# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Compound_4-Lu
_database_code_depnum_ccdc_archive 'CCDC 1410385'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         dr123
_chemical_formula_sum            'C25 H48 Lu N O2 Si'
_chemical_formula_weight         597.70

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   13.396(3)
_cell_length_b                   14.1217(19)
_cell_length_c                   14.991(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.346(17)
_cell_angle_gamma                90.00
_cell_volume                     2798.3(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3611
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      29.57

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    3.590
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.50923
_exptl_absorpt_correction_T_max  0.66496
_exptl_absorpt_process_details   mulabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       PHI
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37029
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.68
_reflns_number_total             5314
_reflns_number_gt                4438
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       X-AREA
_computing_cell_refinement       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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


# start Validation Reply Form
_vrf_PLAT410_Compound_4-Lu       
;
PROBLEM: Short Intra H...H Contact  H23A   ..  H22D    ..       1.88 Ang. 
RESPONSE: H22D is part of a disordered methylene group in one of the thf solvent
          molecules bound to the metal center.
;
# end Validation Reply Form


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0201P)²+1.8583P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5314
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0572
_refine_ls_wR_factor_gt          0.0544
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0612(3) 0.2398(3) 0.0099(2) 0.0355(9) Uani 1 1 d . A .
H1A H 0.0959 0.1797 0.0033 0.053 Uiso 1 1 calc R . .
H1B H 0.1006 0.2920 -0.0099 0.053 Uiso 1 1 calc R . .
H1C H -0.0061 0.2385 -0.0273 0.053 Uiso 1 1 calc R . .
C2 C 0.1010(4) 0.4022(3) 0.2441(4) 0.0488(13) Uani 1 1 d . A .
H2A H 0.1294 0.3859 0.3066 0.073 Uiso 1 1 calc R . .
H2B H 0.0437 0.4454 0.2438 0.073 Uiso 1 1 calc R . .
H2C H 0.1529 0.4331 0.2152 0.073 Uiso 1 1 calc R . .
C3 C 0.0855(4) -0.0078(4) 0.1357(3) 0.0517(14) Uani 1 1 d . . .
H3A H 0.0297 -0.0201 0.0862 0.078 Uiso 1 1 calc R . .
H3B H 0.1262 -0.0654 0.1485 0.078 Uiso 1 1 calc R . .
H3C H 0.1281 0.0432 0.1182 0.078 Uiso 1 1 calc R . .
C4 C 0.1405(4) 0.0212(4) 0.3360(3) 0.0456(12) Uani 1 1 d . . .
H4A H 0.1966 0.0610 0.3235 0.068 Uiso 1 1 calc R . .
H4B H 0.1636 -0.0446 0.3444 0.068 Uiso 1 1 calc R . .
H4C H 0.1173 0.0435 0.3910 0.068 Uiso 1 1 calc R . .
C5 C -0.0587(4) -0.0636(4) 0.2626(4) 0.0545(14) Uani 1 1 d . . .
H5A H -0.0809 -0.0492 0.3203 0.082 Uiso 1 1 calc R . .
H5B H -0.0264 -0.1261 0.2662 0.082 Uiso 1 1 calc R . .
H5C H -0.1173 -0.0637 0.2141 0.082 Uiso 1 1 calc R . .
C6 C -0.1163(3) 0.1571(3) 0.2461(2) 0.0212(7) Uani 1 1 d . . .
C7 C -0.1272(3) 0.1992(3) 0.3307(2) 0.0221(8) Uani 1 1 d . . .
C8 C -0.2237(3) 0.2210(3) 0.3482(3) 0.0277(8) Uani 1 1 d . . .
H8 H -0.2302 0.2501 0.4041 0.033 Uiso 1 1 calc R . .
C9 C -0.3091(3) 0.2019(3) 0.2880(3) 0.0322(9) Uani 1 1 d . . .
H9 H -0.3738 0.2174 0.3018 0.039 Uiso 1 1 calc R . .
C10 C -0.3000(3) 0.1600(3) 0.2067(3) 0.0288(9) Uani 1 1 d . . .
H10 H -0.3593 0.1462 0.1646 0.035 Uiso 1 1 calc R . .
C11 C -0.2053(3) 0.1373(3) 0.1849(3) 0.0229(8) Uani 1 1 d . . .
C12 C -0.0362(3) 0.2193(3) 0.4025(2) 0.0298(9) Uani 1 1 d . . .
H12 H 0.0260 0.2100 0.3746 0.036 Uiso 1 1 calc R . .
C13 C -0.0342(4) 0.3200(3) 0.4389(3) 0.0422(11) Uani 1 1 d . . .
H13A H -0.0302 0.3648 0.3897 0.063 Uiso 1 1 calc R . .
H13B H 0.0249 0.3281 0.4862 0.063 Uiso 1 1 calc R . .
H13C H -0.0960 0.3320 0.4643 0.063 Uiso 1 1 calc R . .
C14 C -0.0324(4) 0.1484(4) 0.4807(3) 0.0485(13) Uani 1 1 d . . .
H14A H -0.0936 0.1549 0.5082 0.073 Uiso 1 1 calc R . .
H14B H 0.0273 0.1611 0.5262 0.073 Uiso 1 1 calc R . .
H14C H -0.0285 0.0838 0.4575 0.073 Uiso 1 1 calc R . .
C15 C -0.2020(3) 0.0926(3) 0.0926(3) 0.0301(9) Uani 1 1 d . . .
H15 H -0.1314 0.0700 0.0920 0.036 Uiso 1 1 calc R . .
C16 C -0.2281(4) 0.1648(3) 0.0161(3) 0.0389(10) Uani 1 1 d . . .
H16A H -0.2948 0.1923 0.0187 0.058 Uiso 1 1 calc R . .
H16B H -0.2293 0.1331 -0.0422 0.058 Uiso 1 1 calc R . .
H16C H -0.1771 0.2151 0.0230 0.058 Uiso 1 1 calc R . .
C17 C -0.2727(4) 0.0075(4) 0.0737(3) 0.0488(13) Uani 1 1 d . . .
H17A H -0.2597 -0.0369 0.1245 0.073 Uiso 1 1 calc R . .
H17B H -0.2606 -0.0241 0.0183 0.073 Uiso 1 1 calc R . .
H17C H -0.3431 0.0291 0.0663 0.073 Uiso 1 1 calc R . .
C18 C -0.0930(4) 0.4164(4) 0.0386(3) 0.0524(14) Uani 1 1 d . . .
H18A H -0.1239 0.3868 -0.0191 0.063 Uiso 1 1 calc R . .
H18B H -0.0219 0.4329 0.0350 0.063 Uiso 1 1 calc R . .
C19 C -0.1507(4) 0.5024(3) 0.0570(4) 0.0478(12) Uani 1 1 d . . .
H19A H -0.1831 0.5328 0.0001 0.057 Uiso 1 1 calc R . .
H19B H -0.1063 0.5491 0.0934 0.057 Uiso 1 1 calc R . .
C20 C -0.2295(3) 0.4632(3) 0.1097(3) 0.0398(11) Uani 1 1 d . . .
H20A H -0.2546 0.5130 0.1470 0.048 Uiso 1 1 calc R . .
H20B H -0.2874 0.4352 0.0688 0.048 Uiso 1 1 calc R . .
C21 C -0.1709(3) 0.3891(3) 0.1677(3) 0.0363(10) Uani 1 1 d . . .
H21A H -0.1360 0.4170 0.2249 0.044 Uiso 1 1 calc R . .
H21B H -0.2164 0.3381 0.1821 0.044 Uiso 1 1 calc R . .
C22A C 0.2817(10) 0.2084(11) 0.1291(9) 0.038(2) Uani 0.532(15) 1 d P A 1
H22A H 0.2855 0.2698 0.0980 0.045 Uiso 0.532(15) 1 calc PR A 1
H22B H 0.2582 0.1591 0.0836 0.045 Uiso 0.532(15) 1 calc PR A 1
C22B C 0.2785(11) 0.1637(13) 0.1448(10) 0.038(2) Uani 0.468(15) 1 d P A 2
H22C H 0.2653 0.1857 0.0813 0.045 Uiso 0.468(15) 1 calc PR A 2
H22D H 0.2642 0.0950 0.1457 0.045 Uiso 0.468(15) 1 calc PR A 2
C23 C 0.3843(4) 0.1819(4) 0.1843(3) 0.0492(13) Uani 1 1 d . . .
H23A H 0.4042 0.1175 0.1681 0.059 Uiso 1 1 calc R A 1
H23B H 0.4369 0.2271 0.1721 0.059 Uiso 1 1 calc R A 1
C24 C 0.3731(4) 0.1856(4) 0.2832(3) 0.0488(13) Uani 1 1 d . A .
H24A H 0.3686 0.1211 0.3079 0.059 Uiso 1 1 calc R . .
H24B H 0.4311 0.2191 0.3192 0.059 Uiso 1 1 calc R . .
C25 C 0.2772(3) 0.2389(4) 0.2836(3) 0.0418(10) Uani 1 1 d . . .
H25A H 0.2445 0.2194 0.3354 0.050 Uiso 1 1 calc R A .
H25B H 0.2901 0.3079 0.2876 0.050 Uiso 1 1 calc R . .
N1 N -0.0195(2) 0.1389(2) 0.2240(2) 0.0218(7) Uani 1 1 d . A .
O1 O -0.0977(2) 0.35207(19) 0.11437(18) 0.0311(6) Uani 1 1 d . A .
O2 O 0.2136(2) 0.2147(2) 0.19811(18) 0.0325(6) Uani 1 1 d . A .
Si1 Si 0.03368(8) 0.02794(8) 0.23848(8) 0.0266(2) Uani 1 1 d . . .
Lu1 Lu 0.044889(13) 0.262069(10) 0.163241(11) 0.02397(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Lu1 2.366(4) . ?
C2 Lu1 2.378(5) . ?
C3 Si1 1.861(5) . ?
C4 Si1 1.875(5) . ?
C5 Si1 1.865(5) . ?
C6 C11 1.409(5) . ?
C6 N1 1.414(5) . ?
C6 C7 1.430(5) . ?
C7 C8 1.394(5) . ?
C7 C12 1.517(5) . ?
C8 C9 1.364(6) . ?
C9 C10 1.378(6) . ?
C10 C11 1.398(5) . ?
C11 C15 1.527(5) . ?
C12 C13 1.522(6) . ?
C12 C14 1.536(6) . ?
C15 C17 1.527(6) . ?
C15 C16 1.532(6) . ?
C18 O1 1.463(5) . ?
C18 C19 1.489(7) . ?
C19 C20 1.521(6) . ?
C20 C21 1.498(6) . ?
C21 O1 1.458(5) . ?
C22A O2 1.489(13) . ?
C22A C23 1.530(14) . ?
C22B O2 1.462(16) . ?
C22B C23 1.467(16) . ?
C23 C24 1.514(7) . ?
C24 C25 1.491(7) . ?
C25 O2 1.460(5) . ?
N1 Si1 1.720(3) . ?
N1 Lu1 2.203(3) . ?
O1 Lu1 2.312(3) . ?
O2 Lu1 2.333(3) . ?

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
C11 C6 N1 121.5(3) . . ?
C11 C6 C7 117.6(3) . . ?
N1 C6 C7 120.9(3) . . ?
C8 C7 C6 119.3(3) . . ?
C8 C7 C12 119.2(3) . . ?
C6 C7 C12 121.5(3) . . ?
C9 C8 C7 122.3(4) . . ?
C8 C9 C10 119.1(4) . . ?
C9 C10 C11 121.2(4) . . ?
C10 C11 C6 120.4(4) . . ?
C10 C11 C15 117.8(3) . . ?
C6 C11 C15 121.8(3) . . ?
C7 C12 C13 113.2(3) . . ?
C7 C12 C14 110.0(4) . . ?
C13 C12 C14 109.9(4) . . ?
C17 C15 C11 112.7(4) . . ?
C17 C15 C16 109.0(4) . . ?
C11 C15 C16 111.5(3) . . ?
O1 C18 C19 105.9(4) . . ?
C18 C19 C20 102.9(4) . . ?
C21 C20 C19 102.3(4) . . ?
O1 C21 C20 105.6(3) . . ?
O2 C22A C23 103.7(8) . . ?
O2 C22B C23 108.3(10) . . ?
C22B C23 C24 99.2(7) . . ?
C22B C23 C22A 26.0(5) . . ?
C24 C23 C22A 107.4(6) . . ?
C25 C24 C23 104.1(4) . . ?
O2 C25 C24 105.0(4) . . ?
C6 N1 Si1 120.9(2) . . ?
C6 N1 Lu1 112.8(2) . . ?
Si1 N1 Lu1 126.14(16) . . ?
C21 O1 C18 108.6(3) . . ?
C21 O1 Lu1 128.1(2) . . ?
C18 O1 Lu1 116.7(3) . . ?
C25 O2 C22B 106.3(7) . . ?
C25 O2 C22A 106.7(6) . . ?
C22B O2 C22A 26.5(5) . . ?
C25 O2 Lu1 122.4(2) . . ?
C22B O2 Lu1 131.2(6) . . ?
C22A O2 Lu1 122.8(5) . . ?
N1 Si1 C3 110.20(19) . . ?
N1 Si1 C5 112.5(2) . . ?
C3 Si1 C5 108.7(3) . . ?
N1 Si1 C4 113.1(2) . . ?
C3 Si1 C4 107.0(2) . . ?
C5 Si1 C4 105.1(2) . . ?
N1 Lu1 O1 101.92(11) . . ?
N1 Lu1 O2 96.36(11) . . ?
O1 Lu1 O2 161.58(10) . . ?
N1 Lu1 C1 113.64(14) . . ?
O1 Lu1 C1 88.12(12) . . ?
O2 Lu1 C1 86.59(12) . . ?
N1 Lu1 C2 123.99(16) . . ?
O1 Lu1 C2 83.13(14) . . ?
O2 Lu1 C2 84.83(14) . . ?
C1 Lu1 C2 122.31(18) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.102
_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_Compound_6-Y
_database_code_depnum_ccdc_archive 'CCDC 1410386'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H50 Ga2 N Si Y'
_chemical_formula_weight         597.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.6911(10)
_cell_length_b                   12.3862(9)
_cell_length_c                   17.5679(12)
_cell_angle_alpha                90
_cell_angle_beta                 112.559(5)
_cell_angle_gamma                90
_cell_volume                     2952.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    24257
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      24.67

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    3.811
_shelx_estimated_absorpt_T_min   0.394
_shelx_estimated_absorpt_T_max   0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4657
_exptl_absorpt_correction_T_max  0.5690
_exptl_absorpt_process_details   Platon/Mulabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       Phi
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41311
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         5.162
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             5984
_reflns_number_gt                4960
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0170P)²+7.2352P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5984
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.0996
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_restrained_S_all      1.263
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4057(4) 0.2380(4) 0.1990(3) 0.0320(11) Uani 1 1 d . . . . .
H1A H 0.3379 0.2179 0.1642 0.048 Uiso 1 1 calc R U . . .
H1B H 0.4129 0.3166 0.1984 0.048 Uiso 1 1 calc R U . . .
H1C H 0.4207 0.2137 0.2556 0.048 Uiso 1 1 calc R U . . .
C2 C 0.4691(4) 0.2160(4) 0.0310(3) 0.0351(12) Uani 1 1 d . . . . .
H2A H 0.4034 0.1897 -0.0039 0.053 Uiso 1 1 calc R U . . .
H2B H 0.5179 0.1871 0.0109 0.053 Uiso 1 1 calc R U . . .
H2C H 0.4700 0.2951 0.0293 0.053 Uiso 1 1 calc R U . . .
C3 C 0.4909(5) 0.0038(5) 0.1540(4) 0.0493(15) Uani 1 1 d . . . . .
H3A H 0.4594 -0.0224 0.0972 0.074 Uiso 1 1 calc R U . . .
H3B H 0.4504 -0.0161 0.1850 0.074 Uiso 1 1 calc R U . . .
H3C H 0.5564 -0.0287 0.1800 0.074 Uiso 1 1 calc R U . . .
C4 C 0.6340(4) 0.2280(6) 0.2199(4) 0.0602(19) Uani 1 1 d . . . . .
H4A H 0.6409 0.2977 0.1963 0.090 Uiso 1 1 calc R U . . .
H4B H 0.6863 0.1791 0.2197 0.090 Uiso 1 1 calc R U . . .
H4C H 0.6391 0.2386 0.2767 0.090 Uiso 1 1 calc R U . . .
C5 C 0.2465(4) 0.4569(4) 0.1051(3) 0.0299(11) Uani 1 1 d . . . . .
H5A H 0.2469 0.3780 0.1008 0.045 Uiso 1 1 calc R U . . .
H5B H 0.1785 0.4833 0.0807 0.045 Uiso 1 1 calc R U . . .
H5C H 0.2758 0.4780 0.1633 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2975(4) 0.4318(4) -0.0657(3) 0.0340(12) Uani 1 1 d . . . . .
H6A H 0.3533 0.3842 -0.0590 0.051 Uiso 1 1 calc R U . . .
H6B H 0.2861 0.4800 -0.1127 0.051 Uiso 1 1 calc R U . . .
H6C H 0.2384 0.3881 -0.0757 0.051 Uiso 1 1 calc R U . . .
C7 C 0.2884(5) 0.6743(5) 0.0125(5) 0.0623(19) Uani 1 1 d . . . . .
H7A H 0.2170 0.6773 -0.0183 0.093 Uiso 1 1 calc R U . . .
H7B H 0.3220 0.7030 -0.0218 0.093 Uiso 1 1 calc R U . . .
H7C H 0.3061 0.7177 0.0628 0.093 Uiso 1 1 calc R U . . .
C8 C 0.4706(4) 0.4957(5) 0.1110(4) 0.0435(14) Uani 1 1 d . . . . .
H8A H 0.4805 0.4181 0.1219 0.065 Uiso 1 1 calc R U . . .
H8B H 0.4893 0.5348 0.1633 0.065 Uiso 1 1 calc R U . . .
H8C H 0.5116 0.5202 0.0816 0.065 Uiso 1 1 calc R U . . .
C9 C 0.1374(3) 0.1965(3) 0.0066(3) 0.0211(9) Uani 1 1 d . . . . .
C10 C 0.0605(3) 0.2718(4) -0.0303(3) 0.0263(10) Uani 1 1 d . . . . .
C11 C -0.0015(4) 0.2988(4) 0.0101(3) 0.0349(12) Uani 1 1 d . . . . .
H11 H -0.0527 0.3497 -0.0145 0.042 Uiso 1 1 calc R U . . .
C12 C 0.0092(4) 0.2539(4) 0.0845(3) 0.0375(12) Uani 1 1 d . . . . .
H12 H -0.0319 0.2763 0.1121 0.045 Uiso 1 1 calc R U . . .
C13 C 0.0799(4) 0.1763(4) 0.1185(3) 0.0295(11) Uani 1 1 d . . . . .
H13 H 0.0859 0.1437 0.1692 0.035 Uiso 1 1 calc R U . . .
C14 C 0.1435(3) 0.1441(4) 0.0805(3) 0.0223(9) Uani 1 1 d . . . . .
C15 C 0.2094(4) 0.0465(4) 0.1140(3) 0.0277(10) Uani 1 1 d . . . . .
H15 H 0.2703 0.0566 0.1023 0.033 Uiso 1 1 calc R U . . .
C16 C 0.2409(4) 0.0290(5) 0.2068(3) 0.0396(13) Uani 1 1 d . . . . .
H16A H 0.2920 -0.0270 0.2253 0.059 Uiso 1 1 calc R U . . .
H16B H 0.1838 0.0060 0.2186 0.059 Uiso 1 1 calc R U . . .
H16C H 0.2672 0.0966 0.2360 0.059 Uiso 1 1 calc R U . . .
C17 C 0.1565(4) -0.0545(4) 0.0682(4) 0.0402(13) Uani 1 1 d . . . . .
H17A H 0.1996 -0.1174 0.0884 0.060 Uiso 1 1 calc R U . . .
H17B H 0.1404 -0.0455 0.0090 0.060 Uiso 1 1 calc R U . . .
H17C H 0.0958 -0.0652 0.0779 0.060 Uiso 1 1 calc R U . . .
C18 C 0.0405(4) 0.3239(4) -0.1136(3) 0.0313(11) Uani 1 1 d . . . . .
H18 H 0.0923 0.2992 -0.1335 0.038 Uiso 1 1 calc R U . . .
C19 C 0.0424(4) 0.4467(4) -0.1104(4) 0.0391(13) Uani 1 1 d . . . . .
H19A H 0.0377 0.4754 -0.1638 0.059 Uiso 1 1 calc R U . . .
H19B H 0.1042 0.4710 -0.0673 0.059 Uiso 1 1 calc R U . . .
H19C H -0.0134 0.4729 -0.0981 0.059 Uiso 1 1 calc R U . . .
C20 C -0.0608(5) 0.2880(5) -0.1768(3) 0.0496(15) Uani 1 1 d . . . . .
H20A H -0.0688 0.3139 -0.2318 0.074 Uiso 1 1 calc R U . . .
H20B H -0.1131 0.3184 -0.1616 0.074 Uiso 1 1 calc R U . . .
H20C H -0.0649 0.2091 -0.1773 0.074 Uiso 1 1 calc R U . . .
C21 C 0.0765(5) 0.0366(5) -0.1569(4) 0.0546(17) Uani 1 1 d . . . . .
H21A H 0.0392 0.0827 -0.2039 0.082 Uiso 1 1 calc R U . . .
H21B H 0.0436 0.0352 -0.1178 0.082 Uiso 1 1 calc R U . . .
H21C H 0.0798 -0.0369 -0.1764 0.082 Uiso 1 1 calc R U . . .
C22 C 0.2382(5) 0.1639(5) -0.1837(3) 0.0472(14) Uani 1 1 d . . . . .
H22A H 0.3077 0.1851 -0.1594 0.071 Uiso 1 1 calc R U . . .
H22B H 0.1971 0.2285 -0.2023 0.071 Uiso 1 1 calc R U . . .
H22C H 0.2274 0.1161 -0.2308 0.071 Uiso 1 1 calc R U . . .
C23 C 0.2924(5) -0.0242(5) -0.0683(4) 0.0454(14) Uani 1 1 d . . . . .
H23A H 0.3599 0.0035 -0.0432 0.068 Uiso 1 1 calc R U . . .
H23B H 0.2863 -0.0705 -0.1153 0.068 Uiso 1 1 calc R U . . .
H23C H 0.2771 -0.0662 -0.0275 0.068 Uiso 1 1 calc R U . . .
N1 N 0.2117(3) 0.1780(3) -0.0256(2) 0.0206(8) Uani 1 1 d . . . . .
Si1 Si 0.20435(10) 0.09136(12) -0.10461(8) 0.0299(3) Uani 1 1 d . . . . .
Ga1 Ga 0.32886(4) 0.52414(4) 0.04200(4) 0.03154(14) Uani 1 1 d . . . . .
Ga2 Ga 0.50390(4) 0.16453(5) 0.15338(4) 0.03502(15) Uani 1 1 d . . . . .
Y1 Y 0.32052(3) 0.29303(4) 0.05009(3) 0.02238(11) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Ga2 2.107(5) . ?
C1 Y1 2.522(5) . ?
C2 Ga2 2.108(5) . ?
C2 Y1 2.520(5) . ?
C3 Ga2 2.000(6) . ?
C4 Ga2 1.981(6) . ?
C5 Ga1 2.101(5) . ?
C5 Y1 2.653(5) . ?
C6 Ga1 2.106(5) . ?
C6 Y1 2.585(5) . ?
C7 Ga1 1.961(6) . ?
C8 Ga1 1.999(5) . ?
C9 C10 1.416(6) . ?
C9 C14 1.424(6) . ?
C9 N1 1.427(5) . ?
C9 Y1 2.770(4) . ?
C10 C11 1.394(7) . ?
C10 C18 1.521(6) . ?
C11 C12 1.372(8) . ?
C12 C13 1.373(7) . ?
C13 C14 1.398(6) . ?
C14 C15 1.519(6) . ?
C15 C17 1.528(7) . ?
C15 C16 1.530(6) . ?
C18 C19 1.522(7) . ?
C18 C20 1.542(7) . ?
C21 Si1 1.874(6) . ?
C22 Si1 1.875(6) . ?
C23 Si1 1.869(6) . ?
N1 Si1 1.725(4) . ?
N1 Y1 2.172(4) . ?
Ga1 Y1 2.8711(7) . ?
Ga2 Y1 3.0550(7) . ?

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
Ga2 C1 Y1 82.07(16) . . ?
Ga2 C2 Y1 82.10(16) . . ?
Ga1 C5 Y1 73.26(14) . . ?
Ga1 C6 Y1 74.71(14) . . ?
C10 C9 C14 118.5(4) . . ?
C10 C9 N1 121.4(4) . . ?
C14 C9 N1 119.9(4) . . ?
C10 C9 Y1 111.2(3) . . ?
C14 C9 Y1 103.3(3) . . ?
N1 C9 Y1 50.86(19) . . ?
C11 C10 C9 119.1(4) . . ?
C11 C10 C18 117.8(4) . . ?
C9 C10 C18 123.1(4) . . ?
C12 C11 C10 122.0(5) . . ?
C11 C12 C13 119.3(5) . . ?
C12 C13 C14 121.7(5) . . ?
C13 C14 C9 119.1(4) . . ?
C13 C14 C15 119.1(4) . . ?
C9 C14 C15 121.5(4) . . ?
C14 C15 C17 109.1(4) . . ?
C14 C15 C16 114.4(4) . . ?
C17 C15 C16 109.2(4) . . ?
C10 C18 C19 113.2(4) . . ?
C10 C18 C20 110.4(4) . . ?
C19 C18 C20 108.3(4) . . ?
C9 N1 Si1 126.6(3) . . ?
C9 N1 Y1 98.5(2) . . ?
Si1 N1 Y1 134.8(2) . . ?
N1 Si1 C23 112.4(2) . . ?
N1 Si1 C21 111.2(2) . . ?
C23 Si1 C21 108.8(3) . . ?
N1 Si1 C22 110.2(2) . . ?
C23 Si1 C22 105.9(3) . . ?
C21 Si1 C22 108.1(3) . . ?
C7 Ga1 C8 117.8(3) . . ?
C7 Ga1 C5 109.8(3) . . ?
C8 Ga1 C5 106.7(2) . . ?
C7 Ga1 C6 109.8(3) . . ?
C8 Ga1 C6 105.5(2) . . ?
C5 Ga1 C6 106.68(19) . . ?
C7 Ga1 Y1 160.8(2) . . ?
C8 Ga1 Y1 81.29(17) . . ?
C5 Ga1 Y1 62.25(13) . . ?
C6 Ga1 Y1 60.26(14) . . ?
C4 Ga2 C3 117.7(3) . . ?
C4 Ga2 C1 104.5(2) . . ?
C3 Ga2 C1 110.3(2) . . ?
C4 Ga2 C2 106.4(3) . . ?
C3 Ga2 C2 108.7(2) . . ?
C1 Ga2 C2 108.89(18) . . ?
C4 Ga2 Y1 125.1(2) . . ?
C3 Ga2 Y1 117.21(19) . . ?
C1 Ga2 Y1 54.85(13) . . ?
C2 Ga2 Y1 54.79(13) . . ?
N1 Y1 C2 98.16(15) . . ?
N1 Y1 C1 114.41(15) . . ?
C2 Y1 C1 85.70(17) . . ?
N1 Y1 C6 96.36(15) . . ?
C2 Y1 C6 90.33(17) . . ?
C1 Y1 C6 149.23(17) . . ?
N1 Y1 C5 114.60(14) . . ?
C2 Y1 C5 146.60(16) . . ?
C1 Y1 C5 86.47(16) . . ?
C6 Y1 C5 80.21(16) . . ?
N1 Y1 C9 30.63(13) . . ?
C2 Y1 C9 126.80(15) . . ?
C1 Y1 C9 102.26(15) . . ?
C6 Y1 C9 104.46(15) . . ?
C5 Y1 C9 86.59(14) . . ?
N1 Y1 Ga1 131.20(10) . . ?
C2 Y1 Ga1 108.39(12) . . ?
C1 Y1 Ga1 107.89(12) . . ?
C6 Y1 Ga1 45.03(12) . . ?
C5 Y1 Ga1 44.49(10) . . ?
C9 Y1 Ga1 118.17(9) . . ?
N1 Y1 Ga2 107.22(9) . . ?
C2 Y1 Ga2 43.12(12) . . ?
C1 Y1 Ga2 43.08(11) . . ?
C6 Y1 Ga2 129.30(12) . . ?
C5 Y1 Ga2 124.98(11) . . ?
C9 Y1 Ga2 118.73(9) . . ?
Ga1 Y1 Ga2 120.28(2) . . ?

_refine_diff_density_max         0.442
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.095

_shelxl_version_number           2013-3


_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_Compound_5-Ho
_database_code_depnum_ccdc_archive 'CCDC 1410387'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H50 Al2 Ho N Si'
_chemical_formula_weight         587.62

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.201(3)
_cell_length_b                   17.328(8)
_cell_length_c                   28.104(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.70(2)
_cell_angle_gamma                90
_cell_volume                     5939(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1234
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      29.49

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_F_000             2416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.773
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5052
_exptl_absorpt_correction_T_max  0.5709
_exptl_absorpt_process_details   mulabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Phi
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83915
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.948
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14719
_reflns_number_gt                11680
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-AREA
_computing_cell_refinement       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+1.1613P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14719
_refine_ls_number_parameters     536
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.0738
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0226(4) 0.5645(2) 0.16823(13) 0.0356(9) Uani 1 1 d . . . . .
H1A H 1.0488 0.6098 0.1525 0.053 Uiso 1 1 calc R U . . .
H1B H 1.0501 0.5639 0.2006 0.053 Uiso 1 1 calc R U . . .
H1C H 0.9439 0.5650 0.1678 0.053 Uiso 1 1 calc R U . . .
C2 C 1.0181(4) 0.3698(2) 0.16723(13) 0.0359(9) Uani 1 1 d . . . . .
H2A H 0.9394 0.3698 0.1652 0.054 Uiso 1 1 calc R U . . .
H2B H 1.0421 0.3707 0.2001 0.054 Uiso 1 1 calc R U . . .
H2C H 1.0454 0.3242 0.1523 0.054 Uiso 1 1 calc R U . . .
C1A C 0.4768(4) 0.8483(2) -0.07091(14) 0.0400(10) Uani 1 1 d . . . . .
H1D H 0.4950 0.8967 -0.0854 0.060 Uiso 1 1 calc R U . . .
H1E H 0.5049 0.8474 -0.0386 0.060 Uiso 1 1 calc R U . . .
H1F H 0.3985 0.8424 -0.0712 0.060 Uiso 1 1 calc R U . . .
C3 C 1.2380(4) 0.4638(3) 0.13541(19) 0.0575(14) Uani 1 1 d . . . . .
H3A H 1.2629 0.4202 0.1176 0.086 Uiso 1 1 calc R U . . .
H3B H 1.2638 0.4594 0.1679 0.086 Uiso 1 1 calc R U . . .
H3C H 1.2659 0.5104 0.1219 0.086 Uiso 1 1 calc R U . . .
C2A C 0.5047(3) 0.6565(2) -0.07594(14) 0.0352(9) Uani 1 1 d . . . . .
H2D H 0.4263 0.6518 -0.0755 0.053 Uiso 1 1 calc R U . . .
H2E H 0.5343 0.6563 -0.0439 0.053 Uiso 1 1 calc R U . . .
H2F H 0.5344 0.6139 -0.0932 0.053 Uiso 1 1 calc R U . . .
C4 C 1.0040(5) 0.4697(3) 0.06981(15) 0.0673(16) Uani 1 1 d . . . . .
H4A H 1.0305 0.5132 0.0524 0.101 Uiso 1 1 calc R U . . .
H4B H 0.9262 0.4744 0.0733 0.101 Uiso 1 1 calc R U . . .
H4C H 1.0195 0.4230 0.0529 0.101 Uiso 1 1 calc R U . . .
C3A C 0.7058(4) 0.7724(3) -0.10767(18) 0.0555(13) Uani 1 1 d . . . . .
H3D H 0.7396 0.7274 -0.1207 0.083 Uiso 1 1 calc R U . . .
H3E H 0.7320 0.7796 -0.0754 0.083 Uiso 1 1 calc R U . . .
H3F H 0.7240 0.8168 -0.1263 0.083 Uiso 1 1 calc R U . . .
C5 C 0.8008(3) 0.3725(2) 0.25389(14) 0.0359(9) Uani 1 1 d . . . . .
H5A H 0.7994 0.3760 0.2880 0.054 Uiso 1 1 calc R U . . .
H5B H 0.8754 0.3722 0.2440 0.054 Uiso 1 1 calc R U . . .
H5C H 0.7651 0.3258 0.2436 0.054 Uiso 1 1 calc R U . . .
C4A C 0.4697(5) 0.7575(3) -0.17145(16) 0.0656(15) Uani 1 1 d . . . . .
H4D H 0.4911 0.8019 -0.1894 0.098 Uiso 1 1 calc R U . . .
H4E H 0.3919 0.7586 -0.1673 0.098 Uiso 1 1 calc R U . . .
H4F H 0.4889 0.7115 -0.1883 0.098 Uiso 1 1 calc R U . . .
C6 C 0.8032(4) 0.5647(2) 0.24638(14) 0.0374(9) Uani 1 1 d . . . . .
H6A H 0.7614 0.5910 0.2698 0.056 Uiso 1 1 calc R U . . .
H6B H 0.8131 0.5982 0.2196 0.056 Uiso 1 1 calc R U . . .
H6C H 0.8735 0.5506 0.2600 0.056 Uiso 1 1 calc R U . . .
C5A C 0.2727(3) 0.8300(2) 0.01534(15) 0.0402(10) Uani 1 1 d . . . . .
H5D H 0.2374 0.8743 0.0012 0.060 Uiso 1 1 calc R U . . .
H5E H 0.3487 0.8296 0.0074 0.060 Uiso 1 1 calc R U . . .
H5F H 0.2668 0.8321 0.0493 0.060 Uiso 1 1 calc R U . . .
C7 C 0.5690(4) 0.4706(3) 0.2436(2) 0.0685(16) Uani 1 1 d . . . . .
H7A H 0.5338 0.5148 0.2293 0.103 Uiso 1 1 calc R U . . .
H7B H 0.5673 0.4749 0.2776 0.103 Uiso 1 1 calc R U . . .
H7C H 0.5312 0.4246 0.2335 0.103 Uiso 1 1 calc R U . . .
C6A C 0.2955(3) 0.6388(2) 0.01088(15) 0.0391(9) Uani 1 1 d . . . . .
H6D H 0.3543 0.6571 0.0314 0.059 Uiso 1 1 calc R U . . .
H6E H 0.3252 0.6146 -0.0166 0.059 Uiso 1 1 calc R U . . .
H6F H 0.2524 0.6020 0.0277 0.059 Uiso 1 1 calc R U . . .
C8 C 0.7439(4) 0.4576(3) 0.15506(15) 0.0486(11) Uani 1 1 d . . . . .
H8A H 0.7251 0.4066 0.1444 0.073 Uiso 1 1 calc R U . . .
H8B H 0.8196 0.4676 0.1489 0.073 Uiso 1 1 calc R U . . .
H8C H 0.6987 0.4946 0.1383 0.073 Uiso 1 1 calc R U . . .
C7A C 0.0534(4) 0.7223(4) 0.0169(2) 0.085(2) Uani 1 1 d . . . . .
H7D H 0.0028 0.7549 -0.0006 0.127 Uiso 1 1 calc R U . . .
H7E H 0.0574 0.7382 0.0496 0.127 Uiso 1 1 calc R U . . .
H7F H 0.0288 0.6698 0.0149 0.127 Uiso 1 1 calc R U . . .
C9 C 1.0554(3) 0.4293(2) 0.31146(11) 0.0233(7) Uani 1 1 d . . . . .
C8A C 0.2075(4) 0.7337(3) -0.08066(16) 0.0540(12) Uani 1 1 d . . . . .
H8D H 0.1840 0.6851 -0.0938 0.081 Uiso 1 1 calc R U . . .
H8E H 0.2820 0.7434 -0.0890 0.081 Uiso 1 1 calc R U . . .
H8F H 0.1612 0.7742 -0.0932 0.081 Uiso 1 1 calc R U . . .
C10 C 0.9799(3) 0.4274(2) 0.34917(12) 0.0285(8) Uani 1 1 d . . . . .
C9A C 0.5403(3) 0.7908(2) 0.06995(11) 0.0241(7) Uani 1 1 d . . . . .
C11 C 0.9538(3) 0.3576(2) 0.36920(14) 0.0364(9) Uani 1 1 d . . . . .
H11A H 0.9051 0.3564 0.3940 0.044 Uiso 1 1 calc R U . . .
C10A C 0.4668(3) 0.7881(2) 0.10833(13) 0.0297(8) Uani 1 1 d . . . . .
C12 C 0.9978(3) 0.2893(2) 0.35342(15) 0.0380(9) Uani 1 1 d . . . . .
H12A H 0.9757 0.2425 0.3663 0.046 Uiso 1 1 calc R U . . .
C11A C 0.4374(3) 0.8565(2) 0.13022(14) 0.0374(9) Uani 1 1 d . . . . .
H11B H 0.3892 0.8547 0.1552 0.045 Uiso 1 1 calc R U . . .
C13 C 1.0741(3) 0.2907(2) 0.31868(13) 0.0324(8) Uani 1 1 d . . . . .
H13A H 1.1044 0.2445 0.3084 0.039 Uiso 1 1 calc R U . . .
C12A C 0.4769(3) 0.9264(2) 0.11615(14) 0.0389(10) Uani 1 1 d . . . . .
H12B H 0.4532 0.9716 0.1305 0.047 Uiso 1 1 calc R U . . .
C14 C 1.1074(3) 0.3597(2) 0.29841(12) 0.0236(7) Uani 1 1 d . . . . .
C13A C 0.5523(3) 0.9295(2) 0.08052(13) 0.0320(8) Uani 1 1 d . . . . .
H13B H 0.5808 0.9770 0.0718 0.038 Uiso 1 1 calc R U . . .
C15 C 1.2068(3) 0.3601(2) 0.26706(13) 0.0297(8) Uani 1 1 d . . . . .
H15A H 1.1969 0.4008 0.2431 0.036 Uiso 1 1 calc R U . . .
C14A C 0.5866(3) 0.8630(2) 0.05743(12) 0.0245(7) Uani 1 1 d . . . . .
C16 C 1.3079(3) 0.3798(3) 0.29864(16) 0.0429(10) Uani 1 1 d . . . . .
H16A H 1.2984 0.4298 0.3126 0.064 Uiso 1 1 calc R U . . .
H16B H 1.3720 0.3800 0.2796 0.064 Uiso 1 1 calc R U . . .
H16C H 1.3164 0.3419 0.3234 0.064 Uiso 1 1 calc R U . . .
C15A C 0.6807(3) 0.8679(2) 0.02327(13) 0.0303(8) Uani 1 1 d . . . . .
H15B H 0.6702 0.8278 -0.0010 0.036 Uiso 1 1 calc R U . . .
C17 C 1.2286(4) 0.2842(2) 0.24150(16) 0.0440(11) Uani 1 1 d . . . . .
H17A H 1.2526 0.2460 0.2643 0.066 Uiso 1 1 calc R U . . .
H17B H 1.2845 0.2918 0.2186 0.066 Uiso 1 1 calc R U . . .
H17C H 1.1625 0.2669 0.2255 0.066 Uiso 1 1 calc R U . . .
C16A C 0.7895(3) 0.8521(3) 0.05075(17) 0.0453(11) Uani 1 1 d . . . . .
H16D H 0.7993 0.8895 0.0757 0.068 Uiso 1 1 calc R U . . .
H16E H 0.8492 0.8556 0.0294 0.068 Uiso 1 1 calc R U . . .
H16F H 0.7877 0.8013 0.0643 0.068 Uiso 1 1 calc R U . . .
C18 C 0.9294(3) 0.4999(2) 0.36950(14) 0.0358(9) Uani 1 1 d . . . . .
H18A H 0.9521 0.5439 0.3502 0.043 Uiso 1 1 calc R U . . .
C17A C 0.6892(4) 0.9461(3) -0.00175(16) 0.0458(11) Uani 1 1 d . . . . .
H17D H 0.6180 0.9615 -0.0137 0.069 Uiso 1 1 calc R U . . .
H17E H 0.7383 0.9419 -0.0277 0.069 Uiso 1 1 calc R U . . .
H17F H 0.7166 0.9840 0.0205 0.069 Uiso 1 1 calc R U . . .
C19 C 0.9702(4) 0.5135(3) 0.42093(16) 0.0583(14) Uani 1 1 d . . . . .
H19A H 0.9417 0.4739 0.4411 0.087 Uiso 1 1 calc R U . . .
H19B H 0.9455 0.5630 0.4315 0.087 Uiso 1 1 calc R U . . .
H19C H 1.0489 0.5120 0.4224 0.087 Uiso 1 1 calc R U . . .
C18A C 0.4234(3) 0.7131(3) 0.12806(15) 0.0397(10) Uani 1 1 d . . . . .
H18B H 0.4449 0.6710 0.1070 0.048 Uiso 1 1 calc R U . . .
C20 C 0.8042(4) 0.4971(3) 0.36850(16) 0.0462(11) Uani 1 1 d . . . . .
H20A H 0.7776 0.4861 0.3367 0.069 Uiso 1 1 calc R U . . .
H20B H 0.7760 0.5461 0.3785 0.069 Uiso 1 1 calc R U . . .
H20C H 0.7802 0.4575 0.3897 0.069 Uiso 1 1 calc R U . . .
C19A C 0.4750(5) 0.6982(4) 0.17787(18) 0.0727(18) Uani 1 1 d . . . . .
H19D H 0.5534 0.6968 0.1759 0.109 Uiso 1 1 calc R U . . .
H19E H 0.4492 0.6498 0.1898 0.109 Uiso 1 1 calc R U . . .
H19F H 0.4545 0.7389 0.1990 0.109 Uiso 1 1 calc R U . . .
C21 C 1.2689(4) 0.5837(3) 0.25551(16) 0.0475(11) Uani 1 1 d . . . . .
H21A H 1.3128 0.5377 0.2559 0.071 Uiso 1 1 calc R U . . .
H21B H 1.3141 0.6272 0.2640 0.071 Uiso 1 1 calc R U . . .
H21C H 1.2372 0.5912 0.2242 0.071 Uiso 1 1 calc R U . . .
C20A C 0.2978(4) 0.7119(3) 0.13158(16) 0.0491(12) Uani 1 1 d . . . . .
H20D H 0.2759 0.7492 0.1547 0.074 Uiso 1 1 calc R U . . .
H20E H 0.2745 0.6614 0.1411 0.074 Uiso 1 1 calc R U . . .
H20F H 0.2647 0.7245 0.1011 0.074 Uiso 1 1 calc R U . . .
C22 C 1.0792(4) 0.6659(2) 0.29724(16) 0.0447(11) Uani 1 1 d . . . . .
H22A H 1.0508 0.6748 0.2655 0.067 Uiso 1 1 calc R U . . .
H22B H 1.1266 0.7077 0.3067 0.067 Uiso 1 1 calc R U . . .
H22C H 1.0195 0.6626 0.3186 0.067 Uiso 1 1 calc R U . . .
C21A C 0.7267(4) 0.6660(3) 0.11242(18) 0.0600(15) Uani 1 1 d . . . . .
H21D H 0.7285 0.7200 0.1201 0.090 Uiso 1 1 calc R U . . .
H24E H 0.8002 0.6467 0.1109 0.090 Uiso 1 1 calc R U . . .
H24F H 0.6884 0.6385 0.1365 0.090 Uiso 1 1 calc R U . . .
C23 C 1.2217(4) 0.5627(3) 0.35965(15) 0.0492(12) Uani 1 1 d . . . . .
H23A H 1.1762 0.5870 0.3826 0.074 Uiso 1 1 calc R U . . .
H23B H 1.2928 0.5864 0.3606 0.074 Uiso 1 1 calc R U . . .
H23C H 1.2289 0.5088 0.3671 0.074 Uiso 1 1 calc R U . . .
C22A C 0.5826(4) 0.5572(2) 0.05339(18) 0.0544(13) Uani 1 1 d . . . . .
H22D H 0.5299 0.5566 0.0781 0.082 Uiso 1 1 calc R U . . .
H22E H 0.6351 0.5167 0.0589 0.082 Uiso 1 1 calc R U . . .
H22F H 0.5457 0.5493 0.0231 0.082 Uiso 1 1 calc R U . . .
C23A C 0.7589(4) 0.6468(3) 0.0067(2) 0.0618(14) Uani 1 1 d . . . . .
H23D H 0.7233 0.6365 -0.0236 0.093 Uiso 1 1 calc R U . . .
H23E H 0.8098 0.6061 0.0142 0.093 Uiso 1 1 calc R U . . .
H23F H 0.7974 0.6950 0.0052 0.093 Uiso 1 1 calc R U . . .
Al1 Al 0.72012(10) 0.46588(7) 0.22410(4) 0.0360(3) Uani 1 1 d . . . . .
Al2 Al 1.07695(11) 0.46642(7) 0.13305(4) 0.0391(3) Uani 1 1 d . . . . .
Al1A Al 0.19780(10) 0.73062(8) -0.01030(5) 0.0386(3) Uani 1 1 d . . . . .
Al2A Al 0.54573(11) 0.75864(8) -0.10881(4) 0.0393(3) Uani 1 1 d . . . . .
Ho1 Ho 0.95646(2) 0.46718(2) 0.22772(2) 0.02428(5) Uani 1 1 d . . . . .
Ho1A Ho 0.43387(2) 0.74286(2) -0.01244(2) 0.02503(5) Uani 1 1 d . . . . .
N1 N 1.0719(2) 0.49744(17) 0.28439(10) 0.0229(6) Uani 1 1 d . . . . .
N1A N 0.5598(2) 0.72429(16) 0.04169(10) 0.0249(6) Uani 1 1 d . . . . .
Si1 Si 1.15780(9) 0.57392(6) 0.29897(4) 0.0299(2) Uani 1 1 d . . . . .
Si1A Si 0.65436(10) 0.65212(6) 0.05343(4) 0.0356(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Al2 2.085(4) . ?
C1 Ho1 2.524(4) . ?
C2 Al2 2.069(4) . ?
C2 Ho1 2.525(4) . ?
C1A Al2A 2.076(4) . ?
C1A Ho1A 2.523(4) . ?
C3 Al2 1.964(5) . ?
C2A Al2A 2.065(4) . ?
C2A Ho1A 2.503(4) . ?
C4 Al2 1.965(5) . ?
C3A Al2A 1.967(5) . ?
C5 Al1 2.059(4) . ?
C5 Ho1 2.631(4) . ?
C4A Al2A 1.966(5) . ?
C6 Al1 2.077(4) . ?
C6 Ho1 2.585(4) . ?
C5A Al1A 2.069(4) . ?
C5A Ho1A 2.616(4) . ?
C7 Al1 1.941(5) . ?
C6A Al1A 2.065(4) . ?
C6A Ho1A 2.569(4) . ?
C8 Al1 1.975(4) . ?
C7A Al1A 1.946(5) . ?
C9 C14 1.416(5) . ?
C9 N1 1.422(4) . ?
C9 C10 1.425(5) . ?
C9 Ho1 2.694(3) . ?
C8A Al1A 1.985(5) . ?
C10 C11 1.376(5) . ?
C10 C18 1.519(5) . ?
C9A C14A 1.422(5) . ?
C9A N1A 1.423(4) . ?
C9A C10A 1.424(5) . ?
C9A Ho1A 2.750(3) . ?
C11 C12 1.378(6) . ?
C10A C11A 1.388(5) . ?
C10A C18A 1.515(5) . ?
C12 C13 1.370(5) . ?
C11A C12A 1.366(6) . ?
C13 C14 1.391(5) . ?
C12A C13A 1.380(5) . ?
C14 C15 1.520(5) . ?
C13A C14A 1.393(5) . ?
C15 C17 1.526(5) . ?
C15 C16 1.537(6) . ?
C14A C15A 1.520(5) . ?
C15A C17A 1.533(5) . ?
C15A C16A 1.540(6) . ?
C18 C20 1.529(6) . ?
C18 C19 1.532(6) . ?
C18A C20A 1.538(6) . ?
C18A C19A 1.539(6) . ?
C21 Si1 1.859(4) . ?
C22 Si1 1.860(4) . ?
C21A Si1A 1.870(4) . ?
C23 Si1 1.864(4) . ?
C22A Si1A 1.864(5) . ?
C23A Si1A 1.860(5) . ?
Al1 Ho1 2.8824(14) . ?
Al2 Ho1 3.0775(14) . ?
Al1A Ho1A 2.8903(14) . ?
Al2A Ho1A 3.0807(14) . ?
Ho1 N1 2.160(3) . ?
Ho1A N1A 2.154(3) . ?
N1 Si1 1.731(3) . ?
N1A Si1A 1.727(3) . ?

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
Al2 C1 Ho1 83.19(14) . . ?
Al2 C2 Ho1 83.49(13) . . ?
Al2A C1A Ho1A 83.50(14) . . ?
Al2A C2A Ho1A 84.24(13) . . ?
Al1 C5 Ho1 74.73(12) . . ?
Al1 C6 Ho1 75.49(13) . . ?
Al1A C5A Ho1A 75.18(12) . . ?
Al1A C6A Ho1A 76.32(14) . . ?
C14 C9 N1 119.8(3) . . ?
C14 C9 C10 118.4(3) . . ?
N1 C9 C10 121.5(3) . . ?
C14 C9 Ho1 100.0(2) . . ?
N1 C9 Ho1 52.95(16) . . ?
C10 C9 Ho1 111.9(2) . . ?
C11 C10 C9 119.2(3) . . ?
C11 C10 C18 118.2(3) . . ?
C9 C10 C18 122.5(3) . . ?
C14A C9A N1A 120.1(3) . . ?
C14A C9A C10A 118.7(3) . . ?
N1A C9A C10A 121.0(3) . . ?
C14A C9A Ho1A 103.8(2) . . ?
N1A C9A Ho1A 50.80(16) . . ?
C10A C9A Ho1A 109.6(2) . . ?
C10 C11 C12 121.8(3) . . ?
C11A C10A C9A 119.0(3) . . ?
C11A C10A C18A 118.2(3) . . ?
C9A C10A C18A 122.7(3) . . ?
C13 C12 C11 119.6(4) . . ?
C12A C11A C10A 122.0(3) . . ?
C12 C13 C14 121.3(4) . . ?
C11A C12A C13A 119.5(4) . . ?
C13 C14 C9 119.3(3) . . ?
C13 C14 C15 119.2(3) . . ?
C9 C14 C15 121.2(3) . . ?
C12A C13A C14A 121.4(4) . . ?
C14 C15 C17 115.0(3) . . ?
C14 C15 C16 107.9(3) . . ?
C17 C15 C16 108.4(3) . . ?
C13A C14A C9A 119.1(3) . . ?
C13A C14A C15A 119.4(3) . . ?
C9A C14A C15A 121.1(3) . . ?
C14A C15A C17A 113.6(3) . . ?
C14A C15A C16A 109.2(3) . . ?
C17A C15A C16A 108.5(3) . . ?
C10 C18 C20 112.5(4) . . ?
C10 C18 C19 111.0(4) . . ?
C20 C18 C19 108.6(3) . . ?
C10A C18A C20A 113.2(4) . . ?
C10A C18A C19A 109.8(4) . . ?
C20A C18A C19A 108.7(4) . . ?
C7 Al1 C8 116.7(3) . . ?
C7 Al1 C5 111.4(2) . . ?
C8 Al1 C5 105.08(19) . . ?
C7 Al1 C6 109.8(2) . . ?
C8 Al1 C6 105.74(19) . . ?
C5 Al1 C6 107.58(18) . . ?
C7 Al1 Ho1 161.3(2) . . ?
C8 Al1 Ho1 81.91(15) . . ?
C5 Al1 Ho1 61.72(12) . . ?
C6 Al1 Ho1 60.27(12) . . ?
C3 Al2 C4 117.2(2) . . ?
C3 Al2 C2 109.0(2) . . ?
C4 Al2 C2 106.8(2) . . ?
C3 Al2 C1 109.6(2) . . ?
C4 Al2 C1 105.3(2) . . ?
C2 Al2 C1 108.65(15) . . ?
C3 Al2 Ho1 118.28(16) . . ?
C4 Al2 Ho1 124.50(18) . . ?
C2 Al2 Ho1 54.60(10) . . ?
C1 Al2 Ho1 54.54(10) . . ?
C7A Al1A C8A 118.3(3) . . ?
C7A Al1A C6A 110.6(3) . . ?
C8A Al1A C6A 104.90(19) . . ?
C7A Al1A C5A 108.7(2) . . ?
C8A Al1A C5A 106.6(2) . . ?
C6A Al1A C5A 107.18(18) . . ?
C7A Al1A Ho1A 158.1(2) . . ?
C8A Al1A Ho1A 83.60(16) . . ?
C6A Al1A Ho1A 59.71(12) . . ?
C5A Al1A Ho1A 61.04(12) . . ?
C4A Al2A C3A 117.2(2) . . ?
C4A Al2A C2A 106.1(2) . . ?
C3A Al2A C2A 110.5(2) . . ?
C4A Al2A C1A 106.2(2) . . ?
C3A Al2A C1A 108.6(2) . . ?
C2A Al2A C1A 107.75(16) . . ?
C4A Al2A Ho1A 125.23(18) . . ?
C3A Al2A Ho1A 117.51(16) . . ?
C2A Al2A Ho1A 53.92(10) . . ?
C1A Al2A Ho1A 54.46(11) . . ?
N1 Ho1 C1 96.41(12) . . ?
N1 Ho1 C2 117.25(12) . . ?
C1 Ho1 C2 83.87(13) . . ?
N1 Ho1 C6 98.72(12) . . ?
C1 Ho1 C6 86.84(13) . . ?
C2 Ho1 C6 143.58(14) . . ?
N1 Ho1 C5 113.94(12) . . ?
C1 Ho1 C5 148.15(13) . . ?
C2 Ho1 C5 90.20(13) . . ?
C6 Ho1 C5 79.54(13) . . ?
N1 Ho1 C9 31.69(10) . . ?
C1 Ho1 C9 126.67(12) . . ?
C2 Ho1 C9 106.91(12) . . ?
C6 Ho1 C9 106.85(12) . . ?
C5 Ho1 C9 84.99(12) . . ?
N1 Ho1 Al1 131.15(8) . . ?
C1 Ho1 Al1 108.73(10) . . ?
C2 Ho1 Al1 106.77(10) . . ?
C6 Ho1 Al1 44.24(10) . . ?
C5 Ho1 Al1 43.55(9) . . ?
C9 Ho1 Al1 116.81(8) . . ?
N1 Ho1 Al2 108.70(8) . . ?
C1 Ho1 Al2 42.27(9) . . ?
C2 Ho1 Al2 41.91(9) . . ?
C6 Ho1 Al2 123.03(10) . . ?
C5 Ho1 Al2 127.32(9) . . ?
C9 Ho1 Al2 122.75(8) . . ?
Al1 Ho1 Al2 118.19(4) . . ?
N1A Ho1A C2A 99.22(13) . . ?
N1A Ho1A C1A 114.26(13) . . ?
C2A Ho1A C1A 83.47(14) . . ?
N1A Ho1A C6A 100.09(13) . . ?
C2A Ho1A C6A 90.31(13) . . ?
C1A Ho1A C6A 145.63(14) . . ?
N1A Ho1A C5A 113.70(12) . . ?
C2A Ho1A C5A 146.75(14) . . ?
C1A Ho1A C5A 87.06(14) . . ?
C6A Ho1A C5A 79.83(14) . . ?
N1A Ho1A C9A 30.80(10) . . ?
C2A Ho1A C9A 128.07(12) . . ?
C1A Ho1A C9A 103.17(13) . . ?
C6A Ho1A C9A 107.14(12) . . ?
C5A Ho1A C9A 85.12(12) . . ?
N1A Ho1A Al1A 131.65(8) . . ?
C2A Ho1A Al1A 109.65(10) . . ?
C1A Ho1A Al1A 107.03(11) . . ?
C6A Ho1A Al1A 43.97(10) . . ?
C5A Ho1A Al1A 43.78(10) . . ?
C9A Ho1A Al1A 116.80(8) . . ?
N1A Ho1A Al2A 107.99(8) . . ?
C2A Ho1A Al2A 41.83(10) . . ?
C1A Ho1A Al2A 42.04(10) . . ?
C6A Ho1A Al2A 126.74(10) . . ?
C5A Ho1A Al2A 124.59(10) . . ?
C9A Ho1A Al2A 120.20(8) . . ?
Al1A Ho1A Al2A 119.50(4) . . ?
C9 N1 Si1 127.1(2) . . ?
C9 N1 Ho1 95.4(2) . . ?
Si1 N1 Ho1 137.52(16) . . ?
C9A N1A Si1A 126.9(2) . . ?
C9A N1A Ho1A 98.4(2) . . ?
Si1A N1A Ho1A 134.57(16) . . ?
N1 Si1 C21 111.24(18) . . ?
N1 Si1 C22 109.99(18) . . ?
C21 Si1 C22 106.9(2) . . ?
N1 Si1 C23 111.74(18) . . ?
C21 Si1 C23 108.5(2) . . ?
C22 Si1 C23 108.3(2) . . ?
N1A Si1A C23A 111.7(2) . . ?
N1A Si1A C22A 109.13(19) . . ?
C23A Si1A C22A 106.7(2) . . ?
N1A Si1A C21A 111.78(19) . . ?
C23A Si1A C21A 108.5(3) . . ?
C22A Si1A C21A 108.9(2) . . ?

_refine_diff_density_max         0.581
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.104

_shelxl_version_number           2013-3


_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_Compound_5-La
_database_code_depnum_ccdc_archive 'CCDC 1410388'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H50 Al2 La N Si'
_chemical_formula_weight         561.60

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'
Al Al 0.0645 0.0514 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.3816(9)
_cell_length_b                   12.6128(8)
_cell_length_c                   12.7570(12)
_cell_angle_alpha                90
_cell_angle_beta                 94.340(8)
_cell_angle_gamma                90
_cell_volume                     1505.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    25625
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      27.27

_exptl_crystal_description       column
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_F_000             584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.526
_shelx_estimated_absorpt_T_min   0.580
_shelx_estimated_absorpt_T_max   0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5420
_exptl_absorpt_correction_T_max  1.1208
_exptl_absorpt_process_details   Platon/mulabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Phi
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22337
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.203
_diffrn_reflns_theta_max         26.740
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6352
_reflns_number_gt                6054
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0361P)²+0.2844P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2756 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.021(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6352
_refine_ls_number_parameters     269
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0644
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.68793(2) 0.37397(2) 0.81904(2) 0.02392(8) Uani 1 1 d . . . . .
Si1 Si 0.66264(13) 0.38708(13) 0.52355(9) 0.0240(3) Uani 1 1 d . . . . .
N1 N 0.6516(4) 0.4351(3) 0.6497(3) 0.0208(7) Uani 1 1 d . . . . .
C1 C 0.9222(5) 0.4595(4) 0.9244(4) 0.0333(11) Uani 1 1 d . . . A 3
H1A H 0.9240 0.3819 0.9284 0.050 Uiso 1 1 calc R U . A 3
H1B H 1.0180 0.4873 0.9440 0.050 Uiso 1 1 calc R U . A 3
H1C H 0.8918 0.4814 0.8525 0.050 Uiso 1 1 calc R U . A 3
C2 C 0.5717(5) 0.4746(5) 0.9804(4) 0.0358(11) Uani 1 1 d . . . A 3
H2A H 0.5636 0.3971 0.9818 0.054 Uiso 1 1 calc R U . A 3
H2B H 0.5467 0.5003 0.9089 0.054 Uiso 1 1 calc R U . A 3
H2C H 0.5066 0.5055 1.0286 0.054 Uiso 1 1 calc R U . A 3
C3 C 0.7878(7) 0.6743(5) 1.0248(5) 0.0479(15) Uani 1 1 d . . . A 3
H3A H 0.7140 0.7015 0.9732 0.072 Uiso 1 1 calc R U . A 3
H3B H 0.8821 0.6972 1.0055 0.072 Uiso 1 1 calc R U . A 3
H3C H 0.7711 0.7019 1.0946 0.072 Uiso 1 1 calc R U . A 3
C4 C 0.8247(7) 0.4522(6) 1.1654(4) 0.0486(15) Uani 1 1 d . . . A 3
H4A H 0.8256 0.3749 1.1576 0.073 Uiso 1 1 calc R U . A 3
H4B H 0.7521 0.4725 1.2129 0.073 Uiso 1 1 calc R U . A 3
H4C H 0.9189 0.4764 1.1944 0.073 Uiso 1 1 calc R U . A 3
C5 C 0.8759(6) 0.2161(4) 0.7514(4) 0.0331(11) Uani 1 1 d . . . B 3
H5A H 0.8558 0.2924 0.7516 0.050 Uiso 1 1 calc R U . B 3
H5B H 0.8646 0.1894 0.6792 0.050 Uiso 1 1 calc R U . B 3
H5C H 0.9741 0.2035 0.7806 0.050 Uiso 1 1 calc R U . B 3
C6 C 0.5316(5) 0.1931(4) 0.7947(4) 0.0329(11) Uani 1 1 d . . . B 3
H6A H 0.4937 0.2333 0.8522 0.049 Uiso 1 1 calc R U . B 3
H6B H 0.4689 0.1327 0.7766 0.049 Uiso 1 1 calc R U . B 3
H6C H 0.5360 0.2392 0.7331 0.049 Uiso 1 1 calc R U . B 3
C7 C 0.7481(7) -0.0141(4) 0.8243(5) 0.0456(14) Uani 1 1 d . . . B 3
H7A H 0.7433 -0.0315 0.7492 0.068 Uiso 1 1 calc R U . B 3
H7B H 0.6686 -0.0483 0.8567 0.068 Uiso 1 1 calc R U . B 3
H7C H 0.8390 -0.0396 0.8582 0.068 Uiso 1 1 calc R U . B 3
C8 C 0.7661(7) 0.1937(5) 0.9878(4) 0.0394(13) Uani 1 1 d . . . B 3
H8A H 0.7443 0.2697 0.9884 0.059 Uiso 1 1 calc R U . B 3
H8B H 0.8659 0.1825 1.0139 0.059 Uiso 1 1 calc R U . B 3
H8C H 0.7031 0.1562 1.0332 0.059 Uiso 1 1 calc R U . B 3
C9 C 0.5915(5) 0.5327(3) 0.6802(3) 0.0206(8) Uani 1 1 d . . . C 3
C10 C 0.4463(5) 0.5377(4) 0.7031(3) 0.0239(9) Uani 1 1 d . . . C 3
C11 C 0.3955(5) 0.6299(4) 0.7491(4) 0.0303(10) Uani 1 1 d . . . C 3
H11 H 0.2978 0.6340 0.7635 0.036 Uiso 1 1 calc R U . C 3
C12 C 0.4840(6) 0.7142(4) 0.7739(4) 0.0324(11) Uani 1 1 d . . . C 3
H12 H 0.4487 0.7746 0.8080 0.039 Uiso 1 1 calc R U . C 3
C13 C 0.6247(6) 0.7109(4) 0.7492(4) 0.0313(10) Uani 1 1 d . . . C 3
H13 H 0.6846 0.7705 0.7647 0.038 Uiso 1 1 calc R U . C 3
C14 C 0.6808(5) 0.6224(4) 0.7022(4) 0.0244(9) Uani 1 1 d . . . C 3
C15 C 0.8325(5) 0.6262(4) 0.6664(4) 0.0297(10) Uani 1 1 d . . . C 3
H15A H 0.8693 0.5519 0.6645 0.036 Uiso 1 1 calc R U . C 3
C16 C 0.8278(7) 0.6711(5) 0.5549(5) 0.0456(14) Uani 1 1 d . . . C 3
H16A H 0.7643 0.6275 0.5080 0.068 Uiso 1 1 calc R U . C 3
H16B H 0.9242 0.6705 0.5302 0.068 Uiso 1 1 calc R U . C 3
H16C H 0.7918 0.7440 0.5549 0.068 Uiso 1 1 calc R U . C 3
C17 C 0.9369(6) 0.6909(4) 0.7384(5) 0.0418(13) Uani 1 1 d . . . C 3
H17A H 0.9393 0.6626 0.8100 0.063 Uiso 1 1 calc R U . C 3
H17B H 0.9057 0.7651 0.7384 0.063 Uiso 1 1 calc R U . C 3
H17C H 1.0326 0.6867 0.7128 0.063 Uiso 1 1 calc R U . C 3
C18 C 0.3396(5) 0.4504(4) 0.6728(5) 0.0344(12) Uani 1 1 d . . . C 3
H18 H 0.3940 0.3885 0.6474 0.041 Uiso 1 1 calc R U . C 3
C19 C 0.2338(7) 0.4871(6) 0.5820(6) 0.0515(15) Uani 1 1 d . . . C 3
H19A H 0.1754 0.4268 0.5560 0.077 Uiso 1 1 calc R U . C 3
H19B H 0.2869 0.5153 0.5249 0.077 Uiso 1 1 calc R U . C 3
H19C H 0.1716 0.5425 0.6072 0.077 Uiso 1 1 calc R U . C 3
C20 C 0.2566(7) 0.4128(5) 0.7645(6) 0.0531(17) Uani 1 1 d . . . C 3
H20A H 0.3239 0.3933 0.8239 0.080 Uiso 1 1 calc R U . C 3
H20B H 0.1983 0.3511 0.7426 0.080 Uiso 1 1 calc R U . C 3
H20C H 0.1943 0.4701 0.7859 0.080 Uiso 1 1 calc R U . C 3
C21 C 0.8507(6) 0.3839(7) 0.4859(4) 0.0432(13) Uani 1 1 d . . . D 3
H21A H 0.9087 0.3401 0.5362 0.065 Uiso 1 1 calc R U . D 3
H21B H 0.8891 0.4562 0.4865 0.065 Uiso 1 1 calc R U . D 3
H21C H 0.8531 0.3539 0.4152 0.065 Uiso 1 1 calc R U . D 3
C22 C 0.5538(7) 0.4657(5) 0.4235(4) 0.0405(13) Uani 1 1 d . . . E 3
H22A H 0.5707 0.5415 0.4362 0.061 Uiso 1 1 calc R U . E 3
H22B H 0.4523 0.4499 0.4284 0.061 Uiso 1 1 calc R U . E 3
H22C H 0.5812 0.4472 0.3531 0.061 Uiso 1 1 calc R U . E 3
C23 C 0.5945(8) 0.2485(4) 0.5172(4) 0.0433(14) Uani 1 1 d . . . F 3
H23A H 0.6511 0.2048 0.5685 0.065 Uiso 1 1 calc R U . F 3
H23B H 0.6026 0.2201 0.4464 0.065 Uiso 1 1 calc R U . F 3
H23C H 0.4941 0.2477 0.5335 0.065 Uiso 1 1 calc R U . F 3
Al1 Al 0.77986(18) 0.51822(14) 1.02701(13) 0.0305(3) Uani 1 1 d . . . A 3
Al2 Al 0.73544(17) 0.13858(11) 0.84157(12) 0.0298(3) Uani 1 1 d . . . B 3


_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 N1 2.295(4) . ?
La1 C1 2.712(5) . ?
La1 C2 2.716(5) . ?
La1 C6 2.717(5) . ?
La1 C9 2.779(4) . ?
La1 C5 2.837(5) . ?
La1 Al2 3.0127(14) . ?
La1 Al1 3.2782(16) . ?
Si1 N1 1.730(4) . ?
Si1 C22 1.860(5) . ?
Si1 C23 1.861(6) . ?
Si1 C21 1.863(5) . ?
N1 C9 1.421(5) . ?
C1 Al1 2.076(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 Al1 2.072(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 Al1 1.971(7) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 Al1 1.968(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 Al2 2.060(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 Al2 2.077(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 Al2 1.943(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 Al2 1.992(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.416(6) . ?
C9 C14 1.423(6) . ?
C10 C11 1.402(6) . ?
C10 C18 1.518(7) . ?
C11 C12 1.371(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.527(6) . ?
C15 C17 1.527(7) . ?
C15 C16 1.529(8) . ?
C15 H15A 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.530(8) . ?
C18 C19 1.539(8) . ?
C18 H18 1.0000 . ?
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 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 . ?

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
N1 La1 C6 97.69(14) . . ?
N1 La1 C9 30.67(12) . . ?
C6 La1 C9 112.66(14) . . ?
N1 La1 C5 90.07(14) . . ?
C6 La1 C5 73.66(16) . . ?
C9 La1 C5 119.46(13) . . ?
N1 La1 Al2 115.55(9) . . ?
C6 La1 Al2 42.12(11) . . ?
C9 La1 Al2 144.06(9) . . ?
C5 La1 Al2 41.11(11) . . ?
N1 La1 Al1 125.92(9) . . ?
C6 La1 Al1 131.70(12) . . ?
C9 La1 Al1 99.72(9) . . ?
C5 La1 Al1 120.27(11) . . ?
Al2 La1 Al1 116.22(4) . . ?
N1 Si1 C22 112.5(2) . . ?
N1 Si1 C23 108.9(2) . . ?
C22 Si1 C23 107.6(3) . . ?
N1 Si1 C21 111.8(2) . . ?
C22 Si1 C21 108.4(3) . . ?
C23 Si1 C21 107.3(4) . . ?
C9 N1 Si1 127.7(3) . . ?
C9 N1 La1 93.8(2) . . ?
Si1 N1 La1 137.97(19) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Al1 C2 H2A 109.5 . . ?
Al1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Al1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Al1 C3 H3A 109.5 . . ?
Al1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Al1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Al1 C4 H4A 109.5 . . ?
Al1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Al1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Al2 C5 La1 74.03(15) . . ?
Al2 C5 H5A 109.5 . . ?
La1 C5 H5A 35.6 . . ?
Al2 C5 H5B 109.5 . . ?
La1 C5 H5B 120.1 . . ?
H5A C5 H5B 109.5 . . ?
Al2 C5 H5C 109.5 . . ?
La1 C5 H5C 125.9 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Al2 C6 La1 76.57(16) . . ?
Al2 C6 H6A 109.5 . . ?
La1 C6 H6A 72.8 . . ?
Al2 C6 H6B 109.5 . . ?
La1 C6 H6B 171.7 . . ?
H6A C6 H6B 109.5 . . ?
Al2 C6 H6C 109.5 . . ?
La1 C6 H6C 62.6 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Al2 C7 H7A 109.5 . . ?
Al2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Al2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Al2 C8 H8A 109.5 . . ?
Al2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Al2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N1 120.2(4) . . ?
C10 C9 C14 119.0(4) . . ?
N1 C9 C14 120.2(4) . . ?
C10 C9 La1 100.0(3) . . ?
N1 C9 La1 55.5(2) . . ?
C14 C9 La1 106.8(3) . . ?
C11 C10 C9 119.1(4) . . ?
C11 C10 C18 118.0(4) . . ?
C9 C10 C18 122.7(4) . . ?
C12 C11 C10 121.4(4) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 119.8(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.5(4) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C9 119.1(4) . . ?
C13 C14 C15 119.7(4) . . ?
C9 C14 C15 120.9(4) . . ?
C14 C15 C17 114.0(4) . . ?
C14 C15 C16 109.1(4) . . ?
C17 C15 C16 109.5(4) . . ?
C14 C15 H15A 108.0 . . ?
C17 C15 H15A 108.0 . . ?
C16 C15 H15A 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C10 C18 C20 113.2(5) . . ?
C10 C18 C19 110.4(5) . . ?
C20 C18 C19 109.4(5) . . ?
C10 C18 H18 107.9 . . ?
C20 C18 H18 107.9 . . ?
C19 C18 H18 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C4 Al1 C3 115.5(3) . . ?
C4 Al1 C2 106.1(3) . . ?
C3 Al1 C2 107.3(3) . . ?
C4 Al1 C1 108.1(3) . . ?
C3 Al1 C1 108.7(3) . . ?
C2 Al1 C1 111.2(2) . . ?
C4 Al1 La1 121.1(2) . . ?
C3 Al1 La1 123.4(2) . . ?
C2 Al1 La1 55.66(15) . . ?
C1 Al1 La1 55.53(15) . . ?
C7 Al2 C8 116.5(3) . . ?
C7 Al2 C5 111.1(3) . . ?
C8 Al2 C5 107.7(2) . . ?
C7 Al2 C6 111.0(3) . . ?
C8 Al2 C6 102.6(2) . . ?
C5 Al2 C6 107.2(2) . . ?
C7 Al2 La1 167.4(2) . . ?
C8 Al2 La1 75.81(18) . . ?
C5 Al2 La1 64.86(14) . . ?
C6 Al2 La1 61.30(14) . . ?

_refine_diff_density_max         0.517
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.065

_shelxl_version_number           2013-3


_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_Compound_5-Nd
_database_code_depnum_ccdc_archive 'CCDC 1410389'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H50 Al2 N Nd Si'
_chemical_formula_weight         566.93

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.2588(5)
_cell_length_b                   17.4136(7)
_cell_length_c                   28.1778(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.984(4)
_cell_angle_gamma                90
_cell_volume                     6011.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    44385
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      27.28

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             2360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.834
_shelx_estimated_absorpt_T_min   0.609
_shelx_estimated_absorpt_T_max   0.711
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_process_details   XRed/XShape

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       PHI
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78595
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.015
_diffrn_reflns_theta_max         26.754
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12710
_reflns_number_gt                10813
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-AREA
_computing_cell_refinement       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0287P)²+4.9113P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12710
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0729
_refine_ls_wR_factor_gt          0.0696
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5129(3) 0.15727(19) 0.42173(12) 0.0366(8) Uani 1 1 d . . . . .
H1A H 0.4334 0.1510 0.4201 0.055 Uiso 1 1 calc R U . . .
H1B H 0.5386 0.1583 0.4551 0.055 Uiso 1 1 calc R U . . .
H1C H 0.5471 0.1142 0.4055 0.055 Uiso 1 1 calc R U . . .
C2 C 0.4862(3) 0.3512(2) 0.42424(13) 0.0402(8) Uani 1 1 d . . . . .
H2A H 0.4065 0.3461 0.4232 0.060 Uiso 1 1 calc R U . . .
H2B H 0.5066 0.3992 0.4088 0.060 Uiso 1 1 calc R U . . .
H2C H 0.5131 0.3516 0.4574 0.060 Uiso 1 1 calc R U . . .
C1A C 0.0188(3) 0.6329(2) 0.16241(12) 0.0385(8) Uani 1 1 d . . . . .
H1D H 0.0543 0.6394 0.1939 0.058 Uiso 1 1 calc R U . . .
H1E H -0.0603 0.6289 0.1657 0.058 Uiso 1 1 calc R U . . .
H1F H 0.0353 0.6773 0.1425 0.058 Uiso 1 1 calc R U . . .
C3 C 0.7142(4) 0.2719(3) 0.39219(16) 0.0559(11) Uani 1 1 d . . . . .
H3A H 0.7404 0.2716 0.4255 0.084 Uiso 1 1 calc R U . . .
H3B H 0.7336 0.3209 0.3775 0.084 Uiso 1 1 calc R U . . .
H3C H 0.7482 0.2296 0.3751 0.084 Uiso 1 1 calc R U . . .
C2A C 0.0249(3) 0.43770(19) 0.16807(12) 0.0377(8) Uani 1 1 d . . . . .
H2D H 0.0595 0.4374 0.1999 0.057 Uiso 1 1 calc R U . . .
H2E H 0.0457 0.3912 0.1510 0.057 Uiso 1 1 calc R U . . .
H2F H -0.0546 0.4391 0.1706 0.057 Uiso 1 1 calc R U . . .
C4 C 0.4807(5) 0.2571(3) 0.32530(14) 0.0676(13) Uani 1 1 d . . . . .
H4A H 0.4020 0.2504 0.3287 0.101 Uiso 1 1 calc R U . . .
H4B H 0.5095 0.2144 0.3069 0.101 Uiso 1 1 calc R U . . .
H4C H 0.4943 0.3056 0.3088 0.101 Uiso 1 1 calc R U . . .
C3A C 0.2367(4) 0.5369(3) 0.13402(19) 0.0658(13) Uani 1 1 d . . . . .
H3D H 0.2628 0.5408 0.1672 0.099 Uiso 1 1 calc R U . . .
H3E H 0.2620 0.5815 0.1163 0.099 Uiso 1 1 calc R U . . .
H3F H 0.2652 0.4898 0.1200 0.099 Uiso 1 1 calc R U . . .
C5 C 0.2897(3) 0.1415(2) 0.51106(14) 0.0439(9) Uani 1 1 d . . . . .
H5A H 0.3637 0.1469 0.4995 0.066 Uiso 1 1 calc R U . . .
H5B H 0.2570 0.0939 0.4986 0.066 Uiso 1 1 calc R U . . .
H5C H 0.2927 0.1398 0.5458 0.066 Uiso 1 1 calc R U . . .
C4A C 0.0007(5) 0.5265(3) 0.06854(14) 0.0747(15) Uani 1 1 d . . . . .
H4D H -0.0784 0.5258 0.0725 0.112 Uiso 1 1 calc R U . . .
H4E H 0.0230 0.4791 0.0528 0.112 Uiso 1 1 calc R U . . .
H4F H 0.0200 0.5707 0.0491 0.112 Uiso 1 1 calc R U . . .
C6 C 0.2677(3) 0.3339(2) 0.51457(13) 0.0414(8) Uani 1 1 d . . . . .
H6A H 0.3428 0.3373 0.5039 0.062 Uiso 1 1 calc R U . . .
H6B H 0.2682 0.3332 0.5494 0.062 Uiso 1 1 calc R U . . .
H6C H 0.2260 0.3784 0.5028 0.062 Uiso 1 1 calc R U . . .
C5A C -0.2052(3) 0.4406(2) 0.24964(13) 0.0402(8) Uani 1 1 d . . . . .
H5D H -0.1286 0.4439 0.2410 0.060 Uiso 1 1 calc R U . . .
H5E H -0.2390 0.3952 0.2347 0.060 Uiso 1 1 calc R U . . .
H5F H -0.2092 0.4364 0.2842 0.060 Uiso 1 1 calc R U . . .
C7 C 0.0479(4) 0.2270(4) 0.5104(2) 0.091(2) Uani 1 1 d . . . . .
H7A H 0.0496 0.2259 0.5452 0.137 Uiso 1 1 calc R U . . .
H7B H 0.0137 0.1799 0.4980 0.137 Uiso 1 1 calc R U . . .
H7C H 0.0058 0.2716 0.4991 0.137 Uiso 1 1 calc R U . . .
C6A C -0.2099(3) 0.63310(19) 0.25623(13) 0.0378(8) Uani 1 1 d . . . . .
H6D H -0.1337 0.6341 0.2468 0.057 Uiso 1 1 calc R U . . .
H6E H -0.2124 0.6302 0.2909 0.057 Uiso 1 1 calc R U . . .
H6F H -0.2469 0.6799 0.2450 0.057 Uiso 1 1 calc R U . . .
C8 C 0.2141(4) 0.2356(2) 0.41890(14) 0.0544(11) Uani 1 1 d . . . . .
H8A H 0.2919 0.2384 0.4123 0.082 Uiso 1 1 calc R U . . .
H8B H 0.1763 0.2804 0.4052 0.082 Uiso 1 1 calc R U . . .
H8C H 0.1830 0.1886 0.4049 0.082 Uiso 1 1 calc R U . . .
C7A C -0.2591(4) 0.5472(2) 0.15784(13) 0.0471(9) Uani 1 1 d . . . . .
H7D H -0.1803 0.5497 0.1534 0.071 Uiso 1 1 calc R U . . .
H7E H -0.2938 0.5939 0.1451 0.071 Uiso 1 1 calc R U . . .
H7F H -0.2894 0.5023 0.1410 0.071 Uiso 1 1 calc R U . . .
C9 C 0.5420(2) 0.28836(17) 0.57253(10) 0.0234(6) Uani 1 1 d . . . . .
C8A C -0.4394(3) 0.5324(3) 0.2435(2) 0.0672(13) Uani 1 1 d . . . . .
H8D H -0.4436 0.5282 0.2781 0.101 Uiso 1 1 calc R U . . .
H8E H -0.4733 0.4871 0.2285 0.101 Uiso 1 1 calc R U . . .
H8F H -0.4779 0.5787 0.2325 0.101 Uiso 1 1 calc R U . . .
C10 C 0.4679(3) 0.28663(19) 0.61025(11) 0.0312(7) Uani 1 1 d . . . . .
C9A C 0.0542(2) 0.57264(17) 0.31502(10) 0.0248(6) Uani 1 1 d . . . . .
C11 C 0.4362(3) 0.3552(2) 0.63076(12) 0.0368(8) Uani 1 1 d . . . . .
H11A H 0.3868 0.3539 0.6560 0.044 Uiso 1 1 calc R U . . .
C10A C -0.0198(3) 0.57402(18) 0.35265(11) 0.0294(7) Uani 1 1 d . . . . .
C12 C 0.4739(3) 0.4246(2) 0.61563(12) 0.0376(8) Uani 1 1 d . . . . .
H12A H 0.4487 0.4709 0.6293 0.045 Uiso 1 1 calc R U . . .
C11A C -0.0481(3) 0.6446(2) 0.37220(12) 0.0381(8) Uani 1 1 d . . . . .
H11B H -0.0970 0.6457 0.3976 0.046 Uiso 1 1 calc R U . . .
C13 C 0.5490(3) 0.42689(18) 0.58028(12) 0.0320(7) Uani 1 1 d . . . . .
H13A H 0.5765 0.4752 0.5705 0.038 Uiso 1 1 calc R U . . .
C12A C -0.0072(3) 0.7127(2) 0.35563(13) 0.0388(8) Uani 1 1 d . . . . .
H12B H -0.0306 0.7602 0.3684 0.047 Uiso 1 1 calc R U . . .
C14 C 0.5857(2) 0.36020(17) 0.55853(10) 0.0247(6) Uani 1 1 d . . . . .
C13A C 0.0679(3) 0.71140(19) 0.32043(12) 0.0333(7) Uani 1 1 d . . . . .
H13B H 0.0967 0.7585 0.3094 0.040 Uiso 1 1 calc R U . . .
C15 C 0.6811(3) 0.36534(18) 0.52561(11) 0.0307(7) Uani 1 1 d . . . . .
H15A H 0.6705 0.3254 0.5004 0.037 Uiso 1 1 calc R U . . .
C14A C 0.1027(2) 0.64292(17) 0.30054(10) 0.0250(6) Uani 1 1 d . . . . .
C16 C 0.6929(3) 0.4430(2) 0.50132(13) 0.0443(9) Uani 1 1 d . . . . .
H16A H 0.7559 0.4417 0.4809 0.066 Uiso 1 1 calc R U . . .
H16B H 0.7036 0.4831 0.5254 0.066 Uiso 1 1 calc R U . . .
H16C H 0.6267 0.4540 0.4820 0.066 Uiso 1 1 calc R U . . .
C15A C 0.2006(3) 0.64298(19) 0.26886(11) 0.0317(7) Uani 1 1 d . . . . .
H15B H 0.1894 0.6022 0.2442 0.038 Uiso 1 1 calc R U . . .
C17 C 0.7866(3) 0.3473(2) 0.55339(14) 0.0443(9) Uani 1 1 d . . . . .
H17A H 0.8482 0.3508 0.5322 0.067 Uiso 1 1 calc R U . . .
H17B H 0.7828 0.2952 0.5664 0.067 Uiso 1 1 calc R U . . .
H17C H 0.7968 0.3842 0.5794 0.067 Uiso 1 1 calc R U . . .
C16A C 0.2206(3) 0.7196(2) 0.24376(14) 0.0438(9) Uani 1 1 d . . . . .
H16D H 0.2843 0.7149 0.2239 0.066 Uiso 1 1 calc R U . . .
H16E H 0.2338 0.7599 0.2675 0.066 Uiso 1 1 calc R U . . .
H16F H 0.1563 0.7329 0.2238 0.066 Uiso 1 1 calc R U . . .
C18 C 0.4247(3) 0.2117(2) 0.63050(13) 0.0393(8) Uani 1 1 d . . . . .
H18 H 0.4484 0.1683 0.6100 0.047 Uiso 1 1 calc R U . . .
C17A C 0.3023(3) 0.6226(2) 0.29942(14) 0.0420(8) Uani 1 1 d . . . . .
H17D H 0.3663 0.6221 0.2795 0.063 Uiso 1 1 calc R U . . .
H17E H 0.2928 0.5717 0.3136 0.063 Uiso 1 1 calc R U . . .
H17F H 0.3127 0.6609 0.3247 0.063 Uiso 1 1 calc R U . . .
C19 C 0.4735(4) 0.1995(3) 0.68090(16) 0.0672(14) Uani 1 1 d . . . . .
H19A H 0.4458 0.1513 0.6938 0.101 Uiso 1 1 calc R U . . .
H19B H 0.4527 0.2423 0.7012 0.101 Uiso 1 1 calc R U . . .
H19C H 0.5533 0.1970 0.6798 0.101 Uiso 1 1 calc R U . . .
C18A C -0.0691(3) 0.5015(2) 0.37307(12) 0.0369(8) Uani 1 1 d . . . . .
H18A H -0.0456 0.4567 0.3537 0.044 Uiso 1 1 calc R U . . .
C20 C 0.2998(3) 0.2099(2) 0.63264(14) 0.0485(10) Uani 1 1 d . . . . .
H20A H 0.2768 0.1606 0.6458 0.073 Uiso 1 1 calc R U . . .
H20B H 0.2675 0.2162 0.6006 0.073 Uiso 1 1 calc R U . . .
H20C H 0.2754 0.2518 0.6529 0.073 Uiso 1 1 calc R U . . .
C19A C -0.0265(4) 0.4896(3) 0.42513(14) 0.0582(11) Uani 1 1 d . . . . .
H19D H -0.0586 0.4427 0.4379 0.087 Uiso 1 1 calc R U . . .
H19E H -0.0472 0.5337 0.4444 0.087 Uiso 1 1 calc R U . . .
H19F H 0.0532 0.4847 0.4259 0.087 Uiso 1 1 calc R U . . .
C21 C 0.7253(4) 0.1586(2) 0.61650(16) 0.0588(12) Uani 1 1 d . . . . .
H21A H 0.6707 0.1627 0.6410 0.088 Uiso 1 1 calc R U . . .
H21B H 0.7702 0.2052 0.6167 0.088 Uiso 1 1 calc R U . . .
H21C H 0.7719 0.1139 0.6230 0.088 Uiso 1 1 calc R U . . .
C20A C -0.1937(3) 0.5036(2) 0.37218(13) 0.0440(9) Uani 1 1 d . . . . .
H20D H -0.2214 0.4558 0.3856 0.066 Uiso 1 1 calc R U . . .
H20E H -0.2215 0.5091 0.3393 0.066 Uiso 1 1 calc R U . . .
H20F H -0.2181 0.5473 0.3910 0.066 Uiso 1 1 calc R U . . .
C22 C 0.7607(3) 0.1423(3) 0.51136(17) 0.0612(12) Uani 1 1 d . . . . .
H22A H 0.8026 0.1903 0.5114 0.092 Uiso 1 1 calc R U . . .
H22B H 0.7252 0.1346 0.4800 0.092 Uiso 1 1 calc R U . . .
H22C H 0.8100 0.0992 0.5185 0.092 Uiso 1 1 calc R U . . .
C21A C 0.2225(4) 0.4377(2) 0.36272(14) 0.0504(10) Uani 1 1 d . . . . .
H21D H 0.2648 0.4855 0.3646 0.076 Uiso 1 1 calc R U . . .
H21E H 0.2711 0.3940 0.3690 0.076 Uiso 1 1 calc R U . . .
H21F H 0.1658 0.4388 0.3864 0.076 Uiso 1 1 calc R U . . .
C23 C 0.5795(4) 0.0548(2) 0.55489(16) 0.0526(11) Uani 1 1 d . . . . .
H23A H 0.5227 0.0553 0.5785 0.079 Uiso 1 1 calc R U . . .
H23B H 0.6304 0.0125 0.5618 0.079 Uiso 1 1 calc R U . . .
H23C H 0.5457 0.0479 0.5232 0.079 Uiso 1 1 calc R U . . .
C22A C 0.2678(3) 0.4193(2) 0.25842(15) 0.0522(10) Uani 1 1 d . . . . .
H22D H 0.3119 0.4663 0.2589 0.078 Uiso 1 1 calc R U . . .
H22E H 0.2350 0.4117 0.2265 0.078 Uiso 1 1 calc R U . . .
H22F H 0.3144 0.3753 0.2669 0.078 Uiso 1 1 calc R U . . .
C23A C 0.0779(3) 0.3371(2) 0.29916(14) 0.0460(9) Uani 1 1 d . . . . .
H23D H 0.0435 0.3316 0.2674 0.069 Uiso 1 1 calc R U . . .
H23E H 0.0215 0.3382 0.3229 0.069 Uiso 1 1 calc R U . . .
H23F H 0.1270 0.2936 0.3055 0.069 Uiso 1 1 calc R U . . .
Al1 Al 0.55442(10) 0.25926(6) 0.38908(4) 0.0392(2) Uani 1 1 d . . . . .
Al2 Al 0.19585(9) 0.23410(7) 0.48840(4) 0.0404(3) Uani 1 1 d . . . . .
Al1A Al 0.07601(10) 0.53410(6) 0.13123(4) 0.0411(3) Uani 1 1 d . . . . .
Al2A Al -0.28733(8) 0.53833(6) 0.22650(4) 0.0355(2) Uani 1 1 d . . . . .
N1 N 0.5639(2) 0.22171(14) 0.54521(9) 0.0253(5) Uani 1 1 d . . . . .
N1A N 0.0721(2) 0.50470(14) 0.28844(9) 0.0241(5) Uani 1 1 d . . . . .
Nd1 Nd 0.43811(2) 0.24547(2) 0.48842(2) 0.02617(5) Uani 1 1 d . . . . .
Nd1A Nd -0.04466(2) 0.53909(2) 0.22961(2) 0.02543(5) Uani 1 1 d . . . . .
Si1 Si 0.65507(8) 0.14766(5) 0.55723(3) 0.0347(2) Uani 1 1 d . . . . .
Si1A Si 0.15750(7) 0.42817(5) 0.30220(3) 0.03070(19) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Al1 2.072(4) . ?
C1 Nd1 2.617(3) . ?
C2 Al1 2.074(4) . ?
C2 Nd1 2.661(4) . ?
C1A Al1A 2.065(4) . ?
C1A Nd1A 2.638(3) . ?
C3 Al1 1.970(5) . ?
C2A Al1A 2.082(4) . ?
C2A Nd1A 2.637(3) . ?
C4 Al1 1.984(4) . ?
C3A Al1A 1.969(5) . ?
C5 Al2 2.069(4) . ?
C5 Nd1 2.661(4) . ?
C4A Al1A 1.969(5) . ?
C6 Al2 2.072(4) . ?
C6 Nd1 2.718(3) . ?
C5A Al2A 2.071(4) . ?
C5A Nd1A 2.685(4) . ?
C7 Al2 1.941(5) . ?
C6A Al2A 2.067(4) . ?
C6A Nd1A 2.730(3) . ?
C8 Al2 1.979(4) . ?
C7A Al2A 1.983(4) . ?
C9 C14 1.422(4) . ?
C9 C10 1.422(4) . ?
C9 N1 1.423(4) . ?
C9 Nd1 2.755(3) . ?
C8A Al2A 1.943(4) . ?
C10 C11 1.388(5) . ?
C10 C18 1.527(5) . ?
C9A C10A 1.419(4) . ?
C9A N1A 1.421(4) . ?
C9A C14A 1.427(4) . ?
C9A Nd1A 2.720(3) . ?
C11 C12 1.368(5) . ?
C10A C11A 1.397(4) . ?
C10A C18A 1.521(5) . ?
C12 C13 1.380(5) . ?
C11A C12A 1.375(5) . ?
C13 C14 1.395(4) . ?
C12A C13A 1.377(5) . ?
C14 C15 1.521(4) . ?
C13A C14A 1.391(4) . ?
C15 C17 1.521(5) . ?
C15 C16 1.524(5) . ?
C14A C15A 1.520(4) . ?
C15A C17A 1.532(5) . ?
C15A C16A 1.534(5) . ?
C18 C20 1.535(5) . ?
C18 C19 1.537(5) . ?
C18A C20A 1.527(5) . ?
C18A C19A 1.554(5) . ?
C21 Si1 1.862(4) . ?
C22 Si1 1.863(5) . ?
C21A Si1A 1.865(4) . ?
C23 Si1 1.863(4) . ?
C22A Si1A 1.868(4) . ?
C23A Si1A 1.862(4) . ?
Al1 Nd1 3.1940(10) . ?
Al2 Nd1 2.9764(11) . ?
Al1A Nd1A 3.1881(10) . ?
Al2A Nd1A 2.9732(10) . ?
N1 Si1 1.732(3) . ?
N1 Nd1 2.222(2) . ?
N1A Si1A 1.730(3) . ?
N1A Nd1A 2.234(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Al1 C1 Nd1 85.02(11) . . ?
Al1 C2 Nd1 83.88(12) . . ?
Al1A C1A Nd1A 84.40(12) . . ?
Al1A C2A Nd1A 84.13(11) . . ?
Al2 C5 Nd1 76.86(12) . . ?
Al2 C6 Nd1 75.49(11) . . ?
Al2A C5A Nd1A 76.16(11) . . ?
Al2A C6A Nd1A 75.20(10) . . ?
C14 C9 C10 118.8(3) . . ?
C14 C9 N1 119.2(3) . . ?
C10 C9 N1 121.6(3) . . ?
C14 C9 Nd1 99.63(18) . . ?
C10 C9 Nd1 110.42(19) . . ?
N1 C9 Nd1 53.40(13) . . ?
C11 C10 C9 119.2(3) . . ?
C11 C10 C18 118.3(3) . . ?
C9 C10 C18 122.4(3) . . ?
C10A C9A N1A 121.5(3) . . ?
C10A C9A C14A 118.9(3) . . ?
N1A C9A C14A 119.3(3) . . ?
C10A C9A Nd1A 112.9(2) . . ?
N1A C9A Nd1A 55.08(14) . . ?
C14A C9A Nd1A 96.24(18) . . ?
C12 C11 C10 121.9(3) . . ?
C11A C10A C9A 118.9(3) . . ?
C11A C10A C18A 118.3(3) . . ?
C9A C10A C18A 122.8(3) . . ?
C11 C12 C13 119.5(3) . . ?
C12A C11A C10A 121.8(3) . . ?
C12 C13 C14 121.8(3) . . ?
C11A C12A C13A 119.4(3) . . ?
C13 C14 C9 118.7(3) . . ?
C13 C14 C15 119.0(3) . . ?
C9 C14 C15 121.7(3) . . ?
C12A C13A C14A 121.8(3) . . ?
C14 C15 C17 109.4(3) . . ?
C14 C15 C16 114.4(3) . . ?
C17 C15 C16 108.8(3) . . ?
C13A C14A C9A 118.9(3) . . ?
C13A C14A C15A 119.7(3) . . ?
C9A C14A C15A 120.9(3) . . ?
C14A C15A C17A 108.3(3) . . ?
C14A C15A C16A 114.4(3) . . ?
C17A C15A C16A 108.7(3) . . ?
C10 C18 C20 113.0(3) . . ?
C10 C18 C19 109.6(3) . . ?
C20 C18 C19 108.6(3) . . ?
C10A C18A C20A 112.6(3) . . ?
C10A C18A C19A 110.1(3) . . ?
C20A C18A C19A 108.8(3) . . ?
C3 Al1 C4 117.6(2) . . ?
C3 Al1 C1 109.59(18) . . ?
C4 Al1 C1 105.98(19) . . ?
C3 Al1 C2 108.02(17) . . ?
C4 Al1 C2 105.58(19) . . ?
C1 Al1 C2 109.88(14) . . ?
C3 Al1 Nd1 116.29(14) . . ?
C4 Al1 Nd1 126.12(17) . . ?
C1 Al1 Nd1 54.72(9) . . ?
C2 Al1 Nd1 55.92(10) . . ?
C7 Al2 C8 117.1(2) . . ?
C7 Al2 C5 111.5(2) . . ?
C8 Al2 C5 103.58(17) . . ?
C7 Al2 C6 109.28(19) . . ?
C8 Al2 C6 106.28(18) . . ?
C5 Al2 C6 108.62(16) . . ?
C7 Al2 Nd1 161.4(2) . . ?
C8 Al2 Nd1 81.52(14) . . ?
C5 Al2 Nd1 60.52(11) . . ?
C6 Al2 Nd1 62.13(10) . . ?
C3A Al1A C4A 118.3(2) . . ?
C3A Al1A C1A 108.44(18) . . ?
C4A Al1A C1A 106.4(2) . . ?
C3A Al1A C2A 108.55(18) . . ?
C4A Al1A C2A 104.65(19) . . ?
C1A Al1A C2A 110.30(14) . . ?
C3A Al1A Nd1A 117.27(16) . . ?
C4A Al1A Nd1A 124.37(18) . . ?
C1A Al1A Nd1A 55.45(10) . . ?
C2A Al1A Nd1A 55.36(9) . . ?
C8A Al2A C7A 116.5(2) . . ?
C8A Al2A C6A 111.94(18) . . ?
C7A Al2A C6A 103.91(16) . . ?
C8A Al2A C5A 109.8(2) . . ?
C7A Al2A C5A 105.76(16) . . ?
C6A Al2A C5A 108.49(15) . . ?
C8A Al2A Nd1A 163.77(17) . . ?
C7A Al2A Nd1A 79.65(13) . . ?
C6A Al2A Nd1A 62.58(10) . . ?
C5A Al2A Nd1A 61.27(10) . . ?
C9 N1 Si1 129.3(2) . . ?
C9 N1 Nd1 95.66(17) . . ?
Si1 N1 Nd1 134.93(13) . . ?
C9A N1A Si1A 128.8(2) . . ?
C9A N1A Nd1A 93.48(17) . . ?
Si1A N1A Nd1A 137.71(14) . . ?
N1 Nd1 C1 98.98(10) . . ?
N1 Nd1 C2 116.98(10) . . ?
C1 Nd1 C2 80.02(11) . . ?
N1 Nd1 C5 99.43(11) . . ?
C1 Nd1 C5 91.85(11) . . ?
C2 Nd1 C5 143.45(12) . . ?
N1 Nd1 C6 115.53(10) . . ?
C1 Nd1 C6 144.98(11) . . ?
C2 Nd1 C6 89.01(11) . . ?
C5 Nd1 C6 77.41(12) . . ?
N1 Nd1 C9 30.94(9) . . ?
C1 Nd1 C9 127.86(10) . . ?
C2 Nd1 C9 106.89(10) . . ?
C5 Nd1 C9 106.14(11) . . ?
C6 Nd1 C9 87.13(10) . . ?
N1 Nd1 Al2 130.93(7) . . ?
C1 Nd1 Al2 109.59(8) . . ?
C2 Nd1 Al2 106.88(8) . . ?
C5 Nd1 Al2 42.61(9) . . ?
C6 Nd1 Al2 42.38(8) . . ?
C9 Nd1 Al2 116.73(6) . . ?
N1 Nd1 Al1 108.99(7) . . ?
C1 Nd1 Al1 40.26(8) . . ?
C2 Nd1 Al1 40.21(8) . . ?
C5 Nd1 Al1 126.24(9) . . ?
C6 Nd1 Al1 124.45(9) . . ?
C9 Nd1 Al1 121.77(7) . . ?
Al2 Nd1 Al1 118.72(3) . . ?
N1A Nd1A C2A 95.45(10) . . ?
N1A Nd1A C1A 120.08(10) . . ?
C2A Nd1A C1A 80.36(11) . . ?
N1A Nd1A C5A 97.38(10) . . ?
C2A Nd1A C5A 88.08(11) . . ?
C1A Nd1A C5A 141.51(11) . . ?
N1A Nd1A C9A 31.44(9) . . ?
C2A Nd1A C9A 125.55(10) . . ?
C1A Nd1A C9A 111.63(10) . . ?
C5A Nd1A C9A 104.98(10) . . ?
N1A Nd1A C6A 114.80(10) . . ?
C2A Nd1A C6A 147.37(11) . . ?
C1A Nd1A C6A 93.78(11) . . ?
C5A Nd1A C6A 76.65(11) . . ?
C9A Nd1A C6A 86.56(10) . . ?
N1A Nd1A Al2A 129.46(7) . . ?
C2A Nd1A Al2A 108.88(9) . . ?
C1A Nd1A Al2A 107.53(8) . . ?
C5A Nd1A Al2A 42.56(8) . . ?
C9A Nd1A Al2A 116.20(7) . . ?
C6A Nd1A Al2A 42.22(8) . . ?
N1A Nd1A Al1A 109.45(7) . . ?
C2A Nd1A Al1A 40.51(8) . . ?
C1A Nd1A Al1A 40.15(8) . . ?
C5A Nd1A Al1A 122.06(8) . . ?
C9A Nd1A Al1A 124.70(7) . . ?
C6A Nd1A Al1A 128.78(8) . . ?
Al2A Nd1A Al1A 117.92(3) . . ?
N1 Si1 C21 111.96(16) . . ?
N1 Si1 C23 108.81(16) . . ?
C21 Si1 C23 109.6(2) . . ?
N1 Si1 C22 111.15(17) . . ?
C21 Si1 C22 108.4(2) . . ?
C23 Si1 C22 106.8(2) . . ?
N1A Si1A C23A 109.51(16) . . ?
N1A Si1A C21A 111.85(15) . . ?
C23A Si1A C21A 108.95(19) . . ?
N1A Si1A C22A 111.21(16) . . ?
C23A Si1A C22A 106.80(19) . . ?
C21A Si1A C22A 108.4(2) . . ?

_refine_diff_density_max         0.730
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.080

_shelxl_version_number           2013-3


_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_dr169decmulabs
_database_code_depnum_ccdc_archive 'CCDC 1410390'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H130 Ho3 N3 O3 Si3'
_chemical_formula_weight         1616.80

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.4783(2)
_cell_length_b                   26.0417(6)
_cell_length_c                   26.4880(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.6370(10)
_cell_angle_gamma                90
_cell_volume                     7847.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    2962
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      29.52

_exptl_crystal_description       plate
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             3304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.081
_shelx_estimated_absorpt_T_min   0.655
_shelx_estimated_absorpt_T_max   0.748
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.64937
_exptl_absorpt_correction_T_max  0.93769
_exptl_absorpt_process_details   mulabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       phi-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            98434
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.952
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14345
_reflns_number_gt                12656
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 ?
;

_vrf_PLAT342_dr169decmulabs      
;
PROBLEM:  Low Bond Precision on  C-C Bonds 
RESPONSE: The crystals showed bad quality and the 
          intensities therefore were low. The solvent molecule 
          and the THF were restraint with 'simu/delu/isor' instruction.		  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+63.9214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14345
_refine_ls_number_parameters     766
_refine_ls_number_restraints     184
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0893
_refine_ls_wR_factor_ref         0.1360
_refine_ls_wR_factor_gt          0.1329
_refine_ls_goodness_of_fit_ref   1.417
_refine_ls_restrained_S_all      1.409
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0262(8) 0.8886(4) 0.7441(4) 0.039(2) Uani 1 1 d . . . . .
H1A H -0.0976 0.9043 0.7252 0.047 Uiso 1 1 calc R U . . .
H1B H -0.0459 0.8671 0.7726 0.047 Uiso 1 1 calc R U . . .
C2 C 0.2596(8) 0.8600(4) 0.7762(4) 0.034(2) Uani 1 1 d . . . . .
H2A H 0.3356 0.8666 0.7644 0.051 Uiso 1 1 calc R U . . .
H2B H 0.2183 0.8328 0.7554 0.051 Uiso 1 1 calc R U . . .
H2C H 0.2722 0.8491 0.8119 0.051 Uiso 1 1 calc R U . . .
C3 C 0.1843(10) 0.9343(4) 0.6773(4) 0.045(3) Uani 1 1 d . . . . .
H3A H 0.1560 0.9463 0.6428 0.068 Uiso 1 1 calc R U . . .
H3B H 0.2702 0.9319 0.6816 0.068 Uiso 1 1 calc R U . . .
H3C H 0.1602 0.9586 0.7022 0.068 Uiso 1 1 calc R U . . .
C4 C 0.0704(9) 0.7684(4) 0.7477(4) 0.042(3) Uani 1 1 d . . . . .
H4A H -0.0022 0.7481 0.7428 0.063 Uiso 1 1 calc R U . . .
H4B H 0.1372 0.7456 0.7584 0.063 Uiso 1 1 calc R U . . .
H4C H 0.0817 0.7852 0.7156 0.063 Uiso 1 1 calc R U . . .
C5 C 0.1219(10) 0.9186(4) 0.8591(4) 0.049(3) Uani 1 1 d . . . . .
H5A H 0.0538 0.9358 0.8702 0.073 Uiso 1 1 calc R U . . .
H5B H 0.1569 0.9409 0.8354 0.073 Uiso 1 1 calc R U . . .
H5C H 0.1802 0.9114 0.8888 0.073 Uiso 1 1 calc R U . . .
C6 C -0.1580(11) 1.0008(6) 0.8304(6) 0.077(4) Uani 1 1 d . . . . .
H6A H -0.1509 0.9635 0.8271 0.115 Uiso 1 1 calc R U . . .
H6B H -0.2391 1.0096 0.8347 0.115 Uiso 1 1 calc R U . . .
H6C H -0.1048 1.0126 0.8601 0.115 Uiso 1 1 calc R U . . .
C7 C -0.1565(13) 1.1029(6) 0.7761(6) 0.080(5) Uani 1 1 d . . . . .
H7A H -0.1828 1.1098 0.8092 0.120 Uiso 1 1 calc R U . . .
H7B H -0.2195 1.1116 0.7488 0.120 Uiso 1 1 calc R U . . .
H7C H -0.0870 1.1237 0.7726 0.120 Uiso 1 1 calc R U . . .
C8 C -0.2208(10) 1.0061(6) 0.7166(6) 0.071(4) Uani 1 1 d . . . . .
H8A H -0.2003 1.0204 0.6847 0.106 Uiso 1 1 calc R U . . .
H8B H -0.3019 1.0155 0.7204 0.106 Uiso 1 1 calc R U . . .
H8C H -0.2134 0.9687 0.7160 0.106 Uiso 1 1 calc R U . . .
C9 C 0.1053(10) 1.0642(4) 0.7634(4) 0.045(3) Uani 1 1 d . . . . .
C10 C 0.1674(11) 1.0856(4) 0.8080(5) 0.052(3) Uani 1 1 d . . . . .
C11 C 0.2490(13) 1.1250(5) 0.8042(6) 0.073(4) Uani 1 1 d . . . . .
H11 H 0.2898 1.1395 0.8344 0.087 Uiso 1 1 calc R U . . .
C12 C 0.2716(14) 1.1432(5) 0.7570(6) 0.073(4) Uani 1 1 d . . . . .
H12 H 0.3298 1.1687 0.7549 0.087 Uiso 1 1 calc R U . . .
C13 C 0.2087(13) 1.1237(5) 0.7139(5) 0.066(4) Uani 1 1 d . . . . .
H13 H 0.2222 1.1371 0.6819 0.079 Uiso 1 1 calc R U . . .
C14 C 0.1256(11) 1.0849(4) 0.7150(5) 0.050(3) Uani 1 1 d . . . . .
C15 C 0.1448(13) 1.0688(5) 0.8608(4) 0.062(4) Uani 1 1 d . . . . .
H15 H 0.0981 1.0363 0.8564 0.075 Uiso 1 1 calc R U . . .
C16 C 0.2532(15) 1.0574(7) 0.8977(6) 0.097(5) Uani 1 1 d . . . . .
H16A H 0.3020 1.0323 0.8826 0.145 Uiso 1 1 calc R U . . .
H16B H 0.2301 1.0434 0.9292 0.145 Uiso 1 1 calc R U . . .
H16C H 0.2980 1.0892 0.9053 0.145 Uiso 1 1 calc R U . . .
C17 C 0.0700(18) 1.1082(8) 0.8861(6) 0.117(7) Uani 1 1 d . . . . .
H17A H 0.0470 1.0934 0.9173 0.175 Uiso 1 1 calc R U . . .
H17B H -0.0006 1.1167 0.8625 0.175 Uiso 1 1 calc R U . . .
H17C H 0.1162 1.1394 0.8945 0.175 Uiso 1 1 calc R U . . .
C18 C 0.0555(11) 1.0667(5) 0.6663(5) 0.056(3) Uani 1 1 d . . . . .
H18 H 0.0241 1.0318 0.6726 0.067 Uiso 1 1 calc R U . . .
C19 C 0.1284(12) 1.0623(5) 0.6214(5) 0.066(4) Uani 1 1 d . . . . .
H19A H 0.1489 1.0968 0.6106 0.098 Uiso 1 1 calc R U . . .
H19B H 0.0822 1.0446 0.5929 0.098 Uiso 1 1 calc R U . . .
H19C H 0.2005 1.0429 0.6323 0.098 Uiso 1 1 calc R U . . .
C20 C -0.0498(13) 1.1024(6) 0.6505(5) 0.079(5) Uani 1 1 d . . . . .
H20A H -0.0948 1.1066 0.6792 0.118 Uiso 1 1 calc R U . . .
H20B H -0.1003 1.0874 0.6215 0.118 Uiso 1 1 calc R U . . .
H20C H -0.0212 1.1360 0.6408 0.118 Uiso 1 1 calc R U . . .
C21 C -0.2097(13) 0.8553(6) 0.5276(5) 0.076(4) Uani 1 1 d . . . . .
H21A H -0.1520 0.8356 0.5115 0.115 Uiso 1 1 calc R U . . .
H21B H -0.2298 0.8868 0.5080 0.115 Uiso 1 1 calc R U . . .
H21C H -0.2807 0.8346 0.5284 0.115 Uiso 1 1 calc R U . . .
C22 C -0.2667(11) 0.8663(6) 0.6346(6) 0.074(4) Uani 1 1 d . . . . .
H22A H -0.2849 0.8299 0.6387 0.111 Uiso 1 1 calc R U . . .
H22B H -0.3368 0.8841 0.6181 0.111 Uiso 1 1 calc R U . . .
H22C H -0.2423 0.8816 0.6682 0.111 Uiso 1 1 calc R U . . .
C23 C -0.1068(12) 0.9421(5) 0.5949(6) 0.072(4) Uani 1 1 d . . . . .
H23A H -0.0727 0.9523 0.6293 0.108 Uiso 1 1 calc R U . . .
H23B H -0.1778 0.9623 0.5844 0.108 Uiso 1 1 calc R U . . .
H23C H -0.0495 0.9481 0.5712 0.108 Uiso 1 1 calc R U . . .
C24 C 0.0152(9) 0.7949(5) 0.5883(4) 0.045(3) Uani 1 1 d . . . . .
C25 C 0.0945(10) 0.8048(5) 0.5519(4) 0.054(3) Uani 1 1 d . . . . .
C26 C 0.1381(12) 0.7631(7) 0.5267(5) 0.072(4) Uani 1 1 d . . . . .
H26 H 0.1914 0.7693 0.5029 0.086 Uiso 1 1 calc R U . . .
C27 C 0.1063(13) 0.7137(7) 0.5354(6) 0.079(5) Uani 1 1 d . . . . .
H27 H 0.1383 0.6863 0.5181 0.094 Uiso 1 1 calc R U . . .
C28 C 0.0278(11) 0.7037(6) 0.5692(5) 0.066(4) Uani 1 1 d . . . . .
H28 H 0.0057 0.6692 0.5749 0.079 Uiso 1 1 calc R U . . .
C29 C -0.0197(10) 0.7434(5) 0.5952(4) 0.049(3) Uani 1 1 d . . . . .
C30 C 0.1316(11) 0.8580(6) 0.5397(5) 0.064(4) Uani 1 1 d . . . . .
H30 H 0.0976 0.8818 0.5635 0.077 Uiso 1 1 calc R U . . .
C31 C 0.0846(16) 0.8748(8) 0.4859(7) 0.119(7) Uani 1 1 d . . . . .
H31A H 0.1164 0.8523 0.4613 0.179 Uiso 1 1 calc R U . . .
H31B H 0.1085 0.9103 0.4806 0.179 Uiso 1 1 calc R U . . .
H31C H -0.0014 0.8725 0.4809 0.179 Uiso 1 1 calc R U . . .
C32 C 0.2636(12) 0.8666(7) 0.5471(6) 0.097(6) Uani 1 1 d . . . . .
H32A H 0.2952 0.8601 0.5827 0.145 Uiso 1 1 calc R U . . .
H32B H 0.2803 0.9022 0.5383 0.145 Uiso 1 1 calc R U . . .
H32C H 0.3004 0.8432 0.5250 0.145 Uiso 1 1 calc R U . . .
C33 C -0.1127(10) 0.7298(5) 0.6291(5) 0.051(3) Uani 1 1 d . . . . .
H33 H -0.1143 0.7581 0.6545 0.062 Uiso 1 1 calc R U . . .
C34 C -0.0893(12) 0.6791(5) 0.6589(5) 0.072(4) Uani 1 1 d . . . . .
H34A H -0.1015 0.6500 0.6353 0.108 Uiso 1 1 calc R U . . .
H34B H -0.1435 0.6763 0.6844 0.108 Uiso 1 1 calc R U . . .
H34C H -0.0081 0.6787 0.6760 0.108 Uiso 1 1 calc R U . . .
C35 C -0.2356(11) 0.7276(6) 0.5968(5) 0.075(4) Uani 1 1 d . . . . .
H35A H -0.2506 0.7599 0.5781 0.112 Uiso 1 1 calc R U . . .
H35B H -0.2959 0.7224 0.6192 0.112 Uiso 1 1 calc R U . . .
H35C H -0.2378 0.6991 0.5725 0.112 Uiso 1 1 calc R U . . .
C36 C -0.3155(11) 0.8645(6) 0.7943(6) 0.070(4) Uani 1 1 d . . . . .
H36A H -0.3148 0.8869 0.8241 0.105 Uiso 1 1 calc R U . . .
H36B H -0.3968 0.8593 0.7784 0.105 Uiso 1 1 calc R U . . .
H36C H -0.2701 0.8805 0.7697 0.105 Uiso 1 1 calc R U . . .
C37 C -0.2525(12) 0.7615(6) 0.7554(5) 0.075(4) Uani 1 1 d . . . . .
H37A H -0.2156 0.7805 0.7299 0.112 Uiso 1 1 calc R U . . .
H37B H -0.3342 0.7537 0.7420 0.112 Uiso 1 1 calc R U . . .
H37C H -0.2096 0.7293 0.7636 0.112 Uiso 1 1 calc R U . . .
C38 C -0.3511(12) 0.7692(7) 0.8552(7) 0.093(5) Uani 1 1 d . . . . .
H38A H -0.3079 0.7608 0.8886 0.139 Uiso 1 1 calc R U . . .
H38B H -0.3827 0.7377 0.8384 0.139 Uiso 1 1 calc R U . . .
H38C H -0.4160 0.7926 0.8596 0.139 Uiso 1 1 calc R U . . .
C39 C -0.0843(9) 0.7903(5) 0.8980(4) 0.049(3) Uani 1 1 d . . . . .
C40 C -0.0563(10) 0.7388(5) 0.9102(4) 0.050(3) Uani 1 1 d . . . . .
C41 C -0.0270(11) 0.7244(6) 0.9610(5) 0.064(4) Uani 1 1 d . . . . .
H41 H -0.0080 0.6896 0.9692 0.077 Uiso 1 1 calc R U . . .
C42 C -0.0252(12) 0.7603(7) 0.9998(5) 0.075(4) Uani 1 1 d . . . . .
H42 H -0.0034 0.7504 1.0343 0.090 Uiso 1 1 calc R U . . .
C43 C -0.0552(13) 0.8102(7) 0.9879(6) 0.074(4) Uani 1 1 d . . . . .
H43 H -0.0551 0.8344 1.0147 0.089 Uiso 1 1 calc R U . . .
C44 C -0.0856(11) 0.8268(5) 0.9380(5) 0.057(3) Uani 1 1 d . . . . .
C45 C -0.0613(11) 0.6971(5) 0.8698(5) 0.062(3) Uani 1 1 d . . . . .
H45 H -0.0861 0.7135 0.8359 0.075 Uiso 1 1 calc R U . . .
C46 C 0.0577(12) 0.6720(5) 0.8680(6) 0.074(4) Uani 1 1 d . . . . .
H46A H 0.1155 0.6983 0.8623 0.111 Uiso 1 1 calc R U . . .
H46B H 0.0514 0.6469 0.8402 0.111 Uiso 1 1 calc R U . . .
H46C H 0.0828 0.6545 0.9004 0.111 Uiso 1 1 calc R U . . .
C47 C -0.1500(14) 0.6544(6) 0.8770(8) 0.106(6) Uani 1 1 d . . . . .
H47A H -0.1276 0.6376 0.9100 0.160 Uiso 1 1 calc R U . . .
H47B H -0.1503 0.6290 0.8497 0.160 Uiso 1 1 calc R U . . .
H47C H -0.2287 0.6693 0.8760 0.160 Uiso 1 1 calc R U . . .
C48 C -0.1253(13) 0.8813(5) 0.9282(5) 0.071(4) Uani 1 1 d . . . . .
H48 H -0.1195 0.8892 0.8917 0.085 Uiso 1 1 calc R U . . .
C49 C -0.2542(15) 0.8879(6) 0.9364(7) 0.101(6) Uani 1 1 d . . . . .
H49A H -0.3029 0.8632 0.9152 0.152 Uiso 1 1 calc R U . . .
H49B H -0.2801 0.9229 0.9269 0.152 Uiso 1 1 calc R U . . .
H49C H -0.2620 0.8819 0.9723 0.152 Uiso 1 1 calc R U . . .
C50 C -0.0489(16) 0.9212(6) 0.9612(5) 0.097(6) Uani 1 1 d . . . . .
H50A H -0.0711 0.9216 0.9957 0.145 Uiso 1 1 calc R U . . .
H50B H -0.0614 0.9554 0.9459 0.145 Uiso 1 1 calc R U . . .
H50C H 0.0343 0.9119 0.9629 0.145 Uiso 1 1 calc R U . . .
C51 C 0.4198(11) 0.9594(6) 0.8326(5) 0.072(4) Uani 1 1 d . . . . .
H51A H 0.4454 0.9243 0.8247 0.086 Uiso 1 1 calc R U . . .
H51B H 0.3876 0.9584 0.8655 0.086 Uiso 1 1 calc R U . . .
C52 C 0.5194(14) 0.9955(9) 0.8354(8) 0.121(8) Uani 1 1 d . . . . .
H52A H 0.5289 1.0138 0.8684 0.145 Uiso 1 1 calc R U . . .
H52B H 0.5931 0.9766 0.8323 0.145 Uiso 1 1 calc R U . . .
C53 C 0.4946(14) 1.0321(7) 0.7935(8) 0.106(6) Uani 1 1 d . . . . .
H53A H 0.5630 1.0352 0.7745 0.127 Uiso 1 1 calc R U . . .
H53B H 0.4767 1.0664 0.8066 0.127 Uiso 1 1 calc R U . . .
C54 C 0.3895(11) 1.0112(5) 0.7593(5) 0.063(4) Uani 1 1 d . . . . .
H54A H 0.3370 1.0394 0.7453 0.076 Uiso 1 1 calc R U . . .
H54B H 0.4147 0.9915 0.7307 0.076 Uiso 1 1 calc R U . . .
C55 C 0.4003(11) 0.8301(6) 0.6759(5) 0.067(3) Uani 1 1 d . U . . .
H55A H 0.4301 0.8310 0.7127 0.081 Uiso 1 1 calc R U . . .
H55B H 0.4039 0.8651 0.6617 0.081 Uiso 1 1 calc R U . . .
C56 C 0.4690(13) 0.7937(6) 0.6488(6) 0.075(3) Uani 1 1 d . U . . .
H56A H 0.5546 0.7965 0.6600 0.090 Uiso 0.38(14) 1 calc R U P A 1
H56B H 0.4526 0.7974 0.6114 0.090 Uiso 0.38(14) 1 calc R U P A 1
H56C H 0.5432 0.7849 0.6707 0.090 Uiso 0.62(14) 1 calc R U P A 2
H56D H 0.4892 0.8099 0.6173 0.090 Uiso 0.62(14) 1 calc R U P A 2
C57A C 0.418(2) 0.7456(11) 0.6674(13) 0.072(3) Uani 0.55(2) 1 d . U P B 1
H57A H 0.4387 0.7154 0.6477 0.087 Uiso 0.55(2) 1 calc R U P B 1
H57B H 0.4450 0.7399 0.7040 0.087 Uiso 0.55(2) 1 calc R U P B 1
C57B C 0.396(3) 0.7442(13) 0.6354(15) 0.069(3) Uani 0.45(2) 1 d . U P B 2
H57C H 0.3787 0.7392 0.5981 0.083 Uiso 0.45(2) 1 calc R U P B 2
H57D H 0.4365 0.7134 0.6510 0.083 Uiso 0.45(2) 1 calc R U P B 2
C58 C 0.2894(11) 0.7562(5) 0.6581(6) 0.066(3) Uani 1 1 d . U . . .
H58A H 0.2567 0.7476 0.6227 0.079 Uiso 0.38(14) 1 calc R U P A 1
H58B H 0.2472 0.7362 0.6818 0.079 Uiso 0.38(14) 1 calc R U P A 1
H58C H 0.2195 0.7446 0.6350 0.079 Uiso 0.62(14) 1 calc R U P A 2
H58D H 0.2911 0.7374 0.6907 0.079 Uiso 0.62(14) 1 calc R U P A 2
C59 C 0.3105(10) 0.7610(5) 0.8622(5) 0.053(3) Uani 1 1 d . . . . .
H59A H 0.3680 0.7834 0.8482 0.064 Uiso 1 1 calc R U . . .
H59B H 0.2844 0.7341 0.8367 0.064 Uiso 1 1 calc R U . . .
C60 C 0.3650(12) 0.7370(5) 0.9110(5) 0.064(3) Uani 1 1 d . U . . .
H60A H 0.3217 0.7060 0.9195 0.077 Uiso 0.44(13) 1 calc R U P B 1
H60B H 0.4486 0.7283 0.9102 0.077 Uiso 0.44(13) 1 calc R U P B 1
H60C H 0.4488 0.7468 0.9188 0.077 Uiso 0.56(13) 1 calc R U P B 2
H60D H 0.3590 0.6991 0.9093 0.077 Uiso 0.56(13) 1 calc R U P B 2
C61A C 0.351(2) 0.7802(11) 0.9471(10) 0.064(4) Uani 0.55(2) 1 d . U P B 1
H61A H 0.4113 0.8071 0.9448 0.076 Uiso 0.55(2) 1 calc R U P B 1
H61B H 0.3575 0.7677 0.9826 0.076 Uiso 0.55(2) 1 calc R U P B 1
C61B C 0.292(3) 0.7590(13) 0.9521(12) 0.066(4) Uani 0.45(2) 1 d . U P B 2
H61C H 0.2390 0.7323 0.9629 0.080 Uiso 0.45(2) 1 calc R U P B 2
H61D H 0.3449 0.7710 0.9824 0.080 Uiso 0.45(2) 1 calc R U P B 2
C62 C 0.2263(11) 0.8004(6) 0.9284(5) 0.062(4) Uani 1 1 d . . . . .
H62A H 0.1668 0.7817 0.9450 0.074 Uiso 0.44(13) 1 calc R U P B 1
H62B H 0.2204 0.8375 0.9357 0.074 Uiso 0.44(13) 1 calc R U P B 1
H62C H 0.2690 0.8331 0.9360 0.074 Uiso 0.56(13) 1 calc R U P B 2
H62D H 0.1492 0.8028 0.9411 0.074 Uiso 0.56(13) 1 calc R U P B 2
Ho1 Ho 0.12792(4) 0.94720(2) 0.76734(2) 0.03612(13) Uani 1 1 d . . . . .
Ho2 Ho 0.09780(4) 0.84692(2) 0.69098(2) 0.03484(12) Uani 1 1 d . . . . .
Ho3 Ho 0.05658(4) 0.83485(2) 0.81480(2) 0.03627(13) Uani 1 1 d . . . . .
N1 N 0.0271(7) 1.0227(3) 0.7661(3) 0.040(2) Uani 1 1 d . . . . .
N2 N -0.0257(7) 0.8355(4) 0.6177(3) 0.043(2) Uani 1 1 d . . . . .
N3 N -0.1083(8) 0.8065(4) 0.8465(3) 0.048(2) Uani 1 1 d . . . . .
O1 O 0.3306(6) 0.9782(3) 0.7918(3) 0.0495(19) Uani 1 1 d . . . . .
O2 O 0.2801(6) 0.8100(3) 0.6673(3) 0.0463(19) Uani 1 1 d . . . . .
O3 O 0.2099(6) 0.7911(3) 0.8739(3) 0.0430(18) Uani 1 1 d . . . . .
Si1 Si -0.1184(3) 1.03277(14) 0.77178(14) 0.0556(9) Uani 1 1 d . . . . .
Si2 Si -0.1454(3) 0.87267(15) 0.59471(13) 0.0525(9) Uani 1 1 d . . . . .
Si3 Si -0.2487(3) 0.80130(15) 0.81466(15) 0.0590(9) Uani 1 1 d . . . . .
C100 C 1.012(3) 0.5106(12) 0.0276(7) 0.196(8) Uani 1 1 d D U . . .
H10A H 1.0981 0.5119 0.0387 0.235 Uiso 1 1 calc R U . . .
H10B H 0.9808 0.5459 0.0288 0.235 Uiso 1 1 calc R U . . .
C110 C 0.954(2) 0.4761(10) 0.0632(9) 0.197(8) Uani 1 1 d D U . . .
H11A H 0.9856 0.4407 0.0624 0.236 Uiso 1 1 calc R U . . .
H11B H 0.8683 0.4750 0.0528 0.236 Uiso 1 1 calc R U . . .
C120 C 0.982(2) 0.4989(11) 0.1167(7) 0.189(8) Uani 1 1 d D U . . .
H12A H 0.9462 0.4777 0.1410 0.283 Uiso 1 1 calc R U . . .
H12B H 0.9513 0.5339 0.1169 0.283 Uiso 1 1 calc R U . . .
H12C H 1.0678 0.4996 0.1265 0.283 Uiso 1 1 calc R U . . .
C200 C 0.4488(19) 0.9905(9) 0.0141(10) 0.158(7) Uani 1 1 d D U . . .
H20D H 0.4774 0.9910 0.0511 0.190 Uiso 1 1 calc R U . . .
H20E H 0.3848 1.0162 0.0081 0.190 Uiso 1 1 calc R U . . .
C210 C 0.394(2) 0.9377(9) 0.0016(9) 0.162(6) Uani 1 1 d D U . . .
H21D H 0.3654 0.9356 -0.0353 0.194 Uiso 1 1 calc R U . . .
H21E H 0.4544 0.9107 0.0100 0.194 Uiso 1 1 calc R U . . .
C220 C 0.2928(19) 0.9295(10) 0.0324(9) 0.165(7) Uani 1 1 d D U . . .
H22D H 0.2579 0.8957 0.0246 0.248 Uiso 1 1 calc R U . . .
H22E H 0.2332 0.9561 0.0236 0.248 Uiso 1 1 calc R U . . .
H22F H 0.3221 0.9315 0.0689 0.248 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Ho1 2.356(10) . ?
C1 Ho2 2.390(10) . ?
C1 Ho3 2.428(10) . ?
C2 Ho1 2.721(10) . ?
C2 Ho3 2.745(9) . ?
C2 Ho2 2.746(9) . ?
C3 Ho2 2.528(11) . ?
C3 Ho1 2.575(11) . ?
C4 Ho3 2.501(11) . ?
C4 Ho2 2.582(10) . ?
C5 Ho3 2.543(11) . ?
C6 Si1 1.870(14) . ?
C7 Si1 1.884(14) . ?
C8 Si1 1.882(14) . ?
C9 C10 1.411(15) . ?
C9 N1 1.413(14) . ?
C9 C14 1.439(16) . ?
C10 C11 1.400(18) . ?
C10 C15 1.519(17) . ?
C11 C12 1.39(2) . ?
C12 C13 1.366(19) . ?
C13 C14 1.392(17) . ?
C14 C18 1.504(17) . ?
C15 C16 1.507(19) . ?
C15 C17 1.55(2) . ?
C18 C20 1.538(16) . ?
C18 C19 1.546(16) . ?
C21 Si2 1.887(13) . ?
C22 Si2 1.865(14) . ?
C23 Si2 1.861(14) . ?
C24 C29 1.419(16) . ?
C24 N2 1.428(14) . ?
C24 C25 1.434(16) . ?
C25 C26 1.402(19) . ?
C25 C30 1.496(19) . ?
C26 C27 1.36(2) . ?
C27 C28 1.378(19) . ?
C28 C29 1.392(17) . ?
C29 C33 1.526(17) . ?
C30 C32 1.519(18) . ?
C30 C31 1.521(19) . ?
C33 C34 1.544(17) . ?
C33 C35 1.551(16) . ?
C36 Si3 1.866(14) . ?
C37 Si3 1.876(15) . ?
C38 Si3 1.890(13) . ?
C39 C40 1.409(17) . ?
C39 N3 1.419(14) . ?
C39 C44 1.423(17) . ?
C40 C41 1.395(17) . ?
C40 C45 1.520(17) . ?
C41 C42 1.387(19) . ?
C42 C43 1.37(2) . ?
C43 C44 1.389(19) . ?
C44 C48 1.504(19) . ?
C45 C46 1.521(18) . ?
C45 C47 1.538(18) . ?
C48 C49 1.534(19) . ?
C48 C50 1.55(2) . ?
C51 O1 1.471(14) . ?
C51 C52 1.475(19) . ?
C52 C53 1.46(2) . ?
C53 C54 1.510(19) . ?
C54 O1 1.446(14) . ?
C55 O2 1.465(14) . ?
C55 C56 1.477(18) . ?
C56 C57A 1.49(3) . ?
C56 C57B 1.55(3) . ?
C57A C58 1.49(3) . ?
C57B C58 1.47(3) . ?
C58 O2 1.427(15) . ?
C59 O3 1.463(13) . ?
C59 C60 1.496(16) . ?
C60 C61A 1.50(3) . ?
C60 C61B 1.57(3) . ?
C61A C62 1.55(3) . ?
C61B C62 1.41(3) . ?
C62 O3 1.449(13) . ?
Ho1 N1 2.278(9) . ?
Ho1 O1 2.466(7) . ?
Ho1 Ho2 3.2932(7) . ?
Ho1 Ho3 3.3294(7) . ?
Ho2 N2 2.266(8) . ?
Ho2 O2 2.459(7) . ?
Ho2 Ho3 3.3900(7) . ?
Ho3 N3 2.292(9) . ?
Ho3 O3 2.473(7) . ?
N1 Si1 1.717(9) . ?
N2 Si2 1.725(9) . ?
N3 Si3 1.722(10) . ?
C100 C110 1.517(10) . ?
C100 C100 1.56(4) 3_765 ?
C110 C120 1.531(10) . ?
C200 C210 1.528(10) . ?
C200 C200 1.56(4) 3_675 ?
C210 C220 1.525(10) . ?

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
Ho1 C1 Ho2 87.9(3) . . ?
Ho1 C1 Ho3 88.2(3) . . ?
Ho2 C1 Ho3 89.4(3) . . ?
Ho1 C2 Ho3 75.1(2) . . ?
Ho1 C2 Ho2 74.1(2) . . ?
Ho3 C2 Ho2 76.2(2) . . ?
Ho2 C3 Ho1 80.4(3) . . ?
Ho3 C4 Ho2 83.6(3) . . ?
C10 C9 N1 120.9(10) . . ?
C10 C9 C14 118.3(11) . . ?
N1 C9 C14 120.8(10) . . ?
C11 C10 C9 119.9(12) . . ?
C11 C10 C15 118.3(12) . . ?
C9 C10 C15 121.8(11) . . ?
C12 C11 C10 121.3(13) . . ?
C13 C12 C11 118.9(13) . . ?
C12 C13 C14 122.7(13) . . ?
C13 C14 C9 118.8(12) . . ?
C13 C14 C18 120.1(11) . . ?
C9 C14 C18 121.0(11) . . ?
C16 C15 C10 115.3(13) . . ?
C16 C15 C17 107.8(12) . . ?
C10 C15 C17 112.3(12) . . ?
C14 C18 C20 110.6(11) . . ?
C14 C18 C19 113.6(11) . . ?
C20 C18 C19 108.8(10) . . ?
C29 C24 N2 120.7(10) . . ?
C29 C24 C25 118.2(11) . . ?
N2 C24 C25 121.2(11) . . ?
C26 C25 C24 118.6(13) . . ?
C26 C25 C30 119.1(12) . . ?
C24 C25 C30 122.4(11) . . ?
C27 C26 C25 122.0(14) . . ?
C26 C27 C28 120.1(14) . . ?
C27 C28 C29 120.9(14) . . ?
C28 C29 C24 120.2(12) . . ?
C28 C29 C33 118.0(12) . . ?
C24 C29 C33 121.8(10) . . ?
C25 C30 C32 114.7(12) . . ?
C25 C30 C31 113.1(12) . . ?
C32 C30 C31 107.5(12) . . ?
C29 C33 C34 114.3(11) . . ?
C29 C33 C35 109.8(10) . . ?
C34 C33 C35 109.5(11) . . ?
C40 C39 N3 120.8(11) . . ?
C40 C39 C44 119.4(11) . . ?
N3 C39 C44 119.8(11) . . ?
C41 C40 C39 119.6(12) . . ?
C41 C40 C45 118.1(12) . . ?
C39 C40 C45 122.3(11) . . ?
C42 C41 C40 120.9(14) . . ?
C43 C42 C41 119.3(14) . . ?
C42 C43 C44 122.5(14) . . ?
C43 C44 C39 118.3(13) . . ?
C43 C44 C48 119.2(12) . . ?
C39 C44 C48 122.3(12) . . ?
C40 C45 C46 112.3(11) . . ?
C40 C45 C47 113.1(12) . . ?
C46 C45 C47 107.7(12) . . ?
C44 C48 C49 110.9(12) . . ?
C44 C48 C50 113.6(13) . . ?
C49 C48 C50 109.3(13) . . ?
O1 C51 C52 106.5(13) . . ?
C53 C52 C51 107.8(13) . . ?
C52 C53 C54 106.2(14) . . ?
O1 C54 C53 104.9(12) . . ?
O2 C55 C56 104.4(11) . . ?
C55 C56 C57A 96.9(16) . . ?
C55 C56 C57B 109.7(16) . . ?
C58 C57A C56 102.4(19) . . ?
C58 C57B C56 101(2) . . ?
O2 C58 C57B 111.3(16) . . ?
O2 C58 C57A 104.4(14) . . ?
O3 C59 C60 106.9(10) . . ?
C61A C60 C59 99.9(14) . . ?
C59 C60 C61B 104.4(14) . . ?
C60 C61A C62 102.8(17) . . ?
C62 C61B C60 106(2) . . ?
C61B C62 O3 107.8(16) . . ?
O3 C62 C61A 104.7(13) . . ?
N1 Ho1 C1 101.1(3) . . ?
N1 Ho1 O1 100.4(3) . . ?
C1 Ho1 O1 158.4(3) . . ?
N1 Ho1 C3 106.8(3) . . ?
C1 Ho1 C3 86.9(3) . . ?
O1 Ho1 C3 86.7(3) . . ?
N1 Ho1 C2 175.1(3) . . ?
C1 Ho1 C2 82.6(3) . . ?
O1 Ho1 C2 75.9(3) . . ?
C3 Ho1 C2 76.5(3) . . ?
N1 Ho1 Ho2 131.6(2) . . ?
C1 Ho1 Ho2 46.5(3) . . ?
O1 Ho1 Ho2 116.06(18) . . ?
C3 Ho1 Ho2 49.2(2) . . ?
C2 Ho1 Ho2 53.32(19) . . ?
N1 Ho1 Ho3 127.8(2) . . ?
C1 Ho1 Ho3 46.8(2) . . ?
O1 Ho1 Ho3 117.34(18) . . ?
C3 Ho1 Ho3 109.9(3) . . ?
C2 Ho1 Ho3 52.8(2) . . ?
Ho2 Ho1 Ho3 61.575(15) . . ?
N2 Ho2 C1 102.1(3) . . ?
N2 Ho2 O2 100.8(3) . . ?
C1 Ho2 O2 157.1(3) . . ?
N2 Ho2 C3 102.0(3) . . ?
C1 Ho2 C3 87.2(4) . . ?
O2 Ho2 C3 87.2(3) . . ?
N2 Ho2 C4 106.5(3) . . ?
C1 Ho2 C4 83.6(3) . . ?
O2 Ho2 C4 90.7(3) . . ?
C3 Ho2 C4 151.3(3) . . ?
N2 Ho2 C2 176.2(3) . . ?
C1 Ho2 C2 81.4(3) . . ?
O2 Ho2 C2 75.7(3) . . ?
C3 Ho2 C2 76.8(3) . . ?
C4 Ho2 C2 75.0(3) . . ?
N2 Ho2 Ho1 129.3(2) . . ?
C1 Ho2 Ho1 45.6(2) . . ?
O2 Ho2 Ho1 116.33(17) . . ?
C3 Ho2 Ho1 50.4(2) . . ?
C4 Ho2 Ho1 106.4(2) . . ?
C2 Ho2 Ho1 52.6(2) . . ?
N2 Ho2 Ho3 131.7(2) . . ?
C1 Ho2 Ho3 45.7(2) . . ?
O2 Ho2 Ho3 116.33(18) . . ?
C3 Ho2 Ho3 109.3(2) . . ?
C4 Ho2 Ho3 47.2(2) . . ?
C2 Ho2 Ho3 51.9(2) . . ?
Ho1 Ho2 Ho3 59.739(15) . . ?
N3 Ho3 C1 102.2(3) . . ?
N3 Ho3 O3 99.9(3) . . ?
C1 Ho3 O3 157.9(3) . . ?
N3 Ho3 C4 99.9(3) . . ?
C1 Ho3 C4 84.6(4) . . ?
O3 Ho3 C4 91.4(3) . . ?
N3 Ho3 C5 108.3(4) . . ?
C1 Ho3 C5 85.6(4) . . ?
O3 Ho3 C5 87.8(3) . . ?
C4 Ho3 C5 151.5(4) . . ?
N3 Ho3 C2 175.0(3) . . ?
C1 Ho3 C2 80.8(3) . . ?
O3 Ho3 C2 77.2(2) . . ?
C4 Ho3 C2 76.3(3) . . ?
C5 Ho3 C2 75.8(3) . . ?
N3 Ho3 Ho1 132.7(2) . . ?
C1 Ho3 Ho1 45.0(2) . . ?
O3 Ho3 Ho1 117.02(17) . . ?
C4 Ho3 Ho1 107.3(2) . . ?
C5 Ho3 Ho1 49.3(2) . . ?
C2 Ho3 Ho1 52.1(2) . . ?
N3 Ho3 Ho2 127.8(2) . . ?
C1 Ho3 Ho2 44.8(2) . . ?
O3 Ho3 Ho2 118.46(16) . . ?
C4 Ho3 Ho2 49.2(2) . . ?
C5 Ho3 Ho2 107.2(2) . . ?
C2 Ho3 Ho2 51.90(19) . . ?
Ho1 Ho3 Ho2 58.686(14) . . ?
C9 N1 Si1 121.2(7) . . ?
C9 N1 Ho1 109.7(6) . . ?
Si1 N1 Ho1 129.0(5) . . ?
C24 N2 Si2 121.8(7) . . ?
C24 N2 Ho2 110.6(6) . . ?
Si2 N2 Ho2 127.4(5) . . ?
C39 N3 Si3 119.8(7) . . ?
C39 N3 Ho3 112.6(7) . . ?
Si3 N3 Ho3 127.6(5) . . ?
C54 O1 C51 107.5(9) . . ?
C54 O1 Ho1 122.5(7) . . ?
C51 O1 Ho1 128.6(7) . . ?
C58 O2 C55 106.6(9) . . ?
C58 O2 Ho2 120.8(7) . . ?
C55 O2 Ho2 129.5(7) . . ?
C62 O3 C59 107.4(8) . . ?
C62 O3 Ho3 122.7(7) . . ?
C59 O3 Ho3 128.9(6) . . ?
N1 Si1 C6 110.5(5) . . ?
N1 Si1 C8 113.0(5) . . ?
C6 Si1 C8 106.6(7) . . ?
N1 Si1 C7 113.0(6) . . ?
C6 Si1 C7 107.2(7) . . ?
C8 Si1 C7 106.2(7) . . ?
N2 Si2 C23 111.5(5) . . ?
N2 Si2 C22 111.7(6) . . ?
C23 Si2 C22 106.3(7) . . ?
N2 Si2 C21 113.0(6) . . ?
C23 Si2 C21 107.4(7) . . ?
C22 Si2 C21 106.6(7) . . ?
N3 Si3 C36 113.2(6) . . ?
N3 Si3 C37 111.7(6) . . ?
C36 Si3 C37 106.5(7) . . ?
N3 Si3 C38 111.6(6) . . ?
C36 Si3 C38 106.9(7) . . ?
C37 Si3 C38 106.5(8) . . ?
C110 C100 C100 110(3) . 3_765 ?
C100 C110 C120 106.8(9) . . ?
C210 C200 C200 120(2) . 3_675 ?
C220 C210 C200 109.2(16) . . ?

_refine_diff_density_max         1.014
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.124

_shelxl_version_number           2013-3


_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_dr143-abscorr
_database_code_depnum_ccdc_archive 'CCDC 1410391'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65 H123 N3 Nd3 O3 Si3'
_chemical_formula_weight         1511.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.7297(6)
_cell_length_b                   25.9702(18)
_cell_length_c                   26.3476(14)
_cell_angle_alpha                90
_cell_angle_beta                 97.592(4)
_cell_angle_gamma                90
_cell_volume                     7955.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    26272
_cell_measurement_theta_min      1.68
_cell_measurement_theta_max      29.24

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_F_000             3120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.012
_shelx_estimated_absorpt_T_min   0.633
_shelx_estimated_absorpt_T_max   0.752
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6330
_exptl_absorpt_correction_T_max  0.7521
_exptl_absorpt_process_details   mulabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe-IPDS II'
_diffrn_measurement_method       Phi
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            93024
_diffrn_reflns_av_unetI/netI     0.0991
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.934
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             16213
_reflns_number_gt                10222
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-AREA
_computing_cell_refinement       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 ?
;

_vrf_RINTA01_dr143-abscorr       
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: The data show rare quality, especially for high theta 
           values.
;
_vrf_PLAT202_dr143-abscorr       
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........    6       
RESPONSE:  n-hexane solvent molecules could not be refined
          anisotropic. The refinement has been done with multiplicity
		  10.500. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0566P)²+0.7204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00016(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         16213
_refine_ls_number_parameters     705
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1358
_refine_ls_wR_factor_gt          0.1196
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 0.2614(7) 0.6428(3) 0.2780(3) 0.047(2) Uani 1 1 d . . . . .
H2A H 0.3331 0.6424 0.3025 0.056 Uiso 1 1 calc R U . . .
H2B H 0.2712 0.6600 0.2453 0.056 Uiso 1 1 calc R U . . .
C1 C -0.0161(6) 0.6119(3) 0.2458(3) 0.0395(18) Uani 1 1 d . . . . .
H1A H 0.0022 0.6441 0.2644 0.059 Uiso 1 1 calc R U . . .
H1B H -0.0886 0.5981 0.2547 0.059 Uiso 1 1 calc R U . . .
H1C H -0.0237 0.6184 0.2089 0.059 Uiso 1 1 calc R U . . .
C3 C 0.1354(8) 0.5805(3) 0.3641(3) 0.056(2) Uani 1 1 d . . . . .
H3A H 0.1398 0.6182 0.3657 0.084 Uiso 1 1 calc R U . . .
H3B H 0.2017 0.5657 0.3858 0.084 Uiso 1 1 calc R U . . .
H3C H 0.0642 0.5690 0.3763 0.084 Uiso 1 1 calc R U . . .
C4 C 0.0752(7) 0.7362(3) 0.2487(3) 0.046(2) Uani 1 1 d . . . . .
H4A H 0.0067 0.7582 0.2452 0.070 Uiso 1 1 calc R U . . .
H4B H 0.0807 0.7187 0.2162 0.070 Uiso 1 1 calc R U . . .
H4C H 0.1439 0.7574 0.2580 0.070 Uiso 1 1 calc R U . . .
C5 C 0.1919(7) 0.5662(3) 0.1755(3) 0.051(2) Uani 1 1 d . . . . .
H5A H 0.2685 0.5641 0.1954 0.077 Uiso 1 1 calc R U . . .
H5B H 0.1982 0.5608 0.1391 0.077 Uiso 1 1 calc R U . . .
H5C H 0.1422 0.5395 0.1872 0.077 Uiso 1 1 calc R U . . .
C6 C -0.1519(10) 0.3945(4) 0.2782(4) 0.087(4) Uani 1 1 d . . . . .
H6A H -0.0902 0.3738 0.2668 0.131 Uiso 1 1 calc R U . . .
H6B H -0.2244 0.3872 0.2564 0.131 Uiso 1 1 calc R U . . .
H6C H -0.1597 0.3860 0.3138 0.131 Uiso 1 1 calc R U . . .
C7 C -0.1479(9) 0.4971(5) 0.3337(4) 0.084(3) Uani 1 1 d . . . . .
H7A H -0.0958 0.4837 0.3629 0.126 Uiso 1 1 calc R U . . .
H7B H -0.2277 0.4901 0.3389 0.126 Uiso 1 1 calc R U . . .
H7C H -0.1367 0.5343 0.3310 0.126 Uiso 1 1 calc R U . . .
C8 C -0.2175(8) 0.4934(4) 0.2192(4) 0.081(3) Uani 1 1 d . . . . .
H8A H -0.2009 0.5301 0.2161 0.121 Uiso 1 1 calc R U . . .
H8B H -0.2970 0.4890 0.2262 0.121 Uiso 1 1 calc R U . . .
H8C H -0.2074 0.4758 0.1872 0.121 Uiso 1 1 calc R U . . .
C9 C 0.1051(7) 0.4359(3) 0.2623(3) 0.0437(19) Uani 1 1 d . . . . .
C10 C 0.1284(7) 0.4168(3) 0.2134(3) 0.048(2) Uani 1 1 d . . . . .
C11 C 0.2145(9) 0.3810(4) 0.2122(4) 0.070(3) Uani 1 1 d . . . . .
H11 H 0.2307 0.3692 0.1798 0.084 Uiso 1 1 calc R U . . .
C12 C 0.2767(11) 0.3619(4) 0.2545(4) 0.080(3) Uani 1 1 d . . . . .
H12 H 0.3338 0.3365 0.2516 0.097 Uiso 1 1 calc R U . . .
C13 C 0.2573(9) 0.3794(4) 0.3021(4) 0.069(3) Uani 1 1 d . . . . .
H13 H 0.3024 0.3663 0.3319 0.083 Uiso 1 1 calc R U . . .
C14 C 0.1723(8) 0.4161(3) 0.3072(3) 0.055(2) Uani 1 1 d . . . . .
C15 C 0.0560(8) 0.4348(3) 0.1652(3) 0.057(2) Uani 1 1 d . . . . .
H15 H 0.0263 0.4699 0.1718 0.068 Uiso 1 1 calc R U . . .
C16 C 0.1239(9) 0.4387(4) 0.1192(3) 0.071(3) Uani 1 1 d . . . . .
H16A H 0.1950 0.4581 0.1292 0.106 Uiso 1 1 calc R U . . .
H16B H 0.0772 0.4565 0.0910 0.106 Uiso 1 1 calc R U . . .
H16C H 0.1429 0.4041 0.1082 0.106 Uiso 1 1 calc R U . . .
C17 C -0.0480(10) 0.3991(5) 0.1519(4) 0.088(4) Uani 1 1 d . . . . .
H17A H -0.0212 0.3638 0.1474 0.132 Uiso 1 1 calc R U . . .
H17B H -0.0933 0.4108 0.1200 0.132 Uiso 1 1 calc R U . . .
H17C H -0.0959 0.3999 0.1796 0.132 Uiso 1 1 calc R U . . .
C18 C 0.1501(9) 0.4327(4) 0.3607(3) 0.065(3) Uani 1 1 d . . . . .
H18 H 0.1018 0.4646 0.3568 0.078 Uiso 1 1 calc R U . . .
C19 C 0.2601(11) 0.4456(4) 0.3960(4) 0.092(4) Uani 1 1 d . . . . .
H19A H 0.2404 0.4605 0.4279 0.138 Uiso 1 1 calc R U . . .
H19B H 0.3053 0.4705 0.3790 0.138 Uiso 1 1 calc R U . . .
H19C H 0.3052 0.4142 0.4037 0.138 Uiso 1 1 calc R U . . .
C20 C 0.0837(13) 0.3923(5) 0.3856(4) 0.108(5) Uani 1 1 d . . . . .
H20A H 0.1313 0.3614 0.3922 0.162 Uiso 1 1 calc R U . . .
H20B H 0.0135 0.3837 0.3628 0.162 Uiso 1 1 calc R U . . .
H20C H 0.0634 0.4056 0.4181 0.162 Uiso 1 1 calc R U . . .
C21 C -0.2470(9) 0.7406(4) 0.2562(4) 0.082(3) Uani 1 1 d . . . . .
H21A H -0.2107 0.7740 0.2649 0.123 Uiso 1 1 calc R U . . .
H21B H -0.3263 0.7460 0.2401 0.123 Uiso 1 1 calc R U . . .
H21C H -0.2038 0.7224 0.2323 0.123 Uiso 1 1 calc R U . . .
C22 C -0.3099(9) 0.6382(4) 0.2945(4) 0.079(3) Uani 1 1 d . . . . .
H22A H -0.2659 0.6233 0.2690 0.119 Uiso 1 1 calc R U . . .
H22B H -0.3901 0.6429 0.2793 0.119 Uiso 1 1 calc R U . . .
H22C H -0.3068 0.6151 0.3240 0.119 Uiso 1 1 calc R U . . .
C23 C -0.3482(10) 0.7329(5) 0.3559(5) 0.104(4) Uani 1 1 d . . . . .
H23A H -0.4153 0.7107 0.3572 0.156 Uiso 1 1 calc R U . . .
H23B H -0.3733 0.7662 0.3410 0.156 Uiso 1 1 calc R U . . .
H23C H -0.3086 0.7382 0.3907 0.156 Uiso 1 1 calc R U . . .
C24 C -0.0821(8) 0.7113(4) 0.3989(3) 0.055(2) Uani 1 1 d . . . . .
C25 C -0.0766(9) 0.6744(4) 0.4401(3) 0.065(3) Uani 1 1 d . . . . .
C26 C -0.0419(10) 0.6905(5) 0.4900(4) 0.083(3) Uani 1 1 d . . . . .
H26 H -0.0375 0.6659 0.5169 0.099 Uiso 1 1 calc R U . . .
C27 C -0.0137(10) 0.7406(5) 0.5018(4) 0.082(3) Uani 1 1 d . . . . .
H27 H 0.0106 0.7504 0.5362 0.098 Uiso 1 1 calc R U . . .
C28 C -0.0209(9) 0.7766(4) 0.4631(4) 0.071(3) Uani 1 1 d . . . . .
H28 H -0.0029 0.8116 0.4713 0.085 Uiso 1 1 calc R U . . .
C29 C -0.0539(8) 0.7627(4) 0.4124(3) 0.055(2) Uani 1 1 d . . . . .
C30 C -0.1159(12) 0.6192(4) 0.4298(4) 0.097(2) Uani 1 1 d . . . . .
H30 H -0.1071 0.6113 0.3934 0.116 Uiso 1 1 calc R U . . .
C31 C -0.0462(12) 0.5784(4) 0.4634(4) 0.097(2) Uani 1 1 d . . . . .
H31A H -0.0614 0.5443 0.4482 0.145 Uiso 1 1 calc R U . . .
H31B H -0.0689 0.5790 0.4978 0.145 Uiso 1 1 calc R U . . .
H31C H 0.0360 0.5862 0.4654 0.145 Uiso 1 1 calc R U . . .
C32 C -0.2430(11) 0.6131(4) 0.4353(4) 0.097(2) Uani 1 1 d . . . . .
H32A H -0.2546 0.6199 0.4708 0.145 Uiso 1 1 calc R U . . .
H32B H -0.2678 0.5780 0.4260 0.145 Uiso 1 1 calc R U . . .
H32C H -0.2883 0.6376 0.4126 0.145 Uiso 1 1 calc R U . . .
C33 C -0.0603(8) 0.8049(4) 0.3717(4) 0.065(3) Uani 1 1 d . . . . .
H33 H -0.0864 0.7888 0.3376 0.078 Uiso 1 1 calc R U . . .
C34 C 0.0561(9) 0.8302(4) 0.3692(4) 0.071(3) Uani 1 1 d . . . . .
H34A H 0.0784 0.8502 0.4005 0.106 Uiso 1 1 calc R U . . .
H34B H 0.0509 0.8531 0.3394 0.106 Uiso 1 1 calc R U . . .
H34C H 0.1140 0.8036 0.3662 0.106 Uiso 1 1 calc R U . . .
C35 C -0.1467(11) 0.8470(5) 0.3810(5) 0.106(4) Uani 1 1 d . . . . .
H35A H -0.1275 0.8607 0.4158 0.159 Uiso 1 1 calc R U . . .
H35B H -0.2244 0.8324 0.3771 0.159 Uiso 1 1 calc R U . . .
H35C H -0.1434 0.8748 0.3561 0.159 Uiso 1 1 calc R U . . .
C36 C -0.2614(8) 0.6342(4) 0.1344(4) 0.080(3) Uani 1 1 d . . . . .
H36A H -0.2326 0.6215 0.1687 0.120 Uiso 1 1 calc R U . . .
H36B H -0.3280 0.6137 0.1200 0.120 Uiso 1 1 calc R U . . .
H36C H -0.2841 0.6704 0.1364 0.120 Uiso 1 1 calc R U . . .
C37 C -0.1055(9) 0.5590(4) 0.0932(4) 0.081(3) Uani 1 1 d . . . . .
H37A H -0.0496 0.5531 0.0692 0.121 Uiso 1 1 calc R U . . .
H37B H -0.1744 0.5382 0.0829 0.121 Uiso 1 1 calc R U . . .
H37C H -0.0715 0.5493 0.1278 0.121 Uiso 1 1 calc R U . . .
C38 C -0.2108(10) 0.6448(4) 0.0253(4) 0.092(4) Uani 1 1 d . . . . .
H38A H -0.1579 0.6670 0.0094 0.138 Uiso 1 1 calc R U . . .
H38B H -0.2838 0.6630 0.0263 0.138 Uiso 1 1 calc R U . . .
H38C H -0.2247 0.6131 0.0053 0.138 Uiso 1 1 calc R U . . .
C39 C 0.0134(7) 0.7072(3) 0.0874(3) 0.047(2) Uani 1 1 d . . . . .
C40 C -0.0172(7) 0.7587(3) 0.0959(3) 0.052(2) Uani 1 1 d . . . . .
C41 C 0.0364(9) 0.7990(4) 0.0724(4) 0.070(3) Uani 1 1 d . . . . .
H41 H 0.0171 0.8337 0.0790 0.084 Uiso 1 1 calc R U . . .
C42 C 0.1162(10) 0.7889(5) 0.0401(4) 0.081(3) Uani 1 1 d . . . . .
H42 H 0.1517 0.8166 0.0246 0.098 Uiso 1 1 calc R U . . .
C43 C 0.1453(9) 0.7389(5) 0.0298(4) 0.072(3) Uani 1 1 d . . . . .
H43 H 0.1993 0.7324 0.0067 0.086 Uiso 1 1 calc R U . . .
C44 C 0.0965(7) 0.6982(4) 0.0530(3) 0.054(2) Uani 1 1 d . . . . .
C45 C -0.1104(7) 0.7722(4) 0.1285(3) 0.055(2) Uani 1 1 d . . . . .
H45 H -0.1126 0.7440 0.1542 0.066 Uiso 1 1 calc R U . . .
C46 C -0.0906(9) 0.8233(4) 0.1583(4) 0.069(3) Uani 1 1 d . . . . .
H46A H -0.0112 0.8246 0.1754 0.104 Uiso 1 1 calc R U . . .
H46B H -0.1438 0.8255 0.1840 0.104 Uiso 1 1 calc R U . . .
H46C H -0.1042 0.8523 0.1345 0.104 Uiso 1 1 calc R U . . .
C47 C -0.2269(8) 0.7734(4) 0.0956(4) 0.076(3) Uani 1 1 d . . . . .
H47A H -0.2282 0.8014 0.0706 0.114 Uiso 1 1 calc R U . . .
H47B H -0.2872 0.7793 0.1175 0.114 Uiso 1 1 calc R U . . .
H47C H -0.2406 0.7405 0.0777 0.114 Uiso 1 1 calc R U . . .
C48 C 0.1330(9) 0.6441(4) 0.0394(3) 0.067(3) Uani 1 1 d . . . . .
H48 H 0.0980 0.6199 0.0624 0.081 Uiso 1 1 calc R U . . .
C49 C 0.2609(9) 0.6346(5) 0.0478(4) 0.088(3) Uani 1 1 d . . . . .
H49A H 0.2984 0.6564 0.0245 0.132 Uiso 1 1 calc R U . . .
H49B H 0.2762 0.5983 0.0410 0.132 Uiso 1 1 calc R U . . .
H49C H 0.2913 0.6429 0.0833 0.132 Uiso 1 1 calc R U . . .
C50 C 0.0864(13) 0.6298(6) -0.0139(5) 0.127(5) Uani 1 1 d . . . . .
H50A H 0.0023 0.6318 -0.0181 0.191 Uiso 1 1 calc R U . . .
H50B H 0.1101 0.5946 -0.0209 0.191 Uiso 1 1 calc R U . . .
H50C H 0.1162 0.6536 -0.0379 0.191 Uiso 1 1 calc R U . . .
C51 C 0.4033(9) 0.4896(4) 0.2603(4) 0.078(3) Uani 1 1 d . . . . .
H51A H 0.4317 0.5088 0.2320 0.093 Uiso 1 1 calc R U . . .
H51B H 0.3500 0.4623 0.2456 0.093 Uiso 1 1 calc R U . . .
C52 C 0.5043(10) 0.4666(5) 0.2969(6) 0.107(4) Uani 1 1 d . . . . .
H52A H 0.4796 0.4355 0.3143 0.128 Uiso 1 1 calc R U . . .
H52B H 0.5691 0.4573 0.2781 0.128 Uiso 1 1 calc R U . . .
C53 C 0.5373(12) 0.5079(6) 0.3337(6) 0.127(5) Uani 1 1 d . . . . .
H53A H 0.6059 0.5262 0.3248 0.152 Uiso 1 1 calc R U . . .
H53B H 0.5559 0.4935 0.3687 0.152 Uiso 1 1 calc R U . . .
C54 C 0.4370(8) 0.5442(4) 0.3317(4) 0.080(3) Uani 1 1 d . . . . .
H54A H 0.4083 0.5458 0.3654 0.096 Uiso 1 1 calc R U . . .
H54B H 0.4597 0.5793 0.3222 0.096 Uiso 1 1 calc R U . . .
C55 C 0.3184(8) 0.7437(4) 0.3642(4) 0.066(3) Uani 1 1 d . . . . .
H55A H 0.2907 0.7709 0.3393 0.080 Uiso 1 1 calc R U . . .
H55B H 0.3723 0.7211 0.3486 0.080 Uiso 1 1 calc R U . . .
C56 C 0.3760(10) 0.7667(5) 0.4119(4) 0.083(3) Uani 1 1 d . . . . .
H56A H 0.3417 0.8004 0.4187 0.099 Uiso 1 1 calc R U . . .
H56B H 0.4594 0.7712 0.4106 0.099 Uiso 1 1 calc R U . . .
C57 C 0.3544(13) 0.7278(6) 0.4510(4) 0.126(5) Uani 1 1 d . . . . .
H57A H 0.3561 0.7442 0.4850 0.152 Uiso 1 1 calc R U . . .
H57B H 0.4133 0.7003 0.4534 0.152 Uiso 1 1 calc R U . . .
C58 C 0.2379(9) 0.7062(4) 0.4333(3) 0.076(3) Uani 1 1 d . . . . .
H58A H 0.2345 0.6692 0.4419 0.091 Uiso 1 1 calc R U . . .
H58B H 0.1780 0.7248 0.4493 0.091 Uiso 1 1 calc R U . . .
C59 C 0.3049(9) 0.7483(4) 0.1602(4) 0.074(2) Uani 1 1 d . . . . .
H59A H 0.3004 0.7675 0.1924 0.089 Uiso 0.720(11) 1 calc R U P A 1
H59B H 0.2420 0.7603 0.1341 0.089 Uiso 0.720(11) 1 calc R U P A 1
H59C H 0.2521 0.7682 0.1791 0.089 Uiso 0.280(11) 1 calc R U P A 2
H59D H 0.2894 0.7569 0.1233 0.089 Uiso 0.280(11) 1 calc R U P A 2
C60 C 0.4170(12) 0.7570(6) 0.1424(7) 0.074(2) Uani 0.720(11) 1 d . . P A 1
H60A H 0.4614 0.7835 0.1636 0.089 Uiso 0.720(11) 1 calc R U P A 1
H60B H 0.4066 0.7685 0.1063 0.089 Uiso 0.720(11) 1 calc R U P A 1
C61 C 0.4775(12) 0.7068(5) 0.1475(6) 0.074(2) Uani 0.720(11) 1 d . . P A 1
H61A H 0.4817 0.6917 0.1133 0.089 Uiso 0.720(11) 1 calc R U P A 1
H61B H 0.5567 0.7113 0.1652 0.089 Uiso 0.720(11) 1 calc R U P A 1
C60A C 0.428(3) 0.7579(15) 0.1810(18) 0.074(2) Uani 0.280(11) 1 d . . P A 2
H60C H 0.4688 0.7736 0.1544 0.089 Uiso 0.280(11) 1 calc R U P A 2
H60D H 0.4324 0.7819 0.2105 0.089 Uiso 0.280(11) 1 calc R U P A 2
C61A C 0.475(3) 0.7133(15) 0.1956(16) 0.074(2) Uani 0.280(11) 1 d . . P A 2
H61C H 0.4855 0.7116 0.2335 0.089 Uiso 0.280(11) 1 calc R U P A 2
H61D H 0.5513 0.7109 0.1841 0.089 Uiso 0.280(11) 1 calc R U P A 2
C62 C 0.4114(8) 0.6737(4) 0.1772(4) 0.071(3) Uani 1 1 d . . . . .
H62A H 0.4424 0.6749 0.2140 0.086 Uiso 0.720(11) 1 calc R U P A 1
H62B H 0.4128 0.6376 0.1652 0.086 Uiso 0.720(11) 1 calc R U P A 1
H62C H 0.4168 0.6450 0.2022 0.086 Uiso 0.280(11) 1 calc R U P A 2
H62D H 0.4358 0.6612 0.1449 0.086 Uiso 0.280(11) 1 calc R U P A 2
N1 N 0.0235(6) 0.4749(2) 0.2656(2) 0.0426(15) Uani 1 1 d . . . . .
N2 N -0.1121(6) 0.6953(3) 0.3478(2) 0.0493(17) Uani 1 1 d . . . . .
N3 N -0.0306(6) 0.6661(3) 0.1138(2) 0.0471(16) Uani 1 1 d . . . . .
Nd1 Nd 0.13676(4) 0.55009(2) 0.26915(2) 0.03987(13) Uani 1 1 d . . . . .
Nd2 Nd 0.06061(4) 0.66848(2) 0.31948(2) 0.03957(13) Uani 1 1 d . . . . .
Nd3 Nd 0.10321(4) 0.65718(2) 0.18804(2) 0.03896(12) Uani 1 1 d . . . . .
O1 O 0.3483(5) 0.5234(2) 0.2926(2) 0.0591(16) Uani 1 1 d . . . . .
O2 O 0.2223(5) 0.7139(2) 0.37799(19) 0.0502(14) Uani 1 1 d . . . . .
O3 O 0.2951(5) 0.6944(2) 0.1686(2) 0.0513(14) Uani 1 1 d . . . . .
Si1 Si -0.1162(2) 0.46499(10) 0.27339(10) 0.0587(7) Uani 1 1 d . . . . .
Si2 Si -0.2473(2) 0.70154(11) 0.31563(11) 0.0634(7) Uani 1 1 d . . . . .
Si3 Si -0.1456(2) 0.62845(11) 0.09229(9) 0.0592(7) Uani 1 1 d . . . . .
C100 C 0.1965(19) 0.0690(9) 0.9688(8) 0.081(6) Uiso 0.5 1 d . . P . .
H10A H 0.2262 0.1035 0.9778 0.122 Uiso 0.5 1 calc R U P . .
H10B H 0.1689 0.0676 0.9320 0.122 Uiso 0.5 1 calc R U P . .
H10C H 0.2579 0.0436 0.9771 0.122 Uiso 0.5 1 calc R U P . .
C101 C 0.1118(17) 0.0587(8) 0.9946(7) 0.068(5) Uiso 0.5 1 d . . P . .
H10D H 0.0546 0.0866 0.9876 0.082 Uiso 0.5 1 calc R U P . .
H10E H 0.1425 0.0609 1.0314 0.082 Uiso 0.5 1 calc R U P . .
C102 C 0.0487(10) 0.0090(7) 0.9868(6) 0.056(4) Uiso 0.5 1 d D . P . .
H10F H 0.1081 -0.0181 0.9929 0.067 Uiso 0.5 1 calc R U P . .
H10G H 0.0199 0.0077 0.9498 0.067 Uiso 0.5 1 calc R U P . .
C200 C 0.0201(18) 0.9978(8) 0.3809(7) 0.075(6) Uiso 0.5 1 d D . P . .
H20D H -0.0638 1.0000 0.3734 0.113 Uiso 0.33(2) 1 calc R U P B 1
H20E H 0.0493 0.9739 0.3568 0.113 Uiso 0.33(2) 1 calc R U P B 1
H20F H 0.0537 1.0320 0.3774 0.113 Uiso 0.33(2) 1 calc R U P B 1
H20G H -0.0274 0.9681 0.3688 0.113 Uiso 0.17(2) 1 calc R U P B 2
H20H H 0.0978 0.9861 0.3942 0.113 Uiso 0.17(2) 1 calc R U P B 2
H20I H 0.0242 1.0217 0.3524 0.113 Uiso 0.17(2) 1 calc R U P B 2
C201 C 0.052(3) 0.9787(14) 0.4342(9) 0.109(16) Uiso 0.33(2) 1 d D . P B 1
H20J H 0.0325 0.9417 0.4351 0.131 Uiso 0.33(2) 1 calc R U P B 1
H20K H 0.1369 0.9816 0.4429 0.131 Uiso 0.33(2) 1 calc R U P B 1
C20A C -0.031(5) 1.0241(19) 0.4219(10) 0.08(2) Uiso 0.17(2) 1 d D . P B 2
H20L H -0.0094 1.0609 0.4217 0.094 Uiso 0.17(2) 1 calc R U P B 2
H20M H -0.1160 1.0223 0.4136 0.094 Uiso 0.17(2) 1 calc R U P B 2
C202 C 0.000(2) 1.0045(10) 0.4730(7) 0.092(7) Uiso 0.5 1 d D . P . .
H20N H -0.0827 1.0053 0.4592 0.110 Uiso 0.33(2) 1 calc R U P B 1
H20O H 0.0269 1.0405 0.4713 0.110 Uiso 0.33(2) 1 calc R U P B 1
H20P H -0.0016 0.9677 0.4631 0.110 Uiso 0.17(2) 1 calc R U P B 2
H20Q H 0.0825 1.0135 0.4755 0.110 Uiso 0.17(2) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 Nd2 2.805(8) . ?
C2 Nd1 2.811(8) . ?
C2 Nd3 2.834(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 Nd1 2.424(8) . ?
C1 Nd3 2.495(7) . ?
C1 Nd2 2.505(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C3 Nd1 2.626(8) . ?
C3 Nd2 2.664(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 Nd2 2.585(8) . ?
C4 Nd3 2.649(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 Nd3 2.622(9) . ?
C5 Nd1 2.666(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 Si1 1.885(10) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 Si1 1.875(10) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 Si1 1.882(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N1 1.404(10) . ?
C9 C14 1.429(11) . ?
C9 C10 1.439(10) . ?
C9 Nd1 2.991(8) . ?
C10 C11 1.376(12) . ?
C10 C15 1.506(11) . ?
C11 C12 1.344(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.397(13) . ?
C13 H13 0.9500 . ?
C14 C18 1.530(12) . ?
C15 C17 1.535(13) . ?
C15 C16 1.539(12) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.507(14) . ?
C18 C19 1.524(14) . ?
C18 H18 1.0000 . ?
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 Si2 1.867(11) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 Si2 1.856(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 Si2 1.877(11) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N2 1.408(10) . ?
C24 C29 1.410(12) . ?
C24 C25 1.442(12) . ?
C24 Nd2 3.056(8) . ?
C25 C26 1.390(13) . ?
C25 C30 1.520(15) . ?
C26 C27 1.367(15) . ?
C26 H26 0.9500 . ?
C27 C28 1.378(14) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(12) . ?
C28 H28 0.9500 . ?
C29 C33 1.528(12) . ?
C30 C32 1.524(17) . ?
C30 C31 1.542(16) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.525(13) . ?
C33 C35 1.533(14) . ?
C33 H33 1.0000 . ?
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 Si3 1.868(11) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 Si3 1.862(11) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 Si3 1.877(10) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 N3 1.409(10) . ?
C39 C40 1.410(12) . ?
C39 C44 1.436(12) . ?
C39 Nd3 3.015(7) . ?
C40 C41 1.406(12) . ?
C40 C45 1.517(12) . ?
C41 C42 1.372(14) . ?
C41 H41 0.9500 . ?
C42 C43 1.379(15) . ?
C42 H42 0.9500 . ?
C43 C44 1.383(13) . ?
C43 H43 0.9500 . ?
C44 C48 1.523(13) . ?
C45 C47 1.518(12) . ?
C45 C46 1.545(12) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C50 1.485(13) . ?
C48 C49 1.508(14) . ?
C48 H48 1.0000 . ?
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 O1 1.434(11) . ?
C51 C52 1.546(15) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.464(17) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.504(15) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 O1 1.468(10) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 O2 1.453(10) . ?
C55 C56 1.472(12) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.488(16) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.493(16) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 O2 1.459(9) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 O3 1.424(11) . ?
C59 C60 1.471(16) . ?
C59 C60A 1.49(4) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 H59C 0.9900 . ?
C59 H59D 0.9900 . ?
C60 C61 1.480(19) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C62 1.456(16) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C60A C61A 1.32(5) . ?
C60A H60C 0.9900 . ?
C60A H60D 0.9900 . ?
C61A C62 1.32(4) . ?
C61A H61C 0.9900 . ?
C61A H61D 0.9900 . ?
C62 O3 1.457(10) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 H62C 0.9900 . ?
C62 H62D 0.9900 . ?
N1 Si1 1.699(7) . ?
N1 Nd1 2.356(6) . ?
N2 Si2 1.705(7) . ?
N2 Nd2 2.354(6) . ?
N3 Si3 1.702(7) . ?
N3 Nd3 2.352(6) . ?
Nd1 O1 2.572(5) . ?
Nd1 Nd3 3.4979(6) . ?
Nd1 Nd2 3.5103(6) . ?
Nd2 O2 2.568(5) . ?
Nd2 Nd3 3.5758(6) . ?
Nd3 O3 2.562(5) . ?
C100 C101 1.30(3) . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
C101 C102 1.49(2) . ?
C101 H10D 0.9900 . ?
C101 H10E 0.9900 . ?
C102 C102 1.489(10) 3_557 ?
C102 H10F 0.9900 . ?
C102 H10G 0.9900 . ?
C200 C20A 1.473(19) . ?
C200 C201 1.491(18) . ?
C200 H20D 0.9800 . ?
C200 H20E 0.9800 . ?
C200 H20F 0.9800 . ?
C200 H20G 0.9800 . ?
C200 H20H 0.9800 . ?
C200 H20I 0.9800 . ?
C201 C202 1.426(18) . ?
C201 H20J 0.9900 . ?
C201 H20K 0.9900 . ?
C20A C202 1.442(19) . ?
C20A H20L 0.9900 . ?
C20A H20M 0.9900 . ?
C202 C202 1.44(4) 3_576 ?
C202 H20N 0.9900 . ?
C202 H20O 0.9900 . ?
C202 H20P 0.9900 . ?
C202 H20Q 0.9900 . ?

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
Nd2 C2 Nd1 77.4(2) . . ?
Nd2 C2 Nd3 78.7(2) . . ?
Nd1 C2 Nd3 76.57(19) . . ?
Nd2 C2 H2A 115.6 . . ?
Nd1 C2 H2A 115.6 . . ?
Nd3 C2 H2A 162.2 . . ?
Nd2 C2 H2B 115.6 . . ?
Nd1 C2 H2B 115.6 . . ?
Nd3 C2 H2B 49.6 . . ?
H2A C2 H2B 112.7 . . ?
Nd1 C1 Nd3 90.6(3) . . ?
Nd1 C1 Nd2 90.8(2) . . ?
Nd3 C1 Nd2 91.3(2) . . ?
Nd1 C1 H1A 109.5 . . ?
Nd3 C1 H1A 78.4 . . ?
Nd1 C1 H1B 109.5 . . ?
Nd3 C1 H1B 153.3 . . ?
Nd2 C1 H1B 105.3 . . ?
H1A C1 H1B 109.5 . . ?
Nd1 C1 H1C 109.5 . . ?
Nd3 C1 H1C 45.3 . . ?
Nd2 C1 H1C 130.1 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Nd1 C3 Nd2 83.1(2) . . ?
Nd1 C3 H3A 109.5 . . ?
Nd1 C3 H3B 109.5 . . ?
Nd2 C3 H3B 141.5 . . ?
H3A C3 H3B 109.5 . . ?
Nd1 C3 H3C 109.5 . . ?
Nd2 C3 H3C 99.3 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Nd2 C4 Nd3 86.2(2) . . ?
Nd2 C4 H4A 109.5 . . ?
Nd3 C4 H4A 123.9 . . ?
Nd2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Nd2 C4 H4C 109.5 . . ?
Nd3 C4 H4C 115.1 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Nd3 C5 Nd1 82.8(2) . . ?
Nd3 C5 H5A 109.5 . . ?
Nd1 C5 H5A 79.2 . . ?
Nd3 C5 H5B 109.5 . . ?
Nd1 C5 H5B 160.3 . . ?
H5A C5 H5B 109.5 . . ?
Nd3 C5 H5C 109.5 . . ?
Nd1 C5 H5C 51.0 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C14 121.0(7) . . ?
N1 C9 C10 121.0(7) . . ?
C14 C9 C10 117.8(8) . . ?
N1 C9 Nd1 50.3(3) . . ?
C14 C9 Nd1 104.9(5) . . ?
C10 C9 Nd1 111.1(5) . . ?
C11 C10 C9 118.8(8) . . ?
C11 C10 C15 121.5(8) . . ?
C9 C10 C15 119.7(8) . . ?
C12 C11 C10 123.3(9) . . ?
C12 C11 H11 118.3 . . ?
C10 C11 H11 118.3 . . ?
C11 C12 C13 119.6(10) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 121.2(9) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C9 119.2(8) . . ?
C13 C14 C18 119.5(8) . . ?
C9 C14 C18 121.2(8) . . ?
C10 C15 C17 110.4(8) . . ?
C10 C15 C16 113.1(8) . . ?
C17 C15 C16 109.8(7) . . ?
C10 C15 H15 107.8 . . ?
C17 C15 H15 107.8 . . ?
C16 C15 H15 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 C18 C19 109.4(8) . . ?
C20 C18 C14 111.4(8) . . ?
C19 C18 C14 112.9(9) . . ?
C20 C18 H18 107.6 . . ?
C19 C18 H18 107.6 . . ?
C14 C18 H18 107.6 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 C29 122.8(8) . . ?
N2 C24 C25 120.2(8) . . ?
C29 C24 C25 117.0(8) . . ?
N2 C24 Nd2 47.8(4) . . ?
C29 C24 Nd2 112.7(6) . . ?
C25 C24 Nd2 107.4(6) . . ?
C26 C25 C24 119.4(10) . . ?
C26 C25 C30 119.8(9) . . ?
C24 C25 C30 120.7(8) . . ?
C27 C26 C25 122.2(10) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C26 C27 C28 119.3(10) . . ?
C26 C27 H27 120.4 . . ?
C28 C27 H27 120.4 . . ?
C27 C28 C29 121.1(10) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C28 C29 C24 121.0(8) . . ?
C28 C29 C33 118.0(9) . . ?
C24 C29 C33 120.9(8) . . ?
C25 C30 C32 111.0(10) . . ?
C25 C30 C31 114.8(11) . . ?
C32 C30 C31 109.0(9) . . ?
C25 C30 H30 107.2 . . ?
C32 C30 H30 107.2 . . ?
C31 C30 H30 107.2 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C29 112.2(8) . . ?
C34 C33 C35 108.3(8) . . ?
C29 C33 C35 111.8(9) . . ?
C34 C33 H33 108.1 . . ?
C29 C33 H33 108.1 . . ?
C35 C33 H33 108.1 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si3 C36 H36A 109.5 . . ?
Si3 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si3 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si3 C37 H37A 109.5 . . ?
Si3 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si3 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si3 C38 H38A 109.5 . . ?
Si3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N3 C39 C40 121.5(8) . . ?
N3 C39 C44 120.7(8) . . ?
C40 C39 C44 117.7(8) . . ?
N3 C39 Nd3 49.3(3) . . ?
C40 C39 Nd3 109.6(5) . . ?
C44 C39 Nd3 107.3(5) . . ?
C41 C40 C39 119.8(9) . . ?
C41 C40 C45 118.4(9) . . ?
C39 C40 C45 121.7(7) . . ?
C42 C41 C40 120.9(10) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C43 120.6(10) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C42 C43 C44 120.4(10) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C39 120.6(9) . . ?
C43 C44 C48 117.1(9) . . ?
C39 C44 C48 122.3(8) . . ?
C40 C45 C47 110.1(7) . . ?
C40 C45 C46 114.5(8) . . ?
C47 C45 C46 109.6(8) . . ?
C40 C45 H45 107.5 . . ?
C47 C45 H45 107.5 . . ?
C46 C45 H45 107.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C50 C48 C49 109.4(9) . . ?
C50 C48 C44 111.9(9) . . ?
C49 C48 C44 115.0(9) . . ?
C50 C48 H48 106.7 . . ?
C49 C48 H48 106.7 . . ?
C44 C48 H48 106.7 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O1 C51 C52 103.5(9) . . ?
O1 C51 H51A 111.1 . . ?
C52 C51 H51A 111.1 . . ?
O1 C51 H51B 111.1 . . ?
C52 C51 H51B 111.1 . . ?
H51A C51 H51B 109.0 . . ?
C53 C52 C51 104.2(10) . . ?
C53 C52 H52A 110.9 . . ?
C51 C52 H52A 110.9 . . ?
C53 C52 H52B 110.9 . . ?
C51 C52 H52B 110.9 . . ?
H52A C52 H52B 108.9 . . ?
C52 C53 C54 107.4(10) . . ?
C52 C53 H53A 110.2 . . ?
C54 C53 H53A 110.2 . . ?
C52 C53 H53B 110.2 . . ?
C54 C53 H53B 110.2 . . ?
H53A C53 H53B 108.5 . . ?
O1 C54 C53 105.8(9) . . ?
O1 C54 H54A 110.6 . . ?
C53 C54 H54A 110.6 . . ?
O1 C54 H54B 110.6 . . ?
C53 C54 H54B 110.6 . . ?
H54A C54 H54B 108.7 . . ?
O2 C55 C56 106.6(8) . . ?
O2 C55 H55A 110.4 . . ?
C56 C55 H55A 110.4 . . ?
O2 C55 H55B 110.4 . . ?
C56 C55 H55B 110.4 . . ?
H55A C55 H55B 108.6 . . ?
C55 C56 C57 102.4(9) . . ?
C55 C56 H56A 111.3 . . ?
C57 C56 H56A 111.3 . . ?
C55 C56 H56B 111.3 . . ?
C57 C56 H56B 111.3 . . ?
H56A C56 H56B 109.2 . . ?
C56 C57 C58 105.7(9) . . ?
C56 C57 H57A 110.6 . . ?
C58 C57 H57A 110.6 . . ?
C56 C57 H57B 110.6 . . ?
C58 C57 H57B 110.6 . . ?
H57A C57 H57B 108.7 . . ?
O2 C58 C57 104.4(8) . . ?
O2 C58 H58A 110.9 . . ?
C57 C58 H58A 110.9 . . ?
O2 C58 H58B 110.9 . . ?
C57 C58 H58B 110.9 . . ?
H58A C58 H58B 108.9 . . ?
O3 C59 C60 107.0(9) . . ?
O3 C59 C60A 101.6(17) . . ?
O3 C59 H59A 110.3 . . ?
C60 C59 H59A 110.3 . . ?
O3 C59 H59B 110.3 . . ?
C60 C59 H59B 110.3 . . ?
H59A C59 H59B 108.6 . . ?
O3 C59 H59C 111.5 . . ?
C60A C59 H59C 111.5 . . ?
O3 C59 H59D 111.5 . . ?
C60A C59 H59D 111.5 . . ?
H59C C59 H59D 109.3 . . ?
C59 C60 C61 106.0(11) . . ?
C59 C60 H60A 110.5 . . ?
C61 C60 H60A 110.5 . . ?
C59 C60 H60B 110.5 . . ?
C61 C60 H60B 110.5 . . ?
H60A C60 H60B 108.7 . . ?
C62 C61 C60 106.6(12) . . ?
C62 C61 H61A 110.4 . . ?
C60 C61 H61A 110.4 . . ?
C62 C61 H61B 110.4 . . ?
C60 C61 H61B 110.4 . . ?
H61A C61 H61B 108.6 . . ?
C61A C60A C59 108(3) . . ?
C61A C60A H60C 110.2 . . ?
C59 C60A H60C 110.2 . . ?
C61A C60A H60D 110.2 . . ?
C59 C60A H60D 110.2 . . ?
H60C C60A H60D 108.5 . . ?
C60A C61A C62 113(3) . . ?
C60A C61A H61C 109.1 . . ?
C62 C61A H61C 109.1 . . ?
C60A C61A H61D 109.1 . . ?
C62 C61A H61D 109.1 . . ?
H61C C61A H61D 107.8 . . ?
C61A C62 O3 103.7(18) . . ?
C61 C62 O3 104.6(9) . . ?
C61 C62 H62A 110.8 . . ?
O3 C62 H62A 110.8 . . ?
C61 C62 H62B 110.8 . . ?
O3 C62 H62B 110.8 . . ?
H62A C62 H62B 108.9 . . ?
C61A C62 H62C 111.0 . . ?
O3 C62 H62C 111.0 . . ?
C61A C62 H62D 111.0 . . ?
O3 C62 H62D 111.0 . . ?
H62C C62 H62D 109.0 . . ?
C9 N1 Si1 125.0(5) . . ?
C9 N1 Nd1 102.4(5) . . ?
Si1 N1 Nd1 132.0(4) . . ?
C24 N2 Si2 123.0(6) . . ?
C24 N2 Nd2 105.9(5) . . ?
Si2 N2 Nd2 130.8(3) . . ?
C39 N3 Si3 126.7(5) . . ?
C39 N3 Nd3 103.8(4) . . ?
Si3 N3 Nd3 129.2(3) . . ?
N1 Nd1 C1 98.3(2) . . ?
N1 Nd1 O1 107.9(2) . . ?
C1 Nd1 O1 153.8(2) . . ?
N1 Nd1 C3 102.3(2) . . ?
C1 Nd1 C3 86.9(2) . . ?
O1 Nd1 C3 88.8(2) . . ?
N1 Nd1 C5 107.3(2) . . ?
C1 Nd1 C5 85.6(2) . . ?
O1 Nd1 C5 85.4(2) . . ?
C3 Nd1 C5 150.2(3) . . ?
N1 Nd1 C2 176.0(2) . . ?
C1 Nd1 C2 79.2(2) . . ?
O1 Nd1 C2 74.7(2) . . ?
C3 Nd1 C2 74.5(3) . . ?
C5 Nd1 C2 75.8(2) . . ?
N1 Nd1 C9 27.3(2) . . ?
C1 Nd1 C9 124.0(2) . . ?
O1 Nd1 C9 81.7(2) . . ?
C3 Nd1 C9 109.9(2) . . ?
C5 Nd1 C9 98.2(2) . . ?
C2 Nd1 C9 156.0(2) . . ?
N1 Nd1 Nd3 128.09(15) . . ?
C1 Nd1 Nd3 45.49(17) . . ?
O1 Nd1 Nd3 112.83(13) . . ?
C3 Nd1 Nd3 109.18(18) . . ?
C5 Nd1 Nd3 48.04(18) . . ?
C2 Nd1 Nd3 52.02(15) . . ?
C9 Nd1 Nd3 138.43(14) . . ?
N1 Nd1 Nd2 124.80(16) . . ?
C1 Nd1 Nd2 45.53(16) . . ?
O1 Nd1 Nd2 115.54(14) . . ?
C3 Nd1 Nd2 48.90(18) . . ?
C5 Nd1 Nd2 108.52(18) . . ?
C2 Nd1 Nd2 51.24(17) . . ?
C9 Nd1 Nd2 148.81(16) . . ?
Nd3 Nd1 Nd2 61.358(13) . . ?
N2 Nd2 C1 100.5(2) . . ?
N2 Nd2 O2 105.8(2) . . ?
C1 Nd2 O2 153.6(2) . . ?
N2 Nd2 C4 99.7(2) . . ?
C1 Nd2 C4 83.8(2) . . ?
O2 Nd2 C4 90.4(2) . . ?
N2 Nd2 C3 111.1(3) . . ?
C1 Nd2 C3 84.4(2) . . ?
O2 Nd2 C3 87.4(2) . . ?
C4 Nd2 C3 148.5(3) . . ?
N2 Nd2 C2 174.6(2) . . ?
C1 Nd2 C2 78.0(2) . . ?
O2 Nd2 C2 75.61(19) . . ?
C4 Nd2 C2 75.0(2) . . ?
C3 Nd2 C2 74.0(3) . . ?
N2 Nd2 C24 26.3(2) . . ?
C1 Nd2 C24 124.8(3) . . ?
O2 Nd2 C24 81.4(2) . . ?
C4 Nd2 C24 109.9(2) . . ?
C3 Nd2 C24 100.8(2) . . ?
C2 Nd2 C24 156.6(2) . . ?
N2 Nd2 Nd1 130.63(17) . . ?
C1 Nd2 Nd1 43.67(17) . . ?
O2 Nd2 Nd1 115.11(13) . . ?
C4 Nd2 Nd1 106.21(17) . . ?
C3 Nd2 Nd1 47.96(17) . . ?
C2 Nd2 Nd1 51.39(16) . . ?
C24 Nd2 Nd1 140.08(18) . . ?
N2 Nd2 Nd3 124.56(16) . . ?
C1 Nd2 Nd3 44.23(17) . . ?
O2 Nd2 Nd3 115.62(12) . . ?
C4 Nd2 Nd3 47.66(17) . . ?
C3 Nd2 Nd3 106.09(18) . . ?
C2 Nd2 Nd3 51.01(15) . . ?
C24 Nd2 Nd3 148.43(16) . . ?
Nd1 Nd2 Nd3 59.150(12) . . ?
N3 Nd3 C1 100.8(2) . . ?
N3 Nd3 O3 107.7(2) . . ?
C1 Nd3 O3 151.4(2) . . ?
N3 Nd3 C5 102.5(2) . . ?
C1 Nd3 C5 85.2(2) . . ?
O3 Nd3 C5 86.6(2) . . ?
N3 Nd3 C4 107.6(2) . . ?
C1 Nd3 C4 82.7(2) . . ?
O3 Nd3 C4 90.6(2) . . ?
C5 Nd3 C4 149.1(2) . . ?
N3 Nd3 C2 178.0(2) . . ?
C1 Nd3 C2 77.6(2) . . ?
O3 Nd3 C2 73.8(2) . . ?
C5 Nd3 C2 76.1(2) . . ?
C4 Nd3 C2 73.6(2) . . ?
N3 Nd3 C39 27.0(2) . . ?
C1 Nd3 C39 125.5(2) . . ?
O3 Nd3 C39 82.9(2) . . ?
C5 Nd3 C39 112.1(2) . . ?
C4 Nd3 C39 98.1(2) . . ?
C2 Nd3 C39 154.9(2) . . ?
N3 Nd3 Nd1 126.55(16) . . ?
C1 Nd3 Nd1 43.87(17) . . ?
O3 Nd3 Nd1 113.04(12) . . ?
C5 Nd3 Nd1 49.14(17) . . ?
C4 Nd3 Nd1 105.08(16) . . ?
C2 Nd3 Nd1 51.41(16) . . ?
C39 Nd3 Nd1 151.42(16) . . ?
N3 Nd3 Nd2 129.34(17) . . ?
C1 Nd3 Nd2 44.46(16) . . ?
O3 Nd3 Nd2 113.65(12) . . ?
C5 Nd3 Nd2 107.76(17) . . ?
C4 Nd3 Nd2 46.16(16) . . ?
C2 Nd3 Nd2 50.29(16) . . ?
C39 Nd3 Nd2 137.64(17) . . ?
Nd1 Nd3 Nd2 59.492(12) . . ?
C51 O1 C54 108.0(7) . . ?
C51 O1 Nd1 121.2(5) . . ?
C54 O1 Nd1 129.9(6) . . ?
C55 O2 C58 108.9(6) . . ?
C55 O2 Nd2 129.1(5) . . ?
C58 O2 Nd2 121.5(5) . . ?
C59 O3 C62 107.1(7) . . ?
C59 O3 Nd3 119.6(5) . . ?
C62 O3 Nd3 131.2(5) . . ?
N1 Si1 C7 109.7(4) . . ?
N1 Si1 C8 111.8(4) . . ?
C7 Si1 C8 107.0(5) . . ?
N1 Si1 C6 112.5(5) . . ?
C7 Si1 C6 107.7(5) . . ?
C8 Si1 C6 107.9(5) . . ?
N2 Si2 C22 111.7(4) . . ?
N2 Si2 C21 111.4(4) . . ?
C22 Si2 C21 105.9(5) . . ?
N2 Si2 C23 112.0(5) . . ?
C22 Si2 C23 107.5(6) . . ?
C21 Si2 C23 108.1(6) . . ?
N3 Si3 C37 111.4(4) . . ?
N3 Si3 C36 111.3(4) . . ?
C37 Si3 C36 105.8(5) . . ?
N3 Si3 C38 112.9(4) . . ?
C37 Si3 C38 107.6(5) . . ?
C36 Si3 C38 107.6(5) . . ?
C101 C100 H10A 109.5 . . ?
C101 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C101 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C100 C101 C102 120.4(18) . . ?
C100 C101 H10D 107.2 . . ?
C102 C101 H10D 107.2 . . ?
C100 C101 H10E 107.2 . . ?
C102 C101 H10E 107.2 . . ?
H10D C101 H10E 106.9 . . ?
C101 C102 C102 127.3(19) . 3_557 ?
C101 C102 H10F 105.5 . . ?
C102 C102 H10F 105.5 3_557 . ?
C101 C102 H10G 105.5 . . ?
C102 C102 H10G 105.5 3_557 . ?
H10F C102 H10G 106.0 . . ?
C201 C200 H20D 109.5 . . ?
C201 C200 H20E 109.5 . . ?
H20D C200 H20E 109.5 . . ?
C201 C200 H20F 109.5 . . ?
H20D C200 H20F 109.5 . . ?
H20E C200 H20F 109.5 . . ?
C20A C200 H20G 109.5 . . ?
C20A C200 H20H 109.5 . . ?
H20G C200 H20H 109.5 . . ?
C20A C200 H20I 109.5 . . ?
H20G C200 H20I 109.5 . . ?
H20H C200 H20I 109.5 . . ?
C202 C201 C200 116(2) . . ?
C202 C201 H20J 108.3 . . ?
C200 C201 H20J 108.3 . . ?
C202 C201 H20K 108.3 . . ?
C200 C201 H20K 108.3 . . ?
H20J C201 H20K 107.4 . . ?
C202 C20A C200 116(2) . . ?
C202 C20A H20L 108.2 . . ?
C200 C20A H20L 108.2 . . ?
C202 C20A H20M 108.2 . . ?
C200 C20A H20M 108.2 . . ?
H20L C20A H20M 107.4 . . ?
C201 C202 C202 133(3) . 3_576 ?
C202 C202 C20A 161(3) 3_576 . ?
C201 C202 H20N 103.9 . . ?
C202 C202 H20N 103.9 3_576 . ?
C201 C202 H20O 103.9 . . ?
C202 C202 H20O 103.9 3_576 . ?
H20N C202 H20O 105.4 . . ?
C202 C202 H20P 95.8 3_576 . ?
C20A C202 H20P 95.8 . . ?
C202 C202 H20Q 95.8 3_576 . ?
C20A C202 H20Q 95.8 . . ?
H20P C202 H20Q 103.3 . . ?

_refine_diff_density_max         1.090
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.116

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_mulds13-2
_database_code_depnum_ccdc_archive 'CCDC 1410392'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61 H114 N3 Nd3 O4 Si3'
_chemical_formula_weight         1470.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.4680(3)
_cell_length_b                   25.6711(4)
_cell_length_c                   19.6447(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.960(2)
_cell_angle_gamma                90
_cell_volume                     6978.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    845
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      28.59

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_F_000             3020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.292
_shelx_estimated_absorpt_T_min   0.501
_shelx_estimated_absorpt_T_max   0.657
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_T_max  0.8388
_exptl_absorpt_process_details   Palton/Mulabs

_exptl_special_details           
;
 ?
;

_vrf_PLAT910_mulds13-2           
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         18 Report
RESPONSE: Measurement has bee done on a Stoe IPDS!
;


_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'PHI scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            102330
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.842
_diffrn_reflns_theta_max         26.760
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14765
_reflns_number_gt                13514
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'POV-Ray v. 3.6/ORTEP3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Restrains have been used for the disordered THF molecules.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²+11.7977P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14765
_refine_ls_number_parameters     713
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.317
_refine_ls_restrained_S_all      1.314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C2 C 0.2997(4) 0.67393(18) 0.2784(2) 0.0355(11) Uani 1 1 d . . . . .
H10J H 0.2629 0.7036 0.2879 0.053 Uiso 1 1 calc R U . . .
H10K H 0.3673 0.6769 0.3074 0.053 Uiso 1 1 calc R U . . .
H10L H 0.2722 0.6415 0.2903 0.053 Uiso 1 1 calc R U . . .
C3 C 0.4667(4) 0.7156(2) 0.1854(3) 0.0396(11) Uani 1 1 d . . . . .
H10G H 0.5134 0.7433 0.2054 0.059 Uiso 1 1 calc R U . . .
H10H H 0.4018 0.7271 0.1846 0.059 Uiso 1 1 calc R U . . .
H10I H 0.4678 0.7079 0.1367 0.059 Uiso 1 1 calc R U . . .
C4 C 0.4473(4) 0.5715(2) 0.3532(3) 0.0457(13) Uani 1 1 d . . . . .
H10A H 0.4340 0.5576 0.3958 0.068 Uiso 1 1 calc R U . . .
H10B H 0.4659 0.6082 0.3609 0.068 Uiso 1 1 calc R U . . .
H10C H 0.5002 0.5517 0.3437 0.068 Uiso 1 1 calc R U . . .
C5 C 0.1588(4) 0.6027(2) 0.1351(3) 0.0513(14) Uani 1 1 d . . . . .
H10D H 0.0947 0.6184 0.1156 0.077 Uiso 1 1 calc R U . . .
H10E H 0.1651 0.5891 0.1828 0.077 Uiso 1 1 calc R U . . .
H10F H 0.1667 0.5742 0.1041 0.077 Uiso 1 1 calc R U . . .
C6 C 0.1158(5) 0.7900(3) 0.2361(3) 0.0555(15) Uani 1 1 d . . . . .
H6A H 0.0494 0.7807 0.2094 0.083 Uiso 1 1 calc R U . . .
H6B H 0.1149 0.8210 0.2651 0.083 Uiso 1 1 calc R U . . .
H6C H 0.1458 0.7610 0.2671 0.083 Uiso 1 1 calc R U . . .
C7 C 0.3080(4) 0.8256(2) 0.2296(3) 0.0554(15) Uani 1 1 d . . . . .
H7A H 0.3397 0.7967 0.2601 0.083 Uiso 1 1 calc R U . . .
H7B H 0.3003 0.8550 0.2593 0.083 Uiso 1 1 calc R U . . .
H7C H 0.3478 0.8364 0.1993 0.083 Uiso 1 1 calc R U . . .
C8 C 0.1296(4) 0.8616(2) 0.1174(3) 0.0511(14) Uani 1 1 d . . . . .
H8A H 0.1795 0.8820 0.1049 0.077 Uiso 1 1 calc R U . . .
H8B H 0.0973 0.8833 0.1446 0.077 Uiso 1 1 calc R U . . .
H8C H 0.0820 0.8494 0.0738 0.077 Uiso 1 1 calc R U . . .
C9 C 0.1499(3) 0.74840(18) 0.0482(3) 0.0337(10) Uani 1 1 d . . . . .
C10 C 0.1958(4) 0.7657(2) -0.0024(3) 0.0383(11) Uani 1 1 d . . . . .
C11 C 0.1519(4) 0.7579(2) -0.0741(3) 0.0480(13) Uani 1 1 d . . . . .
H11 H 0.1840 0.7690 -0.1074 0.058 Uiso 1 1 calc R U . . .
C12 C 0.0626(4) 0.7344(2) -0.0986(3) 0.0516(14) Uani 1 1 d . . . . .
H12 H 0.0340 0.7287 -0.1481 0.062 Uiso 1 1 calc R U . . .
C13 C 0.0154(4) 0.7193(2) -0.0501(3) 0.0446(12) Uani 1 1 d . . . . .
H13 H -0.0465 0.7036 -0.0669 0.054 Uiso 1 1 calc R U . . .
C14 C 0.0553(3) 0.72638(19) 0.0221(3) 0.0367(11) Uani 1 1 d . . . . .
C15 C -0.0057(4) 0.7144(2) 0.0715(3) 0.0418(12) Uani 1 1 d . . . . .
H15 H 0.0387 0.7095 0.1207 0.050 Uiso 1 1 calc R U . . .
C16 C -0.0705(4) 0.7614(2) 0.0719(3) 0.0551(15) Uani 1 1 d . . . . .
H16A H -0.0305 0.7926 0.0854 0.083 Uiso 1 1 calc R U . . .
H16B H -0.1067 0.7554 0.1063 0.083 Uiso 1 1 calc R U . . .
H16C H -0.1157 0.7661 0.0243 0.083 Uiso 1 1 calc R U . . .
C17 C -0.0688(4) 0.6663(2) 0.0518(4) 0.0575(15) Uani 1 1 d . . . . .
H17A H -0.1213 0.6731 0.0082 0.086 Uiso 1 1 calc R U . . .
H17B H -0.0960 0.6577 0.0906 0.086 Uiso 1 1 calc R U . . .
H17C H -0.0298 0.6370 0.0438 0.086 Uiso 1 1 calc R U . . .
C18 C 0.2923(4) 0.7948(2) 0.0205(3) 0.0471(13) Uani 1 1 d . . . . .
H18 H 0.3148 0.7958 0.0736 0.057 Uiso 1 1 calc R U . . .
C19 C 0.2813(5) 0.8505(3) -0.0067(4) 0.0664(18) Uani 1 1 d . . . . .
H19A H 0.3431 0.8688 0.0114 0.100 Uiso 1 1 calc R U . . .
H19B H 0.2319 0.8683 0.0099 0.100 Uiso 1 1 calc R U . . .
H19C H 0.2619 0.8504 -0.0588 0.100 Uiso 1 1 calc R U . . .
C20 C 0.3689(4) 0.7677(3) -0.0050(4) 0.0600(16) Uani 1 1 d . . . . .
H20A H 0.3507 0.7687 -0.0571 0.090 Uiso 1 1 calc R U . . .
H20B H 0.3747 0.7314 0.0110 0.090 Uiso 1 1 calc R U . . .
H20C H 0.4310 0.7854 0.0145 0.090 Uiso 1 1 calc R U . . .
C21 C 0.6544(5) 0.6486(3) 0.0953(3) 0.0593(16) Uani 1 1 d . . . . .
H21A H 0.5910 0.6639 0.0911 0.089 Uiso 1 1 calc R U . . .
H21B H 0.6568 0.6370 0.0484 0.089 Uiso 1 1 calc R U . . .
H21C H 0.7048 0.6747 0.1140 0.089 Uiso 1 1 calc R U . . .
C22 C 0.5896(5) 0.5396(3) 0.1105(3) 0.0651(17) Uani 1 1 d . . . . .
H22A H 0.6112 0.5057 0.1325 0.098 Uiso 1 1 calc R U . . .
H22B H 0.5880 0.5387 0.0603 0.098 Uiso 1 1 calc R U . . .
H22C H 0.5247 0.5471 0.1140 0.098 Uiso 1 1 calc R U . . .
C23 C 0.7999(5) 0.5679(3) 0.1666(4) 0.0692(19) Uani 1 1 d . . . . .
H23A H 0.8465 0.5896 0.2012 0.104 Uiso 1 1 calc R U . . .
H23B H 0.8126 0.5702 0.1203 0.104 Uiso 1 1 calc R U . . .
H23C H 0.8063 0.5317 0.1828 0.104 Uiso 1 1 calc R U . . .
C24 C 0.7235(3) 0.6100(2) 0.3042(3) 0.0376(11) Uani 1 1 d . . . . .
C25 C 0.7794(4) 0.6560(2) 0.3229(3) 0.0454(12) Uani 1 1 d . . . . .
C26 C 0.8426(4) 0.6606(3) 0.3910(3) 0.0558(15) Uani 1 1 d . . . . .
H26 H 0.8806 0.6913 0.4031 0.067 Uiso 1 1 calc R U . . .
C27 C 0.8521(5) 0.6224(3) 0.4417(3) 0.0586(16) Uani 1 1 d . . . . .
H27 H 0.8954 0.6268 0.4881 0.070 Uiso 1 1 calc R U . . .
C28 C 0.7978(4) 0.5779(3) 0.4240(3) 0.0547(15) Uani 1 1 d . . . . .
H28 H 0.8037 0.5516 0.4590 0.066 Uiso 1 1 calc R U . . .
C29 C 0.7346(4) 0.5703(2) 0.3565(3) 0.0433(12) Uani 1 1 d . . . . .
C30 C 0.6820(4) 0.5186(2) 0.3379(3) 0.0500(14) Uani 1 1 d . . . . .
H30 H 0.6167 0.5261 0.3044 0.060 Uiso 1 1 calc R U . . .
C31 C 0.6668(5) 0.4891(3) 0.4013(4) 0.0667(18) Uani 1 1 d . . . . .
H31A H 0.6225 0.4599 0.3841 0.100 Uiso 1 1 calc R U . . .
H31B H 0.6393 0.5127 0.4295 0.100 Uiso 1 1 calc R U . . .
H31C H 0.7290 0.4758 0.4310 0.100 Uiso 1 1 calc R U . . .
C32 C 0.7354(5) 0.4843(2) 0.2989(4) 0.0660(18) Uani 1 1 d . . . . .
H32A H 0.8020 0.4791 0.3287 0.099 Uiso 1 1 calc R U . . .
H32B H 0.7357 0.5011 0.2542 0.099 Uiso 1 1 calc R U . . .
H32C H 0.7029 0.4505 0.2886 0.099 Uiso 1 1 calc R U . . .
C33 C 0.7743(4) 0.6995(2) 0.2700(3) 0.0528(14) Uani 1 1 d . . . . .
H33 H 0.7193 0.6915 0.2268 0.063 Uiso 1 1 calc R U . . .
C34 C 0.7543(5) 0.7520(2) 0.2978(4) 0.0647(17) Uani 1 1 d . . . . .
H34A H 0.6944 0.7502 0.3115 0.097 Uiso 1 1 calc R U . . .
H34B H 0.7474 0.7784 0.2605 0.097 Uiso 1 1 calc R U . . .
H34C H 0.8080 0.7616 0.3393 0.097 Uiso 1 1 calc R U . . .
C35 C 0.8656(6) 0.7027(3) 0.2465(4) 0.083(2) Uani 1 1 d . . . . .
H35A H 0.8609 0.7325 0.2145 0.125 Uiso 1 1 calc R U . . .
H35B H 0.8727 0.6705 0.2216 0.125 Uiso 1 1 calc R U . . .
H35C H 0.9218 0.7071 0.2884 0.125 Uiso 1 1 calc R U . . .
C36 C 0.3093(6) 0.4848(3) 0.0780(4) 0.075(2) Uani 1 1 d . . . . .
H36A H 0.2401 0.4814 0.0534 0.112 Uiso 1 1 calc R U . . .
H36B H 0.3467 0.4720 0.0471 0.112 Uiso 1 1 calc R U . . .
H36C H 0.3249 0.5215 0.0896 0.112 Uiso 1 1 calc R U . . .
C37 C 0.4749(5) 0.4448(3) 0.1978(4) 0.076(2) Uani 1 1 d . . . . .
H37A H 0.4981 0.4798 0.2145 0.114 Uiso 1 1 calc R U . . .
H37B H 0.5030 0.4341 0.1602 0.114 Uiso 1 1 calc R U . . .
H37C H 0.4943 0.4202 0.2375 0.114 Uiso 1 1 calc R U . . .
C38 C 0.3019(7) 0.3766(3) 0.1398(5) 0.085(2) Uani 1 1 d . . . . .
H38A H 0.3576 0.3535 0.1578 0.127 Uiso 1 1 calc R U . . .
H38B H 0.2763 0.3727 0.0881 0.127 Uiso 1 1 calc R U . . .
H38C H 0.2516 0.3674 0.1621 0.127 Uiso 1 1 calc R U . . .
C39 C 0.2345(4) 0.4423(2) 0.2555(3) 0.0469(13) Uani 1 1 d . . . . .
C40 C 0.1333(4) 0.4367(2) 0.2267(4) 0.0623(18) Uani 1 1 d . . . . .
C41 C 0.0823(6) 0.4075(3) 0.2629(6) 0.094(3) Uani 1 1 d . . . . .
H41 H 0.0142 0.4045 0.2434 0.113 Uiso 1 1 calc R U . . .
C42 C 0.1260(7) 0.3832(4) 0.3250(7) 0.116(4) Uani 1 1 d . . . . .
H42 H 0.0891 0.3628 0.3480 0.139 Uiso 1 1 calc R U . . .
C43 C 0.2244(7) 0.3882(3) 0.3549(5) 0.096(3) Uani 1 1 d . . . . .
H43 H 0.2549 0.3717 0.3990 0.115 Uiso 1 1 calc R U . . .
C44 C 0.2797(5) 0.4171(2) 0.3211(4) 0.0606(17) Uani 1 1 d . . . . .
C45 C 0.3884(5) 0.4190(2) 0.3553(4) 0.0595(16) Uani 1 1 d . . . . .
H45 H 0.4157 0.4440 0.3272 0.071 Uiso 1 1 calc R U . . .
C46 C 0.4158(6) 0.4388(3) 0.4321(4) 0.080(2) Uani 1 1 d . . . . .
H46A H 0.3935 0.4139 0.4617 0.120 Uiso 1 1 calc R U . . .
H46B H 0.3853 0.4727 0.4335 0.120 Uiso 1 1 calc R U . . .
H46C H 0.4862 0.4425 0.4502 0.120 Uiso 1 1 calc R U . . .
C47 C 0.4339(6) 0.3661(3) 0.3515(5) 0.080(2) Uani 1 1 d . . . . .
H47A H 0.4066 0.3403 0.3771 0.119 Uiso 1 1 calc R U . . .
H47B H 0.5039 0.3683 0.3733 0.119 Uiso 1 1 calc R U . . .
H47C H 0.4203 0.3555 0.3016 0.119 Uiso 1 1 calc R U . . .
C48 C 0.0792(6) 0.4603(3) 0.1557(5) 0.0909(15) Uani 1 1 d . . . . .
H48 H 0.1256 0.4836 0.1413 0.109 Uiso 1 1 calc R U . . .
C49 C -0.0058(5) 0.4937(3) 0.1583(5) 0.0909(15) Uani 1 1 d . . . . .
H49A H -0.0564 0.4716 0.1669 0.136 Uiso 1 1 calc R U . . .
H49B H -0.0312 0.5120 0.1128 0.136 Uiso 1 1 calc R U . . .
H49C H 0.0152 0.5193 0.1968 0.136 Uiso 1 1 calc R U . . .
C50 C 0.0448(6) 0.4205(3) 0.0974(5) 0.0909(15) Uani 1 1 d . . . . .
H50A H 0.1007 0.4033 0.0885 0.136 Uiso 1 1 calc R U . . .
H50B H 0.0066 0.4378 0.0538 0.136 Uiso 1 1 calc R U . . .
H50C H 0.0048 0.3945 0.1119 0.136 Uiso 1 1 calc R U . . .
C52 C 0.2485(9) 0.6186(6) -0.0972(6) 0.0691(19) Uani 0.661(17) 1 d . U P A 1
H52A H 0.2259 0.5860 -0.1239 0.083 Uiso 0.661(17) 1 calc R U P A 1
H52B H 0.2235 0.6485 -0.1291 0.083 Uiso 0.661(17) 1 calc R U P A 1
C53 C 0.3512(9) 0.6198(6) -0.0735(6) 0.0689(19) Uani 0.661(17) 1 d . U P A 1
H53A H 0.3754 0.6522 -0.0896 0.083 Uiso 0.661(17) 1 calc R U P A 1
H53B H 0.3781 0.5897 -0.0929 0.083 Uiso 0.661(17) 1 calc R U P A 1
C52A C 0.2549(18) 0.5931(12) -0.0872(13) 0.069(2) Uani 0.339(17) 1 d . U P A 2
H52C H 0.2314 0.5567 -0.0939 0.083 Uiso 0.339(17) 1 calc R U P A 2
H52D H 0.2357 0.6110 -0.1339 0.083 Uiso 0.339(17) 1 calc R U P A 2
C53A C 0.3615(17) 0.5944(12) -0.0557(13) 0.069(2) Uani 0.339(17) 1 d . U P A 2
H53C H 0.3879 0.5586 -0.0506 0.083 Uiso 0.339(17) 1 calc R U P A 2
H53D H 0.3915 0.6143 -0.0869 0.083 Uiso 0.339(17) 1 calc R U P A 2
C51 C 0.2135(5) 0.6213(3) -0.0343(3) 0.0617(17) Uani 1 1 d . . . . .
H51A H 0.1605 0.6470 -0.0416 0.074 Uiso 0.661(17) 1 calc R U P A 1
H51B H 0.1896 0.5869 -0.0242 0.074 Uiso 0.661(17) 1 calc R U P A 1
H51C H 0.1753 0.6520 -0.0568 0.074 Uiso 0.339(17) 1 calc R U P A 2
H51D H 0.1713 0.5977 -0.0167 0.074 Uiso 0.339(17) 1 calc R U P A 2
C54 C 0.3812(5) 0.6174(3) 0.0086(4) 0.0622(17) Uani 1 1 d . . . . .
H54A H 0.3954 0.5813 0.0260 0.075 Uiso 0.661(17) 1 calc R U P A 1
H54B H 0.4383 0.6396 0.0299 0.075 Uiso 0.661(17) 1 calc R U P A 1
H54C H 0.4270 0.6464 0.0107 0.075 Uiso 0.339(17) 1 calc R U P A 2
H54D H 0.4131 0.5918 0.0457 0.075 Uiso 0.339(17) 1 calc R U P A 2
C55 C 0.5259(5) 0.7497(2) 0.3685(4) 0.0632(17) Uani 1 1 d D . . . .
H55A H 0.4554 0.7511 0.3617 0.076 Uiso 1 1 calc R U . . .
H55B H 0.5407 0.7705 0.3305 0.076 Uiso 1 1 calc R U . . .
C56 C 0.5797(6) 0.7707(3) 0.4401(3) 0.081(2) Uani 1 1 d D . . . .
H56A H 0.6064 0.8057 0.4361 0.097 Uiso 0.70(4) 1 calc R U P B 1
H56B H 0.5376 0.7727 0.4716 0.097 Uiso 0.70(4) 1 calc R U P B 1
H56C H 0.5335 0.7847 0.4640 0.097 Uiso 0.30(4) 1 calc R U P B 2
H56D H 0.6228 0.7994 0.4347 0.097 Uiso 0.30(4) 1 calc R U P B 2
C57 C 0.6574(8) 0.7323(4) 0.4665(10) 0.0730(18) Uani 0.70(4) 1 d D . P B 1
H57A H 0.6782 0.7312 0.5192 0.088 Uiso 0.70(4) 1 calc R U P B 1
H57B H 0.7139 0.7407 0.4498 0.088 Uiso 0.70(4) 1 calc R U P B 1
C57A C 0.639(3) 0.7275(6) 0.4844(13) 0.0730(18) Uani 0.30(4) 1 d D . P B 2
H57C H 0.7089 0.7352 0.4969 0.088 Uiso 0.30(4) 1 calc R U P B 2
H57D H 0.6206 0.7219 0.5287 0.088 Uiso 0.30(4) 1 calc R U P B 2
C58 C 0.6132(5) 0.6814(3) 0.4362(3) 0.0730(18) Uani 1 1 d D . . . .
H58A H 0.6634 0.6555 0.4347 0.088 Uiso 0.70(4) 1 calc R U P B 1
H58B H 0.5719 0.6669 0.4639 0.088 Uiso 0.70(4) 1 calc R U P B 1
H58C H 0.6731 0.6639 0.4336 0.088 Uiso 0.30(4) 1 calc R U P B 2
H58D H 0.5760 0.6562 0.4560 0.088 Uiso 0.30(4) 1 calc R U P B 2
C59 C 0.0877(5) 0.6023(3) 0.3074(4) 0.0672(18) Uani 1 1 d . . . . .
H59A H 0.0549 0.6089 0.2564 0.081 Uiso 0.70(4) 1 calc R U P B 1
H59B H 0.1048 0.6358 0.3328 0.081 Uiso 0.70(4) 1 calc R U P B 1
H59C H 0.1084 0.6392 0.3093 0.081 Uiso 0.30(4) 1 calc R U P B 2
H59D H 0.0413 0.5958 0.2600 0.081 Uiso 0.30(4) 1 calc R U P B 2
C60 C 0.0233(12) 0.5652(9) 0.3438(9) 0.073(2) Uani 0.512(17) 1 d . U P C 1
H60A H -0.0250 0.5862 0.3586 0.088 Uiso 0.512(17) 1 calc R U P C 1
H60B H -0.0108 0.5380 0.3100 0.088 Uiso 0.512(17) 1 calc R U P C 1
C61 C 0.0920(13) 0.5421(7) 0.4048(10) 0.073(2) Uani 0.512(17) 1 d . U P C 1
H61A H 0.0673 0.5091 0.4188 0.088 Uiso 0.512(17) 1 calc R U P C 1
H61B H 0.1088 0.5662 0.4459 0.088 Uiso 0.512(17) 1 calc R U P C 1
C60A C 0.0421(13) 0.5928(8) 0.3613(10) 0.073(2) Uani 0.488(17) 1 d . U P C 2
H60C H -0.0284 0.5990 0.3437 0.088 Uiso 0.488(17) 1 calc R U P C 2
H60D H 0.0702 0.6146 0.4039 0.088 Uiso 0.488(17) 1 calc R U P C 2
C61A C 0.0658(14) 0.5339(8) 0.3768(12) 0.073(2) Uani 0.488(17) 1 d . U P C 2
H61C H 0.0248 0.5113 0.3391 0.088 Uiso 0.488(17) 1 calc R U P C 2
H61D H 0.0589 0.5233 0.4236 0.088 Uiso 0.488(17) 1 calc R U P C 2
C62 C 0.1757(5) 0.5331(3) 0.3766(4) 0.0693(19) Uani 1 1 d . . . . .
H62A H 0.2367 0.5387 0.4149 0.083 Uiso 0.70(4) 1 calc R U P B 1
H62B H 0.1749 0.4966 0.3601 0.083 Uiso 0.70(4) 1 calc R U P B 1
H62C H 0.2194 0.5463 0.4219 0.083 Uiso 0.30(4) 1 calc R U P B 2
H62D H 0.1964 0.4977 0.3673 0.083 Uiso 0.30(4) 1 calc R U P B 2
N1 N 0.1972(3) 0.75138(15) 0.1220(2) 0.0338(9) Uani 1 1 d . . . . .
N2 N 0.6538(3) 0.60400(17) 0.2374(2) 0.0385(9) Uani 1 1 d . . . . .
N3 N 0.2876(3) 0.47327(15) 0.2206(2) 0.0370(9) Uani 1 1 d . . . . .
Nd1 Nd 0.29137(2) 0.67314(2) 0.14216(2) 0.03352(7) Uani 1 1 d . . . . .
Nd2 Nd 0.51303(2) 0.63106(2) 0.26452(2) 0.03316(7) Uani 1 1 d . . . . .
Nd3 Nd 0.29259(2) 0.56340(2) 0.24458(2) 0.03567(7) Uani 1 1 d . . . . .
O1 O 0.3872(2) 0.60002(13) 0.18749(18) 0.0358(7) Uani 1 1 d . . . . .
O2 O 0.2965(3) 0.63732(16) 0.02386(19) 0.0473(9) Uani 1 1 d . . . . .
O3 O 0.5570(3) 0.69622(15) 0.3660(2) 0.0468(9) Uani 1 1 d . . . . .
O4 O 0.1713(3) 0.56835(15) 0.3176(2) 0.0530(10) Uani 1 1 d . . . . .
Si1 Si 0.18667(10) 0.80418(6) 0.17248(7) 0.0377(3) Uani 1 1 d . . . . .
Si2 Si 0.67478(11) 0.59136(6) 0.15767(8) 0.0441(3) Uani 1 1 d . . . . .
Si3 Si 0.34005(13) 0.44567(6) 0.16173(9) 0.0491(4) Uani 1 1 d . . . . .


_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
C2 Nd1 2.643(5) . ?
C2 Nd3 2.909(5) . ?
C3 Nd2 2.641(5) . ?
C3 Nd1 2.663(5) . ?
C4 Nd3 2.612(6) . ?
C4 Nd2 2.691(5) . ?
C5 Nd1 2.611(6) . ?
C5 Nd3 2.639(6) . ?
C6 Si1 1.870(6) . ?
C7 Si1 1.870(6) . ?
C8 Si1 1.871(6) . ?
C9 N1 1.413(6) . ?
C9 C10 1.418(7) . ?
C9 C14 1.431(7) . ?
C9 Nd1 3.020(5) . ?
C10 C11 1.381(7) . ?
C10 C18 1.530(7) . ?
C11 C12 1.379(8) . ?
C12 C13 1.381(8) . ?
C13 C14 1.378(7) . ?
C14 C15 1.520(7) . ?
C15 C17 1.516(8) . ?
C15 C16 1.530(7) . ?
C18 C20 1.513(8) . ?
C18 C19 1.517(9) . ?
C21 Si2 1.880(6) . ?
C22 Si2 1.865(7) . ?
C23 Si2 1.867(6) . ?
C24 N2 1.411(7) . ?
C24 C25 1.419(7) . ?
C24 C29 1.422(7) . ?
C24 Nd2 2.965(5) . ?
C25 C26 1.388(8) . ?
C25 C33 1.512(8) . ?
C26 C27 1.376(9) . ?
C27 C28 1.372(9) . ?
C28 C29 1.387(8) . ?
C29 C30 1.522(8) . ?
C30 C32 1.519(8) . ?
C30 C31 1.526(8) . ?
C33 C34 1.515(9) . ?
C33 C35 1.523(9) . ?
C36 Si3 1.867(7) . ?
C37 Si3 1.872(7) . ?
C38 Si3 1.869(7) . ?
C39 N3 1.415(6) . ?
C39 C40 1.415(8) . ?
C39 C44 1.418(9) . ?
C40 C41 1.385(10) . ?
C40 C48 1.513(12) . ?
C41 C42 1.354(13) . ?
C42 C43 1.378(13) . ?
C43 C44 1.394(9) . ?
C44 C45 1.521(9) . ?
C45 C47 1.522(9) . ?
C45 C46 1.529(10) . ?
C48 C50 1.507(11) . ?
C48 C49 1.512(10) . ?
C52 C53 1.421(16) . ?
C52 C51 1.468(13) . ?
C53 C54 1.544(14) . ?
C52A C53A 1.49(3) . ?
C52A C51 1.52(2) . ?
C53A C54 1.35(2) . ?
C51 O2 1.454(7) . ?
C54 O2 1.438(7) . ?
C55 O3 1.451(7) . ?
C55 C56 1.494(7) . ?
C56 C57 1.471(8) . ?
C56 C57A 1.512(10) . ?
C57 C58 1.501(8) . ?
C57A C58 1.494(10) . ?
C58 O3 1.432(8) . ?
C59 C60A 1.422(16) . ?
C59 O4 1.457(7) . ?
C59 C60 1.634(18) . ?
C60 C61 1.44(3) . ?
C61 C62 1.490(17) . ?
C60A C61A 1.56(3) . ?
C61A C62 1.592(19) . ?
C62 O4 1.457(8) . ?
N1 Si1 1.712(4) . ?
N1 Nd1 2.394(4) . ?
N2 Si2 1.711(4) . ?
N2 Nd2 2.356(4) . ?
N3 Si3 1.711(4) . ?
N3 Nd3 2.358(4) . ?
Nd1 O1 2.349(3) . ?
Nd1 O2 2.520(4) . ?
Nd1 Nd3 3.4590(4) . ?
Nd1 Nd2 3.5682(4) . ?
Nd2 O1 2.153(3) . ?
Nd2 O3 2.538(4) . ?
Nd2 Nd3 3.5514(4) . ?
Nd3 O1 2.216(3) . ?
Nd3 O4 2.574(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Nd1 C2 Nd3 76.91(12) . . ?
Nd2 C3 Nd1 84.57(15) . . ?
Nd3 C4 Nd2 84.08(15) . . ?
Nd1 C5 Nd3 82.43(16) . . ?
N1 C9 C10 121.1(4) . . ?
N1 C9 C14 121.0(4) . . ?
C10 C9 C14 117.9(4) . . ?
N1 C9 Nd1 50.9(2) . . ?
C10 C9 Nd1 104.9(3) . . ?
C14 C9 Nd1 111.9(3) . . ?
C11 C10 C9 120.0(5) . . ?
C11 C10 C18 118.6(5) . . ?
C9 C10 C18 121.4(5) . . ?
C12 C11 C10 121.7(5) . . ?
C11 C12 C13 118.9(5) . . ?
C14 C13 C12 122.1(5) . . ?
C13 C14 C9 119.4(5) . . ?
C13 C14 C15 118.8(5) . . ?
C9 C14 C15 121.6(4) . . ?
C17 C15 C14 114.9(5) . . ?
C17 C15 C16 108.6(5) . . ?
C14 C15 C16 108.3(4) . . ?
C20 C18 C19 109.2(5) . . ?
C20 C18 C10 111.9(5) . . ?
C19 C18 C10 111.3(5) . . ?
N2 C24 C25 122.0(5) . . ?
N2 C24 C29 119.6(5) . . ?
C25 C24 C29 118.3(5) . . ?
N2 C24 Nd2 51.3(2) . . ?
C25 C24 Nd2 112.4(3) . . ?
C29 C24 Nd2 102.2(3) . . ?
C26 C25 C24 119.1(5) . . ?
C26 C25 C33 119.1(5) . . ?
C24 C25 C33 121.8(5) . . ?
C27 C26 C25 122.4(6) . . ?
C28 C27 C26 118.7(6) . . ?
C27 C28 C29 121.9(6) . . ?
C28 C29 C24 119.6(5) . . ?
C28 C29 C30 119.8(5) . . ?
C24 C29 C30 120.5(5) . . ?
C32 C30 C29 109.6(5) . . ?
C32 C30 C31 109.9(5) . . ?
C29 C30 C31 114.7(5) . . ?
C25 C33 C34 112.7(5) . . ?
C25 C33 C35 112.0(6) . . ?
C34 C33 C35 109.6(5) . . ?
N3 C39 C40 120.5(6) . . ?
N3 C39 C44 121.6(5) . . ?
C40 C39 C44 117.8(5) . . ?
C41 C40 C39 119.6(7) . . ?
C41 C40 C48 118.7(7) . . ?
C39 C40 C48 121.7(6) . . ?
C42 C41 C40 122.3(8) . . ?
C41 C42 C43 119.6(7) . . ?
C42 C43 C44 120.8(8) . . ?
C43 C44 C39 119.9(7) . . ?
C43 C44 C45 118.0(7) . . ?
C39 C44 C45 122.0(5) . . ?
C44 C45 C47 110.8(6) . . ?
C44 C45 C46 112.6(6) . . ?
C47 C45 C46 110.7(6) . . ?
C50 C48 C49 108.6(6) . . ?
C50 C48 C40 113.4(7) . . ?
C49 C48 C40 113.8(8) . . ?
C53 C52 C51 107.9(9) . . ?
C52 C53 C54 106.8(9) . . ?
C53A C52A C51 105.7(17) . . ?
C54 C53A C52A 108.1(17) . . ?
O2 C51 C52 105.4(7) . . ?
O2 C51 C52A 105.8(10) . . ?
C53A C54 O2 113.0(12) . . ?
O2 C54 C53 102.0(6) . . ?
O3 C55 C56 107.0(5) . . ?
C57 C56 C55 103.0(7) . . ?
C55 C56 C57A 109.2(7) . . ?
C56 C57 C58 104.5(7) . . ?
C58 C57A C56 102.8(8) . . ?
O3 C58 C57A 111.4(8) . . ?
O3 C58 C57 101.9(8) . . ?
C60A C59 O4 110.0(9) . . ?
O4 C59 C60 98.5(8) . . ?
C61 C60 C59 105.1(13) . . ?
C60 C61 C62 101.2(13) . . ?
C59 C60A C61A 100.8(14) . . ?
C60A C61A C62 100.1(13) . . ?
O4 C62 C61 110.3(9) . . ?
O4 C62 C61A 100.5(9) . . ?
C9 N1 Si1 122.6(3) . . ?
C9 N1 Nd1 101.9(3) . . ?
Si1 N1 Nd1 135.3(2) . . ?
C24 N2 Si2 127.1(3) . . ?
C24 N2 Nd2 100.8(3) . . ?
Si2 N2 Nd2 131.2(2) . . ?
C39 N3 Si3 120.3(3) . . ?
C39 N3 Nd3 116.4(3) . . ?
Si3 N3 Nd3 123.2(2) . . ?
O1 Nd1 N1 167.80(12) . . ?
O1 Nd1 O2 83.41(12) . . ?
N1 Nd1 O2 108.79(13) . . ?
O1 Nd1 C5 79.03(15) . . ?
N1 Nd1 C5 101.46(16) . . ?
O2 Nd1 C5 85.23(17) . . ?
O1 Nd1 C2 76.97(13) . . ?
N1 Nd1 C2 90.96(14) . . ?
O2 Nd1 C2 158.64(13) . . ?
C5 Nd1 C2 82.84(18) . . ?
O1 Nd1 C3 78.73(13) . . ?
N1 Nd1 C3 98.76(14) . . ?
O2 Nd1 C3 99.30(14) . . ?
C5 Nd1 C3 156.61(17) . . ?
C2 Nd1 C3 85.20(16) . . ?
O1 Nd1 C9 164.26(12) . . ?
N1 Nd1 C9 27.25(13) . . ?
O2 Nd1 C9 82.35(12) . . ?
C5 Nd1 C9 93.10(16) . . ?
C2 Nd1 C9 115.88(14) . . ?
C3 Nd1 C9 110.21(14) . . ?
O1 Nd1 Nd3 39.31(8) . . ?
N1 Nd1 Nd3 133.28(9) . . ?
O2 Nd1 Nd3 104.04(9) . . ?
C5 Nd1 Nd3 49.14(13) . . ?
C2 Nd1 Nd3 55.00(10) . . ?
C3 Nd1 Nd3 107.79(11) . . ?
C9 Nd1 Nd3 139.81(9) . . ?
O1 Nd1 Nd2 35.68(8) . . ?
N1 Nd1 Nd2 136.18(10) . . ?
O2 Nd1 Nd2 104.38(8) . . ?
C5 Nd1 Nd2 109.17(13) . . ?
C2 Nd1 Nd2 63.49(11) . . ?
C3 Nd1 Nd2 47.45(11) . . ?
C9 Nd1 Nd2 157.06(10) . . ?
Nd3 Nd1 Nd2 60.691(7) . . ?
O1 Nd2 N2 109.99(14) . . ?
O1 Nd2 O3 139.76(12) . . ?
N2 Nd2 O3 109.68(14) . . ?
O1 Nd2 C3 82.71(14) . . ?
N2 Nd2 C3 101.34(15) . . ?
O3 Nd2 C3 83.30(15) . . ?
O1 Nd2 C4 81.88(15) . . ?
N2 Nd2 C4 118.09(16) . . ?
O3 Nd2 C4 85.46(15) . . ?
C3 Nd2 C4 140.50(16) . . ?
O1 Nd2 C24 135.30(13) . . ?
N2 Nd2 C24 27.87(14) . . ?
O3 Nd2 C24 84.87(13) . . ?
C3 Nd2 C24 111.69(15) . . ?
C4 Nd2 C24 104.81(15) . . ?
O1 Nd2 Nd3 36.20(9) . . ?
N2 Nd2 Nd3 129.70(11) . . ?
O3 Nd2 Nd3 114.87(9) . . ?
C3 Nd2 Nd3 105.77(11) . . ?
C4 Nd2 Nd3 47.01(12) . . ?
C24 Nd2 Nd3 139.48(10) . . ?
O1 Nd2 Nd1 39.53(9) . . ?
N2 Nd2 Nd1 127.12(10) . . ?
O3 Nd2 Nd1 107.46(9) . . ?
C3 Nd2 Nd1 47.98(11) . . ?
C4 Nd2 Nd1 100.98(12) . . ?
C24 Nd2 Nd1 152.23(10) . . ?
Nd3 Nd2 Nd1 58.134(7) . . ?
O1 Nd3 N3 107.61(13) . . ?
O1 Nd3 O4 152.06(12) . . ?
N3 Nd3 O4 100.01(13) . . ?
O1 Nd3 C4 82.59(15) . . ?
N3 Nd3 C4 102.13(16) . . ?
O4 Nd3 C4 95.85(16) . . ?
O1 Nd3 C5 80.77(15) . . ?
N3 Nd3 C5 103.88(17) . . ?
O4 Nd3 C5 88.76(17) . . ?
C4 Nd3 C5 152.35(17) . . ?
O1 Nd3 C2 73.46(12) . . ?
N3 Nd3 C2 178.40(14) . . ?
O4 Nd3 C2 79.00(13) . . ?
C4 Nd3 C2 76.76(16) . . ?
C5 Nd3 C2 77.40(16) . . ?
O1 Nd3 Nd1 42.19(8) . . ?
N3 Nd3 Nd1 133.49(10) . . ?
O4 Nd3 Nd1 113.30(9) . . ?
C4 Nd3 Nd1 105.55(12) . . ?
C5 Nd3 Nd1 48.43(12) . . ?
C2 Nd3 Nd1 48.09(9) . . ?
O1 Nd3 Nd2 35.02(9) . . ?
N3 Nd3 Nd2 118.42(9) . . ?
O4 Nd3 Nd2 130.59(10) . . ?
C4 Nd3 Nd2 48.91(12) . . ?
C5 Nd3 Nd2 108.95(12) . . ?
C2 Nd3 Nd2 61.75(10) . . ?
Nd1 Nd3 Nd2 61.175(8) . . ?
Nd2 O1 Nd3 108.78(14) . . ?
Nd2 O1 Nd1 104.80(13) . . ?
Nd3 O1 Nd1 98.50(12) . . ?
C54 O2 C51 107.1(4) . . ?
C54 O2 Nd1 125.3(3) . . ?
C51 O2 Nd1 126.0(3) . . ?
C58 O3 C55 108.3(4) . . ?
C58 O3 Nd2 121.5(3) . . ?
C55 O3 Nd2 129.9(3) . . ?
C59 O4 C62 108.9(5) . . ?
C59 O4 Nd3 128.8(4) . . ?
C62 O4 Nd3 122.3(3) . . ?
N1 Si1 C7 110.7(2) . . ?
N1 Si1 C6 113.1(3) . . ?
C7 Si1 C6 105.0(3) . . ?
N1 Si1 C8 112.8(2) . . ?
C7 Si1 C8 107.1(3) . . ?
C6 Si1 C8 107.7(3) . . ?
N2 Si2 C23 113.7(3) . . ?
N2 Si2 C22 108.8(3) . . ?
C23 Si2 C22 107.4(3) . . ?
N2 Si2 C21 114.3(3) . . ?
C23 Si2 C21 106.0(3) . . ?
C22 Si2 C21 106.2(3) . . ?
N3 Si3 C36 109.5(3) . . ?
N3 Si3 C38 112.9(3) . . ?
C36 Si3 C38 109.2(4) . . ?
N3 Si3 C37 111.6(3) . . ?
C36 Si3 C37 107.1(4) . . ?
C38 Si3 C37 106.4(4) . . ?

_refine_diff_density_max         0.958
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.088

_shelxl_version_number           2013-3


_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_Compound_9-Nd
_database_code_depnum_ccdc_archive 'CCDC 1410393'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;
#data_dr27_2015 

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H64 Al N2 Nd Si2'
_chemical_formula_sum            'C34 H64 Al N2 Nd Si2'
_chemical_formula_weight         728.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   17.9545(6)
_cell_length_b                   17.8184(6)
_cell_length_c                   12.2373(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.82
_cell_angle_gamma                90
_cell_volume                     3801.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9459
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      30.52

_exptl_crystal_description       'irregular prism'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_F_000             1532
_exptl_transmission_factor_min   0.5852
_exptl_transmission_factor_max   0.7943
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    1.475
_shelx_estimated_absorpt_T_min   0.471
_shelx_estimated_absorpt_T_max   0.666
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.60230
_exptl_absorpt_correction_T_max  0.74589
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker TXS Rotating anode'
_diffrn_measurement_device_type  'Bruker Pt135 APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32073
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.157
_diffrn_reflns_theta_max         30.516
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5809
_reflns_number_gt                5723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0204P)²+1.8903P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5809
_refine_ls_number_parameters     199
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0141
_refine_ls_wR_factor_ref         0.0391
_refine_ls_wR_factor_gt          0.0389
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.0000 0.23422(2) 0.7500 0.01399(2) Uani 1 2 d S T P . .
Al1 Al 0.0000 0.05294(2) 0.7500 0.02155(8) Uani 1 2 d S T P . .
Si1 Si 0.15998(2) 0.37686(2) 0.74622(2) 0.01796(5) Uani 1 1 d . . . . .
N1 N 0.10082(4) 0.29930(4) 0.71037(6) 0.01550(13) Uani 1 1 d . . . . .
C1 C 0.09766(5) 0.25682(5) 0.61085(8) 0.01575(15) Uani 1 1 d . . . . .
C2 C 0.03697(6) 0.26963(5) 0.51399(8) 0.01938(17) Uani 1 1 d . . . . .
C3 C 0.02810(6) 0.22210(7) 0.42040(9) 0.02420(19) Uani 1 1 d . . . . .
H3A H -0.0128 0.2307 0.3564 0.029 Uiso 1 1 calc R U . . .
C4 C 0.07761(6) 0.16320(6) 0.41964(9) 0.0251(2) Uani 1 1 d . . . . .
H4A H 0.0705 0.1311 0.3560 0.030 Uiso 1 1 calc R U . . .
C5 C 0.13806(6) 0.15103(6) 0.51286(9) 0.02294(18) Uani 1 1 d . . . . .
H5A H 0.1724 0.1107 0.5115 0.028 Uiso 1 1 calc R U . . .
C6 C 0.14959(5) 0.19649(5) 0.60822(8) 0.01784(16) Uani 1 1 d . . . . .
C7 C -0.01725(6) 0.33611(6) 0.50578(9) 0.02511(19) Uani 1 1 d . . . . .
H7A H -0.0019 0.3653 0.5774 0.030 Uiso 1 1 calc R U . . .
C8 C -0.01191(8) 0.38859(8) 0.40809(13) 0.0420(3) Uani 1 1 d . . . . .
H8A H 0.0419 0.4018 0.4139 0.063 Uiso 1 1 calc R U . . .
H8B H -0.0416 0.4343 0.4118 0.063 Uiso 1 1 calc R U . . .
H8C H -0.0326 0.3631 0.3363 0.063 Uiso 1 1 calc R U . . .
C9 C -0.10093(6) 0.31123(7) 0.49128(9) 0.0285(2) Uani 1 1 d . . . . .
H9A H -0.1065 0.2855 0.5597 0.043 Uiso 1 1 calc R U . . .
H9B H -0.1152 0.2770 0.4270 0.043 Uiso 1 1 calc R U . . .
H9C H -0.1345 0.3553 0.4779 0.043 Uiso 1 1 calc R U . . .
C10 C 0.22116(5) 0.18497(5) 0.70232(8) 0.01994(17) Uani 1 1 d . . . . .
H10A H 0.2150 0.2145 0.7691 0.024 Uiso 1 1 calc R U . . .
C11 C 0.23583(7) 0.10306(6) 0.73885(11) 0.0301(2) Uani 1 1 d . . . . .
H11A H 0.1917 0.0837 0.7642 0.045 Uiso 1 1 calc R U . . .
H11B H 0.2819 0.1000 0.8006 0.045 Uiso 1 1 calc R U . . .
H11C H 0.2432 0.0731 0.6751 0.045 Uiso 1 1 calc R U . . .
C12 C 0.29069(6) 0.21637(8) 0.66483(10) 0.0291(2) Uani 1 1 d . . . . .
H12A H 0.2812 0.2690 0.6423 0.044 Uiso 1 1 calc R U . . .
H12B H 0.2989 0.1871 0.6009 0.044 Uiso 1 1 calc R U . . .
H12C H 0.3363 0.2131 0.7273 0.044 Uiso 1 1 calc R U . . .
C13 C 0.10813(6) 0.45317(6) 0.80322(10) 0.02483(19) Uani 1 1 d . . . . .
H13A H 0.0638 0.4696 0.7446 0.037 Uiso 1 1 calc R U . . .
H13B H 0.1429 0.4957 0.8269 0.037 Uiso 1 1 calc R U . . .
H13C H 0.0906 0.4341 0.8679 0.037 Uiso 1 1 calc R U . . .
C14 C 0.18749(7) 0.41586(6) 0.61911(10) 0.0293(2) Uani 1 1 d . . . . .
H14A H 0.1432 0.4413 0.5709 0.044 Uiso 1 1 calc R U . . .
H14B H 0.2041 0.3749 0.5771 0.044 Uiso 1 1 calc R U . . .
H14C H 0.2295 0.4518 0.6429 0.044 Uiso 1 1 calc R U . . .
C15 C 0.25075(6) 0.35816(7) 0.85614(10) 0.0288(2) Uani 1 1 d . . . . .
H15A H 0.2391 0.3277 0.9166 0.043 Uiso 1 1 calc R U . . .
H15B H 0.2735 0.4059 0.8871 0.043 Uiso 1 1 calc R U . . .
H15C H 0.2870 0.3311 0.8220 0.043 Uiso 1 1 calc R U . . .
C16 C 0.06822(6) 0.11991(6) 0.87259(9) 0.02491(19) Uani 1 1 d D . . . .
H16A H 0.1099(8) 0.1510(8) 0.8608(13) 0.037 Uiso 1 1 d D U . . .
H16B H 0.0928(9) 0.0755(7) 0.9161(13) 0.037 Uiso 1 1 d D U . . .
H16C H 0.0427(8) 0.1462(8) 0.9236(13) 0.037 Uiso 1 1 d D U . . .
C17 C -0.06358(7) -0.00702(6) 0.82945(12) 0.0324(2) Uani 1 1 d . . . . .
H17A H -0.1044 -0.0322 0.7742 0.049 Uiso 1 1 calc R U . . .
H17B H -0.0863 0.0262 0.8765 0.049 Uiso 1 1 calc R U . . .
H17C H -0.0314 -0.0446 0.8770 0.049 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 N1 2.2968(8) 2_556 ?
Nd1 N1 2.2969(8) . ?
Nd1 C16 2.6498(10) 2_556 ?
Nd1 C16 2.6498(10) . ?
Nd1 C1 2.7502(9) . ?
Nd1 C1 2.7502(9) 2_556 ?
Nd1 Al1 3.2302(4) . ?
Nd1 H16A 2.579(16) . ?
Nd1 H16C 2.604(16) . ?
Al1 C17 1.9799(11) 2_556 ?
Al1 C17 1.9799(11) . ?
Al1 C16 2.0729(11) 2_556 ?
Al1 C16 2.0729(11) . ?
Si1 N1 1.7344(8) . ?
Si1 C13 1.8741(11) . ?
Si1 C14 1.8746(11) . ?
Si1 C15 1.8784(12) . ?
N1 C1 1.4234(11) . ?
C1 C2 1.4238(13) . ?
C1 C6 1.4285(13) . ?
C2 C3 1.4025(14) . ?
C2 C7 1.5211(15) . ?
C3 C4 1.3769(16) . ?
C3 H3A 0.9500 . ?
C4 C5 1.3909(16) . ?
C4 H4A 0.9500 . ?
C5 C6 1.3948(13) . ?
C5 H5A 0.9500 . ?
C6 C10 1.5206(13) . ?
C7 C9 1.5356(16) . ?
C7 C8 1.5387(17) . ?
C7 H7A 1.0000 . ?
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 C11 1.5307(15) . ?
C10 C12 1.5349(14) . ?
C10 H10A 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.968(12) . ?
C16 H16B 0.997(11) . ?
C16 H16C 0.978(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 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
N1 Nd1 N1 119.36(4) 2_556 . ?
N1 Nd1 C16 103.10(3) 2_556 2_556 ?
N1 Nd1 C16 123.33(3) . 2_556 ?
N1 Nd1 C16 123.33(3) 2_556 . ?
N1 Nd1 C16 103.10(3) . . ?
C16 Nd1 C16 79.53(5) 2_556 . ?
N1 Nd1 C1 135.08(3) 2_556 . ?
N1 Nd1 C1 31.14(3) . . ?
C16 Nd1 C1 92.23(3) 2_556 . ?
C16 Nd1 C1 100.73(3) . . ?
N1 Nd1 C1 31.14(3) 2_556 2_556 ?
N1 Nd1 C1 135.08(3) . 2_556 ?
C16 Nd1 C1 100.73(3) 2_556 2_556 ?
C16 Nd1 C1 92.23(3) . 2_556 ?
C1 Nd1 C1 163.16(4) . 2_556 ?
N1 Nd1 Al1 120.318(19) 2_556 . ?
N1 Nd1 Al1 120.318(19) . . ?
C16 Nd1 Al1 39.76(2) 2_556 . ?
C16 Nd1 Al1 39.76(2) . . ?
C1 Nd1 Al1 98.420(19) . . ?
C1 Nd1 Al1 98.419(19) 2_556 . ?
N1 Nd1 H16A 136.2(3) 2_556 . ?
N1 Nd1 H16A 81.9(3) . . ?
C16 Nd1 H16A 92.7(3) 2_556 . ?
C16 Nd1 H16A 21.3(3) . . ?
C1 Nd1 H16A 83.6(3) . . ?
C1 Nd1 H16A 106.2(3) 2_556 . ?
Al1 Nd1 H16A 54.9(3) . . ?
N1 Nd1 H16C 103.0(3) 2_556 . ?
N1 Nd1 H16C 112.5(3) . . ?
C16 Nd1 H16C 90.3(3) 2_556 . ?
C16 Nd1 H16C 21.4(3) . . ?
C1 Nd1 H16C 119.1(3) . . ?
C1 Nd1 H16C 71.9(3) 2_556 . ?
Al1 Nd1 H16C 53.0(3) . . ?
H16A Nd1 H16C 35.5(3) . . ?
C17 Al1 C17 114.69(7) 2_556 . ?
C17 Al1 C16 105.40(5) 2_556 2_556 ?
C17 Al1 C16 110.84(5) . 2_556 ?
C17 Al1 C16 110.84(5) 2_556 . ?
C17 Al1 C16 105.40(5) . . ?
C16 Al1 C16 109.70(6) 2_556 . ?
C17 Al1 Nd1 122.66(3) 2_556 . ?
C17 Al1 Nd1 122.66(3) . . ?
C16 Al1 Nd1 54.85(3) 2_556 . ?
C16 Al1 Nd1 54.85(3) . . ?
N1 Si1 C13 110.10(4) . . ?
N1 Si1 C14 110.63(4) . . ?
C13 Si1 C14 107.02(5) . . ?
N1 Si1 C15 114.45(5) . . ?
C13 Si1 C15 106.58(5) . . ?
C14 Si1 C15 107.72(6) . . ?
C1 N1 Si1 122.47(6) . . ?
C1 N1 Nd1 92.29(5) . . ?
Si1 N1 Nd1 144.56(4) . . ?
N1 C1 C2 119.54(8) . . ?
N1 C1 C6 121.78(8) . . ?
C2 C1 C6 118.41(8) . . ?
N1 C1 Nd1 56.56(4) . . ?
C2 C1 Nd1 93.70(6) . . ?
C6 C1 Nd1 114.83(6) . . ?
C3 C2 C1 119.86(9) . . ?
C3 C2 C7 118.05(9) . . ?
C1 C2 C7 122.02(9) . . ?
C4 C3 C2 121.22(10) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C3 C4 C5 119.46(9) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 C6 121.77(10) . . ?
C4 C5 H5A 119.1 . . ?
C6 C5 H5A 119.1 . . ?
C5 C6 C1 119.25(9) . . ?
C5 C6 C10 119.00(9) . . ?
C1 C6 C10 121.51(8) . . ?
C2 C7 C9 112.08(9) . . ?
C2 C7 C8 111.52(10) . . ?
C9 C7 C8 109.06(9) . . ?
C2 C7 H7A 108.0 . . ?
C9 C7 H7A 108.0 . . ?
C8 C7 H7A 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C11 113.90(8) . . ?
C6 C10 C12 108.96(8) . . ?
C11 C10 C12 109.85(9) . . ?
C6 C10 H10A 108.0 . . ?
C11 C10 H10A 108.0 . . ?
C12 C10 H10A 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Al1 C16 Nd1 85.38(4) . . ?
Al1 C16 H16A 124.4(10) . . ?
Nd1 C16 H16A 75.2(9) . . ?
Al1 C16 H16B 92.2(9) . . ?
Nd1 C16 H16B 177.6(10) . . ?
H16A C16 H16B 105.9(12) . . ?
Al1 C16 H16C 116.8(10) . . ?
Nd1 C16 H16C 76.7(9) . . ?
H16A C16 H16C 108.5(12) . . ?
H16B C16 H16C 104.8(11) . . ?
Al1 C17 H17A 109.5 . . ?
Al1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Al1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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
C13 Si1 N1 C1 139.00(8) . . . . ?
C14 Si1 N1 C1 20.91(9) . . . . ?
C15 Si1 N1 C1 -100.99(8) . . . . ?
C13 Si1 N1 Nd1 -28.42(9) . . . . ?
C14 Si1 N1 Nd1 -146.50(8) . . . . ?
C15 Si1 N1 Nd1 91.59(8) . . . . ?
Si1 N1 C1 C2 -99.31(9) . . . . ?
Nd1 N1 C1 C2 73.42(8) . . . . ?
Si1 N1 C1 C6 86.73(10) . . . . ?
Nd1 N1 C1 C6 -100.54(8) . . . . ?
Si1 N1 C1 Nd1 -172.74(8) . . . . ?
N1 C1 C2 C3 -172.32(9) . . . . ?
C6 C1 C2 C3 1.84(14) . . . . ?
Nd1 C1 C2 C3 -119.05(9) . . . . ?
N1 C1 C2 C7 10.65(14) . . . . ?
C6 C1 C2 C7 -175.19(9) . . . . ?
Nd1 C1 C2 C7 63.92(9) . . . . ?
C1 C2 C3 C4 -0.61(15) . . . . ?
C7 C2 C3 C4 176.54(10) . . . . ?
C2 C3 C4 C5 -0.70(16) . . . . ?
C3 C4 C5 C6 0.74(15) . . . . ?
C4 C5 C6 C1 0.53(14) . . . . ?
C4 C5 C6 C10 -173.98(9) . . . . ?
N1 C1 C6 C5 172.23(8) . . . . ?
C2 C1 C6 C5 -1.80(13) . . . . ?
Nd1 C1 C6 C5 107.54(9) . . . . ?
N1 C1 C6 C10 -13.41(13) . . . . ?
C2 C1 C6 C10 172.57(8) . . . . ?
Nd1 C1 C6 C10 -78.09(9) . . . . ?
C3 C2 C7 C9 63.69(12) . . . . ?
C1 C2 C7 C9 -119.23(10) . . . . ?
C3 C2 C7 C8 -58.91(13) . . . . ?
C1 C2 C7 C8 118.17(11) . . . . ?
C5 C6 C10 C11 -48.95(12) . . . . ?
C1 C6 C10 C11 136.67(9) . . . . ?
C5 C6 C10 C12 74.06(11) . . . . ?
C1 C6 C10 C12 -100.32(10) . . . . ?

_refine_diff_density_max         0.835
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.055


_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_Compound_9-La
_database_code_depnum_ccdc_archive 'CCDC 1410394'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;
#data_DR29twin_a

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H64 Al La N2 Si2'
_chemical_formula_sum            'C34 H64 Al La N2 Si2'
_chemical_formula_weight         722.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   18.0563(11)
_cell_length_b                   17.8725(11)
_cell_length_c                   12.2151(8)
_cell_angle_alpha                90
_cell_angle_beta                 104.1330(10)
_cell_angle_gamma                90
_cell_volume                     3822.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9995
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      30.06
_exptl_crystal_description       'irregular prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   0.398050
_exptl_transmission_factor_max   0.745986
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    1.226
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'TWINABS. Ver. 2012/1. (Sheldrick, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker TXS Rotating anode'
_diffrn_measurement_device_type  'Bruker Pt135 APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5606
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.628
_diffrn_reflns_theta_max         30.062
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5606
_reflns_number_gt                5204
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_vrf_PLAT971_Compound_9-La       
;
PROBLEM: Check Calcd Residual Density  0.90A From      N1       0.67 eA-3  
RESPONSE: The crystal is distinct trilling. 
          Unevitably, some ghost residual density is present, 
          in particular close to the La metal centre.
          This may also cause the other Alerts.  
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
The crystal is distinct trilling which was indexed using Cell_Now and 
then integrated using all three components. 
The major component was extracted, using all single and composite reflections.
Unevitably, some ghost residual density is present, in particular close to the La metal centre. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+35.7303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5606
_refine_ls_number_parameters     199
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.0000 0.23508(2) 0.7500 0.01493(7) Uani 1 2 d S T P . .
Al1 Al 0.0000 0.05069(8) 0.7500 0.0211(3) Uani 1 2 d S T P . .
Si1 Si 0.16122(5) 0.37869(5) 0.74506(8) 0.01803(18) Uani 1 1 d . . . . .
N1 N 0.10280(15) 0.30107(15) 0.7087(2) 0.0157(5) Uani 1 1 d . . . . .
C1 C 0.09862(18) 0.25844(18) 0.6094(3) 0.0162(5) Uani 1 1 d . . . . .
C2 C 0.03629(19) 0.27039(19) 0.5130(3) 0.0193(6) Uani 1 1 d . . . . .
C3 C 0.0269(2) 0.2226(2) 0.4196(3) 0.0240(7) Uani 1 1 d . . . . .
H3A H -0.0144 0.2309 0.3557 0.029 Uiso 1 1 calc R U . . .
C4 C 0.0760(2) 0.1642(2) 0.4181(3) 0.0247(7) Uani 1 1 d . . . . .
H4A H 0.0684 0.1321 0.3543 0.030 Uiso 1 1 calc R U . . .
C5 C 0.1370(2) 0.1523(2) 0.5109(3) 0.0230(7) Uani 1 1 d . . . . .
H5A H 0.1710 0.1120 0.5093 0.028 Uiso 1 1 calc R U . . .
C6 C 0.14966(19) 0.19809(18) 0.6062(3) 0.0179(6) Uani 1 1 d . . . . .
C7 C -0.0181(2) 0.3358(2) 0.5061(3) 0.0252(7) Uani 1 1 d . . . . .
H7A H -0.0030 0.3641 0.5787 0.030 Uiso 1 1 calc R U . . .
C8 C -0.0126(3) 0.3895(3) 0.4098(4) 0.0405(10) Uani 1 1 d . . . . .
H8A H 0.0409 0.4036 0.4174 0.061 Uiso 1 1 calc R U . . .
H8B H -0.0429 0.4345 0.4137 0.061 Uiso 1 1 calc R U . . .
H8C H -0.0323 0.3646 0.3370 0.061 Uiso 1 1 calc R U . . .
C9 C -0.1015(2) 0.3107(2) 0.4899(3) 0.0283(8) Uani 1 1 d . . . . .
H9A H -0.1072 0.2843 0.5577 0.042 Uiso 1 1 calc R U . . .
H9B H -0.1156 0.2772 0.4247 0.042 Uiso 1 1 calc R U . . .
H9C H -0.1350 0.3547 0.4771 0.042 Uiso 1 1 calc R U . . .
C10 C 0.22148(19) 0.18655(19) 0.7006(3) 0.0199(6) Uani 1 1 d . . . . .
H10A H 0.2157 0.2156 0.7680 0.024 Uiso 1 1 calc R U . . .
C11 C 0.2363(2) 0.1047(2) 0.7359(4) 0.0296(8) Uani 1 1 d . . . . .
H11A H 0.1922 0.0847 0.7596 0.044 Uiso 1 1 calc R U . . .
H11B H 0.2818 0.1014 0.7987 0.044 Uiso 1 1 calc R U . . .
H11C H 0.2444 0.0756 0.6718 0.044 Uiso 1 1 calc R U . . .
C12 C 0.2904(2) 0.2182(2) 0.6627(3) 0.0280(8) Uani 1 1 d . . . . .
H12A H 0.2811 0.2709 0.6416 0.042 Uiso 1 1 calc R U . . .
H12B H 0.2977 0.1898 0.5976 0.042 Uiso 1 1 calc R U . . .
H12C H 0.3363 0.2141 0.7248 0.042 Uiso 1 1 calc R U . . .
C13 C 0.1087(2) 0.4536(2) 0.8025(3) 0.0246(7) Uani 1 1 d . . . . .
H13A H 0.0629 0.4679 0.7449 0.037 Uiso 1 1 calc R U . . .
H13B H 0.1419 0.4974 0.8231 0.037 Uiso 1 1 calc R U . . .
H13C H 0.0939 0.4348 0.8694 0.037 Uiso 1 1 calc R U . . .
C14 C 0.1883(2) 0.4183(2) 0.6181(3) 0.0284(8) Uani 1 1 d . . . . .
H14A H 0.1435 0.4419 0.5684 0.043 Uiso 1 1 calc R U . . .
H14B H 0.2069 0.3780 0.5774 0.043 Uiso 1 1 calc R U . . .
H14C H 0.2286 0.4557 0.6423 0.043 Uiso 1 1 calc R U . . .
C15 C 0.2517(2) 0.3601(2) 0.8559(3) 0.0284(8) Uani 1 1 d . . . . .
H15A H 0.2401 0.3299 0.9166 0.043 Uiso 1 1 calc R U . . .
H15B H 0.2745 0.4078 0.8869 0.043 Uiso 1 1 calc R U . . .
H15C H 0.2878 0.3330 0.8221 0.043 Uiso 1 1 calc R U . . .
C16 C 0.0681(2) 0.1165(2) 0.8743(3) 0.0263(7) Uani 1 1 d D . . . .
H16A H 0.1085(19) 0.1465(19) 0.857(4) 0.039 Uiso 1 1 d D U . . .
H16B H 0.091(2) 0.0706(15) 0.914(4) 0.039 Uiso 1 1 d D U . . .
H16C H 0.043(2) 0.144(2) 0.925(3) 0.039 Uiso 1 1 d D U . . .
C17 C -0.0645(2) -0.0083(2) 0.8278(4) 0.0324(9) Uani 1 1 d . . . . .
H17A H -0.1058 -0.0324 0.7717 0.049 Uiso 1 1 calc R U . . .
H17B H -0.0864 0.0249 0.8755 0.049 Uiso 1 1 calc R U . . .
H17C H -0.0333 -0.0467 0.8749 0.049 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 N1 2.356(3) 2_556 ?
La1 N1 2.356(3) . ?
La1 C16 2.719(4) . ?
La1 C16 2.719(4) 2_556 ?
La1 C1 2.791(3) . ?
La1 C1 2.791(3) 2_556 ?
La1 Al1 3.2955(15) . ?
La1 H16A 2.61(4) . ?
La1 H16C 2.65(4) . ?
Al1 C17 1.978(4) . ?
Al1 C17 1.979(4) 2_556 ?
Al1 C16 2.072(4) 2_556 ?
Al1 C16 2.072(4) . ?
Si1 N1 1.734(3) . ?
Si1 C13 1.873(4) . ?
Si1 C14 1.875(4) . ?
Si1 C15 1.880(4) . ?
N1 C1 1.419(4) . ?
C1 C6 1.425(5) . ?
C1 C2 1.432(4) . ?
C2 C3 1.402(5) . ?
C2 C7 1.515(5) . ?
C3 C4 1.373(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.390(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.395(4) . ?
C5 H5A 0.9500 . ?
C6 C10 1.524(5) . ?
C7 C9 1.537(5) . ?
C7 C8 1.540(6) . ?
C7 H7A 1.0000 . ?
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 C11 1.530(5) . ?
C10 C12 1.537(5) . ?
C10 H10A 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.971(17) . ?
C16 H16B 0.989(17) . ?
C16 H16C 0.981(17) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 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
N1 La1 N1 119.91(13) 2_556 . ?
N1 La1 C16 122.88(11) 2_556 . ?
N1 La1 C16 103.73(11) . . ?
N1 La1 C16 103.73(11) 2_556 2_556 ?
N1 La1 C16 122.88(10) . 2_556 ?
C16 La1 C16 77.65(16) . 2_556 ?
N1 La1 C1 135.36(9) 2_556 . ?
N1 La1 C1 30.53(9) . . ?
C16 La1 C1 101.01(11) . . ?
C16 La1 C1 92.42(10) 2_556 . ?
N1 La1 C1 30.53(9) 2_556 2_556 ?
N1 La1 C1 135.36(9) . 2_556 ?
C16 La1 C1 92.42(11) . 2_556 ?
C16 La1 C1 101.00(11) 2_556 2_556 ?
C1 La1 C1 162.79(13) . 2_556 ?
N1 La1 Al1 120.05(7) 2_556 . ?
N1 La1 Al1 120.05(7) . . ?
C16 La1 Al1 38.83(8) . . ?
C16 La1 Al1 38.83(8) 2_556 . ?
C1 La1 Al1 98.60(7) . . ?
C1 La1 Al1 98.60(7) 2_556 . ?
N1 La1 H16A 137.1(8) 2_556 . ?
N1 La1 H16A 82.9(4) . . ?
C16 La1 H16A 20.9(4) . . ?
C16 La1 H16A 89.3(9) 2_556 . ?
C1 La1 H16A 83.3(6) . . ?
C1 La1 H16A 107.3(7) 2_556 . ?
Al1 La1 H16A 52.6(8) . . ?
N1 La1 H16C 103.1(4) 2_556 . ?
N1 La1 H16C 112.8(9) . . ?
C16 La1 H16C 21.0(4) . . ?
C16 La1 H16C 88.7(9) 2_556 . ?
C1 La1 H16C 118.8(6) . . ?
C1 La1 H16C 72.7(5) 2_556 . ?
Al1 La1 H16C 52.1(8) . . ?
H16A La1 H16C 35.5(5) . . ?
C17 Al1 C17 115.6(2) . 2_556 ?
C17 Al1 C16 109.96(17) . 2_556 ?
C17 Al1 C16 105.32(18) 2_556 2_556 ?
C17 Al1 C16 105.32(18) . . ?
C17 Al1 C16 109.96(17) 2_556 . ?
C16 Al1 C16 110.8(2) 2_556 . ?
C17 Al1 La1 122.21(12) . . ?
C17 Al1 La1 122.21(12) 2_556 . ?
C16 Al1 La1 55.38(11) 2_556 . ?
C16 Al1 La1 55.38(11) . . ?
N1 Si1 C13 109.65(15) . . ?
N1 Si1 C14 110.82(15) . . ?
C13 Si1 C14 107.31(18) . . ?
N1 Si1 C15 114.27(16) . . ?
C13 Si1 C15 106.66(18) . . ?
C14 Si1 C15 107.82(19) . . ?
C1 N1 Si1 123.4(2) . . ?
C1 N1 La1 91.95(18) . . ?
Si1 N1 La1 143.87(15) . . ?
N1 C1 C6 122.0(3) . . ?
N1 C1 C2 119.3(3) . . ?
C6 C1 C2 118.3(3) . . ?
N1 C1 La1 57.52(15) . . ?
C6 C1 La1 114.7(2) . . ?
C2 C1 La1 92.12(19) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 C7 118.5(3) . . ?
C1 C2 C7 121.9(3) . . ?
C4 C3 C2 121.6(3) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 C6 121.8(3) . . ?
C4 C5 H5A 119.1 . . ?
C6 C5 H5A 119.1 . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C10 119.2(3) . . ?
C1 C6 C10 121.2(3) . . ?
C2 C7 C9 112.6(3) . . ?
C2 C7 C8 111.2(3) . . ?
C9 C7 C8 109.1(3) . . ?
C2 C7 H7A 107.9 . . ?
C9 C7 H7A 107.9 . . ?
C8 C7 H7A 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C11 113.6(3) . . ?
C6 C10 C12 108.9(3) . . ?
C11 C10 C12 109.7(3) . . ?
C6 C10 H10A 108.2 . . ?
C11 C10 H10A 108.1 . . ?
C12 C10 H10A 108.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Al1 C16 La1 85.79(13) . . ?
Al1 C16 H16A 120(3) . . ?
La1 C16 H16A 73(2) . . ?
Al1 C16 H16B 89(3) . . ?
La1 C16 H16B 175(3) . . ?
H16A C16 H16B 108(2) . . ?
Al1 C16 H16C 118(3) . . ?
La1 C16 H16C 76(2) . . ?
H16A C16 H16C 110(2) . . ?
H16B C16 H16C 108(2) . . ?
Al1 C17 H17A 109.5 . . ?
Al1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Al1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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
C13 Si1 N1 C1 139.0(3) . . . . ?
C14 Si1 N1 C1 20.7(3) . . . . ?
C15 Si1 N1 C1 -101.4(3) . . . . ?
C13 Si1 N1 La1 -27.8(3) . . . . ?
C14 Si1 N1 La1 -146.1(3) . . . . ?
C15 Si1 N1 La1 91.8(3) . . . . ?
Si1 N1 C1 C6 87.1(3) . . . . ?
La1 N1 C1 C6 -100.7(3) . . . . ?
Si1 N1 C1 C2 -100.1(3) . . . . ?
La1 N1 C1 C2 72.1(3) . . . . ?
Si1 N1 C1 La1 -172.2(3) . . . . ?
N1 C1 C2 C3 -172.6(3) . . . . ?
C6 C1 C2 C3 0.5(5) . . . . ?
La1 C1 C2 C3 -119.1(3) . . . . ?
N1 C1 C2 C7 10.5(5) . . . . ?
C6 C1 C2 C7 -176.4(3) . . . . ?
La1 C1 C2 C7 63.9(3) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
C7 C2 C3 C4 177.3(3) . . . . ?
C2 C3 C4 C5 -0.7(5) . . . . ?
C3 C4 C5 C6 0.4(5) . . . . ?
C4 C5 C6 C1 0.3(5) . . . . ?
C4 C5 C6 C10 -174.5(3) . . . . ?
N1 C1 C6 C5 172.1(3) . . . . ?
C2 C1 C6 C5 -0.8(5) . . . . ?
La1 C1 C6 C5 106.3(3) . . . . ?
N1 C1 C6 C10 -13.1(5) . . . . ?
C2 C1 C6 C10 174.0(3) . . . . ?
La1 C1 C6 C10 -78.9(3) . . . . ?
C3 C2 C7 C9 61.7(4) . . . . ?
C1 C2 C7 C9 -121.3(3) . . . . ?
C3 C2 C7 C8 -61.1(4) . . . . ?
C1 C2 C7 C8 115.9(4) . . . . ?
C5 C6 C10 C11 -47.7(4) . . . . ?
C1 C6 C10 C11 137.6(3) . . . . ?
C5 C6 C10 C12 75.0(4) . . . . ?
C1 C6 C10 C12 -99.8(4) . . . . ?

_refine_diff_density_max         3.402
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.134


_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
