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

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

data_sh4615_a
_database_code_depnum_ccdc_archive 'CCDC 2154213'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Saarland University
Germany
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'lithium diisopropyl indenide dimethoxyethan adduct'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H29 Li O2'
_chemical_formula_sum            'C19 H29 Li O2'
_chemical_formula_weight         296.36

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'
Li Li -0.0003 0.0001 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   8.1149(10)
_cell_length_b                   9.9608(11)
_cell_length_c                   12.9882(16)
_cell_angle_alpha                73.834(4)
_cell_angle_beta                 74.958(4)
_cell_angle_gamma                66.433(4)
_cell_volume                     911.04(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    5392
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.13

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_F_000             324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    0.067
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24467
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.537
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             3309
_reflns_number_gt                2535
_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       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0715P)²+0.5576P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3309
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1645
_refine_ls_wR_factor_gt          0.1505
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
Li1 Li 0.5036(5) 0.2474(5) 0.2679(3) 0.0314(9) Uani 1 1 d . . . . .
O1 O 0.74654(19) 0.10239(19) 0.22625(13) 0.0334(4) Uani 1 1 d . . . . .
O2 O 0.6459(2) 0.35609(19) 0.29065(13) 0.0340(4) Uani 1 1 d . . . . .
C2 C 0.2341(3) 0.3758(3) 0.20398(16) 0.0247(5) Uani 1 1 d . . . . .
C1 C 0.2057(3) 0.3807(3) 0.31535(17) 0.0242(5) Uani 1 1 d . . . . .
H1 H 0.168(3) 0.473(3) 0.3429(18) 0.029 Uiso 1 1 d . U . . .
C3 C 0.2824(3) 0.2241(3) 0.19899(16) 0.0241(5) Uani 1 1 d . . . . .
C4 C 0.3231(3) 0.1487(3) 0.11219(18) 0.0291(5) Uani 1 1 d . . . . .
H4 H 0.323958 0.203221 0.039394 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3610(3) -0.0026(3) 0.13341(19) 0.0328(6) Uani 1 1 d . . . . .
H5 H 0.385393 -0.051562 0.075036 0.039 Uiso 1 1 calc R U . . .
C6 C 0.3643(3) -0.0865(3) 0.2404(2) 0.0339(5) Uani 1 1 d . . . . .
H6 H 0.391638 -0.191157 0.252907 0.041 Uiso 1 1 calc R U . . .
C7 C 0.3288(3) -0.0198(3) 0.32700(19) 0.0301(5) Uani 1 1 d . . . . .
H7 H 0.332722 -0.078267 0.398533 0.036 Uiso 1 1 calc R U . . .
C8 C 0.2866(3) 0.1358(3) 0.30949(17) 0.0255(5) Uani 1 1 d . . . . .
C10 C 0.2177(3) 0.1934(3) 0.50365(17) 0.0289(5) Uani 1 1 d . . . . .
H10 H 0.305888 0.089914 0.523542 0.035 Uiso 1 1 calc R U . . .
C9 C 0.2408(3) 0.2353(3) 0.38084(16) 0.0247(5) Uani 1 1 d . . . . .
C11 C 0.2588(3) 0.2960(3) 0.55280(19) 0.0389(6) Uani 1 1 d . . . . .
H11A H 0.383850 0.293264 0.523151 0.058 Uiso 1 1 calc R U . . .
H11B H 0.245566 0.262525 0.631967 0.058 Uiso 1 1 calc R U . . .
H11C H 0.173342 0.398373 0.534986 0.058 Uiso 1 1 calc R U . . .
C12 C 0.0263(3) 0.1919(3) 0.55307(19) 0.0423(7) Uani 1 1 d . . . . .
H12A H -0.063158 0.292226 0.534479 0.063 Uiso 1 1 calc R U . . .
H12B H 0.016067 0.161193 0.632314 0.063 Uiso 1 1 calc R U . . .
H12C H 0.002949 0.121365 0.524225 0.063 Uiso 1 1 calc R U . . .
C13 C 0.2019(3) 0.5081(3) 0.11046(17) 0.0302(5) Uani 1 1 d . . . . .
H13 H 0.254389 0.468694 0.041553 0.036 Uiso 1 1 calc R U . . .
C14 C 0.2967(4) 0.6130(3) 0.1100(2) 0.0486(7) Uani 1 1 d . . . . .
H14A H 0.278283 0.693377 0.045550 0.073 Uiso 1 1 calc R U . . .
H14B H 0.427543 0.557178 0.108633 0.073 Uiso 1 1 calc R U . . .
H14C H 0.245226 0.656080 0.175673 0.073 Uiso 1 1 calc R U . . .
C15 C -0.0024(3) 0.5941(3) 0.1103(2) 0.0397(6) Uani 1 1 d . . . . .
H15A H -0.019454 0.677921 0.048005 0.059 Uiso 1 1 calc R U . . .
H15B H -0.058330 0.632168 0.177821 0.059 Uiso 1 1 calc R U . . .
H15C H -0.060056 0.527162 0.104912 0.059 Uiso 1 1 calc R U . . .
C16 C 0.7956(3) -0.0013(3) 0.1577(2) 0.0361(6) Uani 1 1 d . . . . .
H16A H 0.813592 0.049117 0.081499 0.054 Uiso 1 1 calc R U . . .
H16B H 0.698119 -0.041432 0.170514 0.054 Uiso 1 1 calc R U . . .
H16C H 0.908952 -0.083245 0.173846 0.054 Uiso 1 1 calc R U . . .
C17 C 0.8848(3) 0.1619(3) 0.2152(2) 0.0351(6) Uani 1 1 d . . . . .
H17A H 0.900408 0.223657 0.141618 0.042 Uiso 1 1 calc R U . . .
H17B H 1.002459 0.079710 0.225581 0.042 Uiso 1 1 calc R U . . .
C18 C 0.8283(3) 0.2544(3) 0.2987(2) 0.0373(6) Uani 1 1 d . . . . .
H18A H 0.832954 0.190069 0.372101 0.045 Uiso 1 1 calc R U . . .
H18B H 0.911225 0.310263 0.285980 0.045 Uiso 1 1 calc R U . . .
C19 C 0.5918(4) 0.4712(3) 0.3488(2) 0.0447(7) Uani 1 1 d . . . . .
H19A H 0.664918 0.535129 0.315155 0.067 Uiso 1 1 calc R U . . .
H19B H 0.610431 0.427547 0.424300 0.067 Uiso 1 1 calc R U . . .
H19C H 0.462518 0.531092 0.347389 0.067 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
Li1 O1 1.967(4) . ?
Li1 O2 1.987(4) . ?
Li1 C1 2.259(4) . ?
Li1 C9 2.280(4) . ?
Li1 C2 2.285(4) . ?
Li1 C3 2.315(4) . ?
Li1 C8 2.316(4) . ?
O1 C16 1.420(3) . ?
O1 C17 1.425(3) . ?
O2 C19 1.409(3) . ?
O2 C18 1.432(3) . ?
C2 C1 1.416(3) . ?
C2 C3 1.417(3) . ?
C2 C13 1.509(3) . ?
C1 C9 1.418(3) . ?
C3 C4 1.422(3) . ?
C3 C8 1.460(3) . ?
C4 C5 1.373(4) . ?
C5 C6 1.409(3) . ?
C6 C7 1.372(3) . ?
C7 C8 1.411(3) . ?
C8 C9 1.420(3) . ?
C10 C9 1.513(3) . ?
C10 C11 1.519(3) . ?
C10 C12 1.523(3) . ?
C13 C14 1.524(3) . ?
C13 C15 1.532(3) . ?
C17 C18 1.482(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
O1 Li1 O2 83.45(15) . . ?
O1 Li1 C1 169.4(2) . . ?
O2 Li1 C1 106.97(19) . . ?
O1 Li1 C9 135.7(2) . . ?
O2 Li1 C9 122.41(19) . . ?
C1 Li1 C9 36.41(10) . . ?
O1 Li1 C2 139.4(2) . . ?
O2 Li1 C2 120.5(2) . . ?
C1 Li1 C2 36.31(9) . . ?
C9 Li1 C2 61.53(11) . . ?
O1 Li1 C3 111.61(19) . . ?
O2 Li1 C3 155.0(2) . . ?
C1 Li1 C3 59.50(11) . . ?
C9 Li1 C3 60.81(11) . . ?
C2 Li1 C3 35.89(10) . . ?
O1 Li1 C8 109.80(19) . . ?
O2 Li1 C8 157.5(2) . . ?
C1 Li1 C8 59.66(12) . . ?
C9 Li1 C8 35.99(9) . . ?
C2 Li1 C8 60.90(11) . . ?
C3 Li1 C8 36.76(9) . . ?
C16 O1 C17 112.86(17) . . ?
C16 O1 Li1 127.90(17) . . ?
C17 O1 Li1 110.68(18) . . ?
C19 O2 C18 112.65(18) . . ?
C19 O2 Li1 130.35(18) . . ?
C18 O2 Li1 108.64(18) . . ?
C1 C2 C3 106.49(19) . . ?
C1 C2 C13 126.5(2) . . ?
C3 C2 C13 126.82(19) . . ?
C1 C2 Li1 70.85(15) . . ?
C3 C2 Li1 73.22(15) . . ?
C13 C2 Li1 125.19(17) . . ?
C2 C1 C9 110.9(2) . . ?
C2 C1 Li1 72.84(15) . . ?
C9 C1 Li1 72.60(16) . . ?
C2 C3 C4 133.5(2) . . ?
C2 C3 C8 108.23(18) . . ?
C4 C3 C8 118.3(2) . . ?
C2 C3 Li1 70.89(15) . . ?
C4 C3 Li1 123.28(16) . . ?
C8 C3 Li1 71.67(15) . . ?
C5 C4 C3 120.1(2) . . ?
C4 C5 C6 121.0(2) . . ?
C7 C6 C5 121.3(2) . . ?
C6 C7 C8 119.8(2) . . ?
C7 C8 C9 132.9(2) . . ?
C7 C8 C3 119.5(2) . . ?
C9 C8 C3 107.66(19) . . ?
C7 C8 Li1 123.87(17) . . ?
C9 C8 Li1 70.61(15) . . ?
C3 C8 Li1 71.57(15) . . ?
C9 C10 C11 112.58(19) . . ?
C9 C10 C12 111.03(17) . . ?
C11 C10 C12 109.7(2) . . ?
C1 C9 C8 106.64(18) . . ?
C1 C9 C10 127.4(2) . . ?
C8 C9 C10 125.7(2) . . ?
C1 C9 Li1 70.99(15) . . ?
C8 C9 Li1 73.40(15) . . ?
C10 C9 Li1 124.99(16) . . ?
C2 C13 C14 112.54(18) . . ?
C2 C13 C15 111.14(18) . . ?
C14 C13 C15 110.3(2) . . ?
O1 C17 C18 108.10(18) . . ?
O2 C18 C17 107.62(18) . . ?

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
C3 C2 C1 C9 2.0(2) . . . . ?
C13 C2 C1 C9 176.82(18) . . . . ?
Li1 C2 C1 C9 -63.05(18) . . . . ?
C3 C2 C1 Li1 65.08(17) . . . . ?
C13 C2 C1 Li1 -120.1(2) . . . . ?
C1 C2 C3 C4 178.4(2) . . . . ?
C13 C2 C3 C4 3.6(4) . . . . ?
Li1 C2 C3 C4 -118.2(2) . . . . ?
C1 C2 C3 C8 -1.2(2) . . . . ?
C13 C2 C3 C8 -175.94(18) . . . . ?
Li1 C2 C3 C8 62.31(16) . . . . ?
C1 C2 C3 Li1 -63.48(16) . . . . ?
C13 C2 C3 Li1 121.7(2) . . . . ?
C2 C3 C4 C5 -178.1(2) . . . . ?
C8 C3 C4 C5 1.4(3) . . . . ?
Li1 C3 C4 C5 87.2(3) . . . . ?
C3 C4 C5 C6 -1.4(3) . . . . ?
C4 C5 C6 C7 0.4(3) . . . . ?
C5 C6 C7 C8 0.5(3) . . . . ?
C6 C7 C8 C9 178.5(2) . . . . ?
C6 C7 C8 C3 -0.4(3) . . . . ?
C6 C7 C8 Li1 -87.1(3) . . . . ?
C2 C3 C8 C7 179.08(18) . . . . ?
C4 C3 C8 C7 -0.5(3) . . . . ?
Li1 C3 C8 C7 -119.1(2) . . . . ?
C2 C3 C8 C9 -0.1(2) . . . . ?
C4 C3 C8 C9 -179.69(17) . . . . ?
Li1 C3 C8 C9 61.75(17) . . . . ?
C2 C3 C8 Li1 -61.82(17) . . . . ?
C4 C3 C8 Li1 118.6(2) . . . . ?
C2 C1 C9 C8 -2.1(2) . . . . ?
Li1 C1 C9 C8 -65.27(16) . . . . ?
C2 C1 C9 C10 -176.80(18) . . . . ?
Li1 C1 C9 C10 120.0(2) . . . . ?
C2 C1 C9 Li1 63.19(17) . . . . ?
C7 C8 C9 C1 -177.7(2) . . . . ?
C3 C8 C9 C1 1.3(2) . . . . ?
Li1 C8 C9 C1 63.65(16) . . . . ?
C7 C8 C9 C10 -2.9(4) . . . . ?
C3 C8 C9 C10 176.12(18) . . . . ?
Li1 C8 C9 C10 -121.5(2) . . . . ?
C7 C8 C9 Li1 118.6(3) . . . . ?
C3 C8 C9 Li1 -62.37(17) . . . . ?
C11 C10 C9 C1 -33.7(3) . . . . ?
C12 C10 C9 C1 89.8(3) . . . . ?
C11 C10 C9 C8 152.5(2) . . . . ?
C12 C10 C9 C8 -84.0(3) . . . . ?
C11 C10 C9 Li1 58.3(3) . . . . ?
C12 C10 C9 Li1 -178.2(2) . . . . ?
C1 C2 C13 C14 52.0(3) . . . . ?
C3 C2 C13 C14 -134.2(2) . . . . ?
Li1 C2 C13 C14 -39.2(3) . . . . ?
C1 C2 C13 C15 -72.2(3) . . . . ?
C3 C2 C13 C15 101.6(3) . . . . ?
Li1 C2 C13 C15 -163.5(2) . . . . ?
C16 O1 C17 C18 -173.63(19) . . . . ?
Li1 O1 C17 C18 35.7(3) . . . . ?
C19 O2 C18 C17 -166.8(2) . . . . ?
Li1 O2 C18 C17 41.4(2) . . . . ?
O1 C17 C18 O2 -50.9(3) . . . . ?

_refine_diff_density_max         0.241
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.050



_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_sh4632_a
_database_code_depnum_ccdc_archive 'CCDC 2154214'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Saarland University
Germany
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'sodium di-tert-butyl indenide tris(dimethoxyethane) adduct'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H30 Na O6, C17 H23'
_chemical_formula_sum            'C29 H53 Na O6'
_chemical_formula_weight         520.70

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'
Na Na 0.0362 0.0249 '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'

_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                   11.6172(2)
_cell_length_b                   15.9650(3)
_cell_length_c                   17.7264(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.5900(10)
_cell_angle_gamma                90
_cell_volume                     3195.64(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9973
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.09

_exptl_crystal_description       cuboid
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.138
_exptl_absorpt_coefficient_mu    0.085
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6877
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49094
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.209
_diffrn_reflns_theta_max         27.115
_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             7058
_reflns_number_gt                5517
_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       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0434P)²+0.9863P] 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         7058
_refine_ls_number_parameters     337
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.0950
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Na1 Na 0.29867(4) 0.23216(3) 0.20442(3) 0.02452(13) Uani 1 1 d . . . . .
O1 O 0.17238(9) 0.35000(6) 0.18058(6) 0.0323(2) Uani 1 1 d . . . . .
O2 O 0.14384(8) 0.20748(6) 0.09353(6) 0.0291(2) Uani 1 1 d . . . . .
O3 O 0.44563(8) 0.31040(7) 0.29542(6) 0.0310(2) Uani 1 1 d . . . . .
O4 O 0.44683(8) 0.27174(6) 0.14118(6) 0.0310(2) Uani 1 1 d . . . . .
O5 O 0.35123(9) 0.08908(6) 0.20420(7) 0.0360(2) Uani 1 1 d . . . . .
O6 O 0.22679(9) 0.15942(6) 0.30479(6) 0.0355(2) Uani 1 1 d . . . . .
C1 C 0.75046(11) 0.23805(8) 0.53213(7) 0.0219(3) Uani 1 1 d . . . . .
H1 H 0.726851 0.216872 0.576266 0.026 Uiso 1 1 calc R U . . .
C2 C 0.77492(11) 0.32309(8) 0.52140(7) 0.0206(3) Uani 1 1 d . . . . .
C3 C 0.80681(10) 0.32783(8) 0.44906(7) 0.0197(3) Uani 1 1 d . . . . .
C4 C 0.84277(11) 0.39455(8) 0.40722(8) 0.0242(3) Uani 1 1 d . . . . .
H4 H 0.846988 0.449822 0.427523 0.029 Uiso 1 1 calc R U . . .
C5 C 0.87171(11) 0.38000(9) 0.33729(8) 0.0290(3) Uani 1 1 d . . . . .
H5 H 0.896977 0.425223 0.310289 0.035 Uiso 1 1 calc R U . . .
C6 C 0.86424(12) 0.29892(9) 0.30548(8) 0.0296(3) Uani 1 1 d . . . . .
H6 H 0.882721 0.290164 0.256641 0.035 Uiso 1 1 calc R U . . .
C7 C 0.83039(11) 0.23209(9) 0.34441(8) 0.0254(3) Uani 1 1 d . . . . .
H7 H 0.826791 0.177639 0.322361 0.030 Uiso 1 1 calc R U . . .
C8 C 0.80100(10) 0.24334(8) 0.41655(7) 0.0199(3) Uani 1 1 d . . . . .
C9 C 0.76526(10) 0.18821(8) 0.46946(7) 0.0210(3) Uani 1 1 d . . . . .
C10 C 0.74584(12) 0.09416(8) 0.46045(8) 0.0265(3) Uani 1 1 d . . . . .
C11 C 0.64699(14) 0.07435(9) 0.38827(10) 0.0397(4) Uani 1 1 d . . . . .
H11A H 0.572540 0.099374 0.394095 0.060 Uiso 1 1 calc R U . . .
H11B H 0.637439 0.013511 0.382614 0.060 Uiso 1 1 calc R U . . .
H11C H 0.668009 0.097528 0.342095 0.060 Uiso 1 1 calc R U . . .
C12 C 0.71047(16) 0.05726(9) 0.53128(10) 0.0441(4) Uani 1 1 d . . . . .
H12A H 0.771428 0.070525 0.578161 0.066 Uiso 1 1 calc R U . . .
H12B H 0.702673 -0.003663 0.525528 0.066 Uiso 1 1 calc R U . . .
H12C H 0.634632 0.081266 0.535571 0.066 Uiso 1 1 calc R U . . .
C13 C 0.85879(14) 0.04944(9) 0.45167(10) 0.0392(4) Uani 1 1 d . . . . .
H13A H 0.921309 0.057273 0.498986 0.059 Uiso 1 1 calc R U . . .
H13B H 0.884578 0.072963 0.407288 0.059 Uiso 1 1 calc R U . . .
H13C H 0.842673 -0.010501 0.443111 0.059 Uiso 1 1 calc R U . . .
C14 C 0.76883(12) 0.39482(8) 0.57661(8) 0.0257(3) Uani 1 1 d . . . . .
C15 C 0.67557(13) 0.45962(9) 0.53827(9) 0.0333(3) Uani 1 1 d . . . . .
H15A H 0.674973 0.506065 0.574319 0.050 Uiso 1 1 calc R U . . .
H15B H 0.597291 0.433134 0.525111 0.050 Uiso 1 1 calc R U . . .
H15C H 0.694941 0.480985 0.490917 0.050 Uiso 1 1 calc R U . . .
C16 C 0.73501(16) 0.36280(10) 0.64975(9) 0.0387(4) Uani 1 1 d . . . . .
H16A H 0.730436 0.410068 0.684194 0.058 Uiso 1 1 calc R U . . .
H16B H 0.795030 0.322999 0.676591 0.058 Uiso 1 1 calc R U . . .
H16C H 0.657880 0.334798 0.635356 0.058 Uiso 1 1 calc R U . . .
C17 C 0.88975(14) 0.43871(10) 0.60186(10) 0.0400(4) Uani 1 1 d . . . . .
H17A H 0.949446 0.398242 0.627852 0.060 Uiso 1 1 calc R U . . .
H17B H 0.884214 0.484444 0.637715 0.060 Uiso 1 1 calc R U . . .
H17C H 0.912569 0.461376 0.556101 0.060 Uiso 1 1 calc R U . . .
C18 C 0.46406(15) 0.29749(11) 0.37717(9) 0.0417(4) Uani 1 1 d . . . . .
H18A H 0.526659 0.335090 0.404689 0.063 Uiso 1 1 calc R U . . .
H18B H 0.487643 0.239245 0.389661 0.063 Uiso 1 1 calc R U . . .
H18C H 0.390519 0.309295 0.393206 0.063 Uiso 1 1 calc R U . . .
C19 C 0.55260(11) 0.30140(9) 0.27021(8) 0.0289(3) Uani 1 1 d . . . . .
H19A H 0.579336 0.242364 0.275852 0.035 Uiso 1 1 calc R U . . .
H19B H 0.615338 0.336809 0.302332 0.035 Uiso 1 1 calc R U . . .
C20 C 0.53061(12) 0.32738(9) 0.18708(8) 0.0294(3) Uani 1 1 d . . . . .
H20A H 0.499689 0.385389 0.181045 0.035 Uiso 1 1 calc R U . . .
H20B H 0.605617 0.325791 0.169753 0.035 Uiso 1 1 calc R U . . .
C21 C 0.42470(15) 0.29141(13) 0.06078(9) 0.0461(4) Uani 1 1 d . . . . .
H21A H 0.498382 0.286359 0.043273 0.069 Uiso 1 1 calc R U . . .
H21B H 0.394822 0.348887 0.052369 0.069 Uiso 1 1 calc R U . . .
H21C H 0.365637 0.252535 0.031310 0.069 Uiso 1 1 calc R U . . .
C22 C 0.16635(17) 0.41005(10) 0.23885(10) 0.0463(4) Uani 1 1 d . . . . .
H22A H 0.246217 0.421113 0.270347 0.070 Uiso 1 1 calc R U . . .
H22B H 0.116733 0.388240 0.272097 0.070 Uiso 1 1 calc R U . . .
H22C H 0.131927 0.462163 0.214236 0.070 Uiso 1 1 calc R U . . .
C23 C 0.05806(12) 0.32796(10) 0.13508(9) 0.0330(3) Uani 1 1 d . . . . .
H23A H 0.011363 0.379257 0.117915 0.040 Uiso 1 1 calc R U . . .
H23B H 0.015314 0.294084 0.166536 0.040 Uiso 1 1 calc R U . . .
C24 C 0.07204(12) 0.27892(9) 0.06621(8) 0.0297(3) Uani 1 1 d . . . . .
H24A H -0.006423 0.260873 0.035235 0.036 Uiso 1 1 calc R U . . .
H24B H 0.110240 0.313823 0.032863 0.036 Uiso 1 1 calc R U . . .
C25 C 0.14673(14) 0.15041(10) 0.03232(9) 0.0373(4) Uani 1 1 d . . . . .
H25A H 0.194959 0.101640 0.053287 0.056 Uiso 1 1 calc R U . . .
H25B H 0.181241 0.178128 -0.006519 0.056 Uiso 1 1 calc R U . . .
H25C H 0.065973 0.132161 0.008056 0.056 Uiso 1 1 calc R U . . .
C26 C 0.12648(18) 0.19079(13) 0.32879(13) 0.0576(5) Uani 1 1 d . . . . .
H26A H 0.140431 0.249309 0.345075 0.086 Uiso 1 1 calc R U . . .
H26B H 0.113400 0.157316 0.372367 0.086 Uiso 1 1 calc R U . . .
H26C H 0.056478 0.187365 0.285478 0.086 Uiso 1 1 calc R U . . .
C27 C 0.20790(12) 0.07522(9) 0.27872(9) 0.0341(3) Uani 1 1 d . . . . .
H27A H 0.144540 0.073130 0.230408 0.041 Uiso 1 1 calc R U . . .
H27B H 0.182701 0.040951 0.318530 0.041 Uiso 1 1 calc R U . . .
C28 C 0.32028(12) 0.04109(9) 0.26404(9) 0.0339(3) Uani 1 1 d . . . . .
H28A H 0.384233 0.044365 0.311976 0.041 Uiso 1 1 calc R U . . .
H28B H 0.309432 -0.018371 0.248114 0.041 Uiso 1 1 calc R U . . .
C29 C 0.44505(14) 0.05238(11) 0.17704(10) 0.0433(4) Uani 1 1 d . . . . .
H29A H 0.420707 -0.003030 0.155249 0.065 Uiso 1 1 calc R U . . .
H29B H 0.514807 0.046680 0.220265 0.065 Uiso 1 1 calc R U . . .
H29C H 0.464475 0.088124 0.136823 0.065 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
Na1 O4 2.3507(11) . ?
Na1 O1 2.3619(11) . ?
Na1 O5 2.3647(11) . ?
Na1 O2 2.3649(10) . ?
Na1 O3 2.4048(11) . ?
Na1 O6 2.4310(12) . ?
Na1 C19 3.1092(14) . ?
Na1 C27 3.1268(15) . ?
O1 C22 1.4231(17) . ?
O1 C23 1.4265(17) . ?
O2 C25 1.4232(17) . ?
O2 C24 1.4288(16) . ?
O3 C19 1.4232(16) . ?
O3 C18 1.4291(17) . ?
O4 C21 1.4225(18) . ?
O4 C20 1.4235(16) . ?
O5 C29 1.4176(18) . ?
O5 C28 1.4214(18) . ?
O6 C27 1.4216(18) . ?
O6 C26 1.4223(19) . ?
C1 C2 1.4092(17) . ?
C1 C9 1.4094(18) . ?
C2 C3 1.4179(18) . ?
C2 C14 1.5189(17) . ?
C3 C4 1.4158(18) . ?
C3 C8 1.4621(17) . ?
C4 C5 1.378(2) . ?
C5 C6 1.406(2) . ?
C6 C7 1.377(2) . ?
C7 C8 1.4105(18) . ?
C8 C9 1.4177(18) . ?
C9 C10 1.5213(17) . ?
C10 C12 1.528(2) . ?
C10 C13 1.5336(19) . ?
C10 C11 1.5381(19) . ?
C14 C16 1.528(2) . ?
C14 C15 1.5362(19) . ?
C14 C17 1.539(2) . ?
C19 C20 1.494(2) . ?
C23 C24 1.491(2) . ?
C27 C28 1.493(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
O4 Na1 O1 101.20(4) . . ?
O4 Na1 O5 92.33(4) . . ?
O1 Na1 O5 156.76(4) . . ?
O4 Na1 O2 98.48(4) . . ?
O1 Na1 O2 70.42(4) . . ?
O5 Na1 O2 89.08(4) . . ?
O4 Na1 O3 72.32(4) . . ?
O1 Na1 O3 91.12(4) . . ?
O5 Na1 O3 111.10(4) . . ?
O2 Na1 O3 157.75(4) . . ?
O4 Na1 O6 153.30(4) . . ?
O1 Na1 O6 101.87(4) . . ?
O5 Na1 O6 70.91(4) . . ?
O2 Na1 O6 101.76(4) . . ?
O3 Na1 O6 93.96(4) . . ?
O4 Na1 C19 49.22(4) . . ?
O1 Na1 C19 106.18(4) . . ?
O5 Na1 C19 96.97(4) . . ?
O2 Na1 C19 147.17(4) . . ?
O3 Na1 C19 26.14(3) . . ?
O6 Na1 C19 110.74(4) . . ?
O4 Na1 C27 140.67(4) . . ?
O1 Na1 C27 117.18(4) . . ?
O5 Na1 C27 48.65(4) . . ?
O2 Na1 C27 87.17(4) . . ?
O3 Na1 C27 112.97(4) . . ?
O6 Na1 C27 25.98(4) . . ?
C19 Na1 C27 120.73(4) . . ?
C22 O1 C23 112.24(12) . . ?
C22 O1 Na1 122.77(9) . . ?
C23 O1 Na1 111.18(8) . . ?
C25 O2 C24 111.66(11) . . ?
C25 O2 Na1 126.21(8) . . ?
C24 O2 Na1 114.72(8) . . ?
C19 O3 C18 111.71(11) . . ?
C19 O3 Na1 105.76(8) . . ?
C18 O3 Na1 121.26(9) . . ?
C21 O4 C20 111.92(11) . . ?
C21 O4 Na1 123.84(9) . . ?
C20 O4 Na1 111.96(8) . . ?
C29 O5 C28 112.34(12) . . ?
C29 O5 Na1 128.26(10) . . ?
C28 O5 Na1 114.13(8) . . ?
C27 O6 C26 110.82(13) . . ?
C27 O6 Na1 105.49(9) . . ?
C26 O6 Na1 119.81(10) . . ?
C2 C1 C9 111.82(11) . . ?
C1 C2 C3 106.10(11) . . ?
C1 C2 C14 126.73(12) . . ?
C3 C2 C14 127.17(11) . . ?
C4 C3 C2 133.30(12) . . ?
C4 C3 C8 118.65(12) . . ?
C2 C3 C8 108.03(11) . . ?
C5 C4 C3 120.59(12) . . ?
C4 C5 C6 120.70(13) . . ?
C7 C6 C5 120.67(13) . . ?
C6 C7 C8 120.93(13) . . ?
C7 C8 C9 133.76(12) . . ?
C7 C8 C3 118.44(12) . . ?
C9 C8 C3 107.79(11) . . ?
C1 C9 C8 106.25(11) . . ?
C1 C9 C10 126.69(12) . . ?
C8 C9 C10 127.06(12) . . ?
C9 C10 C12 110.86(12) . . ?
C9 C10 C13 111.15(11) . . ?
C12 C10 C13 107.80(12) . . ?
C9 C10 C11 110.71(11) . . ?
C12 C10 C11 108.18(12) . . ?
C13 C10 C11 108.01(12) . . ?
C2 C14 C16 110.77(11) . . ?
C2 C14 C15 110.94(11) . . ?
C16 C14 C15 107.78(12) . . ?
C2 C14 C17 110.68(11) . . ?
C16 C14 C17 107.73(12) . . ?
C15 C14 C17 108.83(12) . . ?
O3 C19 C20 108.79(11) . . ?
O3 C19 Na1 48.11(6) . . ?
C20 C19 Na1 78.55(7) . . ?
O4 C20 C19 109.03(11) . . ?
O1 C23 C24 109.05(11) . . ?
O2 C24 C23 107.99(11) . . ?
O6 C27 C28 109.10(11) . . ?
O6 C27 Na1 48.52(6) . . ?
C28 C27 Na1 79.85(8) . . ?
O5 C28 C27 108.56(11) . . ?

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
C9 C1 C2 C3 -0.09(14) . . . . ?
C9 C1 C2 C14 -179.79(11) . . . . ?
C1 C2 C3 C4 -178.56(13) . . . . ?
C14 C2 C3 C4 1.1(2) . . . . ?
C1 C2 C3 C8 -0.05(13) . . . . ?
C14 C2 C3 C8 179.65(11) . . . . ?
C2 C3 C4 C5 178.36(13) . . . . ?
C8 C3 C4 C5 -0.02(17) . . . . ?
C3 C4 C5 C6 1.06(19) . . . . ?
C4 C5 C6 C7 -1.5(2) . . . . ?
C5 C6 C7 C8 0.79(19) . . . . ?
C6 C7 C8 C9 -179.18(13) . . . . ?
C6 C7 C8 C3 0.24(18) . . . . ?
C4 C3 C8 C7 -0.62(16) . . . . ?
C2 C3 C8 C7 -179.39(11) . . . . ?
C4 C3 C8 C9 178.94(10) . . . . ?
C2 C3 C8 C9 0.17(13) . . . . ?
C2 C1 C9 C8 0.20(14) . . . . ?
C2 C1 C9 C10 -179.43(11) . . . . ?
C7 C8 C9 C1 179.24(13) . . . . ?
C3 C8 C9 C1 -0.22(13) . . . . ?
C7 C8 C9 C10 -1.1(2) . . . . ?
C3 C8 C9 C10 179.41(11) . . . . ?
C1 C9 C10 C12 -1.82(18) . . . . ?
C8 C9 C10 C12 178.62(13) . . . . ?
C1 C9 C10 C13 -121.70(14) . . . . ?
C8 C9 C10 C13 58.74(17) . . . . ?
C1 C9 C10 C11 118.25(15) . . . . ?
C8 C9 C10 C11 -61.31(17) . . . . ?
C1 C2 C14 C16 1.68(18) . . . . ?
C3 C2 C14 C16 -177.96(12) . . . . ?
C1 C2 C14 C15 -117.98(14) . . . . ?
C3 C2 C14 C15 62.38(17) . . . . ?
C1 C2 C14 C17 121.11(14) . . . . ?
C3 C2 C14 C17 -58.53(17) . . . . ?
C18 O3 C19 C20 -172.10(12) . . . . ?
Na1 O3 C19 C20 54.06(12) . . . . ?
C18 O3 C19 Na1 133.84(13) . . . . ?
C21 O4 C20 C19 -178.11(12) . . . . ?
Na1 O4 C20 C19 37.85(13) . . . . ?
O3 C19 C20 O4 -63.98(14) . . . . ?
Na1 C19 C20 O4 -26.04(9) . . . . ?
C22 O1 C23 C24 168.72(13) . . . . ?
Na1 O1 C23 C24 -49.51(13) . . . . ?
C25 O2 C24 C23 170.97(12) . . . . ?
Na1 O2 C24 C23 -37.07(13) . . . . ?
O1 C23 C24 O2 57.17(15) . . . . ?
C26 O6 C27 C28 -172.62(14) . . . . ?
Na1 O6 C27 C28 56.28(12) . . . . ?
C26 O6 C27 Na1 131.10(14) . . . . ?
C29 O5 C28 C27 -169.70(12) . . . . ?
Na1 O5 C28 C27 33.72(14) . . . . ?
O6 C27 C28 O5 -62.19(15) . . . . ?
Na1 C27 C28 O5 -22.91(10) . . . . ?

_refine_diff_density_max         0.207
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.040



_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_4696_a
_database_code_depnum_ccdc_archive 'CCDC 2154217'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Saarland University
Germany
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        bis(di-tert-butylindenyl)germanocene
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C17 H23), Ge'
_chemical_formula_sum            'C34 H46 Ge'
_chemical_formula_weight         527.30

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'
Ge Ge 0.1547 1.8001 '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                   10.979(3)
_cell_length_b                   14.731(4)
_cell_length_c                   18.973(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.306(8)
_cell_angle_gamma                90
_cell_volume                     2929.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    148(2)
_cell_measurement_reflns_used    9877
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.10

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.088
_exptl_absorpt_coefficient_mu    1.065
_shelx_estimated_absorpt_T_min   0.774
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6975
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      148(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48002
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.934
_diffrn_reflns_theta_max         27.137
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6464
_reflns_number_gt                5596
_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       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0295P)²+1.2329P] 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         6464
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
Ge1 Ge 0.47674(2) 0.24309(2) 0.69667(2) 0.01675(5) Uani 1 1 d . . . . .
C1 C 0.40682(14) 0.08449(9) 0.71025(8) 0.0190(3) Uani 1 1 d . . . . .
H1 H 0.444746 0.036949 0.690222 0.023 Uiso 1 1 calc R U . . .
C2 C 0.45322(13) 0.11556(9) 0.78387(8) 0.0174(3) Uani 1 1 d . . . . .
C3 C 0.36322(13) 0.18250(9) 0.79232(8) 0.0180(3) Uani 1 1 d . . . . .
C4 C 0.35485(16) 0.23406(11) 0.85376(9) 0.0260(3) Uani 1 1 d . . . . .
H4 H 0.418181 0.228029 0.900175 0.031 Uiso 1 1 calc R U . . .
C5 C 0.25514(18) 0.29244(12) 0.84578(10) 0.0333(4) Uani 1 1 d . . . . .
H5 H 0.249656 0.326822 0.887088 0.040 Uiso 1 1 calc R U . . .
C7 C 0.16455(15) 0.25449(11) 0.71688(10) 0.0278(3) Uani 1 1 d . . . . .
H7 H 0.099751 0.262128 0.671224 0.033 Uiso 1 1 calc R U . . .
C6 C 0.16030(16) 0.30272(12) 0.77760(11) 0.0334(4) Uani 1 1 d . . . . .
H6 H 0.092080 0.343945 0.773710 0.040 Uiso 1 1 calc R U . . .
C9 C 0.29656(14) 0.13313(10) 0.66997(8) 0.0204(3) Uani 1 1 d . . . . .
C8 C 0.26632(14) 0.19292(10) 0.72242(8) 0.0201(3) Uani 1 1 d . . . . .
C10 C 0.21366(16) 0.11328(11) 0.59146(8) 0.0286(4) Uani 1 1 d . . . . .
C11 C 0.27879(19) 0.04427(13) 0.55442(9) 0.0387(4) Uani 1 1 d . . . . .
H11A H 0.224587 0.032713 0.503971 0.058 Uiso 1 1 calc R U . . .
H11B H 0.292330 -0.012544 0.582560 0.058 Uiso 1 1 calc R U . . .
H11C H 0.361189 0.068416 0.552988 0.058 Uiso 1 1 calc R U . . .
C12 C 0.18800(19) 0.19904(13) 0.54349(10) 0.0403(5) Uani 1 1 d . . . . .
H12A H 0.268772 0.222631 0.538934 0.060 Uiso 1 1 calc R U . . .
H12B H 0.147786 0.245080 0.566509 0.060 Uiso 1 1 calc R U . . .
H12C H 0.131044 0.184208 0.494379 0.060 Uiso 1 1 calc R U . . .
C13 C 0.08562(17) 0.07283(14) 0.59432(10) 0.0395(4) Uani 1 1 d . . . . .
H13A H 0.028524 0.065580 0.543976 0.059 Uiso 1 1 calc R U . . .
H13B H 0.046270 0.113697 0.622017 0.059 Uiso 1 1 calc R U . . .
H13C H 0.100732 0.013518 0.618770 0.059 Uiso 1 1 calc R U . . .
C14 C 0.56616(14) 0.07709(10) 0.84395(8) 0.0202(3) Uani 1 1 d . . . . .
C15 C 0.64126(17) 0.01041(13) 0.81171(10) 0.0379(4) Uani 1 1 d . . . . .
H15A H 0.586523 -0.041023 0.789687 0.057 Uiso 1 1 calc R U . . .
H15B H 0.715271 -0.011581 0.850997 0.057 Uiso 1 1 calc R U . . .
H15C H 0.670315 0.040917 0.773714 0.057 Uiso 1 1 calc R U . . .
C16 C 0.65840(16) 0.15217(12) 0.88244(9) 0.0314(4) Uani 1 1 d . . . . .
H16A H 0.693649 0.181874 0.846595 0.047 Uiso 1 1 calc R U . . .
H16B H 0.727922 0.125737 0.922183 0.047 Uiso 1 1 calc R U . . .
H16C H 0.612688 0.196991 0.903201 0.047 Uiso 1 1 calc R U . . .
C17 C 0.51668(17) 0.02688(14) 0.90103(10) 0.0401(5) Uani 1 1 d . . . . .
H17A H 0.459011 -0.022003 0.876540 0.060 Uiso 1 1 calc R U . . .
H17B H 0.470630 0.069569 0.923467 0.060 Uiso 1 1 calc R U . . .
H17C H 0.588885 0.001089 0.939451 0.060 Uiso 1 1 calc R U . . .
C18 C 0.52581(13) 0.35025(9) 0.60445(8) 0.0174(3) Uani 1 1 d . . . . .
H18 H 0.469108 0.352914 0.555682 0.021 Uiso 1 1 calc R U . . .
C19 C 0.51807(13) 0.40729(9) 0.66245(8) 0.0167(3) Uani 1 1 d . . . . .
C20 C 0.62563(13) 0.38467(9) 0.72496(7) 0.0166(3) Uani 1 1 d . . . . .
C21 C 0.67041(14) 0.41916(10) 0.79812(8) 0.0221(3) Uani 1 1 d . . . . .
H21 H 0.623016 0.464229 0.814400 0.027 Uiso 1 1 calc R U . . .
C22 C 0.78235(15) 0.38698(11) 0.84498(8) 0.0253(3) Uani 1 1 d . . . . .
H22 H 0.812671 0.410732 0.893634 0.030 Uiso 1 1 calc R U . . .
C23 C 0.85347(14) 0.31920(11) 0.82234(8) 0.0243(3) Uani 1 1 d . . . . .
H23 H 0.931813 0.299158 0.855614 0.029 Uiso 1 1 calc R U . . .
C24 C 0.81157(14) 0.28184(10) 0.75331(8) 0.0197(3) Uani 1 1 d . . . . .
H24 H 0.859698 0.235476 0.739134 0.024 Uiso 1 1 calc R U . . .
C25 C 0.69568(13) 0.31280(9) 0.70298(7) 0.0161(3) Uani 1 1 d . . . . .
C26 C 0.62887(13) 0.28826(9) 0.62790(7) 0.0165(3) Uani 1 1 d . . . . .
C27 C 0.67507(14) 0.22427(10) 0.57845(8) 0.0207(3) Uani 1 1 d . . . . .
C28 C 0.57457(16) 0.21514(12) 0.50296(8) 0.0280(3) Uani 1 1 d . . . . .
H28A H 0.562504 0.274022 0.477788 0.042 Uiso 1 1 calc R U . . .
H28B H 0.493638 0.195136 0.509703 0.042 Uiso 1 1 calc R U . . .
H28C H 0.603281 0.170422 0.473106 0.042 Uiso 1 1 calc R U . . .
C29 C 0.79723(16) 0.26346(13) 0.56646(9) 0.0319(4) Uani 1 1 d . . . . .
H29A H 0.828387 0.222146 0.535178 0.048 Uiso 1 1 calc R U . . .
H29B H 0.862606 0.270400 0.614237 0.048 Uiso 1 1 calc R U . . .
H29C H 0.778520 0.322809 0.542311 0.048 Uiso 1 1 calc R U . . .
C30 C 0.70153(18) 0.12942(11) 0.61246(9) 0.0316(4) Uani 1 1 d . . . . .
H30A H 0.736490 0.090821 0.581105 0.047 Uiso 1 1 calc R U . . .
H30B H 0.621878 0.102928 0.616300 0.047 Uiso 1 1 calc R U . . .
H30C H 0.763177 0.133778 0.661758 0.047 Uiso 1 1 calc R U . . .
C31 C 0.42332(14) 0.48398(10) 0.65696(8) 0.0217(3) Uani 1 1 d . . . . .
C32 C 0.49561(17) 0.57473(11) 0.67244(12) 0.0371(4) Uani 1 1 d . . . . .
H32A H 0.545071 0.582691 0.637558 0.056 Uiso 1 1 calc R U . . .
H32B H 0.553417 0.574671 0.722987 0.056 Uiso 1 1 calc R U . . .
H32C H 0.434426 0.624659 0.666636 0.056 Uiso 1 1 calc R U . . .
C33 C 0.32846(16) 0.48878(12) 0.57925(9) 0.0324(4) Uani 1 1 d . . . . .
H33A H 0.374928 0.499159 0.543154 0.049 Uiso 1 1 calc R U . . .
H33B H 0.268496 0.538776 0.576898 0.049 Uiso 1 1 calc R U . . .
H33C H 0.281318 0.431472 0.568003 0.049 Uiso 1 1 calc R U . . .
C34 C 0.34781(16) 0.47026(12) 0.71234(10) 0.0326(4) Uani 1 1 d . . . . .
H34A H 0.292997 0.523097 0.711164 0.049 Uiso 1 1 calc R U . . .
H34B H 0.407203 0.463293 0.762087 0.049 Uiso 1 1 calc R U . . .
H34C H 0.294969 0.415636 0.699170 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
Ge1 C9 2.4894(15) . ?
C1 C2 1.413(2) . ?
C1 C9 1.419(2) . ?
C2 C3 1.4382(19) . ?
C2 C14 1.5222(19) . ?
C3 C4 1.417(2) . ?
C3 C8 1.440(2) . ?
C4 C5 1.365(2) . ?
C5 C6 1.407(3) . ?
C7 C6 1.366(3) . ?
C7 C8 1.419(2) . ?
C9 C8 1.440(2) . ?
C9 C10 1.525(2) . ?
C10 C11 1.529(3) . ?
C10 C12 1.533(2) . ?
C10 C13 1.542(2) . ?
C14 C15 1.523(2) . ?
C14 C16 1.530(2) . ?
C14 C17 1.538(2) . ?
C18 C19 1.4071(19) . ?
C18 C26 1.4187(19) . ?
C19 C20 1.4419(19) . ?
C19 C31 1.5182(19) . ?
C20 C21 1.421(2) . ?
C20 C25 1.4413(19) . ?
C21 C22 1.369(2) . ?
C22 C23 1.411(2) . ?
C23 C24 1.368(2) . ?
C24 C25 1.4198(19) . ?
C25 C26 1.4409(19) . ?
C26 C27 1.5196(19) . ?
C27 C30 1.530(2) . ?
C27 C28 1.532(2) . ?
C27 C29 1.538(2) . ?
C31 C34 1.533(2) . ?
C31 C33 1.533(2) . ?
C31 C32 1.538(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
C2 C1 C9 111.58(13) . . ?
C1 C2 C3 105.94(12) . . ?
C1 C2 C14 126.40(13) . . ?
C3 C2 C14 127.25(12) . . ?
C4 C3 C2 132.38(14) . . ?
C4 C3 C8 119.30(13) . . ?
C2 C3 C8 108.31(12) . . ?
C5 C4 C3 119.52(16) . . ?
C4 C5 C6 121.32(16) . . ?
C6 C7 C8 119.59(15) . . ?
C7 C6 C5 121.19(15) . . ?
C1 C9 C8 105.78(12) . . ?
C1 C9 C10 126.51(14) . . ?
C8 C9 C10 126.80(14) . . ?
C1 C9 Ge1 73.73(8) . . ?
C8 C9 Ge1 78.11(8) . . ?
C10 C9 Ge1 122.06(10) . . ?
C7 C8 C9 132.72(14) . . ?
C7 C8 C3 119.09(14) . . ?
C9 C8 C3 108.19(12) . . ?
C9 C10 C11 110.58(14) . . ?
C9 C10 C12 111.87(13) . . ?
C11 C10 C12 107.66(15) . . ?
C9 C10 C13 108.97(13) . . ?
C11 C10 C13 108.36(15) . . ?
C12 C10 C13 109.31(15) . . ?
C2 C14 C15 110.93(13) . . ?
C2 C14 C16 111.36(12) . . ?
C15 C14 C16 107.30(14) . . ?
C2 C14 C17 109.07(12) . . ?
C15 C14 C17 108.63(14) . . ?
C16 C14 C17 109.50(14) . . ?
C19 C18 C26 111.55(12) . . ?
C18 C19 C20 106.27(12) . . ?
C18 C19 C31 126.18(13) . . ?
C20 C19 C31 127.24(12) . . ?
C21 C20 C25 119.07(13) . . ?
C21 C20 C19 132.95(13) . . ?
C25 C20 C19 107.98(12) . . ?
C22 C21 C20 119.55(14) . . ?
C21 C22 C23 121.22(14) . . ?
C24 C23 C22 121.15(14) . . ?
C23 C24 C25 119.57(14) . . ?
C24 C25 C26 132.46(13) . . ?
C24 C25 C20 119.33(13) . . ?
C26 C25 C20 108.17(12) . . ?
C18 C26 C25 105.81(12) . . ?
C18 C26 C27 125.96(12) . . ?
C25 C26 C27 126.92(12) . . ?
C26 C27 C30 111.25(12) . . ?
C26 C27 C28 110.60(12) . . ?
C30 C27 C28 107.92(13) . . ?
C26 C27 C29 108.93(12) . . ?
C30 C27 C29 109.92(13) . . ?
C28 C27 C29 108.18(13) . . ?
C19 C31 C34 110.74(12) . . ?
C19 C31 C33 110.85(12) . . ?
C34 C31 C33 108.31(13) . . ?
C19 C31 C32 109.24(12) . . ?
C34 C31 C32 109.72(14) . . ?
C33 C31 C32 107.94(14) . . ?

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
C9 C1 C2 C3 4.21(16) . . . . ?
C9 C1 C2 C14 177.35(13) . . . . ?
C1 C2 C3 C4 176.73(15) . . . . ?
C14 C2 C3 C4 3.7(3) . . . . ?
C1 C2 C3 C8 -2.11(15) . . . . ?
C14 C2 C3 C8 -175.17(13) . . . . ?
C2 C3 C4 C5 -178.55(16) . . . . ?
C8 C3 C4 C5 0.2(2) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C8 C7 C6 C5 -0.1(2) . . . . ?
C4 C5 C6 C7 0.1(3) . . . . ?
C2 C1 C9 C8 -4.59(16) . . . . ?
C2 C1 C9 C10 -174.22(13) . . . . ?
C2 C1 C9 Ge1 67.62(10) . . . . ?
C6 C7 C8 C9 179.44(15) . . . . ?
C6 C7 C8 C3 0.1(2) . . . . ?
C1 C9 C8 C7 -176.29(15) . . . . ?
C10 C9 C8 C7 -6.7(3) . . . . ?
Ge1 C9 C8 C7 114.62(17) . . . . ?
C1 C9 C8 C3 3.10(15) . . . . ?
C10 C9 C8 C3 172.69(13) . . . . ?
Ge1 C9 C8 C3 -65.99(10) . . . . ?
C4 C3 C8 C7 -0.2(2) . . . . ?
C2 C3 C8 C7 178.85(13) . . . . ?
C4 C3 C8 C9 -179.65(13) . . . . ?
C2 C3 C8 C9 -0.63(16) . . . . ?
C1 C9 C10 C11 -11.2(2) . . . . ?
C8 C9 C10 C11 -178.65(14) . . . . ?
Ge1 C9 C10 C11 81.85(15) . . . . ?
C1 C9 C10 C12 -131.16(17) . . . . ?
C8 C9 C10 C12 61.3(2) . . . . ?
Ge1 C9 C10 C12 -38.15(19) . . . . ?
C1 C9 C10 C13 107.86(18) . . . . ?
C8 C9 C10 C13 -59.6(2) . . . . ?
Ge1 C9 C10 C13 -159.14(12) . . . . ?
C1 C2 C14 C15 10.6(2) . . . . ?
C3 C2 C14 C15 -177.67(15) . . . . ?
C1 C2 C14 C16 130.06(15) . . . . ?
C3 C2 C14 C16 -58.24(19) . . . . ?
C1 C2 C14 C17 -108.99(17) . . . . ?
C3 C2 C14 C17 62.72(19) . . . . ?
C26 C18 C19 C20 3.51(16) . . . . ?
C26 C18 C19 C31 177.45(13) . . . . ?
C18 C19 C20 C21 178.82(15) . . . . ?
C31 C19 C20 C21 5.0(3) . . . . ?
C18 C19 C20 C25 -0.65(15) . . . . ?
C31 C19 C20 C25 -174.51(13) . . . . ?
C25 C20 C21 C22 3.4(2) . . . . ?
C19 C20 C21 C22 -176.04(15) . . . . ?
C20 C21 C22 C23 -0.9(2) . . . . ?
C21 C22 C23 C24 -1.5(2) . . . . ?
C22 C23 C24 C25 1.1(2) . . . . ?
C23 C24 C25 C26 179.12(15) . . . . ?
C23 C24 C25 C20 1.4(2) . . . . ?
C21 C20 C25 C24 -3.7(2) . . . . ?
C19 C20 C25 C24 175.87(12) . . . . ?
C21 C20 C25 C26 178.12(12) . . . . ?
C19 C20 C25 C26 -2.33(15) . . . . ?
C19 C18 C26 C25 -4.92(16) . . . . ?
C19 C18 C26 C27 -172.57(13) . . . . ?
C24 C25 C26 C18 -173.53(15) . . . . ?
C20 C25 C26 C18 4.34(15) . . . . ?
C24 C25 C26 C27 -6.0(3) . . . . ?
C20 C25 C26 C27 171.83(13) . . . . ?
C18 C26 C27 C30 -135.80(15) . . . . ?
C25 C26 C27 C30 59.12(19) . . . . ?
C18 C26 C27 C28 -15.9(2) . . . . ?
C25 C26 C27 C28 179.04(14) . . . . ?
C18 C26 C27 C29 102.89(16) . . . . ?
C25 C26 C27 C29 -62.20(18) . . . . ?
C18 C19 C31 C34 123.71(16) . . . . ?
C20 C19 C31 C34 -63.60(19) . . . . ?
C18 C19 C31 C33 3.5(2) . . . . ?
C20 C19 C31 C33 176.16(14) . . . . ?
C18 C19 C31 C32 -115.34(16) . . . . ?
C20 C19 C31 C32 57.4(2) . . . . ?

_refine_diff_density_max         0.312
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.046



_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_sh4749_a
_database_code_depnum_ccdc_archive 'CCDC 2154216'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Saarland University
Germany
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        bis(di-tert-butylindenyl)plumbocene
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H46 Pb'
_chemical_formula_sum            'C34 H46 Pb'
_chemical_formula_weight         661.90

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'
Pb Pb -3.3944 10.1111 '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                   11.1603(4)
_cell_length_b                   14.9272(5)
_cell_length_c                   18.8917(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.1980(10)
_cell_angle_gamma                90
_cell_volume                     3022.27(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9959
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      28.71

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.092
_exptl_absorpt_coefficient_mu    5.601
_shelx_estimated_absorpt_T_min   0.491
_shelx_estimated_absorpt_T_max   0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6242
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50956
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.245
_diffrn_reflns_theta_max         28.725
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7815
_reflns_number_gt                6262
_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       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0097P)²+2.0099P] 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         7815
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0408
_refine_ls_wR_factor_gt          0.0377
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
Pb1 Pb 0.50133(2) 0.75240(2) 0.30428(2) 0.01965(3) Uani 1 1 d . . . . .
C1 C 0.56990(19) 0.92262(13) 0.27958(11) 0.0184(4) Uani 1 1 d . . . . .
H1 H 0.521546 0.969935 0.291064 0.022 Uiso 1 1 calc R U . . .
C2 C 0.54562(19) 0.88169(13) 0.20991(11) 0.0178(4) Uani 1 1 d . . . . .
C3 C 0.64426(19) 0.81829(14) 0.21461(12) 0.0200(4) Uani 1 1 d . . . . .
C4 C 0.6731(2) 0.75975(16) 0.16287(14) 0.0298(5) Uani 1 1 d . . . . .
H4 H 0.621867 0.758166 0.113417 0.036 Uiso 1 1 calc R U . . .
C5 C 0.7764(2) 0.70493(17) 0.18484(17) 0.0376(6) Uani 1 1 d . . . . .
H5 H 0.795789 0.665640 0.150022 0.045 Uiso 1 1 calc R U . . .
C6 C 0.8534(2) 0.70607(17) 0.25759(17) 0.0367(6) Uani 1 1 d . . . . .
H6 H 0.923019 0.666742 0.271331 0.044 Uiso 1 1 calc R U . . .
C7 C 0.8303(2) 0.76262(16) 0.30894(15) 0.0314(5) Uani 1 1 d . . . . .
H7 H 0.884558 0.763523 0.357622 0.038 Uiso 1 1 calc R U . . .
C8 C 0.72489(19) 0.82006(14) 0.28949(12) 0.0219(4) Uani 1 1 d . . . . .
C9 C 0.67576(19) 0.88429(14) 0.33054(12) 0.0207(4) Uani 1 1 d . . . . .
C10 C 0.7336(2) 0.91613(16) 0.40935(13) 0.0297(5) Uani 1 1 d . . . . .
C11 C 0.8558(3) 0.9656(2) 0.41304(16) 0.0476(8) Uani 1 1 d . . . . .
H11A H 0.914192 0.924437 0.399485 0.071 Uiso 1 1 calc R U . . .
H11B H 0.892716 0.987657 0.463267 0.071 Uiso 1 1 calc R U . . .
H11C H 0.838590 1.016289 0.378708 0.071 Uiso 1 1 calc R U . . .
C12 C 0.6455(3) 0.98022(17) 0.43341(14) 0.0370(6) Uani 1 1 d . . . . .
H12A H 0.567122 0.949290 0.431232 0.056 Uiso 1 1 calc R U . . .
H12B H 0.628451 1.032191 0.400415 0.056 Uiso 1 1 calc R U . . .
H12C H 0.684541 1.000259 0.484001 0.056 Uiso 1 1 calc R U . . .
C13 C 0.7610(3) 0.83765(19) 0.46427(14) 0.0440(7) Uani 1 1 d . . . . .
H13A H 0.815316 0.794232 0.449429 0.066 Uiso 1 1 calc R U . . .
H13B H 0.682555 0.808479 0.464656 0.066 Uiso 1 1 calc R U . . .
H13C H 0.802721 0.860234 0.513725 0.066 Uiso 1 1 calc R U . . .
C14 C 0.4402(2) 0.90634(14) 0.14180(11) 0.0215(4) Uani 1 1 d . . . . .
C15 C 0.3534(2) 0.97447(17) 0.16110(14) 0.0314(5) Uani 1 1 d . . . . .
H15A H 0.320722 0.950439 0.200279 0.047 Uiso 1 1 calc R U . . .
H15B H 0.284020 0.987053 0.117384 0.047 Uiso 1 1 calc R U . . .
H15C H 0.399471 1.029926 0.178108 0.047 Uiso 1 1 calc R U . . .
C16 C 0.4962(2) 0.94737(19) 0.08367(14) 0.0372(6) Uani 1 1 d . . . . .
H16A H 0.550618 0.903391 0.069620 0.056 Uiso 1 1 calc R U . . .
H16B H 0.544847 1.000670 0.104123 0.056 Uiso 1 1 calc R U . . .
H16C H 0.428808 0.964243 0.040122 0.056 Uiso 1 1 calc R U . . .
C17 C 0.3623(2) 0.82361(17) 0.10919(14) 0.0348(6) Uani 1 1 d . . . . .
H17A H 0.416913 0.777479 0.098164 0.052 Uiso 1 1 calc R U . . .
H17B H 0.299019 0.840483 0.063751 0.052 Uiso 1 1 calc R U . . .
H17C H 0.321132 0.800107 0.144860 0.052 Uiso 1 1 calc R U . . .
C18 C 0.44055(18) 0.63284(13) 0.39913(11) 0.0173(4) Uani 1 1 d . . . . .
H18 H 0.493669 0.631240 0.448117 0.021 Uiso 1 1 calc R U . . .
C19 C 0.33569(18) 0.69078(13) 0.37502(11) 0.0167(4) Uani 1 1 d . . . . .
C20 C 0.27775(18) 0.66691(13) 0.29932(11) 0.0160(4) Uani 1 1 d . . . . .
C21 C 0.16688(19) 0.69609(14) 0.24700(12) 0.0204(4) Uani 1 1 d . . . . .
H21 H 0.117375 0.741863 0.259625 0.025 Uiso 1 1 calc R U . . .
C22 C 0.1314(2) 0.65812(15) 0.17828(12) 0.0259(5) Uani 1 1 d . . . . .
H22 H 0.056519 0.677429 0.143775 0.031 Uiso 1 1 calc R U . . .
C23 C 0.2038(2) 0.59111(16) 0.15791(12) 0.0279(5) Uani 1 1 d . . . . .
H23 H 0.176940 0.565729 0.109960 0.034 Uiso 1 1 calc R U . . .
C24 C 0.3127(2) 0.56180(14) 0.20616(12) 0.0234(4) Uani 1 1 d . . . . .
H24 H 0.361698 0.517540 0.191172 0.028 Uiso 1 1 calc R U . . .
C25 C 0.35192(18) 0.59766(13) 0.27846(11) 0.0174(4) Uani 1 1 d . . . . .
C26 C 0.45593(18) 0.57822(13) 0.34155(11) 0.0174(4) Uani 1 1 d . . . . .
C27 C 0.5551(2) 0.50671(14) 0.34732(13) 0.0237(4) Uani 1 1 d . . . . .
C28 C 0.6274(2) 0.52097(18) 0.28984(15) 0.0366(6) Uani 1 1 d . . . . .
H28A H 0.685099 0.470916 0.292007 0.055 Uiso 1 1 calc R U . . .
H28B H 0.674561 0.577093 0.300359 0.055 Uiso 1 1 calc R U . . .
H28C H 0.568501 0.523989 0.240512 0.055 Uiso 1 1 calc R U . . .
C29 C 0.6490(2) 0.50783(17) 0.42390(14) 0.0334(6) Uani 1 1 d . . . . .
H29A H 0.605533 0.495854 0.461361 0.050 Uiso 1 1 calc R U . . .
H29B H 0.689230 0.566730 0.432902 0.050 Uiso 1 1 calc R U . . .
H29C H 0.712496 0.461637 0.426425 0.050 Uiso 1 1 calc R U . . .
C30 C 0.4924(2) 0.41389(15) 0.33560(15) 0.0340(6) Uani 1 1 d . . . . .
H30A H 0.450314 0.403124 0.373919 0.051 Uiso 1 1 calc R U . . .
H30B H 0.555931 0.367656 0.338404 0.051 Uiso 1 1 calc R U . . .
H30C H 0.431164 0.411802 0.287032 0.051 Uiso 1 1 calc R U . . .
C31 C 0.28434(19) 0.75263(14) 0.42336(11) 0.0219(4) Uani 1 1 d . . . . .
C32 C 0.2513(3) 0.84522(16) 0.38817(14) 0.0359(6) Uani 1 1 d . . . . .
H32A H 0.326834 0.873821 0.382041 0.054 Uiso 1 1 calc R U . . .
H32B H 0.215928 0.882412 0.420079 0.054 Uiso 1 1 calc R U . . .
H32C H 0.190095 0.838602 0.339908 0.054 Uiso 1 1 calc R U . . .
C33 C 0.3808(2) 0.76627(16) 0.49836(12) 0.0321(5) Uani 1 1 d . . . . .
H33A H 0.399190 0.708558 0.523815 0.048 Uiso 1 1 calc R U . . .
H33B H 0.347222 0.807706 0.528266 0.048 Uiso 1 1 calc R U . . .
H33C H 0.457554 0.791240 0.490870 0.048 Uiso 1 1 calc R U . . .
C34 C 0.1671(2) 0.70966(18) 0.43673(14) 0.0328(5) Uani 1 1 d . . . . .
H34A H 0.132713 0.749622 0.467301 0.049 Uiso 1 1 calc R U . . .
H34B H 0.189351 0.652164 0.462022 0.049 Uiso 1 1 calc R U . . .
H34C H 0.104600 0.699839 0.389359 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
Pb1 C9 2.715(2) . ?
Pb1 C19 2.725(2) . ?
Pb1 C1 2.7311(19) . ?
Pb1 C18 2.745(2) . ?
Pb1 C2 2.764(2) . ?
Pb1 C26 2.7770(19) . ?
Pb1 C8 2.777(2) . ?
Pb1 C20 2.7808(19) . ?
Pb1 C3 2.809(2) . ?
Pb1 C25 2.8107(19) . ?
C1 C2 1.407(3) . ?
C1 C9 1.420(3) . ?
C2 C3 1.436(3) . ?
C2 C14 1.527(3) . ?
C3 C4 1.414(3) . ?
C3 C8 1.450(3) . ?
C4 C5 1.380(3) . ?
C5 C6 1.403(4) . ?
C6 C7 1.364(4) . ?
C7 C8 1.418(3) . ?
C8 C9 1.435(3) . ?
C9 C10 1.524(3) . ?
C10 C12 1.529(4) . ?
C10 C11 1.536(4) . ?
C10 C13 1.538(3) . ?
C14 C15 1.518(3) . ?
C14 C16 1.534(3) . ?
C14 C17 1.537(3) . ?
C18 C26 1.408(3) . ?
C18 C19 1.424(3) . ?
C19 C20 1.440(3) . ?
C19 C31 1.519(3) . ?
C20 C21 1.420(3) . ?
C20 C25 1.446(3) . ?
C21 C22 1.370(3) . ?
C22 C23 1.405(3) . ?
C23 C24 1.371(3) . ?
C24 C25 1.418(3) . ?
C25 C26 1.442(3) . ?
C26 C27 1.519(3) . ?
C27 C29 1.532(3) . ?
C27 C28 1.538(3) . ?
C27 C30 1.540(3) . ?
C31 C32 1.533(3) . ?
C31 C33 1.535(3) . ?
C31 C34 1.540(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
C9 Pb1 C19 134.82(6) . . ?
C9 Pb1 C1 30.22(6) . . ?
C19 Pb1 C1 131.19(6) . . ?
C9 Pb1 C18 130.34(6) . . ?
C19 Pb1 C18 30.17(6) . . ?
C1 Pb1 C18 148.05(6) . . ?
C9 Pb1 C2 50.46(6) . . ?
C19 Pb1 C2 145.06(6) . . ?
C1 Pb1 C2 29.67(6) . . ?
C18 Pb1 C2 175.09(6) . . ?
C9 Pb1 C26 143.59(6) . . ?
C19 Pb1 C26 50.43(6) . . ?
C1 Pb1 C26 173.74(6) . . ?
C18 Pb1 C26 29.53(6) . . ?
C2 Pb1 C26 153.56(6) . . ?
C9 Pb1 C8 30.26(6) . . ?
C19 Pb1 C8 157.43(6) . . ?
C1 Pb1 C8 48.85(6) . . ?
C18 Pb1 C8 134.00(6) . . ?
C2 Pb1 C8 49.74(6) . . ?
C26 Pb1 C8 126.77(6) . . ?
C9 Pb1 C20 158.39(6) . . ?
C19 Pb1 C20 30.31(6) . . ?
C1 Pb1 C20 135.46(6) . . ?
C18 Pb1 C20 48.76(6) . . ?
C2 Pb1 C20 128.24(6) . . ?
C26 Pb1 C20 49.72(6) . . ?
C8 Pb1 C20 170.54(6) . . ?
C9 Pb1 C3 50.02(6) . . ?
C19 Pb1 C3 172.28(6) . . ?
C1 Pb1 C3 48.53(6) . . ?
C18 Pb1 C3 155.06(6) . . ?
C2 Pb1 C3 29.84(6) . . ?
C26 Pb1 C3 130.94(6) . . ?
C8 Pb1 C3 30.08(6) . . ?
C20 Pb1 C3 142.71(6) . . ?
C9 Pb1 C25 171.10(6) . . ?
C19 Pb1 C25 49.99(6) . . ?
C1 Pb1 C25 156.33(6) . . ?
C18 Pb1 C25 48.42(6) . . ?
C2 Pb1 C25 131.77(6) . . ?
C26 Pb1 C25 29.91(6) . . ?
C8 Pb1 C25 141.96(6) . . ?
C20 Pb1 C25 29.97(6) . . ?
C3 Pb1 C25 126.32(6) . . ?
C2 C1 C9 111.47(18) . . ?
C2 C1 Pb1 76.46(11) . . ?
C9 C1 Pb1 74.28(11) . . ?
C1 C2 C3 106.51(18) . . ?
C1 C2 C14 125.86(19) . . ?
C3 C2 C14 127.47(19) . . ?
C1 C2 Pb1 73.87(12) . . ?
C3 C2 Pb1 76.81(12) . . ?
C14 C2 Pb1 118.53(13) . . ?
C4 C3 C2 133.1(2) . . ?
C4 C3 C8 119.1(2) . . ?
C2 C3 C8 107.75(18) . . ?
C4 C3 Pb1 118.55(14) . . ?
C2 C3 Pb1 73.35(12) . . ?
C8 C3 Pb1 73.75(12) . . ?
C5 C4 C3 119.4(2) . . ?
C4 C5 C6 121.3(2) . . ?
C7 C6 C5 121.2(2) . . ?
C6 C7 C8 119.9(2) . . ?
C7 C8 C9 132.7(2) . . ?
C7 C8 C3 119.1(2) . . ?
C9 C8 C3 108.23(18) . . ?
C7 C8 Pb1 117.21(14) . . ?
C9 C8 Pb1 72.49(11) . . ?
C3 C8 Pb1 76.17(11) . . ?
C1 C9 C8 105.90(18) . . ?
C1 C9 C10 125.6(2) . . ?
C8 C9 C10 127.94(19) . . ?
C1 C9 Pb1 75.50(11) . . ?
C8 C9 Pb1 77.25(12) . . ?
C10 C9 Pb1 119.42(14) . . ?
C9 C10 C12 110.69(19) . . ?
C9 C10 C11 108.8(2) . . ?
C12 C10 C11 108.8(2) . . ?
C9 C10 C13 111.8(2) . . ?
C12 C10 C13 107.4(2) . . ?
C11 C10 C13 109.2(2) . . ?
C15 C14 C2 110.63(18) . . ?
C15 C14 C16 108.6(2) . . ?
C2 C14 C16 109.14(18) . . ?
C15 C14 C17 107.87(19) . . ?
C2 C14 C17 111.17(18) . . ?
C16 C14 C17 109.4(2) . . ?
C26 C18 C19 111.79(17) . . ?
C26 C18 Pb1 76.50(12) . . ?
C19 C18 Pb1 74.16(11) . . ?
C18 C19 C20 105.58(17) . . ?
C18 C19 C31 126.24(17) . . ?
C20 C19 C31 127.38(18) . . ?
C18 C19 Pb1 75.67(11) . . ?
C20 C19 Pb1 76.97(11) . . ?
C31 C19 Pb1 120.73(13) . . ?
C21 C20 C19 132.70(19) . . ?
C21 C20 C25 118.92(18) . . ?
C19 C20 C25 108.35(17) . . ?
C21 C20 Pb1 118.84(13) . . ?
C19 C20 Pb1 72.72(11) . . ?
C25 C20 Pb1 76.16(11) . . ?
C22 C21 C20 119.9(2) . . ?
C21 C22 C23 121.2(2) . . ?
C24 C23 C22 121.0(2) . . ?
C23 C24 C25 119.9(2) . . ?
C24 C25 C26 132.94(19) . . ?
C24 C25 C20 119.08(18) . . ?
C26 C25 C20 107.97(17) . . ?
C24 C25 Pb1 119.10(14) . . ?
C26 C25 Pb1 73.75(11) . . ?
C20 C25 Pb1 73.87(11) . . ?
C18 C26 C25 106.17(17) . . ?
C18 C26 C27 126.50(18) . . ?
C25 C26 C27 127.07(18) . . ?
C18 C26 Pb1 73.97(11) . . ?
C25 C26 Pb1 76.34(11) . . ?
C27 C26 Pb1 119.69(13) . . ?
C26 C27 C29 110.68(18) . . ?
C26 C27 C28 111.54(18) . . ?
C29 C27 C28 108.0(2) . . ?
C26 C27 C30 109.24(18) . . ?
C29 C27 C30 108.02(19) . . ?
C28 C27 C30 109.2(2) . . ?
C19 C31 C32 111.88(18) . . ?
C19 C31 C33 110.51(17) . . ?
C32 C31 C33 107.60(19) . . ?
C19 C31 C34 109.01(18) . . ?
C32 C31 C34 109.52(19) . . ?
C33 C31 C34 108.24(19) . . ?

_refine_diff_density_max         0.358
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.076



_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_sh4628_a
_database_code_depnum_ccdc_archive 'CCDC 2154215'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Saarland University
Germany
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        bis(di-tert-butylindenyl)stannocene
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H46 Sn'
_chemical_formula_sum            'C34 H46 Sn'
_chemical_formula_weight         573.40

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'
Sn Sn -0.6537 1.4246 '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                   11.0857(3)
_cell_length_b                   14.8512(4)
_cell_length_c                   18.8414(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.5710(10)
_cell_angle_gamma                90
_cell_volume                     2988.12(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9672
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      30.48

_exptl_crystal_description       cuboid
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.137
_exptl_absorpt_coefficient_mu    0.874
_shelx_estimated_absorpt_T_min   0.822
_shelx_estimated_absorpt_T_max   0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            64683
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.244
_diffrn_reflns_theta_max         30.524
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9129
_reflns_number_gt                7508
_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       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0171P)²+1.5543P] 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         9129
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0527
_refine_ls_wR_factor_gt          0.0488
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Sn1 Sn 0.50095(2) 0.75210(2) 0.30391(2) 0.01763(3) Uani 1 1 d . . . . .
C1 C 0.56621(12) 0.92081(8) 0.28111(7) 0.0172(2) Uani 1 1 d . . . . .
H1 H 0.517386 0.968306 0.292751 0.021 Uiso 1 1 calc R U . . .
C2 C 0.67142(12) 0.88191(9) 0.33180(7) 0.0191(2) Uani 1 1 d . . . . .
C3 C 0.72277(12) 0.81789(9) 0.29057(8) 0.0201(3) Uani 1 1 d . . . . .
C4 C 0.82915(13) 0.76059(10) 0.30992(9) 0.0285(3) Uani 1 1 d . . . . .
H4 H 0.882664 0.761219 0.358645 0.034 Uiso 1 1 calc R U . . .
C5 C 0.85407(14) 0.70476(11) 0.25832(10) 0.0332(4) Uani 1 1 d . . . . .
H5 H 0.924573 0.665859 0.271777 0.040 Uiso 1 1 calc R U . . .
C7 C 0.67386(15) 0.75793(10) 0.16401(9) 0.0267(3) Uani 1 1 d . . . . .
H7 H 0.622997 0.756285 0.114629 0.032 Uiso 1 1 calc R U . . .
C6 C 0.77747(16) 0.70351(11) 0.18545(10) 0.0334(4) Uani 1 1 d . . . . .
H6 H 0.797781 0.664350 0.150485 0.040 Uiso 1 1 calc R U . . .
C8 C 0.64326(12) 0.81643(9) 0.21583(7) 0.0187(2) Uani 1 1 d . . . . .
C9 C 0.54317(12) 0.87985(8) 0.21090(7) 0.0164(2) Uani 1 1 d . . . . .
C10 C 0.43956(13) 0.90497(9) 0.14295(7) 0.0200(3) Uani 1 1 d . . . . .
C11 C 0.49761(16) 0.94772(12) 0.08564(9) 0.0341(4) Uani 1 1 d . . . . .
H11A H 0.430893 0.965596 0.042289 0.051 Uiso 1 1 calc R U . . .
H11B H 0.552673 0.903972 0.071057 0.051 Uiso 1 1 calc R U . . .
H11C H 0.546318 1.000894 0.107000 0.051 Uiso 1 1 calc R U . . .
C12 C 0.35089(14) 0.97327(11) 0.16238(9) 0.0294(3) Uani 1 1 d . . . . .
H12A H 0.284336 0.988266 0.118060 0.044 Uiso 1 1 calc R U . . .
H12B H 0.397503 1.027939 0.182004 0.044 Uiso 1 1 calc R U . . .
H12C H 0.313811 0.947523 0.199552 0.044 Uiso 1 1 calc R U . . .
C13 C 0.36191(15) 0.82222(11) 0.10933(9) 0.0325(3) Uani 1 1 d . . . . .
H13A H 0.300242 0.839601 0.063589 0.049 Uiso 1 1 calc R U . . .
H13B H 0.318496 0.798417 0.144276 0.049 Uiso 1 1 calc R U . . .
H13C H 0.417471 0.775845 0.098663 0.049 Uiso 1 1 calc R U . . .
C14 C 0.72848(14) 0.91389(10) 0.41065(8) 0.0260(3) Uani 1 1 d . . . . .
C15 C 0.85160(17) 0.96401(13) 0.41408(10) 0.0414(4) Uani 1 1 d . . . . .
H15A H 0.887483 0.986785 0.464125 0.062 Uiso 1 1 calc R U . . .
H15B H 0.834684 1.014546 0.379367 0.062 Uiso 1 1 calc R U . . .
H15C H 0.910948 0.922574 0.400929 0.062 Uiso 1 1 calc R U . . .
C16 C 0.63920(16) 0.97824(11) 0.43449(8) 0.0315(3) Uani 1 1 d . . . . .
H16A H 0.677315 0.998461 0.485057 0.047 Uiso 1 1 calc R U . . .
H16B H 0.560311 0.947119 0.432242 0.047 Uiso 1 1 calc R U . . .
H16C H 0.622701 1.030432 0.401457 0.047 Uiso 1 1 calc R U . . .
C17 C 0.75558(18) 0.83487(12) 0.46540(9) 0.0375(4) Uani 1 1 d . . . . .
H17A H 0.794095 0.857739 0.515115 0.056 Uiso 1 1 calc R U . . .
H17B H 0.812852 0.792457 0.451343 0.056 Uiso 1 1 calc R U . . .
H17C H 0.677049 0.804078 0.464622 0.056 Uiso 1 1 calc R U . . .
C18 C 0.44231(12) 0.63583(8) 0.39872(7) 0.0168(2) Uani 1 1 d . . . . .
H18 H 0.495004 0.634595 0.447651 0.020 Uiso 1 1 calc R U . . .
C19 C 0.45904(12) 0.58032(8) 0.34104(7) 0.0166(2) Uani 1 1 d . . . . .
C20 C 0.35485(12) 0.59962(8) 0.27856(7) 0.0161(2) Uani 1 1 d . . . . .
C21 C 0.31595(13) 0.56267(9) 0.20646(7) 0.0221(3) Uani 1 1 d . . . . .
H21 H 0.365344 0.517937 0.191568 0.027 Uiso 1 1 calc R U . . .
C22 C 0.20694(14) 0.59175(10) 0.15846(8) 0.0254(3) Uani 1 1 d . . . . .
H22 H 0.180601 0.566001 0.110623 0.030 Uiso 1 1 calc R U . . .
C23 C 0.13311(13) 0.65930(10) 0.17885(8) 0.0242(3) Uani 1 1 d . . . . .
H23 H 0.057850 0.678180 0.144579 0.029 Uiso 1 1 calc R U . . .
C24 C 0.16834(12) 0.69804(9) 0.24731(7) 0.0196(2) Uani 1 1 d . . . . .
H24 H 0.118511 0.744141 0.260035 0.024 Uiso 1 1 calc R U . . .
C25 C 0.27983(12) 0.66894(8) 0.29924(7) 0.0156(2) Uani 1 1 d . . . . .
C26 C 0.33733(12) 0.69351(8) 0.37457(7) 0.0160(2) Uani 1 1 d . . . . .
C27 C 0.28422(13) 0.75500(9) 0.42325(7) 0.0205(2) Uani 1 1 d . . . . .
C28 C 0.24975(17) 0.84800(10) 0.38829(9) 0.0330(4) Uani 1 1 d . . . . .
H28A H 0.213155 0.884768 0.420390 0.050 Uiso 1 1 calc R U . . .
H28B H 0.188859 0.841074 0.340142 0.050 Uiso 1 1 calc R U . . .
H28C H 0.325229 0.877579 0.381990 0.050 Uiso 1 1 calc R U . . .
C29 C 0.37963(16) 0.76890(11) 0.49809(8) 0.0302(3) Uani 1 1 d . . . . .
H29A H 0.344767 0.810065 0.528105 0.045 Uiso 1 1 calc R U . . .
H29B H 0.456683 0.794657 0.490615 0.045 Uiso 1 1 calc R U . . .
H29C H 0.398442 0.710858 0.523390 0.045 Uiso 1 1 calc R U . . .
C30 C 0.16677(15) 0.71068(12) 0.43651(9) 0.0313(3) Uani 1 1 d . . . . .
H30A H 0.130727 0.750417 0.466964 0.047 Uiso 1 1 calc R U . . .
H30B H 0.189664 0.653041 0.461875 0.047 Uiso 1 1 calc R U . . .
H30C H 0.105084 0.700329 0.389128 0.047 Uiso 1 1 calc R U . . .
C31 C 0.55810(13) 0.50803(9) 0.34717(8) 0.0217(3) Uani 1 1 d . . . . .
C32 C 0.63062(15) 0.52075(11) 0.28884(9) 0.0333(3) Uani 1 1 d . . . . .
H32A H 0.689508 0.470776 0.291866 0.050 Uiso 1 1 calc R U . . .
H32B H 0.676933 0.577683 0.297798 0.050 Uiso 1 1 calc R U . . .
H32C H 0.571631 0.521915 0.239694 0.050 Uiso 1 1 calc R U . . .
C34 C 0.65215(15) 0.51016(11) 0.42329(9) 0.0332(3) Uani 1 1 d . . . . .
H34A H 0.715685 0.463464 0.425994 0.050 Uiso 1 1 calc R U . . .
H34B H 0.608302 0.499066 0.461212 0.050 Uiso 1 1 calc R U . . .
H34C H 0.692683 0.569324 0.431409 0.050 Uiso 1 1 calc R U . . .
C33 C 0.49459(16) 0.41489(10) 0.33697(10) 0.0327(3) Uani 1 1 d . . . . .
H33A H 0.557982 0.368061 0.339795 0.049 Uiso 1 1 calc R U . . .
H33B H 0.432933 0.412244 0.288768 0.049 Uiso 1 1 calc R U . . .
H33C H 0.452443 0.405128 0.375877 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
Sn1 C2 2.6516(13) . ?
Sn1 C26 2.6676(13) . ?
C1 C9 1.4154(17) . ?
C1 C2 1.4171(18) . ?
C2 C3 1.4385(19) . ?
C2 C14 1.5258(19) . ?
C3 C4 1.4202(19) . ?
C3 C8 1.4470(19) . ?
C4 C5 1.361(2) . ?
C5 C6 1.407(3) . ?
C7 C6 1.374(2) . ?
C7 C8 1.4147(19) . ?
C8 C9 1.4392(18) . ?
C9 C10 1.5192(18) . ?
C10 C12 1.524(2) . ?
C10 C11 1.535(2) . ?
C10 C13 1.536(2) . ?
C14 C16 1.528(2) . ?
C14 C17 1.538(2) . ?
C14 C15 1.541(2) . ?
C18 C19 1.4152(18) . ?
C18 C26 1.4181(17) . ?
C19 C20 1.4396(18) . ?
C19 C31 1.5179(18) . ?
C20 C21 1.4205(18) . ?
C20 C25 1.4413(17) . ?
C21 C22 1.370(2) . ?
C22 C23 1.412(2) . ?
C23 C24 1.3700(19) . ?
C24 C25 1.4221(17) . ?
C25 C26 1.4382(17) . ?
C26 C27 1.5205(18) . ?
C27 C29 1.533(2) . ?
C27 C28 1.5338(19) . ?
C27 C30 1.538(2) . ?
C31 C34 1.530(2) . ?
C31 C32 1.537(2) . ?
C31 C33 1.540(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
C2 Sn1 C26 133.01(4) . . ?
C9 C1 C2 111.36(12) . . ?
C1 C2 C3 106.19(11) . . ?
C1 C2 C14 125.49(12) . . ?
C3 C2 C14 127.65(12) . . ?
C1 C2 Sn1 75.46(7) . . ?
C3 C2 Sn1 77.10(7) . . ?
C14 C2 Sn1 120.43(9) . . ?
C4 C3 C2 132.78(13) . . ?
C4 C3 C8 119.20(13) . . ?
C2 C3 C8 108.03(11) . . ?
C5 C4 C3 119.69(15) . . ?
C4 C5 C6 121.32(14) . . ?
C6 C7 C8 119.67(15) . . ?
C7 C6 C5 121.14(15) . . ?
C7 C8 C9 132.91(13) . . ?
C7 C8 C3 118.98(13) . . ?
C9 C8 C3 108.10(11) . . ?
C1 C9 C8 106.16(11) . . ?
C1 C9 C10 126.02(12) . . ?
C8 C9 C10 127.62(12) . . ?
C9 C10 C12 110.58(11) . . ?
C9 C10 C11 109.24(12) . . ?
C12 C10 C11 108.23(12) . . ?
C9 C10 C13 111.37(11) . . ?
C12 C10 C13 107.78(12) . . ?
C11 C10 C13 109.58(12) . . ?
C2 C14 C16 110.43(12) . . ?
C2 C14 C17 111.77(12) . . ?
C16 C14 C17 107.79(13) . . ?
C2 C14 C15 108.80(13) . . ?
C16 C14 C15 108.78(13) . . ?
C17 C14 C15 109.22(14) . . ?
C19 C18 C26 111.77(11) . . ?
C18 C19 C20 105.68(11) . . ?
C18 C19 C31 126.50(12) . . ?
C20 C19 C31 127.47(11) . . ?
C21 C20 C19 132.54(12) . . ?
C21 C20 C25 119.04(12) . . ?
C19 C20 C25 108.40(11) . . ?
C22 C21 C20 119.80(13) . . ?
C21 C22 C23 121.15(13) . . ?
C24 C23 C22 121.01(13) . . ?
C23 C24 C25 119.71(13) . . ?
C24 C25 C26 132.46(12) . . ?
C24 C25 C20 119.28(11) . . ?
C26 C25 C20 108.24(11) . . ?
C18 C26 C25 105.76(11) . . ?
C18 C26 C27 125.92(11) . . ?
C25 C26 C27 127.37(11) . . ?
C18 C26 Sn1 75.39(7) . . ?
C25 C26 Sn1 76.75(7) . . ?
C27 C26 Sn1 122.03(8) . . ?
C26 C27 C29 110.64(11) . . ?
C26 C27 C28 111.96(11) . . ?
C29 C27 C28 107.74(12) . . ?
C26 C27 C30 108.82(11) . . ?
C29 C27 C30 108.27(12) . . ?
C28 C27 C30 109.33(13) . . ?
C19 C31 C34 110.70(12) . . ?
C19 C31 C32 111.41(11) . . ?
C34 C31 C32 108.18(13) . . ?
C19 C31 C33 109.18(11) . . ?
C34 C31 C33 108.00(12) . . ?
C32 C31 C33 109.30(13) . . ?

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
C9 C1 C2 C3 4.21(15) . . . . ?
C9 C1 C2 C14 175.37(12) . . . . ?
C9 C1 C2 Sn1 -67.40(9) . . . . ?
C1 C2 C3 C4 177.79(14) . . . . ?
C14 C2 C3 C4 6.9(2) . . . . ?
Sn1 C2 C3 C4 -111.77(15) . . . . ?
C1 C2 C3 C8 -2.65(14) . . . . ?
C14 C2 C3 C8 -173.55(13) . . . . ?
Sn1 C2 C3 C8 67.80(9) . . . . ?
C2 C3 C4 C5 178.93(15) . . . . ?
C8 C3 C4 C5 -0.6(2) . . . . ?
C3 C4 C5 C6 1.0(2) . . . . ?
C8 C7 C6 C5 0.1(2) . . . . ?
C4 C5 C6 C7 -0.8(2) . . . . ?
C6 C7 C8 C9 -179.62(14) . . . . ?
C6 C7 C8 C3 0.3(2) . . . . ?
C4 C3 C8 C7 -0.08(19) . . . . ?
C2 C3 C8 C7 -179.71(12) . . . . ?
C4 C3 C8 C9 179.89(12) . . . . ?
C2 C3 C8 C9 0.25(14) . . . . ?
C2 C1 C9 C8 -4.06(14) . . . . ?
C2 C1 C9 C10 -179.12(12) . . . . ?
C7 C8 C9 C1 -177.79(14) . . . . ?
C3 C8 C9 C1 2.25(14) . . . . ?
C7 C8 C9 C10 -2.8(2) . . . . ?
C3 C8 C9 C10 177.21(12) . . . . ?
C1 C9 C10 C12 -7.40(18) . . . . ?
C8 C9 C10 C12 178.59(13) . . . . ?
C1 C9 C10 C11 111.61(15) . . . . ?
C8 C9 C10 C11 -62.40(17) . . . . ?
C1 C9 C10 C13 -127.21(14) . . . . ?
C8 C9 C10 C13 58.78(18) . . . . ?
C1 C2 C14 C16 14.00(19) . . . . ?
C3 C2 C14 C16 -176.76(13) . . . . ?
Sn1 C2 C14 C16 -79.51(13) . . . . ?
C1 C2 C14 C17 133.98(15) . . . . ?
C3 C2 C14 C17 -56.77(19) . . . . ?
Sn1 C2 C14 C17 40.48(16) . . . . ?
C1 C2 C14 C15 -105.33(16) . . . . ?
C3 C2 C14 C15 63.92(18) . . . . ?
Sn1 C2 C14 C15 161.16(10) . . . . ?
C26 C18 C19 C20 -3.83(14) . . . . ?
C26 C18 C19 C31 -177.41(12) . . . . ?
C18 C19 C20 C21 -176.23(14) . . . . ?
C31 C19 C20 C21 -2.7(2) . . . . ?
C18 C19 C20 C25 2.07(14) . . . . ?
C31 C19 C20 C25 175.56(12) . . . . ?
C19 C20 C21 C22 176.68(14) . . . . ?
C25 C20 C21 C22 -1.47(19) . . . . ?
C20 C21 C22 C23 1.2(2) . . . . ?
C21 C22 C23 C24 0.1(2) . . . . ?
C22 C23 C24 C25 -1.1(2) . . . . ?
C23 C24 C25 C26 -177.16(13) . . . . ?
C23 C24 C25 C20 0.69(19) . . . . ?
C21 C20 C25 C24 0.56(18) . . . . ?
C19 C20 C25 C24 -178.01(11) . . . . ?
C21 C20 C25 C26 178.89(11) . . . . ?
C19 C20 C25 C26 0.32(14) . . . . ?
C19 C18 C26 C25 4.03(14) . . . . ?
C19 C18 C26 C27 173.47(12) . . . . ?
C19 C18 C26 Sn1 -67.32(9) . . . . ?
C24 C25 C26 C18 175.45(13) . . . . ?
C20 C25 C26 C18 -2.57(14) . . . . ?
C24 C25 C26 C27 6.2(2) . . . . ?
C20 C25 C26 C27 -171.80(12) . . . . ?
C24 C25 C26 Sn1 -114.17(14) . . . . ?
C20 C25 C26 Sn1 67.81(9) . . . . ?
C18 C26 C27 C29 16.97(19) . . . . ?
C25 C26 C27 C29 -175.87(13) . . . . ?
Sn1 C26 C27 C29 -77.95(13) . . . . ?
C18 C26 C27 C28 137.16(14) . . . . ?
C25 C26 C27 C28 -55.67(18) . . . . ?
Sn1 C26 C27 C28 42.24(15) . . . . ?
C18 C26 C27 C30 -101.87(15) . . . . ?
C25 C26 C27 C30 65.29(17) . . . . ?
Sn1 C26 C27 C30 163.21(9) . . . . ?
C18 C19 C31 C34 -7.64(19) . . . . ?
C20 C19 C31 C34 -179.84(13) . . . . ?
C18 C19 C31 C32 -128.07(14) . . . . ?
C20 C19 C31 C32 59.74(18) . . . . ?
C18 C19 C31 C33 111.12(15) . . . . ?
C20 C19 C31 C33 -61.07(18) . . . . ?

_refine_diff_density_max         0.362
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.057



_chemical_properties_physical    Air-sensitive,Moisture-sensitive
