C9 Si2 C7 C6 -163.4(6) . . . . ?
C20 Si4 C17 U1 159.4(4) . . . . ?
C20 Si4 C17 C21 60.6(7) . . . . ?
C20 Si4 C17 C16 -99.2(7) . . . . ?
C8 Si2 C7 U1 61.9(5) . . . . ?
C8 Si2 C7 C11 160.8(6) . . . . ?
C8 Si2 C7 C6 -38.0(7) . . . . ?
C13 Si3 C15 U1 -44.0(5) . . . . ?
C13 Si3 C15 C22 55.4(7) . . . . ?
C13 Si3 C15 C16 -143.2(6) . . . . ?
C1 Si1 C4 U1 59.9(5) . . . . ?
C1 Si1 C4 C11 -38.5(7) . . . . ?
C1 Si1 C4 C5 159.4(6) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR4.302
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.063
_oxdiff_exptl_absorpt_empirical_full_min 0.437
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-Ce
_database_code_depnum_ccdc_archive 'CCDC 2195638'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   rdpm236
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   02/10/2020
_manchester_internal_process_date 02/10/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 02/10/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 02/10/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 02/10/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 02/10/2020
_manchester_internal_archive_user AW
_refine_special_details          
;
The Si(SiMe3)3 group is disordered over two orientations. The occupanices were
 allowed to freely refine converging at 0.52:0.48. 
Selected chemically equivalent Si-C and C-C distances were 
restrained to be approximately equal.Enhanced rigid bond and 
similarity thermla restraints were applied to disordered groups.
;
_audit_creation_date             2020-10-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[Ce(C5H3-1,3-SiMe3)2{Si(SiMe3)3}]'
_chemical_formula_moiety         'C31 H69 Ce Si8'
_chemical_formula_sum            'C31 H69 Ce Si8'
_chemical_formula_weight         806.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ce1 Si8 C31 H69'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.8079(6)
_cell_length_b                   13.2758(3)
_cell_length_c                   20.3529(6)
_cell_angle_alpha                90
_cell_angle_beta                 111.045(3)
_cell_angle_gamma                90
_cell_volume                     4490.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.3580
_cell_measurement_theta_min      2.8250
_shelx_estimated_absorpt_T_max   0.420
_shelx_estimated_absorpt_T_min   0.089
_exptl_absorpt_coefficient_mu    10.002
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 3 0 0.0580
-10 -3 0 0.0580
-4 0 13 0.2235
4 0 -13 0.2235
3 -8 2 0.0525
-3 8 -2 0.0525

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method -
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.105
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
9.9976 3.0000 0.0042 0.3118 0.9346 0.1013
-9.9976 -3.0000 -0.0042 -0.3118 -0.9346 -0.1013
-4.0034 -0.0105 13.0167 0.0218 0.1074 -0.9792
4.0034 0.0105 -13.0167 -0.0218 -0.1074 0.9792
3.0000 -7.9906 2.0027 -0.9353 0.3164 -0.1422
-3.0000 7.9906 -2.0027 0.9353 -0.3164 0.1422

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8916
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.697
_diffrn_reflns_theta_min         2.835
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -134.00 -58.00   1.00    1.00    --  -45.40 -76.00 -30.00   76
  2  ω    -82.00  22.00   1.00    1.00    --  -45.40  76.00  30.00  104
  3  ω    -82.00   9.00   1.00    1.00    --  -45.40  38.00  30.00   91
  4  ω    -33.00  -8.00   1.00    1.00    --  -45.40 -76.00 -30.00   25
  5  ω   -143.00 -31.00   1.00    1.00    -- -107.20  76.00-150.00  112
  6  ω   -169.00 -76.00   1.00    1.00    -- -107.20 -38.00 -60.00   93
  7  ω    -77.00 -20.00   1.00    1.00    -- -107.20  76.00 -90.00   57
  8  ω   -108.00 -27.00   1.00    1.00    -- -107.20  76.00 -60.00   81
  9  ω   -115.00 -62.00   1.00    1.00    -- -107.20  76.00-180.00   53
 10  ω   -118.00 -82.00   1.00    1.00    -- -107.20  76.00 -90.00   36
 11  ω   -135.00 -76.00   1.00    1.00    -- -107.20  57.00 120.00   59
 12  ω    -50.00 -25.00   1.00    1.00    -- -107.20  57.00 120.00   25
 13  ω   -171.00 -19.00   1.00    1.00    -- -107.20 -19.00 -30.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0035820000
_diffrn_orient_matrix_UB_12      0.1158710000
_diffrn_orient_matrix_UB_13      0.0006656000
_diffrn_orient_matrix_UB_21      0.0922066000
_diffrn_orient_matrix_UB_22      0.0042009000
_diffrn_orient_matrix_UB_23      0.0366128000
_diffrn_orient_matrix_UB_31      0.0092275000
_diffrn_orient_matrix_UB_32      0.0031210000
_diffrn_orient_matrix_UB_33      -0.0723845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8056
_reflns_number_total             8916
_reflns_odcompleteness_completeness 97.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.909
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8916
_refine_ls_number_restraints     666
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0679
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0817P)²+22.5993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.1936
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.648(3)
 0.352(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Si2A-C2A \\sim Si2A-C1A \\sim Si2A-C3A \\sim Si2-C1 \\sim Si2-C2 \\sim Si2-C3
\\sim Si4-C7 \\sim Si4-C9 ~
 Si4-C8 \\sim Si4A-C7A \\sim Si4A-C9A \\sim Si4A-C8A \\sim Si3-C6 \\sim Si3-C4
\\sim Si3-C5 \\sim Si3A-C6A
 \\sim Si3A-C4A \\sim Si3A-C5A
 with sigma of 0.02
 C5-C4 \\sim C6-C5 \\sim C6-C4 \\sim C8A-C7A \\sim C9A-C8A \\sim C9A-C7A \\sim
C8-C7 \\sim C9-C7 \\sim C9-C8 ~
 C2A-C1A \\sim C3A-C1A \\sim C3A-C2A \\sim C3-C1 \\sim C2-C1 \\sim C3-C2 \\sim
C5A-C4A \\sim C6A-C5A \\sim C6A-
 C4A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Si1 \\sim Si2 \\sim Si3 \\sim Si4 \\sim Si2A \\sim Si3A \\sim Si4A \\sim C1
\\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Si2, Si2A, Si3A, C1, C2, C3, C5, C7, C2A, C3A, C4A, C5A, C6A, Si1, Si3, Si4,
 Si4A, C4, C6, C8, C9, C1A, C7A, C8A, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Si2A)=Sof(Si3A)=Sof(Si4A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(Si2)=Sof(Si3)=Sof(Si4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C20(H20), C25(H25), C26(H26), C31(H31)
7.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,
 H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC),
  C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,
 H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.55733(2) 0.38107(3) 0.26376(2) 0.03169(14) Uani 1 1 d . . . . .
Si1 Si 0.42424(11) 0.55031(14) 0.22298(10) 0.0297(4) Uani 1 1 d . U . . .
Si5 Si 0.67810(13) 0.5108(2) 0.44774(12) 0.0459(5) Uani 1 1 d . . . . .
Si6 Si 0.67835(12) 0.49173(15) 0.15866(11) 0.0344(4) Uani 1 1 d . . . . .
Si7 Si 0.52787(14) 0.14198(16) 0.11477(12) 0.0417(5) Uani 1 1 d . . . . .
Si8 Si 0.53232(16) 0.14877(18) 0.39908(13) 0.0485(6) Uani 1 1 d . . . . .
Si2 Si 0.3583(2) 0.5751(3) 0.3050(2) 0.0346(9) Uani 0.523(4) 1 d D U P A 1
Si3 Si 0.3134(2) 0.4913(3) 0.12582(19) 0.0313(8) Uani 0.523(4) 1 d D U P A 1
Si4 Si 0.4416(2) 0.7128(3) 0.1882(2) 0.0373(9) Uani 0.523(4) 1 d D U P A 1
Si2A Si 0.4493(3) 0.7187(3) 0.2655(2) 0.0384(10) Uani 0.477(4) 1 d D U P A 2
Si3A Si 0.3135(2) 0.5042(3) 0.2500(2) 0.0301(9) Uani 0.477(4) 1 d D U P A 2
Si4A Si 0.3631(2) 0.5799(3) 0.1007(2) 0.0326(9) Uani 0.477(4) 1 d D U P A 2
C10 C 0.6827(7) 0.6505(9) 0.4539(7) 0.073(3) Uani 1 1 d . . . . .
H10A H 0.736663 0.673368 0.458489 0.110 Uiso 1 1 calc GR . . . .
H10B H 0.670847 0.672181 0.495198 0.110 Uiso 1 1 calc GR . . . .
H10C H 0.642983 0.679606 0.411334 0.110 Uiso 1 1 calc GR . . . .
C11 C 0.5765(5) 0.4644(8) 0.4421(6) 0.057(2) Uani 1 1 d . . . . .
H11A H 0.534775 0.499197 0.403665 0.086 Uiso 1 1 calc GR . . . .
H11B H 0.568936 0.478054 0.486607 0.086 Uiso 1 1 calc GR . . . .
H11C H 0.572834 0.391735 0.433039 0.086 Uiso 1 1 calc GR . . . .
C12 C 0.7588(7) 0.4514(12) 0.5233(6) 0.090(5) Uani 1 1 d . . . . .
H12A H 0.751048 0.378275 0.521578 0.135 Uiso 1 1 calc GR . . . .
H12B H 0.756489 0.477734 0.567493 0.135 Uiso 1 1 calc GR . . . .
H12C H 0.811372 0.467073 0.520506 0.135 Uiso 1 1 calc GR . . . .
C13 C 0.6920(4) 0.4679(6) 0.3658(4) 0.0382(16) Uani 1 1 d . . . . .
C14 C 0.7171(5) 0.3698(6) 0.3534(4) 0.0394(17) Uani 1 1 d . . . . .
H14 H 0.730119 0.315289 0.385831 0.047 Uiso 1 1 calc R . . . .
C15 C 0.7193(4) 0.3676(6) 0.2856(4) 0.0367(16) Uani 1 1 d . . . . .
H15 H 0.734742 0.311185 0.264677 0.044 Uiso 1 1 calc R . . . .
C16 C 0.6947(4) 0.4627(6) 0.2525(4) 0.0357(15) Uani 1 1 d . . . . .
C17 C 0.7565(5) 0.4247(7) 0.1336(5) 0.0453(19) Uani 1 1 d . . . . .
H17A H 0.809267 0.455108 0.158399 0.068 Uiso 1 1 calc GR . . . .
H17B H 0.743368 0.430465 0.082663 0.068 Uiso 1 1 calc GR . . . .
H17C H 0.757763 0.353472 0.146534 0.068 Uiso 1 1 calc GR . . . .
C18 C 0.5739(5) 0.4449(6) 0.1078(4) 0.0421(17) Uani 1 1 d . . . . .
H18A H 0.571342 0.372177 0.114861 0.063 Uiso 1 1 calc GR . . . .
H18B H 0.560520 0.458905 0.057570 0.063 Uiso 1 1 calc GR . . . .
H18C H 0.535319 0.479315 0.124363 0.063 Uiso 1 1 calc GR . . . .
C19 C 0.6834(5) 0.6301(6) 0.1447(5) 0.0431(18) Uani 1 1 d . . . . .
H19A H 0.650692 0.665577 0.167108 0.065 Uiso 1 1 calc GR . . . .
H19B H 0.662859 0.644614 0.094140 0.065 Uiso 1 1 calc GR . . . .
H19C H 0.739410 0.652715 0.165595 0.065 Uiso 1 1 calc GR . . . .
C20 C 0.6778(4) 0.5233(6) 0.3022(4) 0.0370(16) Uani 1 1 d . . . . .
H20 H 0.659566 0.591038 0.294624 0.044 Uiso 1 1 calc R . . . .
C21 C 0.4551(5) 0.1991(7) 0.0326(4) 0.0465(19) Uani 1 1 d . . . . .
H21A H 0.400207 0.191349 0.032202 0.070 Uiso 1 1 calc GR . . . .
H21B H 0.459667 0.165052 -0.008536 0.070 Uiso 1 1 calc GR . . . .
H21C H 0.467245 0.270864 0.031002 0.070 Uiso 1 1 calc GR . . . .
C22 C 0.5068(8) 0.0037(7) 0.1160(6) 0.069(3) Uani 1 1 d . . . . .
H22A H 0.552755 -0.029689 0.151281 0.104 Uiso 1 1 calc GR . . . .
H22B H 0.497978 -0.025188 0.069471 0.104 Uiso 1 1 calc GR . . . .
H22C H 0.458579 -0.006372 0.127780 0.104 Uiso 1 1 calc GR . . . .
C23 C 0.6338(5) 0.1584(8) 0.1186(6) 0.057(2) Uani 1 1 d . . . . .
H23A H 0.644030 0.229866 0.113073 0.086 Uiso 1 1 calc GR . . . .
H23B H 0.641653 0.119652 0.080537 0.086 Uiso 1 1 calc GR . . . .
H23C H 0.671203 0.134256 0.164047 0.086 Uiso 1 1 calc GR . . . .
C24 C 0.5122(4) 0.1970(5) 0.1939(4) 0.0340(15) Uani 1 1 d . . . . .
C25 C 0.4395(4) 0.2411(5) 0.1941(4) 0.0352(15) Uani 1 1 d . . . . .
H25 H 0.397174 0.265914 0.153941 0.042 Uiso 1 1 calc R . . . .
C26 C 0.4403(5) 0.2422(5) 0.2628(4) 0.0347(15) Uani 1 1 d . . . . .
H26 H 0.398397 0.267402 0.276854 0.042 Uiso 1 1 calc R . . . .
C27 C 0.5138(5) 0.1993(6) 0.3088(4) 0.0404(17) Uani 1 1 d . . . . .
C28 C 0.4651(6) 0.2112(7) 0.4398(5) 0.052(2) Uani 1 1 d . . . . .
H28A H 0.478953 0.282758 0.447274 0.078 Uiso 1 1 calc GR . . . .
H28B H 0.472412 0.179108 0.485006 0.078 Uiso 1 1 calc GR . . . .
H28C H 0.408939 0.204227 0.408251 0.078 Uiso 1 1 calc GR . . . .
C29 C 0.5064(9) 0.0113(8) 0.3872(7) 0.078(3) Uani 1 1 d . . . . .
H29A H 0.449252 0.003552 0.358503 0.117 Uiso 1 1 calc GR . . . .
H29B H 0.517341 -0.019979 0.433333 0.117 Uiso 1 1 calc GR . . . .
H29C H 0.539065 -0.021515 0.363563 0.117 Uiso 1 1 calc GR . . . .
C30 C 0.6404(6) 0.1638(9) 0.4564(5) 0.067(3) Uani 1 1 d . . . . .
H30A H 0.674475 0.133317 0.433218 0.101 Uiso 1 1 calc GR . . . .
H30B H 0.650102 0.130401 0.501604 0.101 Uiso 1 1 calc GR . . . .
H30C H 0.653151 0.235624 0.464280 0.101 Uiso 1 1 calc GR . . . .
C31 C 0.5571(5) 0.1728(5) 0.2646(4) 0.0357(16) Uani 1 1 d . . . . .
H31 H 0.609016 0.142866 0.280477 0.043 Uiso 1 1 calc R . . . .
C1 C 0.4129(8) 0.6696(10) 0.3748(7) 0.046(3) Uani 0.523(4) 1 d D U P A 1
H1A H 0.445429 0.634169 0.417845 0.069 Uiso 0.523(4) 1 calc GR . P A 1
H1B H 0.373594 0.712810 0.384775 0.069 Uiso 0.523(4) 1 calc GR . P A 1
H1C H 0.447900 0.711111 0.358126 0.069 Uiso 0.523(4) 1 calc GR . P A 1
C2 C 0.3521(17) 0.4554(12) 0.3522(10) 0.033(4) Uani 0.523(4) 1 d D U P A 1
H2A H 0.321398 0.404998 0.317946 0.049 Uiso 0.523(4) 1 calc GR . P A 1
H2B H 0.325256 0.468980 0.385724 0.049 Uiso 0.523(4) 1 calc GR . P A 1
H2C H 0.406524 0.429920 0.377651 0.049 Uiso 0.523(4) 1 calc GR . P A 1
C3 C 0.2512(9) 0.6232(17) 0.2662(13) 0.045(5) Uani 0.523(4) 1 d D U P A 1
H3A H 0.251273 0.691901 0.248633 0.067 Uiso 0.523(4) 1 calc GR . P A 1
H3B H 0.227180 0.623303 0.302653 0.067 Uiso 0.523(4) 1 calc GR . P A 1
H3C H 0.219798 0.579319 0.227374 0.067 Uiso 0.523(4) 1 calc GR . P A 1
C4 C 0.2366(9) 0.5905(11) 0.0789(10) 0.046(4) Uani 0.523(4) 1 d D U P A 1
H4A H 0.218381 0.625232 0.112983 0.069 Uiso 0.523(4) 1 calc GR . P A 1
H4B H 0.190600 0.558430 0.042860 0.069 Uiso 0.523(4) 1 calc GR . P A 1
H4C H 0.261187 0.639395 0.056609 0.069 Uiso 0.523(4) 1 calc GR . P A 1
C5 C 0.2556(8) 0.3888(10) 0.1508(8) 0.036(3) Uani 0.523(4) 1 d D U P A 1
H5A H 0.293387 0.341366 0.182868 0.055 Uiso 0.523(4) 1 calc GR . P A 1
H5B H 0.221789 0.353143 0.108360 0.055 Uiso 0.523(4) 1 calc GR . P A 1
H5C H 0.221532 0.418697 0.174266 0.055 Uiso 0.523(4) 1 calc GR . P A 1
C6 C 0.3488(15) 0.4366(13) 0.0567(11) 0.033(4) Uani 0.523(4) 1 d D U P A 1
H6A H 0.376239 0.488882 0.039688 0.049 Uiso 0.523(4) 1 calc GR . P A 1
H6B H 0.302505 0.411364 0.017269 0.049 Uiso 0.523(4) 1 calc GR . P A 1
H6C H 0.386219 0.381052 0.077015 0.049 Uiso 0.523(4) 1 calc GR . P A 1
C7 C 0.3582(9) 0.8046(13) 0.1831(9) 0.045(4) Uani 0.523(4) 1 d D U P A 1
H7A H 0.306329 0.776196 0.153358 0.067 Uiso 0.523(4) 1 calc GR . P A 1
H7B H 0.367320 0.868255 0.162710 0.067 Uiso 0.523(4) 1 calc GR . P A 1
H7C H 0.357908 0.816811 0.230446 0.067 Uiso 0.523(4) 1 calc GR . P A 1
C8 C 0.4473(9) 0.7126(12) 0.0974(6) 0.043(3) Uani 0.523(4) 1 d D U P A 1
H8A H 0.490275 0.667026 0.096639 0.064 Uiso 0.523(4) 1 calc GR . P A 1
H8B H 0.458865 0.780958 0.085393 0.064 Uiso 0.523(4) 1 calc GR . P A 1
H8C H 0.395856 0.689889 0.063037 0.064 Uiso 0.523(4) 1 calc GR . P A 1
C9 C 0.5367(8) 0.774(2) 0.2478(9) 0.043(4) Uani 0.523(4) 1 d D U P A 1
H9A H 0.539932 0.843029 0.231154 0.064 Uiso 0.523(4) 1 calc GR . P A 1
H9B H 0.583213 0.735427 0.247442 0.064 Uiso 0.523(4) 1 calc GR . P A 1
H9C H 0.536403 0.777144 0.295828 0.064 Uiso 0.523(4) 1 calc GR . P A 1
C1A C 0.5481(9) 0.769(2) 0.2658(11) 0.047(5) Uani 0.477(4) 1 d D U P A 2
H1AA H 0.591534 0.723517 0.292383 0.071 Uiso 0.477(4) 1 calc GR . P A 2
H1AB H 0.557698 0.835968 0.287988 0.071 Uiso 0.477(4) 1 calc GR . P A 2
H1AC H 0.546391 0.774774 0.217324 0.071 Uiso 0.477(4) 1 calc GR . P A 2
C2A C 0.4540(11) 0.7259(14) 0.3594(6) 0.049(4) Uani 0.477(4) 1 d D U P A 2
H2AA H 0.401236 0.745335 0.360119 0.074 Uiso 0.477(4) 1 calc GR . P A 2
H2AB H 0.494174 0.776185 0.385086 0.074 Uiso 0.477(4) 1 calc GR . P A 2
H2AC H 0.469227 0.659981 0.381967 0.074 Uiso 0.477(4) 1 calc GR . P A 2
C3A C 0.3711(11) 0.8142(16) 0.2149(10) 0.053(5) Uani 0.477(4) 1 d D U P A 2
H3AA H 0.369374 0.817946 0.166342 0.080 Uiso 0.477(4) 1 calc GR . P A 2
H3AB H 0.385100 0.880407 0.237296 0.080 Uiso 0.477(4) 1 calc GR . P A 2
H3AC H 0.318208 0.793721 0.214974 0.080 Uiso 0.477(4) 1 calc GR . P A 2
C4A C 0.2396(12) 0.6074(16) 0.2481(14) 0.040(5) Uani 0.477(4) 1 d D U P A 2
H4AA H 0.264002 0.653070 0.287864 0.060 Uiso 0.477(4) 1 calc GR . P A 2
H4AB H 0.190823 0.577487 0.251422 0.060 Uiso 0.477(4) 1 calc GR . P A 2
H4AC H 0.225765 0.645068 0.203876 0.060 Uiso 0.477(4) 1 calc GR . P A 2
C5A C 0.3440(19) 0.4476(16) 0.3406(7) 0.032(4) Uani 0.477(4) 1 d D U P A 2
H5AA H 0.379435 0.389820 0.344049 0.047 Uiso 0.477(4) 1 calc GR . P A 2
H5AB H 0.295847 0.425262 0.349236 0.047 Uiso 0.477(4) 1 calc GR . P A 2
H5AC H 0.372443 0.498211 0.375784 0.047 Uiso 0.477(4) 1 calc GR . P A 2
C6A C 0.2523(8) 0.4048(9) 0.1871(7) 0.032(3) Uani 0.477(4) 1 d D U P A 2
H6AA H 0.220635 0.436246 0.142165 0.049 Uiso 0.477(4) 1 calc GR . P A 2
H6AB H 0.216086 0.372108 0.207208 0.049 Uiso 0.477(4) 1 calc GR . P A 2
H6AC H 0.288504 0.354315 0.179457 0.049 Uiso 0.477(4) 1 calc GR . P A 2
C7A C 0.2575(7) 0.6321(13) 0.0709(11) 0.045(4) Uani 0.477(4) 1 d D U P A 2
H7AA H 0.222390 0.584406 0.082805 0.068 Uiso 0.477(4) 1 calc GR . P A 2
H7AB H 0.237566 0.642661 0.019860 0.068 Uiso 0.477(4) 1 calc GR . P A 2
H7AC H 0.257813 0.696493 0.094604 0.068 Uiso 0.477(4) 1 calc GR . P A 2
C8A C 0.3538(14) 0.4579(11) 0.0503(13) 0.030(4) Uani 0.477(4) 1 d D U P A 2
H8AA H 0.406808 0.425909 0.063515 0.045 Uiso 0.477(4) 1 calc GR . P A 2
H8AB H 0.333129 0.471993 -0.000366 0.045 Uiso 0.477(4) 1 calc GR . P A 2
H8AC H 0.316714 0.412525 0.061545 0.045 Uiso 0.477(4) 1 calc GR . P A 2
C9A C 0.4217(9) 0.6681(11) 0.0650(9) 0.046(4) Uani 0.477(4) 1 d D U P A 2
H9AA H 0.455626 0.711658 0.102947 0.069 Uiso 0.477(4) 1 calc GR . P A 2
H9AB H 0.384387 0.709578 0.027681 0.069 Uiso 0.477(4) 1 calc GR . P A 2
H9AC H 0.455767 0.628944 0.045793 0.069 Uiso 0.477(4) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 Si1 3.1530(18) . ?
Ce1 C13 2.795(8) . ?
Ce1 C14 2.778(8) . ?
Ce1 C15 2.761(7) . ?
Ce1 C16 2.760(7) . ?
Ce1 C20 2.752(7) . ?
Ce1 C24 2.796(7) . ?
Ce1 C25 2.780(7) . ?
Ce1 C26 2.778(7) . ?
Ce1 C27 2.788(8) . ?
Ce1 C31 2.765(7) . ?
Si1 Si2 2.383(4) . ?
Si1 Si3 2.370(4) . ?
Si1 Si4 2.325(4) . ?
Si1 Si2A 2.381(4) . ?
Si1 Si3A 2.311(4) . ?
Si1 Si4A 2.363(4) . ?
Si5 C10 1.859(12) . ?
Si5 C11 1.874(9) . ?
Si5 C12 1.861(11) . ?
Si5 C13 1.861(8) . ?
Si6 C16 1.865(8) . ?
Si6 C17 1.870(8) . ?
Si6 C18 1.880(8) . ?
Si6 C19 1.866(8) . ?
Si7 C21 1.870(9) . ?
Si7 C22 1.876(10) . ?
Si7 C23 1.873(9) . ?
Si7 C24 1.878(8) . ?
Si8 C27 1.871(8) . ?
Si8 C28 1.875(9) . ?
Si8 C29 1.877(11) . ?
Si8 C30 1.868(11) . ?
Si2 C1 1.883(10) . ?
Si2 C2 1.880(12) . ?
Si2 C3 1.894(11) . ?
Si3 C4 1.891(10) . ?
Si3 C5 1.882(10) . ?
Si3 C6 1.883(11) . ?
Si4 C7 1.894(11) . ?
Si4 C8 1.888(10) . ?
Si4 C9 1.880(12) . ?
Si2A C1A 1.881(12) . ?
Si2A C2A 1.885(11) . ?
Si2A C3A 1.891(12) . ?
Si3A C4A 1.890(12) . ?
Si3A C5A 1.883(11) . ?
Si3A C6A 1.888(10) . ?
Si4A C7A 1.888(11) . ?
Si4A C8A 1.894(12) . ?
Si4A C9A 1.880(10) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.430(11) . ?
C13 C20 1.429(11) . ?
C14 H14 0.9500 . ?
C14 C15 1.394(11) . ?
C15 H15 0.9500 . ?
C15 C16 1.425(11) . ?
C16 C20 1.407(10) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.424(10) . ?
C24 C31 1.409(11) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(11) . ?
C26 H26 0.9500 . ?
C26 C27 1.426(11) . ?
C27 C31 1.424(11) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Ce1 Si1 105.35(16) . . ?
C13 Ce1 C24 138.7(2) . . ?
C14 Ce1 Si1 135.00(17) . . ?
C14 Ce1 C13 29.7(2) . . ?
C14 Ce1 C24 109.0(2) . . ?
C14 Ce1 C25 134.9(2) . . ?
C14 Ce1 C26 123.9(2) . . ?
C14 Ce1 C27 94.4(2) . . ?
C15 Ce1 Si1 137.01(16) . . ?
C15 Ce1 C13 48.7(2) . . ?
C15 Ce1 C14 29.2(2) . . ?
C15 Ce1 C24 96.8(2) . . ?
C15 Ce1 C25 126.3(2) . . ?
C15 Ce1 C26 134.1(2) . . ?
C15 Ce1 C27 106.8(2) . . ?
C15 Ce1 C31 86.4(2) . . ?
C16 Ce1 Si1 107.65(17) . . ?
C16 Ce1 C13 49.5(2) . . ?
C16 Ce1 C14 49.2(2) . . ?
C16 Ce1 C15 29.9(2) . . ?
C16 Ce1 C24 113.7(2) . . ?
C16 Ce1 C25 138.6(2) . . ?
C16 Ce1 C26 161.0(2) . . ?
C16 Ce1 C27 136.6(2) . . ?
C16 Ce1 C31 113.4(2) . . ?
C20 Ce1 Si1 91.23(17) . . ?
C20 Ce1 C13 29.9(2) . . ?
C20 Ce1 C14 48.7(2) . . ?
C20 Ce1 C15 48.4(2) . . ?
C20 Ce1 C16 29.6(2) . . ?
C20 Ce1 C24 142.8(2) . . ?
C20 Ce1 C25 166.5(2) . . ?
C20 Ce1 C26 164.5(2) . . ?
C20 Ce1 C27 141.3(2) . . ?
C20 Ce1 C31 133.4(2) . . ?
C24 Ce1 Si1 115.93(16) . . ?
C25 Ce1 Si1 89.05(16) . . ?
C25 Ce1 C13 160.6(2) . . ?
C25 Ce1 C24 29.6(2) . . ?
C25 Ce1 C27 48.8(2) . . ?
C26 Ce1 Si1 88.85(16) . . ?
C26 Ce1 C13 136.1(2) . . ?
C26 Ce1 C24 48.6(2) . . ?
C26 Ce1 C25 29.0(2) . . ?
C26 Ce1 C27 29.7(2) . . ?
C27 Ce1 Si1 115.58(17) . . ?
C27 Ce1 C13 112.2(2) . . ?
C27 Ce1 C24 49.3(2) . . ?
C31 Ce1 Si1 135.36(16) . . ?
C31 Ce1 C13 114.3(2) . . ?
C31 Ce1 C14 86.9(2) . . ?
C31 Ce1 C24 29.4(2) . . ?
C31 Ce1 C25 48.1(2) . . ?
C31 Ce1 C26 48.2(2) . . ?
C31 Ce1 C27 29.7(2) . . ?
Si2 Si1 Ce1 115.25(11) . . ?
Si3 Si1 Ce1 107.84(11) . . ?
Si3 Si1 Si2 99.08(14) . . ?
Si4 Si1 Ce1 124.88(12) . . ?
Si4 Si1 Si2 103.76(15) . . ?
Si4 Si1 Si3 102.39(15) . . ?
Si2A Si1 Ce1 123.27(13) . . ?
Si3A Si1 Ce1 111.92(12) . . ?
Si3A Si1 Si2A 103.10(16) . . ?
Si3A Si1 Si4A 100.63(15) . . ?
Si4A Si1 Ce1 114.47(11) . . ?
Si4A Si1 Si2A 100.49(16) . . ?
C10 Si5 C11 110.5(5) . . ?
C10 Si5 C12 111.4(7) . . ?
C10 Si5 C13 110.4(4) . . ?
C12 Si5 C11 110.7(6) . . ?
C12 Si5 C13 107.4(4) . . ?
C13 Si5 C11 106.3(4) . . ?
C16 Si6 C17 108.8(4) . . ?
C16 Si6 C18 104.8(4) . . ?
C16 Si6 C19 111.1(4) . . ?
C17 Si6 C18 112.2(4) . . ?
C19 Si6 C17 110.2(4) . . ?
C19 Si6 C18 109.5(4) . . ?
C21 Si7 C22 109.3(5) . . ?
C21 Si7 C23 110.7(4) . . ?
C21 Si7 C24 109.9(3) . . ?
C22 Si7 C24 106.1(4) . . ?
C23 Si7 C22 108.5(5) . . ?
C23 Si7 C24 112.1(4) . . ?
C27 Si8 C28 111.1(4) . . ?
C27 Si8 C29 105.9(5) . . ?
C28 Si8 C29 108.7(5) . . ?
C30 Si8 C27 110.7(4) . . ?
C30 Si8 C28 110.8(5) . . ?
C30 Si8 C29 109.6(6) . . ?
C1 Si2 Si1 111.7(5) . . ?
C1 Si2 C3 105.0(6) . . ?
C2 Si2 Si1 112.1(10) . . ?
C2 Si2 C1 106.7(7) . . ?
C2 Si2 C3 105.2(8) . . ?
C3 Si2 Si1 115.5(9) . . ?
C4 Si3 Si1 115.2(6) . . ?
C5 Si3 Si1 112.7(5) . . ?
C5 Si3 C4 105.9(6) . . ?
C5 Si3 C6 106.6(6) . . ?
C6 Si3 Si1 110.4(8) . . ?
C6 Si3 C4 105.5(7) . . ?
C7 Si4 Si1 115.3(7) . . ?
C8 Si4 Si1 110.9(5) . . ?
C8 Si4 C7 105.3(6) . . ?
C9 Si4 Si1 113.3(8) . . ?
C9 Si4 C7 105.2(7) . . ?
C9 Si4 C8 106.2(6) . . ?
C1A Si2A Si1 112.9(9) . . ?
C1A Si2A C2A 106.1(7) . . ?
C1A Si2A C3A 105.5(8) . . ?
C2A Si2A Si1 110.5(6) . . ?
C2A Si2A C3A 105.9(7) . . ?
C3A Si2A Si1 115.2(8) . . ?
C4A Si3A Si1 116.7(10) . . ?
C5A Si3A Si1 111.6(10) . . ?
C5A Si3A C4A 105.2(8) . . ?
C5A Si3A C6A 106.1(7) . . ?
C6A Si3A Si1 111.0(5) . . ?
C6A Si3A C4A 105.3(7) . . ?
C7A Si4A Si1 115.4(7) . . ?
C7A Si4A C8A 104.9(7) . . ?
C8A Si4A Si1 110.3(8) . . ?
C9A Si4A Si1 113.6(6) . . ?
C9A Si4A C7A 105.9(6) . . ?
C9A Si4A C8A 106.0(7) . . ?
Si5 C10 H10A 109.5 . . ?
Si5 C10 H10B 109.5 . . ?
Si5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si5 C11 H11A 109.5 . . ?
Si5 C11 H11B 109.5 . . ?
Si5 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si5 C12 H12A 109.5 . . ?
Si5 C12 H12B 109.5 . . ?
Si5 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si5 C13 Ce1 115.9(3) . . ?
C14 C13 Ce1 74.5(4) . . ?
C14 C13 Si5 126.0(6) . . ?
C20 C13 Ce1 73.4(4) . . ?
C20 C13 Si5 128.1(6) . . ?
C20 C13 C14 105.9(7) . . ?
Ce1 C14 H14 115.7 . . ?
C13 C14 Ce1 75.8(4) . . ?
C13 C14 H14 125.8 . . ?
C15 C14 Ce1 74.7(4) . . ?
C15 C14 C13 108.4(7) . . ?
C15 C14 H14 125.8 . . ?
Ce1 C15 H15 115.7 . . ?
C14 C15 Ce1 76.1(4) . . ?
C14 C15 H15 125.1 . . ?
C14 C15 C16 109.7(7) . . ?
C16 C15 Ce1 75.0(4) . . ?
C16 C15 H15 125.1 . . ?
Si6 C16 Ce1 110.4(3) . . ?
C15 C16 Ce1 75.1(4) . . ?
C15 C16 Si6 125.2(6) . . ?
C20 C16 Ce1 74.9(4) . . ?
C20 C16 Si6 128.6(6) . . ?
C20 C16 C15 105.9(7) . . ?
Si6 C17 H17A 109.5 . . ?
Si6 C17 H17B 109.5 . . ?
Si6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si6 C18 H18A 109.5 . . ?
Si6 C18 H18B 109.5 . . ?
Si6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si6 C19 H19A 109.5 . . ?
Si6 C19 H19B 109.5 . . ?
Si6 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Ce1 C20 H20 114.7 . . ?
C13 C20 Ce1 76.8(4) . . ?
C13 C20 H20 124.9 . . ?
C16 C20 Ce1 75.5(4) . . ?
C16 C20 C13 110.1(7) . . ?
C16 C20 H20 124.9 . . ?
Si7 C21 H21A 109.5 . . ?
Si7 C21 H21B 109.5 . . ?
Si7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si7 C22 H22A 109.5 . . ?
Si7 C22 H22B 109.5 . . ?
Si7 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si7 C23 H23A 109.5 . . ?
Si7 C23 H23B 109.5 . . ?
Si7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si7 C24 Ce1 132.2(3) . . ?
C25 C24 Ce1 74.6(4) . . ?
C25 C24 Si7 125.4(6) . . ?
C31 C24 Ce1 74.1(4) . . ?
C31 C24 Si7 125.6(5) . . ?
C31 C24 C25 105.9(6) . . ?
Ce1 C25 H25 115.3 . . ?
C24 C25 Ce1 75.8(4) . . ?
C24 C25 H25 125.5 . . ?
C26 C25 Ce1 75.4(4) . . ?
C26 C25 C24 109.1(7) . . ?
C26 C25 H25 125.5 . . ?
Ce1 C26 H26 115.6 . . ?
C25 C26 Ce1 75.5(4) . . ?
C25 C26 H26 125.4 . . ?
C25 C26 C27 109.3(7) . . ?
C27 C26 Ce1 75.5(4) . . ?
C27 C26 H26 125.4 . . ?
Si8 C27 Ce1 131.4(4) . . ?
C26 C27 Ce1 74.8(4) . . ?
C26 C27 Si8 125.7(6) . . ?
C31 C27 Ce1 74.3(4) . . ?
C31 C27 Si8 126.0(6) . . ?
C31 C27 C26 105.2(7) . . ?
Si8 C28 H28A 109.5 . . ?
Si8 C28 H28B 109.5 . . ?
Si8 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Ce1 C31 H31 114.6 . . ?
C24 C31 Ce1 76.5(4) . . ?
C24 C31 C27 110.6(7) . . ?
C24 C31 H31 124.7 . . ?
C27 C31 Ce1 76.0(4) . . ?
C27 C31 H31 124.7 . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2A C1A H1AA 109.5 . . ?
Si2A C1A H1AB 109.5 . . ?
Si2A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
Si2A C2A H2AA 109.5 . . ?
Si2A C2A H2AB 109.5 . . ?
Si2A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
Si2A C3A H3AA 109.5 . . ?
Si2A C3A H3AB 109.5 . . ?
Si2A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
Si3A C4A H4AA 109.5 . . ?
Si3A C4A H4AB 109.5 . . ?
Si3A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
Si3A C5A H5AA 109.5 . . ?
Si3A C5A H5AB 109.5 . . ?
Si3A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
Si3A C6A H6AA 109.5 . . ?
Si3A C6A H6AB 109.5 . . ?
Si3A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
Si4A C7A H7AA 109.5 . . ?
Si4A C7A H7AB 109.5 . . ?
Si4A C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
Si4A C8A H8AA 109.5 . . ?
Si4A C8A H8AB 109.5 . . ?
Si4A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
Si4A C9A H9AA 109.5 . . ?
Si4A C9A H9AB 109.5 . . ?
Si4A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce1 C13 C14 C15 68.3(6) . . . . ?
Ce1 C13 C20 C16 -68.9(5) . . . . ?
Ce1 C14 C15 C16 68.2(5) . . . . ?
Ce1 C15 C16 Si6 -104.7(5) . . . . ?
Ce1 C15 C16 C20 69.1(5) . . . . ?
Ce1 C16 C20 C13 69.7(5) . . . . ?
Ce1 C24 C25 C26 -68.8(5) . . . . ?
Ce1 C24 C31 C27 69.2(5) . . . . ?
Ce1 C25 C26 C27 -68.7(5) . . . . ?
Ce1 C26 C27 Si8 130.5(6) . . . . ?
Ce1 C26 C27 C31 -68.6(5) . . . . ?
Ce1 C27 C31 C24 -69.5(5) . . . . ?
Si5 C13 C14 Ce1 111.1(6) . . . . ?
Si5 C13 C14 C15 179.4(6) . . . . ?
Si5 C13 C20 Ce1 -110.3(6) . . . . ?
Si5 C13 C20 C16 -179.2(6) . . . . ?
Si6 C16 C20 Ce1 104.3(6) . . . . ?
Si6 C16 C20 C13 174.0(5) . . . . ?
Si7 C24 C25 Ce1 -131.3(5) . . . . ?
Si7 C24 C25 C26 159.9(5) . . . . ?
Si7 C24 C31 Ce1 131.0(6) . . . . ?
Si7 C24 C31 C27 -159.8(6) . . . . ?
Si8 C27 C31 Ce1 -130.2(6) . . . . ?
Si8 C27 C31 C24 160.3(6) . . . . ?
C10 Si5 C13 Ce1 -111.9(5) . . . . ?
C10 Si5 C13 C14 158.9(7) . . . . ?
C10 Si5 C13 C20 -23.2(9) . . . . ?
C11 Si5 C13 Ce1 7.9(5) . . . . ?
C11 Si5 C13 C14 -81.2(7) . . . . ?
C11 Si5 C13 C20 96.6(7) . . . . ?
C12 Si5 C13 Ce1 126.5(6) . . . . ?
C12 Si5 C13 C14 37.3(9) . . . . ?
C12 Si5 C13 C20 -144.8(8) . . . . ?
C13 C14 C15 Ce1 -69.0(5) . . . . ?
C13 C14 C15 C16 -0.8(9) . . . . ?
C14 C13 C20 Ce1 67.9(5) . . . . ?
C14 C13 C20 C16 -1.0(8) . . . . ?
C14 C15 C16 Ce1 -68.9(6) . . . . ?
C14 C15 C16 Si6 -173.6(6) . . . . ?
C14 C15 C16 C20 0.2(9) . . . . ?
C15 C16 C20 Ce1 -69.2(5) . . . . ?
C15 C16 C20 C13 0.5(8) . . . . ?
C17 Si6 C16 Ce1 -123.7(4) . . . . ?
C17 Si6 C16 C15 -37.9(7) . . . . ?
C17 Si6 C16 C20 149.7(7) . . . . ?
C18 Si6 C16 Ce1 -3.4(4) . . . . ?
C18 Si6 C16 C15 82.4(7) . . . . ?
C18 Si6 C16 C20 -90.0(7) . . . . ?
C19 Si6 C16 Ce1 114.8(4) . . . . ?
C19 Si6 C16 C15 -159.4(6) . . . . ?
C19 Si6 C16 C20 28.2(8) . . . . ?
C20 C13 C14 Ce1 -67.2(5) . . . . ?
C20 C13 C14 C15 1.1(9) . . . . ?
C21 Si7 C24 Ce1 -77.7(5) . . . . ?
C21 Si7 C24 C25 24.1(7) . . . . ?
C21 Si7 C24 C31 -179.0(6) . . . . ?
C22 Si7 C24 Ce1 164.2(5) . . . . ?
C22 Si7 C24 C25 -94.0(8) . . . . ?
C22 Si7 C24 C31 62.9(8) . . . . ?
C23 Si7 C24 Ce1 45.9(6) . . . . ?
C23 Si7 C24 C25 147.7(7) . . . . ?
C23 Si7 C24 C31 -55.4(8) . . . . ?
C24 C25 C26 Ce1 69.1(5) . . . . ?
C24 C25 C26 C27 0.4(9) . . . . ?
C25 C24 C31 Ce1 -68.4(5) . . . . ?
C25 C24 C31 C27 0.8(8) . . . . ?
C25 C26 C27 Ce1 68.7(5) . . . . ?
C25 C26 C27 Si8 -160.9(6) . . . . ?
C25 C26 C27 C31 0.1(8) . . . . ?
C26 C27 C31 Ce1 69.0(5) . . . . ?
C26 C27 C31 C24 -0.6(8) . . . . ?
C28 Si8 C27 Ce1 75.2(6) . . . . ?
C28 Si8 C27 C26 -26.5(8) . . . . ?
C28 Si8 C27 C31 176.4(7) . . . . ?
C29 Si8 C27 Ce1 -167.0(6) . . . . ?
C29 Si8 C27 C26 91.3(8) . . . . ?
C29 Si8 C27 C31 -65.8(9) . . . . ?
C30 Si8 C27 Ce1 -48.3(7) . . . . ?
C30 Si8 C27 C26 -150.0(7) . . . . ?
C30 Si8 C27 C31 52.9(9) . . . . ?
C31 C24 C25 Ce1 68.1(5) . . . . ?
C31 C24 C25 C26 -0.7(8) . . . . ?

_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 1s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_type   custom
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.598
_oxdiff_exptl_absorpt_empirical_full_min 0.520
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.648(3)
2 0.352(3)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-Zr
_database_code_depnum_ccdc_archive 'CCDC 2195636'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   ldpm172
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   27/11/2020
_manchester_internal_process_date 27/11/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 09/12/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 09/12/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 15/12/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 15/12/2020
_manchester_internal_archive_user AW
_audit_author_email              
;
benjamin.reant@postgrad.manchester.ac.uk, david.mills@manchester.ac.uk    
;
_refine_special_details          -
_audit_creation_date             2020-12-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        "[Zr(Cp'')2{Si(SiMe3)3}]"
_chemical_formula_moiety         'C31 H69 Si8 Zr'
_chemical_formula_sum            'C31 H69 Si8 Zr'
_chemical_formula_weight         757.80
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Zr1 Si8 C31'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_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'

_cell_length_a                   37.0378(4)
_cell_length_b                   11.77080(10)
_cell_length_c                   20.1996(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8806.31(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    22918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.3430
_cell_measurement_theta_min      3.9210
_shelx_estimated_absorpt_T_max   0.769
_shelx_estimated_absorpt_T_min   0.417
_exptl_absorpt_coefficient_mu    4.260
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3256
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-23 2 0 0.0324
23 -2 0 0.0324
1 0 -13 0.1225
-1 0 13 0.1225
-6 -7 0 0.0576
6 7 0 0.0486

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 
'Crystallised from concentrated pentane solution at -25 oC'
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.065
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-23.0296 1.9912 -0.0054 0.9325 -0.3393 0.0078
23.0296 -1.9912 0.0054 -0.9325 0.3393 -0.0078
1.0395 0.0010 -12.9772 -0.0277 0.0183 -0.9900
-1.0395 -0.0010 12.9772 0.0277 -0.0183 0.9900
-5.9533 -7.0026 -0.0140 0.3230 0.8930 0.0166
5.9533 7.0026 0.0140 -0.3230 -0.8930 -0.0166

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57189
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.347
_diffrn_reflns_theta_min         2.386
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     54.00  81.00   1.00    1.00    --   44.70  60.00-120.00   27
  2  ω     89.00 134.00   1.00    1.00    --   44.70  60.00  90.00   45
  3  ω    -44.00  65.00   1.00    1.00    --   44.70  60.00 -60.00  109
  4  ω     63.00 125.00   1.00    1.00    --   44.70  30.00 -60.00   62
  5  ω    -45.00  53.00   1.00    1.00    --   44.70  60.00-120.00   98
  6  ω    -11.00  16.00   1.00    1.00    --   44.70  60.00  90.00   27
  7  ω     82.00 131.00   1.00    1.00    --  108.20  50.00  30.00   49
  8  ω     83.00 197.00   1.00    1.00    --  108.20  50.00 -90.00  114
  9  ω     26.00  52.00   1.00    1.00    --  108.20  50.00  60.00   26
 10  ω     62.00 197.00   1.00    1.00    --  108.20  50.00 -30.00  135
 11  ω     19.00 198.00   1.00    1.00    --  108.20   0.00-150.00  179
 12  ω    133.00 198.00   1.00    1.00    --  108.20  50.00  30.00   65
 13  ω    112.00 156.00   1.00    1.00    --  108.20  50.00 -60.00   44
 14  ω    103.00 162.00   1.00    1.00    --  108.20  50.00  60.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0414330000
_diffrn_orient_matrix_UB_12      -0.0109002000
_diffrn_orient_matrix_UB_13      -0.0011861000
_diffrn_orient_matrix_UB_21      0.0034517000
_diffrn_orient_matrix_UB_22      -0.1304616000
_diffrn_orient_matrix_UB_23      -0.0011430000
_diffrn_orient_matrix_UB_31      -0.0005339000
_diffrn_orient_matrix_UB_32      -0.0020679000
_diffrn_orient_matrix_UB_33      0.0762453000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.593
_reflns_Friedel_fraction_full    0.659
_reflns_Friedel_fraction_max     0.604
_reflns_number_gt                13759
_reflns_number_total             14550
_reflns_odcompleteness_completeness 97.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.684
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.480(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         14550
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0560P)²+11.3200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1045
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.52
 0.48
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C20(H20), C21(H21), C26(H26), C27(H27), C45(H45),
 C46(H46), C51(H51), C52(H52), C57(H57), C58(H58)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.24680(2) 0.75353(4) 0.61050(3) 0.02045(10) Uani 1 1 d . . . . .
Si1 Si 0.25103(4) 0.88212(12) 0.73281(9) 0.0234(3) Uani 1 1 d . . . . .
Si2 Si 0.30125(5) 1.00823(14) 0.73534(10) 0.0343(4) Uani 1 1 d . . . . .
Si3 Si 0.26254(5) 0.77209(15) 0.82793(10) 0.0364(4) Uani 1 1 d . . . . .
Si4 Si 0.20477(5) 1.00014(14) 0.77470(10) 0.0354(4) Uani 1 1 d . . . . .
Si5 Si 0.30683(4) 0.87284(13) 0.45766(9) 0.0281(3) Uani 1 1 d . . . . .
Si6 Si 0.29974(4) 0.45182(13) 0.60297(9) 0.0285(3) Uani 1 1 d . . . . .
Si7 Si 0.17112(4) 0.53609(13) 0.67242(8) 0.0275(3) Uani 1 1 d . . . . .
Si8 Si 0.17717(4) 0.97096(13) 0.53061(8) 0.0268(3) Uani 1 1 d . . . . .
C1 C 0.3014(2) 1.1185(6) 0.8034(4) 0.0432(17) Uani 1 1 d . . . . .
H1A H 0.280336 1.168237 0.798450 0.065 Uiso 1 1 calc GR . . . .
H1B H 0.323506 1.163858 0.800581 0.065 Uiso 1 1 calc GR . . . .
H1C H 0.300354 1.080493 0.846566 0.065 Uiso 1 1 calc GR . . . .
C2 C 0.30110(18) 1.0946(5) 0.6563(3) 0.0349(14) Uani 1 1 d . . . . .
H2A H 0.297725 1.043881 0.618350 0.052 Uiso 1 1 calc GR . . . .
H2B H 0.324165 1.134703 0.651897 0.052 Uiso 1 1 calc GR . . . .
H2C H 0.281350 1.149925 0.657805 0.052 Uiso 1 1 calc GR . . . .
C3 C 0.34586(17) 0.9284(6) 0.7432(4) 0.0418(16) Uani 1 1 d . . . . .
H3A H 0.347582 0.894343 0.787334 0.063 Uiso 1 1 calc GR . . . .
H3B H 0.365958 0.981362 0.736636 0.063 Uiso 1 1 calc GR . . . .
H3C H 0.346958 0.868434 0.709568 0.063 Uiso 1 1 calc GR . . . .
C4 C 0.28885(19) 0.8488(6) 0.8954(4) 0.0439(16) Uani 1 1 d . . . . .
H4A H 0.312545 0.871309 0.878274 0.066 Uiso 1 1 calc GR . . . .
H4B H 0.292046 0.798043 0.933421 0.066 Uiso 1 1 calc GR . . . .
H4C H 0.275496 0.916630 0.909327 0.066 Uiso 1 1 calc GR . . . .
C5 C 0.2905(2) 0.6449(6) 0.8099(4) 0.0466(18) Uani 1 1 d . . . . .
H5A H 0.279305 0.601125 0.774106 0.070 Uiso 1 1 calc GR . . . .
H5B H 0.292146 0.597545 0.849723 0.070 Uiso 1 1 calc GR . . . .
H5C H 0.314731 0.668843 0.796472 0.070 Uiso 1 1 calc GR . . . .
C6 C 0.21919(19) 0.7182(6) 0.8664(4) 0.0477(18) Uani 1 1 d . . . . .
H6A H 0.201651 0.780399 0.868974 0.072 Uiso 1 1 calc GR . . . .
H6B H 0.224172 0.689618 0.911081 0.072 Uiso 1 1 calc GR . . . .
H6C H 0.209307 0.656731 0.839202 0.072 Uiso 1 1 calc GR . . . .
C7 C 0.21247(19) 1.0356(6) 0.8649(3) 0.0425(16) Uani 1 1 d . . . . .
H7A H 0.212824 0.965362 0.890996 0.064 Uiso 1 1 calc GR . . . .
H7B H 0.192941 1.084785 0.880767 0.064 Uiso 1 1 calc GR . . . .
H7C H 0.235622 1.074996 0.869833 0.064 Uiso 1 1 calc GR . . . .
C8 C 0.15806(16) 0.9348(6) 0.7758(4) 0.0376(14) Uani 1 1 d . . . . .
H8A H 0.149621 0.923936 0.730259 0.056 Uiso 1 1 calc GR . . . .
H8B H 0.141416 0.985477 0.799283 0.056 Uiso 1 1 calc GR . . . .
H8C H 0.158957 0.861235 0.798440 0.056 Uiso 1 1 calc GR . . . .
C9 C 0.2017(2) 1.1404(6) 0.7293(4) 0.0469(17) Uani 1 1 d . . . . .
H9A H 0.225062 1.179455 0.731711 0.070 Uiso 1 1 calc GR . . . .
H9B H 0.183095 1.187797 0.749929 0.070 Uiso 1 1 calc GR . . . .
H9C H 0.195456 1.126631 0.682902 0.070 Uiso 1 1 calc GR . . . .
C10 C 0.32263(17) 1.0166(5) 0.4839(3) 0.0358(14) Uani 1 1 d . . . . .
H10A H 0.332403 1.057208 0.445476 0.054 Uiso 1 1 calc GR . . . .
H10B H 0.341485 1.008636 0.517575 0.054 Uiso 1 1 calc GR . . . .
H10C H 0.302291 1.059486 0.502277 0.054 Uiso 1 1 calc GR . . . .
C11 C 0.26610(16) 0.8819(5) 0.4033(3) 0.0348(14) Uani 1 1 d . . . . .
H11A H 0.246051 0.915443 0.428218 0.052 Uiso 1 1 calc GR . . . .
H11B H 0.259347 0.805489 0.388505 0.052 Uiso 1 1 calc GR . . . .
H11C H 0.271540 0.929396 0.364764 0.052 Uiso 1 1 calc GR . . . .
C12 C 0.34467(15) 0.8072(6) 0.4087(3) 0.0383(15) Uani 1 1 d . . . . .
H12A H 0.353999 0.862708 0.376891 0.057 Uiso 1 1 calc GR . . . .
H12B H 0.335645 0.740399 0.384922 0.057 Uiso 1 1 calc GR . . . .
H12C H 0.364069 0.784166 0.438867 0.057 Uiso 1 1 calc GR . . . .
C13 C 0.29839(14) 0.7815(5) 0.5319(3) 0.0230(11) Uani 1 1 d . . . . .
C14 C 0.31301(14) 0.7976(5) 0.5969(3) 0.0254(12) Uani 1 1 d . . . . .
H14 H 0.322608 0.866934 0.613368 0.030 Uiso 1 1 calc R . . . .
C15 C 0.31104(13) 0.6960(4) 0.6325(3) 0.0229(11) Uani 1 1 d . . . . .
H15 H 0.319175 0.685540 0.676714 0.027 Uiso 1 1 calc R . . . .
C16 C 0.29506(15) 0.6110(5) 0.5926(3) 0.0264(12) Uani 1 1 d . . . . .
C17 C 0.30716(18) 0.4120(5) 0.6907(4) 0.0386(15) Uani 1 1 d . . . . .
H17A H 0.324573 0.464426 0.710783 0.058 Uiso 1 1 calc GR . . . .
H17B H 0.316594 0.334331 0.693017 0.058 Uiso 1 1 calc GR . . . .
H17C H 0.284227 0.416257 0.714826 0.058 Uiso 1 1 calc GR . . . .
C18 C 0.26083(19) 0.3739(5) 0.5653(4) 0.0363(15) Uani 1 1 d . . . . .
H18A H 0.238821 0.390407 0.590484 0.054 Uiso 1 1 calc GR . . . .
H18B H 0.265622 0.292041 0.566480 0.054 Uiso 1 1 calc GR . . . .
H18C H 0.257666 0.398410 0.519343 0.054 Uiso 1 1 calc GR . . . .
C19 C 0.34026(19) 0.4110(6) 0.5542(5) 0.052(2) Uani 1 1 d . . . . .
H19A H 0.336735 0.432278 0.507795 0.078 Uiso 1 1 calc GR . . . .
H19B H 0.343919 0.328680 0.557381 0.078 Uiso 1 1 calc GR . . . .
H19C H 0.361494 0.450372 0.571863 0.078 Uiso 1 1 calc GR . . . .
C20 C 0.28803(14) 0.6638(5) 0.5305(3) 0.0259(12) Uani 1 1 d . . . . .
H20 H 0.277876 0.626344 0.493229 0.031 Uiso 1 1 calc R . . . .
C21 C 0.18084(14) 0.7689(4) 0.6189(3) 0.0222(11) Uani 1 1 d . . . . .
H21 H 0.171279 0.806734 0.656553 0.027 Uiso 1 1 calc R . . . .
C22 C 0.18781(13) 0.6495(5) 0.6154(3) 0.0249(11) Uani 1 1 d . . . . .
C23 C 0.13538(17) 0.5979(6) 0.7264(3) 0.0382(14) Uani 1 1 d . . . . .
H23A H 0.146073 0.655409 0.755492 0.057 Uiso 1 1 calc GR . . . .
H23B H 0.124545 0.537585 0.753361 0.057 Uiso 1 1 calc GR . . . .
H23C H 0.116713 0.633099 0.698839 0.057 Uiso 1 1 calc GR . . . .
C24 C 0.15275(17) 0.4190(5) 0.6192(4) 0.0381(15) Uani 1 1 d . . . . .
H24A H 0.132166 0.447423 0.593645 0.057 Uiso 1 1 calc GR . . . .
H24B H 0.144873 0.355842 0.647365 0.057 Uiso 1 1 calc GR . . . .
H24C H 0.171607 0.392505 0.588907 0.057 Uiso 1 1 calc GR . . . .
C25 C 0.20669(18) 0.4761(6) 0.7269(3) 0.0393(15) Uani 1 1 d . . . . .
H25A H 0.225478 0.440602 0.699718 0.059 Uiso 1 1 calc GR . . . .
H25B H 0.196010 0.418908 0.756265 0.059 Uiso 1 1 calc GR . . . .
H25C H 0.217366 0.537008 0.753565 0.059 Uiso 1 1 calc GR . . . .
C26 C 0.20156(15) 0.6313(5) 0.5506(3) 0.0264(12) Uani 1 1 d . . . . .
H26 H 0.208931 0.560126 0.533010 0.032 Uiso 1 1 calc R . . . .
C27 C 0.20253(14) 0.7368(5) 0.5161(3) 0.0243(12) Uani 1 1 d . . . . .
H27 H 0.210319 0.746632 0.471673 0.029 Uiso 1 1 calc R . . . .
C28 C 0.19025(14) 0.8239(5) 0.5578(3) 0.0260(12) Uani 1 1 d . . . . .
C29 C 0.13905(18) 1.0213(6) 0.5826(4) 0.0419(16) Uani 1 1 d . . . . .
H29A H 0.118302 0.970623 0.576699 0.063 Uiso 1 1 calc GR . . . .
H29B H 0.132371 1.098551 0.569340 0.063 Uiso 1 1 calc GR . . . .
H29C H 0.146364 1.021214 0.629235 0.063 Uiso 1 1 calc GR . . . .
C30 C 0.16071(17) 0.9598(6) 0.4435(3) 0.0375(14) Uani 1 1 d . . . . .
H30A H 0.179471 0.925076 0.415895 0.056 Uiso 1 1 calc GR . . . .
H30B H 0.155111 1.035864 0.426565 0.056 Uiso 1 1 calc GR . . . .
H30C H 0.138903 0.912722 0.442200 0.056 Uiso 1 1 calc GR . . . .
C31 C 0.21518(18) 1.0739(5) 0.5358(4) 0.0382(15) Uani 1 1 d . . . . .
H31A H 0.226902 1.067152 0.579143 0.057 Uiso 1 1 calc GR . . . .
H31B H 0.205908 1.151239 0.530214 0.057 Uiso 1 1 calc GR . . . .
H31C H 0.232763 1.057401 0.500855 0.057 Uiso 1 1 calc GR . . . .
Zr2 Zr 0.00218(2) 0.88096(3) 0.38942(3) 0.02088(10) Uani 1 1 d . . . . .
Si9 Si 0.00034(4) 0.76361(13) 0.26299(9) 0.0237(3) Uani 1 1 d . . . . .
Si10 Si 0.04885(4) 0.75639(13) 0.18704(8) 0.0271(3) Uani 1 1 d . . . . .
Si11 Si -0.04739(4) 0.82352(13) 0.19334(8) 0.0263(3) Uani 1 1 d . . . . .
Si12 Si -0.01294(4) 0.56771(13) 0.27258(8) 0.0286(3) Uani 1 1 d . . . . .
Si13 Si 0.07313(4) 0.66615(13) 0.47236(9) 0.0301(3) Uani 1 1 d . . . . .
Si14 Si 0.07499(4) 1.10017(13) 0.32789(8) 0.0269(3) Uani 1 1 d . . . . .
Si15 Si -0.05323(4) 1.17829(12) 0.39919(8) 0.0257(3) Uani 1 1 d . . . . .
Si16 Si -0.05684(4) 0.75063(12) 0.53946(8) 0.0256(3) Uani 1 1 d . . . . .
C32 C 0.09493(17) 0.7253(6) 0.2237(4) 0.0383(15) Uani 1 1 d . . . . .
H32A H 0.101894 0.787140 0.253519 0.057 Uiso 1 1 calc GR . . . .
H32B H 0.112729 0.718790 0.187977 0.057 Uiso 1 1 calc GR . . . .
H32C H 0.093985 0.653760 0.248472 0.057 Uiso 1 1 calc GR . . . .
C33 C 0.05252(17) 0.8942(5) 0.1395(3) 0.0350(14) Uani 1 1 d . . . . .
H33A H 0.029789 0.908851 0.116210 0.052 Uiso 1 1 calc GR . . . .
H33B H 0.072244 0.888663 0.107350 0.052 Uiso 1 1 calc GR . . . .
H33C H 0.057431 0.956569 0.170383 0.052 Uiso 1 1 calc GR . . . .
C34 C 0.04403(19) 0.6427(5) 0.1215(3) 0.0396(15) Uani 1 1 d . . . . .
H34A H 0.048761 0.568103 0.141209 0.059 Uiso 1 1 calc GR . . . .
H34B H 0.061374 0.656835 0.085817 0.059 Uiso 1 1 calc GR . . . .
H34C H 0.019453 0.644310 0.103568 0.059 Uiso 1 1 calc GR . . . .
C35 C -0.04685(16) 0.9824(5) 0.1837(3) 0.0326(13) Uani 1 1 d . . . . .
H35A H -0.044219 1.018040 0.227266 0.049 Uiso 1 1 calc GR . . . .
H35B H -0.069516 1.007437 0.163334 0.049 Uiso 1 1 calc GR . . . .
H35C H -0.026534 1.004582 0.155407 0.049 Uiso 1 1 calc GR . . . .
C36 C -0.09286(16) 0.7791(5) 0.2270(3) 0.0300(12) Uani 1 1 d . . . . .
H36A H -0.094545 0.696048 0.227064 0.045 Uiso 1 1 calc GR . . . .
H36B H -0.112016 0.810708 0.199025 0.045 Uiso 1 1 calc GR . . . .
H36C H -0.095596 0.807634 0.272285 0.045 Uiso 1 1 calc GR . . . .
C37 C -0.04672(17) 0.7678(6) 0.1057(3) 0.0372(14) Uani 1 1 d . . . . .
H37A H -0.025505 0.797771 0.082497 0.056 Uiso 1 1 calc GR . . . .
H37B H -0.068677 0.792217 0.082597 0.056 Uiso 1 1 calc GR . . . .
H37C H -0.045641 0.684669 0.106367 0.056 Uiso 1 1 calc GR . . . .
C38 C -0.03424(18) 0.4997(5) 0.1973(3) 0.0371(14) Uani 1 1 d . . . . .
H38A H -0.057575 0.535809 0.188308 0.056 Uiso 1 1 calc GR . . . .
H38B H -0.037882 0.418473 0.205569 0.056 Uiso 1 1 calc GR . . . .
H38C H -0.018306 0.509597 0.158999 0.056 Uiso 1 1 calc GR . . . .
C39 C -0.04646(18) 0.5436(5) 0.3410(3) 0.0361(14) Uani 1 1 d . . . . .
H39A H -0.037650 0.579199 0.381792 0.054 Uiso 1 1 calc GR . . . .
H39B H -0.049475 0.461776 0.348258 0.054 Uiso 1 1 calc GR . . . .
H39C H -0.069730 0.577102 0.328733 0.054 Uiso 1 1 calc GR . . . .
C40 C 0.02920(19) 0.4834(5) 0.2911(4) 0.0409(15) Uani 1 1 d . . . . .
H40A H 0.044215 0.479100 0.251274 0.061 Uiso 1 1 calc GR . . . .
H40B H 0.022491 0.406517 0.305136 0.061 Uiso 1 1 calc GR . . . .
H40C H 0.042764 0.520771 0.326640 0.061 Uiso 1 1 calc GR . . . .
C41 C 0.11033(18) 0.6169(6) 0.4172(4) 0.0451(17) Uani 1 1 d . . . . .
H41A H 0.117738 0.540148 0.430264 0.068 Uiso 1 1 calc GR . . . .
H41B H 0.130937 0.668672 0.421212 0.068 Uiso 1 1 calc GR . . . .
H41C H 0.101878 0.615950 0.371273 0.068 Uiso 1 1 calc GR . . . .
C42 C 0.03613(17) 0.5575(5) 0.4733(4) 0.0389(15) Uani 1 1 d . . . . .
H42A H 0.024563 0.554757 0.429647 0.058 Uiso 1 1 calc GR . . . .
H42B H 0.018184 0.578119 0.506813 0.058 Uiso 1 1 calc GR . . . .
H42C H 0.046303 0.482772 0.483760 0.058 Uiso 1 1 calc GR . . . .
C43 C 0.09039(19) 0.6840(6) 0.5584(4) 0.0449(17) Uani 1 1 d . . . . .
H43A H 0.095340 0.609149 0.577665 0.067 Uiso 1 1 calc GR . . . .
H43B H 0.072236 0.723304 0.585228 0.067 Uiso 1 1 calc GR . . . .
H43C H 0.112685 0.728792 0.557553 0.067 Uiso 1 1 calc GR . . . .
C44 C 0.05865(14) 0.8121(5) 0.4436(3) 0.0265(12) Uani 1 1 d . . . . .
C45 C 0.04517(15) 0.8994(5) 0.4854(3) 0.0285(13) Uani 1 1 d . . . . .
H45 H 0.036827 0.889104 0.529461 0.034 Uiso 1 1 calc R . . . .
C46 C 0.04612(14) 1.0032(5) 0.4513(3) 0.0270(12) Uani 1 1 d . . . . .
H46 H 0.038338 1.074160 0.468644 0.032 Uiso 1 1 calc R . . . .
C47 C 0.06055(13) 0.9858(4) 0.3868(3) 0.0254(11) Uani 1 1 d . . . . .
C48 C 0.09145(18) 1.2239(5) 0.3778(4) 0.0386(15) Uani 1 1 d . . . . .
H48A H 0.072247 1.249330 0.407730 0.058 Uiso 1 1 calc GR . . . .
H48B H 0.098165 1.286119 0.348075 0.058 Uiso 1 1 calc GR . . . .
H48C H 0.112557 1.200829 0.403845 0.058 Uiso 1 1 calc GR . . . .
C49 C 0.03761(15) 1.1471(5) 0.2725(3) 0.0356(14) Uani 1 1 d . . . . .
H49A H 0.026975 1.080752 0.250616 0.053 Uiso 1 1 calc GR . . . .
H49B H 0.047133 1.199342 0.238997 0.053 Uiso 1 1 calc GR . . . .
H49C H 0.019083 1.185855 0.298744 0.053 Uiso 1 1 calc GR . . . .
C50 C 0.11235(15) 1.0442(5) 0.2759(3) 0.0329(13) Uani 1 1 d . . . . .
H50A H 0.131781 1.016175 0.304506 0.049 Uiso 1 1 calc GR . . . .
H50B H 0.121635 1.105029 0.247499 0.049 Uiso 1 1 calc GR . . . .
H50C H 0.103337 0.981872 0.248318 0.049 Uiso 1 1 calc GR . . . .
C51 C 0.06804(14) 0.8664(4) 0.3837(3) 0.0255(11) Uani 1 1 d . . . . .
H51 H 0.078010 0.828792 0.346357 0.031 Uiso 1 1 calc R . . . .
C52 C -0.03996(14) 0.9630(4) 0.4698(3) 0.0235(11) Uani 1 1 d . . . . .
H52 H -0.029897 0.998323 0.507814 0.028 Uiso 1 1 calc R . . . .
C53 C -0.04759(14) 1.0205(5) 0.4102(3) 0.0245(11) Uani 1 1 d . . . . .
C54 C -0.01394(17) 1.2582(5) 0.4338(3) 0.0321(14) Uani 1 1 d . . . . .
H54A H -0.008207 1.228994 0.478029 0.048 Uiso 1 1 calc GR . . . .
H54B H -0.020011 1.339042 0.436848 0.048 Uiso 1 1 calc GR . . . .
H54C H 0.007018 1.248392 0.404751 0.048 Uiso 1 1 calc GR . . . .
C55 C -0.09432(17) 1.2213(5) 0.4471(4) 0.0384(15) Uani 1 1 d . . . . .
H55A H -0.115453 1.180992 0.429667 0.058 Uiso 1 1 calc GR . . . .
H55B H -0.098015 1.303358 0.442703 0.058 Uiso 1 1 calc GR . . . .
H55C H -0.091011 1.201898 0.493852 0.058 Uiso 1 1 calc GR . . . .
C56 C -0.06221(17) 1.2122(5) 0.3106(3) 0.0327(13) Uani 1 1 d . . . . .
H56A H -0.040532 1.196530 0.284319 0.049 Uiso 1 1 calc GR . . . .
H56B H -0.068593 1.292722 0.306400 0.049 Uiso 1 1 calc GR . . . .
H56C H -0.082222 1.165341 0.294466 0.049 Uiso 1 1 calc GR . . . .
C57 C -0.06249(14) 0.9366(5) 0.3678(3) 0.0256(12) Uani 1 1 d . . . . .
H57 H -0.070457 0.949247 0.323724 0.031 Uiso 1 1 calc R . . . .
C58 C -0.06363(14) 0.8325(4) 0.4011(3) 0.0244(11) Uani 1 1 d . . . . .
H58 H -0.072699 0.763711 0.382911 0.029 Uiso 1 1 calc R . . . .
C59 C -0.04923(13) 0.8445(4) 0.4661(3) 0.0247(11) Uani 1 1 d . . . . .
C60 C -0.01750(17) 0.7515(5) 0.5975(3) 0.0332(14) Uani 1 1 d . . . . .
H60A H 0.004055 0.724090 0.574337 0.050 Uiso 1 1 calc GR . . . .
H60B H -0.022636 0.701837 0.635276 0.050 Uiso 1 1 calc GR . . . .
H60C H -0.013292 0.829116 0.613317 0.050 Uiso 1 1 calc GR . . . .
C61 C -0.09634(17) 0.8112(5) 0.5846(3) 0.0350(14) Uani 1 1 d . . . . .
H61A H -0.090898 0.889338 0.598042 0.053 Uiso 1 1 calc GR . . . .
H61B H -0.101368 0.765112 0.623887 0.053 Uiso 1 1 calc GR . . . .
H61C H -0.117500 0.811032 0.555434 0.053 Uiso 1 1 calc GR . . . .
C62 C -0.06826(17) 0.6026(5) 0.5149(3) 0.0325(13) Uani 1 1 d . . . . .
H62A H -0.085007 0.604144 0.477345 0.049 Uiso 1 1 calc GR . . . .
H62B H -0.079623 0.563409 0.552284 0.049 Uiso 1 1 calc GR . . . .
H62C H -0.046176 0.562358 0.502133 0.049 Uiso 1 1 calc GR . . . .


_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
Zr1 Si1 2.9015(17) . ?
Zr1 C13 2.505(5) . ?
Zr1 C14 2.521(5) . ?
Zr1 C15 2.514(5) . ?
Zr1 C16 2.478(6) . ?
Zr1 C20 2.461(6) . ?
Zr1 C21 2.456(5) . ?
Zr1 C22 2.507(5) . ?
Zr1 C26 2.519(6) . ?
Zr1 C27 2.522(6) . ?
Zr1 C28 2.492(5) . ?
Si1 Si2 2.380(2) . ?
Si1 Si3 2.356(2) . ?
Si1 Si4 2.362(2) . ?
Si2 C1 1.891(6) . ?
Si2 C2 1.892(7) . ?
Si2 C3 1.907(7) . ?
Si3 C4 1.904(7) . ?
Si3 C5 1.856(7) . ?
Si3 C6 1.894(7) . ?
Si4 C7 1.892(7) . ?
Si4 C8 1.893(6) . ?
Si4 C9 1.891(7) . ?
Si5 C10 1.867(6) . ?
Si5 C11 1.869(6) . ?
Si5 C12 1.881(6) . ?
Si5 C13 1.872(6) . ?
Si6 C16 1.893(6) . ?
Si6 C17 1.854(7) . ?
Si6 C18 1.870(7) . ?
Si6 C19 1.858(7) . ?
Si7 C22 1.868(6) . ?
Si7 C23 1.863(7) . ?
Si7 C24 1.875(7) . ?
Si7 C25 1.857(7) . ?
Si8 C28 1.880(6) . ?
Si8 C29 1.857(7) . ?
Si8 C30 1.867(7) . ?
Si8 C31 1.860(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.433(8) . ?
C13 C20 1.438(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.398(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.415(8) . ?
C16 C20 1.423(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.431(7) . ?
C21 C28 1.437(8) . ?
C22 C26 1.422(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.424(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.402(8) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Zr2 Si9 2.9042(18) . ?
Zr2 C44 2.496(5) . ?
Zr2 C45 2.518(6) . ?
Zr2 C46 2.507(5) . ?
Zr2 C47 2.490(5) . ?
Zr2 C51 2.448(5) . ?
Zr2 C52 2.450(5) . ?
Zr2 C53 2.504(5) . ?
Zr2 C57 2.521(5) . ?
Zr2 C58 2.514(5) . ?
Zr2 C59 2.491(5) . ?
Si9 Si10 2.364(2) . ?
Si9 Si11 2.367(2) . ?
Si9 Si12 2.366(2) . ?
Si10 C32 1.896(7) . ?
Si10 C33 1.890(6) . ?
Si10 C34 1.890(7) . ?
Si11 C35 1.881(6) . ?
Si11 C36 1.890(6) . ?
Si11 C37 1.889(7) . ?
Si12 C38 1.891(6) . ?
Si12 C39 1.880(7) . ?
Si12 C40 1.887(7) . ?
Si13 C41 1.864(7) . ?
Si13 C42 1.875(6) . ?
Si13 C43 1.864(7) . ?
Si13 C44 1.891(6) . ?
Si14 C47 1.875(6) . ?
Si14 C48 1.873(7) . ?
Si14 C49 1.864(6) . ?
Si14 C50 1.858(6) . ?
Si15 C53 1.882(6) . ?
Si15 C54 1.869(7) . ?
Si15 C55 1.873(6) . ?
Si15 C56 1.864(7) . ?
Si16 C59 1.870(6) . ?
Si16 C60 1.870(6) . ?
Si16 C61 1.865(6) . ?
Si16 C62 1.860(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.421(8) . ?
C44 C51 1.412(9) . ?
C45 H45 0.9500 . ?
C45 C46 1.403(8) . ?
C46 H46 0.9500 . ?
C46 C47 1.424(9) . ?
C47 C51 1.434(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C52 C53 1.409(8) . ?
C52 C59 1.438(7) . ?
C53 C57 1.419(8) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57 0.9500 . ?
C57 C58 1.398(8) . ?
C58 H58 0.9500 . ?
C58 C59 1.425(8) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Zr1 Si1 115.45(13) . . ?
C13 Zr1 C14 33.12(18) . . ?
C13 Zr1 C15 54.95(18) . . ?
C13 Zr1 C22 138.93(19) . . ?
C13 Zr1 C26 106.13(19) . . ?
C13 Zr1 C27 91.56(19) . . ?
C14 Zr1 Si1 86.14(13) . . ?
C14 Zr1 C27 124.48(19) . . ?
C15 Zr1 Si1 86.50(13) . . ?
C15 Zr1 C14 32.23(17) . . ?
C15 Zr1 C26 124.12(18) . . ?
C15 Zr1 C27 136.72(19) . . ?
C16 Zr1 Si1 116.02(14) . . ?
C16 Zr1 C13 56.38(18) . . ?
C16 Zr1 C14 54.69(18) . . ?
C16 Zr1 C15 32.92(18) . . ?
C16 Zr1 C22 107.67(18) . . ?
C16 Zr1 C26 91.31(19) . . ?
C16 Zr1 C27 107.79(19) . . ?
C16 Zr1 C28 140.3(2) . . ?
C20 Zr1 Si1 138.54(13) . . ?
C20 Zr1 C13 33.64(17) . . ?
C20 Zr1 C14 54.10(18) . . ?
C20 Zr1 C15 54.08(19) . . ?
C20 Zr1 C16 33.49(19) . . ?
C20 Zr1 C22 110.91(19) . . ?
C20 Zr1 C26 81.49(19) . . ?
C20 Zr1 C27 82.73(19) . . ?
C20 Zr1 C28 112.55(19) . . ?
C21 Zr1 Si1 87.51(13) . . ?
C21 Zr1 C13 142.45(19) . . ?
C21 Zr1 C14 163.73(18) . . ?
C21 Zr1 C15 161.69(18) . . ?
C21 Zr1 C16 141.03(17) . . ?
C21 Zr1 C20 133.95(19) . . ?
C21 Zr1 C22 33.50(17) . . ?
C21 Zr1 C26 54.08(18) . . ?
C21 Zr1 C27 53.93(19) . . ?
C21 Zr1 C28 33.76(19) . . ?
C22 Zr1 Si1 105.55(14) . . ?
C22 Zr1 C14 162.27(18) . . ?
C22 Zr1 C15 133.34(17) . . ?
C22 Zr1 C26 32.87(19) . . ?
C22 Zr1 C27 54.91(19) . . ?
C26 Zr1 Si1 138.00(14) . . ?
C26 Zr1 C14 135.43(19) . . ?
C26 Zr1 C27 32.81(18) . . ?
C27 Zr1 Si1 136.01(14) . . ?
C28 Zr1 Si1 103.65(14) . . ?
C28 Zr1 C13 109.07(19) . . ?
C28 Zr1 C14 134.65(18) . . ?
C28 Zr1 C15 163.95(19) . . ?
C28 Zr1 C22 56.40(18) . . ?
C28 Zr1 C26 54.90(18) . . ?
C28 Zr1 C27 32.47(19) . . ?
Si2 Si1 Zr1 112.69(8) . . ?
Si3 Si1 Zr1 114.67(7) . . ?
Si3 Si1 Si2 100.59(9) . . ?
Si3 Si1 Si4 99.35(9) . . ?
Si4 Si1 Zr1 124.93(8) . . ?
Si4 Si1 Si2 101.09(8) . . ?
C1 Si2 Si1 116.5(2) . . ?
C1 Si2 C2 104.2(3) . . ?
C1 Si2 C3 106.0(3) . . ?
C2 Si2 Si1 108.3(2) . . ?
C2 Si2 C3 109.7(3) . . ?
C3 Si2 Si1 111.8(2) . . ?
C4 Si3 Si1 114.6(2) . . ?
C5 Si3 Si1 112.6(3) . . ?
C5 Si3 C4 103.7(3) . . ?
C5 Si3 C6 106.4(3) . . ?
C6 Si3 Si1 111.5(3) . . ?
C6 Si3 C4 107.4(4) . . ?
C7 Si4 Si1 111.4(2) . . ?
C7 Si4 C8 102.5(3) . . ?
C8 Si4 Si1 115.3(2) . . ?
C9 Si4 Si1 112.5(3) . . ?
C9 Si4 C7 106.4(3) . . ?
C9 Si4 C8 107.8(3) . . ?
C10 Si5 C11 111.6(3) . . ?
C10 Si5 C12 106.7(3) . . ?
C10 Si5 C13 110.2(3) . . ?
C11 Si5 C12 108.4(3) . . ?
C11 Si5 C13 111.6(3) . . ?
C13 Si5 C12 108.0(3) . . ?
C17 Si6 C16 111.7(3) . . ?
C17 Si6 C18 112.3(3) . . ?
C17 Si6 C19 108.8(4) . . ?
C18 Si6 C16 111.7(3) . . ?
C19 Si6 C16 105.8(3) . . ?
C19 Si6 C18 106.3(4) . . ?
C22 Si7 C24 107.0(3) . . ?
C23 Si7 C22 108.5(3) . . ?
C23 Si7 C24 111.4(3) . . ?
C25 Si7 C22 113.7(3) . . ?
C25 Si7 C23 107.8(3) . . ?
C25 Si7 C24 108.5(3) . . ?
C29 Si8 C28 108.9(3) . . ?
C29 Si8 C30 107.9(3) . . ?
C29 Si8 C31 109.6(3) . . ?
C30 Si8 C28 107.1(3) . . ?
C31 Si8 C28 112.8(3) . . ?
C31 Si8 C30 110.3(3) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si5 C10 H10A 109.5 . . ?
Si5 C10 H10B 109.5 . . ?
Si5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si5 C11 H11A 109.5 . . ?
Si5 C11 H11B 109.5 . . ?
Si5 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si5 C12 H12A 109.5 . . ?
Si5 C12 H12B 109.5 . . ?
Si5 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si5 C13 Zr1 135.3(3) . . ?
C14 C13 Zr1 74.1(3) . . ?
C14 C13 Si5 126.5(4) . . ?
C14 C13 C20 104.3(5) . . ?
C20 C13 Zr1 71.5(3) . . ?
C20 C13 Si5 125.6(4) . . ?
Zr1 C14 H14 120.2 . . ?
C13 C14 Zr1 72.8(3) . . ?
C13 C14 H14 125.1 . . ?
C15 C14 Zr1 73.6(3) . . ?
C15 C14 C13 109.8(5) . . ?
C15 C14 H14 125.1 . . ?
Zr1 C15 H15 120.1 . . ?
C14 C15 Zr1 74.2(3) . . ?
C14 C15 H15 125.3 . . ?
C14 C15 C16 109.5(5) . . ?
C16 C15 Zr1 72.2(3) . . ?
C16 C15 H15 125.3 . . ?
Si6 C16 Zr1 136.1(3) . . ?
C15 C16 Zr1 74.9(3) . . ?
C15 C16 Si6 126.7(4) . . ?
C15 C16 C20 105.7(5) . . ?
C20 C16 Zr1 72.6(3) . . ?
C20 C16 Si6 123.1(4) . . ?
Si6 C17 H17A 109.5 . . ?
Si6 C17 H17B 109.5 . . ?
Si6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si6 C18 H18A 109.5 . . ?
Si6 C18 H18B 109.5 . . ?
Si6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si6 C19 H19A 109.5 . . ?
Si6 C19 H19B 109.5 . . ?
Si6 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Zr1 C20 H20 118.3 . . ?
C13 C20 Zr1 74.9(3) . . ?
C13 C20 H20 124.6 . . ?
C16 C20 Zr1 73.9(3) . . ?
C16 C20 C13 110.7(5) . . ?
C16 C20 H20 124.6 . . ?
Zr1 C21 H21 117.4 . . ?
C22 C21 Zr1 75.2(3) . . ?
C22 C21 H21 124.6 . . ?
C22 C21 C28 110.9(5) . . ?
C28 C21 Zr1 74.5(3) . . ?
C28 C21 H21 124.6 . . ?
Si7 C22 Zr1 131.5(3) . . ?
C21 C22 Zr1 71.3(3) . . ?
C21 C22 Si7 127.7(4) . . ?
C26 C22 Zr1 74.0(3) . . ?
C26 C22 Si7 125.4(4) . . ?
C26 C22 C21 104.9(5) . . ?
Si7 C23 H23A 109.5 . . ?
Si7 C23 H23B 109.5 . . ?
Si7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si7 C24 H24A 109.5 . . ?
Si7 C24 H24B 109.5 . . ?
Si7 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si7 C25 H25A 109.5 . . ?
Si7 C25 H25B 109.5 . . ?
Si7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Zr1 C26 H26 119.5 . . ?
C22 C26 Zr1 73.1(3) . . ?
C22 C26 H26 125.4 . . ?
C22 C26 C27 109.2(5) . . ?
C27 C26 Zr1 73.7(3) . . ?
C27 C26 H26 125.4 . . ?
Zr1 C27 H27 120.5 . . ?
C26 C27 Zr1 73.4(3) . . ?
C26 C27 H27 125.2 . . ?
C28 C27 Zr1 72.6(3) . . ?
C28 C27 C26 109.6(5) . . ?
C28 C27 H27 125.2 . . ?
Si8 C28 Zr1 130.4(3) . . ?
C21 C28 Zr1 71.7(3) . . ?
C21 C28 Si8 127.1(4) . . ?
C27 C28 Zr1 75.0(3) . . ?
C27 C28 Si8 125.6(4) . . ?
C27 C28 C21 105.4(5) . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si8 C31 H31A 109.5 . . ?
Si8 C31 H31B 109.5 . . ?
Si8 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C44 Zr2 Si9 104.53(15) . . ?
C44 Zr2 C45 32.91(19) . . ?
C44 Zr2 C46 54.81(18) . . ?
C44 Zr2 C53 139.13(19) . . ?
C44 Zr2 C57 163.01(19) . . ?
C44 Zr2 C58 134.24(18) . . ?
C45 Zr2 Si9 137.12(14) . . ?
C45 Zr2 C57 135.36(19) . . ?
C46 Zr2 Si9 136.63(14) . . ?
C46 Zr2 C45 32.43(18) . . ?
C46 Zr2 C57 123.63(18) . . ?
C46 Zr2 C58 135.48(19) . . ?
C47 Zr2 Si9 103.73(15) . . ?
C47 Zr2 C44 56.14(18) . . ?
C47 Zr2 C45 54.9(2) . . ?
C47 Zr2 C46 33.1(2) . . ?
C47 Zr2 C53 108.51(17) . . ?
C47 Zr2 C57 133.82(18) . . ?
C47 Zr2 C58 162.97(17) . . ?
C47 Zr2 C59 139.7(2) . . ?
C51 Zr2 Si9 87.07(15) . . ?
C51 Zr2 C44 33.2(2) . . ?
C51 Zr2 C45 54.0(2) . . ?
C51 Zr2 C46 54.32(19) . . ?
C51 Zr2 C47 33.75(17) . . ?
C51 Zr2 C52 133.9(2) . . ?
C51 Zr2 C53 141.92(17) . . ?
C51 Zr2 C57 163.08(19) . . ?
C51 Zr2 C58 162.64(18) . . ?
C51 Zr2 C59 141.1(2) . . ?
C52 Zr2 Si9 139.03(13) . . ?
C52 Zr2 C44 111.8(2) . . ?
C52 Zr2 C45 81.89(19) . . ?
C52 Zr2 C46 81.77(19) . . ?
C52 Zr2 C47 111.83(18) . . ?
C52 Zr2 C53 33.01(18) . . ?
C52 Zr2 C57 53.63(19) . . ?
C52 Zr2 C58 53.84(18) . . ?
C52 Zr2 C59 33.83(17) . . ?
C53 Zr2 Si9 116.24(13) . . ?
C53 Zr2 C45 106.25(19) . . ?
C53 Zr2 C46 91.01(18) . . ?
C53 Zr2 C57 32.79(18) . . ?
C53 Zr2 C58 54.52(17) . . ?
C57 Zr2 Si9 87.09(14) . . ?
C58 Zr2 Si9 87.22(13) . . ?
C58 Zr2 C45 124.1(2) . . ?
C58 Zr2 C57 32.24(17) . . ?
C59 Zr2 Si9 116.54(14) . . ?
C59 Zr2 C44 108.17(19) . . ?
C59 Zr2 C45 91.1(2) . . ?
C59 Zr2 C46 106.55(19) . . ?
C59 Zr2 C53 56.37(17) . . ?
C59 Zr2 C57 54.99(18) . . ?
C59 Zr2 C58 33.07(19) . . ?
Si10 Si9 Zr2 124.74(7) . . ?
Si10 Si9 Si11 101.10(9) . . ?
Si10 Si9 Si12 100.15(8) . . ?
Si11 Si9 Zr2 113.49(7) . . ?
Si12 Si9 Zr2 113.36(8) . . ?
Si12 Si9 Si11 100.58(8) . . ?
C32 Si10 Si9 116.0(2) . . ?
C33 Si10 Si9 110.7(2) . . ?
C33 Si10 C32 107.4(3) . . ?
C33 Si10 C34 105.0(3) . . ?
C34 Si10 Si9 114.1(2) . . ?
C34 Si10 C32 102.8(3) . . ?
C35 Si11 Si9 110.5(2) . . ?
C35 Si11 C36 108.8(3) . . ?
C35 Si11 C37 104.3(3) . . ?
C36 Si11 Si9 111.7(2) . . ?
C37 Si11 Si9 116.4(2) . . ?
C37 Si11 C36 104.6(3) . . ?
C38 Si12 Si9 115.7(2) . . ?
C39 Si12 Si9 110.2(2) . . ?
C39 Si12 C38 104.6(3) . . ?
C39 Si12 C40 108.7(3) . . ?
C40 Si12 Si9 110.9(2) . . ?
C40 Si12 C38 106.4(3) . . ?
C41 Si13 C42 109.5(3) . . ?
C41 Si13 C44 108.0(3) . . ?
C42 Si13 C44 114.6(3) . . ?
C43 Si13 C41 109.8(3) . . ?
C43 Si13 C42 108.6(3) . . ?
C43 Si13 C44 106.3(3) . . ?
C48 Si14 C47 108.0(3) . . ?
C49 Si14 C47 112.5(3) . . ?
C49 Si14 C48 109.6(3) . . ?
C50 Si14 C47 108.5(3) . . ?
C50 Si14 C48 109.7(3) . . ?
C50 Si14 C49 108.6(3) . . ?
C54 Si15 C53 111.5(3) . . ?
C54 Si15 C55 107.7(3) . . ?
C55 Si15 C53 107.2(3) . . ?
C56 Si15 C53 110.2(3) . . ?
C56 Si15 C54 113.0(3) . . ?
C56 Si15 C55 107.0(3) . . ?
C59 Si16 C60 112.1(3) . . ?
C61 Si16 C59 106.2(3) . . ?
C61 Si16 C60 107.6(3) . . ?
C62 Si16 C59 112.1(3) . . ?
C62 Si16 C60 110.5(3) . . ?
C62 Si16 C61 108.1(3) . . ?
Si10 C32 H32A 109.5 . . ?
Si10 C32 H32B 109.5 . . ?
Si10 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si10 C33 H33A 109.5 . . ?
Si10 C33 H33B 109.5 . . ?
Si10 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si10 C34 H34A 109.5 . . ?
Si10 C34 H34B 109.5 . . ?
Si10 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si11 C35 H35A 109.5 . . ?
Si11 C35 H35B 109.5 . . ?
Si11 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si11 C36 H36A 109.5 . . ?
Si11 C36 H36B 109.5 . . ?
Si11 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si11 C37 H37A 109.5 . . ?
Si11 C37 H37B 109.5 . . ?
Si11 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si12 C38 H38A 109.5 . . ?
Si12 C38 H38B 109.5 . . ?
Si12 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si12 C39 H39A 109.5 . . ?
Si12 C39 H39B 109.5 . . ?
Si12 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Si12 C40 H40A 109.5 . . ?
Si12 C40 H40B 109.5 . . ?
Si12 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Si13 C41 H41A 109.5 . . ?
Si13 C41 H41B 109.5 . . ?
Si13 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si13 C42 H42A 109.5 . . ?
Si13 C42 H42B 109.5 . . ?
Si13 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si13 C43 H43A 109.5 . . ?
Si13 C43 H43B 109.5 . . ?
Si13 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si13 C44 Zr2 131.9(3) . . ?
C45 C44 Zr2 74.4(3) . . ?
C45 C44 Si13 125.1(5) . . ?
C51 C44 Zr2 71.5(3) . . ?
C51 C44 Si13 127.2(4) . . ?
C51 C44 C45 105.5(5) . . ?
Zr2 C45 H45 120.3 . . ?
C44 C45 Zr2 72.7(3) . . ?
C44 C45 H45 125.4 . . ?
C46 C45 Zr2 73.3(3) . . ?
C46 C45 C44 109.3(5) . . ?
C46 C45 H45 125.4 . . ?
Zr2 C46 H46 119.4 . . ?
C45 C46 Zr2 74.2(3) . . ?
C45 C46 H46 125.3 . . ?
C45 C46 C47 109.4(5) . . ?
C47 C46 Zr2 72.8(3) . . ?
C47 C46 H46 125.3 . . ?
Si14 C47 Zr2 128.1(3) . . ?
C46 C47 Zr2 74.1(3) . . ?
C46 C47 Si14 125.8(4) . . ?
C46 C47 C51 104.7(5) . . ?
C51 C47 Zr2 71.5(3) . . ?
C51 C47 Si14 128.4(5) . . ?
Si14 C48 H48A 109.5 . . ?
Si14 C48 H48B 109.5 . . ?
Si14 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si14 C49 H49A 109.5 . . ?
Si14 C49 H49B 109.5 . . ?
Si14 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Si14 C50 H50A 109.5 . . ?
Si14 C50 H50B 109.5 . . ?
Si14 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Zr2 C51 H51 117.2 . . ?
C44 C51 Zr2 75.3(3) . . ?
C44 C51 C47 111.1(5) . . ?
C44 C51 H51 124.5 . . ?
C47 C51 Zr2 74.7(3) . . ?
C47 C51 H51 124.5 . . ?
Zr2 C52 H52 117.3 . . ?
C53 C52 Zr2 75.6(3) . . ?
C53 C52 H52 124.0 . . ?
C53 C52 C59 112.0(5) . . ?
C59 C52 Zr2 74.7(3) . . ?
C59 C52 H52 124.0 . . ?
Si15 C53 Zr2 135.2(3) . . ?
C52 C53 Zr2 71.4(3) . . ?
C52 C53 Si15 126.7(4) . . ?
C52 C53 C57 105.0(5) . . ?
C57 C53 Zr2 74.3(3) . . ?
C57 C53 Si15 124.9(4) . . ?
Si15 C54 H54A 109.5 . . ?
Si15 C54 H54B 109.5 . . ?
Si15 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
Si15 C55 H55A 109.5 . . ?
Si15 C55 H55B 109.5 . . ?
Si15 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
Si15 C56 H56A 109.5 . . ?
Si15 C56 H56B 109.5 . . ?
Si15 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
Zr2 C57 H57 119.9 . . ?
C53 C57 Zr2 72.9(3) . . ?
C53 C57 H57 125.3 . . ?
C58 C57 Zr2 73.6(3) . . ?
C58 C57 C53 109.4(5) . . ?
C58 C57 H57 125.3 . . ?
Zr2 C58 H58 120.0 . . ?
C57 C58 Zr2 74.2(3) . . ?
C57 C58 H58 124.9 . . ?
C57 C58 C59 110.1(5) . . ?
C59 C58 Zr2 72.6(3) . . ?
C59 C58 H58 124.9 . . ?
Si16 C59 Zr2 135.2(3) . . ?
C52 C59 Zr2 71.5(3) . . ?
C52 C59 Si16 124.6(5) . . ?
C58 C59 Zr2 74.4(3) . . ?
C58 C59 Si16 128.0(4) . . ?
C58 C59 C52 103.5(5) . . ?
Si16 C60 H60A 109.5 . . ?
Si16 C60 H60B 109.5 . . ?
Si16 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
Si16 C61 H61A 109.5 . . ?
Si16 C61 H61B 109.5 . . ?
Si16 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
Si16 C62 H62A 109.5 . . ?
Si16 C62 H62B 109.5 . . ?
Si16 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 C13 C14 C15 64.8(4) . . . . ?
Zr1 C13 C20 C16 -65.8(4) . . . . ?
Zr1 C14 C15 C16 64.0(4) . . . . ?
Zr1 C15 C16 Si6 -136.8(5) . . . . ?
Zr1 C15 C16 C20 66.6(4) . . . . ?
Zr1 C16 C20 C13 66.4(4) . . . . ?
Zr1 C21 C22 Si7 128.4(4) . . . . ?
Zr1 C21 C22 C26 -67.0(4) . . . . ?
Zr1 C21 C28 Si8 -127.3(4) . . . . ?
Zr1 C21 C28 C27 68.1(4) . . . . ?
Zr1 C22 C26 C27 -65.5(4) . . . . ?
Zr1 C26 C27 C28 -64.0(4) . . . . ?
Zr1 C27 C28 Si8 129.2(4) . . . . ?
Zr1 C27 C28 C21 -65.8(4) . . . . ?
Si5 C13 C14 Zr1 135.0(4) . . . . ?
Si5 C13 C14 C15 -160.1(4) . . . . ?
Si5 C13 C20 Zr1 -133.0(4) . . . . ?
Si5 C13 C20 C16 161.2(4) . . . . ?
Si6 C16 C20 Zr1 134.1(4) . . . . ?
Si6 C16 C20 C13 -159.4(4) . . . . ?
Si7 C22 C26 Zr1 -129.9(4) . . . . ?
Si7 C22 C26 C27 164.6(4) . . . . ?
C10 Si5 C13 Zr1 84.2(4) . . . . ?
C10 Si5 C13 C14 -21.0(6) . . . . ?
C10 Si5 C13 C20 -176.2(5) . . . . ?
C11 Si5 C13 Zr1 -40.4(5) . . . . ?
C11 Si5 C13 C14 -145.6(5) . . . . ?
C11 Si5 C13 C20 59.2(5) . . . . ?
C12 Si5 C13 Zr1 -159.6(4) . . . . ?
C12 Si5 C13 C14 95.3(5) . . . . ?
C12 Si5 C13 C20 -59.9(5) . . . . ?
C13 C14 C15 Zr1 -64.3(4) . . . . ?
C13 C14 C15 C16 -0.3(6) . . . . ?
C14 C13 C20 Zr1 67.4(4) . . . . ?
C14 C13 C20 C16 1.6(6) . . . . ?
C14 C15 C16 Zr1 -65.3(4) . . . . ?
C14 C15 C16 Si6 157.8(4) . . . . ?
C14 C15 C16 C20 1.3(6) . . . . ?
C15 C16 C20 Zr1 -68.2(4) . . . . ?
C15 C16 C20 C13 -1.8(6) . . . . ?
C17 Si6 C16 Zr1 -78.6(5) . . . . ?
C17 Si6 C16 C15 29.3(6) . . . . ?
C17 Si6 C16 C20 -177.9(5) . . . . ?
C18 Si6 C16 Zr1 48.1(5) . . . . ?
C18 Si6 C16 C15 155.9(5) . . . . ?
C18 Si6 C16 C20 -51.3(6) . . . . ?
C19 Si6 C16 Zr1 163.3(4) . . . . ?
C19 Si6 C16 C15 -88.9(6) . . . . ?
C19 Si6 C16 C20 63.9(6) . . . . ?
C20 C13 C14 Zr1 -65.6(3) . . . . ?
C20 C13 C14 C15 -0.8(6) . . . . ?
C21 C22 C26 Zr1 65.1(3) . . . . ?
C21 C22 C26 C27 -0.4(6) . . . . ?
C22 C21 C28 Zr1 -67.1(4) . . . . ?
C22 C21 C28 Si8 165.7(4) . . . . ?
C22 C21 C28 C27 1.0(6) . . . . ?
C22 C26 C27 Zr1 65.1(4) . . . . ?
C22 C26 C27 C28 1.0(6) . . . . ?
C23 Si7 C22 Zr1 109.9(4) . . . . ?
C23 Si7 C22 C21 11.7(6) . . . . ?
C23 Si7 C22 C26 -149.9(5) . . . . ?
C24 Si7 C22 Zr1 -129.8(4) . . . . ?
C24 Si7 C22 C21 132.0(5) . . . . ?
C24 Si7 C22 C26 -29.7(5) . . . . ?
C25 Si7 C22 Zr1 -10.0(5) . . . . ?
C25 Si7 C22 C21 -108.2(5) . . . . ?
C25 Si7 C22 C26 90.1(5) . . . . ?
C26 C27 C28 Zr1 64.6(4) . . . . ?
C26 C27 C28 Si8 -166.2(4) . . . . ?
C26 C27 C28 C21 -1.2(6) . . . . ?
C28 C21 C22 Zr1 66.6(4) . . . . ?
C28 C21 C22 Si7 -164.9(4) . . . . ?
C28 C21 C22 C26 -0.3(6) . . . . ?
C29 Si8 C28 Zr1 -114.0(4) . . . . ?
C29 Si8 C28 C21 -16.7(6) . . . . ?
C29 Si8 C28 C27 145.1(5) . . . . ?
C30 Si8 C28 Zr1 129.5(4) . . . . ?
C30 Si8 C28 C21 -133.2(5) . . . . ?
C30 Si8 C28 C27 28.6(5) . . . . ?
C31 Si8 C28 Zr1 8.0(5) . . . . ?
C31 Si8 C28 C21 105.3(5) . . . . ?
C31 Si8 C28 C27 -92.9(5) . . . . ?
Zr2 C44 C45 C46 -64.7(4) . . . . ?
Zr2 C44 C51 C47 66.9(4) . . . . ?
Zr2 C45 C46 C47 -64.8(4) . . . . ?
Zr2 C46 C47 Si14 125.9(4) . . . . ?
Zr2 C46 C47 C51 -65.5(4) . . . . ?
Zr2 C47 C51 C44 -67.2(4) . . . . ?
Zr2 C52 C53 Si15 -133.0(4) . . . . ?
Zr2 C52 C53 C57 67.2(4) . . . . ?
Zr2 C52 C59 Si16 132.7(4) . . . . ?
Zr2 C52 C59 C58 -68.1(3) . . . . ?
Zr2 C53 C57 C58 65.1(4) . . . . ?
Zr2 C57 C58 C59 64.2(4) . . . . ?
Zr2 C58 C59 Si16 -135.7(4) . . . . ?
Zr2 C58 C59 C52 66.0(3) . . . . ?
Si13 C44 C45 Zr2 -130.6(4) . . . . ?
Si13 C44 C45 C46 164.7(4) . . . . ?
Si13 C44 C51 Zr2 129.0(4) . . . . ?
Si13 C44 C51 C47 -164.1(4) . . . . ?
Si14 C47 C51 Zr2 -124.5(5) . . . . ?
Si14 C47 C51 C44 168.3(4) . . . . ?
Si15 C53 C57 Zr2 134.6(4) . . . . ?
Si15 C53 C57 C58 -160.3(4) . . . . ?
C41 Si13 C44 Zr2 110.9(4) . . . . ?
C41 Si13 C44 C45 -148.3(5) . . . . ?
C41 Si13 C44 C51 12.4(6) . . . . ?
C42 Si13 C44 Zr2 -11.4(5) . . . . ?
C42 Si13 C44 C45 89.4(5) . . . . ?
C42 Si13 C44 C51 -109.9(5) . . . . ?
C43 Si13 C44 Zr2 -131.4(4) . . . . ?
C43 Si13 C44 C45 -30.5(5) . . . . ?
C43 Si13 C44 C51 130.2(5) . . . . ?
C44 C45 C46 Zr2 64.3(4) . . . . ?
C44 C45 C46 C47 -0.5(6) . . . . ?
C45 C44 C51 Zr2 -67.2(4) . . . . ?
C45 C44 C51 C47 -0.4(6) . . . . ?
C45 C46 C47 Zr2 65.7(4) . . . . ?
C45 C46 C47 Si14 -168.4(4) . . . . ?
C45 C46 C47 C51 0.3(6) . . . . ?
C46 C47 C51 Zr2 67.3(4) . . . . ?
C46 C47 C51 C44 0.1(6) . . . . ?
C48 Si14 C47 Zr2 128.5(4) . . . . ?
C48 Si14 C47 C46 30.6(5) . . . . ?
C48 Si14 C47 C51 -135.3(5) . . . . ?
C49 Si14 C47 Zr2 7.4(4) . . . . ?
C49 Si14 C47 C46 -90.4(5) . . . . ?
C49 Si14 C47 C51 103.7(5) . . . . ?
C50 Si14 C47 Zr2 -112.7(3) . . . . ?
C50 Si14 C47 C46 149.5(5) . . . . ?
C50 Si14 C47 C51 -16.4(6) . . . . ?
C51 C44 C45 Zr2 65.2(4) . . . . ?
C51 C44 C45 C46 0.5(6) . . . . ?
C52 C53 C57 Zr2 -65.2(4) . . . . ?
C52 C53 C57 C58 -0.1(6) . . . . ?
C53 C52 C59 Zr2 67.1(4) . . . . ?
C53 C52 C59 Si16 -160.1(4) . . . . ?
C53 C52 C59 C58 -1.0(6) . . . . ?
C53 C57 C58 Zr2 -64.7(4) . . . . ?
C53 C57 C58 C59 -0.5(6) . . . . ?
C54 Si15 C53 Zr2 -47.9(5) . . . . ?
C54 Si15 C53 C52 52.7(6) . . . . ?
C54 Si15 C53 C57 -151.4(5) . . . . ?
C55 Si15 C53 Zr2 -165.5(4) . . . . ?
C55 Si15 C53 C52 -64.9(5) . . . . ?
C55 Si15 C53 C57 91.0(5) . . . . ?
C56 Si15 C53 Zr2 78.3(4) . . . . ?
C56 Si15 C53 C52 179.0(5) . . . . ?
C56 Si15 C53 C57 -25.1(6) . . . . ?
C57 C58 C59 Zr2 -65.2(4) . . . . ?
C57 C58 C59 Si16 159.1(4) . . . . ?
C57 C58 C59 C52 0.9(6) . . . . ?
C59 C52 C53 Zr2 -66.6(4) . . . . ?
C59 C52 C53 Si15 160.4(4) . . . . ?
C59 C52 C53 C57 0.7(6) . . . . ?
C60 Si16 C59 Zr2 43.5(5) . . . . ?
C60 Si16 C59 C52 -55.0(5) . . . . ?
C60 Si16 C59 C58 151.0(5) . . . . ?
C61 Si16 C59 Zr2 160.8(4) . . . . ?
C61 Si16 C59 C52 62.3(5) . . . . ?
C61 Si16 C59 C58 -91.7(5) . . . . ?
C62 Si16 C59 Zr2 -81.4(4) . . . . ?
C62 Si16 C59 C52 -179.9(4) . . . . ?
C62 Si16 C59 C58 26.1(6) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR4.352
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.696
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.52
2 0.48
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-U
_database_code_depnum_ccdc_archive 'CCDC 2195640'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   rdpm197
_manchester_internal_coll_client BR/PC
_manchester_internal_coll_user   BR/PC
_manchester_internal_coll_date   31/10/2019
_manchester_internal_process_date 31/10/2019
_manchester_internal_process_user BR
_manchester_internal_solution_date 31/10/2019
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 31/10/2019
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 06/11/2019
_manchester_internal_validation_user AW
_manchester_internal_archive_date 06/11/2019
_manchester_internal_archive_user AW
_refine_special_details          
'The Si(SiMe3)3 group is disordered over two orientations. Selected chemicially equivalent Si-Si and Si-C bond distances in the disordered unit were restrained to be approximately equal.'
_audit_creation_date             2019-11-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        "[U(Cp'')2{Si(SiMe3)3}]"
_chemical_formula_moiety         'C31 H69 Si8 U'
_chemical_formula_sum            'C31 H69 Si8 U'
_chemical_formula_weight         904.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U1 Si12 C27'
_chemical_oxdiff_usercomment     br
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.9833(8)
_cell_length_b                   13.2292(5)
_cell_length_c                   20.4047(13)
_cell_angle_alpha                90
_cell_angle_beta                 111.407(6)
_cell_angle_gamma                90
_cell_volume                     4519.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12728
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.7010
_cell_measurement_theta_min      2.8130
_shelx_estimated_absorpt_T_max   0.688
_shelx_estimated_absorpt_T_min   0.259
_exptl_absorpt_coefficient_mu    12.266
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1836
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 8 3 0.0231
5 -8 -3 0.0231
7 4 -11 0.0713
-7 -4 11 0.0713
8 2 6 0.0284
-8 -2 -6 0.0044

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 'Crystallised from pentane at -25 oC'
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.033
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.9869 8.0187 3.0391 -0.3008 -0.7465 0.6426
4.9869 -8.0187 -3.0391 0.3008 0.7465 -0.6426
6.8942 4.0706 -10.9078 -0.2654 -0.6738 -0.6899
-6.8942 -4.0706 10.9078 0.2654 0.6738 0.6899
7.8794 2.0205 6.0890 -0.9687 0.3834 -0.0229
-7.8794 -2.0205 -6.0890 0.9687 -0.3834 0.0229

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43377
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         2.810
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00   2.00   0.50    1.12    --  -45.90  74.00  16.00   86
  2  ω    -44.00  -8.00   0.50    1.12    --  -45.90 -74.00-111.00   72
  3  ω   -114.00 -89.00   0.50    1.12    --  -45.90 -74.00-111.00   50
  4  ω   -154.00 -83.00   0.50    5.30    -- -107.20 -74.00-111.00  142
  5  ω   -110.00 -76.00   0.50    5.30    -- -107.20  74.00  16.00   68
  6  ω    -15.00  11.00   0.50    1.12    --    5.00  74.00  16.00   52
  7  ω    -84.00  42.00   0.50    1.12    --  -45.90  38.00  90.00  252
  8  ω    -77.00  14.00   0.50    1.12    --  -45.90  57.00-180.00  182
  9  ω   -110.00 -70.00   0.50    5.30    -- -107.20 -76.00 -30.00   80
 10  ω   -147.00 -27.00   0.50    5.30    -- -107.20  76.00 150.00  240
 11  ω   -131.00-105.00   0.50    5.30    -- -107.20  76.00  60.00   52
 12  ω   -106.00 -80.00   0.50    5.30    -- -107.20 -76.00 -60.00   52
 13  ω   -143.00-103.00   0.50    5.30    -- -107.20  71.00 121.01   80
 14  ω    -97.00 -64.00   0.50    5.30    -- -107.20  71.00 121.01   66
 15  ω    -47.00 -21.00   0.50    5.30    -- -107.20  71.00 121.01   52
 16  ω   -194.00-169.00   0.50    5.30    -- -107.20 -57.00 -90.00   50
 17  ω   -142.00-116.00   0.50    5.30    -- -107.20 -57.00 -90.00   52
 18  ω   -196.00 -75.00   0.50    5.30    -- -107.20 -57.00-180.00  242
 19  ω    -75.00 -26.00   0.50    5.30    -- -107.20  76.00  60.00   98
 20  ω   -196.00-125.00   0.50    5.30    -- -107.20 -38.00 -90.00  142
 21  ω   -185.00-138.00   0.50    5.30    -- -107.20 -76.00 -60.00   94
 22  ω   -196.00-143.00   0.50    5.30    -- -107.20 -57.00 150.00  106
 23  ω   -113.00 -88.00   0.50    5.30    -- -107.20 -57.00 150.00   50
 24  ω   -144.00 -95.00   0.50    5.30    -- -107.20  76.00  90.00   98
 25  ω    -43.00 -18.00   0.50    5.30    -- -107.20  76.00  90.00   50
 26  ω   -194.00-169.00   0.50    5.30    -- -107.20 -38.00   0.00   50
 27  ω   -151.00 -80.00   0.50    5.30    -- -107.20 -38.00   0.00  142
 28  ω   -112.00 -87.00   0.50    5.30    -- -107.20  76.00-180.00   50
 29  ω   -130.00 -18.00   0.50    5.30    -- -107.20  57.00-120.00  224
 30  ω   -127.00-102.00   0.50    5.30    -- -107.20  76.00 120.00   50
 31  ω   -169.00-144.00   0.50    5.30    -- -107.20 -76.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0714817000
_diffrn_orient_matrix_UB_12      -0.0648853000
_diffrn_orient_matrix_UB_13      -0.0450629000
_diffrn_orient_matrix_UB_21      0.0338351000
_diffrn_orient_matrix_UB_22      -0.0907384000
_diffrn_orient_matrix_UB_23      0.0492930000
_diffrn_orient_matrix_UB_31      -0.0470323000
_diffrn_orient_matrix_UB_32      0.0334492000
_diffrn_orient_matrix_UB_33      0.0460063000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6715
_reflns_number_total             8268
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.059
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8268
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0503
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0385P)²+14.2312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1288
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2A-Si1 \\sim Si4-Si1 \\sim Si4A-Si1 \\sim Si3-Si1 \\sim Si3A-Si1 \\sim
Si2-Si1
 with sigma of 0.02
 Si4-C9 \\sim Si4-C8 \\sim Si4-C7 \\sim Si4A-C9A \\sim Si4A-C7A \\sim Si4A-C8A
\\sim Si2A-C2A \\sim Si2A-
 C3A \\sim Si2A-C1A \\sim Si2-C2 \\sim Si2-C1 \\sim Si2-C3 \\sim Si3A-C5A \\sim
Si3A-C4A \\sim Si3A-C6A ~
 Si3-C4 \\sim Si3-C6 \\sim Si3-C5
 with sigma of 0.01
3. Others
 Sof(Si2A)=Sof(Si3A)=Sof(Si4A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(Si2)=Sof(Si3)=Sof(Si4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C20(H20), C25(H25), C26(H26), C31(H31)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,
 H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC),
  C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,
 H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.55446(2) 0.62043(2) 0.26411(2) 0.04559(11) Uani 1 1 d . . . . .
Si1 Si 0.42376(11) 0.45281(14) 0.22238(10) 0.0391(4) Uani 1 1 d D . . . .
Si5 Si 0.67576(14) 0.4965(3) 0.44863(13) 0.0684(7) Uani 1 1 d . . . . .
Si6 Si 0.67578(12) 0.51212(17) 0.16074(12) 0.0504(5) Uani 1 1 d . . . . .
Si7 Si 0.52851(17) 0.86075(18) 0.11722(14) 0.0615(6) Uani 1 1 d . . . . .
Si8 Si 0.52995(18) 0.8535(2) 0.39853(15) 0.0685(7) Uani 1 1 d . . . . .
C10 C 0.6823(9) 0.3552(11) 0.4554(9) 0.114(5) Uani 1 1 d . . . . .
H10A H 0.681168 0.333894 0.501006 0.171 Uiso 1 1 calc GR . . . .
H10B H 0.732257 0.332513 0.451159 0.171 Uiso 1 1 calc GR . . . .
H10C H 0.636917 0.325209 0.417481 0.171 Uiso 1 1 calc GR . . . .
C11 C 0.5741(6) 0.5404(9) 0.4400(7) 0.082(3) Uani 1 1 d . . . . .
H11A H 0.533763 0.498111 0.405539 0.123 Uiso 1 1 calc GR . . . .
H11B H 0.566932 0.610884 0.424247 0.123 Uiso 1 1 calc GR . . . .
H11C H 0.568059 0.535108 0.485738 0.123 Uiso 1 1 calc GR . . . .
C12 C 0.7537(7) 0.5580(14) 0.5243(6) 0.124(7) Uani 1 1 d . . . . .
H12A H 0.746974 0.538173 0.568012 0.186 Uiso 1 1 calc GR . . . .
H12B H 0.748877 0.631620 0.518843 0.186 Uiso 1 1 calc GR . . . .
H12C H 0.806615 0.536860 0.525914 0.186 Uiso 1 1 calc GR . . . .
C13 C 0.6878(5) 0.5384(7) 0.3675(5) 0.057(2) Uani 1 1 d . . . . .
C14 C 0.7118(5) 0.6365(7) 0.3533(4) 0.055(2) Uani 1 1 d . . . . .
H14 H 0.725334 0.691301 0.385564 0.066 Uiso 1 1 calc R . . . .
C15 C 0.7124(5) 0.6400(7) 0.2851(4) 0.0534(19) Uani 1 1 d . . . . .
H15 H 0.725354 0.697581 0.263599 0.064 Uiso 1 1 calc R . . . .
C16 C 0.6903(4) 0.5430(6) 0.2527(4) 0.0503(18) Uani 1 1 d . . . . .
C17 C 0.7531(6) 0.5793(9) 0.1368(5) 0.069(3) Uani 1 1 d . . . . .
H17A H 0.751197 0.651758 0.146229 0.104 Uiso 1 1 calc GR . . . .
H17B H 0.742817 0.569070 0.086701 0.104 Uiso 1 1 calc GR . . . .
H17C H 0.805993 0.552653 0.164909 0.104 Uiso 1 1 calc GR . . . .
C18 C 0.5721(5) 0.5571(7) 0.1089(5) 0.062(2) Uani 1 1 d . . . . .
H18A H 0.533542 0.517367 0.121795 0.093 Uiso 1 1 calc GR . . . .
H18B H 0.561241 0.548876 0.058475 0.093 Uiso 1 1 calc GR . . . .
H18C H 0.567259 0.628637 0.119170 0.093 Uiso 1 1 calc GR . . . .
C19 C 0.6812(6) 0.3727(7) 0.1492(6) 0.070(3) Uani 1 1 d . . . . .
H19A H 0.736086 0.349508 0.174073 0.105 Uiso 1 1 calc GR . . . .
H19B H 0.664930 0.356862 0.099035 0.105 Uiso 1 1 calc GR . . . .
H19C H 0.645384 0.338528 0.168593 0.105 Uiso 1 1 calc GR . . . .
C20 C 0.6748(5) 0.4826(7) 0.3042(5) 0.055(2) Uani 1 1 d . . . . .
H20 H 0.658009 0.414100 0.297307 0.066 Uiso 1 1 calc R . . . .
C21 C 0.6336(7) 0.8450(10) 0.1221(7) 0.088(3) Uani 1 1 d . . . . .
H21A H 0.642578 0.887887 0.086533 0.132 Uiso 1 1 calc GR . . . .
H21B H 0.642819 0.774122 0.113271 0.132 Uiso 1 1 calc GR . . . .
H21C H 0.670460 0.864638 0.168991 0.132 Uiso 1 1 calc GR . . . .
C22 C 0.5062(10) 0.9993(9) 0.1190(7) 0.108(5) Uani 1 1 d . . . . .
H22A H 0.553904 1.034523 0.150211 0.163 Uiso 1 1 calc GR . . . .
H22B H 0.462503 1.008519 0.136376 0.163 Uiso 1 1 calc GR . . . .
H22C H 0.490450 1.027134 0.071341 0.163 Uiso 1 1 calc GR . . . .
C23 C 0.4571(6) 0.8051(7) 0.0336(5) 0.065(2) Uani 1 1 d . . . . .
H23A H 0.458758 0.844370 -0.006589 0.097 Uiso 1 1 calc GR . . . .
H23B H 0.402893 0.806738 0.034217 0.097 Uiso 1 1 calc GR . . . .
H23C H 0.472266 0.734924 0.029272 0.097 Uiso 1 1 calc GR . . . .
C24 C 0.5134(5) 0.8046(6) 0.1950(4) 0.0501(18) Uani 1 1 d . . . . .
C25 C 0.4393(5) 0.7603(6) 0.1932(4) 0.0463(17) Uani 1 1 d . . . . .
H25 H 0.397648 0.735804 0.152509 0.056 Uiso 1 1 calc R . . . .
C26 C 0.4395(5) 0.7598(6) 0.2619(4) 0.0473(17) Uani 1 1 d . . . . .
H26 H 0.397207 0.735160 0.274871 0.057 Uiso 1 1 calc R . . . .
C27 C 0.5126(5) 0.8018(6) 0.3098(4) 0.0513(18) Uani 1 1 d . . . . .
C28 C 0.4641(6) 0.7910(8) 0.4392(5) 0.073(3) Uani 1 1 d . . . . .
H28A H 0.408232 0.797643 0.407679 0.109 Uiso 1 1 calc GR . . . .
H28B H 0.471580 0.823374 0.484369 0.109 Uiso 1 1 calc GR . . . .
H28C H 0.478106 0.719246 0.446909 0.109 Uiso 1 1 calc GR . . . .
C29 C 0.5045(11) 0.9906(9) 0.3854(8) 0.123(6) Uani 1 1 d . . . . .
H29A H 0.482326 1.005709 0.334911 0.185 Uiso 1 1 calc GR . . . .
H29B H 0.552767 1.031002 0.407985 0.185 Uiso 1 1 calc GR . . . .
H29C H 0.464893 1.007116 0.406411 0.185 Uiso 1 1 calc GR . . . .
C30 C 0.6369(7) 0.8407(11) 0.4569(6) 0.100(4) Uani 1 1 d . . . . .
H30A H 0.650634 0.768893 0.465036 0.151 Uiso 1 1 calc GR . . . .
H30B H 0.645631 0.873987 0.502050 0.151 Uiso 1 1 calc GR . . . .
H30C H 0.670732 0.872438 0.434454 0.151 Uiso 1 1 calc GR . . . .
C31 C 0.5573(5) 0.8287(6) 0.2672(4) 0.0514(18) Uani 1 1 d . . . . .
H31 H 0.608958 0.858499 0.284420 0.062 Uiso 1 1 calc R . . . .
Si2 Si 0.4418(3) 0.2900(3) 0.1874(3) 0.0522(12) Uani 0.477(4) 1 d D . P A 1
Si3 Si 0.3131(2) 0.5112(3) 0.1239(2) 0.0441(10) Uani 0.477(4) 1 d D . P A 1
Si4 Si 0.3581(3) 0.4263(3) 0.3032(2) 0.0484(11) Uani 0.477(4) 1 d D . P A 1
C1 C 0.362(2) 0.194(3) 0.1826(17) 0.071(9) Uani 0.477(4) 1 d D . P A 1
H1A H 0.357740 0.188513 0.228839 0.106 Uiso 0.477(4) 1 calc GR . P A 1
H1B H 0.376910 0.128704 0.168672 0.106 Uiso 0.477(4) 1 calc GR . P A 1
H1C H 0.311154 0.216498 0.147817 0.106 Uiso 0.477(4) 1 calc GR . P A 1
C2 C 0.5375(12) 0.230(3) 0.2473(10) 0.047(6) Uani 0.477(4) 1 d D . P A 1
H2A H 0.582600 0.274133 0.250990 0.070 Uiso 0.477(4) 1 calc GR . P A 1
H2B H 0.544517 0.164419 0.228014 0.070 Uiso 0.477(4) 1 calc GR . P A 1
H2C H 0.535109 0.220260 0.294132 0.070 Uiso 0.477(4) 1 calc GR . P A 1
C3 C 0.4466(13) 0.2892(15) 0.0966(7) 0.059(5) Uani 0.477(4) 1 d D . P A 1
H3A H 0.399695 0.323966 0.063696 0.088 Uiso 0.477(4) 1 calc GR . P A 1
H3B H 0.447531 0.219281 0.081094 0.088 Uiso 0.477(4) 1 calc GR . P A 1
H3C H 0.495193 0.324119 0.097757 0.088 Uiso 0.477(4) 1 calc GR . P A 1
C4 C 0.2355(13) 0.4136(16) 0.0771(13) 0.071(7) Uani 0.477(4) 1 d D . P A 1
H4A H 0.258886 0.363751 0.054716 0.106 Uiso 0.477(4) 1 calc GR . P A 1
H4B H 0.190099 0.446701 0.041146 0.106 Uiso 0.477(4) 1 calc GR . P A 1
H4C H 0.217261 0.379526 0.111183 0.106 Uiso 0.477(4) 1 calc GR . P A 1
C5 C 0.350(4) 0.565(3) 0.056(3) 0.055(11) Uani 0.477(4) 1 d D . P A 1
H5A H 0.382748 0.624781 0.074884 0.082 Uiso 0.477(4) 1 calc GR . P A 1
H5B H 0.304264 0.583644 0.013682 0.082 Uiso 0.477(4) 1 calc GR . P A 1
H5C H 0.382176 0.513922 0.043315 0.082 Uiso 0.477(4) 1 calc GR . P A 1
C6 C 0.2581(12) 0.6150(14) 0.1504(10) 0.058(5) Uani 0.477(4) 1 d D . P A 1
H6A H 0.220359 0.585234 0.169529 0.088 Uiso 0.477(4) 1 calc GR . P A 1
H6B H 0.228783 0.656289 0.109142 0.088 Uiso 0.477(4) 1 calc GR . P A 1
H6C H 0.296400 0.657570 0.186321 0.088 Uiso 0.477(4) 1 calc GR . P A 1
C7 C 0.2522(12) 0.379(3) 0.264(3) 0.064(11) Uani 0.477(4) 1 d D . P A 1
H7A H 0.222390 0.419702 0.222579 0.096 Uiso 0.477(4) 1 calc GR . P A 1
H7B H 0.226864 0.383738 0.298812 0.096 Uiso 0.477(4) 1 calc GR . P A 1
H7C H 0.252422 0.308016 0.249578 0.096 Uiso 0.477(4) 1 calc GR . P A 1
C8 C 0.355(4) 0.5492(15) 0.3487(17) 0.051(12) Uani 0.477(4) 1 d D . P A 1
H8A H 0.407038 0.582571 0.362572 0.077 Uiso 0.477(4) 1 calc GR . P A 1
H8B H 0.342098 0.535824 0.390604 0.077 Uiso 0.477(4) 1 calc GR . P A 1
H8C H 0.313875 0.593164 0.316465 0.077 Uiso 0.477(4) 1 calc GR . P A 1
C9 C 0.4196(16) 0.341(2) 0.3771(11) 0.100(11) Uani 0.477(4) 1 d D . P A 1
H9A H 0.460989 0.307847 0.364119 0.150 Uiso 0.477(4) 1 calc GR . P A 1
H9B H 0.384962 0.289577 0.385699 0.150 Uiso 0.477(4) 1 calc GR . P A 1
H9C H 0.444764 0.381087 0.419885 0.150 Uiso 0.477(4) 1 calc GR . P A 1
Si2A Si 0.4505(3) 0.2849(3) 0.2669(2) 0.0524(11) Uani 0.523(4) 1 d D . P A 2
Si3A Si 0.3638(2) 0.4214(3) 0.1005(2) 0.0443(9) Uani 0.523(4) 1 d D . P A 2
Si4A Si 0.3129(2) 0.4985(3) 0.24902(18) 0.0390(9) Uani 0.523(4) 1 d D . P A 2
C1A C 0.3725(18) 0.191(2) 0.2158(13) 0.068(8) Uani 0.523(4) 1 d D . P A 2
H1AA H 0.320174 0.211871 0.215469 0.102 Uiso 0.523(4) 1 calc GR . P A 2
H1AB H 0.385858 0.124012 0.237932 0.102 Uiso 0.523(4) 1 calc GR . P A 2
H1AC H 0.370950 0.187064 0.167330 0.102 Uiso 0.523(4) 1 calc GR . P A 2
C2A C 0.4513(12) 0.2812(12) 0.3597(6) 0.067(5) Uani 0.523(4) 1 d D . P A 2
H2AA H 0.501090 0.311022 0.391986 0.100 Uiso 0.523(4) 1 calc GR . P A 2
H2AB H 0.447504 0.210873 0.373361 0.100 Uiso 0.523(4) 1 calc GR . P A 2
H2AC H 0.405753 0.319643 0.362053 0.100 Uiso 0.523(4) 1 calc GR . P A 2
C3A C 0.5494(12) 0.230(3) 0.2729(11) 0.065(7) Uani 0.523(4) 1 d D . P A 2
H3AA H 0.552957 0.230182 0.226080 0.098 Uiso 0.523(4) 1 calc GR . P A 2
H3AB H 0.554032 0.160870 0.290700 0.098 Uiso 0.523(4) 1 calc GR . P A 2
H3AC H 0.592831 0.271391 0.304990 0.098 Uiso 0.523(4) 1 calc GR . P A 2
C4A C 0.2601(7) 0.3666(16) 0.0711(12) 0.060(5) Uani 0.523(4) 1 d D . P A 2
H4AA H 0.262733 0.297494 0.089126 0.091 Uiso 0.523(4) 1 calc GR . P A 2
H4AB H 0.236741 0.365601 0.019556 0.091 Uiso 0.523(4) 1 calc GR . P A 2
H4AC H 0.226881 0.408155 0.089354 0.091 Uiso 0.523(4) 1 calc GR . P A 2
C5A C 0.4284(12) 0.3380(19) 0.0688(10) 0.079(7) Uani 0.523(4) 1 d D . P A 2
H5AA H 0.448708 0.376956 0.038009 0.118 Uiso 0.523(4) 1 calc GR . P A 2
H5AB H 0.396831 0.280794 0.042589 0.118 Uiso 0.523(4) 1 calc GR . P A 2
H5AC H 0.473413 0.312850 0.109303 0.118 Uiso 0.523(4) 1 calc GR . P A 2
C6A C 0.349(3) 0.543(2) 0.049(2) 0.043(8) Uani 0.523(4) 1 d D . P A 2
H6AA H 0.315379 0.588665 0.063758 0.064 Uiso 0.523(4) 1 calc GR . P A 2
H6AB H 0.323762 0.528468 -0.001227 0.064 Uiso 0.523(4) 1 calc GR . P A 2
H6AC H 0.401337 0.574856 0.058297 0.064 Uiso 0.523(4) 1 calc GR . P A 2
C7A C 0.2402(16) 0.394(2) 0.246(2) 0.059(9) Uani 0.523(4) 1 d D . P A 2
H7AA H 0.222125 0.361958 0.199678 0.089 Uiso 0.523(4) 1 calc GR . P A 2
H7AB H 0.194177 0.422898 0.254439 0.089 Uiso 0.523(4) 1 calc GR . P A 2
H7AC H 0.266547 0.344211 0.282453 0.089 Uiso 0.523(4) 1 calc GR . P A 2
C8A C 0.2517(8) 0.5956(10) 0.1840(8) 0.048(4) Uani 0.523(4) 1 d D . P A 2
H8AA H 0.287358 0.642209 0.172359 0.072 Uiso 0.523(4) 1 calc GR . P A 2
H8AB H 0.218930 0.633556 0.204818 0.072 Uiso 0.523(4) 1 calc GR . P A 2
H8AC H 0.216880 0.561558 0.141156 0.072 Uiso 0.523(4) 1 calc GR . P A 2
C9A C 0.341(3) 0.551(2) 0.3405(9) 0.050(11) Uani 0.523(4) 1 d D . P A 2
H9AA H 0.374145 0.502379 0.374720 0.075 Uiso 0.523(4) 1 calc GR . P A 2
H9AB H 0.292508 0.565238 0.350254 0.075 Uiso 0.523(4) 1 calc GR . P A 2
H9AC H 0.371066 0.614381 0.344203 0.075 Uiso 0.523(4) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Si1 3.1155(18) . ?
U1 C13 2.772(8) . ?
U1 C14 2.757(8) . ?
U1 C15 2.725(7) . ?
U1 C16 2.737(7) . ?
U1 C20 2.718(8) . ?
U1 C24 2.776(8) . ?
U1 C25 2.760(8) . ?
U1 C26 2.758(7) . ?
U1 C27 2.775(8) . ?
U1 C31 2.756(8) . ?
Si1 Si2 2.329(5) . ?
Si1 Si3 2.382(4) . ?
Si1 Si4 2.379(4) . ?
Si1 Si2A 2.381(4) . ?
Si1 Si3A 2.359(4) . ?
Si1 Si4A 2.330(4) . ?
Si5 C10 1.876(14) . ?
Si5 C11 1.865(10) . ?
Si5 C12 1.852(12) . ?
Si5 C13 1.832(9) . ?
Si6 C16 1.843(8) . ?
Si6 C17 1.859(9) . ?
Si6 C18 1.874(8) . ?
Si6 C19 1.866(9) . ?
Si7 C21 1.867(11) . ?
Si7 C22 1.880(12) . ?
Si7 C23 1.872(11) . ?
Si7 C24 1.860(8) . ?
Si8 C27 1.853(8) . ?
Si8 C28 1.868(10) . ?
Si8 C29 1.866(14) . ?
Si8 C30 1.865(13) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.429(12) . ?
C13 C20 1.431(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.396(12) . ?
C15 H15 0.9500 . ?
C15 C16 1.432(12) . ?
C16 C20 1.425(11) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.444(11) . ?
C24 C31 1.431(11) . ?
C25 H25 0.9500 . ?
C25 C26 1.400(11) . ?
C26 H26 0.9500 . ?
C26 C27 1.433(11) . ?
C27 C31 1.427(11) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 0.9500 . ?
Si2 C1 1.882(8) . ?
Si2 C2 1.883(8) . ?
Si2 C3 1.887(8) . ?
Si3 C4 1.885(8) . ?
Si3 C5 1.884(9) . ?
Si3 C6 1.883(8) . ?
Si4 C7 1.884(8) . ?
Si4 C8 1.883(9) . ?
Si4 C9 1.885(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
Si2A C1A 1.882(8) . ?
Si2A C2A 1.889(8) . ?
Si2A C3A 1.884(8) . ?
Si3A C4A 1.884(8) . ?
Si3A C5A 1.879(8) . ?
Si3A C6A 1.883(8) . ?
Si4A C7A 1.884(8) . ?
Si4A C8A 1.885(8) . ?
Si4A C9A 1.882(8) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 U1 Si1 106.6(2) . . ?
C13 U1 C24 136.5(3) . . ?
C13 U1 C27 110.4(3) . . ?
C14 U1 Si1 136.48(19) . . ?
C14 U1 C13 30.0(3) . . ?
C14 U1 C24 106.6(3) . . ?
C14 U1 C25 133.4(3) . . ?
C14 U1 C26 122.8(3) . . ?
C14 U1 C27 92.9(3) . . ?
C15 U1 Si1 138.54(19) . . ?
C15 U1 C13 49.8(3) . . ?
C15 U1 C14 29.5(2) . . ?
C15 U1 C16 30.4(2) . . ?
C15 U1 C24 93.7(2) . . ?
C15 U1 C25 123.9(2) . . ?
C15 U1 C26 132.1(2) . . ?
C15 U1 C27 105.1(2) . . ?
C15 U1 C31 83.8(2) . . ?
C16 U1 Si1 108.55(18) . . ?
C16 U1 C13 50.7(2) . . ?
C16 U1 C14 49.6(3) . . ?
C16 U1 C24 111.4(2) . . ?
C16 U1 C25 136.8(2) . . ?
C16 U1 C26 159.4(2) . . ?
C16 U1 C27 135.4(2) . . ?
C16 U1 C31 111.5(2) . . ?
C20 U1 Si1 92.49(19) . . ?
C20 U1 C13 30.2(3) . . ?
C20 U1 C14 48.7(3) . . ?
C20 U1 C15 49.2(3) . . ?
C20 U1 C16 30.3(2) . . ?
C20 U1 C24 140.9(2) . . ?
C20 U1 C25 166.0(2) . . ?
C20 U1 C26 164.4(3) . . ?
C20 U1 C27 139.7(3) . . ?
C20 U1 C31 131.1(3) . . ?
C24 U1 Si1 116.85(18) . . ?
C25 U1 Si1 89.26(17) . . ?
C25 U1 C13 159.4(3) . . ?
C25 U1 C24 30.2(2) . . ?
C25 U1 C27 49.7(2) . . ?
C26 U1 Si1 89.15(17) . . ?
C26 U1 C13 135.2(3) . . ?
C26 U1 C24 49.2(2) . . ?
C26 U1 C25 29.4(2) . . ?
C26 U1 C27 30.0(2) . . ?
C27 U1 Si1 115.92(17) . . ?
C27 U1 C24 50.0(2) . . ?
C31 U1 Si1 136.37(17) . . ?
C31 U1 C13 111.7(3) . . ?
C31 U1 C14 84.4(3) . . ?
C31 U1 C24 30.0(2) . . ?
C31 U1 C25 49.1(2) . . ?
C31 U1 C26 48.7(2) . . ?
C31 U1 C27 29.9(2) . . ?
Si2 Si1 U1 124.50(13) . . ?
Si2 Si1 Si3 102.06(17) . . ?
Si2 Si1 Si4 103.65(18) . . ?
Si3 Si1 U1 108.31(12) . . ?
Si4 Si1 U1 115.54(13) . . ?
Si4 Si1 Si3 99.17(16) . . ?
Si2A Si1 U1 122.18(12) . . ?
Si3A Si1 U1 114.97(11) . . ?
Si3A Si1 Si2A 100.92(17) . . ?
Si4A Si1 U1 112.08(11) . . ?
Si4A Si1 Si2A 102.92(15) . . ?
Si4A Si1 Si3A 101.03(15) . . ?
C11 Si5 C10 110.5(6) . . ?
C12 Si5 C10 111.6(8) . . ?
C12 Si5 C11 111.1(7) . . ?
C13 Si5 C10 110.0(6) . . ?
C13 Si5 C11 104.9(5) . . ?
C13 Si5 C12 108.5(5) . . ?
C16 Si6 C17 108.6(4) . . ?
C16 Si6 C18 104.3(4) . . ?
C16 Si6 C19 110.6(4) . . ?
C17 Si6 C18 112.6(5) . . ?
C17 Si6 C19 111.2(5) . . ?
C19 Si6 C18 109.2(5) . . ?
C21 Si7 C22 109.1(6) . . ?
C21 Si7 C23 110.4(5) . . ?
C23 Si7 C22 108.7(6) . . ?
C24 Si7 C21 111.7(5) . . ?
C24 Si7 C22 105.9(5) . . ?
C24 Si7 C23 110.8(4) . . ?
C27 Si8 C28 111.3(4) . . ?
C27 Si8 C29 105.9(5) . . ?
C27 Si8 C30 110.9(5) . . ?
C29 Si8 C28 109.4(6) . . ?
C30 Si8 C28 110.4(6) . . ?
C30 Si8 C29 108.8(7) . . ?
Si5 C10 H10A 109.5 . . ?
Si5 C10 H10B 109.5 . . ?
Si5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si5 C11 H11A 109.5 . . ?
Si5 C11 H11B 109.5 . . ?
Si5 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si5 C12 H12A 109.5 . . ?
Si5 C12 H12B 109.5 . . ?
Si5 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si5 C13 U1 116.8(4) . . ?
C14 C13 U1 74.4(5) . . ?
C14 C13 Si5 127.0(7) . . ?
C14 C13 C20 104.3(7) . . ?
C20 C13 U1 72.8(4) . . ?
C20 C13 Si5 128.7(7) . . ?
U1 C14 H14 117.3 . . ?
C13 C14 U1 75.6(5) . . ?
C13 C14 H14 124.9 . . ?
C15 C14 U1 74.0(5) . . ?
C15 C14 C13 110.2(8) . . ?
C15 C14 H14 124.9 . . ?
U1 C15 H15 114.9 . . ?
C14 C15 U1 76.5(4) . . ?
C14 C15 H15 125.4 . . ?
C14 C15 C16 109.2(7) . . ?
C16 C15 U1 75.3(4) . . ?
C16 C15 H15 125.4 . . ?
Si6 C16 U1 111.7(3) . . ?
C15 C16 U1 74.4(4) . . ?
C15 C16 Si6 125.5(6) . . ?
C20 C16 U1 74.1(4) . . ?
C20 C16 Si6 129.3(7) . . ?
C20 C16 C15 104.9(7) . . ?
Si6 C17 H17A 109.5 . . ?
Si6 C17 H17B 109.5 . . ?
Si6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si6 C18 H18A 109.5 . . ?
Si6 C18 H18B 109.5 . . ?
Si6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si6 C19 H19A 109.5 . . ?
Si6 C19 H19B 109.5 . . ?
Si6 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
U1 C20 H20 114.8 . . ?
C13 C20 U1 77.0(5) . . ?
C13 C20 H20 124.3 . . ?
C16 C20 U1 75.6(4) . . ?
C16 C20 C13 111.4(8) . . ?
C16 C20 H20 124.3 . . ?
Si7 C21 H21A 109.5 . . ?
Si7 C21 H21B 109.5 . . ?
Si7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si7 C22 H22A 109.5 . . ?
Si7 C22 H22B 109.5 . . ?
Si7 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si7 C23 H23A 109.5 . . ?
Si7 C23 H23B 109.5 . . ?
Si7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si7 C24 U1 133.6(4) . . ?
C25 C24 U1 74.3(4) . . ?
C25 C24 Si7 124.1(6) . . ?
C31 C24 U1 74.2(4) . . ?
C31 C24 Si7 126.3(6) . . ?
C31 C24 C25 105.9(7) . . ?
U1 C25 H25 115.5 . . ?
C24 C25 U1 75.5(4) . . ?
C24 C25 H25 125.9 . . ?
C26 C25 U1 75.2(4) . . ?
C26 C25 C24 108.2(7) . . ?
C26 C25 H25 125.9 . . ?
U1 C26 H26 115.9 . . ?
C25 C26 U1 75.4(4) . . ?
C25 C26 H26 124.8 . . ?
C25 C26 C27 110.3(7) . . ?
C27 C26 U1 75.7(4) . . ?
C27 C26 H26 124.8 . . ?
Si8 C27 U1 132.7(4) . . ?
C26 C27 U1 74.3(4) . . ?
C26 C27 Si8 126.5(6) . . ?
C31 C27 U1 74.3(4) . . ?
C31 C27 Si8 124.8(6) . . ?
C31 C27 C26 105.2(7) . . ?
Si8 C28 H28A 109.5 . . ?
Si8 C28 H28B 109.5 . . ?
Si8 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
U1 C31 H31 115.5 . . ?
C24 C31 U1 75.8(4) . . ?
C24 C31 H31 124.8 . . ?
C27 C31 U1 75.8(4) . . ?
C27 C31 C24 110.4(7) . . ?
C27 C31 H31 124.8 . . ?
C1 Si2 Si1 116.7(13) . . ?
C1 Si2 C2 104.3(19) . . ?
C1 Si2 C3 104.6(11) . . ?
C2 Si2 Si1 112.8(11) . . ?
C2 Si2 C3 106.1(10) . . ?
C3 Si2 Si1 111.5(6) . . ?
C4 Si3 Si1 116.1(9) . . ?
C5 Si3 Si1 109.5(18) . . ?
C5 Si3 C4 106(2) . . ?
C6 Si3 Si1 111.1(6) . . ?
C6 Si3 C4 106.0(12) . . ?
C6 Si3 C5 107.5(15) . . ?
C7 Si4 Si1 115.7(17) . . ?
C7 Si4 C9 110.3(16) . . ?
C8 Si4 Si1 109.1(13) . . ?
C8 Si4 C7 107(3) . . ?
C8 Si4 C9 103.8(16) . . ?
C9 Si4 Si1 110.4(7) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1A Si2A Si1 113.6(12) . . ?
C1A Si2A C2A 105.7(10) . . ?
C1A Si2A C3A 106.0(17) . . ?
C2A Si2A Si1 109.5(5) . . ?
C3A Si2A Si1 115.9(13) . . ?
C3A Si2A C2A 105.3(9) . . ?
C4A Si3A Si1 114.9(7) . . ?
C5A Si3A Si1 111.3(7) . . ?
C5A Si3A C4A 109.2(11) . . ?
C5A Si3A C6A 106.7(13) . . ?
C6A Si3A Si1 110.7(15) . . ?
C6A Si3A C4A 103.4(17) . . ?
C7A Si4A Si1 116.4(13) . . ?
C7A Si4A C8A 104.8(12) . . ?
C8A Si4A Si1 110.0(5) . . ?
C9A Si4A Si1 112.6(18) . . ?
C9A Si4A C7A 104(2) . . ?
C9A Si4A C8A 108.7(12) . . ?
Si2A C1A H1AA 109.5 . . ?
Si2A C1A H1AB 109.5 . . ?
Si2A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
Si2A C2A H2AA 109.5 . . ?
Si2A C2A H2AB 109.5 . . ?
Si2A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
Si2A C3A H3AA 109.5 . . ?
Si2A C3A H3AB 109.5 . . ?
Si2A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
Si3A C4A H4AA 109.5 . . ?
Si3A C4A H4AB 109.5 . . ?
Si3A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
Si3A C5A H5AA 109.5 . . ?
Si3A C5A H5AB 109.5 . . ?
Si3A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
Si3A C6A H6AA 109.5 . . ?
Si3A C6A H6AB 109.5 . . ?
Si3A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
Si4A C7A H7AA 109.5 . . ?
Si4A C7A H7AB 109.5 . . ?
Si4A C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
Si4A C8A H8AA 109.5 . . ?
Si4A C8A H8AB 109.5 . . ?
Si4A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
Si4A C9A H9AA 109.5 . . ?
Si4A C9A H9AB 109.5 . . ?
Si4A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 C13 C14 C15 -66.6(6) . . . . ?
U1 C13 C20 C16 68.6(5) . . . . ?
U1 C14 C15 C16 -68.9(6) . . . . ?
U1 C15 C16 Si6 105.8(6) . . . . ?
U1 C15 C16 C20 -68.3(5) . . . . ?
U1 C16 C20 C13 -69.5(6) . . . . ?
U1 C24 C25 C26 68.8(5) . . . . ?
U1 C24 C31 C27 -68.6(6) . . . . ?
U1 C25 C26 C27 68.3(6) . . . . ?
U1 C26 C27 Si8 -131.9(7) . . . . ?
U1 C26 C27 C31 68.5(5) . . . . ?
U1 C27 C31 C24 68.6(6) . . . . ?
Si5 C13 C14 U1 -112.1(6) . . . . ?
Si5 C13 C14 C15 -178.7(6) . . . . ?
Si5 C13 C20 U1 110.9(6) . . . . ?
Si5 C13 C20 C16 179.5(6) . . . . ?
Si6 C16 C20 U1 -105.3(6) . . . . ?
Si6 C16 C20 C13 -174.8(6) . . . . ?
Si7 C24 C25 U1 132.4(6) . . . . ?
Si7 C24 C25 C26 -158.8(6) . . . . ?
Si7 C24 C31 U1 -133.0(6) . . . . ?
Si7 C24 C31 C27 158.4(6) . . . . ?
Si8 C27 C31 U1 131.5(7) . . . . ?
Si8 C27 C31 C24 -159.9(6) . . . . ?
C10 Si5 C13 U1 111.3(6) . . . . ?
C10 Si5 C13 C14 -158.4(8) . . . . ?
C10 Si5 C13 C20 22.5(9) . . . . ?
C11 Si5 C13 U1 -7.5(6) . . . . ?
C11 Si5 C13 C14 82.7(8) . . . . ?
C11 Si5 C13 C20 -96.4(8) . . . . ?
C12 Si5 C13 U1 -126.3(7) . . . . ?
C12 Si5 C13 C14 -36.0(10) . . . . ?
C12 Si5 C13 C20 144.9(9) . . . . ?
C13 C14 C15 U1 67.6(6) . . . . ?
C13 C14 C15 C16 -1.2(10) . . . . ?
C14 C13 C20 U1 -68.4(5) . . . . ?
C14 C13 C20 C16 0.3(9) . . . . ?
C14 C15 C16 U1 69.7(6) . . . . ?
C14 C15 C16 Si6 175.5(6) . . . . ?
C14 C15 C16 C20 1.4(9) . . . . ?
C15 C16 C20 U1 68.5(5) . . . . ?
C15 C16 C20 C13 -1.0(9) . . . . ?
C17 Si6 C16 U1 124.7(5) . . . . ?
C17 Si6 C16 C15 38.9(8) . . . . ?
C17 Si6 C16 C20 -148.5(7) . . . . ?
C18 Si6 C16 U1 4.4(5) . . . . ?
C18 Si6 C16 C15 -81.5(7) . . . . ?
C18 Si6 C16 C20 91.2(7) . . . . ?
C19 Si6 C16 U1 -113.0(4) . . . . ?
C19 Si6 C16 C15 161.2(7) . . . . ?
C19 Si6 C16 C20 -26.2(8) . . . . ?
C20 C13 C14 U1 67.2(5) . . . . ?
C20 C13 C14 C15 0.6(9) . . . . ?
C21 Si7 C24 U1 -47.3(7) . . . . ?
C21 Si7 C24 C25 -148.4(7) . . . . ?
C21 Si7 C24 C31 56.2(9) . . . . ?
C22 Si7 C24 U1 -166.0(7) . . . . ?
C22 Si7 C24 C25 92.9(8) . . . . ?
C22 Si7 C24 C31 -62.4(9) . . . . ?
C23 Si7 C24 U1 76.3(6) . . . . ?
C23 Si7 C24 C25 -24.9(8) . . . . ?
C23 Si7 C24 C31 179.8(7) . . . . ?
C24 C25 C26 U1 -69.0(5) . . . . ?
C24 C25 C26 C27 -0.6(9) . . . . ?
C25 C24 C31 U1 68.1(5) . . . . ?
C25 C24 C31 C27 -0.5(9) . . . . ?
C25 C26 C27 U1 -68.1(5) . . . . ?
C25 C26 C27 Si8 159.9(6) . . . . ?
C25 C26 C27 C31 0.3(9) . . . . ?
C26 C27 C31 U1 -68.5(5) . . . . ?
C26 C27 C31 C24 0.2(9) . . . . ?
C28 Si8 C27 U1 -74.2(7) . . . . ?
C28 Si8 C27 C26 28.8(9) . . . . ?
C28 Si8 C27 C31 -175.4(8) . . . . ?
C29 Si8 C27 U1 167.0(7) . . . . ?
C29 Si8 C27 C26 -90.0(9) . . . . ?
C29 Si8 C27 C31 65.8(10) . . . . ?
C30 Si8 C27 U1 49.1(7) . . . . ?
C30 Si8 C27 C26 152.1(8) . . . . ?
C30 Si8 C27 C31 -52.0(10) . . . . ?
C31 C24 C25 U1 -68.1(5) . . . . ?
C31 C24 C25 C26 0.7(8) . . . . ?

_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 5.30s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_type   custom
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.906
_oxdiff_exptl_absorpt_empirical_full_min 0.422
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-Nd
_database_code_depnum_ccdc_archive 'CCDC 2195639'
loop_
_audit_author_name
_audit_author_address
'Ashley Wooles'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-08 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_manchester_internal_diff_code   ldpm171
_manchester_internal_coll_client IV
_manchester_internal_coll_user   IV
_manchester_internal_coll_date   27/11/2020
_manchester_internal_process_date 27/11/2020
_manchester_internal_process_user BR
_manchester_internal_solution_date 09/12/2020
_manchester_internal_solution_user BR
_manchester_internal_refinement_date 09/12/2020
_manchester_internal_refinement_user BR
_manchester_internal_validation_date 15/12/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 15/12/2020
_manchester_internal_archive_user AW
_refine_special_details          
;Refined as a two component Twin. Twin law: 

2-axis (   1   0   0 ) [   3   0   1 ], Angle () [] =  1.57 Deg, Freq =    44                                                       
        *************                
( 1.000    0.000    0.622)   (h1)   (h2)                   Nr Overlap =   980                                                       
( 0.000   -1.000    0.000) * (k1) = (k2)                         BASF =  0.36                                                       
( 0.000    0.000   -1.000)   (l1)   (l2)                        DEL-R =-0.040  

The Si(SiMe3)3 group is disordered over two orientations. 
The occupancies were allowed to freely refine converging at a final ratio of 0.53:0.47.
 Selected chemically equivalent Si-Si and Si-C distances within the disordered silyls were restrained to be approximately equal.
 Enhanced rigid bond and similarity thermal restraints were applied to the disordered silyl. 
Antibumping restraints were applied to prevent close H-H contacts in disordered components.,Twin
;
_audit_creation_date             2020-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        "[Nd(Cp'')2{Si(SiMe3)3}]"
_chemical_formula_moiety         'C31 H69 Nd Si8'
_chemical_formula_sum            'C31 H69 Nd Si8'
_chemical_formula_weight         810.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nd Si8 C31'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.7679(5)
_cell_length_b                   13.2234(3)
_cell_length_c                   20.3700(6)
_cell_angle_alpha                90
_cell_angle_beta                 110.891(3)
_cell_angle_gamma                90
_cell_volume                     4471.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.5710
_cell_measurement_theta_min      2.6430
_shelx_estimated_absorpt_T_max   0.608
_shelx_estimated_absorpt_T_min   0.189
_exptl_absorpt_coefficient_mu    11.038
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -9 0 0.0252
1 9 0 0.0252
-5 1 13 0.1081
5 -1 -13 0.1081
10 -1 1 0.0288
-10 1 -1 0.0898

_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method 
'Crystallised from concentrated pentane solution at -25oC'
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9831 -8.9820 -0.0808 0.9810 -0.3763 0.0272
0.9831 8.9820 0.0808 -0.9810 0.3763 -0.0272
-4.9851 0.9956 13.0286 -0.0646 0.0759 -0.9906
4.9851 -0.9956 -13.0286 0.0646 -0.0759 0.9906
10.0231 -0.9936 0.9659 -0.3170 -0.9140 -0.0251
-10.0231 0.9936 -0.9659 0.3170 0.9140 0.0251

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7945
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.841
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    103.00 133.00   1.00    1.00    --   44.70  60.00 -60.00   30
  2  ω     27.00 134.00   1.00    1.00    --   44.70  20.00-120.00  107
  3  ω    -45.00  35.00   1.00    1.00    --   44.70  60.00 120.00   80
  4  ω    -45.00   3.00   1.00    1.00    --   44.70  60.00 -60.00   48
  5  ω    -44.00   4.00   1.00    1.00    --   44.70  60.00-120.00   48
  6  ω     67.00 134.00   1.00    1.00    --   44.70  60.00 120.00   67
  7  ω     28.00  53.00   1.00    1.00    --  108.20  50.00 -30.00   25
  8  ω     68.00 180.00   1.00    1.00    --  108.20  50.00-150.00  112
  9  ω     68.00 197.00   1.00    1.00    --  108.20  50.00 -90.00  129
 10  ω     20.00 197.00   1.00    1.00    --  108.20  50.00 -60.00  177
 11  ω    127.00 154.00   1.00    1.00    --  108.20  50.00-180.00   27
 12  ω     40.00  89.00   1.00    1.00    --  108.20  50.00-180.00   49
 13  ω     20.00 196.00   1.00    1.00    --  108.20  50.00-120.00  176
 14  ω    151.00 176.00   1.00    1.00    --  108.20  50.00 -30.00   25
 15  ω    107.00 134.00   1.00    1.00    --  108.20  30.00  90.00   27
 16  ω    148.00 173.00   1.00    1.00    --  108.20  50.00 150.00   25
 17  ω     38.00  73.00   1.00    1.00    --  108.20  30.00  90.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407886000
_diffrn_orient_matrix_UB_12      -0.1046392000
_diffrn_orient_matrix_UB_13      -0.0125724000
_diffrn_orient_matrix_UB_21      -0.0832198000
_diffrn_orient_matrix_UB_22      0.0512741000
_diffrn_orient_matrix_UB_23      -0.0299364000
_diffrn_orient_matrix_UB_31      0.0043615000
_diffrn_orient_matrix_UB_32      -0.0028412000
_diffrn_orient_matrix_UB_33      -0.0741461000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7409
_reflns_number_total             7945
_reflns_odcompleteness_completeness 96.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.074
_refine_diff_density_min         -1.875
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7945
_refine_ls_number_restraints     830
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0680
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0942P)²+30.9131P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2147
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si3-C4 \\sim Si3-C5 \\sim Si3-C6 \\sim Si4A-C7A \\sim Si4A-C9A \\sim Si4A-C8A
\\sim Si4-C7 \\sim Si4-C9 ~
 Si4-C8 \\sim Si2A-C1A \\sim Si2A-C3A \\sim Si2A-C2A \\sim Si2-C2 \\sim Si2-C3
\\sim Si2-C1 \\sim Si3A-C4A
 \\sim Si3A-C6A \\sim Si3A-C5A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Si1 \\sim Si2 \\sim Si3 \\sim Si4 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim Si2A \\sim Si3A \\sim Si4A \\sim C1A
\\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Si2A)=Sof(Si3A)=Sof(Si4A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(Si2)=Sof(Si3)=Sof(Si4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C20(H20), C21(H21), C26(H26), C27(H27)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,
 H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,
 H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.55604(3) 0.38223(3) 0.26234(3) 0.02735(18) Uani 1 1 d . U . . .
Si1 Si 0.42438(13) 0.54973(17) 0.22295(12) 0.0251(5) Uani 1 1 d . U . . .
Si2 Si 0.3576(3) 0.5740(3) 0.3040(2) 0.0303(11) Uani 0.532(5) 1 d D U P A 1
Si3 Si 0.3132(3) 0.4899(3) 0.1255(2) 0.0279(10) Uani 0.532(5) 1 d D U P A 1
Si4 Si 0.4413(3) 0.7123(3) 0.1878(3) 0.0329(11) Uani 0.532(5) 1 d D U P A 1
Si5 Si 0.67622(15) 0.5125(2) 0.44701(15) 0.0399(6) Uani 1 1 d . U . . .
Si6 Si 0.67694(14) 0.49192(18) 0.15802(13) 0.0286(5) Uani 1 1 d . U . . .
Si7 Si 0.52870(18) 0.1424(2) 0.11546(16) 0.0383(6) Uani 1 1 d . U . . .
Si8 Si 0.53261(19) 0.1513(2) 0.39886(16) 0.0437(7) Uani 1 1 d . U . . .
C1 C 0.352(3) 0.4521(17) 0.3500(13) 0.028(5) Uani 0.532(5) 1 d D U P A 1
H1A H 0.326491 0.464499 0.384550 0.042 Uiso 0.532(5) 1 calc GR . P A 1
H1B H 0.406698 0.425843 0.373857 0.042 Uiso 0.532(5) 1 calc GR . P A 1
H1C H 0.320444 0.402524 0.315369 0.042 Uiso 0.532(5) 1 calc GR . P A 1
C2 C 0.4129(9) 0.6682(12) 0.3737(9) 0.036(4) Uani 0.532(5) 1 d D U P A 1
H2A H 0.374012 0.713811 0.382501 0.055 Uiso 0.532(5) 1 calc GR . P A 1
H2B H 0.449838 0.707592 0.357736 0.055 Uiso 0.532(5) 1 calc GR . P A 1
H2C H 0.443520 0.632365 0.417097 0.055 Uiso 0.532(5) 1 calc GR . P A 1
C3 C 0.2506(9) 0.621(2) 0.2683(14) 0.036(5) Uani 0.532(5) 1 d D U P A 1
H3A H 0.215640 0.568714 0.238972 0.054 Uiso 0.532(5) 1 calc GR . P A 1
H3B H 0.247693 0.682001 0.239914 0.054 Uiso 0.532(5) 1 calc GR . P A 1
H3C H 0.232776 0.637639 0.307351 0.054 Uiso 0.532(5) 1 calc GR . P A 1
C4 C 0.2551(10) 0.3873(12) 0.1508(10) 0.033(4) Uani 0.532(5) 1 d D U P A 1
H4A H 0.292759 0.338140 0.181234 0.050 Uiso 0.532(5) 1 calc GR . P A 1
H4B H 0.219532 0.353250 0.108307 0.050 Uiso 0.532(5) 1 calc GR . P A 1
H4C H 0.222662 0.417254 0.175909 0.050 Uiso 0.532(5) 1 calc GR . P A 1
C5 C 0.2368(11) 0.5894(14) 0.0793(12) 0.039(4) Uani 0.532(5) 1 d D U P A 1
H5A H 0.215341 0.620300 0.112687 0.059 Uiso 0.532(5) 1 calc GR . P A 1
H5B H 0.192775 0.558254 0.040770 0.059 Uiso 0.532(5) 1 calc GR . P A 1
H5C H 0.262667 0.641546 0.060366 0.059 Uiso 0.532(5) 1 calc GR . P A 1
C6 C 0.346(3) 0.440(2) 0.0535(19) 0.034(5) Uani 0.532(5) 1 d D U P A 1
H6A H 0.375271 0.493109 0.038650 0.050 Uiso 0.532(5) 1 calc GR . P A 1
H6B H 0.298923 0.419251 0.013361 0.050 Uiso 0.532(5) 1 calc GR . P A 1
H6C H 0.381882 0.381692 0.070903 0.050 Uiso 0.532(5) 1 calc GR . P A 1
C7 C 0.4465(12) 0.7117(16) 0.0970(6) 0.037(4) Uani 0.532(5) 1 d D U P A 1
H7A H 0.479392 0.654493 0.092595 0.056 Uiso 0.532(5) 1 calc GR . P A 1
H7B H 0.470781 0.775029 0.089290 0.056 Uiso 0.532(5) 1 calc GR . P A 1
H7C H 0.392017 0.705371 0.062035 0.056 Uiso 0.532(5) 1 calc GR . P A 1
C8 C 0.3590(13) 0.8047(17) 0.1836(14) 0.042(5) Uani 0.532(5) 1 d D U P A 1
H8A H 0.308264 0.782616 0.147763 0.063 Uiso 0.532(5) 1 calc GR . P A 1
H8B H 0.373196 0.871908 0.171481 0.063 Uiso 0.532(5) 1 calc GR . P A 1
H8C H 0.352585 0.807489 0.229424 0.063 Uiso 0.532(5) 1 calc GR . P A 1
C9 C 0.5348(12) 0.777(2) 0.2482(11) 0.035(5) Uani 0.532(5) 1 d D U P A 1
H9A H 0.536154 0.772863 0.296677 0.053 Uiso 0.532(5) 1 calc GR . P A 1
H9B H 0.534482 0.847848 0.234506 0.053 Uiso 0.532(5) 1 calc GR . P A 1
H9C H 0.582546 0.743164 0.244992 0.053 Uiso 0.532(5) 1 calc GR . P A 1
C10 C 0.6793(9) 0.6526(10) 0.4507(9) 0.069(4) Uani 1 1 d . U . . .
H10A H 0.635370 0.680068 0.410334 0.104 Uiso 1 1 calc GR . . . .
H10B H 0.731037 0.676305 0.449495 0.104 Uiso 1 1 calc GR . . . .
H10C H 0.673138 0.675384 0.494300 0.104 Uiso 1 1 calc GR . . . .
C11 C 0.5762(7) 0.4670(9) 0.4471(7) 0.052(3) Uani 1 1 d . U . . .
H11A H 0.565057 0.498103 0.486364 0.079 Uiso 1 1 calc GR . . . .
H11B H 0.577532 0.393262 0.452338 0.079 Uiso 1 1 calc GR . . . .
H11C H 0.533856 0.485810 0.402754 0.079 Uiso 1 1 calc GR . . . .
C12 C 0.7597(8) 0.4567(15) 0.5223(6) 0.082(5) Uani 1 1 d . U . . .
H12A H 0.811151 0.485888 0.524138 0.123 Uiso 1 1 calc GR . . . .
H12B H 0.760859 0.383312 0.516146 0.123 Uiso 1 1 calc GR . . . .
H12C H 0.751088 0.471654 0.566210 0.123 Uiso 1 1 calc GR . . . .
C13 C 0.6871(5) 0.4679(7) 0.3636(5) 0.0335(18) Uani 1 1 d . U . . .
C14 C 0.7127(5) 0.3695(7) 0.3518(5) 0.0333(18) Uani 1 1 d . U . . .
H14 H 0.725678 0.315212 0.384443 0.040 Uiso 1 1 calc R . . . .
C15 C 0.7153(5) 0.3666(7) 0.2841(5) 0.0330(18) Uani 1 1 d . U . . .
H15 H 0.730948 0.309662 0.263571 0.040 Uiso 1 1 calc R . . . .
C16 C 0.6913(6) 0.4609(7) 0.2509(5) 0.0329(18) Uani 1 1 d . U . . .
C17 C 0.7560(6) 0.4261(8) 0.1342(6) 0.041(2) Uani 1 1 d . U . . .
H17A H 0.808734 0.455838 0.160561 0.061 Uiso 1 1 calc GR . . . .
H17B H 0.744632 0.433693 0.083730 0.061 Uiso 1 1 calc GR . . . .
H17C H 0.756482 0.354160 0.145839 0.061 Uiso 1 1 calc GR . . . .
C18 C 0.5728(6) 0.4451(8) 0.1063(6) 0.042(2) Uani 1 1 d . U . . .
H18A H 0.572872 0.371011 0.105311 0.062 Uiso 1 1 calc GR . . . .
H18B H 0.555997 0.471186 0.058179 0.062 Uiso 1 1 calc GR . . . .
H18C H 0.535265 0.468684 0.128438 0.062 Uiso 1 1 calc GR . . . .
C19 C 0.6814(6) 0.6310(7) 0.1450(6) 0.041(2) Uani 1 1 d . U . . .
H19A H 0.650402 0.665954 0.169435 0.062 Uiso 1 1 calc GR . . . .
H19B H 0.658541 0.646551 0.094704 0.062 Uiso 1 1 calc GR . . . .
H19C H 0.737598 0.653549 0.164026 0.062 Uiso 1 1 calc GR . . . .
C20 C 0.6740(6) 0.5237(7) 0.3000(5) 0.0339(19) Uani 1 1 d . U . . .
H20 H 0.656508 0.592024 0.292078 0.041 Uiso 1 1 calc R . . . .
C21 C 0.5586(5) 0.1768(7) 0.2648(5) 0.0324(18) Uani 1 1 d . U . . .
H21 H 0.611030 0.147949 0.280941 0.039 Uiso 1 1 calc R . . . .
C22 C 0.5136(6) 0.1988(7) 0.1941(5) 0.0337(18) Uani 1 1 d . U . . .
C23 C 0.6334(7) 0.1576(10) 0.1181(7) 0.053(3) Uani 1 1 d . U . . .
H23A H 0.642466 0.228212 0.108271 0.079 Uiso 1 1 calc GR . . . .
H23B H 0.642082 0.113705 0.082724 0.079 Uiso 1 1 calc GR . . . .
H23C H 0.671167 0.138995 0.164852 0.079 Uiso 1 1 calc GR . . . .
C24 C 0.5082(10) 0.0043(9) 0.1176(8) 0.069(4) Uani 1 1 d . U . . .
H24A H 0.554337 -0.028640 0.153038 0.103 Uiso 1 1 calc GR . . . .
H24B H 0.499720 -0.025297 0.071347 0.103 Uiso 1 1 calc GR . . . .
H24C H 0.459928 -0.005777 0.129398 0.103 Uiso 1 1 calc GR . . . .
C25 C 0.4556(6) 0.1978(9) 0.0330(6) 0.044(2) Uani 1 1 d . U . . .
H25A H 0.400668 0.189478 0.032749 0.065 Uiso 1 1 calc GR . . . .
H25B H 0.460619 0.163089 -0.007695 0.065 Uiso 1 1 calc GR . . . .
H25C H 0.467128 0.269945 0.030830 0.065 Uiso 1 1 calc GR . . . .
C26 C 0.4401(5) 0.2434(7) 0.1944(5) 0.0296(17) Uani 1 1 d . U . . .
H26 H 0.397552 0.267580 0.154243 0.036 Uiso 1 1 calc R . . . .
C27 C 0.4411(5) 0.2456(7) 0.2632(5) 0.0292(17) Uani 1 1 d . U . . .
H27 H 0.399002 0.271216 0.276975 0.035 Uiso 1 1 calc R . . . .
C28 C 0.5146(6) 0.2038(7) 0.3095(5) 0.0343(18) Uani 1 1 d . U . . .
C29 C 0.4650(7) 0.2116(9) 0.4400(6) 0.046(2) Uani 1 1 d . U . . .
H29A H 0.479776 0.282936 0.449823 0.068 Uiso 1 1 calc GR . . . .
H29B H 0.470785 0.176722 0.483965 0.068 Uiso 1 1 calc GR . . . .
H29C H 0.408948 0.206874 0.407724 0.068 Uiso 1 1 calc GR . . . .
C30 C 0.6403(7) 0.1650(11) 0.4559(7) 0.061(3) Uani 1 1 d . U . . .
H30A H 0.674521 0.148369 0.428878 0.092 Uiso 1 1 calc GR . . . .
H30B H 0.652480 0.118900 0.496073 0.092 Uiso 1 1 calc GR . . . .
H30C H 0.650619 0.234779 0.472885 0.092 Uiso 1 1 calc GR . . . .
C31 C 0.5078(11) 0.0154(10) 0.3867(8) 0.075(4) Uani 1 1 d . U . . .
H31A H 0.453477 0.007034 0.351745 0.113 Uiso 1 1 calc GR . . . .
H31B H 0.509964 -0.014042 0.431492 0.113 Uiso 1 1 calc GR . . . .
H31C H 0.546762 -0.019006 0.370395 0.113 Uiso 1 1 calc GR . . . .
Si2A Si 0.4496(3) 0.7190(4) 0.2659(3) 0.0315(12) Uani 0.468(5) 1 d D U P A 2
Si3A Si 0.3130(3) 0.5045(4) 0.2501(3) 0.0263(11) Uani 0.468(5) 1 d D U P A 2
Si4A Si 0.3634(3) 0.5795(4) 0.1009(3) 0.0292(12) Uani 0.468(5) 1 d D U P A 2
C1A C 0.4525(16) 0.7282(18) 0.3589(7) 0.042(4) Uani 0.468(5) 1 d D U P A 2
H1AA H 0.488193 0.675714 0.387594 0.063 Uiso 0.468(5) 1 calc GR . P A 2
H1AB H 0.398068 0.718682 0.359623 0.063 Uiso 0.468(5) 1 calc GR . P A 2
H1AC H 0.472697 0.794943 0.378065 0.063 Uiso 0.468(5) 1 calc GR . P A 2
C2A C 0.5490(11) 0.769(3) 0.2665(16) 0.035(5) Uani 0.468(5) 1 d D U P A 2
H2AA H 0.553864 0.840833 0.279906 0.053 Uiso 0.468(5) 1 calc GR . P A 2
H2AB H 0.551731 0.762207 0.219544 0.053 Uiso 0.468(5) 1 calc GR . P A 2
H2AC H 0.593001 0.730981 0.300426 0.053 Uiso 0.468(5) 1 calc GR . P A 2
C3A C 0.3702(15) 0.8122(19) 0.2146(14) 0.041(5) Uani 0.468(5) 1 d D U P A 2
H3AA H 0.381783 0.878538 0.237368 0.062 Uiso 0.468(5) 1 calc GR . P A 2
H3AB H 0.317200 0.788927 0.213004 0.062 Uiso 0.468(5) 1 calc GR . P A 2
H3AC H 0.370266 0.817505 0.166597 0.062 Uiso 0.468(5) 1 calc GR . P A 2
C4A C 0.341(3) 0.451(3) 0.3415(10) 0.029(5) Uani 0.468(5) 1 d D U P A 2
H4AA H 0.377594 0.394375 0.347298 0.043 Uiso 0.468(5) 1 calc GR . P A 2
H4AB H 0.291775 0.428407 0.348769 0.043 Uiso 0.468(5) 1 calc GR . P A 2
H4AC H 0.366857 0.504093 0.375938 0.043 Uiso 0.468(5) 1 calc GR . P A 2
C5A C 0.2401(14) 0.6104(19) 0.2445(15) 0.032(5) Uani 0.468(5) 1 d D U P A 2
H5AA H 0.266545 0.662036 0.279630 0.048 Uiso 0.468(5) 1 calc GR . P A 2
H5AB H 0.193203 0.583660 0.253451 0.048 Uiso 0.468(5) 1 calc GR . P A 2
H5AC H 0.222532 0.640484 0.197456 0.048 Uiso 0.468(5) 1 calc GR . P A 2
C6A C 0.2526(11) 0.4041(12) 0.1881(9) 0.030(4) Uani 0.468(5) 1 d D U P A 2
H6AA H 0.226617 0.433307 0.141254 0.046 Uiso 0.468(5) 1 calc GR . P A 2
H6AB H 0.211432 0.377692 0.205201 0.046 Uiso 0.468(5) 1 calc GR . P A 2
H6AC H 0.288446 0.348985 0.185728 0.046 Uiso 0.468(5) 1 calc GR . P A 2
C7A C 0.356(3) 0.4561(18) 0.053(2) 0.030(5) Uani 0.468(5) 1 d D U P A 2
H7AA H 0.324635 0.407562 0.069281 0.046 Uiso 0.468(5) 1 calc GR . P A 2
H7AB H 0.409675 0.429228 0.061500 0.046 Uiso 0.468(5) 1 calc GR . P A 2
H7AC H 0.328248 0.467325 0.002153 0.046 Uiso 0.468(5) 1 calc GR . P A 2
C8A C 0.2581(8) 0.6322(19) 0.0702(14) 0.038(4) Uani 0.468(5) 1 d D U P A 2
H8AA H 0.241044 0.649197 0.020157 0.057 Uiso 0.468(5) 1 calc GR . P A 2
H8AB H 0.257058 0.693190 0.097154 0.057 Uiso 0.468(5) 1 calc GR . P A 2
H8AC H 0.221380 0.581590 0.077202 0.057 Uiso 0.468(5) 1 calc GR . P A 2
C9A C 0.4225(13) 0.6684(16) 0.0657(12) 0.041(4) Uani 0.468(5) 1 d D U P A 2
H9AA H 0.385757 0.716465 0.033258 0.061 Uiso 0.468(5) 1 calc GR . P A 2
H9AB H 0.451047 0.629626 0.040784 0.061 Uiso 0.468(5) 1 calc GR . P A 2
H9AC H 0.461671 0.705354 0.104756 0.061 Uiso 0.468(5) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 Si1 3.112(2) . ?
Nd1 C13 2.745(9) . ?
Nd1 C14 2.734(9) . ?
Nd1 C15 2.712(9) . ?
Nd1 C16 2.704(9) . ?
Nd1 C20 2.709(9) . ?
Nd1 C21 2.717(9) . ?
Nd1 C22 2.764(9) . ?
Nd1 C26 2.738(9) . ?
Nd1 C27 2.731(8) . ?
Nd1 C28 2.745(9) . ?
Si1 Si2 2.374(5) . ?
Si1 Si3 2.382(5) . ?
Si1 Si4 2.319(5) . ?
Si1 Si2A 2.386(6) . ?
Si1 Si3A 2.314(6) . ?
Si1 Si4A 2.364(6) . ?
Si2 C1 1.884(9) . ?
Si2 C2 1.881(8) . ?
Si2 C3 1.883(8) . ?
Si3 C4 1.883(8) . ?
Si3 C5 1.884(8) . ?
Si3 C6 1.885(8) . ?
Si4 C7 1.883(8) . ?
Si4 C8 1.885(8) . ?
Si4 C9 1.883(8) . ?
Si5 C10 1.853(14) . ?
Si5 C11 1.877(11) . ?
Si5 C12 1.864(13) . ?
Si5 C13 1.873(10) . ?
Si6 C16 1.862(10) . ?
Si6 C17 1.858(10) . ?
Si6 C18 1.878(10) . ?
Si6 C19 1.863(10) . ?
Si7 C22 1.870(10) . ?
Si7 C23 1.853(11) . ?
Si7 C24 1.866(12) . ?
Si7 C25 1.867(12) . ?
Si8 C28 1.866(10) . ?
Si8 C29 1.871(11) . ?
Si8 C30 1.860(13) . ?
Si8 C31 1.846(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.425(13) . ?
C13 C20 1.437(14) . ?
C14 H14 0.9500 . ?
C14 C15 1.396(14) . ?
C15 H15 0.9500 . ?
C15 C16 1.410(13) . ?
C16 C20 1.415(13) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.406(14) . ?
C21 C28 1.441(13) . ?
C22 C26 1.436(12) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.394(13) . ?
C27 H27 0.9500 . ?
C27 C28 1.422(13) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Si2A C1A 1.882(8) . ?
Si2A C2A 1.882(8) . ?
Si2A C3A 1.885(8) . ?
Si3A C4A 1.884(9) . ?
Si3A C5A 1.883(8) . ?
Si3A C6A 1.882(8) . ?
Si4A C7A 1.885(8) . ?
Si4A C8A 1.881(8) . ?
Si4A C9A 1.881(8) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Nd1 Si1 105.0(2) . . ?
C13 Nd1 C22 138.3(3) . . ?
C13 Nd1 C28 110.7(3) . . ?
C14 Nd1 Si1 135.1(2) . . ?
C14 Nd1 C13 30.2(3) . . ?
C14 Nd1 C22 108.2(3) . . ?
C14 Nd1 C26 134.4(3) . . ?
C14 Nd1 C28 92.9(3) . . ?
C15 Nd1 Si1 137.8(2) . . ?
C15 Nd1 C13 49.6(3) . . ?
C15 Nd1 C14 29.7(3) . . ?
C15 Nd1 C21 84.9(3) . . ?
C15 Nd1 C22 95.6(3) . . ?
C15 Nd1 C26 125.8(3) . . ?
C15 Nd1 C27 133.5(3) . . ?
C15 Nd1 C28 105.8(3) . . ?
C16 Nd1 Si1 108.3(2) . . ?
C16 Nd1 C13 50.5(3) . . ?
C16 Nd1 C14 49.9(3) . . ?
C16 Nd1 C15 30.2(3) . . ?
C16 Nd1 C20 30.3(3) . . ?
C16 Nd1 C21 112.1(3) . . ?
C16 Nd1 C22 112.7(3) . . ?
C16 Nd1 C26 138.3(3) . . ?
C16 Nd1 C27 160.8(3) . . ?
C16 Nd1 C28 135.9(3) . . ?
C20 Nd1 Si1 90.9(2) . . ?
C20 Nd1 C13 30.5(3) . . ?
C20 Nd1 C14 49.7(3) . . ?
C20 Nd1 C15 49.4(3) . . ?
C20 Nd1 C21 132.8(3) . . ?
C20 Nd1 C22 142.5(3) . . ?
C20 Nd1 C26 166.7(3) . . ?
C20 Nd1 C27 163.8(3) . . ?
C20 Nd1 C28 140.5(3) . . ?
C21 Nd1 Si1 136.3(2) . . ?
C21 Nd1 C13 113.2(3) . . ?
C21 Nd1 C14 85.4(3) . . ?
C21 Nd1 C22 29.7(3) . . ?
C21 Nd1 C26 49.0(3) . . ?
C21 Nd1 C27 49.2(3) . . ?
C21 Nd1 C28 30.6(3) . . ?
C22 Nd1 Si1 116.7(2) . . ?
C26 Nd1 Si1 89.20(19) . . ?
C26 Nd1 C13 160.1(3) . . ?
C26 Nd1 C22 30.3(3) . . ?
C26 Nd1 C28 49.7(3) . . ?
C27 Nd1 Si1 88.70(19) . . ?
C27 Nd1 C13 134.8(3) . . ?
C27 Nd1 C14 122.8(3) . . ?
C27 Nd1 C22 49.6(3) . . ?
C27 Nd1 C26 29.5(3) . . ?
C27 Nd1 C28 30.1(3) . . ?
C28 Nd1 Si1 115.5(2) . . ?
C28 Nd1 C22 50.4(3) . . ?
Si2 Si1 Nd1 115.68(14) . . ?
Si2 Si1 Si3 98.77(17) . . ?
Si3 Si1 Nd1 107.59(13) . . ?
Si4 Si1 Nd1 124.82(14) . . ?
Si4 Si1 Si2 103.98(19) . . ?
Si4 Si1 Si3 102.19(18) . . ?
Si2A Si1 Nd1 123.19(15) . . ?
Si3A Si1 Nd1 112.50(14) . . ?
Si3A Si1 Si2A 102.7(2) . . ?
Si3A Si1 Si4A 100.57(19) . . ?
Si4A Si1 Nd1 114.24(15) . . ?
Si4A Si1 Si2A 100.7(2) . . ?
C1 Si2 Si1 110.9(13) . . ?
C2 Si2 Si1 111.0(6) . . ?
C2 Si2 C1 107.3(11) . . ?
C2 Si2 C3 104.8(10) . . ?
C3 Si2 Si1 117.5(9) . . ?
C3 Si2 C1 104.6(16) . . ?
C4 Si3 Si1 112.6(6) . . ?
C4 Si3 C5 105.8(9) . . ?
C4 Si3 C6 108.3(11) . . ?
C5 Si3 Si1 114.8(8) . . ?
C5 Si3 C6 103.0(17) . . ?
C6 Si3 Si1 111.6(13) . . ?
C7 Si4 Si1 110.9(7) . . ?
C7 Si4 C8 105.5(11) . . ?
C7 Si4 C9 107.6(11) . . ?
C8 Si4 Si1 115.5(9) . . ?
C9 Si4 Si1 113.5(10) . . ?
C9 Si4 C8 103.1(14) . . ?
C10 Si5 C11 109.6(6) . . ?
C10 Si5 C12 111.0(8) . . ?
C10 Si5 C13 109.9(6) . . ?
C12 Si5 C11 110.4(7) . . ?
C12 Si5 C13 108.2(5) . . ?
C13 Si5 C11 107.7(5) . . ?
C16 Si6 C18 104.4(5) . . ?
C16 Si6 C19 111.4(5) . . ?
C17 Si6 C16 108.6(5) . . ?
C17 Si6 C18 112.6(5) . . ?
C17 Si6 C19 110.5(5) . . ?
C19 Si6 C18 109.2(5) . . ?
C23 Si7 C22 112.4(5) . . ?
C23 Si7 C24 107.9(6) . . ?
C23 Si7 C25 110.7(5) . . ?
C24 Si7 C22 106.4(5) . . ?
C24 Si7 C25 109.0(6) . . ?
C25 Si7 C22 110.3(5) . . ?
C28 Si8 C29 111.3(5) . . ?
C30 Si8 C28 110.8(5) . . ?
C30 Si8 C29 111.1(6) . . ?
C31 Si8 C28 106.3(6) . . ?
C31 Si8 C29 108.3(6) . . ?
C31 Si8 C30 108.8(7) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si5 C10 H10A 109.5 . . ?
Si5 C10 H10B 109.5 . . ?
Si5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si5 C11 H11A 109.5 . . ?
Si5 C11 H11B 109.5 . . ?
Si5 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si5 C12 H12A 109.5 . . ?
Si5 C12 H12B 109.5 . . ?
Si5 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si5 C13 Nd1 118.5(4) . . ?
C14 C13 Nd1 74.5(5) . . ?
C14 C13 Si5 125.6(8) . . ?
C14 C13 C20 106.0(8) . . ?
C20 C13 Nd1 73.3(5) . . ?
C20 C13 Si5 128.3(7) . . ?
Nd1 C14 H14 116.7 . . ?
C13 C14 Nd1 75.3(5) . . ?
C13 C14 H14 125.8 . . ?
C15 C14 Nd1 74.2(5) . . ?
C15 C14 C13 108.5(9) . . ?
C15 C14 H14 125.8 . . ?
Nd1 C15 H15 116.1 . . ?
C14 C15 Nd1 76.0(5) . . ?
C14 C15 H15 125.1 . . ?
C14 C15 C16 109.8(9) . . ?
C16 C15 Nd1 74.6(5) . . ?
C16 C15 H15 125.1 . . ?
Si6 C16 Nd1 111.6(4) . . ?
C15 C16 Nd1 75.2(5) . . ?
C15 C16 Si6 126.2(7) . . ?
C15 C16 C20 106.5(9) . . ?
C20 C16 Nd1 75.0(5) . . ?
C20 C16 Si6 127.0(7) . . ?
Si6 C17 H17A 109.5 . . ?
Si6 C17 H17B 109.5 . . ?
Si6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si6 C18 H18A 109.5 . . ?
Si6 C18 H18B 109.5 . . ?
Si6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si6 C19 H19A 109.5 . . ?
Si6 C19 H19B 109.5 . . ?
Si6 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Nd1 C20 H20 115.8 . . ?
C13 C20 Nd1 76.1(5) . . ?
C13 C20 H20 125.4 . . ?
C16 C20 Nd1 74.7(5) . . ?
C16 C20 C13 109.2(8) . . ?
C16 C20 H20 125.4 . . ?
Nd1 C21 H21 114.6 . . ?
C22 C21 Nd1 77.0(5) . . ?
C22 C21 H21 124.5 . . ?
C22 C21 C28 110.9(8) . . ?
C28 C21 Nd1 75.8(5) . . ?
C28 C21 H21 124.5 . . ?
Si7 C22 Nd1 133.2(4) . . ?
C21 C22 Nd1 73.3(5) . . ?
C21 C22 Si7 126.3(7) . . ?
C21 C22 C26 105.4(8) . . ?
C26 C22 Nd1 73.9(5) . . ?
C26 C22 Si7 125.2(8) . . ?
Si7 C23 H23A 109.5 . . ?
Si7 C23 H23B 109.5 . . ?
Si7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si7 C24 H24A 109.5 . . ?
Si7 C24 H24B 109.5 . . ?
Si7 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si7 C25 H25A 109.5 . . ?
Si7 C25 H25B 109.5 . . ?
Si7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Nd1 C26 H26 115.7 . . ?
C22 C26 Nd1 75.9(5) . . ?
C22 C26 H26 125.4 . . ?
C27 C26 Nd1 75.0(5) . . ?
C27 C26 C22 109.2(9) . . ?
C27 C26 H26 125.4 . . ?
Nd1 C27 H27 115.8 . . ?
C26 C27 Nd1 75.5(5) . . ?
C26 C27 H27 125.1 . . ?
C26 C27 C28 109.7(8) . . ?
C28 C27 Nd1 75.5(5) . . ?
C28 C27 H27 125.1 . . ?
Si8 C28 Nd1 133.4(5) . . ?
C21 C28 Nd1 73.6(5) . . ?
C21 C28 Si8 125.5(7) . . ?
C27 C28 Nd1 74.4(5) . . ?
C27 C28 Si8 126.1(7) . . ?
C27 C28 C21 104.7(8) . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si8 C31 H31A 109.5 . . ?
Si8 C31 H31B 109.5 . . ?
Si8 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1A Si2A Si1 111.4(8) . . ?
C1A Si2A C2A 106.4(12) . . ?
C1A Si2A C3A 105.2(12) . . ?
C2A Si2A Si1 112.8(11) . . ?
C2A Si2A C3A 106.7(14) . . ?
C3A Si2A Si1 113.8(10) . . ?
C4A Si3A Si1 112.9(16) . . ?
C5A Si3A Si1 115.0(11) . . ?
C5A Si3A C4A 105.5(19) . . ?
C6A Si3A Si1 110.7(7) . . ?
C6A Si3A C4A 106.6(13) . . ?
C6A Si3A C5A 105.6(11) . . ?
C7A Si4A Si1 109.0(16) . . ?
C8A Si4A Si1 116.1(9) . . ?
C8A Si4A C7A 105.5(18) . . ?
C9A Si4A Si1 113.3(8) . . ?
C9A Si4A C7A 106.8(13) . . ?
C9A Si4A C8A 105.5(11) . . ?
Si2A C1A H1AA 109.5 . . ?
Si2A C1A H1AB 109.5 . . ?
Si2A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
Si2A C2A H2AA 109.5 . . ?
Si2A C2A H2AB 109.5 . . ?
Si2A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
Si2A C3A H3AA 109.5 . . ?
Si2A C3A H3AB 109.5 . . ?
Si2A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
Si3A C4A H4AA 109.5 . . ?
Si3A C4A H4AB 109.5 . . ?
Si3A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
Si3A C5A H5AA 109.5 . . ?
Si3A C5A H5AB 109.5 . . ?
Si3A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
Si3A C6A H6AA 109.5 . . ?
Si3A C6A H6AB 109.5 . . ?
Si3A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
Si4A C7A H7AA 109.5 . . ?
Si4A C7A H7AB 109.5 . . ?
Si4A C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
Si4A C8A H8AA 109.5 . . ?
Si4A C8A H8AB 109.5 . . ?
Si4A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
Si4A C9A H9AA 109.5 . . ?
Si4A C9A H9AB 109.5 . . ?
Si4A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 C13 C14 C15 67.5(7) . . . . ?
Nd1 C13 C20 C16 -68.0(6) . . . . ?
Nd1 C14 C15 C16 67.7(7) . . . . ?
Nd1 C15 C16 Si6 -106.2(7) . . . . ?
Nd1 C15 C16 C20 69.1(6) . . . . ?
Nd1 C16 C20 C13 69.0(6) . . . . ?
Nd1 C21 C22 Si7 131.8(7) . . . . ?
Nd1 C21 C22 C26 -67.4(6) . . . . ?
Nd1 C21 C28 Si8 -132.0(8) . . . . ?
Nd1 C21 C28 C27 68.5(6) . . . . ?
Nd1 C22 C26 C27 -68.3(6) . . . . ?
Nd1 C26 C27 C28 -68.4(6) . . . . ?
Nd1 C27 C28 Si8 132.8(8) . . . . ?
Nd1 C27 C28 C21 -67.9(6) . . . . ?
Si5 C13 C14 Nd1 114.2(7) . . . . ?
Si5 C13 C14 C15 -178.3(7) . . . . ?
Si5 C13 C20 Nd1 -113.5(7) . . . . ?
Si5 C13 C20 C16 178.5(7) . . . . ?
Si6 C16 C20 Nd1 106.0(7) . . . . ?
Si6 C16 C20 C13 175.0(7) . . . . ?
Si7 C22 C26 Nd1 -131.9(7) . . . . ?
Si7 C22 C26 C27 159.9(7) . . . . ?
C10 Si5 C13 Nd1 -110.2(6) . . . . ?
C10 Si5 C13 C14 158.9(9) . . . . ?
C10 Si5 C13 C20 -19.4(10) . . . . ?
C11 Si5 C13 Nd1 9.1(6) . . . . ?
C11 Si5 C13 C14 -81.7(9) . . . . ?
C11 Si5 C13 C20 99.9(9) . . . . ?
C12 Si5 C13 Nd1 128.5(8) . . . . ?
C12 Si5 C13 C14 37.6(11) . . . . ?
C12 Si5 C13 C20 -140.8(10) . . . . ?
C13 C14 C15 Nd1 -68.2(6) . . . . ?
C13 C14 C15 C16 -0.5(11) . . . . ?
C14 C13 C20 Nd1 67.9(6) . . . . ?
C14 C13 C20 C16 -0.1(10) . . . . ?
C14 C15 C16 Nd1 -68.6(7) . . . . ?
C14 C15 C16 Si6 -174.8(7) . . . . ?
C14 C15 C16 C20 0.4(11) . . . . ?
C15 C16 C20 Nd1 -69.2(6) . . . . ?
C15 C16 C20 C13 -0.2(10) . . . . ?
C17 Si6 C16 Nd1 -124.8(5) . . . . ?
C17 Si6 C16 C15 -37.7(10) . . . . ?
C17 Si6 C16 C20 148.0(8) . . . . ?
C18 Si6 C16 Nd1 -4.5(5) . . . . ?
C18 Si6 C16 C15 82.7(9) . . . . ?
C18 Si6 C16 C20 -91.6(9) . . . . ?
C19 Si6 C16 Nd1 113.2(5) . . . . ?
C19 Si6 C16 C15 -159.6(8) . . . . ?
C19 Si6 C16 C20 26.1(10) . . . . ?
C20 C13 C14 Nd1 -67.1(6) . . . . ?
C20 C13 C14 C15 0.4(10) . . . . ?
C21 C22 C26 Nd1 67.1(6) . . . . ?
C21 C22 C26 C27 -1.2(10) . . . . ?
C22 C21 C28 Nd1 -69.8(7) . . . . ?
C22 C21 C28 Si8 158.2(7) . . . . ?
C22 C21 C28 C27 -1.3(10) . . . . ?
C22 C26 C27 Nd1 68.9(6) . . . . ?
C22 C26 C27 C28 0.4(10) . . . . ?
C23 Si7 C22 Nd1 46.9(8) . . . . ?
C23 Si7 C22 C21 -54.7(10) . . . . ?
C23 Si7 C22 C26 148.2(8) . . . . ?
C24 Si7 C22 Nd1 164.7(7) . . . . ?
C24 Si7 C22 C21 63.2(10) . . . . ?
C24 Si7 C22 C26 -94.0(10) . . . . ?
C25 Si7 C22 Nd1 -77.1(7) . . . . ?
C25 Si7 C22 C21 -178.7(8) . . . . ?
C25 Si7 C22 C26 24.1(10) . . . . ?
C26 C27 C28 Nd1 68.4(6) . . . . ?
C26 C27 C28 Si8 -158.8(7) . . . . ?
C26 C27 C28 C21 0.5(10) . . . . ?
C28 C21 C22 Nd1 69.0(7) . . . . ?
C28 C21 C22 Si7 -159.3(7) . . . . ?
C28 C21 C22 C26 1.5(10) . . . . ?
C29 Si8 C28 Nd1 76.0(7) . . . . ?
C29 Si8 C28 C21 177.4(8) . . . . ?
C29 Si8 C28 C27 -27.4(10) . . . . ?
C30 Si8 C28 Nd1 -48.2(8) . . . . ?
C30 Si8 C28 C21 53.2(10) . . . . ?
C30 Si8 C28 C27 -151.6(9) . . . . ?
C31 Si8 C28 Nd1 -166.2(7) . . . . ?
C31 Si8 C28 C21 -64.8(10) . . . . ?
C31 Si8 C28 C27 90.4(10) . . . . ?

_audit_author_email              
;
benjamin.reant@postgrad.manchester.ac.uk, david.mills@manchester.ac.uk    
;
_olex2_exptl_crystal_mounting_method 'Mounted from fomblin oil'
_olex2_submission_original_sample_id BR4.351
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.948
_oxdiff_exptl_absorpt_empirical_full_min 0.624
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
